# Electronic Supplementary Material (ESI) for Chemical Communications.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_100K
_database_code_depnum_ccdc_archive 'CCDC 2260940'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.727(3)
_cell_length_b                   21.727(3)
_cell_length_c                   21.727(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10257(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5433
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      31.00

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.531
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            147143
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         1.360
_diffrn_reflns_theta_max         27.836
_diffrn_reflns_theta_full        27.836
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             7555
_reflns_number_gt                7035
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.854
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with distance
 restraints and displacement parameters restraints.
 The anilate is disordered over two equivalent positions sharing the 
 coordinated C-O groups. The two components were refined with displacement
 parameters restraints as well as a FLAT restraint for the C atoms. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 948 cubic angstrom with a total of 167 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol (ca. 10 per cell). Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
 
 Details of SQUEEZE results (before refinement of BF4 disorder):

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.081  0.174  0.155       949       167 ' '
   2  0.120  0.380  0.620         7         0 ' '
   3  0.380  0.620  0.120         7         0 ' '
   4  0.620  0.120  0.380         7         0 ' '
   5  0.880  0.880  0.880         7         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?


 Details of SQUEEZE results on a 200 K data set of the same crystal
 after measurements up to 400 K:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.084  0.137  0.139      1771        72 ' '
   2  0.106  0.394  0.606        10         0 ' '
   3  0.394  0.606  0.106        10         0 ' '
   4  0.606  0.106  0.394        10         0 ' '
   5  0.894  0.894  0.894        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_100K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        948 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 948 cubic angstrom with a total of 167 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol (ca. 10 per cell). Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1986P)²+0.5140P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3015 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.080(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7555
_refine_ls_number_parameters     530
_refine_ls_number_restraints     245
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0837
_refine_ls_wR_factor_ref         0.2480
_refine_ls_wR_factor_gt          0.2413
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45535(3) 0.45535(3) 0.45535(3) 0.0874(4) Uani 1 3 d S T P . .
Fe2 Fe 0.17335(5) 0.17335(5) 0.17335(5) 0.1346(7) Uani 1 3 d S T P . .
N1 N 0.5153(2) 0.4210(2) 0.5156(2) 0.0951(10) Uani 1 1 d . . . . .
N2 N 0.4053(2) 0.3907(2) 0.4918(2) 0.0912(9) Uani 1 1 d . . . . .
N3 N 0.3451(2) 0.3734(2) 0.4892(2) 0.0961(11) Uani 1 1 d D . . . .
H3 H 0.319(4) 0.391(5) 0.463(4) 0.144 Uiso 1 1 d D U . . .
N4 N 0.1410(3) 0.2517(3) 0.2852(3) 0.1105(14) Uani 1 1 d D . . . .
H4 H 0.160(5) 0.241(6) 0.321(3) 0.166 Uiso 1 1 d D U . . .
N5 N 0.1370(3) 0.2363(4) 0.2259(3) 0.1213(17) Uani 1 1 d . . . . .
N6 N 0.1125(5) 0.2053(7) 0.1135(5) 0.170(4) Uani 1 1 d . . . . .
C1 C 0.5743(3) 0.4379(3) 0.5246(3) 0.1006(13) Uani 1 1 d . . . . .
H1A H 0.591359 0.468601 0.498569 0.121 Uiso 1 1 calc R U . . .
C2 C 0.6113(4) 0.4124(4) 0.5699(4) 0.122(2) Uani 1 1 d . . . . .
H2A H 0.652469 0.426172 0.574927 0.146 Uiso 1 1 calc R U . . .
C3 C 0.5886(4) 0.3679(4) 0.6069(4) 0.127(2) Uani 1 1 d . . . . .
H3A H 0.613744 0.349366 0.637561 0.153 Uiso 1 1 calc R U . . .
C4 C 0.5291(4) 0.3504(3) 0.5994(4) 0.122(2) Uani 1 1 d . . . . .
H4A H 0.512005 0.320097 0.625950 0.146 Uiso 1 1 calc R U . . .
C5 C 0.4927(3) 0.3761(3) 0.5533(3) 0.1018(14) Uani 1 1 d . . . . .
C6 C 0.4292(3) 0.3614(3) 0.5415(3) 0.1010(13) Uani 1 1 d . . . . .
C7 C 0.3851(4) 0.3259(3) 0.5700(3) 0.1090(16) Uani 1 1 d . . . . .
H7A H 0.390347 0.301683 0.606051 0.131 Uiso 1 1 calc R U . . .
C8 C 0.3328(3) 0.3323(3) 0.5366(3) 0.1068(16) Uani 1 1 d . . . . .
C9 C 0.2227(3) 0.3215(4) 0.5071(3) 0.1136(18) Uani 1 1 d . . . . .
H9A H 0.229438 0.347955 0.472962 0.136 Uiso 1 1 calc R U . . .
C10 C 0.2709(3) 0.3070(3) 0.5455(3) 0.1078(16) Uani 1 1 d . . . . .
C11 C 0.2617(5) 0.2658(4) 0.5957(3) 0.129(2) Uani 1 1 d . . . . .
H11A H 0.295399 0.252621 0.620251 0.155 Uiso 1 1 calc R U . . .
C12 C 0.2038(6) 0.2458(6) 0.6078(4) 0.153(4) Uani 1 1 d . . . . .
H12A H 0.196720 0.221448 0.643466 0.184 Uiso 1 1 calc R U . . .
C13 C 0.1555(6) 0.2597(6) 0.5703(5) 0.153(4) Uani 1 1 d . . . . .
H13A H 0.115751 0.243787 0.579389 0.184 Uiso 1 1 calc R U . . .
C14 C 0.1639(4) 0.2976(4) 0.5177(4) 0.122(2) Uani 1 1 d . . . . .
C15 C 0.1258(3) 0.2993(4) 0.4110(4) 0.1178(19) Uani 1 1 d . . . . .
H15A H 0.165357 0.285711 0.398297 0.141 Uiso 1 1 calc R U . . .
C16 C 0.1158(4) 0.3096(5) 0.4744(4) 0.137(3) Uani 1 1 d . . . . .
C17 C 0.0594(4) 0.3314(6) 0.4921(5) 0.144(3) Uani 1 1 d . . . . .
H17A H 0.050498 0.338218 0.534361 0.173 Uiso 1 1 calc R U . . .
C18 C 0.0147(5) 0.3437(6) 0.4467(7) 0.168(4) Uani 1 1 d . . . . .
H18A H -0.023581 0.361068 0.458653 0.202 Uiso 1 1 calc R U . . .
C19 C 0.0255(4) 0.3310(6) 0.3843(6) 0.154(4) Uani 1 1 d . . . . .
H19A H -0.005707 0.338507 0.354618 0.184 Uiso 1 1 calc R U . . .
C20 C 0.0817(3) 0.3076(5) 0.3666(5) 0.128(2) Uani 1 1 d . . . . .
C21 C 0.0911(3) 0.2881(4) 0.3017(4) 0.122(2) Uani 1 1 d . . . . .
C22 C 0.0557(4) 0.2945(5) 0.2487(5) 0.134(3) Uani 1 1 d . . . . .
H22A H 0.018269 0.316731 0.244963 0.161 Uiso 1 1 calc R U . . .
C23 C 0.0853(4) 0.2625(5) 0.2028(5) 0.131(3) Uani 1 1 d . . . . .
C24 C 0.0741(6) 0.2477(8) 0.1373(6) 0.167(5) Uani 1 1 d . . . . .
C25 C 0.0228(7) 0.2749(9) 0.1075(7) 0.185(5) Uani 1 1 d . . . . .
H25A H -0.005350 0.301216 0.128203 0.222 Uiso 1 1 calc R U . . .
C26 C 0.0169(12) 0.2595(15) 0.0440(10) 0.242(10) Uani 1 1 d . . . . .
H26A H -0.011881 0.280600 0.018715 0.291 Uiso 1 1 calc R U . . .
C27 C 0.0526(13) 0.2147(16) 0.0205(9) 0.264(13) Uani 1 1 d . . . . .
H27A H 0.045060 0.200050 -0.020043 0.317 Uiso 1 1 calc R U . . .
C28 C 0.1057(9) 0.1869(13) 0.0584(7) 0.243(10) Uani 1 1 d . . . . .
H28A H 0.132441 0.156905 0.041152 0.291 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31567(4) 0.31567(4) 0.31567(4) 0.0928(4) Uani 1 3 d S T P . .
O1 O 0.28212(17) 0.38241(18) 0.37043(17) 0.0915(8) Uani 1 1 d . . . . .
O2 O 0.24893(19) 0.34642(19) 0.26056(18) 0.0951(8) Uani 1 1 d . . . . .
C29 C 0.2349(3) 0.4111(3) 0.3474(3) 0.1030(14) Uani 1 1 d . . . . .
C30 C 0.2164(3) 0.3908(3) 0.2835(3) 0.1052(15) Uani 1 1 d . . . . .
O3 O 0.1085(7) 0.5137(8) 0.2448(7) 0.143(4) Uani 0.5 1 d . U P A 1
O4 O 0.1389(7) 0.5481(6) 0.3630(7) 0.130(4) Uani 0.5 1 d . U P A 1
C31 C 0.1731(9) 0.4291(8) 0.2472(10) 0.118(4) Uani 0.5 1 d . U P A 1
H31A H 0.163991 0.418578 0.205713 0.141 Uiso 0.5 1 calc R U P A 1
C32 C 0.1450(7) 0.4823(8) 0.2752(8) 0.117(3) Uani 0.5 1 d . U P A 1
C33 C 0.1614(7) 0.5004(7) 0.3424(7) 0.108(3) Uani 0.5 1 d . U P A 1
C34 C 0.2064(9) 0.4656(7) 0.3739(10) 0.096(3) Uani 0.5 1 d . U P A 1
H34A H 0.218606 0.478369 0.413968 0.116 Uiso 0.5 1 calc R U P A 1
O3B O 0.0791(7) 0.4703(11) 0.2677(9) 0.174(5) Uani 0.5 1 d . U P A 2
O4B O 0.1149(8) 0.5179(10) 0.3728(10) 0.165(6) Uani 0.5 1 d . U P A 2
C31B C 0.1679(9) 0.4067(8) 0.2608(11) 0.126(4) Uani 0.5 1 d . U P A 2
H31B H 0.158126 0.393730 0.220195 0.151 Uiso 0.5 1 calc R U P A 2
C32B C 0.1255(8) 0.4444(9) 0.2933(9) 0.129(3) Uani 0.5 1 d . U P A 2
C33B C 0.1458(9) 0.4717(10) 0.3517(11) 0.130(3) Uani 0.5 1 d . U P A 2
C34B C 0.2009(10) 0.4451(10) 0.3798(13) 0.117(4) Uani 0.5 1 d . U P A 2
H34B H 0.210784 0.453343 0.421620 0.140 Uiso 0.5 1 calc R U P A 2
O1S O 0.3946(7) 0.2675(7) 0.7035(5) 0.233(6) Uani 1 1 d D U . . .
H1S H 0.402256 0.235287 0.723511 0.349 Uiso 1 1 d R U . . .
C1S C 0.4113(13) 0.3187(12) 0.7422(12) 0.280(11) Uani 1 1 d D U . . .
H1S1 H 0.417061 0.307477 0.785507 0.421 Uiso 1 1 d R U . . .
H1S2 H 0.381151 0.352117 0.739217 0.421 Uiso 1 1 d R U . . .
H1S3 H 0.450591 0.332257 0.724787 0.421 Uiso 1 1 d R U . . .
B1 B -0.1120(9) 0.3903(10) 0.0946(9) 0.146(12) Uani 0.3333 1 d D U P B -1
F1 F -0.1126(16) 0.3618(16) 0.1516(10) 0.25(2) Uani 0.3333 1 d D U P B -1
F2 F -0.0550(9) 0.4171(18) 0.0884(19) 0.208(16) Uani 0.3333 1 d D U P B -1
F3 F -0.1568(10) 0.4341(11) 0.0869(16) 0.193(13) Uani 0.3333 1 d D U P B -1
F4 F -0.1215(11) 0.3451(9) 0.0517(11) 0.150(7) Uani 0.3333 1 d D U P B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.945(5) 9 ?
Fe1 N2 1.945(5) 5 ?
Fe1 N2 1.945(5) . ?
Fe1 N1 1.993(5) . ?
Fe1 N1 1.993(5) 5 ?
Fe1 N1 1.993(5) 9 ?
Fe2 N5 1.948(8) . ?
Fe2 N5 1.948(8) 5 ?
Fe2 N5 1.948(8) 9 ?
Fe2 N6 1.980(11) 9 ?
Fe2 N6 1.980(11) 5 ?
Fe2 N6 1.980(11) . ?
N1 C1 1.346(8) . ?
N1 C5 1.367(8) . ?
N2 C6 1.357(7) . ?
N2 N3 1.362(7) . ?
N3 C8 1.389(8) . ?
N3 H3 0.89(3) . ?
N4 N5 1.336(10) . ?
N4 C21 1.390(10) . ?
N4 H4 0.90(3) . ?
N5 C23 1.355(11) . ?
N6 C28 1.272(18) . ?
N6 C24 1.35(2) . ?
C1 C2 1.387(10) . ?
C1 H1A 0.9500 . ?
C2 C3 1.350(13) . ?
C2 H2A 0.9500 . ?
C3 C4 1.360(13) . ?
C3 H3A 0.9500 . ?
C4 C5 1.392(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.437(10) . ?
C6 C7 1.378(9) . ?
C7 C8 1.357(11) . ?
C7 H7A 0.9500 . ?
C8 C10 1.465(9) . ?
C9 C10 1.376(11) . ?
C9 C14 1.398(10) . ?
C9 H9A 0.9500 . ?
C10 C11 1.425(10) . ?
C11 C12 1.356(14) . ?
C11 H11A 0.9500 . ?
C12 C13 1.363(17) . ?
C12 H12A 0.9500 . ?
C13 C14 1.422(14) . ?
C13 H13A 0.9500 . ?
C14 C16 1.430(14) . ?
C15 C20 1.371(13) . ?
C15 C16 1.414(12) . ?
C15 H15A 0.9500 . ?
C16 C17 1.368(12) . ?
C17 C18 1.409(19) . ?
C17 H17A 0.9500 . ?
C18 C19 1.40(2) . ?
C18 H18A 0.9500 . ?
C19 C20 1.377(12) . ?
C19 H19A 0.9500 . ?
C20 C21 1.486(14) . ?
C21 C22 1.391(13) . ?
C22 C23 1.376(15) . ?
C22 H22A 0.9500 . ?
C23 C24 1.480(18) . ?
C24 C25 1.42(2) . ?
C25 C26 1.42(3) . ?
C25 H25A 0.9500 . ?
C26 C27 1.35(3) . ?
C26 H26A 0.9500 . ?
C27 C28 1.54(3) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.996(4) 9 ?
Fe3 O2 1.996(4) 5 ?
Fe3 O2 1.996(4) . ?
Fe3 O1 2.012(4) 9 ?
Fe3 O1 2.012(4) 5 ?
Fe3 O1 2.012(4) . ?
O1 C29 1.300(7) . ?
O2 C30 1.296(8) . ?
C29 C34B 1.26(3) . ?
C29 C34 1.455(17) . ?
C29 C30 1.512(9) . ?
C30 C31B 1.21(2) . ?
C30 C31 1.482(19) . ?
O3 C32 1.237(18) . ?
O4 C33 1.231(19) . ?
C31 C32 1.44(2) . ?
C31 H31A 0.9500 . ?
C32 C33 1.55(2) . ?
C33 C34 1.413(19) . ?
C34 H34A 0.9500 . ?
O3B C32B 1.28(2) . ?
O4B C33B 1.29(2) . ?
C31B C32B 1.42(2) . ?
C31B H31B 0.9500 . ?
C32B C33B 1.47(2) . ?
C33B C34B 1.46(3) . ?
C34B H34B 0.9500 . ?
O1S C1S 1.440(13) . ?
O1S H1S 0.8398 . ?
C1S H1S1 0.9801 . ?
C1S H1S2 0.9798 . ?
C1S H1S3 0.9800 . ?
B1 F3 1.370(16) . ?
B1 F4 1.371(17) . ?
B1 F2 1.375(14) . ?
B1 F1 1.384(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.81(18) 9 5 ?
N2 Fe1 N2 96.81(18) 9 . ?
N2 Fe1 N2 96.81(18) 5 . ?
N2 Fe1 N1 172.91(19) 9 . ?
N2 Fe1 N1 89.91(18) 5 . ?
N2 Fe1 N1 80.1(2) . . ?
N2 Fe1 N1 89.91(18) 9 5 ?
N2 Fe1 N1 80.1(2) 5 5 ?
N2 Fe1 N1 172.91(19) . 5 ?
N1 Fe1 N1 93.5(2) . 5 ?
N2 Fe1 N1 80.1(2) 9 9 ?
N2 Fe1 N1 172.91(19) 5 9 ?
N2 Fe1 N1 89.91(18) . 9 ?
N1 Fe1 N1 93.5(2) . 9 ?
N1 Fe1 N1 93.5(2) 5 9 ?
N5 Fe2 N5 96.3(2) . 5 ?
N5 Fe2 N5 96.3(2) . 9 ?
N5 Fe2 N5 96.3(2) 5 9 ?
N5 Fe2 N6 173.7(4) . 9 ?
N5 Fe2 N6 89.9(4) 5 9 ?
N5 Fe2 N6 82.4(4) 9 9 ?
N5 Fe2 N6 89.9(4) . 5 ?
N5 Fe2 N6 82.4(4) 5 5 ?
N5 Fe2 N6 173.7(4) 9 5 ?
N6 Fe2 N6 91.5(5) 9 5 ?
N5 Fe2 N6 82.4(4) . . ?
N5 Fe2 N6 173.7(4) 5 . ?
N5 Fe2 N6 89.9(4) 9 . ?
N6 Fe2 N6 91.5(5) 9 . ?
N6 Fe2 N6 91.5(5) 5 . ?
C1 N1 C5 116.8(5) . . ?
C1 N1 Fe1 128.0(4) . . ?
C5 N1 Fe1 115.2(4) . . ?
C6 N2 N3 105.8(5) . . ?
C6 N2 Fe1 116.6(4) . . ?
N3 N2 Fe1 136.0(4) . . ?
N2 N3 C8 109.3(5) . . ?
N2 N3 H3 122(7) . . ?
C8 N3 H3 129(7) . . ?
N5 N4 C21 109.9(7) . . ?
N5 N4 H4 142(8) . . ?
C21 N4 H4 106(8) . . ?
N4 N5 C23 107.8(8) . . ?
N4 N5 Fe2 135.7(6) . . ?
C23 N5 Fe2 114.4(7) . . ?
C28 N6 C24 120.3(16) . . ?
C28 N6 Fe2 125.9(15) . . ?
C24 N6 Fe2 113.8(8) . . ?
N1 C1 C2 123.0(7) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 119.9(7) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 118.4(7) . . ?
C2 C3 H3A 120.8 . . ?
C4 C3 H3A 120.8 . . ?
C3 C4 C5 121.0(7) . . ?
C3 C4 H4A 119.5 . . ?
C5 C4 H4A 119.5 . . ?
N1 C5 C4 120.9(7) . . ?
N1 C5 C6 113.4(6) . . ?
C4 C5 C6 125.7(6) . . ?
N2 C6 C7 110.7(6) . . ?
N2 C6 C5 114.0(5) . . ?
C7 C6 C5 135.3(6) . . ?
C8 C7 C6 106.6(6) . . ?
C8 C7 H7A 126.7 . . ?
C6 C7 H7A 126.7 . . ?
C7 C8 N3 107.5(6) . . ?
C7 C8 C10 131.3(6) . . ?
N3 C8 C10 121.1(6) . . ?
C10 C9 C14 120.7(7) . . ?
C10 C9 H9A 119.6 . . ?
C14 C9 H9A 119.6 . . ?
C9 C10 C11 120.1(7) . . ?
C9 C10 C8 122.2(6) . . ?
C11 C10 C8 117.8(7) . . ?
C12 C11 C10 118.7(10) . . ?
C12 C11 H11A 120.7 . . ?
C10 C11 H11A 120.7 . . ?
C11 C12 C13 121.8(8) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C12 C13 C14 120.7(8) . . ?
C12 C13 H13A 119.7 . . ?
C14 C13 H13A 119.7 . . ?
C9 C14 C13 117.7(9) . . ?
C9 C14 C16 119.5(7) . . ?
C13 C14 C16 122.7(8) . . ?
C20 C15 C16 123.8(7) . . ?
C20 C15 H15A 118.1 . . ?
C16 C15 H15A 118.1 . . ?
C17 C16 C15 117.8(10) . . ?
C17 C16 C14 122.2(8) . . ?
C15 C16 C14 120.0(7) . . ?
C16 C17 C18 119.1(10) . . ?
C16 C17 H17A 120.5 . . ?
C18 C17 H17A 120.5 . . ?
C19 C18 C17 121.6(9) . . ?
C19 C18 H18A 119.2 . . ?
C17 C18 H18A 119.2 . . ?
C20 C19 C18 119.4(12) . . ?
C20 C19 H19A 120.3 . . ?
C18 C19 H19A 120.3 . . ?
C15 C20 C19 118.2(10) . . ?
C15 C20 C21 122.2(7) . . ?
C19 C20 C21 119.5(10) . . ?
N4 C21 C22 105.9(8) . . ?
N4 C21 C20 121.0(7) . . ?
C22 C21 C20 132.9(8) . . ?
C23 C22 C21 107.0(8) . . ?
C23 C22 H22A 126.5 . . ?
C21 C22 H22A 126.5 . . ?
N5 C23 C22 109.3(8) . . ?
N5 C23 C24 113.7(11) . . ?
C22 C23 C24 136.9(10) . . ?
N6 C24 C25 126.7(14) . . ?
N6 C24 C23 114.5(11) . . ?
C25 C24 C23 118.5(16) . . ?
C24 C25 C26 114(2) . . ?
C24 C25 H25A 122.8 . . ?
C26 C25 H25A 122.8 . . ?
C27 C26 C25 119.0(19) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
C26 C27 C28 120.8(17) . . ?
C26 C27 H27A 119.6 . . ?
C28 C27 H27A 119.6 . . ?
N6 C28 C27 118(2) . . ?
N6 C28 H28A 121.1 . . ?
C27 C28 H28A 121.1 . . ?
O2 Fe3 O2 90.47(17) 9 5 ?
O2 Fe3 O2 90.47(17) 9 . ?
O2 Fe3 O2 90.47(17) 5 . ?
O2 Fe3 O1 81.39(14) 9 9 ?
O2 Fe3 O1 169.48(15) 5 9 ?
O2 Fe3 O1 96.22(16) . 9 ?
O2 Fe3 O1 96.22(16) 9 5 ?
O2 Fe3 O1 81.39(14) 5 5 ?
O2 Fe3 O1 169.48(15) . 5 ?
O1 Fe3 O1 92.81(16) 9 5 ?
O2 Fe3 O1 169.48(15) 9 . ?
O2 Fe3 O1 96.22(16) 5 . ?
O2 Fe3 O1 81.39(14) . . ?
O1 Fe3 O1 92.81(15) 9 . ?
O1 Fe3 O1 92.81(15) 5 . ?
C29 O1 Fe3 113.8(4) . . ?
C30 O2 Fe3 114.5(4) . . ?
C34B C29 O1 122.0(13) . . ?
O1 C29 C34 125.0(9) . . ?
C34B C29 C30 121.9(12) . . ?
O1 C29 C30 115.0(5) . . ?
C34 C29 C30 119.2(10) . . ?
C31B C30 O2 121.9(11) . . ?
O2 C30 C31 123.9(10) . . ?
C31B C30 C29 121.5(12) . . ?
O2 C30 C29 115.2(5) . . ?
C31 C30 C29 119.7(10) . . ?
C32 C31 C30 119.5(16) . . ?
C32 C31 H31A 120.2 . . ?
C30 C31 H31A 120.2 . . ?
O3 C32 C31 119.3(16) . . ?
O3 C32 C33 120.5(13) . . ?
C31 C32 C33 120.1(13) . . ?
O4 C33 C34 123.3(16) . . ?
O4 C33 C32 117.6(12) . . ?
C34 C33 C32 118.6(13) . . ?
C33 C34 C29 122.5(16) . . ?
C33 C34 H34A 118.8 . . ?
C29 C34 H34A 118.8 . . ?
C30 C31B C32B 121.7(18) . . ?
C30 C31B H31B 119.2 . . ?
C32B C31B H31B 119.2 . . ?
O3B C32B C31B 123.2(17) . . ?
O3B C32B C33B 115.7(15) . . ?
C31B C32B C33B 117.8(14) . . ?
O4B C33B C34B 125.7(17) . . ?
O4B C33B C32B 117.7(17) . . ?
C34B C33B C32B 116.6(16) . . ?
C29 C34B C33B 119(2) . . ?
C29 C34B H34B 120.7 . . ?
C33B C34B H34B 120.7 . . ?
C1S O1S H1S 107.0 . . ?
O1S C1S H1S1 113.6 . . ?
O1S C1S H1S2 111.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 103.1 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F3 B1 F4 107.9(16) . . ?
F3 B1 F2 109.5(19) . . ?
F4 B1 F2 112(2) . . ?
F3 B1 F1 114(2) . . ?
F4 B1 F1 107(2) . . ?
F2 B1 F1 106.6(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(3) 2.17(7) 2.926(7) 143(9) . yes
N4 H4 O2 0.90(3) 2.27(10) 2.918(7) 129(10) 5 yes

_refine_diff_density_max         0.951
_refine_diff_density_min         -0.465
_refine_diff_density_rms         0.096

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_200K
_database_code_depnum_ccdc_archive 'CCDC 2260941'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.827(3)
_cell_length_b                   21.827(3)
_cell_length_c                   21.827(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10399(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6682
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      33.77

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.523
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            172861
_diffrn_reflns_av_unetI/netI     0.0242
_diffrn_reflns_av_R_equivalents  0.0695
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.915
_diffrn_reflns_theta_max         29.524
_diffrn_reflns_theta_full        29.524
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8995
_reflns_number_gt                8748
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with distance
 and displacement parameters restraints.
 The anilate is disordered over two equivalent positions sharing the 
 coordinated C-O groups. The two components were refined with displacement
 parameters restraints as well as a FLAT restraint for the C atoms. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1120 cubic angstrom with a total of 140 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
 
 Details of SQUEEZE results before refinement of the BF4 disorder:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.083  0.158  0.142      1120       140 ' '
   2  0.134  0.366  0.634         9         0 ' '
   3  0.366  0.634  0.134         9         0 ' '
   4  0.634  0.134  0.366         9         0 ' '
   5  0.866  0.866  0.866         9         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?



 Details of SQUEEZE results on a 200 K data set of the same crystal
 after measurements up to 400 K:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.084  0.137  0.139      1771        72 ' '
   2  0.106  0.394  0.606        10         0 ' '
   3  0.394  0.606  0.106        10         0 ' '
   4  0.606  0.106  0.394        10         0 ' '
   5  0.894  0.894  0.894        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_200K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1120 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1120 cubic angstrom with a total of 140 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1385P)²+0.1358P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.029(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3926 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.073(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8995
_refine_ls_number_parameters     530
_refine_ls_number_restraints     242
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0554
_refine_ls_wR_factor_ref         0.1660
_refine_ls_wR_factor_gt          0.1647
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.089
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29501(2) 0.29501(2) 0.29501(2) 0.06526(19) Uani 1 3 d S T P . .
Fe2 Fe 0.57523(2) 0.57523(2) 0.57523(2) 0.0866(3) Uani 1 3 d S T P . .
N1 N 0.23509(12) 0.32902(12) 0.23477(12) 0.0717(5) Uani 1 1 d . . . . .
N2 N 0.25905(11) 0.35989(11) 0.34484(11) 0.0692(5) Uani 1 1 d . . . . .
N3 N 0.26119(11) 0.37688(12) 0.40444(12) 0.0707(5) Uani 1 1 d D . . . .
H3 H 0.287(2) 0.367(3) 0.432(2) 0.106 Uiso 1 1 d D U . . .
N4 N 0.46374(14) 0.49716(14) 0.60854(12) 0.0783(6) Uani 1 1 d D . . . .
H4 H 0.432(2) 0.503(3) 0.582(2) 0.117 Uiso 1 1 d D U . . .
N5 N 0.52311(14) 0.51201(15) 0.61163(13) 0.0817(6) Uani 1 1 d . . . . .
N6 N 0.63305(19) 0.5409(2) 0.6378(2) 0.1083(11) Uani 1 1 d . . . . .
C1 C 0.22767(17) 0.31177(16) 0.17614(15) 0.0806(7) Uani 1 1 d . . . . .
H1A H 0.253584 0.280911 0.159700 0.097 Uiso 1 1 calc R U . . .
C2 C 0.1827(2) 0.3381(2) 0.13862(18) 0.0967(10) Uani 1 1 d . . . . .
H2A H 0.177972 0.324645 0.097494 0.116 Uiso 1 1 calc R U . . .
C3 C 0.1458(2) 0.3831(2) 0.1615(2) 0.1016(11) Uani 1 1 d . . . . .
H3B H 0.115573 0.401585 0.136260 0.122 Uiso 1 1 calc R U . . .
C4 C 0.1528(2) 0.40158(19) 0.2217(2) 0.0941(9) Uani 1 1 d . . . . .
H4B H 0.126977 0.432201 0.238735 0.113 Uiso 1 1 calc R U . . .
C5 C 0.19855(15) 0.37435(14) 0.25695(16) 0.0765(6) Uani 1 1 d . . . . .
C6 C 0.21037(14) 0.38877(14) 0.32081(15) 0.0743(6) Uani 1 1 d . . . . .
C7 C 0.18096(16) 0.42484(17) 0.36417(18) 0.0838(7) Uani 1 1 d . . . . .
H7A H 0.145530 0.449490 0.358566 0.101 Uiso 1 1 calc R U . . .
C8 C 0.21441(13) 0.41703(15) 0.41705(16) 0.0784(7) Uani 1 1 d . . . . .
C9 C 0.20486(14) 0.44290(17) 0.47833(17) 0.0831(7) Uani 1 1 d . . . . .
C10 C 0.15477(19) 0.4827(2) 0.4876(2) 0.1041(12) Uani 1 1 d . . . . .
H10A H 0.129176 0.494314 0.454367 0.125 Uiso 1 1 calc R U . . .
C11 C 0.1438(2) 0.5043(3) 0.5458(3) 0.1250(18) Uani 1 1 d . . . . .
H11A H 0.109283 0.529931 0.552742 0.150 Uiso 1 1 calc R U . . .
C12 C 0.1814(2) 0.4898(3) 0.5942(2) 0.1146(15) Uani 1 1 d . . . . .
H12A H 0.172533 0.505080 0.633942 0.138 Uiso 1 1 calc R U . . .
C13 C 0.23241(18) 0.4528(2) 0.58513(18) 0.0946(10) Uani 1 1 d . . . . .
C14 C 0.24393(15) 0.42879(18) 0.52661(16) 0.0841(8) Uani 1 1 d . . . . .
H14A H 0.278343 0.402974 0.519993 0.101 Uiso 1 1 calc R U . . .
C15 C 0.27642(19) 0.4402(2) 0.63304(17) 0.0969(11) Uani 1 1 d . . . . .
C16 C 0.2591(3) 0.4186(3) 0.6904(2) 0.1220(18) Uani 1 1 d . . . . .
H16A H 0.217029 0.411743 0.699476 0.146 Uiso 1 1 calc R U . . .
C17 C 0.3039(3) 0.4070(4) 0.7348(2) 0.1275(19) Uani 1 1 d . . . . .
H17A H 0.292124 0.389880 0.773060 0.153 Uiso 1 1 calc R U . . .
C18 C 0.3646(3) 0.4198(3) 0.7240(2) 0.1123(15) Uani 1 1 d . . . . .
H18A H 0.394022 0.413115 0.755372 0.135 Uiso 1 1 calc R U . . .
C19 C 0.3833(2) 0.4427(2) 0.66725(16) 0.0912(9) Uani 1 1 d . . . . .
C20 C 0.33882(17) 0.4518(2) 0.62275(14) 0.0871(8) Uani 1 1 d . . . . .
H20A H 0.351130 0.466543 0.583675 0.105 Uiso 1 1 calc R U . . .
C21 C 0.44695(19) 0.46228(18) 0.65720(14) 0.0851(8) Uani 1 1 d . . . . .
C22 C 0.4993(2) 0.4546(2) 0.69304(17) 0.0969(10) Uani 1 1 d . . . . .
H22A H 0.502782 0.432125 0.730133 0.116 Uiso 1 1 calc R U . . .
C23 C 0.5444(2) 0.48639(19) 0.66343(17) 0.0900(9) Uani 1 1 d . . . . .
C24 C 0.6091(2) 0.4995(3) 0.6760(2) 0.1041(12) Uani 1 1 d . . . . .
C25 C 0.6412(3) 0.4732(4) 0.7243(3) 0.133(2) Uani 1 1 d . . . . .
H25A H 0.622319 0.444828 0.751413 0.159 Uiso 1 1 calc R U . . .
C26 C 0.7035(4) 0.4906(6) 0.7312(5) 0.172(4) Uani 1 1 d . . . . .
H26A H 0.728022 0.472840 0.762498 0.207 Uiso 1 1 calc R U . . .
C27 C 0.7280(4) 0.5336(7) 0.6919(5) 0.185(5) Uani 1 1 d . . . . .
H27A H 0.769288 0.546523 0.696761 0.222 Uiso 1 1 calc R U . . .
C28 C 0.6923(3) 0.5580(5) 0.6454(4) 0.143(2) Uani 1 1 d . . . . .
H28A H 0.709705 0.587175 0.618213 0.172 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43387(2) 0.43387(2) 0.43387(2) 0.06628(18) Uani 1 3 d S T P . .
O1 O 0.37952(9) 0.36798(10) 0.46721(9) 0.0687(4) Uani 1 1 d . . . . .
O2 O 0.48866(9) 0.40352(9) 0.50047(10) 0.0697(4) Uani 1 1 d . . . . .
C29 C 0.40235(13) 0.33935(15) 0.51484(13) 0.0718(5) Uani 1 1 d . . . . .
C30 C 0.46564(14) 0.35971(15) 0.53299(13) 0.0752(6) Uani 1 1 d . . . . .
O3 O 0.4838(6) 0.2795(6) 0.6704(4) 0.145(4) Uani 0.5 1 d . U P A 1
O4 O 0.3749(7) 0.2347(6) 0.6345(6) 0.144(5) Uani 0.5 1 d . U P A 1
C31 C 0.4935(8) 0.3401(6) 0.5818(7) 0.096(3) Uani 0.5 1 d . U P A 1
H31A H 0.534021 0.353248 0.590782 0.115 Uiso 0.5 1 calc R U P A 1
C32 C 0.4623(6) 0.2979(6) 0.6225(6) 0.107(3) Uani 0.5 1 d . U P A 1
C33 C 0.3998(7) 0.2735(6) 0.6023(6) 0.104(3) Uani 0.5 1 d . U P A 1
C34 C 0.3702(10) 0.3005(9) 0.5481(9) 0.093(4) Uani 0.5 1 d . U P A 1
H34A H 0.329319 0.290212 0.537405 0.111 Uiso 0.5 1 calc R U P A 1
O3B O 0.5002(5) 0.2436(6) 0.6455(5) 0.130(3) Uani 0.5 1 d . U P A 2
O4B O 0.3848(6) 0.2071(5) 0.6135(7) 0.126(4) Uani 0.5 1 d . U P A 2
C31B C 0.4973(9) 0.3225(7) 0.5776(8) 0.099(3) Uani 0.5 1 d . U P A 2
H31B H 0.538256 0.333322 0.587779 0.119 Uiso 0.5 1 calc R U P A 2
C32B C 0.4721(6) 0.2722(5) 0.6065(5) 0.095(2) Uani 0.5 1 d . U P A 2
C33B C 0.4061(6) 0.2528(5) 0.5888(6) 0.091(2) Uani 0.5 1 d . U P A 2
C34B C 0.3757(8) 0.2879(7) 0.5436(9) 0.078(2) Uani 0.5 1 d . U P A 2
H34B H 0.335332 0.276348 0.532078 0.094 Uiso 0.5 1 calc R U P A 2
O1S O 0.0468(5) 0.4830(7) 0.3569(7) 0.261(5) Uani 1 1 d . U . . .
H1S H 0.021971 0.514244 0.353156 0.392 Uiso 1 1 d R U . . .
C1S C 0.0110(11) 0.4207(13) 0.3341(10) 0.300(9) Uani 1 1 d . U . . .
H1S1 H -0.029238 0.432720 0.318122 0.450 Uiso 1 1 d R U . . .
H1S2 H 0.005562 0.390950 0.367302 0.450 Uiso 1 1 d R U . . .
H1S3 H 0.035262 0.402230 0.301232 0.450 Uiso 1 1 d R U . . .
B1 B 0.1490(9) 0.1409(10) 0.1417(10) 0.126(6) Uani 0.3333 1 d D U P B -1
F1 F 0.1561(15) 0.1800(15) 0.0935(14) 0.187(15) Uani 0.3333 1 d D U P B -1
F2 F 0.1587(17) 0.1715(14) 0.1946(8) 0.240(15) Uani 0.3333 1 d D U P B -1
F3 F 0.0926(8) 0.1132(11) 0.1452(13) 0.205(11) Uani 0.3333 1 d D U P B -1
F4 F 0.1910(10) 0.0943(9) 0.1364(14) 0.142(6) Uani 0.3333 1 d D U P B -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.951(2) . ?
Fe1 N2 1.951(2) 5 ?
Fe1 N2 1.951(2) 9 ?
Fe1 N1 1.997(3) 5 ?
Fe1 N1 1.997(3) 9 ?
Fe1 N1 1.998(2) . ?
Fe2 N5 1.957(3) . ?
Fe2 N5 1.957(3) 9 ?
Fe2 N5 1.957(3) 5 ?
Fe2 N6 2.005(4) 9 ?
Fe2 N6 2.005(4) 5 ?
Fe2 N6 2.005(4) . ?
N1 C1 1.344(4) . ?
N1 C5 1.360(4) . ?
N2 C6 1.342(4) . ?
N2 N3 1.353(3) . ?
N3 C8 1.373(4) . ?
N3 H3 0.85(3) . ?
N4 N5 1.338(4) . ?
N4 C21 1.357(5) . ?
N4 H4 0.92(3) . ?
N5 C23 1.345(5) . ?
N6 C24 1.335(7) . ?
N6 C28 1.355(7) . ?
C1 C2 1.401(5) . ?
C1 H1A 0.9500 . ?
C2 C3 1.365(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.384(7) . ?
C3 H3B 0.9500 . ?
C4 C5 1.393(5) . ?
C4 H4B 0.9500 . ?
C5 C6 1.452(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.376(5) . ?
C7 H7A 0.9500 . ?
C8 C9 1.467(5) . ?
C9 C14 1.390(6) . ?
C9 C10 1.411(5) . ?
C10 C11 1.376(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.375(9) . ?
C11 H11A 0.9500 . ?
C12 C13 1.389(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.403(5) . ?
C13 C15 1.446(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.392(6) . ?
C15 C20 1.403(5) . ?
C16 C17 1.399(10) . ?
C16 H16A 0.9500 . ?
C17 C18 1.375(9) . ?
C17 H17A 0.9500 . ?
C18 C19 1.397(5) . ?
C18 H18A 0.9500 . ?
C19 C20 1.387(6) . ?
C19 C21 1.471(6) . ?
C20 H20A 0.9500 . ?
C21 C22 1.394(6) . ?
C22 C23 1.368(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.465(6) . ?
C24 C25 1.392(7) . ?
C25 C26 1.421(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.379(16) . ?
C26 H26A 0.9500 . ?
C27 C28 1.387(12) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.995(2) 9 ?
Fe3 O2 1.995(2) . ?
Fe3 O2 1.996(2) 5 ?
Fe3 O1 2.0013(19) . ?
Fe3 O1 2.0013(19) 5 ?
Fe3 O1 2.0013(19) 9 ?
O1 C29 1.311(4) . ?
O2 C30 1.293(4) . ?
C29 C34 1.32(2) . ?
C29 C34B 1.412(17) . ?
C29 C30 1.504(4) . ?
C30 C31 1.300(16) . ?
C30 C31B 1.445(19) . ?
O3 C32 1.215(13) . ?
O4 C33 1.227(16) . ?
C31 C32 1.448(14) . ?
C31 H31A 0.9500 . ?
C32 C33 1.529(15) . ?
C33 C34 1.47(2) . ?
C34 H34A 0.9500 . ?
O3B C32B 1.220(12) . ?
O4B C33B 1.226(14) . ?
C31B C32B 1.380(16) . ?
C31B H31B 0.9500 . ?
C32B C33B 1.550(16) . ?
C33B C34B 1.415(18) . ?
C34B H34B 0.9500 . ?
O1S C1S 1.65(3) . ?
O1S H1S 0.8743 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9798 . ?
C1S H1S3 0.9800 . ?
B1 F2 1.351(14) . ?
B1 F1 1.364(16) . ?
B1 F4 1.373(16) . ?
B1 F3 1.375(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.41(10) . 5 ?
N2 Fe1 N2 96.41(10) . 9 ?
N2 Fe1 N2 96.41(10) 5 9 ?
N2 Fe1 N1 90.19(10) . 5 ?
N2 Fe1 N1 80.43(10) 5 5 ?
N2 Fe1 N1 172.98(10) 9 5 ?
N2 Fe1 N1 172.98(10) . 9 ?
N2 Fe1 N1 90.19(10) 5 9 ?
N2 Fe1 N1 80.43(10) 9 9 ?
N1 Fe1 N1 93.26(10) 5 9 ?
N2 Fe1 N1 80.43(10) . . ?
N2 Fe1 N1 172.98(10) 5 . ?
N2 Fe1 N1 90.19(10) 9 . ?
N1 Fe1 N1 93.26(10) 5 . ?
N1 Fe1 N1 93.26(10) 9 . ?
N5 Fe2 N5 96.46(11) . 9 ?
N5 Fe2 N5 96.46(11) . 5 ?
N5 Fe2 N5 96.46(11) 9 5 ?
N5 Fe2 N6 90.45(17) . 9 ?
N5 Fe2 N6 79.98(16) 9 9 ?
N5 Fe2 N6 172.57(17) 5 9 ?
N5 Fe2 N6 172.57(17) . 5 ?
N5 Fe2 N6 90.45(17) 9 5 ?
N5 Fe2 N6 79.98(16) 5 5 ?
N6 Fe2 N6 93.46(19) 9 5 ?
N5 Fe2 N6 79.98(16) . . ?
N5 Fe2 N6 172.57(17) 9 . ?
N5 Fe2 N6 90.45(16) 5 . ?
N6 Fe2 N6 93.46(19) 9 . ?
N6 Fe2 N6 93.46(19) 5 . ?
C1 N1 C5 118.2(3) . . ?
C1 N1 Fe1 127.0(2) . . ?
C5 N1 Fe1 114.8(2) . . ?
C6 N2 N3 105.9(2) . . ?
C6 N2 Fe1 116.2(2) . . ?
N3 N2 Fe1 136.14(19) . . ?
N2 N3 C8 110.0(3) . . ?
N2 N3 H3 129(4) . . ?
C8 N3 H3 121(4) . . ?
N5 N4 C21 111.0(3) . . ?
N5 N4 H4 137(4) . . ?
C21 N4 H4 112(4) . . ?
N4 N5 C23 106.1(3) . . ?
N4 N5 Fe2 135.5(2) . . ?
C23 N5 Fe2 115.7(3) . . ?
C24 N6 C28 118.9(5) . . ?
C24 N6 Fe2 115.5(3) . . ?
C28 N6 Fe2 125.5(5) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3B 120.3 . . ?
C4 C3 H3B 120.3 . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 H4B 120.7 . . ?
C5 C4 H4B 120.7 . . ?
N1 C5 C4 122.3(3) . . ?
N1 C5 C6 113.3(3) . . ?
C4 C5 C6 124.4(3) . . ?
N2 C6 C7 111.5(3) . . ?
N2 C6 C5 114.5(3) . . ?
C7 C6 C5 134.0(3) . . ?
C8 C7 C6 104.8(3) . . ?
C8 C7 H7A 127.6 . . ?
C6 C7 H7A 127.6 . . ?
N3 C8 C7 107.8(3) . . ?
N3 C8 C9 122.3(3) . . ?
C7 C8 C9 129.9(3) . . ?
C14 C9 C10 120.2(3) . . ?
C14 C9 C8 121.2(3) . . ?
C10 C9 C8 118.5(4) . . ?
C11 C10 C9 118.6(5) . . ?
C11 C10 H10A 120.7 . . ?
C9 C10 H10A 120.7 . . ?
C12 C11 C10 121.7(4) . . ?
C12 C11 H11A 119.1 . . ?
C10 C11 H11A 119.1 . . ?
C11 C12 C13 120.2(4) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C12 C13 C14 119.3(4) . . ?
C12 C13 C15 122.6(4) . . ?
C14 C13 C15 117.9(4) . . ?
C9 C14 C13 119.8(3) . . ?
C9 C14 H14A 120.1 . . ?
C13 C14 H14A 120.1 . . ?
C16 C15 C20 118.0(5) . . ?
C16 C15 C13 122.3(4) . . ?
C20 C15 C13 119.7(3) . . ?
C15 C16 C17 119.6(5) . . ?
C15 C16 H16A 120.2 . . ?
C17 C16 H16A 120.2 . . ?
C18 C17 C16 121.2(4) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 120.4(5) . . ?
C17 C18 H18A 119.8 . . ?
C19 C18 H18A 119.8 . . ?
C20 C19 C18 117.9(4) . . ?
C20 C19 C21 121.0(3) . . ?
C18 C19 C21 120.8(4) . . ?
C19 C20 C15 122.7(3) . . ?
C19 C20 H20A 118.6 . . ?
C15 C20 H20A 118.6 . . ?
N4 C21 C22 106.6(4) . . ?
N4 C21 C19 122.3(3) . . ?
C22 C21 C19 131.0(3) . . ?
C23 C22 C21 105.3(3) . . ?
C23 C22 H22A 127.3 . . ?
C21 C22 H22A 127.3 . . ?
N5 C23 C22 111.0(4) . . ?
N5 C23 C24 114.1(4) . . ?
C22 C23 C24 134.9(4) . . ?
N6 C24 C25 123.7(5) . . ?
N6 C24 C23 113.2(4) . . ?
C25 C24 C23 123.0(6) . . ?
C24 C25 C26 116.9(8) . . ?
C24 C25 H25A 121.6 . . ?
C26 C25 H25A 121.6 . . ?
C27 C26 C25 119.2(7) . . ?
C27 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
C26 C27 C28 119.9(7) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
N6 C28 C27 121.4(8) . . ?
N6 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
O2 Fe3 O2 90.24(9) 9 . ?
O2 Fe3 O2 90.24(9) 9 5 ?
O2 Fe3 O2 90.24(9) . 5 ?
O2 Fe3 O1 96.25(9) 9 . ?
O2 Fe3 O1 81.48(8) . . ?
O2 Fe3 O1 169.48(8) 5 . ?
O2 Fe3 O1 169.48(8) 9 5 ?
O2 Fe3 O1 96.25(9) . 5 ?
O2 Fe3 O1 81.48(8) 5 5 ?
O1 Fe3 O1 92.91(8) . 5 ?
O2 Fe3 O1 81.48(8) 9 9 ?
O2 Fe3 O1 169.48(8) . 9 ?
O2 Fe3 O1 96.25(9) 5 9 ?
O1 Fe3 O1 92.91(8) . 9 ?
O1 Fe3 O1 92.91(8) 5 9 ?
C29 O1 Fe3 113.92(17) . . ?
C30 O2 Fe3 114.37(18) . . ?
O1 C29 C34 122.8(8) . . ?
O1 C29 C34B 125.1(8) . . ?
O1 C29 C30 114.6(2) . . ?
C34 C29 C30 122.2(8) . . ?
C34B C29 C30 119.8(8) . . ?
O2 C30 C31 120.8(6) . . ?
O2 C30 C31B 126.9(7) . . ?
O2 C30 C29 115.5(3) . . ?
C31 C30 C29 123.3(7) . . ?
C31B C30 C29 116.8(7) . . ?
C30 C31 C32 119.4(12) . . ?
C30 C31 H31A 120.3 . . ?
C32 C31 H31A 120.3 . . ?
O3 C32 C31 123.8(11) . . ?
O3 C32 C33 118.5(10) . . ?
C31 C32 C33 117.7(10) . . ?
O4 C33 C34 122.8(14) . . ?
O4 C33 C32 118.1(11) . . ?
C34 C33 C32 118.9(11) . . ?
C29 C34 C33 117.8(15) . . ?
C29 C34 H34A 121.1 . . ?
C33 C34 H34A 121.1 . . ?
C32B C31B C30 124.3(15) . . ?
C32B C31B H31B 117.8 . . ?
C30 C31B H31B 117.8 . . ?
O3B C32B C31B 121.7(13) . . ?
O3B C32B C33B 120.0(10) . . ?
C31B C32B C33B 118.3(11) . . ?
O4B C33B C34B 124.6(13) . . ?
O4B C33B C32B 117.8(10) . . ?
C34B C33B C32B 117.6(11) . . ?
C29 C34B C33B 123.1(14) . . ?
C29 C34B H34B 118.4 . . ?
C33B C34B H34B 118.4 . . ?
C1S O1S H1S 108.8 . . ?
O1S C1S H1S1 108.2 . . ?
O1S C1S H1S2 112.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 107.7 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F1 109(2) . . ?
F2 B1 F4 109(2) . . ?
F1 B1 F4 108.9(19) . . ?
F2 B1 F3 108.1(19) . . ?
F1 B1 F3 115(2) . . ?
F4 B1 F3 106.0(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.85(3) 2.16(4) 2.930(3) 150(5) . yes
N4 H4 O2 0.92(3) 2.13(4) 2.929(3) 145(6) 9 yes

_refine_diff_density_max         0.934
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.075

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_320K
_database_code_depnum_ccdc_archive 'CCDC 2260943'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.7(C H4 O)'
_chemical_formula_sum            'C104.70 H76.80 B F4 Fe3 N18 O14.70'
_chemical_formula_weight         2076.62

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.611(3)
_cell_length_b                   21.611(3)
_cell_length_c                   21.611(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10093(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    6423
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.42

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.373
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.539
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.72032
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            164306
_diffrn_reflns_av_unetI/netI     0.0225
_diffrn_reflns_av_R_equivalents  0.0602
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.351
_diffrn_reflns_theta_max         29.108
_diffrn_reflns_theta_full        29.108
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8704
_reflns_number_gt                8410
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.9 (i.e. 2.7 MeOH per formula unit).
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0921P)²+0.1171P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0319(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3777 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.078(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8704
_refine_ls_number_parameters     476
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1134
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45310(2) 0.45310(2) 0.45310(2) 0.05913(13) Uani 1 3 d S T P . .
Fe2 Fe 0.16545(2) 0.16545(2) 0.16545(2) 0.06557(15) Uani 1 3 d S T P . .
N1 N 0.50730(9) 0.41975(9) 0.52140(9) 0.0669(4) Uani 1 1 d . . . . .
N2 N 0.39608(8) 0.39245(9) 0.49003(8) 0.0626(3) Uani 1 1 d . . . . .
N3 N 0.33595(8) 0.37674(9) 0.48366(8) 0.0635(3) Uani 1 1 d D . . . .
H3 H 0.3175(18) 0.3916(19) 0.4487(14) 0.095 Uiso 1 1 d D U . . .
N4 N 0.12898(9) 0.25584(11) 0.27419(10) 0.0727(4) Uani 1 1 d D . . . .
H4 H 0.1661(15) 0.253(2) 0.293(2) 0.109 Uiso 1 1 d D U . . .
N5 N 0.12666(9) 0.23627(11) 0.21526(9) 0.0714(4) Uani 1 1 d . . . . .
N6 N 0.09917(12) 0.19963(12) 0.10382(11) 0.0806(5) Uani 1 1 d . . . . .
C1 C 0.56585(11) 0.43585(13) 0.53419(14) 0.0775(6) Uani 1 1 d . . . . .
H1A H 0.586161 0.463019 0.507711 0.093 Uiso 1 1 calc R U . . .
C2 C 0.59720(15) 0.41340(16) 0.58559(17) 0.0923(8) Uani 1 1 d . . . . .
H2A H 0.637489 0.426120 0.593789 0.111 Uiso 1 1 calc R U . . .
C3 C 0.56806(17) 0.37224(19) 0.62410(18) 0.1000(10) Uani 1 1 d . . . . .
H3A H 0.588584 0.356529 0.658504 0.120 Uiso 1 1 calc R U . . .
C4 C 0.50781(15) 0.35420(17) 0.61144(16) 0.0900(8) Uani 1 1 d . . . . .
H4A H 0.487288 0.326199 0.636872 0.108 Uiso 1 1 calc R U . . .
C5 C 0.47895(11) 0.37913(11) 0.55967(11) 0.0701(5) Uani 1 1 d . . . . .
C6 C 0.41499(11) 0.36615(11) 0.54235(10) 0.0676(4) Uani 1 1 d . . . . .
C7 C 0.36749(12) 0.33273(13) 0.57010(11) 0.0740(5) Uani 1 1 d . . . . .
H7A H 0.369235 0.310297 0.606784 0.089 Uiso 1 1 calc R U . . .
C8 C 0.31741(11) 0.34002(11) 0.53156(10) 0.0674(4) Uani 1 1 d . . . . .
C9 C 0.20736(11) 0.33239(14) 0.49717(11) 0.0750(5) Uani 1 1 d . . . . .
H9A H 0.215761 0.359485 0.464806 0.090 Uiso 1 1 calc R U . . .
C10 C 0.25434(11) 0.31519(12) 0.53724(10) 0.0707(5) Uani 1 1 d . . . . .
C11 C 0.24145(15) 0.27448(16) 0.58543(13) 0.0849(7) Uani 1 1 d . . . . .
H11A H 0.272674 0.262402 0.612477 0.102 Uiso 1 1 calc R U . . .
C12 C 0.18177(19) 0.2520(2) 0.59293(17) 0.1066(11) Uani 1 1 d . . . . .
H12A H 0.173140 0.224517 0.624916 0.128 Uiso 1 1 calc R U . . .
C13 C 0.13588(16) 0.2698(2) 0.55387(16) 0.1027(10) Uani 1 1 d . . . . .
H13A H 0.095910 0.255121 0.560101 0.123 Uiso 1 1 calc R U . . .
C14 C 0.14758(12) 0.30939(16) 0.50497(12) 0.0815(6) Uani 1 1 d . . . . .
C15 C 0.11186(11) 0.30775(14) 0.39652(12) 0.0774(6) Uani 1 1 d . . . . .
H15A H 0.150898 0.293153 0.385796 0.093 Uiso 1 1 calc R U . . .
C16 C 0.09951(12) 0.32211(18) 0.45853(14) 0.0873(7) Uani 1 1 d . . . . .
C17 C 0.04109(17) 0.3450(3) 0.47357(19) 0.1262(18) Uani 1 1 d . . . . .
H17A H 0.031706 0.354843 0.514398 0.151 Uiso 1 1 calc R U . . .
C18 C -0.00267(18) 0.3531(4) 0.4281(2) 0.143(2) Uani 1 1 d . . . . .
H18A H -0.041345 0.368869 0.438385 0.171 Uiso 1 1 calc R U . . .
C19 C 0.01002(16) 0.3380(3) 0.3671(2) 0.1175(14) Uani 1 1 d . . . . .
H19A H -0.020082 0.343550 0.336833 0.141 Uiso 1 1 calc R U . . .
C20 C 0.06789(12) 0.31463(17) 0.35113(14) 0.0828(6) Uani 1 1 d . . . . .
C21 C 0.07902(11) 0.29135(13) 0.28816(12) 0.0743(5) Uani 1 1 d . . . . .
C22 C 0.04275(13) 0.29439(14) 0.23598(13) 0.0798(6) Uani 1 1 d . . . . .
H22A H 0.005425 0.315273 0.231196 0.096 Uiso 1 1 calc R U . . .
C23 C 0.07409(12) 0.25935(12) 0.19181(12) 0.0737(5) Uani 1 1 d . . . . .
C24 C 0.05942(14) 0.24150(13) 0.12801(13) 0.0790(6) Uani 1 1 d . . . . .
C25 C 0.0087(2) 0.2644(2) 0.09655(19) 0.1063(11) Uani 1 1 d . . . . .
H25A H -0.018363 0.291946 0.115453 0.128 Uiso 1 1 calc R U . . .
C26 C -0.0007(3) 0.2453(3) 0.0367(2) 0.1322(18) Uani 1 1 d . . . . .
H26A H -0.034054 0.260471 0.014059 0.159 Uiso 1 1 calc R U . . .
C27 C 0.0398(3) 0.2034(3) 0.0103(2) 0.1309(17) Uani 1 1 d . . . . .
H27A H 0.033929 0.189964 -0.030198 0.157 Uiso 1 1 calc R U . . .
C28 C 0.0895(2) 0.1815(2) 0.04478(16) 0.1055(10) Uani 1 1 d . . . . .
H28A H 0.116793 0.153571 0.026727 0.127 Uiso 1 1 calc R U . . .
Fe3 Fe 0.30955(2) 0.30955(2) 0.30955(2) 0.06452(14) Uani 1 3 d S T P . .
O1 O 0.27763(7) 0.38014(8) 0.36078(7) 0.0652(3) Uani 1 1 d . . . . .
O2 O 0.24676(8) 0.34137(8) 0.24984(7) 0.0692(4) Uani 1 1 d . . . . .
O3 O 0.11251(15) 0.51076(17) 0.22671(14) 0.1219(11) Uani 1 1 d . U . . .
O4 O 0.13887(17) 0.54621(17) 0.34272(15) 0.1297(12) Uani 1 1 d . U . . .
C29 C 0.23478(10) 0.41279(11) 0.33322(10) 0.0642(4) Uani 1 1 d . . . . .
C30 C 0.21849(11) 0.39161(11) 0.26868(10) 0.0663(4) Uani 1 1 d . . . . .
C31 C 0.17791(13) 0.42431(16) 0.23393(13) 0.0834(7) Uani 1 1 d . . . . .
H31A H 0.168656 0.410566 0.194214 0.100 Uiso 1 1 calc R U . . .
C32 C 0.14902(14) 0.47899(17) 0.25628(14) 0.0878(7) Uani 1 1 d . U . . .
C33 C 0.16401(14) 0.49917(16) 0.32352(14) 0.0860(7) Uani 1 1 d . U . . .
C34 C 0.20677(12) 0.46322(13) 0.35835(12) 0.0756(5) Uani 1 1 d . . . . .
H34A H 0.215698 0.474380 0.398938 0.091 Uiso 1 1 calc R U . . .
O1S O 0.2832(8) 0.1158(8) 0.6904(8) 0.359(8) Uani 0.9 1 d . U P . .
H1S H 0.286658 0.091565 0.719404 0.539 Uiso 0.9 1 d R U P . .
C1S C 0.2320(5) 0.1042(6) 0.6542(4) 0.182(3) Uani 0.9 1 d . U P . .
H1S1 H 0.195494 0.107992 0.679147 0.273 Uiso 0.9 1 d R U P . .
H1S2 H 0.236014 0.062332 0.639957 0.273 Uiso 0.9 1 d R U P . .
H1S3 H 0.228954 0.131482 0.619247 0.273 Uiso 0.9 1 d R U P . .
B1 B -0.1147(8) 0.3829(9) 0.1193(11) 0.131(3) Uani 0.3333 1 d D U P A -1
F1 F -0.1057(9) 0.3555(9) 0.1776(9) 0.189(7) Uani 0.3333 1 d D U P A -1
F2 F -0.0592(5) 0.4119(7) 0.1072(9) 0.198(6) Uani 0.3333 1 d D U P A -1
F3 F -0.1631(8) 0.4239(8) 0.1224(10) 0.177(7) Uani 0.3333 1 d D U P A -1
F4 F -0.1273(9) 0.3369(8) 0.0772(10) 0.161(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9681(19) . ?
Fe1 N2 1.9681(19) 9 ?
Fe1 N2 1.9681(19) 5 ?
Fe1 N1 2.0174(19) 9 ?
Fe1 N1 2.0174(19) 5 ?
Fe1 N1 2.0174(19) . ?
Fe2 N5 2.050(2) 5 ?
Fe2 N5 2.050(2) 9 ?
Fe2 N5 2.050(2) . ?
Fe2 N6 2.091(2) . ?
Fe2 N6 2.091(2) 9 ?
Fe2 N6 2.091(2) 5 ?
N1 C1 1.341(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.330(3) . ?
N2 N3 1.350(3) . ?
N3 C8 1.365(3) . ?
N3 H3 0.91(2) . ?
N4 N5 1.343(3) . ?
N4 C21 1.359(3) . ?
N4 H4 0.90(2) . ?
N5 C23 1.340(3) . ?
N6 C28 1.351(4) . ?
N6 C24 1.353(4) . ?
C1 C2 1.389(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.371(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.387(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.389(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.459(3) . ?
C6 C7 1.391(3) . ?
C7 C8 1.375(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.470(3) . ?
C9 C10 1.385(4) . ?
C9 C14 1.394(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.392(4) . ?
C11 C12 1.388(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.358(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.383(5) . ?
C13 H13A 0.9300 . ?
C14 C16 1.470(4) . ?
C15 C20 1.374(4) . ?
C15 C16 1.401(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.394(4) . ?
C17 C18 1.376(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.384(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.393(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.471(4) . ?
C21 C22 1.375(4) . ?
C22 C23 1.394(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.466(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.373(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.384(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.389(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9948(16) . ?
Fe3 O2 1.9948(16) 5 ?
Fe3 O2 1.9949(16) 9 ?
Fe3 O1 2.0071(16) 9 ?
Fe3 O1 2.0071(16) 5 ?
Fe3 O1 2.0071(16) . ?
O1 C29 1.308(3) . ?
O2 C30 1.311(3) . ?
O3 C32 1.226(4) . ?
O4 C33 1.225(4) . ?
C29 C34 1.360(3) . ?
C29 C30 1.510(3) . ?
C30 C31 1.354(3) . ?
C31 C32 1.421(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.551(4) . ?
C33 C34 1.423(4) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.377(15) . ?
O1S H1S 0.8202 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9603 . ?
C1S H1S3 0.9596 . ?
B1 F3 1.37(2) . ?
B1 F2 1.377(15) . ?
B1 F4 1.377(18) . ?
B1 F1 1.406(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.14(7) . 9 ?
N2 Fe1 N2 96.14(7) . 5 ?
N2 Fe1 N2 96.14(7) 9 5 ?
N2 Fe1 N1 91.61(8) . 9 ?
N2 Fe1 N1 80.15(8) 9 9 ?
N2 Fe1 N1 171.74(8) 5 9 ?
N2 Fe1 N1 171.74(8) . 5 ?
N2 Fe1 N1 91.61(8) 9 5 ?
N2 Fe1 N1 80.15(8) 5 5 ?
N1 Fe1 N1 92.52(8) 9 5 ?
N2 Fe1 N1 80.15(8) . . ?
N2 Fe1 N1 171.74(8) 9 . ?
N2 Fe1 N1 91.61(8) 5 . ?
N1 Fe1 N1 92.52(8) 9 . ?
N1 Fe1 N1 92.52(8) 5 . ?
N5 Fe2 N5 97.35(8) 5 9 ?
N5 Fe2 N5 97.35(8) 5 . ?
N5 Fe2 N5 97.35(8) 9 . ?
N5 Fe2 N6 168.42(9) 5 . ?
N5 Fe2 N6 93.76(9) 9 . ?
N5 Fe2 N6 77.91(9) . . ?
N5 Fe2 N6 93.76(9) 5 9 ?
N5 Fe2 N6 77.91(9) 9 9 ?
N5 Fe2 N6 168.42(9) . 9 ?
N6 Fe2 N6 91.76(10) . 9 ?
N5 Fe2 N6 77.91(9) 5 5 ?
N5 Fe2 N6 168.42(9) 9 5 ?
N5 Fe2 N6 93.76(9) . 5 ?
N6 Fe2 N6 91.76(10) . 5 ?
N6 Fe2 N6 91.76(10) 9 5 ?
C1 N1 C5 118.0(2) . . ?
C1 N1 Fe1 127.30(18) . . ?
C5 N1 Fe1 114.59(15) . . ?
C6 N2 N3 105.96(18) . . ?
C6 N2 Fe1 115.91(15) . . ?
N3 N2 Fe1 136.78(14) . . ?
N2 N3 C8 110.58(18) . . ?
N2 N3 H3 115(3) . . ?
C8 N3 H3 135(3) . . ?
N5 N4 C21 111.0(2) . . ?
N5 N4 H4 116(3) . . ?
C21 N4 H4 130(3) . . ?
C23 N5 N4 105.8(2) . . ?
C23 N5 Fe2 115.20(18) . . ?
N4 N5 Fe2 135.86(16) . . ?
C28 N6 C24 117.4(3) . . ?
C28 N6 Fe2 127.3(2) . . ?
C24 N6 Fe2 115.16(18) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.1(3) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.7(2) . . ?
N1 C5 C6 113.4(2) . . ?
C4 C5 C6 123.9(2) . . ?
N2 C6 C7 111.2(2) . . ?
N2 C6 C5 115.3(2) . . ?
C7 C6 C5 133.5(2) . . ?
C8 C7 C6 105.1(2) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 107.2(2) . . ?
N3 C8 C10 123.2(2) . . ?
C7 C8 C10 129.6(2) . . ?
C10 C9 C14 120.5(2) . . ?
C10 C9 H9A 119.7 . . ?
C14 C9 H9A 119.7 . . ?
C9 C10 C11 119.4(2) . . ?
C9 C10 C8 122.0(2) . . ?
C11 C10 C8 118.6(2) . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C13 C12 C11 120.4(3) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C12 C13 C14 121.1(3) . . ?
C12 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C13 C14 C9 118.8(3) . . ?
C13 C14 C16 120.5(3) . . ?
C9 C14 C16 120.4(3) . . ?
C20 C15 C16 121.8(2) . . ?
C20 C15 H15A 119.1 . . ?
C16 C15 H15A 119.1 . . ?
C17 C16 C15 118.3(3) . . ?
C17 C16 C14 123.2(3) . . ?
C15 C16 C14 118.5(2) . . ?
C18 C17 C16 120.1(3) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 121.0(3) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C15 C20 C19 118.9(3) . . ?
C15 C20 C21 120.7(2) . . ?
C19 C20 C21 120.0(3) . . ?
N4 C21 C22 107.3(2) . . ?
N4 C21 C20 121.9(2) . . ?
C22 C21 C20 130.5(2) . . ?
C21 C22 C23 105.0(2) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 110.8(2) . . ?
N5 C23 C24 116.2(2) . . ?
C22 C23 C24 133.0(2) . . ?
N6 C24 C25 123.6(3) . . ?
N6 C24 C23 113.7(2) . . ?
C25 C24 C23 122.7(3) . . ?
C26 C25 C24 118.3(4) . . ?
C26 C25 H25A 120.8 . . ?
C24 C25 H25A 120.8 . . ?
C25 C26 C27 119.4(4) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C26 C27 C28 119.4(4) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
N6 C28 C27 121.9(4) . . ?
N6 C28 H28A 119.1 . . ?
C27 C28 H28A 119.1 . . ?
O2 Fe3 O2 90.99(8) . 5 ?
O2 Fe3 O2 90.99(8) . 9 ?
O2 Fe3 O2 90.99(8) 5 9 ?
O2 Fe3 O1 96.00(7) . 9 ?
O2 Fe3 O1 170.18(7) 5 9 ?
O2 Fe3 O1 82.02(6) 9 9 ?
O2 Fe3 O1 170.18(7) . 5 ?
O2 Fe3 O1 82.02(6) 5 5 ?
O2 Fe3 O1 96.00(7) 9 5 ?
O1 Fe3 O1 91.81(7) 9 5 ?
O2 Fe3 O1 82.02(6) . . ?
O2 Fe3 O1 96.00(7) 5 . ?
O2 Fe3 O1 170.18(7) 9 . ?
O1 Fe3 O1 91.81(7) 9 . ?
O1 Fe3 O1 91.81(7) 5 . ?
C29 O1 Fe3 113.72(13) . . ?
C30 O2 Fe3 113.68(14) . . ?
O1 C29 C34 124.5(2) . . ?
O1 C29 C30 114.98(19) . . ?
C34 C29 C30 120.5(2) . . ?
O2 C30 C31 124.2(2) . . ?
O2 C30 C29 115.43(19) . . ?
C31 C30 C29 120.4(2) . . ?
C30 C31 C32 122.0(2) . . ?
C30 C31 H31A 119.0 . . ?
C32 C31 H31A 119.0 . . ?
O3 C32 C31 124.8(3) . . ?
O3 C32 C33 117.7(3) . . ?
C31 C32 C33 117.4(2) . . ?
O4 C33 C34 124.2(3) . . ?
O4 C33 C32 117.3(3) . . ?
C34 C33 C32 118.5(2) . . ?
C29 C34 C33 121.0(2) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 113.1 . . ?
O1S C1S H1S1 109.0 . . ?
O1S C1S H1S2 106.3 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 113.1 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F3 B1 F2 112.3(16) . . ?
F3 B1 F4 110.3(16) . . ?
F2 B1 F4 112.0(17) . . ?
F3 B1 F1 109.4(17) . . ?
F2 B1 F1 104.1(15) . . ?
F4 B1 F1 108.4(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.91(2) 2.10(3) 2.940(2) 152(4) . yes
N4 H4 O2 0.90(2) 2.09(3) 2.995(3) 177(5) 5 yes

_refine_diff_density_max         0.346
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.063

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_340K
_database_code_depnum_ccdc_archive 'CCDC 2260945'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.286(C H4 O)'
_chemical_formula_sum            'C104.29 H75.14 B F4 Fe3 N18 O14.29'
_chemical_formula_weight         2063.34

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.599(3)
_cell_length_b                   21.599(3)
_cell_length_c                   21.599(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10076(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    340(2)
_cell_measurement_reflns_used    6505
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.89

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_F_000             4236
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.539
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      340(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            166151
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0596
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.368
_diffrn_reflns_theta_max         29.506
_diffrn_reflns_theta_full        29.506
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8696
_reflns_number_gt                8462
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disorder by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.762 (i.e. 2.286 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0668P)²+0.2171P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0181(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3813 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.068(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8696
_refine_ls_number_parameters     479
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0323
_refine_ls_wR_factor_ref         0.0965
_refine_ls_wR_factor_gt          0.0959
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29684(2) 0.29684(2) 0.29684(2) 0.05947(12) Uani 1 3 d S T P . .
Fe2 Fe 0.58458(2) 0.58458(2) 0.58458(2) 0.06618(13) Uani 1 3 d S T P . .
N1 N 0.22757(9) 0.33033(8) 0.24318(8) 0.0685(4) Uani 1 1 d . . . . .
N2 N 0.25981(7) 0.35745(8) 0.35442(8) 0.0636(3) Uani 1 1 d . . . . .
N3 N 0.26628(8) 0.37324(8) 0.41450(8) 0.0649(3) Uani 1 1 d D . . . .
H3 H 0.3023(13) 0.3646(17) 0.4317(16) 0.097 Uiso 1 1 d D U . . .
N4 N 0.47599(9) 0.49267(11) 0.62192(9) 0.0739(4) Uani 1 1 d D . . . .
H4 H 0.4559(18) 0.4963(19) 0.5868(14) 0.111 Uiso 1 1 d D U . . .
N5 N 0.53482(9) 0.51268(10) 0.62395(9) 0.0728(4) Uani 1 1 d . . . . .
N6 N 0.64652(10) 0.54975(11) 0.65206(11) 0.0815(5) Uani 1 1 d . . . . .
C1 C 0.21449(13) 0.31449(12) 0.18438(11) 0.0809(5) Uani 1 1 d . . . . .
H1A H 0.240988 0.287582 0.163696 0.097 Uiso 1 1 calc R U . . .
C2 C 0.16311(17) 0.33682(15) 0.15375(14) 0.0958(8) Uani 1 1 d . . . . .
H2A H 0.154756 0.324277 0.113418 0.115 Uiso 1 1 calc R U . . .
C3 C 0.12445(17) 0.37761(17) 0.18319(16) 0.1036(9) Uani 1 1 d . . . . .
H3B H 0.089464 0.392763 0.163169 0.124 Uiso 1 1 calc R U . . .
C4 C 0.13804(15) 0.39600(15) 0.24297(15) 0.0929(7) Uani 1 1 d . . . . .
H4B H 0.113209 0.424642 0.263397 0.111 Uiso 1 1 calc R U . . .
C5 C 0.18960(10) 0.37070(11) 0.27181(10) 0.0716(4) Uani 1 1 d . . . . .
C6 C 0.20725(10) 0.38359(10) 0.33568(10) 0.0686(4) Uani 1 1 d . . . . .
C7 C 0.17959(10) 0.41707(12) 0.38338(11) 0.0750(5) Uani 1 1 d . . . . .
H7A H 0.142851 0.439480 0.381848 0.090 Uiso 1 1 calc R U . . .
C8 C 0.21857(9) 0.40970(10) 0.43330(10) 0.0682(4) Uani 1 1 d . . . . .
C9 C 0.21312(9) 0.43444(11) 0.49662(10) 0.0722(5) Uani 1 1 d . . . . .
C10 C 0.16532(13) 0.47566(16) 0.50948(14) 0.0887(7) Uani 1 1 d . . . . .
H10A H 0.138532 0.488169 0.478171 0.106 Uiso 1 1 calc R U . . .
C11 C 0.15782(16) 0.4980(2) 0.56918(17) 0.1111(11) Uani 1 1 d . . . . .
H11A H 0.126001 0.525674 0.577852 0.133 Uiso 1 1 calc R U . . .
C12 C 0.19659(15) 0.4797(2) 0.61494(15) 0.1083(11) Uani 1 1 d . . . . .
H12A H 0.190229 0.494217 0.654971 0.130 Uiso 1 1 calc R U . . .
C13 C 0.24552(11) 0.43982(15) 0.60344(11) 0.0827(6) Uani 1 1 d . . . . .
C14 C 0.25300(10) 0.41696(13) 0.54335(10) 0.0764(5) Uani 1 1 d . . . . .
H14A H 0.285193 0.389682 0.534794 0.092 Uiso 1 1 calc R U . . .
C15 C 0.29170(13) 0.42701(16) 0.65132(11) 0.0877(7) Uani 1 1 d . . . . .
C16 C 0.27675(18) 0.4038(3) 0.70975(16) 0.1243(15) Uani 1 1 d . . . . .
H16A H 0.235782 0.394826 0.719481 0.149 Uiso 1 1 calc R U . . .
C17 C 0.3226(2) 0.3942(3) 0.75300(16) 0.143(2) Uani 1 1 d . . . . .
H17A H 0.312467 0.376649 0.791013 0.171 Uiso 1 1 calc R U . . .
C18 C 0.38300(18) 0.4099(2) 0.74099(14) 0.1161(12) Uani 1 1 d . . . . .
H18A H 0.413119 0.404398 0.771259 0.139 Uiso 1 1 calc R U . . .
C19 C 0.39923(12) 0.43432(14) 0.68323(11) 0.0821(6) Uani 1 1 d . . . . .
C20 C 0.35362(11) 0.44123(13) 0.63944(10) 0.0783(5) Uani 1 1 d . . . . .
H20A H 0.364396 0.455930 0.600434 0.094 Uiso 1 1 calc R U . . .
C21 C 0.46179(11) 0.45791(12) 0.67230(10) 0.0741(5) Uani 1 1 d . . . . .
C22 C 0.51420(12) 0.45604(13) 0.70886(12) 0.0808(5) Uani 1 1 d . . . . .
H22A H 0.519034 0.435827 0.746567 0.097 Uiso 1 1 calc R U . . .
C23 C 0.55804(12) 0.49069(11) 0.67739(11) 0.0743(5) Uani 1 1 d . . . . .
C24 C 0.62167(12) 0.50873(12) 0.69210(13) 0.0805(5) Uani 1 1 d . . . . .
C25 C 0.65317(17) 0.48605(18) 0.74331(19) 0.1055(10) Uani 1 1 d . . . . .
H25A H 0.634146 0.458609 0.770493 0.127 Uiso 1 1 calc R U . . .
C26 C 0.7126(2) 0.5049(2) 0.7528(3) 0.1355(16) Uani 1 1 d . . . . .
H26A H 0.735093 0.489692 0.786264 0.163 Uiso 1 1 calc R U . . .
C27 C 0.73936(17) 0.5469(3) 0.7123(3) 0.1325(15) Uani 1 1 d . . . . .
H27A H 0.779600 0.560869 0.718667 0.159 Uiso 1 1 calc R U . . .
C28 C 0.70536(15) 0.56765(18) 0.6626(2) 0.1090(10) Uani 1 1 d . . . . .
H28A H 0.723765 0.595172 0.635063 0.131 Uiso 1 1 calc R U . . .
Fe3 Fe 0.44048(2) 0.44048(2) 0.44048(2) 0.06603(13) Uani 1 3 d S T P . .
O1 O 0.38959(6) 0.36972(7) 0.47239(7) 0.0666(3) Uani 1 1 d . . . . .
O2 O 0.50081(7) 0.40856(8) 0.50263(8) 0.0706(3) Uani 1 1 d . . . . .
O3 O 0.52442(13) 0.24036(17) 0.63760(14) 0.1320(11) Uani 1 1 d . . . . .
O4 O 0.40855(14) 0.20406(16) 0.61156(15) 0.1340(11) Uani 1 1 d . U . . .
C29 C 0.41750(9) 0.33703(10) 0.51528(9) 0.0651(4) Uani 1 1 d . . . . .
C30 C 0.48195(9) 0.35855(10) 0.53134(10) 0.0676(4) Uani 1 1 d . . . . .
C31 C 0.51708(12) 0.32634(15) 0.57202(12) 0.0860(7) Uani 1 1 d . . . . .
H31A H 0.556788 0.340303 0.581113 0.103 Uiso 1 1 calc R U . . .
C32 C 0.49479(13) 0.27163(16) 0.60125(13) 0.0911(7) Uani 1 1 d . U . . .
C33 C 0.42748(13) 0.25087(15) 0.58617(13) 0.0897(7) Uani 1 1 d . U . . .
C34 C 0.39255(11) 0.28698(13) 0.54342(11) 0.0771(5) Uani 1 1 d . . . . .
H34A H 0.351858 0.275930 0.534718 0.092 Uiso 1 1 calc R U . . .
O1S O -0.0356(6) 0.4410(7) 0.3672(9) 0.306(7) Uani 0.762(13) 1 d . U P . .
H1S H -0.025104 0.477347 0.370260 0.458 Uiso 0.762(13) 1 calc R U P . .
C1S C 0.0169(5) 0.4040(4) 0.3552(6) 0.179(4) Uani 0.762(13) 1 d . U P . .
H1S1 H 0.045294 0.407077 0.389304 0.268 Uiso 0.762(13) 1 calc R U P . .
H1S2 H 0.036844 0.418107 0.318066 0.268 Uiso 0.762(13) 1 calc R U P . .
H1S3 H 0.004411 0.361654 0.350147 0.268 Uiso 0.762(13) 1 calc R U P . .
B1 B 0.1343(8) 0.1291(10) 0.1319(10) 0.138(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1228(8) 0.1712(10) 0.0856(8) 0.174(7) Uani 0.3333 1 d D U P A -1
F2 F 0.1883(5) 0.1436(8) 0.1633(8) 0.198(5) Uani 0.3333 1 d D U P A -1
F3 F 0.0844(8) 0.1235(10) 0.1708(8) 0.179(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1452(9) 0.0709(8) 0.1045(9) 0.193(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9748(18) . ?
Fe1 N2 1.9749(18) 9 ?
Fe1 N2 1.9749(18) 5 ?
Fe1 N1 2.0262(18) . ?
Fe1 N1 2.0262(18) 9 ?
Fe1 N1 2.0262(18) 5 ?
Fe2 N5 2.071(2) 9 ?
Fe2 N5 2.071(2) 5 ?
Fe2 N5 2.071(2) . ?
Fe2 N6 2.117(2) . ?
Fe2 N6 2.117(2) 9 ?
Fe2 N6 2.117(2) 5 ?
N1 C1 1.345(3) . ?
N1 C5 1.347(3) . ?
N2 C6 1.331(3) . ?
N2 N3 1.349(2) . ?
N3 C8 1.359(3) . ?
N3 H3 0.88(2) . ?
N4 N5 1.343(3) . ?
N4 C21 1.357(3) . ?
N4 H4 0.88(2) . ?
N5 C23 1.345(3) . ?
N6 C28 1.348(4) . ?
N6 C24 1.349(4) . ?
C1 C2 1.379(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.370(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.383(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.388(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.458(3) . ?
C6 C7 1.394(3) . ?
C7 C8 1.377(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.473(3) . ?
C9 C14 1.380(4) . ?
C9 C10 1.391(3) . ?
C10 C11 1.386(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.354(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.386(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.398(3) . ?
C13 C15 1.463(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.396(4) . ?
C15 C20 1.396(3) . ?
C16 C17 1.377(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.373(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.399(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.374(4) . ?
C19 C21 1.463(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(3) . ?
C22 C23 1.385(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.464(4) . ?
C24 C25 1.388(4) . ?
C25 C26 1.363(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.387(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.376(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9936(15) 5 ?
Fe3 O2 1.9937(15) 9 ?
Fe3 O2 1.9937(15) . ?
Fe3 O1 2.0047(15) . ?
Fe3 O1 2.0047(15) 5 ?
Fe3 O1 2.0047(15) 9 ?
O1 C29 1.312(2) . ?
O2 C30 1.311(3) . ?
O3 C32 1.218(4) . ?
O4 C33 1.221(3) . ?
C29 C34 1.352(3) . ?
C29 C30 1.508(3) . ?
C30 C31 1.353(3) . ?
C31 C32 1.424(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.556(4) . ?
C33 C34 1.425(3) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.413(14) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F3 1.373(19) . ?
B1 F1 1.374(18) . ?
B1 F2 1.384(14) . ?
B1 F4 1.409(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.09(7) . 9 ?
N2 Fe1 N2 96.09(7) . 5 ?
N2 Fe1 N2 96.09(7) 9 5 ?
N2 Fe1 N1 79.89(7) . . ?
N2 Fe1 N1 91.90(7) 9 . ?
N2 Fe1 N1 171.41(7) 5 . ?
N2 Fe1 N1 171.41(7) . 9 ?
N2 Fe1 N1 79.89(7) 9 9 ?
N2 Fe1 N1 91.90(7) 5 9 ?
N1 Fe1 N1 92.60(7) . 9 ?
N2 Fe1 N1 91.89(7) . 5 ?
N2 Fe1 N1 171.42(7) 9 5 ?
N2 Fe1 N1 79.89(7) 5 5 ?
N1 Fe1 N1 92.60(7) . 5 ?
N1 Fe1 N1 92.60(7) 9 5 ?
N5 Fe2 N5 97.57(7) 9 5 ?
N5 Fe2 N5 97.57(7) 9 . ?
N5 Fe2 N5 97.57(7) 5 . ?
N5 Fe2 N6 167.73(8) 9 . ?
N5 Fe2 N6 94.15(8) 5 . ?
N5 Fe2 N6 77.22(8) . . ?
N5 Fe2 N6 77.22(8) 9 9 ?
N5 Fe2 N6 167.73(8) 5 9 ?
N5 Fe2 N6 94.15(8) . 9 ?
N6 Fe2 N6 91.96(9) . 9 ?
N5 Fe2 N6 94.15(8) 9 5 ?
N5 Fe2 N6 77.22(8) 5 5 ?
N5 Fe2 N6 167.73(8) . 5 ?
N6 Fe2 N6 91.96(9) . 5 ?
N6 Fe2 N6 91.96(9) 9 5 ?
C1 N1 C5 118.0(2) . . ?
C1 N1 Fe1 127.18(17) . . ?
C5 N1 Fe1 114.71(14) . . ?
C6 N2 N3 105.89(17) . . ?
C6 N2 Fe1 115.80(14) . . ?
N3 N2 Fe1 137.00(13) . . ?
N2 N3 C8 110.82(17) . . ?
N2 N3 H3 116(2) . . ?
C8 N3 H3 132(2) . . ?
N5 N4 C21 111.46(19) . . ?
N5 N4 H4 118(3) . . ?
C21 N4 H4 129(3) . . ?
N4 N5 C23 105.5(2) . . ?
N4 N5 Fe2 135.98(15) . . ?
C23 N5 Fe2 115.06(17) . . ?
C28 N6 C24 117.1(3) . . ?
C28 N6 Fe2 127.6(2) . . ?
C24 N6 Fe2 115.04(16) . . ?
N1 C1 C2 122.2(3) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 H4B 120.8 . . ?
C5 C4 H4B 120.8 . . ?
N1 C5 C4 122.5(2) . . ?
N1 C5 C6 113.49(19) . . ?
C4 C5 C6 124.0(2) . . ?
N2 C6 C7 111.16(19) . . ?
N2 C6 C5 115.46(19) . . ?
C7 C6 C5 133.4(2) . . ?
C8 C7 C6 104.88(19) . . ?
C8 C7 H7A 127.6 . . ?
C6 C7 H7A 127.6 . . ?
N3 C8 C7 107.25(19) . . ?
N3 C8 C9 123.24(19) . . ?
C7 C8 C9 129.5(2) . . ?
C14 C9 C10 119.5(2) . . ?
C14 C9 C8 122.0(2) . . ?
C10 C9 C8 118.5(2) . . ?
C11 C10 C9 119.7(3) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.3(3) . . ?
C12 C13 C15 120.7(3) . . ?
C14 C13 C15 120.7(2) . . ?
C9 C14 C13 120.7(2) . . ?
C9 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C16 C15 C20 117.8(3) . . ?
C16 C15 C13 123.3(3) . . ?
C20 C15 C13 118.8(2) . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C18 C17 C16 121.2(3) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 120.0(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C18 118.4(3) . . ?
C20 C19 C21 120.9(2) . . ?
C18 C19 C21 120.4(3) . . ?
C19 C20 C15 122.4(2) . . ?
C19 C20 H20A 118.8 . . ?
C15 C20 H20A 118.8 . . ?
N4 C21 C22 106.8(2) . . ?
N4 C21 C19 122.1(2) . . ?
C22 C21 C19 130.9(2) . . ?
C21 C22 C23 105.3(2) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 110.9(2) . . ?
N5 C23 C24 116.3(2) . . ?
C22 C23 C24 132.8(2) . . ?
N6 C24 C25 123.2(3) . . ?
N6 C24 C23 114.2(2) . . ?
C25 C24 C23 122.6(3) . . ?
C26 C25 C24 118.5(4) . . ?
C26 C25 H25A 120.8 . . ?
C24 C25 H25A 120.8 . . ?
C25 C26 C27 119.5(4) . . ?
C25 C26 H26A 120.2 . . ?
C27 C26 H26A 120.2 . . ?
C28 C27 C26 118.9(3) . . ?
C28 C27 H27A 120.6 . . ?
C26 C27 H27A 120.6 . . ?
N6 C28 C27 122.8(4) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 91.08(7) 5 9 ?
O2 Fe3 O2 91.08(7) 5 . ?
O2 Fe3 O2 91.08(7) 9 . ?
O2 Fe3 O1 170.50(6) 5 . ?
O2 Fe3 O1 95.68(7) 9 . ?
O2 Fe3 O1 82.14(6) . . ?
O2 Fe3 O1 82.14(6) 5 5 ?
O2 Fe3 O1 170.50(6) 9 5 ?
O2 Fe3 O1 95.68(7) . 5 ?
O1 Fe3 O1 91.86(6) . 5 ?
O2 Fe3 O1 95.68(7) 5 9 ?
O2 Fe3 O1 82.14(6) 9 9 ?
O2 Fe3 O1 170.50(6) . 9 ?
O1 Fe3 O1 91.87(6) . 9 ?
O1 Fe3 O1 91.86(6) 5 9 ?
C29 O1 Fe3 113.66(12) . . ?
C30 O2 Fe3 113.61(13) . . ?
O1 C29 C34 124.39(19) . . ?
O1 C29 C30 114.88(18) . . ?
C34 C29 C30 120.72(19) . . ?
O2 C30 C31 123.8(2) . . ?
O2 C30 C29 115.60(18) . . ?
C31 C30 C29 120.6(2) . . ?
C30 C31 C32 121.7(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.7(3) . . ?
O3 C32 C33 117.8(3) . . ?
C31 C32 C33 117.6(2) . . ?
O4 C33 C34 124.6(3) . . ?
O4 C33 C32 117.2(3) . . ?
C34 C33 C32 118.2(2) . . ?
C29 C34 C33 121.2(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F3 B1 F1 111.2(15) . . ?
F3 B1 F2 112.4(16) . . ?
F1 B1 F2 111.0(16) . . ?
F3 B1 F4 108.0(17) . . ?
F1 B1 F4 108.4(16) . . ?
F2 B1 F4 105.5(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(2) 2.08(3) 2.943(2) 165(3) . yes
N4 H4 O2 0.88(2) 2.12(2) 3.002(2) 178(4) 9 yes

_refine_diff_density_max         0.182
_refine_diff_density_min         -0.194
_refine_diff_density_rms         0.041

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_300K
_database_code_depnum_ccdc_archive 'CCDC 2260942'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.855(3)
_cell_length_b                   21.855(3)
_cell_length_c                   21.855(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10439(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6724
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      34.00

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.521
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            171961
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.352
_diffrn_reflns_theta_max         29.519
_diffrn_reflns_theta_full        29.519
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9009
_reflns_number_gt                8668
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disorder by symmetry and was refined with both distance
 and displacement parameters restraints.
 The anilate is disordered over two equivalent positions sharing the 
 coordinated C-O groups. The two components were refined with displacement
 parameters restraints as well as a FLAT restraint for the C atoms. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1125 cubic angstrom with a total of 117 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
 
 Details of SQUEEZE results (before BF4 disorder refinement):

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.080  0.176  0.170      1125       117 ' '
   2  0.138  0.362  0.638        11         0 ' '
   3  0.361  0.638  0.138        11         0 ' '
   4  0.638  0.138  0.362        11         0 ' '
   5  0.861  0.861  0.861        11         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?


 Details of SQUEEZE results on a 200 K data set of the same crystal
 after measurements up to 400 K:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.084  0.137  0.139      1771        72 ' '
   2  0.106  0.394  0.606        10         0 ' '
   3  0.394  0.606  0.106        10         0 ' '
   4  0.606  0.106  0.394        10         0 ' '
   5  0.894  0.894  0.894        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_300K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1125 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1125 cubic angstrom with a total of 117 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 72 electron per cell at 200 K,
 after measurements done up to 380 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1221P)²+0.0335P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.039(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3879 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.081(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9009
_refine_ls_number_parameters     476
_refine_ls_number_restraints     89
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0487
_refine_ls_wR_factor_ref         0.1397
_refine_ls_wR_factor_gt          0.1382
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29640(2) 0.29640(2) 0.29640(2) 0.06592(16) Uani 1 3 d S T P . .
Fe2 Fe 0.57732(2) 0.57732(2) 0.57732(2) 0.07582(18) Uani 1 3 d S T P . .
N1 N 0.23436(10) 0.33045(10) 0.23766(10) 0.0744(4) Uani 1 1 d . . . . .
N2 N 0.26010(9) 0.35994(10) 0.34825(9) 0.0693(4) Uani 1 1 d . . . . .
N3 N 0.26293(9) 0.37621(10) 0.40780(10) 0.0722(4) Uani 1 1 d . . . . .
H3 H 0.294(3) 0.367(2) 0.426(2) 0.108 Uiso 1 1 d . U . . .
N4 N 0.46707(11) 0.49599(12) 0.61164(10) 0.0779(5) Uani 1 1 d . . . . .
H4 H 0.444(3) 0.495(3) 0.582(3) 0.117 Uiso 1 1 d . U . . .
N5 N 0.52637(11) 0.51208(12) 0.61385(10) 0.0781(5) Uani 1 1 d . . . . .
N6 N 0.63634(13) 0.54335(16) 0.64022(14) 0.0936(7) Uani 1 1 d . . . . .
C1 C 0.22548(16) 0.31369(15) 0.17959(13) 0.0852(6) Uani 1 1 d . . . . .
H1A H 0.251095 0.284298 0.162555 0.102 Uiso 1 1 calc R U . . .
C2 C 0.1792(2) 0.33868(19) 0.14369(17) 0.1054(11) Uani 1 1 d . . . . .
H2A H 0.173567 0.325446 0.103640 0.126 Uiso 1 1 calc R U . . .
C3 C 0.1420(2) 0.3831(2) 0.1680(2) 0.1091(11) Uani 1 1 d . . . . .
H3B H 0.111013 0.400514 0.144655 0.131 Uiso 1 1 calc R U . . .
C4 C 0.1515(2) 0.40161(18) 0.22831(19) 0.1025(10) Uani 1 1 d . . . . .
H4B H 0.127138 0.431900 0.245662 0.123 Uiso 1 1 calc R U . . .
C5 C 0.19755(13) 0.37432(13) 0.26190(13) 0.0796(6) Uani 1 1 d . . . . .
C6 C 0.21053(12) 0.38819(12) 0.32513(13) 0.0771(5) Uani 1 1 d . . . . .
C7 C 0.18207(13) 0.42353(15) 0.37019(16) 0.0877(7) Uani 1 1 d . . . . .
H7A H 0.147164 0.447479 0.365913 0.105 Uiso 1 1 calc R U . . .
C8 C 0.21634(11) 0.41547(13) 0.42187(14) 0.0788(6) Uani 1 1 d . . . . .
C9 C 0.20840(12) 0.44126(14) 0.48381(15) 0.0843(6) Uani 1 1 d . . . . .
C10 C 0.15868(18) 0.4802(2) 0.4944(2) 0.1093(11) Uani 1 1 d . . . . .
H10A H 0.132817 0.491397 0.462541 0.131 Uiso 1 1 calc R U . . .
C11 C 0.1486(2) 0.5019(3) 0.5529(3) 0.1364(19) Uani 1 1 d . . . . .
H11A H 0.115223 0.527231 0.560310 0.164 Uiso 1 1 calc R U . . .
C12 C 0.1867(2) 0.4866(3) 0.6000(2) 0.1271(16) Uani 1 1 d . . . . .
H12A H 0.178887 0.501290 0.639214 0.152 Uiso 1 1 calc R U . . .
C13 C 0.23629(15) 0.4499(2) 0.58971(16) 0.0984(9) Uani 1 1 d . . . . .
C14 C 0.24632(13) 0.42615(16) 0.53115(14) 0.0858(7) Uani 1 1 d . . . . .
H14A H 0.279072 0.399834 0.524384 0.103 Uiso 1 1 calc R U . . .
C15 C 0.28180(16) 0.4367(2) 0.63817(14) 0.1012(10) Uani 1 1 d . . . . .
C16 C 0.2664(3) 0.4141(4) 0.6961(2) 0.142(2) Uani 1 1 d . . . . .
H16A H 0.225824 0.404652 0.704640 0.171 Uiso 1 1 calc R U . . .
C17 C 0.3089(3) 0.4058(4) 0.7396(2) 0.142(2) Uani 1 1 d . . . . .
H17A H 0.297158 0.391758 0.778080 0.171 Uiso 1 1 calc R U . . .
C18 C 0.3703(3) 0.4179(3) 0.72788(17) 0.1251(16) Uani 1 1 d . . . . .
H18A H 0.399646 0.410463 0.757800 0.150 Uiso 1 1 calc R U . . .
C19 C 0.38779(16) 0.44127(19) 0.67076(13) 0.0923(8) Uani 1 1 d . . . . .
C20 C 0.34347(15) 0.44914(17) 0.62703(13) 0.0910(7) Uani 1 1 d . . . . .
H20A H 0.354921 0.463247 0.588552 0.109 Uiso 1 1 calc R U . . .
C21 C 0.45117(16) 0.46097(15) 0.66031(12) 0.0853(6) Uani 1 1 d . . . . .
C22 C 0.50374(19) 0.45510(17) 0.69604(14) 0.0941(8) Uani 1 1 d . . . . .
H22A H 0.507735 0.434063 0.732810 0.113 Uiso 1 1 calc R U . . .
C23 C 0.54836(15) 0.48704(15) 0.66532(14) 0.0853(6) Uani 1 1 d . . . . .
C24 C 0.61238(16) 0.50185(18) 0.67879(16) 0.0946(8) Uani 1 1 d . . . . .
C25 C 0.6435(2) 0.4762(3) 0.7276(2) 0.1263(15) Uani 1 1 d . . . . .
H25A H 0.624493 0.449168 0.754353 0.152 Uiso 1 1 calc R U . . .
C26 C 0.7048(3) 0.4926(4) 0.7347(3) 0.155(2) Uani 1 1 d . . . . .
H26A H 0.728642 0.473411 0.764319 0.186 Uiso 1 1 calc R U . . .
C27 C 0.7306(3) 0.5381(4) 0.6973(4) 0.156(2) Uani 1 1 d . . . . .
H27A H 0.769850 0.552917 0.704409 0.187 Uiso 1 1 calc R U . . .
C28 C 0.6949(2) 0.5602(3) 0.6490(3) 0.1246(15) Uani 1 1 d . . . . .
H28A H 0.712462 0.587814 0.621691 0.150 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43562(2) 0.43562(2) 0.43562(2) 0.06704(16) Uani 1 3 d S T P . .
O1 O 0.38220(7) 0.36859(8) 0.46871(8) 0.0699(3) Uani 1 1 d . . . . .
O2 O 0.49158(7) 0.40487(8) 0.50090(8) 0.0713(4) Uani 1 1 d . . . . .
O3 O 0.5020(2) 0.2539(4) 0.6510(3) 0.228(4) Uani 1 1 d . U . . .
O4 O 0.3880(2) 0.2180(3) 0.6220(2) 0.175(2) Uani 1 1 d . U . . .
C29 C 0.40627(10) 0.33912(12) 0.51467(10) 0.0705(5) Uani 1 1 d . . . . .
C30 C 0.46967(11) 0.35924(12) 0.53216(11) 0.0732(5) Uani 1 1 d . . . . .
C31 C 0.50094(16) 0.3304(2) 0.57700(17) 0.1064(12) Uani 1 1 d . . . . .
H31A H 0.540323 0.343352 0.586597 0.128 Uiso 1 1 calc R U . . .
C32 C 0.4751(2) 0.2812(3) 0.6095(2) 0.134(2) Uani 1 1 d . U . . .
C33 C 0.4099(2) 0.2600(3) 0.5926(2) 0.1220(15) Uani 1 1 d . U . . .
C34 C 0.37877(14) 0.29198(17) 0.54504(15) 0.0900(7) Uani 1 1 d . . . . .
H34A H 0.339152 0.280534 0.534550 0.108 Uiso 1 1 calc R U . . .
O1S O 0.0406(15) 0.4714(9) 0.3651(10) 0.482(13) Uani 1 1 d . U . . .
H1S H 0.011338 0.494061 0.371064 0.723 Uiso 1 1 d R U . . .
C1S C 0.0147(18) 0.4104(12) 0.3444(12) 0.436(14) Uani 1 1 d . U . . .
H1S1 H 0.037639 0.397012 0.309369 0.654 Uiso 1 1 d R U . . .
H1S2 H -0.027881 0.413012 0.333799 0.654 Uiso 1 1 d R U . . .
H1S3 H 0.019859 0.381592 0.377139 0.654 Uiso 1 1 d R U . . .
B1 B 0.1415(10) 0.1433(9) 0.1416(10) 0.130(2) Uani 0.3333 1 d D U P A -1
F1 F 0.1377(12) 0.1889(8) 0.1000(8) 0.167(7) Uani 0.3333 1 d D U P A -1
F2 F 0.1906(7) 0.1474(9) 0.1769(11) 0.203(7) Uani 0.3333 1 d D U P A -1
F3 F 0.0892(9) 0.1426(10) 0.1747(11) 0.170(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1465(11) 0.0886(7) 0.1115(10) 0.195(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.960(2) 9 ?
Fe1 N2 1.960(2) 5 ?
Fe1 N2 1.960(2) . ?
Fe1 N1 2.010(2) . ?
Fe1 N1 2.010(2) 9 ?
Fe1 N1 2.010(2) 5 ?
Fe2 N5 1.978(3) . ?
Fe2 N5 1.978(3) 9 ?
Fe2 N5 1.978(3) 5 ?
Fe2 N6 2.026(3) 9 ?
Fe2 N6 2.026(3) 5 ?
Fe2 N6 2.026(3) . ?
N1 C1 1.335(4) . ?
N1 C5 1.359(4) . ?
N2 C6 1.345(3) . ?
N2 N3 1.350(3) . ?
N3 C8 1.367(3) . ?
N3 H3 0.81(6) . ?
N4 N5 1.344(4) . ?
N4 C21 1.356(4) . ?
N4 H4 0.82(6) . ?
N5 C23 1.340(4) . ?
N6 C24 1.344(5) . ?
N6 C28 1.346(5) . ?
C1 C2 1.391(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.373(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.394(6) . ?
C3 H3B 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H4B 0.9300 . ?
C5 C6 1.443(4) . ?
C6 C7 1.398(4) . ?
C7 C8 1.367(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.477(4) . ?
C9 C14 1.366(5) . ?
C9 C10 1.400(5) . ?
C10 C11 1.380(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.366(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.367(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.399(4) . ?
C13 C15 1.481(6) . ?
C14 H14A 0.9300 . ?
C15 C20 1.396(5) . ?
C15 C16 1.401(5) . ?
C16 C17 1.341(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.392(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.402(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.371(5) . ?
C19 C21 1.468(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.395(5) . ?
C22 C23 1.374(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.466(5) . ?
C24 C25 1.384(5) . ?
C25 C26 1.395(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.405(11) . ?
C26 H26A 0.9300 . ?
C27 C28 1.399(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9958(16) 5 ?
Fe3 O2 1.9958(16) 9 ?
Fe3 O2 1.9958(16) . ?
Fe3 O1 2.0078(17) . ?
Fe3 O1 2.0078(17) 5 ?
Fe3 O1 2.0078(17) 9 ?
O1 C29 1.304(3) . ?
O2 C30 1.300(3) . ?
O3 C32 1.234(5) . ?
O4 C33 1.219(5) . ?
C29 C34 1.365(4) . ?
C29 C30 1.503(3) . ?
C30 C31 1.351(4) . ?
C31 C32 1.407(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.542(6) . ?
C33 C34 1.425(5) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.52(3) . ?
O1S H1S 0.8197 . ?
C1S H1S1 0.9602 . ?
C1S H1S2 0.9599 . ?
C1S H1S3 0.9601 . ?
B1 F2 1.324(17) . ?
B1 F1 1.35(2) . ?
B1 F3 1.35(2) . ?
B1 F4 1.369(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.38(8) 9 5 ?
N2 Fe1 N2 96.38(8) 9 . ?
N2 Fe1 N2 96.38(8) 5 . ?
N2 Fe1 N1 90.30(9) 9 . ?
N2 Fe1 N1 172.90(9) 5 . ?
N2 Fe1 N1 80.44(9) . . ?
N2 Fe1 N1 80.44(9) 9 9 ?
N2 Fe1 N1 90.30(9) 5 9 ?
N2 Fe1 N1 172.90(9) . 9 ?
N1 Fe1 N1 93.18(9) . 9 ?
N2 Fe1 N1 172.90(9) 9 5 ?
N2 Fe1 N1 80.44(9) 5 5 ?
N2 Fe1 N1 90.30(9) . 5 ?
N1 Fe1 N1 93.19(9) . 5 ?
N1 Fe1 N1 93.19(9) 9 5 ?
N5 Fe2 N5 96.45(9) . 9 ?
N5 Fe2 N5 96.45(9) . 5 ?
N5 Fe2 N5 96.45(9) 9 5 ?
N5 Fe2 N6 91.48(11) . 9 ?
N5 Fe2 N6 79.65(11) 9 9 ?
N5 Fe2 N6 171.53(11) 5 9 ?
N5 Fe2 N6 171.53(11) . 5 ?
N5 Fe2 N6 91.48(11) 9 5 ?
N5 Fe2 N6 79.65(11) 5 5 ?
N6 Fe2 N6 92.87(13) 9 5 ?
N5 Fe2 N6 79.65(11) . . ?
N5 Fe2 N6 171.53(11) 9 . ?
N5 Fe2 N6 91.48(11) 5 . ?
N6 Fe2 N6 92.87(13) 9 . ?
N6 Fe2 N6 92.87(13) 5 . ?
C1 N1 C5 118.5(2) . . ?
C1 N1 Fe1 127.1(2) . . ?
C5 N1 Fe1 114.31(18) . . ?
C6 N2 N3 106.2(2) . . ?
C6 N2 Fe1 115.70(18) . . ?
N3 N2 Fe1 136.48(16) . . ?
N2 N3 C8 110.4(2) . . ?
N2 N3 H3 116(4) . . ?
C8 N3 H3 132(4) . . ?
N5 N4 C21 111.5(2) . . ?
N5 N4 H4 129(4) . . ?
C21 N4 H4 116(4) . . ?
C23 N5 N4 105.6(3) . . ?
C23 N5 Fe2 115.5(2) . . ?
N4 N5 Fe2 135.83(19) . . ?
C24 N6 C28 117.8(3) . . ?
C24 N6 Fe2 115.1(2) . . ?
C28 N6 Fe2 127.0(3) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 118.9(3) . . ?
C2 C3 H3B 120.5 . . ?
C4 C3 H3B 120.5 . . ?
C5 C4 C3 119.0(3) . . ?
C5 C4 H4B 120.5 . . ?
C3 C4 H4B 120.5 . . ?
N1 C5 C4 121.9(3) . . ?
N1 C5 C6 113.9(2) . . ?
C4 C5 C6 124.2(3) . . ?
N2 C6 C7 110.3(3) . . ?
N2 C6 C5 114.9(2) . . ?
C7 C6 C5 134.7(3) . . ?
C8 C7 C6 105.5(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 107.7(2) . . ?
N3 C8 C9 122.2(3) . . ?
C7 C8 C9 130.1(2) . . ?
C14 C9 C10 119.5(3) . . ?
C14 C9 C8 122.0(3) . . ?
C10 C9 C8 118.4(3) . . ?
C11 C10 C9 119.1(5) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
C12 C11 C10 121.1(4) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C11 C12 C13 120.1(4) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C12 C13 C14 119.6(4) . . ?
C12 C13 C15 121.9(3) . . ?
C14 C13 C15 118.5(3) . . ?
C9 C14 C13 120.5(3) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C20 C15 C16 117.2(4) . . ?
C20 C15 C13 119.1(3) . . ?
C16 C15 C13 123.7(4) . . ?
C17 C16 C15 121.6(4) . . ?
C17 C16 H16A 119.2 . . ?
C15 C16 H16A 119.2 . . ?
C16 C17 C18 120.7(4) . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C17 C18 C19 119.8(4) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 118.3(4) . . ?
C20 C19 C21 121.4(3) . . ?
C18 C19 C21 120.2(4) . . ?
C19 C20 C15 122.4(3) . . ?
C19 C20 H20A 118.8 . . ?
C15 C20 H20A 118.8 . . ?
N4 C21 C22 106.3(3) . . ?
N4 C21 C19 122.0(3) . . ?
C22 C21 C19 131.5(3) . . ?
C23 C22 C21 105.3(3) . . ?
C23 C22 H22A 127.3 . . ?
C21 C22 H22A 127.3 . . ?
N5 C23 C22 111.3(3) . . ?
N5 C23 C24 114.9(3) . . ?
C22 C23 C24 133.7(3) . . ?
N6 C24 C25 124.4(4) . . ?
N6 C24 C23 113.3(3) . . ?
C25 C24 C23 122.3(4) . . ?
C24 C25 C26 117.1(6) . . ?
C24 C25 H25A 121.5 . . ?
C26 C25 H25A 121.5 . . ?
C25 C26 C27 120.1(5) . . ?
C25 C26 H26A 120.0 . . ?
C27 C26 H26A 120.0 . . ?
C28 C27 C26 117.5(5) . . ?
C28 C27 H27A 121.3 . . ?
C26 C27 H27A 121.3 . . ?
N6 C28 C27 122.8(5) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 90.51(8) 5 9 ?
O2 Fe3 O2 90.51(8) 5 . ?
O2 Fe3 O2 90.51(8) 9 . ?
O2 Fe3 O1 169.74(7) 5 . ?
O2 Fe3 O1 96.03(7) 9 . ?
O2 Fe3 O1 81.56(6) . . ?
O2 Fe3 O1 81.55(6) 5 5 ?
O2 Fe3 O1 169.74(7) 9 5 ?
O2 Fe3 O1 96.03(7) . 5 ?
O1 Fe3 O1 92.76(7) . 5 ?
O2 Fe3 O1 96.03(7) 5 9 ?
O2 Fe3 O1 81.55(6) 9 9 ?
O2 Fe3 O1 169.74(7) . 9 ?
O1 Fe3 O1 92.76(7) . 9 ?
O1 Fe3 O1 92.76(7) 5 9 ?
C29 O1 Fe3 113.79(14) . . ?
C30 O2 Fe3 114.09(15) . . ?
O1 C29 C34 124.7(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.2(2) . . ?
O2 C30 C31 123.6(2) . . ?
O2 C30 C29 115.5(2) . . ?
C31 C30 C29 121.0(2) . . ?
C30 C31 C32 121.3(3) . . ?
C30 C31 H31A 119.3 . . ?
C32 C31 H31A 119.3 . . ?
O3 C32 C31 123.4(4) . . ?
O3 C32 C33 118.0(4) . . ?
C31 C32 C33 118.6(3) . . ?
O4 C33 C34 124.4(4) . . ?
O4 C33 C32 117.6(4) . . ?
C34 C33 C32 118.0(3) . . ?
C29 C34 C33 120.9(3) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 106.6 . . ?
O1S C1S H1S1 108.0 . . ?
O1S C1S H1S2 112.4 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 108.0 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F1 113.1(17) . . ?
F2 B1 F3 111.9(17) . . ?
F1 B1 F3 108.4(18) . . ?
F2 B1 F4 105.9(17) . . ?
F1 B1 F4 109.1(16) . . ?
F3 B1 F4 108.2(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.81(6) 2.14(6) 2.932(3) 165(5) . yes
N4 H4 O2 0.82(6) 2.16(6) 2.957(3) 164(5) 9 yes

_refine_diff_density_max         0.587
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.071

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_350K
_database_code_depnum_ccdc_archive 'CCDC 2260946'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 1.885(C H4 O)'
_chemical_formula_sum            'C103.88 H73.54 B F4 Fe3 N18 O13.88'
_chemical_formula_weight         2050.48


loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.625(3)
_cell_length_b                   21.625(3)
_cell_length_c                   21.625(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10113(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    6375
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      33.31

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_F_000             421
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.536
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            165620
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0547
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         29.505
_diffrn_reflns_theta_full        29.505
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8713
_reflns_number_gt                8309
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.6283 (i.e. 1.884 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0817P)²+0.1305P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0137(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3695 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8713
_refine_ls_number_parameters     477
_refine_ls_number_restraints     91
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0345
_refine_ls_wR_factor_ref         0.1086
_refine_ls_wR_factor_gt          0.1074
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45283(2) 0.45283(2) 0.45283(2) 0.06697(13) Uani 1 3 d S T P . .
Fe2 Fe 0.16627(2) 0.16627(2) 0.16627(2) 0.07427(15) Uani 1 3 d S T P . .
N1 N 0.50682(9) 0.41900(9) 0.52182(10) 0.0772(4) Uani 1 1 d . . . . .
N2 N 0.39570(8) 0.39171(9) 0.48999(8) 0.0720(4) Uani 1 1 d . . . . .
N3 N 0.33559(9) 0.37599(9) 0.48380(8) 0.0730(4) Uani 1 1 d D . . . .
H3 H 0.3138(18) 0.3796(19) 0.4487(14) 0.109 Uiso 1 1 d D U . . .
N4 N 0.12881(9) 0.25781(11) 0.27495(10) 0.0816(5) Uani 1 1 d D . . . .
H4 H 0.1644(15) 0.249(2) 0.295(2) 0.122 Uiso 1 1 d D U . . .
N5 N 0.12693(9) 0.23825(11) 0.21627(10) 0.0802(4) Uani 1 1 d . . . . .
N6 N 0.09883(13) 0.20113(12) 0.10416(11) 0.0901(5) Uani 1 1 d . . . . .
C1 C 0.56582(12) 0.43535(14) 0.53493(16) 0.0911(6) Uani 1 1 d . . . . .
H1A H 0.586322 0.462627 0.508762 0.109 Uiso 1 1 calc R U . . .
C2 C 0.59618(15) 0.41262(17) 0.58597(18) 0.1060(9) Uani 1 1 d . . . . .
H2A H 0.636258 0.425543 0.594722 0.127 Uiso 1 1 calc R U . . .
C3 C 0.56741(19) 0.37106(19) 0.6238(2) 0.1172(12) Uani 1 1 d . . . . .
H3A H 0.587978 0.355023 0.657976 0.141 Uiso 1 1 calc R U . . .
C4 C 0.50786(17) 0.35311(17) 0.61094(17) 0.1031(8) Uani 1 1 d . . . . .
H4A H 0.487635 0.324546 0.635933 0.124 Uiso 1 1 calc R U . . .
C5 C 0.47860(12) 0.37850(12) 0.55990(12) 0.0806(5) Uani 1 1 d . . . . .
C6 C 0.41440(11) 0.36550(11) 0.54238(11) 0.0764(5) Uani 1 1 d . . . . .
C7 C 0.36734(13) 0.33213(13) 0.56993(12) 0.0845(5) Uani 1 1 d . . . . .
H7A H 0.369252 0.309725 0.606588 0.101 Uiso 1 1 calc R U . . .
C8 C 0.31712(11) 0.33911(12) 0.53157(10) 0.0771(5) Uani 1 1 d . . . . .
C9 C 0.20702(12) 0.33213(14) 0.49752(11) 0.0853(6) Uani 1 1 d . . . . .
H9A H 0.215384 0.359550 0.465460 0.102 Uiso 1 1 calc R U . . .
C10 C 0.25404(12) 0.31445(13) 0.53716(10) 0.0813(5) Uani 1 1 d . . . . .
C11 C 0.24140(17) 0.27343(18) 0.58495(15) 0.1017(8) Uani 1 1 d . . . . .
H11A H 0.272722 0.261438 0.611864 0.122 Uiso 1 1 calc R U . . .
C12 C 0.1821(2) 0.2504(2) 0.59249(19) 0.1251(13) Uani 1 1 d . . . . .
H12A H 0.173803 0.221985 0.623687 0.150 Uiso 1 1 calc R U . . .
C13 C 0.13568(17) 0.2695(2) 0.55395(17) 0.1202(12) Uani 1 1 d . . . . .
H13A H 0.095578 0.255566 0.560696 0.144 Uiso 1 1 calc R U . . .
C14 C 0.14722(13) 0.30925(17) 0.50516(12) 0.0936(7) Uani 1 1 d . . . . .
C15 C 0.11116(11) 0.30809(15) 0.39731(12) 0.0878(6) Uani 1 1 d . . . . .
H15A H 0.149887 0.292812 0.386518 0.105 Uiso 1 1 calc R U . . .
C16 C 0.09942(12) 0.32264(18) 0.45925(14) 0.0987(8) Uani 1 1 d . . . . .
C17 C 0.04094(17) 0.3461(3) 0.4742(2) 0.1386(18) Uani 1 1 d . . . . .
H17A H 0.031472 0.355813 0.515017 0.166 Uiso 1 1 calc R U . . .
C18 C -0.00222(18) 0.3547(3) 0.4288(2) 0.148(2) Uani 1 1 d . . . . .
H18A H -0.040647 0.370957 0.439197 0.177 Uiso 1 1 calc R U . . .
C19 C 0.00991(16) 0.3398(3) 0.3682(2) 0.1248(13) Uani 1 1 d . . . . .
H19A H -0.020204 0.345799 0.338117 0.150 Uiso 1 1 calc R U . . .
C20 C 0.06741(12) 0.31562(16) 0.35197(14) 0.0916(7) Uani 1 1 d . . . . .
C21 C 0.07825(11) 0.29220(13) 0.28934(13) 0.0828(5) Uani 1 1 d . . . . .
C22 C 0.04186(13) 0.29418(14) 0.23671(14) 0.0895(6) Uani 1 1 d . . . . .
H22A H 0.004129 0.314225 0.231807 0.107 Uiso 1 1 calc R U . . .
C23 C 0.07357(12) 0.26003(12) 0.19307(13) 0.0825(5) Uani 1 1 d . . . . .
C24 C 0.05894(14) 0.24232(14) 0.12914(13) 0.0897(6) Uani 1 1 d . . . . .
C25 C 0.0085(2) 0.2646(2) 0.0982(2) 0.1193(12) Uani 1 1 d . . . . .
H25A H -0.018376 0.292100 0.117404 0.143 Uiso 1 1 calc R U . . .
C26 C -0.0020(3) 0.2460(3) 0.0384(2) 0.1463(18) Uani 1 1 d . . . . .
H26A H -0.036088 0.260540 0.016522 0.176 Uiso 1 1 calc R U . . .
C27 C 0.0392(3) 0.2052(3) 0.0114(2) 0.1472(18) Uani 1 1 d . . . . .
H27A H 0.033680 0.192549 -0.029364 0.177 Uiso 1 1 calc R U . . .
C28 C 0.0884(2) 0.1837(2) 0.04547(16) 0.1192(12) Uani 1 1 d . . . . .
H28A H 0.115577 0.155855 0.027113 0.143 Uiso 1 1 calc R U . . .
Fe3 Fe 0.30992(2) 0.30992(2) 0.30992(2) 0.07449(14) Uani 1 3 d S T P . .
O1 O 0.27783(8) 0.38056(8) 0.36071(7) 0.0742(3) Uani 1 1 d . . . . .
O2 O 0.24775(9) 0.34160(8) 0.24973(7) 0.0793(4) Uani 1 1 d . . . . .
O3 O 0.11084(16) 0.5080(2) 0.22693(15) 0.1509(14) Uani 1 1 d . U . . .
O4 O 0.13643(18) 0.54383(18) 0.34290(16) 0.1535(15) Uani 1 1 d . U . . .
C29 C 0.23479(10) 0.41251(11) 0.33329(10) 0.0735(4) Uani 1 1 d . . . . .
C30 C 0.21874(11) 0.39105(11) 0.26895(10) 0.0761(5) Uani 1 1 d . . . . .
C31 C 0.17771(13) 0.42306(16) 0.23388(13) 0.0953(8) Uani 1 1 d . . . . .
H31A H 0.169059 0.409665 0.193942 0.114 Uiso 1 1 calc R U . . .
C32 C 0.14766(15) 0.4769(2) 0.25723(15) 0.1046(9) Uani 1 1 d . U . . .
C33 C 0.16255(15) 0.49723(18) 0.32355(15) 0.1010(8) Uani 1 1 d . U . . .
C34 C 0.20607(12) 0.46206(14) 0.35843(12) 0.0855(6) Uani 1 1 d . . . . .
H34A H 0.214816 0.473337 0.398998 0.103 Uiso 1 1 calc R U . . .
O1S O 0.2842(8) 0.1206(8) 0.6925(8) 0.306(9) Uani 0.628(14) 1 d . U P . .
H1S H 0.316193 0.121346 0.672189 0.459 Uiso 0.628(14) 1 d R U P . .
C1S C 0.2316(6) 0.1041(7) 0.6532(6) 0.182(5) Uani 0.628(14) 1 d . U P . .
H1S1 H 0.193844 0.105134 0.676574 0.273 Uiso 0.628(14) 1 d R U P . .
H1S2 H 0.238954 0.062844 0.638724 0.273 Uiso 0.628(14) 1 d R U P . .
H1S3 H 0.228304 0.131664 0.618574 0.273 Uiso 0.628(14) 1 d R U P . .
B1 B -0.1189(11) 0.3845(8) 0.1162(11) 0.145(3) Uani 0.3333 1 d D U P A -1
F1 F -0.0762(10) 0.3743(9) 0.1614(9) 0.183(7) Uani 0.3333 1 d D U P A -1
F2 F -0.1033(8) 0.4359(7) 0.0837(12) 0.199(5) Uani 0.3333 1 d D U P A -1
F3 F -0.1758(8) 0.3967(10) 0.1436(10) 0.200(7) Uani 0.3333 1 d D U P A -1
F4 F -0.1245(10) 0.3347(9) 0.0780(10) 0.194(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.980(2) . ?
Fe1 N2 1.980(2) 5 ?
Fe1 N2 1.980(2) 9 ?
Fe1 N1 2.031(2) . ?
Fe1 N1 2.031(2) 5 ?
Fe1 N1 2.031(2) 9 ?
Fe2 N5 2.077(2) . ?
Fe2 N5 2.077(2) 5 ?
Fe2 N5 2.077(2) 9 ?
Fe2 N6 2.121(2) . ?
Fe2 N6 2.121(2) 9 ?
Fe2 N6 2.121(2) 5 ?
N1 C5 1.348(3) . ?
N1 C1 1.354(3) . ?
N2 C6 1.330(3) . ?
N2 N3 1.350(3) . ?
N3 C8 1.365(3) . ?
N3 H3 0.90(2) . ?
N4 N5 1.338(3) . ?
N4 C21 1.358(3) . ?
N4 H4 0.90(2) . ?
N5 C23 1.344(3) . ?
N6 C28 1.343(4) . ?
N6 C24 1.353(4) . ?
C1 C2 1.375(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.365(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.373(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.386(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.466(3) . ?
C6 C7 1.382(4) . ?
C7 C8 1.375(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.470(3) . ?
C9 C10 1.384(4) . ?
C9 C14 1.394(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.389(4) . ?
C11 C12 1.386(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.368(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.383(5) . ?
C13 H13A 0.9300 . ?
C14 C16 1.462(5) . ?
C15 C20 1.372(4) . ?
C15 C16 1.399(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.400(4) . ?
C17 C18 1.367(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.375(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.394(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.465(4) . ?
C21 C22 1.384(4) . ?
C22 C23 1.381(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.469(4) . ?
C24 C25 1.367(4) . ?
C25 C26 1.373(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.383(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.377(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9927(17) 9 ?
Fe3 O2 1.9927(17) . ?
Fe3 O2 1.9927(17) 5 ?
Fe3 O1 2.0054(16) . ?
Fe3 O1 2.0054(16) 5 ?
Fe3 O1 2.0054(16) 9 ?
O1 C29 1.302(3) . ?
O2 C30 1.308(3) . ?
O3 C32 1.231(4) . ?
O4 C33 1.229(4) . ?
C29 C34 1.353(4) . ?
C29 C30 1.507(3) . ?
C30 C31 1.357(4) . ?
C31 C32 1.425(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.534(5) . ?
C33 C34 1.426(4) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.464(18) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9603 . ?
C1S H1S2 0.9599 . ?
C1S H1S3 0.9599 . ?
B1 F2 1.359(15) . ?
B1 F1 1.363(19) . ?
B1 F4 1.363(19) . ?
B1 F3 1.391(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.18(7) . 5 ?
N2 Fe1 N2 96.18(7) . 9 ?
N2 Fe1 N2 96.18(7) 5 9 ?
N2 Fe1 N1 79.64(8) . . ?
N2 Fe1 N1 91.85(8) 5 . ?
N2 Fe1 N1 171.32(8) 9 . ?
N2 Fe1 N1 171.32(8) . 5 ?
N2 Fe1 N1 79.64(8) 5 5 ?
N2 Fe1 N1 91.85(8) 9 5 ?
N1 Fe1 N1 92.83(8) . 5 ?
N2 Fe1 N1 91.85(8) . 9 ?
N2 Fe1 N1 171.32(8) 5 9 ?
N2 Fe1 N1 79.64(8) 9 9 ?
N1 Fe1 N1 92.83(8) . 9 ?
N1 Fe1 N1 92.83(8) 5 9 ?
N5 Fe2 N5 97.47(8) . 5 ?
N5 Fe2 N5 97.47(8) . 9 ?
N5 Fe2 N5 97.47(8) 5 9 ?
N5 Fe2 N6 77.39(9) . . ?
N5 Fe2 N6 167.91(9) 5 . ?
N5 Fe2 N6 94.07(9) 9 . ?
N5 Fe2 N6 167.91(9) . 9 ?
N5 Fe2 N6 94.07(9) 5 9 ?
N5 Fe2 N6 77.40(9) 9 9 ?
N6 Fe2 N6 91.94(10) . 9 ?
N5 Fe2 N6 94.07(9) . 5 ?
N5 Fe2 N6 77.40(9) 5 5 ?
N5 Fe2 N6 167.91(9) 9 5 ?
N6 Fe2 N6 91.94(10) . 5 ?
N6 Fe2 N6 91.94(10) 9 5 ?
C5 N1 C1 117.9(2) . . ?
C5 N1 Fe1 114.99(15) . . ?
C1 N1 Fe1 126.98(19) . . ?
C6 N2 N3 105.66(18) . . ?
C6 N2 Fe1 116.14(16) . . ?
N3 N2 Fe1 136.77(15) . . ?
N2 N3 C8 110.72(19) . . ?
N2 N3 H3 125(3) . . ?
C8 N3 H3 122(3) . . ?
N5 N4 C21 111.5(2) . . ?
N5 N4 H4 114(3) . . ?
C21 N4 H4 134(3) . . ?
N4 N5 C23 105.6(2) . . ?
N4 N5 Fe2 135.89(16) . . ?
C23 N5 Fe2 114.84(18) . . ?
C28 N6 C24 117.1(3) . . ?
C28 N6 Fe2 127.9(2) . . ?
C24 N6 Fe2 114.82(18) . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C3 C2 C1 119.9(3) . . ?
C3 C2 H2A 120.1 . . ?
C1 C2 H2A 120.1 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.5(3) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 113.3(2) . . ?
C4 C5 C6 124.2(3) . . ?
N2 C6 C7 111.5(2) . . ?
N2 C6 C5 115.2(2) . . ?
C7 C6 C5 133.3(2) . . ?
C8 C7 C6 105.3(2) . . ?
C8 C7 H7A 127.3 . . ?
C6 C7 H7A 127.3 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C10 123.1(2) . . ?
C7 C8 C10 130.1(2) . . ?
C10 C9 C14 120.7(3) . . ?
C10 C9 H9A 119.7 . . ?
C14 C9 H9A 119.7 . . ?
C9 C10 C11 119.5(3) . . ?
C9 C10 C8 122.1(2) . . ?
C11 C10 C8 118.4(3) . . ?
C12 C11 C10 119.9(3) . . ?
C12 C11 H11A 120.0 . . ?
C10 C11 H11A 120.0 . . ?
C13 C12 C11 119.9(3) . . ?
C13 C12 H12A 120.1 . . ?
C11 C12 H12A 120.1 . . ?
C12 C13 C14 121.3(3) . . ?
C12 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
C13 C14 C9 118.6(3) . . ?
C13 C14 C16 120.9(3) . . ?
C9 C14 C16 120.3(3) . . ?
C20 C15 C16 122.2(2) . . ?
C20 C15 H15A 118.9 . . ?
C16 C15 H15A 118.9 . . ?
C15 C16 C17 117.8(3) . . ?
C15 C16 C14 118.5(2) . . ?
C17 C16 C14 123.6(3) . . ?
C18 C17 C16 120.0(3) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 121.5(3) . . ?
C17 C18 H18A 119.3 . . ?
C19 C18 H18A 119.3 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19A 120.1 . . ?
C20 C19 H19A 120.1 . . ?
C15 C20 C19 118.6(3) . . ?
C15 C20 C21 120.6(2) . . ?
C19 C20 C21 120.4(3) . . ?
N4 C21 C22 106.6(2) . . ?
N4 C21 C20 122.0(2) . . ?
C22 C21 C20 131.2(2) . . ?
C23 C22 C21 105.3(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.0(2) . . ?
N5 C23 C24 116.4(2) . . ?
C22 C23 C24 132.5(2) . . ?
N6 C24 C25 123.0(3) . . ?
N6 C24 C23 114.2(2) . . ?
C25 C24 C23 122.8(3) . . ?
C24 C25 C26 119.4(4) . . ?
C24 C25 H25A 120.3 . . ?
C26 C25 H25A 120.3 . . ?
C25 C26 C27 118.5(4) . . ?
C25 C26 H26A 120.7 . . ?
C27 C26 H26A 120.7 . . ?
C28 C27 C26 119.2(4) . . ?
C28 C27 H27A 120.4 . . ?
C26 C27 H27A 120.4 . . ?
N6 C28 C27 122.8(4) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 90.91(8) 9 . ?
O2 Fe3 O2 90.91(8) 9 5 ?
O2 Fe3 O2 90.91(8) . 5 ?
O2 Fe3 O1 170.42(7) 9 . ?
O2 Fe3 O1 82.09(6) . . ?
O2 Fe3 O1 95.71(7) 5 . ?
O2 Fe3 O1 95.72(7) 9 5 ?
O2 Fe3 O1 170.42(7) . 5 ?
O2 Fe3 O1 82.09(6) 5 5 ?
O1 Fe3 O1 92.05(7) . 5 ?
O2 Fe3 O1 82.09(6) 9 9 ?
O2 Fe3 O1 95.72(7) . 9 ?
O2 Fe3 O1 170.42(7) 5 9 ?
O1 Fe3 O1 92.05(7) . 9 ?
O1 Fe3 O1 92.05(7) 5 9 ?
C29 O1 Fe3 113.72(14) . . ?
C30 O2 Fe3 113.40(14) . . ?
O1 C29 C34 124.4(2) . . ?
O1 C29 C30 114.9(2) . . ?
C34 C29 C30 120.6(2) . . ?
O2 C30 C31 123.6(2) . . ?
O2 C30 C29 115.8(2) . . ?
C31 C30 C29 120.6(2) . . ?
C30 C31 C32 121.1(3) . . ?
C30 C31 H31A 119.4 . . ?
C32 C31 H31A 119.4 . . ?
O3 C32 C31 123.6(3) . . ?
O3 C32 C33 118.4(3) . . ?
C31 C32 C33 118.0(3) . . ?
O4 C33 C34 124.1(3) . . ?
O4 C33 C32 117.2(3) . . ?
C34 C33 C32 118.7(3) . . ?
C29 C34 C33 120.9(2) . . ?
C29 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
C1S O1S H1S 110.4 . . ?
O1S C1S H1S1 110.5 . . ?
O1S C1S H1S2 106.7 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 111.1 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F1 109.5(17) . . ?
F2 B1 F4 110.8(17) . . ?
F1 B1 F4 111.6(16) . . ?
F2 B1 F3 106.6(15) . . ?
F1 B1 F3 109.0(17) . . ?
F4 B1 F3 109.2(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(2) 2.06(3) 2.942(2) 169(4) . yes
N4 H4 O2 0.90(2) 2.11(3) 2.994(3) 168(4) 5 yes

_refine_diff_density_max         0.217
_refine_diff_density_min         -0.169
_refine_diff_density_rms         0.038

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_330K
_database_code_depnum_ccdc_archive 'CCDC 2260944'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.593(C H4 O)'
_chemical_formula_sum            'C104.59 H76.36 B F4 Fe3 N18 O14.59'
_chemical_formula_weight         2073.17

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.579(3)
_cell_length_b                   21.579(3)
_cell_length_c                   21.579(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10048(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    330(2)
_cell_measurement_reflns_used    6487
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.95

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.370
_exptl_crystal_F_000             4263
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.541
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      330(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            166566
_diffrn_reflns_av_unetI/netI     0.0270
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.369
_diffrn_reflns_theta_max         29.517
_diffrn_reflns_theta_full        29.517
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8674
_reflns_number_gt                8520
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.864 (i.e. 2.593 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0680P)²+0.2307P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0315(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3871 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.059(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8674
_refine_ls_number_parameters     477
_refine_ls_number_restraints     83
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0319
_refine_ls_wR_factor_ref         0.0930
_refine_ls_wR_factor_gt          0.0926
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29665(2) 0.29665(2) 0.29665(2) 0.05388(11) Uani 1 3 d S T P . .
Fe2 Fe 0.58517(2) 0.58517(2) 0.58517(2) 0.06020(12) Uani 1 3 d S T P . .
N1 N 0.22748(8) 0.33012(8) 0.24308(7) 0.0623(3) Uani 1 1 d . . . . .
N2 N 0.25989(7) 0.35694(8) 0.35439(7) 0.0575(3) Uani 1 1 d . . . . .
N3 N 0.26648(7) 0.37265(8) 0.41463(7) 0.0586(3) Uani 1 1 d D . . . .
H3 H 0.3007(12) 0.3639(16) 0.4350(15) 0.088 Uiso 1 1 d D U . . .
N4 N 0.47645(8) 0.49316(10) 0.62229(8) 0.0680(4) Uani 1 1 d D . . . .
H4 H 0.4547(17) 0.4984(18) 0.5865(14) 0.102 Uiso 1 1 d D U . . .
N5 N 0.53555(8) 0.51330(9) 0.62441(8) 0.0668(4) Uani 1 1 d . . . . .
N6 N 0.64726(9) 0.55063(10) 0.65255(10) 0.0746(4) Uani 1 1 d . . . . .
C1 C 0.21429(12) 0.31399(12) 0.18409(10) 0.0736(5) Uani 1 1 d . . . . .
H1A H 0.240901 0.287230 0.163271 0.088 Uiso 1 1 calc R U . . .
C2 C 0.16244(15) 0.33605(14) 0.15375(13) 0.0874(7) Uani 1 1 d . . . . .
H2A H 0.153761 0.323251 0.113526 0.105 Uiso 1 1 calc R U . . .
C3 C 0.12360(15) 0.37722(16) 0.18351(15) 0.0941(8) Uani 1 1 d . . . . .
H3B H 0.088814 0.392843 0.163425 0.113 Uiso 1 1 calc R U . . .
C4 C 0.13706(14) 0.39488(14) 0.24342(14) 0.0853(7) Uani 1 1 d . . . . .
H4B H 0.111808 0.422864 0.264326 0.102 Uiso 1 1 calc R U . . .
C5 C 0.18911(9) 0.36998(10) 0.27186(10) 0.0650(4) Uani 1 1 d . . . . .
C6 C 0.20687(9) 0.38317(9) 0.33575(9) 0.0623(4) Uani 1 1 d . . . . .
C7 C 0.17940(9) 0.41636(11) 0.38371(10) 0.0681(4) Uani 1 1 d . . . . .
H7A H 0.142503 0.438585 0.382393 0.082 Uiso 1 1 calc R U . . .
C8 C 0.21853(8) 0.40924(9) 0.43348(9) 0.0616(4) Uani 1 1 d . . . . .
C9 C 0.21318(9) 0.43393(10) 0.49679(9) 0.0648(4) Uani 1 1 d . . . . .
C10 C 0.16524(11) 0.47508(14) 0.50962(13) 0.0797(6) Uani 1 1 d . . . . .
H10A H 0.138333 0.487445 0.478310 0.096 Uiso 1 1 calc R U . . .
C11 C 0.15777(15) 0.49767(18) 0.56965(16) 0.1001(9) Uani 1 1 d . . . . .
H11A H 0.126021 0.525486 0.578362 0.120 Uiso 1 1 calc R U . . .
C12 C 0.19667(14) 0.47919(19) 0.61535(14) 0.0975(9) Uani 1 1 d . . . . .
H12A H 0.190357 0.493564 0.655485 0.117 Uiso 1 1 calc R U . . .
C13 C 0.24571(10) 0.43931(14) 0.60360(10) 0.0754(5) Uani 1 1 d . . . . .
C14 C 0.25338(9) 0.41654(12) 0.54380(9) 0.0691(4) Uani 1 1 d . . . . .
H14A H 0.285758 0.389402 0.535261 0.083 Uiso 1 1 calc R U . . .
C15 C 0.29236(12) 0.42628(15) 0.65160(10) 0.0814(6) Uani 1 1 d . . . . .
C16 C 0.27743(16) 0.4033(2) 0.71045(14) 0.1158(13) Uani 1 1 d . . . . .
H16A H 0.236474 0.393845 0.719959 0.139 Uiso 1 1 calc R U . . .
C17 C 0.3227(2) 0.3948(3) 0.75404(15) 0.1334(18) Uani 1 1 d . . . . .
H17A H 0.312443 0.377824 0.792326 0.160 Uiso 1 1 calc R U . . .
C18 C 0.38352(17) 0.4110(2) 0.74176(13) 0.1087(11) Uani 1 1 d . . . . .
H18A H 0.413615 0.406265 0.772245 0.130 Uiso 1 1 calc R U . . .
C19 C 0.39976(11) 0.43448(14) 0.68378(10) 0.0757(5) Uani 1 1 d . . . . .
C20 C 0.35412(10) 0.44119(12) 0.63947(9) 0.0717(5) Uani 1 1 d . . . . .
H20A H 0.364815 0.456052 0.600452 0.086 Uiso 1 1 calc R U . . .
C21 C 0.46236(11) 0.45809(11) 0.67263(9) 0.0681(4) Uani 1 1 d . . . . .
C22 C 0.51515(11) 0.45596(11) 0.70914(11) 0.0737(5) Uani 1 1 d . . . . .
H22A H 0.520259 0.435389 0.746671 0.088 Uiso 1 1 calc R U . . .
C23 C 0.55868(11) 0.49111(10) 0.67762(10) 0.0678(4) Uani 1 1 d . . . . .
C24 C 0.62252(11) 0.50931(11) 0.69253(12) 0.0731(5) Uani 1 1 d . . . . .
C25 C 0.65403(15) 0.48650(17) 0.74341(18) 0.0981(9) Uani 1 1 d . . . . .
H25A H 0.635077 0.458851 0.770502 0.118 Uiso 1 1 calc R U . . .
C26 C 0.71402(19) 0.5056(2) 0.7531(2) 0.1240(14) Uani 1 1 d . . . . .
H26A H 0.736579 0.490357 0.786468 0.149 Uiso 1 1 calc R U . . .
C27 C 0.74048(16) 0.5476(2) 0.7128(3) 0.1261(15) Uani 1 1 d . . . . .
H27A H 0.780801 0.561458 0.719092 0.151 Uiso 1 1 calc R U . . .
C28 C 0.70613(14) 0.56884(17) 0.66289(18) 0.1005(9) Uani 1 1 d . . . . .
H28A H 0.724350 0.596694 0.635510 0.121 Uiso 1 1 calc R U . . .
Fe3 Fe 0.44076(2) 0.44076(2) 0.44076(2) 0.05961(12) Uani 1 3 d S T P . .
O1 O 0.38992(6) 0.36974(7) 0.47256(7) 0.0606(3) Uani 1 1 d . . . . .
O2 O 0.50111(6) 0.40880(7) 0.50308(7) 0.0645(3) Uani 1 1 d . . . . .
O3 O 0.52558(12) 0.23878(15) 0.63668(13) 0.1168(9) Uani 1 1 d . . . . .
O4 O 0.40931(13) 0.20252(14) 0.61040(14) 0.1187(9) Uani 1 1 d . U . . .
C29 C 0.41783(8) 0.33682(9) 0.51503(8) 0.0589(3) Uani 1 1 d . . . . .
C30 C 0.48239(9) 0.35828(9) 0.53136(9) 0.0613(4) Uani 1 1 d . . . . .
C31 C 0.51771(11) 0.32558(13) 0.57149(11) 0.0782(6) Uani 1 1 d . . . . .
H31A H 0.557599 0.339280 0.580366 0.094 Uiso 1 1 calc R U . . .
C32 C 0.49540(12) 0.27082(14) 0.60042(12) 0.0815(6) Uani 1 1 d . U . . .
C33 C 0.42834(12) 0.24998(13) 0.58534(12) 0.0804(6) Uani 1 1 d . U . . .
C34 C 0.39293(10) 0.28617(11) 0.54292(10) 0.0701(5) Uani 1 1 d . . . . .
H34A H 0.352230 0.274964 0.534228 0.084 Uiso 1 1 calc R U . . .
O1S O -0.0334(5) 0.4404(6) 0.3671(6) 0.303(6) Uani 0.864(14) 1 d . U P . .
H1S H -0.021985 0.475910 0.374397 0.454 Uiso 0.864(14) 1 d R U P . .
C1S C 0.0182(4) 0.4040(3) 0.3560(4) 0.158(3) Uani 0.864(14) 1 d . U P . .
H1S1 H 0.034356 0.387200 0.393850 0.236 Uiso 0.864(14) 1 d R U P . .
H1S2 H 0.049506 0.428630 0.336120 0.236 Uiso 0.864(14) 1 d R U P . .
H1S3 H 0.006086 0.370810 0.328980 0.236 Uiso 0.864(14) 1 d R U P . .
B1 B 0.1290(10) 0.1311(9) 0.1337(8) 0.127(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1238(10) 0.1708(8) 0.0846(8) 0.175(7) Uani 0.3333 1 d D U P A -1
F2 F 0.1435(8) 0.1628(7) 0.1873(5) 0.193(5) Uani 0.3333 1 d D U P A -1
F3 F 0.0711(8) 0.1045(8) 0.1447(9) 0.181(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1711(9) 0.0854(7) 0.1226(7) 0.165(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9683(16) . ?
Fe1 N2 1.9684(16) 5 ?
Fe1 N2 1.9684(16) 9 ?
Fe1 N1 2.0213(17) . ?
Fe1 N1 2.0214(17) 5 ?
Fe1 N1 2.0214(17) 9 ?
Fe2 N5 2.066(2) . ?
Fe2 N5 2.066(2) 9 ?
Fe2 N5 2.066(2) 5 ?
Fe2 N6 2.113(2) . ?
Fe2 N6 2.113(2) 9 ?
Fe2 N6 2.113(2) 5 ?
N1 C5 1.346(3) . ?
N1 C1 1.350(3) . ?
N2 C6 1.338(2) . ?
N2 N3 1.351(2) . ?
N3 C8 1.364(2) . ?
N3 H3 0.88(2) . ?
N4 N5 1.348(3) . ?
N4 C21 1.358(3) . ?
N4 H4 0.91(2) . ?
N5 C23 1.340(3) . ?
N6 C28 1.348(4) . ?
N6 C24 1.351(3) . ?
C1 C2 1.381(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.380(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.379(4) . ?
C3 H3B 0.9300 . ?
C4 C5 1.388(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.459(3) . ?
C6 C7 1.391(3) . ?
C7 C8 1.375(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.471(3) . ?
C9 C14 1.386(3) . ?
C9 C10 1.391(3) . ?
C10 C11 1.393(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.355(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.387(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.391(3) . ?
C13 C15 1.472(4) . ?
C14 H14A 0.9300 . ?
C15 C20 1.396(3) . ?
C15 C16 1.401(3) . ?
C16 C17 1.368(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.385(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.380(3) . ?
C19 C21 1.464(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.386(3) . ?
C22 C23 1.386(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.468(3) . ?
C24 C25 1.382(3) . ?
C25 C26 1.375(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.379(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.386(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9950(14) . ?
Fe3 O2 1.9950(14) 9 ?
Fe3 O2 1.9951(14) 5 ?
Fe3 O1 2.0057(14) 9 ?
Fe3 O1 2.0057(14) 5 ?
Fe3 O1 2.0058(14) . ?
O1 C29 1.307(2) . ?
O2 C30 1.313(2) . ?
O3 C32 1.231(3) . ?
O4 C33 1.229(3) . ?
C29 C34 1.359(3) . ?
C29 C30 1.510(3) . ?
C30 C31 1.352(3) . ?
C31 C32 1.421(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.550(4) . ?
C33 C34 1.425(3) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.384(11) . ?
O1S H1S 0.8198 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9601 . ?
C1S H1S3 0.9599 . ?
B1 F4 1.363(17) . ?
B1 F1 1.367(19) . ?
B1 F2 1.379(14) . ?
B1 F3 1.396(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 95.91(6) . 5 ?
N2 Fe1 N2 95.91(6) . 9 ?
N2 Fe1 N2 95.91(6) 5 9 ?
N2 Fe1 N1 80.11(7) . . ?
N2 Fe1 N1 171.67(7) 5 . ?
N2 Fe1 N1 91.80(7) 9 . ?
N2 Fe1 N1 91.80(7) . 5 ?
N2 Fe1 N1 80.11(7) 5 5 ?
N2 Fe1 N1 171.67(7) 9 5 ?
N1 Fe1 N1 92.64(7) . 5 ?
N2 Fe1 N1 171.67(7) . 9 ?
N2 Fe1 N1 91.80(7) 5 9 ?
N2 Fe1 N1 80.11(7) 9 9 ?
N1 Fe1 N1 92.64(7) . 9 ?
N1 Fe1 N1 92.64(7) 5 9 ?
N5 Fe2 N5 97.53(7) . 9 ?
N5 Fe2 N5 97.54(7) . 5 ?
N5 Fe2 N5 97.54(7) 9 5 ?
N5 Fe2 N6 77.40(7) . . ?
N5 Fe2 N6 167.72(8) 9 . ?
N5 Fe2 N6 94.23(8) 5 . ?
N5 Fe2 N6 94.23(8) . 9 ?
N5 Fe2 N6 77.39(7) 9 9 ?
N5 Fe2 N6 167.73(8) 5 9 ?
N6 Fe2 N6 91.72(8) . 9 ?
N5 Fe2 N6 167.73(8) . 5 ?
N5 Fe2 N6 94.23(8) 9 5 ?
N5 Fe2 N6 77.39(7) 5 5 ?
N6 Fe2 N6 91.72(8) . 5 ?
N6 Fe2 N6 91.72(8) 9 5 ?
C5 N1 C1 118.05(18) . . ?
C5 N1 Fe1 114.76(13) . . ?
C1 N1 Fe1 127.07(16) . . ?
C6 N2 N3 105.84(15) . . ?
C6 N2 Fe1 115.71(13) . . ?
N3 N2 Fe1 137.11(12) . . ?
N2 N3 C8 110.65(16) . . ?
N2 N3 H3 121(2) . . ?
C8 N3 H3 128(2) . . ?
N5 N4 C21 111.35(18) . . ?
N5 N4 H4 118(3) . . ?
C21 N4 H4 129(3) . . ?
C23 N5 N4 105.44(18) . . ?
C23 N5 Fe2 115.23(15) . . ?
N4 N5 Fe2 135.91(14) . . ?
C28 N6 C24 117.3(2) . . ?
C28 N6 Fe2 127.5(2) . . ?
C24 N6 Fe2 114.94(15) . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3B 120.4 . . ?
C2 C3 H3B 120.4 . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 H4B 120.7 . . ?
C5 C4 H4B 120.7 . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 C6 113.53(17) . . ?
C4 C5 C6 123.7(2) . . ?
N2 C6 C7 111.00(17) . . ?
N2 C6 C5 115.21(17) . . ?
C7 C6 C5 133.75(18) . . ?
C8 C7 C6 105.18(17) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.32(17) . . ?
N3 C8 C9 123.12(18) . . ?
C7 C8 C9 129.56(18) . . ?
C14 C9 C10 119.5(2) . . ?
C14 C9 C8 122.16(18) . . ?
C10 C9 C8 118.3(2) . . ?
C9 C10 C11 119.6(3) . . ?
C9 C10 H10A 120.2 . . ?
C11 C10 H10A 120.2 . . ?
C12 C11 C10 120.1(3) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.5(2) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.7(2) . . ?
C12 C13 C15 120.8(2) . . ?
C14 C13 C15 120.3(2) . . ?
C9 C14 C13 120.6(2) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C20 C15 C16 118.1(3) . . ?
C20 C15 C13 118.5(2) . . ?
C16 C15 C13 123.3(2) . . ?
C17 C16 C15 120.5(3) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 120.7(3) . . ?
C16 C17 H17A 119.6 . . ?
C18 C17 H17A 119.6 . . ?
C17 C18 C19 120.1(3) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C20 C19 C18 118.7(2) . . ?
C20 C19 C21 120.5(2) . . ?
C18 C19 C21 120.4(2) . . ?
C19 C20 C15 121.8(2) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 106.8(2) . . ?
N4 C21 C19 122.1(2) . . ?
C22 C21 C19 130.8(2) . . ?
C21 C22 C23 105.06(19) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.3(2) . . ?
N5 C23 C24 116.2(2) . . ?
C22 C23 C24 132.4(2) . . ?
N6 C24 C25 123.2(3) . . ?
N6 C24 C23 114.0(2) . . ?
C25 C24 C23 122.7(2) . . ?
C26 C25 C24 118.5(3) . . ?
C26 C25 H25A 120.8 . . ?
C24 C25 H25A 120.8 . . ?
C25 C26 C27 119.5(3) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C26 C27 C28 119.1(3) . . ?
C26 C27 H27A 120.5 . . ?
C28 C27 H27A 120.5 . . ?
N6 C28 C27 122.4(3) . . ?
N6 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
O2 Fe3 O2 91.07(6) . 9 ?
O2 Fe3 O2 91.07(7) . 5 ?
O2 Fe3 O2 91.06(7) 9 5 ?
O2 Fe3 O1 170.30(6) . 9 ?
O2 Fe3 O1 82.08(5) 9 9 ?
O2 Fe3 O1 95.90(6) 5 9 ?
O2 Fe3 O1 95.90(6) . 5 ?
O2 Fe3 O1 170.30(6) 9 5 ?
O2 Fe3 O1 82.08(5) 5 5 ?
O1 Fe3 O1 91.75(6) 9 5 ?
O2 Fe3 O1 82.08(5) . . ?
O2 Fe3 O1 95.90(6) 9 . ?
O2 Fe3 O1 170.30(6) 5 . ?
O1 Fe3 O1 91.75(6) 9 . ?
O1 Fe3 O1 91.75(6) 5 . ?
C29 O1 Fe3 113.78(12) . . ?
C30 O2 Fe3 113.55(12) . . ?
O1 C29 C34 124.46(18) . . ?
O1 C29 C30 114.98(16) . . ?
C34 C29 C30 120.56(17) . . ?
O2 C30 C31 123.88(18) . . ?
O2 C30 C29 115.47(16) . . ?
C31 C30 C29 120.63(19) . . ?
C30 C31 C32 121.6(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.6(3) . . ?
O3 C32 C33 117.7(3) . . ?
C31 C32 C33 117.8(2) . . ?
O4 C33 C34 124.1(2) . . ?
O4 C33 C32 117.5(2) . . ?
C34 C33 C32 118.4(2) . . ?
C29 C34 C33 120.88(19) . . ?
C29 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
C1S O1S H1S 108.7 . . ?
O1S C1S H1S1 111.1 . . ?
O1S C1S H1S2 109.3 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 108.0 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F4 B1 F1 111.8(15) . . ?
F4 B1 F2 110.8(16) . . ?
F1 B1 F2 111.1(15) . . ?
F4 B1 F3 109.2(15) . . ?
F1 B1 F3 108.4(17) . . ?
F2 B1 F3 105.3(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(2) 2.09(2) 2.943(2) 162(3) . yes
N4 H4 O2 0.91(2) 2.09(2) 3.002(2) 175(4) 9 yes

_refine_diff_density_max         0.208
_refine_diff_density_min         -0.218
_refine_diff_density_rms         0.052

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_360K
_database_code_depnum_ccdc_archive 'CCDC 2260947'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 1.386(C H4 O)'
_chemical_formula_sum            'C103.39 H71.55 B F4 Fe3 N18 O13.39'
_chemical_formula_weight         2034.50

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.692(3)
_cell_length_b                   21.692(3)
_cell_length_c                   21.692(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10207(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    360(2)
_cell_measurement_reflns_used    6138
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      32.59

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.324
_exptl_crystal_F_000             4176
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.530
_shelx_estimated_absorpt_T_min   0.879
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      360(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            165683
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_av_R_equivalents  0.0531
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         29.518
_diffrn_reflns_theta_full        29.518
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8828
_reflns_number_gt                8073
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.4619 (i.e. 1.386 MeOH per formula unit).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1134P)²+0.0118P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0172(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3535 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.094(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8828
_refine_ls_number_parameters     477
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0455
_refine_ls_wR_factor_ref         0.1373
_refine_ls_wR_factor_gt          0.1342
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29752(2) 0.29752(2) 0.29752(2) 0.07502(16) Uani 1 3 d S T P . .
Fe2 Fe 0.58188(2) 0.58188(2) 0.58188(2) 0.08206(18) Uani 1 3 d S T P . .
N1 N 0.22914(12) 0.33153(11) 0.24255(11) 0.0858(5) Uani 1 1 d . . . . .
N2 N 0.25988(10) 0.35948(11) 0.35421(10) 0.0803(4) Uani 1 1 d . . . . .
N3 N 0.26552(10) 0.37499(12) 0.41443(11) 0.0830(5) Uani 1 1 d D . . . .
H3 H 0.2964(19) 0.367(3) 0.440(2) 0.124 Uiso 1 1 d D U . . .
N4 N 0.47323(12) 0.49147(14) 0.61950(11) 0.0898(6) Uani 1 1 d D . . . .
H4 H 0.449(2) 0.501(3) 0.5878(19) 0.135 Uiso 1 1 d D U . . .
N5 N 0.53200(11) 0.51052(13) 0.62110(11) 0.0879(5) Uani 1 1 d . . . . .
N6 N 0.64349(14) 0.54699(15) 0.64860(16) 0.1012(6) Uani 1 1 d . . . . .
C1 C 0.2161(2) 0.31523(17) 0.18446(15) 0.1009(8) Uani 1 1 d . . . . .
H1A H 0.241518 0.287068 0.164517 0.121 Uiso 1 1 calc R U . . .
C2 C 0.1657(3) 0.3391(2) 0.15321(19) 0.1219(13) Uani 1 1 d . . . . .
H2A H 0.157403 0.326689 0.113032 0.146 Uiso 1 1 calc R U . . .
C3 C 0.1287(3) 0.3807(2) 0.1815(2) 0.1328(16) Uani 1 1 d . . . . .
H3B H 0.094445 0.396553 0.161061 0.159 Uiso 1 1 calc R U . . .
C4 C 0.1418(2) 0.3990(2) 0.2395(2) 0.1177(12) Uani 1 1 d . . . . .
H4B H 0.117684 0.428835 0.258651 0.141 Uiso 1 1 calc R U . . .
C5 C 0.19131(14) 0.37306(14) 0.27030(14) 0.0899(6) Uani 1 1 d . . . . .
C6 C 0.20822(13) 0.38587(13) 0.33436(13) 0.0859(6) Uani 1 1 d . . . . .
C7 C 0.18054(14) 0.41976(16) 0.38081(17) 0.0945(7) Uani 1 1 d . . . . .
H7A H 0.144296 0.442519 0.378263 0.113 Uiso 1 1 calc R U . . .
C8 C 0.21841(12) 0.41259(14) 0.43217(14) 0.0868(6) Uani 1 1 d . . . . .
C9 C 0.21235(13) 0.43755(16) 0.49477(15) 0.0924(7) Uani 1 1 d . . . . .
C10 C 0.16462(18) 0.4794(3) 0.5054(2) 0.1214(13) Uani 1 1 d . . . . .
H10A H 0.138750 0.491942 0.473592 0.146 Uiso 1 1 calc R U . . .
C11 C 0.1568(2) 0.5021(3) 0.5663(3) 0.146(2) Uani 1 1 d . . . . .
H11A H 0.125905 0.530596 0.574631 0.175 Uiso 1 1 calc R U . . .
C12 C 0.1943(2) 0.4823(4) 0.6124(2) 0.146(2) Uani 1 1 d . . . . .
H12A H 0.186979 0.495822 0.652429 0.175 Uiso 1 1 calc R U . . .
C13 C 0.24337(15) 0.4425(2) 0.60140(16) 0.1057(9) Uani 1 1 d . . . . .
C14 C 0.25090(14) 0.41969(18) 0.54157(15) 0.0960(7) Uani 1 1 d . . . . .
H14A H 0.282566 0.391967 0.533405 0.115 Uiso 1 1 calc R U . . .
C15 C 0.28905(17) 0.4282(2) 0.64864(15) 0.1078(10) Uani 1 1 d . . . . .
C16 C 0.2741(3) 0.4050(4) 0.7071(2) 0.161(3) Uani 1 1 d . . . . .
H16A H 0.233235 0.396847 0.717108 0.193 Uiso 1 1 calc R U . . .
C17 C 0.3196(3) 0.3944(4) 0.7492(2) 0.163(3) Uani 1 1 d . . . . .
H17A H 0.309710 0.376051 0.786698 0.196 Uiso 1 1 calc R U . . .
C18 C 0.3798(3) 0.4104(4) 0.7373(2) 0.141(2) Uani 1 1 d . . . . .
H18A H 0.409839 0.404512 0.767399 0.169 Uiso 1 1 calc R U . . .
C19 C 0.39594(17) 0.43512(19) 0.68065(15) 0.1009(8) Uani 1 1 d . . . . .
C20 C 0.35088(15) 0.44272(18) 0.63724(13) 0.0978(8) Uani 1 1 d . . . . .
H20A H 0.361708 0.458095 0.598716 0.117 Uiso 1 1 calc R U . . .
C21 C 0.45843(15) 0.45759(16) 0.67022(13) 0.0916(7) Uani 1 1 d . . . . .
C22 C 0.51126(17) 0.45526(17) 0.70625(16) 0.0986(8) Uani 1 1 d . . . . .
H22A H 0.516040 0.435409 0.743947 0.118 Uiso 1 1 calc R U . . .
C23 C 0.55512(15) 0.48846(15) 0.67456(15) 0.0920(6) Uani 1 1 d . . . . .
C24 C 0.61884(16) 0.50628(17) 0.68895(17) 0.0991(8) Uani 1 1 d . . . . .
C25 C 0.6499(3) 0.4818(3) 0.7373(3) 0.1379(18) Uani 1 1 d . . . . .
H25A H 0.631379 0.452975 0.763061 0.166 Uiso 1 1 calc R U . . .
C26 C 0.7107(3) 0.5013(3) 0.7473(4) 0.170(3) Uani 1 1 d . . . . .
H26A H 0.733069 0.486220 0.780631 0.204 Uiso 1 1 calc R U . . .
C27 C 0.7363(3) 0.5416(4) 0.7084(4) 0.164(3) Uani 1 1 d . . . . .
H27A H 0.776678 0.554554 0.714580 0.197 Uiso 1 1 calc R U . . .
C28 C 0.70254(19) 0.5643(3) 0.6587(3) 0.1314(15) Uani 1 1 d . . . . .
H28A H 0.721079 0.592061 0.631761 0.158 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43887(2) 0.43887(2) 0.43887(2) 0.08316(18) Uani 1 3 d S T P . .
O1 O 0.38781(8) 0.36884(10) 0.47136(9) 0.0829(4) Uani 1 1 d . . . . .
O2 O 0.49889(9) 0.40792(10) 0.50104(10) 0.0877(5) Uani 1 1 d . . . . .
O3 O 0.51902(19) 0.2470(3) 0.6430(2) 0.180(2) Uani 1 1 d . . . . .
O4 O 0.4025(2) 0.2123(2) 0.6186(2) 0.175(2) Uani 1 1 d . U . . .
C29 C 0.41486(12) 0.33796(13) 0.51543(12) 0.0817(5) Uani 1 1 d . . . . .
C30 C 0.47903(12) 0.35897(13) 0.53089(13) 0.0839(5) Uani 1 1 d . . . . .
C31 C 0.51370(16) 0.3290(2) 0.57342(17) 0.1051(9) Uani 1 1 d . . . . .
H31A H 0.553286 0.342836 0.582331 0.126 Uiso 1 1 calc R U . . .
C32 C 0.4895(2) 0.2761(3) 0.6047(2) 0.1255(14) Uani 1 1 d . U . . .
C33 C 0.42372(19) 0.2557(2) 0.59040(19) 0.1178(12) Uani 1 1 d . U . . .
C34 C 0.38946(15) 0.28944(19) 0.54493(14) 0.0977(8) Uani 1 1 d . . . . .
H34A H 0.349276 0.277707 0.535685 0.117 Uiso 1 1 calc R U . . .
O1S O 0.0625(11) 0.6362(13) 0.4650(13) 0.300(13) Uani 0.462(15) 1 d D U P . .
H1S H 0.026966 0.626067 0.473121 0.450 Uiso 0.462(15) 1 d R U P . .
C1S C 0.0965(10) 0.6468(15) 0.5208(13) 0.240(13) Uani 0.462(15) 1 d D U P . .
H1S1 H 0.113870 0.687452 0.519928 0.360 Uiso 0.462(15) 1 d R U P . .
H1S2 H 0.128870 0.616922 0.524808 0.360 Uiso 0.462(15) 1 d R U P . .
H1S3 H 0.068840 0.643292 0.555208 0.360 Uiso 0.462(15) 1 d R U P . .
B1 B 0.1371(7) 0.1373(10) 0.1403(11) 0.161(4) Uani 0.3333 1 d D U P A -1
F1 F 0.1321(11) 0.1846(10) 0.1001(12) 0.210(9) Uani 0.3333 1 d D U P A -1
F2 F 0.1858(11) 0.1522(8) 0.1801(16) 0.228(8) Uani 0.3333 1 d D U P A -1
F3 F 0.0856(9) 0.1307(10) 0.1751(11) 0.181(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1523(10) 0.0831(9) 0.1126(8) 0.187(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.996(2) . ?
Fe1 N2 1.996(2) 9 ?
Fe1 N2 1.996(2) 5 ?
Fe1 N1 2.041(2) 5 ?
Fe1 N1 2.041(2) 9 ?
Fe1 N1 2.041(2) . ?
Fe2 N5 2.071(3) . ?
Fe2 N5 2.071(3) 9 ?
Fe2 N5 2.071(3) 5 ?
Fe2 N6 2.110(3) . ?
Fe2 N6 2.110(3) 9 ?
Fe2 N6 2.110(3) 5 ?
N1 C1 1.339(4) . ?
N1 C5 1.359(4) . ?
N2 C6 1.330(3) . ?
N2 N3 1.355(3) . ?
N3 C8 1.363(4) . ?
N3 H3 0.89(3) . ?
N4 N5 1.341(4) . ?
N4 C21 1.361(4) . ?
N4 H4 0.89(3) . ?
N5 C23 1.351(4) . ?
N6 C28 1.353(5) . ?
N6 C24 1.353(5) . ?
C1 C2 1.386(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.355(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.350(7) . ?
C3 H3B 0.9300 . ?
C4 C5 1.385(5) . ?
C4 H4B 0.9300 . ?
C5 C6 1.464(4) . ?
C6 C7 1.384(4) . ?
C7 C8 1.393(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.468(4) . ?
C9 C14 1.371(5) . ?
C9 C10 1.396(5) . ?
C10 C11 1.420(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.391(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.399(5) . ?
C13 C15 1.459(6) . ?
C14 H14A 0.9300 . ?
C15 C20 1.400(4) . ?
C15 C16 1.402(5) . ?
C16 C17 1.365(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.376(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.386(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.367(5) . ?
C19 C21 1.458(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.388(5) . ?
C22 C23 1.377(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.469(5) . ?
C24 C25 1.354(5) . ?
C25 C26 1.403(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.335(10) . ?
C26 H26A 0.9300 . ?
C27 C28 1.394(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.991(2) 5 ?
Fe3 O2 1.991(2) 9 ?
Fe3 O2 1.991(2) . ?
Fe3 O1 2.0078(19) 9 ?
Fe3 O1 2.0078(19) 5 ?
Fe3 O1 2.0078(19) . ?
O1 C29 1.307(3) . ?
O2 C30 1.316(3) . ?
O3 C32 1.224(5) . ?
O4 C33 1.215(5) . ?
C29 C34 1.349(4) . ?
C29 C30 1.502(4) . ?
C30 C31 1.356(4) . ?
C31 C32 1.433(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.525(6) . ?
C33 C34 1.435(5) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.44(2) . ?
O1S H1S 0.8201 . ?
C1S H1S1 0.9598 . ?
C1S H1S2 0.9599 . ?
C1S H1S3 0.9601 . ?
B1 F1 1.353(19) . ?
B1 F3 1.354(18) . ?
B1 F4 1.361(19) . ?
B1 F2 1.402(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.46(9) . 9 ?
N2 Fe1 N2 96.46(9) . 5 ?
N2 Fe1 N2 96.46(9) 9 5 ?
N2 Fe1 N1 91.58(10) . 5 ?
N2 Fe1 N1 171.41(10) 9 5 ?
N2 Fe1 N1 79.58(9) 5 5 ?
N2 Fe1 N1 171.41(10) . 9 ?
N2 Fe1 N1 79.58(9) 9 9 ?
N2 Fe1 N1 91.58(10) 5 9 ?
N1 Fe1 N1 92.83(10) 5 9 ?
N2 Fe1 N1 79.59(9) . . ?
N2 Fe1 N1 91.58(10) 9 . ?
N2 Fe1 N1 171.41(10) 5 . ?
N1 Fe1 N1 92.83(10) 5 . ?
N1 Fe1 N1 92.83(10) 9 . ?
N5 Fe2 N5 97.54(9) . 9 ?
N5 Fe2 N5 97.54(9) . 5 ?
N5 Fe2 N5 97.54(9) 9 5 ?
N5 Fe2 N6 77.35(11) . . ?
N5 Fe2 N6 168.18(11) 9 . ?
N5 Fe2 N6 93.73(11) 5 . ?
N5 Fe2 N6 93.73(11) . 9 ?
N5 Fe2 N6 77.36(11) 9 9 ?
N5 Fe2 N6 168.18(11) 5 9 ?
N6 Fe2 N6 92.22(13) . 9 ?
N5 Fe2 N6 168.18(11) . 5 ?
N5 Fe2 N6 93.73(11) 9 5 ?
N5 Fe2 N6 77.36(11) 5 5 ?
N6 Fe2 N6 92.22(13) . 5 ?
N6 Fe2 N6 92.22(13) 9 5 ?
C1 N1 C5 117.6(3) . . ?
C1 N1 Fe1 127.4(2) . . ?
C5 N1 Fe1 114.81(19) . . ?
C6 N2 N3 106.3(2) . . ?
C6 N2 Fe1 115.78(19) . . ?
N3 N2 Fe1 136.42(18) . . ?
N2 N3 C8 110.7(2) . . ?
N2 N3 H3 129(4) . . ?
C8 N3 H3 120(4) . . ?
N5 N4 C21 111.7(3) . . ?
N5 N4 H4 121(4) . . ?
C21 N4 H4 128(4) . . ?
N4 N5 C23 105.4(3) . . ?
N4 N5 Fe2 135.8(2) . . ?
C23 N5 Fe2 115.1(2) . . ?
C28 N6 C24 116.8(4) . . ?
C28 N6 Fe2 127.7(3) . . ?
C24 N6 Fe2 115.3(2) . . ?
N1 C1 C2 121.9(4) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C4 C3 C2 119.5(4) . . ?
C4 C3 H3B 120.2 . . ?
C2 C3 H3B 120.2 . . ?
C3 C4 C5 119.6(4) . . ?
C3 C4 H4B 120.2 . . ?
C5 C4 H4B 120.2 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 113.3(3) . . ?
C4 C5 C6 125.1(3) . . ?
N2 C6 C7 111.0(3) . . ?
N2 C6 C5 115.9(3) . . ?
C7 C6 C5 133.1(3) . . ?
C6 C7 C8 105.5(3) . . ?
C6 C7 H7A 127.3 . . ?
C8 C7 H7A 127.3 . . ?
N3 C8 C7 106.4(3) . . ?
N3 C8 C9 123.3(3) . . ?
C7 C8 C9 130.2(3) . . ?
C14 C9 C10 120.9(3) . . ?
C14 C9 C8 121.7(3) . . ?
C10 C9 C8 117.3(3) . . ?
C9 C10 C11 117.9(5) . . ?
C9 C10 H10A 121.1 . . ?
C11 C10 H10A 121.1 . . ?
C12 C11 C10 120.3(5) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.8(4) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C12 C13 C14 117.9(4) . . ?
C12 C13 C15 122.1(4) . . ?
C14 C13 C15 119.8(3) . . ?
C9 C14 C13 121.0(3) . . ?
C9 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C20 C15 C16 117.5(4) . . ?
C20 C15 C13 118.6(3) . . ?
C16 C15 C13 123.7(4) . . ?
C17 C16 C15 120.0(4) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.2(4) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C17 C18 C19 120.2(5) . . ?
C17 C18 H18A 119.9 . . ?
C19 C18 H18A 119.9 . . ?
C20 C19 C18 118.5(4) . . ?
C20 C19 C21 121.2(3) . . ?
C18 C19 C21 120.1(4) . . ?
C19 C20 C15 122.4(3) . . ?
C19 C20 H20A 118.8 . . ?
C15 C20 H20A 118.8 . . ?
N4 C21 C22 106.3(3) . . ?
N4 C21 C19 121.7(3) . . ?
C22 C21 C19 131.9(3) . . ?
C23 C22 C21 105.7(3) . . ?
C23 C22 H22A 127.2 . . ?
C21 C22 H22A 127.2 . . ?
N5 C23 C22 110.9(3) . . ?
N5 C23 C24 116.0(3) . . ?
C22 C23 C24 133.0(3) . . ?
N6 C24 C25 124.1(4) . . ?
N6 C24 C23 114.0(3) . . ?
C25 C24 C23 121.9(4) . . ?
C24 C25 C26 118.0(5) . . ?
C24 C25 H25A 121.0 . . ?
C26 C25 H25A 121.0 . . ?
C27 C26 C25 119.4(5) . . ?
C27 C26 H26A 120.3 . . ?
C25 C26 H26A 120.3 . . ?
C26 C27 C28 120.2(5) . . ?
C26 C27 H27A 119.9 . . ?
C28 C27 H27A 119.9 . . ?
N6 C28 C27 121.6(5) . . ?
N6 C28 H28A 119.2 . . ?
C27 C28 H28A 119.2 . . ?
O2 Fe3 O2 90.35(9) 5 9 ?
O2 Fe3 O2 90.35(9) 5 . ?
O2 Fe3 O2 90.35(9) 9 . ?
O2 Fe3 O1 95.57(9) 5 9 ?
O2 Fe3 O1 82.41(7) 9 9 ?
O2 Fe3 O1 170.65(8) . 9 ?
O2 Fe3 O1 82.41(7) 5 5 ?
O2 Fe3 O1 170.65(8) 9 5 ?
O2 Fe3 O1 95.57(9) . 5 ?
O1 Fe3 O1 92.39(8) 9 5 ?
O2 Fe3 O1 170.65(8) 5 . ?
O2 Fe3 O1 95.57(9) 9 . ?
O2 Fe3 O1 82.41(7) . . ?
O1 Fe3 O1 92.39(8) 9 . ?
O1 Fe3 O1 92.39(8) 5 . ?
C29 O1 Fe3 113.39(17) . . ?
C30 O2 Fe3 113.03(17) . . ?
O1 C29 C34 124.3(3) . . ?
O1 C29 C30 115.1(2) . . ?
C34 C29 C30 120.6(3) . . ?
O2 C30 C31 122.7(3) . . ?
O2 C30 C29 116.0(2) . . ?
C31 C30 C29 121.3(3) . . ?
C30 C31 C32 120.2(3) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
O3 C32 C31 122.9(4) . . ?
O3 C32 C33 118.6(4) . . ?
C31 C32 C33 118.6(3) . . ?
O4 C33 C34 123.1(4) . . ?
O4 C33 C32 118.4(4) . . ?
C34 C33 C32 118.5(3) . . ?
C29 C34 C33 120.8(3) . . ?
C29 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
C1S O1S H1S 110.1 . . ?
O1S C1S H1S1 109.4 . . ?
O1S C1S H1S2 110.1 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 108.8 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F1 B1 F3 111.9(16) . . ?
F1 B1 F4 112.9(18) . . ?
F3 B1 F4 110.8(17) . . ?
F1 B1 F2 106.4(16) . . ?
F3 B1 F2 107.7(17) . . ?
F4 B1 F2 106.7(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(3) 2.10(3) 2.929(3) 156(5) . yes
N4 H4 O2 0.89(3) 2.13(3) 2.982(3) 162(5) 9 yes

_refine_diff_density_max         0.314
_refine_diff_density_min         -0.305
_refine_diff_density_rms         0.057

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_380K
_database_code_depnum_ccdc_archive 'CCDC 2260948'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.785(3)
_cell_length_b                   21.785(3)
_cell_length_c                   21.785(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10339(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    380(2)
_cell_measurement_reflns_used    6056
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.27

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.279
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.521
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      380(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            169227
_diffrn_reflns_av_unetI/netI     0.0235
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.919
_diffrn_reflns_theta_max         29.511
_diffrn_reflns_theta_full        29.511
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8920
_reflns_number_gt                8071
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
;

_vrf_PLAT601_lb2205_fresh1_380K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1805 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1805 cubic angstrom with less than 50 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse remaining lattice methanol. We however believe that although
 there may still be some diffuse lattice solvent, the amount is necessarily
 vanishingly small. Consequently we have decided to not use the structure
 refined after PLATON/SQUEEZE treatment, and report the present structure
 with a large empty void. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1046P)²+0.0576P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0091(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3485 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.081(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8920
_refine_ls_number_parameters     446
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0416
_refine_ls_wR_factor_ref         0.1359
_refine_ls_wR_factor_gt          0.1322
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.102
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29810(2) 0.29810(2) 0.29810(2) 0.08001(16) Uani 1 3 d S T P . .
Fe2 Fe 0.57985(2) 0.57985(2) 0.57985(2) 0.08473(18) Uani 1 3 d S T P . .
N1 N 0.22997(13) 0.33256(12) 0.24208(11) 0.0935(5) Uani 1 1 d . . . . .
N2 N 0.26002(10) 0.36104(11) 0.35380(11) 0.0859(5) Uani 1 1 d . . . . .
N3 N 0.26539(10) 0.37697(12) 0.41375(11) 0.0891(5) Uani 1 1 d D . . . .
H3 H 0.2987(17) 0.362(2) 0.433(2) 0.134 Uiso 1 1 d D U . . .
N4 N 0.47126(11) 0.49043(14) 0.61783(11) 0.0928(6) Uani 1 1 d D . . . .
H4 H 0.454(2) 0.509(2) 0.5857(19) 0.139 Uiso 1 1 d D U . . .
N5 N 0.53034(11) 0.50877(13) 0.61918(11) 0.0921(5) Uani 1 1 d . . . . .
N6 N 0.64112(13) 0.54494(15) 0.64683(16) 0.1074(7) Uani 1 1 d . . . . .
C1 C 0.2179(2) 0.31619(18) 0.18448(15) 0.1079(9) Uani 1 1 d . . . . .
H1A H 0.243321 0.287780 0.165267 0.130 Uiso 1 1 calc R U . . .
C2 C 0.1683(3) 0.3403(2) 0.1521(2) 0.1351(16) Uani 1 1 d . . . . .
H2A H 0.160257 0.327444 0.112199 0.162 Uiso 1 1 calc R U . . .
C3 C 0.1320(3) 0.3828(3) 0.1795(2) 0.1392(16) Uani 1 1 d . . . . .
H3B H 0.098798 0.399461 0.158442 0.167 Uiso 1 1 calc R U . . .
C4 C 0.1444(2) 0.4009(2) 0.2379(2) 0.1270(13) Uani 1 1 d . . . . .
H4B H 0.120283 0.430636 0.256797 0.152 Uiso 1 1 calc R U . . .
C5 C 0.19366(16) 0.37469(15) 0.26922(15) 0.0969(7) Uani 1 1 d . . . . .
C6 C 0.20946(14) 0.38815(14) 0.33334(14) 0.0911(6) Uani 1 1 d . . . . .
C7 C 0.18145(14) 0.42205(16) 0.37951(17) 0.1009(8) Uani 1 1 d . . . . .
H7A H 0.145605 0.445047 0.376483 0.121 Uiso 1 1 calc R U . . .
C8 C 0.21797(13) 0.41451(15) 0.43098(15) 0.0939(6) Uani 1 1 d . . . . .
C9 C 0.21157(13) 0.43915(18) 0.49270(16) 0.1005(8) Uani 1 1 d . . . . .
C10 C 0.1644(2) 0.4810(3) 0.5044(3) 0.1354(16) Uani 1 1 d . . . . .
H10A H 0.138401 0.493179 0.472769 0.162 Uiso 1 1 calc R U . . .
C11 C 0.1561(3) 0.5042(4) 0.5630(3) 0.168(3) Uani 1 1 d . . . . .
H11A H 0.125537 0.532998 0.570480 0.202 Uiso 1 1 calc R U . . .
C12 C 0.1935(2) 0.4845(4) 0.6101(3) 0.165(3) Uani 1 1 d . . . . .
H12A H 0.186095 0.498255 0.649832 0.199 Uiso 1 1 calc R U . . .
C13 C 0.24186(16) 0.4446(2) 0.59957(16) 0.1177(11) Uani 1 1 d . . . . .
C14 C 0.24995(14) 0.42165(18) 0.54007(15) 0.1034(8) Uani 1 1 d . . . . .
H14A H 0.281684 0.394165 0.532319 0.124 Uiso 1 1 calc R U . . .
C15 C 0.28782(17) 0.4306(2) 0.64721(16) 0.1172(11) Uani 1 1 d . . . . .
C16 C 0.2712(3) 0.4069(4) 0.7042(2) 0.166(3) Uani 1 1 d . . . . .
H16A H 0.230429 0.398198 0.713249 0.199 Uiso 1 1 calc R U . . .
C17 C 0.3169(3) 0.3966(4) 0.7471(2) 0.168(3) Uani 1 1 d . . . . .
H17A H 0.306048 0.381152 0.785350 0.201 Uiso 1 1 calc R U . . .
C18 C 0.3777(3) 0.4084(3) 0.7352(2) 0.1436(18) Uani 1 1 d . . . . .
H18A H 0.407643 0.398800 0.764009 0.172 Uiso 1 1 calc R U . . .
C19 C 0.39371(17) 0.4349(2) 0.67910(14) 0.1051(8) Uani 1 1 d . . . . .
C20 C 0.34833(16) 0.44341(19) 0.63577(14) 0.1052(8) Uani 1 1 d . . . . .
H20A H 0.359214 0.458469 0.597336 0.126 Uiso 1 1 calc R U . . .
C21 C 0.45664(15) 0.45666(16) 0.66808(13) 0.0956(7) Uani 1 1 d . . . . .
C22 C 0.50957(18) 0.45417(17) 0.70388(16) 0.1051(8) Uani 1 1 d . . . . .
H22A H 0.514383 0.434689 0.741561 0.126 Uiso 1 1 calc R U . . .
C23 C 0.55317(15) 0.48655(15) 0.67181(15) 0.0964(7) Uani 1 1 d . . . . .
C24 C 0.61663(16) 0.50405(18) 0.68653(18) 0.1067(9) Uani 1 1 d . . . . .
C25 C 0.6475(3) 0.4809(3) 0.7362(3) 0.1443(18) Uani 1 1 d . . . . .
H25A H 0.628882 0.453590 0.763220 0.173 Uiso 1 1 calc R U . . .
C26 C 0.7077(3) 0.4998(4) 0.7446(3) 0.170(2) Uani 1 1 d . . . . .
H26A H 0.730145 0.485116 0.777792 0.204 Uiso 1 1 calc R U . . .
C27 C 0.7342(2) 0.5397(3) 0.7045(4) 0.166(2) Uani 1 1 d . . . . .
H27A H 0.774819 0.551806 0.709823 0.199 Uiso 1 1 calc R U . . .
C28 C 0.7007(2) 0.5617(3) 0.6565(3) 0.1418(17) Uani 1 1 d . . . . .
H28A H 0.719044 0.589113 0.629389 0.170 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43759(2) 0.43759(2) 0.43759(2) 0.08576(18) Uani 1 3 d S T P . .
O1 O 0.38639(8) 0.36863(9) 0.47098(9) 0.0856(4) Uani 1 1 d . . . . .
O2 O 0.49734(9) 0.40657(10) 0.49943(10) 0.0906(5) Uani 1 1 d . . . . .
O3 O 0.5153(2) 0.2506(3) 0.6463(2) 0.217(3) Uani 1 1 d . . . . .
O4 O 0.3994(2) 0.2162(3) 0.6221(2) 0.194(2) Uani 1 1 d . U . . .
C29 C 0.41259(12) 0.33891(14) 0.51552(12) 0.0855(5) Uani 1 1 d . . . . .
C30 C 0.47677(12) 0.35997(13) 0.53099(12) 0.0862(5) Uani 1 1 d . . . . .
C31 C 0.51068(16) 0.3307(2) 0.57424(17) 0.1143(11) Uani 1 1 d . . . . .
H31A H 0.550468 0.343954 0.582289 0.137 Uiso 1 1 calc R U . . .
C32 C 0.4863(2) 0.2804(3) 0.6073(2) 0.1313(15) Uani 1 1 d . U . . .
C33 C 0.4202(2) 0.2608(3) 0.59341(19) 0.1299(15) Uani 1 1 d . U . . .
C34 C 0.38718(16) 0.29234(19) 0.54664(15) 0.1036(8) Uani 1 1 d . . . . .
H34A H 0.347229 0.280381 0.537522 0.124 Uiso 1 1 calc R U . . .
B1 B 0.1397(5) 0.1397(5) 0.1397(5) 0.187(4) Uani 1 3 d DS TU P . 1
F1 F 0.1383(9) 0.1736(14) 0.0864(7) 0.223(5) Uani 0.3333 1 d D U P . 1
F2 F 0.1750(4) 0.1750(4) 0.1750(4) 0.325(6) Uani 1 3 d DS TU P . 1
F3 F 0.0907(7) 0.1172(11) 0.1567(11) 0.218(6) Uani 0.3333 1 d D U P . 1
F4 F 0.1824(10) 0.0931(7) 0.1264(12) 0.225(6) Uani 0.3333 1 d D U P . 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.010(2) 5 ?
Fe1 N2 2.010(2) 9 ?
Fe1 N2 2.010(2) . ?
Fe1 N1 2.063(3) 5 ?
Fe1 N1 2.063(3) 9 ?
Fe1 N1 2.063(3) . ?
Fe2 N5 2.073(3) 9 ?
Fe2 N5 2.073(3) 5 ?
Fe2 N5 2.073(3) . ?
Fe2 N6 2.119(3) 9 ?
Fe2 N6 2.119(3) 5 ?
Fe2 N6 2.119(3) . ?
N1 C1 1.331(4) . ?
N1 C5 1.348(5) . ?
N2 C6 1.327(4) . ?
N2 N3 1.356(3) . ?
N3 C8 1.370(4) . ?
N3 H3 0.90(3) . ?
N4 N5 1.348(4) . ?
N4 C21 1.357(4) . ?
N4 H4 0.90(3) . ?
N5 C23 1.340(4) . ?
N6 C24 1.351(5) . ?
N6 C28 1.364(5) . ?
C1 C2 1.393(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.357(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.359(7) . ?
C3 H3B 0.9300 . ?
C4 C5 1.394(5) . ?
C4 H4B 0.9300 . ?
C5 C6 1.468(4) . ?
C6 C7 1.389(5) . ?
C7 C8 1.385(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.454(4) . ?
C9 C14 1.382(5) . ?
C9 C10 1.397(6) . ?
C10 C11 1.384(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.380(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.384(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.401(5) . ?
C13 C15 1.474(6) . ?
C14 H14A 0.9300 . ?
C15 C20 1.370(5) . ?
C15 C16 1.393(6) . ?
C16 C17 1.382(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.373(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.380(5) . ?
C19 C21 1.471(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.393(5) . ?
C22 C23 1.374(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.469(5) . ?
C24 C25 1.371(5) . ?
C25 C26 1.387(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.360(10) . ?
C26 H26A 0.9300 . ?
C27 C28 1.363(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.991(2) 5 ?
Fe3 O2 1.991(2) 9 ?
Fe3 O2 1.991(2) . ?
Fe3 O1 2.0076(19) 9 ?
Fe3 O1 2.0076(19) 5 ?
Fe3 O1 2.0076(19) . ?
O1 C29 1.299(3) . ?
O2 C30 1.305(3) . ?
O3 C32 1.242(5) . ?
O4 C33 1.240(5) . ?
C29 C34 1.340(4) . ?
C29 C30 1.510(4) . ?
C30 C31 1.356(4) . ?
C31 C32 1.414(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.533(6) . ?
C33 C34 1.424(5) . ?
C34 H34A 0.9300 . ?
B1 F3 1.231(14) 5 ?
B1 F3 1.231(14) 9 ?
B1 F3 1.231(14) . ?
B1 F2 1.334(17) . ?
B1 F1 1.375(16) 9 ?
B1 F1 1.375(16) 5 ?
B1 F1 1.375(16) . ?
B1 F4 1.406(15) . ?
B1 F4 1.406(15) 9 ?
B1 F4 1.406(15) 5 ?
F1 F4 0.36(3) 5 ?
F1 F3 0.60(3) 9 ?
F3 F4 0.59(3) 9 ?
F3 F3 1.77(3) 9 ?
F3 F3 1.77(3) 5 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.83(9) 5 9 ?
N2 Fe1 N2 96.83(9) 5 . ?
N2 Fe1 N2 96.83(9) 9 . ?
N2 Fe1 N1 79.16(10) 5 5 ?
N2 Fe1 N1 171.11(10) 9 5 ?
N2 Fe1 N1 91.55(10) . 5 ?
N2 Fe1 N1 91.54(10) 5 9 ?
N2 Fe1 N1 79.16(10) 9 9 ?
N2 Fe1 N1 171.11(10) . 9 ?
N1 Fe1 N1 92.95(10) 5 9 ?
N2 Fe1 N1 171.11(10) 5 . ?
N2 Fe1 N1 91.54(10) 9 . ?
N2 Fe1 N1 79.16(10) . . ?
N1 Fe1 N1 92.95(10) 5 . ?
N1 Fe1 N1 92.95(10) 9 . ?
N5 Fe2 N5 97.77(9) 9 5 ?
N5 Fe2 N5 97.77(9) 9 . ?
N5 Fe2 N5 97.76(9) 5 . ?
N5 Fe2 N6 77.00(11) 9 9 ?
N5 Fe2 N6 167.83(12) 5 9 ?
N5 Fe2 N6 93.86(12) . 9 ?
N5 Fe2 N6 93.85(12) 9 5 ?
N5 Fe2 N6 77.00(11) 5 5 ?
N5 Fe2 N6 167.83(12) . 5 ?
N6 Fe2 N6 92.27(12) 9 5 ?
N5 Fe2 N6 167.83(12) 9 . ?
N5 Fe2 N6 93.86(12) 5 . ?
N5 Fe2 N6 77.00(11) . . ?
N6 Fe2 N6 92.26(12) 9 . ?
N6 Fe2 N6 92.27(12) 5 . ?
C1 N1 C5 118.7(3) . . ?
C1 N1 Fe1 127.1(3) . . ?
C5 N1 Fe1 114.23(19) . . ?
C6 N2 N3 106.3(2) . . ?
C6 N2 Fe1 116.3(2) . . ?
N3 N2 Fe1 136.06(19) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 115(3) . . ?
C8 N3 H3 134(3) . . ?
N5 N4 C21 111.5(2) . . ?
N5 N4 H4 107(4) . . ?
C21 N4 H4 141(4) . . ?
C23 N5 N4 105.4(3) . . ?
C23 N5 Fe2 115.5(2) . . ?
N4 N5 Fe2 135.2(2) . . ?
C24 N6 C28 117.0(4) . . ?
C24 N6 Fe2 115.4(2) . . ?
C28 N6 Fe2 127.5(3) . . ?
N1 C1 C2 122.0(4) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.2(4) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.6(4) . . ?
C2 C3 H3B 120.2 . . ?
C4 C3 H3B 120.2 . . ?
C3 C4 C5 119.5(4) . . ?
C3 C4 H4B 120.3 . . ?
C5 C4 H4B 120.3 . . ?
N1 C5 C4 121.1(3) . . ?
N1 C5 C6 114.6(3) . . ?
C4 C5 C6 124.3(3) . . ?
N2 C6 C7 111.0(3) . . ?
N2 C6 C5 115.2(3) . . ?
C7 C6 C5 133.8(3) . . ?
C8 C7 C6 105.7(3) . . ?
C8 C7 H7A 127.1 . . ?
C6 C7 H7A 127.1 . . ?
N3 C8 C7 106.4(3) . . ?
N3 C8 C9 123.1(3) . . ?
C7 C8 C9 130.5(3) . . ?
C14 C9 C10 119.3(4) . . ?
C14 C9 C8 122.0(3) . . ?
C10 C9 C8 118.7(4) . . ?
C11 C10 C9 120.1(5) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C12 C11 C10 119.7(5) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 121.4(4) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.3(4) . . ?
C12 C13 C15 122.0(4) . . ?
C14 C13 C15 119.4(4) . . ?
C9 C14 C13 121.1(3) . . ?
C9 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C20 C15 C16 119.2(4) . . ?
C20 C15 C13 118.9(3) . . ?
C16 C15 C13 121.9(4) . . ?
C17 C16 C15 118.4(4) . . ?
C17 C16 H16A 120.8 . . ?
C15 C16 H16A 120.8 . . ?
C18 C17 C16 122.4(4) . . ?
C18 C17 H17A 118.8 . . ?
C16 C17 H17A 118.8 . . ?
C17 C18 C19 118.9(5) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.4(4) . . ?
C20 C19 C21 120.8(3) . . ?
C18 C19 C21 120.7(4) . . ?
C15 C20 C19 122.5(3) . . ?
C15 C20 H20A 118.7 . . ?
C19 C20 H20A 118.7 . . ?
N4 C21 C22 106.2(3) . . ?
N4 C21 C19 121.7(3) . . ?
C22 C21 C19 131.9(3) . . ?
C23 C22 C21 105.5(3) . . ?
C23 C22 H22A 127.2 . . ?
C21 C22 H22A 127.2 . . ?
N5 C23 C22 111.3(3) . . ?
N5 C23 C24 116.2(3) . . ?
C22 C23 C24 132.3(3) . . ?
N6 C24 C25 123.6(4) . . ?
N6 C24 C23 113.8(3) . . ?
C25 C24 C23 122.6(4) . . ?
C24 C25 C26 117.3(5) . . ?
C24 C25 H25A 121.3 . . ?
C26 C25 H25A 121.3 . . ?
C27 C26 C25 120.5(5) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 119.3(5) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
C27 C28 N6 122.3(5) . . ?
C27 C28 H28A 118.9 . . ?
N6 C28 H28A 118.9 . . ?
O2 Fe3 O2 90.53(9) 5 9 ?
O2 Fe3 O2 90.53(9) 5 . ?
O2 Fe3 O2 90.53(9) 9 . ?
O2 Fe3 O1 94.64(9) 5 9 ?
O2 Fe3 O1 82.19(7) 9 9 ?
O2 Fe3 O1 171.10(8) . 9 ?
O2 Fe3 O1 82.19(7) 5 5 ?
O2 Fe3 O1 171.10(8) 9 5 ?
O2 Fe3 O1 94.64(9) . 5 ?
O1 Fe3 O1 93.24(8) 9 5 ?
O2 Fe3 O1 171.10(8) 5 . ?
O2 Fe3 O1 94.64(9) 9 . ?
O2 Fe3 O1 82.19(7) . . ?
O1 Fe3 O1 93.24(8) 9 . ?
O1 Fe3 O1 93.25(8) 5 . ?
C29 O1 Fe3 113.56(16) . . ?
C30 O2 Fe3 113.31(16) . . ?
O1 C29 C34 125.0(3) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.0(3) . . ?
O2 C30 C31 123.0(3) . . ?
O2 C30 C29 115.9(2) . . ?
C31 C30 C29 121.1(3) . . ?
C30 C31 C32 120.9(3) . . ?
C30 C31 H31A 119.6 . . ?
C32 C31 H31A 119.6 . . ?
O3 C32 C31 124.3(4) . . ?
O3 C32 C33 117.8(4) . . ?
C31 C32 C33 117.9(3) . . ?
O4 C33 C34 123.6(4) . . ?
O4 C33 C32 117.6(4) . . ?
C34 C33 C32 118.8(3) . . ?
C29 C34 C33 121.2(3) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F3 B1 F3 92.2(16) 5 9 ?
F3 B1 F3 92.2(16) 5 . ?
F3 B1 F3 92.2(16) 9 . ?
F3 B1 F2 123.7(12) 5 . ?
F3 B1 F2 123.7(12) 9 . ?
F3 B1 F2 123.7(12) . . ?
F3 B1 F1 25.6(14) 5 9 ?
F3 B1 F1 116.7(15) 9 9 ?
F3 B1 F1 98(2) . 9 ?
F2 B1 F1 100.9(14) . 9 ?
F3 B1 F1 116.7(15) 5 5 ?
F3 B1 F1 98(2) 9 5 ?
F3 B1 F1 25.6(14) . 5 ?
F2 B1 F1 100.9(14) . 5 ?
F1 B1 F1 116.5(9) 9 5 ?
F3 B1 F1 98(2) 5 . ?
F3 B1 F1 25.6(14) 9 . ?
F3 B1 F1 116.7(15) . . ?
F2 B1 F1 100.9(14) . . ?
F1 B1 F1 116.5(9) 9 . ?
F1 B1 F1 116.5(9) 5 . ?
F3 B1 F4 25.0(14) 5 . ?
F3 B1 F4 108(2) 9 . ?
F3 B1 F4 110.4(15) . . ?
F2 B1 F4 98.8(13) . . ?
F1 B1 F4 14.6(12) 9 . ?
F1 B1 F4 130.8(13) 5 . ?
F1 B1 F4 103.1(12) . . ?
F3 B1 F4 108(2) 5 9 ?
F3 B1 F4 110.4(15) 9 9 ?
F3 B1 F4 25.0(14) . 9 ?
F2 B1 F4 98.8(13) . 9 ?
F1 B1 F4 103.1(12) 9 9 ?
F1 B1 F4 14.6(12) 5 9 ?
F1 B1 F4 130.8(13) . 9 ?
F4 B1 F4 117.7(7) . 9 ?
F3 B1 F4 110.4(15) 5 5 ?
F3 B1 F4 25.0(14) 9 5 ?
F3 B1 F4 108(2) . 5 ?
F2 B1 F4 98.8(13) . 5 ?
F1 B1 F4 130.8(13) 9 5 ?
F1 B1 F4 103.1(12) 5 5 ?
F1 B1 F4 14.6(12) . 5 ?
F4 B1 F4 117.7(7) . 5 ?
F4 B1 F4 117.7(7) 9 5 ?
F4 F1 F3 73(6) 5 9 ?
F4 F1 B1 88(4) 5 . ?
F3 F1 B1 63(2) 9 . ?
F4 F3 F1 35(3) 9 5 ?
F4 F3 B1 94(2) 9 . ?
F1 F3 B1 91(2) 5 . ?
F4 F3 F3 125(3) 9 9 ?
F1 F3 F3 100(5) 5 9 ?
B1 F3 F3 43.9(8) . 9 ?
F4 F3 F3 119(3) 9 5 ?
F1 F3 F3 133(2) 5 5 ?
B1 F3 F3 43.9(8) . 5 ?
F3 F3 F3 59.997(2) 9 5 ?
F1 F4 F3 73(6) 9 5 ?
F1 F4 B1 78(4) 9 . ?
F3 F4 B1 60.8(18) 5 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(3) 2.09(3) 2.922(3) 154(5) . yes
N4 H4 O2 0.90(3) 2.19(4) 2.986(3) 147(5) 9 yes

_refine_diff_density_max         0.229
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.045

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_350Kd
_database_code_depnum_ccdc_archive 'CCDC 2260949'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.769(3)
_cell_length_b                   21.769(3)
_cell_length_c                   21.769(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10316(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    6231
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      32.64

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            169355
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0534
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.920
_diffrn_reflns_theta_max         29.516
_diffrn_reflns_theta_full        29.516
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8877
_reflns_number_gt                8343
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
;

_vrf_PLAT601_lb2205_fresh1_350Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1799 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1799 cubic angstrom with less than 50 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0804P)²+0.1780P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0071(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3677 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.075(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8877
_refine_ls_number_parameters     458
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.1128
_refine_ls_wR_factor_gt          0.1108
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.065
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29790(2) 0.29790(2) 0.29790(2) 0.07171(14) Uani 1 3 d S T P . .
Fe2 Fe 0.57932(2) 0.57932(2) 0.57932(2) 0.07565(15) Uani 1 3 d S T P . .
N1 N 0.23171(11) 0.33218(10) 0.24191(9) 0.0824(5) Uani 1 1 d . . . . .
N2 N 0.26047(9) 0.36049(10) 0.35279(9) 0.0764(4) Uani 1 1 d . . . . .
N3 N 0.26528(9) 0.37605(10) 0.41289(9) 0.0793(4) Uani 1 1 d D . . . .
H3 H 0.3011(14) 0.3620(19) 0.4306(18) 0.119 Uiso 1 1 d D U . . .
N4 N 0.47081(10) 0.49122(12) 0.61669(9) 0.0837(5) Uani 1 1 d D . . . .
H4 H 0.4440(17) 0.503(2) 0.5873(16) 0.126 Uiso 1 1 d D U . . .
N5 N 0.52991(10) 0.50927(11) 0.61807(9) 0.0821(5) Uani 1 1 d . . . . .
N6 N 0.64075(11) 0.54464(12) 0.64419(13) 0.0953(6) Uani 1 1 d . . . . .
C1 C 0.22031(17) 0.31583(15) 0.18331(13) 0.0967(7) Uani 1 1 d . . . . .
H1A H 0.245780 0.287025 0.164684 0.116 Uiso 1 1 calc R U . . .
C2 C 0.1722(2) 0.34024(18) 0.14981(16) 0.1192(12) Uani 1 1 d . . . . .
H2A H 0.165254 0.327619 0.109597 0.143 Uiso 1 1 calc R U . . .
C3 C 0.1350(2) 0.3832(2) 0.1766(2) 0.1268(13) Uani 1 1 d . . . . .
H3B H 0.101932 0.399583 0.154967 0.152 Uiso 1 1 calc R U . . .
C4 C 0.14695(19) 0.40201(18) 0.23617(18) 0.1120(10) Uani 1 1 d . . . . .
H4B H 0.123291 0.432480 0.254528 0.134 Uiso 1 1 calc R U . . .
C5 C 0.19494(13) 0.37458(12) 0.26801(12) 0.0852(6) Uani 1 1 d . . . . .
C6 C 0.21023(12) 0.38818(12) 0.33173(12) 0.0821(5) Uani 1 1 d . . . . .
C7 C 0.18198(12) 0.42222(14) 0.37786(14) 0.0913(6) Uani 1 1 d . . . . .
H7A H 0.146222 0.445372 0.374664 0.110 Uiso 1 1 calc R U . . .
C8 C 0.21821(11) 0.41441(13) 0.42944(13) 0.0846(5) Uani 1 1 d . . . . .
C9 C 0.21140(11) 0.43923(14) 0.49165(13) 0.0898(6) Uani 1 1 d . . . . .
C10 C 0.16453(17) 0.4816(2) 0.5029(2) 0.1236(13) Uani 1 1 d . . . . .
H10A H 0.139072 0.494586 0.471131 0.148 Uiso 1 1 calc R U . . .
C11 C 0.1563(2) 0.5044(3) 0.5621(2) 0.155(2) Uani 1 1 d . . . . .
H11A H 0.125274 0.532673 0.569961 0.186 Uiso 1 1 calc R U . . .
C12 C 0.19322(19) 0.4854(3) 0.6083(2) 0.150(2) Uani 1 1 d . . . . .
H12A H 0.186327 0.500118 0.647835 0.180 Uiso 1 1 calc R U . . .
C13 C 0.24115(14) 0.44452(19) 0.59839(14) 0.1051(9) Uani 1 1 d . . . . .
C14 C 0.24946(12) 0.42205(15) 0.53897(13) 0.0925(7) Uani 1 1 d . . . . .
H14A H 0.281469 0.394832 0.531209 0.111 Uiso 1 1 calc R U . . .
C15 C 0.28706(14) 0.42983(19) 0.64603(13) 0.1038(9) Uani 1 1 d . . . . .
C16 C 0.2723(2) 0.4057(3) 0.70374(19) 0.147(2) Uani 1 1 d . . . . .
H16A H 0.231719 0.396006 0.712974 0.177 Uiso 1 1 calc R U . . .
C17 C 0.3169(2) 0.3964(3) 0.74637(18) 0.1491(19) Uani 1 1 d . . . . .
H17A H 0.306235 0.380721 0.784644 0.179 Uiso 1 1 calc R U . . .
C18 C 0.3778(2) 0.4096(3) 0.73425(17) 0.1304(14) Uani 1 1 d . . . . .
H18A H 0.407938 0.401730 0.763529 0.156 Uiso 1 1 calc R U . . .
C19 C 0.39358(14) 0.43498(17) 0.67751(12) 0.0957(7) Uani 1 1 d . . . . .
C20 C 0.34813(13) 0.44356(15) 0.63446(12) 0.0932(7) Uani 1 1 d . . . . .
H20A H 0.358794 0.459164 0.596145 0.112 Uiso 1 1 calc R U . . .
C21 C 0.45642(14) 0.45670(14) 0.66638(12) 0.0882(6) Uani 1 1 d . . . . .
C22 C 0.50974(15) 0.45328(15) 0.70200(13) 0.0938(7) Uani 1 1 d . . . . .
H22A H 0.514792 0.433041 0.739283 0.113 Uiso 1 1 calc R U . . .
C23 C 0.55303(13) 0.48621(13) 0.67016(12) 0.0866(6) Uani 1 1 d . . . . .
C24 C 0.61708(14) 0.50315(15) 0.68395(15) 0.0957(7) Uani 1 1 d . . . . .
C25 C 0.6493(2) 0.4796(2) 0.7323(2) 0.1339(15) Uani 1 1 d . . . . .
H25A H 0.631028 0.452048 0.759328 0.161 Uiso 1 1 calc R U . . .
C26 C 0.7092(2) 0.4975(3) 0.7403(3) 0.156(2) Uani 1 1 d . . . . .
H26A H 0.732111 0.482177 0.772955 0.187 Uiso 1 1 calc R U . . .
C27 C 0.7347(2) 0.5380(3) 0.7001(3) 0.156(2) Uani 1 1 d . . . . .
H27A H 0.775535 0.549659 0.704609 0.187 Uiso 1 1 calc R U . . .
C28 C 0.70013(16) 0.5615(2) 0.6528(2) 0.1242(12) Uani 1 1 d . . . . .
H28A H 0.717870 0.589705 0.626006 0.149 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43695(2) 0.43695(2) 0.43695(2) 0.07766(15) Uani 1 3 d S T P . .
O1 O 0.38549(7) 0.36793(8) 0.47036(8) 0.0781(4) Uani 1 1 d . . . . .
O2 O 0.49663(8) 0.40624(8) 0.49938(9) 0.0814(4) Uani 1 1 d . . . . .
O3 O 0.51387(17) 0.2507(3) 0.64621(19) 0.194(2) Uani 1 1 d . . . . .
O4 O 0.39815(17) 0.2150(2) 0.62105(18) 0.1773(19) Uani 1 1 d . U . . .
C29 C 0.41157(10) 0.33853(12) 0.51534(11) 0.0771(5) Uani 1 1 d . . . . .
C30 C 0.47576(11) 0.35954(12) 0.53062(11) 0.0788(5) Uani 1 1 d . . . . .
C31 C 0.50935(14) 0.32996(18) 0.57398(15) 0.1048(9) Uani 1 1 d . . . . .
H31A H 0.549336 0.342939 0.581565 0.126 Uiso 1 1 calc R U . . .
C32 C 0.48557(17) 0.2801(2) 0.60795(17) 0.1228(13) Uani 1 1 d . U . . .
C33 C 0.41861(17) 0.2593(2) 0.59329(17) 0.1170(12) Uani 1 1 d . U . . .
C34 C 0.38535(13) 0.29164(16) 0.54624(13) 0.0937(7) Uani 1 1 d . . . . .
H34A H 0.345264 0.280106 0.537018 0.112 Uiso 1 1 calc R U . . .
B1 B 0.1390(10) 0.1419(11) 0.1421(9) 0.137(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1371(10) 0.1801(9) 0.0926(10) 0.182(8) Uani 0.3333 1 d D U P A -1
F2 F 0.1495(9) 0.1716(12) 0.1935(7) 0.222(7) Uani 0.3333 1 d D U P A -1
F3 F 0.0813(8) 0.1147(9) 0.1491(8) 0.201(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1806(10) 0.0961(10) 0.1325(10) 0.177(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.987(2) . ?
Fe1 N2 1.987(2) 9 ?
Fe1 N2 1.987(2) 5 ?
Fe1 N1 2.029(2) 5 ?
Fe1 N1 2.029(2) 9 ?
Fe1 N1 2.030(2) . ?
Fe2 N5 2.048(2) . ?
Fe2 N5 2.048(2) 9 ?
Fe2 N5 2.048(2) 5 ?
Fe2 N6 2.086(2) 9 ?
Fe2 N6 2.086(2) 5 ?
Fe2 N6 2.086(2) . ?
N1 C5 1.347(4) . ?
N1 C1 1.347(4) . ?
N2 C6 1.330(3) . ?
N2 N3 1.355(3) . ?
N3 C8 1.370(3) . ?
N3 H3 0.92(2) . ?
N4 N5 1.346(3) . ?
N4 C21 1.354(4) . ?
N4 H4 0.90(2) . ?
N5 C23 1.338(3) . ?
N6 C24 1.353(4) . ?
N6 C28 1.357(4) . ?
C1 C2 1.382(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(6) . ?
C3 H3B 0.9300 . ?
C4 C5 1.389(4) . ?
C4 H4B 0.9300 . ?
C5 C6 1.457(4) . ?
C6 C7 1.391(4) . ?
C7 C8 1.383(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.465(4) . ?
C9 C14 1.374(4) . ?
C9 C10 1.398(5) . ?
C10 C11 1.393(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.352(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.388(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C15 1.475(5) . ?
C14 H14A 0.9300 . ?
C15 C20 1.386(4) . ?
C15 C16 1.399(5) . ?
C16 C17 1.359(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.382(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.396(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.375(4) . ?
C19 C21 1.467(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.398(4) . ?
C22 C23 1.372(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.473(4) . ?
C24 C25 1.365(5) . ?
C25 C26 1.371(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.360(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.375(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9955(17) 5 ?
Fe3 O2 1.9955(17) 9 ?
Fe3 O2 1.9955(17) . ?
Fe3 O1 2.0104(17) . ?
Fe3 O1 2.0104(17) 5 ?
Fe3 O1 2.0104(17) 9 ?
O1 C29 1.300(3) . ?
O2 C30 1.305(3) . ?
O3 C32 1.218(5) . ?
O4 C33 1.221(5) . ?
C29 C34 1.349(4) . ?
C29 C30 1.507(3) . ?
C30 C31 1.356(4) . ?
C31 C32 1.411(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.560(5) . ?
C33 C34 1.439(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.312(14) . ?
B1 F1 1.36(2) . ?
B1 F4 1.363(19) . ?
B1 F3 1.398(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.63(8) . 9 ?
N2 Fe1 N2 96.63(8) . 5 ?
N2 Fe1 N2 96.63(8) 9 5 ?
N2 Fe1 N1 91.11(8) . 5 ?
N2 Fe1 N1 171.72(8) 9 5 ?
N2 Fe1 N1 79.51(8) 5 5 ?
N2 Fe1 N1 171.72(8) . 9 ?
N2 Fe1 N1 79.51(8) 9 9 ?
N2 Fe1 N1 91.11(8) 5 9 ?
N1 Fe1 N1 93.18(9) 5 9 ?
N2 Fe1 N1 79.51(8) . . ?
N2 Fe1 N1 91.11(8) 9 . ?
N2 Fe1 N1 171.72(8) 5 . ?
N1 Fe1 N1 93.18(9) 5 . ?
N1 Fe1 N1 93.18(9) 9 . ?
N5 Fe2 N5 97.59(8) . 9 ?
N5 Fe2 N5 97.59(8) . 5 ?
N5 Fe2 N5 97.59(8) 9 5 ?
N5 Fe2 N6 92.86(10) . 9 ?
N5 Fe2 N6 77.78(9) 9 9 ?
N5 Fe2 N6 169.07(10) 5 9 ?
N5 Fe2 N6 169.07(10) . 5 ?
N5 Fe2 N6 92.86(10) 9 5 ?
N5 Fe2 N6 77.78(9) 5 5 ?
N6 Fe2 N6 92.47(10) 9 5 ?
N5 Fe2 N6 77.78(9) . . ?
N5 Fe2 N6 169.07(10) 9 . ?
N5 Fe2 N6 92.86(10) 5 . ?
N6 Fe2 N6 92.47(10) 9 . ?
N6 Fe2 N6 92.47(10) 5 . ?
C5 N1 C1 118.1(2) . . ?
C5 N1 Fe1 114.85(16) . . ?
C1 N1 Fe1 127.0(2) . . ?
C6 N2 N3 106.4(2) . . ?
C6 N2 Fe1 116.14(17) . . ?
N3 N2 Fe1 136.07(16) . . ?
N2 N3 C8 110.4(2) . . ?
N2 N3 H3 113(3) . . ?
C8 N3 H3 136(3) . . ?
N5 N4 C21 111.5(2) . . ?
N5 N4 H4 123(3) . . ?
C21 N4 H4 125(3) . . ?
C23 N5 N4 105.6(2) . . ?
C23 N5 Fe2 115.53(19) . . ?
N4 N5 Fe2 135.27(18) . . ?
C24 N6 C28 117.1(3) . . ?
C24 N6 Fe2 115.50(19) . . ?
C28 N6 Fe2 127.3(3) . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4B 120.6 . . ?
C5 C4 H4B 120.6 . . ?
N1 C5 C4 122.1(3) . . ?
N1 C5 C6 113.9(2) . . ?
C4 C5 C6 124.0(3) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.1(2) . . ?
C7 C6 C5 134.0(2) . . ?
C8 C7 C6 105.6(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.7(2) . . ?
N3 C8 C9 122.9(2) . . ?
C7 C8 C9 130.4(2) . . ?
C14 C9 C10 119.2(3) . . ?
C14 C9 C8 122.1(3) . . ?
C10 C9 C8 118.6(3) . . ?
C11 C10 C9 119.4(4) . . ?
C11 C10 H10A 120.3 . . ?
C9 C10 H10A 120.3 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.8(4) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C12 C13 C14 117.8(3) . . ?
C12 C13 C15 122.6(3) . . ?
C14 C13 C15 119.2(3) . . ?
C9 C14 C13 121.4(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C20 C15 C16 117.7(3) . . ?
C20 C15 C13 118.4(3) . . ?
C16 C15 C13 123.8(3) . . ?
C17 C16 C15 120.3(4) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 121.6(3) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 C21 120.9(3) . . ?
C18 C19 C21 120.2(3) . . ?
C19 C20 C15 122.5(3) . . ?
C19 C20 H20A 118.8 . . ?
C15 C20 H20A 118.8 . . ?
N4 C21 C22 106.3(2) . . ?
N4 C21 C19 121.8(3) . . ?
C22 C21 C19 131.7(3) . . ?
C23 C22 C21 105.2(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.5(3) . . ?
N5 C23 C24 115.8(3) . . ?
C22 C23 C24 132.7(3) . . ?
N6 C24 C25 123.2(3) . . ?
N6 C24 C23 113.4(2) . . ?
C25 C24 C23 123.4(3) . . ?
C24 C25 C26 118.7(5) . . ?
C24 C25 H25A 120.6 . . ?
C26 C25 H25A 120.6 . . ?
C27 C26 C25 119.3(4) . . ?
C27 C26 H26A 120.3 . . ?
C25 C26 H26A 120.3 . . ?
C26 C27 C28 120.0(4) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
N6 C28 C27 121.6(4) . . ?
N6 C28 H28A 119.2 . . ?
C27 C28 H28A 119.2 . . ?
O2 Fe3 O2 90.17(8) 5 9 ?
O2 Fe3 O2 90.17(8) 5 . ?
O2 Fe3 O2 90.17(8) 9 . ?
O2 Fe3 O1 170.87(7) 5 . ?
O2 Fe3 O1 94.97(7) 9 . ?
O2 Fe3 O1 82.30(6) . . ?
O2 Fe3 O1 82.30(6) 5 5 ?
O2 Fe3 O1 170.87(7) 9 5 ?
O2 Fe3 O1 94.98(7) . 5 ?
O1 Fe3 O1 93.18(7) . 5 ?
O2 Fe3 O1 94.98(7) 5 9 ?
O2 Fe3 O1 82.30(6) 9 9 ?
O2 Fe3 O1 170.87(7) . 9 ?
O1 Fe3 O1 93.18(7) . 9 ?
O1 Fe3 O1 93.18(7) 5 9 ?
C29 O1 Fe3 113.39(15) . . ?
C30 O2 Fe3 112.91(14) . . ?
O1 C29 C34 124.3(2) . . ?
O1 C29 C30 114.9(2) . . ?
C34 C29 C30 120.8(2) . . ?
O2 C30 C31 123.0(2) . . ?
O2 C30 C29 116.4(2) . . ?
C31 C30 C29 120.6(2) . . ?
C30 C31 C32 122.1(3) . . ?
C30 C31 H31A 118.9 . . ?
C32 C31 H31A 118.9 . . ?
O3 C32 C31 125.3(4) . . ?
O3 C32 C33 117.4(4) . . ?
C31 C32 C33 117.3(3) . . ?
O4 C33 C34 123.7(3) . . ?
O4 C33 C32 118.0(3) . . ?
C34 C33 C32 118.3(3) . . ?
C29 C34 C33 120.8(3) . . ?
C29 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
F2 B1 F1 112.3(17) . . ?
F2 B1 F4 112.1(17) . . ?
F1 B1 F4 110.2(17) . . ?
F2 B1 F3 105.8(15) . . ?
F1 B1 F3 108.5(17) . . ?
F4 B1 F3 107.7(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.92(2) 2.04(3) 2.906(3) 157(4) . yes
N4 H4 O2 0.90(2) 2.14(3) 2.973(3) 153(4) 9 yes

_refine_diff_density_max         0.202
_refine_diff_density_min         -0.350
_refine_diff_density_rms         0.042

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_320Kd
_database_code_depnum_ccdc_archive 'CCDC 2260950'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.743(3)
_cell_length_b                   21.743(3)
_cell_length_c                   21.743(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10279(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    6619
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      33.95

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.524
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            168499
_diffrn_reflns_av_unetI/netI     0.0196
_diffrn_reflns_av_R_equivalents  0.0481
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.359
_diffrn_reflns_theta_max         29.499
_diffrn_reflns_theta_full        29.499
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8851
_reflns_number_gt                8490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1844 cubic angstrom with a total of 71 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
 
 Details of SQUEEZE results (before BF4 disorder refinement):

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.113  0.145  0.134      1844        71 ' '
   2  0.144  0.356  0.644        10         0 ' '
   3  0.356  0.644  0.144        10         0 ' '
   4  0.644  0.144  0.356        10         0 ' '
   5  0.856  0.856  0.856        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_320Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1838 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1844 cubic angstrom with a total of 71 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0682P)²+0.2614P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8851
_refine_ls_number_parameters     458
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0323
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0988
_refine_ls_wR_factor_gt          0.0977
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.063
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29779(2) 0.29779(2) 0.29779(2) 0.06352(12) Uani 1 3 d S T P . .
Fe2 Fe 0.57918(2) 0.57918(2) 0.57918(2) 0.06691(13) Uani 1 3 d S T P . .
N1 N 0.23274(9) 0.33192(9) 0.24125(8) 0.0718(4) Uani 1 1 d . . . . .
N2 N 0.26082(8) 0.36014(8) 0.35220(8) 0.0678(3) Uani 1 1 d . . . . .
N3 N 0.26514(8) 0.37561(9) 0.41218(8) 0.0692(4) Uani 1 1 d D . . . .
H3 H 0.2992(13) 0.3617(17) 0.4312(16) 0.104 Uiso 1 1 d D U . . .
N4 N 0.47087(9) 0.49255(11) 0.61579(8) 0.0736(4) Uani 1 1 d D . . . .
H4 H 0.4476(15) 0.5027(17) 0.5852(14) 0.110 Uiso 1 1 d D U . . .
N5 N 0.53028(9) 0.51035(10) 0.61712(8) 0.0727(4) Uani 1 1 d . . . . .
N6 N 0.64077(10) 0.54479(11) 0.64206(11) 0.0835(5) Uani 1 1 d . . . . .
C1 C 0.22168(14) 0.31540(13) 0.18285(11) 0.0842(6) Uani 1 1 d . . . . .
H1A H 0.247068 0.286285 0.164480 0.101 Uiso 1 1 calc R U . . .
C2 C 0.17391(18) 0.34013(16) 0.14901(14) 0.1034(9) Uani 1 1 d . . . . .
H2A H 0.166963 0.327149 0.108853 0.124 Uiso 1 1 calc R U . . .
C3 C 0.13675(18) 0.38401(17) 0.17515(16) 0.1089(10) Uani 1 1 d . . . . .
H3B H 0.104551 0.401204 0.152863 0.131 Uiso 1 1 calc R U . . .
C4 C 0.14782(16) 0.40221(15) 0.23479(15) 0.0973(8) Uani 1 1 d . . . . .
H4B H 0.123536 0.432207 0.253227 0.117 Uiso 1 1 calc R U . . .
C5 C 0.19591(11) 0.37497(11) 0.26700(11) 0.0754(5) Uani 1 1 d . . . . .
C6 C 0.21066(10) 0.38822(11) 0.33084(11) 0.0731(5) Uani 1 1 d . . . . .
C7 C 0.18242(11) 0.42242(12) 0.37684(12) 0.0811(6) Uani 1 1 d . . . . .
H7A H 0.146778 0.445828 0.373479 0.097 Uiso 1 1 calc R U . . .
C8 C 0.21831(10) 0.41441(11) 0.42851(11) 0.0744(5) Uani 1 1 d . . . . .
C9 C 0.21117(10) 0.43938(12) 0.49072(12) 0.0801(5) Uani 1 1 d . . . . .
C10 C 0.16380(15) 0.4812(2) 0.50194(17) 0.1091(10) Uani 1 1 d . . . . .
H10A H 0.138045 0.493624 0.470142 0.131 Uiso 1 1 calc R U . . .
C11 C 0.15540(18) 0.5041(3) 0.5610(2) 0.1382(17) Uani 1 1 d . . . . .
H11A H 0.124522 0.532704 0.568585 0.166 Uiso 1 1 calc R U . . .
C12 C 0.19247(16) 0.4847(2) 0.60830(17) 0.1267(14) Uani 1 1 d . . . . .
H12A H 0.184927 0.498554 0.648051 0.152 Uiso 1 1 calc R U . . .
C13 C 0.24100(12) 0.44469(16) 0.59770(12) 0.0929(7) Uani 1 1 d . . . . .
C14 C 0.24920(11) 0.42218(13) 0.53810(11) 0.0810(6) Uani 1 1 d . . . . .
H14A H 0.281201 0.394889 0.530326 0.097 Uiso 1 1 calc R U . . .
C15 C 0.28681(13) 0.43031(16) 0.64561(12) 0.0926(7) Uani 1 1 d . . . . .
C16 C 0.27173(18) 0.4061(3) 0.70282(16) 0.1296(15) Uani 1 1 d . . . . .
H16A H 0.231034 0.396678 0.712047 0.155 Uiso 1 1 calc R U . . .
C17 C 0.3169(2) 0.3961(3) 0.74559(16) 0.1382(17) Uani 1 1 d . . . . .
H17A H 0.306293 0.379971 0.783775 0.166 Uiso 1 1 calc R U . . .
C18 C 0.37816(18) 0.4093(2) 0.73340(15) 0.1183(12) Uani 1 1 d . . . . .
H18A H 0.408365 0.401041 0.762539 0.142 Uiso 1 1 calc R U . . .
C19 C 0.39379(12) 0.43524(14) 0.67648(11) 0.0848(6) Uani 1 1 d . . . . .
C20 C 0.34837(12) 0.44405(13) 0.63340(11) 0.0832(6) Uani 1 1 d . . . . .
H20A H 0.358943 0.459624 0.594993 0.100 Uiso 1 1 calc R U . . .
C21 C 0.45702(12) 0.45697(12) 0.66532(10) 0.0781(5) Uani 1 1 d . . . . .
C22 C 0.50994(13) 0.45278(13) 0.70027(12) 0.0849(6) Uani 1 1 d . . . . .
H22A H 0.515048 0.431808 0.737200 0.102 Uiso 1 1 calc R U . . .
C23 C 0.55357(12) 0.48632(11) 0.66874(11) 0.0768(5) Uani 1 1 d . . . . .
C24 C 0.61757(12) 0.50309(13) 0.68181(13) 0.0854(6) Uani 1 1 d . . . . .
C25 C 0.65044(18) 0.47925(18) 0.7303(2) 0.1151(11) Uani 1 1 d . . . . .
H25A H 0.632595 0.451442 0.757424 0.138 Uiso 1 1 calc R U . . .
C26 C 0.71073(19) 0.4978(2) 0.7374(2) 0.1374(16) Uani 1 1 d . . . . .
H26A H 0.734236 0.482379 0.769643 0.165 Uiso 1 1 calc R U . . .
C27 C 0.73570(17) 0.5388(2) 0.6972(2) 0.1366(16) Uani 1 1 d . . . . .
H27A H 0.776411 0.551206 0.701500 0.164 Uiso 1 1 calc R U . . .
C28 C 0.69995(14) 0.56182(18) 0.64987(19) 0.1082(9) Uani 1 1 d . . . . .
H28A H 0.717214 0.589882 0.622604 0.130 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43679(2) 0.43679(2) 0.43679(2) 0.06980(13) Uani 1 3 d S T P . .
O1 O 0.38496(6) 0.36798(7) 0.47008(7) 0.0690(3) Uani 1 1 d . . . . .
O2 O 0.49598(7) 0.40597(7) 0.49979(8) 0.0726(3) Uani 1 1 d . . . . .
O3 O 0.51269(15) 0.2505(2) 0.64656(16) 0.181(2) Uani 1 1 d . . . . .
O4 O 0.39735(15) 0.21492(18) 0.62138(16) 0.1634(17) Uani 1 1 d . U . . .
C29 C 0.41098(9) 0.33830(10) 0.51518(9) 0.0690(4) Uani 1 1 d . . . . .
C30 C 0.47499(9) 0.35923(11) 0.53083(10) 0.0709(4) Uani 1 1 d . . . . .
C31 C 0.50843(12) 0.32977(16) 0.57427(13) 0.0947(8) Uani 1 1 d . . . . .
H31A H 0.548360 0.342865 0.582245 0.114 Uiso 1 1 calc R U . . .
C32 C 0.48424(15) 0.2796(2) 0.60788(15) 0.1113(11) Uani 1 1 d . U . . .
C33 C 0.41778(15) 0.25823(18) 0.59281(15) 0.1049(10) Uani 1 1 d . U . . .
C34 C 0.38480(11) 0.29095(14) 0.54599(12) 0.0839(6) Uani 1 1 d . . . . .
H34A H 0.344693 0.279426 0.536623 0.101 Uiso 1 1 calc R U . . .
B1 B 0.1437(12) 0.1422(10) 0.1417(10) 0.121(2) Uani 0.3333 1 d D U P A -1
F1 F 0.1171(10) 0.1546(10) 0.0865(7) 0.182(6) Uani 0.3333 1 d D U P A -1
F2 F 0.1799(14) 0.1908(10) 0.1548(7) 0.204(7) Uani 0.3333 1 d D U P A -1
F3 F 0.1008(10) 0.1364(12) 0.1862(11) 0.173(8) Uani 0.3333 1 d D U P A -1
F4 F 0.1787(13) 0.0906(11) 0.1376(10) 0.161(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9708(18) . ?
Fe1 N2 1.9708(18) 9 ?
Fe1 N2 1.9708(18) 5 ?
Fe1 N1 2.0154(19) 5 ?
Fe1 N1 2.0154(19) 9 ?
Fe1 N1 2.0154(19) . ?
Fe2 N5 2.013(2) 9 ?
Fe2 N5 2.013(2) 5 ?
Fe2 N5 2.013(2) . ?
Fe2 N6 2.055(2) 9 ?
Fe2 N6 2.055(2) 5 ?
Fe2 N6 2.055(2) . ?
N1 C1 1.341(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.333(3) . ?
N2 N3 1.350(2) . ?
N3 C8 1.369(3) . ?
N3 H3 0.90(2) . ?
N4 N5 1.349(3) . ?
N4 C21 1.360(3) . ?
N4 H4 0.86(2) . ?
N5 C23 1.338(3) . ?
N6 C28 1.350(4) . ?
N6 C24 1.350(4) . ?
C1 C2 1.382(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.373(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.377(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.391(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.453(3) . ?
C6 C7 1.389(3) . ?
C7 C8 1.379(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.466(3) . ?
C9 C14 1.373(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.390(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.373(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.386(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.396(3) . ?
C13 C15 1.475(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.390(4) . ?
C15 C20 1.397(3) . ?
C16 C17 1.371(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.387(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.402(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.374(4) . ?
C19 C21 1.474(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.382(4) . ?
C22 C23 1.379(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.466(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.380(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.361(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.383(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9954(15) 5 ?
Fe3 O2 1.9954(15) 9 ?
Fe3 O2 1.9954(15) . ?
Fe3 O1 2.0079(15) 9 ?
Fe3 O1 2.0079(15) 5 ?
Fe3 O1 2.0080(15) . ?
O1 C29 1.303(3) . ?
O2 C30 1.303(3) . ?
O3 C32 1.220(4) . ?
O4 C33 1.212(4) . ?
C29 C34 1.354(3) . ?
C29 C30 1.503(3) . ?
C30 C31 1.353(3) . ?
C31 C32 1.415(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.553(4) . ?
C33 C34 1.434(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.348(14) . ?
B1 F3 1.35(2) . ?
B1 F1 1.358(18) . ?
B1 F4 1.36(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.45(7) . 9 ?
N2 Fe1 N2 96.46(7) . 5 ?
N2 Fe1 N2 96.46(7) 9 5 ?
N2 Fe1 N1 90.74(7) . 5 ?
N2 Fe1 N1 172.32(7) 9 5 ?
N2 Fe1 N1 80.02(7) 5 5 ?
N2 Fe1 N1 172.32(7) . 9 ?
N2 Fe1 N1 80.02(7) 9 9 ?
N2 Fe1 N1 90.74(7) 5 9 ?
N1 Fe1 N1 93.15(8) 5 9 ?
N2 Fe1 N1 80.02(7) . . ?
N2 Fe1 N1 90.74(7) 9 . ?
N2 Fe1 N1 172.32(7) 5 . ?
N1 Fe1 N1 93.15(8) 5 . ?
N1 Fe1 N1 93.15(8) 9 . ?
N5 Fe2 N5 97.38(7) 9 5 ?
N5 Fe2 N5 97.38(7) 9 . ?
N5 Fe2 N5 97.38(7) 5 . ?
N5 Fe2 N6 78.52(8) 9 9 ?
N5 Fe2 N6 170.18(9) 5 9 ?
N5 Fe2 N6 92.03(9) . 9 ?
N5 Fe2 N6 92.03(9) 9 5 ?
N5 Fe2 N6 78.52(8) 5 5 ?
N5 Fe2 N6 170.18(8) . 5 ?
N6 Fe2 N6 92.62(9) 9 5 ?
N5 Fe2 N6 170.18(8) 9 . ?
N5 Fe2 N6 92.03(9) 5 . ?
N5 Fe2 N6 78.52(8) . . ?
N6 Fe2 N6 92.62(9) 9 . ?
N6 Fe2 N6 92.62(9) 5 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.20(18) . . ?
C5 N1 Fe1 114.69(15) . . ?
C6 N2 N3 106.22(17) . . ?
C6 N2 Fe1 116.07(15) . . ?
N3 N2 Fe1 136.29(14) . . ?
N2 N3 C8 110.62(18) . . ?
N2 N3 H3 115(2) . . ?
C8 N3 H3 134(2) . . ?
N5 N4 C21 111.01(19) . . ?
N5 N4 H4 120(3) . . ?
C21 N4 H4 129(3) . . ?
C23 N5 N4 105.6(2) . . ?
C23 N5 Fe2 115.74(17) . . ?
N4 N5 Fe2 135.29(16) . . ?
C28 N6 C24 117.4(3) . . ?
C28 N6 Fe2 127.3(2) . . ?
C24 N6 Fe2 115.26(17) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.5(3) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.9(3) . . ?
C3 C4 H4B 120.6 . . ?
C5 C4 H4B 120.6 . . ?
N1 C5 C4 122.1(2) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 124.2(2) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.0(2) . . ?
C7 C6 C5 134.1(2) . . ?
C8 C7 C6 105.6(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.7(2) . . ?
N3 C8 C9 123.1(2) . . ?
C7 C8 C9 130.2(2) . . ?
C14 C9 C10 119.4(3) . . ?
C14 C9 C8 121.9(2) . . ?
C10 C9 C8 118.7(3) . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10A 120.3 . . ?
C9 C10 H10A 120.3 . . ?
C12 C11 C10 120.3(3) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 118.1(3) . . ?
C12 C13 C15 122.0(3) . . ?
C14 C13 C15 119.7(3) . . ?
C9 C14 C13 121.6(2) . . ?
C9 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
C16 C15 C20 118.5(3) . . ?
C16 C15 C13 123.6(3) . . ?
C20 C15 C13 117.9(2) . . ?
C17 C16 C15 119.9(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 121.7(3) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C19 119.0(3) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.9(3) . . ?
C20 C19 C21 120.9(2) . . ?
C18 C19 C21 120.0(3) . . ?
C19 C20 C15 121.9(2) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 106.8(2) . . ?
N4 C21 C19 121.3(2) . . ?
C22 C21 C19 131.7(2) . . ?
C23 C22 C21 105.3(2) . . ?
C23 C22 H22A 127.3 . . ?
C21 C22 H22A 127.3 . . ?
N5 C23 C22 111.3(2) . . ?
N5 C23 C24 115.1(2) . . ?
C22 C23 C24 133.5(2) . . ?
N6 C24 C25 123.3(3) . . ?
N6 C24 C23 113.4(2) . . ?
C25 C24 C23 123.2(3) . . ?
C24 C25 C26 118.0(4) . . ?
C24 C25 H25A 121.0 . . ?
C26 C25 H25A 121.0 . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C26 C27 C28 119.4(3) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
N6 C28 C27 122.0(4) . . ?
N6 C28 H28A 119.0 . . ?
C27 C28 H28A 119.0 . . ?
O2 Fe3 O2 90.25(7) 5 9 ?
O2 Fe3 O2 90.25(7) 5 . ?
O2 Fe3 O2 90.25(7) 9 . ?
O2 Fe3 O1 95.19(7) 5 9 ?
O2 Fe3 O1 82.20(6) 9 9 ?
O2 Fe3 O1 170.69(6) . 9 ?
O2 Fe3 O1 82.20(6) 5 5 ?
O2 Fe3 O1 170.69(6) 9 5 ?
O2 Fe3 O1 95.19(7) . 5 ?
O1 Fe3 O1 93.03(6) 9 5 ?
O2 Fe3 O1 170.70(6) 5 . ?
O2 Fe3 O1 95.19(7) 9 . ?
O2 Fe3 O1 82.20(6) . . ?
O1 Fe3 O1 93.03(6) 9 . ?
O1 Fe3 O1 93.03(6) 5 . ?
C29 O1 Fe3 113.37(13) . . ?
C30 O2 Fe3 113.07(13) . . ?
O1 C29 C34 124.5(2) . . ?
O1 C29 C30 114.99(19) . . ?
C34 C29 C30 120.5(2) . . ?
O2 C30 C31 122.9(2) . . ?
O2 C30 C29 116.30(19) . . ?
C31 C30 C29 120.8(2) . . ?
C30 C31 C32 121.7(2) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O3 C32 C31 124.5(3) . . ?
O3 C32 C33 117.5(3) . . ?
C31 C32 C33 117.9(2) . . ?
O4 C33 C34 124.5(3) . . ?
O4 C33 C32 117.7(3) . . ?
C34 C33 C32 117.8(2) . . ?
C29 C34 C33 121.2(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F3 109.1(15) . . ?
F2 B1 F1 106.2(16) . . ?
F3 B1 F1 110.9(17) . . ?
F2 B1 F4 109.5(17) . . ?
F3 B1 F4 110.9(18) . . ?
F1 B1 F4 110.1(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(2) 2.05(3) 2.898(2) 156(3) . yes
N4 H4 O2 0.86(2) 2.14(3) 2.967(2) 160(3) 9 yes

_refine_diff_density_max         0.168
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.038

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_300Kd
_database_code_depnum_ccdc_archive 'CCDC 2260951'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.719(3)
_cell_length_b                   21.719(3)
_cell_length_c                   21.719(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10245(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6596
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      33.89

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            167560
_diffrn_reflns_av_unetI/netI     0.0192
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.924
_diffrn_reflns_theta_max         29.516
_diffrn_reflns_theta_full        29.516
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8844
_reflns_number_gt                8563
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with distance
 restraints as well as displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1829 cubic angstrom with a total of 51 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
 
 Details of SQUEEZE results (before BF4 disorder refinement):

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.113  0.149  0.141      1829        51 ' '
   2  0.144  0.356  0.644        10         1 ' '
   3  0.356  0.644  0.144        10         1 ' '
   4  0.644  0.144  0.356        10         1 ' '
   5  0.856  0.856  0.856        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_300Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1826 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1829 cubic angstrom with a total of 51 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0696P)²+0.3244P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0070(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3833 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.076(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8844
_refine_ls_number_parameters     458
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0335
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0986
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29778(2) 0.29778(2) 0.29778(2) 0.06134(12) Uani 1 3 d S T P . .
Fe2 Fe 0.57940(2) 0.57940(2) 0.57940(2) 0.06475(13) Uani 1 3 d S T P . .
N1 N 0.23295(9) 0.33183(9) 0.24119(8) 0.0686(4) Uani 1 1 d . . . . .
N2 N 0.26089(8) 0.36013(8) 0.35201(8) 0.0653(3) Uani 1 1 d . . . . .
N3 N 0.26526(8) 0.37560(9) 0.41211(8) 0.0664(4) Uani 1 1 d D . . . .
H3 H 0.3002(13) 0.3609(16) 0.4301(16) 0.100 Uiso 1 1 d D U . . .
N4 N 0.47113(9) 0.49330(10) 0.61562(8) 0.0701(4) Uani 1 1 d D . . . .
H4 H 0.4496(15) 0.5013(17) 0.5829(13) 0.105 Uiso 1 1 d D U . . .
N5 N 0.53058(9) 0.51101(9) 0.61703(9) 0.0695(4) Uani 1 1 d . . . . .
N6 N 0.64114(10) 0.54530(10) 0.64146(11) 0.0794(5) Uani 1 1 d . . . . .
C1 C 0.22219(14) 0.31538(12) 0.18267(11) 0.0802(6) Uani 1 1 d . . . . .
H1A H 0.247937 0.286537 0.164270 0.096 Uiso 1 1 calc R U . . .
C2 C 0.17410(17) 0.33978(15) 0.14865(13) 0.0980(9) Uani 1 1 d . . . . .
H2A H 0.167163 0.326562 0.108521 0.118 Uiso 1 1 calc R U . . .
C3 C 0.13678(17) 0.38362(17) 0.17466(16) 0.1030(9) Uani 1 1 d . . . . .
H3B H 0.104608 0.400811 0.152234 0.124 Uiso 1 1 calc R U . . .
C4 C 0.14769(15) 0.40193(14) 0.23476(14) 0.0926(8) Uani 1 1 d . . . . .
H4B H 0.123177 0.431733 0.253305 0.111 Uiso 1 1 calc R U . . .
C5 C 0.19598(11) 0.37488(11) 0.26677(11) 0.0720(5) Uani 1 1 d . . . . .
C6 C 0.21068(10) 0.38818(11) 0.33058(11) 0.0706(4) Uani 1 1 d . . . . .
C7 C 0.18245(11) 0.42254(12) 0.37659(12) 0.0782(5) Uani 1 1 d . . . . .
H7A H 0.146845 0.446082 0.373189 0.094 Uiso 1 1 calc R U . . .
C8 C 0.21831(9) 0.41439(11) 0.42831(11) 0.0717(5) Uani 1 1 d . . . . .
C9 C 0.21109(10) 0.43937(12) 0.49066(12) 0.0767(5) Uani 1 1 d . . . . .
C10 C 0.16347(15) 0.48106(19) 0.50246(17) 0.1035(10) Uani 1 1 d . . . . .
H10A H 0.137484 0.493381 0.470736 0.124 Uiso 1 1 calc R U . . .
C11 C 0.15499(18) 0.5039(3) 0.5610(2) 0.1314(16) Uani 1 1 d . . . . .
H11A H 0.123886 0.532371 0.568580 0.158 Uiso 1 1 calc R U . . .
C12 C 0.19244(16) 0.4848(2) 0.60841(17) 0.1206(14) Uani 1 1 d . . . . .
H12A H 0.185011 0.498822 0.648169 0.145 Uiso 1 1 calc R U . . .
C13 C 0.24101(12) 0.44491(16) 0.59777(12) 0.0881(7) Uani 1 1 d . . . . .
C14 C 0.24934(11) 0.42217(13) 0.53829(11) 0.0782(5) Uani 1 1 d . . . . .
H14A H 0.281381 0.394824 0.530609 0.094 Uiso 1 1 calc R U . . .
C15 C 0.28713(12) 0.43061(16) 0.64574(12) 0.0890(7) Uani 1 1 d . . . . .
C16 C 0.27212(18) 0.4068(2) 0.70313(15) 0.1231(14) Uani 1 1 d . . . . .
H16A H 0.231367 0.397422 0.712396 0.148 Uiso 1 1 calc R U . . .
C17 C 0.3171(2) 0.3970(3) 0.74604(16) 0.1325(16) Uani 1 1 d . . . . .
H17A H 0.306431 0.381377 0.784455 0.159 Uiso 1 1 calc R U . . .
C18 C 0.37854(17) 0.4099(2) 0.73346(14) 0.1125(12) Uani 1 1 d . . . . .
H18A H 0.408856 0.401614 0.762538 0.135 Uiso 1 1 calc R U . . .
C19 C 0.39415(12) 0.43561(14) 0.67628(11) 0.0814(6) Uani 1 1 d . . . . .
C20 C 0.34859(12) 0.44426(13) 0.63335(11) 0.0797(6) Uani 1 1 d . . . . .
H20A H 0.359051 0.459710 0.594812 0.096 Uiso 1 1 calc R U . . .
C21 C 0.45757(12) 0.45734(12) 0.66490(10) 0.0751(5) Uani 1 1 d . . . . .
C22 C 0.51061(13) 0.45259(13) 0.69968(11) 0.0808(6) Uani 1 1 d . . . . .
H22A H 0.515813 0.431136 0.736369 0.097 Uiso 1 1 calc R U . . .
C23 C 0.55417(12) 0.48650(11) 0.66832(11) 0.0736(5) Uani 1 1 d . . . . .
C24 C 0.61827(12) 0.50314(13) 0.68116(13) 0.0815(6) Uani 1 1 d . . . . .
C25 C 0.65162(17) 0.47925(17) 0.72925(19) 0.1082(10) Uani 1 1 d . . . . .
H25A H 0.634002 0.451393 0.756588 0.130 Uiso 1 1 calc R U . . .
C26 C 0.71208(19) 0.4978(2) 0.7359(2) 0.1299(15) Uani 1 1 d . . . . .
H26A H 0.735960 0.481979 0.767707 0.156 Uiso 1 1 calc R U . . .
C27 C 0.73664(17) 0.5390(2) 0.6958(2) 0.1282(15) Uani 1 1 d . . . . .
H27A H 0.777401 0.551503 0.699841 0.154 Uiso 1 1 calc R U . . .
C28 C 0.70029(14) 0.56225(17) 0.64903(18) 0.1015(9) Uani 1 1 d . . . . .
H28A H 0.717296 0.590591 0.621802 0.122 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43700(2) 0.43700(2) 0.43700(2) 0.06851(13) Uani 1 3 d S T P . .
O1 O 0.38485(7) 0.36816(7) 0.47027(7) 0.0670(3) Uani 1 1 d . . . . .
O2 O 0.49602(7) 0.40615(7) 0.50022(8) 0.0708(3) Uani 1 1 d . . . . .
O3 O 0.51311(14) 0.2488(2) 0.64582(16) 0.1712(19) Uani 1 1 d . . . . .
O4 O 0.39739(14) 0.21357(18) 0.62033(16) 0.1562(16) Uani 1 1 d . U . . .
C29 C 0.41089(9) 0.33819(11) 0.51520(10) 0.0672(4) Uani 1 1 d . . . . .
C30 C 0.47513(10) 0.35904(11) 0.53111(10) 0.0690(4) Uani 1 1 d . . . . .
C31 C 0.50864(12) 0.32917(16) 0.57414(13) 0.0916(8) Uani 1 1 d . . . . .
H31A H 0.548650 0.342178 0.582107 0.110 Uiso 1 1 calc R U . . .
C32 C 0.48455(15) 0.2786(2) 0.60741(14) 0.1069(11) Uani 1 1 d . U . . .
C33 C 0.41789(15) 0.25728(18) 0.59208(15) 0.1014(10) Uani 1 1 d . U . . .
C34 C 0.38462(11) 0.29069(14) 0.54586(12) 0.0809(6) Uani 1 1 d . . . . .
H34A H 0.344292 0.279527 0.536786 0.097 Uiso 1 1 calc R U . . .
B1 B 0.1433(9) 0.1420(10) 0.1420(11) 0.1141(19) Uani 0.3333 1 d D U P A -1
F1 F 0.1330(11) 0.1837(10) 0.0959(10) 0.149(6) Uani 0.3333 1 d D U P A -1
F2 F 0.1938(7) 0.1560(10) 0.1734(13) 0.198(6) Uani 0.3333 1 d D U P A -1
F3 F 0.0934(11) 0.1394(11) 0.1801(11) 0.162(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1538(8) 0.0852(7) 0.1159(9) 0.179(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9655(18) . ?
Fe1 N2 1.9656(18) 9 ?
Fe1 N2 1.9656(18) 5 ?
Fe1 N1 2.0099(19) . ?
Fe1 N1 2.0099(19) 9 ?
Fe1 N1 2.0099(19) 5 ?
Fe2 N5 2.000(2) . ?
Fe2 N5 2.000(2) 9 ?
Fe2 N5 2.000(2) 5 ?
Fe2 N6 2.040(2) 9 ?
Fe2 N6 2.040(2) 5 ?
Fe2 N6 2.040(2) . ?
N1 C1 1.341(3) . ?
N1 C5 1.352(3) . ?
N2 C6 1.333(3) . ?
N2 N3 1.351(2) . ?
N3 C8 1.369(3) . ?
N3 H3 0.91(2) . ?
N4 N5 1.348(3) . ?
N4 C21 1.357(3) . ?
N4 H4 0.87(2) . ?
N5 C23 1.337(3) . ?
N6 C28 1.346(4) . ?
N6 C24 1.352(4) . ?
C1 C2 1.385(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.385(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.389(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.451(3) . ?
C6 C7 1.390(3) . ?
C7 C8 1.378(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.467(3) . ?
C9 C14 1.378(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.378(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.376(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.384(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.395(3) . ?
C13 C15 1.478(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.389(4) . ?
C15 C20 1.394(3) . ?
C16 C17 1.367(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.390(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.403(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.372(4) . ?
C19 C21 1.477(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(4) . ?
C22 C23 1.379(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.465(4) . ?
C24 C25 1.373(4) . ?
C25 C26 1.381(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.358(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.382(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9943(16) 5 ?
Fe3 O2 1.9943(16) 9 ?
Fe3 O2 1.9943(16) . ?
Fe3 O1 2.0101(15) . ?
Fe3 O1 2.0102(15) 5 ?
Fe3 O1 2.0102(15) 9 ?
O1 C29 1.302(3) . ?
O2 C30 1.305(3) . ?
O3 C32 1.225(4) . ?
O4 C33 1.215(4) . ?
C29 C34 1.354(3) . ?
C29 C30 1.507(3) . ?
C30 C31 1.350(3) . ?
C31 C32 1.415(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.556(4) . ?
C33 C34 1.434(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.328(13) . ?
B1 F3 1.36(2) . ?
B1 F1 1.369(19) . ?
B1 F4 1.376(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.45(7) . 9 ?
N2 Fe1 N2 96.45(7) . 5 ?
N2 Fe1 N2 96.45(7) 9 5 ?
N2 Fe1 N1 80.06(7) . . ?
N2 Fe1 N1 90.73(7) 9 . ?
N2 Fe1 N1 172.35(7) 5 . ?
N2 Fe1 N1 172.35(7) . 9 ?
N2 Fe1 N1 80.06(7) 9 9 ?
N2 Fe1 N1 90.73(7) 5 9 ?
N1 Fe1 N1 93.12(8) . 9 ?
N2 Fe1 N1 90.74(7) . 5 ?
N2 Fe1 N1 172.35(7) 9 5 ?
N2 Fe1 N1 80.06(7) 5 5 ?
N1 Fe1 N1 93.12(8) . 5 ?
N1 Fe1 N1 93.12(8) 9 5 ?
N5 Fe2 N5 97.27(7) . 9 ?
N5 Fe2 N5 97.27(7) . 5 ?
N5 Fe2 N5 97.27(7) 9 5 ?
N5 Fe2 N6 91.70(8) . 9 ?
N5 Fe2 N6 78.98(8) 9 9 ?
N5 Fe2 N6 170.68(8) 5 9 ?
N5 Fe2 N6 170.68(8) . 5 ?
N5 Fe2 N6 91.70(8) 9 5 ?
N5 Fe2 N6 78.98(8) 5 5 ?
N6 Fe2 N6 92.53(9) 9 5 ?
N5 Fe2 N6 78.98(8) . . ?
N5 Fe2 N6 170.68(8) 9 . ?
N5 Fe2 N6 91.70(8) 5 . ?
N6 Fe2 N6 92.53(9) 9 . ?
N6 Fe2 N6 92.53(9) 5 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.14(17) . . ?
C5 N1 Fe1 114.79(15) . . ?
C6 N2 N3 106.33(17) . . ?
C6 N2 Fe1 116.04(15) . . ?
N3 N2 Fe1 136.19(14) . . ?
N2 N3 C8 110.43(18) . . ?
N2 N3 H3 113(2) . . ?
C8 N3 H3 137(2) . . ?
N5 N4 C21 110.7(2) . . ?
N5 N4 H4 119(2) . . ?
C21 N4 H4 130(3) . . ?
C23 N5 N4 105.82(19) . . ?
C23 N5 Fe2 115.67(16) . . ?
N4 N5 Fe2 135.30(15) . . ?
C28 N6 C24 117.2(2) . . ?
C28 N6 Fe2 127.5(2) . . ?
C24 N6 Fe2 115.19(17) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.4(3) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3B 120.5 . . ?
C4 C3 H3B 120.5 . . ?
C3 C4 C5 118.7(3) . . ?
C3 C4 H4B 120.7 . . ?
C5 C4 H4B 120.7 . . ?
N1 C5 C4 122.4(2) . . ?
N1 C5 C6 113.5(2) . . ?
C4 C5 C6 124.1(2) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.0(2) . . ?
C7 C6 C5 134.2(2) . . ?
C8 C7 C6 105.5(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.9(2) . . ?
N3 C8 C9 123.0(2) . . ?
C7 C8 C9 130.1(2) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 C8 121.9(2) . . ?
C10 C9 C8 119.2(3) . . ?
C11 C10 C9 120.1(3) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 118.4(3) . . ?
C12 C13 C15 122.0(3) . . ?
C14 C13 C15 119.4(3) . . ?
C9 C14 C13 121.4(2) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.5(3) . . ?
C16 C15 C13 123.5(3) . . ?
C20 C15 C13 117.9(2) . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C16 C17 C18 121.4(3) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C17 C18 C19 119.1(3) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 121.0(2) . . ?
C18 C19 C21 120.0(3) . . ?
C19 C20 C15 122.0(2) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 107.1(2) . . ?
N4 C21 C19 121.2(2) . . ?
C22 C21 C19 131.5(2) . . ?
C23 C22 C21 105.2(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.2(2) . . ?
N5 C23 C24 115.1(2) . . ?
C22 C23 C24 133.6(2) . . ?
N6 C24 C25 123.2(3) . . ?
N6 C24 C23 113.2(2) . . ?
C25 C24 C23 123.6(3) . . ?
C24 C25 C26 118.1(3) . . ?
C24 C25 H25A 121.0 . . ?
C26 C25 H25A 121.0 . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.3(3) . . ?
N6 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
O2 Fe3 O2 90.27(7) 5 9 ?
O2 Fe3 O2 90.27(7) 5 . ?
O2 Fe3 O2 90.27(7) 9 . ?
O2 Fe3 O1 170.67(6) 5 . ?
O2 Fe3 O1 95.27(7) 9 . ?
O2 Fe3 O1 82.23(6) . . ?
O2 Fe3 O1 82.23(6) 5 5 ?
O2 Fe3 O1 170.68(6) 9 5 ?
O2 Fe3 O1 95.27(7) . 5 ?
O1 Fe3 O1 92.91(6) . 5 ?
O2 Fe3 O1 95.27(7) 5 9 ?
O2 Fe3 O1 82.23(6) 9 9 ?
O2 Fe3 O1 170.68(6) . 9 ?
O1 Fe3 O1 92.91(6) . 9 ?
O1 Fe3 O1 92.91(6) 5 9 ?
C29 O1 Fe3 113.36(13) . . ?
C30 O2 Fe3 113.20(13) . . ?
O1 C29 C34 124.5(2) . . ?
O1 C29 C30 115.07(19) . . ?
C34 C29 C30 120.4(2) . . ?
O2 C30 C31 123.0(2) . . ?
O2 C30 C29 116.07(19) . . ?
C31 C30 C29 120.9(2) . . ?
C30 C31 C32 121.8(2) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O3 C32 C31 124.8(3) . . ?
O3 C32 C33 117.3(3) . . ?
C31 C32 C33 117.8(2) . . ?
O4 C33 C34 124.4(3) . . ?
O4 C33 C32 117.8(3) . . ?
C34 C33 C32 117.9(2) . . ?
C29 C34 C33 121.2(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F3 110.8(16) . . ?
F2 B1 F1 111.1(17) . . ?
F3 B1 F1 109.9(17) . . ?
F2 B1 F4 106.3(15) . . ?
F3 B1 F4 110.2(16) . . ?
F1 B1 F4 108.5(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.91(2) 2.04(3) 2.893(2) 155(3) . yes
N4 H4 O2 0.87(2) 2.11(2) 2.960(2) 166(3) 9 yes

_refine_diff_density_max         0.235
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.039

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh1_200Kd
_database_code_depnum_ccdc_archive 'CCDC 2260952'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.626(3)
_cell_length_b                   21.626(3)
_cell_length_c                   21.626(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10114(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    200(2)
_cell_measurement_reflns_used    6518
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.89

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.307
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.532
_shelx_estimated_absorpt_T_min   0.878
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      200(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            165987
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0560
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.933
_diffrn_reflns_theta_max         29.523
_diffrn_reflns_theta_full        29.523
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8753
_reflns_number_gt                8649
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1771 cubic angstrom with a total of 72 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
 
 Details of SQUEEZE results (before refinement of B4r disorder):

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.084  0.137  0.139      1771        72 ' '
   2  0.106  0.394  0.606        10         0 ' '
   3  0.394  0.606  0.106        10         0 ' '
   4  0.606  0.106  0.394        10         0 ' '
   5  0.894  0.894  0.894        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh1_200Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1767 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1771 cubic angstrom with a total of 72 electrons.
 Clearly, these figures could only agree with a very small amount of 
 very diffuse lattice methanol. Nevertheless the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0575P)²+0.7198P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0049(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3927 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.066(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8753
_refine_ls_number_parameters     458
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0310
_refine_ls_wR_factor_ref         0.0897
_refine_ls_wR_factor_gt          0.0895
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45208(2) 0.45208(2) 0.45208(2) 0.04454(11) Uani 1 3 d S T P . .
Fe2 Fe 0.16940(2) 0.16940(2) 0.16940(2) 0.04751(12) Uani 1 3 d S T P . .
N1 N 0.50906(8) 0.41826(8) 0.51685(8) 0.0493(3) Uani 1 1 d . . . . .
N2 N 0.39756(8) 0.38964(8) 0.48889(8) 0.0474(3) Uani 1 1 d . . . . .
N3 N 0.33742(8) 0.37401(8) 0.48435(8) 0.0480(3) Uani 1 1 d D . . . .
H3 H 0.3204(14) 0.3862(15) 0.4485(12) 0.072 Uiso 1 1 d D U . . .
N4 N 0.13392(8) 0.25475(9) 0.27754(8) 0.0498(3) Uani 1 1 d D . . . .
H4 H 0.1678(12) 0.2494(15) 0.2971(14) 0.075 Uiso 1 1 d D U . . .
N5 N 0.13255(8) 0.23690(8) 0.21787(8) 0.0494(3) Uani 1 1 d . . . . .
N6 N 0.10964(9) 0.20310(9) 0.10717(9) 0.0553(4) Uani 1 1 d . . . . .
C1 C 0.56748(10) 0.43497(11) 0.52785(11) 0.0571(5) Uani 1 1 d . . . . .
H1A H 0.586398 0.464297 0.501165 0.069 Uiso 1 1 calc R U . . .
C2 C 0.60169(11) 0.41122(13) 0.57673(14) 0.0679(6) Uani 1 1 d . . . . .
H2A H 0.642674 0.425224 0.584084 0.081 Uiso 1 1 calc R U . . .
C3 C 0.57531(13) 0.36690(14) 0.61457(14) 0.0717(6) Uani 1 1 d . . . . .
H3A H 0.598131 0.349576 0.647871 0.086 Uiso 1 1 calc R U . . .
C4 C 0.51506(12) 0.34813(12) 0.60318(13) 0.0654(6) Uani 1 1 d . . . . .
H4A H 0.496004 0.317463 0.628204 0.079 Uiso 1 1 calc R U . . .
C5 C 0.48320(10) 0.37508(9) 0.55445(10) 0.0515(4) Uani 1 1 d . . . . .
C6 C 0.41922(10) 0.36170(10) 0.53953(9) 0.0512(4) Uani 1 1 d . . . . .
C7 C 0.37276(11) 0.32714(11) 0.56800(10) 0.0560(4) Uani 1 1 d . . . . .
H7A H 0.376115 0.303089 0.604603 0.067 Uiso 1 1 calc R U . . .
C8 C 0.32103(10) 0.33528(10) 0.53182(9) 0.0519(4) Uani 1 1 d . . . . .
C9 C 0.21049(10) 0.32774(11) 0.50014(10) 0.0563(4) Uani 1 1 d . . . . .
H9A H 0.218344 0.355833 0.467286 0.068 Uiso 1 1 calc R U . . .
C10 C 0.25854(11) 0.31030(11) 0.53906(9) 0.0553(4) Uani 1 1 d . . . . .
C11 C 0.24659(14) 0.26831(14) 0.58693(13) 0.0716(6) Uani 1 1 d . . . . .
H11A H 0.279111 0.255082 0.613326 0.086 Uiso 1 1 calc R U . . .
C12 C 0.18687(16) 0.24611(18) 0.59560(15) 0.0889(9) Uani 1 1 d . . . . .
H12A H 0.178700 0.217978 0.628334 0.107 Uiso 1 1 calc R U . . .
C13 C 0.13966(14) 0.26438(18) 0.55744(14) 0.0828(9) Uani 1 1 d . . . . .
H13A H 0.098950 0.249426 0.564426 0.099 Uiso 1 1 calc R U . . .
C14 C 0.15090(11) 0.30459(13) 0.50861(11) 0.0631(5) Uani 1 1 d . . . . .
C15 C 0.11609(10) 0.30551(11) 0.40016(10) 0.0573(5) Uani 1 1 d . . . . .
H15A H 0.155971 0.290401 0.389632 0.069 Uiso 1 1 calc R U . . .
C16 C 0.10274(11) 0.31870(13) 0.46210(11) 0.0640(6) Uani 1 1 d . . . . .
C17 C 0.04479(13) 0.34185(19) 0.47689(15) 0.0873(9) Uani 1 1 d . . . . .
H17A H 0.034663 0.350442 0.518767 0.105 Uiso 1 1 calc R U . . .
C18 C 0.00186(14) 0.3524(2) 0.43101(16) 0.0943(11) Uani 1 1 d . . . . .
H18A H -0.037228 0.369530 0.441436 0.113 Uiso 1 1 calc R U . . .
C19 C 0.01497(12) 0.33839(17) 0.36972(14) 0.0788(8) Uani 1 1 d . . . . .
H19A H -0.015161 0.345366 0.338523 0.095 Uiso 1 1 calc R U . . .
C20 C 0.07303(10) 0.31383(12) 0.35413(11) 0.0590(5) Uani 1 1 d . . . . .
C21 C 0.08483(9) 0.29210(10) 0.29073(10) 0.0534(4) Uani 1 1 d . . . . .
C22 C 0.05038(10) 0.29740(11) 0.23732(11) 0.0573(5) Uani 1 1 d . . . . .
H22A H 0.013217 0.320126 0.231684 0.069 Uiso 1 1 calc R U . . .
C23 C 0.08172(10) 0.26235(10) 0.19353(10) 0.0530(4) Uani 1 1 d . . . . .
C24 C 0.06934(11) 0.24592(11) 0.12941(11) 0.0575(5) Uani 1 1 d . . . . .
C25 C 0.02175(14) 0.27021(14) 0.09484(13) 0.0731(7) Uani 1 1 d . . . . .
H25A H -0.005998 0.299362 0.112448 0.088 Uiso 1 1 calc R U . . .
C26 C 0.01497(18) 0.25151(17) 0.03405(15) 0.0892(10) Uani 1 1 d . . . . .
H26A H -0.017689 0.267277 0.009263 0.107 Uiso 1 1 calc R U . . .
C27 C 0.05659(17) 0.20950(17) 0.01014(14) 0.0867(9) Uani 1 1 d . . . . .
H27A H 0.053595 0.196870 -0.031826 0.104 Uiso 1 1 calc R U . . .
C28 C 0.10268(13) 0.18588(13) 0.04762(12) 0.0683(6) Uani 1 1 d . . . . .
H28A H 0.130536 0.156384 0.030777 0.082 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31179(2) 0.31179(2) 0.31179(2) 0.05287(13) Uani 1 3 d S T P . .
O1 O 0.27878(7) 0.38062(7) 0.36453(6) 0.0499(3) Uani 1 1 d . . . . .
O2 O 0.24794(7) 0.34293(7) 0.25309(7) 0.0534(3) Uani 1 1 d . . . . .
O3 O 0.10771(12) 0.50684(15) 0.23339(11) 0.1094(10) Uani 1 1 d . U . . .
O4 O 0.13323(13) 0.54162(14) 0.35071(11) 0.1063(10) Uani 1 1 d . U . . .
C29 C 0.23445(9) 0.41196(10) 0.33824(9) 0.0502(4) Uani 1 1 d . . . . .
C30 C 0.21822(9) 0.39147(10) 0.27346(9) 0.0522(4) Uani 1 1 d . . . . .
C31 C 0.17620(12) 0.42280(14) 0.23918(11) 0.0663(6) Uani 1 1 d . . . . .
H31A H 0.167433 0.409166 0.198354 0.080 Uiso 1 1 calc R U . . .
C32 C 0.14487(12) 0.47560(16) 0.26277(12) 0.0752(7) Uani 1 1 d . U . . .
C33 C 0.15992(12) 0.49602(15) 0.33046(13) 0.0719(7) Uani 1 1 d . U . . .
C34 C 0.20478(10) 0.46057(12) 0.36440(10) 0.0592(5) Uani 1 1 d . . . . .
H34A H 0.213798 0.471439 0.405993 0.071 Uiso 1 1 calc R U . . .
B1 B -0.1066(10) 0.3922(8) 0.1073(9) 0.0751(15) Uani 0.3333 1 d D U P A -1
F1 F -0.0713(15) 0.3846(9) 0.1598(10) 0.101(5) Uani 0.3333 1 d D U P A -1
F2 F -0.0681(13) 0.4121(6) 0.0604(10) 0.152(6) Uani 0.3333 1 d D U P A -1
F3 F -0.1505(8) 0.4368(10) 0.1129(13) 0.121(7) Uani 0.3333 1 d D U P A -1
F4 F -0.1303(10) 0.3371(7) 0.0883(11) 0.117(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9612(17) 9 ?
Fe1 N2 1.9612(17) 5 ?
Fe1 N2 1.9612(17) . ?
Fe1 N1 2.0040(17) . ?
Fe1 N1 2.0041(17) 5 ?
Fe1 N1 2.0041(17) 9 ?
Fe2 N5 1.9658(18) . ?
Fe2 N5 1.9658(18) 9 ?
Fe2 N5 1.9658(18) 5 ?
Fe2 N6 2.0033(18) 9 ?
Fe2 N6 2.0033(18) 5 ?
Fe2 N6 2.0033(18) . ?
N1 C1 1.335(3) . ?
N1 C5 1.359(3) . ?
N2 C6 1.336(3) . ?
N2 N3 1.347(2) . ?
N3 C8 1.371(3) . ?
N3 H3 0.90(2) . ?
N4 N5 1.347(2) . ?
N4 C21 1.364(3) . ?
N4 H4 0.85(2) . ?
N5 C23 1.337(3) . ?
N6 C28 1.349(3) . ?
N6 C24 1.360(3) . ?
C1 C2 1.389(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.383(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.387(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.387(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.450(3) . ?
C6 C7 1.396(3) . ?
C7 C8 1.376(3) . ?
C7 H7A 0.9500 . ?
C8 C10 1.464(3) . ?
C9 C10 1.389(3) . ?
C9 C14 1.395(3) . ?
C9 H9A 0.9500 . ?
C10 C11 1.401(3) . ?
C11 C12 1.390(4) . ?
C11 H11A 0.9500 . ?
C12 C13 1.371(5) . ?
C12 H12A 0.9500 . ?
C13 C14 1.389(4) . ?
C13 H13A 0.9500 . ?
C14 C16 1.480(4) . ?
C15 C20 1.375(3) . ?
C15 C16 1.400(3) . ?
C15 H15A 0.9500 . ?
C16 C17 1.387(3) . ?
C17 C18 1.378(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.389(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.404(3) . ?
C19 H19A 0.9500 . ?
C20 C21 1.472(3) . ?
C21 C22 1.379(3) . ?
C22 C23 1.390(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.456(3) . ?
C24 C25 1.376(3) . ?
C25 C26 1.383(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.379(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.382(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.9928(15) 9 ?
Fe3 O2 1.9929(15) . ?
Fe3 O2 1.9929(15) 5 ?
Fe3 O1 2.0065(15) . ?
Fe3 O1 2.0066(15) 5 ?
Fe3 O1 2.0066(15) 9 ?
O1 C29 1.305(2) . ?
O2 C30 1.307(3) . ?
O3 C32 1.227(3) . ?
O4 C33 1.224(3) . ?
C29 C34 1.355(3) . ?
C29 C30 1.511(3) . ?
C30 C31 1.354(3) . ?
C31 C32 1.422(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.563(4) . ?
C33 C34 1.438(3) . ?
C34 H34A 0.9500 . ?
B1 F3 1.358(19) . ?
B1 F4 1.362(17) . ?
B1 F1 1.378(18) . ?
B1 F2 1.381(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.29(7) 9 5 ?
N2 Fe1 N2 96.29(7) 9 . ?
N2 Fe1 N2 96.29(7) 5 . ?
N2 Fe1 N1 172.60(7) 9 . ?
N2 Fe1 N1 90.70(7) 5 . ?
N2 Fe1 N1 80.49(7) . . ?
N2 Fe1 N1 90.70(7) 9 5 ?
N2 Fe1 N1 80.49(7) 5 5 ?
N2 Fe1 N1 172.60(7) . 5 ?
N1 Fe1 N1 92.85(7) . 5 ?
N2 Fe1 N1 80.49(7) 9 9 ?
N2 Fe1 N1 172.60(7) 5 9 ?
N2 Fe1 N1 90.70(7) . 9 ?
N1 Fe1 N1 92.85(7) . 9 ?
N1 Fe1 N1 92.85(7) 5 9 ?
N5 Fe2 N5 96.97(7) . 9 ?
N5 Fe2 N5 96.97(7) . 5 ?
N5 Fe2 N5 96.97(7) 9 5 ?
N5 Fe2 N6 172.04(7) . 9 ?
N5 Fe2 N6 80.01(7) 9 9 ?
N5 Fe2 N6 90.73(7) 5 9 ?
N5 Fe2 N6 90.73(7) . 5 ?
N5 Fe2 N6 172.04(7) 9 5 ?
N5 Fe2 N6 80.01(7) 5 5 ?
N6 Fe2 N6 92.62(8) 9 5 ?
N5 Fe2 N6 80.01(7) . . ?
N5 Fe2 N6 90.73(7) 9 . ?
N5 Fe2 N6 172.04(7) 5 . ?
N6 Fe2 N6 92.62(8) 9 . ?
N6 Fe2 N6 92.62(8) 5 . ?
C1 N1 C5 117.96(19) . . ?
C1 N1 Fe1 127.41(15) . . ?
C5 N1 Fe1 114.58(14) . . ?
C6 N2 N3 106.55(16) . . ?
C6 N2 Fe1 115.68(14) . . ?
N3 N2 Fe1 136.34(13) . . ?
N2 N3 C8 110.38(17) . . ?
N2 N3 H3 113(2) . . ?
C8 N3 H3 136(2) . . ?
N5 N4 C21 110.66(18) . . ?
N5 N4 H4 117(2) . . ?
C21 N4 H4 130(2) . . ?
C23 N5 N4 106.10(17) . . ?
C23 N5 Fe2 115.41(15) . . ?
N4 N5 Fe2 135.60(14) . . ?
C28 N6 C24 117.0(2) . . ?
C28 N6 Fe2 127.80(17) . . ?
C24 N6 Fe2 115.06(15) . . ?
N1 C1 C2 122.6(2) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.0(2) . . ?
C2 C3 H3A 120.5 . . ?
C4 C3 H3A 120.5 . . ?
C3 C4 C5 118.6(2) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 122.6(2) . . ?
N1 C5 C6 113.38(18) . . ?
C4 C5 C6 124.0(2) . . ?
N2 C6 C7 110.58(19) . . ?
N2 C6 C5 115.27(18) . . ?
C7 C6 C5 134.10(19) . . ?
C8 C7 C6 105.43(18) . . ?
C8 C7 H7A 127.3 . . ?
C6 C7 H7A 127.3 . . ?
N3 C8 C7 107.07(18) . . ?
N3 C8 C10 122.96(19) . . ?
C7 C8 C10 129.97(19) . . ?
C10 C9 C14 120.9(2) . . ?
C10 C9 H9A 119.5 . . ?
C14 C9 H9A 119.5 . . ?
C9 C10 C11 119.1(2) . . ?
C9 C10 C8 121.70(19) . . ?
C11 C10 C8 119.2(2) . . ?
C12 C11 C10 119.7(3) . . ?
C12 C11 H11A 120.2 . . ?
C10 C11 H11A 120.2 . . ?
C13 C12 C11 120.7(3) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
C12 C13 C14 120.5(2) . . ?
C12 C13 H13A 119.8 . . ?
C14 C13 H13A 119.8 . . ?
C13 C14 C9 119.1(2) . . ?
C13 C14 C16 121.5(2) . . ?
C9 C14 C16 119.1(2) . . ?
C20 C15 C16 121.8(2) . . ?
C20 C15 H15A 119.1 . . ?
C16 C15 H15A 119.1 . . ?
C17 C16 C15 118.7(3) . . ?
C17 C16 C14 123.6(2) . . ?
C15 C16 C14 117.6(2) . . ?
C18 C17 C16 120.2(3) . . ?
C18 C17 H17A 119.9 . . ?
C16 C17 H17A 119.9 . . ?
C17 C18 C19 120.9(3) . . ?
C17 C18 H18A 119.6 . . ?
C19 C18 H18A 119.6 . . ?
C18 C19 C20 119.6(3) . . ?
C18 C19 H19A 120.2 . . ?
C20 C19 H19A 120.2 . . ?
C15 C20 C19 118.8(2) . . ?
C15 C20 C21 121.01(19) . . ?
C19 C20 C21 120.0(2) . . ?
N4 C21 C22 107.12(19) . . ?
N4 C21 C20 121.3(2) . . ?
C22 C21 C20 131.3(2) . . ?
C21 C22 C23 105.20(19) . . ?
C21 C22 H22A 127.4 . . ?
C23 C22 H22A 127.4 . . ?
N5 C23 C22 110.92(19) . . ?
N5 C23 C24 115.19(19) . . ?
C22 C23 C24 133.8(2) . . ?
N6 C24 C25 123.2(2) . . ?
N6 C24 C23 112.66(19) . . ?
C25 C24 C23 124.2(2) . . ?
C24 C25 C26 118.9(3) . . ?
C24 C25 H25A 120.5 . . ?
C26 C25 H25A 120.5 . . ?
C27 C26 C25 118.7(3) . . ?
C27 C26 H26A 120.7 . . ?
C25 C26 H26A 120.7 . . ?
C26 C27 C28 119.6(3) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
N6 C28 C27 122.6(3) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 90.46(6) 9 . ?
O2 Fe3 O2 90.46(6) 9 5 ?
O2 Fe3 O2 90.46(6) . 5 ?
O2 Fe3 O1 170.61(6) 9 . ?
O2 Fe3 O1 82.24(6) . . ?
O2 Fe3 O1 95.47(6) 5 . ?
O2 Fe3 O1 95.47(6) 9 5 ?
O2 Fe3 O1 170.61(6) . 5 ?
O2 Fe3 O1 82.24(6) 5 5 ?
O1 Fe3 O1 92.55(6) . 5 ?
O2 Fe3 O1 82.24(6) 9 9 ?
O2 Fe3 O1 95.47(6) . 9 ?
O2 Fe3 O1 170.61(6) 5 9 ?
O1 Fe3 O1 92.55(6) . 9 ?
O1 Fe3 O1 92.55(6) 5 9 ?
C29 O1 Fe3 113.52(13) . . ?
C30 O2 Fe3 113.42(13) . . ?
O1 C29 C34 124.67(19) . . ?
O1 C29 C30 115.00(18) . . ?
C34 C29 C30 120.30(19) . . ?
O2 C30 C31 123.2(2) . . ?
O2 C30 C29 115.70(18) . . ?
C31 C30 C29 121.1(2) . . ?
C30 C31 C32 121.7(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.6(3) . . ?
O3 C32 C33 117.7(3) . . ?
C31 C32 C33 117.6(2) . . ?
O4 C33 C34 124.4(2) . . ?
O4 C33 C32 117.7(2) . . ?
C34 C33 C32 117.9(2) . . ?
C29 C34 C33 121.3(2) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F3 B1 F4 112.6(16) . . ?
F3 B1 F1 113.6(17) . . ?
F4 B1 F1 110.6(13) . . ?
F3 B1 F2 105.4(12) . . ?
F4 B1 F2 106.1(14) . . ?
F1 B1 F2 108.0(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(2) 2.03(2) 2.888(2) 159(3) . yes
N4 H4 O2 0.85(2) 2.09(2) 2.943(2) 173(3) 5 yes

_refine_diff_density_max         0.262
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.042

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_280K
_database_code_depnum_ccdc_archive 'CCDC 2261720'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.957(3)
_cell_length_b                   21.957(3)
_cell_length_c                   21.957(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10586(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    280(2)
_cell_measurement_reflns_used    6817
_cell_measurement_theta_min      1.35
_cell_measurement_theta_max      3389

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.514
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      280(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            173621
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_av_R_equivalents  0.0743
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.346
_diffrn_reflns_theta_max         29.479
_diffrn_reflns_theta_full        29.479
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9109
_reflns_number_gt                8918
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1259 cubic angstrom with a total of 136 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 80 electron per cell at 300 K,
 after measurements done up to 400 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
 
 Details of SQUEEZE results before refinement of BF4 disorder:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.089  0.154  0.143      1259       136 ' '
   2  0.116  0.384  0.616         8         1 ' '
   3  0.384  0.616  0.116         8         1 ' '
   4  0.616  0.116  0.384         8         1 ' '
   5  0.884  0.884  0.884         9         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?



 Details of SQUEEZE results on a 300 K data set of the same crystal
 after measurements up to 400 K:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.118  0.151  0.141      1841        80 ' '
   2  0.144  0.356  0.644        10         0 ' '
   3  0.356  0.644  0.144        10         0 ' '
   4  0.644  0.144  0.356        10         0 ' '
   5  0.856  0.856  0.856        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh2_280K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1259 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1259 cubic angstrom with a total of 136 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 80 electron per cell at 300 K,
 after measurements done up to 400 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1265P)²+0.0326P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.058(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 4053 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.076(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9109
_refine_ls_number_parameters     466
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0498
_refine_ls_wR_factor_ref         0.1435
_refine_ls_wR_factor_gt          0.1428
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45443(2) 0.45443(2) 0.45443(2) 0.06107(16) Uani 1 3 d S T P . .
Fe2 Fe 0.17541(2) 0.17541(2) 0.17541(2) 0.07466(19) Uani 1 3 d S T P . .
N1 N 0.51473(10) 0.42023(10) 0.51384(10) 0.0686(4) Uani 1 1 d . . . . .
N2 N 0.40495(9) 0.38962(9) 0.49013(9) 0.0654(4) Uani 1 1 d . . . . .
N3 N 0.34607(9) 0.37287(10) 0.48844(9) 0.0664(4) Uani 1 1 d D . . . .
H3 H 0.3182(17) 0.384(2) 0.4637(18) 0.100 Uiso 1 1 d D U . . .
N4 N 0.14202(9) 0.25312(11) 0.28678(10) 0.0716(4) Uani 1 1 d D . . . .
H4 H 0.1779(16) 0.249(2) 0.307(2) 0.107 Uiso 1 1 d D U . . .
N5 N 0.13930(9) 0.23829(11) 0.22744(10) 0.0728(5) Uani 1 1 d . . . . .
N6 N 0.11320(15) 0.20888(18) 0.11758(14) 0.0977(8) Uani 1 1 d . . . . .
C1 C 0.57326(12) 0.43713(14) 0.52111(14) 0.0798(6) Uani 1 1 d . . . . .
H1A H 0.588978 0.467800 0.496478 0.096 Uiso 1 1 calc R U . . .
C2 C 0.61082(15) 0.41021(18) 0.5642(2) 0.1016(10) Uani 1 1 d . . . . .
H2A H 0.651288 0.422236 0.567649 0.122 Uiso 1 1 calc R U . . .
C3 C 0.58802(17) 0.3659(2) 0.6016(2) 0.1015(10) Uani 1 1 d . . . . .
H3A H 0.612469 0.348435 0.631410 0.122 Uiso 1 1 calc R U . . .
C4 C 0.52814(17) 0.34731(17) 0.59449(19) 0.0965(9) Uani 1 1 d . . . . .
H4A H 0.511961 0.316746 0.618943 0.116 Uiso 1 1 calc R U . . .
C5 C 0.49270(12) 0.37535(12) 0.55000(12) 0.0735(5) Uani 1 1 d . . . . .
C6 C 0.42918(12) 0.36068(12) 0.53845(12) 0.0727(5) Uani 1 1 d . . . . .
C7 C 0.38605(14) 0.32497(15) 0.56744(13) 0.0826(7) Uani 1 1 d . . . . .
H7A H 0.391487 0.300779 0.601786 0.099 Uiso 1 1 calc R U . . .
C8 C 0.33334(12) 0.33303(13) 0.53440(11) 0.0738(5) Uani 1 1 d . . . . .
C9 C 0.22424(13) 0.32105(15) 0.50557(11) 0.0796(6) Uani 1 1 d . . . . .
H9A H 0.230606 0.345937 0.471892 0.096 Uiso 1 1 calc R U . . .
C10 C 0.27251(13) 0.30731(14) 0.54411(11) 0.0781(6) Uani 1 1 d . . . . .
C11 C 0.2626(2) 0.2686(2) 0.59406(17) 0.1069(11) Uani 1 1 d . . . . .
H11A H 0.294946 0.258095 0.619317 0.128 Uiso 1 1 calc R U . . .
C12 C 0.2056(3) 0.2463(3) 0.6058(2) 0.134(2) Uani 1 1 d . . . . .
H12A H 0.199308 0.220507 0.638761 0.160 Uiso 1 1 calc R U . . .
C13 C 0.1565(2) 0.2624(3) 0.5678(2) 0.1212(15) Uani 1 1 d . . . . .
H13A H 0.117375 0.249068 0.577048 0.145 Uiso 1 1 calc R U . . .
C14 C 0.16644(15) 0.29777(18) 0.51707(14) 0.0915(9) Uani 1 1 d . . . . .
C15 C 0.12815(11) 0.29777(16) 0.41103(14) 0.0821(6) Uani 1 1 d . . . . .
H15A H 0.166156 0.283379 0.399104 0.099 Uiso 1 1 calc R U . . .
C16 C 0.11788(13) 0.3099(2) 0.47281(15) 0.0929(9) Uani 1 1 d . . . . .
C17 C 0.06070(19) 0.3322(3) 0.4896(2) 0.1263(18) Uani 1 1 d . . . . .
H17A H 0.052351 0.340293 0.530310 0.152 Uiso 1 1 calc R U . . .
C18 C 0.01688(19) 0.3422(3) 0.4464(3) 0.136(2) Uani 1 1 d . . . . .
H18A H -0.020664 0.357833 0.458147 0.163 Uiso 1 1 calc R U . . .
C19 C 0.02719(16) 0.3295(3) 0.3859(2) 0.1142(14) Uani 1 1 d . . . . .
H19A H -0.003332 0.336307 0.357363 0.137 Uiso 1 1 calc R U . . .
C20 C 0.08400(12) 0.30634(17) 0.36732(16) 0.0863(7) Uani 1 1 d . . . . .
C21 C 0.09342(11) 0.28811(14) 0.30368(15) 0.0800(6) Uani 1 1 d . . . . .
C22 C 0.05803(14) 0.29520(18) 0.2517(2) 0.0929(8) Uani 1 1 d . . . . .
H22A H 0.021692 0.316704 0.248320 0.112 Uiso 1 1 calc R U . . .
C23 C 0.08759(13) 0.26406(15) 0.20634(16) 0.0832(6) Uani 1 1 d . . . . .
C24 C 0.07481(17) 0.25103(18) 0.14232(17) 0.0937(8) Uani 1 1 d . . . . .
C25 C 0.0267(2) 0.2772(3) 0.1106(3) 0.1256(16) Uani 1 1 d . . . . .
H25A H -0.000007 0.304348 0.129264 0.151 Uiso 1 1 calc R U . . .
C26 C 0.0202(3) 0.2608(4) 0.0490(3) 0.154(3) Uani 1 1 d . . . . .
H26A H -0.008721 0.280105 0.024743 0.185 Uiso 1 1 calc R U . . .
C27 C 0.0565(4) 0.2165(5) 0.0250(3) 0.163(3) Uani 1 1 d . . . . .
H27A H 0.049850 0.202508 -0.014438 0.195 Uiso 1 1 calc R U . . .
C28 C 0.1036(3) 0.1922(3) 0.0598(2) 0.1313(18) Uani 1 1 d . . . . .
H28A H 0.129226 0.163376 0.042238 0.158 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31618(2) 0.31618(2) 0.31618(2) 0.05868(15) Uani 1 3 d S T P . .
O1 O 0.28295(7) 0.38163(8) 0.37049(6) 0.0634(3) Uani 1 1 d . . . . .
O2 O 0.24972(7) 0.34613(7) 0.26173(7) 0.0631(3) Uani 1 1 d . . . . .
O3 O 0.0910(3) 0.4860(4) 0.2606(2) 0.206(3) Uani 1 1 d . U . . .
O4 O 0.1252(3) 0.5267(3) 0.3702(2) 0.191(3) Uani 1 1 d . U . . .
C29 C 0.23540(10) 0.41013(11) 0.34785(9) 0.0646(4) Uani 1 1 d . . . . .
C30 C 0.21706(10) 0.38978(11) 0.28519(10) 0.0657(4) Uani 1 1 d . . . . .
C31 C 0.16974(16) 0.4160(2) 0.25603(14) 0.0978(11) Uani 1 1 d . . . . .
H31A H 0.158892 0.402383 0.217435 0.117 Uiso 1 1 calc R U . . .
C32 C 0.1360(2) 0.4645(3) 0.2835(2) 0.1296(19) Uani 1 1 d . U . . .
C33 C 0.1546(2) 0.4852(2) 0.34730(19) 0.1183(16) Uani 1 1 d . U . . .
C34 C 0.20418(16) 0.45527(16) 0.37673(13) 0.0860(7) Uani 1 1 d . . . . .
H34A H 0.215287 0.466682 0.415976 0.103 Uiso 1 1 calc R U . . .
O1S O 0.3958(12) 0.2642(11) 0.6978(11) 0.426(11) Uiso 1 1 d D . . . .
H1S H 0.366565 0.255937 0.719396 0.638 Uiso 1 1 d R U . . .
C1S C 0.4113(17) 0.3305(13) 0.7174(15) 0.44(2) Uiso 1 1 d D . . . .
H1S1 H 0.446483 0.339679 0.693081 0.662 Uiso 1 1 d R U . . .
H1S2 H 0.421343 0.334699 0.759721 0.662 Uiso 1 1 d R U . . .
H1S3 H 0.378973 0.358129 0.707240 0.662 Uiso 1 1 d R U . . .
B1 B -0.1067(10) 0.3956(10) 0.1063(8) 0.129(3) Uani 0.3333 1 d D U P A -1
F1 F -0.0758(11) 0.3949(11) 0.1596(9) 0.178(7) Uani 0.3333 1 d D U P A -1
F2 F -0.0698(12) 0.3950(9) 0.0603(8) 0.221(8) Uani 0.3333 1 d D U P A -1
F3 F -0.1488(9) 0.4403(9) 0.1055(11) 0.172(6) Uani 0.3333 1 d D U P A -1
F4 F -0.1381(10) 0.3408(7) 0.1027(10) 0.187(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9545(19) 5 ?
Fe1 N2 1.9545(19) 9 ?
Fe1 N2 1.9546(19) . ?
Fe1 N1 2.005(2) . ?
Fe1 N1 2.005(2) 5 ?
Fe1 N1 2.005(2) 9 ?
Fe2 N5 1.960(3) . ?
Fe2 N5 1.960(3) 9 ?
Fe2 N5 1.960(3) 5 ?
Fe2 N6 2.004(3) . ?
Fe2 N6 2.004(3) 9 ?
Fe2 N6 2.004(3) 5 ?
N1 C1 1.347(3) . ?
N1 C5 1.355(3) . ?
N2 N3 1.345(3) . ?
N2 C6 1.346(3) . ?
N3 C8 1.365(3) . ?
N3 H3 0.85(3) . ?
N4 N5 1.344(3) . ?
N4 C21 1.366(3) . ?
N4 H4 0.91(3) . ?
N5 C23 1.350(3) . ?
N6 C28 1.338(5) . ?
N6 C24 1.365(6) . ?
C1 C2 1.387(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.385(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.392(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.454(4) . ?
C6 C7 1.384(4) . ?
C7 C8 1.377(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.466(4) . ?
C9 C10 1.389(4) . ?
C9 C14 1.391(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.404(4) . ?
C11 C12 1.368(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.407(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.376(5) . ?
C13 H13A 0.9300 . ?
C14 C16 1.467(5) . ?
C15 C20 1.377(5) . ?
C15 C16 1.401(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.397(5) . ?
C17 C18 1.369(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.374(8) . ?
C18 H18A 0.9300 . ?
C19 C20 1.408(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.468(5) . ?
C21 C22 1.390(5) . ?
C22 C23 1.371(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.462(5) . ?
C24 C25 1.390(5) . ?
C25 C26 1.408(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.365(12) . ?
C26 H26A 0.9300 . ?
C27 C28 1.391(9) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9978(15) 9 ?
Fe3 O2 1.9978(15) 5 ?
Fe3 O2 1.9978(15) . ?
Fe3 O1 2.0048(15) . ?
Fe3 O1 2.0048(15) 5 ?
Fe3 O1 2.0048(15) 9 ?
O1 C29 1.315(3) . ?
O2 C30 1.303(3) . ?
O3 C32 1.206(5) . ?
O4 C33 1.223(4) . ?
C29 C34 1.362(3) . ?
C29 C30 1.502(3) . ?
C30 C31 1.350(3) . ?
C31 C32 1.429(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.528(5) . ?
C33 C34 1.427(4) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.56(2) . ?
O1S H1S 0.8197 . ?
C1S H1S1 0.9601 . ?
C1S H1S2 0.9601 . ?
C1S H1S3 0.9599 . ?
B1 F2 1.295(16) . ?
B1 F3 1.35(2) . ?
B1 F1 1.35(2) . ?
B1 F4 1.388(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.32(8) 5 9 ?
N2 Fe1 N2 96.33(8) 5 . ?
N2 Fe1 N2 96.32(8) 9 . ?
N2 Fe1 N1 90.04(8) 5 . ?
N2 Fe1 N1 173.15(9) 9 . ?
N2 Fe1 N1 80.41(8) . . ?
N2 Fe1 N1 80.41(9) 5 5 ?
N2 Fe1 N1 90.04(8) 9 5 ?
N2 Fe1 N1 173.16(9) . 5 ?
N1 Fe1 N1 93.52(9) . 5 ?
N2 Fe1 N1 173.16(9) 5 9 ?
N2 Fe1 N1 80.41(8) 9 9 ?
N2 Fe1 N1 90.03(8) . 9 ?
N1 Fe1 N1 93.52(9) . 9 ?
N1 Fe1 N1 93.52(9) 5 9 ?
N5 Fe2 N5 96.33(8) . 9 ?
N5 Fe2 N5 96.33(8) . 5 ?
N5 Fe2 N5 96.33(8) 9 5 ?
N5 Fe2 N6 80.52(12) . . ?
N5 Fe2 N6 90.57(13) 9 . ?
N5 Fe2 N6 172.71(13) 5 . ?
N5 Fe2 N6 172.71(13) . 9 ?
N5 Fe2 N6 80.52(12) 9 9 ?
N5 Fe2 N6 90.57(13) 5 9 ?
N6 Fe2 N6 92.89(15) . 9 ?
N5 Fe2 N6 90.57(13) . 5 ?
N5 Fe2 N6 172.71(13) 9 5 ?
N5 Fe2 N6 80.52(12) 5 5 ?
N6 Fe2 N6 92.89(15) . 5 ?
N6 Fe2 N6 92.89(15) 9 5 ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.16(19) . . ?
C5 N1 Fe1 114.71(17) . . ?
N3 N2 C6 105.8(2) . . ?
N3 N2 Fe1 136.27(16) . . ?
C6 N2 Fe1 116.11(17) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 129(3) . . ?
C8 N3 H3 121(3) . . ?
N5 N4 C21 111.4(2) . . ?
N5 N4 H4 119(3) . . ?
C21 N4 H4 127(3) . . ?
N4 N5 C23 105.6(2) . . ?
N4 N5 Fe2 135.87(18) . . ?
C23 N5 Fe2 115.8(2) . . ?
C28 N6 C24 117.8(4) . . ?
C28 N6 Fe2 127.4(4) . . ?
C24 N6 Fe2 114.7(2) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.6(3) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C3 C4 C5 118.6(3) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 122.2(3) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 124.1(3) . . ?
N2 C6 C7 111.1(2) . . ?
N2 C6 C5 114.3(2) . . ?
C7 C6 C5 134.6(2) . . ?
C8 C7 C6 105.1(2) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 107.5(2) . . ?
N3 C8 C10 122.8(2) . . ?
C7 C8 C10 129.8(2) . . ?
C10 C9 C14 120.4(3) . . ?
C10 C9 H9A 119.8 . . ?
C14 C9 H9A 119.8 . . ?
C9 C10 C11 119.3(3) . . ?
C9 C10 C8 121.5(2) . . ?
C11 C10 C8 119.2(3) . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 120.0(4) . . ?
C11 C12 H12A 120.0 . . ?
C13 C12 H12A 120.0 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C13 C14 C9 119.9(4) . . ?
C13 C14 C16 121.6(3) . . ?
C9 C14 C16 118.4(3) . . ?
C20 C15 C16 122.4(3) . . ?
C20 C15 H15A 118.8 . . ?
C16 C15 H15A 118.8 . . ?
C17 C16 C15 117.8(4) . . ?
C17 C16 C14 122.8(3) . . ?
C15 C16 C14 119.3(3) . . ?
C18 C17 C16 120.3(4) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C19 121.4(3) . . ?
C17 C18 H18A 119.3 . . ?
C19 C18 H18A 119.3 . . ?
C18 C19 C20 119.9(4) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C15 C20 C19 118.1(3) . . ?
C15 C20 C21 121.8(2) . . ?
C19 C20 C21 120.0(3) . . ?
N4 C21 C22 106.1(3) . . ?
N4 C21 C20 121.5(3) . . ?
C22 C21 C20 132.3(3) . . ?
C23 C22 C21 106.0(3) . . ?
C23 C22 H22A 127.0 . . ?
C21 C22 H22A 127.0 . . ?
N5 C23 C22 111.0(3) . . ?
N5 C23 C24 114.2(3) . . ?
C22 C23 C24 134.8(3) . . ?
N6 C24 C25 123.5(4) . . ?
N6 C24 C23 113.4(3) . . ?
C25 C24 C23 123.1(4) . . ?
C24 C25 C26 116.9(6) . . ?
C24 C25 H25A 121.6 . . ?
C26 C25 H25A 121.6 . . ?
C27 C26 C25 119.6(5) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 119.7(5) . . ?
C26 C27 H27A 120.1 . . ?
C28 C27 H27A 120.1 . . ?
N6 C28 C27 122.2(6) . . ?
N6 C28 H28A 118.9 . . ?
C27 C28 H28A 118.9 . . ?
O2 Fe3 O2 90.02(7) 9 5 ?
O2 Fe3 O2 90.01(7) 9 . ?
O2 Fe3 O2 90.01(7) 5 . ?
O2 Fe3 O1 169.48(6) 9 . ?
O2 Fe3 O1 96.31(7) 5 . ?
O2 Fe3 O1 81.61(6) . . ?
O2 Fe3 O1 96.32(7) 9 5 ?
O2 Fe3 O1 81.62(6) 5 5 ?
O2 Fe3 O1 169.48(6) . 5 ?
O1 Fe3 O1 92.93(7) . 5 ?
O2 Fe3 O1 81.61(6) 9 9 ?
O2 Fe3 O1 169.48(6) 5 9 ?
O2 Fe3 O1 96.31(7) . 9 ?
O1 Fe3 O1 92.93(7) . 9 ?
O1 Fe3 O1 92.93(7) 5 9 ?
C29 O1 Fe3 113.91(13) . . ?
C30 O2 Fe3 114.05(13) . . ?
O1 C29 C34 124.8(2) . . ?
O1 C29 C30 114.69(19) . . ?
C34 C29 C30 120.5(2) . . ?
O2 C30 C31 123.4(2) . . ?
O2 C30 C29 115.69(19) . . ?
C31 C30 C29 120.9(2) . . ?
C30 C31 C32 121.1(3) . . ?
C30 C31 H31A 119.5 . . ?
C32 C31 H31A 119.5 . . ?
O3 C32 C31 122.7(4) . . ?
O3 C32 C33 118.9(4) . . ?
C31 C32 C33 118.1(3) . . ?
O4 C33 C34 124.0(4) . . ?
O4 C33 C32 117.3(3) . . ?
C34 C33 C32 118.8(3) . . ?
C29 C34 C33 120.6(3) . . ?
C29 C34 H34A 119.7 . . ?
C33 C34 H34A 119.7 . . ?
C1S O1S H1S 102.6 . . ?
O1S C1S H1S1 102.6 . . ?
O1S C1S H1S2 114.1 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 111.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F3 115.2(16) . . ?
F2 B1 F1 111.2(18) . . ?
F3 B1 F1 111.3(18) . . ?
F2 B1 F4 105.0(17) . . ?
F3 B1 F4 106.8(16) . . ?
F1 B1 F4 106.8(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.85(3) 2.19(3) 2.944(2) 147(4) . yes
N4 H4 O2 0.91(3) 2.03(3) 2.935(3) 172(5) 5 yes

_refine_diff_density_max         0.668
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.075

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_300K
_database_code_depnum_ccdc_archive 'CCDC 2261721'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.828(3)
_cell_length_b                   21.828(3)
_cell_length_c                   21.828(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10400(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6437
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      33.76

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.523
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            168719
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0660
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.354
_diffrn_reflns_theta_max         29.522
_diffrn_reflns_theta_full        29.522
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8999
_reflns_number_gt                8624
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 restraints and displacement parameters restraints. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1206P)²+0.0608P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0257(17)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3817 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.092(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8999
_refine_ls_number_parameters     476
_refine_ls_number_restraints     103
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1425
_refine_ls_wR_factor_gt          0.1412
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29699(2) 0.29699(2) 0.29699(2) 0.06828(16) Uani 1 3 d S T P . .
Fe2 Fe 0.57886(2) 0.57886(2) 0.57886(2) 0.07816(18) Uani 1 3 d S T P . .
N1 N 0.23359(11) 0.33118(11) 0.23944(10) 0.0768(5) Uani 1 1 d . . . . .
N2 N 0.26044(9) 0.36014(10) 0.34982(10) 0.0718(4) Uani 1 1 d . . . . .
N3 N 0.26392(10) 0.37597(11) 0.40960(10) 0.0738(4) Uani 1 1 d . . . . .
H3 H 0.291(3) 0.368(3) 0.424(3) 0.111 Uiso 1 1 d . U . . .
N4 N 0.46919(11) 0.49604(13) 0.61338(10) 0.0815(5) Uani 1 1 d D . . . .
H4 H 0.446(2) 0.501(3) 0.5806(18) 0.122 Uiso 1 1 d D U . . .
N5 N 0.52853(11) 0.51246(12) 0.61542(11) 0.0814(5) Uani 1 1 d . . . . .
N6 N 0.63855(13) 0.54477(16) 0.64149(15) 0.0956(7) Uani 1 1 d . . . . .
C1 C 0.22396(17) 0.31450(15) 0.18105(13) 0.0879(7) Uani 1 1 d . . . . .
H1A H 0.249569 0.285370 0.163418 0.106 Uiso 1 1 calc R U . . .
C2 C 0.1770(2) 0.3394(2) 0.14619(18) 0.1095(11) Uani 1 1 d . . . . .
H2A H 0.170988 0.326584 0.105997 0.131 Uiso 1 1 calc R U . . .
C3 C 0.1395(2) 0.3830(2) 0.1715(2) 0.1162(13) Uani 1 1 d . . . . .
H3B H 0.107909 0.400135 0.148713 0.139 Uiso 1 1 calc R U . . .
C4 C 0.1494(2) 0.4012(2) 0.2319(2) 0.1083(11) Uani 1 1 d . . . . .
H4B H 0.124815 0.430974 0.249973 0.130 Uiso 1 1 calc R U . . .
C5 C 0.19659(14) 0.37411(14) 0.26420(14) 0.0816(6) Uani 1 1 d . . . . .
C6 C 0.21028(13) 0.38793(13) 0.32789(14) 0.0798(5) Uani 1 1 d . . . . .
C7 C 0.18196(14) 0.42216(16) 0.37310(17) 0.0891(7) Uani 1 1 d . . . . .
H7A H 0.146519 0.445493 0.369255 0.107 Uiso 1 1 calc R U . . .
C8 C 0.21705(11) 0.41456(13) 0.42493(14) 0.0795(5) Uani 1 1 d . . . . .
C9 C 0.20926(12) 0.43990(15) 0.48658(15) 0.0862(7) Uani 1 1 d . . . . .
C10 C 0.16051(18) 0.4796(2) 0.4980(2) 0.1113(11) Uani 1 1 d . . . . .
H10A H 0.134042 0.490503 0.466440 0.134 Uiso 1 1 calc R U . . .
C11 C 0.1516(2) 0.5028(3) 0.5563(3) 0.139(2) Uani 1 1 d . . . . .
H11A H 0.119612 0.529948 0.563618 0.167 Uiso 1 1 calc R U . . .
C12 C 0.1895(2) 0.4859(3) 0.6032(2) 0.1286(17) Uani 1 1 d . . . . .
H12A H 0.181703 0.500116 0.642556 0.154 Uiso 1 1 calc R U . . .
C13 C 0.23891(16) 0.4484(2) 0.59310(17) 0.1013(10) Uani 1 1 d . . . . .
C14 C 0.24789(13) 0.42453(17) 0.53408(14) 0.0893(7) Uani 1 1 d . . . . .
H14A H 0.280405 0.397950 0.526916 0.107 Uiso 1 1 calc R U . . .
C15 C 0.28434(16) 0.4353(2) 0.64103(15) 0.1021(10) Uani 1 1 d . . . . .
C16 C 0.2688(3) 0.4137(3) 0.6989(2) 0.139(2) Uani 1 1 d . . . . .
H16A H 0.228089 0.404646 0.707736 0.167 Uiso 1 1 calc R U . . .
C17 C 0.3124(3) 0.4055(4) 0.7428(2) 0.148(2) Uani 1 1 d . . . . .
H17A H 0.300591 0.392736 0.781708 0.178 Uiso 1 1 calc R U . . .
C18 C 0.3740(3) 0.4159(3) 0.73097(19) 0.1322(18) Uani 1 1 d . . . . .
H18A H 0.403551 0.407173 0.760378 0.159 Uiso 1 1 calc R U . . .
C19 C 0.39087(17) 0.4400(2) 0.67304(14) 0.0964(8) Uani 1 1 d . . . . .
C20 C 0.34674(16) 0.44747(18) 0.62992(13) 0.0926(8) Uani 1 1 d . . . . .
H20A H 0.358214 0.461228 0.591267 0.111 Uiso 1 1 calc R U . . .
C21 C 0.45401(17) 0.46040(16) 0.66190(12) 0.0881(7) Uani 1 1 d . . . . .
C22 C 0.50684(18) 0.45422(18) 0.69753(15) 0.0955(8) Uani 1 1 d . . . . .
H22A H 0.511256 0.432497 0.733915 0.115 Uiso 1 1 calc R U . . .
C23 C 0.55116(16) 0.48756(16) 0.66672(14) 0.0879(7) Uani 1 1 d . . . . .
C24 C 0.61500(17) 0.50342(19) 0.68099(17) 0.0971(8) Uani 1 1 d . . . . .
C25 C 0.6464(2) 0.4789(3) 0.7288(3) 0.1276(15) Uani 1 1 d . . . . .
H25A H 0.627774 0.451884 0.756032 0.153 Uiso 1 1 calc R U . . .
C26 C 0.7083(3) 0.4959(4) 0.7356(3) 0.152(2) Uani 1 1 d . . . . .
H26A H 0.732422 0.476574 0.764911 0.182 Uiso 1 1 calc R U . . .
C27 C 0.7331(3) 0.5406(4) 0.6995(4) 0.157(2) Uani 1 1 d . . . . .
H27A H 0.772331 0.555578 0.706579 0.188 Uiso 1 1 calc R U . . .
C28 C 0.6969(2) 0.5629(3) 0.6513(3) 0.1272(16) Uani 1 1 d . . . . .
H28A H 0.713952 0.591658 0.624869 0.153 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43675(2) 0.43675(2) 0.43675(2) 0.07108(16) Uani 1 3 d S T P . .
O1 O 0.38387(8) 0.36914(8) 0.46971(8) 0.0732(4) Uani 1 1 d . . . . .
O2 O 0.49352(8) 0.40600(8) 0.50170(9) 0.0754(4) Uani 1 1 d . . . . .
O3 O 0.5079(2) 0.2487(3) 0.6460(3) 0.206(3) Uani 1 1 d . U . . .
O4 O 0.3928(2) 0.2138(3) 0.6185(2) 0.171(2) Uani 1 1 d . U . . .
C29 C 0.40832(11) 0.33921(12) 0.51490(11) 0.0742(5) Uani 1 1 d . . . . .
C30 C 0.47229(12) 0.35933(13) 0.53217(12) 0.0766(5) Uani 1 1 d . . . . .
C31 C 0.50429(17) 0.3286(2) 0.57556(17) 0.1075(12) Uani 1 1 d . . . . .
H31A H 0.543816 0.341423 0.584989 0.129 Uiso 1 1 calc R U . . .
C32 C 0.4795(2) 0.2777(3) 0.6070(2) 0.1237(16) Uani 1 1 d . U . . .
C33 C 0.4140(2) 0.2573(3) 0.5911(2) 0.1173(14) Uani 1 1 d . U . . .
C34 C 0.38153(14) 0.29142(17) 0.54505(15) 0.0914(8) Uani 1 1 d . . . . .
H34A H 0.341391 0.280712 0.535606 0.110 Uiso 1 1 calc R U . . .
O1S O 0.0282(16) 0.4417(16) 0.3498(15) 0.575(17) Uani 1 1 d D U . . .
H1S H 0.041797 0.406725 0.352146 0.863 Uiso 1 1 d R U . . .
C1S C -0.0458(18) 0.438(2) 0.360(2) 0.588(19) Uani 1 1 d D U . . .
H1S1 H -0.054180 0.424919 0.401299 0.883 Uiso 1 1 d R U . . .
H1S2 H -0.063360 0.409969 0.331649 0.883 Uiso 1 1 d R U . . .
H1S3 H -0.063260 0.478219 0.354019 0.883 Uiso 1 1 d R U . . .
B1 B 0.1396(11) 0.1412(9) 0.1394(10) 0.133(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1072(12) 0.1501(14) 0.0843(9) 0.205(8) Uani 0.3333 1 d D U P A -1
F2 F 0.1775(11) 0.1890(8) 0.1461(8) 0.212(8) Uani 0.3333 1 d D U P A -1
F3 F 0.0978(7) 0.1377(13) 0.1864(10) 0.179(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1723(15) 0.0871(10) 0.1344(12) 0.175(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.966(2) . ?
Fe1 N2 1.966(2) 9 ?
Fe1 N2 1.966(2) 5 ?
Fe1 N1 2.013(2) 5 ?
Fe1 N1 2.013(2) 9 ?
Fe1 N1 2.013(2) . ?
Fe2 N5 1.986(3) 9 ?
Fe2 N5 1.986(3) 5 ?
Fe2 N5 1.986(3) . ?
Fe2 N6 2.030(3) 9 ?
Fe2 N6 2.030(3) 5 ?
Fe2 N6 2.030(3) . ?
N1 C1 1.342(4) . ?
N1 C5 1.350(4) . ?
N2 C6 1.340(3) . ?
N2 N3 1.352(3) . ?
N3 C8 1.367(3) . ?
N3 H3 0.69(6) . ?
N4 N5 1.345(4) . ?
N4 C21 1.355(4) . ?
N4 H4 0.88(3) . ?
N5 C23 1.339(4) . ?
N6 C24 1.350(6) . ?
N6 C28 1.352(5) . ?
C1 C2 1.387(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.393(7) . ?
C3 H3B 0.9300 . ?
C4 C5 1.382(4) . ?
C4 H4B 0.9300 . ?
C5 C6 1.454(4) . ?
C6 C7 1.383(4) . ?
C7 C8 1.376(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.465(4) . ?
C9 C14 1.378(5) . ?
C9 C10 1.395(5) . ?
C10 C11 1.383(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.372(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.403(4) . ?
C13 C15 1.469(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.391(5) . ?
C15 C20 1.409(5) . ?
C16 C17 1.363(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.387(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.418(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.356(5) . ?
C19 C21 1.469(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.397(5) . ?
C22 C23 1.385(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.469(5) . ?
C24 C25 1.359(5) . ?
C25 C26 1.408(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.366(10) . ?
C26 H26A 0.9300 . ?
C27 C28 1.402(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9990(18) 9 ?
Fe3 O2 1.9990(18) . ?
Fe3 O2 1.9991(18) 5 ?
Fe3 O1 2.0071(17) 9 ?
Fe3 O1 2.0071(17) 5 ?
Fe3 O1 2.0071(17) . ?
O1 C29 1.298(3) . ?
O2 C30 1.302(3) . ?
O3 C32 1.229(5) . ?
O4 C33 1.214(5) . ?
C29 C34 1.365(4) . ?
C29 C30 1.512(4) . ?
C30 C31 1.354(4) . ?
C31 C32 1.414(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.537(6) . ?
C33 C34 1.437(5) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.63(2) . ?
O1S H1S 0.8199 . ?
C1S H1S1 0.9601 . ?
C1S H1S2 0.9599 . ?
C1S H1S3 0.9601 . ?
B1 F2 1.340(15) . ?
B1 F3 1.38(2) . ?
B1 F4 1.38(2) . ?
B1 F1 1.407(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.39(8) . 9 ?
N2 Fe1 N2 96.39(8) . 5 ?
N2 Fe1 N2 96.39(8) 9 5 ?
N2 Fe1 N1 90.65(9) . 5 ?
N2 Fe1 N1 172.44(9) 9 5 ?
N2 Fe1 N1 80.04(9) 5 5 ?
N2 Fe1 N1 172.44(9) . 9 ?
N2 Fe1 N1 80.04(9) 9 9 ?
N2 Fe1 N1 90.65(9) 5 9 ?
N1 Fe1 N1 93.28(10) 5 9 ?
N2 Fe1 N1 80.04(9) . . ?
N2 Fe1 N1 90.65(9) 9 . ?
N2 Fe1 N1 172.44(9) 5 . ?
N1 Fe1 N1 93.28(10) 5 . ?
N1 Fe1 N1 93.28(10) 9 . ?
N5 Fe2 N5 96.42(10) 9 5 ?
N5 Fe2 N5 96.41(10) 9 . ?
N5 Fe2 N5 96.42(10) 5 . ?
N5 Fe2 N6 79.45(11) 9 9 ?
N5 Fe2 N6 171.22(12) 5 9 ?
N5 Fe2 N6 91.76(12) . 9 ?
N5 Fe2 N6 91.77(12) 9 5 ?
N5 Fe2 N6 79.45(11) 5 5 ?
N5 Fe2 N6 171.22(12) . 5 ?
N6 Fe2 N6 92.87(13) 9 5 ?
N5 Fe2 N6 171.22(12) 9 . ?
N5 Fe2 N6 91.77(12) 5 . ?
N5 Fe2 N6 79.45(11) . . ?
N6 Fe2 N6 92.86(13) 9 . ?
N6 Fe2 N6 92.86(13) 5 . ?
C1 N1 C5 118.4(3) . . ?
C1 N1 Fe1 126.9(2) . . ?
C5 N1 Fe1 114.76(19) . . ?
C6 N2 N3 106.0(2) . . ?
C6 N2 Fe1 116.07(19) . . ?
N3 N2 Fe1 136.25(17) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 116(5) . . ?
C8 N3 H3 132(5) . . ?
N5 N4 C21 111.3(3) . . ?
N5 N4 H4 123(4) . . ?
C21 N4 H4 125(4) . . ?
C23 N5 N4 106.0(3) . . ?
C23 N5 Fe2 115.3(2) . . ?
N4 N5 Fe2 135.6(2) . . ?
C24 N6 C28 117.0(4) . . ?
C24 N6 Fe2 115.5(2) . . ?
C28 N6 Fe2 127.2(3) . . ?
N1 C1 C2 122.0(3) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.4(4) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C5 C4 C3 118.4(4) . . ?
C5 C4 H4B 120.8 . . ?
C3 C4 H4B 120.8 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 113.8(2) . . ?
C4 C5 C6 123.5(3) . . ?
N2 C6 C7 110.8(3) . . ?
N2 C6 C5 114.6(3) . . ?
C7 C6 C5 134.6(3) . . ?
C8 C7 C6 105.8(2) . . ?
C8 C7 H7A 127.1 . . ?
C6 C7 H7A 127.1 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C9 123.0(3) . . ?
C7 C8 C9 130.2(3) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 C8 121.9(3) . . ?
C10 C9 C8 119.2(3) . . ?
C11 C10 C9 119.9(5) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C12 C11 C10 120.3(4) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.1(4) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C12 C13 C14 118.6(4) . . ?
C12 C13 C15 122.1(4) . . ?
C14 C13 C15 119.2(3) . . ?
C9 C14 C13 121.0(3) . . ?
C9 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C16 C15 C20 117.2(4) . . ?
C16 C15 C13 123.2(4) . . ?
C20 C15 C13 119.6(3) . . ?
C17 C16 C15 120.8(4) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 121.6(4) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C19 118.6(5) . . ?
C17 C18 H18A 120.7 . . ?
C19 C18 H18A 120.7 . . ?
C20 C19 C18 118.6(4) . . ?
C20 C19 C21 121.0(3) . . ?
C18 C19 C21 120.3(4) . . ?
C19 C20 C15 123.0(3) . . ?
C19 C20 H20A 118.5 . . ?
C15 C20 H20A 118.5 . . ?
N4 C21 C22 106.8(3) . . ?
N4 C21 C19 122.2(3) . . ?
C22 C21 C19 130.8(3) . . ?
C23 C22 C21 104.8(3) . . ?
C23 C22 H22A 127.6 . . ?
C21 C22 H22A 127.6 . . ?
N5 C23 C22 111.2(3) . . ?
N5 C23 C24 115.6(3) . . ?
C22 C23 C24 133.1(3) . . ?
N6 C24 C25 124.2(4) . . ?
N6 C24 C23 112.5(3) . . ?
C25 C24 C23 123.3(4) . . ?
C24 C25 C26 117.4(6) . . ?
C24 C25 H25A 121.3 . . ?
C26 C25 H25A 121.3 . . ?
C27 C26 C25 120.5(5) . . ?
C27 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C26 C27 C28 117.3(5) . . ?
C26 C27 H27A 121.4 . . ?
C28 C27 H27A 121.4 . . ?
N6 C28 C27 123.2(6) . . ?
N6 C28 H28A 118.4 . . ?
C27 C28 H28A 118.4 . . ?
O2 Fe3 O2 90.39(8) 9 . ?
O2 Fe3 O2 90.39(8) 9 5 ?
O2 Fe3 O2 90.39(8) . 5 ?
O2 Fe3 O1 81.68(7) 9 9 ?
O2 Fe3 O1 169.77(7) . 9 ?
O2 Fe3 O1 96.10(8) 5 9 ?
O2 Fe3 O1 169.77(7) 9 5 ?
O2 Fe3 O1 96.10(8) . 5 ?
O2 Fe3 O1 81.68(7) 5 5 ?
O1 Fe3 O1 92.68(7) 9 5 ?
O2 Fe3 O1 96.10(8) 9 . ?
O2 Fe3 O1 81.69(7) . . ?
O2 Fe3 O1 169.77(7) 5 . ?
O1 Fe3 O1 92.68(7) 9 . ?
O1 Fe3 O1 92.68(7) 5 . ?
C29 O1 Fe3 113.95(15) . . ?
C30 O2 Fe3 113.86(16) . . ?
O1 C29 C34 125.1(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 119.8(2) . . ?
O2 C30 C31 124.1(3) . . ?
O2 C30 C29 115.4(2) . . ?
C31 C30 C29 120.5(3) . . ?
C30 C31 C32 122.0(3) . . ?
C30 C31 H31A 119.0 . . ?
C32 C31 H31A 119.0 . . ?
O3 C32 C31 123.1(4) . . ?
O3 C32 C33 118.5(4) . . ?
C31 C32 C33 118.3(3) . . ?
O4 C33 C34 124.3(4) . . ?
O4 C33 C32 117.9(4) . . ?
C34 C33 C32 117.8(3) . . ?
C29 C34 C33 121.5(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C1S O1S H1S 108.0 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.4 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F3 111.7(16) . . ?
F2 B1 F4 110.9(17) . . ?
F3 B1 F4 110.6(18) . . ?
F2 B1 F1 107.2(16) . . ?
F3 B1 F1 108.1(17) . . ?
F4 B1 F1 108.1(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.69(6) 2.25(6) 2.932(3) 166(6) . yes
N4 H4 O2 0.88(3) 2.09(3) 2.960(3) 168(5) 9 yes

_refine_diff_density_max         0.644
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.076

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_250K
_database_code_depnum_ccdc_archive 'CCDC 2261719'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   22.009(3)
_cell_length_b                   22.009(3)
_cell_length_c                   22.009(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10661(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    6887
_cell_measurement_theta_min      1.34
_cell_measurement_theta_max      34.01

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.511
_shelx_estimated_absorpt_T_min   0.883
_shelx_estimated_absorpt_T_max   0.905
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            177460
_diffrn_reflns_av_unetI/netI     0.0328
_diffrn_reflns_av_R_equivalents  0.0931
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.899
_diffrn_reflns_theta_max         29.513
_diffrn_reflns_theta_full        29.513
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9195
_reflns_number_gt                9127
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.861
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disorder by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1378 cubic angstrom with a total of 233 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 80 electron per cell at 300 K,
 after measurements done up to 400 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
 
 Details of SQUEEZE results (before BF4 disorder refinement):

loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.094  0.136  0.141      1378       233 ' '
   2  0.117  0.383  0.617         9         0 ' '
   3  0.383  0.617  0.117         9         0 ' '
   4  0.617  0.117  0.383         9         0 ' '
   5  0.883  0.883  0.883         9         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?



 Details of SQUEEZE results on a 300 K data set of the same crystal
 after measurements up to 400 K:

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.118  0.151  0.141      1841        80 ' '
   2  0.144  0.356  0.644        10         0 ' '
   3  0.356  0.644  0.144        10         0 ' '
   4  0.644  0.144  0.356        10         0 ' '
   5  0.856  0.856  0.856        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?
;

_vrf_PLAT601_lb2205_fresh2_250K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1378 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1378 cubic angstrom with a total of 233 electrons.
 These figures could agree with a small amount of very diffuse lattice
 methanol. Nevertherless the same crystal was then 
 measured at numerous temperatures, eventually losing its lattice MeOH
 molecule, but there remained a similar, though somewhat smaller, electron
 residual density throughout the whole thermal cycling process. We therefore
 believe that although there may be some additional diffuse lattice solvent,
 the amount is necessarily smaller than derived from the electron count. 
 Considering the same crystal still showed 80 electron per cell at 300 K,
 after measurements done up to 400 K, we estimate that the amount of
 additional lattice diffuse MeOH cannot exceed 1 molecule per formula
 unit, and may well be much lower. Consequently we have decided to not
 use the structure refined after PLATON/SQUEEZE treatment, and report the
 present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1166P)²+0.2555P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.081(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 4180 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.054(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9195
_refine_ls_number_parameters     476
_refine_ls_number_restraints     88
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0510
_refine_ls_wR_factor_ref         0.1447
_refine_ls_wR_factor_gt          0.1445
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_restrained_S_all      1.122
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45476(2) 0.45476(2) 0.45476(2) 0.04970(17) Uani 1 3 d S T P . .
Fe2 Fe 0.17689(2) 0.17689(2) 0.17689(2) 0.0651(2) Uani 1 3 d S T P . .
N1 N 0.51592(10) 0.42075(10) 0.51253(10) 0.0563(4) Uani 1 1 d . . . . .
N2 N 0.40684(9) 0.38923(10) 0.49014(10) 0.0538(4) Uani 1 1 d . . . . .
N3 N 0.34781(10) 0.37224(10) 0.48896(9) 0.0547(4) Uani 1 1 d D . . . .
H3 H 0.3234(19) 0.381(2) 0.4600(17) 0.082 Uiso 1 1 d D U . . .
N4 N 0.14400(9) 0.25219(11) 0.28896(11) 0.0590(5) Uani 1 1 d D . . . .
H4 H 0.1795(15) 0.253(2) 0.309(2) 0.088 Uiso 1 1 d D U . . .
N5 N 0.14077(10) 0.23876(11) 0.22937(11) 0.0609(5) Uani 1 1 d . . . . .
N6 N 0.11454(16) 0.21062(19) 0.12018(15) 0.0859(9) Uani 1 1 d . . . . .
C1 C 0.57422(13) 0.43770(14) 0.51938(15) 0.0662(6) Uani 1 1 d . . . . .
H1A H 0.589432 0.469275 0.494970 0.079 Uiso 1 1 calc R U . . .
C2 C 0.61272(15) 0.41041(18) 0.5611(2) 0.0824(9) Uani 1 1 d . . . . .
H2A H 0.653673 0.422256 0.563688 0.099 Uiso 1 1 calc R U . . .
C3 C 0.59030(18) 0.3660(2) 0.5983(2) 0.0881(10) Uani 1 1 d . . . . .
H3A H 0.615403 0.348359 0.628068 0.106 Uiso 1 1 calc R U . . .
C4 C 0.53098(17) 0.34707(18) 0.59228(19) 0.0804(9) Uani 1 1 d . . . . .
H4A H 0.515252 0.316058 0.617084 0.096 Uiso 1 1 calc R U . . .
C5 C 0.49488(12) 0.37502(13) 0.54852(13) 0.0610(5) Uani 1 1 d . . . . .
C6 C 0.43172(13) 0.36032(12) 0.53755(12) 0.0602(5) Uani 1 1 d . . . . .
C7 C 0.38922(15) 0.32341(15) 0.56680(14) 0.0689(7) Uani 1 1 d . . . . .
H7A H 0.395339 0.298469 0.600932 0.083 Uiso 1 1 calc R U . . .
C8 C 0.33612(13) 0.33176(13) 0.53430(11) 0.0608(5) Uani 1 1 d . . . . .
C9 C 0.22707(13) 0.31903(16) 0.50666(12) 0.0662(6) Uani 1 1 d . . . . .
H9A H 0.233230 0.343601 0.472281 0.079 Uiso 1 1 calc R U . . .
C10 C 0.27575(13) 0.30604(14) 0.54495(12) 0.0649(6) Uani 1 1 d . . . . .
C11 C 0.2663(2) 0.2683(2) 0.59555(17) 0.0914(11) Uani 1 1 d . . . . .
H11A H 0.299090 0.257433 0.620656 0.110 Uiso 1 1 calc R U . . .
C12 C 0.2092(3) 0.2474(3) 0.6081(2) 0.119(2) Uani 1 1 d . . . . .
H12A H 0.202631 0.223441 0.642896 0.143 Uiso 1 1 calc R U . . .
C13 C 0.1603(2) 0.2612(3) 0.56969(19) 0.1010(15) Uani 1 1 d . . . . .
H13A H 0.121225 0.246686 0.578781 0.121 Uiso 1 1 calc R U . . .
C14 C 0.16963(14) 0.29612(18) 0.51868(14) 0.0744(8) Uani 1 1 d . . . . .
C15 C 0.13072(11) 0.29592(16) 0.41333(14) 0.0671(6) Uani 1 1 d . . . . .
H15A H 0.168949 0.281378 0.401020 0.080 Uiso 1 1 calc R U . . .
C16 C 0.12063(14) 0.3077(2) 0.47478(16) 0.0779(8) Uani 1 1 d . . . . .
C17 C 0.06396(19) 0.3282(3) 0.4928(2) 0.1081(16) Uani 1 1 d . . . . .
H17A H 0.055332 0.333790 0.534240 0.130 Uiso 1 1 calc R U . . .
C18 C 0.01954(18) 0.3405(3) 0.4489(3) 0.1138(18) Uani 1 1 d . . . . .
H18A H -0.017820 0.357345 0.460946 0.137 Uiso 1 1 calc R U . . .
C19 C 0.02980(16) 0.3283(3) 0.3883(2) 0.0949(12) Uani 1 1 d . . . . .
H19A H -0.000851 0.335504 0.359457 0.114 Uiso 1 1 calc R U . . .
C20 C 0.08611(12) 0.30498(17) 0.36996(16) 0.0709(7) Uani 1 1 d . . . . .
C21 C 0.09540(11) 0.28693(15) 0.30639(15) 0.0666(6) Uani 1 1 d . . . . .
C22 C 0.05974(14) 0.29477(18) 0.2548(2) 0.0799(8) Uani 1 1 d . . . . .
H22A H 0.022895 0.316180 0.251998 0.096 Uiso 1 1 calc R U . . .
C23 C 0.08957(13) 0.26464(15) 0.20860(16) 0.0690(6) Uani 1 1 d . . . . .
C24 C 0.07683(17) 0.2527(2) 0.14461(18) 0.0831(9) Uani 1 1 d . . . . .
C25 C 0.0290(2) 0.2798(3) 0.1138(3) 0.1085(15) Uani 1 1 d . . . . .
H25A H 0.002033 0.306924 0.132850 0.130 Uiso 1 1 calc R U . . .
C26 C 0.0232(3) 0.2638(5) 0.0509(3) 0.141(3) Uani 1 1 d . . . . .
H26A H -0.006229 0.282906 0.026565 0.169 Uiso 1 1 calc R U . . .
C27 C 0.0594(4) 0.2220(5) 0.0271(3) 0.155(3) Uani 1 1 d . . . . .
H27A H 0.054008 0.210267 -0.013613 0.186 Uiso 1 1 calc R U . . .
C28 C 0.1056(3) 0.1951(4) 0.0617(2) 0.128(2) Uani 1 1 d . . . . .
H28A H 0.130779 0.165606 0.043746 0.154 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31689(2) 0.31689(2) 0.31689(2) 0.04616(16) Uani 1 3 d S T P . .
O1 O 0.28350(8) 0.38136(8) 0.37166(7) 0.0518(3) Uani 1 1 d . . . . .
O2 O 0.24982(7) 0.34661(7) 0.26349(7) 0.0501(3) Uani 1 1 d . . . . .
O3 O 0.0867(2) 0.4806(3) 0.2663(2) 0.166(3) Uani 1 1 d . U . . .
O4 O 0.1237(3) 0.5230(3) 0.3747(2) 0.162(3) Uani 1 1 d . U . . .
C29 C 0.23522(11) 0.40946(11) 0.34980(10) 0.0530(4) Uani 1 1 d . . . . .
C30 C 0.21635(11) 0.38914(11) 0.28733(10) 0.0529(4) Uani 1 1 d . . . . .
C31 C 0.16795(16) 0.41365(18) 0.25917(14) 0.0760(8) Uani 1 1 d . . . . .
H31A H 0.157260 0.400041 0.220120 0.091 Uiso 1 1 calc R U . . .
C32 C 0.1324(2) 0.4602(3) 0.28772(19) 0.1042(16) Uani 1 1 d . U . . .
C33 C 0.1528(2) 0.4824(3) 0.35100(19) 0.1022(15) Uani 1 1 d . U . . .
C34 C 0.20409(17) 0.45382(17) 0.37920(14) 0.0760(8) Uani 1 1 d . . . . .
H34A H 0.216244 0.465908 0.418322 0.091 Uiso 1 1 calc R U . . .
O1S O 0.4014(8) 0.2650(9) 0.6976(6) 0.333(10) Uani 1 1 d D U . . .
H1S H 0.371915 0.252099 0.717228 0.500 Uiso 1 1 d R U . . .
C1S C 0.4226(10) 0.3242(12) 0.7275(9) 0.334(12) Uani 1 1 d D U . . .
H1S1 H 0.423269 0.319613 0.771360 0.502 Uiso 1 1 d R U . . .
H1S2 H 0.394619 0.356433 0.716560 0.502 Uiso 1 1 d R U . . .
H1S3 H 0.463019 0.334283 0.713190 0.502 Uiso 1 1 d R U . . .
B1 B -0.1085(8) 0.3991(9) 0.1054(6) 0.118(7) Uani 0.3333 1 d D U P A -1
F1 F -0.0672(11) 0.4068(13) 0.1505(12) 0.162(12) Uani 0.3333 1 d D U P A -1
F2 F -0.0808(14) 0.4011(15) 0.0525(8) 0.228(14) Uani 0.3333 1 d D U P A -1
F3 F -0.1570(8) 0.4369(14) 0.1122(16) 0.141(9) Uani 0.3333 1 d D U P A -1
F4 F -0.1283(13) 0.3393(9) 0.0983(10) 0.189(13) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.949(2) . ?
Fe1 N2 1.949(2) 9 ?
Fe1 N2 1.949(2) 5 ?
Fe1 N1 1.997(2) . ?
Fe1 N1 1.997(2) 9 ?
Fe1 N1 1.997(2) 5 ?
Fe2 N5 1.955(3) . ?
Fe2 N5 1.955(3) 9 ?
Fe2 N5 1.955(3) 5 ?
Fe2 N6 1.998(3) . ?
Fe2 N6 1.998(3) 9 ?
Fe2 N6 1.998(3) 5 ?
N1 C1 1.345(3) . ?
N1 C5 1.362(4) . ?
N2 C6 1.339(3) . ?
N2 N3 1.352(3) . ?
N3 C8 1.362(3) . ?
N3 H3 0.86(3) . ?
N4 N5 1.346(3) . ?
N4 C21 1.370(4) . ?
N4 H4 0.90(3) . ?
N5 C23 1.343(3) . ?
N6 C28 1.346(5) . ?
N6 C24 1.355(6) . ?
C1 C2 1.386(4) . ?
C1 H1A 0.9400 . ?
C2 C3 1.369(6) . ?
C2 H2A 0.9400 . ?
C3 C4 1.377(5) . ?
C3 H3A 0.9400 . ?
C4 C5 1.392(4) . ?
C4 H4A 0.9400 . ?
C5 C6 1.448(4) . ?
C6 C7 1.396(4) . ?
C7 C8 1.383(4) . ?
C7 H7A 0.9400 . ?
C8 C10 1.463(4) . ?
C9 C14 1.387(4) . ?
C9 C10 1.393(4) . ?
C9 H9A 0.9400 . ?
C10 C11 1.405(4) . ?
C11 C12 1.366(6) . ?
C11 H11A 0.9400 . ?
C12 C13 1.402(7) . ?
C12 H12A 0.9400 . ?
C13 C14 1.375(5) . ?
C13 H13A 0.9400 . ?
C14 C16 1.470(5) . ?
C15 C20 1.384(5) . ?
C15 C16 1.395(4) . ?
C15 H15A 0.9400 . ?
C16 C17 1.384(5) . ?
C17 C18 1.401(8) . ?
C17 H17A 0.9400 . ?
C18 C19 1.380(8) . ?
C18 H18A 0.9400 . ?
C19 C20 1.400(4) . ?
C19 H19A 0.9400 . ?
C20 C21 1.469(5) . ?
C21 C22 1.391(5) . ?
C22 C23 1.380(6) . ?
C22 H22A 0.9400 . ?
C23 C24 1.460(5) . ?
C24 C25 1.388(5) . ?
C25 C26 1.434(9) . ?
C25 H25A 0.9400 . ?
C26 C27 1.324(13) . ?
C26 H26A 0.9400 . ?
C27 C28 1.402(10) . ?
C27 H27A 0.9400 . ?
C28 H28A 0.9400 . ?
Fe3 O2 1.9971(15) 5 ?
Fe3 O2 1.9971(15) . ?
Fe3 O2 1.9971(15) 9 ?
Fe3 O1 2.0015(16) . ?
Fe3 O1 2.0015(16) 5 ?
Fe3 O1 2.0015(16) 9 ?
O1 C29 1.320(3) . ?
O2 C30 1.302(3) . ?
O3 C32 1.196(5) . ?
O4 C33 1.218(5) . ?
C29 C34 1.357(3) . ?
C29 C30 1.504(3) . ?
C30 C31 1.345(4) . ?
C31 C32 1.434(4) . ?
C31 H31A 0.9400 . ?
C32 C33 1.543(5) . ?
C33 C34 1.433(5) . ?
C34 H34A 0.9400 . ?
O1S C1S 1.53(2) . ?
O1S H1S 0.8298 . ?
C1S H1S1 0.9700 . ?
C1S H1S2 0.9701 . ?
C1S H1S3 0.9700 . ?
B1 F2 1.314(13) . ?
B1 F1 1.356(14) . ?
B1 F3 1.361(14) . ?
B1 F4 1.395(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.39(8) . 9 ?
N2 Fe1 N2 96.39(8) . 5 ?
N2 Fe1 N2 96.39(8) 9 5 ?
N2 Fe1 N1 80.38(9) . . ?
N2 Fe1 N1 173.20(9) 9 . ?
N2 Fe1 N1 89.94(9) 5 . ?
N2 Fe1 N1 89.94(9) . 9 ?
N2 Fe1 N1 80.38(9) 9 9 ?
N2 Fe1 N1 173.20(9) 5 9 ?
N1 Fe1 N1 93.57(9) . 9 ?
N2 Fe1 N1 173.20(9) . 5 ?
N2 Fe1 N1 89.94(9) 9 5 ?
N2 Fe1 N1 80.38(9) 5 5 ?
N1 Fe1 N1 93.57(9) . 5 ?
N1 Fe1 N1 93.57(9) 9 5 ?
N5 Fe2 N5 96.43(9) . 9 ?
N5 Fe2 N5 96.42(9) . 5 ?
N5 Fe2 N5 96.43(9) 9 5 ?
N5 Fe2 N6 80.27(12) . . ?
N5 Fe2 N6 90.28(13) 9 . ?
N5 Fe2 N6 172.84(13) 5 . ?
N5 Fe2 N6 172.84(13) . 9 ?
N5 Fe2 N6 80.27(12) 9 9 ?
N5 Fe2 N6 90.28(13) 5 9 ?
N6 Fe2 N6 93.34(15) . 9 ?
N5 Fe2 N6 90.28(13) . 5 ?
N5 Fe2 N6 172.84(13) 9 5 ?
N5 Fe2 N6 80.27(12) 5 5 ?
N6 Fe2 N6 93.34(15) . 5 ?
N6 Fe2 N6 93.34(15) 9 5 ?
C1 N1 C5 117.7(2) . . ?
C1 N1 Fe1 127.6(2) . . ?
C5 N1 Fe1 114.72(17) . . ?
C6 N2 N3 106.1(2) . . ?
C6 N2 Fe1 116.20(17) . . ?
N3 N2 Fe1 135.79(17) . . ?
N2 N3 C8 110.4(2) . . ?
N2 N3 H3 123(3) . . ?
C8 N3 H3 125(3) . . ?
N5 N4 C21 110.7(2) . . ?
N5 N4 H4 122(3) . . ?
C21 N4 H4 122(3) . . ?
C23 N5 N4 106.4(2) . . ?
C23 N5 Fe2 115.8(2) . . ?
N4 N5 Fe2 135.01(18) . . ?
C28 N6 C24 117.6(4) . . ?
C28 N6 Fe2 127.1(4) . . ?
C24 N6 Fe2 115.3(2) . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 120.0(3) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
N1 C5 C4 122.3(3) . . ?
N1 C5 C6 113.2(2) . . ?
C4 C5 C6 124.4(3) . . ?
N2 C6 C7 111.2(2) . . ?
N2 C6 C5 114.6(2) . . ?
C7 C6 C5 134.1(2) . . ?
C8 C7 C6 104.5(2) . . ?
C8 C7 H7A 127.8 . . ?
C6 C7 H7A 127.8 . . ?
N3 C8 C7 107.8(2) . . ?
N3 C8 C10 122.8(2) . . ?
C7 C8 C10 129.3(2) . . ?
C14 C9 C10 120.8(3) . . ?
C14 C9 H9A 119.6 . . ?
C10 C9 H9A 119.6 . . ?
C9 C10 C11 119.1(3) . . ?
C9 C10 C8 121.5(2) . . ?
C11 C10 C8 119.4(3) . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C11 C12 C13 120.6(4) . . ?
C11 C12 H12A 119.7 . . ?
C13 C12 H12A 119.7 . . ?
C14 C13 C12 120.0(3) . . ?
C14 C13 H13A 120.0 . . ?
C12 C13 H13A 120.0 . . ?
C13 C14 C9 119.6(3) . . ?
C13 C14 C16 121.6(3) . . ?
C9 C14 C16 118.7(3) . . ?
C20 C15 C16 121.9(3) . . ?
C20 C15 H15A 119.0 . . ?
C16 C15 H15A 119.0 . . ?
C17 C16 C15 118.8(4) . . ?
C17 C16 C14 122.0(3) . . ?
C15 C16 C14 119.2(3) . . ?
C16 C17 C18 119.6(4) . . ?
C16 C17 H17A 120.2 . . ?
C18 C17 H17A 120.2 . . ?
C19 C18 C17 121.0(3) . . ?
C19 C18 H18A 119.5 . . ?
C17 C18 H18A 119.5 . . ?
C18 C19 C20 119.7(4) . . ?
C18 C19 H19A 120.2 . . ?
C20 C19 H19A 120.2 . . ?
C15 C20 C19 118.8(3) . . ?
C15 C20 C21 121.3(3) . . ?
C19 C20 C21 119.8(3) . . ?
N4 C21 C22 106.3(3) . . ?
N4 C21 C20 121.8(3) . . ?
C22 C21 C20 131.7(3) . . ?
C23 C22 C21 105.9(3) . . ?
C23 C22 H22A 127.1 . . ?
C21 C22 H22A 127.1 . . ?
N5 C23 C22 110.6(3) . . ?
N5 C23 C24 114.4(3) . . ?
C22 C23 C24 134.9(3) . . ?
N6 C24 C25 124.4(4) . . ?
N6 C24 C23 112.8(3) . . ?
C25 C24 C23 122.7(5) . . ?
C24 C25 C26 115.7(6) . . ?
C24 C25 H25A 122.2 . . ?
C26 C25 H25A 122.2 . . ?
C27 C26 C25 120.0(5) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 121.0(6) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
N6 C28 C27 121.2(7) . . ?
N6 C28 H28A 119.4 . . ?
C27 C28 H28A 119.4 . . ?
O2 Fe3 O2 89.99(7) 5 . ?
O2 Fe3 O2 89.99(7) 5 9 ?
O2 Fe3 O2 89.99(7) . 9 ?
O2 Fe3 O1 96.35(7) 5 . ?
O2 Fe3 O1 81.42(6) . . ?
O2 Fe3 O1 169.29(7) 9 . ?
O2 Fe3 O1 81.42(6) 5 5 ?
O2 Fe3 O1 169.29(7) . 5 ?
O2 Fe3 O1 96.36(7) 9 5 ?
O1 Fe3 O1 93.12(7) . 5 ?
O2 Fe3 O1 169.29(7) 5 9 ?
O2 Fe3 O1 96.36(7) . 9 ?
O2 Fe3 O1 81.42(6) 9 9 ?
O1 Fe3 O1 93.13(7) . 9 ?
O1 Fe3 O1 93.12(7) 5 9 ?
C29 O1 Fe3 114.09(14) . . ?
C30 O2 Fe3 114.62(14) . . ?
O1 C29 C34 124.7(2) . . ?
O1 C29 C30 114.58(19) . . ?
C34 C29 C30 120.7(2) . . ?
O2 C30 C31 123.4(2) . . ?
O2 C30 C29 115.2(2) . . ?
C31 C30 C29 121.4(2) . . ?
C30 C31 C32 121.1(3) . . ?
C30 C31 H31A 119.4 . . ?
C32 C31 H31A 119.4 . . ?
O3 C32 C31 123.6(4) . . ?
O3 C32 C33 118.8(4) . . ?
C31 C32 C33 117.6(3) . . ?
O4 C33 C34 123.4(4) . . ?
O4 C33 C32 117.8(4) . . ?
C34 C33 C32 118.8(3) . . ?
C29 C34 C33 120.4(3) . . ?
C29 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C1S O1S H1S 107.7 . . ?
O1S C1S H1S1 110.1 . . ?
O1S C1S H1S2 108.8 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F1 109(2) . . ?
F2 B1 F3 116(2) . . ?
F1 B1 F3 111.6(19) . . ?
F2 B1 F4 94.4(15) . . ?
F1 B1 F4 114.1(18) . . ?
F3 B1 F4 110.1(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.86(3) 2.13(3) 2.951(3) 159(5) . yes
N4 H4 O2 0.90(3) 2.03(3) 2.920(3) 174(5) 5 yes

_refine_diff_density_max         0.780
_refine_diff_density_min         -0.410
_refine_diff_density_rms         0.084

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_310K
_database_code_depnum_ccdc_archive 'CCDC 2261722'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.634(3)
_cell_length_b                   21.634(3)
_cell_length_c                   21.634(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10125(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    310(2)
_cell_measurement_reflns_used    6241
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      32.86

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.369
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      310(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            160788
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_av_R_equivalents  0.0652
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.932
_diffrn_reflns_theta_max         29.511
_diffrn_reflns_theta_full        29.511
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8759
_reflns_number_gt                8030
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disorder by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1556P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.026(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3490 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.113(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8759
_refine_ls_number_parameters     466
_refine_ls_number_restraints     85
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.1803
_refine_ls_wR_factor_gt          0.1767
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29712(2) 0.29712(2) 0.29712(2) 0.0662(2) Uani 1 3 d S T P . .
Fe2 Fe 0.58347(3) 0.58347(3) 0.58347(3) 0.0737(2) Uani 1 3 d S T P . .
N1 N 0.23030(15) 0.33083(14) 0.24231(14) 0.0751(6) Uani 1 1 d . . . . .
N2 N 0.26047(13) 0.35790(14) 0.35361(13) 0.0698(5) Uani 1 1 d . . . . .
N3 N 0.26592(13) 0.37379(14) 0.41333(14) 0.0712(6) Uani 1 1 d D . . . .
H3 H 0.302(2) 0.361(3) 0.432(3) 0.107 Uiso 1 1 d D U . . .
N4 N 0.47457(16) 0.49476(18) 0.61950(15) 0.0811(7) Uani 1 1 d D . . . .
H4 H 0.450(3) 0.499(4) 0.585(2) 0.122 Uiso 1 1 d D U . . .
N5 N 0.53340(16) 0.51375(17) 0.62138(16) 0.0810(7) Uani 1 1 d . . . . .
N6 N 0.64513(18) 0.54986(19) 0.6478(2) 0.0899(8) Uani 1 1 d . . . . .
C1 C 0.2180(2) 0.3140(2) 0.18378(18) 0.0866(9) Uani 1 1 d . . . . .
H1A H 0.244070 0.285802 0.164435 0.104 Uiso 1 1 calc R U . . .
C2 C 0.1680(3) 0.3371(3) 0.1512(2) 0.1027(14) Uani 1 1 d . . . . .
H2A H 0.161000 0.325111 0.110546 0.123 Uiso 1 1 calc R U . . .
C3 C 0.1275(3) 0.3794(3) 0.1808(3) 0.1081(16) Uani 1 1 d . . . . .
H3B H 0.092931 0.394826 0.160426 0.130 Uiso 1 1 calc R U . . .
C4 C 0.1407(3) 0.3968(3) 0.2400(3) 0.1029(14) Uani 1 1 d . . . . .
H4B H 0.115596 0.425227 0.260304 0.124 Uiso 1 1 calc R U . . .
C5 C 0.19169(17) 0.37199(18) 0.26969(17) 0.0778(7) Uani 1 1 d . . . . .
C6 C 0.20835(16) 0.38485(17) 0.33407(17) 0.0755(7) Uani 1 1 d . . . . .
C7 C 0.18035(17) 0.4185(2) 0.3810(2) 0.0814(8) Uani 1 1 d . . . . .
H7A H 0.143821 0.441029 0.378819 0.098 Uiso 1 1 calc R U . . .
C8 C 0.21851(16) 0.41114(18) 0.43155(18) 0.0763(7) Uani 1 1 d . . . . .
C9 C 0.21232(16) 0.43569(19) 0.49435(19) 0.0803(8) Uani 1 1 d . . . . .
C10 C 0.1643(2) 0.4770(3) 0.5065(3) 0.0975(12) Uani 1 1 d . . . . .
H10A H 0.138039 0.489295 0.474706 0.117 Uiso 1 1 calc R U . . .
C11 C 0.1556(3) 0.4994(4) 0.5649(3) 0.1155(18) Uani 1 1 d . . . . .
H11A H 0.122896 0.526100 0.572914 0.139 Uiso 1 1 calc R U . . .
C12 C 0.1952(3) 0.4826(4) 0.6120(3) 0.1163(18) Uani 1 1 d . . . . .
H12A H 0.189146 0.498313 0.651587 0.140 Uiso 1 1 calc R U . . .
C13 C 0.2439(2) 0.4424(3) 0.6007(2) 0.0946(11) Uani 1 1 d . . . . .
C14 C 0.25194(17) 0.4193(2) 0.54092(19) 0.0843(9) Uani 1 1 d . . . . .
H14A H 0.284552 0.392581 0.532659 0.101 Uiso 1 1 calc R U . . .
C15 C 0.2904(2) 0.4304(3) 0.64865(19) 0.0977(13) Uani 1 1 d . . . . .
C16 C 0.2742(3) 0.4076(5) 0.7069(3) 0.143(3) Uani 1 1 d . . . . .
H16A H 0.233348 0.397960 0.716149 0.171 Uiso 1 1 calc R U . . .
C17 C 0.3208(4) 0.3996(6) 0.7508(3) 0.154(4) Uani 1 1 d . . . . .
H17A H 0.310670 0.384171 0.789689 0.185 Uiso 1 1 calc R U . . .
C18 C 0.3809(4) 0.4140(5) 0.7379(2) 0.126(2) Uani 1 1 d . . . . .
H18A H 0.410951 0.408156 0.768046 0.151 Uiso 1 1 calc R U . . .
C19 C 0.3983(2) 0.4374(3) 0.67950(19) 0.0922(10) Uani 1 1 d . . . . .
C20 C 0.3522(2) 0.4442(2) 0.63639(17) 0.0872(9) Uani 1 1 d . . . . .
H20A H 0.362672 0.458540 0.597252 0.105 Uiso 1 1 calc R U . . .
C21 C 0.4610(2) 0.4593(2) 0.66856(18) 0.0839(9) Uani 1 1 d . . . . .
C22 C 0.5125(2) 0.4560(2) 0.7049(2) 0.0911(10) Uani 1 1 d . . . . .
H22A H 0.516682 0.435240 0.742336 0.109 Uiso 1 1 calc R U . . .
C23 C 0.55714(19) 0.4902(2) 0.6741(2) 0.0831(8) Uani 1 1 d . . . . .
C24 C 0.6207(2) 0.5072(2) 0.6884(2) 0.0894(10) Uani 1 1 d . . . . .
C25 C 0.6539(3) 0.4829(3) 0.7361(3) 0.1143(17) Uani 1 1 d . . . . .
H25A H 0.635898 0.454433 0.762769 0.137 Uiso 1 1 calc R U . . .
C26 C 0.7137(4) 0.5007(4) 0.7446(5) 0.144(3) Uani 1 1 d . . . . .
H26A H 0.737311 0.482924 0.775748 0.173 Uiso 1 1 calc R U . . .
C27 C 0.7382(4) 0.5439(5) 0.7077(6) 0.151(3) Uani 1 1 d . . . . .
H27A H 0.778116 0.558179 0.714821 0.181 Uiso 1 1 calc R U . . .
C28 C 0.7038(3) 0.5673(3) 0.6585(4) 0.1115(15) Uani 1 1 d . . . . .
H28A H 0.722036 0.596059 0.632239 0.134 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43988(2) 0.43988(2) 0.43988(2) 0.0717(2) Uani 1 3 d S T P . .
O1 O 0.38819(11) 0.36977(12) 0.47185(12) 0.0729(5) Uani 1 1 d . . . . .
O2 O 0.49859(11) 0.40779(13) 0.50264(13) 0.0760(6) Uani 1 1 d . . . . .
O3 O 0.5204(2) 0.2404(3) 0.6389(3) 0.148(2) Uani 1 1 d . U . . .
O4 O 0.4039(3) 0.2054(3) 0.6122(3) 0.146(2) Uani 1 1 d . U . . .
C29 C 0.41492(16) 0.33779(17) 0.51524(15) 0.0722(6) Uani 1 1 d . . . . .
C30 C 0.47931(16) 0.35840(18) 0.53174(16) 0.0745(7) Uani 1 1 d . . . . .
C31 C 0.5143(2) 0.3266(2) 0.5732(2) 0.0920(11) Uani 1 1 d . . . . .
H31A H 0.553528 0.340836 0.583516 0.110 Uiso 1 1 calc R U . . .
C32 C 0.4910(3) 0.2710(3) 0.6009(2) 0.1032(14) Uani 1 1 d . U . . .
C33 C 0.4244(2) 0.2513(3) 0.5866(2) 0.0972(12) Uani 1 1 d . U . . .
C34 C 0.38897(18) 0.2881(2) 0.54329(19) 0.0840(9) Uani 1 1 d . . . . .
H34A H 0.348192 0.277544 0.534677 0.101 Uiso 1 1 calc R U . . .
O1S O 0.0205(15) 0.4025(16) 0.3520(16) 0.408(14) Uiso 1 1 d D . . . .
H1S H 0.026639 0.367388 0.339009 0.613 Uiso 1 1 d R U . . .
C1S C -0.049(2) 0.411(3) 0.366(3) 0.48(3) Uiso 1 1 d D . . . .
H1S1 H -0.056369 0.407057 0.409115 0.713 Uiso 1 1 d R U . . .
H1S2 H -0.072189 0.380377 0.343625 0.713 Uiso 1 1 d R U . . .
H1S3 H -0.061759 0.451567 0.352195 0.713 Uiso 1 1 d R U . . .
B1 B 0.1367(11) 0.1435(12) 0.1462(11) 0.444(10) Uani 0.3333 1 d D U P A -1
F1 F 0.1310(10) 0.1861(11) 0.0990(9) 0.511(12) Uani 1 1 d D U . A -1
F2 F 0.1728(18) 0.1673(18) 0.1934(13) 0.441(15) Uani 0.3333 1 d D U P A -1
F3 F 0.0781(8) 0.1297(11) 0.1674(10) 0.475(11) Uani 1 1 d D U . A -1
F4 F 0.1631(11) 0.0896(11) 0.1233(10) 0.524(12) Uani 1 1 d D U . A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.962(3) 9 ?
Fe1 N2 1.962(3) 5 ?
Fe1 N2 1.962(3) . ?
Fe1 N1 2.007(3) . ?
Fe1 N1 2.007(3) 9 ?
Fe1 N1 2.007(3) 5 ?
Fe2 N5 2.030(4) . ?
Fe2 N5 2.030(4) 9 ?
Fe2 N5 2.030(4) 5 ?
Fe2 N6 2.060(4) 9 ?
Fe2 N6 2.060(4) 5 ?
Fe2 N6 2.060(4) . ?
N1 C1 1.344(5) . ?
N1 C5 1.357(5) . ?
N2 C6 1.338(4) . ?
N2 N3 1.342(4) . ?
N3 C8 1.364(4) . ?
N3 H3 0.92(3) . ?
N4 N5 1.338(5) . ?
N4 C21 1.342(5) . ?
N4 H4 0.91(3) . ?
N5 C23 1.350(5) . ?
N6 C28 1.345(7) . ?
N6 C24 1.380(7) . ?
C1 C2 1.385(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.419(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.366(7) . ?
C3 H3B 0.9300 . ?
C4 C5 1.385(6) . ?
C4 H4B 0.9300 . ?
C5 C6 1.465(5) . ?
C6 C7 1.388(5) . ?
C7 C8 1.379(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.465(5) . ?
C9 C14 1.369(6) . ?
C9 C10 1.396(6) . ?
C10 C11 1.366(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.380(11) . ?
C11 H11A 0.9300 . ?
C12 C13 1.388(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.398(6) . ?
C13 C15 1.468(7) . ?
C14 H14A 0.9300 . ?
C15 C20 1.396(6) . ?
C15 C16 1.397(7) . ?
C16 C17 1.396(12) . ?
C16 H16A 0.9300 . ?
C17 C18 1.367(11) . ?
C17 H17A 0.9300 . ?
C18 C19 1.412(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.372(7) . ?
C19 C21 1.457(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.365(7) . ?
C22 C23 1.388(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.456(6) . ?
C24 C25 1.364(7) . ?
C25 C26 1.360(10) . ?
C25 H25A 0.9300 . ?
C26 C27 1.338(14) . ?
C26 H26A 0.9300 . ?
C27 C28 1.394(10) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.984(3) 5 ?
Fe3 O2 1.985(3) 9 ?
Fe3 O2 1.985(3) . ?
Fe3 O1 2.007(2) . ?
Fe3 O1 2.007(2) 5 ?
Fe3 O1 2.007(2) 9 ?
O1 C29 1.302(4) . ?
O2 C30 1.308(5) . ?
O3 C32 1.231(6) . ?
O4 C33 1.222(6) . ?
C29 C34 1.356(5) . ?
C29 C30 1.506(5) . ?
C30 C31 1.361(5) . ?
C31 C32 1.435(7) . ?
C31 H31A 0.9300 . ?
C32 C33 1.534(7) . ?
C33 C34 1.448(6) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.54(3) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9599 . ?
C1S H1S2 0.9599 . ?
C1S H1S3 0.9600 . ?
B1 F1 1.38(2) . ?
B1 F3 1.38(2) . ?
B1 F2 1.38(2) . ?
B1 F4 1.39(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.02(11) 9 5 ?
N2 Fe1 N2 96.03(11) 9 . ?
N2 Fe1 N2 96.02(11) 5 . ?
N2 Fe1 N1 91.01(12) 9 . ?
N2 Fe1 N1 172.43(12) 5 . ?
N2 Fe1 N1 80.41(12) . . ?
N2 Fe1 N1 80.41(12) 9 9 ?
N2 Fe1 N1 91.01(12) 5 9 ?
N2 Fe1 N1 172.43(12) . 9 ?
N1 Fe1 N1 92.92(13) . 9 ?
N2 Fe1 N1 172.43(12) 9 5 ?
N2 Fe1 N1 80.41(12) 5 5 ?
N2 Fe1 N1 91.01(12) . 5 ?
N1 Fe1 N1 92.92(13) . 5 ?
N1 Fe1 N1 92.92(13) 9 5 ?
N5 Fe2 N5 96.85(14) . 9 ?
N5 Fe2 N5 96.85(13) . 5 ?
N5 Fe2 N5 96.85(13) 9 5 ?
N5 Fe2 N6 92.98(15) . 9 ?
N5 Fe2 N6 79.06(15) 9 9 ?
N5 Fe2 N6 169.76(15) 5 9 ?
N5 Fe2 N6 169.76(15) . 5 ?
N5 Fe2 N6 92.98(15) 9 5 ?
N5 Fe2 N6 79.06(15) 5 5 ?
N6 Fe2 N6 91.70(16) 9 5 ?
N5 Fe2 N6 79.07(15) . . ?
N5 Fe2 N6 169.76(15) 9 . ?
N5 Fe2 N6 92.98(15) 5 . ?
N6 Fe2 N6 91.70(16) 9 . ?
N6 Fe2 N6 91.70(16) 5 . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Fe1 126.9(3) . . ?
C5 N1 Fe1 115.1(2) . . ?
C6 N2 N3 105.5(3) . . ?
C6 N2 Fe1 115.8(2) . . ?
N3 N2 Fe1 137.4(2) . . ?
N2 N3 C8 111.3(3) . . ?
N2 N3 H3 114(4) . . ?
C8 N3 H3 134(4) . . ?
N5 N4 C21 111.1(4) . . ?
N5 N4 H4 123(5) . . ?
C21 N4 H4 125(5) . . ?
N4 N5 C23 105.8(3) . . ?
N4 N5 Fe2 136.3(3) . . ?
C23 N5 Fe2 114.7(3) . . ?
C28 N6 C24 116.1(4) . . ?
C28 N6 Fe2 128.9(4) . . ?
C24 N6 Fe2 114.7(3) . . ?
N1 C1 C2 122.4(4) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C1 C2 C3 119.1(4) . . ?
C1 C2 H2A 120.5 . . ?
C3 C2 H2A 120.5 . . ?
C4 C3 C2 118.2(4) . . ?
C4 C3 H3B 120.9 . . ?
C2 C3 H3B 120.9 . . ?
C3 C4 C5 119.6(5) . . ?
C3 C4 H4B 120.2 . . ?
C5 C4 H4B 120.2 . . ?
N1 C5 C4 122.9(4) . . ?
N1 C5 C6 112.8(3) . . ?
C4 C5 C6 124.2(4) . . ?
N2 C6 C7 111.4(3) . . ?
N2 C6 C5 115.1(3) . . ?
C7 C6 C5 133.4(3) . . ?
C8 C7 C6 105.0(3) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 106.8(3) . . ?
N3 C8 C9 123.5(3) . . ?
C7 C8 C9 129.7(3) . . ?
C14 C9 C10 119.6(4) . . ?
C14 C9 C8 122.1(3) . . ?
C10 C9 C8 118.3(4) . . ?
C11 C10 C9 120.2(6) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 120.4(5) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C11 C12 C13 120.4(5) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C12 C13 C14 118.7(5) . . ?
C12 C13 C15 120.5(5) . . ?
C14 C13 C15 120.3(4) . . ?
C9 C14 C13 120.7(4) . . ?
C9 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C20 C15 C16 119.1(5) . . ?
C20 C15 C13 119.0(4) . . ?
C16 C15 C13 121.9(5) . . ?
C17 C16 C15 118.5(5) . . ?
C17 C16 H16A 120.7 . . ?
C15 C16 H16A 120.7 . . ?
C18 C17 C16 121.2(5) . . ?
C18 C17 H17A 119.4 . . ?
C16 C17 H17A 119.4 . . ?
C17 C18 C19 121.3(6) . . ?
C17 C18 H18A 119.4 . . ?
C19 C18 H18A 119.4 . . ?
C20 C19 C18 116.9(5) . . ?
C20 C19 C21 122.1(4) . . ?
C18 C19 C21 120.7(5) . . ?
C19 C20 C15 122.9(4) . . ?
C19 C20 H20A 118.5 . . ?
C15 C20 H20A 118.5 . . ?
N4 C21 C22 107.9(4) . . ?
N4 C21 C19 121.2(4) . . ?
C22 C21 C19 130.5(4) . . ?
C21 C22 C23 105.2(4) . . ?
C21 C22 H22A 127.4 . . ?
C23 C22 H22A 127.4 . . ?
N5 C23 C22 110.0(4) . . ?
N5 C23 C24 116.3(4) . . ?
C22 C23 C24 133.6(4) . . ?
C25 C24 N6 122.5(5) . . ?
C25 C24 C23 124.2(5) . . ?
N6 C24 C23 113.3(4) . . ?
C26 C25 C24 119.6(7) . . ?
C26 C25 H25A 120.2 . . ?
C24 C25 H25A 120.2 . . ?
C27 C26 C25 119.6(6) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 119.8(7) . . ?
C26 C27 H27A 120.1 . . ?
C28 C27 H27A 120.1 . . ?
N6 C28 C27 122.2(7) . . ?
N6 C28 H28A 118.9 . . ?
C27 C28 H28A 118.9 . . ?
O2 Fe3 O2 91.46(12) 5 9 ?
O2 Fe3 O2 91.46(12) 5 . ?
O2 Fe3 O2 91.46(12) 9 . ?
O2 Fe3 O1 170.14(10) 5 . ?
O2 Fe3 O1 95.83(11) 9 . ?
O2 Fe3 O1 81.75(10) . . ?
O2 Fe3 O1 81.75(10) 5 5 ?
O2 Fe3 O1 170.14(10) 9 5 ?
O2 Fe3 O1 95.83(11) . 5 ?
O1 Fe3 O1 91.79(11) . 5 ?
O2 Fe3 O1 95.83(11) 5 9 ?
O2 Fe3 O1 81.75(10) 9 9 ?
O2 Fe3 O1 170.14(10) . 9 ?
O1 Fe3 O1 91.79(11) . 9 ?
O1 Fe3 O1 91.79(11) 5 9 ?
C29 O1 Fe3 113.7(2) . . ?
C30 O2 Fe3 114.3(2) . . ?
O1 C29 C34 124.1(3) . . ?
O1 C29 C30 115.1(3) . . ?
C34 C29 C30 120.8(3) . . ?
O2 C30 C31 123.6(3) . . ?
O2 C30 C29 115.0(3) . . ?
C31 C30 C29 121.4(4) . . ?
C30 C31 C32 120.3(4) . . ?
C30 C31 H31A 119.9 . . ?
C32 C31 H31A 119.9 . . ?
O3 C32 C31 123.2(5) . . ?
O3 C32 C33 118.1(5) . . ?
C31 C32 C33 118.6(4) . . ?
O4 C33 C34 123.2(5) . . ?
O4 C33 C32 118.4(4) . . ?
C34 C33 C32 118.4(4) . . ?
C29 C34 C33 120.3(4) . . ?
C29 C34 H34A 119.8 . . ?
C33 C34 H34A 119.8 . . ?
C1S O1S H1S 109.7 . . ?
O1S C1S H1S1 109.7 . . ?
O1S C1S H1S2 109.2 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F1 B1 F3 107.9(17) . . ?
F1 B1 F2 110.4(18) . . ?
F3 B1 F2 110.7(18) . . ?
F1 B1 F4 109.4(17) . . ?
F3 B1 F4 108.3(18) . . ?
F2 B1 F4 110.1(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.92(3) 2.06(4) 2.934(4) 157(6) . yes
N4 H4 O2 0.91(3) 2.09(3) 2.993(4) 170(7) 9 yes

_refine_diff_density_max         0.646
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.119

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_320K
_database_code_depnum_ccdc_archive 'CCDC 2261723'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 3(C H4 O)'
_chemical_formula_sum            'C105 H78 B F4 Fe3 N18 O15'
_chemical_formula_weight         2086.21

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.578(3)
_cell_length_b                   21.578(3)
_cell_length_c                   21.578(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10047(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    320(2)
_cell_measurement_reflns_used    6501
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.83

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             4292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.542
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      320(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            162392
_diffrn_reflns_av_unetI/netI     0.0186
_diffrn_reflns_av_R_equivalents  0.0433
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.369
_diffrn_reflns_theta_max         29.519
_diffrn_reflns_theta_full        29.519
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8663
_reflns_number_gt                8402
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule also was refined with displacement
 parameters restraints and a distance restraint.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0801P)²+0.1743P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0131(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3793 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.083(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8663
_refine_ls_number_parameters     478
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0356
_refine_ls_wR_factor_ref         0.1024
_refine_ls_wR_factor_gt          0.1016
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.068
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45325(2) 0.45325(2) 0.45325(2) 0.05591(12) Uani 1 3 d S T P . .
Fe2 Fe 0.16493(2) 0.16493(2) 0.16493(2) 0.06185(13) Uani 1 3 d S T P . .
N1 N 0.50704(8) 0.41994(8) 0.52204(9) 0.0636(4) Uani 1 1 d . . . . .
N2 N 0.39564(8) 0.39295(8) 0.49004(8) 0.0594(3) Uani 1 1 d . . . . .
N3 N 0.33568(8) 0.37713(8) 0.48358(8) 0.0602(3) Uani 1 1 d D . . . .
H3 H 0.3156(16) 0.3814(18) 0.4483(13) 0.090 Uiso 1 1 d D U . . .
N4 N 0.12824(9) 0.25607(11) 0.27365(9) 0.0698(4) Uani 1 1 d D . . . .
H4 H 0.1639(15) 0.2462(19) 0.2936(19) 0.105 Uiso 1 1 d D U . . .
N5 N 0.12609(9) 0.23615(10) 0.21459(9) 0.0681(4) Uani 1 1 d . . . . .
N6 N 0.09816(11) 0.19936(11) 0.10303(10) 0.0762(5) Uani 1 1 d . . . . .
C1 C 0.56582(11) 0.43610(12) 0.53493(13) 0.0751(5) Uani 1 1 d . . . . .
H1A H 0.586467 0.462999 0.508327 0.090 Uiso 1 1 calc R U . . .
C2 C 0.59650(14) 0.41380(15) 0.58674(16) 0.0883(7) Uani 1 1 d . . . . .
H2A H 0.636810 0.426519 0.595177 0.106 Uiso 1 1 calc R U . . .
C3 C 0.56708(16) 0.37276(17) 0.62563(17) 0.0957(9) Uani 1 1 d . . . . .
H3A H 0.587354 0.357186 0.660327 0.115 Uiso 1 1 calc R U . . .
C4 C 0.50681(14) 0.35493(15) 0.61242(15) 0.0860(7) Uani 1 1 d . . . . .
H4A H 0.485969 0.327046 0.637829 0.103 Uiso 1 1 calc R U . . .
C5 C 0.47837(10) 0.37967(11) 0.56044(10) 0.0664(4) Uani 1 1 d . . . . .
C6 C 0.41454(10) 0.36659(10) 0.54288(10) 0.0642(4) Uani 1 1 d . . . . .
C7 C 0.36670(11) 0.33362(12) 0.57048(10) 0.0696(5) Uani 1 1 d . . . . .
H7A H 0.368070 0.311511 0.607448 0.084 Uiso 1 1 calc R U . . .
C8 C 0.31686(10) 0.34066(10) 0.53144(9) 0.0634(4) Uani 1 1 d . . . . .
C9 C 0.20666(10) 0.33310(13) 0.49676(10) 0.0709(5) Uani 1 1 d . . . . .
H9A H 0.215241 0.360208 0.464372 0.085 Uiso 1 1 calc R U . . .
C10 C 0.25359(10) 0.31579(11) 0.53687(9) 0.0666(4) Uani 1 1 d . . . . .
C11 C 0.24091(14) 0.27498(15) 0.58515(12) 0.0813(6) Uani 1 1 d . . . . .
H11A H 0.272161 0.263039 0.612324 0.098 Uiso 1 1 calc R U . . .
C12 C 0.18093(17) 0.2522(2) 0.59241(16) 0.1004(10) Uani 1 1 d . . . . .
H12A H 0.172331 0.224356 0.624193 0.120 Uiso 1 1 calc R U . . .
C13 C 0.13501(15) 0.2702(2) 0.55350(15) 0.0984(10) Uani 1 1 d . . . . .
H13A H 0.094988 0.255455 0.559737 0.118 Uiso 1 1 calc R U . . .
C14 C 0.14669(11) 0.31040(15) 0.50434(11) 0.0771(6) Uani 1 1 d . . . . .
C15 C 0.11118(10) 0.30826(13) 0.39612(11) 0.0730(5) Uani 1 1 d . . . . .
H15A H 0.150251 0.293412 0.385602 0.088 Uiso 1 1 calc R U . . .
C16 C 0.09870(11) 0.32319(16) 0.45773(13) 0.0837(7) Uani 1 1 d . . . . .
C17 C 0.04011(15) 0.3455(3) 0.47295(18) 0.1187(15) Uani 1 1 d . . . . .
H17A H 0.030529 0.354774 0.513937 0.142 Uiso 1 1 calc R U . . .
C18 C -0.00364(16) 0.3539(3) 0.4273(2) 0.1348(19) Uani 1 1 d . . . . .
H18A H -0.042219 0.370123 0.437535 0.162 Uiso 1 1 calc R U . . .
C19 C 0.00898(14) 0.3385(2) 0.36633(19) 0.1127(13) Uani 1 1 d . . . . .
H19A H -0.021226 0.343796 0.336053 0.135 Uiso 1 1 calc R U . . .
C20 C 0.06699(11) 0.31498(15) 0.35033(13) 0.0784(6) Uani 1 1 d . . . . .
C21 C 0.07794(10) 0.29138(12) 0.28763(11) 0.0701(5) Uani 1 1 d . . . . .
C22 C 0.04177(12) 0.29397(13) 0.23479(12) 0.0760(5) Uani 1 1 d . . . . .
H22A H 0.004379 0.314784 0.229677 0.091 Uiso 1 1 calc R U . . .
C23 C 0.07301(11) 0.25905(11) 0.19126(11) 0.0698(5) Uani 1 1 d . . . . .
C24 C 0.05831(13) 0.24101(12) 0.12740(12) 0.0751(5) Uani 1 1 d . . . . .
C25 C 0.00818(19) 0.26422(19) 0.09557(17) 0.1007(10) Uani 1 1 d . . . . .
H25A H -0.018721 0.292242 0.114232 0.121 Uiso 1 1 calc R U . . .
C26 C -0.0013(2) 0.2451(2) 0.03557(19) 0.1219(14) Uani 1 1 d . . . . .
H26A H -0.034559 0.260341 0.012890 0.146 Uiso 1 1 calc R U . . .
C27 C 0.0391(3) 0.2029(2) 0.00920(18) 0.1262(15) Uani 1 1 d . . . . .
H27A H 0.033315 0.189400 -0.031312 0.151 Uiso 1 1 calc R U . . .
C28 C 0.0882(2) 0.18126(18) 0.04411(14) 0.0998(9) Uani 1 1 d . . . . .
H28A H 0.115468 0.153059 0.026241 0.120 Uiso 1 1 calc R U . . .
Fe3 Fe 0.30925(2) 0.30925(2) 0.30925(2) 0.06120(13) Uani 1 3 d S T P . .
O1 O 0.27745(7) 0.38013(7) 0.36031(6) 0.0622(3) Uani 1 1 d . . . . .
O2 O 0.24668(8) 0.34113(8) 0.24915(7) 0.0656(3) Uani 1 1 d . . . . .
O3 O 0.11332(14) 0.51133(16) 0.22550(13) 0.1178(10) Uani 1 1 d . U . . .
O4 O 0.13949(15) 0.54721(15) 0.34164(14) 0.1211(10) Uani 1 1 d . U . . .
C29 C 0.23500(9) 0.41307(10) 0.33262(9) 0.0608(4) Uani 1 1 d . . . . .
C30 C 0.21852(10) 0.39165(10) 0.26813(9) 0.0628(4) Uani 1 1 d . . . . .
C31 C 0.17820(12) 0.42454(14) 0.23273(12) 0.0793(6) Uani 1 1 d . . . . .
H31A H 0.169145 0.410835 0.192881 0.095 Uiso 1 1 calc R U . . .
C32 C 0.14952(13) 0.47942(16) 0.25516(13) 0.0827(6) Uani 1 1 d . U . . .
C33 C 0.16465(13) 0.49972(14) 0.32234(13) 0.0814(6) Uani 1 1 d . U . . .
C34 C 0.20706(11) 0.46376(12) 0.35749(11) 0.0719(5) Uani 1 1 d . . . . .
H34A H 0.215862 0.475055 0.398137 0.086 Uiso 1 1 calc R U . . .
O1S O 0.3948(6) 0.3460(3) 0.7315(4) 0.231(3) Uani 1 1 d D U . . .
H1S H 0.388271 0.382401 0.740246 0.347 Uiso 1 1 calc R U . . .
C1S C 0.3836(6) 0.3083(6) 0.7845(6) 0.254(6) Uani 1 1 d D U . . .
H1S1 H 0.417384 0.312614 0.813140 0.382 Uiso 1 1 calc R U . . .
H1S2 H 0.380118 0.265752 0.771990 0.382 Uiso 1 1 calc R U . . .
H1S3 H 0.345797 0.321128 0.804143 0.382 Uiso 1 1 calc R U . . .
B1 B -0.1206(10) 0.3832(8) 0.1183(10) 0.125(3) Uani 0.3333 1 d D U P A -1
F1 F -0.0782(10) 0.3723(8) 0.1638(8) 0.158(7) Uani 0.3333 1 d D U P A -1
F2 F -0.1067(8) 0.4373(5) 0.0873(8) 0.191(6) Uani 0.3333 1 d D U P A -1
F3 F -0.1778(8) 0.3947(9) 0.1450(9) 0.182(7) Uani 0.3333 1 d D U P A -1
F4 F -0.1246(10) 0.3350(8) 0.0777(8) 0.173(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9670(17) 9 ?
Fe1 N2 1.9670(17) 5 ?
Fe1 N2 1.9670(18) . ?
Fe1 N1 2.0167(18) . ?
Fe1 N1 2.0167(18) 9 ?
Fe1 N1 2.0167(18) 5 ?
Fe2 N5 2.052(2) . ?
Fe2 N5 2.053(2) 5 ?
Fe2 N5 2.053(2) 9 ?
Fe2 N6 2.100(2) . ?
Fe2 N6 2.101(2) 9 ?
Fe2 N6 2.101(2) 5 ?
N1 C1 1.345(3) . ?
N1 C5 1.351(3) . ?
N2 C6 1.338(3) . ?
N2 N3 1.345(2) . ?
N3 C8 1.360(3) . ?
N3 H3 0.88(2) . ?
N4 N5 1.346(3) . ?
N4 C21 1.360(3) . ?
N4 H4 0.91(2) . ?
N5 C23 1.345(3) . ?
N6 C28 1.347(4) . ?
N6 C24 1.350(4) . ?
C1 C2 1.385(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.375(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.386(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.456(3) . ?
C6 C7 1.388(3) . ?
C7 C8 1.375(3) . ?
C7 H7A 0.9300 . ?
C8 C10 1.471(3) . ?
C9 C10 1.383(3) . ?
C9 C14 1.393(3) . ?
C9 H9A 0.9300 . ?
C10 C11 1.391(3) . ?
C11 C12 1.394(4) . ?
C11 H11A 0.9300 . ?
C12 C13 1.356(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.393(4) . ?
C13 H13A 0.9300 . ?
C14 C16 1.470(4) . ?
C15 C20 1.381(4) . ?
C15 C16 1.394(3) . ?
C15 H15A 0.9300 . ?
C16 C17 1.392(4) . ?
C17 C18 1.376(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.384(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.394(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.465(4) . ?
C21 C22 1.383(3) . ?
C22 C23 1.380(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.467(4) . ?
C24 C25 1.376(4) . ?
C25 C26 1.374(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.381(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.382(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9943(15) 9 ?
Fe3 O2 1.9944(15) 5 ?
Fe3 O2 1.9944(15) . ?
Fe3 O1 2.0060(15) 9 ?
Fe3 O1 2.0060(15) 5 ?
Fe3 O1 2.0060(15) . ?
O1 C29 1.304(2) . ?
O2 C30 1.313(3) . ?
O3 C32 1.222(4) . ?
O4 C33 1.232(3) . ?
C29 C34 1.359(3) . ?
C29 C30 1.509(3) . ?
C30 C31 1.358(3) . ?
C31 C32 1.421(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.549(4) . ?
C33 C34 1.419(3) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.424(11) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F4 1.36(2) . ?
B1 F1 1.363(18) . ?
B1 F2 1.380(14) . ?
B1 F3 1.385(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 95.96(7) 9 5 ?
N2 Fe1 N2 95.96(7) 9 . ?
N2 Fe1 N2 95.96(7) 5 . ?
N2 Fe1 N1 171.81(7) 9 . ?
N2 Fe1 N1 91.68(7) 5 . ?
N2 Fe1 N1 80.26(7) . . ?
N2 Fe1 N1 80.27(7) 9 9 ?
N2 Fe1 N1 171.81(7) 5 9 ?
N2 Fe1 N1 91.68(7) . 9 ?
N1 Fe1 N1 92.52(7) . 9 ?
N2 Fe1 N1 91.68(7) 9 5 ?
N2 Fe1 N1 80.27(7) 5 5 ?
N2 Fe1 N1 171.81(7) . 5 ?
N1 Fe1 N1 92.52(8) . 5 ?
N1 Fe1 N1 92.52(7) 9 5 ?
N5 Fe2 N5 97.35(7) . 5 ?
N5 Fe2 N5 97.35(7) . 9 ?
N5 Fe2 N5 97.35(7) 5 9 ?
N5 Fe2 N6 77.70(8) . . ?
N5 Fe2 N6 168.16(8) 5 . ?
N5 Fe2 N6 93.97(9) 9 . ?
N5 Fe2 N6 168.16(8) . 9 ?
N5 Fe2 N6 93.97(9) 5 9 ?
N5 Fe2 N6 77.71(8) 9 9 ?
N6 Fe2 N6 91.80(9) . 9 ?
N5 Fe2 N6 93.97(9) . 5 ?
N5 Fe2 N6 77.71(8) 5 5 ?
N5 Fe2 N6 168.16(8) 9 5 ?
N6 Fe2 N6 91.80(9) . 5 ?
N6 Fe2 N6 91.80(9) 9 5 ?
C1 N1 C5 118.2(2) . . ?
C1 N1 Fe1 127.06(17) . . ?
C5 N1 Fe1 114.66(14) . . ?
C6 N2 N3 105.88(16) . . ?
C6 N2 Fe1 115.63(14) . . ?
N3 N2 Fe1 137.21(13) . . ?
N2 N3 C8 110.80(17) . . ?
N2 N3 H3 122(3) . . ?
C8 N3 H3 125(3) . . ?
N5 N4 C21 111.19(19) . . ?
N5 N4 H4 114(3) . . ?
C21 N4 H4 135(3) . . ?
C23 N5 N4 105.5(2) . . ?
C23 N5 Fe2 115.30(17) . . ?
N4 N5 Fe2 136.01(16) . . ?
C28 N6 C24 117.3(3) . . ?
C28 N6 Fe2 127.4(2) . . ?
C24 N6 Fe2 115.12(17) . . ?
N1 C1 C2 121.8(3) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 119.7(3) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.1(3) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 C6 113.47(18) . . ?
C4 C5 C6 123.7(2) . . ?
N2 C6 C7 110.91(19) . . ?
N2 C6 C5 115.32(19) . . ?
C7 C6 C5 133.7(2) . . ?
C8 C7 C6 105.21(19) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.20(19) . . ?
N3 C8 C10 123.25(19) . . ?
C7 C8 C10 129.5(2) . . ?
C10 C9 C14 120.8(2) . . ?
C10 C9 H9A 119.6 . . ?
C14 C9 H9A 119.6 . . ?
C9 C10 C11 119.7(2) . . ?
C9 C10 C8 122.1(2) . . ?
C11 C10 C8 118.2(2) . . ?
C10 C11 C12 119.4(3) . . ?
C10 C11 H11A 120.3 . . ?
C12 C11 H11A 120.3 . . ?
C13 C12 C11 120.5(3) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C12 C13 C14 121.2(3) . . ?
C12 C13 H13A 119.4 . . ?
C14 C13 H13A 119.4 . . ?
C9 C14 C13 118.4(3) . . ?
C9 C14 C16 120.5(2) . . ?
C13 C14 C16 120.7(3) . . ?
C20 C15 C16 121.6(2) . . ?
C20 C15 H15A 119.2 . . ?
C16 C15 H15A 119.2 . . ?
C17 C16 C15 118.7(3) . . ?
C17 C16 C14 122.9(3) . . ?
C15 C16 C14 118.2(2) . . ?
C18 C17 C16 119.9(3) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C17 C18 C19 120.9(3) . . ?
C17 C18 H18A 119.5 . . ?
C19 C18 H18A 119.5 . . ?
C18 C19 C20 120.0(3) . . ?
C18 C19 H19A 120.0 . . ?
C20 C19 H19A 120.0 . . ?
C15 C20 C19 118.8(3) . . ?
C15 C20 C21 120.9(2) . . ?
C19 C20 C21 120.0(3) . . ?
N4 C21 C22 106.9(2) . . ?
N4 C21 C20 121.9(2) . . ?
C22 C21 C20 131.0(2) . . ?
C23 C22 C21 105.3(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.2(2) . . ?
N5 C23 C24 116.0(2) . . ?
C22 C23 C24 132.8(2) . . ?
N6 C24 C25 123.3(3) . . ?
N6 C24 C23 113.9(2) . . ?
C25 C24 C23 122.9(3) . . ?
C26 C25 C24 118.5(4) . . ?
C26 C25 H25A 120.7 . . ?
C24 C25 H25A 120.7 . . ?
C25 C26 C27 119.5(3) . . ?
C25 C26 H26A 120.2 . . ?
C27 C26 H26A 120.2 . . ?
C26 C27 C28 118.8(3) . . ?
C26 C27 H27A 120.6 . . ?
C28 C27 H27A 120.6 . . ?
N6 C28 C27 122.6(4) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 91.02(7) 9 5 ?
O2 Fe3 O2 91.02(7) 9 . ?
O2 Fe3 O2 91.01(7) 5 . ?
O2 Fe3 O1 82.10(6) 9 9 ?
O2 Fe3 O1 170.25(6) 5 9 ?
O2 Fe3 O1 95.98(7) . 9 ?
O2 Fe3 O1 95.98(7) 9 5 ?
O2 Fe3 O1 82.11(6) 5 5 ?
O2 Fe3 O1 170.25(6) . 5 ?
O1 Fe3 O1 91.71(6) 9 5 ?
O2 Fe3 O1 170.25(6) 9 . ?
O2 Fe3 O1 95.98(7) 5 . ?
O2 Fe3 O1 82.10(6) . . ?
O1 Fe3 O1 91.71(6) 9 . ?
O1 Fe3 O1 91.71(6) 5 . ?
C29 O1 Fe3 113.83(13) . . ?
C30 O2 Fe3 113.38(13) . . ?
O1 C29 C34 124.69(19) . . ?
O1 C29 C30 114.90(18) . . ?
C34 C29 C30 120.40(19) . . ?
O2 C30 C31 123.7(2) . . ?
O2 C30 C29 115.64(18) . . ?
C31 C30 C29 120.6(2) . . ?
C30 C31 C32 121.5(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.7(3) . . ?
O3 C32 C33 117.7(3) . . ?
C31 C32 C33 117.6(2) . . ?
O4 C33 C34 123.9(3) . . ?
O4 C33 C32 117.3(3) . . ?
C34 C33 C32 118.8(2) . . ?
C29 C34 C33 121.0(2) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F4 B1 F1 111.9(16) . . ?
F4 B1 F2 110.4(16) . . ?
F1 B1 F2 110.4(16) . . ?
F4 B1 F3 110.4(17) . . ?
F1 B1 F3 109.3(16) . . ?
F2 B1 F3 104.1(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(2) 2.07(2) 2.942(2) 171(4) . yes
N4 H4 O2 0.91(2) 2.11(3) 2.995(2) 166(4) 5 yes

_refine_diff_density_max         0.272
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.060

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_325K_
_database_code_depnum_ccdc_archive 'CCDC 2261724'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.445(C H4 O)'
_chemical_formula_sum            'C104.45 H75.78 B F4 Fe3 N18 O14.45'
_chemical_formula_weight         2068.42

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.573(3)
_cell_length_b                   21.573(3)
_cell_length_c                   21.573(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10040(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    325(2)
_cell_measurement_reflns_used    6522
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.95

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             4252
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.541
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      325(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            164664
_diffrn_reflns_av_unetI/netI     0.0236
_diffrn_reflns_av_R_equivalents  0.0598
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.370
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_full        29.507
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8650
_reflns_number_gt                8470
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.815 (i.e. 2.445 MeOH per formula unit).
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0690P)²+0.2097P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0224(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3847 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8650
_refine_ls_number_parameters     479
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0329
_refine_ls_wR_factor_ref         0.0934
_refine_ls_wR_factor_gt          0.0930
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29667(2) 0.29667(2) 0.29667(2) 0.05430(11) Uani 1 3 d S T P . .
Fe2 Fe 0.58529(2) 0.58529(2) 0.58529(2) 0.06021(12) Uani 1 3 d S T P . .
N1 N 0.22756(8) 0.32998(8) 0.24299(7) 0.0619(3) Uani 1 1 d . . . . .
N2 N 0.25991(7) 0.35687(8) 0.35447(7) 0.0578(3) Uani 1 1 d . . . . .
N3 N 0.26652(7) 0.37266(8) 0.41450(7) 0.0586(3) Uani 1 1 d D . . . .
H3 H 0.3026(12) 0.3669(16) 0.4341(15) 0.088 Uiso 1 1 d D U . . .
N4 N 0.47671(8) 0.49352(10) 0.62227(8) 0.0681(4) Uani 1 1 d D . . . .
H4 H 0.4553(17) 0.5028(18) 0.5876(14) 0.102 Uiso 1 1 d D U . . .
N5 N 0.53566(8) 0.51376(9) 0.62438(8) 0.0666(4) Uani 1 1 d . . . . .
N6 N 0.64745(9) 0.55084(10) 0.65252(10) 0.0742(4) Uani 1 1 d . . . . .
C1 C 0.21445(12) 0.31385(12) 0.18419(10) 0.0736(5) Uani 1 1 d . . . . .
H1A H 0.241039 0.287036 0.163401 0.088 Uiso 1 1 calc R U . . .
C2 C 0.16245(15) 0.33607(14) 0.15371(13) 0.0869(7) Uani 1 1 d . . . . .
H2A H 0.153830 0.323379 0.113424 0.104 Uiso 1 1 calc R U . . .
C3 C 0.12367(15) 0.37703(16) 0.18345(15) 0.0937(8) Uani 1 1 d . . . . .
H3B H 0.088881 0.392648 0.163341 0.112 Uiso 1 1 calc R U . . .
C4 C 0.13701(13) 0.39472(14) 0.24361(14) 0.0844(6) Uani 1 1 d . . . . .
H4B H 0.111582 0.422507 0.264579 0.101 Uiso 1 1 calc R U . . .
C5 C 0.18913(9) 0.37009(10) 0.27194(10) 0.0649(4) Uani 1 1 d . . . . .
C6 C 0.20690(9) 0.38309(9) 0.33576(9) 0.0625(4) Uani 1 1 d . . . . .
C7 C 0.17937(9) 0.41624(11) 0.38373(10) 0.0683(4) Uani 1 1 d . . . . .
H7A H 0.142435 0.438429 0.382435 0.082 Uiso 1 1 calc R U . . .
C8 C 0.21856(8) 0.40912(9) 0.43347(9) 0.0618(4) Uani 1 1 d . . . . .
C9 C 0.21321(9) 0.43397(10) 0.49677(9) 0.0648(4) Uani 1 1 d . . . . .
C10 C 0.16508(11) 0.47518(14) 0.50945(13) 0.0798(6) Uani 1 1 d . . . . .
H10A H 0.138108 0.487501 0.478164 0.096 Uiso 1 1 calc R U . . .
C11 C 0.15786(14) 0.49770(18) 0.56955(15) 0.0986(9) Uani 1 1 d . . . . .
H11A H 0.126051 0.525452 0.578297 0.118 Uiso 1 1 calc R U . . .
C12 C 0.19687(14) 0.47946(19) 0.61545(13) 0.0967(9) Uani 1 1 d . . . . .
H12A H 0.190686 0.494147 0.655504 0.116 Uiso 1 1 calc R U . . .
C13 C 0.24592(10) 0.43924(14) 0.60377(10) 0.0755(5) Uani 1 1 d . . . . .
C14 C 0.25347(9) 0.41650(12) 0.54373(10) 0.0692(4) Uani 1 1 d . . . . .
H14A H 0.285821 0.389345 0.535100 0.083 Uiso 1 1 calc R U . . .
C15 C 0.29260(12) 0.42632(15) 0.65165(10) 0.0816(6) Uani 1 1 d . . . . .
C16 C 0.27743(16) 0.4037(2) 0.71030(14) 0.1157(13) Uani 1 1 d . . . . .
H16A H 0.236413 0.394328 0.719692 0.139 Uiso 1 1 calc R U . . .
C17 C 0.3226(2) 0.3952(3) 0.75414(15) 0.1326(18) Uani 1 1 d . . . . .
H17A H 0.312187 0.378732 0.792596 0.159 Uiso 1 1 calc R U . . .
C18 C 0.38390(17) 0.4111(2) 0.74162(13) 0.1099(12) Uani 1 1 d . . . . .
H18A H 0.414152 0.405912 0.771900 0.132 Uiso 1 1 calc R U . . .
C19 C 0.39985(11) 0.43468(14) 0.68362(10) 0.0759(5) Uani 1 1 d . . . . .
C20 C 0.35420(10) 0.44131(12) 0.63940(9) 0.0715(5) Uani 1 1 d . . . . .
H20A H 0.364818 0.456192 0.600358 0.086 Uiso 1 1 calc R U . . .
C21 C 0.46266(10) 0.45831(11) 0.67253(9) 0.0680(4) Uani 1 1 d . . . . .
C22 C 0.51548(11) 0.45614(12) 0.70892(11) 0.0740(5) Uani 1 1 d . . . . .
H22A H 0.520564 0.435501 0.746423 0.089 Uiso 1 1 calc R U . . .
C23 C 0.55900(11) 0.49116(10) 0.67766(10) 0.0678(4) Uani 1 1 d . . . . .
C24 C 0.62268(11) 0.50929(11) 0.69234(12) 0.0730(5) Uani 1 1 d . . . . .
C25 C 0.65444(16) 0.48640(17) 0.74291(18) 0.0985(9) Uani 1 1 d . . . . .
H25A H 0.635650 0.458522 0.769894 0.118 Uiso 1 1 calc R U . . .
C26 C 0.71446(18) 0.5057(2) 0.7526(2) 0.1213(13) Uani 1 1 d . . . . .
H26A H 0.737039 0.490506 0.786095 0.146 Uiso 1 1 calc R U . . .
C27 C 0.74069(16) 0.5475(2) 0.7124(3) 0.1257(14) Uani 1 1 d . . . . .
H27A H 0.781109 0.561155 0.718530 0.151 Uiso 1 1 calc R U . . .
C28 C 0.70621(14) 0.56900(17) 0.66270(18) 0.0991(9) Uani 1 1 d . . . . .
H28A H 0.724343 0.597000 0.635403 0.119 Uiso 1 1 calc R U . . .
Fe3 Fe 0.44087(2) 0.44087(2) 0.44087(2) 0.05981(12) Uani 1 3 d S T P . .
O1 O 0.38995(6) 0.36986(7) 0.47262(7) 0.0607(3) Uani 1 1 d . . . . .
O2 O 0.50112(6) 0.40891(7) 0.50331(7) 0.0643(3) Uani 1 1 d . . . . .
O3 O 0.52541(12) 0.23856(15) 0.63653(13) 0.1160(9) Uani 1 1 d . U . . .
O4 O 0.40927(13) 0.20234(14) 0.61034(13) 0.1173(9) Uani 1 1 d . U . . .
C29 C 0.41784(8) 0.33686(9) 0.51502(8) 0.0593(3) Uani 1 1 d . . . . .
C30 C 0.48239(9) 0.35831(9) 0.53140(9) 0.0614(4) Uani 1 1 d . . . . .
C31 C 0.51783(11) 0.32542(13) 0.57161(11) 0.0774(6) Uani 1 1 d . . . . .
H31A H 0.557691 0.339166 0.580598 0.093 Uiso 1 1 calc R U . . .
C32 C 0.49552(12) 0.27044(14) 0.60036(12) 0.0811(6) Uani 1 1 d . U . . .
C33 C 0.42825(12) 0.24991(13) 0.58519(12) 0.0801(6) Uani 1 1 d . U . . .
C34 C 0.39299(10) 0.28603(11) 0.54282(10) 0.0701(5) Uani 1 1 d . . . . .
H34A H 0.352332 0.274735 0.533985 0.084 Uiso 1 1 calc R U . . .
O1S O 0.0183(3) 0.4045(3) 0.3559(5) 0.193(3) Uani 0.815(12) 1 d D U P . .
H1S H 0.009543 0.368215 0.362750 0.289 Uiso 0.815(12) 1 calc R U P . .
C1S C -0.0327(5) 0.4413(5) 0.3670(6) 0.203(5) Uani 0.815(12) 1 d D U P . .
H1S1 H -0.050191 0.430805 0.406522 0.304 Uiso 0.815(12) 1 calc R U P . .
H1S2 H -0.063019 0.434553 0.335093 0.304 Uiso 0.815(12) 1 calc R U P . .
H1S3 H -0.020461 0.484057 0.367013 0.304 Uiso 0.815(12) 1 calc R U P . .
B1 B 0.1289(10) 0.1312(9) 0.1330(8) 0.126(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1245(10) 0.1716(8) 0.0845(8) 0.177(7) Uani 0.3333 1 d D U P A -1
F2 F 0.1442(8) 0.1624(8) 0.1865(5) 0.190(5) Uani 0.3333 1 d D U P A -1
F3 F 0.0712(8) 0.1049(8) 0.1444(8) 0.179(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1710(10) 0.0853(7) 0.1221(8) 0.158(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9674(16) . ?
Fe1 N2 1.9674(16) 5 ?
Fe1 N2 1.9674(16) 9 ?
Fe1 N1 2.0198(16) 5 ?
Fe1 N1 2.0198(16) 9 ?
Fe1 N1 2.0198(16) . ?
Fe2 N5 2.059(2) 9 ?
Fe2 N5 2.059(2) 5 ?
Fe2 N5 2.059(2) . ?
Fe2 N6 2.110(2) . ?
Fe2 N6 2.110(2) 9 ?
Fe2 N6 2.110(2) 5 ?
N1 C1 1.346(3) . ?
N1 C5 1.351(3) . ?
N2 C6 1.338(2) . ?
N2 N3 1.347(2) . ?
N3 C8 1.363(2) . ?
N3 H3 0.89(2) . ?
N4 N5 1.345(3) . ?
N4 C21 1.358(3) . ?
N4 H4 0.90(2) . ?
N5 C23 1.346(3) . ?
N6 C28 1.345(3) . ?
N6 C24 1.352(3) . ?
C1 C2 1.386(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.376(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.383(4) . ?
C3 H3B 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.456(3) . ?
C6 C7 1.391(3) . ?
C7 C8 1.375(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.471(3) . ?
C9 C14 1.387(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.393(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.391(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.395(3) . ?
C13 C15 1.469(4) . ?
C14 H14A 0.9300 . ?
C15 C20 1.393(3) . ?
C15 C16 1.395(3) . ?
C16 C17 1.370(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.393(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.394(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.378(3) . ?
C19 C21 1.467(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.384(3) . ?
C22 C23 1.381(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.463(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.376(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.373(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.386(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9948(14) 9 ?
Fe3 O2 1.9948(14) . ?
Fe3 O2 1.9948(14) 5 ?
Fe3 O1 2.0056(14) 9 ?
Fe3 O1 2.0056(14) 5 ?
Fe3 O1 2.0056(14) . ?
O1 C29 1.306(2) . ?
O2 C30 1.312(2) . ?
O3 C32 1.224(3) . ?
O4 C33 1.231(3) . ?
C29 C34 1.360(3) . ?
C29 C30 1.509(3) . ?
C30 C31 1.357(3) . ?
C31 C32 1.423(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.552(4) . ?
C33 C34 1.422(3) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.377(10) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F4 1.364(18) . ?
B1 F1 1.364(19) . ?
B1 F2 1.377(13) . ?
B1 F3 1.390(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 95.91(6) . 5 ?
N2 Fe1 N2 95.91(6) . 9 ?
N2 Fe1 N2 95.91(6) 5 9 ?
N2 Fe1 N1 91.76(7) . 5 ?
N2 Fe1 N1 80.27(7) 5 5 ?
N2 Fe1 N1 171.76(7) 9 5 ?
N2 Fe1 N1 171.76(7) . 9 ?
N2 Fe1 N1 91.77(7) 5 9 ?
N2 Fe1 N1 80.27(7) 9 9 ?
N1 Fe1 N1 92.49(7) 5 9 ?
N2 Fe1 N1 80.27(7) . . ?
N2 Fe1 N1 171.76(7) 5 . ?
N2 Fe1 N1 91.77(7) 9 . ?
N1 Fe1 N1 92.49(7) 5 . ?
N1 Fe1 N1 92.49(7) 9 . ?
N5 Fe2 N5 97.49(7) 9 5 ?
N5 Fe2 N5 97.49(7) 9 . ?
N5 Fe2 N5 97.48(7) 5 . ?
N5 Fe2 N6 167.92(8) 9 . ?
N5 Fe2 N6 94.11(8) 5 . ?
N5 Fe2 N6 77.59(7) . . ?
N5 Fe2 N6 77.59(7) 9 9 ?
N5 Fe2 N6 167.92(8) 5 9 ?
N5 Fe2 N6 94.11(8) . 9 ?
N6 Fe2 N6 91.66(8) . 9 ?
N5 Fe2 N6 94.11(8) 9 5 ?
N5 Fe2 N6 77.59(7) 5 5 ?
N5 Fe2 N6 167.92(8) . 5 ?
N6 Fe2 N6 91.67(8) . 5 ?
N6 Fe2 N6 91.66(8) 9 5 ?
C1 N1 C5 118.18(18) . . ?
C1 N1 Fe1 127.14(16) . . ?
C5 N1 Fe1 114.57(13) . . ?
C6 N2 N3 105.88(15) . . ?
C6 N2 Fe1 115.61(13) . . ?
N3 N2 Fe1 137.21(12) . . ?
N2 N3 C8 110.76(16) . . ?
N2 N3 H3 121(2) . . ?
C8 N3 H3 127(2) . . ?
N5 N4 C21 111.43(18) . . ?
N5 N4 H4 116(3) . . ?
C21 N4 H4 132(3) . . ?
N4 N5 C23 105.37(18) . . ?
N4 N5 Fe2 136.13(14) . . ?
C23 N5 Fe2 115.25(15) . . ?
C28 N6 C24 117.5(2) . . ?
C28 N6 Fe2 127.5(2) . . ?
C24 N6 Fe2 114.78(15) . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.2(2) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.5(3) . . ?
C3 C4 H4B 120.8 . . ?
C5 C4 H4B 120.8 . . ?
N1 C5 C4 122.7(2) . . ?
N1 C5 C6 113.49(17) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 110.96(18) . . ?
N2 C6 C5 115.38(17) . . ?
C7 C6 C5 133.62(18) . . ?
C8 C7 C6 105.12(17) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.28(18) . . ?
N3 C8 C9 123.26(18) . . ?
C7 C8 C9 129.45(18) . . ?
C14 C9 C10 119.8(2) . . ?
C14 C9 C8 122.00(18) . . ?
C10 C9 C8 118.2(2) . . ?
C11 C10 C9 119.2(3) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.5(2) . . ?
C12 C13 C15 120.8(2) . . ?
C14 C13 C15 120.4(2) . . ?
C9 C14 C13 120.7(2) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C20 C15 C16 118.5(3) . . ?
C20 C15 C13 118.5(2) . . ?
C16 C15 C13 122.9(2) . . ?
C17 C16 C15 120.4(3) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C16 C17 C18 120.6(3) . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 118.9(3) . . ?
C20 C19 C21 120.7(2) . . ?
C18 C19 C21 120.1(2) . . ?
C19 C20 C15 121.7(2) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 106.7(2) . . ?
N4 C21 C19 122.0(2) . . ?
C22 C21 C19 131.0(2) . . ?
C23 C22 C21 105.32(19) . . ?
C23 C22 H22A 127.3 . . ?
C21 C22 H22A 127.3 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 116.1(2) . . ?
C22 C23 C24 132.8(2) . . ?
N6 C24 C25 122.9(3) . . ?
N6 C24 C23 114.3(2) . . ?
C25 C24 C23 122.8(2) . . ?
C26 C25 C24 118.7(3) . . ?
C26 C25 H25A 120.7 . . ?
C24 C25 H25A 120.7 . . ?
C27 C26 C25 119.3(3) . . ?
C27 C26 H26A 120.3 . . ?
C25 C26 H26A 120.3 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.3(3) . . ?
N6 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
O2 Fe3 O2 91.07(6) 9 . ?
O2 Fe3 O2 91.06(7) 9 5 ?
O2 Fe3 O2 91.06(7) . 5 ?
O2 Fe3 O1 82.09(5) 9 9 ?
O2 Fe3 O1 170.25(6) . 9 ?
O2 Fe3 O1 95.97(6) 5 9 ?
O2 Fe3 O1 170.25(6) 9 5 ?
O2 Fe3 O1 95.97(6) . 5 ?
O2 Fe3 O1 82.09(5) 5 5 ?
O1 Fe3 O1 91.69(6) 9 5 ?
O2 Fe3 O1 95.97(6) 9 . ?
O2 Fe3 O1 82.09(5) . . ?
O2 Fe3 O1 170.26(6) 5 . ?
O1 Fe3 O1 91.69(6) 9 . ?
O1 Fe3 O1 91.69(6) 5 . ?
C29 O1 Fe3 113.77(12) . . ?
C30 O2 Fe3 113.49(12) . . ?
O1 C29 C34 124.52(18) . . ?
O1 C29 C30 114.96(16) . . ?
C34 C29 C30 120.51(17) . . ?
O2 C30 C31 123.82(18) . . ?
O2 C30 C29 115.54(16) . . ?
C31 C30 C29 120.62(19) . . ?
C30 C31 C32 121.6(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.6(3) . . ?
O3 C32 C33 117.8(3) . . ?
C31 C32 C33 117.5(2) . . ?
O4 C33 C34 124.2(2) . . ?
O4 C33 C32 117.1(2) . . ?
C34 C33 C32 118.6(2) . . ?
C29 C34 C33 120.97(19) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F4 B1 F1 112.3(16) . . ?
F4 B1 F2 109.9(16) . . ?
F1 B1 F2 110.3(16) . . ?
F4 B1 F3 109.2(16) . . ?
F1 B1 F3 109.5(17) . . ?
F2 B1 F3 105.3(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(2) 2.06(2) 2.944(2) 169(3) . yes
N4 H4 O2 0.90(2) 2.12(3) 3.002(2) 167(4) 9 yes

_refine_diff_density_max         0.243
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.054

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_330K
_database_code_depnum_ccdc_archive 'CCDC 2261725'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.407(C H4 O)'
_chemical_formula_sum            'C104.41 H75.64 B F4 Fe3 N18 O14.41'
_chemical_formula_weight         2067.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.579(3)
_cell_length_b                   21.579(3)
_cell_length_c                   21.579(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10048(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    330(2)
_cell_measurement_reflns_used    6520
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.89

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_F_000             4249
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.540
_shelx_estimated_absorpt_T_min   0.876
_shelx_estimated_absorpt_T_max   0.899
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      330(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            164569
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0645
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.369
_diffrn_reflns_theta_max         29.517
_diffrn_reflns_theta_full        29.517
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8677
_reflns_number_gt                8479
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.8023 (i.e. 2.407 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0713P)²+0.1338P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0246(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3840 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.066(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8677
_refine_ls_number_parameters     479
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0951
_refine_ls_wR_factor_gt          0.0947
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.083
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29674(2) 0.29674(2) 0.29674(2) 0.05665(11) Uani 1 3 d S T P . .
Fe2 Fe 0.58517(2) 0.58517(2) 0.58517(2) 0.06279(12) Uani 1 3 d S T P . .
N1 N 0.22756(8) 0.33014(8) 0.24308(8) 0.0650(3) Uani 1 1 d . . . . .
N2 N 0.25995(7) 0.35705(8) 0.35456(7) 0.0604(3) Uani 1 1 d . . . . .
N3 N 0.26652(7) 0.37280(8) 0.41459(7) 0.0614(3) Uani 1 1 d D . . . .
H3 H 0.3022(12) 0.3669(16) 0.4342(15) 0.092 Uiso 1 1 d D U . . .
N4 N 0.47658(8) 0.49328(10) 0.62230(8) 0.0705(4) Uani 1 1 d D . . . .
H4 H 0.4555(17) 0.5022(18) 0.5876(14) 0.106 Uiso 1 1 d D U . . .
N5 N 0.53551(8) 0.51350(9) 0.62436(8) 0.0691(4) Uani 1 1 d . . . . .
N6 N 0.64730(9) 0.55063(10) 0.65270(10) 0.0774(4) Uani 1 1 d . . . . .
C1 C 0.21441(12) 0.31401(12) 0.18426(10) 0.0770(5) Uani 1 1 d . . . . .
H1A H 0.241037 0.287262 0.163459 0.092 Uiso 1 1 calc R U . . .
C2 C 0.16248(15) 0.33605(14) 0.15386(13) 0.0907(7) Uani 1 1 d . . . . .
H2A H 0.153749 0.323130 0.113688 0.109 Uiso 1 1 calc R U . . .
C3 C 0.12377(16) 0.37726(16) 0.18347(15) 0.0975(8) Uani 1 1 d . . . . .
H3B H 0.089125 0.393045 0.163266 0.117 Uiso 1 1 calc R U . . .
C4 C 0.13711(14) 0.39487(14) 0.24367(14) 0.0878(7) Uani 1 1 d . . . . .
H4B H 0.111700 0.422648 0.264640 0.105 Uiso 1 1 calc R U . . .
C5 C 0.18919(9) 0.37018(10) 0.27200(10) 0.0678(4) Uani 1 1 d . . . . .
C6 C 0.20695(9) 0.38328(9) 0.33580(9) 0.0653(4) Uani 1 1 d . . . . .
C7 C 0.17939(9) 0.41638(11) 0.38384(10) 0.0711(4) Uani 1 1 d . . . . .
H7A H 0.142442 0.438532 0.382578 0.085 Uiso 1 1 calc R U . . .
C8 C 0.21859(8) 0.40924(9) 0.43352(9) 0.0644(4) Uani 1 1 d . . . . .
C9 C 0.21328(9) 0.43404(10) 0.49680(9) 0.0678(4) Uani 1 1 d . . . . .
C10 C 0.16514(11) 0.47519(14) 0.50958(13) 0.0832(6) Uani 1 1 d . . . . .
H10A H 0.138076 0.487401 0.478344 0.100 Uiso 1 1 calc R U . . .
C11 C 0.15798(15) 0.49782(18) 0.56959(16) 0.1027(9) Uani 1 1 d . . . . .
H11A H 0.126352 0.525788 0.578245 0.123 Uiso 1 1 calc R U . . .
C12 C 0.19666(14) 0.47944(19) 0.61541(14) 0.1007(9) Uani 1 1 d . . . . .
H12A H 0.190286 0.493926 0.655500 0.121 Uiso 1 1 calc R U . . .
C13 C 0.24582(10) 0.43928(14) 0.60375(10) 0.0784(5) Uani 1 1 d . . . . .
C14 C 0.25343(9) 0.41659(12) 0.54379(9) 0.0720(4) Uani 1 1 d . . . . .
H14A H 0.285782 0.389444 0.535203 0.086 Uiso 1 1 calc R U . . .
C15 C 0.29234(12) 0.42636(15) 0.65168(10) 0.0847(6) Uani 1 1 d . . . . .
C16 C 0.27739(16) 0.4037(2) 0.71037(14) 0.1188(13) Uani 1 1 d . . . . .
H16A H 0.236372 0.394532 0.719899 0.143 Uiso 1 1 calc R U . . .
C17 C 0.3225(2) 0.3949(3) 0.75405(15) 0.1352(18) Uani 1 1 d . . . . .
H17A H 0.312235 0.377973 0.792309 0.162 Uiso 1 1 calc R U . . .
C18 C 0.38359(17) 0.4111(2) 0.74175(13) 0.1126(11) Uani 1 1 d . . . . .
H18A H 0.413723 0.406343 0.772184 0.135 Uiso 1 1 calc R U . . .
C19 C 0.39969(12) 0.43455(14) 0.68361(10) 0.0788(5) Uani 1 1 d . . . . .
C20 C 0.35409(10) 0.44123(12) 0.63950(9) 0.0743(5) Uani 1 1 d . . . . .
H20A H 0.364738 0.456063 0.600459 0.089 Uiso 1 1 calc R U . . .
C21 C 0.46249(10) 0.45819(11) 0.67259(9) 0.0704(4) Uani 1 1 d . . . . .
C22 C 0.51524(11) 0.45610(12) 0.70914(11) 0.0768(5) Uani 1 1 d . . . . .
H22A H 0.520267 0.435575 0.746702 0.092 Uiso 1 1 calc R U . . .
C23 C 0.55879(11) 0.49109(10) 0.67775(10) 0.0704(4) Uani 1 1 d . . . . .
C24 C 0.62244(11) 0.50918(11) 0.69253(12) 0.0758(5) Uani 1 1 d . . . . .
C25 C 0.65424(16) 0.48645(17) 0.74312(18) 0.1010(9) Uani 1 1 d . . . . .
H25A H 0.635367 0.458696 0.770154 0.121 Uiso 1 1 calc R U . . .
C26 C 0.71408(18) 0.5054(2) 0.7529(2) 0.1252(14) Uani 1 1 d . . . . .
H26A H 0.736566 0.490147 0.786385 0.150 Uiso 1 1 calc R U . . .
C27 C 0.74047(16) 0.5472(2) 0.7127(3) 0.1306(15) Uani 1 1 d . . . . .
H27A H 0.780878 0.560885 0.718843 0.157 Uiso 1 1 calc R U . . .
C28 C 0.70621(14) 0.56871(17) 0.66290(18) 0.1030(9) Uani 1 1 d . . . . .
H28A H 0.724453 0.596579 0.635551 0.124 Uiso 1 1 calc R U . . .
Fe3 Fe 0.44083(2) 0.44083(2) 0.44083(2) 0.06247(12) Uani 1 3 d S T P . .
O1 O 0.38989(6) 0.36983(7) 0.47259(6) 0.0634(3) Uani 1 1 d . . . . .
O2 O 0.50114(6) 0.40891(7) 0.50323(7) 0.0671(3) Uani 1 1 d . . . . .
O3 O 0.52536(12) 0.23891(15) 0.63679(13) 0.1209(9) Uani 1 1 d . . . . .
O4 O 0.40927(13) 0.20266(14) 0.61057(14) 0.1211(9) Uani 1 1 d . U . . .
C29 C 0.41785(8) 0.33698(9) 0.51502(8) 0.0620(3) Uani 1 1 d . . . . .
C30 C 0.48234(9) 0.35841(9) 0.53138(9) 0.0643(4) Uani 1 1 d . . . . .
C31 C 0.51788(11) 0.32564(13) 0.57166(11) 0.0811(6) Uani 1 1 d . . . . .
H31A H 0.557730 0.339385 0.580615 0.097 Uiso 1 1 calc R U . . .
C32 C 0.49546(12) 0.27069(15) 0.60050(12) 0.0846(6) Uani 1 1 d . U . . .
C33 C 0.42821(12) 0.25013(14) 0.58534(12) 0.0836(6) Uani 1 1 d . U . . .
C34 C 0.39297(10) 0.28623(11) 0.54297(10) 0.0733(5) Uani 1 1 d . . . . .
H34A H 0.352292 0.274986 0.534230 0.088 Uiso 1 1 calc R U . . .
O1S O 0.0182(3) 0.4043(3) 0.3559(5) 0.200(4) Uani 0.802(13) 1 d D U P . .
H1S H 0.010598 0.368372 0.365607 0.301 Uiso 0.802(13) 1 calc R U P . .
C1S C -0.0333(6) 0.4407(6) 0.3669(6) 0.212(5) Uani 0.802(13) 1 d D U P . .
H1S1 H -0.049993 0.430907 0.406956 0.318 Uiso 0.802(13) 1 calc R U P . .
H1S2 H -0.063949 0.432764 0.335685 0.318 Uiso 0.802(13) 1 calc R U P . .
H1S3 H -0.021611 0.483574 0.365744 0.318 Uiso 0.802(13) 1 calc R U P . .
B1 B 0.1330(8) 0.1290(10) 0.1314(9) 0.129(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1222(7) 0.1712(9) 0.0855(8) 0.166(6) Uani 0.3333 1 d D U P A -1
F2 F 0.1867(5) 0.1436(8) 0.1626(7) 0.193(5) Uani 0.3333 1 d D U P A -1
F3 F 0.0842(8) 0.1240(10) 0.1713(8) 0.176(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1441(8) 0.0713(8) 0.1043(8) 0.183(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9699(16) 5 ?
Fe1 N2 1.9699(16) 9 ?
Fe1 N2 1.9699(16) . ?
Fe1 N1 2.0220(17) 5 ?
Fe1 N1 2.0220(17) 9 ?
Fe1 N1 2.0221(17) . ?
Fe2 N5 2.063(2) 9 ?
Fe2 N5 2.063(2) 5 ?
Fe2 N5 2.063(2) . ?
Fe2 N6 2.116(2) . ?
Fe2 N6 2.116(2) 9 ?
Fe2 N6 2.116(2) 5 ?
N1 C1 1.346(3) . ?
N1 C5 1.350(3) . ?
N2 C6 1.339(2) . ?
N2 N3 1.347(2) . ?
N3 C8 1.362(2) . ?
N3 H3 0.89(2) . ?
N4 N5 1.345(3) . ?
N4 C21 1.358(3) . ?
N4 H4 0.90(2) . ?
N5 C23 1.347(3) . ?
N6 C28 1.348(3) . ?
N6 C24 1.352(3) . ?
C1 C2 1.383(3) . ?
C1 H1A 0.9300 . ?
C2 C3 1.377(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.384(4) . ?
C3 H3B 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.457(3) . ?
C6 C7 1.392(3) . ?
C7 C8 1.374(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.471(3) . ?
C9 C14 1.386(3) . ?
C9 C10 1.394(3) . ?
C10 C11 1.392(4) . ?
C10 H10A 0.9300 . ?
C11 C12 1.354(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.393(4) . ?
C12 H12A 0.9300 . ?
C13 C14 1.393(3) . ?
C13 C15 1.468(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.395(3) . ?
C15 C20 1.396(3) . ?
C16 C17 1.369(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.388(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.397(3) . ?
C18 H18A 0.9300 . ?
C19 C20 1.377(3) . ?
C19 C21 1.467(3) . ?
C20 H20A 0.9300 . ?
C21 C22 1.386(3) . ?
C22 C23 1.383(3) . ?
C22 H22A 0.9300 . ?
C23 C24 1.463(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.371(5) . ?
C25 H25A 0.9300 . ?
C26 C27 1.376(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.384(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9950(14) 5 ?
Fe3 O2 1.9951(14) 9 ?
Fe3 O2 1.9951(14) . ?
Fe3 O1 2.0064(14) . ?
Fe3 O1 2.0064(14) 9 ?
Fe3 O1 2.0064(14) 5 ?
O1 C29 1.306(2) . ?
O2 C30 1.312(2) . ?
O3 C32 1.225(3) . ?
O4 C33 1.230(3) . ?
C29 C34 1.361(3) . ?
C29 C30 1.508(3) . ?
C30 C31 1.358(3) . ?
C31 C32 1.424(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.552(4) . ?
C33 C34 1.422(3) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.379(11) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F3 1.363(19) . ?
B1 F1 1.367(18) . ?
B1 F2 1.375(13) . ?
B1 F4 1.397(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 95.91(6) 5 9 ?
N2 Fe1 N2 95.91(6) 5 . ?
N2 Fe1 N2 95.91(6) 9 . ?
N2 Fe1 N1 80.20(7) 5 5 ?
N2 Fe1 N1 171.71(7) 9 5 ?
N2 Fe1 N1 91.79(7) . 5 ?
N2 Fe1 N1 91.79(7) 5 9 ?
N2 Fe1 N1 80.20(7) 9 9 ?
N2 Fe1 N1 171.71(7) . 9 ?
N1 Fe1 N1 92.55(7) 5 9 ?
N2 Fe1 N1 171.71(7) 5 . ?
N2 Fe1 N1 91.79(7) 9 . ?
N2 Fe1 N1 80.20(7) . . ?
N1 Fe1 N1 92.55(7) 5 . ?
N1 Fe1 N1 92.55(7) 9 . ?
N5 Fe2 N5 97.52(7) 9 5 ?
N5 Fe2 N5 97.52(7) 9 . ?
N5 Fe2 N5 97.52(7) 5 . ?
N5 Fe2 N6 167.76(8) 9 . ?
N5 Fe2 N6 94.22(8) 5 . ?
N5 Fe2 N6 77.45(7) . . ?
N5 Fe2 N6 77.45(7) 9 9 ?
N5 Fe2 N6 167.76(8) 5 9 ?
N5 Fe2 N6 94.22(8) . 9 ?
N6 Fe2 N6 91.69(8) . 9 ?
N5 Fe2 N6 94.22(8) 9 5 ?
N5 Fe2 N6 77.45(7) 5 5 ?
N5 Fe2 N6 167.76(8) . 5 ?
N6 Fe2 N6 91.69(8) . 5 ?
N6 Fe2 N6 91.69(8) 9 5 ?
C1 N1 C5 118.17(19) . . ?
C1 N1 Fe1 127.11(16) . . ?
C5 N1 Fe1 114.60(13) . . ?
C6 N2 N3 105.90(15) . . ?
C6 N2 Fe1 115.60(13) . . ?
N3 N2 Fe1 137.18(12) . . ?
N2 N3 C8 110.75(16) . . ?
N2 N3 H3 121(2) . . ?
C8 N3 H3 127(2) . . ?
N5 N4 C21 111.47(18) . . ?
N5 N4 H4 116(3) . . ?
C21 N4 H4 132(3) . . ?
N4 N5 C23 105.33(18) . . ?
N4 N5 Fe2 136.11(14) . . ?
C23 N5 Fe2 115.23(15) . . ?
C28 N6 C24 117.5(2) . . ?
C28 N6 Fe2 127.5(2) . . ?
C24 N6 Fe2 114.81(15) . . ?
N1 C1 C2 121.9(2) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.6(2) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.5(3) . . ?
C3 C4 H4B 120.7 . . ?
C5 C4 H4B 120.7 . . ?
N1 C5 C4 122.7(2) . . ?
N1 C5 C6 113.56(17) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 110.90(17) . . ?
N2 C6 C5 115.37(17) . . ?
C7 C6 C5 133.69(18) . . ?
C8 C7 C6 105.09(17) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 107.35(18) . . ?
N3 C8 C9 123.21(18) . . ?
C7 C8 C9 129.44(18) . . ?
C14 C9 C10 119.6(2) . . ?
C14 C9 C8 122.10(18) . . ?
C10 C9 C8 118.3(2) . . ?
C11 C10 C9 119.3(3) . . ?
C11 C10 H10A 120.3 . . ?
C9 C10 H10A 120.3 . . ?
C12 C11 C10 120.5(3) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 121.3(2) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.4(2) . . ?
C12 C13 C15 120.8(2) . . ?
C14 C13 C15 120.5(2) . . ?
C9 C14 C13 120.7(2) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C16 C15 C20 118.2(3) . . ?
C16 C15 C13 123.2(2) . . ?
C20 C15 C13 118.5(2) . . ?
C17 C16 C15 120.6(3) . . ?
C17 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C16 C17 C18 120.6(3) . . ?
C16 C17 H17A 119.7 . . ?
C18 C17 H17A 119.7 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 120.8(2) . . ?
C18 C19 C21 120.1(2) . . ?
C19 C20 C15 121.9(2) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 106.8(2) . . ?
N4 C21 C19 122.02(19) . . ?
C22 C21 C19 130.9(2) . . ?
C23 C22 C21 105.16(19) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.21(19) . . ?
N5 C23 C24 116.2(2) . . ?
C22 C23 C24 132.6(2) . . ?
N6 C24 C25 122.8(3) . . ?
N6 C24 C23 114.2(2) . . ?
C25 C24 C23 123.0(2) . . ?
C26 C25 C24 119.0(3) . . ?
C26 C25 H25A 120.5 . . ?
C24 C25 H25A 120.5 . . ?
C25 C26 C27 119.2(3) . . ?
C25 C26 H26A 120.4 . . ?
C27 C26 H26A 120.4 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.3(3) . . ?
N6 C28 H28A 118.9 . . ?
C27 C28 H28A 118.9 . . ?
O2 Fe3 O2 91.03(6) 5 9 ?
O2 Fe3 O2 91.03(6) 5 . ?
O2 Fe3 O2 91.03(6) 9 . ?
O2 Fe3 O1 170.31(6) 5 . ?
O2 Fe3 O1 95.93(6) 9 . ?
O2 Fe3 O1 82.14(5) . . ?
O2 Fe3 O1 95.94(6) 5 9 ?
O2 Fe3 O1 82.14(5) 9 9 ?
O2 Fe3 O1 170.31(6) . 9 ?
O1 Fe3 O1 91.69(6) . 9 ?
O2 Fe3 O1 82.14(5) 5 5 ?
O2 Fe3 O1 170.31(6) 9 5 ?
O2 Fe3 O1 95.94(6) . 5 ?
O1 Fe3 O1 91.69(6) . 5 ?
O1 Fe3 O1 91.69(6) 9 5 ?
C29 O1 Fe3 113.63(12) . . ?
C30 O2 Fe3 113.43(12) . . ?
O1 C29 C34 124.43(18) . . ?
O1 C29 C30 115.09(17) . . ?
C34 C29 C30 120.48(18) . . ?
O2 C30 C31 123.68(18) . . ?
O2 C30 C29 115.57(16) . . ?
C31 C30 C29 120.74(19) . . ?
C30 C31 C32 121.4(2) . . ?
C30 C31 H31A 119.3 . . ?
C32 C31 H31A 119.3 . . ?
O3 C32 C31 124.5(3) . . ?
O3 C32 C33 117.8(3) . . ?
C31 C32 C33 117.6(2) . . ?
O4 C33 C34 124.3(2) . . ?
O4 C33 C32 117.1(2) . . ?
C34 C33 C32 118.6(2) . . ?
C29 C34 C33 120.99(19) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F3 B1 F1 112.3(15) . . ?
F3 B1 F2 111.1(16) . . ?
F1 B1 F2 110.3(16) . . ?
F3 B1 F4 108.9(17) . . ?
F1 B1 F4 108.6(16) . . ?
F2 B1 F4 105.3(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(2) 2.07(2) 2.942(2) 169(3) . yes
N4 H4 O2 0.90(2) 2.12(3) 3.002(2) 168(4) 9 yes

_refine_diff_density_max         0.264
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.054

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_340K
_database_code_depnum_ccdc_archive 'CCDC 2261726'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 2.272(C H4 O)'
_chemical_formula_sum            'C104.27 H75.07 B F4 Fe3 N18 O14.27'
_chemical_formula_weight         2062.89

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.604(3)
_cell_length_b                   21.604(3)
_cell_length_c                   21.604(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10083(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    340(2)
_cell_measurement_reflns_used    6453
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      33.89

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             4238
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      340(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            163352
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_av_R_equivalents  0.1078
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.368
_diffrn_reflns_theta_max         29.518
_diffrn_reflns_theta_full        29.518
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8710
_reflns_number_gt                8327
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.7574 (i.e. 2.272 MeOH per formula unit).
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0822P)²+0.0088P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0192(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3699 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.049(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8710
_refine_ls_number_parameters     479
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0378
_refine_ls_wR_factor_ref         0.1076
_refine_ls_wR_factor_gt          0.1068
_refine_ls_goodness_of_fit_ref   1.072
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29696(2) 0.29696(2) 0.29696(2) 0.05766(12) Uani 1 3 d S T P . .
Fe2 Fe 0.58474(2) 0.58474(2) 0.58474(2) 0.06421(14) Uani 1 3 d S T P . .
N1 N 0.22763(9) 0.33044(9) 0.24316(8) 0.0668(4) Uani 1 1 d . . . . .
N2 N 0.26004(8) 0.35753(9) 0.35471(8) 0.0620(3) Uani 1 1 d . . . . .
N3 N 0.26643(8) 0.37333(9) 0.41466(8) 0.0628(3) Uani 1 1 d D . . . .
H3 H 0.3016(14) 0.3670(18) 0.4346(17) 0.094 Uiso 1 1 d D U . . .
N4 N 0.47616(9) 0.49286(11) 0.62211(9) 0.0717(4) Uani 1 1 d D . . . .
H4 H 0.4541(19) 0.502(2) 0.5892(16) 0.107 Uiso 1 1 d D U . . .
N5 N 0.53508(9) 0.51284(10) 0.62407(9) 0.0703(4) Uani 1 1 d . . . . .
N6 N 0.64677(10) 0.54997(11) 0.65242(12) 0.0802(5) Uani 1 1 d . . . . .
C1 C 0.21440(14) 0.31435(13) 0.18459(11) 0.0797(6) Uani 1 1 d . . . . .
H1A H 0.240928 0.287480 0.163915 0.096 Uiso 1 1 calc R U . . .
C2 C 0.16260(17) 0.33641(16) 0.15391(14) 0.0943(8) Uani 1 1 d . . . . .
H2A H 0.153934 0.323490 0.113767 0.113 Uiso 1 1 calc R U . . .
C3 C 0.12421(18) 0.37753(18) 0.18337(17) 0.1025(10) Uani 1 1 d . . . . .
H3B H 0.089517 0.393160 0.163242 0.123 Uiso 1 1 calc R U . . .
C4 C 0.13769(16) 0.39555(16) 0.24351(16) 0.0918(8) Uani 1 1 d . . . . .
H4B H 0.112534 0.423666 0.264247 0.110 Uiso 1 1 calc R U . . .
C5 C 0.18953(10) 0.37067(11) 0.27198(10) 0.0691(4) Uani 1 1 d . . . . .
C6 C 0.20727(10) 0.38384(10) 0.33586(10) 0.0668(4) Uani 1 1 d . . . . .
C7 C 0.17954(10) 0.41689(12) 0.38376(12) 0.0728(5) Uani 1 1 d . . . . .
H7A H 0.142603 0.438960 0.382396 0.087 Uiso 1 1 calc R U . . .
C8 C 0.21853(9) 0.40982(11) 0.43344(10) 0.0664(4) Uani 1 1 d . . . . .
C9 C 0.21321(10) 0.43451(12) 0.49660(11) 0.0705(5) Uani 1 1 d . . . . .
C10 C 0.16503(13) 0.47541(17) 0.50954(15) 0.0876(7) Uani 1 1 d . . . . .
H10A H 0.137868 0.487429 0.478377 0.105 Uiso 1 1 calc R U . . .
C11 C 0.15782(17) 0.4981(2) 0.56923(18) 0.1084(11) Uani 1 1 d . . . . .
H11A H 0.126261 0.526104 0.577808 0.130 Uiso 1 1 calc R U . . .
C12 C 0.19650(16) 0.4797(2) 0.61510(16) 0.1061(11) Uani 1 1 d . . . . .
H12A H 0.190148 0.494219 0.655136 0.127 Uiso 1 1 calc R U . . .
C13 C 0.24550(12) 0.43961(16) 0.60347(12) 0.0819(6) Uani 1 1 d . . . . .
C14 C 0.25327(10) 0.41696(13) 0.54357(11) 0.0742(5) Uani 1 1 d . . . . .
H14A H 0.285589 0.389840 0.535035 0.089 Uiso 1 1 calc R U . . .
C15 C 0.29194(13) 0.42673(17) 0.65160(11) 0.0872(7) Uani 1 1 d . . . . .
C16 C 0.27666(18) 0.4041(3) 0.71001(16) 0.1220(15) Uani 1 1 d . . . . .
H16A H 0.235695 0.394850 0.719469 0.146 Uiso 1 1 calc R U . . .
C17 C 0.3220(2) 0.3954(3) 0.75352(17) 0.140(2) Uani 1 1 d . . . . .
H17A H 0.311561 0.378889 0.791876 0.168 Uiso 1 1 calc R U . . .
C18 C 0.3832(2) 0.4108(3) 0.74142(15) 0.1163(13) Uani 1 1 d . . . . .
H18A H 0.413251 0.405448 0.771739 0.140 Uiso 1 1 calc R U . . .
C19 C 0.39931(13) 0.43447(15) 0.68341(11) 0.0811(6) Uani 1 1 d . . . . .
C20 C 0.35372(11) 0.44149(13) 0.63942(10) 0.0762(5) Uani 1 1 d . . . . .
H20A H 0.364356 0.456473 0.600494 0.091 Uiso 1 1 calc R U . . .
C21 C 0.46203(12) 0.45806(12) 0.67250(10) 0.0723(5) Uani 1 1 d . . . . .
C22 C 0.51441(13) 0.45601(13) 0.70912(12) 0.0792(6) Uani 1 1 d . . . . .
H22A H 0.519248 0.435754 0.746793 0.095 Uiso 1 1 calc R U . . .
C23 C 0.55825(12) 0.49071(11) 0.67750(11) 0.0718(5) Uani 1 1 d . . . . .
C24 C 0.62188(12) 0.50876(13) 0.69230(13) 0.0783(5) Uani 1 1 d . . . . .
C25 C 0.65368(18) 0.48595(19) 0.7428(2) 0.1048(10) Uani 1 1 d . . . . .
H25A H 0.634741 0.458094 0.769640 0.126 Uiso 1 1 calc R U . . .
C26 C 0.7130(2) 0.5046(2) 0.7531(3) 0.1292(16) Uani 1 1 d . . . . .
H26A H 0.735097 0.489388 0.786730 0.155 Uiso 1 1 calc R U . . .
C27 C 0.73996(18) 0.5463(3) 0.7128(3) 0.1346(18) Uani 1 1 d . . . . .
H27A H 0.780438 0.559579 0.719061 0.162 Uiso 1 1 calc R U . . .
C28 C 0.70568(16) 0.56832(19) 0.6627(2) 0.1050(10) Uani 1 1 d . . . . .
H28A H 0.723874 0.596384 0.635585 0.126 Uiso 1 1 calc R U . . .
Fe3 Fe 0.44066(2) 0.44066(2) 0.44066(2) 0.06414(13) Uani 1 3 d S T P . .
O1 O 0.38981(6) 0.36982(7) 0.47253(7) 0.0645(3) Uani 1 1 d . . . . .
O2 O 0.50093(7) 0.40883(8) 0.50296(8) 0.0688(3) Uani 1 1 d . . . . .
O3 O 0.52482(14) 0.24003(18) 0.63751(15) 0.1286(12) Uani 1 1 d . . . . .
O4 O 0.40891(15) 0.20346(16) 0.61118(16) 0.1281(11) Uani 1 1 d . U . . .
C29 C 0.41754(9) 0.33726(10) 0.51517(9) 0.0634(4) Uani 1 1 d . . . . .
C30 C 0.48218(9) 0.35854(11) 0.53139(10) 0.0659(4) Uani 1 1 d . . . . .
C31 C 0.51736(12) 0.32603(16) 0.57178(13) 0.0842(7) Uani 1 1 d . . . . .
H31A H 0.557188 0.339741 0.580654 0.101 Uiso 1 1 calc R U . . .
C32 C 0.49499(14) 0.27144(17) 0.60097(13) 0.0888(7) Uani 1 1 d . U . . .
C33 C 0.42778(14) 0.25097(16) 0.58617(14) 0.0872(7) Uani 1 1 d . U . . .
C34 C 0.39283(11) 0.28697(13) 0.54322(11) 0.0754(5) Uani 1 1 d . . . . .
H34A H 0.352259 0.275656 0.534316 0.090 Uiso 1 1 calc R U . . .
O1S O 0.0181(4) 0.4044(4) 0.3564(6) 0.209(5) Uani 0.757(15) 1 d D U P . .
H1S H 0.010340 0.367796 0.362787 0.314 Uiso 0.757(15) 1 calc R U P . .
C1S C -0.0345(7) 0.4393(7) 0.3663(7) 0.223(7) Uani 0.757(15) 1 d D U P . .
H1S1 H -0.052756 0.427975 0.405156 0.334 Uiso 0.757(15) 1 calc R U P . .
H1S2 H -0.063570 0.431848 0.333507 0.334 Uiso 0.757(15) 1 calc R U P . .
H1S3 H -0.023734 0.482430 0.366974 0.334 Uiso 0.757(15) 1 calc R U P . .
B1 B 0.1340(8) 0.1289(10) 0.1312(9) 0.138(4) Uani 0.3333 1 d D U P A -1
F1 F 0.1227(8) 0.1715(10) 0.0856(8) 0.171(7) Uani 0.3333 1 d D U P A -1
F2 F 0.1876(5) 0.1419(9) 0.1623(7) 0.197(6) Uani 0.3333 1 d D U P A -1
F3 F 0.0846(8) 0.1232(10) 0.1708(8) 0.176(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1439(9) 0.0712(8) 0.1031(9) 0.189(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9761(18) . ?
Fe1 N2 1.9761(18) 9 ?
Fe1 N2 1.9761(18) 5 ?
Fe1 N1 2.0291(19) 5 ?
Fe1 N1 2.0291(19) 9 ?
Fe1 N1 2.0292(19) . ?
Fe2 N5 2.070(2) 9 ?
Fe2 N5 2.070(2) 5 ?
Fe2 N5 2.070(2) . ?
Fe2 N6 2.121(2) 9 ?
Fe2 N6 2.121(2) 5 ?
Fe2 N6 2.121(2) . ?
N1 C1 1.343(3) . ?
N1 C5 1.349(3) . ?
N2 C6 1.337(3) . ?
N2 N3 1.346(2) . ?
N3 C8 1.363(3) . ?
N3 H3 0.88(2) . ?
N4 N5 1.345(3) . ?
N4 C21 1.358(3) . ?
N4 H4 0.88(2) . ?
N5 C23 1.346(3) . ?
N6 C24 1.350(4) . ?
N6 C28 1.351(4) . ?
C1 C2 1.385(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.372(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.387(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.386(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.460(3) . ?
C6 C7 1.393(3) . ?
C7 C8 1.373(3) . ?
C7 H7A 0.9300 . ?
C8 C9 1.470(3) . ?
C9 C14 1.387(4) . ?
C9 C10 1.394(4) . ?
C10 C11 1.389(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.356(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.391(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.394(3) . ?
C13 C15 1.471(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.393(4) . ?
C15 C20 1.397(3) . ?
C16 C17 1.370(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.388(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.398(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.377(4) . ?
C19 C21 1.467(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(4) . ?
C22 C23 1.388(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.464(4) . ?
C24 C25 1.381(4) . ?
C25 C26 1.361(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.381(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.396(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9950(15) 9 ?
Fe3 O2 1.9950(16) . ?
Fe3 O2 1.9951(16) 5 ?
Fe3 O1 2.0057(15) . ?
Fe3 O1 2.0057(15) 5 ?
Fe3 O1 2.0057(15) 9 ?
O1 C29 1.305(2) . ?
O2 C30 1.312(3) . ?
O3 C32 1.224(4) . ?
O4 C33 1.229(4) . ?
C29 C34 1.354(3) . ?
C29 C30 1.511(3) . ?
C30 C31 1.354(3) . ?
C31 C32 1.422(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.551(4) . ?
C33 C34 1.427(4) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.380(13) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F2 1.368(15) . ?
B1 F1 1.370(18) . ?
B1 F3 1.372(19) . ?
B1 F4 1.405(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 95.97(7) . 9 ?
N2 Fe1 N2 95.97(7) . 5 ?
N2 Fe1 N2 95.97(7) 9 5 ?
N2 Fe1 N1 91.87(7) . 5 ?
N2 Fe1 N1 171.57(7) 9 5 ?
N2 Fe1 N1 80.08(7) 5 5 ?
N2 Fe1 N1 171.57(7) . 9 ?
N2 Fe1 N1 80.08(7) 9 9 ?
N2 Fe1 N1 91.87(7) 5 9 ?
N1 Fe1 N1 92.55(8) 5 9 ?
N2 Fe1 N1 80.08(7) . . ?
N2 Fe1 N1 91.86(7) 9 . ?
N2 Fe1 N1 171.57(7) 5 . ?
N1 Fe1 N1 92.55(8) 5 . ?
N1 Fe1 N1 92.55(8) 9 . ?
N5 Fe2 N5 97.58(7) 9 5 ?
N5 Fe2 N5 97.58(7) 9 . ?
N5 Fe2 N5 97.58(7) 5 . ?
N5 Fe2 N6 77.21(8) 9 9 ?
N5 Fe2 N6 167.62(9) 5 9 ?
N5 Fe2 N6 94.26(9) . 9 ?
N5 Fe2 N6 94.26(9) 9 5 ?
N5 Fe2 N6 77.21(8) 5 5 ?
N5 Fe2 N6 167.62(9) . 5 ?
N6 Fe2 N6 91.86(9) 9 5 ?
N5 Fe2 N6 167.62(9) 9 . ?
N5 Fe2 N6 94.26(9) 5 . ?
N5 Fe2 N6 77.21(8) . . ?
N6 Fe2 N6 91.86(9) 9 . ?
N6 Fe2 N6 91.86(9) 5 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.19(18) . . ?
C5 N1 Fe1 114.56(14) . . ?
C6 N2 N3 105.81(17) . . ?
C6 N2 Fe1 115.67(15) . . ?
N3 N2 Fe1 137.21(14) . . ?
N2 N3 C8 110.81(17) . . ?
N2 N3 H3 121(3) . . ?
C8 N3 H3 127(3) . . ?
N5 N4 C21 111.4(2) . . ?
N5 N4 H4 118(3) . . ?
C21 N4 H4 131(3) . . ?
N4 N5 C23 105.4(2) . . ?
N4 N5 Fe2 135.92(16) . . ?
C23 N5 Fe2 115.20(17) . . ?
C24 N6 C28 117.6(3) . . ?
C24 N6 Fe2 114.94(17) . . ?
C28 N6 Fe2 127.2(2) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3B 120.3 . . ?
C4 C3 H3B 120.3 . . ?
C5 C4 C3 118.4(3) . . ?
C5 C4 H4B 120.8 . . ?
C3 C4 H4B 120.8 . . ?
N1 C5 C4 122.5(2) . . ?
N1 C5 C6 113.67(19) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 111.0(2) . . ?
N2 C6 C5 115.39(19) . . ?
C7 C6 C5 133.6(2) . . ?
C8 C7 C6 105.06(19) . . ?
C8 C7 H7A 127.5 . . ?
C6 C7 H7A 127.5 . . ?
N3 C8 C7 107.31(19) . . ?
N3 C8 C9 123.1(2) . . ?
C7 C8 C9 129.6(2) . . ?
C14 C9 C10 119.5(2) . . ?
C14 C9 C8 122.1(2) . . ?
C10 C9 C8 118.3(2) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.4(3) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.3(3) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 118.6(3) . . ?
C12 C13 C15 120.6(3) . . ?
C14 C13 C15 120.5(3) . . ?
C9 C14 C13 120.6(2) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C16 C15 C20 118.5(3) . . ?
C16 C15 C13 123.0(3) . . ?
C20 C15 C13 118.4(2) . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.2(3) . . ?
C16 C17 H17A 119.4 . . ?
C18 C17 H17A 119.4 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 C21 120.8(2) . . ?
C18 C19 C21 120.1(3) . . ?
C19 C20 C15 121.9(2) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 107.0(2) . . ?
N4 C21 C19 121.9(2) . . ?
C22 C21 C19 130.8(2) . . ?
C21 C22 C23 105.1(2) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 116.2(2) . . ?
C22 C23 C24 132.6(2) . . ?
N6 C24 C25 122.8(3) . . ?
N6 C24 C23 114.2(2) . . ?
C25 C24 C23 123.0(3) . . ?
C26 C25 C24 119.4(4) . . ?
C26 C25 H25A 120.3 . . ?
C24 C25 H25A 120.3 . . ?
C25 C26 C27 119.2(4) . . ?
C25 C26 H26A 120.4 . . ?
C27 C26 H26A 120.4 . . ?
C26 C27 C28 119.1(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 121.8(4) . . ?
N6 C28 H28A 119.1 . . ?
C27 C28 H28A 119.1 . . ?
O2 Fe3 O2 90.98(7) 9 . ?
O2 Fe3 O2 90.98(7) 9 5 ?
O2 Fe3 O2 90.98(7) . 5 ?
O2 Fe3 O1 95.85(7) 9 . ?
O2 Fe3 O1 82.12(6) . . ?
O2 Fe3 O1 170.35(6) 5 . ?
O2 Fe3 O1 170.35(6) 9 5 ?
O2 Fe3 O1 95.85(7) . 5 ?
O2 Fe3 O1 82.12(6) 5 5 ?
O1 Fe3 O1 91.84(6) . 5 ?
O2 Fe3 O1 82.12(6) 9 9 ?
O2 Fe3 O1 170.35(6) . 9 ?
O2 Fe3 O1 95.85(7) 5 9 ?
O1 Fe3 O1 91.84(6) . 9 ?
O1 Fe3 O1 91.84(6) 5 9 ?
C29 O1 Fe3 113.72(13) . . ?
C30 O2 Fe3 113.56(13) . . ?
O1 C29 C34 124.6(2) . . ?
O1 C29 C30 115.09(18) . . ?
C34 C29 C30 120.31(19) . . ?
O2 C30 C31 123.9(2) . . ?
O2 C30 C29 115.37(18) . . ?
C31 C30 C29 120.7(2) . . ?
C30 C31 C32 121.7(2) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O3 C32 C31 124.5(3) . . ?
O3 C32 C33 117.9(3) . . ?
C31 C32 C33 117.6(2) . . ?
O4 C33 C34 124.4(3) . . ?
O4 C33 C32 117.2(3) . . ?
C34 C33 C32 118.3(2) . . ?
C29 C34 C33 121.3(2) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F1 111.4(16) . . ?
F2 B1 F3 111.8(16) . . ?
F1 B1 F3 111.8(16) . . ?
F2 B1 F4 105.4(15) . . ?
F1 B1 F4 108.2(16) . . ?
F3 B1 F4 107.9(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(2) 2.08(3) 2.945(2) 168(4) . yes
N4 H4 O2 0.88(2) 2.14(3) 3.003(2) 165(4) 9 yes

_refine_diff_density_max         0.230
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.055

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_360K
_database_code_depnum_ccdc_archive 'CCDC 2261728'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 1.550(C H4 O)'
_chemical_formula_sum            'C103.55 H72.20 B F4 Fe3 N18 O13.55'
_chemical_formula_weight         2039.78

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.662(3)
_cell_length_b                   21.662(3)
_cell_length_c                   21.662(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10165(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    360(2)
_cell_measurement_reflns_used    6148
_cell_measurement_theta_min      1.93
_cell_measurement_theta_max      32.64

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_F_000             4189
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.533
_shelx_estimated_absorpt_T_min   0.878
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      360(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            163912
_diffrn_reflns_av_unetI/netI     0.0330
_diffrn_reflns_av_R_equivalents  0.0797
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.929
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_full        29.507
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8767
_reflns_number_gt                7973
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.5169 (i.e. 1.550 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1025P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0133(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3462 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.074(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8767
_refine_ls_number_parameters     477
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0439
_refine_ls_wR_factor_ref         0.1266
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29753(2) 0.29753(2) 0.29753(2) 0.07455(15) Uani 1 3 d S T P . .
Fe2 Fe 0.58282(2) 0.58282(2) 0.58282(2) 0.08201(17) Uani 1 3 d S T P . .
N1 N 0.22856(11) 0.33152(10) 0.24306(10) 0.0856(5) Uani 1 1 d . . . . .
N2 N 0.25999(9) 0.35902(10) 0.35448(10) 0.0799(4) Uani 1 1 d . . . . .
N3 N 0.26586(9) 0.37486(11) 0.41449(10) 0.0814(4) Uani 1 1 d D . . . .
H3 H 0.3055(13) 0.382(2) 0.419(2) 0.122 Uiso 1 1 d D U . . .
N4 N 0.47405(11) 0.49170(13) 0.62060(11) 0.0894(5) Uani 1 1 d D . . . .
H4 H 0.452(2) 0.504(2) 0.5879(19) 0.134 Uiso 1 1 d D U . . .
N5 N 0.53310(11) 0.51100(12) 0.62216(11) 0.0886(5) Uani 1 1 d . . . . .
N6 N 0.64452(12) 0.54793(14) 0.65054(15) 0.0998(6) Uani 1 1 d . . . . .
C1 C 0.21582(18) 0.31526(16) 0.18445(14) 0.0992(7) Uani 1 1 d . . . . .
H1A H 0.242207 0.288228 0.164037 0.119 Uiso 1 1 calc R U . . .
C2 C 0.1641(2) 0.3379(2) 0.15355(17) 0.1193(12) Uani 1 1 d . . . . .
H2A H 0.155041 0.324817 0.113670 0.143 Uiso 1 1 calc R U . . .
C3 C 0.1268(2) 0.3797(2) 0.1828(2) 0.1306(14) Uani 1 1 d . . . . .
H3B H 0.092341 0.395402 0.162610 0.157 Uiso 1 1 calc R U . . .
C4 C 0.1398(2) 0.39822(19) 0.2411(2) 0.1135(10) Uani 1 1 d . . . . .
H4B H 0.115384 0.427459 0.260860 0.136 Uiso 1 1 calc R U . . .
C5 C 0.19098(13) 0.37234(14) 0.27092(14) 0.0898(6) Uani 1 1 d . . . . .
C6 C 0.20791(12) 0.38559(12) 0.33523(13) 0.0851(5) Uani 1 1 d . . . . .
C7 C 0.18030(13) 0.41893(15) 0.38223(15) 0.0931(6) Uani 1 1 d . . . . .
H7A H 0.143732 0.441324 0.380207 0.112 Uiso 1 1 calc R U . . .
C8 C 0.21841(11) 0.41193(14) 0.43258(13) 0.0860(5) Uani 1 1 d . . . . .
C9 C 0.21261(12) 0.43675(16) 0.49569(14) 0.0920(6) Uani 1 1 d . . . . .
C10 C 0.16461(18) 0.4782(2) 0.5073(2) 0.1164(11) Uani 1 1 d . . . . .
H10A H 0.138151 0.490529 0.475808 0.140 Uiso 1 1 calc R U . . .
C11 C 0.1573(2) 0.5006(3) 0.5671(3) 0.147(2) Uani 1 1 d . . . . .
H11A H 0.125933 0.528645 0.575409 0.176 Uiso 1 1 calc R U . . .
C12 C 0.1953(2) 0.4820(3) 0.6135(2) 0.1362(16) Uani 1 1 d . . . . .
H12A H 0.188628 0.496465 0.653415 0.163 Uiso 1 1 calc R U . . .
C13 C 0.24410(15) 0.4417(2) 0.60224(15) 0.1053(9) Uani 1 1 d . . . . .
C14 C 0.25187(13) 0.41903(17) 0.54240(14) 0.0944(7) Uani 1 1 d . . . . .
H14A H 0.283882 0.391678 0.534035 0.113 Uiso 1 1 calc R U . . .
C15 C 0.28985(16) 0.4280(2) 0.64992(14) 0.1077(9) Uani 1 1 d . . . . .
C16 C 0.2751(2) 0.4052(4) 0.7079(2) 0.148(2) Uani 1 1 d . . . . .
H16A H 0.234286 0.395832 0.717253 0.178 Uiso 1 1 calc R U . . .
C17 C 0.3197(3) 0.3964(4) 0.7513(2) 0.160(2) Uani 1 1 d . . . . .
H17A H 0.309055 0.380416 0.789652 0.192 Uiso 1 1 calc R U . . .
C18 C 0.3803(2) 0.4107(3) 0.73916(18) 0.1325(15) Uani 1 1 d . . . . .
H18A H 0.410330 0.404516 0.769192 0.159 Uiso 1 1 calc R U . . .
C19 C 0.39653(16) 0.43461(18) 0.68152(14) 0.1006(8) Uani 1 1 d . . . . .
C20 C 0.35224(14) 0.44206(17) 0.63838(13) 0.0979(7) Uani 1 1 d . . . . .
H20A H 0.363302 0.457009 0.599690 0.118 Uiso 1 1 calc R U . . .
C21 C 0.45954(14) 0.45770(15) 0.67086(12) 0.0904(6) Uani 1 1 d . . . . .
C22 C 0.51240(16) 0.45530(16) 0.70709(15) 0.0987(7) Uani 1 1 d . . . . .
H22A H 0.517311 0.435054 0.744627 0.118 Uiso 1 1 calc R U . . .
C23 C 0.55597(14) 0.48923(15) 0.67564(14) 0.0914(6) Uani 1 1 d . . . . .
C24 C 0.62007(15) 0.50701(16) 0.69002(16) 0.0991(7) Uani 1 1 d . . . . .
C25 C 0.6503(2) 0.4833(2) 0.7397(3) 0.1304(15) Uani 1 1 d . . . . .
H25A H 0.631063 0.455534 0.766297 0.156 Uiso 1 1 calc R U . . .
C26 C 0.7119(3) 0.5023(3) 0.7496(4) 0.161(2) Uani 1 1 d . . . . .
H26A H 0.734644 0.486568 0.782401 0.194 Uiso 1 1 calc R U . . .
C27 C 0.7367(2) 0.5429(3) 0.7110(4) 0.164(2) Uani 1 1 d . . . . .
H27A H 0.776662 0.556902 0.717871 0.196 Uiso 1 1 calc R U . . .
C28 C 0.70370(19) 0.5649(2) 0.6605(3) 0.1292(14) Uani 1 1 d . . . . .
H28A H 0.722781 0.591792 0.632983 0.155 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43961(2) 0.43961(2) 0.43961(2) 0.08288(17) Uani 1 3 d S T P . .
O1 O 0.38862(8) 0.36945(9) 0.47171(9) 0.0825(4) Uani 1 1 d . . . . .
O2 O 0.49971(8) 0.40818(9) 0.50160(10) 0.0874(4) Uani 1 1 d . . . . .
O3 O 0.52084(18) 0.2456(3) 0.6415(2) 0.180(2) Uani 1 1 d . . . . .
O4 O 0.4047(2) 0.2105(2) 0.6165(2) 0.174(2) Uani 1 1 d . U . . .
C29 C 0.41591(12) 0.33815(13) 0.51547(11) 0.0816(5) Uani 1 1 d . . . . .
C30 C 0.48002(12) 0.35917(13) 0.53124(12) 0.0844(5) Uani 1 1 d . . . . .
C31 C 0.51509(15) 0.3279(2) 0.57295(16) 0.1056(9) Uani 1 1 d . . . . .
H31A H 0.554980 0.341312 0.581476 0.127 Uiso 1 1 calc R U . . .
C32 C 0.49138(18) 0.2751(3) 0.60355(18) 0.1215(13) Uani 1 1 d . U . . .
C33 C 0.42524(17) 0.2544(2) 0.58873(17) 0.1140(11) Uani 1 1 d . U . . .
C34 C 0.39076(14) 0.28907(17) 0.54446(14) 0.0964(7) Uani 1 1 d . . . . .
H34A H 0.350353 0.277649 0.535486 0.116 Uiso 1 1 calc R U . . .
O1S O 0.0204(8) 0.4038(7) 0.3550(10) 0.248(9) Uani 0.517(16) 1 d D U P . .
H1S H 0.010740 0.367797 0.361767 0.372 Uiso 0.517(16) 1 d R U P . .
C1S C -0.0333(11) 0.4459(11) 0.3712(13) 0.252(11) Uani 0.517(16) 1 d D U P . .
H1S1 H -0.019212 0.487832 0.372911 0.378 Uiso 0.517(16) 1 d R U P . .
H1S2 H -0.049872 0.434191 0.410601 0.378 Uiso 0.517(16) 1 d R U P . .
H1S3 H -0.064862 0.442141 0.340251 0.378 Uiso 0.517(16) 1 d R U P . .
B1 B 0.1341(11) 0.1347(11) 0.1365(7) 0.161(4) Uani 0.3333 1 d D U P A -1
F1 F 0.1303(11) 0.1733(9) 0.0862(10) 0.202(8) Uani 0.3333 1 d D U P A -1
F2 F 0.1490(9) 0.1652(13) 0.1906(9) 0.228(8) Uani 0.3333 1 d D U P A -1
F3 F 0.0758(9) 0.1079(10) 0.1470(9) 0.201(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1769(10) 0.0886(10) 0.1249(9) 0.213(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.989(2) . ?
Fe1 N2 1.989(2) 5 ?
Fe1 N2 1.989(2) 9 ?
Fe1 N1 2.041(2) . ?
Fe1 N1 2.041(2) 9 ?
Fe1 N1 2.041(2) 5 ?
Fe2 N5 2.075(3) . ?
Fe2 N5 2.075(3) 9 ?
Fe2 N5 2.075(3) 5 ?
Fe2 N6 2.124(3) . ?
Fe2 N6 2.124(3) 9 ?
Fe2 N6 2.124(3) 5 ?
N1 C5 1.345(4) . ?
N1 C1 1.346(4) . ?
N2 C6 1.333(3) . ?
N2 N3 1.350(3) . ?
N3 C8 1.362(3) . ?
N3 H3 0.88(3) . ?
N4 N5 1.346(4) . ?
N4 C21 1.351(4) . ?
N4 H4 0.89(3) . ?
N5 C23 1.345(4) . ?
N6 C24 1.341(5) . ?
N6 C28 1.351(5) . ?
C1 C2 1.395(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.369(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.355(6) . ?
C3 H3B 0.9300 . ?
C4 C5 1.399(4) . ?
C4 H4B 0.9300 . ?
C5 C6 1.469(4) . ?
C6 C7 1.384(4) . ?
C7 C8 1.376(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.474(4) . ?
C9 C14 1.376(5) . ?
C9 C10 1.396(5) . ?
C10 C11 1.392(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.361(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.392(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.396(4) . ?
C13 C15 1.462(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(5) . ?
C15 C20 1.408(4) . ?
C16 C17 1.361(8) . ?
C16 H16A 0.9300 . ?
C17 C18 1.373(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.397(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.349(5) . ?
C19 C21 1.472(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.389(4) . ?
C22 C23 1.377(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.474(5) . ?
C24 C25 1.361(5) . ?
C25 C26 1.412(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.327(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.391(7) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9904(19) 9 ?
Fe3 O2 1.9904(19) . ?
Fe3 O2 1.9904(19) 5 ?
Fe3 O1 2.0033(18) 9 ?
Fe3 O1 2.0033(18) 5 ?
Fe3 O1 2.0033(18) . ?
O1 C29 1.307(3) . ?
O2 C30 1.312(3) . ?
O3 C32 1.220(5) . ?
O4 C33 1.209(5) . ?
C29 C34 1.350(4) . ?
C29 C30 1.501(4) . ?
C30 C31 1.361(4) . ?
C31 C32 1.419(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.535(5) . ?
C33 C34 1.429(5) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.52(2) . ?
O1S H1S 0.8201 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9601 . ?
C1S H1S3 0.9600 . ?
B1 F1 1.376(19) . ?
B1 F2 1.383(16) . ?
B1 F4 1.387(19) . ?
B1 F3 1.41(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.43(8) . 5 ?
N2 Fe1 N2 96.43(8) . 9 ?
N2 Fe1 N2 96.43(8) 5 9 ?
N2 Fe1 N1 79.50(9) . . ?
N2 Fe1 N1 171.26(9) 5 . ?
N2 Fe1 N1 91.73(9) 9 . ?
N2 Fe1 N1 171.27(9) . 9 ?
N2 Fe1 N1 91.72(9) 5 9 ?
N2 Fe1 N1 79.50(9) 9 9 ?
N1 Fe1 N1 92.84(9) . 9 ?
N2 Fe1 N1 91.72(9) . 5 ?
N2 Fe1 N1 79.50(9) 5 5 ?
N2 Fe1 N1 171.27(9) 9 5 ?
N1 Fe1 N1 92.83(9) . 5 ?
N1 Fe1 N1 92.84(9) 9 5 ?
N5 Fe2 N5 97.58(9) . 9 ?
N5 Fe2 N5 97.58(9) . 5 ?
N5 Fe2 N5 97.58(9) 9 5 ?
N5 Fe2 N6 77.07(10) . . ?
N5 Fe2 N6 167.56(10) 9 . ?
N5 Fe2 N6 94.28(11) 5 . ?
N5 Fe2 N6 94.28(11) . 9 ?
N5 Fe2 N6 77.07(10) 9 9 ?
N5 Fe2 N6 167.56(11) 5 9 ?
N6 Fe2 N6 92.01(12) . 9 ?
N5 Fe2 N6 167.56(11) . 5 ?
N5 Fe2 N6 94.28(11) 9 5 ?
N5 Fe2 N6 77.07(10) 5 5 ?
N6 Fe2 N6 92.01(12) . 5 ?
N6 Fe2 N6 92.01(12) 9 5 ?
C5 N1 C1 118.1(3) . . ?
C5 N1 Fe1 114.89(18) . . ?
C1 N1 Fe1 126.9(2) . . ?
C6 N2 N3 105.7(2) . . ?
C6 N2 Fe1 116.16(18) . . ?
N3 N2 Fe1 136.77(17) . . ?
N2 N3 C8 110.8(2) . . ?
N2 N3 H3 104(3) . . ?
C8 N3 H3 127(3) . . ?
N5 N4 C21 111.7(2) . . ?
N5 N4 H4 116(4) . . ?
C21 N4 H4 132(4) . . ?
C23 N5 N4 105.2(2) . . ?
C23 N5 Fe2 115.2(2) . . ?
N4 N5 Fe2 135.70(19) . . ?
C24 N6 C28 117.0(3) . . ?
C24 N6 Fe2 115.3(2) . . ?
C28 N6 Fe2 127.6(3) . . ?
N1 C1 C2 121.7(3) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C4 C3 C2 120.3(3) . . ?
C4 C3 H3B 119.8 . . ?
C2 C3 H3B 119.8 . . ?
C3 C4 C5 118.4(4) . . ?
C3 C4 H4B 120.8 . . ?
C5 C4 H4B 120.8 . . ?
N1 C5 C4 122.4(3) . . ?
N1 C5 C6 113.8(2) . . ?
C4 C5 C6 123.8(3) . . ?
N2 C6 C7 111.1(2) . . ?
N2 C6 C5 115.1(2) . . ?
C7 C6 C5 133.8(3) . . ?
C8 C7 C6 105.4(2) . . ?
C8 C7 H7A 127.3 . . ?
C6 C7 H7A 127.3 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C9 123.1(3) . . ?
C7 C8 C9 130.1(3) . . ?
C14 C9 C10 120.5(3) . . ?
C14 C9 C8 121.8(3) . . ?
C10 C9 C8 117.7(3) . . ?
C11 C10 C9 118.4(4) . . ?
C11 C10 H10A 120.8 . . ?
C9 C10 H10A 120.8 . . ?
C12 C11 C10 121.1(4) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C11 C12 C13 120.9(4) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 118.4(4) . . ?
C12 C13 C15 121.2(3) . . ?
C14 C13 C15 120.2(3) . . ?
C9 C14 C13 120.7(3) . . ?
C9 C14 H14A 119.7 . . ?
C13 C14 H14A 119.7 . . ?
C16 C15 C20 117.3(4) . . ?
C16 C15 C13 123.8(3) . . ?
C20 C15 C13 118.8(3) . . ?
C17 C16 C15 120.8(4) . . ?
C17 C16 H16A 119.6 . . ?
C15 C16 H16A 119.6 . . ?
C16 C17 C18 121.0(4) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
C17 C18 C19 119.7(4) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C20 C19 C18 119.0(4) . . ?
C20 C19 C21 120.7(3) . . ?
C18 C19 C21 120.0(4) . . ?
C19 C20 C15 122.3(3) . . ?
C19 C20 H20A 118.9 . . ?
C15 C20 H20A 118.9 . . ?
N4 C21 C22 106.5(3) . . ?
N4 C21 C19 121.8(3) . . ?
C22 C21 C19 131.5(3) . . ?
C23 C22 C21 105.4(3) . . ?
C23 C22 H22A 127.3 . . ?
C21 C22 H22A 127.3 . . ?
N5 C23 C22 111.1(3) . . ?
N5 C23 C24 115.9(3) . . ?
C22 C23 C24 132.9(3) . . ?
N6 C24 C25 124.4(4) . . ?
N6 C24 C23 114.2(3) . . ?
C25 C24 C23 121.4(4) . . ?
C24 C25 C26 117.6(5) . . ?
C24 C25 H25A 121.2 . . ?
C26 C25 H25A 121.2 . . ?
C27 C26 C25 118.7(5) . . ?
C27 C26 H26A 120.6 . . ?
C25 C26 H26A 120.6 . . ?
C26 C27 C28 121.0(4) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
N6 C28 C27 121.3(5) . . ?
N6 C28 H28A 119.4 . . ?
C27 C28 H28A 119.4 . . ?
O2 Fe3 O2 90.76(9) 9 . ?
O2 Fe3 O2 90.76(9) 9 5 ?
O2 Fe3 O2 90.76(9) . 5 ?
O2 Fe3 O1 82.36(7) 9 9 ?
O2 Fe3 O1 170.73(8) . 9 ?
O2 Fe3 O1 95.52(9) 5 9 ?
O2 Fe3 O1 170.73(8) 9 5 ?
O2 Fe3 O1 95.52(9) . 5 ?
O2 Fe3 O1 82.36(7) 5 5 ?
O1 Fe3 O1 92.08(8) 9 5 ?
O2 Fe3 O1 95.52(9) 9 . ?
O2 Fe3 O1 82.36(7) . . ?
O2 Fe3 O1 170.73(8) 5 . ?
O1 Fe3 O1 92.08(8) 9 . ?
O1 Fe3 O1 92.08(8) 5 . ?
C29 O1 Fe3 113.32(16) . . ?
C30 O2 Fe3 113.23(16) . . ?
O1 C29 C34 124.3(2) . . ?
O1 C29 C30 115.2(2) . . ?
C34 C29 C30 120.4(2) . . ?
O2 C30 C31 123.1(3) . . ?
O2 C30 C29 115.8(2) . . ?
C31 C30 C29 121.1(3) . . ?
C30 C31 C32 120.6(3) . . ?
C30 C31 H31A 119.7 . . ?
C32 C31 H31A 119.7 . . ?
O3 C32 C31 123.2(4) . . ?
O3 C32 C33 118.4(4) . . ?
C31 C32 C33 118.4(3) . . ?
O4 C33 C34 123.7(3) . . ?
O4 C33 C32 118.0(3) . . ?
C34 C33 C32 118.3(3) . . ?
C29 C34 C33 121.0(3) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F1 B1 F2 113.2(17) . . ?
F1 B1 F4 109.5(14) . . ?
F2 B1 F4 110.0(17) . . ?
F1 B1 F3 109.0(17) . . ?
F2 B1 F3 105.6(13) . . ?
F4 B1 F3 109.5(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(3) 2.15(3) 2.936(3) 149(5) . yes
N4 H4 O2 0.89(3) 2.13(3) 2.990(3) 160(5) 9 yes

_refine_diff_density_max         0.264
_refine_diff_density_min         -0.302
_refine_diff_density_rms         0.061

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_370K
_database_code_depnum_ccdc_archive 'CCDC 2261729'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.731(3)
_cell_length_b                   21.731(3)
_cell_length_c                   21.731(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10262(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    370(2)
_cell_measurement_reflns_used    5784
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      31.80

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.288
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      370(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            159413
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.360
_diffrn_reflns_theta_max         29.063
_diffrn_reflns_theta_full        29.063
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8482
_reflns_number_gt                7600
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;

_vrf_PLAT601_lb2205_fresh2_370K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1838 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1196P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0257(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3275 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.090(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8482
_refine_ls_number_parameters     458
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0506
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1442
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45213(2) 0.45213(2) 0.45213(2) 0.08287(19) Uani 1 3 d S T P . .
Fe2 Fe 0.16873(2) 0.16873(2) 0.16873(2) 0.0895(2) Uani 1 3 d S T P . .
N1 N 0.50748(12) 0.41840(13) 0.52081(14) 0.0958(6) Uani 1 1 d . . . . .
N2 N 0.39588(12) 0.38967(12) 0.48973(11) 0.0889(5) Uani 1 1 d . . . . .
N3 N 0.33608(12) 0.37402(14) 0.48438(11) 0.0917(6) Uani 1 1 d D . . . .
H3 H 0.314(2) 0.385(3) 0.4529(19) 0.137 Uiso 1 1 d D U . . .
N4 N 0.13113(12) 0.25880(16) 0.27746(13) 0.0972(6) Uani 1 1 d D . . . .
H4 H 0.161(2) 0.245(3) 0.302(2) 0.146 Uiso 1 1 d D U . . .
N5 N 0.12919(13) 0.23983(14) 0.21835(13) 0.0957(6) Uani 1 1 d . . . . .
N6 N 0.10113(18) 0.20355(16) 0.10706(15) 0.1091(7) Uani 1 1 d . . . . .
C1 C 0.56553(17) 0.43434(19) 0.5333(2) 0.1098(9) Uani 1 1 d . . . . .
H1A H 0.585764 0.461787 0.507472 0.132 Uiso 1 1 calc R U . . .
C2 C 0.5968(2) 0.4105(2) 0.5849(3) 0.1366(17) Uani 1 1 d . . . . .
H2A H 0.636533 0.423438 0.593890 0.164 Uiso 1 1 calc R U . . .
C3 C 0.5689(3) 0.3690(3) 0.6209(3) 0.1447(19) Uani 1 1 d . . . . .
H3A H 0.589491 0.352578 0.654613 0.174 Uiso 1 1 calc R U . . .
C4 C 0.5100(2) 0.3508(2) 0.6081(3) 0.1246(13) Uani 1 1 d . . . . .
H4A H 0.490354 0.321894 0.632858 0.150 Uiso 1 1 calc R U . . .
C5 C 0.47997(16) 0.37593(16) 0.55796(17) 0.0990(7) Uani 1 1 d . . . . .
C6 C 0.41576(15) 0.36313(15) 0.54169(15) 0.0938(7) Uani 1 1 d . . . . .
C7 C 0.36931(19) 0.32937(17) 0.56927(16) 0.1023(8) Uani 1 1 d . . . . .
H7A H 0.371826 0.306701 0.605486 0.123 Uiso 1 1 calc R U . . .
C8 C 0.31837(16) 0.33639(17) 0.53172(14) 0.0965(7) Uani 1 1 d . . . . .
C9 C 0.20868(16) 0.3298(2) 0.49939(16) 0.1049(8) Uani 1 1 d . . . . .
H9A H 0.216736 0.357621 0.467901 0.126 Uiso 1 1 calc R U . . .
C10 C 0.25576(17) 0.31190(19) 0.53796(14) 0.1030(8) Uani 1 1 d . . . . .
C11 C 0.2444(3) 0.2702(3) 0.5858(2) 0.1316(15) Uani 1 1 d . . . . .
H11A H 0.275905 0.258031 0.612076 0.158 Uiso 1 1 calc R U . . .
C12 C 0.1846(3) 0.2470(4) 0.5933(3) 0.168(3) Uani 1 1 d . . . . .
H12A H 0.176696 0.218410 0.624163 0.202 Uiso 1 1 calc R U . . .
C13 C 0.1384(3) 0.2658(4) 0.5563(3) 0.159(2) Uani 1 1 d . . . . .
H13A H 0.098756 0.251534 0.563547 0.191 Uiso 1 1 calc R U . . .
C14 C 0.14877(18) 0.3067(3) 0.50680(17) 0.1182(12) Uani 1 1 d . . . . .
C15 C 0.11276(15) 0.3072(2) 0.39971(18) 0.1078(9) Uani 1 1 d . . . . .
H15A H 0.151274 0.292002 0.388854 0.129 Uiso 1 1 calc R U . . .
C16 C 0.10133(17) 0.3211(2) 0.46127(19) 0.1164(11) Uani 1 1 d . . . . .
C17 C 0.0441(2) 0.3455(5) 0.4759(3) 0.169(3) Uani 1 1 d . . . . .
H17A H 0.035281 0.356122 0.516426 0.203 Uiso 1 1 calc R U . . .
C18 C 0.0006(3) 0.3539(5) 0.4313(3) 0.177(3) Uani 1 1 d . . . . .
H18A H -0.038135 0.368629 0.442003 0.212 Uiso 1 1 calc R U . . .
C19 C 0.0134(2) 0.3409(4) 0.3713(3) 0.149(2) Uani 1 1 d . . . . .
H19A H -0.015629 0.349402 0.340985 0.179 Uiso 1 1 calc R U . . .
C20 C 0.07002(16) 0.3149(2) 0.35519(19) 0.1099(10) Uani 1 1 d . . . . .
C21 C 0.08023(15) 0.29288(18) 0.29137(17) 0.0995(8) Uani 1 1 d . . . . .
C22 C 0.04449(18) 0.29541(19) 0.23986(19) 0.1081(9) Uani 1 1 d . . . . .
H22A H 0.006842 0.315266 0.235373 0.130 Uiso 1 1 calc R U . . .
C23 C 0.07602(17) 0.26224(17) 0.19578(17) 0.1003(7) Uani 1 1 d . . . . .
C24 C 0.0617(2) 0.2442(2) 0.13158(19) 0.1113(10) Uani 1 1 d . . . . .
C25 C 0.0111(3) 0.2675(3) 0.1015(3) 0.150(2) Uani 1 1 d . . . . .
H25A H -0.016052 0.294413 0.120775 0.180 Uiso 1 1 calc R U . . .
C26 C 0.0025(5) 0.2485(4) 0.0400(4) 0.194(4) Uani 1 1 d . . . . .
H26A H -0.029864 0.264185 0.016781 0.232 Uiso 1 1 calc R U . . .
C27 C 0.0411(4) 0.2078(4) 0.0155(3) 0.166(3) Uani 1 1 d . . . . .
H27A H 0.034329 0.193562 -0.024242 0.199 Uiso 1 1 calc R U . . .
C28 C 0.0913(3) 0.1864(3) 0.0484(2) 0.1431(17) Uani 1 1 d . . . . .
H28A H 0.118835 0.159637 0.029486 0.172 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31139(2) 0.31139(2) 0.31139(2) 0.0912(2) Uani 1 3 d S T P . .
O1 O 0.27851(10) 0.38095(11) 0.36253(9) 0.0910(5) Uani 1 1 d . . . . .
O2 O 0.24951(11) 0.34251(11) 0.25130(10) 0.0947(5) Uani 1 1 d . . . . .
O3 O 0.1056(3) 0.5014(3) 0.2315(2) 0.208(3) Uani 1 1 d . U . . .
O4 O 0.1307(3) 0.5366(3) 0.3481(2) 0.190(3) Uani 1 1 d . U . . .
C29 C 0.23477(14) 0.41139(16) 0.33575(13) 0.0901(6) Uani 1 1 d . . . . .
C30 C 0.21912(14) 0.39028(16) 0.27169(14) 0.0922(6) Uani 1 1 d . . . . .
C31 C 0.17604(19) 0.4201(2) 0.23711(18) 0.1175(12) Uani 1 1 d . . . . .
H31A H 0.166938 0.406313 0.197623 0.141 Uiso 1 1 calc R U . . .
C32 C 0.1449(2) 0.4727(3) 0.2618(2) 0.1351(16) Uani 1 1 d . U . . .
C33 C 0.1593(2) 0.4933(3) 0.3271(2) 0.1294(15) Uani 1 1 d . U . . .
C34 C 0.20442(16) 0.4597(2) 0.36110(17) 0.1062(9) Uani 1 1 d . . . . .
H34A H 0.213201 0.471212 0.401382 0.127 Uiso 1 1 calc R U . . .
B1 B -0.1114(9) 0.3883(9) 0.1094(11) 0.182(5) Uani 0.3333 1 d D U P A -1
F1 F -0.0627(10) 0.3889(11) 0.1490(11) 0.238(10) Uani 0.3333 1 d D U P A -1
F2 F -0.0963(12) 0.422(2) 0.0587(15) 0.269(10) Uani 0.3333 1 d D U P A -1
F3 F -0.1622(10) 0.4143(15) 0.1368(14) 0.211(9) Uani 0.3333 1 d D U P A -1
F4 F -0.1260(12) 0.3294(10) 0.0924(18) 0.217(10) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.001(3) 9 ?
Fe1 N2 2.001(3) 5 ?
Fe1 N2 2.001(3) . ?
Fe1 N1 2.052(3) . ?
Fe1 N1 2.052(3) 9 ?
Fe1 N1 2.052(3) 5 ?
Fe2 N5 2.071(3) . ?
Fe2 N5 2.071(3) 5 ?
Fe2 N5 2.071(3) 9 ?
Fe2 N6 2.128(3) . ?
Fe2 N6 2.128(3) 9 ?
Fe2 N6 2.128(3) 5 ?
N1 C1 1.336(5) . ?
N1 C5 1.364(5) . ?
N2 C6 1.339(4) . ?
N2 N3 1.348(4) . ?
N3 C8 1.369(4) . ?
N3 H3 0.87(3) . ?
N4 N5 1.350(4) . ?
N4 C21 1.365(5) . ?
N4 H4 0.88(3) . ?
N5 C23 1.346(4) . ?
N6 C24 1.341(6) . ?
N6 C28 1.345(6) . ?
C1 C2 1.409(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.338(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.368(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.383(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.466(5) . ?
C6 C7 1.384(5) . ?
C7 C8 1.384(5) . ?
C7 H7A 0.9300 . ?
C8 C10 1.467(5) . ?
C9 C10 1.379(6) . ?
C9 C14 1.404(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.402(6) . ?
C11 C12 1.403(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.350(10) . ?
C12 H12A 0.9300 . ?
C13 C14 1.413(8) . ?
C13 H13A 0.9300 . ?
C14 C16 1.463(7) . ?
C15 C20 1.352(6) . ?
C15 C16 1.394(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.389(6) . ?
C17 C18 1.366(10) . ?
C17 H17A 0.9300 . ?
C18 C19 1.363(9) . ?
C18 H18A 0.9300 . ?
C19 C20 1.399(6) . ?
C19 H19A 0.9300 . ?
C20 C21 1.484(5) . ?
C21 C22 1.363(5) . ?
C22 C23 1.381(6) . ?
C22 H22A 0.9300 . ?
C23 C24 1.482(6) . ?
C24 C25 1.375(6) . ?
C25 C26 1.413(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.329(11) . ?
C26 H26A 0.9300 . ?
C27 C28 1.384(9) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.993(2) 5 ?
Fe3 O2 1.993(2) . ?
Fe3 O2 1.993(2) 9 ?
Fe3 O1 2.008(2) . ?
Fe3 O1 2.008(2) 5 ?
Fe3 O1 2.008(2) 9 ?
O1 C29 1.296(4) . ?
O2 C30 1.308(4) . ?
O3 C32 1.246(6) . ?
O4 C33 1.216(6) . ?
C29 C34 1.357(5) . ?
C29 C30 1.505(4) . ?
C30 C31 1.364(5) . ?
C31 C32 1.433(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.521(7) . ?
C33 C34 1.428(6) . ?
C34 H34A 0.9300 . ?
B1 F2 1.359(19) . ?
B1 F1 1.364(19) . ?
B1 F4 1.368(18) . ?
B1 F3 1.38(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.44(10) 9 5 ?
N2 Fe1 N2 96.44(10) 9 . ?
N2 Fe1 N2 96.44(10) 5 . ?
N2 Fe1 N1 170.99(11) 9 . ?
N2 Fe1 N1 92.05(11) 5 . ?
N2 Fe1 N1 79.56(11) . . ?
N2 Fe1 N1 79.56(11) 9 9 ?
N2 Fe1 N1 170.99(11) 5 9 ?
N2 Fe1 N1 92.05(11) . 9 ?
N1 Fe1 N1 92.45(11) . 9 ?
N2 Fe1 N1 92.05(11) 9 5 ?
N2 Fe1 N1 79.56(11) 5 5 ?
N2 Fe1 N1 170.99(11) . 5 ?
N1 Fe1 N1 92.45(11) . 5 ?
N1 Fe1 N1 92.45(11) 9 5 ?
N5 Fe2 N5 97.88(10) . 5 ?
N5 Fe2 N5 97.88(10) . 9 ?
N5 Fe2 N5 97.88(10) 5 9 ?
N5 Fe2 N6 77.07(12) . . ?
N5 Fe2 N6 167.72(12) 5 . ?
N5 Fe2 N6 93.93(13) 9 . ?
N5 Fe2 N6 167.71(12) . 9 ?
N5 Fe2 N6 93.93(13) 5 9 ?
N5 Fe2 N6 77.06(12) 9 9 ?
N6 Fe2 N6 91.99(14) . 9 ?
N5 Fe2 N6 93.93(13) . 5 ?
N5 Fe2 N6 77.06(12) 5 5 ?
N5 Fe2 N6 167.71(12) 9 5 ?
N6 Fe2 N6 91.99(14) . 5 ?
N6 Fe2 N6 91.99(14) 9 5 ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Fe1 127.5(3) . . ?
C5 N1 Fe1 114.5(2) . . ?
C6 N2 N3 106.0(3) . . ?
C6 N2 Fe1 116.0(2) . . ?
N3 N2 Fe1 136.4(2) . . ?
N2 N3 C8 110.9(3) . . ?
N2 N3 H3 123(4) . . ?
C8 N3 H3 126(4) . . ?
N5 N4 C21 110.6(3) . . ?
N5 N4 H4 119(4) . . ?
C21 N4 H4 130(4) . . ?
C23 N5 N4 105.2(3) . . ?
C23 N5 Fe2 115.9(2) . . ?
N4 N5 Fe2 135.3(2) . . ?
C24 N6 C28 117.2(4) . . ?
C24 N6 Fe2 115.2(3) . . ?
C28 N6 Fe2 127.5(4) . . ?
N1 C1 C2 121.4(4) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C3 C2 C1 119.7(4) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 120.0(4) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 119.1(5) . . ?
C3 C4 H4A 120.4 . . ?
C5 C4 H4A 120.4 . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C6 113.7(3) . . ?
C4 C5 C6 124.3(4) . . ?
N2 C6 C7 111.0(3) . . ?
N2 C6 C5 115.4(3) . . ?
C7 C6 C5 133.6(3) . . ?
C8 C7 C6 105.6(3) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.5(3) . . ?
N3 C8 C10 123.1(3) . . ?
C7 C8 C10 130.3(3) . . ?
C10 C9 C14 121.2(4) . . ?
C10 C9 H9A 119.4 . . ?
C14 C9 H9A 119.4 . . ?
C9 C10 C11 120.2(4) . . ?
C9 C10 C8 122.0(3) . . ?
C11 C10 C8 117.8(4) . . ?
C10 C11 C12 118.8(5) . . ?
C10 C11 H11A 120.6 . . ?
C12 C11 H11A 120.6 . . ?
C13 C12 C11 120.7(5) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C12 C13 C14 121.8(5) . . ?
C12 C13 H13A 119.1 . . ?
C14 C13 H13A 119.1 . . ?
C9 C14 C13 117.3(5) . . ?
C9 C14 C16 120.0(4) . . ?
C13 C14 C16 122.5(4) . . ?
C20 C15 C16 122.5(3) . . ?
C20 C15 H15A 118.7 . . ?
C16 C15 H15A 118.7 . . ?
C17 C16 C15 117.5(5) . . ?
C17 C16 C14 123.9(4) . . ?
C15 C16 C14 118.5(3) . . ?
C18 C17 C16 120.5(5) . . ?
C18 C17 H17A 119.7 . . ?
C16 C17 H17A 119.7 . . ?
C19 C18 C17 120.7(5) . . ?
C19 C18 H18A 119.7 . . ?
C17 C18 H18A 119.7 . . ?
C18 C19 C20 120.1(5) . . ?
C18 C19 H19A 119.9 . . ?
C20 C19 H19A 119.9 . . ?
C15 C20 C19 118.4(4) . . ?
C15 C20 C21 121.8(3) . . ?
C19 C20 C21 119.7(4) . . ?
C22 C21 N4 107.6(3) . . ?
C22 C21 C20 132.0(3) . . ?
N4 C21 C20 120.2(3) . . ?
C21 C22 C23 105.4(3) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 111.2(3) . . ?
N5 C23 C24 115.3(3) . . ?
C22 C23 C24 133.4(3) . . ?
N6 C24 C25 124.4(4) . . ?
N6 C24 C23 114.5(3) . . ?
C25 C24 C23 121.1(4) . . ?
C24 C25 C26 116.6(6) . . ?
C24 C25 H25A 121.7 . . ?
C26 C25 H25A 121.7 . . ?
C27 C26 C25 119.3(6) . . ?
C27 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
C26 C27 C28 121.0(5) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
N6 C28 C27 121.4(6) . . ?
N6 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
O2 Fe3 O2 90.53(10) 5 . ?
O2 Fe3 O2 90.53(10) 5 9 ?
O2 Fe3 O2 90.53(10) . 9 ?
O2 Fe3 O1 95.00(10) 5 . ?
O2 Fe3 O1 82.36(8) . . ?
O2 Fe3 O1 171.02(9) 9 . ?
O2 Fe3 O1 82.36(8) 5 5 ?
O2 Fe3 O1 171.02(9) . 5 ?
O2 Fe3 O1 94.99(10) 9 5 ?
O1 Fe3 O1 92.75(9) . 5 ?
O2 Fe3 O1 171.02(9) 5 9 ?
O2 Fe3 O1 95.00(10) . 9 ?
O2 Fe3 O1 82.36(8) 9 9 ?
O1 Fe3 O1 92.75(9) . 9 ?
O1 Fe3 O1 92.75(9) 5 9 ?
C29 O1 Fe3 113.37(19) . . ?
C30 O2 Fe3 112.84(19) . . ?
O1 C29 C34 124.7(3) . . ?
O1 C29 C30 115.2(3) . . ?
C34 C29 C30 120.1(3) . . ?
O2 C30 C31 122.5(3) . . ?
O2 C30 C29 116.2(3) . . ?
C31 C30 C29 121.3(3) . . ?
C30 C31 C32 119.8(3) . . ?
C30 C31 H31A 120.1 . . ?
C32 C31 H31A 120.1 . . ?
O3 C32 C31 121.7(5) . . ?
O3 C32 C33 119.1(5) . . ?
C31 C32 C33 119.2(4) . . ?
O4 C33 C34 123.6(4) . . ?
O4 C33 C32 118.2(4) . . ?
C34 C33 C32 118.2(4) . . ?
C29 C34 C33 121.3(3) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F1 108.5(15) . . ?
F2 B1 F4 109.6(18) . . ?
F1 B1 F4 111.1(17) . . ?
F2 B1 F3 109.0(17) . . ?
F1 B1 F3 110.1(17) . . ?
F4 B1 F3 108.5(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.87(3) 2.11(3) 2.932(3) 158(6) . yes
N4 H4 O2 0.88(3) 2.16(4) 2.976(4) 154(6) 5 yes

_refine_diff_density_max         0.354
_refine_diff_density_min         -0.258
_refine_diff_density_rms         0.074

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_400K
_database_code_depnum_ccdc_archive 'CCDC 2261731'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.809(3)
_cell_length_b                   21.809(3)
_cell_length_c                   21.809(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10373(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    5553
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      31.15

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.274
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.519
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            157894
_diffrn_reflns_av_unetI/netI     0.0206
_diffrn_reflns_av_R_equivalents  0.0510
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.916
_diffrn_reflns_theta_max         28.646
_diffrn_reflns_theta_full        28.646
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8252
_reflns_number_gt                7489
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.856
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with 1,2 distance
 restraints as well as displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;

_vrf_PLAT601_lb2205_fresh2_400K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1842 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1842 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1095P)²+0.0469P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0038(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3226 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.079(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8252
_refine_ls_number_parameters     459
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0413
_refine_ls_wR_factor_ref         0.1376
_refine_ls_wR_factor_gt          0.1333
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29847(2) 0.29847(2) 0.29847(2) 0.08814(18) Uani 1 3 d S T P . .
Fe2 Fe 0.57962(2) 0.57962(2) 0.57962(2) 0.09148(19) Uani 1 3 d S T P . .
N1 N 0.22921(15) 0.33297(13) 0.24303(12) 0.1048(7) Uani 1 1 d . . . . .
N2 N 0.26061(11) 0.36180(12) 0.35399(12) 0.0946(5) Uani 1 1 d . . . . .
N3 N 0.26536(11) 0.37807(14) 0.41401(12) 0.0976(6) Uani 1 1 d D . . . .
H3 H 0.3019(17) 0.369(3) 0.434(2) 0.146 Uiso 1 1 d D U . . .
N4 N 0.47087(12) 0.48994(15) 0.61779(11) 0.0991(6) Uani 1 1 d D . . . .
H4 H 0.4368(18) 0.494(3) 0.593(2) 0.149 Uiso 1 1 d D U . . .
N5 N 0.52963(12) 0.50829(14) 0.61935(12) 0.0985(6) Uani 1 1 d . . . . .
N6 N 0.64093(14) 0.54461(16) 0.64786(17) 0.1144(7) Uani 1 1 d . . . . .
C1 C 0.2167(2) 0.3165(2) 0.18499(17) 0.1218(11) Uani 1 1 d . . . . .
H1A H 0.241768 0.287838 0.165802 0.146 Uiso 1 1 calc R U . . .
C2 C 0.1678(3) 0.3407(3) 0.1530(2) 0.151(2) Uani 1 1 d . . . . .
H2A H 0.160694 0.329178 0.112560 0.181 Uiso 1 1 calc R U . . .
C3 C 0.1302(3) 0.3817(3) 0.1812(3) 0.162(2) Uani 1 1 d . . . . .
H3B H 0.095246 0.395983 0.161355 0.194 Uiso 1 1 calc R U . . .
C4 C 0.1442(3) 0.4019(2) 0.2394(2) 0.1394(15) Uani 1 1 d . . . . .
H4B H 0.121549 0.433008 0.257774 0.167 Uiso 1 1 calc R U . . .
C5 C 0.19308(17) 0.37471(16) 0.26995(16) 0.1062(8) Uani 1 1 d . . . . .
C6 C 0.20910(15) 0.38872(15) 0.33388(15) 0.1000(7) Uani 1 1 d . . . . .
C7 C 0.18125(15) 0.42259(18) 0.37883(19) 0.1092(8) Uani 1 1 d . . . . .
H7A H 0.145361 0.445358 0.375341 0.131 Uiso 1 1 calc R U . . .
C8 C 0.21811(14) 0.41586(17) 0.43139(16) 0.1032(7) Uani 1 1 d . . . . .
C9 C 0.21144(15) 0.44059(19) 0.49295(18) 0.1109(9) Uani 1 1 d . . . . .
C10 C 0.1647(2) 0.4818(3) 0.5049(3) 0.1474(18) Uani 1 1 d . . . . .
H10A H 0.138841 0.494320 0.473401 0.177 Uiso 1 1 calc R U . . .
C11 C 0.1562(3) 0.5044(5) 0.5628(3) 0.197(4) Uani 1 1 d . . . . .
H11A H 0.125582 0.533092 0.570208 0.236 Uiso 1 1 calc R U . . .
C12 C 0.1927(3) 0.4847(4) 0.6100(3) 0.173(3) Uani 1 1 d . . . . .
H12A H 0.184149 0.497858 0.649636 0.208 Uiso 1 1 calc R U . . .
C13 C 0.24227(17) 0.4456(3) 0.60021(18) 0.1277(13) Uani 1 1 d . . . . .
C14 C 0.24981(15) 0.4230(2) 0.53985(16) 0.1105(9) Uani 1 1 d . . . . .
H14A H 0.281456 0.395613 0.531690 0.133 Uiso 1 1 calc R U . . .
C15 C 0.28705(19) 0.4302(3) 0.64674(17) 0.1279(13) Uani 1 1 d . . . . .
C16 C 0.2721(3) 0.4057(4) 0.7039(2) 0.174(3) Uani 1 1 d . . . . .
H16A H 0.231732 0.394961 0.712442 0.209 Uiso 1 1 calc R U . . .
C17 C 0.3164(3) 0.3974(4) 0.7476(2) 0.173(3) Uani 1 1 d . . . . .
H17A H 0.305224 0.382870 0.786059 0.208 Uiso 1 1 calc R U . . .
C18 C 0.3762(3) 0.4097(4) 0.7361(2) 0.157(2) Uani 1 1 d . . . . .
H18A H 0.406010 0.401522 0.765489 0.189 Uiso 1 1 calc R U . . .
C19 C 0.39269(18) 0.4354(2) 0.67851(15) 0.1146(10) Uani 1 1 d . . . . .
C20 C 0.34793(17) 0.4440(2) 0.63604(15) 0.1121(9) Uani 1 1 d . . . . .
H20A H 0.358786 0.459957 0.598009 0.135 Uiso 1 1 calc R U . . .
C21 C 0.45641(16) 0.45664(17) 0.66839(15) 0.1033(8) Uani 1 1 d . . . . .
C22 C 0.5083(2) 0.45483(19) 0.70462(17) 0.1147(9) Uani 1 1 d . . . . .
H22A H 0.512699 0.436275 0.742761 0.138 Uiso 1 1 calc R U . . .
C23 C 0.55249(17) 0.48667(17) 0.67179(16) 0.1047(8) Uani 1 1 d . . . . .
C24 C 0.61584(18) 0.5039(2) 0.68693(19) 0.1157(9) Uani 1 1 d . . . . .
C25 C 0.6473(3) 0.4807(3) 0.7363(3) 0.1508(19) Uani 1 1 d . . . . .
H25A H 0.627963 0.454250 0.763580 0.181 Uiso 1 1 calc R U . . .
C26 C 0.7062(3) 0.4964(4) 0.7449(4) 0.191(3) Uani 1 1 d . . . . .
H26A H 0.728349 0.479872 0.777331 0.229 Uiso 1 1 calc R U . . .
C27 C 0.7345(3) 0.5386(4) 0.7037(4) 0.182(3) Uani 1 1 d . . . . .
H27A H 0.775491 0.549562 0.707909 0.219 Uiso 1 1 calc R U . . .
C28 C 0.6991(2) 0.5625(3) 0.6577(3) 0.1471(17) Uani 1 1 d . . . . .
H28A H 0.716001 0.592270 0.632289 0.177 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43770(2) 0.43770(2) 0.43770(2) 0.09267(19) Uani 1 3 d S T P . .
O1 O 0.38638(9) 0.36898(10) 0.47109(10) 0.0939(4) Uani 1 1 d . . . . .
O2 O 0.49768(9) 0.40693(10) 0.49966(11) 0.0964(5) Uani 1 1 d . . . . .
O3 O 0.5146(2) 0.2531(4) 0.6476(3) 0.232(4) Uani 1 1 d . . . . .
O4 O 0.3990(2) 0.2175(3) 0.6224(2) 0.204(3) Uani 1 1 d . U . . .
C29 C 0.41247(13) 0.33969(15) 0.51600(13) 0.0928(6) Uani 1 1 d . . . . .
C30 C 0.47700(13) 0.36032(15) 0.53089(13) 0.0947(6) Uani 1 1 d . . . . .
C31 C 0.51039(17) 0.3320(2) 0.57461(19) 0.1254(13) Uani 1 1 d . . . . .
H31A H 0.549973 0.345573 0.582839 0.150 Uiso 1 1 calc R U . . .
C32 C 0.4861(2) 0.2820(3) 0.6082(2) 0.1462(18) Uani 1 1 d . U . . .
C33 C 0.4200(2) 0.2606(3) 0.5935(2) 0.1379(16) Uani 1 1 d . U . . .
C34 C 0.38664(17) 0.2927(2) 0.54672(17) 0.1122(9) Uani 1 1 d . . . . .
H34A H 0.346698 0.281002 0.537488 0.135 Uiso 1 1 calc R U . . .
B1 B 0.1392(12) 0.1359(12) 0.1398(9) 0.240(8) Uani 0.3333 1 d D U P A -1
F1 F 0.1259(13) 0.1775(14) 0.0921(7) 0.254(11) Uani 0.3333 1 d D U P A -1
F2 F 0.1914(10) 0.1549(12) 0.1695(13) 0.312(11) Uani 0.3333 1 d D U P A -1
F3 F 0.0890(12) 0.1342(11) 0.1780(10) 0.265(11) Uani 0.3333 1 d D U P A -1
F4 F 0.1464(12) 0.0786(10) 0.1124(11) 0.297(11) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.014(3) 9 ?
Fe1 N2 2.014(3) 5 ?
Fe1 N2 2.014(3) . ?
Fe1 N1 2.076(3) . ?
Fe1 N1 2.076(3) 9 ?
Fe1 N1 2.076(3) 5 ?
Fe2 N5 2.088(3) 9 ?
Fe2 N5 2.088(3) 5 ?
Fe2 N5 2.088(3) . ?
Fe2 N6 2.141(3) . ?
Fe2 N6 2.141(3) 9 ?
Fe2 N6 2.141(3) 5 ?
N1 C5 1.339(5) . ?
N1 C1 1.344(5) . ?
N2 C6 1.341(4) . ?
N2 N3 1.360(4) . ?
N3 C8 1.373(4) . ?
N3 H3 0.93(3) . ?
N4 N5 1.343(4) . ?
N4 C21 1.358(4) . ?
N4 H4 0.92(3) . ?
N5 C23 1.334(4) . ?
N6 C28 1.346(6) . ?
N6 C24 1.347(6) . ?
C1 C2 1.379(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.361(9) . ?
C2 H2A 0.9300 . ?
C3 C4 1.378(8) . ?
C3 H3B 0.9300 . ?
C4 C5 1.390(6) . ?
C4 H4B 0.9300 . ?
C5 C6 1.469(5) . ?
C6 C7 1.370(5) . ?
C7 C8 1.408(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.454(5) . ?
C9 C14 1.376(6) . ?
C9 C10 1.385(6) . ?
C10 C11 1.367(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.369(10) . ?
C11 H11A 0.9300 . ?
C12 C13 1.393(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.416(5) . ?
C13 C15 1.448(7) . ?
C14 H14A 0.9300 . ?
C15 C20 1.381(5) . ?
C15 C16 1.395(6) . ?
C16 C17 1.369(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.354(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.422(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.359(6) . ?
C19 C21 1.481(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.381(5) . ?
C22 C23 1.387(6) . ?
C22 H22A 0.9300 . ?
C23 C24 1.469(5) . ?
C24 C25 1.373(6) . ?
C25 C26 1.342(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.428(11) . ?
C26 H26A 0.9300 . ?
C27 C28 1.367(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.997(2) 5 ?
Fe3 O2 1.997(2) 9 ?
Fe3 O2 1.997(2) . ?
Fe3 O1 2.007(2) 9 ?
Fe3 O1 2.007(2) 5 ?
Fe3 O1 2.007(2) . ?
O1 C29 1.301(4) . ?
O2 C30 1.304(4) . ?
O3 C32 1.233(6) . ?
O4 C33 1.219(6) . ?
C29 C34 1.347(5) . ?
C29 C30 1.513(4) . ?
C30 C31 1.349(5) . ?
C31 C32 1.415(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.551(6) . ?
C33 C34 1.436(6) . ?
C34 H34A 0.9300 . ?
B1 F2 1.37(2) . ?
B1 F3 1.38(2) . ?
B1 F4 1.39(2) . ?
B1 F1 1.410(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.62(9) 9 5 ?
N2 Fe1 N2 96.62(9) 9 . ?
N2 Fe1 N2 96.62(9) 5 . ?
N2 Fe1 N1 92.43(11) 9 . ?
N2 Fe1 N1 170.25(11) 5 . ?
N2 Fe1 N1 78.65(10) . . ?
N2 Fe1 N1 78.66(10) 9 9 ?
N2 Fe1 N1 92.43(11) 5 9 ?
N2 Fe1 N1 170.25(11) . 9 ?
N1 Fe1 N1 92.93(11) . 9 ?
N2 Fe1 N1 170.25(11) 9 5 ?
N2 Fe1 N1 78.66(10) 5 5 ?
N2 Fe1 N1 92.42(11) . 5 ?
N1 Fe1 N1 92.93(11) . 5 ?
N1 Fe1 N1 92.93(11) 9 5 ?
N5 Fe2 N5 97.86(10) 9 5 ?
N5 Fe2 N5 97.86(10) 9 . ?
N5 Fe2 N5 97.86(10) 5 . ?
N5 Fe2 N6 167.44(12) 9 . ?
N5 Fe2 N6 94.16(12) 5 . ?
N5 Fe2 N6 76.82(11) . . ?
N5 Fe2 N6 76.82(11) 9 9 ?
N5 Fe2 N6 167.44(12) 5 9 ?
N5 Fe2 N6 94.16(12) . 9 ?
N6 Fe2 N6 92.09(13) . 9 ?
N5 Fe2 N6 94.16(12) 9 5 ?
N5 Fe2 N6 76.82(11) 5 5 ?
N5 Fe2 N6 167.44(12) . 5 ?
N6 Fe2 N6 92.09(13) . 5 ?
N6 Fe2 N6 92.09(13) 9 5 ?
C5 N1 C1 118.4(3) . . ?
C5 N1 Fe1 114.8(2) . . ?
C1 N1 Fe1 126.8(3) . . ?
C6 N2 N3 105.3(3) . . ?
C6 N2 Fe1 116.5(2) . . ?
N3 N2 Fe1 136.6(2) . . ?
N2 N3 C8 111.4(3) . . ?
N2 N3 H3 117(4) . . ?
C8 N3 H3 130(4) . . ?
N5 N4 C21 111.1(3) . . ?
N5 N4 H4 140(4) . . ?
C21 N4 H4 109(4) . . ?
C23 N5 N4 105.8(3) . . ?
C23 N5 Fe2 115.1(2) . . ?
N4 N5 Fe2 135.2(2) . . ?
C28 N6 C24 118.2(4) . . ?
C28 N6 Fe2 126.7(3) . . ?
C24 N6 Fe2 114.9(2) . . ?
N1 C1 C2 122.1(5) . . ?
N1 C1 H1A 119.0 . . ?
C2 C1 H1A 119.0 . . ?
C3 C2 C1 119.3(4) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3B 120.2 . . ?
C4 C3 H3B 120.2 . . ?
C3 C4 C5 118.4(5) . . ?
C3 C4 H4B 120.8 . . ?
C5 C4 H4B 120.8 . . ?
N1 C5 C4 122.1(4) . . ?
N1 C5 C6 114.7(3) . . ?
C4 C5 C6 123.3(4) . . ?
N2 C6 C7 111.9(3) . . ?
N2 C6 C5 114.7(3) . . ?
C7 C6 C5 133.3(3) . . ?
C6 C7 C8 105.9(3) . . ?
C6 C7 H7A 127.1 . . ?
C8 C7 H7A 127.1 . . ?
N3 C8 C7 105.4(3) . . ?
N3 C8 C9 123.6(3) . . ?
C7 C8 C9 131.0(3) . . ?
C14 C9 C10 119.2(4) . . ?
C14 C9 C8 121.5(3) . . ?
C10 C9 C8 119.3(4) . . ?
C11 C10 C9 120.5(6) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 120.2(6) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
C11 C12 C13 121.9(5) . . ?
C11 C12 H12A 119.1 . . ?
C13 C12 H12A 119.1 . . ?
C12 C13 C14 116.5(4) . . ?
C12 C13 C15 124.0(4) . . ?
C14 C13 C15 119.5(4) . . ?
C9 C14 C13 121.6(4) . . ?
C9 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
C20 C15 C16 117.3(5) . . ?
C20 C15 C13 118.6(4) . . ?
C16 C15 C13 123.9(4) . . ?
C17 C16 C15 120.5(5) . . ?
C17 C16 H16A 119.8 . . ?
C15 C16 H16A 119.8 . . ?
C18 C17 C16 121.7(4) . . ?
C18 C17 H17A 119.2 . . ?
C16 C17 H17A 119.2 . . ?
C17 C18 C19 119.0(5) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.4(4) . . ?
C20 C19 C21 122.0(3) . . ?
C18 C19 C21 119.5(4) . . ?
C19 C20 C15 123.1(3) . . ?
C19 C20 H20A 118.5 . . ?
C15 C20 H20A 118.5 . . ?
N4 C21 C22 106.8(3) . . ?
N4 C21 C19 120.4(3) . . ?
C22 C21 C19 132.4(3) . . ?
C21 C22 C23 105.1(3) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.1(3) . . ?
N5 C23 C24 117.0(3) . . ?
C22 C23 C24 131.7(3) . . ?
N6 C24 C25 122.4(4) . . ?
N6 C24 C23 114.1(3) . . ?
C25 C24 C23 123.5(4) . . ?
C26 C25 C24 119.6(6) . . ?
C26 C25 H25A 120.2 . . ?
C24 C25 H25A 120.2 . . ?
C25 C26 C27 119.4(5) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C28 C27 C26 117.6(5) . . ?
C28 C27 H27A 121.2 . . ?
C26 C27 H27A 121.2 . . ?
N6 C28 C27 122.6(6) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 90.24(9) 5 9 ?
O2 Fe3 O2 90.24(9) 5 . ?
O2 Fe3 O2 90.24(9) 9 . ?
O2 Fe3 O1 94.60(9) 5 9 ?
O2 Fe3 O1 82.46(8) 9 9 ?
O2 Fe3 O1 171.25(9) . 9 ?
O2 Fe3 O1 82.46(8) 5 5 ?
O2 Fe3 O1 171.25(9) 9 5 ?
O2 Fe3 O1 94.60(9) . 5 ?
O1 Fe3 O1 93.26(9) 9 5 ?
O2 Fe3 O1 171.25(9) 5 . ?
O2 Fe3 O1 94.60(9) 9 . ?
O2 Fe3 O1 82.46(8) . . ?
O1 Fe3 O1 93.26(9) 9 . ?
O1 Fe3 O1 93.26(9) 5 . ?
C29 O1 Fe3 113.34(18) . . ?
C30 O2 Fe3 112.88(18) . . ?
O1 C29 C34 124.4(3) . . ?
O1 C29 C30 115.0(3) . . ?
C34 C29 C30 120.6(3) . . ?
O2 C30 C31 122.6(3) . . ?
O2 C30 C29 116.2(3) . . ?
C31 C30 C29 121.2(3) . . ?
C30 C31 C32 121.1(3) . . ?
C30 C31 H31A 119.5 . . ?
C32 C31 H31A 119.5 . . ?
O3 C32 C31 124.5(5) . . ?
O3 C32 C33 117.2(5) . . ?
C31 C32 C33 118.3(3) . . ?
O4 C33 C34 123.6(4) . . ?
O4 C33 C32 118.4(4) . . ?
C34 C33 C32 118.0(4) . . ?
C29 C34 C33 120.9(3) . . ?
C29 C34 H34A 119.6 . . ?
C33 C34 H34A 119.6 . . ?
F2 B1 F3 112.4(17) . . ?
F2 B1 F4 112.3(18) . . ?
F3 B1 F4 109.1(18) . . ?
F2 B1 F1 108.9(18) . . ?
F3 B1 F1 107.5(17) . . ?
F4 B1 F1 106.4(15) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.93(3) 2.02(3) 2.925(3) 167(5) . yes
N4 H4 O2 0.92(3) 2.19(4) 2.975(3) 143(5) 9 yes

_refine_diff_density_max         0.254
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.040

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_380K
_database_code_depnum_ccdc_archive 'CCDC 2261730'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.768(3)
_cell_length_b                   21.768(3)
_cell_length_c                   21.768(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10315(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    380(2)
_cell_measurement_reflns_used    5715
_cell_measurement_theta_min      1.37
_cell_measurement_theta_max      31.60

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      380(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            161073
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.358
_diffrn_reflns_theta_max         29.085
_diffrn_reflns_theta_full        29.085
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8533
_reflns_number_gt                7577
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;

_vrf_PLAT601_lb2205_fresh2_380K  
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1800 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1800 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1089P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0096(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3244 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.071(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8533
_refine_ls_number_parameters     458
_refine_ls_number_restraints     84
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.1362
_refine_ls_wR_factor_gt          0.1323
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45194(2) 0.45194(2) 0.45194(2) 0.08396(17) Uani 1 3 d S T P . .
Fe2 Fe 0.16975(2) 0.16975(2) 0.16975(2) 0.08893(19) Uani 1 3 d S T P . .
N1 N 0.50747(11) 0.41770(12) 0.52050(14) 0.0983(6) Uani 1 1 d . . . . .
N2 N 0.39603(11) 0.38898(12) 0.48958(11) 0.0900(5) Uani 1 1 d . . . . .
N3 N 0.33629(11) 0.37314(13) 0.48469(11) 0.0928(5) Uani 1 1 d D . . . .
H3 H 0.312(2) 0.385(3) 0.4519(19) 0.139 Uiso 1 1 d D U . . .
N4 N 0.13178(11) 0.25933(15) 0.27844(12) 0.0973(6) Uani 1 1 d D . . . .
H4 H 0.1637(19) 0.249(3) 0.303(2) 0.146 Uiso 1 1 d D U . . .
N5 N 0.13038(12) 0.24101(13) 0.21953(12) 0.0959(6) Uani 1 1 d . . . . .
N6 N 0.10223(17) 0.20470(15) 0.10813(14) 0.1111(7) Uani 1 1 d . . . . .
C1 C 0.56531(16) 0.43411(18) 0.5326(2) 0.1127(9) Uani 1 1 d . . . . .
H1A H 0.584790 0.462371 0.507133 0.135 Uiso 1 1 calc R U . . .
C2 C 0.5973(2) 0.4096(2) 0.5829(3) 0.1418(17) Uani 1 1 d . . . . .
H2A H 0.637583 0.421547 0.590662 0.170 Uiso 1 1 calc R U . . .
C3 C 0.5697(3) 0.3691(3) 0.6194(3) 0.1505(19) Uani 1 1 d . . . . .
H3A H 0.590256 0.353815 0.653590 0.181 Uiso 1 1 calc R U . . .
C4 C 0.5109(2) 0.3497(2) 0.6067(2) 0.1305(13) Uani 1 1 d . . . . .
H4A H 0.491989 0.319948 0.630797 0.157 Uiso 1 1 calc R U . . .
C5 C 0.48028(15) 0.37559(15) 0.55706(16) 0.1008(7) Uani 1 1 d . . . . .
C6 C 0.41618(14) 0.36225(14) 0.54105(14) 0.0949(6) Uani 1 1 d . . . . .
C7 C 0.37053(17) 0.32865(17) 0.56918(15) 0.1042(8) Uani 1 1 d . . . . .
H7A H 0.373569 0.306160 0.605377 0.125 Uiso 1 1 calc R U . . .
C8 C 0.31873(15) 0.33544(16) 0.53197(13) 0.0986(7) Uani 1 1 d . . . . .
C9 C 0.20975(15) 0.32837(19) 0.50000(15) 0.1063(8) Uani 1 1 d . . . . .
H9A H 0.217750 0.355962 0.468382 0.128 Uiso 1 1 calc R U . . .
C10 C 0.25677(17) 0.31083(18) 0.53832(14) 0.1054(8) Uani 1 1 d . . . . .
C11 C 0.2453(3) 0.2688(3) 0.5858(2) 0.1395(16) Uani 1 1 d . . . . .
H11A H 0.276788 0.256527 0.612036 0.167 Uiso 1 1 calc R U . . .
C12 C 0.1864(3) 0.2458(4) 0.5930(3) 0.180(3) Uani 1 1 d . . . . .
H12A H 0.178731 0.216727 0.623335 0.215 Uiso 1 1 calc R U . . .
C13 C 0.1398(3) 0.2652(4) 0.5565(2) 0.164(2) Uani 1 1 d . . . . .
H13A H 0.100114 0.251231 0.564248 0.197 Uiso 1 1 calc R U . . .
C14 C 0.14977(17) 0.3055(2) 0.50759(16) 0.1218(12) Uani 1 1 d . . . . .
C15 C 0.11369(14) 0.30652(19) 0.40149(17) 0.1088(9) Uani 1 1 d . . . . .
H15A H 0.151906 0.290642 0.390865 0.131 Uiso 1 1 calc R U . . .
C16 C 0.10246(16) 0.3202(2) 0.46193(18) 0.1196(11) Uani 1 1 d . . . . .
C17 C 0.0457(2) 0.3434(4) 0.4779(3) 0.172(3) Uani 1 1 d . . . . .
H17A H 0.036899 0.352901 0.518576 0.207 Uiso 1 1 calc R U . . .
C18 C 0.0020(2) 0.3525(4) 0.4326(3) 0.175(3) Uani 1 1 d . . . . .
H18A H -0.036637 0.367003 0.443750 0.210 Uiso 1 1 calc R U . . .
C19 C 0.0139(2) 0.3409(3) 0.3720(3) 0.152(2) Uani 1 1 d . . . . .
H19A H -0.015184 0.349813 0.341920 0.182 Uiso 1 1 calc R U . . .
C20 C 0.07105(15) 0.3153(2) 0.35614(17) 0.1090(9) Uani 1 1 d . . . . .
C21 C 0.08141(14) 0.29349(16) 0.29256(16) 0.0994(7) Uani 1 1 d . . . . .
C22 C 0.04532(17) 0.29562(18) 0.24019(18) 0.1094(8) Uani 1 1 d . . . . .
H22A H 0.007429 0.314788 0.235478 0.131 Uiso 1 1 calc R U . . .
C23 C 0.07782(15) 0.26309(16) 0.19650(16) 0.1010(7) Uani 1 1 d . . . . .
C24 C 0.06272(18) 0.24549(19) 0.13324(17) 0.1119(9) Uani 1 1 d . . . . .
C25 C 0.0126(3) 0.2680(3) 0.1018(3) 0.1471(18) Uani 1 1 d . . . . .
H25A H -0.015012 0.294381 0.120983 0.176 Uiso 1 1 calc R U . . .
C26 C 0.0040(4) 0.2508(4) 0.0422(3) 0.178(3) Uani 1 1 d . . . . .
H26A H -0.029075 0.265953 0.019853 0.214 Uiso 1 1 calc R U . . .
C27 C 0.0453(4) 0.2104(4) 0.0150(3) 0.179(3) Uani 1 1 d . . . . .
H27A H 0.041502 0.199709 -0.026169 0.215 Uiso 1 1 calc R U . . .
C28 C 0.0917(3) 0.1865(3) 0.0503(2) 0.1476(17) Uani 1 1 d . . . . .
H28A H 0.116884 0.156389 0.033408 0.177 Uiso 1 1 calc R U . . .
Fe3 Fe 0.31207(2) 0.31207(2) 0.31207(2) 0.09057(19) Uani 1 3 d S T P . .
O1 O 0.27880(9) 0.38124(10) 0.36318(9) 0.0905(4) Uani 1 1 d . . . . .
O2 O 0.24993(10) 0.34299(10) 0.25212(9) 0.0944(5) Uani 1 1 d . . . . .
O3 O 0.1040(2) 0.4995(3) 0.2341(2) 0.214(3) Uani 1 1 d . U . . .
O4 O 0.1285(2) 0.5344(3) 0.3499(2) 0.195(2) Uani 1 1 d . U . . .
C29 C 0.23455(13) 0.41079(14) 0.33707(12) 0.0902(6) Uani 1 1 d . . . . .
C30 C 0.21918(13) 0.39004(14) 0.27251(13) 0.0919(6) Uani 1 1 d . . . . .
C31 C 0.17591(18) 0.4188(2) 0.23864(17) 0.1198(12) Uani 1 1 d . . . . .
H31A H 0.167512 0.405309 0.198993 0.144 Uiso 1 1 calc R U . . .
C32 C 0.1430(2) 0.4698(3) 0.2633(2) 0.1405(17) Uani 1 1 d . U . . .
C33 C 0.1578(2) 0.4910(3) 0.3289(2) 0.1321(15) Uani 1 1 d . U . . .
C34 C 0.20378(16) 0.45855(19) 0.36251(16) 0.1082(8) Uani 1 1 d . . . . .
H34A H 0.212818 0.470405 0.402550 0.130 Uiso 1 1 calc R U . . .
B1 B -0.1082(11) 0.3878(12) 0.1110(11) 0.185(5) Uani 0.3333 1 d D U P A -1
F1 F -0.1003(12) 0.3576(11) 0.1672(9) 0.250(9) Uani 0.3333 1 d D U P A -1
F2 F -0.0572(11) 0.4192(17) 0.0961(12) 0.254(8) Uani 0.3333 1 d D U P A -1
F3 F -0.1591(13) 0.4241(11) 0.1150(12) 0.217(9) Uani 0.3333 1 d D U P A -1
F4 F -0.1202(12) 0.3420(11) 0.0680(10) 0.217(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.008(2) . ?
Fe1 N2 2.008(2) 5 ?
Fe1 N2 2.008(2) 9 ?
Fe1 N1 2.060(3) 5 ?
Fe1 N1 2.060(3) 9 ?
Fe1 N1 2.060(3) . ?
Fe2 N5 2.077(3) . ?
Fe2 N5 2.077(3) 9 ?
Fe2 N5 2.077(3) 5 ?
Fe2 N6 2.130(3) 9 ?
Fe2 N6 2.130(3) 5 ?
Fe2 N6 2.130(3) . ?
N1 C1 1.335(4) . ?
N1 C5 1.351(5) . ?
N2 C6 1.336(4) . ?
N2 N3 1.350(3) . ?
N3 C8 1.371(4) . ?
N3 H3 0.92(3) . ?
N4 N5 1.343(4) . ?
N4 C21 1.360(4) . ?
N4 H4 0.90(3) . ?
N5 C23 1.338(4) . ?
N6 C28 1.339(5) . ?
N6 C24 1.352(6) . ?
C1 C2 1.404(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.329(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.377(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.467(4) . ?
C6 C7 1.378(5) . ?
C7 C8 1.396(5) . ?
C7 H7A 0.9300 . ?
C8 C10 1.458(5) . ?
C9 C10 1.374(5) . ?
C9 C14 1.407(5) . ?
C9 H9A 0.9300 . ?
C10 C11 1.403(6) . ?
C11 C12 1.386(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.357(10) . ?
C12 H12A 0.9300 . ?
C13 C14 1.397(7) . ?
C13 H13A 0.9300 . ?
C14 C16 1.467(6) . ?
C15 C20 1.368(6) . ?
C15 C16 1.371(5) . ?
C15 H15A 0.9300 . ?
C16 C17 1.380(6) . ?
C17 C18 1.384(9) . ?
C17 H17A 0.9300 . ?
C18 C19 1.369(8) . ?
C18 H18A 0.9300 . ?
C19 C20 1.407(5) . ?
C19 H19A 0.9300 . ?
C20 C21 1.480(5) . ?
C21 C22 1.385(5) . ?
C22 C23 1.381(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.467(5) . ?
C24 C25 1.378(6) . ?
C25 C26 1.365(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.388(11) . ?
C26 H26A 0.9300 . ?
C27 C28 1.372(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.996(2) 9 ?
Fe3 O2 1.996(2) . ?
Fe3 O2 1.996(2) 5 ?
Fe3 O1 2.007(2) . ?
Fe3 O1 2.007(2) 5 ?
Fe3 O1 2.007(2) 9 ?
O1 C29 1.290(4) . ?
O2 C30 1.301(4) . ?
O3 C32 1.243(6) . ?
O4 C33 1.228(6) . ?
C29 C34 1.355(5) . ?
C29 C30 1.514(4) . ?
C30 C31 1.351(4) . ?
C31 C32 1.426(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.536(6) . ?
C33 C34 1.426(5) . ?
C34 H34A 0.9300 . ?
B1 F2 1.344(18) . ?
B1 F3 1.37(2) . ?
B1 F4 1.39(2) . ?
B1 F1 1.40(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.44(9) . 5 ?
N2 Fe1 N2 96.44(9) . 9 ?
N2 Fe1 N2 96.44(9) 5 9 ?
N2 Fe1 N1 170.87(11) . 5 ?
N2 Fe1 N1 79.23(10) 5 5 ?
N2 Fe1 N1 92.05(10) 9 5 ?
N2 Fe1 N1 92.05(10) . 9 ?
N2 Fe1 N1 170.87(11) 5 9 ?
N2 Fe1 N1 79.23(10) 9 9 ?
N1 Fe1 N1 92.82(11) 5 9 ?
N2 Fe1 N1 79.23(10) . . ?
N2 Fe1 N1 92.05(10) 5 . ?
N2 Fe1 N1 170.87(10) 9 . ?
N1 Fe1 N1 92.82(11) 5 . ?
N1 Fe1 N1 92.82(11) 9 . ?
N5 Fe2 N5 97.69(10) . 9 ?
N5 Fe2 N5 97.68(10) . 5 ?
N5 Fe2 N5 97.69(10) 9 5 ?
N5 Fe2 N6 167.81(12) . 9 ?
N5 Fe2 N6 77.12(11) 9 9 ?
N5 Fe2 N6 93.97(12) 5 9 ?
N5 Fe2 N6 93.97(12) . 5 ?
N5 Fe2 N6 167.81(12) 9 5 ?
N5 Fe2 N6 77.12(11) 5 5 ?
N6 Fe2 N6 92.11(13) 9 5 ?
N5 Fe2 N6 77.12(11) . . ?
N5 Fe2 N6 93.97(12) 9 . ?
N5 Fe2 N6 167.81(12) 5 . ?
N6 Fe2 N6 92.11(13) 9 . ?
N6 Fe2 N6 92.11(13) 5 . ?
C1 N1 C5 118.6(3) . . ?
C1 N1 Fe1 126.8(3) . . ?
C5 N1 Fe1 114.5(2) . . ?
C6 N2 N3 105.7(2) . . ?
C6 N2 Fe1 116.1(2) . . ?
N3 N2 Fe1 136.6(2) . . ?
N2 N3 C8 111.2(2) . . ?
N2 N3 H3 123(4) . . ?
C8 N3 H3 126(4) . . ?
N5 N4 C21 111.1(3) . . ?
N5 N4 H4 121(4) . . ?
C21 N4 H4 128(4) . . ?
C23 N5 N4 105.7(3) . . ?
C23 N5 Fe2 115.2(2) . . ?
N4 N5 Fe2 135.3(2) . . ?
C28 N6 C24 117.8(4) . . ?
C28 N6 Fe2 127.2(3) . . ?
C24 N6 Fe2 114.8(2) . . ?
N1 C1 C2 121.3(4) . . ?
N1 C1 H1A 119.3 . . ?
C2 C1 H1A 119.3 . . ?
C3 C2 C1 119.6(4) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C2 C3 C4 120.2(4) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 121.6(3) . . ?
N1 C5 C6 114.3(3) . . ?
C4 C5 C6 124.1(3) . . ?
N2 C6 C7 111.5(3) . . ?
N2 C6 C5 115.2(3) . . ?
C7 C6 C5 133.3(3) . . ?
C6 C7 C8 105.6(3) . . ?
C6 C7 H7A 127.2 . . ?
C8 C7 H7A 127.2 . . ?
N3 C8 C7 105.9(3) . . ?
N3 C8 C10 123.3(3) . . ?
C7 C8 C10 130.8(3) . . ?
C10 C9 C14 121.4(4) . . ?
C10 C9 H9A 119.3 . . ?
C14 C9 H9A 119.3 . . ?
C9 C10 C11 119.8(4) . . ?
C9 C10 C8 122.0(3) . . ?
C11 C10 C8 118.3(4) . . ?
C12 C11 C10 118.8(5) . . ?
C12 C11 H11A 120.6 . . ?
C10 C11 H11A 120.6 . . ?
C13 C12 C11 121.0(5) . . ?
C13 C12 H12A 119.5 . . ?
C11 C12 H12A 119.5 . . ?
C12 C13 C14 121.6(4) . . ?
C12 C13 H13A 119.2 . . ?
C14 C13 H13A 119.2 . . ?
C13 C14 C9 117.2(4) . . ?
C13 C14 C16 123.0(4) . . ?
C9 C14 C16 119.7(4) . . ?
C20 C15 C16 122.8(3) . . ?
C20 C15 H15A 118.6 . . ?
C16 C15 H15A 118.6 . . ?
C15 C16 C17 118.7(4) . . ?
C15 C16 C14 118.5(3) . . ?
C17 C16 C14 122.6(4) . . ?
C16 C17 C18 119.3(4) . . ?
C16 C17 H17A 120.3 . . ?
C18 C17 H17A 120.3 . . ?
C19 C18 C17 122.0(4) . . ?
C19 C18 H18A 119.0 . . ?
C17 C18 H18A 119.0 . . ?
C18 C19 C20 118.5(5) . . ?
C18 C19 H19A 120.8 . . ?
C20 C19 H19A 120.8 . . ?
C15 C20 C19 118.6(4) . . ?
C15 C20 C21 121.8(3) . . ?
C19 C20 C21 119.4(4) . . ?
N4 C21 C22 106.8(3) . . ?
N4 C21 C20 120.6(3) . . ?
C22 C21 C20 132.2(3) . . ?
C23 C22 C21 105.0(3) . . ?
C23 C22 H22A 127.5 . . ?
C21 C22 H22A 127.5 . . ?
N5 C23 C22 111.4(3) . . ?
N5 C23 C24 116.7(3) . . ?
C22 C23 C24 131.7(3) . . ?
N6 C24 C25 122.5(4) . . ?
N6 C24 C23 114.1(3) . . ?
C25 C24 C23 123.4(4) . . ?
C26 C25 C24 118.9(6) . . ?
C26 C25 H25A 120.6 . . ?
C24 C25 H25A 120.6 . . ?
C25 C26 C27 119.4(5) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C28 C27 C26 118.6(5) . . ?
C28 C27 H27A 120.7 . . ?
C26 C27 H27A 120.7 . . ?
N6 C28 C27 122.7(6) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 90.33(9) 9 . ?
O2 Fe3 O2 90.33(9) 9 5 ?
O2 Fe3 O2 90.33(9) . 5 ?
O2 Fe3 O1 170.92(8) 9 . ?
O2 Fe3 O1 82.24(7) . . ?
O2 Fe3 O1 94.91(9) 5 . ?
O2 Fe3 O1 94.91(9) 9 5 ?
O2 Fe3 O1 170.92(8) . 5 ?
O2 Fe3 O1 82.24(7) 5 5 ?
O1 Fe3 O1 93.15(8) . 5 ?
O2 Fe3 O1 82.24(7) 9 9 ?
O2 Fe3 O1 94.91(9) . 9 ?
O2 Fe3 O1 170.92(8) 5 9 ?
O1 Fe3 O1 93.14(8) . 9 ?
O1 Fe3 O1 93.14(8) 5 9 ?
C29 O1 Fe3 113.53(17) . . ?
C30 O2 Fe3 113.00(17) . . ?
O1 C29 C34 124.9(3) . . ?
O1 C29 C30 115.2(2) . . ?
C34 C29 C30 119.9(3) . . ?
O2 C30 C31 122.5(3) . . ?
O2 C30 C29 116.0(2) . . ?
C31 C30 C29 121.5(3) . . ?
C30 C31 C32 120.4(3) . . ?
C30 C31 H31A 119.8 . . ?
C32 C31 H31A 119.8 . . ?
O3 C32 C31 123.8(4) . . ?
O3 C32 C33 117.6(4) . . ?
C31 C32 C33 118.6(3) . . ?
O4 C33 C34 123.7(4) . . ?
O4 C33 C32 117.9(4) . . ?
C34 C33 C32 118.4(3) . . ?
C29 C34 C33 121.2(3) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F3 113.0(17) . . ?
F2 B1 F4 110.9(18) . . ?
F3 B1 F4 107.7(17) . . ?
F2 B1 F1 110.4(16) . . ?
F3 B1 F1 108.5(18) . . ?
F4 B1 F1 106.0(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.92(3) 2.06(3) 2.931(3) 156(5) . yes
N4 H4 O2 0.90(3) 2.11(3) 2.980(3) 161(5) 5 yes

_refine_diff_density_max         0.393
_refine_diff_density_min         -0.316
_refine_diff_density_rms         0.061

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_350Kd
_database_code_depnum_ccdc_archive 'CCDC 2261732'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.772(3)
_cell_length_b                   21.772(3)
_cell_length_c                   21.772(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10320(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    6415
_cell_measurement_theta_min      1.92
_cell_measurement_theta_max      33.09

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.881
_shelx_estimated_absorpt_T_max   0.903
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            168619
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.920
_diffrn_reflns_theta_max         29.512
_diffrn_reflns_theta_full        29.512
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8870
_reflns_number_gt                8355
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.859
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;

_vrf_PLAT601_lb2205_fresh2_350Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1870 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1870 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0867P)²+0.1225P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0046(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3678 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.077(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8870
_refine_ls_number_parameters     458
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0373
_refine_ls_R_factor_gt           0.0362
_refine_ls_wR_factor_ref         0.1153
_refine_ls_wR_factor_gt          0.1133
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_restrained_S_all      1.059
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29803(2) 0.29803(2) 0.29803(2) 0.07345(14) Uani 1 3 d S T P . .
Fe2 Fe 0.57909(2) 0.57909(2) 0.57909(2) 0.07686(15) Uani 1 3 d S T P . .
N1 N 0.23206(11) 0.33226(10) 0.24173(9) 0.0847(5) Uani 1 1 d . . . . .
N2 N 0.26070(9) 0.36067(9) 0.35279(9) 0.0787(4) Uani 1 1 d . . . . .
N3 N 0.26518(9) 0.37629(10) 0.41278(9) 0.0808(4) Uani 1 1 d D . . . .
H3 H 0.2979(15) 0.368(2) 0.4333(18) 0.121 Uiso 1 1 d D U . . .
N4 N 0.47068(10) 0.49137(12) 0.61631(9) 0.0852(5) Uani 1 1 d D . . . .
H4 H 0.4483(18) 0.504(2) 0.5861(16) 0.128 Uiso 1 1 d D U . . .
N5 N 0.52989(10) 0.50920(11) 0.61768(9) 0.0840(5) Uani 1 1 d . . . . .
N6 N 0.64062(11) 0.54450(12) 0.64364(13) 0.0968(6) Uani 1 1 d . . . . .
C1 C 0.22079(17) 0.31611(15) 0.18334(13) 0.0981(7) Uani 1 1 d . . . . .
H1A H 0.246310 0.287449 0.164582 0.118 Uiso 1 1 calc R U . . .
C2 C 0.1727(2) 0.34054(19) 0.15017(16) 0.1220(12) Uani 1 1 d . . . . .
H2A H 0.165225 0.327456 0.110197 0.146 Uiso 1 1 calc R U . . .
C3 C 0.1361(2) 0.3841(2) 0.17656(19) 0.1273(13) Uani 1 1 d . . . . .
H3B H 0.103728 0.401293 0.154544 0.153 Uiso 1 1 calc R U . . .
C4 C 0.14736(19) 0.40242(17) 0.23575(17) 0.1123(9) Uani 1 1 d . . . . .
H4B H 0.123436 0.432636 0.254163 0.135 Uiso 1 1 calc R U . . .
C5 C 0.19528(13) 0.37489(12) 0.26767(12) 0.0865(5) Uani 1 1 d . . . . .
C6 C 0.21042(11) 0.38826(12) 0.33172(12) 0.0837(5) Uani 1 1 d . . . . .
C7 C 0.18219(12) 0.42233(14) 0.37786(14) 0.0939(6) Uani 1 1 d . . . . .
H7A H 0.146382 0.445407 0.374683 0.113 Uiso 1 1 calc R U . . .
C8 C 0.21834(11) 0.41473(13) 0.42916(13) 0.0868(5) Uani 1 1 d . . . . .
C9 C 0.21140(11) 0.43974(14) 0.49133(14) 0.0930(6) Uani 1 1 d . . . . .
C10 C 0.16415(18) 0.4813(2) 0.5024(2) 0.1256(13) Uani 1 1 d . . . . .
H10A H 0.138675 0.493983 0.470565 0.151 Uiso 1 1 calc R U . . .
C11 C 0.1553(2) 0.5038(3) 0.5615(3) 0.164(2) Uani 1 1 d . . . . .
H11A H 0.123848 0.531695 0.569186 0.197 Uiso 1 1 calc R U . . .
C12 C 0.19301(19) 0.4850(3) 0.6088(2) 0.1477(19) Uani 1 1 d . . . . .
H12A H 0.185986 0.499539 0.648333 0.177 Uiso 1 1 calc R U . . .
C13 C 0.24126(14) 0.44482(19) 0.59822(14) 0.1077(9) Uani 1 1 d . . . . .
C14 C 0.24931(12) 0.42227(16) 0.53837(12) 0.0948(7) Uani 1 1 d . . . . .
H14A H 0.281093 0.394843 0.530492 0.114 Uiso 1 1 calc R U . . .
C15 C 0.28680(14) 0.42998(19) 0.64600(13) 0.1065(9) Uani 1 1 d . . . . .
C16 C 0.2716(2) 0.4054(3) 0.70275(18) 0.1460(19) Uani 1 1 d . . . . .
H16A H 0.231065 0.395449 0.711623 0.175 Uiso 1 1 calc R U . . .
C17 C 0.3162(2) 0.3960(3) 0.74536(18) 0.152(2) Uani 1 1 d . . . . .
H17A H 0.305326 0.379629 0.783291 0.183 Uiso 1 1 calc R U . . .
C18 C 0.3779(2) 0.4100(3) 0.73416(17) 0.1336(15) Uani 1 1 d . . . . .
H18A H 0.407804 0.402856 0.763822 0.160 Uiso 1 1 calc R U . . .
C19 C 0.39324(14) 0.43491(17) 0.67733(12) 0.0977(7) Uani 1 1 d . . . . .
C20 C 0.34817(13) 0.44411(16) 0.63426(12) 0.0957(7) Uani 1 1 d . . . . .
H20A H 0.358836 0.460222 0.596170 0.115 Uiso 1 1 calc R U . . .
C21 C 0.45666(13) 0.45662(14) 0.66628(12) 0.0893(6) Uani 1 1 d . . . . .
C22 C 0.50923(15) 0.45304(15) 0.70176(13) 0.0972(7) Uani 1 1 d . . . . .
H22A H 0.514078 0.432774 0.739055 0.117 Uiso 1 1 calc R U . . .
C23 C 0.55314(13) 0.48620(13) 0.66971(12) 0.0877(6) Uani 1 1 d . . . . .
C24 C 0.61680(14) 0.50312(15) 0.68335(14) 0.0969(7) Uani 1 1 d . . . . .
C25 C 0.6494(2) 0.4794(2) 0.7319(2) 0.1350(15) Uani 1 1 d . . . . .
H25A H 0.631153 0.451632 0.758769 0.162 Uiso 1 1 calc R U . . .
C26 C 0.7090(2) 0.4972(3) 0.7399(3) 0.161(2) Uani 1 1 d . . . . .
H26A H 0.731895 0.481850 0.772540 0.193 Uiso 1 1 calc R U . . .
C27 C 0.7348(2) 0.5380(3) 0.6993(3) 0.155(2) Uani 1 1 d . . . . .
H27A H 0.775653 0.549773 0.703854 0.186 Uiso 1 1 calc R U . . .
C28 C 0.69997(16) 0.5614(2) 0.6518(2) 0.1247(12) Uani 1 1 d . . . . .
H28A H 0.717604 0.589398 0.624812 0.150 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43685(2) 0.43685(2) 0.43685(2) 0.07945(15) Uani 1 3 d S T P . .
O1 O 0.38540(7) 0.36795(8) 0.47021(8) 0.0790(3) Uani 1 1 d . . . . .
O2 O 0.49642(8) 0.40599(8) 0.49931(8) 0.0827(4) Uani 1 1 d . . . . .
O3 O 0.51270(17) 0.2524(3) 0.64756(19) 0.196(2) Uani 1 1 d . . . . .
O4 O 0.39790(17) 0.2166(2) 0.62221(19) 0.181(2) Uani 1 1 d . U . . .
C29 C 0.41138(10) 0.33882(12) 0.51521(10) 0.0791(5) Uani 1 1 d . . . . .
C30 C 0.47552(10) 0.35962(12) 0.53060(11) 0.0809(5) Uani 1 1 d . . . . .
C31 C 0.50854(14) 0.33053(18) 0.57408(15) 0.1062(9) Uani 1 1 d . . . . .
H31A H 0.548499 0.343515 0.581771 0.127 Uiso 1 1 calc R U . . .
C32 C 0.48463(17) 0.2811(2) 0.60826(17) 0.1233(13) Uani 1 1 d . U . . .
C33 C 0.41831(17) 0.2596(2) 0.59350(17) 0.1186(11) Uani 1 1 d . U . . .
C34 C 0.38515(13) 0.29177(15) 0.54654(13) 0.0952(7) Uani 1 1 d . . . . .
H34A H 0.345048 0.280216 0.537430 0.114 Uiso 1 1 calc R U . . .
B1 B 0.1405(10) 0.1414(11) 0.1436(8) 0.141(3) Uani 0.3333 1 d D U P A -1
F1 F 0.1385(12) 0.1803(11) 0.0943(11) 0.192(8) Uani 0.3333 1 d D U P A -1
F2 F 0.1549(11) 0.1724(15) 0.1951(8) 0.228(7) Uani 0.3333 1 d D U P A -1
F3 F 0.0836(8) 0.1157(10) 0.1539(9) 0.195(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1820(10) 0.0950(11) 0.1332(12) 0.174(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.985(2) . ?
Fe1 N2 1.985(2) 5 ?
Fe1 N2 1.985(2) 9 ?
Fe1 N1 2.030(2) 5 ?
Fe1 N1 2.030(2) 9 ?
Fe1 N1 2.030(2) . ?
Fe2 N5 2.042(2) . ?
Fe2 N5 2.042(2) 9 ?
Fe2 N5 2.042(2) 5 ?
Fe2 N6 2.083(2) . ?
Fe2 N6 2.083(2) 9 ?
Fe2 N6 2.083(2) 5 ?
N1 C1 1.342(4) . ?
N1 C5 1.350(4) . ?
N2 C6 1.330(3) . ?
N2 N3 1.353(3) . ?
N3 C8 1.367(3) . ?
N3 H3 0.86(2) . ?
N4 N5 1.346(3) . ?
N4 C21 1.360(4) . ?
N4 H4 0.86(2) . ?
N5 C23 1.338(3) . ?
N6 C24 1.352(4) . ?
N6 C28 1.355(4) . ?
C1 C2 1.379(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.366(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.371(6) . ?
C3 H3B 0.9300 . ?
C4 C5 1.389(4) . ?
C4 H4B 0.9300 . ?
C5 C6 1.462(4) . ?
C6 C7 1.392(4) . ?
C7 C8 1.376(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.467(4) . ?
C9 C14 1.369(4) . ?
C9 C10 1.392(5) . ?
C10 C11 1.390(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.379(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.387(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.403(4) . ?
C13 C15 1.473(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(5) . ?
C15 C20 1.395(4) . ?
C16 C17 1.358(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.399(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.392(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.372(4) . ?
C19 C21 1.479(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.383(4) . ?
C22 C23 1.386(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.465(4) . ?
C24 C25 1.373(5) . ?
C25 C26 1.367(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.372(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.381(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9956(17) 9 ?
Fe3 O2 1.9956(17) . ?
Fe3 O2 1.9957(17) 5 ?
Fe3 O1 2.0082(16) 9 ?
Fe3 O1 2.0082(16) 5 ?
Fe3 O1 2.0082(16) . ?
O1 C29 1.297(3) . ?
O2 C30 1.300(3) . ?
O3 C32 1.223(5) . ?
O4 C33 1.210(4) . ?
C29 C34 1.357(4) . ?
C29 C30 1.506(3) . ?
C30 C31 1.347(4) . ?
C31 C32 1.408(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.552(5) . ?
C33 C34 1.435(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.346(14) . ?
B1 F1 1.368(19) . ?
B1 F4 1.372(19) . ?
B1 F3 1.378(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.58(8) . 5 ?
N2 Fe1 N2 96.58(8) . 9 ?
N2 Fe1 N2 96.58(8) 5 9 ?
N2 Fe1 N1 91.05(8) . 5 ?
N2 Fe1 N1 79.68(8) 5 5 ?
N2 Fe1 N1 171.86(8) 9 5 ?
N2 Fe1 N1 171.86(8) . 9 ?
N2 Fe1 N1 91.05(8) 5 9 ?
N2 Fe1 N1 79.68(8) 9 9 ?
N1 Fe1 N1 93.10(9) 5 9 ?
N2 Fe1 N1 79.68(8) . . ?
N2 Fe1 N1 171.86(8) 5 . ?
N2 Fe1 N1 91.05(8) 9 . ?
N1 Fe1 N1 93.10(9) 5 . ?
N1 Fe1 N1 93.10(9) 9 . ?
N5 Fe2 N5 97.56(8) . 9 ?
N5 Fe2 N5 97.56(8) . 5 ?
N5 Fe2 N5 97.56(8) 9 5 ?
N5 Fe2 N6 77.89(9) . . ?
N5 Fe2 N6 169.20(10) 9 . ?
N5 Fe2 N6 92.78(10) 5 . ?
N5 Fe2 N6 92.78(10) . 9 ?
N5 Fe2 N6 77.90(9) 9 9 ?
N5 Fe2 N6 169.20(10) 5 9 ?
N6 Fe2 N6 92.44(10) . 9 ?
N5 Fe2 N6 169.20(10) . 5 ?
N5 Fe2 N6 92.77(10) 9 5 ?
N5 Fe2 N6 77.90(9) 5 5 ?
N6 Fe2 N6 92.44(10) . 5 ?
N6 Fe2 N6 92.44(10) 9 5 ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Fe1 127.3(2) . . ?
C5 N1 Fe1 114.81(17) . . ?
C6 N2 N3 106.2(2) . . ?
C6 N2 Fe1 116.10(17) . . ?
N3 N2 Fe1 136.29(16) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 120(3) . . ?
C8 N3 H3 128(3) . . ?
N5 N4 C21 110.9(2) . . ?
N5 N4 H4 118(3) . . ?
C21 N4 H4 131(3) . . ?
C23 N5 N4 105.8(2) . . ?
C23 N5 Fe2 115.39(19) . . ?
N4 N5 Fe2 135.07(17) . . ?
C24 N6 C28 117.6(3) . . ?
C24 N6 Fe2 115.19(19) . . ?
C28 N6 Fe2 127.1(3) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.4(3) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3B 120.3 . . ?
C4 C3 H3B 120.3 . . ?
C3 C4 C5 118.7(3) . . ?
C3 C4 H4B 120.7 . . ?
C5 C4 H4B 120.7 . . ?
N1 C5 C4 122.2(3) . . ?
N1 C5 C6 113.7(2) . . ?
C4 C5 C6 124.1(3) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.1(2) . . ?
C7 C6 C5 134.0(2) . . ?
C8 C7 C6 105.6(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C9 123.0(2) . . ?
C7 C8 C9 130.2(2) . . ?
C14 C9 C10 119.8(3) . . ?
C14 C9 C8 121.7(3) . . ?
C10 C9 C8 118.6(3) . . ?
C11 C10 C9 119.5(4) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.2(4) . . ?
C12 C11 H11A 119.9 . . ?
C10 C11 H11A 119.9 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 118.0(4) . . ?
C12 C13 C15 122.1(3) . . ?
C14 C13 C15 119.7(3) . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.5(3) . . ?
C16 C15 C13 123.6(3) . . ?
C20 C15 C13 117.8(3) . . ?
C17 C16 C15 119.8(4) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 122.3(3) . . ?
C16 C17 H17A 118.9 . . ?
C18 C17 H17A 118.9 . . ?
C19 C18 C17 118.1(4) . . ?
C19 C18 H18A 121.0 . . ?
C17 C18 H18A 121.0 . . ?
C20 C19 C18 119.5(3) . . ?
C20 C19 C21 120.7(2) . . ?
C18 C19 C21 119.5(3) . . ?
C19 C20 C15 121.9(3) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 107.0(2) . . ?
N4 C21 C19 121.2(2) . . ?
C22 C21 C19 131.6(3) . . ?
C21 C22 C23 105.1(2) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 115.8(3) . . ?
C22 C23 C24 133.0(3) . . ?
N6 C24 C25 123.0(3) . . ?
N6 C24 C23 113.6(2) . . ?
C25 C24 C23 123.4(3) . . ?
C26 C25 C24 118.8(5) . . ?
C26 C25 H25A 120.6 . . ?
C24 C25 H25A 120.6 . . ?
C25 C26 C27 119.4(4) . . ?
C25 C26 H26A 120.3 . . ?
C27 C26 H26A 120.3 . . ?
C26 C27 C28 119.7(4) . . ?
C26 C27 H27A 120.2 . . ?
C28 C27 H27A 120.2 . . ?
N6 C28 C27 121.5(4) . . ?
N6 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
O2 Fe3 O2 90.31(8) 9 . ?
O2 Fe3 O2 90.31(8) 9 5 ?
O2 Fe3 O2 90.31(8) . 5 ?
O2 Fe3 O1 82.22(6) 9 9 ?
O2 Fe3 O1 170.87(7) . 9 ?
O2 Fe3 O1 94.94(7) 5 9 ?
O2 Fe3 O1 170.87(7) 9 5 ?
O2 Fe3 O1 94.94(7) . 5 ?
O2 Fe3 O1 82.22(6) 5 5 ?
O1 Fe3 O1 93.16(7) 9 5 ?
O2 Fe3 O1 94.94(7) 9 . ?
O2 Fe3 O1 82.22(6) . . ?
O2 Fe3 O1 170.87(7) 5 . ?
O1 Fe3 O1 93.16(7) 9 . ?
O1 Fe3 O1 93.16(7) 5 . ?
C29 O1 Fe3 113.28(14) . . ?
C30 O2 Fe3 113.02(14) . . ?
O1 C29 C34 124.4(2) . . ?
O1 C29 C30 115.2(2) . . ?
C34 C29 C30 120.4(2) . . ?
O2 C30 C31 123.1(2) . . ?
O2 C30 C29 116.2(2) . . ?
C31 C30 C29 120.7(2) . . ?
C30 C31 C32 122.2(3) . . ?
C30 C31 H31A 118.9 . . ?
C32 C31 H31A 118.9 . . ?
O3 C32 C31 125.1(3) . . ?
O3 C32 C33 117.1(4) . . ?
C31 C32 C33 117.8(3) . . ?
O4 C33 C34 124.2(3) . . ?
O4 C33 C32 117.9(3) . . ?
C34 C33 C32 117.9(3) . . ?
C29 C34 C33 121.0(3) . . ?
C29 C34 H34A 119.5 . . ?
C33 C34 H34A 119.5 . . ?
F2 B1 F1 110.4(16) . . ?
F2 B1 F4 110.8(17) . . ?
F1 B1 F4 110.3(17) . . ?
F2 B1 F3 106.1(14) . . ?
F1 B1 F3 110.5(17) . . ?
F4 B1 F3 108.7(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.86(2) 2.07(3) 2.907(3) 164(4) . yes
N4 H4 O2 0.86(2) 2.16(3) 2.971(3) 156(4) 9 yes

_refine_diff_density_max         0.302
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.044

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_350K
_database_code_depnum_ccdc_archive 'CCDC 2261727'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4, 1.872(C H4 O)'
_chemical_formula_sum            'C103.87 H73.49 B F4 Fe3 N18 O13.87'
_chemical_formula_weight         2050.06

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.631(3)
_cell_length_b                   21.631(3)
_cell_length_c                   21.631(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10121(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    350(2)
_cell_measurement_reflns_used    6519
_cell_measurement_theta_min      1.67
_cell_measurement_theta_max      33.65

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.345
_exptl_crystal_F_000             4211
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.536
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.901
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      350(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            164595
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_av_R_equivalents  0.0813
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.673
_diffrn_reflns_theta_max         29.515
_diffrn_reflns_theta_full        29.515
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8764
_reflns_number_gt                8163
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.860
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 and displacement parameters restraints. 
 The lattice methanol molecule was refined with displacement
 parameters restraints and a distance restraint, and its occupancy
 considered partial refining to 0.624 (i.e. 1.872 MeOH per formula unit).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0890P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0230(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3590 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.063(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8764
_refine_ls_number_parameters     479
_refine_ls_number_restraints     92
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0400
_refine_ls_wR_factor_ref         0.1143
_refine_ls_wR_factor_gt          0.1131
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.45279(2) 0.45279(2) 0.45279(2) 0.06862(13) Uani 1 3 d S T P . .
Fe2 Fe 0.16593(2) 0.16593(2) 0.16593(2) 0.07561(15) Uani 1 3 d S T P . .
N1 N 0.50676(9) 0.41913(9) 0.52200(10) 0.0790(4) Uani 1 1 d . . . . .
N2 N 0.39547(9) 0.39189(9) 0.48980(8) 0.0737(4) Uani 1 1 d . . . . .
N3 N 0.33543(9) 0.37600(9) 0.48377(8) 0.0746(4) Uani 1 1 d D . . . .
H3 H 0.3130(18) 0.378(2) 0.4488(15) 0.112 Uiso 1 1 d D U . . .
N4 N 0.12848(10) 0.25767(12) 0.27450(10) 0.0832(5) Uani 1 1 d D . . . .
H4 H 0.1621(16) 0.247(2) 0.294(2) 0.125 Uiso 1 1 d D U . . .
N5 N 0.12659(10) 0.23783(11) 0.21581(10) 0.0819(4) Uani 1 1 d . . . . .
N6 N 0.09831(13) 0.20071(12) 0.10382(11) 0.0915(5) Uani 1 1 d . . . . .
C1 C 0.56551(12) 0.43559(14) 0.53514(16) 0.0927(6) Uani 1 1 d . . . . .
H1A H 0.586069 0.462695 0.508856 0.111 Uiso 1 1 calc R U . . .
C2 C 0.59584(15) 0.41315(17) 0.58667(19) 0.1067(9) Uani 1 1 d . . . . .
H2A H 0.635758 0.426399 0.595601 0.128 Uiso 1 1 calc R U . . .
C3 C 0.56721(19) 0.3716(2) 0.6245(2) 0.1198(12) Uani 1 1 d . . . . .
H3A H 0.587804 0.355443 0.658582 0.144 Uiso 1 1 calc R U . . .
C4 C 0.50693(17) 0.35351(17) 0.61138(17) 0.1046(8) Uani 1 1 d . . . . .
H4A H 0.486440 0.325269 0.636503 0.126 Uiso 1 1 calc R U . . .
C5 C 0.47825(11) 0.37859(12) 0.56014(12) 0.0820(5) Uani 1 1 d . . . . .
C6 C 0.41420(11) 0.36551(11) 0.54241(11) 0.0784(5) Uani 1 1 d . . . . .
C7 C 0.36671(13) 0.33224(13) 0.57005(11) 0.0857(5) Uani 1 1 d . . . . .
H7A H 0.368395 0.309945 0.606767 0.103 Uiso 1 1 calc R U . . .
C8 C 0.31677(11) 0.33933(12) 0.53153(10) 0.0784(5) Uani 1 1 d . . . . .
C9 C 0.20686(12) 0.33235(15) 0.49734(11) 0.0864(6) Uani 1 1 d . . . . .
H9A H 0.215323 0.359879 0.465421 0.104 Uiso 1 1 calc R U . . .
C10 C 0.25374(12) 0.31446(13) 0.53692(10) 0.0834(5) Uani 1 1 d . . . . .
C11 C 0.24117(17) 0.27366(19) 0.58487(15) 0.1027(8) Uani 1 1 d . . . . .
H11A H 0.272463 0.261782 0.611856 0.123 Uiso 1 1 calc R U . . .
C12 C 0.1818(2) 0.2507(2) 0.59238(19) 0.1268(13) Uani 1 1 d . . . . .
H12A H 0.173490 0.222309 0.623587 0.152 Uiso 1 1 calc R U . . .
C13 C 0.13528(17) 0.2698(3) 0.55380(17) 0.1227(13) Uani 1 1 d . . . . .
H13A H 0.095188 0.255908 0.560672 0.147 Uiso 1 1 calc R U . . .
C14 C 0.14672(13) 0.30947(17) 0.50481(13) 0.0946(7) Uani 1 1 d . . . . .
C15 C 0.11093(11) 0.30827(15) 0.39705(12) 0.0885(6) Uani 1 1 d . . . . .
H15A H 0.149756 0.293261 0.386304 0.106 Uiso 1 1 calc R U . . .
C16 C 0.09894(12) 0.32276(19) 0.45879(14) 0.1010(8) Uani 1 1 d . . . . .
C17 C 0.04078(18) 0.3456(3) 0.4742(2) 0.1399(18) Uani 1 1 d . . . . .
H17A H 0.031277 0.354970 0.515031 0.168 Uiso 1 1 calc R U . . .
C18 C -0.00264(18) 0.3541(3) 0.4282(2) 0.1469(19) Uani 1 1 d . . . . .
H18A H -0.041022 0.370507 0.438569 0.176 Uiso 1 1 calc R U . . .
C19 C 0.00920(16) 0.3391(3) 0.3677(2) 0.1272(14) Uani 1 1 d . . . . .
H19A H -0.021051 0.344541 0.337614 0.153 Uiso 1 1 calc R U . . .
C20 C 0.06710(12) 0.31552(16) 0.35172(14) 0.0929(6) Uani 1 1 d . . . . .
C21 C 0.07788(11) 0.29209(13) 0.28888(13) 0.0837(5) Uani 1 1 d . . . . .
C22 C 0.04136(13) 0.29404(14) 0.23626(14) 0.0916(6) Uani 1 1 d . . . . .
H22A H 0.003620 0.314042 0.231397 0.110 Uiso 1 1 calc R U . . .
C23 C 0.07307(12) 0.25988(12) 0.19261(13) 0.0837(5) Uani 1 1 d . . . . .
C24 C 0.05827(14) 0.24201(14) 0.12895(13) 0.0915(6) Uani 1 1 d . . . . .
C25 C 0.0079(2) 0.2645(2) 0.0978(2) 0.1214(12) Uani 1 1 d . . . . .
H25A H -0.018907 0.292090 0.116979 0.146 Uiso 1 1 calc R U . . .
C26 C -0.0026(3) 0.2461(3) 0.0378(2) 0.1429(17) Uani 1 1 d . . . . .
H26A H -0.036432 0.260777 0.015810 0.171 Uiso 1 1 calc R U . . .
C27 C 0.0387(3) 0.2049(3) 0.0112(2) 0.1511(19) Uani 1 1 d . . . . .
H27A H 0.033125 0.191909 -0.029452 0.181 Uiso 1 1 calc R U . . .
C28 C 0.0877(2) 0.1835(2) 0.04505(17) 0.1203(12) Uani 1 1 d . . . . .
H28A H 0.114929 0.155879 0.026546 0.144 Uiso 1 1 calc R U . . .
Fe3 Fe 0.30965(2) 0.30965(2) 0.30965(2) 0.07608(15) Uani 1 3 d S T P . .
O1 O 0.27766(8) 0.38023(8) 0.36045(7) 0.0757(3) Uani 1 1 d . . . . .
O2 O 0.24746(9) 0.34123(8) 0.24941(7) 0.0803(4) Uani 1 1 d . . . . .
O3 O 0.11155(16) 0.5087(2) 0.22659(15) 0.1477(14) Uani 1 1 d . U . . .
O4 O 0.13699(18) 0.54436(19) 0.34253(16) 0.1506(14) Uani 1 1 d . U . . .
C29 C 0.23481(10) 0.41246(11) 0.33292(10) 0.0751(4) Uani 1 1 d . . . . .
C30 C 0.21878(11) 0.39112(12) 0.26861(10) 0.0779(5) Uani 1 1 d . . . . .
C31 C 0.17772(14) 0.42320(17) 0.23336(13) 0.0968(8) Uani 1 1 d . . . . .
H31A H 0.168855 0.409484 0.193591 0.116 Uiso 1 1 calc R U . . .
C32 C 0.14805(15) 0.4774(2) 0.25620(15) 0.1039(9) Uani 1 1 d . U . . .
C33 C 0.16288(15) 0.49748(18) 0.32334(15) 0.1019(8) Uani 1 1 d . U . . .
C34 C 0.20633(12) 0.46233(14) 0.35783(12) 0.0870(6) Uani 1 1 d . . . . .
H34A H 0.215390 0.473779 0.398268 0.104 Uiso 1 1 calc R U . . .
O1S O 0.3945(7) 0.3463(5) 0.7317(5) 0.216(5) Uani 0.624(14) 1 d D U P . .
H1S H 0.385154 0.382265 0.738922 0.324 Uiso 0.624(14) 1 calc R U P . .
C1S C 0.3817(9) 0.3094(8) 0.7842(8) 0.233(8) Uani 0.624(14) 1 d D U P . .
H1S1 H 0.409321 0.320372 0.817143 0.350 Uiso 0.624(14) 1 calc R U P . .
H1S2 H 0.387187 0.266551 0.773948 0.350 Uiso 0.624(14) 1 calc R U P . .
H1S3 H 0.339773 0.316190 0.797192 0.350 Uiso 0.624(14) 1 calc R U P . .
B1 B -0.1152(8) 0.3827(11) 0.1191(11) 0.151(4) Uani 0.3333 1 d D U P A -1
F1 F -0.1029(10) 0.3554(10) 0.1759(9) 0.201(7) Uani 0.3333 1 d D U P A -1
F2 F -0.0638(7) 0.4149(11) 0.1033(8) 0.202(5) Uani 0.3333 1 d D U P A -1
F3 F -0.1648(9) 0.4212(10) 0.1255(11) 0.197(8) Uani 0.3333 1 d D U P A -1
F4 F -0.1261(8) 0.3373(9) 0.0766(10) 0.184(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.978(2) 9 ?
Fe1 N2 1.978(2) 5 ?
Fe1 N2 1.978(2) . ?
Fe1 N1 2.033(2) . ?
Fe1 N1 2.033(2) 9 ?
Fe1 N1 2.033(2) 5 ?
Fe2 N5 2.075(2) . ?
Fe2 N5 2.075(2) 9 ?
Fe2 N5 2.075(2) 5 ?
Fe2 N6 2.124(2) 5 ?
Fe2 N6 2.124(2) 9 ?
Fe2 N6 2.124(2) . ?
N1 C1 1.350(3) . ?
N1 C5 1.353(3) . ?
N2 C6 1.336(3) . ?
N2 N3 1.350(3) . ?
N3 C8 1.364(3) . ?
N3 H3 0.90(2) . ?
N4 N5 1.341(3) . ?
N4 C21 1.360(3) . ?
N4 H4 0.88(3) . ?
N5 C23 1.349(3) . ?
N6 C28 1.344(4) . ?
N6 C24 1.358(4) . ?
C1 C2 1.381(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.364(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.390(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.381(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.465(3) . ?
C6 C7 1.389(4) . ?
C7 C8 1.373(4) . ?
C7 H7A 0.9300 . ?
C8 C10 1.470(3) . ?
C9 C10 1.383(4) . ?
C9 C14 1.401(4) . ?
C9 H9A 0.9300 . ?
C10 C11 1.389(4) . ?
C11 C12 1.387(5) . ?
C11 H11A 0.9300 . ?
C12 C13 1.371(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.385(5) . ?
C13 H13A 0.9300 . ?
C14 C16 1.463(5) . ?
C15 C20 1.373(4) . ?
C15 C16 1.396(4) . ?
C15 H15A 0.9300 . ?
C16 C17 1.392(4) . ?
C17 C18 1.380(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.374(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.395(4) . ?
C19 H19A 0.9300 . ?
C20 C21 1.469(4) . ?
C21 C22 1.386(4) . ?
C22 C23 1.381(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.466(4) . ?
C24 C25 1.370(4) . ?
C25 C26 1.376(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.386(8) . ?
C26 H26A 0.9300 . ?
C27 C28 1.369(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9936(17) 9 ?
Fe3 O2 1.9936(17) 5 ?
Fe3 O2 1.9936(17) . ?
Fe3 O1 2.0042(16) . ?
Fe3 O1 2.0043(16) 5 ?
Fe3 O1 2.0043(16) 9 ?
O1 C29 1.304(3) . ?
O2 C30 1.312(3) . ?
O3 C32 1.221(4) . ?
O4 C33 1.231(4) . ?
C29 C34 1.354(4) . ?
C29 C30 1.506(3) . ?
C30 C31 1.361(4) . ?
C31 C32 1.425(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.549(5) . ?
C33 C34 1.421(4) . ?
C34 H34A 0.9300 . ?
O1S C1S 1.416(16) . ?
O1S H1S 0.8200 . ?
C1S H1S1 0.9600 . ?
C1S H1S2 0.9600 . ?
C1S H1S3 0.9600 . ?
B1 F2 1.356(15) . ?
B1 F3 1.365(19) . ?
B1 F4 1.37(2) . ?
B1 F1 1.39(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.07(7) 9 5 ?
N2 Fe1 N2 96.07(7) 9 . ?
N2 Fe1 N2 96.07(7) 5 . ?
N2 Fe1 N1 171.38(8) 9 . ?
N2 Fe1 N1 91.92(8) 5 . ?
N2 Fe1 N1 79.83(8) . . ?
N2 Fe1 N1 79.83(8) 9 9 ?
N2 Fe1 N1 171.38(8) 5 9 ?
N2 Fe1 N1 91.92(8) . 9 ?
N1 Fe1 N1 92.67(8) . 9 ?
N2 Fe1 N1 91.92(8) 9 5 ?
N2 Fe1 N1 79.83(8) 5 5 ?
N2 Fe1 N1 171.38(8) . 5 ?
N1 Fe1 N1 92.67(8) . 5 ?
N1 Fe1 N1 92.67(8) 9 5 ?
N5 Fe2 N5 97.52(8) . 9 ?
N5 Fe2 N5 97.53(8) . 5 ?
N5 Fe2 N5 97.52(8) 9 5 ?
N5 Fe2 N6 94.16(9) . 5 ?
N5 Fe2 N6 167.79(9) 9 5 ?
N5 Fe2 N6 77.35(9) 5 5 ?
N5 Fe2 N6 167.79(9) . 9 ?
N5 Fe2 N6 77.35(9) 9 9 ?
N5 Fe2 N6 94.16(9) 5 9 ?
N6 Fe2 N6 91.85(10) 5 9 ?
N5 Fe2 N6 77.35(9) . . ?
N5 Fe2 N6 94.16(9) 9 . ?
N5 Fe2 N6 167.79(9) 5 . ?
N6 Fe2 N6 91.85(10) 5 . ?
N6 Fe2 N6 91.85(10) 9 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 126.9(2) . . ?
C5 N1 Fe1 114.80(16) . . ?
C6 N2 N3 105.39(19) . . ?
C6 N2 Fe1 116.04(16) . . ?
N3 N2 Fe1 137.18(15) . . ?
N2 N3 C8 111.08(19) . . ?
N2 N3 H3 126(3) . . ?
C8 N3 H3 121(3) . . ?
N5 N4 C21 111.5(2) . . ?
N5 N4 H4 114(3) . . ?
C21 N4 H4 135(3) . . ?
N4 N5 C23 105.4(2) . . ?
N4 N5 Fe2 136.03(17) . . ?
C23 N5 Fe2 115.06(18) . . ?
C28 N6 C24 116.8(3) . . ?
C28 N6 Fe2 128.2(3) . . ?
C24 N6 Fe2 114.78(18) . . ?
N1 C1 C2 121.6(3) . . ?
N1 C1 H1A 119.2 . . ?
C2 C1 H1A 119.2 . . ?
C3 C2 C1 120.0(3) . . ?
C3 C2 H2A 120.0 . . ?
C1 C2 H2A 120.0 . . ?
C2 C3 C4 119.3(3) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 118.3(3) . . ?
C5 C4 H4A 120.8 . . ?
C3 C4 H4A 120.8 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 113.4(2) . . ?
C4 C5 C6 124.0(3) . . ?
N2 C6 C7 111.3(2) . . ?
N2 C6 C5 115.3(2) . . ?
C7 C6 C5 133.4(2) . . ?
C8 C7 C6 105.2(2) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.0(2) . . ?
N3 C8 C10 123.2(2) . . ?
C7 C8 C10 129.8(2) . . ?
C10 C9 C14 120.7(3) . . ?
C10 C9 H9A 119.6 . . ?
C14 C9 H9A 119.6 . . ?
C9 C10 C11 119.8(3) . . ?
C9 C10 C8 121.9(2) . . ?
C11 C10 C8 118.3(3) . . ?
C12 C11 C10 119.8(3) . . ?
C12 C11 H11A 120.1 . . ?
C10 C11 H11A 120.1 . . ?
C13 C12 C11 120.0(4) . . ?
C13 C12 H12A 120.0 . . ?
C11 C12 H12A 120.0 . . ?
C12 C13 C14 121.4(3) . . ?
C12 C13 H13A 119.3 . . ?
C14 C13 H13A 119.3 . . ?
C13 C14 C9 118.2(3) . . ?
C13 C14 C16 121.0(3) . . ?
C9 C14 C16 120.5(3) . . ?
C20 C15 C16 122.0(2) . . ?
C20 C15 H15A 119.0 . . ?
C16 C15 H15A 119.0 . . ?
C17 C16 C15 118.4(3) . . ?
C17 C16 C14 123.1(3) . . ?
C15 C16 C14 118.4(2) . . ?
C18 C17 C16 119.4(3) . . ?
C18 C17 H17A 120.3 . . ?
C16 C17 H17A 120.3 . . ?
C19 C18 C17 121.9(3) . . ?
C19 C18 H18A 119.1 . . ?
C17 C18 H18A 119.1 . . ?
C18 C19 C20 119.3(4) . . ?
C18 C19 H19A 120.3 . . ?
C20 C19 H19A 120.3 . . ?
C15 C20 C19 119.0(3) . . ?
C15 C20 C21 120.8(2) . . ?
C19 C20 C21 119.8(3) . . ?
N4 C21 C22 106.7(2) . . ?
N4 C21 C20 121.9(2) . . ?
C22 C21 C20 131.2(2) . . ?
C23 C22 C21 105.2(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.2(2) . . ?
N5 C23 C24 116.3(2) . . ?
C22 C23 C24 132.4(2) . . ?
N6 C24 C25 122.9(3) . . ?
N6 C24 C23 114.2(2) . . ?
C25 C24 C23 122.8(3) . . ?
C24 C25 C26 119.5(4) . . ?
C24 C25 H25A 120.3 . . ?
C26 C25 H25A 120.3 . . ?
C25 C26 C27 118.2(4) . . ?
C25 C26 H26A 120.9 . . ?
C27 C26 H26A 120.9 . . ?
C28 C27 C26 119.5(4) . . ?
C28 C27 H27A 120.3 . . ?
C26 C27 H27A 120.3 . . ?
N6 C28 C27 123.0(4) . . ?
N6 C28 H28A 118.5 . . ?
C27 C28 H28A 118.5 . . ?
O2 Fe3 O2 90.81(8) 9 5 ?
O2 Fe3 O2 90.80(8) 9 . ?
O2 Fe3 O2 90.80(8) 5 . ?
O2 Fe3 O1 170.45(7) 9 . ?
O2 Fe3 O1 95.77(8) 5 . ?
O2 Fe3 O1 82.21(6) . . ?
O2 Fe3 O1 95.77(8) 9 5 ?
O2 Fe3 O1 82.21(6) 5 5 ?
O2 Fe3 O1 170.45(7) . 5 ?
O1 Fe3 O1 91.99(7) . 5 ?
O2 Fe3 O1 82.20(6) 9 9 ?
O2 Fe3 O1 170.45(7) 5 9 ?
O2 Fe3 O1 95.77(8) . 9 ?
O1 Fe3 O1 91.99(7) . 9 ?
O1 Fe3 O1 91.99(7) 5 9 ?
C29 O1 Fe3 113.73(14) . . ?
C30 O2 Fe3 113.19(14) . . ?
O1 C29 C34 124.6(2) . . ?
O1 C29 C30 114.9(2) . . ?
C34 C29 C30 120.5(2) . . ?
O2 C30 C31 123.4(2) . . ?
O2 C30 C29 115.8(2) . . ?
C31 C30 C29 120.8(2) . . ?
C30 C31 C32 121.3(3) . . ?
C30 C31 H31A 119.4 . . ?
C32 C31 H31A 119.4 . . ?
O3 C32 C31 124.4(3) . . ?
O3 C32 C33 118.1(3) . . ?
C31 C32 C33 117.5(3) . . ?
O4 C33 C34 124.4(3) . . ?
O4 C33 C32 116.9(3) . . ?
C34 C33 C32 118.6(3) . . ?
C29 C34 C33 121.2(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
C1S O1S H1S 109.5 . . ?
O1S C1S H1S1 109.5 . . ?
O1S C1S H1S2 109.5 . . ?
H1S1 C1S H1S2 109.5 . . ?
O1S C1S H1S3 109.5 . . ?
H1S1 C1S H1S3 109.5 . . ?
H1S2 C1S H1S3 109.5 . . ?
F2 B1 F3 111.0(17) . . ?
F2 B1 F4 109.9(17) . . ?
F3 B1 F4 111.8(16) . . ?
F2 B1 F1 106.5(15) . . ?
F3 B1 F1 108.7(17) . . ?
F4 B1 F1 108.7(17) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(2) 2.06(3) 2.947(2) 169(4) . yes
N4 H4 O2 0.88(3) 2.14(3) 2.996(3) 164(5) 5 yes

_refine_diff_density_max         0.325
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.078

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205_fresh2_300Kd
_database_code_depnum_ccdc_archive 'CCDC 2261733'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0066 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0065
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0186 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3512 0.8903
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.725(3)
_cell_length_b                   21.725(3)
_cell_length_c                   21.725(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10254(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    6583
_cell_measurement_theta_min      1.36
_cell_measurement_theta_max      33.71

_exptl_crystal_description       block
_exptl_crystal_colour            'dark orange'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.525
_shelx_estimated_absorpt_T_min   0.880
_shelx_estimated_absorpt_T_max   0.902
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.93
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_process_details   XDS/XSCALE
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.72932
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'ALBA XALOC beamline'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'MD2M - Maatel + Dectris PILATUS 6M'
_diffrn_measurement_method       'ω rotation'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            167046
_diffrn_reflns_av_unetI/netI     0.0194
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.924
_diffrn_reflns_theta_max         29.507
_diffrn_reflns_theta_full        29.507
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8837
_reflns_number_gt                8554
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'autoPROC package'
_computing_cell_refinement       XDS
_computing_data_reduction        
;
autoPROC (Vonrhein, C., Flensburg, C., Keller, P., Sharff, A., Smart, O., Paciorek, W., Womack, T. & Bricogne, G. (2011). Acta Cryst. D67, 293-302)
XDS (Kabsch, W. (2010). Acta Cryst. D66, 125-132)
pointless (Evans, P.R. (2006). Acta Cryst. D62, 72-82)
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. Hydrogens were placed
 geometrically on their carrier atom and refined with a riding model,
 except those on the pyrazole N that were found in a difference Fourier
 map and refined with their thermal parameter 1.5 times that of their
 carrier N and a distance restraint.
 The BF4 anion is disordered by symmetry and was refined with both distance
 restraints as well as displacement parameters restraints. 
 At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1732 cubic angstrom with <100 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 

 Details of SQUEEZE analysis :
# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.118  0.151  0.141      1841        80 ' '
   2  0.144  0.356  0.644        10         0 ' '
   3  0.356  0.644  0.144        10         0 ' '
   4  0.644  0.144  0.356        10         0 ' '
   5  0.856  0.856  0.856        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205_fresh2_300Kd 
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        1837 Ang**3      
RESPONSE: At the end of the refinement, there remained an area of the cell with
 only very weak electron density peaks. Analysis with PLATON/SQUEEZE
 returned a void of 1841 cubic angstrom with a total of 80 electrons.
 While these figures could agree with a very small amount of 
 very diffuse lattice methanol, the same crystal has 
 presented similar amount of residual electrons throughout a whole thermal 
 cycling process over which it has lost its initial lattice MeOH solvent. 
 We therefore believe that although there may still be some diffuse lattice
 solvent, the amount is necessarily vanishingly small. Consequently we have 
 decided to not use the structure refined after PLATON/SQUEEZE treatment, 
 and report the present structure with a large empty void. 
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0771P)²+0.2794P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_extinction_coef       0.0046(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 3826 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.081(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8837
_refine_ls_number_parameters     459
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0340
_refine_ls_wR_factor_ref         0.1044
_refine_ls_wR_factor_gt          0.1035
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29787(2) 0.29787(2) 0.29787(2) 0.06263(12) Uani 1 3 d S T P . .
Fe2 Fe 0.57919(2) 0.57919(2) 0.57919(2) 0.06569(13) Uani 1 3 d S T P . .
N1 N 0.23335(9) 0.33191(9) 0.24098(8) 0.0704(4) Uani 1 1 d . . . . .
N2 N 0.26101(8) 0.36026(9) 0.35204(8) 0.0666(3) Uani 1 1 d . . . . .
N3 N 0.26520(8) 0.37584(9) 0.41214(8) 0.0680(4) Uani 1 1 d D . . . .
H3 H 0.2979(13) 0.3625(18) 0.4317(16) 0.102 Uiso 1 1 d D U . . .
N4 N 0.47099(9) 0.49342(10) 0.61541(9) 0.0715(4) Uani 1 1 d D . . . .
H4 H 0.4486(16) 0.5036(17) 0.5841(14) 0.107 Uiso 1 1 d D U . . .
N5 N 0.53050(9) 0.51090(9) 0.61668(9) 0.0706(4) Uani 1 1 d . . . . .
N6 N 0.64087(10) 0.54498(11) 0.64109(11) 0.0804(5) Uani 1 1 d . . . . .
C1 C 0.22251(14) 0.31553(13) 0.18285(11) 0.0812(6) Uani 1 1 d . . . . .
H1A H 0.248010 0.286366 0.164635 0.097 Uiso 1 1 calc R U . . .
C2 C 0.17479(18) 0.34022(16) 0.14846(14) 0.0996(9) Uani 1 1 d . . . . .
H2A H 0.168080 0.327197 0.108242 0.120 Uiso 1 1 calc R U . . .
C3 C 0.13748(18) 0.38421(18) 0.17455(16) 0.1041(9) Uani 1 1 d . . . . .
H3B H 0.105348 0.401437 0.152126 0.125 Uiso 1 1 calc R U . . .
C4 C 0.14829(16) 0.40240(15) 0.23425(15) 0.0937(8) Uani 1 1 d . . . . .
H4B H 0.123918 0.432409 0.252626 0.112 Uiso 1 1 calc R U . . .
C5 C 0.19627(11) 0.37514(11) 0.26658(11) 0.0732(5) Uani 1 1 d . . . . .
C6 C 0.21089(10) 0.38849(11) 0.33059(11) 0.0717(5) Uani 1 1 d . . . . .
C7 C 0.18262(11) 0.42270(13) 0.37655(13) 0.0795(5) Uani 1 1 d . . . . .
H7A H 0.146980 0.446169 0.373147 0.095 Uiso 1 1 calc R U . . .
C8 C 0.21830(10) 0.41463(11) 0.42808(11) 0.0732(5) Uani 1 1 d . . . . .
C9 C 0.21106(10) 0.43965(13) 0.49046(12) 0.0786(5) Uani 1 1 d . . . . .
C10 C 0.16364(16) 0.4814(2) 0.50202(17) 0.1055(10) Uani 1 1 d . . . . .
H10A H 0.137890 0.493791 0.470156 0.127 Uiso 1 1 calc R U . . .
C11 C 0.15485(19) 0.5043(3) 0.5606(2) 0.1355(17) Uani 1 1 d . . . . .
H11A H 0.123824 0.532803 0.568016 0.163 Uiso 1 1 calc R U . . .
C12 C 0.19232(17) 0.4846(3) 0.60844(18) 0.1226(14) Uani 1 1 d . . . . .
H12A H 0.184606 0.498240 0.648286 0.147 Uiso 1 1 calc R U . . .
C13 C 0.24099(12) 0.44510(16) 0.59762(13) 0.0903(7) Uani 1 1 d . . . . .
C14 C 0.24922(11) 0.42241(13) 0.53804(11) 0.0797(6) Uani 1 1 d . . . . .
H14A H 0.281207 0.395023 0.530317 0.096 Uiso 1 1 calc R U . . .
C15 C 0.28691(13) 0.43080(16) 0.64550(12) 0.0907(7) Uani 1 1 d . . . . .
C16 C 0.27166(18) 0.4068(3) 0.70266(16) 0.1253(15) Uani 1 1 d . . . . .
H16A H 0.230902 0.397517 0.711877 0.150 Uiso 1 1 calc R U . . .
C17 C 0.3168(2) 0.3968(3) 0.74549(16) 0.1344(17) Uani 1 1 d . . . . .
H17A H 0.306120 0.380827 0.783747 0.161 Uiso 1 1 calc R U . . .
C18 C 0.37855(18) 0.4098(2) 0.73326(15) 0.1146(12) Uani 1 1 d . . . . .
H18A H 0.408826 0.401626 0.762382 0.137 Uiso 1 1 calc R U . . .
C19 C 0.39393(12) 0.43565(14) 0.67611(11) 0.0826(6) Uani 1 1 d . . . . .
C20 C 0.34853(12) 0.44443(14) 0.63322(11) 0.0813(6) Uani 1 1 d . . . . .
H20A H 0.359070 0.459954 0.594739 0.098 Uiso 1 1 calc R U . . .
C21 C 0.45740(12) 0.45730(12) 0.66472(11) 0.0760(5) Uani 1 1 d . . . . .
C22 C 0.51031(13) 0.45262(13) 0.69945(12) 0.0828(6) Uani 1 1 d . . . . .
H22A H 0.515448 0.431285 0.736209 0.099 Uiso 1 1 calc R U . . .
C23 C 0.55406(12) 0.48638(11) 0.66802(11) 0.0744(5) Uani 1 1 d . . . . .
C24 C 0.61797(13) 0.50306(13) 0.68075(13) 0.0824(6) Uani 1 1 d . . . . .
C25 C 0.65156(17) 0.47918(18) 0.72919(19) 0.1093(10) Uani 1 1 d . . . . .
H25A H 0.633961 0.451321 0.756514 0.131 Uiso 1 1 calc R U . . .
C26 C 0.7117(2) 0.4977(2) 0.7359(2) 0.1318(15) Uani 1 1 d . . . . .
H26A H 0.735452 0.482335 0.768033 0.158 Uiso 1 1 calc R U . . .
C27 C 0.73662(17) 0.5388(2) 0.6952(2) 0.1283(15) Uani 1 1 d . . . . .
H27A H 0.777468 0.551065 0.699040 0.154 Uiso 1 1 calc R U . . .
C28 C 0.70033(14) 0.56199(18) 0.64837(18) 0.1023(9) Uani 1 1 d . . . . .
H28A H 0.717337 0.590144 0.620970 0.123 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43689(2) 0.43689(2) 0.43689(2) 0.06986(14) Uani 1 3 d S T P . .
O1 O 0.38473(7) 0.36818(7) 0.47014(7) 0.0681(3) Uani 1 1 d . . . . .
O2 O 0.49581(7) 0.40601(8) 0.50012(8) 0.0718(3) Uani 1 1 d . . . . .
O3 O 0.51215(15) 0.2500(2) 0.64648(17) 0.175(2) Uani 1 1 d . . . . .
O4 O 0.39704(15) 0.21450(19) 0.62100(16) 0.1571(16) Uani 1 1 d . U . . .
C29 C 0.41066(10) 0.33848(11) 0.51513(10) 0.0684(4) Uani 1 1 d . . . . .
C30 C 0.47483(10) 0.35907(11) 0.53104(10) 0.0704(4) Uani 1 1 d . . . . .
C31 C 0.50822(13) 0.32942(16) 0.57424(13) 0.0925(8) Uani 1 1 d . . . . .
H31A H 0.548269 0.342327 0.582124 0.111 Uiso 1 1 calc R U . . .
C32 C 0.48392(15) 0.2793(2) 0.60781(15) 0.1084(11) Uani 1 1 d . U . . .
C33 C 0.41738(15) 0.25803(19) 0.59260(15) 0.1024(10) Uani 1 1 d . U . . .
C34 C 0.38444(12) 0.29099(14) 0.54597(12) 0.0821(6) Uani 1 1 d . . . . .
H34A H 0.344246 0.279585 0.536658 0.099 Uiso 1 1 calc R U . . .
B1 B 0.1423(11) 0.1437(9) 0.1432(10) 0.1152(19) Uani 0.3333 1 d D U P A -1
F1 F 0.1167(9) 0.1547(8) 0.0869(7) 0.173(5) Uani 0.3333 1 d D U P A -1
F2 F 0.1746(15) 0.1941(8) 0.1578(11) 0.197(6) Uani 0.3333 1 d D U P A -1
F3 F 0.0966(11) 0.1333(12) 0.1849(9) 0.152(6) Uani 0.3333 1 d D U P A -1
F4 F 0.1805(12) 0.0941(11) 0.1410(12) 0.168(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9654(18) . ?
Fe1 N2 1.9655(18) 5 ?
Fe1 N2 1.9655(18) 9 ?
Fe1 N1 2.0098(19) 5 ?
Fe1 N1 2.0098(19) 9 ?
Fe1 N1 2.0099(19) . ?
Fe2 N5 1.996(2) 5 ?
Fe2 N5 1.996(2) 9 ?
Fe2 N5 1.996(2) . ?
Fe2 N6 2.039(2) 9 ?
Fe2 N6 2.039(2) 5 ?
Fe2 N6 2.039(2) . ?
N1 C1 1.333(3) . ?
N1 C5 1.356(3) . ?
N2 C6 1.334(3) . ?
N2 N3 1.352(3) . ?
N3 C8 1.367(3) . ?
N3 H3 0.88(2) . ?
N4 N5 1.348(3) . ?
N4 C21 1.360(3) . ?
N4 H4 0.86(2) . ?
N5 C23 1.338(3) . ?
N6 C24 1.349(4) . ?
N6 C28 1.353(4) . ?
C1 C2 1.386(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.375(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.376(5) . ?
C3 H3B 0.9300 . ?
C4 C5 1.390(3) . ?
C4 H4B 0.9300 . ?
C5 C6 1.456(3) . ?
C6 C7 1.388(3) . ?
C7 C8 1.373(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.469(3) . ?
C9 C14 1.377(4) . ?
C9 C10 1.395(4) . ?
C10 C11 1.380(5) . ?
C10 H10A 0.9300 . ?
C11 C12 1.387(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.397(4) . ?
C13 C15 1.474(4) . ?
C14 H14A 0.9300 . ?
C15 C16 1.387(4) . ?
C15 C20 1.397(3) . ?
C16 C17 1.370(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.396(5) . ?
C17 H17A 0.9300 . ?
C18 C19 1.403(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.370(4) . ?
C19 C21 1.478(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.379(4) . ?
C22 C23 1.381(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.461(4) . ?
C24 C25 1.382(4) . ?
C25 C26 1.376(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.368(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.382(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9940(16) 9 ?
Fe3 O2 1.9940(16) . ?
Fe3 O2 1.9941(16) 5 ?
Fe3 O1 2.0084(15) . ?
Fe3 O1 2.0084(15) 5 ?
Fe3 O1 2.0084(15) 9 ?
O1 C29 1.300(3) . ?
O2 C30 1.303(3) . ?
O3 C32 1.219(4) . ?
O4 C33 1.213(4) . ?
C29 C34 1.356(3) . ?
C29 C30 1.504(3) . ?
C30 C31 1.350(3) . ?
C31 C32 1.413(4) . ?
C31 H31A 0.9300 . ?
C32 C33 1.553(4) . ?
C33 C34 1.432(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.338(13) . ?
B1 F4 1.363(19) . ?
B1 F3 1.36(2) . ?
B1 F1 1.364(18) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.43(7) . 5 ?
N2 Fe1 N2 96.43(7) . 9 ?
N2 Fe1 N2 96.43(7) 5 9 ?
N2 Fe1 N1 90.58(8) . 5 ?
N2 Fe1 N1 80.23(7) 5 5 ?
N2 Fe1 N1 172.55(8) 9 5 ?
N2 Fe1 N1 172.55(8) . 9 ?
N2 Fe1 N1 90.58(8) 5 9 ?
N2 Fe1 N1 80.23(7) 9 9 ?
N1 Fe1 N1 93.10(8) 5 9 ?
N2 Fe1 N1 80.23(7) . . ?
N2 Fe1 N1 172.55(8) 5 . ?
N2 Fe1 N1 90.58(8) 9 . ?
N1 Fe1 N1 93.10(8) 5 . ?
N1 Fe1 N1 93.10(8) 9 . ?
N5 Fe2 N5 97.23(7) 5 9 ?
N5 Fe2 N5 97.22(7) 5 . ?
N5 Fe2 N5 97.22(8) 9 . ?
N5 Fe2 N6 170.73(9) 5 9 ?
N5 Fe2 N6 78.94(8) 9 9 ?
N5 Fe2 N6 91.66(9) . 9 ?
N5 Fe2 N6 78.94(8) 5 5 ?
N5 Fe2 N6 91.66(9) 9 5 ?
N5 Fe2 N6 170.73(9) . 5 ?
N6 Fe2 N6 92.66(9) 9 5 ?
N5 Fe2 N6 91.65(9) 5 . ?
N5 Fe2 N6 170.73(9) 9 . ?
N5 Fe2 N6 78.94(8) . . ?
N6 Fe2 N6 92.66(9) 9 . ?
N6 Fe2 N6 92.66(9) 5 . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Fe1 127.41(18) . . ?
C5 N1 Fe1 114.63(15) . . ?
C6 N2 N3 106.10(18) . . ?
C6 N2 Fe1 116.13(15) . . ?
N3 N2 Fe1 136.34(14) . . ?
N2 N3 C8 110.42(18) . . ?
N2 N3 H3 116(3) . . ?
C8 N3 H3 133(3) . . ?
N5 N4 C21 110.8(2) . . ?
N5 N4 H4 119(3) . . ?
C21 N4 H4 130(3) . . ?
C23 N5 N4 105.8(2) . . ?
C23 N5 Fe2 115.69(17) . . ?
N4 N5 Fe2 135.19(16) . . ?
C24 N6 C28 117.5(2) . . ?
C24 N6 Fe2 115.16(17) . . ?
C28 N6 Fe2 127.2(2) . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.2(3) . . ?
C2 C3 H3B 120.4 . . ?
C4 C3 H3B 120.4 . . ?
C3 C4 C5 118.8(3) . . ?
C3 C4 H4B 120.6 . . ?
C5 C4 H4B 120.6 . . ?
N1 C5 C4 122.2(2) . . ?
N1 C5 C6 113.6(2) . . ?
C4 C5 C6 124.2(2) . . ?
N2 C6 C7 110.9(2) . . ?
N2 C6 C5 114.9(2) . . ?
C7 C6 C5 134.2(2) . . ?
C8 C7 C6 105.6(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 107.0(2) . . ?
N3 C8 C9 122.8(2) . . ?
C7 C8 C9 130.2(2) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 C8 121.8(2) . . ?
C10 C9 C8 119.1(3) . . ?
C11 C10 C9 120.2(4) . . ?
C11 C10 H10A 119.9 . . ?
C9 C10 H10A 119.9 . . ?
C10 C11 C12 119.9(3) . . ?
C10 C11 H11A 120.0 . . ?
C12 C11 H11A 120.0 . . ?
C13 C12 C11 120.8(3) . . ?
C13 C12 H12A 119.6 . . ?
C11 C12 H12A 119.6 . . ?
C12 C13 C14 118.4(3) . . ?
C12 C13 C15 121.9(3) . . ?
C14 C13 C15 119.5(3) . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.7(3) . . ?
C16 C15 C13 123.3(3) . . ?
C20 C15 C13 118.0(2) . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 121.8(3) . . ?
C16 C17 H17A 119.1 . . ?
C18 C17 H17A 119.1 . . ?
C17 C18 C19 118.6(3) . . ?
C17 C18 H18A 120.7 . . ?
C19 C18 H18A 120.7 . . ?
C20 C19 C18 119.1(3) . . ?
C20 C19 C21 120.9(2) . . ?
C18 C19 C21 119.9(3) . . ?
C19 C20 C15 122.0(2) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 107.0(2) . . ?
N4 C21 C19 121.2(2) . . ?
C22 C21 C19 131.5(2) . . ?
C21 C22 C23 105.3(2) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 115.0(2) . . ?
C22 C23 C24 133.8(2) . . ?
N6 C24 C25 123.1(3) . . ?
N6 C24 C23 113.4(2) . . ?
C25 C24 C23 123.6(3) . . ?
C26 C25 C24 118.2(4) . . ?
C26 C25 H25A 120.9 . . ?
C24 C25 H25A 120.9 . . ?
C27 C26 C25 119.9(3) . . ?
C27 C26 H26A 120.1 . . ?
C25 C26 H26A 120.1 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.1(4) . . ?
N6 C28 H28A 119.0 . . ?
C27 C28 H28A 119.0 . . ?
O2 Fe3 O2 90.31(7) 9 . ?
O2 Fe3 O2 90.31(7) 9 5 ?
O2 Fe3 O2 90.31(7) . 5 ?
O2 Fe3 O1 95.24(7) 9 . ?
O2 Fe3 O1 82.20(6) . . ?
O2 Fe3 O1 170.68(6) 5 . ?
O2 Fe3 O1 170.69(6) 9 5 ?
O2 Fe3 O1 95.24(7) . 5 ?
O2 Fe3 O1 82.20(6) 5 5 ?
O1 Fe3 O1 92.92(6) . 5 ?
O2 Fe3 O1 82.20(6) 9 9 ?
O2 Fe3 O1 170.69(6) . 9 ?
O2 Fe3 O1 95.24(7) 5 9 ?
O1 Fe3 O1 92.92(6) . 9 ?
O1 Fe3 O1 92.92(6) 5 9 ?
C29 O1 Fe3 113.27(13) . . ?
C30 O2 Fe3 113.19(13) . . ?
O1 C29 C34 124.6(2) . . ?
O1 C29 C30 115.3(2) . . ?
C34 C29 C30 120.1(2) . . ?
O2 C30 C31 122.9(2) . . ?
O2 C30 C29 116.00(19) . . ?
C31 C30 C29 121.1(2) . . ?
C30 C31 C32 121.7(2) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O3 C32 C31 124.7(3) . . ?
O3 C32 C33 117.4(3) . . ?
C31 C32 C33 117.8(2) . . ?
O4 C33 C34 124.6(3) . . ?
O4 C33 C32 117.6(3) . . ?
C34 C33 C32 117.9(3) . . ?
C29 C34 C33 121.3(2) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F2 B1 F4 109.7(16) . . ?
F2 B1 F3 111.1(16) . . ?
F4 B1 F3 109.6(17) . . ?
F2 B1 F1 106.5(15) . . ?
F4 B1 F1 110.8(16) . . ?
F3 B1 F1 109.2(16) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(2) 2.07(3) 2.891(2) 156(4) . yes
N4 H4 O2 0.86(2) 2.13(3) 2.961(2) 161(3) 9 yes

_refine_diff_density_max         0.283
_refine_diff_density_min         -0.373
_refine_diff_density_rms         0.046

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-300K
_database_code_depnum_ccdc_archive 'CCDC 2261757'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.6924(5)
_cell_length_b                   21.6924(5)
_cell_length_c                   21.6924(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10207.6(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    300(2)
_cell_measurement_reflns_used    9385
_cell_measurement_theta_min      3.04
_cell_measurement_theta_max      27.31

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      300(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            154529
_diffrn_reflns_av_unetI/netI     0.0271
_diffrn_reflns_av_R_equivalents  0.0450
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.153
_diffrn_reflns_theta_max         27.862
_diffrn_reflns_theta_full        27.850
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7528
_reflns_number_gt                7094
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.852
_reflns_Friedel_fraction_max     0.995
_reflns_Friedel_fraction_full    0.995

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1834 cubic angstrom  with only 122 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.159  0.117  0.620      1834       122 ' '
   2  0.144  0.856  0.356        10         0 ' '
   3  0.356  0.144  0.856        10         0 ' '
   4  0.644  0.644  0.644        10         0 ' '
   5  0.856  0.356  0.144        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-300K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1834 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1834 cubic angstrom  with only 122 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.159  0.117  0.620      1834       122 ' '
   2  0.144  0.856  0.356        10         0 ' '
   3  0.356  0.144  0.856        10         0 ' '
   4  0.644  0.644  0.644        10         0 ' '
   5  0.856  0.356  0.144        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0610P)²+0.5845P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3123 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7528
_refine_ls_number_parameters     457
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0353
_refine_ls_wR_factor_ref         0.0928
_refine_ls_wR_factor_gt          0.0912
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.082
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.29798(2) 0.79798(2) 0.70202(2) 0.04710(14) Uani 1 3 d S T P . .
Fe2 Fe 0.57907(2) 1.07907(2) 0.42093(2) 0.04915(15) Uani 1 3 d S T P . .
N1 N 0.24114(10) 0.73356(10) 0.66804(10) 0.0544(5) Uani 1 1 d . . . . .
N2 N 0.35206(9) 0.76105(9) 0.63959(10) 0.0509(4) Uani 1 1 d . . . . .
N3 N 0.41204(10) 0.76520(9) 0.62404(10) 0.0521(4) Uani 1 1 d D . . . .
H3 H 0.4305(16) 0.8000(13) 0.6370(17) 0.078 Uiso 1 1 d D U . . .
N4 N 0.61538(10) 0.97090(10) 0.50677(12) 0.0553(5) Uani 1 1 d D . . . .
H4 H 0.5832(14) 0.9484(15) 0.5008(17) 0.083 Uiso 1 1 d D U . . .
N5 N 0.61651(10) 1.03047(10) 0.48913(11) 0.0546(5) Uani 1 1 d . . . . .
N6 N 0.64095(11) 1.14065(11) 0.45525(12) 0.0631(5) Uani 1 1 d . . . . .
C1 C 0.18295(12) 0.72278(15) 0.68436(14) 0.0654(7) Uani 1 1 d . . . . .
H1A H 0.164727 0.748284 0.713607 0.078 Uiso 1 1 calc R U . . .
C2 C 0.14855(15) 0.67520(19) 0.65957(17) 0.0832(10) Uani 1 1 d . . . . .
H2A H 0.108277 0.668432 0.672611 0.100 Uiso 1 1 calc R U . . .
C3 C 0.17453(17) 0.6382(2) 0.61561(19) 0.0882(11) Uani 1 1 d . . . . .
H3A H 0.151858 0.606327 0.598122 0.106 Uiso 1 1 calc R U . . .
C4 C 0.23426(16) 0.64850(17) 0.59746(16) 0.0774(9) Uani 1 1 d . . . . .
H4A H 0.252665 0.623862 0.567590 0.093 Uiso 1 1 calc R U . . .
C5 C 0.26652(13) 0.69652(13) 0.62472(12) 0.0579(6) Uani 1 1 d . . . . .
C6 C 0.33061(13) 0.71106(12) 0.61139(12) 0.0562(6) Uani 1 1 d . . . . .
C7 C 0.37639(14) 0.68293(12) 0.57713(14) 0.0636(6) Uani 1 1 d . . . . .
H7A H 0.372905 0.647372 0.553434 0.076 Uiso 1 1 calc R U . . .
C8 C 0.42805(13) 0.71848(11) 0.58540(13) 0.0571(6) Uani 1 1 d . . . . .
C9 C 0.49039(13) 0.71108(12) 0.56031(14) 0.0614(6) Uani 1 1 d . . . . .
C10 C 0.50176(19) 0.66375(17) 0.5188(2) 0.0885(11) Uani 1 1 d . . . . .
H10A H 0.469876 0.638018 0.506206 0.106 Uiso 1 1 calc R U . . .
C11 C 0.5607(2) 0.6551(2) 0.4963(3) 0.1161(17) Uani 1 1 d . . . . .
H11A H 0.568350 0.623428 0.468422 0.139 Uiso 1 1 calc R U . . .
C12 C 0.60796(19) 0.69248(18) 0.5147(3) 0.1052(15) Uani 1 1 d . . . . .
H12A H 0.647610 0.685254 0.500141 0.126 Uiso 1 1 calc R U . . .
C13 C 0.59753(14) 0.74094(14) 0.55478(17) 0.0735(8) Uani 1 1 d . . . . .
C14 C 0.53782(13) 0.74925(12) 0.57747(15) 0.0638(7) Uani 1 1 d . . . . .
H14A H 0.530054 0.781352 0.604800 0.077 Uiso 1 1 calc R U . . .
C15 C 0.64545(13) 0.78700(14) 0.56893(17) 0.0736(8) Uani 1 1 d . . . . .
C16 C 0.70258(17) 0.77195(19) 0.5933(3) 0.1071(15) Uani 1 1 d . . . . .
H16A H 0.711890 0.731124 0.602505 0.129 Uiso 1 1 calc R U . . .
C17 C 0.74523(18) 0.8171(2) 0.6038(3) 0.1188(18) Uani 1 1 d . . . . .
H17A H 0.783303 0.806606 0.620494 0.143 Uiso 1 1 calc R U . . .
C18 C 0.73292(16) 0.87805(19) 0.5902(2) 0.0966(13) Uani 1 1 d . . . . .
H18A H 0.762235 0.908314 0.598134 0.116 Uiso 1 1 calc R U . . .
C19 C 0.67587(13) 0.89391(14) 0.56441(16) 0.0666(7) Uani 1 1 d . . . . .
C20 C 0.63305(12) 0.84833(13) 0.55543(15) 0.0650(7) Uani 1 1 d . . . . .
H20A H 0.594514 0.858798 0.539827 0.078 Uiso 1 1 calc R U . . .
C21 C 0.66467(12) 0.95724(13) 0.54261(13) 0.0590(6) Uani 1 1 d . . . . .
C22 C 0.69904(13) 1.01013(14) 0.54748(14) 0.0659(7) Uani 1 1 d . . . . .
H22A H 0.735722 1.015322 0.569057 0.079 Uiso 1 1 calc R U . . .
C23 C 0.66783(12) 1.05388(13) 0.51371(12) 0.0578(6) Uani 1 1 d . . . . .
C24 C 0.68050(14) 1.11792(14) 0.49716(14) 0.0651(7) Uani 1 1 d . . . . .
C25 C 0.7286(2) 1.15128(18) 0.52116(19) 0.0908(11) Uani 1 1 d . . . . .
H25A H 0.755910 1.133685 0.549103 0.109 Uiso 1 1 calc R U . . .
C26 C 0.7351(2) 1.2118(2) 0.5025(2) 0.1096(15) Uani 1 1 d . . . . .
H26A H 0.766913 1.235761 0.518362 0.131 Uiso 1 1 calc R U . . .
C27 C 0.6952(2) 1.23635(19) 0.4612(2) 0.1084(15) Uani 1 1 d . . . . .
H27A H 0.699078 1.277156 0.448610 0.130 Uiso 1 1 calc R U . . .
C28 C 0.64878(19) 1.19981(15) 0.43817(18) 0.0833(9) Uani 1 1 d . . . . .
H28A H 0.621649 1.216675 0.409580 0.100 Uiso 1 1 calc R U . . .
Fe3 Fe 0.43679(2) 0.93679(2) 0.56321(2) 0.05435(16) Uani 1 3 d S T P . .
O1 O 0.46993(8) 0.88469(8) 0.63178(8) 0.0525(4) Uani 1 1 d . . . . .
O2 O 0.49989(9) 0.99578(8) 0.59399(8) 0.0548(4) Uani 1 1 d . . . . .
O3 O 0.62142(17) 0.89644(15) 0.78489(19) 0.1359(16) Uani 1 1 d . . . . .
O4 O 0.64713(17) 1.01199(16) 0.7490(2) 0.1516(19) Uani 1 1 d . . . . .
C29 C 0.51516(11) 0.91063(11) 0.66154(12) 0.0534(5) Uani 1 1 d . . . . .
C30 C 0.53097(12) 0.97468(11) 0.64061(12) 0.0547(5) Uani 1 1 d . . . . .
C31 C 0.57453(15) 1.00817(14) 0.67035(17) 0.0745(8) Uani 1 1 d . . . . .
H31A H 0.582379 1.048329 0.657558 0.089 Uiso 1 1 calc R U . . .
C32 C 0.60820(16) 0.98368(16) 0.7201(2) 0.0901(12) Uani 1 1 d . . . . .
C33 C 0.59278(16) 0.91690(17) 0.7415(2) 0.0855(10) Uani 1 1 d . . . . .
C34 C 0.54617(13) 0.88427(13) 0.70849(15) 0.0668(7) Uani 1 1 d . . . . .
H34A H 0.536988 0.843895 0.719620 0.080 Uiso 1 1 calc R U . . .
B1 B 0.1408(12) 0.6463(11) 0.8581(9) 0.090(3) Uani 0.3333 1 d D U P A -1
F1 F 0.0860(12) 0.6196(15) 0.8442(11) 0.160(10) Uani 0.3333 1 d D U P A -1
F2 F 0.1562(8) 0.6812(16) 0.8101(13) 0.192(11) Uani 0.3333 1 d D U P A -1
F3 F 0.1355(12) 0.6793(16) 0.9105(12) 0.113(7) Uani 0.3333 1 d D U P A -1
F4 F 0.1876(14) 0.6053(12) 0.8599(18) 0.152(13) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.963(2) . ?
Fe1 N2 1.963(2) 8_656 ?
Fe1 N2 1.963(2) 11_466 ?
Fe1 N1 2.004(2) . ?
Fe1 N1 2.004(2) 8_656 ?
Fe1 N1 2.004(2) 11_466 ?
Fe2 N5 1.990(2) 11_466 ?
Fe2 N5 1.990(2) 8_656 ?
Fe2 N5 1.990(2) . ?
Fe2 N6 2.035(2) 11_466 ?
Fe2 N6 2.035(2) 8_656 ?
Fe2 N6 2.035(2) . ?
N1 C1 1.332(4) . ?
N1 C5 1.354(4) . ?
N2 C6 1.329(3) . ?
N2 N3 1.347(3) . ?
N3 C8 1.360(3) . ?
N3 H3 0.90(2) . ?
N4 N5 1.348(3) . ?
N4 C21 1.355(4) . ?
N4 H4 0.86(2) . ?
N5 C23 1.335(3) . ?
N6 C24 1.344(4) . ?
N6 C28 1.347(4) . ?
C1 C2 1.383(4) . ?
C1 H1A 0.9300 . ?
C2 C3 1.367(5) . ?
C2 H2A 0.9300 . ?
C3 C4 1.372(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.387(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.455(4) . ?
C6 C7 1.382(4) . ?
C7 C8 1.372(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.466(4) . ?
C9 C14 1.372(4) . ?
C9 C10 1.387(4) . ?
C10 C11 1.382(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.382(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.397(4) . ?
C13 C15 1.474(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(5) . ?
C15 C20 1.389(4) . ?
C16 C17 1.367(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.380(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.401(4) . ?
C18 H18A 0.9300 . ?
C19 C20 1.371(4) . ?
C19 C21 1.473(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.372(4) . ?
C22 C23 1.377(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.461(4) . ?
C24 C25 1.372(4) . ?
C25 C26 1.381(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.356(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.375(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9895(17) . ?
Fe3 O2 1.9895(17) 11_466 ?
Fe3 O2 1.9895(17) 8_656 ?
Fe3 O1 2.0015(17) . ?
Fe3 O1 2.0016(17) 11_466 ?
Fe3 O1 2.0016(17) 8_656 ?
O1 C29 1.302(3) . ?
O2 C30 1.299(3) . ?
O3 C33 1.212(4) . ?
O4 C32 1.217(4) . ?
C29 C34 1.348(4) . ?
C29 C30 1.501(4) . ?
C30 C31 1.355(4) . ?
C31 C32 1.408(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.557(5) . ?
C33 C34 1.427(4) . ?
C34 H34A 0.9300 . ?
B1 F2 1.331(13) . ?
B1 F3 1.347(15) . ?
B1 F4 1.351(16) . ?
B1 F1 1.356(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.49(8) . 8_656 ?
N2 Fe1 N2 96.49(8) . 11_466 ?
N2 Fe1 N2 96.49(8) 8_656 11_466 ?
N2 Fe1 N1 80.18(8) . . ?
N2 Fe1 N1 172.50(9) 8_656 . ?
N2 Fe1 N1 90.58(9) 11_466 . ?
N2 Fe1 N1 90.58(8) . 8_656 ?
N2 Fe1 N1 80.17(8) 8_656 8_656 ?
N2 Fe1 N1 172.50(9) 11_466 8_656 ?
N1 Fe1 N1 93.09(9) . 8_656 ?
N2 Fe1 N1 172.50(9) . 11_466 ?
N2 Fe1 N1 90.58(8) 8_656 11_466 ?
N2 Fe1 N1 80.17(8) 11_466 11_466 ?
N1 Fe1 N1 93.08(9) . 11_466 ?
N1 Fe1 N1 93.09(9) 8_656 11_466 ?
N5 Fe2 N5 97.23(8) 11_466 8_656 ?
N5 Fe2 N5 97.23(8) 11_466 . ?
N5 Fe2 N5 97.23(8) 8_656 . ?
N5 Fe2 N6 78.84(9) 11_466 11_466 ?
N5 Fe2 N6 170.71(9) 8_656 11_466 ?
N5 Fe2 N6 91.64(9) . 11_466 ?
N5 Fe2 N6 91.65(9) 11_466 8_656 ?
N5 Fe2 N6 78.84(9) 8_656 8_656 ?
N5 Fe2 N6 170.71(9) . 8_656 ?
N6 Fe2 N6 92.78(10) 11_466 8_656 ?
N5 Fe2 N6 170.71(9) 11_466 . ?
N5 Fe2 N6 91.64(9) 8_656 . ?
N5 Fe2 N6 78.84(9) . . ?
N6 Fe2 N6 92.78(10) 11_466 . ?
N6 Fe2 N6 92.78(10) 8_656 . ?
C1 N1 C5 117.8(2) . . ?
C1 N1 Fe1 127.4(2) . . ?
C5 N1 Fe1 114.77(17) . . ?
C6 N2 N3 106.1(2) . . ?
C6 N2 Fe1 116.18(17) . . ?
N3 N2 Fe1 136.29(17) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 114(2) . . ?
C8 N3 H3 135(2) . . ?
N5 N4 C21 111.0(2) . . ?
N5 N4 H4 121(3) . . ?
C21 N4 H4 127(3) . . ?
C23 N5 N4 105.4(2) . . ?
C23 N5 Fe2 115.85(19) . . ?
N4 N5 Fe2 135.37(18) . . ?
C24 N6 C28 117.1(3) . . ?
C24 N6 Fe2 115.33(19) . . ?
C28 N6 Fe2 127.5(2) . . ?
N1 C1 C2 122.6(3) . . ?
N1 C1 H1A 118.7 . . ?
C2 C1 H1A 118.7 . . ?
C3 C2 C1 119.1(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
N1 C5 C4 122.4(3) . . ?
N1 C5 C6 113.5(2) . . ?
C4 C5 C6 124.1(3) . . ?
N2 C6 C7 110.9(2) . . ?
N2 C6 C5 114.8(2) . . ?
C7 C6 C5 134.2(3) . . ?
C8 C7 C6 105.6(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.9(2) . . ?
N3 C8 C9 123.1(2) . . ?
C7 C8 C9 130.0(3) . . ?
C14 C9 C10 119.3(3) . . ?
C14 C9 C8 121.6(3) . . ?
C10 C9 C8 119.1(3) . . ?
C11 C10 C9 119.6(4) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.6(4) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C14 118.1(3) . . ?
C12 C13 C15 122.1(3) . . ?
C14 C13 C15 119.5(3) . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.6(3) . . ?
C16 C15 C13 123.4(3) . . ?
C20 C15 C13 118.0(3) . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.3(3) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C17 C18 C19 119.4(4) . . ?
C17 C18 H18A 120.3 . . ?
C19 C18 H18A 120.3 . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 C21 121.0(3) . . ?
C18 C19 C21 120.2(3) . . ?
C19 C20 C15 122.0(3) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 106.9(2) . . ?
N4 C21 C19 121.2(3) . . ?
C22 C21 C19 131.7(3) . . ?
C21 C22 C23 105.5(2) . . ?
C21 C22 H22A 127.2 . . ?
C23 C22 H22A 127.2 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 114.9(3) . . ?
C22 C23 C24 133.9(3) . . ?
N6 C24 C25 123.3(3) . . ?
N6 C24 C23 113.3(2) . . ?
C25 C24 C23 123.5(3) . . ?
C24 C25 C26 117.9(4) . . ?
C24 C25 H25A 121.0 . . ?
C26 C25 H25A 121.0 . . ?
C27 C26 C25 120.1(4) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 118.8(4) . . ?
C26 C27 H27A 120.6 . . ?
C28 C27 H27A 120.6 . . ?
N6 C28 C27 122.8(4) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 90.24(8) . 11_466 ?
O2 Fe3 O2 90.24(8) . 8_656 ?
O2 Fe3 O2 90.24(8) 11_466 8_656 ?
O2 Fe3 O1 82.34(6) . . ?
O2 Fe3 O1 95.21(7) 11_466 . ?
O2 Fe3 O1 170.79(7) 8_656 . ?
O2 Fe3 O1 170.79(7) . 11_466 ?
O2 Fe3 O1 82.33(6) 11_466 11_466 ?
O2 Fe3 O1 95.21(7) 8_656 11_466 ?
O1 Fe3 O1 92.88(7) . 11_466 ?
O2 Fe3 O1 95.21(7) . 8_656 ?
O2 Fe3 O1 170.79(7) 11_466 8_656 ?
O2 Fe3 O1 82.33(6) 8_656 8_656 ?
O1 Fe3 O1 92.88(7) . 8_656 ?
O1 Fe3 O1 92.88(7) 11_466 8_656 ?
C29 O1 Fe3 113.28(15) . . ?
C30 O2 Fe3 113.06(15) . . ?
O1 C29 C34 124.6(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.5(2) . . ?
O2 C30 C31 122.9(2) . . ?
O2 C30 C29 116.3(2) . . ?
C31 C30 C29 120.8(2) . . ?
C30 C31 C32 121.6(3) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O4 C32 C31 124.3(3) . . ?
O4 C32 C33 117.7(3) . . ?
C31 C32 C33 117.9(3) . . ?
O3 C33 C34 124.8(3) . . ?
O3 C33 C32 117.5(3) . . ?
C34 C33 C32 117.6(3) . . ?
C29 C34 C33 121.5(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F2 B1 F3 112(2) . . ?
F2 B1 F4 102(2) . . ?
F3 B1 F4 113(2) . . ?
F2 B1 F1 106.8(18) . . ?
F3 B1 F1 110(2) . . ?
F4 B1 F1 113(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(2) 2.03(3) 2.885(3) 158(3) . yes
N4 H4 O2 0.86(2) 2.11(2) 2.955(3) 168(3) 11_466 yes

_refine_diff_density_max         0.472
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.074

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-370K
_database_code_depnum_ccdc_archive 'CCDC 2261758'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.7604(5)
_cell_length_b                   21.7604(5)
_cell_length_c                   21.7604(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10303.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    370(2)
_cell_measurement_reflns_used    9934
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      24.79

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.521
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.666
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      370(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            129519
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0442
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.146
_diffrn_reflns_theta_max         24.792
_diffrn_reflns_theta_full        24.760
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             5490
_reflns_number_gt                5179
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.838
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1859 cubic angstrom  with only 52 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of the BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.170  0.093  0.579      1859        52 ' '
   2  0.106  0.894  0.394        10         0 ' '
   3  0.394  0.106  0.894        10         0 ' '
   4  0.606  0.606  0.606        10         0 ' '
   5  0.894  0.394  0.106        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-370K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1859 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1859 cubic angstrom  with only 52 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.170  0.093  0.579      1859        52 ' '
   2  0.106  0.894  0.394        10         0 ' '
   3  0.394  0.106  0.894        10         0 ' '
   4  0.606  0.606  0.606        10         0 ' '
   5  0.894  0.394  0.106        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0581P)²+0.5992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5490
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0856
_refine_ls_wR_factor_gt          0.0839
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.067
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54865(2) 0.45135(2) 0.95135(2) 0.0635(2) Uani 1 3 d S T P . .
Fe2 Fe 0.82916(2) 0.17084(2) 0.67084(2) 0.0655(2) Uani 1 3 d S T P . .
N1 N 0.58327(13) 0.51859(14) 1.00747(12) 0.0767(7) Uani 1 1 d . . . . .
N2 N 0.61176(12) 0.48912(12) 0.89642(12) 0.0692(6) Uani 1 1 d . . . . .
N3 N 0.62749(13) 0.48468(12) 0.83644(13) 0.0719(6) Uani 1 1 d . . . . .
H3 H 0.615(2) 0.449(2) 0.814(2) 0.108 Uiso 1 1 d . U . . .
N4 N 0.74016(15) 0.27922(12) 0.63292(12) 0.0740(7) Uani 1 1 d D . . . .
H4 H 0.748(2) 0.3009(19) 0.6661(15) 0.111 Uiso 1 1 d D U . . .
N5 N 0.75833(13) 0.22012(12) 0.63154(12) 0.0721(6) Uani 1 1 d . . . . .
N6 N 0.79377(15) 0.10950(14) 0.60462(15) 0.0860(8) Uani 1 1 d . . . . .
C1 C 0.56718(19) 0.5305(2) 1.06521(17) 0.0930(11) Uani 1 1 d . . . . .
H1A H 0.538330 0.505102 1.083949 0.112 Uiso 1 1 calc R U . . .
C2 C 0.5911(2) 0.5784(3) 1.0984(2) 0.1196(17) Uani 1 1 d . . . . .
H2A H 0.578084 0.585731 1.138411 0.144 Uiso 1 1 calc R U . . .
C3 C 0.6341(3) 0.6147(3) 1.0720(2) 0.1270(18) Uani 1 1 d . . . . .
H3A H 0.650882 0.647347 1.093830 0.152 Uiso 1 1 calc R U . . .
C4 C 0.6529(2) 0.6031(2) 1.0125(2) 0.1069(13) Uani 1 1 d . . . . .
H4A H 0.683106 0.626945 0.993996 0.128 Uiso 1 1 calc R U . . .
C5 C 0.62550(16) 0.55506(18) 0.98115(17) 0.0796(9) Uani 1 1 d . . . . .
C6 C 0.63904(15) 0.53958(15) 0.91713(16) 0.0753(8) Uani 1 1 d . . . . .
C7 C 0.67274(18) 0.56734(16) 0.87158(18) 0.0835(9) Uani 1 1 d . . . . .
H7A H 0.695888 0.603115 0.874826 0.100 Uiso 1 1 calc R U . . .
C8 C 0.66522(17) 0.53126(14) 0.82001(16) 0.0774(8) Uani 1 1 d . . . . .
C9 C 0.69013(18) 0.53844(15) 0.75774(17) 0.0835(9) Uani 1 1 d . . . . .
C10 C 0.7321(3) 0.5850(2) 0.7467(2) 0.1239(18) Uani 1 1 d . . . . .
H10A H 0.745329 0.610259 0.778518 0.149 Uiso 1 1 calc R U . . .
C11 C 0.7539(4) 0.5934(3) 0.6877(3) 0.162(3) Uani 1 1 d . . . . .
H11A H 0.781950 0.624654 0.679864 0.194 Uiso 1 1 calc R U . . .
C12 C 0.7352(4) 0.5566(2) 0.6412(3) 0.147(2) Uani 1 1 d . . . . .
H12A H 0.749394 0.564084 0.601607 0.177 Uiso 1 1 calc R U . . .
C13 C 0.6954(2) 0.50847(18) 0.65127(18) 0.1010(13) Uani 1 1 d . . . . .
C14 C 0.67278(19) 0.50040(16) 0.71054(16) 0.0848(10) Uani 1 1 d . . . . .
H14A H 0.645346 0.468567 0.718322 0.102 Uiso 1 1 calc R U . . .
C15 C 0.6801(2) 0.46292(18) 0.60343(17) 0.0980(12) Uani 1 1 d . . . . .
C16 C 0.6556(3) 0.4783(3) 0.5471(2) 0.142(2) Uani 1 1 d . . . . .
H16A H 0.646678 0.519084 0.537996 0.170 Uiso 1 1 calc R U . . .
C17 C 0.6443(4) 0.4328(3) 0.5043(2) 0.154(3) Uani 1 1 d . . . . .
H17A H 0.626452 0.443312 0.466949 0.185 Uiso 1 1 calc R U . . .
C18 C 0.6588(3) 0.3727(2) 0.5155(2) 0.1281(18) Uani 1 1 d . . . . .
H18A H 0.651576 0.342788 0.485831 0.154 Uiso 1 1 calc R U . . .
C19 C 0.6846(2) 0.35673(18) 0.57219(16) 0.0875(10) Uani 1 1 d . . . . .
C20 C 0.6937(2) 0.40165(17) 0.61457(16) 0.0864(10) Uani 1 1 d . . . . .
H20A H 0.709830 0.390879 0.652666 0.104 Uiso 1 1 calc R U . . .
C21 C 0.70649(17) 0.29380(17) 0.58277(15) 0.0771(9) Uani 1 1 d . . . . .
C22 C 0.70383(18) 0.24162(19) 0.54752(17) 0.0879(10) Uani 1 1 d . . . . .
H22A H 0.684181 0.237007 0.509854 0.105 Uiso 1 1 calc R U . . .
C23 C 0.73636(16) 0.19722(17) 0.57943(16) 0.0766(8) Uani 1 1 d . . . . .
C24 C 0.75293(18) 0.13391(18) 0.56537(18) 0.0868(10) Uani 1 1 d . . . . .
C25 C 0.7300(3) 0.1018(2) 0.5166(3) 0.1239(17) Uani 1 1 d . . . . .
H25A H 0.702878 0.120177 0.489121 0.149 Uiso 1 1 calc R U . . .
C26 C 0.7477(3) 0.0421(3) 0.5091(3) 0.151(2) Uani 1 1 d . . . . .
H26A H 0.731682 0.019168 0.476772 0.182 Uiso 1 1 calc R U . . .
C27 C 0.7884(3) 0.0161(3) 0.5484(3) 0.151(2) Uani 1 1 d . . . . .
H27A H 0.801091 -0.024359 0.543100 0.181 Uiso 1 1 calc R U . . .
C28 C 0.8104(2) 0.0506(2) 0.5959(3) 0.1149(15) Uani 1 1 d . . . . .
H28A H 0.837865 0.032686 0.623328 0.138 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68722(2) 0.31278(2) 0.81278(2) 0.0687(2) Uani 1 3 d S T P . .
O1 O 0.61862(10) 0.36410(9) 0.77973(10) 0.0680(5) Uani 1 1 d . . . . .
O2 O 0.65654(10) 0.25313(9) 0.75066(10) 0.0708(5) Uani 1 1 d . . . . .
O3 O 0.4685(2) 0.3523(2) 0.6270(2) 0.176(2) Uani 1 1 d . . . . .
O4 O 0.5047(3) 0.2366(2) 0.6017(2) 0.192(3) Uani 1 1 d . . . . .
C29 C 0.58951(15) 0.33815(14) 0.73436(14) 0.0692(7) Uani 1 1 d . . . . .
C30 C 0.61039(15) 0.27389(14) 0.71893(14) 0.0706(7) Uani 1 1 d . . . . .
C31 C 0.5820(2) 0.24115(18) 0.67534(18) 0.0940(11) Uani 1 1 d . . . . .
H31A H 0.595109 0.201252 0.667456 0.113 Uiso 1 1 calc R U . . .
C32 C 0.5327(3) 0.2654(2) 0.6411(2) 0.1165(16) Uani 1 1 d . . . . .
C33 C 0.5115(2) 0.3317(2) 0.6559(2) 0.1090(14) Uani 1 1 d . . . . .
C34 C 0.54305(19) 0.36409(17) 0.70294(17) 0.0869(10) Uani 1 1 d . . . . .
H34A H 0.531315 0.404120 0.712255 0.104 Uiso 1 1 calc R U . . .
B1 B 0.6072(13) 0.1090(12) 0.3920(10) 0.132(3) Uani 0.3333 1 d D U P A -1
F1 F 0.6518(16) 0.0669(14) 0.3819(16) 0.181(9) Uani 0.3333 1 d D U P A -1
F2 F 0.5743(17) 0.0968(10) 0.4429(10) 0.210(7) Uani 0.3333 1 d D U P A -1
F3 F 0.6338(12) 0.1650(10) 0.4015(9) 0.186(7) Uani 0.3333 1 d D U P A -1
F4 F 0.5690(13) 0.1106(16) 0.3427(15) 0.175(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.997(3) . ?
Fe1 N2 1.997(3) 10_646 ?
Fe1 N2 1.997(3) 7_665 ?
Fe1 N1 2.049(3) . ?
Fe1 N1 2.049(3) 10_646 ?
Fe1 N1 2.049(3) 7_665 ?
Fe2 N5 2.063(3) . ?
Fe2 N5 2.063(3) 10_646 ?
Fe2 N5 2.063(3) 7_665 ?
Fe2 N6 2.110(3) . ?
Fe2 N6 2.110(3) 10_646 ?
Fe2 N6 2.110(3) 7_665 ?
N1 C1 1.330(5) . ?
N1 C5 1.343(5) . ?
N2 C6 1.327(4) . ?
N2 N3 1.353(4) . ?
N3 C8 1.353(4) . ?
N3 H3 0.96(5) . ?
N4 N5 1.346(4) . ?
N4 C21 1.352(5) . ?
N4 H4 0.88(3) . ?
N5 C23 1.328(4) . ?
N6 C24 1.342(5) . ?
N6 C28 1.346(5) . ?
C1 C2 1.371(6) . ?
C1 H1A 0.9300 . ?
C2 C3 1.352(7) . ?
C2 H2A 0.9300 . ?
C3 C4 1.381(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.382(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.463(5) . ?
C6 C7 1.373(5) . ?
C7 C8 1.379(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.468(5) . ?
C9 C14 1.372(5) . ?
C9 C10 1.385(6) . ?
C10 C11 1.381(7) . ?
C10 H10A 0.9300 . ?
C11 C12 1.353(8) . ?
C11 H11A 0.9300 . ?
C12 C13 1.376(7) . ?
C12 H12A 0.9300 . ?
C13 C14 1.392(5) . ?
C13 C15 1.476(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.377(6) . ?
C15 C20 1.387(5) . ?
C16 C17 1.382(8) . ?
C16 H16A 0.9300 . ?
C17 C18 1.367(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.399(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.358(5) . ?
C19 C21 1.468(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.371(5) . ?
C22 C23 1.384(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.457(5) . ?
C24 C25 1.366(6) . ?
C25 C26 1.364(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.357(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.364(7) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.989(2) . ?
Fe3 O2 1.989(2) 7_665 ?
Fe3 O2 1.989(2) 10_646 ?
Fe3 O1 1.998(2) 7_665 ?
Fe3 O1 1.998(2) 10_646 ?
Fe3 O1 1.998(2) . ?
O1 C29 1.302(4) . ?
O2 C30 1.300(4) . ?
O3 C33 1.213(5) . ?
O4 C32 1.224(5) . ?
C29 C34 1.345(5) . ?
C29 C30 1.508(4) . ?
C30 C31 1.338(5) . ?
C31 C32 1.408(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.550(6) . ?
C33 C34 1.420(6) . ?
C34 H34A 0.9300 . ?
B1 F2 1.345(14) . ?
B1 F1 1.353(15) . ?
B1 F4 1.357(15) . ?
B1 F3 1.366(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.76(10) . 10_646 ?
N2 Fe1 N2 96.76(10) . 7_665 ?
N2 Fe1 N2 96.76(10) 10_646 7_665 ?
N2 Fe1 N1 79.05(11) . . ?
N2 Fe1 N1 171.17(11) 10_646 . ?
N2 Fe1 N1 91.47(11) 7_665 . ?
N2 Fe1 N1 91.47(11) . 10_646 ?
N2 Fe1 N1 79.05(11) 10_646 10_646 ?
N2 Fe1 N1 171.17(11) 7_665 10_646 ?
N1 Fe1 N1 93.21(11) . 10_646 ?
N2 Fe1 N1 171.17(11) . 7_665 ?
N2 Fe1 N1 91.47(11) 10_646 7_665 ?
N2 Fe1 N1 79.05(11) 7_665 7_665 ?
N1 Fe1 N1 93.21(11) . 7_665 ?
N1 Fe1 N1 93.21(11) 10_646 7_665 ?
N5 Fe2 N5 97.87(10) . 10_646 ?
N5 Fe2 N5 97.87(10) . 7_665 ?
N5 Fe2 N5 97.87(10) 10_646 7_665 ?
N5 Fe2 N6 76.88(11) . . ?
N5 Fe2 N6 93.34(12) 10_646 . ?
N5 Fe2 N6 168.21(12) 7_665 . ?
N5 Fe2 N6 168.21(12) . 10_646 ?
N5 Fe2 N6 76.88(11) 10_646 10_646 ?
N5 Fe2 N6 93.34(12) 7_665 10_646 ?
N6 Fe2 N6 92.75(12) . 10_646 ?
N5 Fe2 N6 93.34(12) . 7_665 ?
N5 Fe2 N6 168.21(12) 10_646 7_665 ?
N5 Fe2 N6 76.88(11) 7_665 7_665 ?
N6 Fe2 N6 92.75(12) . 7_665 ?
N6 Fe2 N6 92.75(12) 10_646 7_665 ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Fe1 127.2(3) . . ?
C5 N1 Fe1 114.8(2) . . ?
C6 N2 N3 105.9(3) . . ?
C6 N2 Fe1 116.4(2) . . ?
N3 N2 Fe1 136.2(2) . . ?
C8 N3 N2 110.8(3) . . ?
C8 N3 H3 131(3) . . ?
N2 N3 H3 118(3) . . ?
N5 N4 C21 111.4(3) . . ?
N5 N4 H4 119(3) . . ?
C21 N4 H4 130(3) . . ?
C23 N5 N4 105.8(3) . . ?
C23 N5 Fe2 115.3(2) . . ?
N4 N5 Fe2 135.0(2) . . ?
C24 N6 C28 117.7(3) . . ?
C24 N6 Fe2 115.2(2) . . ?
C28 N6 Fe2 126.9(3) . . ?
N1 C1 C2 123.0(4) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 118.9(4) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.7(4) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C3 C4 C5 118.2(4) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.1(4) . . ?
N1 C5 C6 114.1(3) . . ?
C4 C5 C6 123.8(4) . . ?
N2 C6 C7 111.0(3) . . ?
N2 C6 C5 115.1(3) . . ?
C7 C6 C5 133.9(3) . . ?
C6 C7 C8 105.9(3) . . ?
C6 C7 H7A 127.1 . . ?
C8 C7 H7A 127.1 . . ?
N3 C8 C7 106.5(3) . . ?
N3 C8 C9 123.2(3) . . ?
C7 C8 C9 130.3(3) . . ?
C14 C9 C10 119.5(4) . . ?
C14 C9 C8 121.7(3) . . ?
C10 C9 C8 118.8(4) . . ?
C11 C10 C9 119.0(5) . . ?
C11 C10 H10A 120.5 . . ?
C9 C10 H10A 120.5 . . ?
C12 C11 C10 120.9(5) . . ?
C12 C11 H11A 119.5 . . ?
C10 C11 H11A 119.5 . . ?
C11 C12 C13 121.4(5) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 117.8(4) . . ?
C12 C13 C15 122.8(4) . . ?
C14 C13 C15 119.3(4) . . ?
C9 C14 C13 121.3(4) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.2(4) . . ?
C16 C15 C13 123.5(4) . . ?
C20 C15 C13 118.3(3) . . ?
C15 C16 C17 119.6(4) . . ?
C15 C16 H16A 120.2 . . ?
C17 C16 H16A 120.2 . . ?
C18 C17 C16 121.6(4) . . ?
C18 C17 H17A 119.2 . . ?
C16 C17 H17A 119.2 . . ?
C17 C18 C19 119.1(5) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 118.6(4) . . ?
C20 C19 C21 121.2(3) . . ?
C18 C19 C21 120.0(4) . . ?
C19 C20 C15 122.8(3) . . ?
C19 C20 H20A 118.6 . . ?
C15 C20 H20A 118.6 . . ?
N4 C21 C22 106.3(3) . . ?
N4 C21 C19 121.4(3) . . ?
C22 C21 C19 132.1(3) . . ?
C21 C22 C23 106.0(3) . . ?
C21 C22 H22A 127.0 . . ?
C23 C22 H22A 127.0 . . ?
N5 C23 C22 110.5(3) . . ?
N5 C23 C24 116.4(3) . . ?
C22 C23 C24 132.9(3) . . ?
N6 C24 C25 122.3(4) . . ?
N6 C24 C23 113.9(3) . . ?
C25 C24 C23 123.8(4) . . ?
C26 C25 C24 118.5(5) . . ?
C26 C25 H25A 120.8 . . ?
C24 C25 H25A 120.8 . . ?
C27 C26 C25 120.4(5) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C26 C27 C28 118.5(5) . . ?
C26 C27 H27A 120.7 . . ?
C28 C27 H27A 120.7 . . ?
N6 C28 C27 122.5(5) . . ?
N6 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
O2 Fe3 O2 90.21(9) . 7_665 ?
O2 Fe3 O2 90.21(9) . 10_646 ?
O2 Fe3 O2 90.21(9) 7_665 10_646 ?
O2 Fe3 O1 171.10(9) . 7_665 ?
O2 Fe3 O1 82.50(8) 7_665 7_665 ?
O2 Fe3 O1 94.89(9) 10_646 7_665 ?
O2 Fe3 O1 94.89(9) . 10_646 ?
O2 Fe3 O1 171.10(9) 7_665 10_646 ?
O2 Fe3 O1 82.50(8) 10_646 10_646 ?
O1 Fe3 O1 93.00(9) 7_665 10_646 ?
O2 Fe3 O1 82.50(8) . . ?
O2 Fe3 O1 94.89(9) 7_665 . ?
O2 Fe3 O1 171.10(9) 10_646 . ?
O1 Fe3 O1 93.00(9) 7_665 . ?
O1 Fe3 O1 93.01(9) 10_646 . ?
C29 O1 Fe3 113.21(19) . . ?
C30 O2 Fe3 113.18(19) . . ?
O1 C29 C34 124.7(3) . . ?
O1 C29 C30 115.1(3) . . ?
C34 C29 C30 120.2(3) . . ?
O2 C30 C31 123.3(3) . . ?
O2 C30 C29 115.9(3) . . ?
C31 C30 C29 120.8(3) . . ?
C30 C31 C32 121.9(3) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O4 C32 C31 124.0(4) . . ?
O4 C32 C33 118.2(4) . . ?
C31 C32 C33 117.7(3) . . ?
O3 C33 C34 124.3(4) . . ?
O3 C33 C32 117.8(4) . . ?
C34 C33 C32 117.9(4) . . ?
C29 C34 C33 121.5(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F2 B1 F1 113(2) . . ?
F2 B1 F4 109(2) . . ?
F1 B1 F4 109(2) . . ?
F2 B1 F3 106.1(16) . . ?
F1 B1 F3 109(2) . . ?
F4 B1 F3 111(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.96(5) 1.99(5) 2.906(3) 158(4) . yes
N4 H4 O2 0.88(3) 2.11(3) 2.973(3) 168(4) 7_665 yes

_refine_diff_density_max         0.206
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.046

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-400K
_database_code_depnum_ccdc_archive 'CCDC 2261759'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.7661(4)
_cell_length_b                   21.7661(4)
_cell_length_c                   21.7661(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10312.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    400(2)
_cell_measurement_reflns_used    9406
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      24.21

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.521
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      400(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83710
_diffrn_reflns_av_unetI/netI     0.0238
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.919
_diffrn_reflns_theta_max         24.509
_diffrn_reflns_theta_full        24.460
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             5322
_reflns_number_gt                4962
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.835
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1843 cubic angstrom  with only 50 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results before refinement of the BF4 disorder:
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.149 -0.088 -0.079      1843        50 ' '
   2  0.110  0.110  0.110        11         0 ' '
   3  0.390  0.890  0.610        11         0 ' '
   4  0.610  0.390  0.890        11         0 ' '
   5  0.890  0.610  0.390        11         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-400K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1843 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1843 cubic angstrom  with only 50 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.149 -0.088 -0.079      1843        50 ' '
   2  0.110  0.110  0.110        11         0 ' '
   3  0.390  0.890  0.610        11         0 ' '
   4  0.610  0.390  0.890        11         0 ' '
   5  0.890  0.610  0.390        11         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0673P)²+0.2394P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2167 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.022(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5322
_refine_ls_number_parameters     457
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0337
_refine_ls_R_factor_gt           0.0314
_refine_ls_wR_factor_ref         0.0920
_refine_ls_wR_factor_gt          0.0901
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.95095(2) 0.45095(2) 0.04905(2) 0.0721(2) Uani 1 3 d S T P . .
Fe2 Fe 0.67053(2) 0.17053(2) 0.32947(2) 0.0737(2) Uani 1 3 d S T P . .
N1 N 0.91612(14) 0.52020(15) -0.00663(13) 0.0881(8) Uani 1 1 d . . . . .
N2 N 0.88753(13) 0.48922(12) 0.10470(13) 0.0777(6) Uani 1 1 d . . . . .
N3 N 0.87128(14) 0.48461(13) 0.16417(13) 0.0812(7) Uani 1 1 d D . . . .
H3 H 0.886(2) 0.4519(16) 0.184(2) 0.122 Uiso 1 1 d D U . . .
N4 N 0.76035(15) 0.27900(13) 0.36800(13) 0.0820(7) Uani 1 1 d D . . . .
H4 H 0.749(2) 0.300(2) 0.3346(16) 0.123 Uiso 1 1 d D U . . .
N5 N 0.74191(14) 0.22006(13) 0.36925(13) 0.0801(7) Uani 1 1 d . . . . .
N6 N 0.70617(16) 0.10929(15) 0.39749(16) 0.0949(8) Uani 1 1 d . . . . .
C1 C 0.9321(2) 0.5326(2) -0.06429(18) 0.1059(12) Uani 1 1 d . . . . .
H1A H 0.960435 0.507081 -0.083565 0.127 Uiso 1 1 calc R U . . .
C2 C 0.9088(3) 0.5811(3) -0.0964(2) 0.137(2) Uani 1 1 d . . . . .
H2A H 0.921834 0.588823 -0.136379 0.164 Uiso 1 1 calc R U . . .
C3 C 0.8669(3) 0.6175(3) -0.0699(3) 0.146(2) Uani 1 1 d . . . . .
H3A H 0.850500 0.650571 -0.091420 0.175 Uiso 1 1 calc R U . . .
C4 C 0.8478(2) 0.6055(3) -0.0096(2) 0.1236(16) Uani 1 1 d . . . . .
H4A H 0.818234 0.629756 0.009496 0.148 Uiso 1 1 calc R U . . .
C5 C 0.87462(17) 0.55630(19) 0.02049(18) 0.0898(10) Uani 1 1 d . . . . .
C6 C 0.86098(16) 0.54026(17) 0.08400(18) 0.0849(9) Uani 1 1 d . . . . .
C7 C 0.82720(19) 0.56804(17) 0.12988(19) 0.0924(10) Uani 1 1 d . . . . .
H7A H 0.804572 0.604159 0.126919 0.111 Uiso 1 1 calc R U . . .
C8 C 0.83384(18) 0.53141(16) 0.18078(18) 0.0873(9) Uani 1 1 d . . . . .
C9 C 0.8093(2) 0.53833(16) 0.24325(19) 0.0946(10) Uani 1 1 d . . . . .
C10 C 0.7680(3) 0.5852(2) 0.2549(3) 0.140(2) Uani 1 1 d . . . . .
H10A H 0.755392 0.610995 0.223293 0.168 Uiso 1 1 calc R U . . .
C11 C 0.7457(4) 0.5933(3) 0.3128(3) 0.180(3) Uani 1 1 d . . . . .
H11A H 0.717300 0.624327 0.320311 0.216 Uiso 1 1 calc R U . . .
C12 C 0.7646(4) 0.5566(3) 0.3601(3) 0.168(3) Uani 1 1 d . . . . .
H12A H 0.750726 0.564370 0.399768 0.201 Uiso 1 1 calc R U . . .
C13 C 0.8040(3) 0.50828(19) 0.3498(2) 0.1126(14) Uani 1 1 d . . . . .
C14 C 0.8264(2) 0.50015(17) 0.29008(17) 0.0940(10) Uani 1 1 d . . . . .
H14A H 0.853566 0.468121 0.282106 0.113 Uiso 1 1 calc R U . . .
C15 C 0.8196(2) 0.46278(19) 0.39735(18) 0.1094(13) Uani 1 1 d . . . . .
C16 C 0.8445(4) 0.4785(3) 0.4532(2) 0.156(3) Uani 1 1 d . . . . .
H16A H 0.853774 0.519300 0.461898 0.188 Uiso 1 1 calc R U . . .
C17 C 0.8553(4) 0.4338(3) 0.4956(3) 0.167(3) Uani 1 1 d . . . . .
H17A H 0.872492 0.444879 0.533110 0.200 Uiso 1 1 calc R U . . .
C18 C 0.8418(3) 0.3724(3) 0.4850(2) 0.142(2) Uani 1 1 d . . . . .
H18A H 0.850014 0.342613 0.514485 0.171 Uiso 1 1 calc R U . . .
C19 C 0.8154(2) 0.35677(19) 0.42869(17) 0.0967(11) Uani 1 1 d . . . . .
C20 C 0.8059(2) 0.40173(18) 0.38631(17) 0.0967(11) Uani 1 1 d . . . . .
H20A H 0.789494 0.390957 0.348352 0.116 Uiso 1 1 calc R U . . .
C21 C 0.79352(18) 0.29381(18) 0.41839(16) 0.0859(9) Uani 1 1 d . . . . .
C22 C 0.79537(19) 0.2421(2) 0.45393(18) 0.0976(11) Uani 1 1 d . . . . .
H22A H 0.814472 0.237635 0.491885 0.117 Uiso 1 1 calc R U . . .
C23 C 0.76302(18) 0.19770(18) 0.42191(17) 0.0864(9) Uani 1 1 d . . . . .
C24 C 0.7462(2) 0.13440(19) 0.43646(19) 0.0974(11) Uani 1 1 d . . . . .
C25 C 0.7693(3) 0.1030(3) 0.4858(3) 0.138(2) Uani 1 1 d . . . . .
H25A H 0.796122 0.121814 0.513267 0.165 Uiso 1 1 calc R U . . .
C26 C 0.7515(3) 0.0426(3) 0.4936(4) 0.168(3) Uani 1 1 d . . . . .
H26A H 0.767011 0.019860 0.526250 0.202 Uiso 1 1 calc R U . . .
C27 C 0.7114(3) 0.0162(3) 0.4538(4) 0.167(3) Uani 1 1 d . . . . .
H27A H 0.699143 -0.024505 0.458409 0.200 Uiso 1 1 calc R U . . .
C28 C 0.6899(3) 0.0511(2) 0.4071(3) 0.1268(16) Uani 1 1 d . . . . .
H28A H 0.662023 0.033362 0.380026 0.152 Uiso 1 1 calc R U . . .
Fe3 Fe 0.81225(2) 0.31225(2) 0.18775(2) 0.0761(2) Uani 1 3 d S T P . .
O1 O 0.77920(10) 0.38068(10) 0.13662(9) 0.0760(5) Uani 1 1 d . . . . .
O2 O 0.75032(11) 0.34290(10) 0.24752(9) 0.0782(6) Uani 1 1 d . . . . .
O3 O 0.6260(2) 0.5300(3) 0.1485(2) 0.196(3) Uani 1 1 d . . . . .
O4 O 0.6008(2) 0.4937(3) 0.2639(2) 0.206(3) Uani 1 1 d . . . . .
C29 C 0.73401(15) 0.40980(16) 0.16263(15) 0.0770(8) Uani 1 1 d . . . . .
C30 C 0.71867(15) 0.38902(16) 0.22665(15) 0.0783(8) Uani 1 1 d . . . . .
C31 C 0.67511(19) 0.4174(2) 0.25957(19) 0.1041(13) Uani 1 1 d . . . . .
H31A H 0.667426 0.404500 0.299558 0.125 Uiso 1 1 calc R U . . .
C32 C 0.6407(2) 0.4664(3) 0.2351(2) 0.1261(17) Uani 1 1 d . . . . .
C33 C 0.6554(2) 0.4871(3) 0.1690(2) 0.1190(15) Uani 1 1 d . . . . .
C34 C 0.70228(18) 0.4561(2) 0.13691(19) 0.0968(11) Uani 1 1 d . . . . .
H34A H 0.711503 0.468049 0.096926 0.116 Uiso 1 1 calc R U . . .
B1 B 0.8898(12) 0.1078(9) 0.6101(13) 0.158(4) Uani 0.3333 1 d D U P A -1
F1 F 0.8329(11) 0.1009(11) 0.6380(13) 0.223(9) Uani 0.3333 1 d D U P A -1
F2 F 0.9024(12) 0.0559(9) 0.5778(16) 0.238(8) Uani 0.3333 1 d D U P A -1
F3 F 0.8899(15) 0.1559(13) 0.5696(13) 0.199(9) Uani 0.3333 1 d D U P A -1
F4 F 0.9302(13) 0.1214(15) 0.6566(15) 0.199(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.017(3) . ?
Fe1 N2 2.017(3) 8_645 ?
Fe1 N2 2.017(3) 11_556 ?
Fe1 N1 2.077(3) . ?
Fe1 N1 2.078(3) 11_556 ?
Fe1 N1 2.078(3) 8_645 ?
Fe2 N5 2.080(3) . ?
Fe2 N5 2.080(3) 11_556 ?
Fe2 N5 2.080(3) 8_645 ?
Fe2 N6 2.138(3) 11_556 ?
Fe2 N6 2.138(3) . ?
Fe2 N6 2.138(3) 8_645 ?
N1 C1 1.330(5) . ?
N1 C5 1.335(5) . ?
N2 C6 1.331(4) . ?
N2 N3 1.346(4) . ?
N3 C8 1.354(5) . ?
N3 H3 0.89(3) . ?
N4 N5 1.345(4) . ?
N4 C21 1.352(5) . ?
N4 H4 0.89(3) . ?
N5 C23 1.327(5) . ?
N6 C28 1.332(6) . ?
N6 C24 1.334(5) . ?
C1 C2 1.365(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.338(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.401(8) . ?
C3 H3A 0.9300 . ?
C4 C5 1.385(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.456(5) . ?
C6 C7 1.380(6) . ?
C7 C8 1.373(6) . ?
C7 H7A 0.9300 . ?
C8 C9 1.468(5) . ?
C9 C14 1.367(6) . ?
C9 C10 1.383(7) . ?
C10 C11 1.362(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.367(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.375(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.400(6) . ?
C13 C15 1.472(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.373(7) . ?
C15 C20 1.383(6) . ?
C16 C17 1.362(9) . ?
C16 H16A 0.9300 . ?
C17 C18 1.388(8) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.361(6) . ?
C19 C21 1.468(6) . ?
C20 H20A 0.9300 . ?
C21 C22 1.366(6) . ?
C22 C23 1.384(6) . ?
C22 H22A 0.9300 . ?
C23 C24 1.460(6) . ?
C24 C25 1.368(6) . ?
C25 C26 1.383(9) . ?
C25 H25A 0.9300 . ?
C26 C27 1.357(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.352(8) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.989(2) . ?
Fe3 O2 1.989(2) 8_645 ?
Fe3 O2 1.989(2) 11_556 ?
Fe3 O1 1.994(2) 11_556 ?
Fe3 O1 1.994(2) . ?
Fe3 O1 1.994(2) 8_645 ?
O1 C29 1.300(4) . ?
O2 C30 1.299(4) . ?
O3 C33 1.218(6) . ?
O4 C32 1.226(6) . ?
C29 C34 1.345(5) . ?
C29 C30 1.503(5) . ?
C30 C31 1.340(5) . ?
C31 C32 1.407(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.540(7) . ?
C33 C34 1.408(6) . ?
C34 H34A 0.9300 . ?
B1 F2 1.358(14) . ?
B1 F3 1.370(15) . ?
B1 F4 1.372(16) . ?
B1 F1 1.386(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.88(11) . 8_645 ?
N2 Fe1 N2 96.88(11) . 11_556 ?
N2 Fe1 N2 96.88(11) 8_645 11_556 ?
N2 Fe1 N1 78.52(11) . . ?
N2 Fe1 N1 92.09(11) 8_645 . ?
N2 Fe1 N1 170.37(12) 11_556 . ?
N2 Fe1 N1 92.09(11) . 11_556 ?
N2 Fe1 N1 170.37(12) 8_645 11_556 ?
N2 Fe1 N1 78.52(11) 11_556 11_556 ?
N1 Fe1 N1 93.11(12) . 11_556 ?
N2 Fe1 N1 170.37(12) . 8_645 ?
N2 Fe1 N1 78.52(11) 8_645 8_645 ?
N2 Fe1 N1 92.09(11) 11_556 8_645 ?
N1 Fe1 N1 93.11(12) . 8_645 ?
N1 Fe1 N1 93.11(12) 11_556 8_645 ?
N5 Fe2 N5 98.03(10) . 11_556 ?
N5 Fe2 N5 98.03(10) . 8_645 ?
N5 Fe2 N5 98.02(10) 11_556 8_645 ?
N5 Fe2 N6 167.36(12) . 11_556 ?
N5 Fe2 N6 76.34(12) 11_556 11_556 ?
N5 Fe2 N6 94.00(12) 8_645 11_556 ?
N5 Fe2 N6 76.34(12) . . ?
N5 Fe2 N6 94.00(12) 11_556 . ?
N5 Fe2 N6 167.36(12) 8_645 . ?
N6 Fe2 N6 92.62(13) 11_556 . ?
N5 Fe2 N6 94.00(12) . 8_645 ?
N5 Fe2 N6 167.36(12) 11_556 8_645 ?
N5 Fe2 N6 76.34(12) 8_645 8_645 ?
N6 Fe2 N6 92.62(13) 11_556 8_645 ?
N6 Fe2 N6 92.62(13) . 8_645 ?
C1 N1 C5 118.3(4) . . ?
C1 N1 Fe1 127.0(3) . . ?
C5 N1 Fe1 114.6(2) . . ?
C6 N2 N3 105.9(3) . . ?
C6 N2 Fe1 116.0(2) . . ?
N3 N2 Fe1 136.6(2) . . ?
N2 N3 C8 111.0(3) . . ?
N2 N3 H3 116(3) . . ?
C8 N3 H3 133(3) . . ?
N5 N4 C21 111.7(3) . . ?
N5 N4 H4 115(3) . . ?
C21 N4 H4 133(3) . . ?
C23 N5 N4 105.3(3) . . ?
C23 N5 Fe2 115.3(3) . . ?
N4 N5 Fe2 135.2(2) . . ?
C28 N6 C24 117.6(4) . . ?
C28 N6 Fe2 127.3(3) . . ?
C24 N6 Fe2 115.0(3) . . ?
N1 C1 C2 122.9(5) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 119.3(5) . . ?
C3 C2 H2A 120.3 . . ?
C1 C2 H2A 120.3 . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C5 C4 C3 117.5(5) . . ?
C5 C4 H4A 121.2 . . ?
C3 C4 H4A 121.2 . . ?
N1 C5 C4 122.1(4) . . ?
N1 C5 C6 114.6(3) . . ?
C4 C5 C6 123.3(4) . . ?
N2 C6 C7 110.6(3) . . ?
N2 C6 C5 115.7(3) . . ?
C7 C6 C5 133.7(3) . . ?
C8 C7 C6 105.9(3) . . ?
C8 C7 H7A 127.1 . . ?
C6 C7 H7A 127.1 . . ?
N3 C8 C7 106.5(3) . . ?
N3 C8 C9 122.9(4) . . ?
C7 C8 C9 130.5(4) . . ?
C14 C9 C10 119.2(4) . . ?
C14 C9 C8 121.9(4) . . ?
C10 C9 C8 118.8(4) . . ?
C11 C10 C9 119.8(6) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C10 C11 C12 120.9(6) . . ?
C10 C11 H11A 119.5 . . ?
C12 C11 H11A 119.5 . . ?
C11 C12 C13 120.8(5) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C14 117.8(5) . . ?
C12 C13 C15 122.9(5) . . ?
C14 C13 C15 119.1(4) . . ?
C9 C14 C13 121.4(4) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.6(5) . . ?
C16 C15 C13 123.0(4) . . ?
C20 C15 C13 118.3(4) . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 H16A 120.3 . . ?
C15 C16 H16A 120.3 . . ?
C16 C17 C18 122.6(5) . . ?
C16 C17 H17A 118.7 . . ?
C18 C17 H17A 118.7 . . ?
C17 C18 C19 117.9(5) . . ?
C17 C18 H18A 121.0 . . ?
C19 C18 H18A 121.0 . . ?
C20 C19 C18 118.9(4) . . ?
C20 C19 C21 121.2(3) . . ?
C18 C19 C21 119.7(4) . . ?
C19 C20 C15 122.7(4) . . ?
C19 C20 H20A 118.6 . . ?
C15 C20 H20A 118.6 . . ?
N4 C21 C22 106.2(3) . . ?
N4 C21 C19 121.3(3) . . ?
C22 C21 C19 132.3(4) . . ?
C21 C22 C23 106.0(3) . . ?
C21 C22 H22A 127.0 . . ?
C23 C22 H22A 127.0 . . ?
N5 C23 C22 110.8(3) . . ?
N5 C23 C24 116.5(4) . . ?
C22 C23 C24 132.6(3) . . ?
N6 C24 C25 122.3(4) . . ?
N6 C24 C23 114.3(3) . . ?
C25 C24 C23 123.3(4) . . ?
C24 C25 C26 117.9(6) . . ?
C24 C25 H25A 121.1 . . ?
C26 C25 H25A 121.1 . . ?
C27 C26 C25 120.4(5) . . ?
C27 C26 H26A 119.8 . . ?
C25 C26 H26A 119.8 . . ?
C28 C27 C26 117.6(5) . . ?
C28 C27 H27A 121.2 . . ?
C26 C27 H27A 121.2 . . ?
N6 C28 C27 124.1(6) . . ?
N6 C28 H28A 117.9 . . ?
C27 C28 H28A 117.9 . . ?
O2 Fe3 O2 90.20(10) . 8_645 ?
O2 Fe3 O2 90.20(10) . 11_556 ?
O2 Fe3 O2 90.20(10) 8_645 11_556 ?
O2 Fe3 O1 94.76(9) . 11_556 ?
O2 Fe3 O1 171.20(9) 8_645 11_556 ?
O2 Fe3 O1 82.53(8) 11_556 11_556 ?
O2 Fe3 O1 82.53(8) . . ?
O2 Fe3 O1 94.76(9) 8_645 . ?
O2 Fe3 O1 171.20(9) 11_556 . ?
O1 Fe3 O1 93.10(9) 11_556 . ?
O2 Fe3 O1 171.20(9) . 8_645 ?
O2 Fe3 O1 82.53(8) 8_645 8_645 ?
O2 Fe3 O1 94.76(9) 11_556 8_645 ?
O1 Fe3 O1 93.10(9) 11_556 8_645 ?
O1 Fe3 O1 93.10(9) . 8_645 ?
C29 O1 Fe3 113.2(2) . . ?
C30 O2 Fe3 112.94(19) . . ?
O1 C29 C34 125.0(3) . . ?
O1 C29 C30 115.2(3) . . ?
C34 C29 C30 119.9(3) . . ?
O2 C30 C31 123.0(3) . . ?
O2 C30 C29 116.0(3) . . ?
C31 C30 C29 121.0(3) . . ?
C30 C31 C32 121.6(4) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O4 C32 C31 123.4(5) . . ?
O4 C32 C33 118.9(5) . . ?
C31 C32 C33 117.7(4) . . ?
O3 C33 C34 124.5(4) . . ?
O3 C33 C32 117.2(4) . . ?
C34 C33 C32 118.3(4) . . ?
C29 C34 C33 121.6(4) . . ?
C29 C34 H34A 119.2 . . ?
C33 C34 H34A 119.2 . . ?
F2 B1 F3 108(2) . . ?
F2 B1 F4 116(3) . . ?
F3 B1 F4 108(2) . . ?
F2 B1 F1 108.4(18) . . ?
F3 B1 F1 112(2) . . ?
F4 B1 F1 106(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(3) 2.09(3) 2.920(4) 155(4) 11_556 yes
N4 H4 O2 0.89(3) 2.11(3) 2.976(4) 162(4) . yes

_refine_diff_density_max         0.204
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.045

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-325K
_database_code_depnum_ccdc_archive 'CCDC 2261761'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.7017(3)
_cell_length_b                   21.7017(3)
_cell_length_c                   21.7017(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10220.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    325(2)
_cell_measurement_reflns_used    9328
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      25.91

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.293
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.526
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.658
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      325(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            140083
_diffrn_reflns_av_unetI/netI     0.0205
_diffrn_reflns_av_R_equivalents  0.0467
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.152
_diffrn_reflns_theta_max         26.091
_diffrn_reflns_theta_full        25.209
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6254
_reflns_number_gt                5904
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_max     0.990
_reflns_Friedel_fraction_full    0.994

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1856 cubic angstrom  with only 35 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results before refinement of the BF4 disorder:
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.174  0.093  0.576      1856        35 ' '
   2  0.106  0.893  0.394         9         1 ' '
   3  0.393  0.106  0.894         9         1 ' '
   4  0.606  0.606  0.606         9         1 ' '
   5  0.893  0.393  0.106         9         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-325K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1856 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1856 cubic angstrom  with only 35 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.174  0.093  0.576      1856        35 ' '
   2  0.106  0.893  0.394         9         1 ' '
   3  0.393  0.106  0.894         9         1 ' '
   4  0.606  0.606  0.606         9         1 ' '
   5  0.893  0.393  0.106         9         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0546P)²+0.6667P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2594 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6254
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_ref         0.0839
_refine_ls_wR_factor_gt          0.0823
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.060
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54806(2) 0.45194(2) 0.95194(2) 0.05483(17) Uani 1 3 d S T P . .
Fe2 Fe 0.82898(2) 0.17102(2) 0.67102(2) 0.05730(17) Uani 1 3 d S T P . .
N1 N 0.58218(11) 0.51691(12) 1.00854(10) 0.0638(5) Uani 1 1 d . . . . .
N2 N 0.61057(11) 0.48910(10) 0.89769(10) 0.0593(5) Uani 1 1 d . . . . .
N3 N 0.62615(11) 0.48483(11) 0.83779(11) 0.0607(5) Uani 1 1 d . . . . .
H3 H 0.6136(18) 0.4502(18) 0.8177(18) 0.091 Uiso 1 1 d . U . . .
N4 N 0.74218(13) 0.27935(11) 0.63412(11) 0.0644(6) Uani 1 1 d D . . . .
H4 H 0.7489(18) 0.3016(16) 0.6669(14) 0.097 Uiso 1 1 d D U . . .
N5 N 0.75984(12) 0.21977(11) 0.63298(11) 0.0637(6) Uani 1 1 d . . . . .
N6 N 0.79435(13) 0.10956(12) 0.60778(13) 0.0741(6) Uani 1 1 d . . . . .
C1 C 0.56609(16) 0.52786(17) 1.06682(14) 0.0776(8) Uani 1 1 d . . . . .
H1A H 0.537069 0.502281 1.085254 0.093 Uiso 1 1 calc R U . . .
C2 C 0.59063(19) 0.5754(2) 1.10086(17) 0.0978(12) Uani 1 1 d . . . . .
H2A H 0.577511 0.582422 1.141052 0.117 Uiso 1 1 calc R U . . .
C3 C 0.6346(2) 0.6123(2) 1.07471(19) 0.1039(13) Uani 1 1 d . . . . .
H3A H 0.652125 0.644273 1.097179 0.125 Uiso 1 1 calc R U . . .
C4 C 0.65267(18) 0.60160(19) 1.01515(18) 0.0904(10) Uani 1 1 d . . . . .
H4A H 0.682638 0.626018 0.996656 0.108 Uiso 1 1 calc R U . . .
C5 C 0.62532(14) 0.55371(15) 0.98311(14) 0.0677(7) Uani 1 1 d . . . . .
C6 C 0.63868(13) 0.53912(13) 0.91907(14) 0.0650(7) Uani 1 1 d . . . . .
C7 C 0.67282(15) 0.56707(14) 0.87333(15) 0.0729(8) Uani 1 1 d . . . . .
H7A H 0.696431 0.602670 0.876751 0.087 Uiso 1 1 calc R U . . .
C8 C 0.66470(14) 0.53142(12) 0.82167(14) 0.0666(7) Uani 1 1 d . . . . .
C9 C 0.68978(15) 0.53887(13) 0.75935(14) 0.0716(8) Uani 1 1 d . . . . .
C10 C 0.7313(2) 0.58590(18) 0.7481(2) 0.1038(13) Uani 1 1 d . . . . .
H10A H 0.743890 0.611636 0.779926 0.125 Uiso 1 1 calc R U . . .
C11 C 0.7538(3) 0.5944(2) 0.6892(2) 0.135(2) Uani 1 1 d . . . . .
H11A H 0.781990 0.625780 0.681531 0.162 Uiso 1 1 calc R U . . .
C12 C 0.7352(3) 0.5572(2) 0.6425(2) 0.1229(18) Uani 1 1 d . . . . .
H12A H 0.749795 0.564400 0.602844 0.147 Uiso 1 1 calc R U . . .
C13 C 0.6951(2) 0.50904(15) 0.65249(15) 0.0864(10) Uani 1 1 d . . . . .
C14 C 0.67278(16) 0.50080(14) 0.71191(14) 0.0736(8) Uani 1 1 d . . . . .
H14A H 0.645586 0.468609 0.719715 0.088 Uiso 1 1 calc R U . . .
C15 C 0.68079(19) 0.46312(15) 0.60452(14) 0.0848(10) Uani 1 1 d . . . . .
C16 C 0.6561(3) 0.4782(2) 0.54754(19) 0.1225(18) Uani 1 1 d . . . . .
H16A H 0.646813 0.518979 0.538365 0.147 Uiso 1 1 calc R U . . .
C17 C 0.6456(3) 0.4333(2) 0.5050(2) 0.135(2) Uani 1 1 d . . . . .
H17A H 0.628828 0.444014 0.467039 0.162 Uiso 1 1 calc R U . . .
C18 C 0.6591(3) 0.3724(2) 0.51671(18) 0.1117(15) Uani 1 1 d . . . . .
H18A H 0.651113 0.342238 0.487312 0.134 Uiso 1 1 calc R U . . .
C19 C 0.68513(17) 0.35656(15) 0.57368(14) 0.0763(8) Uani 1 1 d . . . . .
C20 C 0.69432(16) 0.40178(15) 0.61640(14) 0.0751(8) Uani 1 1 d . . . . .
H20A H 0.710173 0.391121 0.654758 0.090 Uiso 1 1 calc R U . . .
C21 C 0.70700(15) 0.29337(15) 0.58462(13) 0.0686(7) Uani 1 1 d . . . . .
C22 C 0.70281(15) 0.24058(16) 0.54996(15) 0.0759(8) Uani 1 1 d . . . . .
H22A H 0.681834 0.235514 0.512941 0.091 Uiso 1 1 calc R U . . .
C23 C 0.73615(14) 0.19671(15) 0.58147(14) 0.0669(7) Uani 1 1 d . . . . .
C24 C 0.75281(16) 0.13282(15) 0.56832(15) 0.0762(8) Uani 1 1 d . . . . .
C25 C 0.7290(2) 0.0998(2) 0.5200(2) 0.1064(13) Uani 1 1 d . . . . .
H25A H 0.701181 0.117523 0.492706 0.128 Uiso 1 1 calc R U . . .
C26 C 0.7475(3) 0.0397(2) 0.5132(3) 0.1292(18) Uani 1 1 d . . . . .
H26A H 0.731773 0.015984 0.481124 0.155 Uiso 1 1 calc R U . . .
C27 C 0.7887(3) 0.0147(2) 0.5530(3) 0.1275(18) Uani 1 1 d . . . . .
H27A H 0.801311 -0.026054 0.548709 0.153 Uiso 1 1 calc R U . . .
C28 C 0.8112(2) 0.05054(17) 0.5996(2) 0.0969(11) Uani 1 1 d . . . . .
H28A H 0.839445 0.033337 0.626836 0.116 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68672(2) 0.31328(2) 0.81328(2) 0.06165(18) Uani 1 3 d S T P . .
O1 O 0.61822(9) 0.36515(8) 0.78012(9) 0.0597(4) Uani 1 1 d . . . . .
O2 O 0.65604(9) 0.25401(8) 0.75052(9) 0.0626(4) Uani 1 1 d . . . . .
O3 O 0.4664(2) 0.35361(16) 0.62771(18) 0.1553(18) Uani 1 1 d . . . . .
O4 O 0.5028(2) 0.23799(17) 0.60213(19) 0.174(2) Uani 1 1 d . . . . .
C29 C 0.58873(14) 0.33924(13) 0.73488(13) 0.0612(6) Uani 1 1 d . . . . .
C30 C 0.60970(13) 0.27517(13) 0.71917(13) 0.0626(6) Uani 1 1 d . . . . .
C31 C 0.58044(18) 0.24200(16) 0.67536(16) 0.0848(10) Uani 1 1 d . . . . .
H31A H 0.593361 0.201900 0.667502 0.102 Uiso 1 1 calc R U . . .
C32 C 0.5311(2) 0.26633(18) 0.64139(18) 0.1036(14) Uani 1 1 d . . . . .
C33 C 0.5097(2) 0.33294(18) 0.65666(18) 0.0969(12) Uani 1 1 d . . . . .
C34 C 0.54210(17) 0.36560(15) 0.70352(15) 0.0765(8) Uani 1 1 d . . . . .
H34A H 0.530839 0.405933 0.712629 0.092 Uiso 1 1 calc R U . . .
B1 B 0.6073(10) 0.1075(9) 0.3940(12) 0.114(2) Uani 0.3333 1 d D U P A -1
F1 F 0.6635(9) 0.0961(8) 0.3691(11) 0.168(6) Uani 0.3333 1 d D U P A -1
F2 F 0.5952(9) 0.0575(9) 0.4282(15) 0.189(7) Uani 0.3333 1 d D U P A -1
F3 F 0.6099(16) 0.1580(14) 0.4309(14) 0.153(7) Uani 0.3333 1 d D U P A -1
F4 F 0.5634(14) 0.1159(16) 0.3506(14) 0.160(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.969(2) . ?
Fe1 N2 1.969(2) 10_646 ?
Fe1 N2 1.969(2) 7_665 ?
Fe1 N1 2.011(2) 10_646 ?
Fe1 N1 2.011(2) 7_665 ?
Fe1 N1 2.011(2) . ?
Fe2 N5 2.013(3) 7_665 ?
Fe2 N5 2.013(3) 10_646 ?
Fe2 N5 2.013(3) . ?
Fe2 N6 2.056(3) . ?
Fe2 N6 2.056(3) 10_646 ?
Fe2 N6 2.056(3) 7_665 ?
N1 C1 1.333(4) . ?
N1 C5 1.349(4) . ?
N2 C6 1.329(4) . ?
N2 N3 1.346(3) . ?
N3 C8 1.358(4) . ?
N3 H3 0.91(4) . ?
N4 N5 1.349(4) . ?
N4 C21 1.353(4) . ?
N4 H4 0.87(2) . ?
N5 C23 1.328(4) . ?
N6 C24 1.342(4) . ?
N6 C28 1.344(4) . ?
C1 C2 1.376(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.370(6) . ?
C3 H3A 0.9300 . ?
C4 C5 1.384(5) . ?
C4 H4A 0.9300 . ?
C5 C6 1.455(4) . ?
C6 C7 1.379(4) . ?
C7 C8 1.373(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.467(4) . ?
C9 C14 1.371(5) . ?
C9 C10 1.383(5) . ?
C10 C11 1.380(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(7) . ?
C11 H11A 0.9300 . ?
C12 C13 1.377(6) . ?
C12 H12A 0.9300 . ?
C13 C14 1.389(5) . ?
C13 C15 1.474(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.386(5) . ?
C15 C20 1.387(4) . ?
C16 C17 1.362(7) . ?
C16 H16A 0.9300 . ?
C17 C18 1.378(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.402(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.365(5) . ?
C19 C21 1.470(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.374(5) . ?
C22 C23 1.377(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.461(5) . ?
C24 C25 1.371(5) . ?
C25 C26 1.373(7) . ?
C25 H25A 0.9300 . ?
C26 C27 1.356(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.366(6) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9882(19) . ?
Fe3 O2 1.9882(19) 7_665 ?
Fe3 O2 1.9882(19) 10_646 ?
Fe3 O1 1.9986(18) . ?
Fe3 O1 1.9987(18) 7_665 ?
Fe3 O1 1.9987(18) 10_646 ?
O1 C29 1.300(3) . ?
O2 C30 1.298(3) . ?
O3 C33 1.215(5) . ?
O4 C32 1.217(5) . ?
C29 C34 1.347(4) . ?
C29 C30 1.502(4) . ?
C30 C31 1.351(4) . ?
C31 C32 1.402(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.555(5) . ?
C33 C34 1.426(5) . ?
C34 H34A 0.9300 . ?
B1 F2 1.341(13) . ?
B1 F4 1.351(15) . ?
B1 F1 1.357(14) . ?
B1 F3 1.358(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.62(9) . 10_646 ?
N2 Fe1 N2 96.62(9) . 7_665 ?
N2 Fe1 N2 96.62(9) 10_646 7_665 ?
N2 Fe1 N1 90.72(9) . 10_646 ?
N2 Fe1 N1 79.88(9) 10_646 10_646 ?
N2 Fe1 N1 172.21(10) 7_665 10_646 ?
N2 Fe1 N1 172.21(10) . 7_665 ?
N2 Fe1 N1 90.72(9) 10_646 7_665 ?
N2 Fe1 N1 79.88(9) 7_665 7_665 ?
N1 Fe1 N1 93.14(10) 10_646 7_665 ?
N2 Fe1 N1 79.89(9) . . ?
N2 Fe1 N1 172.20(9) 10_646 . ?
N2 Fe1 N1 90.73(9) 7_665 . ?
N1 Fe1 N1 93.14(9) 10_646 . ?
N1 Fe1 N1 93.14(9) 7_665 . ?
N5 Fe2 N5 97.44(9) 7_665 10_646 ?
N5 Fe2 N5 97.44(9) 7_665 . ?
N5 Fe2 N5 97.43(9) 10_646 . ?
N5 Fe2 N6 169.83(10) 7_665 . ?
N5 Fe2 N6 92.26(10) 10_646 . ?
N5 Fe2 N6 78.15(10) . . ?
N5 Fe2 N6 92.25(10) 7_665 10_646 ?
N5 Fe2 N6 78.16(10) 10_646 10_646 ?
N5 Fe2 N6 169.82(10) . 10_646 ?
N6 Fe2 N6 92.76(11) . 10_646 ?
N5 Fe2 N6 78.16(10) 7_665 7_665 ?
N5 Fe2 N6 169.83(10) 10_646 7_665 ?
N5 Fe2 N6 92.26(10) . 7_665 ?
N6 Fe2 N6 92.76(11) . 7_665 ?
N6 Fe2 N6 92.76(11) 10_646 7_665 ?
C1 N1 C5 117.7(3) . . ?
C1 N1 Fe1 127.4(2) . . ?
C5 N1 Fe1 114.87(19) . . ?
C6 N2 N3 106.2(2) . . ?
C6 N2 Fe1 116.24(19) . . ?
N3 N2 Fe1 136.22(19) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 116(3) . . ?
C8 N3 H3 133(3) . . ?
N5 N4 C21 111.2(2) . . ?
N5 N4 H4 120(3) . . ?
C21 N4 H4 128(3) . . ?
C23 N5 N4 105.5(2) . . ?
C23 N5 Fe2 115.8(2) . . ?
N4 N5 Fe2 135.08(19) . . ?
C24 N6 C28 117.2(3) . . ?
C24 N6 Fe2 115.3(2) . . ?
C28 N6 Fe2 127.4(3) . . ?
N1 C1 C2 122.8(3) . . ?
N1 C1 H1A 118.6 . . ?
C2 C1 H1A 118.6 . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C3 C4 C5 118.6(4) . . ?
C3 C4 H4A 120.7 . . ?
C5 C4 H4A 120.7 . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 113.6(3) . . ?
C4 C5 C6 123.9(3) . . ?
N2 C6 C7 110.8(3) . . ?
N2 C6 C5 114.8(3) . . ?
C7 C6 C5 134.4(3) . . ?
C8 C7 C6 105.7(3) . . ?
C8 C7 H7A 127.1 . . ?
C6 C7 H7A 127.1 . . ?
N3 C8 C7 106.7(3) . . ?
N3 C8 C9 123.2(3) . . ?
C7 C8 C9 130.0(3) . . ?
C14 C9 C10 119.2(3) . . ?
C14 C9 C8 121.7(3) . . ?
C10 C9 C8 119.1(3) . . ?
C11 C10 C9 119.6(4) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.4(4) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 117.7(4) . . ?
C12 C13 C15 122.3(3) . . ?
C14 C13 C15 119.7(3) . . ?
C9 C14 C13 121.7(3) . . ?
C9 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C16 C15 C20 118.3(4) . . ?
C16 C15 C13 123.5(3) . . ?
C20 C15 C13 118.2(3) . . ?
C17 C16 C15 120.1(4) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.7(4) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C19 118.9(4) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 120.9(3) . . ?
C18 C19 C21 120.0(3) . . ?
C19 C20 C15 122.2(3) . . ?
C19 C20 H20A 118.9 . . ?
C15 C20 H20A 118.9 . . ?
N4 C21 C22 106.5(3) . . ?
N4 C21 C19 121.4(3) . . ?
C22 C21 C19 131.9(3) . . ?
C21 C22 C23 105.7(3) . . ?
C21 C22 H22A 127.2 . . ?
C23 C22 H22A 127.2 . . ?
N5 C23 C22 111.1(3) . . ?
N5 C23 C24 115.2(3) . . ?
C22 C23 C24 133.6(3) . . ?
N6 C24 C25 123.0(3) . . ?
N6 C24 C23 113.5(3) . . ?
C25 C24 C23 123.6(3) . . ?
C24 C25 C26 118.0(4) . . ?
C24 C25 H25A 121.0 . . ?
C26 C25 H25A 121.0 . . ?
C27 C26 C25 120.3(4) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 118.6(4) . . ?
C26 C27 H27A 120.7 . . ?
C28 C27 H27A 120.7 . . ?
N6 C28 C27 122.9(4) . . ?
N6 C28 H28A 118.5 . . ?
C27 C28 H28A 118.5 . . ?
O2 Fe3 O2 90.16(8) . 7_665 ?
O2 Fe3 O2 90.16(8) . 10_646 ?
O2 Fe3 O2 90.16(8) 7_665 10_646 ?
O2 Fe3 O1 82.45(7) . . ?
O2 Fe3 O1 95.05(8) 7_665 . ?
O2 Fe3 O1 170.95(8) 10_646 . ?
O2 Fe3 O1 170.95(8) . 7_665 ?
O2 Fe3 O1 82.45(7) 7_665 7_665 ?
O2 Fe3 O1 95.05(8) 10_646 7_665 ?
O1 Fe3 O1 92.97(8) . 7_665 ?
O2 Fe3 O1 95.05(8) . 10_646 ?
O2 Fe3 O1 170.95(8) 7_665 10_646 ?
O2 Fe3 O1 82.45(7) 10_646 10_646 ?
O1 Fe3 O1 92.97(8) . 10_646 ?
O1 Fe3 O1 92.97(8) 7_665 10_646 ?
C29 O1 Fe3 113.24(17) . . ?
C30 O2 Fe3 112.93(17) . . ?
O1 C29 C34 124.6(3) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.4(3) . . ?
O2 C30 C31 123.0(3) . . ?
O2 C30 C29 116.3(2) . . ?
C31 C30 C29 120.7(3) . . ?
C30 C31 C32 121.9(3) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O4 C32 C31 124.3(4) . . ?
O4 C32 C33 117.9(4) . . ?
C31 C32 C33 117.8(3) . . ?
O3 C33 C34 124.5(4) . . ?
O3 C33 C32 117.7(3) . . ?
C34 C33 C32 117.8(3) . . ?
C29 C34 C33 121.4(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F2 B1 F4 111(2) . . ?
F2 B1 F1 104.4(14) . . ?
F4 B1 F1 112(2) . . ?
F2 B1 F3 109(2) . . ?
F4 B1 F3 109(2) . . ?
F1 B1 F3 110(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.91(4) 2.02(4) 2.888(3) 159(4) . yes
N4 H4 O2 0.87(2) 2.10(3) 2.960(3) 168(4) 7_665 yes

_refine_diff_density_max         0.283
_refine_diff_density_min         -0.235
_refine_diff_density_rms         0.027

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-270K
_database_code_depnum_ccdc_archive 'CCDC 2261763'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.6594(3)
_cell_length_b                   21.6594(3)
_cell_length_c                   21.6594(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10161.1(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    270(2)
_cell_measurement_reflns_used    9561
_cell_measurement_theta_min      2.73
_cell_measurement_theta_max      26.39

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.301
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.529
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.656
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      270(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            142572
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.156
_diffrn_reflns_theta_max         26.411
_diffrn_reflns_theta_full        26.040
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6479
_reflns_number_gt                6172
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.846
_reflns_Friedel_fraction_max     0.998
_reflns_Friedel_fraction_full    0.998

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1832 cubic angstrom  with only 60 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of the BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.161 -0.094 -0.088      1832        60 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-270K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1832 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1832 cubic angstrom  with only 60 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.161 -0.094 -0.088      1832        60 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0531P)²+1.1285P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2745 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6479
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0298
_refine_ls_wR_factor_ref         0.0834
_refine_ls_wR_factor_gt          0.0822
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54801(2) 0.54801(2) 0.54801(2) 0.04557(15) Uani 1 3 d S T P . .
Fe2 Fe 0.82928(2) 0.82928(2) 0.82928(2) 0.04747(16) Uani 1 3 d S T P . .
N1 N 0.49096(10) 0.58200(10) 0.48380(11) 0.0521(5) Uani 1 1 d . . . . .
N2 N 0.60198(10) 0.61057(10) 0.51115(10) 0.0491(5) Uani 1 1 d . . . . .
N3 N 0.66182(10) 0.62619(11) 0.51522(10) 0.0501(5) Uani 1 1 d . . . . .
H3 H 0.6798(17) 0.6134(17) 0.5496(18) 0.075 Uiso 1 1 d . U . . .
N4 N 0.86517(10) 0.74423(12) 0.72104(10) 0.0513(5) Uani 1 1 d D . . . .
H4 H 0.8323(13) 0.7507(16) 0.6996(15) 0.077 Uiso 1 1 d D U . . .
N5 N 0.86630(10) 0.76169(11) 0.78091(11) 0.0512(5) Uani 1 1 d . . . . .
N6 N 0.89003(12) 0.79524(12) 0.89097(11) 0.0593(6) Uani 1 1 d . . . . .
C1 C 0.43262(13) 0.56555(15) 0.47341(16) 0.0624(7) Uani 1 1 d . . . . .
H1A H 0.414420 0.536459 0.499219 0.075 Uiso 1 1 calc R U . . .
C2 C 0.39811(16) 0.59018(18) 0.42560(19) 0.0783(10) Uani 1 1 d . . . . .
H2A H 0.357887 0.576831 0.418727 0.094 Uiso 1 1 calc R U . . .
C3 C 0.42387(18) 0.63441(19) 0.3886(2) 0.0836(11) Uani 1 1 d . . . . .
H3A H 0.400971 0.651990 0.356791 0.100 Uiso 1 1 calc R U . . .
C4 C 0.48371(17) 0.65268(16) 0.39864(17) 0.0729(9) Uani 1 1 d . . . . .
H4A H 0.502077 0.682535 0.373838 0.088 Uiso 1 1 calc R U . . .
C5 C 0.51611(14) 0.62547(13) 0.44674(14) 0.0553(6) Uani 1 1 d . . . . .
C6 C 0.58029(14) 0.63885(13) 0.46120(13) 0.0544(6) Uani 1 1 d . . . . .
C7 C 0.62591(14) 0.67334(15) 0.43305(13) 0.0604(7) Uani 1 1 d . . . . .
H7A H 0.622241 0.697196 0.397541 0.072 Uiso 1 1 calc R U . . .
C8 C 0.67776(14) 0.66504(13) 0.46842(12) 0.0547(6) Uani 1 1 d . . . . .
C9 C 0.74011(14) 0.69015(14) 0.46085(13) 0.0588(7) Uani 1 1 d . . . . .
C10 C 0.75170(19) 0.7315(2) 0.41334(17) 0.0848(11) Uani 1 1 d . . . . .
H10A H 0.719867 0.743906 0.387320 0.102 Uiso 1 1 calc R U . . .
C11 C 0.8105(2) 0.7543(3) 0.4048(2) 0.1093(17) Uani 1 1 d . . . . .
H11A H 0.818052 0.782539 0.373381 0.131 Uiso 1 1 calc R U . . .
C12 C 0.85788(19) 0.7356(3) 0.44220(18) 0.1007(15) Uani 1 1 d . . . . .
H12A H 0.897627 0.750071 0.434790 0.121 Uiso 1 1 calc R U . . .
C13 C 0.84755(15) 0.69558(18) 0.49086(15) 0.0711(9) Uani 1 1 d . . . . .
C14 C 0.78782(14) 0.67297(15) 0.49925(13) 0.0607(7) Uani 1 1 d . . . . .
H14A H 0.780039 0.645702 0.531492 0.073 Uiso 1 1 calc R U . . .
C15 C 0.89545(14) 0.68145(18) 0.53703(15) 0.0701(8) Uani 1 1 d . . . . .
C16 C 0.95275(17) 0.6575(3) 0.52194(19) 0.1005(15) Uani 1 1 d . . . . .
H16A H 0.962215 0.648468 0.481035 0.121 Uiso 1 1 calc R U . . .
C17 C 0.99520(19) 0.6471(3) 0.5671(2) 0.1121(17) Uani 1 1 d . . . . .
H17A H 1.033506 0.630895 0.556469 0.134 Uiso 1 1 calc R U . . .
C18 C 0.98287(17) 0.6600(2) 0.6284(2) 0.0925(13) Uani 1 1 d . . . . .
H18A H 1.012085 0.651667 0.658785 0.111 Uiso 1 1 calc R U . . .
C19 C 0.92547(13) 0.68596(16) 0.64416(15) 0.0632(7) Uani 1 1 d . . . . .
C20 C 0.88284(13) 0.69479(15) 0.59860(14) 0.0619(7) Uani 1 1 d . . . . .
H20A H 0.844151 0.710203 0.609029 0.074 Uiso 1 1 calc R U . . .
C21 C 0.91421(13) 0.70772(14) 0.70748(14) 0.0565(7) Uani 1 1 d . . . . .
C22 C 0.94849(14) 0.70246(14) 0.76075(15) 0.0619(7) Uani 1 1 d . . . . .
H22A H 0.984966 0.680462 0.766145 0.074 Uiso 1 1 calc R U . . .
C23 C 0.91730(13) 0.73666(13) 0.80436(14) 0.0548(6) Uani 1 1 d . . . . .
C24 C 0.92979(14) 0.75300(15) 0.86846(14) 0.0614(7) Uani 1 1 d . . . . .
C25 C 0.97746(19) 0.72872(19) 0.90250(18) 0.0837(11) Uani 1 1 d . . . . .
H25A H 1.004673 0.700347 0.885228 0.100 Uiso 1 1 calc R U . . .
C26 C 0.9839(2) 0.7475(2) 0.9629(2) 0.1008(14) Uani 1 1 d . . . . .
H26A H 1.015611 0.731700 0.987076 0.121 Uiso 1 1 calc R U . . .
C27 C 0.9438(2) 0.7891(2) 0.98704(19) 0.0995(14) Uani 1 1 d . . . . .
H27A H 0.947592 0.801898 1.027868 0.119 Uiso 1 1 calc R U . . .
C28 C 0.89759(18) 0.81214(18) 0.95013(16) 0.0775(9) Uani 1 1 d . . . . .
H28A H 0.870287 0.840717 0.966917 0.093 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68703(2) 0.68703(2) 0.68703(2) 0.05347(17) Uani 1 3 d S T P . .
O1 O 0.72011(9) 0.61863(9) 0.63447(8) 0.0503(4) Uani 1 1 d . . . . .
O2 O 0.75052(9) 0.65629(9) 0.74578(8) 0.0530(4) Uani 1 1 d . . . . .
O3 O 0.87076(17) 0.46389(18) 0.64623(15) 0.1293(15) Uani 1 1 d . . . . .
O4 O 0.89640(17) 0.4996(2) 0.76231(16) 0.1425(18) Uani 1 1 d . . . . .
C29 C 0.76524(12) 0.58848(13) 0.66042(13) 0.0521(6) Uani 1 1 d . . . . .
C30 C 0.78125(13) 0.60930(13) 0.72459(13) 0.0539(6) Uani 1 1 d . . . . .
C31 C 0.82482(16) 0.57929(18) 0.75818(15) 0.0725(9) Uani 1 1 d . . . . .
H31A H 0.833081 0.592380 0.798226 0.087 Uiso 1 1 calc R U . . .
C32 C 0.85777(17) 0.5289(2) 0.73388(17) 0.0875(12) Uani 1 1 d . . . . .
C33 C 0.84235(17) 0.5079(2) 0.66678(17) 0.0812(10) Uani 1 1 d . . . . .
C34 C 0.79596(14) 0.54137(16) 0.63396(14) 0.0649(8) Uani 1 1 d . . . . .
H34A H 0.786805 0.530415 0.593464 0.078 Uiso 1 1 calc R U . . .
F1 F 0.3702(10) 0.3376(9) 0.4084(12) 0.144(7) Uani 0.3333 1 d D U P A -1
B1 B 0.3953(12) 0.3930(8) 0.3928(9) 0.091(2) Uani 0.3333 1 d D U P A -1
F2 F 0.4318(15) 0.4079(7) 0.4414(10) 0.164(7) Uani 0.3333 1 d D U P A -1
F3 F 0.4304(15) 0.3855(12) 0.3413(12) 0.120(6) Uani 0.3333 1 d D U P A -1
F4 F 0.3525(10) 0.4385(12) 0.3910(15) 0.144(8) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.960(2) . ?
Fe1 N2 1.960(2) 5 ?
Fe1 N2 1.960(2) 9 ?
Fe1 N1 2.001(2) 5 ?
Fe1 N1 2.001(2) 9 ?
Fe1 N1 2.001(2) . ?
Fe2 N5 1.971(2) . ?
Fe2 N5 1.971(2) 9 ?
Fe2 N5 1.971(2) 5 ?
Fe2 N6 2.015(2) 9 ?
Fe2 N6 2.015(2) 5 ?
Fe2 N6 2.015(2) . ?
N1 C1 1.332(4) . ?
N1 C5 1.352(4) . ?
N2 C6 1.329(3) . ?
N2 N3 1.342(3) . ?
N3 C8 1.362(4) . ?
N3 H3 0.88(4) . ?
N4 N5 1.351(3) . ?
N4 C21 1.356(4) . ?
N4 H4 0.86(2) . ?
N5 C23 1.331(4) . ?
N6 C28 1.343(4) . ?
N6 C24 1.348(4) . ?
C1 C2 1.384(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.373(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.454(4) . ?
C6 C7 1.381(4) . ?
C7 C8 1.371(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.465(4) . ?
C9 C14 1.378(4) . ?
C9 C10 1.388(5) . ?
C10 C11 1.378(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.368(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.383(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.395(4) . ?
C13 C15 1.473(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.384(5) . ?
C15 C20 1.392(4) . ?
C16 C17 1.361(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.383(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.406(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.365(4) . ?
C19 C21 1.471(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.377(4) . ?
C22 C23 1.377(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.458(4) . ?
C24 C25 1.373(5) . ?
C25 C26 1.377(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.355(6) . ?
C26 H26A 0.9300 . ?
C27 C28 1.375(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9884(19) 9 ?
Fe3 O2 1.9884(19) 5 ?
Fe3 O2 1.9884(19) . ?
Fe3 O1 2.0011(18) . ?
Fe3 O1 2.0011(18) 5 ?
Fe3 O1 2.0011(18) 9 ?
O1 C29 1.303(3) . ?
O2 C30 1.300(3) . ?
O3 C33 1.218(4) . ?
O4 C32 1.217(5) . ?
C29 C34 1.346(4) . ?
C29 C30 1.502(4) . ?
C30 C31 1.357(4) . ?
C31 C32 1.407(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.559(5) . ?
C33 C34 1.429(5) . ?
C34 H34A 0.9300 . ?
F1 B1 1.360(14) . ?
B1 F4 1.354(15) . ?
B1 F2 1.356(12) . ?
B1 F3 1.360(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.44(9) . 5 ?
N2 Fe1 N2 96.44(9) . 9 ?
N2 Fe1 N2 96.44(9) 5 9 ?
N2 Fe1 N1 172.59(9) . 5 ?
N2 Fe1 N1 80.26(9) 5 5 ?
N2 Fe1 N1 90.54(9) 9 5 ?
N2 Fe1 N1 90.54(9) . 9 ?
N2 Fe1 N1 172.59(9) 5 9 ?
N2 Fe1 N1 80.26(9) 9 9 ?
N1 Fe1 N1 93.09(9) 5 9 ?
N2 Fe1 N1 80.26(9) . . ?
N2 Fe1 N1 90.54(9) 5 . ?
N2 Fe1 N1 172.59(9) 9 . ?
N1 Fe1 N1 93.09(9) 5 . ?
N1 Fe1 N1 93.09(9) 9 . ?
N5 Fe2 N5 97.09(9) . 9 ?
N5 Fe2 N5 97.10(9) . 5 ?
N5 Fe2 N5 97.10(9) 9 5 ?
N5 Fe2 N6 171.35(10) . 9 ?
N5 Fe2 N6 79.34(10) 9 9 ?
N5 Fe2 N6 91.19(10) 5 9 ?
N5 Fe2 N6 91.19(10) . 5 ?
N5 Fe2 N6 171.35(10) 9 5 ?
N5 Fe2 N6 79.34(10) 5 5 ?
N6 Fe2 N6 92.79(10) 9 5 ?
N5 Fe2 N6 79.34(10) . . ?
N5 Fe2 N6 91.19(10) 9 . ?
N5 Fe2 N6 171.35(10) 5 . ?
N6 Fe2 N6 92.79(10) 9 . ?
N6 Fe2 N6 92.79(10) 5 . ?
C1 N1 C5 117.9(3) . . ?
C1 N1 Fe1 127.2(2) . . ?
C5 N1 Fe1 114.85(19) . . ?
C6 N2 N3 106.2(2) . . ?
C6 N2 Fe1 116.06(19) . . ?
N3 N2 Fe1 136.34(18) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 114(2) . . ?
C8 N3 H3 135(2) . . ?
N5 N4 C21 110.9(2) . . ?
N5 N4 H4 119(3) . . ?
C21 N4 H4 129(3) . . ?
C23 N5 N4 105.5(2) . . ?
C23 N5 Fe2 115.9(2) . . ?
N4 N5 Fe2 135.31(18) . . ?
C28 N6 C24 116.9(3) . . ?
C28 N6 Fe2 127.8(2) . . ?
C24 N6 Fe2 115.2(2) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
N1 C5 C4 122.5(3) . . ?
N1 C5 C6 113.3(2) . . ?
C4 C5 C6 124.1(3) . . ?
N2 C6 C7 110.8(3) . . ?
N2 C6 C5 114.9(3) . . ?
C7 C6 C5 134.2(3) . . ?
C8 C7 C6 105.6(3) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C9 123.1(3) . . ?
C7 C8 C9 130.1(3) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 C8 121.6(3) . . ?
C10 C9 C8 119.3(3) . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C12 C11 C10 120.5(4) . . ?
C12 C11 H11A 119.7 . . ?
C10 C11 H11A 119.7 . . ?
C11 C12 C13 121.0(3) . . ?
C11 C12 H12A 119.5 . . ?
C13 C12 H12A 119.5 . . ?
C12 C13 C14 118.0(3) . . ?
C12 C13 C15 122.2(3) . . ?
C14 C13 C15 119.4(3) . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.7(3) . . ?
C16 C15 C13 123.3(3) . . ?
C20 C15 C13 118.0(3) . . ?
C17 C16 C15 119.8(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 121.8(3) . . ?
C16 C17 H17A 119.1 . . ?
C18 C17 H17A 119.1 . . ?
C17 C18 C19 118.9(4) . . ?
C17 C18 H18A 120.5 . . ?
C19 C18 H18A 120.5 . . ?
C20 C19 C18 118.6(3) . . ?
C20 C19 C21 121.2(3) . . ?
C18 C19 C21 120.0(3) . . ?
C19 C20 C15 122.1(3) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 106.8(3) . . ?
N4 C21 C19 121.2(3) . . ?
C22 C21 C19 131.7(3) . . ?
C21 C22 C23 105.4(3) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 111.4(3) . . ?
N5 C23 C24 114.7(3) . . ?
C22 C23 C24 133.8(3) . . ?
N6 C24 C25 123.1(3) . . ?
N6 C24 C23 113.0(3) . . ?
C25 C24 C23 123.9(3) . . ?
C24 C25 C26 118.2(4) . . ?
C24 C25 H25A 120.9 . . ?
C26 C25 H25A 120.9 . . ?
C27 C26 C25 119.9(4) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 118.8(4) . . ?
C26 C27 H27A 120.6 . . ?
C28 C27 H27A 120.6 . . ?
N6 C28 C27 123.0(4) . . ?
N6 C28 H28A 118.5 . . ?
C27 C28 H28A 118.5 . . ?
O2 Fe3 O2 90.19(8) 9 5 ?
O2 Fe3 O2 90.19(8) 9 . ?
O2 Fe3 O2 90.19(8) 5 . ?
O2 Fe3 O1 170.81(7) 9 . ?
O2 Fe3 O1 95.30(8) 5 . ?
O2 Fe3 O1 82.45(7) . . ?
O2 Fe3 O1 95.30(8) 9 5 ?
O2 Fe3 O1 82.45(7) 5 5 ?
O2 Fe3 O1 170.81(8) . 5 ?
O1 Fe3 O1 92.73(8) . 5 ?
O2 Fe3 O1 82.45(7) 9 9 ?
O2 Fe3 O1 170.81(7) 5 9 ?
O2 Fe3 O1 95.30(8) . 9 ?
O1 Fe3 O1 92.73(8) . 9 ?
O1 Fe3 O1 92.73(8) 5 9 ?
C29 O1 Fe3 113.21(17) . . ?
C30 O2 Fe3 112.97(17) . . ?
O1 C29 C34 124.5(3) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.5(3) . . ?
O2 C30 C31 122.8(3) . . ?
O2 C30 C29 116.3(2) . . ?
C31 C30 C29 120.8(3) . . ?
C30 C31 C32 121.6(3) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O4 C32 C31 124.3(3) . . ?
O4 C32 C33 117.9(3) . . ?
C31 C32 C33 117.8(3) . . ?
O3 C33 C34 124.8(3) . . ?
O3 C33 C32 117.4(3) . . ?
C34 C33 C32 117.8(3) . . ?
C29 C34 C33 121.4(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F4 B1 F2 104.3(17) . . ?
F4 B1 F1 112(2) . . ?
F2 B1 F1 104.6(15) . . ?
F4 B1 F3 116(2) . . ?
F2 B1 F3 109.8(19) . . ?
F1 B1 F3 108.8(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.88(4) 2.04(4) 2.880(3) 159(3) . yes
N4 H4 O2 0.86(2) 2.10(2) 2.945(3) 169(3) 5 yes

_refine_diff_density_max         0.284
_refine_diff_density_min         -0.242
_refine_diff_density_rms         0.036

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-290K
_database_code_depnum_ccdc_archive 'CCDC 2261762'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.6790(3)
_cell_length_b                   21.6790(3)
_cell_length_c                   21.6790(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10188.7(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    290(2)
_cell_measurement_reflns_used    9706
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      25.71

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.527
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      290(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            143701
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_av_R_equivalents  0.0623
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.927
_diffrn_reflns_theta_max         26.426
_diffrn_reflns_theta_full        26.040
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             6488
_reflns_number_gt                6123
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.843
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1843 cubic angstrom  with only 22 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results before refinement of the BF4 disorder:
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.159  0.117  0.620      1843        22 ' '
   2  0.144  0.856  0.356        10         1 ' '
   3  0.356  0.144  0.856        10         1 ' '
   4  0.644  0.644  0.644        10         1 ' '
   5  0.856  0.356  0.144        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-290K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1843 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1843 cubic angstrom  with only 22 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.159  0.117  0.620      1843        22 ' '
   2  0.144  0.856  0.356        10         1 ' '
   3  0.356  0.144  0.856        10         1 ' '
   4  0.644  0.644  0.644        10         1 ' '
   5  0.856  0.356  0.144        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0559P)²+0.8204P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2712 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.021(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         6488
_refine_ls_number_parameters     457
_refine_ls_number_restraints     51
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0299
_refine_ls_wR_factor_ref         0.0841
_refine_ls_wR_factor_gt          0.0825
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_restrained_S_all      1.043
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.70202(2) 0.29798(2) 0.79798(2) 0.04804(16) Uani 1 3 d S T P . .
Fe2 Fe 0.42090(2) 0.57910(2) 1.07910(2) 0.05010(16) Uani 1 3 d S T P . .
N1 N 0.76630(11) 0.33199(10) 0.74108(10) 0.0552(5) Uani 1 1 d . . . . .
N2 N 0.73896(10) 0.36052(10) 0.85200(10) 0.0521(5) Uani 1 1 d . . . . .
N3 N 0.73488(10) 0.37608(11) 0.91188(10) 0.0528(5) Uani 1 1 d D . . . .
H3 H 0.7004(13) 0.3630(17) 0.9302(16) 0.079 Uiso 1 1 d D U . . .
N4 N 0.52912(10) 0.49362(12) 1.11525(10) 0.0553(5) Uani 1 1 d D . . . .
H4 H 0.5514(16) 0.4996(17) 1.0833(14) 0.083 Uiso 1 1 d D U . . .
N5 N 0.46939(10) 0.51109(11) 1.11644(10) 0.0544(5) Uani 1 1 d . . . . .
N6 N 0.35933(11) 0.54489(12) 1.14057(12) 0.0632(6) Uani 1 1 d . . . . .
C1 C 0.77683(16) 0.31564(15) 0.68273(13) 0.0664(7) Uani 1 1 d . . . . .
H1A H 0.751233 0.286443 0.664498 0.080 Uiso 1 1 calc R U . . .
C2 C 0.82439(19) 0.34052(18) 0.64838(16) 0.0838(10) Uani 1 1 d . . . . .
H2A H 0.831179 0.327430 0.608093 0.101 Uiso 1 1 calc R U . . .
C3 C 0.8614(2) 0.38462(19) 0.67426(18) 0.0888(11) Uani 1 1 d . . . . .
H3A H 0.893201 0.402192 0.651470 0.107 Uiso 1 1 calc R U . . .
C4 C 0.85130(18) 0.40271(17) 0.73393(17) 0.0777(9) Uani 1 1 d . . . . .
H4A H 0.875975 0.432597 0.752329 0.093 Uiso 1 1 calc R U . . .
C5 C 0.80330(14) 0.37530(13) 0.76625(13) 0.0586(6) Uani 1 1 d . . . . .
C6 C 0.78889(13) 0.38878(13) 0.83039(13) 0.0570(6) Uani 1 1 d . . . . .
C7 C 0.81696(13) 0.42313(15) 0.87605(15) 0.0641(7) Uani 1 1 d . . . . .
H7A H 0.852491 0.446899 0.872477 0.077 Uiso 1 1 calc R U . . .
C8 C 0.78152(12) 0.41488(13) 0.92782(13) 0.0578(6) Uani 1 1 d . . . . .
C9 C 0.78909(13) 0.44006(14) 0.99014(14) 0.0623(7) Uani 1 1 d . . . . .
C10 C 0.83641(17) 0.4813(2) 1.00165(19) 0.0904(11) Uani 1 1 d . . . . .
H10A H 0.862326 0.493737 0.969807 0.108 Uiso 1 1 calc R U . . .
C11 C 0.8450(2) 0.5040(3) 1.0605(2) 0.1177(18) Uani 1 1 d . . . . .
H11A H 0.876489 0.532156 1.068074 0.141 Uiso 1 1 calc R U . . .
C12 C 0.80774(19) 0.4853(3) 1.10765(19) 0.1068(16) Uani 1 1 d . . . . .
H12A H 0.815198 0.499648 1.147383 0.128 Uiso 1 1 calc R U . . .
C13 C 0.75914(15) 0.44545(18) 1.09739(14) 0.0751(9) Uani 1 1 d . . . . .
C14 C 0.75085(13) 0.42285(15) 1.03775(14) 0.0642(7) Uani 1 1 d . . . . .
H14A H 0.718719 0.395509 1.029982 0.077 Uiso 1 1 calc R U . . .
C15 C 0.71307(15) 0.43123(18) 1.14532(14) 0.0746(9) Uani 1 1 d . . . . .
C16 C 0.7282(2) 0.4070(3) 1.20250(18) 0.1075(16) Uani 1 1 d . . . . .
H16A H 0.769060 0.398077 1.211887 0.129 Uiso 1 1 calc R U . . .
C17 C 0.6832(2) 0.3964(3) 1.24491(19) 0.1192(18) Uani 1 1 d . . . . .
H17A H 0.693772 0.379749 1.282992 0.143 Uiso 1 1 calc R U . . .
C18 C 0.6220(2) 0.4098(2) 1.23272(17) 0.0978(13) Uani 1 1 d . . . . .
H18A H 0.591722 0.401620 1.262004 0.117 Uiso 1 1 calc R U . . .
C19 C 0.60615(15) 0.43579(16) 1.17558(13) 0.0667(8) Uani 1 1 d . . . . .
C20 C 0.65155(14) 0.44461(15) 1.13296(13) 0.0655(7) Uani 1 1 d . . . . .
H20A H 0.641036 0.460088 1.094354 0.079 Uiso 1 1 calc R U . . .
C21 C 0.54283(14) 0.45752(14) 1.16444(13) 0.0599(7) Uani 1 1 d . . . . .
C22 C 0.48980(15) 0.45254(15) 1.19876(14) 0.0664(7) Uani 1 1 d . . . . .
H22A H 0.484535 0.430841 1.235392 0.080 Uiso 1 1 calc R U . . .
C23 C 0.44607(14) 0.48643(13) 1.16755(13) 0.0584(6) Uani 1 1 d . . . . .
C24 C 0.38203(14) 0.50284(15) 1.18014(15) 0.0657(7) Uani 1 1 d . . . . .
C25 C 0.34825(19) 0.47870(19) 1.2279(2) 0.0910(11) Uani 1 1 d . . . . .
H25A H 0.365618 0.450443 1.255130 0.109 Uiso 1 1 calc R U . . .
C26 C 0.2879(2) 0.4975(2) 1.2345(2) 0.1091(15) Uani 1 1 d . . . . .
H26A H 0.263837 0.481748 1.266370 0.131 Uiso 1 1 calc R U . . .
C27 C 0.2635(2) 0.5389(2) 1.1946(2) 0.1081(15) Uani 1 1 d . . . . .
H27A H 0.222749 0.551633 1.198445 0.130 Uiso 1 1 calc R U . . .
C28 C 0.30017(16) 0.56179(19) 1.14822(19) 0.0833(10) Uani 1 1 d . . . . .
H28A H 0.283294 0.590244 1.120906 0.100 Uiso 1 1 calc R U . . .
Fe3 Fe 0.56317(2) 0.43683(2) 0.93683(2) 0.05545(17) Uani 1 3 d S T P . .
O1 O 0.61546(8) 0.36838(9) 0.97000(8) 0.0528(4) Uani 1 1 d . . . . .
O2 O 0.50424(8) 0.40614(9) 1.00009(9) 0.0553(4) Uani 1 1 d . . . . .
O3 O 0.60392(15) 0.21497(19) 1.12143(17) 0.1373(16) Uani 1 1 d . . . . .
O4 O 0.48824(16) 0.2509(2) 1.14720(18) 0.1534(19) Uani 1 1 d . . . . .
C29 C 0.58963(12) 0.33855(13) 1.01515(12) 0.0546(6) Uani 1 1 d . . . . .
C30 C 0.52552(12) 0.35942(13) 1.03109(13) 0.0559(6) Uani 1 1 d . . . . .
C31 C 0.49213(15) 0.32966(18) 1.07472(15) 0.0757(9) Uani 1 1 d . . . . .
H31A H 0.452001 0.342545 1.082695 0.091 Uiso 1 1 calc R U . . .
C32 C 0.51652(17) 0.2798(2) 1.10825(17) 0.0918(12) Uani 1 1 d . . . . .
C33 C 0.58333(17) 0.2585(2) 1.09270(17) 0.0856(11) Uani 1 1 d . . . . .
C34 C 0.61607(14) 0.29160(16) 1.04618(14) 0.0681(8) Uani 1 1 d . . . . .
H34A H 0.656519 0.280565 1.037082 0.082 Uiso 1 1 calc R U . . .
B1 B 0.8554(9) 0.1417(13) 0.6439(10) 0.093(3) Uani 0.3333 1 d D U P A -1
F1 F 0.9122(9) 0.1201(14) 0.6566(10) 0.159(9) Uani 0.3333 1 d D U P A -1
F2 F 0.8382(17) 0.1728(17) 0.6943(7) 0.202(13) Uani 0.3333 1 d D U P A -1
F3 F 0.8552(16) 0.1833(16) 0.5979(15) 0.151(15) Uani 0.3333 1 d D U P A -1
F4 F 0.8155(17) 0.0961(13) 0.631(2) 0.130(11) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.962(2) 10_646 ?
Fe1 N2 1.962(2) 7_665 ?
Fe1 N2 1.962(2) . ?
Fe1 N1 2.002(2) 10_646 ?
Fe1 N1 2.002(2) 7_665 ?
Fe1 N1 2.002(2) . ?
Fe2 N5 1.983(2) 7_665 ?
Fe2 N5 1.983(2) 10_646 ?
Fe2 N5 1.983(2) . ?
Fe2 N6 2.027(2) . ?
Fe2 N6 2.027(2) 10_646 ?
Fe2 N6 2.027(2) 7_665 ?
N1 C1 1.333(4) . ?
N1 C5 1.350(4) . ?
N2 C6 1.329(3) . ?
N2 N3 1.344(3) . ?
N3 C8 1.360(4) . ?
N3 H3 0.89(2) . ?
N4 N5 1.349(3) . ?
N4 C21 1.356(4) . ?
N4 H4 0.85(2) . ?
N5 C23 1.330(4) . ?
N6 C28 1.344(4) . ?
N6 C24 1.345(4) . ?
C1 C2 1.381(5) . ?
C1 H1A 0.9300 . ?
C2 C3 1.368(6) . ?
C2 H2A 0.9300 . ?
C3 C4 1.369(5) . ?
C3 H3A 0.9300 . ?
C4 C5 1.388(4) . ?
C4 H4A 0.9300 . ?
C5 C6 1.455(4) . ?
C6 C7 1.380(4) . ?
C7 C8 1.372(4) . ?
C7 H7A 0.9300 . ?
C8 C9 1.466(4) . ?
C9 C14 1.375(4) . ?
C9 C10 1.384(5) . ?
C10 C11 1.380(6) . ?
C10 H10A 0.9300 . ?
C11 C12 1.365(6) . ?
C11 H11A 0.9300 . ?
C12 C13 1.380(5) . ?
C12 H12A 0.9300 . ?
C13 C14 1.394(4) . ?
C13 C15 1.474(5) . ?
C14 H14A 0.9300 . ?
C15 C16 1.385(5) . ?
C15 C20 1.391(4) . ?
C16 C17 1.361(6) . ?
C16 H16A 0.9300 . ?
C17 C18 1.383(6) . ?
C17 H17A 0.9300 . ?
C18 C19 1.404(5) . ?
C18 H18A 0.9300 . ?
C19 C20 1.363(4) . ?
C19 C21 1.471(4) . ?
C20 H20A 0.9300 . ?
C21 C22 1.374(4) . ?
C22 C23 1.377(4) . ?
C22 H22A 0.9300 . ?
C23 C24 1.459(4) . ?
C24 C25 1.372(5) . ?
C25 C26 1.378(6) . ?
C25 H25A 0.9300 . ?
C26 C27 1.354(7) . ?
C26 H26A 0.9300 . ?
C27 C28 1.373(5) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.9887(18) 7_665 ?
Fe3 O2 1.9887(18) 10_646 ?
Fe3 O2 1.9887(18) . ?
Fe3 O1 2.0012(18) . ?
Fe3 O1 2.0012(18) 7_665 ?
Fe3 O1 2.0012(18) 10_646 ?
O1 C29 1.300(3) . ?
O2 C30 1.300(3) . ?
O3 C33 1.215(4) . ?
O4 C32 1.218(5) . ?
C29 C34 1.348(4) . ?
C29 C30 1.502(4) . ?
C30 C31 1.354(4) . ?
C31 C32 1.405(5) . ?
C31 H31A 0.9300 . ?
C32 C33 1.558(5) . ?
C33 C34 1.427(5) . ?
C34 H34A 0.9300 . ?
B1 F2 1.336(14) . ?
B1 F4 1.341(15) . ?
B1 F3 1.344(15) . ?
B1 F1 1.348(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.50(9) 10_646 7_665 ?
N2 Fe1 N2 96.50(9) 10_646 . ?
N2 Fe1 N2 96.50(9) 7_665 . ?
N2 Fe1 N1 80.16(9) 10_646 10_646 ?
N2 Fe1 N1 90.55(9) 7_665 10_646 ?
N2 Fe1 N1 172.52(9) . 10_646 ?
N2 Fe1 N1 172.52(9) 10_646 7_665 ?
N2 Fe1 N1 80.16(9) 7_665 7_665 ?
N2 Fe1 N1 90.55(9) . 7_665 ?
N1 Fe1 N1 93.13(9) 10_646 7_665 ?
N2 Fe1 N1 90.56(9) 10_646 . ?
N2 Fe1 N1 172.52(9) 7_665 . ?
N2 Fe1 N1 80.16(9) . . ?
N1 Fe1 N1 93.12(9) 10_646 . ?
N1 Fe1 N1 93.12(9) 7_665 . ?
N5 Fe2 N5 97.23(9) 7_665 10_646 ?
N5 Fe2 N5 97.22(9) 7_665 . ?
N5 Fe2 N5 97.23(9) 10_646 . ?
N5 Fe2 N6 91.49(10) 7_665 . ?
N5 Fe2 N6 170.89(10) 10_646 . ?
N5 Fe2 N6 78.97(10) . . ?
N5 Fe2 N6 170.89(10) 7_665 10_646 ?
N5 Fe2 N6 78.97(10) 10_646 10_646 ?
N5 Fe2 N6 91.49(10) . 10_646 ?
N6 Fe2 N6 92.78(10) . 10_646 ?
N5 Fe2 N6 78.97(10) 7_665 7_665 ?
N5 Fe2 N6 91.49(10) 10_646 7_665 ?
N5 Fe2 N6 170.89(10) . 7_665 ?
N6 Fe2 N6 92.78(10) . 7_665 ?
N6 Fe2 N6 92.78(10) 10_646 7_665 ?
C1 N1 C5 117.8(3) . . ?
C1 N1 Fe1 127.3(2) . . ?
C5 N1 Fe1 114.88(19) . . ?
C6 N2 N3 106.2(2) . . ?
C6 N2 Fe1 116.14(19) . . ?
N3 N2 Fe1 136.29(18) . . ?
N2 N3 C8 110.6(2) . . ?
N2 N3 H3 114(2) . . ?
C8 N3 H3 135(2) . . ?
N5 N4 C21 110.9(2) . . ?
N5 N4 H4 121(3) . . ?
C21 N4 H4 127(3) . . ?
C23 N5 N4 105.5(2) . . ?
C23 N5 Fe2 115.9(2) . . ?
N4 N5 Fe2 135.19(18) . . ?
C28 N6 C24 117.1(3) . . ?
C28 N6 Fe2 127.6(2) . . ?
C24 N6 Fe2 115.2(2) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.3(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.3(3) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.6(3) . . ?
N1 C5 C6 113.5(2) . . ?
C4 C5 C6 123.9(3) . . ?
N2 C6 C7 110.8(3) . . ?
N2 C6 C5 114.8(3) . . ?
C7 C6 C5 134.4(3) . . ?
C8 C7 C6 105.6(3) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 106.8(2) . . ?
N3 C8 C9 123.2(3) . . ?
C7 C8 C9 130.0(3) . . ?
C14 C9 C10 119.1(3) . . ?
C14 C9 C8 121.5(3) . . ?
C10 C9 C8 119.3(3) . . ?
C11 C10 C9 119.8(4) . . ?
C11 C10 H10A 120.1 . . ?
C9 C10 H10A 120.1 . . ?
C12 C11 C10 120.4(4) . . ?
C12 C11 H11A 119.8 . . ?
C10 C11 H11A 119.8 . . ?
C11 C12 C13 121.1(4) . . ?
C11 C12 H12A 119.4 . . ?
C13 C12 H12A 119.4 . . ?
C12 C13 C14 117.9(3) . . ?
C12 C13 C15 122.3(3) . . ?
C14 C13 C15 119.5(3) . . ?
C9 C14 C13 121.5(3) . . ?
C9 C14 H14A 119.2 . . ?
C13 C14 H14A 119.2 . . ?
C16 C15 C20 118.6(3) . . ?
C16 C15 C13 123.4(3) . . ?
C20 C15 C13 118.1(3) . . ?
C17 C16 C15 120.0(4) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.5(4) . . ?
C16 C17 H17A 119.2 . . ?
C18 C17 H17A 119.2 . . ?
C17 C18 C19 119.2(4) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 118.5(3) . . ?
C20 C19 C21 121.2(3) . . ?
C18 C19 C21 120.1(3) . . ?
C19 C20 C15 122.2(3) . . ?
C19 C20 H20A 118.9 . . ?
C15 C20 H20A 118.9 . . ?
N4 C21 C22 106.7(3) . . ?
N4 C21 C19 121.2(3) . . ?
C22 C21 C19 131.8(3) . . ?
C21 C22 C23 105.5(3) . . ?
C21 C22 H22A 127.2 . . ?
C23 C22 H22A 127.2 . . ?
N5 C23 C22 111.2(3) . . ?
N5 C23 C24 114.8(3) . . ?
C22 C23 C24 133.9(3) . . ?
N6 C24 C25 123.0(3) . . ?
N6 C24 C23 113.2(3) . . ?
C25 C24 C23 123.8(3) . . ?
C24 C25 C26 118.2(4) . . ?
C24 C25 H25A 120.9 . . ?
C26 C25 H25A 120.9 . . ?
C27 C26 C25 120.0(4) . . ?
C27 C26 H26A 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C26 C27 C28 118.8(4) . . ?
C26 C27 H27A 120.6 . . ?
C28 C27 H27A 120.6 . . ?
N6 C28 C27 122.9(4) . . ?
N6 C28 H28A 118.5 . . ?
C27 C28 H28A 118.5 . . ?
O2 Fe3 O2 90.16(8) 7_665 10_646 ?
O2 Fe3 O2 90.16(8) 7_665 . ?
O2 Fe3 O2 90.16(8) 10_646 . ?
O2 Fe3 O1 170.82(7) 7_665 . ?
O2 Fe3 O1 95.22(8) 10_646 . ?
O2 Fe3 O1 82.41(7) . . ?
O2 Fe3 O1 82.42(7) 7_665 7_665 ?
O2 Fe3 O1 170.82(7) 10_646 7_665 ?
O2 Fe3 O1 95.22(8) . 7_665 ?
O1 Fe3 O1 92.85(8) . 7_665 ?
O2 Fe3 O1 95.23(8) 7_665 10_646 ?
O2 Fe3 O1 82.42(7) 10_646 10_646 ?
O2 Fe3 O1 170.82(7) . 10_646 ?
O1 Fe3 O1 92.86(8) . 10_646 ?
O1 Fe3 O1 92.85(8) 7_665 10_646 ?
C29 O1 Fe3 113.30(16) . . ?
C30 O2 Fe3 112.91(16) . . ?
O1 C29 C34 124.6(3) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.4(3) . . ?
O2 C30 C31 122.9(3) . . ?
O2 C30 C29 116.4(2) . . ?
C31 C30 C29 120.8(3) . . ?
C30 C31 C32 121.8(3) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O4 C32 C31 124.4(3) . . ?
O4 C32 C33 117.7(3) . . ?
C31 C32 C33 117.8(3) . . ?
O3 C33 C34 124.8(3) . . ?
O3 C33 C32 117.5(3) . . ?
C34 C33 C32 117.8(3) . . ?
C29 C34 C33 121.4(3) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F2 B1 F4 111(2) . . ?
F2 B1 F3 106(2) . . ?
F4 B1 F3 110(3) . . ?
F2 B1 F1 105.3(18) . . ?
F4 B1 F1 112(3) . . ?
F3 B1 F1 113(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(2) 2.04(3) 2.884(3) 158(3) . yes
N4 H4 O2 0.85(2) 2.11(2) 2.950(3) 168(3) 10_646 yes

_refine_diff_density_max         0.349
_refine_diff_density_min         -0.192
_refine_diff_density_rms         0.035

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-150K
_database_code_depnum_ccdc_archive 'CCDC 2261766'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.5393(4)
_cell_length_b                   21.5393(4)
_cell_length_c                   21.5393(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9993.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9865
_cell_measurement_theta_min      2.74
_cell_measurement_theta_max      27.83

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.678
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            305142
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_av_R_equivalents  0.0584
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.168
_diffrn_reflns_theta_max         27.860
_diffrn_reflns_theta_full        27.850
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7381
_reflns_number_gt                7241
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.853
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.999

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1685 cubic angstrom  with only 165 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of the BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.160 -0.094 -0.086      1738       165 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-150K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1685 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1693 cubic angstrom  with only 109 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.160 -0.094 -0.086      1738       165 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0585P)²+1.9052P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3273 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7381
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0891
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_restrained_S_all      1.078
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54772(2) 0.54772(2) 0.54772(2) 0.02859(13) Uani 1 3 d S T P . .
Fe2 Fe 0.83095(2) 0.83095(2) 0.83095(2) 0.03048(13) Uani 1 3 d S T P . .
N1 N 0.49073(10) 0.58166(10) 0.48284(10) 0.0332(4) Uani 1 1 d . . . . .
N2 N 0.60231(9) 0.61045(9) 0.51100(9) 0.0313(4) Uani 1 1 d . . . . .
N3 N 0.66251(10) 0.62618(9) 0.51546(9) 0.0315(4) Uani 1 1 d . . . . .
H3 H 0.6805(16) 0.6157(17) 0.5522(17) 0.047 Uiso 1 1 d . U . . .
N4 N 0.86653(10) 0.74529(10) 0.72254(10) 0.0325(4) Uani 1 1 d D . . . .
H4 H 0.8318(13) 0.7515(16) 0.7019(15) 0.049 Uiso 1 1 d D U . . .
N5 N 0.86780(10) 0.76345(10) 0.78261(10) 0.0329(4) Uani 1 1 d . . . . .
N6 N 0.89078(10) 0.79715(10) 0.89347(10) 0.0372(4) Uani 1 1 d . . . . .
C1 C 0.43203(12) 0.56445(12) 0.47179(13) 0.0390(5) Uani 1 1 d . . . . .
H1A H 0.413077 0.534993 0.498589 0.047 Uiso 1 1 calc R U . . .
C2 C 0.39786(14) 0.58819(14) 0.42247(15) 0.0479(7) Uani 1 1 d . . . . .
H2A H 0.356734 0.574116 0.414979 0.057 Uiso 1 1 calc R U . . .
C3 C 0.42453(15) 0.63263(15) 0.38438(15) 0.0498(7) Uani 1 1 d . . . . .
H3A H 0.401810 0.649693 0.350650 0.060 Uiso 1 1 calc R U . . .
C4 C 0.48465(14) 0.65180(14) 0.39613(14) 0.0449(6) Uani 1 1 d . . . . .
H4A H 0.503732 0.682799 0.371223 0.054 Uiso 1 1 calc R U . . .
C5 C 0.51637(12) 0.62480(11) 0.44501(12) 0.0344(5) Uani 1 1 d . . . . .
C6 C 0.58071(12) 0.63841(11) 0.46011(11) 0.0341(5) Uani 1 1 d . . . . .
C7 C 0.62704(13) 0.67318(13) 0.43167(12) 0.0383(5) Uani 1 1 d . . . . .
H7A H 0.623607 0.697399 0.394971 0.046 Uiso 1 1 calc R U . . .
C8 C 0.67883(12) 0.66504(12) 0.46796(11) 0.0352(5) Uani 1 1 d . . . . .
C9 C 0.74158(12) 0.69001(12) 0.46055(11) 0.0375(5) Uani 1 1 d . . . . .
C10 C 0.75353(15) 0.73203(16) 0.41258(14) 0.0490(7) Uani 1 1 d . . . . .
H10A H 0.720910 0.745268 0.386016 0.059 Uiso 1 1 calc R U . . .
C11 C 0.81320(17) 0.75421(19) 0.40403(16) 0.0619(9) Uani 1 1 d . . . . .
H11A H 0.821280 0.782645 0.371306 0.074 Uiso 1 1 calc R U . . .
C12 C 0.86089(15) 0.73581(19) 0.44204(15) 0.0580(9) Uani 1 1 d . . . . .
H12A H 0.901784 0.750640 0.434739 0.070 Uiso 1 1 calc R U . . .
C13 C 0.84960(13) 0.69558(15) 0.49117(13) 0.0438(6) Uani 1 1 d . . . . .
C14 C 0.78968(12) 0.67242(13) 0.49980(12) 0.0385(5) Uani 1 1 d . . . . .
H14A H 0.781693 0.644339 0.532861 0.046 Uiso 1 1 calc R U . . .
C15 C 0.89774(12) 0.68156(15) 0.53791(13) 0.0442(6) Uani 1 1 d . . . . .
C16 C 0.95607(15) 0.6585(2) 0.52274(16) 0.0623(9) Uani 1 1 d . . . . .
H16A H 0.966171 0.649858 0.480684 0.075 Uiso 1 1 calc R U . . .
C17 C 0.99934(16) 0.6482(2) 0.56895(18) 0.0684(10) Uani 1 1 d . . . . .
H17A H 1.038872 0.631660 0.558483 0.082 Uiso 1 1 calc R U . . .
C18 C 0.98581(14) 0.66156(19) 0.63022(16) 0.0564(8) Uani 1 1 d . . . . .
H18A H 1.015875 0.654184 0.661633 0.068 Uiso 1 1 calc R U . . .
C19 C 0.92753(12) 0.68608(13) 0.64587(13) 0.0404(6) Uani 1 1 d . . . . .
C20 C 0.88423(12) 0.69432(13) 0.59972(12) 0.0388(5) Uani 1 1 d . . . . .
H20A H 0.844059 0.709112 0.610333 0.047 Uiso 1 1 calc R U . . .
C21 C 0.91561(11) 0.70788(12) 0.70946(12) 0.0353(5) Uani 1 1 d . . . . .
C22 C 0.95033(12) 0.70246(12) 0.76315(13) 0.0390(5) Uani 1 1 d . . . . .
H22A H 0.987578 0.679535 0.768846 0.047 Uiso 1 1 calc R U . . .
C23 C 0.91897(12) 0.73774(12) 0.80684(12) 0.0353(5) Uani 1 1 d . . . . .
C24 C 0.93115(13) 0.75437(13) 0.87121(13) 0.0387(5) Uani 1 1 d . . . . .
C25 C 0.97877(15) 0.72988(15) 0.90594(15) 0.0505(7) Uani 1 1 d . . . . .
H25A H 1.006806 0.700796 0.888228 0.061 Uiso 1 1 calc R U . . .
C26 C 0.98516(18) 0.74830(18) 0.96707(16) 0.0616(9) Uani 1 1 d . . . . .
H26A H 1.017593 0.731999 0.992131 0.074 Uiso 1 1 calc R U . . .
C27 C 0.94364(18) 0.79078(18) 0.99110(15) 0.0597(8) Uani 1 1 d . . . . .
H27A H 0.946711 0.803708 1.033158 0.072 Uiso 1 1 calc R U . . .
C28 C 0.89751(15) 0.81426(15) 0.95314(14) 0.0467(6) Uani 1 1 d . . . . .
H28A H 0.869343 0.843750 0.969938 0.056 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68848(2) 0.68848(2) 0.68848(2) 0.03702(15) Uani 1 3 d S T P . .
O1 O 0.72135(8) 0.61956(8) 0.63547(8) 0.0329(3) Uani 1 1 d . . . . .
O2 O 0.75227(8) 0.65744(8) 0.74740(8) 0.0357(4) Uani 1 1 d . . . . .
O3 O 0.86601(13) 0.45711(14) 0.65020(12) 0.0728(8) Uani 1 1 d . . . . .
O4 O 0.89124(13) 0.49203(15) 0.76820(12) 0.0720(8) Uani 1 1 d . . . . .
C29 C 0.76559(11) 0.58801(12) 0.66213(11) 0.0347(5) Uani 1 1 d . . . . .
C30 C 0.78155(12) 0.60863(13) 0.72702(12) 0.0364(5) Uani 1 1 d . . . . .
C31 C 0.82355(14) 0.57671(15) 0.76194(13) 0.0458(6) Uani 1 1 d . . . . .
H31A H 0.832385 0.590441 0.802911 0.055 Uiso 1 1 calc R U . . .
C32 C 0.85441(14) 0.52342(17) 0.73848(14) 0.0510(7) Uani 1 1 d . . . . .
C33 C 0.83947(14) 0.50312(16) 0.67033(14) 0.0493(7) Uani 1 1 d . . . . .
C34 C 0.79495(13) 0.53907(14) 0.63603(12) 0.0416(6) Uani 1 1 d . . . . .
H34A H 0.785975 0.528233 0.594228 0.050 Uiso 1 1 calc R U . . .
B1 B 0.3925(7) 0.3929(10) 0.3928(11) 0.0507(15) Uani 0.3333 1 d D U P A -1
F1 F 0.3825(12) 0.3395(13) 0.4260(18) 0.067(4) Uani 0.3333 1 d D U P A -1
F2 F 0.4160(7) 0.4383(14) 0.4313(19) 0.101(6) Uani 0.3333 1 d D U P A -1
F3 F 0.4368(12) 0.3880(14) 0.3473(10) 0.087(6) Uani 0.3333 1 d D U P A -1
F4 F 0.3376(9) 0.4147(15) 0.3689(13) 0.081(6) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.958(2) . ?
Fe1 N2 1.958(2) 9 ?
Fe1 N2 1.958(2) 5 ?
Fe1 N1 1.998(2) 5 ?
Fe1 N1 1.998(2) 9 ?
Fe1 N1 1.999(2) . ?
Fe2 N5 1.957(2) 5 ?
Fe2 N5 1.957(2) 9 ?
Fe2 N5 1.957(2) . ?
Fe2 N6 2.001(2) 5 ?
Fe2 N6 2.001(2) 9 ?
Fe2 N6 2.001(2) . ?
N1 C1 1.339(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.334(3) . ?
N2 N3 1.344(3) . ?
N3 C8 1.368(3) . ?
N3 H3 0.91(4) . ?
N4 N5 1.352(3) . ?
N4 C21 1.359(3) . ?
N4 H4 0.88(2) . ?
N5 C23 1.339(3) . ?
N6 C28 1.345(4) . ?
N6 C24 1.355(4) . ?
C1 C2 1.390(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.385(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.383(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.383(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.453(4) . ?
C6 C7 1.390(4) . ?
C7 C8 1.373(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.463(4) . ?
C9 C14 1.390(4) . ?
C9 C10 1.398(4) . ?
C10 C11 1.383(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.372(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.389(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.396(4) . ?
C13 C15 1.476(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.390(4) . ?
C15 C20 1.390(4) . ?
C16 C17 1.382(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.382(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.403(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.374(4) . ?
C19 C21 1.471(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.382(4) . ?
C22 C23 1.386(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.456(4) . ?
C24 C25 1.375(4) . ?
C25 C26 1.382(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.380(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.383(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.9863(18) 5 ?
Fe3 O2 1.9863(18) . ?
Fe3 O2 1.9863(18) 9 ?
Fe3 O1 2.0022(17) . ?
Fe3 O1 2.0022(17) 5 ?
Fe3 O1 2.0022(18) 9 ?
O1 C29 1.304(3) . ?
O2 C30 1.302(3) . ?
O3 C33 1.224(4) . ?
O4 C32 1.223(4) . ?
C29 C34 1.352(4) . ?
C29 C30 1.506(4) . ?
C30 C31 1.363(4) . ?
C31 C32 1.419(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.565(4) . ?
C33 C34 1.437(4) . ?
C34 H34A 0.9500 . ?
B1 F3 1.373(14) . ?
B1 F1 1.370(14) . ?
B1 F2 1.377(10) . ?
B1 F4 1.373(13) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.13(8) . 9 ?
N2 Fe1 N2 96.14(8) . 5 ?
N2 Fe1 N2 96.13(8) 9 5 ?
N2 Fe1 N1 172.54(9) . 5 ?
N2 Fe1 N1 90.85(8) 9 5 ?
N2 Fe1 N1 80.45(8) 5 5 ?
N2 Fe1 N1 90.84(8) . 9 ?
N2 Fe1 N1 80.45(8) 9 9 ?
N2 Fe1 N1 172.54(9) 5 9 ?
N1 Fe1 N1 92.92(8) 5 9 ?
N2 Fe1 N1 80.45(8) . . ?
N2 Fe1 N1 172.54(9) 9 . ?
N2 Fe1 N1 90.85(8) 5 . ?
N1 Fe1 N1 92.92(8) 5 . ?
N1 Fe1 N1 92.92(8) 9 . ?
N5 Fe2 N5 97.00(8) 5 9 ?
N5 Fe2 N5 97.00(8) 5 . ?
N5 Fe2 N5 97.00(8) 9 . ?
N5 Fe2 N6 80.01(9) 5 5 ?
N5 Fe2 N6 172.06(9) 9 5 ?
N5 Fe2 N6 90.68(9) . 5 ?
N5 Fe2 N6 90.68(9) 5 9 ?
N5 Fe2 N6 80.01(9) 9 9 ?
N5 Fe2 N6 172.06(9) . 9 ?
N6 Fe2 N6 92.62(9) 5 9 ?
N5 Fe2 N6 172.06(9) 5 . ?
N5 Fe2 N6 90.68(9) 9 . ?
N5 Fe2 N6 80.01(9) . . ?
N6 Fe2 N6 92.62(9) 5 . ?
N6 Fe2 N6 92.62(9) 9 . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Fe1 127.09(18) . . ?
C5 N1 Fe1 114.92(17) . . ?
C6 N2 N3 106.4(2) . . ?
C6 N2 Fe1 115.71(17) . . ?
N3 N2 Fe1 136.44(16) . . ?
N2 N3 C8 110.4(2) . . ?
N2 N3 H3 114(2) . . ?
C8 N3 H3 134(2) . . ?
N5 N4 C21 110.8(2) . . ?
N5 N4 H4 117(2) . . ?
C21 N4 H4 130(2) . . ?
C23 N5 N4 105.7(2) . . ?
C23 N5 Fe2 115.70(18) . . ?
N4 N5 Fe2 135.73(17) . . ?
C28 N6 C24 117.1(2) . . ?
C28 N6 Fe2 127.8(2) . . ?
C24 N6 Fe2 115.00(18) . . ?
N1 C1 C2 122.3(3) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.2(3) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C4 C3 C2 119.1(3) . . ?
C4 C3 H3A 120.4 . . ?
C2 C3 H3A 120.4 . . ?
C3 C4 C5 118.4(3) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
N1 C5 C4 123.0(2) . . ?
N1 C5 C6 113.1(2) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.2(2) . . ?
C7 C6 C5 134.0(2) . . ?
C8 C7 C6 105.3(2) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.2(2) . . ?
N3 C8 C9 122.9(2) . . ?
C7 C8 C9 129.9(2) . . ?
C14 C9 C10 119.3(3) . . ?
C14 C9 C8 121.5(2) . . ?
C10 C9 C8 119.3(3) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11A 119.5 . . ?
C10 C11 H11A 119.5 . . ?
C11 C12 C13 120.2(3) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C12 C13 C14 119.1(3) . . ?
C12 C13 C15 121.6(3) . . ?
C14 C13 C15 119.0(3) . . ?
C9 C14 C13 120.7(3) . . ?
C9 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C16 C15 C20 119.0(3) . . ?
C16 C15 C13 123.2(3) . . ?
C20 C15 C13 117.7(2) . . ?
C17 C16 C15 119.9(3) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C16 C17 C18 120.8(3) . . ?
C16 C17 H17A 119.6 . . ?
C18 C17 H17A 119.6 . . ?
C17 C18 C19 119.8(3) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 120.9(2) . . ?
C18 C19 C21 120.0(3) . . ?
C19 C20 C15 121.7(2) . . ?
C19 C20 H20A 119.2 . . ?
C15 C20 H20A 119.2 . . ?
N4 C21 C22 107.3(2) . . ?
N4 C21 C19 121.2(2) . . ?
C22 C21 C19 131.1(2) . . ?
C21 C22 C23 105.0(2) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.3(2) . . ?
N5 C23 C24 114.7(2) . . ?
C22 C23 C24 133.9(2) . . ?
N6 C24 C25 123.2(3) . . ?
N6 C24 C23 112.9(2) . . ?
C25 C24 C23 123.9(3) . . ?
C24 C25 C26 118.9(3) . . ?
C24 C25 H25A 120.6 . . ?
C26 C25 H25A 120.6 . . ?
C27 C26 C25 118.9(3) . . ?
C27 C26 H26A 120.6 . . ?
C25 C26 H26A 120.6 . . ?
C26 C27 C28 119.1(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.8(3) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 90.34(8) 5 . ?
O2 Fe3 O2 90.34(8) 5 9 ?
O2 Fe3 O2 90.34(8) . 9 ?
O2 Fe3 O1 95.45(7) 5 . ?
O2 Fe3 O1 82.54(7) . . ?
O2 Fe3 O1 170.83(7) 9 . ?
O2 Fe3 O1 82.54(7) 5 5 ?
O2 Fe3 O1 170.83(7) . 5 ?
O2 Fe3 O1 95.45(7) 9 5 ?
O1 Fe3 O1 92.35(7) . 5 ?
O2 Fe3 O1 170.83(7) 5 9 ?
O2 Fe3 O1 95.45(7) . 9 ?
O2 Fe3 O1 82.54(7) 9 9 ?
O1 Fe3 O1 92.35(7) . 9 ?
O1 Fe3 O1 92.35(7) 5 9 ?
C29 O1 Fe3 113.19(16) . . ?
C30 O2 Fe3 113.04(16) . . ?
O1 C29 C34 124.4(2) . . ?
O1 C29 C30 114.9(2) . . ?
C34 C29 C30 120.6(2) . . ?
O2 C30 C31 122.9(2) . . ?
O2 C30 C29 116.1(2) . . ?
C31 C30 C29 121.0(2) . . ?
C30 C31 C32 121.5(3) . . ?
C30 C31 H31A 119.3 . . ?
C32 C31 H31A 119.3 . . ?
O4 C32 C31 124.4(3) . . ?
O4 C32 C33 118.0(3) . . ?
C31 C32 C33 117.6(3) . . ?
O3 C33 C34 124.5(3) . . ?
O3 C33 C32 117.6(3) . . ?
C34 C33 C32 118.0(3) . . ?
C29 C34 C33 121.2(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F3 B1 F1 115(2) . . ?
F3 B1 F2 103.2(15) . . ?
F1 B1 F2 109.9(18) . . ?
F3 B1 F4 110.9(18) . . ?
F1 B1 F4 110.3(19) . . ?
F2 B1 F4 107.4(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.91(4) 2.00(4) 2.882(3) 163(3) . yes
N4 H4 O2 0.88(2) 2.05(2) 2.928(3) 171(3) 5 yes

_refine_diff_density_max         0.413
_refine_diff_density_min         -0.397
_refine_diff_density_rms         0.073

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-390K
_database_code_depnum_ccdc_archive 'CCDC 2261760'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.7575(3)
_cell_length_b                   21.7575(3)
_cell_length_c                   21.7575(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10299.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    390(2)
_cell_measurement_reflns_used    9563
_cell_measurement_theta_min      2.71
_cell_measurement_theta_max      24.26

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.522
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.950
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.651
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      390(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            124944
_diffrn_reflns_av_unetI/netI     0.0213
_diffrn_reflns_av_R_equivalents  0.0447
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.146
_diffrn_reflns_theta_max         24.498
_diffrn_reflns_theta_full        24.460
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.994
_reflns_number_total             5285
_reflns_number_gt                4993
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.834
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1845 cubic angstrom  with only 40 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of the BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.150 -0.088 -0.079      1845        40 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-390K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1845 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1845 cubic angstrom  with only 40 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.150 -0.088 -0.079      1845        40 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0569P)²+0.6104P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.024(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         5285
_refine_ls_number_parameters     457
_refine_ls_number_restraints     61
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0846
_refine_ls_wR_factor_gt          0.0831
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_restrained_S_all      1.056
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.95113(2) 0.45113(2) 0.04887(2) 0.0704(2) Uani 1 3 d S T P . .
Fe2 Fe 0.67060(2) 0.17060(2) 0.32940(2) 0.0723(2) Uani 1 3 d S T P . .
N1 N 0.91642(14) 0.51979(14) -0.00708(13) 0.0857(7) Uani 1 1 d . . . . .
N2 N 0.88774(13) 0.48930(12) 0.10430(12) 0.0767(6) Uani 1 1 d . . . . .
N3 N 0.87163(14) 0.48478(12) 0.16398(13) 0.0795(7) Uani 1 1 d D . . . .
H3 H 0.884(2) 0.4512(16) 0.1847(19) 0.119 Uiso 1 1 d D U . . .
N4 N 0.76021(15) 0.27919(13) 0.36770(12) 0.0798(7) Uani 1 1 d D . . . .
H4 H 0.750(2) 0.3002(19) 0.3342(16) 0.120 Uiso 1 1 d D U . . .
N5 N 0.74190(13) 0.22013(13) 0.36891(12) 0.0789(7) Uani 1 1 d . . . . .
N6 N 0.70613(15) 0.10939(14) 0.39682(16) 0.0942(8) Uani 1 1 d . . . . .
C1 C 0.9324(2) 0.5322(2) -0.06472(17) 0.1029(12) Uani 1 1 d . . . . .
H1A H 0.960924 0.506782 -0.083907 0.123 Uiso 1 1 calc R U . . .
C2 C 0.9088(2) 0.5806(3) -0.0971(2) 0.1326(19) Uani 1 1 d . . . . .
H2A H 0.921977 0.588544 -0.136943 0.159 Uiso 1 1 calc R U . . .
C3 C 0.8662(3) 0.6166(3) -0.0705(3) 0.140(2) Uani 1 1 d . . . . .
H3A H 0.849378 0.649463 -0.092076 0.168 Uiso 1 1 calc R U . . .
C4 C 0.8475(2) 0.6047(2) -0.0108(2) 0.1193(15) Uani 1 1 d . . . . .
H4A H 0.817709 0.628810 0.008096 0.143 Uiso 1 1 calc R U . . .
C5 C 0.87452(16) 0.55590(18) 0.01986(17) 0.0876(9) Uani 1 1 d . . . . .
C6 C 0.86082(16) 0.54015(16) 0.08362(17) 0.0822(8) Uani 1 1 d . . . . .
C7 C 0.82720(18) 0.56783(16) 0.12932(18) 0.0908(10) Uani 1 1 d . . . . .
H7A H 0.804357 0.603821 0.126250 0.109 Uiso 1 1 calc R U . . .
C8 C 0.83421(17) 0.53145(15) 0.18054(17) 0.0851(9) Uani 1 1 d . . . . .
C9 C 0.80954(19) 0.53846(15) 0.24287(18) 0.0920(10) Uani 1 1 d . . . . .
C10 C 0.7676(3) 0.5851(2) 0.2539(3) 0.1368(19) Uani 1 1 d . . . . .
H10A H 0.754379 0.610448 0.222053 0.164 Uiso 1 1 calc R U . . .
C11 C 0.7458(4) 0.5934(3) 0.3129(3) 0.175(3) Uani 1 1 d . . . . .
H11A H 0.717877 0.624846 0.320889 0.210 Uiso 1 1 calc R U . . .
C12 C 0.7645(4) 0.5563(3) 0.3595(3) 0.164(3) Uani 1 1 d . . . . .
H12A H 0.750119 0.563533 0.399084 0.197 Uiso 1 1 calc R U . . .
C13 C 0.8041(3) 0.50840(18) 0.34932(18) 0.1101(14) Uani 1 1 d . . . . .
C14 C 0.8265(2) 0.50036(16) 0.28972(17) 0.0926(10) Uani 1 1 d . . . . .
H14A H 0.853701 0.468318 0.281784 0.111 Uiso 1 1 calc R U . . .
C15 C 0.8193(2) 0.46289(19) 0.39698(17) 0.1072(13) Uani 1 1 d . . . . .
C16 C 0.8441(4) 0.4783(3) 0.4533(2) 0.155(3) Uani 1 1 d . . . . .
H16A H 0.853364 0.519051 0.462282 0.186 Uiso 1 1 calc R U . . .
C17 C 0.8551(4) 0.4334(3) 0.4958(3) 0.166(3) Uani 1 1 d . . . . .
H17A H 0.872420 0.444162 0.533296 0.199 Uiso 1 1 calc R U . . .
C18 C 0.8412(3) 0.3727(3) 0.4848(2) 0.139(2) Uani 1 1 d . . . . .
H18A H 0.849072 0.342887 0.514364 0.167 Uiso 1 1 calc R U . . .
C19 C 0.8152(2) 0.35691(18) 0.42839(16) 0.0953(10) Uani 1 1 d . . . . .
C20 C 0.8059(2) 0.40186(17) 0.38596(16) 0.0945(10) Uani 1 1 d . . . . .
H20A H 0.789758 0.391026 0.347886 0.113 Uiso 1 1 calc R U . . .
C21 C 0.79326(17) 0.29397(17) 0.41808(15) 0.0845(9) Uani 1 1 d . . . . .
C22 C 0.79531(18) 0.24202(19) 0.45364(17) 0.0950(10) Uani 1 1 d . . . . .
H22A H 0.814423 0.237579 0.491619 0.114 Uiso 1 1 calc R U . . .
C23 C 0.76324(17) 0.19762(17) 0.42162(16) 0.0850(9) Uani 1 1 d . . . . .
C24 C 0.74649(19) 0.13422(18) 0.43618(18) 0.0952(10) Uani 1 1 d . . . . .
C25 C 0.7697(3) 0.1027(2) 0.4853(3) 0.1342(18) Uani 1 1 d . . . . .
H25A H 0.796696 0.121328 0.512681 0.161 Uiso 1 1 calc R U . . .
C26 C 0.7517(3) 0.0427(3) 0.4929(4) 0.167(3) Uani 1 1 d . . . . .
H26A H 0.767509 0.019815 0.525385 0.200 Uiso 1 1 calc R U . . .
C27 C 0.7112(3) 0.0163(3) 0.4534(3) 0.162(3) Uani 1 1 d . . . . .
H27A H 0.698649 -0.024217 0.458479 0.195 Uiso 1 1 calc R U . . .
C28 C 0.6894(3) 0.0509(2) 0.4062(3) 0.1248(16) Uani 1 1 d . . . . .
H28A H 0.661591 0.033048 0.379146 0.150 Uiso 1 1 calc R U . . .
Fe3 Fe 0.81241(2) 0.31241(2) 0.18759(2) 0.0750(2) Uani 1 3 d S T P . .
O1 O 0.77938(10) 0.38089(10) 0.13637(9) 0.0745(5) Uani 1 1 d . . . . .
O2 O 0.75044(10) 0.34314(10) 0.24737(9) 0.0769(5) Uani 1 1 d . . . . .
O3 O 0.6264(2) 0.5307(2) 0.1481(2) 0.191(2) Uani 1 1 d . . . . .
O4 O 0.6013(2) 0.4946(3) 0.2637(2) 0.207(3) Uani 1 1 d . . . . .
C29 C 0.73409(15) 0.41002(16) 0.16240(14) 0.0757(8) Uani 1 1 d . . . . .
C30 C 0.71875(15) 0.38929(15) 0.22649(15) 0.0769(8) Uani 1 1 d . . . . .
C31 C 0.67533(18) 0.4176(2) 0.25924(18) 0.1017(12) Uani 1 1 d . . . . .
H31A H 0.667575 0.404586 0.299226 0.122 Uiso 1 1 calc R U . . .
C32 C 0.6411(2) 0.4664(3) 0.2347(2) 0.1257(17) Uani 1 1 d . . . . .
C33 C 0.6558(2) 0.4878(3) 0.1690(2) 0.1185(15) Uani 1 1 d . . . . .
C34 C 0.70254(17) 0.4564(2) 0.13646(18) 0.0957(11) Uani 1 1 d . . . . .
H34A H 0.711646 0.468156 0.096375 0.115 Uiso 1 1 calc R U . . .
B1 B 0.8911(14) 0.1098(12) 0.6083(9) 0.151(4) Uani 0.3333 1 d D U P A -1
F1 F 0.8456(16) 0.0687(14) 0.6191(15) 0.199(9) Uani 0.3333 1 d D U P A -1
F2 F 0.9236(16) 0.0979(11) 0.5567(9) 0.227(8) Uani 0.3333 1 d D U P A -1
F3 F 0.8645(12) 0.1660(11) 0.5993(10) 0.208(8) Uani 0.3333 1 d D U P A -1
F4 F 0.9308(13) 0.1108(16) 0.6564(14) 0.194(9) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.012(3) . ?
Fe1 N2 2.012(3) 8_645 ?
Fe1 N2 2.012(3) 11_556 ?
Fe1 N1 2.070(3) . ?
Fe1 N1 2.070(3) 11_556 ?
Fe1 N1 2.070(3) 8_645 ?
Fe2 N5 2.075(3) 11_556 ?
Fe2 N5 2.075(3) 8_645 ?
Fe2 N5 2.075(3) . ?
Fe2 N6 2.127(3) 11_556 ?
Fe2 N6 2.127(3) . ?
Fe2 N6 2.127(3) 8_645 ?
N1 C1 1.329(5) . ?
N1 C5 1.339(5) . ?
N2 C6 1.330(4) . ?
N2 N3 1.349(4) . ?
N3 C8 1.350(5) . ?
N3 H3 0.90(3) . ?
N4 N5 1.345(4) . ?
N4 C21 1.350(5) . ?
N4 H4 0.89(3) . ?
N5 C23 1.331(4) . ?
N6 C28 1.340(5) . ?
N6 C24 1.340(5) . ?
C1 C2 1.368(7) . ?
C1 H1A 0.9300 . ?
C2 C3 1.344(8) . ?
C2 H2A 0.9300 . ?
C3 C4 1.385(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.385(6) . ?
C4 H4A 0.9300 . ?
C5 C6 1.460(5) . ?
C6 C7 1.373(5) . ?
C7 C8 1.375(5) . ?
C7 H7A 0.9300 . ?
C8 C9 1.467(5) . ?
C9 C14 1.365(6) . ?
C9 C10 1.386(6) . ?
C10 C11 1.382(8) . ?
C10 H10A 0.9300 . ?
C11 C12 1.358(9) . ?
C11 H11A 0.9300 . ?
C12 C13 1.370(8) . ?
C12 H12A 0.9300 . ?
C13 C14 1.397(6) . ?
C13 C15 1.472(6) . ?
C14 H14A 0.9300 . ?
C15 C16 1.380(6) . ?
C15 C20 1.381(5) . ?
C16 C17 1.366(8) . ?
C16 H16A 0.9300 . ?
C17 C18 1.374(7) . ?
C17 H17A 0.9300 . ?
C18 C19 1.395(6) . ?
C18 H18A 0.9300 . ?
C19 C20 1.360(6) . ?
C19 C21 1.467(5) . ?
C20 H20A 0.9300 . ?
C21 C22 1.371(5) . ?
C22 C23 1.380(5) . ?
C22 H22A 0.9300 . ?
C23 C24 1.462(5) . ?
C24 C25 1.366(6) . ?
C25 C26 1.374(8) . ?
C25 H25A 0.9300 . ?
C26 C27 1.359(9) . ?
C26 H26A 0.9300 . ?
C27 C28 1.356(7) . ?
C27 H27A 0.9300 . ?
C28 H28A 0.9300 . ?
Fe3 O2 1.989(2) 8_645 ?
Fe3 O2 1.989(2) 11_556 ?
Fe3 O2 1.989(2) . ?
Fe3 O1 1.995(2) 11_556 ?
Fe3 O1 1.995(2) . ?
Fe3 O1 1.995(2) 8_645 ?
O1 C29 1.301(4) . ?
O2 C30 1.300(4) . ?
O3 C33 1.219(5) . ?
O4 C32 1.233(6) . ?
C29 C34 1.345(5) . ?
C29 C30 1.503(5) . ?
C30 C31 1.334(5) . ?
C31 C32 1.404(6) . ?
C31 H31A 0.9300 . ?
C32 C33 1.538(6) . ?
C33 C34 1.415(6) . ?
C34 H34A 0.9300 . ?
B1 F2 1.351(14) . ?
B1 F1 1.356(15) . ?
B1 F4 1.357(15) . ?
B1 F3 1.366(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.87(10) . 8_645 ?
N2 Fe1 N2 96.87(10) . 11_556 ?
N2 Fe1 N2 96.87(10) 8_645 11_556 ?
N2 Fe1 N1 78.72(11) . . ?
N2 Fe1 N1 91.90(11) 8_645 . ?
N2 Fe1 N1 170.62(11) 11_556 . ?
N2 Fe1 N1 91.90(11) . 11_556 ?
N2 Fe1 N1 170.62(11) 8_645 11_556 ?
N2 Fe1 N1 78.72(11) 11_556 11_556 ?
N1 Fe1 N1 93.07(11) . 11_556 ?
N2 Fe1 N1 170.62(11) . 8_645 ?
N2 Fe1 N1 78.72(11) 8_645 8_645 ?
N2 Fe1 N1 91.90(11) 11_556 8_645 ?
N1 Fe1 N1 93.07(11) . 8_645 ?
N1 Fe1 N1 93.07(11) 11_556 8_645 ?
N5 Fe2 N5 97.85(10) 11_556 8_645 ?
N5 Fe2 N5 97.85(10) 11_556 . ?
N5 Fe2 N5 97.85(10) 8_645 . ?
N5 Fe2 N6 76.57(11) 11_556 11_556 ?
N5 Fe2 N6 93.86(12) 8_645 11_556 ?
N5 Fe2 N6 167.64(12) . 11_556 ?
N5 Fe2 N6 93.86(12) 11_556 . ?
N5 Fe2 N6 167.64(12) 8_645 . ?
N5 Fe2 N6 76.57(11) . . ?
N6 Fe2 N6 92.66(13) 11_556 . ?
N5 Fe2 N6 167.64(12) 11_556 8_645 ?
N5 Fe2 N6 76.57(11) 8_645 8_645 ?
N5 Fe2 N6 93.87(12) . 8_645 ?
N6 Fe2 N6 92.66(13) 11_556 8_645 ?
N6 Fe2 N6 92.66(13) . 8_645 ?
C1 N1 C5 118.2(3) . . ?
C1 N1 Fe1 127.3(3) . . ?
C5 N1 Fe1 114.5(2) . . ?
C6 N2 N3 105.8(3) . . ?
C6 N2 Fe1 116.3(2) . . ?
N3 N2 Fe1 136.5(2) . . ?
N2 N3 C8 111.0(3) . . ?
N2 N3 H3 118(3) . . ?
C8 N3 H3 131(3) . . ?
N5 N4 C21 111.7(3) . . ?
N5 N4 H4 116(3) . . ?
C21 N4 H4 132(3) . . ?
C23 N5 N4 105.4(3) . . ?
C23 N5 Fe2 115.3(2) . . ?
N4 N5 Fe2 135.2(2) . . ?
C28 N6 C24 117.6(4) . . ?
C28 N6 Fe2 127.0(3) . . ?
C24 N6 Fe2 115.2(2) . . ?
N1 C1 C2 122.9(4) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C3 C2 C1 119.1(4) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C2 C3 C4 119.8(4) . . ?
C2 C3 H3A 120.1 . . ?
C4 C3 H3A 120.1 . . ?
C3 C4 C5 118.1(5) . . ?
C3 C4 H4A 121.0 . . ?
C5 C4 H4A 121.0 . . ?
N1 C5 C4 121.8(4) . . ?
N1 C5 C6 114.7(3) . . ?
C4 C5 C6 123.5(4) . . ?
N2 C6 C7 110.7(3) . . ?
N2 C6 C5 115.3(3) . . ?
C7 C6 C5 133.9(3) . . ?
C6 C7 C8 106.0(3) . . ?
C6 C7 H7A 127.0 . . ?
C8 C7 H7A 127.0 . . ?
N3 C8 C7 106.5(3) . . ?
N3 C8 C9 123.1(3) . . ?
C7 C8 C9 130.5(3) . . ?
C14 C9 C10 119.6(4) . . ?
C14 C9 C8 121.9(3) . . ?
C10 C9 C8 118.5(4) . . ?
C11 C10 C9 118.9(5) . . ?
C11 C10 H10A 120.6 . . ?
C9 C10 H10A 120.6 . . ?
C12 C11 C10 120.8(5) . . ?
C12 C11 H11A 119.6 . . ?
C10 C11 H11A 119.6 . . ?
C11 C12 C13 121.4(5) . . ?
C11 C12 H12A 119.3 . . ?
C13 C12 H12A 119.3 . . ?
C12 C13 C14 117.7(5) . . ?
C12 C13 C15 122.7(4) . . ?
C14 C13 C15 119.4(4) . . ?
C9 C14 C13 121.5(4) . . ?
C9 C14 H14A 119.3 . . ?
C13 C14 H14A 119.3 . . ?
C16 C15 C20 118.1(5) . . ?
C16 C15 C13 123.4(4) . . ?
C20 C15 C13 118.5(4) . . ?
C17 C16 C15 119.7(5) . . ?
C17 C16 H16A 120.2 . . ?
C15 C16 H16A 120.2 . . ?
C16 C17 C18 122.1(5) . . ?
C16 C17 H17A 118.9 . . ?
C18 C17 H17A 118.9 . . ?
C17 C18 C19 118.6(5) . . ?
C17 C18 H18A 120.7 . . ?
C19 C18 H18A 120.7 . . ?
C20 C19 C18 118.7(4) . . ?
C20 C19 C21 121.3(3) . . ?
C18 C19 C21 119.8(4) . . ?
C19 C20 C15 122.8(4) . . ?
C19 C20 H20A 118.6 . . ?
C15 C20 H20A 118.6 . . ?
N4 C21 C22 106.2(3) . . ?
N4 C21 C19 121.3(3) . . ?
C22 C21 C19 132.3(3) . . ?
C21 C22 C23 106.0(3) . . ?
C21 C22 H22A 127.0 . . ?
C23 C22 H22A 127.0 . . ?
N5 C23 C22 110.7(3) . . ?
N5 C23 C24 116.6(3) . . ?
C22 C23 C24 132.6(3) . . ?
N6 C24 C25 122.7(4) . . ?
N6 C24 C23 113.9(3) . . ?
C25 C24 C23 123.4(4) . . ?
C24 C25 C26 117.8(5) . . ?
C24 C25 H25A 121.1 . . ?
C26 C25 H25A 121.1 . . ?
C27 C26 C25 120.6(5) . . ?
C27 C26 H26A 119.7 . . ?
C25 C26 H26A 119.7 . . ?
C28 C27 C26 118.1(5) . . ?
C28 C27 H27A 120.9 . . ?
C26 C27 H27A 120.9 . . ?
N6 C28 C27 123.2(5) . . ?
N6 C28 H28A 118.4 . . ?
C27 C28 H28A 118.4 . . ?
O2 Fe3 O2 90.25(9) 8_645 11_556 ?
O2 Fe3 O2 90.25(9) 8_645 . ?
O2 Fe3 O2 90.25(9) 11_556 . ?
O2 Fe3 O1 171.22(9) 8_645 11_556 ?
O2 Fe3 O1 82.53(8) 11_556 11_556 ?
O2 Fe3 O1 94.76(9) . 11_556 ?
O2 Fe3 O1 94.76(9) 8_645 . ?
O2 Fe3 O1 171.22(9) 11_556 . ?
O2 Fe3 O1 82.53(8) . . ?
O1 Fe3 O1 93.04(9) 11_556 . ?
O2 Fe3 O1 82.53(8) 8_645 8_645 ?
O2 Fe3 O1 94.76(9) 11_556 8_645 ?
O2 Fe3 O1 171.22(9) . 8_645 ?
O1 Fe3 O1 93.04(9) 11_556 8_645 ?
O1 Fe3 O1 93.04(9) . 8_645 ?
C29 O1 Fe3 113.17(19) . . ?
C30 O2 Fe3 112.99(19) . . ?
O1 C29 C34 124.7(3) . . ?
O1 C29 C30 115.2(3) . . ?
C34 C29 C30 120.1(3) . . ?
O2 C30 C31 123.0(3) . . ?
O2 C30 C29 116.0(3) . . ?
C31 C30 C29 121.0(3) . . ?
C30 C31 C32 121.5(4) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O4 C32 C31 123.7(4) . . ?
O4 C32 C33 118.1(4) . . ?
C31 C32 C33 118.1(4) . . ?
O3 C33 C34 124.0(4) . . ?
O3 C33 C32 118.0(4) . . ?
C34 C33 C32 118.0(4) . . ?
C29 C34 C33 121.3(4) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F1 114(3) . . ?
F2 B1 F4 108(2) . . ?
F1 B1 F4 110(2) . . ?
F2 B1 F3 105.9(17) . . ?
F1 B1 F3 108(2) . . ?
F4 B1 F3 112(2) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.90(3) 2.06(3) 2.917(3) 159(4) 11_556 yes
N4 H4 O2 0.89(3) 2.11(3) 2.972(3) 165(4) . yes

_refine_diff_density_max         0.202
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.026

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-250K
_database_code_depnum_ccdc_archive 'CCDC 2261764'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.6411(3)
_cell_length_b                   21.6411(3)
_cell_length_c                   21.6411(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10135.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    250(2)
_cell_measurement_reflns_used    9459
_cell_measurement_theta_min      2.89
_cell_measurement_theta_max      27.54

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.530
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.660
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      250(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            153634
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_av_R_equivalents  0.0461
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         2.158
_diffrn_reflns_theta_max         27.895
_diffrn_reflns_theta_full        27.850
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             7482
_reflns_number_gt                7152
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.851
_reflns_Friedel_fraction_max     0.996
_reflns_Friedel_fraction_full    0.996

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1801 cubic angstrom  with only 69 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results (before refinement of the BF4 disorder):
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.165 -0.096 -0.086      1801        69 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-250K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1801 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1801 cubic angstrom  with only 69 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.165 -0.096 -0.086      1801        69 ' '
   2  0.106  0.106  0.106        10         1 ' '
   3  0.394  0.894  0.606        10         1 ' '
   4  0.606  0.394  0.894        10         1 ' '
   5  0.894  0.606  0.394        10         1 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0634P)²+0.9131P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3158 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.026(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         7482
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0329
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0931
_refine_ls_wR_factor_gt          0.0918
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54800(2) 0.54800(2) 0.54800(2) 0.04235(14) Uani 1 3 d S T P . .
Fe2 Fe 0.82952(2) 0.82952(2) 0.82952(2) 0.04429(14) Uani 1 3 d S T P . .
N1 N 0.49097(10) 0.58194(10) 0.48376(10) 0.0486(4) Uani 1 1 d . . . . .
N2 N 0.60195(9) 0.61065(10) 0.51121(10) 0.0459(4) Uani 1 1 d . . . . .
N3 N 0.66188(10) 0.62626(10) 0.51537(10) 0.0467(4) Uani 1 1 d . . . . .
H3 H 0.6789(17) 0.6125(17) 0.5512(17) 0.070 Uiso 1 1 d . U . . .
N4 N 0.86524(10) 0.74452(11) 0.72127(10) 0.0478(5) Uani 1 1 d D . . . .
H4 H 0.8325(13) 0.7509(16) 0.7009(15) 0.072 Uiso 1 1 d D U . . .
N5 N 0.86638(10) 0.76209(10) 0.78116(10) 0.0473(4) Uani 1 1 d . . . . .
N6 N 0.88980(11) 0.79553(11) 0.89136(11) 0.0550(5) Uani 1 1 d . . . . .
C1 C 0.43257(12) 0.56535(14) 0.47343(15) 0.0575(6) Uani 1 1 d . . . . .
H1A H 0.414157 0.536092 0.499728 0.069 Uiso 1 1 calc R U . . .
C2 C 0.39791(15) 0.58976(17) 0.42516(18) 0.0726(9) Uani 1 1 d . . . . .
H2A H 0.357261 0.576158 0.418134 0.087 Uiso 1 1 calc R U . . .
C3 C 0.42395(17) 0.63407(18) 0.38787(18) 0.0773(9) Uani 1 1 d . . . . .
H3A H 0.400919 0.651689 0.355527 0.093 Uiso 1 1 calc R U . . .
C4 C 0.48391(16) 0.65251(15) 0.39813(16) 0.0676(8) Uani 1 1 d . . . . .
H4A H 0.502580 0.682669 0.373057 0.081 Uiso 1 1 calc R U . . .
C5 C 0.51619(13) 0.62532(12) 0.44664(13) 0.0515(5) Uani 1 1 d . . . . .
C6 C 0.58023(13) 0.63880(12) 0.46111(12) 0.0506(5) Uani 1 1 d . . . . .
C7 C 0.62601(14) 0.67345(14) 0.43280(12) 0.0563(6) Uani 1 1 d . . . . .
H7A H 0.622352 0.697563 0.396851 0.068 Uiso 1 1 calc R U . . .
C8 C 0.67783(13) 0.66511(13) 0.46836(11) 0.0514(6) Uani 1 1 d . . . . .
C9 C 0.74025(13) 0.69025(13) 0.46078(12) 0.0549(6) Uani 1 1 d . . . . .
C10 C 0.75218(18) 0.7317(2) 0.41321(16) 0.0776(10) Uani 1 1 d . . . . .
H10A H 0.720058 0.743899 0.386639 0.093 Uiso 1 1 calc R U . . .
C11 C 0.8107(2) 0.7549(2) 0.40479(19) 0.1004(15) Uani 1 1 d . . . . .
H11A H 0.818098 0.783945 0.373364 0.120 Uiso 1 1 calc R U . . .
C12 C 0.85843(18) 0.7358(2) 0.44214(17) 0.0927(13) Uani 1 1 d . . . . .
H12A H 0.898718 0.750115 0.434479 0.111 Uiso 1 1 calc R U . . .
C13 C 0.84784(14) 0.69582(17) 0.49084(14) 0.0654(8) Uani 1 1 d . . . . .
C14 C 0.78809(13) 0.67295(14) 0.49946(12) 0.0561(6) Uani 1 1 d . . . . .
H14A H 0.780281 0.645344 0.532073 0.067 Uiso 1 1 calc R U . . .
C15 C 0.89580(13) 0.68156(17) 0.53724(14) 0.0651(8) Uani 1 1 d . . . . .
C16 C 0.95339(17) 0.6581(2) 0.52219(18) 0.0927(13) Uani 1 1 d . . . . .
H16A H 0.963041 0.649109 0.480798 0.111 Uiso 1 1 calc R U . . .
C17 C 0.99601(18) 0.6480(3) 0.5673(2) 0.1028(15) Uani 1 1 d . . . . .
H17A H 1.034958 0.632023 0.556530 0.123 Uiso 1 1 calc R U . . .
C18 C 0.98324(16) 0.6606(2) 0.62879(18) 0.0852(11) Uani 1 1 d . . . . .
H18A H 1.012728 0.652255 0.659569 0.102 Uiso 1 1 calc R U . . .
C19 C 0.92568(13) 0.68615(15) 0.64449(14) 0.0585(7) Uani 1 1 d . . . . .
C20 C 0.88283(12) 0.69478(14) 0.59879(13) 0.0576(6) Uani 1 1 d . . . . .
H20A H 0.843546 0.710058 0.609288 0.069 Uiso 1 1 calc R U . . .
C21 C 0.91418(12) 0.70781(13) 0.70796(13) 0.0519(6) Uani 1 1 d . . . . .
C22 C 0.94849(13) 0.70228(14) 0.76136(14) 0.0572(6) Uani 1 1 d . . . . .
H22A H 0.985248 0.679801 0.766897 0.069 Uiso 1 1 calc R U . . .
C23 C 0.91735(12) 0.73674(12) 0.80480(13) 0.0515(6) Uani 1 1 d . . . . .
C24 C 0.92964(14) 0.75309(14) 0.86898(13) 0.0569(6) Uani 1 1 d . . . . .
C25 C 0.97707(18) 0.72872(18) 0.90319(17) 0.0766(9) Uani 1 1 d . . . . .
H25A H 1.004549 0.699967 0.885727 0.092 Uiso 1 1 calc R U . . .
C26 C 0.9836(2) 0.7473(2) 0.96376(18) 0.0916(12) Uani 1 1 d . . . . .
H26A H 1.015524 0.731115 0.988306 0.110 Uiso 1 1 calc R U . . .
C27 C 0.9436(2) 0.7891(2) 0.98765(18) 0.0922(12) Uani 1 1 d . . . . .
H27A H 0.947312 0.801951 1.028979 0.111 Uiso 1 1 calc R U . . .
C28 C 0.89723(17) 0.81264(17) 0.95056(15) 0.0713(8) Uani 1 1 d . . . . .
H28A H 0.869797 0.841791 0.967439 0.086 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68727(2) 0.68727(2) 0.68727(2) 0.05041(16) Uani 1 3 d S T P . .
O1 O 0.72031(8) 0.61884(8) 0.63455(8) 0.0473(4) Uani 1 1 d . . . . .
O2 O 0.75092(9) 0.65652(8) 0.74596(8) 0.0501(4) Uani 1 1 d . . . . .
O3 O 0.86987(16) 0.46261(18) 0.64673(14) 0.1198(14) Uani 1 1 d . . . . .
O4 O 0.89531(16) 0.4979(2) 0.76331(15) 0.1283(16) Uani 1 1 d . . . . .
C29 C 0.76542(12) 0.58856(13) 0.66054(12) 0.0489(5) Uani 1 1 d . . . . .
C30 C 0.78135(12) 0.60926(13) 0.72490(12) 0.0504(5) Uani 1 1 d . . . . .
C31 C 0.82467(15) 0.57883(17) 0.75872(14) 0.0678(8) Uani 1 1 d . . . . .
H31A H 0.833095 0.592174 0.799191 0.081 Uiso 1 1 calc R U . . .
C32 C 0.85731(16) 0.5278(2) 0.73472(16) 0.0807(11) Uani 1 1 d . . . . .
C33 C 0.84188(16) 0.50696(19) 0.66721(16) 0.0756(9) Uani 1 1 d . . . . .
C34 C 0.79577(13) 0.54112(15) 0.63401(13) 0.0604(7) Uani 1 1 d . . . . .
H34A H 0.786573 0.530207 0.592992 0.072 Uiso 1 1 calc R U . . .
B1 B 0.3930(8) 0.3930(9) 0.3943(11) 0.084(2) Uani 0.3333 1 d D U P A -1
F1 F 0.3853(12) 0.3414(11) 0.4297(15) 0.111(5) Uani 0.3333 1 d D U P A -1
F2 F 0.4093(7) 0.4416(11) 0.4308(16) 0.159(7) Uani 0.3333 1 d D U P A -1
F3 F 0.4388(11) 0.3897(15) 0.3514(10) 0.136(8) Uani 0.3333 1 d D U P A -1
F4 F 0.3373(8) 0.4096(12) 0.3701(10) 0.134(7) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.958(2) . ?
Fe1 N2 1.958(2) 9 ?
Fe1 N2 1.958(2) 5 ?
Fe1 N1 1.999(2) . ?
Fe1 N1 1.999(2) 9 ?
Fe1 N1 1.999(2) 5 ?
Fe2 N5 1.965(2) . ?
Fe2 N5 1.965(2) 9 ?
Fe2 N5 1.965(2) 5 ?
Fe2 N6 2.008(2) 5 ?
Fe2 N6 2.008(2) 9 ?
Fe2 N6 2.009(2) . ?
N1 C1 1.333(4) . ?
N1 C5 1.351(4) . ?
N2 C6 1.330(3) . ?
N2 N3 1.343(3) . ?
N3 C8 1.364(3) . ?
N3 H3 0.91(4) . ?
N4 N5 1.351(3) . ?
N4 C21 1.355(3) . ?
N4 H4 0.85(2) . ?
N5 C23 1.334(3) . ?
N6 C28 1.343(4) . ?
N6 C24 1.350(4) . ?
C1 C2 1.390(4) . ?
C1 H1A 0.9400 . ?
C2 C3 1.374(5) . ?
C2 H2A 0.9400 . ?
C3 C4 1.376(5) . ?
C3 H3A 0.9400 . ?
C4 C5 1.391(4) . ?
C4 H4A 0.9400 . ?
C5 C6 1.451(4) . ?
C6 C7 1.385(4) . ?
C7 C8 1.372(4) . ?
C7 H7A 0.9400 . ?
C8 C9 1.465(4) . ?
C9 C14 1.383(4) . ?
C9 C10 1.390(4) . ?
C10 C11 1.374(5) . ?
C10 H10A 0.9400 . ?
C11 C12 1.375(6) . ?
C11 H11A 0.9400 . ?
C12 C13 1.383(5) . ?
C12 H12A 0.9400 . ?
C13 C14 1.397(4) . ?
C13 C15 1.477(5) . ?
C14 H14A 0.9400 . ?
C15 C16 1.385(4) . ?
C15 C20 1.391(4) . ?
C16 C17 1.361(6) . ?
C16 H16A 0.9400 . ?
C17 C18 1.387(5) . ?
C17 H17A 0.9400 . ?
C18 C19 1.404(4) . ?
C18 H18A 0.9400 . ?
C19 C20 1.369(4) . ?
C19 C21 1.472(4) . ?
C20 H20A 0.9400 . ?
C21 C22 1.379(4) . ?
C22 C23 1.376(4) . ?
C22 H22A 0.9400 . ?
C23 C24 1.458(4) . ?
C24 C25 1.371(4) . ?
C25 C26 1.378(5) . ?
C25 H25A 0.9400 . ?
C26 C27 1.354(6) . ?
C26 H26A 0.9400 . ?
C27 C28 1.382(5) . ?
C27 H27A 0.9400 . ?
C28 H28A 0.9400 . ?
Fe3 O2 1.9883(18) 5 ?
Fe3 O2 1.9883(18) . ?
Fe3 O2 1.9883(18) 9 ?
Fe3 O1 2.0015(17) 9 ?
Fe3 O1 2.0015(17) 5 ?
Fe3 O1 2.0016(17) . ?
O1 C29 1.303(3) . ?
O2 C30 1.299(3) . ?
O3 C33 1.218(4) . ?
O4 C32 1.216(4) . ?
C29 C34 1.347(4) . ?
C29 C30 1.503(4) . ?
C30 C31 1.360(4) . ?
C31 C32 1.410(5) . ?
C31 H31A 0.9400 . ?
C32 C33 1.565(5) . ?
C33 C34 1.435(4) . ?
C34 H34A 0.9400 . ?
B1 F3 1.359(14) . ?
B1 F4 1.362(14) . ?
B1 F2 1.363(12) . ?
B1 F1 1.364(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.39(8) . 9 ?
N2 Fe1 N2 96.38(8) . 5 ?
N2 Fe1 N2 96.39(8) 9 5 ?
N2 Fe1 N1 80.27(9) . . ?
N2 Fe1 N1 172.52(9) 9 . ?
N2 Fe1 N1 90.65(9) 5 . ?
N2 Fe1 N1 90.65(9) . 9 ?
N2 Fe1 N1 80.27(9) 9 9 ?
N2 Fe1 N1 172.52(9) 5 9 ?
N1 Fe1 N1 93.03(9) . 9 ?
N2 Fe1 N1 172.52(9) . 5 ?
N2 Fe1 N1 90.65(9) 9 5 ?
N2 Fe1 N1 80.27(9) 5 5 ?
N1 Fe1 N1 93.03(9) . 5 ?
N1 Fe1 N1 93.03(9) 9 5 ?
N5 Fe2 N5 97.02(8) . 9 ?
N5 Fe2 N5 97.02(8) . 5 ?
N5 Fe2 N5 97.02(8) 9 5 ?
N5 Fe2 N6 90.97(9) . 5 ?
N5 Fe2 N6 171.67(9) 9 5 ?
N5 Fe2 N6 79.58(9) 5 5 ?
N5 Fe2 N6 171.67(9) . 9 ?
N5 Fe2 N6 79.58(9) 9 9 ?
N5 Fe2 N6 90.97(9) 5 9 ?
N6 Fe2 N6 92.81(10) 5 9 ?
N5 Fe2 N6 79.58(9) . . ?
N5 Fe2 N6 90.97(9) 9 . ?
N5 Fe2 N6 171.67(9) 5 . ?
N6 Fe2 N6 92.81(10) 5 . ?
N6 Fe2 N6 92.81(10) 9 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.1(2) . . ?
C5 N1 Fe1 114.81(18) . . ?
C6 N2 N3 106.3(2) . . ?
C6 N2 Fe1 115.98(18) . . ?
N3 N2 Fe1 136.26(17) . . ?
N2 N3 C8 110.4(2) . . ?
N2 N3 H3 112(2) . . ?
C8 N3 H3 137(2) . . ?
N5 N4 C21 110.8(2) . . ?
N5 N4 H4 118(3) . . ?
C21 N4 H4 130(3) . . ?
C23 N5 N4 105.5(2) . . ?
C23 N5 Fe2 115.90(18) . . ?
N4 N5 Fe2 135.44(17) . . ?
C28 N6 C24 117.0(3) . . ?
C28 N6 Fe2 127.8(2) . . ?
C24 N6 Fe2 115.15(19) . . ?
N1 C1 C2 122.4(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 119.0(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C2 C3 C4 119.6(3) . . ?
C2 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 118.2(3) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.7(3) . . ?
N1 C5 C6 113.4(2) . . ?
C4 C5 C6 123.9(3) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 114.9(2) . . ?
C7 C6 C5 134.2(2) . . ?
C8 C7 C6 105.4(2) . . ?
C8 C7 H7A 127.3 . . ?
C6 C7 H7A 127.3 . . ?
N3 C8 C7 107.0(2) . . ?
N3 C8 C9 123.1(2) . . ?
C7 C8 C9 129.9(2) . . ?
C14 C9 C10 118.9(3) . . ?
C14 C9 C8 121.5(2) . . ?
C10 C9 C8 119.6(3) . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10A 119.8 . . ?
C9 C10 H10A 119.8 . . ?
C10 C11 C12 120.3(4) . . ?
C10 C11 H11A 119.9 . . ?
C12 C11 H11A 119.9 . . ?
C11 C12 C13 120.8(3) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C12 C13 C14 118.5(3) . . ?
C12 C13 C15 122.2(3) . . ?
C14 C13 C15 119.1(3) . . ?
C9 C14 C13 121.1(3) . . ?
C9 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C16 C15 C20 118.8(3) . . ?
C16 C15 C13 123.3(3) . . ?
C20 C15 C13 117.8(3) . . ?
C17 C16 C15 120.0(3) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 121.4(3) . . ?
C16 C17 H17A 119.3 . . ?
C18 C17 H17A 119.3 . . ?
C17 C18 C19 119.1(4) . . ?
C17 C18 H18A 120.4 . . ?
C19 C18 H18A 120.4 . . ?
C20 C19 C18 118.7(3) . . ?
C20 C19 C21 121.1(2) . . ?
C18 C19 C21 120.1(3) . . ?
C19 C20 C15 121.8(3) . . ?
C19 C20 H20A 119.1 . . ?
C15 C20 H20A 119.1 . . ?
N4 C21 C22 107.1(2) . . ?
N4 C21 C19 121.1(3) . . ?
C22 C21 C19 131.5(3) . . ?
C23 C22 C21 105.2(2) . . ?
C23 C22 H22A 127.4 . . ?
C21 C22 H22A 127.4 . . ?
N5 C23 C22 111.5(2) . . ?
N5 C23 C24 114.6(2) . . ?
C22 C23 C24 133.9(3) . . ?
N6 C24 C25 123.1(3) . . ?
N6 C24 C23 113.0(2) . . ?
C25 C24 C23 123.9(3) . . ?
C24 C25 C26 118.5(3) . . ?
C24 C25 H25A 120.7 . . ?
C26 C25 H25A 120.7 . . ?
C27 C26 C25 119.5(3) . . ?
C27 C26 H26A 120.2 . . ?
C25 C26 H26A 120.2 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.6(3) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 90.18(8) 5 . ?
O2 Fe3 O2 90.18(8) 5 9 ?
O2 Fe3 O2 90.18(8) . 9 ?
O2 Fe3 O1 170.79(7) 5 9 ?
O2 Fe3 O1 95.37(7) . 9 ?
O2 Fe3 O1 82.47(7) 9 9 ?
O2 Fe3 O1 82.48(7) 5 5 ?
O2 Fe3 O1 170.79(7) . 5 ?
O2 Fe3 O1 95.37(7) 9 5 ?
O1 Fe3 O1 92.65(7) 9 5 ?
O2 Fe3 O1 95.37(7) 5 . ?
O2 Fe3 O1 82.48(7) . . ?
O2 Fe3 O1 170.79(7) 9 . ?
O1 Fe3 O1 92.65(7) 9 . ?
O1 Fe3 O1 92.65(7) 5 . ?
C29 O1 Fe3 113.17(16) . . ?
C30 O2 Fe3 112.98(16) . . ?
O1 C29 C34 124.4(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.7(2) . . ?
O2 C30 C31 122.8(2) . . ?
O2 C30 C29 116.3(2) . . ?
C31 C30 C29 120.8(2) . . ?
C30 C31 C32 121.8(3) . . ?
C30 C31 H31A 119.1 . . ?
C32 C31 H31A 119.1 . . ?
O4 C32 C31 124.6(3) . . ?
O4 C32 C33 117.8(3) . . ?
C31 C32 C33 117.5(3) . . ?
O3 C33 C34 124.7(3) . . ?
O3 C33 C32 117.4(3) . . ?
C34 C33 C32 117.9(3) . . ?
C29 C34 C33 121.2(3) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F3 B1 F4 113(2) . . ?
F3 B1 F2 104.2(16) . . ?
F4 B1 F2 104.4(14) . . ?
F3 B1 F1 116(2) . . ?
F4 B1 F1 108.9(17) . . ?
F2 B1 F1 109.7(19) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.91(4) 2.02(4) 2.877(3) 157(3) . yes
N4 H4 O2 0.85(2) 2.11(2) 2.940(3) 170(3) 5 yes

_refine_diff_density_max         0.363
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.042

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-190K
_database_code_depnum_ccdc_archive 'CCDC 2261765'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.5786(3)
_cell_length_b                   21.5786(3)
_cell_length_c                   21.5786(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10047.8(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    190(2)
_cell_measurement_reflns_used    9485
_cell_measurement_theta_min      3.06
_cell_measurement_theta_max      28.84

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.535
_shelx_estimated_absorpt_T_min   0.939
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.665
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      190(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            165609
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_av_R_equivalents  0.0615
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         2.164
_diffrn_reflns_theta_max         29.092
_diffrn_reflns_theta_full        29.069
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8353
_reflns_number_gt                7916
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.857
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1685 cubic angstrom  with only 165 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results before refinement of the BF4 disorder:
# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.155 -0.095 -0.085      1778       126 ' '
   2  0.106  0.106  0.106        10         0 ' '
   3  0.394  0.894  0.606        10         0 ' '
   4  0.606  0.394  0.894        10         0 ' '
   5  0.894  0.606  0.394        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_vrf_PLAT601_lb2205-190K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1778 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1778 cubic angstrom  with only 126 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.155 -0.095 -0.085      1778       126 ' '
   2  0.106  0.106  0.106        10         0 ' '
   3  0.394  0.894  0.606        10         0 ' '
   4  0.606  0.394  0.894        10         0 ' '
   5  0.894  0.606  0.394        10         0 ' '
_platon_squeeze_void_probe_radius                  1.20
_platon_squeeze_details                           ?

;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0646P)²+1.1379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3495 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(2)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8353
_refine_ls_number_parameters     445
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0351
_refine_ls_R_factor_gt           0.0333
_refine_ls_wR_factor_ref         0.0963
_refine_ls_wR_factor_gt          0.0946
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.072
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.54790(2) 0.54790(2) 0.54790(2) 0.03388(12) Uani 1 3 d S T P . .
Fe2 Fe 0.83034(2) 0.83034(2) 0.83034(2) 0.03595(13) Uani 1 3 d S T P . .
N1 N 0.49073(9) 0.58180(9) 0.48331(9) 0.0387(4) Uani 1 1 d . . . . .
N2 N 0.60226(9) 0.61060(9) 0.51098(9) 0.0371(4) Uani 1 1 d . . . . .
N3 N 0.66229(9) 0.62633(9) 0.51540(9) 0.0374(4) Uani 1 1 d . . . . .
H3 H 0.6798(16) 0.6152(16) 0.5512(17) 0.056 Uiso 1 1 d . U . . .
N4 N 0.86589(9) 0.74515(10) 0.72214(9) 0.0383(4) Uani 1 1 d D . . . .
H4 H 0.8310(12) 0.7498(16) 0.7043(15) 0.057 Uiso 1 1 d D U . . .
N5 N 0.86715(9) 0.76303(9) 0.78197(9) 0.0382(4) Uani 1 1 d . . . . .
N6 N 0.89015(10) 0.79660(10) 0.89260(10) 0.0437(4) Uani 1 1 d . . . . .
C1 C 0.43231(12) 0.56495(13) 0.47257(13) 0.0464(5) Uani 1 1 d . . . . .
H1A H 0.413533 0.535426 0.499294 0.056 Uiso 1 1 calc R U . . .
C2 C 0.39781(13) 0.58891(15) 0.42377(16) 0.0573(7) Uani 1 1 d . . . . .
H2A H 0.356676 0.575003 0.416501 0.069 Uiso 1 1 calc R U . . .
C3 C 0.42437(15) 0.63339(16) 0.38591(16) 0.0601(7) Uani 1 1 d . . . . .
H3A H 0.401402 0.650814 0.352637 0.072 Uiso 1 1 calc R U . . .
C4 C 0.48450(14) 0.65220(14) 0.39693(14) 0.0533(6) Uani 1 1 d . . . . .
H4A H 0.503551 0.682887 0.371765 0.064 Uiso 1 1 calc R U . . .
C5 C 0.51641(12) 0.62507(11) 0.44579(12) 0.0409(5) Uani 1 1 d . . . . .
C6 C 0.58053(12) 0.63862(11) 0.46052(11) 0.0404(5) Uani 1 1 d . . . . .
C7 C 0.62681(12) 0.67335(12) 0.43225(12) 0.0448(5) Uani 1 1 d . . . . .
H7A H 0.623324 0.697651 0.395706 0.054 Uiso 1 1 calc R U . . .
C8 C 0.67855(12) 0.66519(12) 0.46819(10) 0.0410(5) Uani 1 1 d . . . . .
C9 C 0.74102(12) 0.69020(12) 0.46064(11) 0.0441(5) Uani 1 1 d . . . . .
C10 C 0.75291(16) 0.73220(16) 0.41284(14) 0.0593(7) Uani 1 1 d . . . . .
H10A H 0.720327 0.745416 0.386349 0.071 Uiso 1 1 calc R U . . .
C11 C 0.81231(18) 0.7544(2) 0.40436(17) 0.0768(11) Uani 1 1 d . . . . .
H11A H 0.820321 0.782821 0.371734 0.092 Uiso 1 1 calc R U . . .
C12 C 0.85980(16) 0.7361(2) 0.44208(16) 0.0710(10) Uani 1 1 d . . . . .
H12A H 0.900530 0.751154 0.434848 0.085 Uiso 1 1 calc R U . . .
C13 C 0.84884(12) 0.69566(15) 0.49089(13) 0.0517(6) Uani 1 1 d . . . . .
C14 C 0.78905(12) 0.67266(13) 0.49967(11) 0.0452(5) Uani 1 1 d . . . . .
H14A H 0.781128 0.644686 0.532727 0.054 Uiso 1 1 calc R U . . .
C15 C 0.89702(12) 0.68167(15) 0.53760(12) 0.0518(6) Uani 1 1 d . . . . .
C16 C 0.95497(15) 0.6585(2) 0.52258(16) 0.0736(10) Uani 1 1 d . . . . .
H16A H 0.965008 0.649958 0.480583 0.088 Uiso 1 1 calc R U . . .
C17 C 0.99788(16) 0.6480(2) 0.56825(19) 0.0822(12) Uani 1 1 d . . . . .
H17A H 1.037233 0.631367 0.557650 0.099 Uiso 1 1 calc R U . . .
C18 C 0.98462(14) 0.6614(2) 0.62973(16) 0.0670(9) Uani 1 1 d . . . . .
H18A H 1.014613 0.653682 0.661019 0.080 Uiso 1 1 calc R U . . .
C19 C 0.92676(12) 0.68625(14) 0.64540(13) 0.0476(6) Uani 1 1 d . . . . .
C20 C 0.88349(12) 0.69468(13) 0.59945(12) 0.0460(5) Uani 1 1 d . . . . .
H20A H 0.843484 0.709696 0.610037 0.055 Uiso 1 1 calc R U . . .
C21 C 0.91490(11) 0.70778(12) 0.70881(12) 0.0420(5) Uani 1 1 d . . . . .
C22 C 0.94928(12) 0.70229(12) 0.76249(13) 0.0458(5) Uani 1 1 d . . . . .
H22A H 0.986407 0.679321 0.768188 0.055 Uiso 1 1 calc R U . . .
C23 C 0.91812(11) 0.73740(11) 0.80626(12) 0.0413(5) Uani 1 1 d . . . . .
C24 C 0.93030(12) 0.75371(13) 0.87030(12) 0.0458(5) Uani 1 1 d . . . . .
C25 C 0.97767(16) 0.72908(16) 0.90500(15) 0.0603(7) Uani 1 1 d . . . . .
H25A H 1.005330 0.699639 0.887505 0.072 Uiso 1 1 calc R U . . .
C26 C 0.98432(19) 0.74796(18) 0.96586(17) 0.0726(10) Uani 1 1 d . . . . .
H26A H 1.016911 0.731966 0.990763 0.087 Uiso 1 1 calc R U . . .
C27 C 0.94328(18) 0.79000(19) 0.98972(16) 0.0715(9) Uani 1 1 d . . . . .
H27A H 0.946475 0.802774 1.031724 0.086 Uiso 1 1 calc R U . . .
C28 C 0.89705(15) 0.81375(15) 0.95207(13) 0.0550(6) Uani 1 1 d . . . . .
H28A H 0.869138 0.843315 0.968946 0.066 Uiso 1 1 calc R U . . .
Fe3 Fe 0.68800(2) 0.68800(2) 0.68800(2) 0.04238(14) Uani 1 3 d S T P . .
O1 O 0.72097(8) 0.61935(8) 0.63509(7) 0.0385(3) Uani 1 1 d . . . . .
O2 O 0.75178(8) 0.65704(8) 0.74677(8) 0.0416(4) Uani 1 1 d . . . . .
O3 O 0.86755(14) 0.45915(15) 0.64863(12) 0.0908(10) Uani 1 1 d . . . . .
O4 O 0.89281(14) 0.49431(16) 0.76623(13) 0.0923(10) Uani 1 1 d . . . . .
C29 C 0.76554(11) 0.58827(12) 0.66138(11) 0.0403(5) Uani 1 1 d . . . . .
C30 C 0.78162(11) 0.60884(12) 0.72622(11) 0.0417(5) Uani 1 1 d . . . . .
C31 C 0.82401(14) 0.57763(15) 0.76054(13) 0.0544(7) Uani 1 1 d . . . . .
H31A H 0.832780 0.591300 0.801457 0.065 Uiso 1 1 calc R U . . .
C32 C 0.85555(14) 0.52510(18) 0.73686(14) 0.0617(8) Uani 1 1 d . . . . .
C33 C 0.84053(14) 0.50474(17) 0.66888(14) 0.0593(7) Uani 1 1 d . . . . .
C34 C 0.79528(12) 0.54002(14) 0.63520(12) 0.0485(6) Uani 1 1 d . . . . .
H34A H 0.786116 0.529099 0.593543 0.058 Uiso 1 1 calc R U . . .
B1 B 0.39308(19) 0.39308(19) 0.39308(19) 0.0627(12) Uani 1 3 d DS TU P . 1
F1 F 0.3928(9) 0.3427(10) 0.4336(12) 0.100(4) Uani 0.3333 1 d D U P . 1
F2 F 0.42921(17) 0.42921(17) 0.42921(17) 0.175(3) Uani 1 3 d DS TU P . 1
F3 F 0.4336(13) 0.3767(14) 0.3462(9) 0.098(4) Uani 0.3333 1 d D U P . 1
F4 F 0.3388(6) 0.4123(7) 0.3745(13) 0.094(4) Uani 0.3333 1 d D U P . 1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9598(19) . ?
Fe1 N2 1.9599(19) 9 ?
Fe1 N2 1.9599(19) 5 ?
Fe1 N1 2.000(2) . ?
Fe1 N1 2.000(2) 5 ?
Fe1 N1 2.000(2) 9 ?
Fe2 N5 1.957(2) . ?
Fe2 N5 1.957(2) 9 ?
Fe2 N5 1.957(2) 5 ?
Fe2 N6 2.000(2) 9 ?
Fe2 N6 2.000(2) 5 ?
Fe2 N6 2.000(2) . ?
N1 C1 1.332(3) . ?
N1 C5 1.354(3) . ?
N2 C6 1.331(3) . ?
N2 N3 1.342(3) . ?
N3 C8 1.365(3) . ?
N3 H3 0.89(4) . ?
N4 N5 1.348(3) . ?
N4 C21 1.361(3) . ?
N4 H4 0.85(2) . ?
N5 C23 1.338(3) . ?
N6 C28 1.344(4) . ?
N6 C24 1.356(4) . ?
C1 C2 1.389(4) . ?
C1 H1A 0.9500 . ?
C2 C3 1.385(5) . ?
C2 H2A 0.9500 . ?
C3 C4 1.380(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.389(4) . ?
C4 H4A 0.9500 . ?
C5 C6 1.449(4) . ?
C6 C7 1.390(4) . ?
C7 C8 1.371(4) . ?
C7 H7A 0.9500 . ?
C8 C9 1.461(3) . ?
C9 C14 1.388(4) . ?
C9 C10 1.397(4) . ?
C10 C11 1.380(5) . ?
C10 H10A 0.9500 . ?
C11 C12 1.367(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.388(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.395(4) . ?
C13 C15 1.479(4) . ?
C14 H14A 0.9500 . ?
C15 C16 1.385(4) . ?
C15 C20 1.395(4) . ?
C16 C17 1.371(6) . ?
C16 H16A 0.9500 . ?
C17 C18 1.387(5) . ?
C17 H17A 0.9500 . ?
C18 C19 1.400(4) . ?
C18 H18A 0.9500 . ?
C19 C20 1.374(4) . ?
C19 C21 1.467(4) . ?
C20 H20A 0.9500 . ?
C21 C22 1.381(4) . ?
C22 C23 1.385(4) . ?
C22 H22A 0.9500 . ?
C23 C24 1.450(4) . ?
C24 C25 1.374(4) . ?
C25 C26 1.382(5) . ?
C25 H25A 0.9500 . ?
C26 C27 1.368(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.385(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.9871(17) 9 ?
Fe3 O2 1.9871(17) 5 ?
Fe3 O2 1.9871(17) . ?
Fe3 O1 2.0013(17) . ?
Fe3 O1 2.0014(17) 5 ?
Fe3 O1 2.0014(17) 9 ?
O1 C29 1.302(3) . ?
O2 C30 1.301(3) . ?
O3 C33 1.224(4) . ?
O4 C32 1.220(4) . ?
C29 C34 1.347(4) . ?
C29 C30 1.508(3) . ?
C30 C31 1.356(4) . ?
C31 C32 1.417(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.565(4) . ?
C33 C34 1.436(4) . ?
C34 H34A 0.9500 . ?
B1 F4 1.305(10) . ?
B1 F4 1.305(10) 9 ?
B1 F4 1.305(10) 5 ?
B1 F2 1.350(9) . ?
B1 F3 1.384(12) 9 ?
B1 F3 1.384(12) 5 ?
B1 F3 1.384(12) . ?
B1 F1 1.394(11) . ?
B1 F1 1.394(11) 5 ?
B1 F1 1.394(11) 9 ?
F1 F3 0.36(4) 9 ?
F1 F4 0.61(3) 5 ?
F3 F4 0.49(4) 9 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.36(8) . 9 ?
N2 Fe1 N2 96.36(8) . 5 ?
N2 Fe1 N2 96.36(8) 9 5 ?
N2 Fe1 N1 80.41(8) . . ?
N2 Fe1 N1 172.58(8) 9 . ?
N2 Fe1 N1 90.65(8) 5 . ?
N2 Fe1 N1 172.58(8) . 5 ?
N2 Fe1 N1 90.65(8) 9 5 ?
N2 Fe1 N1 80.41(8) 5 5 ?
N1 Fe1 N1 92.90(8) . 5 ?
N2 Fe1 N1 90.65(8) . 9 ?
N2 Fe1 N1 80.41(8) 9 9 ?
N2 Fe1 N1 172.58(8) 5 9 ?
N1 Fe1 N1 92.90(8) . 9 ?
N1 Fe1 N1 92.90(8) 5 9 ?
N5 Fe2 N5 97.00(8) . 9 ?
N5 Fe2 N5 97.00(8) . 5 ?
N5 Fe2 N5 97.00(8) 9 5 ?
N5 Fe2 N6 172.05(9) . 9 ?
N5 Fe2 N6 79.99(9) 9 9 ?
N5 Fe2 N6 90.69(9) 5 9 ?
N5 Fe2 N6 90.69(9) . 5 ?
N5 Fe2 N6 172.05(9) 9 5 ?
N5 Fe2 N6 79.99(9) 5 5 ?
N6 Fe2 N6 92.63(9) 9 5 ?
N5 Fe2 N6 79.99(9) . . ?
N5 Fe2 N6 90.69(9) 9 . ?
N5 Fe2 N6 172.05(9) 5 . ?
N6 Fe2 N6 92.64(9) 9 . ?
N6 Fe2 N6 92.63(9) 5 . ?
C1 N1 C5 118.1(2) . . ?
C1 N1 Fe1 127.23(18) . . ?
C5 N1 Fe1 114.60(16) . . ?
C6 N2 N3 106.45(19) . . ?
C6 N2 Fe1 115.81(17) . . ?
N3 N2 Fe1 136.32(16) . . ?
N2 N3 C8 110.5(2) . . ?
N2 N3 H3 114(2) . . ?
C8 N3 H3 135(2) . . ?
N5 N4 C21 110.9(2) . . ?
N5 N4 H4 115(2) . . ?
C21 N4 H4 131(2) . . ?
C23 N5 N4 105.9(2) . . ?
C23 N5 Fe2 115.57(17) . . ?
N4 N5 Fe2 135.66(16) . . ?
C28 N6 C24 117.1(2) . . ?
C28 N6 Fe2 127.8(2) . . ?
C24 N6 Fe2 114.99(18) . . ?
N1 C1 C2 122.5(3) . . ?
N1 C1 H1A 118.8 . . ?
C2 C1 H1A 118.8 . . ?
C3 C2 C1 118.9(3) . . ?
C3 C2 H2A 120.5 . . ?
C1 C2 H2A 120.5 . . ?
C4 C3 C2 119.4(3) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 118.2(3) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.8(2) . . ?
N1 C5 C6 113.5(2) . . ?
C4 C5 C6 123.7(2) . . ?
N2 C6 C7 110.5(2) . . ?
N2 C6 C5 115.1(2) . . ?
C7 C6 C5 134.3(2) . . ?
C8 C7 C6 105.5(2) . . ?
C8 C7 H7A 127.2 . . ?
C6 C7 H7A 127.2 . . ?
N3 C8 C7 107.0(2) . . ?
N3 C8 C9 123.2(2) . . ?
C7 C8 C9 129.9(2) . . ?
C14 C9 C10 119.2(3) . . ?
C14 C9 C8 121.4(2) . . ?
C10 C9 C8 119.4(3) . . ?
C11 C10 C9 119.6(3) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 121.1(3) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C11 C12 C13 120.4(3) . . ?
C11 C12 H12A 119.8 . . ?
C13 C12 H12A 119.8 . . ?
C12 C13 C14 119.0(3) . . ?
C12 C13 C15 121.7(3) . . ?
C14 C13 C15 119.0(3) . . ?
C9 C14 C13 120.7(3) . . ?
C9 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C16 C15 C20 119.0(3) . . ?
C16 C15 C13 123.3(3) . . ?
C20 C15 C13 117.6(2) . . ?
C17 C16 C15 120.1(3) . . ?
C17 C16 H16A 120.0 . . ?
C15 C16 H16A 120.0 . . ?
C16 C17 C18 120.9(3) . . ?
C16 C17 H17A 119.6 . . ?
C18 C17 H17A 119.6 . . ?
C17 C18 C19 119.6(3) . . ?
C17 C18 H18A 120.2 . . ?
C19 C18 H18A 120.2 . . ?
C20 C19 C18 118.8(3) . . ?
C20 C19 C21 120.8(2) . . ?
C18 C19 C21 120.1(3) . . ?
C19 C20 C15 121.4(2) . . ?
C19 C20 H20A 119.3 . . ?
C15 C20 H20A 119.3 . . ?
N4 C21 C22 106.9(2) . . ?
N4 C21 C19 121.3(2) . . ?
C22 C21 C19 131.4(2) . . ?
C21 C22 C23 105.3(2) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 111.0(2) . . ?
N5 C23 C24 115.0(2) . . ?
C22 C23 C24 134.0(2) . . ?
N6 C24 C25 123.1(3) . . ?
N6 C24 C23 112.8(2) . . ?
C25 C24 C23 124.1(3) . . ?
C24 C25 C26 118.7(3) . . ?
C24 C25 H25A 120.6 . . ?
C26 C25 H25A 120.6 . . ?
C27 C26 C25 119.1(3) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
C26 C27 C28 119.4(3) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
N6 C28 C27 122.6(3) . . ?
N6 C28 H28A 118.7 . . ?
C27 C28 H28A 118.7 . . ?
O2 Fe3 O2 90.31(7) 9 5 ?
O2 Fe3 O2 90.31(7) 9 . ?
O2 Fe3 O2 90.31(7) 5 . ?
O2 Fe3 O1 170.81(7) 9 . ?
O2 Fe3 O1 95.39(7) 5 . ?
O2 Fe3 O1 82.47(6) . . ?
O2 Fe3 O1 95.39(7) 9 5 ?
O2 Fe3 O1 82.47(6) 5 5 ?
O2 Fe3 O1 170.81(7) . 5 ?
O1 Fe3 O1 92.50(7) . 5 ?
O2 Fe3 O1 82.48(7) 9 9 ?
O2 Fe3 O1 170.81(7) 5 9 ?
O2 Fe3 O1 95.39(7) . 9 ?
O1 Fe3 O1 92.50(7) . 9 ?
O1 Fe3 O1 92.50(7) 5 9 ?
C29 O1 Fe3 113.27(15) . . ?
C30 O2 Fe3 113.21(15) . . ?
O1 C29 C34 124.5(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.4(2) . . ?
O2 C30 C31 123.0(2) . . ?
O2 C30 C29 115.9(2) . . ?
C31 C30 C29 121.0(2) . . ?
C30 C31 C32 121.6(3) . . ?
C30 C31 H31A 119.2 . . ?
C32 C31 H31A 119.2 . . ?
O4 C32 C31 124.4(3) . . ?
O4 C32 C33 118.0(3) . . ?
C31 C32 C33 117.6(3) . . ?
O3 C33 C34 124.7(3) . . ?
O3 C33 C32 117.5(3) . . ?
C34 C33 C32 117.8(3) . . ?
C29 C34 C33 121.4(2) . . ?
C29 C34 H34A 119.3 . . ?
C33 C34 H34A 119.3 . . ?
F4 B1 F4 96.2(12) . 9 ?
F4 B1 F4 96.2(12) . 5 ?
F4 B1 F4 96.2(12) 9 5 ?
F4 B1 F2 120.8(9) . . ?
F4 B1 F2 120.8(9) 9 . ?
F4 B1 F2 120.8(9) 5 . ?
F4 B1 F3 101(2) . 9 ?
F4 B1 F3 115.1(16) 9 9 ?
F4 B1 F3 20.7(16) 5 9 ?
F2 B1 F3 101.8(15) . 9 ?
F4 B1 F3 20.7(16) . 5 ?
F4 B1 F3 101(2) 9 5 ?
F4 B1 F3 115.1(16) 5 5 ?
F2 B1 F3 101.8(15) . 5 ?
F3 B1 F3 115.9(10) 9 5 ?
F4 B1 F3 115.1(16) . . ?
F4 B1 F3 20.7(16) 9 . ?
F4 B1 F3 101(2) 5 . ?
F2 B1 F3 101.8(16) . . ?
F3 B1 F3 115.9(10) 9 . ?
F3 B1 F3 115.9(10) 5 . ?
F4 B1 F1 115.9(13) . . ?
F4 B1 F1 109(2) 9 . ?
F4 B1 F1 25.9(12) 5 . ?
F2 B1 F1 95.2(12) . . ?
F3 B1 F1 14.7(16) 9 . ?
F3 B1 F1 130.5(14) 5 . ?
F3 B1 F1 105.2(14) . . ?
F4 B1 F1 109(2) . 5 ?
F4 B1 F1 25.9(12) 9 5 ?
F4 B1 F1 115.9(13) 5 5 ?
F2 B1 F1 95.2(13) . 5 ?
F3 B1 F1 130.5(14) 9 5 ?
F3 B1 F1 105.2(14) 5 5 ?
F3 B1 F1 14.7(16) . 5 ?
F1 B1 F1 119.2(4) . 5 ?
F4 B1 F1 25.9(12) . 9 ?
F4 B1 F1 115.9(13) 9 9 ?
F4 B1 F1 109(2) 5 9 ?
F2 B1 F1 95.2(12) . 9 ?
F3 B1 F1 105.2(14) 9 9 ?
F3 B1 F1 14.7(16) 5 9 ?
F3 B1 F1 130.5(14) . 9 ?
F1 B1 F1 119.2(4) . 9 ?
F1 B1 F1 119.2(4) 5 9 ?
F3 F1 F4 53(7) 9 5 ?
F3 F1 B1 81(3) 9 . ?
F4 F1 B1 68.9(15) 5 . ?
F1 F3 F4 91(8) 5 9 ?
F1 F3 B1 84(3) 5 . ?
F4 F3 B1 71(2) 9 . ?
F3 F4 F1 36(4) 5 9 ?
F3 F4 B1 89(3) 5 . ?
F1 F4 B1 85.3(18) 9 . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.89(4) 2.02(4) 2.880(3) 162(3) . yes
N4 H4 O2 0.85(2) 2.08(2) 2.933(3) 174(3) 5 yes

_refine_diff_density_max         0.404
_refine_diff_density_min         -0.317
_refine_diff_density_rms         0.055

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_lb2205-110K
_database_code_depnum_ccdc_archive 'CCDC 2261767'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-19 deposited with the CCDC.	2023-08-03 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, C18 H6 Fe O12, B F4'
_chemical_formula_sum            'C102 H66 B F4 Fe3 N18 O12'
_chemical_formula_weight         1990.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
B B 0.0017 0.0007
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
N N 0.0065 0.0035
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
O O 0.0115 0.0064
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
F F 0.0185 0.0109
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      cubic
_space_group_IT_number           198
_space_group_name_H-M_alt        'P 21 3'
_space_group_name_Hall           'P 2ac 2ab 3'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'z, x, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z, x'
'-y, z+1/2, -x+1/2'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z, x+1/2'

_cell_length_a                   21.4991(4)
_cell_length_b                   21.4991(4)
_cell_length_c                   21.4991(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     9937.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    110(2)
_cell_measurement_reflns_used    9627
_cell_measurement_theta_min      2.748
_cell_measurement_theta_max      29.518

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.330
_exptl_crystal_F_000             4076
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.541
_shelx_estimated_absorpt_T_min   0.938
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.676
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_process_details   'SADABS-2016/2 - Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      110(2)
_diffrn_radiation_wavelength     0.7288
_diffrn_radiation_type           synchrotron
_diffrn_radiation_source         'Advanced Light Source station 12.2.1'
_diffrn_radiation_monochromator  'silicon 111'
_diffrn_measurement_device_type  'Bruker D8 with PHOTON II detector'
_diffrn_measurement_method       'shutterless /f and /w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            330486
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_av_R_equivalents  0.0599
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.172
_diffrn_reflns_theta_max         29.538
_diffrn_reflns_theta_full        29.500
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             8615
_reflns_number_gt                8445
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.858
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. 
 Hydrogens on the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogen were placed 
 geometrically on their carrier atom and refined with a riding model. The BF4
 anion is disordered by symmetry over three positions on the same central B1
 site, and was refined with distance and displacement parameters restraints.
 At the end of the refinement there remained a void with only
 weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
 a void volume of 1693 cubic angstrom  with only 109 electrons, i.e. what 
 would correspond to a small amount of very diffuse lattice MeOH per formula unit.
 The same analysis done on data for the same crystal measured at higher temperatures
 up to 400 K systematically gives a large void with similar electron count. We have 
 chosen not to use the SQUEEZED data, and let the model with empty void as 
 it likely corresponds more to reality.

 Details of SQUEEZE results before refinement of the BF4 disorder:
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.173  0.109  0.581      1693       109 ' '
   2  0.106  0.894  0.394         9         0 ' '
   3  0.393  0.106  0.894         9         0 ' '
   4  0.606  0.606  0.606         9         0 ' '
   5  0.893  0.394  0.106         9         0 ' '
_platon_squeeze_void_probe_radius                  1.20

;

_vrf_PLAT601_lb2205-110K         
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .       1685 Ang**3       
RESPONSE: At the end of the refinement there remained a void with only
weak electron density peaks. Analysis with PLATON/SQUEEZE (see below) gave 
a void volume of 1693 cubic angstrom  with only 109 electrons, i.e. what 
would correspond to a small amount of very diffuse lattice MeOH per formula unit.
The same analysis done on data for the same crystal measured at higher temperatures
up to 400 K systematically gives a large void with similar electron count. We have 
chosen not to use the SQUEEZED data, and let the model with empty void as 
it likely corresponds more to reality.

# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1 -0.173  0.109  0.581      1693       109 ' '
   2  0.106  0.894  0.394         9         0 ' '
   3  0.393  0.106  0.894         9         0 ' '
   4  0.606  0.606  0.606         9         0 ' '
   5  0.893  0.394  0.106         9         0 ' '
_platon_squeeze_void_probe_radius                  1.20

;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0597P)²+2.1661P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3813 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.0270(18)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8615
_refine_ls_number_parameters     457
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0316
_refine_ls_wR_factor_ref         0.0914
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.95247(2) 0.54753(2) 0.45247(2) 0.02355(11) Uani 1 3 d S T P . .
Fe2 Fe 0.66856(2) 0.83144(2) 0.16856(2) 0.02532(11) Uani 1 3 d S T P . .
N1 N 1.00952(9) 0.58141(8) 0.51752(9) 0.0274(3) Uani 1 1 d . . . . .
N2 N 0.89776(8) 0.61018(8) 0.48918(8) 0.0258(3) Uani 1 1 d . . . . .
N3 N 0.83731(8) 0.62600(8) 0.48461(8) 0.0262(3) Uani 1 1 d . . . . .
H3 H 0.8188(15) 0.6162(15) 0.4462(16) 0.039 Uiso 1 1 d . U . . .
N4 N 0.63290(8) 0.74554(9) 0.27704(9) 0.0271(3) Uani 1 1 d D . . . .
H4 H 0.6665(13) 0.7524(15) 0.2994(14) 0.041 Uiso 1 1 d D U . . .
N5 N 0.63161(9) 0.76386(9) 0.21700(9) 0.0273(3) Uani 1 1 d . . . . .
N6 N 0.60874(9) 0.79765(9) 0.10585(9) 0.0310(4) Uani 1 1 d . . . . .
C1 C 1.06820(11) 0.56397(11) 0.52887(11) 0.0329(4) Uani 1 1 d . . . . .
H1A H 1.087289 0.534553 0.501989 0.039 Uiso 1 1 calc R U . . .
C2 C 1.10220(12) 0.58745(13) 0.57869(13) 0.0396(5) Uani 1 1 d . . . . .
H2A H 1.143322 0.573234 0.586393 0.048 Uiso 1 1 calc R U . . .
C3 C 1.07531(13) 0.63184(13) 0.61692(13) 0.0412(5) Uani 1 1 d . . . . .
H3A H 1.097886 0.648696 0.650960 0.049 Uiso 1 1 calc R U . . .
C4 C 1.01523(12) 0.65127(12) 0.60488(12) 0.0366(5) Uani 1 1 d . . . . .
H4A H 0.996089 0.682311 0.629833 0.044 Uiso 1 1 calc R U . . .
C5 C 0.98358(10) 0.62447(10) 0.55562(10) 0.0285(4) Uani 1 1 d . . . . .
C6 C 0.91931(10) 0.63816(10) 0.54036(10) 0.0284(4) Uani 1 1 d . . . . .
C7 C 0.87281(11) 0.67315(11) 0.56878(10) 0.0315(4) Uani 1 1 d . . . . .
H7A H 0.876172 0.697455 0.605534 0.038 Uiso 1 1 calc R U . . .
C8 C 0.82089(11) 0.66495(10) 0.53218(9) 0.0289(4) Uani 1 1 d . . . . .
C9 C 0.75803(11) 0.68993(11) 0.53953(10) 0.0308(4) Uani 1 1 d . . . . .
C10 C 0.74584(13) 0.73199(13) 0.58784(12) 0.0395(5) Uani 1 1 d . . . . .
H10A H 0.778537 0.745084 0.614526 0.047 Uiso 1 1 calc R U . . .
C11 C 0.68626(15) 0.75440(15) 0.59663(13) 0.0485(7) Uani 1 1 d . . . . .
H11A H 0.678166 0.782784 0.629515 0.058 Uiso 1 1 calc R U . . .
C12 C 0.63828(13) 0.73589(16) 0.55798(13) 0.0458(6) Uani 1 1 d . . . . .
H12A H 0.597306 0.750844 0.565035 0.055 Uiso 1 1 calc R U . . .
C13 C 0.64982(11) 0.69546(13) 0.50885(11) 0.0355(5) Uani 1 1 d . . . . .
C14 C 0.70991(11) 0.67222(12) 0.50030(10) 0.0321(4) Uani 1 1 d . . . . .
H14A H 0.717921 0.643983 0.467272 0.039 Uiso 1 1 calc R U . . .
C15 C 0.60173(11) 0.68155(13) 0.46202(11) 0.0364(5) Uani 1 1 d . . . . .
C16 C 0.54296(13) 0.65861(17) 0.47728(14) 0.0503(7) Uani 1 1 d . . . . .
H16A H 0.532797 0.650012 0.519411 0.060 Uiso 1 1 calc R U . . .
C17 C 0.49948(13) 0.64842(19) 0.43085(15) 0.0557(8) Uani 1 1 d . . . . .
H17A H 0.459849 0.631896 0.441275 0.067 Uiso 1 1 calc R U . . .
C18 C 0.51312(12) 0.66202(16) 0.36947(14) 0.0454(6) Uani 1 1 d . . . . .
H18A H 0.482879 0.655098 0.338012 0.054 Uiso 1 1 calc R U . . .
C19 C 0.57169(11) 0.68604(12) 0.35378(11) 0.0333(5) Uani 1 1 d . . . . .
C20 C 0.61541(10) 0.69419(11) 0.40011(11) 0.0318(4) Uani 1 1 d . . . . .
H20A H 0.655746 0.708750 0.389442 0.038 Uiso 1 1 calc R U . . .
C21 C 0.58375(10) 0.70791(11) 0.29024(11) 0.0295(4) Uani 1 1 d . . . . .
C22 C 0.54882(11) 0.70251(11) 0.23651(11) 0.0320(4) Uani 1 1 d . . . . .
H22A H 0.511519 0.679518 0.230840 0.038 Uiso 1 1 calc R U . . .
C23 C 0.58026(10) 0.73814(10) 0.19253(11) 0.0296(4) Uani 1 1 d . . . . .
C24 C 0.56813(11) 0.75489(11) 0.12817(11) 0.0322(4) Uani 1 1 d . . . . .
C25 C 0.52014(13) 0.73038(13) 0.09329(13) 0.0415(6) Uani 1 1 d . . . . .
H25A H 0.491809 0.701499 0.111066 0.050 Uiso 1 1 calc R U . . .
C26 C 0.51415(16) 0.74874(15) 0.03192(14) 0.0506(7) Uani 1 1 d . . . . .
H26A H 0.481825 0.732308 0.006667 0.061 Uiso 1 1 calc R U . . .
C27 C 0.55580(15) 0.79127(15) 0.00787(13) 0.0489(7) Uani 1 1 d . . . . .
H27A H 0.552727 0.804226 -0.034258 0.059 Uiso 1 1 calc R U . . .
C28 C 0.60212(13) 0.81480(13) 0.04591(12) 0.0384(5) Uani 1 1 d . . . . .
H28A H 0.630420 0.844256 0.029065 0.046 Uiso 1 1 calc R U . . .
Fe3 Fe 0.81117(2) 0.68883(2) 0.31117(2) 0.03132(13) Uani 1 3 d S T P . .
O1 O 0.77839(7) 0.61984(7) 0.36424(7) 0.0276(3) Uani 1 1 d . . . . .
O2 O 0.74735(8) 0.65768(8) 0.25196(7) 0.0303(3) Uani 1 1 d . . . . .
O3 O 0.63522(11) 0.45528(12) 0.34849(10) 0.0566(6) Uani 1 1 d . . . . .
O4 O 0.61004(11) 0.49034(12) 0.23022(10) 0.0556(6) Uani 1 1 d . . . . .
C29 C 0.73428(10) 0.58768(11) 0.33721(10) 0.0292(4) Uani 1 1 d . . . . .
C30 C 0.71833(11) 0.60817(11) 0.27226(11) 0.0311(4) Uani 1 1 d . . . . .
C31 C 0.67713(12) 0.57593(13) 0.23683(11) 0.0376(5) Uani 1 1 d . . . . .
H31A H 0.668525 0.589670 0.195726 0.045 Uiso 1 1 calc R U . . .
C32 C 0.64652(12) 0.52182(14) 0.26011(12) 0.0404(5) Uani 1 1 d . . . . .
C33 C 0.66138(12) 0.50166(13) 0.32851(12) 0.0397(5) Uani 1 1 d . . . . .
C34 C 0.70532(11) 0.53822(12) 0.36326(11) 0.0342(5) Uani 1 1 d . . . . .
H34A H 0.714161 0.527478 0.405201 0.041 Uiso 1 1 calc R U . . .
B1 B 1.1062(12) 0.3925(9) 0.6082(10) 0.0398(12) Uani 0.3333 1 d D U P A -1
F1 F 1.1543(10) 0.4348(16) 0.6158(15) 0.065(6) Uani 0.3333 1 d D U P A -1
F2 F 1.0691(18) 0.4182(7) 0.5631(14) 0.078(5) Uani 0.3333 1 d D U P A -1
F3 F 1.1296(12) 0.3367(9) 0.5864(11) 0.061(5) Uani 0.3333 1 d D U P A -1
F4 F 1.0729(19) 0.3812(12) 0.6619(13) 0.052(4) Uani 0.3333 1 d D U P A -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 1.9548(18) . ?
Fe1 N2 1.9548(18) 12_664 ?
Fe1 N2 1.9548(18) 6_566 ?
Fe1 N1 1.9977(18) 12_664 ?
Fe1 N1 1.9977(18) 6_566 ?
Fe1 N1 1.9977(19) . ?
Fe2 N5 1.9563(19) 12_664 ?
Fe2 N5 1.9562(19) . ?
Fe2 N5 1.9563(19) 6_566 ?
Fe2 N6 1.9997(19) 12_664 ?
Fe2 N6 1.9997(19) . ?
Fe2 N6 1.9997(19) 6_566 ?
N1 C1 1.338(3) . ?
N1 C5 1.356(3) . ?
N2 C6 1.337(3) . ?
N2 N3 1.347(2) . ?
N3 C8 1.368(3) . ?
N3 H3 0.94(3) . ?
N4 N5 1.350(3) . ?
N4 C21 1.361(3) . ?
N4 H4 0.88(2) . ?
N5 C23 1.342(3) . ?
N6 C28 1.348(3) . ?
N6 C24 1.356(3) . ?
C1 C2 1.391(3) . ?
C1 H1A 0.9500 . ?
C2 C3 1.386(4) . ?
C2 H2A 0.9500 . ?
C3 C4 1.382(4) . ?
C3 H3A 0.9500 . ?
C4 C5 1.384(3) . ?
C4 H4A 0.9500 . ?
C5 C6 1.450(3) . ?
C6 C7 1.392(3) . ?
C7 C8 1.377(3) . ?
C7 H7A 0.9500 . ?
C8 C9 1.463(3) . ?
C9 C14 1.388(3) . ?
C9 C10 1.402(3) . ?
C10 C11 1.382(4) . ?
C10 H10A 0.9500 . ?
C11 C12 1.383(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.390(4) . ?
C12 H12A 0.9500 . ?
C13 C14 1.397(3) . ?
C13 C15 1.474(4) . ?
C14 H14A 0.9500 . ?
C15 C20 1.390(3) . ?
C15 C16 1.395(3) . ?
C16 C17 1.385(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.383(4) . ?
C17 H17A 0.9500 . ?
C18 C19 1.402(3) . ?
C18 H18A 0.9500 . ?
C19 C20 1.381(3) . ?
C19 C21 1.468(3) . ?
C20 H20A 0.9500 . ?
C21 C22 1.383(3) . ?
C22 C23 1.392(3) . ?
C22 H22A 0.9500 . ?
C23 C24 1.454(3) . ?
C24 C25 1.380(3) . ?
C25 C26 1.383(4) . ?
C25 H25A 0.9500 . ?
C26 C27 1.380(5) . ?
C26 H26A 0.9500 . ?
C27 C28 1.384(4) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
Fe3 O2 1.9878(16) 12_664 ?
Fe3 O2 1.9879(16) . ?
Fe3 O2 1.9879(16) 6_566 ?
Fe3 O1 1.9995(16) 6_566 ?
Fe3 O1 1.9995(16) 12_664 ?
Fe3 O1 1.9995(16) . ?
O1 C29 1.310(3) . ?
O2 C30 1.309(3) . ?
O3 C33 1.223(3) . ?
O4 C32 1.219(3) . ?
C29 C34 1.353(3) . ?
C29 C30 1.504(3) . ?
C30 C31 1.358(3) . ?
C31 C32 1.427(4) . ?
C31 H31A 0.9500 . ?
C32 C33 1.566(4) . ?
C33 C34 1.438(3) . ?
C34 H34A 0.9500 . ?
B1 F2 1.372(9) . ?
B1 F4 1.380(14) . ?
B1 F3 1.383(13) . ?
B1 F1 1.386(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 96.11(7) . 12_664 ?
N2 Fe1 N2 96.11(7) . 6_566 ?
N2 Fe1 N2 96.11(7) 12_664 6_566 ?
N2 Fe1 N1 90.86(7) . 12_664 ?
N2 Fe1 N1 80.53(8) 12_664 12_664 ?
N2 Fe1 N1 172.56(8) 6_566 12_664 ?
N2 Fe1 N1 172.57(8) . 6_566 ?
N2 Fe1 N1 90.86(7) 12_664 6_566 ?
N2 Fe1 N1 80.53(8) 6_566 6_566 ?
N1 Fe1 N1 92.84(7) 12_664 6_566 ?
N2 Fe1 N1 80.53(8) . . ?
N2 Fe1 N1 172.56(8) 12_664 . ?
N2 Fe1 N1 90.86(7) 6_566 . ?
N1 Fe1 N1 92.83(7) 12_664 . ?
N1 Fe1 N1 92.84(7) 6_566 . ?
N5 Fe2 N5 97.03(8) 12_664 . ?
N5 Fe2 N5 97.03(8) 12_664 6_566 ?
N5 Fe2 N5 97.03(8) . 6_566 ?
N5 Fe2 N6 80.09(8) 12_664 12_664 ?
N5 Fe2 N6 172.14(8) . 12_664 ?
N5 Fe2 N6 90.60(8) 6_566 12_664 ?
N5 Fe2 N6 90.60(8) 12_664 . ?
N5 Fe2 N6 80.09(8) . . ?
N5 Fe2 N6 172.14(8) 6_566 . ?
N6 Fe2 N6 92.58(8) 12_664 . ?
N5 Fe2 N6 172.14(8) 12_664 6_566 ?
N5 Fe2 N6 90.60(8) . 6_566 ?
N5 Fe2 N6 80.09(8) 6_566 6_566 ?
N6 Fe2 N6 92.58(8) 12_664 6_566 ?
N6 Fe2 N6 92.58(8) . 6_566 ?
C1 N1 C5 118.0(2) . . ?
C1 N1 Fe1 127.16(16) . . ?
C5 N1 Fe1 114.79(15) . . ?
C6 N2 N3 106.31(17) . . ?
C6 N2 Fe1 115.71(15) . . ?
N3 N2 Fe1 136.48(14) . . ?
N2 N3 C8 110.42(18) . . ?
N2 N3 H3 115(2) . . ?
C8 N3 H3 133(2) . . ?
N5 N4 C21 110.92(19) . . ?
N5 N4 H4 119(2) . . ?
C21 N4 H4 129(2) . . ?
C23 N5 N4 105.75(18) . . ?
C23 N5 Fe2 115.56(16) . . ?
N4 N5 Fe2 135.86(15) . . ?
C28 N6 C24 117.1(2) . . ?
C28 N6 Fe2 127.81(17) . . ?
C24 N6 Fe2 114.96(16) . . ?
N1 C1 C2 122.3(2) . . ?
N1 C1 H1A 118.9 . . ?
C2 C1 H1A 118.9 . . ?
C3 C2 C1 119.2(2) . . ?
C3 C2 H2A 120.4 . . ?
C1 C2 H2A 120.4 . . ?
C4 C3 C2 119.1(2) . . ?
C4 C3 H3A 120.4 . . ?
C2 C3 H3A 120.4 . . ?
C3 C4 C5 118.5(2) . . ?
C3 C4 H4A 120.8 . . ?
C5 C4 H4A 120.8 . . ?
N1 C5 C4 123.0(2) . . ?
N1 C5 C6 113.18(19) . . ?
C4 C5 C6 123.8(2) . . ?
N2 C6 C7 110.8(2) . . ?
N2 C6 C5 115.15(19) . . ?
C7 C6 C5 134.0(2) . . ?
C8 C7 C6 105.19(19) . . ?
C8 C7 H7A 127.4 . . ?
C6 C7 H7A 127.4 . . ?
N3 C8 C7 107.24(19) . . ?
N3 C8 C9 123.0(2) . . ?
C7 C8 C9 129.8(2) . . ?
C14 C9 C10 119.2(2) . . ?
C14 C9 C8 121.5(2) . . ?
C10 C9 C8 119.3(2) . . ?
C11 C10 C9 120.0(3) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 120.6(2) . . ?
C10 C11 H11A 119.7 . . ?
C12 C11 H11A 119.7 . . ?
C11 C12 C13 120.2(2) . . ?
C11 C12 H12A 119.9 . . ?
C13 C12 H12A 119.9 . . ?
C12 C13 C14 119.2(2) . . ?
C12 C13 C15 121.4(2) . . ?
C14 C13 C15 119.1(2) . . ?
C9 C14 C13 120.7(2) . . ?
C9 C14 H14A 119.6 . . ?
C13 C14 H14A 119.6 . . ?
C20 C15 C16 119.1(2) . . ?
C20 C15 C13 117.8(2) . . ?
C16 C15 C13 123.1(2) . . ?
C17 C16 C15 119.8(2) . . ?
C17 C16 H16A 120.1 . . ?
C15 C16 H16A 120.1 . . ?
C18 C17 C16 120.7(3) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 119.9(3) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 119.0(2) . . ?
C20 C19 C21 120.7(2) . . ?
C18 C19 C21 120.0(2) . . ?
C19 C20 C15 121.5(2) . . ?
C19 C20 H20A 119.3 . . ?
C15 C20 H20A 119.3 . . ?
N4 C21 C22 107.3(2) . . ?
N4 C21 C19 121.5(2) . . ?
C22 C21 C19 130.9(2) . . ?
C21 C22 C23 104.9(2) . . ?
C21 C22 H22A 127.5 . . ?
C23 C22 H22A 127.5 . . ?
N5 C23 C22 111.1(2) . . ?
N5 C23 C24 114.8(2) . . ?
C22 C23 C24 134.1(2) . . ?
N6 C24 C25 123.2(2) . . ?
N6 C24 C23 112.9(2) . . ?
C25 C24 C23 123.8(2) . . ?
C24 C25 C26 118.6(2) . . ?
C24 C25 H25A 120.7 . . ?
C26 C25 H25A 120.7 . . ?
C27 C26 C25 119.1(3) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
C26 C27 C28 119.2(3) . . ?
C26 C27 H27A 120.4 . . ?
C28 C27 H27A 120.4 . . ?
N6 C28 C27 122.7(3) . . ?
N6 C28 H28A 118.6 . . ?
C27 C28 H28A 118.6 . . ?
O2 Fe3 O2 90.37(7) 12_664 . ?
O2 Fe3 O2 90.36(7) 12_664 6_566 ?
O2 Fe3 O2 90.36(7) . 6_566 ?
O2 Fe3 O1 95.39(7) 12_664 6_566 ?
O2 Fe3 O1 170.97(6) . 6_566 ?
O2 Fe3 O1 82.66(6) 6_566 6_566 ?
O2 Fe3 O1 82.66(6) 12_664 12_664 ?
O2 Fe3 O1 95.39(7) . 12_664 ?
O2 Fe3 O1 170.97(6) 6_566 12_664 ?
O1 Fe3 O1 92.25(7) 6_566 12_664 ?
O2 Fe3 O1 170.96(6) 12_664 . ?
O2 Fe3 O1 82.66(6) . . ?
O2 Fe3 O1 95.39(7) 6_566 . ?
O1 Fe3 O1 92.25(7) 6_566 . ?
O1 Fe3 O1 92.25(7) 12_664 . ?
C29 O1 Fe3 113.19(14) . . ?
C30 O2 Fe3 112.92(14) . . ?
O1 C29 C34 124.4(2) . . ?
O1 C29 C30 115.0(2) . . ?
C34 C29 C30 120.6(2) . . ?
O2 C30 C31 122.6(2) . . ?
O2 C30 C29 116.1(2) . . ?
C31 C30 C29 121.3(2) . . ?
C30 C31 C32 121.3(2) . . ?
C30 C31 H31A 119.3 . . ?
C32 C31 H31A 119.3 . . ?
O4 C32 C31 124.4(2) . . ?
O4 C32 C33 118.2(2) . . ?
C31 C32 C33 117.4(2) . . ?
O3 C33 C34 124.4(2) . . ?
O3 C33 C32 117.5(2) . . ?
C34 C33 C32 118.1(2) . . ?
C29 C34 C33 121.1(2) . . ?
C29 C34 H34A 119.4 . . ?
C33 C34 H34A 119.4 . . ?
F2 B1 F4 111.0(17) . . ?
F2 B1 F3 108.7(14) . . ?
F4 B1 F3 108.6(18) . . ?
F2 B1 F1 104.6(15) . . ?
F4 B1 F1 114(2) . . ?
F3 B1 F1 109.8(18) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3 O1 0.94(3) 1.97(3) 2.884(2) 165(3) . yes
N4 H4 O2 0.88(2) 2.06(2) 2.923(2) 168(3) 6_566 yes

_refine_diff_density_max         0.502
_refine_diff_density_min         -0.367
_refine_diff_density_rms         0.067


