# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_lb2135_a_sq
_database_code_depnum_ccdc_archive 'CCDC 2172376'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C78 H56 Fe2 N18, 2(F6 P), F6 Si, C4 H10 O, C H4 O'
_chemical_formula_sum            'C83 H70 F18 Fe2 N18 O2 P2 Si'
_chemical_formula_weight         1895.29

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'
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'
Si Si 0.0866 0.0751
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1071 0.1002
'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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.2482(8)
_cell_length_b                   26.1224(12)
_cell_length_c                   18.8989(9)
_cell_angle_alpha                90
_cell_angle_beta                 105.110(2)
_cell_angle_gamma                90
_cell_volume                     8220.8(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9325
_cell_measurement_theta_min      2.398
_cell_measurement_theta_max      26.032

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_F_000             3865
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.538
_shelx_estimated_absorpt_T_min   0.900
_shelx_estimated_absorpt_T_max   0.984
_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      100(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            213367
_diffrn_reflns_av_unetI/netI     0.0255
_diffrn_reflns_av_R_equivalents  0.0517
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.032
_diffrn_reflns_theta_max         26.177
_diffrn_reflns_theta_full        26.040
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             15186
_reflns_number_gt                12564
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. One of the PF6 anion was 
 refined disordered over two positions with relative occupancies 0.738:0.262
 (P2:P3), using 1,2 and 1,3 distance restraints as well as displacement parameters 
 restraints.
 Hydrogens on four of the six pyrazole N were refined freely with their thermal
 parameter 1.5 times of their carrier N atom. The rest of hydrogens were placed 
 geometrically on their carrier atom and refined with a riding model, including 
 the remaining two hydrogens on pyrazole N (AFIX 43), as their free refinement 
 was not fully satisfactory. A small void with very weak and diffuse electron
 density remained at the end of the refinement that could not be refined as
 lattice solvent. The model/data was therefore analyzed using 
 PLATON/SQUEEZE that found two main voids of 232 cubic angstroms with 42
 electrons per void. These figures are reasonable for 2 diffuse 
 methanol molecules per void, and this was thus reflected in the formula,
 i.e. 1 additional 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)+(0.1266P)²+11.5091P] 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_number_reflns         15186
_refine_ls_number_parameters     1202
_refine_ls_number_restraints     422
_refine_ls_R_factor_all          0.0791
_refine_ls_R_factor_gt           0.0682
_refine_ls_wR_factor_ref         0.2190
_refine_ls_wR_factor_gt          0.2064
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.242
_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 0.48880(3) 0.33474(2) 0.42405(3) 0.04085(16) Uani 1 1 d . . . . .
Fe2 Fe 0.06739(3) 0.31721(2) 0.71253(3) 0.05136(18) Uani 1 1 d . . . . .
N1 N 0.5705(2) 0.26740(12) 0.4529(2) 0.0531(8) Uani 1 1 d . . . . .
N2 N 0.51569(18) 0.32865(12) 0.54169(19) 0.0460(7) Uani 1 1 d . . . . .
N3 N 0.50781(19) 0.36076(13) 0.59467(19) 0.0454(7) Uani 1 1 d . . . . .
H3 H 0.469(3) 0.381(2) 0.586(3) 0.068 Uiso 1 1 d . U . . .
N4 N 0.2113(2) 0.40197(17) 0.7508(2) 0.0584(9) Uani 1 1 d . . . . .
H4 H 0.245(4) 0.384(2) 0.728(3) 0.088 Uiso 1 1 d . U . . .
N5 N 0.1397(2) 0.38158(16) 0.75312(19) 0.0584(9) Uani 1 1 d . . . . .
N6 N -0.0064(2) 0.36266(19) 0.7640(3) 0.0766(14) Uani 1 1 d . . . . .
N7 N 0.58366(18) 0.38600(12) 0.41375(18) 0.0442(7) Uani 1 1 d . . . . .
N8 N 0.43868(17) 0.41066(11) 0.42530(17) 0.0407(6) Uani 1 1 d . . . . .
N9 N 0.36877(18) 0.43260(12) 0.42729(18) 0.0418(7) Uani 1 1 d . . . . .
H9 H 0.335(3) 0.4155(19) 0.440(3) 0.063 Uiso 1 1 d . U . . .
N10 N 0.0513(2) 0.38748(14) 0.5688(2) 0.0537(8) Uani 1 1 d . . . . .
H10 H 0.096(4) 0.404(2) 0.587(3) 0.081 Uiso 1 1 d . U . . .
N11 N 0.03588(19) 0.34584(14) 0.6048(2) 0.0524(8) Uani 1 1 d . . . . .
N12 N -0.0283(2) 0.26618(15) 0.6555(2) 0.0575(9) Uani 1 1 d . . . . .
N13 N 0.4621(2) 0.31430(12) 0.30618(19) 0.0474(7) Uani 1 1 d . . . . .
N14 N 0.38321(19) 0.28958(12) 0.40221(18) 0.0445(7) Uani 1 1 d . . . . .
N15 N 0.3460(2) 0.26675(12) 0.4473(2) 0.0464(7) Uani 1 1 d . . . . .
H15 H 0.344(3) 0.283(2) 0.488(3) 0.070 Uiso 1 1 d . U . . .
N16 N 0.1705(2) 0.25236(14) 0.62970(19) 0.0513(8) Uani 1 1 d . . . . .
H16 H 0.174(3) 0.278(2) 0.606(3) 0.077 Uiso 1 1 d . U . . .
N17 N 0.1509(2) 0.26488(13) 0.69187(18) 0.0496(8) Uani 1 1 d . . . . .
N18 N 0.0946(2) 0.26696(14) 0.80803(19) 0.0534(8) Uani 1 1 d . . . . .
C1 C 0.5890(3) 0.23241(17) 0.4074(3) 0.0650(12) Uani 1 1 d . . . . .
H1A H 0.569046 0.237270 0.356072 0.078 Uiso 1 1 calc R U . . .
C2 C 0.6355(3) 0.19005(18) 0.4320(4) 0.0776(16) Uani 1 1 d . . . . .
H2A H 0.646111 0.165834 0.398205 0.093 Uiso 1 1 calc R U . . .
C3 C 0.6669(3) 0.1831(2) 0.5073(4) 0.0805(16) Uani 1 1 d . . . . .
H3A H 0.699799 0.154253 0.525301 0.097 Uiso 1 1 calc R U . . .
C4 C 0.6499(3) 0.21831(17) 0.5553(3) 0.0703(13) Uani 1 1 d . . . . .
H4A H 0.670506 0.214436 0.606763 0.084 Uiso 1 1 calc R U . . .
C5 C 0.6009(2) 0.26027(16) 0.5257(3) 0.0549(10) Uani 1 1 d . . . . .
C6 C 0.5779(2) 0.29866(15) 0.5727(2) 0.0491(9) Uani 1 1 d . . . . .
C7 C 0.6095(2) 0.31156(16) 0.6460(2) 0.0521(10) Uani 1 1 d . . . . .
H7A H 0.653754 0.296138 0.680076 0.063 Uiso 1 1 calc R U . . .
C8 C 0.5627(2) 0.35162(16) 0.6583(2) 0.0483(9) Uani 1 1 d . . . . .
C9 C 0.5703(2) 0.38529(17) 0.7222(2) 0.0518(9) Uani 1 1 d . . . . .
C10 C 0.6467(3) 0.39420(19) 0.7689(3) 0.0615(11) Uani 1 1 d . . . . .
H10A H 0.692188 0.376359 0.762055 0.074 Uiso 1 1 calc R U . . .
C11 C 0.6550(3) 0.4291(2) 0.8249(3) 0.0726(14) Uani 1 1 d . . . . .
H11A H 0.706494 0.434559 0.857373 0.087 Uiso 1 1 calc R U . . .
C12 C 0.5905(3) 0.4560(2) 0.8346(3) 0.0680(12) Uani 1 1 d . . . . .
H12A H 0.598165 0.480499 0.872996 0.082 Uiso 1 1 calc R U . . .
C13 C 0.5134(3) 0.44789(18) 0.7888(2) 0.0576(10) Uani 1 1 d . . . . .
C14 C 0.5051(2) 0.41168(16) 0.7335(2) 0.0504(9) Uani 1 1 d . . . . .
H14A H 0.453112 0.404840 0.702633 0.061 Uiso 1 1 calc R U . . .
C15 C 0.4422(3) 0.4762(2) 0.7969(2) 0.0597(11) Uani 1 1 d . . . . .
C16 C 0.4440(3) 0.5286(2) 0.8129(3) 0.0761(14) Uani 1 1 d . . . . .
H16A H 0.492615 0.547188 0.818893 0.091 Uiso 1 1 calc R U . . .
C17 C 0.3752(4) 0.5536(3) 0.8200(4) 0.095(2) Uani 1 1 d . . . . .
H17A H 0.377637 0.588972 0.831961 0.114 Uiso 1 1 calc R U . . .
C18 C 0.3038(4) 0.5276(2) 0.8099(3) 0.0826(16) Uani 1 1 d . . . . .
H18A H 0.256751 0.545300 0.813293 0.099 Uiso 1 1 calc R U . . .
C19 C 0.3006(3) 0.4753(2) 0.7946(2) 0.0619(11) Uani 1 1 d . . . . .
C20 C 0.3694(3) 0.45055(19) 0.7879(2) 0.0560(10) Uani 1 1 d . . . . .
H20A H 0.366936 0.415014 0.776900 0.067 Uiso 1 1 calc R U . . .
C21 C 0.2264(3) 0.44696(19) 0.7877(2) 0.0584(11) Uani 1 1 d . . . . .
C22 C 0.1611(3) 0.4558(2) 0.8159(3) 0.0635(12) Uani 1 1 d . . . . .
H22A H 0.152999 0.484104 0.844634 0.076 Uiso 1 1 calc R U . . .
C23 C 0.1096(3) 0.41414(19) 0.7930(3) 0.0614(11) Uani 1 1 d . . . . .
C24 C 0.0319(3) 0.4025(2) 0.8054(3) 0.0711(13) Uani 1 1 d . U . . .
C25 C -0.0009(4) 0.4272(2) 0.8535(4) 0.0952(16) Uani 1 1 d . U . . .
H25A H 0.026565 0.455366 0.880709 0.114 Uiso 1 1 calc R U . . .
C26 C -0.0732(4) 0.4121(3) 0.8634(5) 0.1162(19) Uani 1 1 d . U . . .
H26A H -0.095308 0.428878 0.898248 0.139 Uiso 1 1 calc R U . . .
C27 C -0.1129(4) 0.3727(3) 0.8225(5) 0.1081(18) Uani 1 1 d . U . . .
H27A H -0.163460 0.361788 0.828161 0.130 Uiso 1 1 calc R U . . .
C28 C -0.0787(3) 0.3485(3) 0.7721(4) 0.0915(15) Uani 1 1 d . U . . .
H28A H -0.106963 0.321400 0.742925 0.110 Uiso 1 1 calc R U . . .
C31 C 0.6569(2) 0.37186(16) 0.4093(3) 0.0574(11) Uani 1 1 d . . . . .
H31A H 0.670602 0.336573 0.413970 0.069 Uiso 1 1 calc R U . . .
C32 C 0.7134(2) 0.40629(17) 0.3982(3) 0.0642(12) Uani 1 1 d . . . . .
H32A H 0.764730 0.394806 0.395346 0.077 Uiso 1 1 calc R U . . .
C33 C 0.6940(2) 0.45754(17) 0.3914(3) 0.0583(11) Uani 1 1 d . . . . .
H33A H 0.731922 0.482026 0.384070 0.070 Uiso 1 1 calc R U . . .
C34 C 0.6185(2) 0.47269(15) 0.3954(2) 0.0488(9) Uani 1 1 d . . . . .
H34A H 0.603773 0.507817 0.390949 0.059 Uiso 1 1 calc R U . . .
C35 C 0.5648(2) 0.43635(14) 0.4059(2) 0.0414(8) Uani 1 1 d . . . . .
C36 C 0.4832(2) 0.44898(14) 0.4105(2) 0.0398(7) Uani 1 1 d . . . . .
C37 C 0.4417(2) 0.49519(14) 0.4029(2) 0.0408(8) Uani 1 1 d . . . . .
H37A H 0.460308 0.527852 0.392485 0.049 Uiso 1 1 calc R U . . .
C38 C 0.3678(2) 0.48331(14) 0.4140(2) 0.0405(8) Uani 1 1 d . . . . .
C39 C 0.2969(2) 0.51569(14) 0.4111(2) 0.0427(8) Uani 1 1 d . . . . .
C40 C 0.3024(2) 0.56847(15) 0.4062(2) 0.0510(9) Uani 1 1 d . . . . .
H40A H 0.352493 0.583900 0.406982 0.061 Uiso 1 1 calc R U . . .
C41 C 0.2352(3) 0.59866(16) 0.4001(3) 0.0587(11) Uani 1 1 d . . . . .
H41A H 0.239396 0.634800 0.396922 0.070 Uiso 1 1 calc R U . . .
C42 C 0.1621(3) 0.57672(16) 0.3986(3) 0.0550(10) Uani 1 1 d . . . . .
H42A H 0.115931 0.597737 0.393058 0.066 Uiso 1 1 calc R U . . .
C43 C 0.1556(2) 0.52424(16) 0.4052(2) 0.0474(9) Uani 1 1 d . . . . .
C44 C 0.2236(2) 0.49418(15) 0.4109(2) 0.0434(8) Uani 1 1 d . . . . .
H44A H 0.219492 0.458066 0.414655 0.052 Uiso 1 1 calc R U . . .
C45 C 0.0781(2) 0.49931(16) 0.4049(2) 0.0519(9) Uani 1 1 d . . . . .
C46 C 0.0062(3) 0.51466(19) 0.3566(3) 0.0649(12) Uani 1 1 d . . . . .
H46A H 0.006297 0.542324 0.323931 0.078 Uiso 1 1 calc R U . . .
C47 C -0.0646(3) 0.4903(2) 0.3554(3) 0.0774(16) Uani 1 1 d . . . . .
H47A H -0.113134 0.501603 0.322492 0.093 Uiso 1 1 calc R U . . .
C48 C -0.0660(3) 0.4498(2) 0.4016(3) 0.0729(14) Uani 1 1 d . . . . .
H48A H -0.115161 0.432697 0.399719 0.087 Uiso 1 1 calc R U . . .
C49 C 0.0050(2) 0.43366(17) 0.4512(3) 0.0543(10) Uani 1 1 d . . . . .
C50 C 0.0763(2) 0.45855(15) 0.4525(2) 0.0481(9) Uani 1 1 d . . . . .
H50A H 0.124622 0.447785 0.486191 0.058 Uiso 1 1 calc R U . . .
C51 C 0.0015(2) 0.39088(16) 0.5009(2) 0.0496(9) Uani 1 1 d . . . . .
C52 C -0.0485(2) 0.34919(16) 0.4923(2) 0.0491(9) Uani 1 1 d . . . . .
H52A H -0.090415 0.340570 0.450314 0.059 Uiso 1 1 calc R U . . .
C53 C -0.0249(2) 0.32208(16) 0.5581(2) 0.0480(9) Uani 1 1 d . . . . .
C54 C -0.0542(2) 0.27484(17) 0.5834(2) 0.0520(9) Uani 1 1 d . . . . .
C55 C -0.1026(3) 0.24068(19) 0.5353(3) 0.0638(11) Uani 1 1 d . . . . .
H55A H -0.120186 0.247949 0.484397 0.077 Uiso 1 1 calc R U . . .
C56 C -0.1246(3) 0.1956(2) 0.5637(3) 0.0723(13) Uani 1 1 d . . . . .
H56A H -0.156431 0.170915 0.532082 0.087 Uiso 1 1 calc R U . . .
C57 C -0.0999(3) 0.1870(2) 0.6379(3) 0.0702(13) Uani 1 1 d . . . . .
H57A H -0.115264 0.156701 0.658621 0.084 Uiso 1 1 calc R U . . .
C58 C -0.0529(3) 0.2229(2) 0.6813(3) 0.0669(12) Uani 1 1 d . . . . .
H58A H -0.036678 0.216967 0.732607 0.080 Uiso 1 1 calc R U . . .
C61 C 0.5001(3) 0.33064(17) 0.2571(3) 0.0558(10) Uani 1 1 d . . . . .
H61A H 0.537192 0.358090 0.270419 0.067 Uiso 1 1 calc R U . . .
C62 C 0.4883(3) 0.30959(19) 0.1877(3) 0.0624(11) Uani 1 1 d . . . . .
H62A H 0.516343 0.322467 0.154407 0.075 Uiso 1 1 calc R U . . .
C63 C 0.4352(3) 0.26976(18) 0.1683(3) 0.0592(11) Uani 1 1 d . . . . .
H63A H 0.426677 0.254253 0.121392 0.071 Uiso 1 1 calc R U . . .
C64 C 0.3940(2) 0.25230(16) 0.2174(2) 0.0522(9) Uani 1 1 d . . . . .
H64A H 0.356547 0.225022 0.204686 0.063 Uiso 1 1 calc R U . . .
C65 C 0.4086(2) 0.27547(15) 0.2856(2) 0.0465(8) Uani 1 1 d . . . . .
C66 C 0.3700(2) 0.25990(14) 0.3427(2) 0.0445(8) Uani 1 1 d . . . . .
C67 C 0.3234(2) 0.21724(15) 0.3504(2) 0.0477(9) Uani 1 1 d . . . . .
H67A H 0.305567 0.190342 0.316167 0.057 Uiso 1 1 calc R U . . .
C68 C 0.3092(2) 0.22296(14) 0.4188(2) 0.0474(9) Uani 1 1 d . . . . .
C69 C 0.2676(3) 0.19078(15) 0.4611(2) 0.0529(10) Uani 1 1 d . . . . .
C70 C 0.2510(4) 0.13967(18) 0.4432(3) 0.0752(15) Uani 1 1 d . . . . .
H70A H 0.263060 0.125573 0.401010 0.090 Uiso 1 1 calc R U . . .
C71 C 0.2168(4) 0.1093(2) 0.4870(3) 0.0907(19) Uani 1 1 d . . . . .
H71A H 0.207468 0.074061 0.475397 0.109 Uiso 1 1 calc R U . . .
C72 C 0.1962(4) 0.12905(19) 0.5464(3) 0.0792(16) Uani 1 1 d . . . . .
H72A H 0.171905 0.107692 0.575226 0.095 Uiso 1 1 calc R U . . .
C73 C 0.2106(3) 0.18036(16) 0.5649(3) 0.0579(10) Uani 1 1 d . . . . .
C74 C 0.2469(2) 0.21078(15) 0.5215(2) 0.0504(9) Uani 1 1 d . . . . .
H74A H 0.257481 0.245811 0.533843 0.060 Uiso 1 1 calc R U . . .
C75 C 0.1884(3) 0.20242(17) 0.6275(2) 0.0545(10) Uani 1 1 d . . . . .
C76 C 0.1786(3) 0.18107(17) 0.6914(3) 0.0591(11) Uani 1 1 d . . . . .
H76A H 0.186268 0.146280 0.706274 0.071 Uiso 1 1 calc R U . . .
C77 C 0.1554(2) 0.22104(16) 0.7293(2) 0.0508(9) Uani 1 1 d . . . . .
C78 C 0.1310(2) 0.22337(17) 0.7975(2) 0.0520(9) Uani 1 1 d . . . . .
C79 C 0.1418(3) 0.18286(19) 0.8468(3) 0.0609(11) Uani 1 1 d . . . . .
H79A H 0.169175 0.152724 0.838690 0.073 Uiso 1 1 calc R U . . .
C80 C 0.1125(3) 0.1872(2) 0.9070(3) 0.0648(12) Uani 1 1 d . . . . .
H80A H 0.116664 0.159360 0.940158 0.078 Uiso 1 1 calc R U . . .
C81 C 0.0769(3) 0.2322(2) 0.9190(3) 0.0644(12) Uani 1 1 d . . . . .
H81A H 0.057472 0.236229 0.961319 0.077 Uiso 1 1 calc R U . . .
C82 C 0.0697(3) 0.27142(19) 0.8689(2) 0.0583(10) Uani 1 1 d . . . . .
H82A H 0.046075 0.302761 0.878016 0.070 Uiso 1 1 calc R U . . .
Si1 Si 0.28028(6) 0.37267(4) 0.57610(5) 0.0386(2) Uani 1 1 d . . . . .
F1 F 0.25978(12) 0.38259(8) 0.48475(11) 0.0436(5) Uani 1 1 d . . . . .
F2 F 0.33665(13) 0.32072(8) 0.56747(12) 0.0444(5) Uani 1 1 d . . . . .
F3 F 0.36260(12) 0.40950(8) 0.58775(12) 0.0443(5) Uani 1 1 d . . . . .
F4 F 0.19829(13) 0.33535(8) 0.56178(12) 0.0466(5) Uani 1 1 d . . . . .
F5 F 0.22510(12) 0.42280(8) 0.58834(12) 0.0468(5) Uani 1 1 d . . . . .
F6 F 0.30169(13) 0.36011(9) 0.66724(12) 0.0492(5) Uani 1 1 d . . . . .
P1 P 0.78127(7) 0.27458(5) 0.30382(7) 0.0629(3) Uani 1 1 d . . . . .
F7 F 0.8120(3) 0.32829(15) 0.2873(3) 0.1123(13) Uani 1 1 d . . . . .
F8 F 0.87177(16) 0.25696(14) 0.33535(17) 0.0837(9) Uani 1 1 d . . . . .
F9 F 0.77950(16) 0.29390(13) 0.38287(16) 0.0756(8) Uani 1 1 d . . . . .
F10 F 0.69065(18) 0.29248(18) 0.2723(2) 0.1058(13) Uani 1 1 d . . . . .
F11 F 0.7501(2) 0.22035(14) 0.3205(2) 0.1040(12) Uani 1 1 d . . . . .
F12 F 0.78375(18) 0.25374(16) 0.22515(18) 0.0958(11) Uani 1 1 d . . . . .
P2 P 0.1748(3) 0.55000(12) 0.97854(17) 0.1259(11) Uani 0.738(5) 1 d D U P A 1
F13 F 0.2068(5) 0.59455(19) 1.0266(3) 0.128(2) Uani 0.738(5) 1 d D U P A 1
F14 F 0.1816(5) 0.57669(18) 0.9099(3) 0.121(2) Uani 0.738(5) 1 d D U P A 1
F15 F 0.1168(4) 0.5094(2) 0.9447(4) 0.138(2) Uani 0.738(5) 1 d D U P A 1
F16 F 0.1703(5) 0.5227(3) 1.0533(4) 0.154(2) Uani 0.738(5) 1 d D U P A 1
F17 F 0.2515(4) 0.5262(2) 0.9873(3) 0.1179(15) Uani 0.738(5) 1 d D U P A 1
F18 F 0.0907(4) 0.5815(3) 0.9787(4) 0.157(2) Uani 0.738(5) 1 d D U P A 1
P3 P 0.1601(8) 0.5216(5) 0.9859(7) 0.159(3) Uani 0.262(5) 1 d D U P A 2
F19 F 0.1878(12) 0.5784(6) 1.0291(9) 0.108(3) Uani 0.262(5) 1 d D U P A 2
F20 F 0.1416(15) 0.5537(7) 0.9121(8) 0.151(4) Uani 0.262(5) 1 d D U P A 2
F21 F 0.1361(15) 0.4673(7) 0.9905(14) 0.194(4) Uani 0.262(5) 1 d D U P A 2
F22 F 0.2362(10) 0.5059(6) 1.0501(8) 0.126(3) Uani 0.262(5) 1 d D U P A 2
F23 F 0.2381(9) 0.5057(5) 0.9535(7) 0.111(3) Uani 0.262(5) 1 d D U P A 2
F24 F 0.0881(12) 0.5303(10) 1.0167(14) 0.185(4) Uani 0.262(5) 1 d D U P A 2
O1S O 0.1897(3) 0.43495(14) 0.2328(2) 0.0849(11) Uani 1 1 d . . . . .
C1S C 0.3269(4) 0.4256(3) 0.2332(3) 0.0883(17) Uani 1 1 d . . . . .
H1SA H 0.316070 0.399734 0.194353 0.132 Uiso 1 1 calc R U . . .
H1SB H 0.334957 0.408802 0.280922 0.132 Uiso 1 1 calc R U . . .
H1SC H 0.375398 0.444813 0.232035 0.132 Uiso 1 1 calc R U . . .
C2S C 0.2564(4) 0.4620(2) 0.2214(3) 0.0839(16) Uani 1 1 d . . . . .
H2SA H 0.269899 0.491048 0.256045 0.101 Uiso 1 1 calc R U . . .
H2SB H 0.243443 0.475791 0.170831 0.101 Uiso 1 1 calc R U . . .
C3S C 0.1174(4) 0.4635(2) 0.2117(4) 0.0944(19) Uani 1 1 d . . . . .
H3SA H 0.107717 0.474494 0.160018 0.113 Uiso 1 1 calc R U . . .
H3SB H 0.121760 0.494572 0.242623 0.113 Uiso 1 1 calc R U . . .
C4S C 0.0487(4) 0.4311(3) 0.2206(5) 0.116(3) Uani 1 1 d . . . . .
H4SA H 0.043854 0.400784 0.189115 0.174 Uiso 1 1 calc R U . . .
H4SB H -0.001212 0.450924 0.206514 0.174 Uiso 1 1 calc R U . . .
H4SC H 0.058516 0.420312 0.271818 0.174 Uiso 1 1 calc R U . . .


_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 N14 2.118(3) . ?
Fe1 N2 2.156(4) . ?
Fe1 N7 2.162(3) . ?
Fe1 N8 2.166(3) . ?
Fe1 N13 2.219(3) . ?
Fe1 N1 2.230(3) . ?
Fe2 N17 2.095(4) . ?
Fe2 N11 2.103(3) . ?
Fe2 N5 2.115(4) . ?
Fe2 N6 2.149(5) . ?
Fe2 N12 2.176(4) . ?
Fe2 N18 2.182(3) . ?
N1 C1 1.349(6) . ?
N1 C5 1.352(6) . ?
N2 C6 1.334(5) . ?
N2 N3 1.340(5) . ?
N3 C8 1.344(5) . ?
N3 H3 0.83(5) . ?
N4 N5 1.356(5) . ?
N4 C21 1.357(6) . ?
N4 H4 0.93(6) . ?
N5 C23 1.328(6) . ?
N6 C28 1.347(6) . ?
N6 C24 1.365(8) . ?
N7 C31 1.340(5) . ?
N7 C35 1.354(5) . ?
N8 C36 1.335(5) . ?
N8 N9 1.344(4) . ?
N9 C38 1.348(5) . ?
N9 H9 0.81(5) . ?
N10 N11 1.346(5) . ?
N10 C51 1.348(6) . ?
N10 H10 0.87(6) . ?
N11 C53 1.334(5) . ?
N12 C54 1.338(6) . ?
N12 C58 1.343(6) . ?
N13 C61 1.339(5) . ?
N13 C65 1.357(5) . ?
N14 N15 1.334(4) . ?
N14 C66 1.336(5) . ?
N15 C68 1.351(5) . ?
N15 H15 0.89(5) . ?
N16 C75 1.344(6) . ?
N16 N17 1.345(5) . ?
N16 H16 0.82(6) . ?
N17 C77 1.337(5) . ?
N18 C82 1.334(5) . ?
N18 C78 1.339(6) . ?
C1 C2 1.374(7) . ?
C1 H1A 0.9500 . ?
C2 C3 1.397(9) . ?
C2 H2A 0.9500 . ?
C3 C4 1.377(8) . ?
C3 H3A 0.9500 . ?
C4 C5 1.407(6) . ?
C4 H4A 0.9500 . ?
C5 C6 1.462(6) . ?
C6 C7 1.391(6) . ?
C7 C8 1.378(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.471(6) . ?
C9 C14 1.384(6) . ?
C9 C10 1.401(6) . ?
C10 C11 1.374(7) . ?
C10 H10A 0.9500 . ?
C11 C12 1.369(7) . ?
C11 H11A 0.9500 . ?
C12 C13 1.401(6) . ?
C12 H12A 0.9500 . ?
C13 C14 1.389(6) . ?
C13 C15 1.475(6) . ?
C14 H14A 0.9500 . ?
C15 C20 1.394(6) . ?
C15 C16 1.399(7) . ?
C16 C17 1.392(8) . ?
C16 H16A 0.9500 . ?
C17 C18 1.375(8) . ?
C17 H17A 0.9500 . ?
C18 C19 1.396(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.386(6) . ?
C19 C21 1.453(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.385(6) . ?
C22 C23 1.400(7) . ?
C22 H22A 0.9500 . ?
C23 C24 1.451(6) . ?
C24 C25 1.355(8) . ?
C25 C26 1.365(8) . ?
C25 H25A 0.9500 . ?
C26 C27 1.361(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.396(10) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C31 C32 1.381(6) . ?
C31 H31A 0.9500 . ?
C32 C33 1.378(6) . ?
C32 H32A 0.9500 . ?
C33 C34 1.383(6) . ?
C33 H33A 0.9500 . ?
C34 C35 1.375(5) . ?
C34 H34A 0.9500 . ?
C35 C36 1.471(5) . ?
C36 C37 1.391(5) . ?
C37 C38 1.380(5) . ?
C37 H37A 0.9500 . ?
C38 C39 1.476(5) . ?
C39 C44 1.382(5) . ?
C39 C40 1.387(5) . ?
C40 C41 1.382(6) . ?
C40 H40A 0.9500 . ?
C41 C42 1.379(6) . ?
C41 H41A 0.9500 . ?
C42 C43 1.384(6) . ?
C42 H42A 0.9500 . ?
C43 C44 1.391(5) . ?
C43 C45 1.486(5) . ?
C44 H44A 0.9500 . ?
C45 C46 1.394(6) . ?
C45 C50 1.399(6) . ?
C46 C47 1.373(7) . ?
C46 H46A 0.9500 . ?
C47 C48 1.377(7) . ?
C47 H47A 0.9500 . ?
C48 C49 1.400(6) . ?
C48 H48A 0.9500 . ?
C49 C50 1.385(6) . ?
C49 C51 1.471(6) . ?
C50 H50A 0.9500 . ?
C51 C52 1.372(6) . ?
C52 C53 1.397(6) . ?
C52 H52A 0.9500 . ?
C53 C54 1.460(6) . ?
C54 C55 1.386(6) . ?
C55 C56 1.387(7) . ?
C55 H55A 0.9500 . ?
C56 C57 1.375(8) . ?
C56 H56A 0.9500 . ?
C57 C58 1.365(7) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C61 C62 1.386(6) . ?
C61 H61A 0.9500 . ?
C62 C63 1.371(6) . ?
C62 H62A 0.9500 . ?
C63 C64 1.386(6) . ?
C63 H63A 0.9500 . ?
C64 C65 1.386(6) . ?
C64 H64A 0.9500 . ?
C65 C66 1.465(5) . ?
C66 C67 1.404(5) . ?
C67 C68 1.386(6) . ?
C67 H67A 0.9500 . ?
C68 C69 1.469(6) . ?
C69 C74 1.385(6) . ?
C69 C70 1.389(6) . ?
C70 C71 1.384(7) . ?
C70 H70A 0.9500 . ?
C71 C72 1.365(8) . ?
C71 H71A 0.9500 . ?
C72 C73 1.391(6) . ?
C72 H72A 0.9500 . ?
C73 C74 1.401(6) . ?
C73 C75 1.455(6) . ?
C74 H74A 0.9500 . ?
C75 C76 1.380(6) . ?
C76 C77 1.383(6) . ?
C76 H76A 0.9500 . ?
C77 C78 1.459(6) . ?
C78 C79 1.390(6) . ?
C79 C80 1.366(7) . ?
C79 H79A 0.9500 . ?
C80 C81 1.372(7) . ?
C80 H80A 0.9500 . ?
C81 C82 1.380(6) . ?
C81 H81A 0.9500 . ?
C82 H82A 0.9500 . ?
Si1 F5 1.670(2) . ?
Si1 F4 1.680(2) . ?
Si1 F3 1.681(2) . ?
Si1 F1 1.690(2) . ?
Si1 F6 1.697(2) . ?
Si1 F2 1.702(2) . ?
P1 F7 1.560(4) . ?
P1 F11 1.576(4) . ?
P1 F9 1.585(3) . ?
P1 F8 1.587(3) . ?
P1 F10 1.591(3) . ?
P1 F12 1.594(3) . ?
P2 F17 1.431(7) . ?
P2 F15 1.484(7) . ?
P2 F13 1.491(6) . ?
P2 F14 1.505(6) . ?
P2 F16 1.603(6) . ?
P2 F18 1.668(8) . ?
P3 F21 1.486(13) . ?
P3 F24 1.520(13) . ?
P3 F20 1.586(12) . ?
P3 F22 1.592(13) . ?
P3 F23 1.670(12) . ?
P3 F19 1.700(12) . ?
O1S C2S 1.415(7) . ?
O1S C3S 1.419(7) . ?
C1S C2S 1.513(9) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C4S 1.501(10) . ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C4S H4SA 0.9800 . ?
C4S H4SB 0.9800 . ?
C4S H4SC 0.9800 . ?

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
N14 Fe1 N2 95.90(12) . . ?
N14 Fe1 N7 163.70(13) . . ?
N2 Fe1 N7 100.03(12) . . ?
N14 Fe1 N8 100.76(11) . . ?
N2 Fe1 N8 92.03(12) . . ?
N7 Fe1 N8 75.37(11) . . ?
N14 Fe1 N13 74.18(12) . . ?
N2 Fe1 N13 161.85(12) . . ?
N7 Fe1 N13 91.30(12) . . ?
N8 Fe1 N13 104.61(12) . . ?
N14 Fe1 N1 93.70(12) . . ?
N2 Fe1 N1 74.78(13) . . ?
N7 Fe1 N1 93.78(12) . . ?
N8 Fe1 N1 161.41(13) . . ?
N13 Fe1 N1 90.47(13) . . ?
N17 Fe2 N11 93.92(13) . . ?
N17 Fe2 N5 102.55(14) . . ?
N11 Fe2 N5 92.73(14) . . ?
N17 Fe2 N6 164.07(14) . . ?
N11 Fe2 N6 101.99(14) . . ?
N5 Fe2 N6 76.08(17) . . ?
N17 Fe2 N12 88.70(14) . . ?
N11 Fe2 N12 76.52(13) . . ?
N5 Fe2 N12 165.06(14) . . ?
N6 Fe2 N12 95.78(17) . . ?
N17 Fe2 N18 75.60(13) . . ?
N11 Fe2 N18 163.83(15) . . ?
N5 Fe2 N18 101.47(14) . . ?
N6 Fe2 N18 89.04(14) . . ?
N12 Fe2 N18 90.76(14) . . ?
C1 N1 C5 117.5(4) . . ?
C1 N1 Fe1 128.2(4) . . ?
C5 N1 Fe1 114.2(3) . . ?
C6 N2 N3 105.4(3) . . ?
C6 N2 Fe1 115.4(3) . . ?
N3 N2 Fe1 133.5(3) . . ?
N2 N3 C8 111.9(3) . . ?
N2 N3 H3 119(4) . . ?
C8 N3 H3 129(4) . . ?
N5 N4 C21 112.3(4) . . ?
N5 N4 H4 120(4) . . ?
C21 N4 H4 128(4) . . ?
C23 N5 N4 105.1(4) . . ?
C23 N5 Fe2 115.7(3) . . ?
N4 N5 Fe2 139.2(3) . . ?
C28 N6 C24 117.9(6) . . ?
C28 N6 Fe2 125.1(5) . . ?
C24 N6 Fe2 115.2(3) . . ?
C31 N7 C35 117.6(3) . . ?
C31 N7 Fe1 125.7(3) . . ?
C35 N7 Fe1 116.5(2) . . ?
C36 N8 N9 104.8(3) . . ?
C36 N8 Fe1 115.5(2) . . ?
N9 N8 Fe1 138.9(2) . . ?
N8 N9 C38 112.4(3) . . ?
N8 N9 H9 119(4) . . ?
C38 N9 H9 128(4) . . ?
N11 N10 C51 111.9(3) . . ?
N11 N10 H10 118(4) . . ?
C51 N10 H10 128(4) . . ?
C53 N11 N10 105.4(3) . . ?
C53 N11 Fe2 115.8(3) . . ?
N10 N11 Fe2 137.9(3) . . ?
C54 N12 C58 117.3(4) . . ?
C54 N12 Fe2 114.2(3) . . ?
C58 N12 Fe2 127.3(3) . . ?
C61 N13 C65 117.3(4) . . ?
C61 N13 Fe1 127.5(3) . . ?
C65 N13 Fe1 114.5(3) . . ?
N15 N14 C66 105.9(3) . . ?
N15 N14 Fe1 131.0(3) . . ?
C66 N14 Fe1 115.9(2) . . ?
N14 N15 C68 112.2(3) . . ?
N14 N15 H15 119(3) . . ?
C68 N15 H15 129(3) . . ?
C75 N16 N17 112.0(3) . . ?
C75 N16 H16 137(4) . . ?
N17 N16 H16 110(4) . . ?
C77 N17 N16 105.1(4) . . ?
C77 N17 Fe2 114.1(3) . . ?
N16 N17 Fe2 131.5(3) . . ?
C82 N18 C78 118.1(4) . . ?
C82 N18 Fe2 127.8(3) . . ?
C78 N18 Fe2 113.4(3) . . ?
N1 C1 C2 123.0(5) . . ?
N1 C1 H1A 118.5 . . ?
C2 C1 H1A 118.5 . . ?
C1 C2 C3 119.1(5) . . ?
C1 C2 H2A 120.4 . . ?
C3 C2 H2A 120.4 . . ?
C4 C3 C2 119.4(5) . . ?
C4 C3 H3A 120.3 . . ?
C2 C3 H3A 120.3 . . ?
C3 C4 C5 117.9(6) . . ?
C3 C4 H4A 121.0 . . ?
C5 C4 H4A 121.0 . . ?
N1 C5 C4 123.0(4) . . ?
N1 C5 C6 115.4(4) . . ?
C4 C5 C6 121.5(5) . . ?
N2 C6 C7 110.9(4) . . ?
N2 C6 C5 116.8(4) . . ?
C7 C6 C5 132.3(4) . . ?
C8 C7 C6 104.9(4) . . ?
C8 C7 H7A 127.6 . . ?
C6 C7 H7A 127.6 . . ?
N3 C8 C7 106.9(4) . . ?
N3 C8 C9 121.3(4) . . ?
C7 C8 C9 131.4(4) . . ?
C14 C9 C10 119.3(4) . . ?
C14 C9 C8 121.5(4) . . ?
C10 C9 C8 119.0(4) . . ?
C11 C10 C9 119.2(4) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C12 C11 C10 121.3(4) . . ?
C12 C11 H11A 119.4 . . ?
C10 C11 H11A 119.4 . . ?
C11 C12 C13 120.8(5) . . ?
C11 C12 H12A 119.6 . . ?
C13 C12 H12A 119.6 . . ?
C14 C13 C12 117.6(4) . . ?
C14 C13 C15 119.5(4) . . ?
C12 C13 C15 122.8(4) . . ?
C9 C14 C13 121.8(4) . . ?
C9 C14 H14A 119.1 . . ?
C13 C14 H14A 119.1 . . ?
C20 C15 C16 117.7(4) . . ?
C20 C15 C13 119.6(4) . . ?
C16 C15 C13 122.7(4) . . ?
C17 C16 C15 120.6(5) . . ?
C17 C16 H16A 119.7 . . ?
C15 C16 H16A 119.7 . . ?
C18 C17 C16 120.7(6) . . ?
C18 C17 H17A 119.6 . . ?
C16 C17 H17A 119.6 . . ?
C17 C18 C19 119.8(5) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 119.1(5) . . ?
C20 C19 C21 120.6(5) . . ?
C18 C19 C21 120.2(4) . . ?
C19 C20 C15 122.1(5) . . ?
C19 C20 H20A 119.0 . . ?
C15 C20 H20A 119.0 . . ?
N4 C21 C22 105.9(4) . . ?
N4 C21 C19 122.3(4) . . ?
C22 C21 C19 131.7(5) . . ?
C21 C22 C23 105.4(5) . . ?
C21 C22 H22A 127.3 . . ?
C23 C22 H22A 127.3 . . ?
N5 C23 C22 111.2(4) . . ?
N5 C23 C24 118.1(5) . . ?
C22 C23 C24 130.6(5) . . ?
C25 C24 N6 121.6(5) . . ?
C25 C24 C23 125.1(6) . . ?
N6 C24 C23 113.4(5) . . ?
C24 C25 C26 120.7(8) . . ?
C24 C25 H25A 119.6 . . ?
C26 C25 H25A 119.6 . . ?
C27 C26 C25 118.9(7) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
C26 C27 C28 119.4(6) . . ?
C26 C27 H27A 120.3 . . ?
C28 C27 H27A 120.3 . . ?
N6 C28 C27 121.4(7) . . ?
N6 C28 H28A 119.3 . . ?
C27 C28 H28A 119.3 . . ?
N7 C31 C32 123.0(4) . . ?
N7 C31 H31A 118.5 . . ?
C32 C31 H31A 118.5 . . ?
C33 C32 C31 118.9(4) . . ?
C33 C32 H32A 120.5 . . ?
C31 C32 H32A 120.5 . . ?
C32 C33 C34 118.8(4) . . ?
C32 C33 H33A 120.6 . . ?
C34 C33 H33A 120.6 . . ?
C35 C34 C33 119.3(4) . . ?
C35 C34 H34A 120.4 . . ?
C33 C34 H34A 120.4 . . ?
N7 C35 C34 122.4(3) . . ?
N7 C35 C36 114.7(3) . . ?
C34 C35 C36 123.0(3) . . ?
N8 C36 C37 111.3(3) . . ?
N8 C36 C35 117.1(3) . . ?
C37 C36 C35 131.5(3) . . ?
C38 C37 C36 105.1(3) . . ?
C38 C37 H37A 127.5 . . ?
C36 C37 H37A 127.5 . . ?
N9 C38 C37 106.4(3) . . ?
N9 C38 C39 122.7(3) . . ?
C37 C38 C39 130.9(3) . . ?
C44 C39 C40 118.9(3) . . ?
C44 C39 C38 121.0(3) . . ?
C40 C39 C38 120.1(3) . . ?
C41 C40 C39 120.1(4) . . ?
C41 C40 H40A 119.9 . . ?
C39 C40 H40A 119.9 . . ?
C42 C41 C40 120.5(4) . . ?
C42 C41 H41A 119.8 . . ?
C40 C41 H41A 119.8 . . ?
C41 C42 C43 120.3(4) . . ?
C41 C42 H42A 119.9 . . ?
C43 C42 H42A 119.9 . . ?
C42 C43 C44 118.7(4) . . ?
C42 C43 C45 121.8(4) . . ?
C44 C43 C45 119.5(4) . . ?
C39 C44 C43 121.5(4) . . ?
C39 C44 H44A 119.3 . . ?
C43 C44 H44A 119.3 . . ?
C46 C45 C50 118.4(4) . . ?
C46 C45 C43 121.4(4) . . ?
C50 C45 C43 120.2(3) . . ?
C47 C46 C45 120.9(4) . . ?
C47 C46 H46A 119.6 . . ?
C45 C46 H46A 119.6 . . ?
C46 C47 C48 120.6(4) . . ?
C46 C47 H47A 119.7 . . ?
C48 C47 H47A 119.7 . . ?
C47 C48 C49 119.9(4) . . ?
C47 C48 H48A 120.0 . . ?
C49 C48 H48A 120.0 . . ?
C50 C49 C48 119.3(4) . . ?
C50 C49 C51 122.0(4) . . ?
C48 C49 C51 118.8(4) . . ?
C49 C50 C45 120.9(4) . . ?
C49 C50 H50A 119.5 . . ?
C45 C50 H50A 119.5 . . ?
N10 C51 C52 106.6(4) . . ?
N10 C51 C49 122.4(4) . . ?
C52 C51 C49 131.0(4) . . ?
C51 C52 C53 105.5(4) . . ?
C51 C52 H52A 127.2 . . ?
C53 C52 H52A 127.2 . . ?
N11 C53 C52 110.5(4) . . ?
N11 C53 C54 117.2(4) . . ?
C52 C53 C54 132.4(4) . . ?
N12 C54 C55 122.8(4) . . ?
N12 C54 C53 115.1(4) . . ?
C55 C54 C53 122.0(4) . . ?
C54 C55 C56 118.2(5) . . ?
C54 C55 H55A 120.9 . . ?
C56 C55 H55A 120.9 . . ?
C57 C56 C55 119.3(5) . . ?
C57 C56 H56A 120.3 . . ?
C55 C56 H56A 120.3 . . ?
C58 C57 C56 118.5(4) . . ?
C58 C57 H57A 120.7 . . ?
C56 C57 H57A 120.7 . . ?
N12 C58 C57 123.8(5) . . ?
N12 C58 H58A 118.1 . . ?
C57 C58 H58A 118.1 . . ?
N13 C61 C62 123.4(4) . . ?
N13 C61 H61A 118.3 . . ?
C62 C61 H61A 118.3 . . ?
C63 C62 C61 118.5(4) . . ?
C63 C62 H62A 120.7 . . ?
C61 C62 H62A 120.7 . . ?
C62 C63 C64 119.5(4) . . ?
C62 C63 H63A 120.2 . . ?
C64 C63 H63A 120.2 . . ?
C65 C64 C63 118.6(4) . . ?
C65 C64 H64A 120.7 . . ?
C63 C64 H64A 120.7 . . ?
N13 C65 C64 122.5(4) . . ?
N13 C65 C66 113.7(3) . . ?
C64 C65 C66 123.8(4) . . ?
N14 C66 C67 110.5(3) . . ?
N14 C66 C65 116.6(3) . . ?
C67 C66 C65 132.8(4) . . ?
C68 C67 C66 104.9(3) . . ?
C68 C67 H67A 127.6 . . ?
C66 C67 H67A 127.6 . . ?
N15 C68 C67 106.5(3) . . ?
N15 C68 C69 120.9(4) . . ?
C67 C68 C69 132.6(4) . . ?
C74 C69 C70 118.8(4) . . ?
C74 C69 C68 120.0(4) . . ?
C70 C69 C68 121.1(4) . . ?
C71 C70 C69 120.0(5) . . ?
C71 C70 H70A 120.0 . . ?
C69 C70 H70A 120.0 . . ?
C72 C71 C70 121.2(5) . . ?
C72 C71 H71A 119.4 . . ?
C70 C71 H71A 119.4 . . ?
C71 C72 C73 120.2(5) . . ?
C71 C72 H72A 119.9 . . ?
C73 C72 H72A 119.9 . . ?
C72 C73 C74 118.5(4) . . ?
C72 C73 C75 121.3(4) . . ?
C74 C73 C75 120.2(4) . . ?
C69 C74 C73 121.3(4) . . ?
C69 C74 H74A 119.4 . . ?
C73 C74 H74A 119.4 . . ?
N16 C75 C76 106.5(4) . . ?
N16 C75 C73 121.4(4) . . ?
C76 C75 C73 132.1(4) . . ?
C75 C76 C77 105.4(4) . . ?
C75 C76 H76A 127.3 . . ?
C77 C76 H76A 127.3 . . ?
N17 C77 C76 111.0(4) . . ?
N17 C77 C78 116.2(4) . . ?
C76 C77 C78 132.7(4) . . ?
N18 C78 C79 122.3(4) . . ?
N18 C78 C77 114.9(4) . . ?
C79 C78 C77 122.7(4) . . ?
C80 C79 C78 118.7(5) . . ?
C80 C79 H79A 120.6 . . ?
C78 C79 H79A 120.6 . . ?
C79 C80 C81 119.2(4) . . ?
C79 C80 H80A 120.4 . . ?
C81 C80 H80A 120.4 . . ?
C80 C81 C82 119.2(4) . . ?
C80 C81 H81A 120.4 . . ?
C82 C81 H81A 120.4 . . ?
N18 C82 C81 122.4(5) . . ?
N18 C82 H82A 118.8 . . ?
C81 C82 H82A 118.8 . . ?
F5 Si1 F4 89.49(11) . . ?
F5 Si1 F3 91.46(11) . . ?
F4 Si1 F3 178.16(13) . . ?
F5 Si1 F1 92.65(11) . . ?
F4 Si1 F1 88.92(11) . . ?
F3 Si1 F1 89.46(11) . . ?
F5 Si1 F6 89.55(12) . . ?
F4 Si1 F6 90.15(12) . . ?
F3 Si1 F6 91.42(12) . . ?
F1 Si1 F6 177.60(13) . . ?
F5 Si1 F2 177.46(12) . . ?
F4 Si1 F2 89.99(11) . . ?
F3 Si1 F2 89.13(11) . . ?
F1 Si1 F2 89.82(11) . . ?
F6 Si1 F2 87.96(11) . . ?
F7 P1 F11 179.9(4) . . ?
F7 P1 F9 89.6(2) . . ?
F11 P1 F9 90.4(2) . . ?
F7 P1 F8 89.1(2) . . ?
F11 P1 F8 91.0(2) . . ?
F9 P1 F8 89.84(16) . . ?
F7 P1 F10 90.7(3) . . ?
F11 P1 F10 89.2(2) . . ?
F9 P1 F10 90.08(17) . . ?
F8 P1 F10 179.8(2) . . ?
F7 P1 F12 91.6(2) . . ?
F11 P1 F12 88.4(2) . . ?
F9 P1 F12 178.5(2) . . ?
F8 P1 F12 89.33(17) . . ?
F10 P1 F12 90.76(18) . . ?
F17 P2 F15 103.8(4) . . ?
F17 P2 F13 94.8(4) . . ?
F15 P2 F13 157.2(5) . . ?
F17 P2 F14 91.3(4) . . ?
F15 P2 F14 99.0(4) . . ?
F13 P2 F14 93.7(4) . . ?
F17 P2 F16 87.8(4) . . ?
F15 P2 F16 83.1(4) . . ?
F13 P2 F16 84.6(4) . . ?
F14 P2 F16 177.9(5) . . ?
F17 P2 F18 172.5(4) . . ?
F15 P2 F18 82.2(4) . . ?
F13 P2 F18 78.4(4) . . ?
F14 P2 F18 92.2(4) . . ?
F16 P2 F18 88.6(4) . . ?
F21 P3 F24 81.4(13) . . ?
F21 P3 F20 124.1(15) . . ?
F24 P3 F20 105.2(14) . . ?
F21 P3 F22 84.0(12) . . ?
F24 P3 F22 109.8(13) . . ?
F20 P3 F22 138.0(13) . . ?
F21 P3 F23 92.7(11) . . ?
F24 P3 F23 174.1(13) . . ?
F20 P3 F23 78.8(10) . . ?
F22 P3 F23 68.4(9) . . ?
F21 P3 F19 148.4(14) . . ?
F24 P3 F19 80.9(11) . . ?
F20 P3 F19 85.9(10) . . ?
F22 P3 F19 77.7(10) . . ?
F23 P3 F19 103.9(9) . . ?
C2S O1S C3S 112.6(5) . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
O1S C2S C1S 108.6(5) . . ?
O1S C2S H2SA 110.0 . . ?
C1S C2S H2SA 110.0 . . ?
O1S C2S H2SB 110.0 . . ?
C1S C2S H2SB 110.0 . . ?
H2SA C2S H2SB 108.4 . . ?
O1S C3S C4S 109.4(5) . . ?
O1S C3S H3SA 109.8 . . ?
C4S C3S H3SA 109.8 . . ?
O1S C3S H3SB 109.8 . . ?
C4S C3S H3SB 109.8 . . ?
H3SA C3S H3SB 108.2 . . ?
C3S C4S H4SA 109.5 . . ?
C3S C4S H4SB 109.5 . . ?
H4SA C4S H4SB 109.5 . . ?
C3S C4S H4SC 109.5 . . ?
H4SA C4S H4SC 109.5 . . ?
H4SB C4S H4SC 109.5 . . ?

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 F3 0.83(5) 2.00(5) 2.782(4) 158(5) . yes
N4 H4 F6 0.93(6) 1.81(6) 2.721(4) 167(5) . yes
N9 H9 F1 0.81(5) 1.93(5) 2.736(4) 169(5) . yes
N10 H10 F5 0.87(6) 2.27(6) 3.065(4) 152(5) . yes
N15 H15 F2 0.89(5) 1.82(5) 2.713(4) 175(5) . yes
N16 H16 F4 0.82(6) 1.82(6) 2.626(4) 171(6) . yes

_refine_diff_density_max         1.479
_refine_diff_density_min         -1.383
_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_972md492
_database_code_depnum_ccdc_archive 'CCDC 2172380'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C84 H60 Fe2 N18, 4(Cl O4), 20(C2 H3 N)'
_chemical_formula_sum            'C124 H120 Cl4 Fe2 N38 O16'
_chemical_formula_weight         2652.05

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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, -y, -z'

_cell_length_a                   18.685(2)
_cell_length_b                   19.364(2)
_cell_length_c                   19.401(2)
_cell_angle_alpha                68.021(6)
_cell_angle_beta                 88.515(7)
_cell_angle_gamma                67.719(6)
_cell_volume                     5968.1(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3710
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      17.20

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.475
_exptl_crystal_F_000             2727
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.266
_exptl_crystal_size_mid          0.132
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.524
_shelx_estimated_absorpt_T_min   0.903
_shelx_estimated_absorpt_T_max   0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.555
_exptl_absorpt_correction_T_max  0.744
_exptl_absorpt_process_details   'SADABS-2008/1, Bruker AXS'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'multilayer monochromator ImuS'
_diffrn_measurement_device_type  'Bruker APEX II QUAZAR'
_diffrn_measurement_method       'φ and ω rotation with narrow frames'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18937
_diffrn_reflns_av_unetI/netI     0.0735
_diffrn_reflns_av_R_equivalents  0.0594
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.142
_diffrn_reflns_theta_max         17.324
_diffrn_reflns_theta_full        17.324
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             7187
_reflns_number_gt                4837
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 2'
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. One of the
 perchlorate ion is disordered over two positions with relative
 occupancies refining to 0.478:0.522 (for Cl4:Cl5). Due to heavy
 disorder all the perchlorate ions and lattice acetonitrile 
 molecules were refined with 1,2 and 1,3 distance restraints, as
 well as displacement parameters restraints. Displacement parameters
 restraints were also necessary to refine some of the carbon atoms 
 of the main residue. Even with these restraints, the refinement
 would not converge without some further atoms become NPD, so that
 eventually a RIGU order was applied to all atoms in the structural model.
 Hydrogens were placed geometrically where possible and refined
 with a riding model. Probably at the origin of the poor quality of the
 data, a huge void remained at the end of the
 refinement with only diffuse residual electron density. It
 was analyzed and taken into account with PLATON/SQUEEZE that 
 recovered a total of 777 electrons per cell in one large void 
 of 1853 cubic angstrom, resulting in an improvement of ca. 12%
 in R1. These figures are reasonable for 16 additional diffuse 
 acetonitrile molecules per formula unit, 32 per cell. These were 
 included in the formula, formula weight, mu and density.
;

_vrf_THETM01_972md492            
;
PROBLEM:  The value of sine(theta_max)/wavelength is less than 0.550
            Calculated sin(theta_max)/wavelength =    0.4190
RESPONSE: Diffraction decreased significantly at resolutions better
than 1.2 angstrom and the present data were cut at 1.19 angstrom
where Rsigma was above 30% and completeness dropped abruptly. This poor 
diffraction results in poor thetamax and theta full values, as well as
a poor data over parameters ratio. The weak diffraction is likely in part
to be related with the large diffuse solvent void in the structure.
;

_vrf_PLAT088_972md492            
;
PROBLEM:  Poor Data / Parameter Ratio ....................       5.63 Note  
RESPONSE: Diffraction decreased significantly at resolutions better
than 1.2 angstrom and the present data were cut at 1.19 angstrom
where Rsigma was above 30% and completeness dropped abruptly. This poor 
diffraction results in poor thetamax and theta full values, as well as
a poor data over parameters ratio. The weak diffraction is likely in part
to be related with the large diffuse solvent void in the structure.
;

_vrf_ABSMU01_972md492            
;
PROBLEM:   The ratio of given/expected absorption coefficient lies
               outside the range 0.90 <> 1.10
            Calculated value of mu =     0.415
            Value of mu given      =     0.524
RESPONSE: A large diffuse solvent void in the structure remaining at
the end of the refinement was analyzed and taken into account with
PLATON/SQUEEZE that recovered a total of 777 electrons per cell in
one large void of 1853 cubic angstrom. These figures were ascribed
to 16 additional diffuse acetonitrile molecules per formula unit,
32 per cell. These molecules were included in the formula, 
formula weight, mu and density, resulting in this discrepancy with 
the values calculated from the atomic list.
;

_vrf_CHEMW01_972md492            
;
PROBLEM:   The ratio of given/expected molecular weight as calculated
            from the _chemical_formula_sum lies outside
            the range 0.99 <> 1.01
            Calculated formula weight =  2551.2732
            Formula weight given      =  2652.0500
RESPONSE: A large diffuse solvent void in the structure remaining at
the end of the refinement was analyzed and taken into account with
PLATON/SQUEEZE that recovered a total of 777 electrons per cell in
one large void of 1853 cubic angstrom. These figures were ascribed
to 16 additional diffuse acetonitrile molecules per formula unit,
32 per cell. These molecules were included in the formula, 
formula weight, mu and density, resulting in this discrepancy with 
the values calculated from the atomic list.
;

_vrf_FORMU01_972md492            
;
PROBLEM:   There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.
RESPONSE: A large diffuse solvent void in the structure remaining at
the end of the refinement was analyzed and taken into account with
PLATON/SQUEEZE that recovered a total of 777 electrons per cell in
one large void of 1853 cubic angstrom. These figures were ascribed
to 16 additional diffuse acetonitrile molecules per formula unit,
32 per cell. These molecules were included in the formula, 
formula weight, mu and density, resulting in this discrepancy with 
the values calculated from the atomic list.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1792P)²+63.2521P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         7187
_refine_ls_number_parameters     1276
_refine_ls_number_restraints     1776
_refine_ls_R_factor_all          0.1385
_refine_ls_R_factor_gt           0.0999
_refine_ls_wR_factor_ref         0.3245
_refine_ls_wR_factor_gt          0.2821
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.006
_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 0.35968(12) 0.76863(13) -0.03752(12) 0.0326(8) Uani 1 1 d . . . . .
Fe2 Fe 0.25322(12) 0.85957(13) 0.48958(12) 0.0337(8) Uani 1 1 d . . . . .
N1 N 0.3632(7) 0.6685(7) -0.0489(6) 0.027(3) Uani 1 1 d . . . . .
N2 N 0.2707(7) 0.7573(8) 0.0129(6) 0.033(3) Uani 1 1 d . . . . .
N3 N 0.2126(7) 0.8010(8) 0.0403(6) 0.040(3) Uani 1 1 d . . . . .
H3B H 0.212299 0.842922 0.048350 0.048 Uiso 1 1 calc R U . . .
N4 N 0.1480(7) 0.9347(8) 0.3415(7) 0.042(3) Uani 1 1 d . . . . .
H4B H 0.150168 0.889747 0.338453 0.050 Uiso 1 1 calc R U . . .
N5 N 0.1892(6) 0.9383(7) 0.3966(7) 0.029(3) Uani 1 1 d . . . . .
N6 N 0.2440(7) 0.9626(7) 0.4977(7) 0.035(3) Uani 1 1 d . . . . .
N7 N 0.2880(7) 0.8468(7) -0.1300(6) 0.030(3) Uani 1 1 d . . . . .
N8 N 0.3486(6) 0.8704(7) -0.0296(7) 0.029(3) Uani 1 1 d . . . . .
N9 N 0.3810(7) 0.8901(7) 0.0178(7) 0.032(3) Uani 1 1 d . . . . .
H9A H 0.409897 0.855866 0.061188 0.039 Uiso 1 1 calc R U . . .
N10 N 0.3795(7) 0.8857(7) 0.3903(7) 0.033(3) Uani 1 1 d . . . . .
H10B H 0.349418 0.918100 0.347151 0.040 Uiso 1 1 calc R U . . .
N11 N 0.3538(7) 0.8529(7) 0.4533(7) 0.031(3) Uani 1 1 d . . . . .
N12 N 0.3246(7) 0.7872(7) 0.5863(7) 0.029(3) Uani 1 1 d . . . . .
N13 N 0.4549(7) 0.7661(7) -0.0872(7) 0.030(3) Uani 1 1 d . . . . .
N14 N 0.4406(7) 0.6985(7) 0.0505(7) 0.028(3) Uani 1 1 d . . . . .
N15 N 0.4422(7) 0.6578(7) 0.1223(7) 0.034(3) Uani 1 1 d . . . . .
H15A H 0.400834 0.658219 0.145235 0.041 Uiso 1 1 calc R U . . .
N16 N 0.3021(7) 0.7088(7) 0.4537(7) 0.037(3) Uani 1 1 d . . . . .
H16B H 0.341154 0.714187 0.428958 0.044 Uiso 1 1 calc R U . . .
N17 N 0.2532(7) 0.7635(7) 0.4784(7) 0.032(3) Uani 1 1 d . . . . .
N18 N 0.1581(7) 0.8544(7) 0.5353(6) 0.030(3) Uani 1 1 d . . . . .
C1 C 0.4164(8) 0.6222(9) -0.0769(8) 0.025(4) Uani 1 1 d . . . . .
H1A H 0.458670 0.636282 -0.095305 0.030 Uiso 1 1 calc R U . . .
C2 C 0.4121(10) 0.5540(10) -0.0801(8) 0.039(4) Uani 1 1 d . . . . .
H2A H 0.452044 0.520873 -0.099012 0.047 Uiso 1 1 calc R U . . .
C3 C 0.3518(10) 0.5340(10) -0.0565(9) 0.045(4) Uani 1 1 d . . . . .
H3A H 0.347680 0.488522 -0.061179 0.054 Uiso 1 1 calc R U . . .
C4 C 0.2960(10) 0.5795(10) -0.0255(8) 0.040(4) Uani 1 1 d . . . . .
H4A H 0.254024 0.565067 -0.006719 0.048 Uiso 1 1 calc R U . . .
C5 C 0.3031(9) 0.6473(9) -0.0227(8) 0.031(4) Uani 1 1 d . . . . .
C6 C 0.2494(9) 0.6994(10) 0.0091(8) 0.034(4) Uani 1 1 d . . . . .
C7 C 0.1773(9) 0.7077(11) 0.0351(8) 0.046(4) Uani 1 1 d . . . . .
H7A H 0.149886 0.674269 0.038726 0.056 Uiso 1 1 calc R U . . .
C8 C 0.1538(10) 0.7741(11) 0.0543(9) 0.047(4) Uani 1 1 d . . . . .
C9 C 0.0802(10) 0.8153(12) 0.0788(9) 0.062(3) Uani 1 1 d . U . . .
C10 C 0.0141(9) 0.8072(12) 0.0626(9) 0.066(3) Uani 1 1 d . U . . .
H10A H 0.017279 0.770339 0.040144 0.079 Uiso 1 1 calc R U . . .
C11 C -0.0556(10) 0.8499(13) 0.0775(10) 0.071(3) Uani 1 1 d . U . . .
H11A H -0.099767 0.838989 0.070704 0.085 Uiso 1 1 calc R U . . .
C12 C -0.0627(10) 0.9096(12) 0.1026(10) 0.069(3) Uani 1 1 d . U . . .
H12A H -0.113024 0.942579 0.108763 0.083 Uiso 1 1 calc R U . . .
C13 C 0.0021(10) 0.9231(12) 0.1194(9) 0.064(3) Uani 1 1 d . U . . .
C14 C 0.0736(10) 0.8698(11) 0.1091(9) 0.060(3) Uani 1 1 d . U . . .
H14A H 0.120155 0.872316 0.124304 0.071 Uiso 1 1 calc R U . . .
C15 C -0.0029(10) 0.9854(12) 0.1468(10) 0.065(3) Uani 1 1 d . U . . .
C16 C -0.0619(10) 1.0628(12) 0.1196(10) 0.071(3) Uani 1 1 d . U . . .
H16A H -0.102772 1.074031 0.083826 0.085 Uiso 1 1 calc R U . . .
C17 C -0.0657(10) 1.1238(13) 0.1400(10) 0.071(4) Uani 1 1 d . U . . .
H17A H -0.104778 1.177028 0.115718 0.085 Uiso 1 1 calc R U . . .
C18 C -0.0115(9) 1.1060(12) 0.1967(9) 0.067(4) Uani 1 1 d . U . . .
H18A H -0.014827 1.147075 0.213727 0.080 Uiso 1 1 calc R U . . .
C19 C 0.0470(10) 1.0313(12) 0.2295(10) 0.061(3) Uani 1 1 d . U . . .
C20 C 0.0512(9) 0.9720(12) 0.2036(9) 0.061(3) Uani 1 1 d . U . . .
H20A H 0.092745 0.920015 0.225686 0.073 Uiso 1 1 calc R U . . .
C21 C 0.1015(9) 1.0141(10) 0.2904(9) 0.040(4) Uani 1 1 d . . . . .
C22 C 0.1179(9) 1.0642(10) 0.3157(9) 0.041(4) Uani 1 1 d . . . . .
H22A H 0.097440 1.121763 0.292498 0.049 Uiso 1 1 calc R U . . .
C23 C 0.1689(8) 1.0164(9) 0.3807(9) 0.031(4) Uani 1 1 d . . . . .
C24 C 0.2026(9) 1.0317(10) 0.4366(9) 0.040(4) Uani 1 1 d . . . . .
C25 C 0.1950(11) 1.1065(11) 0.4337(10) 0.062(5) Uani 1 1 d . . . . .
H25A H 0.167579 1.154198 0.390427 0.075 Uiso 1 1 calc R U . . .
C26 C 0.2266(12) 1.1119(12) 0.4924(11) 0.072(6) Uani 1 1 d . . . . .
H26A H 0.220029 1.163868 0.490051 0.087 Uiso 1 1 calc R U . . .
C27 C 0.2678(11) 1.0447(11) 0.5550(10) 0.059(5) Uani 1 1 d . . . . .
H27A H 0.289373 1.048769 0.596445 0.071 Uiso 1 1 calc R U . . .
C28 C 0.2766(9) 0.9700(10) 0.5550(9) 0.042(4) Uani 1 1 d . . . . .
H28A H 0.306694 0.922045 0.596893 0.051 Uiso 1 1 calc R U . . .
C29 C 0.2551(9) 0.8314(11) -0.1805(9) 0.043(4) Uani 1 1 d . . . . .
H29A H 0.263581 0.777041 -0.171718 0.052 Uiso 1 1 calc R U . . .
C30 C 0.2079(9) 0.8959(11) -0.2469(9) 0.048(5) Uani 1 1 d . . . . .
H30A H 0.185330 0.883433 -0.281574 0.058 Uiso 1 1 calc R U . . .
C31 C 0.1939(9) 0.9740(11) -0.2624(10) 0.052(5) Uani 1 1 d . . . . .
H31A H 0.163991 1.016357 -0.307979 0.063 Uiso 1 1 calc R U . . .
C32 C 0.2250(9) 0.9896(10) -0.2088(8) 0.040(4) Uani 1 1 d . . . . .
H32A H 0.214023 1.044190 -0.216110 0.048 Uiso 1 1 calc R U . . .
C33 C 0.2700(8) 0.9294(9) -0.1473(8) 0.025(4) Uani 1 1 d . . . . .
C34 C 0.3061(8) 0.9389(9) -0.0856(8) 0.027(4) Uani 1 1 d . . . . .
C35 C 0.3148(8) 1.0042(9) -0.0792(8) 0.029(4) Uani 1 1 d . U . . .
H35A H 0.293078 1.059431 -0.113344 0.034 Uiso 1 1 calc R U . . .
C36 C 0.3615(8) 0.9711(9) -0.0125(8) 0.028(4) Uani 1 1 d . . . . .
C37 C 0.3941(8) 1.0112(9) 0.0228(9) 0.032(4) Uani 1 1 d . . . . .
C38 C 0.3956(9) 1.0850(10) -0.0190(10) 0.044(4) Uani 1 1 d . . . . .
H38A H 0.372592 1.111296 -0.070048 0.053 Uiso 1 1 calc R U . . .
C39 C 0.4287(9) 1.1230(9) 0.0091(9) 0.041(4) Uani 1 1 d . . . . .
H39A H 0.428688 1.174616 -0.021136 0.049 Uiso 1 1 calc R U . . .
C40 C 0.4629(9) 1.0819(9) 0.0852(9) 0.040(4) Uani 1 1 d . . . . .
H40A H 0.487314 1.106035 0.106039 0.048 Uiso 1 1 calc R U . . .
C41 C 0.4618(8) 1.0096(9) 0.1288(9) 0.030(4) Uani 1 1 d . . . . .
C42 C 0.4257(8) 0.9720(10) 0.1013(9) 0.035(4) Uani 1 1 d . . . . .
H42A H 0.421987 0.922665 0.132966 0.042 Uiso 1 1 calc R U . . .
C43 C 0.4995(9) 0.9680(9) 0.2081(9) 0.036(4) Uani 1 1 d . . . . .
C44 C 0.5739(9) 0.9655(10) 0.2275(10) 0.047(5) Uani 1 1 d . . . . .
H44A H 0.600455 0.988780 0.189163 0.056 Uiso 1 1 calc R U . . .
C45 C 0.6063(10) 0.9313(10) 0.2983(10) 0.049(5) Uani 1 1 d . . . . .
H45A H 0.656415 0.929211 0.309532 0.059 Uiso 1 1 calc R U . . .
C46 C 0.5698(9) 0.8989(11) 0.3557(10) 0.050(5) Uani 1 1 d . . . . .
H46A H 0.592954 0.877483 0.406268 0.060 Uiso 1 1 calc R U . . .
C47 C 0.4969(9) 0.8976(9) 0.3391(9) 0.034(4) Uani 1 1 d . . . . .
C48 C 0.4653(9) 0.9304(9) 0.2662(9) 0.035(4) Uani 1 1 d . . . . .
H48A H 0.417745 0.927355 0.254591 0.042 Uiso 1 1 calc R U . . .
C49 C 0.4569(9) 0.8636(9) 0.4001(9) 0.034(4) Uani 1 1 d . . . . .
C50 C 0.4838(9) 0.8144(9) 0.4755(9) 0.037(4) Uani 1 1 d . . . . .
H50A H 0.535561 0.791113 0.500419 0.044 Uiso 1 1 calc R U . . .
C51 C 0.4178(9) 0.8072(9) 0.5060(9) 0.033(4) Uani 1 1 d . . . . .
C52 C 0.4023(9) 0.7707(9) 0.5807(9) 0.034(4) Uani 1 1 d . . . . .
C53 C 0.4585(9) 0.7213(9) 0.6435(9) 0.043(4) Uani 1 1 d . . . . .
H53A H 0.512172 0.710347 0.639445 0.052 Uiso 1 1 calc R U . . .
C54 C 0.4348(9) 0.6883(10) 0.7127(9) 0.045(5) Uani 1 1 d . . . . .
H54A H 0.472315 0.654150 0.756195 0.054 Uiso 1 1 calc R U . . .
C55 C 0.3570(9) 0.7054(10) 0.7175(9) 0.047(5) Uani 1 1 d . . . . .
H55A H 0.339548 0.683327 0.763865 0.057 Uiso 1 1 calc R U . . .
C56 C 0.3048(9) 0.7561(9) 0.6522(9) 0.035(4) Uani 1 1 d . . . . .
H56A H 0.250777 0.768970 0.655756 0.042 Uiso 1 1 calc R U . . .
C57 C 0.4585(10) 0.7982(9) -0.1621(9) 0.039(4) Uani 1 1 d . . . . .
H57A H 0.410592 0.830487 -0.194834 0.047 Uiso 1 1 calc R U . . .
C58 C 0.5267(10) 0.7870(10) -0.1937(10) 0.053(5) Uani 1 1 d . . . . .
H58A H 0.526524 0.810743 -0.246395 0.064 Uiso 1 1 calc R U . . .
C59 C 0.5977(11) 0.7380(12) -0.1432(10) 0.066(6) Uani 1 1 d . . . . .
H59A H 0.646566 0.726284 -0.161732 0.080 Uiso 1 1 calc R U . . .
C60 C 0.5944(9) 0.7086(10) -0.0693(10) 0.048(5) Uani 1 1 d . . . . .
H60A H 0.641634 0.679184 -0.035556 0.057 Uiso 1 1 calc R U . . .
C61 C 0.5230(9) 0.7201(9) -0.0402(9) 0.029(4) Uani 1 1 d . . . . .
C62 C 0.5132(9) 0.6850(9) 0.0368(9) 0.026(4) Uani 1 1 d . . . . .
C63 C 0.5636(10) 0.6338(9) 0.1025(9) 0.037(4) Uani 1 1 d . . . . .
H63A H 0.618884 0.615308 0.109331 0.044 Uiso 1 1 calc R U . . .
C64 C 0.5167(10) 0.6153(9) 0.1555(9) 0.038(4) Uani 1 1 d . . . . .
C65 C 0.5347(11) 0.5587(10) 0.2373(9) 0.048(4) Uani 1 1 d . . . . .
C66 C 0.6111(11) 0.5024(10) 0.2635(10) 0.058(5) Uani 1 1 d . . . . .
H66A H 0.651035 0.503396 0.232283 0.069 Uiso 1 1 calc R U . . .
C67 C 0.6273(13) 0.4461(11) 0.3345(11) 0.082(5) Uani 1 1 d . U . . .
H67A H 0.679632 0.408296 0.353349 0.098 Uiso 1 1 calc R U . . .
C68 C 0.5721(13) 0.4419(11) 0.3790(11) 0.077(4) Uani 1 1 d . U . . .
H68A H 0.584651 0.398090 0.426687 0.093 Uiso 1 1 calc R U . . .
C69 C 0.4958(12) 0.5017(11) 0.3559(10) 0.069(4) Uani 1 1 d . U . . .
C70 C 0.4780(10) 0.5596(9) 0.2829(9) 0.044(4) Uani 1 1 d . . . . .
H70A H 0.426394 0.599844 0.264805 0.053 Uiso 1 1 calc R U . . .
C71 C 0.4366(13) 0.5001(11) 0.4039(11) 0.080(4) Uani 1 1 d . U . . .
C72 C 0.4298(14) 0.4262(12) 0.4463(12) 0.094(4) Uani 1 1 d . U . . .
H72A H 0.464278 0.376951 0.443162 0.113 Uiso 1 1 calc R U . . .
C73 C 0.3704(14) 0.4267(13) 0.4939(12) 0.097(4) Uani 1 1 d . U . . .
H73A H 0.363489 0.377977 0.521251 0.116 Uiso 1 1 calc R U . . .
C74 C 0.3259(14) 0.4936(12) 0.4997(12) 0.093(4) Uani 1 1 d . U . . .
H74A H 0.288512 0.491420 0.533729 0.112 Uiso 1 1 calc R U . . .
C75 C 0.3291(14) 0.5705(12) 0.4585(11) 0.081(5) Uani 1 1 d . U . . .
C76 C 0.3874(10) 0.5693(10) 0.4133(9) 0.053(5) Uani 1 1 d . . . . .
H76A H 0.394032 0.618399 0.387304 0.064 Uiso 1 1 calc R U . . .
C77 C 0.2819(11) 0.6422(11) 0.4729(10) 0.056(5) Uani 1 1 d . . . . .
C78 C 0.2185(10) 0.6586(10) 0.5149(9) 0.052(5) Uani 1 1 d . . . . .
H78A H 0.192102 0.624276 0.538450 0.062 Uiso 1 1 calc R U . . .
C79 C 0.2031(9) 0.7341(10) 0.5145(9) 0.033(4) Uani 1 1 d . . . . .
C80 C 0.1481(9) 0.7850(10) 0.5457(9) 0.037(4) Uani 1 1 d . . . . .
C81 C 0.0894(10) 0.7668(11) 0.5879(9) 0.051(5) Uani 1 1 d . . . . .
H81A H 0.085003 0.716583 0.598711 0.062 Uiso 1 1 calc R U . . .
C82 C 0.0406(10) 0.8215(11) 0.6119(10) 0.055(5) Uani 1 1 d . . . . .
H82A H -0.000146 0.810910 0.638327 0.066 Uiso 1 1 calc R U . . .
C83 C 0.0486(10) 0.8925(11) 0.5988(9) 0.048(5) Uani 1 1 d . . . . .
H83A H 0.013569 0.931626 0.615466 0.058 Uiso 1 1 calc R U . . .
C84 C 0.1085(9) 0.9062(9) 0.5609(8) 0.032(4) Uani 1 1 d . . . . .
H84A H 0.114520 0.955103 0.552682 0.039 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3278(4) 0.8093(4) 0.2590(3) 0.101(2) Uani 1 1 d D U . . .
O1 O 0.2700(9) 0.7815(9) 0.2634(9) 0.166(5) Uani 1 1 d D U . . .
O2 O 0.2993(8) 0.8888(7) 0.2511(7) 0.094(3) Uani 1 1 d D U . . .
O3 O 0.3824(7) 0.7608(7) 0.3253(6) 0.088(4) Uani 1 1 d D U . . .
O4 O 0.3696(10) 0.8012(9) 0.1992(7) 0.154(5) Uani 1 1 d D U . . .
Cl2 Cl 0.2959(4) 0.2971(4) 0.3895(4) 0.131(3) Uani 1 1 d D U . . .
O5 O 0.2434(10) 0.3727(9) 0.3871(11) 0.191(6) Uani 1 1 d D U . . .
O6 O 0.3236(8) 0.2422(9) 0.4636(7) 0.132(5) Uani 1 1 d D U . . .
O7 O 0.2530(9) 0.2681(9) 0.3572(9) 0.171(6) Uani 1 1 d D U . . .
O8 O 0.3562(8) 0.3052(10) 0.3515(9) 0.194(7) Uani 1 1 d D U . . .
Cl3 Cl 0.1762(4) 0.4451(4) 0.0095(4) 0.121(2) Uani 1 1 d D U . . .
O9 O 0.1563(7) 0.5149(8) 0.0289(8) 0.120(4) Uani 1 1 d D U . . .
O10 O 0.1077(8) 0.4550(9) -0.0322(10) 0.161(5) Uani 1 1 d D U . . .
O11 O 0.2372(8) 0.4426(8) -0.0385(8) 0.117(4) Uani 1 1 d D U . . .
O12 O 0.2025(9) 0.3719(8) 0.0753(9) 0.168(6) Uani 1 1 d D U . . .
Cl4 Cl 0.8645(10) 0.5148(9) 0.3466(10) 0.123(4) Uani 0.478(11) 1 d D U P A 1
O13 O 0.8933(19) 0.4352(17) 0.3876(18) 0.130(6) Uani 0.478(11) 1 d D U P A 1
O14 O 0.9050(18) 0.5294(18) 0.2894(17) 0.137(6) Uani 0.478(11) 1 d D U P A 1
O15 O 0.8663(19) 0.5543(18) 0.3879(17) 0.147(6) Uani 0.478(11) 1 d D U P A 1
O16 O 0.7905(15) 0.538(2) 0.3186(19) 0.129(5) Uani 0.478(11) 1 d D U P A 1
Cl5 Cl 0.8184(9) 0.5231(10) 0.3081(10) 0.126(4) Uani 0.522(11) 1 d D U P A 2
O17 O 0.8610(16) 0.4420(15) 0.3541(16) 0.129(6) Uani 0.522(11) 1 d D U P A 2
O18 O 0.8682(15) 0.5605(17) 0.2743(17) 0.138(6) Uani 0.522(11) 1 d D U P A 2
O19 O 0.7736(16) 0.5635(16) 0.3511(15) 0.133(6) Uani 0.522(11) 1 d D U P A 2
O20 O 0.7681(16) 0.5287(17) 0.2524(16) 0.137(6) Uani 0.522(11) 1 d D U P A 2
N1S N 0.5374(12) 0.0884(12) 0.3835(12) 0.092(7) Uani 1 1 d D . . . .
C1S C 0.4826(14) 0.0799(15) 0.3955(12) 0.081(8) Uani 1 1 d D . . . .
C2S C 0.4125(12) 0.0656(12) 0.4120(13) 0.099(8) Uani 1 1 d D . . . .
H2S1 H 0.414108 0.040195 0.466444 0.149 Uiso 1 1 calc R U . . .
H2S2 H 0.408790 0.029535 0.389071 0.149 Uiso 1 1 calc R U . . .
H2S3 H 0.366863 0.117380 0.391656 0.149 Uiso 1 1 calc R U . . .
N2S N 0.2087(9) 0.9485(11) 0.0591(10) 0.077(5) Uani 1 1 d D . . . .
C3S C 0.2049(12) 0.9946(12) 0.0808(12) 0.073(7) Uani 1 1 d D . . . .
C4S C 0.1973(12) 1.0582(12) 0.1064(12) 0.093(7) Uani 1 1 d D . . . .
H4S1 H 0.224503 1.091030 0.075888 0.140 Uiso 1 1 calc R U . . .
H4S2 H 0.220384 1.033685 0.159085 0.140 Uiso 1 1 calc R U . . .
H4S3 H 0.141947 1.092797 0.101528 0.140 Uiso 1 1 calc R U . . .
N3S N 0.1830(11) 0.7125(11) -0.2137(10) 0.085(5) Uani 1 1 d D U . . .
C5S C 0.1644(15) 0.6644(14) -0.2097(14) 0.095(6) Uani 1 1 d D U . . .
C6S C 0.1363(14) 0.6036(13) -0.2077(14) 0.127(7) Uani 1 1 d D U . . .
H6S1 H 0.099205 0.624905 -0.252801 0.190 Uiso 1 1 calc R U . . .
H6S2 H 0.110194 0.589906 -0.163086 0.190 Uiso 1 1 calc R U . . .
H6S3 H 0.180409 0.554717 -0.205808 0.190 Uiso 1 1 calc R U . . .
N4S N 0.2934(10) 0.0627(11) 0.2699(10) 0.083(5) Uani 1 1 d D U . . .
C7S C 0.2656(13) 0.1291(13) 0.2384(14) 0.101(7) Uani 1 1 d D U . . .
C8S C 0.2264(13) 0.2165(11) 0.2168(15) 0.138(9) Uani 1 1 d D U . . .
H8S1 H 0.170583 0.231071 0.220685 0.208 Uiso 1 1 calc R U . . .
H8S2 H 0.233194 0.244679 0.164981 0.208 Uiso 1 1 calc R U . . .
H8S3 H 0.248892 0.232649 0.250237 0.208 Uiso 1 1 calc R U . . .


_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 1.950(13) . ?
Fe1 N7 1.964(12) . ?
Fe1 N8 1.967(12) . ?
Fe1 N14 1.971(13) . ?
Fe1 N13 1.994(12) . ?
Fe1 N1 2.009(12) . ?
Fe2 N5 1.918(12) . ?
Fe2 N17 1.952(13) . ?
Fe2 N11 1.964(12) . ?
Fe2 N18 1.986(12) . ?
Fe2 N6 2.002(12) . ?
Fe2 N12 2.003(12) . ?
N1 C1 1.322(16) . ?
N1 C5 1.362(18) . ?
N2 N3 1.336(15) . ?
N2 C6 1.350(18) . ?
N3 C8 1.37(2) . ?
N3 H3B 0.8800 . ?
N4 N5 1.372(16) . ?
N4 C21 1.411(19) . ?
N4 H4B 0.8800 . ?
N5 C23 1.323(17) . ?
N6 C28 1.358(18) . ?
N6 C24 1.367(19) . ?
N7 C29 1.348(17) . ?
N7 C33 1.407(17) . ?
N8 C34 1.318(17) . ?
N8 N9 1.349(15) . ?
N9 C36 1.351(17) . ?
N9 H9A 0.8800 . ?
N10 N11 1.322(15) . ?
N10 C49 1.340(17) . ?
N10 H10B 0.8800 . ?
N11 C51 1.357(18) . ?
N12 C56 1.305(17) . ?
N12 C52 1.374(18) . ?
N13 C61 1.355(17) . ?
N13 C57 1.362(18) . ?
N14 N15 1.314(15) . ?
N14 C62 1.322(17) . ?
N15 C64 1.347(18) . ?
N15 H15A 0.8800 . ?
N16 N17 1.346(15) . ?
N16 C77 1.39(2) . ?
N16 H16B 0.8800 . ?
N17 C79 1.328(18) . ?
N18 C84 1.324(17) . ?
N18 C80 1.366(18) . ?
C1 C2 1.377(19) . ?
C1 H1A 0.9500 . ?
C2 C3 1.34(2) . ?
C2 H2A 0.9500 . ?
C3 C4 1.38(2) . ?
C3 H3A 0.9500 . ?
C4 C5 1.39(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.44(2) . ?
C6 C7 1.40(2) . ?
C7 C8 1.38(2) . ?
C7 H7A 0.9500 . ?
C8 C9 1.47(2) . ?
C9 C14 1.36(2) . ?
C9 C10 1.36(2) . ?
C10 C11 1.34(2) . ?
C10 H10A 0.9500 . ?
C11 C12 1.37(2) . ?
C11 H11A 0.9500 . ?
C12 C13 1.40(2) . ?
C12 H12A 0.9500 . ?
C13 C14 1.41(2) . ?
C13 C15 1.46(2) . ?
C14 H14A 0.9500 . ?
C15 C16 1.39(2) . ?
C15 C20 1.40(2) . ?
C16 C17 1.36(2) . ?
C16 H16A 0.9500 . ?
C17 C18 1.37(2) . ?
C17 H17A 0.9500 . ?
C18 C19 1.36(2) . ?
C18 H18A 0.9500 . ?
C19 C20 1.39(2) . ?
C19 C21 1.43(2) . ?
C20 H20A 0.9500 . ?
C21 C22 1.37(2) . ?
C22 C23 1.37(2) . ?
C22 H22A 0.9500 . ?
C23 C24 1.44(2) . ?
C24 C25 1.38(2) . ?
C25 C26 1.35(2) . ?
C25 H25A 0.9500 . ?
C26 C27 1.37(2) . ?
C26 H26A 0.9500 . ?
C27 C28 1.39(2) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C29 C30 1.42(2) . ?
C29 H29A 0.9500 . ?
C30 C31 1.34(2) . ?
C30 H30A 0.9500 . ?
C31 C32 1.38(2) . ?
C31 H31A 0.9500 . ?
C32 C33 1.326(19) . ?
C32 H32A 0.9500 . ?
C33 C34 1.49(2) . ?
C34 C35 1.382(19) . ?
C35 C36 1.364(19) . ?
C35 H35A 0.9500 . ?
C36 C37 1.49(2) . ?
C37 C38 1.36(2) . ?
C37 C42 1.44(2) . ?
C38 C39 1.37(2) . ?
C38 H38A 0.9500 . ?
C39 C40 1.42(2) . ?
C39 H39A 0.9500 . ?
C40 C41 1.35(2) . ?
C40 H40A 0.9500 . ?
C41 C42 1.398(19) . ?
C41 C43 1.49(2) . ?
C42 H42A 0.9500 . ?
C43 C48 1.38(2) . ?
C43 C44 1.43(2) . ?
C44 C45 1.32(2) . ?
C44 H44A 0.9500 . ?
C45 C46 1.36(2) . ?
C45 H45A 0.9500 . ?
C46 C47 1.42(2) . ?
C46 H46A 0.9500 . ?
C47 C48 1.36(2) . ?
C47 C49 1.46(2) . ?
C48 H48A 0.9500 . ?
C49 C50 1.39(2) . ?
C50 C51 1.39(2) . ?
C50 H50A 0.9500 . ?
C51 C52 1.43(2) . ?
C52 C53 1.39(2) . ?
C53 C54 1.40(2) . ?
C53 H53A 0.9500 . ?
C54 C55 1.37(2) . ?
C54 H54A 0.9500 . ?
C55 C56 1.39(2) . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
C57 C58 1.38(2) . ?
C57 H57A 0.9500 . ?
C58 C59 1.43(2) . ?
C58 H58A 0.9500 . ?
C59 C60 1.34(2) . ?
C59 H59A 0.9500 . ?
C60 C61 1.40(2) . ?
C60 H60A 0.9500 . ?
C61 C62 1.43(2) . ?
C62 C63 1.38(2) . ?
C63 C64 1.37(2) . ?
C63 H63A 0.9500 . ?
C64 C65 1.51(2) . ?
C65 C70 1.36(2) . ?
C65 C66 1.39(2) . ?
C66 C67 1.35(2) . ?
C66 H66A 0.9500 . ?
C67 C68 1.33(3) . ?
C67 H67A 0.9500 . ?
C68 C69 1.40(3) . ?
C68 H68A 0.9500 . ?
C69 C70 1.39(2) . ?
C69 C71 1.43(3) . ?
C70 H70A 0.9500 . ?
C71 C76 1.38(2) . ?
C71 C72 1.41(3) . ?
C72 C73 1.43(3) . ?
C72 H72A 0.9500 . ?
C73 C74 1.29(2) . ?
C73 H73A 0.9500 . ?
C74 C75 1.43(3) . ?
C74 H74A 0.9500 . ?
C75 C76 1.38(2) . ?
C75 C77 1.46(3) . ?
C76 H76A 0.9500 . ?
C77 C78 1.42(2) . ?
C78 C79 1.38(2) . ?
C78 H78A 0.9500 . ?
C79 C80 1.43(2) . ?
C80 C81 1.42(2) . ?
C81 C82 1.34(2) . ?
C81 H81A 0.9500 . ?
C82 C83 1.37(2) . ?
C82 H82A 0.9500 . ?
C83 C84 1.38(2) . ?
C83 H83A 0.9500 . ?
C84 H84A 0.9500 . ?
Cl1 O1 1.367(12) . ?
Cl1 O2 1.371(11) . ?
Cl1 O4 1.406(12) . ?
Cl1 O3 1.419(11) . ?
Cl2 O8 1.358(13) . ?
Cl2 O6 1.394(12) . ?
Cl2 O5 1.402(13) . ?
Cl2 O7 1.407(13) . ?
Cl3 O12 1.425(12) . ?
Cl3 O10 1.443(12) . ?
Cl3 O9 1.450(12) . ?
Cl3 O11 1.451(12) . ?
Cl4 O15 1.31(2) . ?
Cl4 O14 1.33(2) . ?
Cl4 O13 1.33(2) . ?
Cl4 O16 1.34(2) . ?
Cl5 O17 1.39(2) . ?
Cl5 O20 1.40(2) . ?
Cl5 O18 1.40(2) . ?
Cl5 O19 1.40(2) . ?
N1S C1S 1.102(16) . ?
C1S C2S 1.444(18) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
N2S C3S 1.101(15) . ?
C3S C4S 1.450(18) . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
N3S C5S 1.088(15) . ?
C5S C6S 1.450(18) . ?
C6S H6S1 0.9800 . ?
C6S H6S2 0.9800 . ?
C6S H6S3 0.9800 . ?
N4S C7S 1.104(15) . ?
C7S C8S 1.457(19) . ?
C8S H8S1 0.9800 . ?
C8S H8S2 0.9800 . ?
C8S H8S3 0.9800 . ?

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 N7 89.4(5) . . ?
N2 Fe1 N8 97.0(5) . . ?
N7 Fe1 N8 80.6(5) . . ?
N2 Fe1 N14 97.3(5) . . ?
N7 Fe1 N14 172.3(5) . . ?
N8 Fe1 N14 94.6(5) . . ?
N2 Fe1 N13 173.0(5) . . ?
N7 Fe1 N13 93.6(5) . . ?
N8 Fe1 N13 89.7(5) . . ?
N14 Fe1 N13 80.2(5) . . ?
N2 Fe1 N1 80.7(5) . . ?
N7 Fe1 N1 96.1(5) . . ?
N8 Fe1 N1 176.0(5) . . ?
N14 Fe1 N1 88.9(4) . . ?
N13 Fe1 N1 92.7(5) . . ?
N5 Fe2 N17 97.1(5) . . ?
N5 Fe2 N11 96.2(5) . . ?
N17 Fe2 N11 96.6(5) . . ?
N5 Fe2 N18 89.7(5) . . ?
N17 Fe2 N18 80.4(5) . . ?
N11 Fe2 N18 173.6(5) . . ?
N5 Fe2 N6 79.4(5) . . ?
N17 Fe2 N6 175.4(5) . . ?
N11 Fe2 N6 86.9(5) . . ?
N18 Fe2 N6 96.4(5) . . ?
N5 Fe2 N12 173.3(5) . . ?
N17 Fe2 N12 89.2(5) . . ?
N11 Fe2 N12 80.5(5) . . ?
N18 Fe2 N12 93.8(5) . . ?
N6 Fe2 N12 94.5(5) . . ?
C1 N1 C5 118.4(13) . . ?
C1 N1 Fe1 128.0(11) . . ?
C5 N1 Fe1 113.6(10) . . ?
N3 N2 C6 105.2(13) . . ?
N3 N2 Fe1 137.1(11) . . ?
C6 N2 Fe1 116.2(11) . . ?
N2 N3 C8 113.1(14) . . ?
N2 N3 H3B 123.4 . . ?
C8 N3 H3B 123.4 . . ?
N5 N4 C21 109.6(13) . . ?
N5 N4 H4B 125.2 . . ?
C21 N4 H4B 125.2 . . ?
C23 N5 N4 105.9(12) . . ?
C23 N5 Fe2 119.3(11) . . ?
N4 N5 Fe2 134.3(10) . . ?
C28 N6 C24 118.2(14) . . ?
C28 N6 Fe2 127.2(11) . . ?
C24 N6 Fe2 114.6(10) . . ?
C29 N7 C33 115.3(13) . . ?
C29 N7 Fe1 128.2(11) . . ?
C33 N7 Fe1 116.4(9) . . ?
C34 N8 N9 106.9(12) . . ?
C34 N8 Fe1 117.4(10) . . ?
N9 N8 Fe1 135.3(10) . . ?
N8 N9 C36 108.6(12) . . ?
N8 N9 H9A 125.7 . . ?
C36 N9 H9A 125.7 . . ?
N11 N10 C49 111.9(13) . . ?
N11 N10 H10B 124.1 . . ?
C49 N10 H10B 124.1 . . ?
N10 N11 C51 105.8(12) . . ?
N10 N11 Fe2 138.1(10) . . ?
C51 N11 Fe2 115.9(11) . . ?
C56 N12 C52 118.4(13) . . ?
C56 N12 Fe2 127.0(10) . . ?
C52 N12 Fe2 114.6(10) . . ?
C61 N13 C57 118.0(13) . . ?
C61 N13 Fe1 114.5(10) . . ?
C57 N13 Fe1 127.1(10) . . ?
N15 N14 C62 108.2(13) . . ?
N15 N14 Fe1 136.3(10) . . ?
C62 N14 Fe1 115.5(11) . . ?
N14 N15 C64 109.6(14) . . ?
N14 N15 H15A 125.2 . . ?
C64 N15 H15A 125.2 . . ?
N17 N16 C77 110.0(14) . . ?
N17 N16 H16B 125.0 . . ?
C77 N16 H16B 125.0 . . ?
C79 N17 N16 108.1(13) . . ?
C79 N17 Fe2 115.9(11) . . ?
N16 N17 Fe2 134.6(10) . . ?
C84 N18 C80 118.2(14) . . ?
C84 N18 Fe2 127.9(11) . . ?
C80 N18 Fe2 113.7(10) . . ?
N1 C1 C2 121.7(15) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C3 C2 C1 120.3(16) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 119.9(16) . . ?
C2 C3 H3A 120.0 . . ?
C4 C3 H3A 120.0 . . ?
C3 C4 C5 117.8(16) . . ?
C3 C4 H4A 121.1 . . ?
C5 C4 H4A 121.1 . . ?
N1 C5 C4 121.8(14) . . ?
N1 C5 C6 114.8(14) . . ?
C4 C5 C6 123.4(15) . . ?
N2 C6 C7 110.1(15) . . ?
N2 C6 C5 114.1(15) . . ?
C7 C6 C5 135.7(16) . . ?
C8 C7 C6 106.6(16) . . ?
C8 C7 H7A 126.7 . . ?
C6 C7 H7A 126.7 . . ?
N3 C8 C7 105.0(15) . . ?
N3 C8 C9 124.2(17) . . ?
C7 C8 C9 130.7(17) . . ?
C14 C9 C10 117.8(17) . . ?
C14 C9 C8 121.5(17) . . ?
C10 C9 C8 120.1(17) . . ?
C11 C10 C9 121.9(19) . . ?
C11 C10 H10A 119.1 . . ?
C9 C10 H10A 119.1 . . ?
C10 C11 C12 119.7(19) . . ?
C10 C11 H11A 120.1 . . ?
C12 C11 H11A 120.1 . . ?
C11 C12 C13 121.9(18) . . ?
C11 C12 H12A 119.0 . . ?
C13 C12 H12A 119.0 . . ?
C12 C13 C14 114.0(18) . . ?
C12 C13 C15 123.6(17) . . ?
C14 C13 C15 122.4(17) . . ?
C9 C14 C13 124.2(17) . . ?
C9 C14 H14A 117.9 . . ?
C13 C14 H14A 117.9 . . ?
C16 C15 C20 113.7(18) . . ?
C16 C15 C13 123.5(17) . . ?
C20 C15 C13 122.9(16) . . ?
C17 C16 C15 125.2(18) . . ?
C17 C16 H16A 117.4 . . ?
C15 C16 H16A 117.4 . . ?
C16 C17 C18 117.8(18) . . ?
C16 C17 H17A 121.1 . . ?
C18 C17 H17A 121.1 . . ?
C19 C18 C17 121.8(19) . . ?
C19 C18 H18A 119.1 . . ?
C17 C18 H18A 119.1 . . ?
C18 C19 C20 118.3(17) . . ?
C18 C19 C21 120.2(18) . . ?
C20 C19 C21 121.4(16) . . ?
C19 C20 C15 123.1(17) . . ?
C19 C20 H20A 118.5 . . ?
C15 C20 H20A 118.5 . . ?
C22 C21 N4 105.1(14) . . ?
C22 C21 C19 131.4(16) . . ?
N4 C21 C19 123.4(16) . . ?
C21 C22 C23 107.7(15) . . ?
C21 C22 H22A 126.1 . . ?
C23 C22 H22A 126.1 . . ?
N5 C23 C22 111.6(15) . . ?
N5 C23 C24 113.4(15) . . ?
C22 C23 C24 134.9(16) . . ?
N6 C24 C25 120.3(15) . . ?
N6 C24 C23 113.1(15) . . ?
C25 C24 C23 126.5(16) . . ?
C26 C25 C24 119.9(18) . . ?
C26 C25 H25A 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C25 C26 C27 121.9(19) . . ?
C25 C26 H26A 119.0 . . ?
C27 C26 H26A 119.0 . . ?
C26 C27 C28 116.6(17) . . ?
C26 C27 H27A 121.7 . . ?
C28 C27 H27A 121.7 . . ?
N6 C28 C27 123.0(16) . . ?
N6 C28 H28A 118.5 . . ?
C27 C28 H28A 118.5 . . ?
N7 C29 C30 120.4(15) . . ?
N7 C29 H29A 119.8 . . ?
C30 C29 H29A 119.8 . . ?
C31 C30 C29 122.4(16) . . ?
C31 C30 H30A 118.8 . . ?
C29 C30 H30A 118.8 . . ?
C30 C31 C32 116.8(17) . . ?
C30 C31 H31A 121.6 . . ?
C32 C31 H31A 121.6 . . ?
C33 C32 C31 120.7(16) . . ?
C33 C32 H32A 119.6 . . ?
C31 C32 H32A 119.6 . . ?
C32 C33 N7 124.2(14) . . ?
C32 C33 C34 125.4(14) . . ?
N7 C33 C34 110.4(12) . . ?
N8 C34 C35 111.1(13) . . ?
N8 C34 C33 115.0(13) . . ?
C35 C34 C33 133.1(14) . . ?
C36 C35 C34 104.1(13) . . ?
C36 C35 H35A 127.9 . . ?
C34 C35 H35A 127.9 . . ?
N9 C36 C35 109.0(13) . . ?
N9 C36 C37 121.9(13) . . ?
C35 C36 C37 128.9(14) . . ?
C38 C37 C42 119.2(14) . . ?
C38 C37 C36 120.3(15) . . ?
C42 C37 C36 120.5(13) . . ?
C37 C38 C39 123.2(16) . . ?
C37 C38 H38A 118.4 . . ?
C39 C38 H38A 118.4 . . ?
C38 C39 C40 117.0(15) . . ?
C38 C39 H39A 121.5 . . ?
C40 C39 H39A 121.5 . . ?
C41 C40 C39 121.9(15) . . ?
C41 C40 H40A 119.1 . . ?
C39 C40 H40A 119.1 . . ?
C40 C41 C42 121.4(15) . . ?
C40 C41 C43 120.1(14) . . ?
C42 C41 C43 118.5(14) . . ?
C41 C42 C37 117.2(14) . . ?
C41 C42 H42A 121.4 . . ?
C37 C42 H42A 121.4 . . ?
C48 C43 C44 116.8(14) . . ?
C48 C43 C41 122.6(14) . . ?
C44 C43 C41 120.6(15) . . ?
C45 C44 C43 120.8(16) . . ?
C45 C44 H44A 119.6 . . ?
C43 C44 H44A 119.6 . . ?
C44 C45 C46 122.0(17) . . ?
C44 C45 H45A 119.0 . . ?
C46 C45 H45A 119.0 . . ?
C45 C46 C47 119.3(15) . . ?
C45 C46 H46A 120.3 . . ?
C47 C46 H46A 120.3 . . ?
C48 C47 C46 118.3(15) . . ?
C48 C47 C49 121.8(14) . . ?
C46 C47 C49 119.9(14) . . ?
C47 C48 C43 122.6(15) . . ?
C47 C48 H48A 118.7 . . ?
C43 C48 H48A 118.7 . . ?
N10 C49 C50 107.6(15) . . ?
N10 C49 C47 121.1(14) . . ?
C50 C49 C47 130.9(14) . . ?
C51 C50 C49 104.2(14) . . ?
C51 C50 H50A 127.9 . . ?
C49 C50 H50A 127.9 . . ?
N11 C51 C50 110.5(14) . . ?
N11 C51 C52 115.1(14) . . ?
C50 C51 C52 133.9(15) . . ?
N12 C52 C53 120.8(14) . . ?
N12 C52 C51 113.9(14) . . ?
C53 C52 C51 125.3(15) . . ?
C52 C53 C54 118.9(15) . . ?
C52 C53 H53A 120.6 . . ?
C54 C53 H53A 120.6 . . ?
C55 C54 C53 119.6(15) . . ?
C55 C54 H54A 120.2 . . ?
C53 C54 H54A 120.2 . . ?
C54 C55 C56 117.7(16) . . ?
C54 C55 H55A 121.1 . . ?
C56 C55 H55A 121.1 . . ?
N12 C56 C55 124.5(15) . . ?
N12 C56 H56A 117.7 . . ?
C55 C56 H56A 117.7 . . ?
N13 C57 C58 124.5(16) . . ?
N13 C57 H57A 117.7 . . ?
C58 C57 H57A 117.7 . . ?
C57 C58 C59 116.5(16) . . ?
C57 C58 H58A 121.8 . . ?
C59 C58 H58A 121.8 . . ?
C60 C59 C58 119.1(17) . . ?
C60 C59 H59A 120.5 . . ?
C58 C59 H59A 120.5 . . ?
C59 C60 C61 121.9(16) . . ?
C59 C60 H60A 119.0 . . ?
C61 C60 H60A 119.0 . . ?
N13 C61 C60 119.9(14) . . ?
N13 C61 C62 113.8(14) . . ?
C60 C61 C62 126.3(15) . . ?
N14 C62 C63 109.5(15) . . ?
N14 C62 C61 115.9(14) . . ?
C63 C62 C61 134.5(15) . . ?
C64 C63 C62 104.9(15) . . ?
C64 C63 H63A 127.5 . . ?
C62 C63 H63A 127.5 . . ?
N15 C64 C63 107.7(15) . . ?
N15 C64 C65 120.0(16) . . ?
C63 C64 C65 132.3(16) . . ?
C70 C65 C66 121.0(16) . . ?
C70 C65 C64 121.8(16) . . ?
C66 C65 C64 117.1(16) . . ?
C67 C66 C65 118.3(19) . . ?
C67 C66 H66A 120.8 . . ?
C65 C66 H66A 120.8 . . ?
C68 C67 C66 122(2) . . ?
C68 C67 H67A 118.9 . . ?
C66 C67 H67A 118.9 . . ?
C67 C68 C69 120(2) . . ?
C67 C68 H68A 119.8 . . ?
C69 C68 H68A 119.8 . . ?
C70 C69 C68 117.8(19) . . ?
C70 C69 C71 120.7(18) . . ?
C68 C69 C71 121.3(18) . . ?
C65 C70 C69 119.8(17) . . ?
C65 C70 H70A 120.1 . . ?
C69 C70 H70A 120.1 . . ?
C76 C71 C72 118.1(19) . . ?
C76 C71 C69 121.5(18) . . ?
C72 C71 C69 120.3(18) . . ?
C71 C72 C73 118.8(19) . . ?
C71 C72 H72A 120.6 . . ?
C73 C72 H72A 120.6 . . ?
C74 C73 C72 120(2) . . ?
C74 C73 H73A 120.1 . . ?
C72 C73 H73A 120.1 . . ?
C73 C74 C75 124(2) . . ?
C73 C74 H74A 117.8 . . ?
C75 C74 H74A 117.8 . . ?
C76 C75 C74 115.3(18) . . ?
C76 C75 C77 122.6(18) . . ?
C74 C75 C77 121.4(19) . . ?
C75 C76 C71 123.3(18) . . ?
C75 C76 H76A 118.4 . . ?
C71 C76 H76A 118.4 . . ?
N16 C77 C78 104.9(15) . . ?
N16 C77 C75 121.8(17) . . ?
C78 C77 C75 132.7(18) . . ?
C79 C78 C77 106.1(16) . . ?
C79 C78 H78A 126.9 . . ?
C77 C78 H78A 126.9 . . ?
N17 C79 C78 110.7(15) . . ?
N17 C79 C80 114.7(15) . . ?
C78 C79 C80 134.5(16) . . ?
N18 C80 C81 120.3(15) . . ?
N18 C80 C79 114.0(15) . . ?
C81 C80 C79 125.6(15) . . ?
C82 C81 C80 118.9(17) . . ?
C82 C81 H81A 120.6 . . ?
C80 C81 H81A 120.6 . . ?
C81 C82 C83 120.7(18) . . ?
C81 C82 H82A 119.7 . . ?
C83 C82 H82A 119.7 . . ?
C82 C83 C84 118.6(16) . . ?
C82 C83 H83A 120.7 . . ?
C84 C83 H83A 120.7 . . ?
N18 C84 C83 123.2(15) . . ?
N18 C84 H84A 118.4 . . ?
C83 C84 H84A 118.4 . . ?
O1 Cl1 O2 112.0(9) . . ?
O1 Cl1 O4 111.0(9) . . ?
O2 Cl1 O4 109.3(8) . . ?
O1 Cl1 O3 109.1(8) . . ?
O2 Cl1 O3 108.9(7) . . ?
O4 Cl1 O3 106.3(8) . . ?
O8 Cl2 O6 110.3(8) . . ?
O8 Cl2 O5 110.4(9) . . ?
O6 Cl2 O5 110.4(10) . . ?
O8 Cl2 O7 111.5(11) . . ?
O6 Cl2 O7 107.7(8) . . ?
O5 Cl2 O7 106.5(9) . . ?
O12 Cl3 O10 111.2(8) . . ?
O12 Cl3 O9 110.6(9) . . ?
O10 Cl3 O9 107.8(8) . . ?
O12 Cl3 O11 109.4(8) . . ?
O10 Cl3 O11 108.2(9) . . ?
O9 Cl3 O11 109.6(7) . . ?
O15 Cl4 O14 111.7(13) . . ?
O15 Cl4 O13 110.5(13) . . ?
O14 Cl4 O13 108.9(12) . . ?
O15 Cl4 O16 109.2(13) . . ?
O14 Cl4 O16 108.1(13) . . ?
O13 Cl4 O16 108.5(13) . . ?
O17 Cl5 O20 110.0(12) . . ?
O17 Cl5 O18 110.5(12) . . ?
O20 Cl5 O18 109.1(12) . . ?
O17 Cl5 O19 109.4(12) . . ?
O20 Cl5 O19 108.6(12) . . ?
O18 Cl5 O19 109.2(12) . . ?
N1S C1S C2S 178(3) . . ?
C1S C2S H2S1 109.5 . . ?
C1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
C1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N2S C3S C4S 177(3) . . ?
C3S C4S H4S1 109.5 . . ?
C3S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
C3S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
N3S C5S C6S 177(3) . . ?
C5S C6S H6S1 109.5 . . ?
C5S C6S H6S2 109.5 . . ?
H6S1 C6S H6S2 109.5 . . ?
C5S C6S H6S3 109.5 . . ?
H6S1 C6S H6S3 109.5 . . ?
H6S2 C6S H6S3 109.5 . . ?
N4S C7S C8S 165(3) . . ?
C7S C8S H8S1 109.5 . . ?
C7S C8S H8S2 109.5 . . ?
H8S1 C8S H8S2 109.5 . . ?
C7S C8S H8S3 109.5 . . ?
H8S1 C8S H8S3 109.5 . . ?
H8S2 C8S H8S3 109.5 . . ?

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
N16 H16B O3 0.88 2.13 2.923(18) 149.3 . yes
N10 H10B O2 0.88 2.44 3.094(17) 131.2 . yes
N3 H3B N2S 0.88 2.11 2.99(2) 175.7 . yes

_refine_diff_density_max         0.854
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.110




####################################################################### 
# 
# 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_lbjc58b_sq
_database_code_depnum_ccdc_archive 'CCDC 2172378'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C82 H64 Fe2 N18, 2(F6 P), F6 Si, 2(C H4 O), C7 H8'
_chemical_formula_sum            'C91 H80 F18 Fe2 N18 O2 P2 Si'
_chemical_formula_weight         2001.46

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'
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'
Si Si 0.0866 0.0751
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
P P 0.1072 0.1003
'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      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C c'
_space_group_name_Hall           'C -2yc'

_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, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'

_cell_length_a                   22.696(4)
_cell_length_b                   27.095(5)
_cell_length_c                   17.870(4)
_cell_angle_alpha                90
_cell_angle_beta                 125.911(10)
_cell_angle_gamma                90
_cell_volume                     8900(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    43154
_cell_measurement_theta_max      32.42
_cell_measurement_theta_min      1.55

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_F_000             4092
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.524
_shelx_estimated_absorpt_T_min   0.933
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_T_min  0.984
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   
;
CCP4 7.0.078: AIMLESS, version 0.7.4 : 13/12/18
Scaling & analysis of unmerged intensities, absorption correction using spherical harmonics
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72931
_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 at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            64653
_diffrn_reflns_av_unetI/netI     0.0813
_diffrn_reflns_av_R_equivalents  0.0773
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.542
_diffrn_reflns_theta_max         28.670
_diffrn_reflns_theta_full        28.670
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 0.973
_reflns_number_total             20656
_reflns_number_gt                19704
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.991
_reflns_Friedel_fraction_max     0.970
_reflns_Friedel_fraction_full    0.970

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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       'Global Phasing autoPROC package'
_computing_cell_refinement       
'DIALS 2theta refinement, DIALS 1.14.13-g10ecfbb15-release'
_computing_data_reduction        
;
aimless (Evans, P. R. and Murshudov, G. N., 2013)
ccp4 (Winn, M. D. et al., 2011)
DIALS 1.14.13-g10ecfbb15-release (Winter, G. et al., 2018)
pointless (Evans, P., 2006)
XIA2 0.5.902-gffa11588-dials-1.14 (Winter, G., 2010)
;
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. One of the PF6- anion
 is disordered over two positions with relative occupancies 0.524:0.476.
 These and the lattice methanol molecule were refined with distance and
 displacement parameters restraints. C30 was also refined with displacement
 parameters restraints due to disorder. Hydrogens were placed geometrically
 on their carrier and refined with a riding model, except those on the
 lattice methanol oxygens (AFIX 147 then AFIX 3). An area remained at the
 end of the refinement that contained only weak electron density peaks that
 could not be satisfactorily modeled as lattice solvent (neither methanol nor
 acetonitirile nor toluene). The corresponding volume was analyzed and taken 
 into account by PLATON/SQUEEZE that recovered a total of 240 (4x60) electrons 
 over four voids of 247 cubic angstrom each. These figures would agree with 
 1 diffuse toluene molecules per void, 4 per cell and thus 1 per formula unit, as
 has been reflected.
;

_vrf_PLAT413_lbjc58b_sq          
;
PROBLEM: Short Inter XH3 .. XHn        
RESPONSE: These alerts all involve hydrogens from the lattice methanol
molecules or from C30, all atoms showing heavy disordered and refined
with displacement parameters restraints (and distance restraint for the
lattice methanol). Since these hydrogens were placed at calculated 
positions, these short contacts are likely due ill-defined positions
and disorder.
;

_vrf_PLAT420_lbjc58b_sq          
;
PROBLEM: D-H Bond Without Acceptor        
RESPONSE: There is in fact an acceptor for the methanol hydrogens,
except the H-bond is weak. The acceptors are fluorine atoms from the
SiF62- or one of the PF6- anions.
;

_vrf_PLAT480_lbjc58b_sq          
;
PROBLEM: Long H...A H-Bond Reported        
RESPONSE: Indeed, these H-bonds are rather long/weak, but these
are the only acceptors available for the lattice methanol.
;

_vrf_PLAT029_lbjc58b_sq          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.976       
RESPONSE: Data were acquired at a synchrotron beamline dedicated to
protein crystallography that only allows high-accuracy phi scan and a
mini-kappa (0 to 90 degrees). These conditions put limitations on the 
completeness, resulting in a relatively low completeness at theta_full.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0992P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 9234 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.116(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         20656
_refine_ls_number_parameters     1212
_refine_ls_number_restraints     306
_refine_ls_R_factor_all          0.0536
_refine_ls_R_factor_gt           0.0526
_refine_ls_wR_factor_ref         0.1496
_refine_ls_wR_factor_gt          0.1483
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_restrained_S_all      1.073
_refine_ls_shift/su_max          0.007
_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 0.63705(3) 0.42068(2) 0.45632(3) 0.03045(12) Uani 1 1 d . . . . .
Fe2 Fe 0.22831(3) 0.42607(2) 0.53545(3) 0.02967(12) Uani 1 1 d . . . . .
N1 N 0.7172(2) 0.48108(12) 0.5341(3) 0.0375(7) Uani 1 1 d . . . . .
N2 N 0.66110(18) 0.41974(11) 0.5934(2) 0.0315(6) Uani 1 1 d . . . . .
N3 N 0.64700(17) 0.38945(11) 0.6417(2) 0.0306(6) Uani 1 1 d . . . . .
H3B H 0.610207 0.368695 0.615830 0.037 Uiso 1 1 calc R U . . .
N4 N 0.35663(19) 0.34989(13) 0.6423(2) 0.0367(7) Uani 1 1 d . . . . .
H4A H 0.391556 0.367994 0.648791 0.044 Uiso 1 1 calc R U . . .
N5 N 0.2876(2) 0.36567(13) 0.6001(2) 0.0377(7) Uani 1 1 d . . . . .
N6 N 0.1515(2) 0.38035(15) 0.5239(3) 0.0411(7) Uani 1 1 d . . . . .
N7 N 0.72718(19) 0.37086(13) 0.4903(2) 0.0362(7) Uani 1 1 d . . . . .
N8 N 0.58912(17) 0.34816(11) 0.4247(2) 0.0308(6) Uani 1 1 d . . . . .
N9 N 0.52364(17) 0.32732(11) 0.3882(2) 0.0309(6) Uani 1 1 d . . . . .
H9A H 0.485268 0.343471 0.376010 0.037 Uiso 1 1 calc R U . . .
N10 N 0.22630(18) 0.36206(12) 0.3874(2) 0.0354(6) Uani 1 1 d . . . . .
H10A H 0.264375 0.343271 0.424693 0.042 Uiso 1 1 calc R U . . .
N11 N 0.20759(19) 0.40145(12) 0.4152(2) 0.0352(7) Uani 1 1 d . . . . .
N12 N 0.14845(19) 0.47457(12) 0.4422(2) 0.0348(6) Uani 1 1 d . . . . .
N13 N 0.61884(19) 0.44622(12) 0.3270(2) 0.0338(6) Uani 1 1 d . . . . .
N14 N 0.54107(19) 0.46615(11) 0.3892(2) 0.0329(6) Uani 1 1 d . . . . .
N15 N 0.5030(2) 0.48648(11) 0.4171(2) 0.0345(6) Uani 1 1 d . . . . .
H15B H 0.500508 0.473677 0.460488 0.041 Uiso 1 1 calc R U . . .
N16 N 0.3282(2) 0.49148(12) 0.5129(3) 0.0411(8) Uani 1 1 d . . . . .
H16A H 0.329890 0.472982 0.473724 0.049 Uiso 1 1 calc R U . . .
N17 N 0.3047(2) 0.47538(12) 0.5624(3) 0.0379(7) Uani 1 1 d . . . . .
N18 N 0.24429(19) 0.46314(13) 0.6453(2) 0.0360(7) Uani 1 1 d . . . . .
C1 C 0.8939(4) 0.5807(2) 0.7142(6) 0.0706(18) Uani 1 1 d . . . . .
H1A H 0.910296 0.575108 0.777906 0.106 Uiso 1 1 calc R U . . .
H1B H 0.934120 0.574432 0.709524 0.106 Uiso 1 1 calc R U . . .
H1C H 0.877586 0.614986 0.696689 0.106 Uiso 1 1 calc R U . . .
C2 C 0.7419(3) 0.51381(17) 0.5011(4) 0.0465(10) Uani 1 1 d . . . . .
H2A H 0.719467 0.514473 0.436470 0.056 Uiso 1 1 calc R U . . .
C3 C 0.7980(3) 0.54611(18) 0.5570(5) 0.0557(12) Uani 1 1 d . . . . .
H3A H 0.813361 0.568408 0.530672 0.067 Uiso 1 1 calc R U . . .
C4 C 0.8316(3) 0.54632(17) 0.6502(4) 0.0500(11) Uani 1 1 d . . . . .
C5 C 0.8059(3) 0.51309(16) 0.6860(3) 0.0434(9) Uani 1 1 d . . . . .
H5A H 0.827043 0.512299 0.750200 0.052 Uiso 1 1 calc R U . . .
C6 C 0.7489(2) 0.48148(13) 0.6248(3) 0.0353(7) Uani 1 1 d . . . . .
C7 C 0.7205(2) 0.44494(12) 0.6573(3) 0.0311(7) Uani 1 1 d . . . . .
C8 C 0.7446(2) 0.43101(14) 0.7465(3) 0.0340(7) Uani 1 1 d . . . . .
H8A H 0.785397 0.443573 0.803409 0.041 Uiso 1 1 calc R U . . .
C9 C 0.6959(2) 0.39478(13) 0.7342(3) 0.0335(7) Uani 1 1 d . . . . .
C10 C 0.6956(2) 0.36394(14) 0.8007(3) 0.0357(7) Uani 1 1 d . . . . .
C11 C 0.7599(2) 0.35630(19) 0.8880(3) 0.0472(10) Uani 1 1 d . . . . .
H11A H 0.802626 0.373615 0.905338 0.057 Uiso 1 1 calc R U . . .
C12 C 0.7629(3) 0.3234(2) 0.9511(3) 0.0575(13) Uani 1 1 d . . . . .
H12A H 0.806809 0.318850 1.010941 0.069 Uiso 1 1 calc R U . . .
C13 C 0.6995(3) 0.2974(2) 0.9236(3) 0.0475(10) Uani 1 1 d . . . . .
H13A H 0.701034 0.274455 0.964857 0.057 Uiso 1 1 calc R U . . .
C14 C 0.6347(2) 0.30497(16) 0.8369(3) 0.0388(8) Uani 1 1 d . . . . .
C15 C 0.6334(2) 0.33856(14) 0.7768(3) 0.0357(7) Uani 1 1 d . . . . .
H15A H 0.588884 0.344307 0.718051 0.043 Uiso 1 1 calc R U . . .
C16 C 0.5675(2) 0.27801(15) 0.8066(3) 0.0382(8) Uani 1 1 d . . . . .
C17 C 0.5691(3) 0.22677(17) 0.8197(3) 0.0445(9) Uani 1 1 d . . . . .
H17A H 0.614196 0.209609 0.852860 0.053 Uiso 1 1 calc R U . . .
C18 C 0.5043(3) 0.20106(17) 0.7837(4) 0.0515(11) Uani 1 1 d . . . . .
H18A H 0.505561 0.166335 0.791891 0.062 Uiso 1 1 calc R U . . .
C19 C 0.4391(3) 0.22521(16) 0.7371(3) 0.0454(9) Uani 1 1 d . . . . .
H19A H 0.395633 0.207318 0.714045 0.054 Uiso 1 1 calc R U . . .
C20 C 0.4362(2) 0.27669(15) 0.7230(3) 0.0384(8) Uani 1 1 d . . . . .
C21 C 0.5014(2) 0.30188(15) 0.7590(3) 0.0382(8) Uani 1 1 d . . . . .
H21A H 0.500125 0.336561 0.750331 0.046 Uiso 1 1 calc R U . . .
C22 C 0.3660(2) 0.30260(16) 0.6738(3) 0.0383(8) Uani 1 1 d . . . . .
C23 C 0.2990(2) 0.28687(16) 0.6502(3) 0.0405(8) Uani 1 1 d . . . . .
H23A H 0.287262 0.255661 0.662477 0.049 Uiso 1 1 calc R U . . .
C24 C 0.2523(2) 0.32710(16) 0.6042(3) 0.0368(8) Uani 1 1 d . . . . .
C25 C 0.1747(2) 0.33413(18) 0.5588(3) 0.0419(9) Uani 1 1 d . . . . .
C26 C 0.1274(3) 0.2971(2) 0.5487(4) 0.0567(13) Uani 1 1 d . . . . .
H26A H 0.145042 0.264856 0.571898 0.068 Uiso 1 1 calc R U . . .
C27 C 0.0541(3) 0.3083(3) 0.5041(4) 0.0652(16) Uani 1 1 d . . . . .
C28 C 0.0316(3) 0.3559(3) 0.4729(4) 0.0635(15) Uani 1 1 d . . . . .
H28A H -0.017717 0.364607 0.444651 0.076 Uiso 1 1 calc R U . . .
C29 C 0.0799(3) 0.3913(2) 0.4821(4) 0.0517(11) Uani 1 1 d . . . . .
H29A H 0.062691 0.423697 0.459010 0.062 Uiso 1 1 calc R U . . .
C30 C 0.0025(4) 0.2668(4) 0.4883(7) 0.104(3) Uani 1 1 d . U . . .
H30A H 0.030232 0.236315 0.516282 0.155 Uiso 1 1 calc R U . . .
H30B H -0.022148 0.275683 0.516680 0.155 Uiso 1 1 calc R U . . .
H30C H -0.033764 0.261817 0.421799 0.155 Uiso 1 1 calc R U . . .
C31 C 0.8891(3) 0.2567(2) 0.5796(5) 0.0628(14) Uani 1 1 d . . . . .
H31A H 0.864835 0.224538 0.564165 0.094 Uiso 1 1 calc R U . . .
H31B H 0.913816 0.259935 0.549653 0.094 Uiso 1 1 calc R U . . .
H31C H 0.924845 0.259302 0.646696 0.094 Uiso 1 1 calc R U . . .
C32 C 0.7972(3) 0.38249(18) 0.5297(4) 0.0472(10) Uani 1 1 d . . . . .
H32A H 0.810711 0.416328 0.538857 0.057 Uiso 1 1 calc R U . . .
C33 C 0.8507(2) 0.3471(2) 0.5575(4) 0.0509(11) Uani 1 1 d . . . . .
H33A H 0.899409 0.357050 0.584529 0.061 Uiso 1 1 calc R U . . .
C34 C 0.8331(3) 0.29739(19) 0.5459(4) 0.0470(10) Uani 1 1 d . . . . .
C35 C 0.7601(2) 0.28512(16) 0.5024(3) 0.0418(8) Uani 1 1 d . . . . .
H35A H 0.745138 0.251552 0.491463 0.050 Uiso 1 1 calc R U . . .
C36 C 0.7091(2) 0.32295(14) 0.4750(3) 0.0331(7) Uani 1 1 d . . . . .
C37 C 0.6326(2) 0.31155(13) 0.4325(3) 0.0321(7) Uani 1 1 d . . . . .
C38 C 0.5939(2) 0.26719(13) 0.3998(3) 0.0344(7) Uani 1 1 d . . . . .
H38A H 0.611558 0.236016 0.396803 0.041 Uiso 1 1 calc R U . . .
C39 C 0.5242(2) 0.27836(13) 0.3727(3) 0.0322(7) Uani 1 1 d . . . . .
C40 C 0.4606(2) 0.24644(14) 0.3365(3) 0.0359(7) Uani 1 1 d . . . . .
C41 C 0.4700(3) 0.19511(16) 0.3390(4) 0.0513(11) Uani 1 1 d . . . . .
H41A H 0.516701 0.181607 0.363673 0.062 Uiso 1 1 calc R U . . .
C42 C 0.4107(3) 0.16427(17) 0.3051(5) 0.0603(15) Uani 1 1 d . . . . .
H42A H 0.416965 0.129548 0.306277 0.072 Uiso 1 1 calc R U . . .
C43 C 0.3426(3) 0.18319(16) 0.2698(4) 0.0492(11) Uani 1 1 d . . . . .
H43A H 0.302544 0.161496 0.246630 0.059 Uiso 1 1 calc R U . . .
C44 C 0.3324(2) 0.23428(14) 0.2680(3) 0.0376(8) Uani 1 1 d . . . . .
C45 C 0.3918(2) 0.26521(13) 0.3005(3) 0.0348(7) Uani 1 1 d . . . . .
H45A H 0.385111 0.299935 0.298059 0.042 Uiso 1 1 calc R U . . .
C46 C 0.2602(2) 0.25388(15) 0.2337(3) 0.0375(8) Uani 1 1 d . . . . .
C47 C 0.1958(2) 0.23375(17) 0.1574(3) 0.0428(9) Uani 1 1 d . . . . .
H47A H 0.198474 0.206214 0.126589 0.051 Uiso 1 1 calc R U . . .
C48 C 0.1282(3) 0.25289(19) 0.1256(3) 0.0463(10) Uani 1 1 d . . . . .
H48A H 0.085413 0.238840 0.072898 0.056 Uiso 1 1 calc R U . . .
C49 C 0.1230(3) 0.29253(18) 0.1706(3) 0.0445(9) Uani 1 1 d . . . . .
H49A H 0.076721 0.305393 0.149443 0.053 Uiso 1 1 calc R U . . .
C50 C 0.1864(2) 0.31339(15) 0.2472(3) 0.0355(7) Uani 1 1 d . . . . .
C51 C 0.2546(2) 0.29454(15) 0.2787(3) 0.0360(7) Uani 1 1 d . . . . .
H51A H 0.297382 0.309127 0.330536 0.043 Uiso 1 1 calc R U . . .
C52 C 0.1792(2) 0.35488(15) 0.2948(3) 0.0356(7) Uani 1 1 d . . . . .
C53 C 0.1262(2) 0.39134(16) 0.2610(3) 0.0372(8) Uani 1 1 d . . . . .
H53A H 0.085022 0.396103 0.199001 0.045 Uiso 1 1 calc R U . . .
C54 C 0.1470(2) 0.41945(14) 0.3386(3) 0.0330(7) Uani 1 1 d . . . . .
C55 C 0.1164(2) 0.46333(15) 0.3525(3) 0.0361(7) Uani 1 1 d . . . . .
C56 C 0.0595(3) 0.49019(18) 0.2799(3) 0.0456(9) Uani 1 1 d . . . . .
H56A H 0.038506 0.480821 0.217781 0.055 Uiso 1 1 calc R U . . .
C57 C 0.0333(3) 0.5315(2) 0.2994(4) 0.0533(11) Uani 1 1 d . . . . .
C58 C 0.0662(3) 0.5425(2) 0.3914(4) 0.0561(12) Uani 1 1 d . . . . .
H58A H 0.049822 0.569880 0.407709 0.067 Uiso 1 1 calc R U . . .
C59 C 0.1221(3) 0.51414(17) 0.4590(3) 0.0443(9) Uani 1 1 d . . . . .
H59A H 0.143741 0.522895 0.521519 0.053 Uiso 1 1 calc R U . . .
C60 C -0.0293(4) 0.5615(3) 0.2209(5) 0.077(2) Uani 1 1 d . . . . .
H60A H -0.044321 0.547431 0.161580 0.116 Uiso 1 1 calc R U . . .
H60B H -0.070329 0.560870 0.225206 0.116 Uiso 1 1 calc R U . . .
H60C H -0.013425 0.595732 0.225172 0.116 Uiso 1 1 calc R U . . .
C61 C 0.6565(2) 0.43221(14) 0.2951(3) 0.0368(8) Uani 1 1 d . . . . .
H61A H 0.690621 0.406100 0.325763 0.044 Uiso 1 1 calc R U . . .
C62 C 0.6483(3) 0.45397(16) 0.2190(3) 0.0420(9) Uani 1 1 d . . . . .
H62A H 0.676289 0.443297 0.198246 0.050 Uiso 1 1 calc R U . . .
C63 C 0.5979(2) 0.49170(16) 0.1744(3) 0.0398(8) Uani 1 1 d . . . . .
H63A H 0.590934 0.507210 0.122102 0.048 Uiso 1 1 calc R U . . .
C64 C 0.5577(2) 0.50692(14) 0.2057(3) 0.0336(7) Uani 1 1 d . . . . .
H64A H 0.522976 0.532761 0.175444 0.040 Uiso 1 1 calc R U . . .
C65 C 0.5693(2) 0.48340(13) 0.2825(3) 0.0315(7) Uani 1 1 d . . . . .
C66 C 0.5315(2) 0.49651(13) 0.3235(3) 0.0311(7) Uani 1 1 d . . . . .
C67 C 0.4856(2) 0.53609(14) 0.3087(3) 0.0339(7) Uani 1 1 d . . . . .
H67A H 0.469463 0.562228 0.265428 0.041 Uiso 1 1 calc R U . . .
C68 C 0.4689(2) 0.52848(14) 0.3718(3) 0.0343(7) Uani 1 1 d . . . . .
C69 C 0.4268(2) 0.55765(13) 0.3950(3) 0.0343(7) Uani 1 1 d . . . . .
C70 C 0.4066(3) 0.60633(15) 0.3654(3) 0.0421(9) Uani 1 1 d . . . . .
H70A H 0.417783 0.620905 0.326699 0.050 Uiso 1 1 calc R U . . .
C71 C 0.3701(3) 0.63359(16) 0.3926(4) 0.0501(11) Uani 1 1 d . . . . .
H71A H 0.356963 0.666829 0.372631 0.060 Uiso 1 1 calc R U . . .
C72 C 0.3526(3) 0.61307(15) 0.4482(3) 0.0441(9) Uani 1 1 d . . . . .
H72A H 0.327285 0.632068 0.465588 0.053 Uiso 1 1 calc R U . . .
C73 C 0.3724(2) 0.56413(14) 0.4788(3) 0.0368(8) Uani 1 1 d . . . . .
C74 C 0.4096(2) 0.53693(14) 0.4515(3) 0.0358(8) Uani 1 1 d . . . . .
H74A H 0.423232 0.503796 0.471927 0.043 Uiso 1 1 calc R U . . .
C75 C 0.3490(2) 0.53928(14) 0.5304(3) 0.0362(7) Uani 1 1 d . . . . .
C76 C 0.3382(2) 0.55558(15) 0.5948(3) 0.0400(8) Uani 1 1 d . . . . .
H76A H 0.347125 0.587698 0.620700 0.048 Uiso 1 1 calc R U . . .
C77 C 0.3112(2) 0.51458(14) 0.6137(3) 0.0335(7) Uani 1 1 d . . . . .
C78 C 0.2827(2) 0.50658(15) 0.6675(3) 0.0346(7) Uani 1 1 d . . . . .
C79 C 0.2895(2) 0.53982(19) 0.7311(3) 0.0438(9) Uani 1 1 d . . . . .
H79A H 0.316066 0.569627 0.744842 0.053 Uiso 1 1 calc R U . . .
C80 C 0.2562(3) 0.5284(2) 0.7744(3) 0.0521(11) Uani 1 1 d . . . . .
H80A H 0.258858 0.550803 0.817101 0.063 Uiso 1 1 calc R U . . .
C81 C 0.2194(3) 0.4842(2) 0.7547(3) 0.0523(11) Uani 1 1 d . . . . .
H81A H 0.197293 0.475752 0.784558 0.063 Uiso 1 1 calc R U . . .
C82 C 0.2151(2) 0.45200(18) 0.6904(3) 0.0430(9) Uani 1 1 d . . . . .
H82A H 0.190829 0.421313 0.678336 0.052 Uiso 1 1 calc R U . . .
Si1 Si 0.43605(5) 0.37867(3) 0.50552(6) 0.02624(17) Uani 1 1 d . . . . .
F1 F 0.49198(13) 0.42731(7) 0.52754(16) 0.0328(4) Uani 1 1 d . . . . .
F2 F 0.50895(13) 0.34087(8) 0.55629(17) 0.0367(5) Uani 1 1 d . . . . .
F3 F 0.38043(13) 0.33197(8) 0.48740(17) 0.0371(5) Uani 1 1 d . . . . .
F4 F 0.36332(14) 0.41707(8) 0.45153(17) 0.0372(5) Uani 1 1 d . . . . .
F5 F 0.44958(13) 0.39060(8) 0.60830(15) 0.0353(4) Uani 1 1 d . . . . .
F6 F 0.42154(13) 0.37007(9) 0.40188(16) 0.0368(5) Uani 1 1 d . . . . .
P1 P 0.14076(13) 0.65815(9) 0.27980(15) 0.0829(6) Uani 1 1 d . . . . .
F7 F 0.1976(3) 0.6872(2) 0.3722(4) 0.1117(19) Uani 1 1 d . . . . .
F8 F 0.1782(4) 0.6073(2) 0.3352(6) 0.121(2) Uani 1 1 d . . . . .
F9 F 0.0863(4) 0.6262(4) 0.1905(6) 0.147(3) Uani 1 1 d . . . . .
F10 F 0.1032(4) 0.7071(3) 0.2267(6) 0.143(3) Uani 1 1 d . . . . .
F11 F 0.0900(3) 0.6561(2) 0.3123(5) 0.1079(17) Uani 1 1 d . . . . .
F12 F 0.1945(3) 0.6599(2) 0.2511(4) 0.1069(17) Uani 1 1 d . . . . .
P2 P 0.9504(2) 0.5218(3) 0.4866(2) 0.0707(14) Uani 0.524(11) 1 d D U P A 1
F13 F 0.9247(9) 0.5699(6) 0.4285(10) 0.117(4) Uani 0.524(11) 1 d D U P A 1
F14 F 0.9466(7) 0.5479(7) 0.5617(8) 0.118(4) Uani 0.524(11) 1 d D U P A 1
F15 F 0.9787(10) 0.4736(6) 0.5487(10) 0.139(4) Uani 0.524(11) 1 d D U P A 1
F16 F 0.9576(8) 0.4902(7) 0.4181(10) 0.120(4) Uani 0.524(11) 1 d D U P A 1
F17 F 0.8708(6) 0.5029(6) 0.4337(10) 0.092(3) Uani 0.524(11) 1 d D U P A 1
F18 F 1.0301(5) 0.5408(7) 0.5393(8) 0.116(4) Uani 0.524(11) 1 d D U P A 1
P2B P 0.9326(4) 0.4925(4) 0.4728(4) 0.0831(19) Uani 0.476(11) 1 d D U P A 2
F13B F 0.9202(8) 0.5426(7) 0.4166(12) 0.118(4) Uani 0.476(11) 1 d D U P A 2
F14B F 0.9232(8) 0.5150(6) 0.5465(9) 0.105(3) Uani 0.476(11) 1 d D U P A 2
F15B F 0.9458(8) 0.4415(5) 0.5198(9) 0.105(3) Uani 0.476(11) 1 d D U P A 2
F16B F 0.9390(10) 0.4663(8) 0.3970(10) 0.129(5) Uani 0.476(11) 1 d D U P A 2
F17B F 0.8477(7) 0.4877(7) 0.4060(11) 0.103(4) Uani 0.476(11) 1 d D U P A 2
F18B F 1.0166(7) 0.5048(7) 0.5382(9) 0.108(3) Uani 0.476(11) 1 d D U P A 2
O1S O 0.4344(5) 0.2195(3) 0.5228(5) 0.126(3) Uani 1 1 d D U . . .
H1S H 0.474156 0.234554 0.556176 0.189 Uiso 1 1 d R U . . .
C1S C 0.4418(4) 0.1704(3) 0.5595(6) 0.088(2) Uani 1 1 d D U . . .
H1S1 H 0.482551 0.169826 0.625185 0.132 Uiso 1 1 calc R U . . .
H1S2 H 0.451119 0.146740 0.525947 0.132 Uiso 1 1 calc R U . . .
H1S3 H 0.396888 0.161270 0.552051 0.132 Uiso 1 1 calc R U . . .
O2S O 0.1926(8) 0.3552(4) 0.0478(8) 0.168(4) Uani 1 1 d D U . . .
H2S H 0.164777 0.330863 0.032507 0.252 Uiso 1 1 d R U . . .
C2S C 0.2668(8) 0.3382(4) 0.0973(10) 0.149(4) Uani 1 1 d D U . . .
H2S1 H 0.299913 0.364719 0.137137 0.223 Uiso 1 1 calc R U . . .
H2S2 H 0.277074 0.328800 0.053028 0.223 Uiso 1 1 calc R U . . .
H2S3 H 0.273788 0.309574 0.135190 0.223 Uiso 1 1 calc R U . . .


_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 N14 2.153(3) . ?
Fe1 N8 2.155(3) . ?
Fe1 N2 2.175(3) . ?
Fe1 N13 2.206(3) . ?
Fe1 N7 2.218(3) . ?
Fe1 N1 2.225(4) . ?
Fe2 N5 1.999(4) . ?
Fe2 N17 2.010(4) . ?
Fe2 N11 2.025(3) . ?
Fe2 N18 2.039(4) . ?
Fe2 N6 2.048(4) . ?
Fe2 N12 2.060(3) . ?
N1 C6 1.333(6) . ?
N1 C2 1.355(5) . ?
N2 C7 1.334(5) . ?
N2 N3 1.359(4) . ?
N3 C9 1.353(5) . ?
N3 H3B 0.8800 . ?
N4 N5 1.350(5) . ?
N4 C22 1.365(5) . ?
N4 H4A 0.8800 . ?
N5 C24 1.345(5) . ?
N6 C25 1.360(6) . ?
N6 C29 1.366(6) . ?
N7 C36 1.340(5) . ?
N7 C32 1.345(6) . ?
N8 C37 1.347(5) . ?
N8 N9 1.347(4) . ?
N9 C39 1.357(4) . ?
N9 H9A 0.8800 . ?
N10 N11 1.347(4) . ?
N10 C52 1.359(5) . ?
N10 H10A 0.8800 . ?
N11 C54 1.340(5) . ?
N12 C59 1.344(5) . ?
N12 C55 1.352(5) . ?
N13 C61 1.331(5) . ?
N13 C65 1.365(5) . ?
N14 C66 1.343(4) . ?
N14 N15 1.345(4) . ?
N15 C68 1.347(5) . ?
N15 H15B 0.8800 . ?
N16 N17 1.347(4) . ?
N16 C75 1.351(5) . ?
N16 H16A 0.8800 . ?
N17 C77 1.353(5) . ?
N18 C82 1.345(5) . ?
N18 C78 1.378(5) . ?
C1 C4 1.509(7) . ?
C1 H1A 0.9800 . ?
C1 H1B 0.9800 . ?
C1 H1C 0.9800 . ?
C2 C3 1.376(7) . ?
C2 H2A 0.9500 . ?
C3 C4 1.366(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.412(6) . ?
C5 C6 1.395(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.473(5) . ?
C7 C8 1.401(5) . ?
C8 C9 1.395(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.456(5) . ?
C10 C11 1.392(6) . ?
C10 C15 1.394(6) . ?
C11 C12 1.407(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.406(7) . ?
C12 H12A 0.9500 . ?
C13 C14 1.391(6) . ?
C13 H13A 0.9500 . ?
C14 C15 1.394(5) . ?
C14 C16 1.477(6) . ?
C15 H15A 0.9500 . ?
C16 C21 1.377(6) . ?
C16 C17 1.405(6) . ?
C17 C18 1.399(7) . ?
C17 H17A 0.9500 . ?
C18 C19 1.365(8) . ?
C18 H18A 0.9500 . ?
C19 C20 1.412(6) . ?
C19 H19A 0.9500 . ?
C20 C21 1.398(6) . ?
C20 C22 1.469(6) . ?
C21 H21A 0.9500 . ?
C22 C23 1.387(6) . ?
C23 C24 1.402(6) . ?
C23 H23A 0.9500 . ?
C24 C25 1.456(6) . ?
C25 C26 1.401(6) . ?
C26 C27 1.392(8) . ?
C26 H26A 0.9500 . ?
C27 C28 1.376(10) . ?
C27 C30 1.527(8) . ?
C28 C29 1.392(8) . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9500 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C34 1.515(7) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.389(7) . ?
C32 H32A 0.9500 . ?
C33 C34 1.386(7) . ?
C33 H33A 0.9500 . ?
C34 C35 1.397(6) . ?
C35 C36 1.402(5) . ?
C35 H35A 0.9500 . ?
C36 C37 1.463(5) . ?
C37 C38 1.398(5) . ?
C38 C39 1.390(5) . ?
C38 H38A 0.9500 . ?
C39 C40 1.467(5) . ?
C40 C45 1.391(6) . ?
C40 C41 1.404(5) . ?
C41 C42 1.387(7) . ?
C41 H41A 0.9500 . ?
C42 C43 1.379(7) . ?
C42 H42A 0.9500 . ?
C43 C44 1.401(6) . ?
C43 H43A 0.9500 . ?
C44 C45 1.391(5) . ?
C44 C46 1.472(6) . ?
C45 H45A 0.9500 . ?
C46 C47 1.397(6) . ?
C46 C51 1.413(5) . ?
C47 C48 1.387(7) . ?
C47 H47A 0.9500 . ?
C48 C49 1.388(6) . ?
C48 H48A 0.9500 . ?
C49 C50 1.397(6) . ?
C49 H49A 0.9500 . ?
C50 C51 1.398(6) . ?
C50 C52 1.475(5) . ?
C51 H51A 0.9500 . ?
C52 C53 1.391(6) . ?
C53 C54 1.399(5) . ?
C53 H53A 0.9500 . ?
C54 C55 1.469(5) . ?
C55 C56 1.384(6) . ?
C56 C57 1.404(6) . ?
C56 H56A 0.9500 . ?
C57 C58 1.382(8) . ?
C57 C60 1.520(7) . ?
C58 C59 1.364(7) . ?
C58 H58A 0.9500 . ?
C59 H59A 0.9500 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.391(6) . ?
C61 H61A 0.9500 . ?
C62 C63 1.385(6) . ?
C62 H62A 0.9500 . ?
C63 C64 1.383(5) . ?
C63 H63A 0.9500 . ?
C64 C65 1.391(5) . ?
C64 H64A 0.9500 . ?
C65 C66 1.462(5) . ?
C66 C67 1.408(5) . ?
C67 C68 1.398(5) . ?
C67 H67A 0.9500 . ?
C68 C69 1.474(5) . ?
C69 C70 1.395(5) . ?
C69 C74 1.398(5) . ?
C70 C71 1.394(6) . ?
C70 H70A 0.9500 . ?
C71 C72 1.384(6) . ?
C71 H71A 0.9500 . ?
C72 C73 1.404(5) . ?
C72 H72A 0.9500 . ?
C73 C74 1.405(5) . ?
C73 C75 1.470(5) . ?
C74 H74A 0.9500 . ?
C75 C76 1.383(5) . ?
C76 C77 1.403(5) . ?
C76 H76A 0.9500 . ?
C77 C78 1.454(5) . ?
C78 C79 1.386(6) . ?
C79 C80 1.397(6) . ?
C79 H79A 0.9500 . ?
C80 C81 1.381(8) . ?
C80 H80A 0.9500 . ?
C81 C82 1.399(7) . ?
C81 H81A 0.9500 . ?
C82 H82A 0.9500 . ?
Si1 F3 1.679(2) . ?
Si1 F2 1.688(2) . ?
Si1 F4 1.694(3) . ?
Si1 F6 1.696(2) . ?
Si1 F5 1.706(2) . ?
Si1 F1 1.708(2) . ?
P1 F10 1.560(8) . ?
P1 F11 1.567(6) . ?
P1 F12 1.577(5) . ?
P1 F9 1.584(7) . ?
P1 F7 1.585(6) . ?
P1 F8 1.617(7) . ?
P2 F13 1.551(12) . ?
P2 F17 1.556(11) . ?
P2 F18 1.557(10) . ?
P2 F14 1.565(10) . ?
P2 F16 1.578(10) . ?
P2 F15 1.586(13) . ?
P2B F15B 1.552(12) . ?
P2B F17B 1.567(13) . ?
P2B F14B 1.573(11) . ?
P2B F18B 1.582(13) . ?
P2B F16B 1.611(12) . ?
P2B F13B 1.613(13) . ?
O1S C1S 1.449(6) . ?
O1S H1S 0.8402 . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.443(7) . ?
O2S H2S 0.8399 . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?

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
N14 Fe1 N8 100.69(12) . . ?
N14 Fe1 N2 97.93(12) . . ?
N8 Fe1 N2 92.23(12) . . ?
N14 Fe1 N13 74.35(12) . . ?
N8 Fe1 N13 104.83(12) . . ?
N2 Fe1 N13 162.22(12) . . ?
N14 Fe1 N7 165.92(13) . . ?
N8 Fe1 N7 76.08(12) . . ?
N2 Fe1 N7 95.90(13) . . ?
N13 Fe1 N7 93.06(13) . . ?
N14 Fe1 N1 96.69(13) . . ?
N8 Fe1 N1 159.44(13) . . ?
N2 Fe1 N1 74.44(12) . . ?
N13 Fe1 N1 90.35(13) . . ?
N7 Fe1 N1 89.54(13) . . ?
N5 Fe2 N17 102.25(14) . . ?
N5 Fe2 N11 90.12(13) . . ?
N17 Fe2 N11 96.00(14) . . ?
N5 Fe2 N18 99.67(14) . . ?
N17 Fe2 N18 78.46(14) . . ?
N11 Fe2 N18 169.56(14) . . ?
N5 Fe2 N6 78.92(15) . . ?
N17 Fe2 N6 171.63(14) . . ?
N11 Fe2 N6 92.28(14) . . ?
N18 Fe2 N6 93.17(14) . . ?
N5 Fe2 N12 164.50(14) . . ?
N17 Fe2 N12 89.76(14) . . ?
N11 Fe2 N12 78.78(13) . . ?
N18 Fe2 N12 92.25(13) . . ?
N6 Fe2 N12 90.63(15) . . ?
C6 N1 C2 117.3(4) . . ?
C6 N1 Fe1 115.2(2) . . ?
C2 N1 Fe1 127.2(3) . . ?
C7 N2 N3 105.2(3) . . ?
C7 N2 Fe1 114.7(2) . . ?
N3 N2 Fe1 136.5(2) . . ?
C9 N3 N2 112.4(3) . . ?
C9 N3 H3B 123.8 . . ?
N2 N3 H3B 123.8 . . ?
N5 N4 C22 112.2(3) . . ?
N5 N4 H4A 123.9 . . ?
C22 N4 H4A 123.9 . . ?
C24 N5 N4 104.9(4) . . ?
C24 N5 Fe2 116.5(3) . . ?
N4 N5 Fe2 138.6(3) . . ?
C25 N6 C29 117.9(4) . . ?
C25 N6 Fe2 115.7(3) . . ?
C29 N6 Fe2 126.4(4) . . ?
C36 N7 C32 117.4(4) . . ?
C36 N7 Fe1 114.2(3) . . ?
C32 N7 Fe1 128.2(3) . . ?
C37 N8 N9 105.9(3) . . ?
C37 N8 Fe1 114.7(2) . . ?
N9 N8 Fe1 138.9(2) . . ?
N8 N9 C39 111.7(3) . . ?
N8 N9 H9A 124.2 . . ?
C39 N9 H9A 124.2 . . ?
N11 N10 C52 111.7(3) . . ?
N11 N10 H10A 124.2 . . ?
C52 N10 H10A 124.2 . . ?
C54 N11 N10 105.6(3) . . ?
C54 N11 Fe2 115.1(2) . . ?
N10 N11 Fe2 136.5(3) . . ?
C59 N12 C55 116.4(4) . . ?
C59 N12 Fe2 128.6(3) . . ?
C55 N12 Fe2 114.9(3) . . ?
C61 N13 C65 118.5(3) . . ?
C61 N13 Fe1 125.9(3) . . ?
C65 N13 Fe1 115.3(2) . . ?
C66 N14 N15 105.3(3) . . ?
C66 N14 Fe1 115.5(2) . . ?
N15 N14 Fe1 133.5(2) . . ?
N14 N15 C68 112.9(3) . . ?
N14 N15 H15B 123.5 . . ?
C68 N15 H15B 123.5 . . ?
N17 N16 C75 112.2(3) . . ?
N17 N16 H16A 123.9 . . ?
C75 N16 H16A 123.9 . . ?
N16 N17 C77 105.3(3) . . ?
N16 N17 Fe2 132.5(3) . . ?
C77 N17 Fe2 114.9(3) . . ?
C82 N18 C78 118.0(4) . . ?
C82 N18 Fe2 126.5(3) . . ?
C78 N18 Fe2 115.1(2) . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
N1 C2 C3 122.8(5) . . ?
N1 C2 H2A 118.6 . . ?
C3 C2 H2A 118.6 . . ?
C4 C3 C2 120.4(4) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C3 C4 C5 117.7(4) . . ?
C3 C4 C1 122.1(5) . . ?
C5 C4 C1 120.2(5) . . ?
C6 C5 C4 118.5(5) . . ?
C6 C5 H5A 120.7 . . ?
C4 C5 H5A 120.7 . . ?
N1 C6 C5 123.2(4) . . ?
N1 C6 C7 115.1(3) . . ?
C5 C6 C7 121.6(4) . . ?
N2 C7 C8 111.1(3) . . ?
N2 C7 C6 117.5(3) . . ?
C8 C7 C6 131.3(4) . . ?
C9 C8 C7 105.4(3) . . ?
C9 C8 H8A 127.3 . . ?
C7 C8 H8A 127.3 . . ?
N3 C9 C8 106.0(3) . . ?
N3 C9 C10 122.8(3) . . ?
C8 C9 C10 131.1(4) . . ?
C11 C10 C15 118.5(4) . . ?
C11 C10 C9 119.8(4) . . ?
C15 C10 C9 121.5(4) . . ?
C10 C11 C12 121.2(4) . . ?
C10 C11 H11A 119.4 . . ?
C12 C11 H11A 119.4 . . ?
C13 C12 C11 118.6(4) . . ?
C13 C12 H12A 120.7 . . ?
C11 C12 H12A 120.7 . . ?
C14 C13 C12 120.8(4) . . ?
C14 C13 H13A 119.6 . . ?
C12 C13 H13A 119.6 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 C16 121.7(4) . . ?
C15 C14 C16 119.3(4) . . ?
C14 C15 C10 121.8(4) . . ?
C14 C15 H15A 119.1 . . ?
C10 C15 H15A 119.1 . . ?
C21 C16 C17 118.6(4) . . ?
C21 C16 C14 120.7(4) . . ?
C17 C16 C14 120.5(4) . . ?
C18 C17 C16 119.9(4) . . ?
C18 C17 H17A 120.0 . . ?
C16 C17 H17A 120.0 . . ?
C19 C18 C17 120.9(4) . . ?
C19 C18 H18A 119.6 . . ?
C17 C18 H18A 119.6 . . ?
C18 C19 C20 120.2(4) . . ?
C18 C19 H19A 119.9 . . ?
C20 C19 H19A 119.9 . . ?
C21 C20 C19 118.2(4) . . ?
C21 C20 C22 121.7(4) . . ?
C19 C20 C22 120.0(4) . . ?
C16 C21 C20 122.1(4) . . ?
C16 C21 H21A 119.0 . . ?
C20 C21 H21A 119.0 . . ?
N4 C22 C23 106.5(4) . . ?
N4 C22 C20 123.2(4) . . ?
C23 C22 C20 130.2(4) . . ?
C22 C23 C24 104.9(4) . . ?
C22 C23 H23A 127.6 . . ?
C24 C23 H23A 127.6 . . ?
N5 C24 C23 111.5(4) . . ?
N5 C24 C25 115.6(4) . . ?
C23 C24 C25 132.8(4) . . ?
N6 C25 C26 122.6(5) . . ?
N6 C25 C24 113.1(4) . . ?
C26 C25 C24 124.3(5) . . ?
C27 C26 C25 119.0(6) . . ?
C27 C26 H26A 120.5 . . ?
C25 C26 H26A 120.5 . . ?
C28 C27 C26 118.1(5) . . ?
C28 C27 C30 123.5(6) . . ?
C26 C27 C30 118.3(7) . . ?
C27 C28 C29 121.2(5) . . ?
C27 C28 H28A 119.4 . . ?
C29 C28 H28A 119.4 . . ?
N6 C29 C28 121.0(6) . . ?
N6 C29 H29A 119.5 . . ?
C28 C29 H29A 119.5 . . ?
C27 C30 H30A 109.5 . . ?
C27 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C27 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C34 C31 H31A 109.5 . . ?
C34 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C34 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N7 C32 C33 122.8(4) . . ?
N7 C32 H32A 118.6 . . ?
C33 C32 H32A 118.6 . . ?
C34 C33 C32 120.2(4) . . ?
C34 C33 H33A 119.9 . . ?
C32 C33 H33A 119.9 . . ?
C33 C34 C35 117.3(4) . . ?
C33 C34 C31 123.2(5) . . ?
C35 C34 C31 119.5(5) . . ?
C34 C35 C36 119.2(4) . . ?
C34 C35 H35A 120.4 . . ?
C36 C35 H35A 120.4 . . ?
N7 C36 C35 123.1(4) . . ?
N7 C36 C37 116.0(3) . . ?
C35 C36 C37 120.8(3) . . ?
N8 C37 C38 110.4(3) . . ?
N8 C37 C36 118.2(3) . . ?
C38 C37 C36 131.4(3) . . ?
C39 C38 C37 105.4(3) . . ?
C39 C38 H38A 127.3 . . ?
C37 C38 H38A 127.3 . . ?
N9 C39 C38 106.6(3) . . ?
N9 C39 C40 122.8(3) . . ?
C38 C39 C40 130.5(3) . . ?
C45 C40 C41 119.1(4) . . ?
C45 C40 C39 122.4(3) . . ?
C41 C40 C39 118.6(4) . . ?
C42 C41 C40 119.5(4) . . ?
C42 C41 H41A 120.3 . . ?
C40 C41 H41A 120.3 . . ?
C43 C42 C41 121.1(4) . . ?
C43 C42 H42A 119.5 . . ?
C41 C42 H42A 119.5 . . ?
C42 C43 C44 120.2(4) . . ?
C42 C43 H43A 119.9 . . ?
C44 C43 H43A 119.9 . . ?
C45 C44 C43 118.7(4) . . ?
C45 C44 C46 121.7(3) . . ?
C43 C44 C46 119.6(4) . . ?
C40 C45 C44 121.5(4) . . ?
C40 C45 H45A 119.2 . . ?
C44 C45 H45A 119.2 . . ?
C47 C46 C51 117.9(4) . . ?
C47 C46 C44 122.5(3) . . ?
C51 C46 C44 119.6(3) . . ?
C48 C47 C46 121.7(4) . . ?
C48 C47 H47A 119.1 . . ?
C46 C47 H47A 119.1 . . ?
C47 C48 C49 120.1(4) . . ?
C47 C48 H48A 119.9 . . ?
C49 C48 H48A 119.9 . . ?
C48 C49 C50 119.5(4) . . ?
C48 C49 H49A 120.3 . . ?
C50 C49 H49A 120.3 . . ?
C49 C50 C51 120.5(4) . . ?
C49 C50 C52 118.4(4) . . ?
C51 C50 C52 121.1(3) . . ?
C50 C51 C46 120.2(4) . . ?
C50 C51 H51A 119.9 . . ?
C46 C51 H51A 119.9 . . ?
N10 C52 C53 106.8(3) . . ?
N10 C52 C50 122.5(4) . . ?
C53 C52 C50 130.6(4) . . ?
C52 C53 C54 104.7(3) . . ?
C52 C53 H53A 127.7 . . ?
C54 C53 H53A 127.7 . . ?
N11 C54 C53 111.2(3) . . ?
N11 C54 C55 115.2(3) . . ?
C53 C54 C55 133.6(4) . . ?
N12 C55 C56 123.4(4) . . ?
N12 C55 C54 113.8(4) . . ?
C56 C55 C54 122.7(4) . . ?
C55 C56 C57 119.0(4) . . ?
C55 C56 H56A 120.5 . . ?
C57 C56 H56A 120.5 . . ?
C58 C57 C56 117.1(4) . . ?
C58 C57 C60 122.9(5) . . ?
C56 C57 C60 120.0(5) . . ?
C59 C58 C57 120.4(4) . . ?
C59 C58 H58A 119.8 . . ?
C57 C58 H58A 119.8 . . ?
N12 C59 C58 123.8(4) . . ?
N12 C59 H59A 118.1 . . ?
C58 C59 H59A 118.1 . . ?
C57 C60 H60A 109.5 . . ?
C57 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C57 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N13 C61 C62 123.1(4) . . ?
N13 C61 H61A 118.4 . . ?
C62 C61 H61A 118.4 . . ?
C63 C62 C61 117.9(4) . . ?
C63 C62 H62A 121.1 . . ?
C61 C62 H62A 121.1 . . ?
C64 C63 C62 120.4(4) . . ?
C64 C63 H63A 119.8 . . ?
C62 C63 H63A 119.8 . . ?
C63 C64 C65 118.2(4) . . ?
C63 C64 H64A 120.9 . . ?
C65 C64 H64A 120.9 . . ?
N13 C65 C64 121.9(3) . . ?
N13 C65 C66 114.3(3) . . ?
C64 C65 C66 123.8(3) . . ?
N14 C66 C67 110.7(3) . . ?
N14 C66 C65 116.6(3) . . ?
C67 C66 C65 132.7(3) . . ?
C68 C67 C66 104.9(3) . . ?
C68 C67 H67A 127.5 . . ?
C66 C67 H67A 127.5 . . ?
N15 C68 C67 106.2(3) . . ?
N15 C68 C69 121.5(3) . . ?
C67 C68 C69 132.3(3) . . ?
C70 C69 C74 119.0(3) . . ?
C70 C69 C68 121.6(3) . . ?
C74 C69 C68 119.4(3) . . ?
C71 C70 C69 119.9(4) . . ?
C71 C70 H70A 120.0 . . ?
C69 C70 H70A 120.0 . . ?
C72 C71 C70 121.1(4) . . ?
C72 C71 H71A 119.4 . . ?
C70 C71 H71A 119.4 . . ?
C71 C72 C73 119.9(4) . . ?
C71 C72 H72A 120.1 . . ?
C73 C72 H72A 120.1 . . ?
C72 C73 C74 118.7(3) . . ?
C72 C73 C75 121.8(4) . . ?
C74 C73 C75 119.2(3) . . ?
C69 C74 C73 121.3(3) . . ?
C69 C74 H74A 119.3 . . ?
C73 C74 H74A 119.3 . . ?
N16 C75 C76 106.9(3) . . ?
N16 C75 C73 120.0(3) . . ?
C76 C75 C73 133.0(4) . . ?
C75 C76 C77 105.3(3) . . ?
C75 C76 H76A 127.3 . . ?
C77 C76 H76A 127.3 . . ?
N17 C77 C76 110.3(3) . . ?
N17 C77 C78 114.6(3) . . ?
C76 C77 C78 134.7(4) . . ?
N18 C78 C79 122.6(4) . . ?
N18 C78 C77 112.8(3) . . ?
C79 C78 C77 124.5(4) . . ?
C78 C79 C80 118.3(4) . . ?
C78 C79 H79A 120.9 . . ?
C80 C79 H79A 120.9 . . ?
C81 C80 C79 119.6(4) . . ?
C81 C80 H80A 120.2 . . ?
C79 C80 H80A 120.2 . . ?
C80 C81 C82 119.3(4) . . ?
C80 C81 H81A 120.4 . . ?
C82 C81 H81A 120.4 . . ?
N18 C82 C81 122.1(4) . . ?
N18 C82 H82A 119.0 . . ?
C81 C82 H82A 119.0 . . ?
F3 Si1 F2 92.03(12) . . ?
F3 Si1 F4 88.96(13) . . ?
F2 Si1 F4 177.91(14) . . ?
F3 Si1 F6 92.48(13) . . ?
F2 Si1 F6 90.28(12) . . ?
F4 Si1 F6 87.83(12) . . ?
F3 Si1 F5 89.46(12) . . ?
F2 Si1 F5 92.03(13) . . ?
F4 Si1 F5 89.82(13) . . ?
F6 Si1 F5 176.92(13) . . ?
F3 Si1 F1 177.32(13) . . ?
F2 Si1 F1 89.00(12) . . ?
F4 Si1 F1 90.09(12) . . ?
F6 Si1 F1 89.98(12) . . ?
F5 Si1 F1 88.03(11) . . ?
F10 P1 F11 89.9(4) . . ?
F10 P1 F12 91.5(4) . . ?
F11 P1 F12 177.8(4) . . ?
F10 P1 F9 91.5(5) . . ?
F11 P1 F9 92.6(4) . . ?
F12 P1 F9 89.1(4) . . ?
F10 P1 F7 91.9(5) . . ?
F11 P1 F7 87.6(3) . . ?
F12 P1 F7 90.6(3) . . ?
F9 P1 F7 176.6(5) . . ?
F10 P1 F8 178.7(4) . . ?
F11 P1 F8 88.9(3) . . ?
F12 P1 F8 89.8(3) . . ?
F9 P1 F8 88.3(5) . . ?
F7 P1 F8 88.3(4) . . ?
F13 P2 F17 91.3(8) . . ?
F13 P2 F18 88.6(9) . . ?
F17 P2 F18 179.9(11) . . ?
F13 P2 F14 90.3(10) . . ?
F17 P2 F14 92.3(8) . . ?
F18 P2 F14 87.8(7) . . ?
F13 P2 F16 96.2(10) . . ?
F17 P2 F16 87.8(8) . . ?
F18 P2 F16 92.1(7) . . ?
F14 P2 F16 173.5(11) . . ?
F13 P2 F15 178.2(10) . . ?
F17 P2 F15 90.2(9) . . ?
F18 P2 F15 89.9(9) . . ?
F14 P2 F15 88.6(9) . . ?
F16 P2 F15 84.9(10) . . ?
F15B P2B F17B 95.8(9) . . ?
F15B P2B F14B 88.3(8) . . ?
F17B P2B F14B 87.8(8) . . ?
F15B P2B F18B 91.2(8) . . ?
F17B P2B F18B 172.6(10) . . ?
F14B P2B F18B 89.9(8) . . ?
F15B P2B F16B 88.8(9) . . ?
F17B P2B F16B 90.0(10) . . ?
F14B P2B F16B 176.2(11) . . ?
F18B P2B F16B 92.7(9) . . ?
F15B P2B F13B 173.9(10) . . ?
F17B P2B F13B 84.7(8) . . ?
F14B P2B F13B 97.8(10) . . ?
F18B P2B F13B 88.7(8) . . ?
F16B P2B F13B 85.1(10) . . ?
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 . . ?
C2S O2S H2S 109.5 . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?

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 H3B F2 0.88 2.03 2.876(4) 161.3 . yes
N4 H4A F5 0.88 1.94 2.746(4) 152.2 . yes
N9 H9A F6 0.88 1.90 2.726(4) 155.8 . yes
N10 H10A F3 0.88 2.20 2.960(4) 144.9 . yes
N15 H15B F1 0.88 1.82 2.665(4) 159.4 . yes
N16 H16A F4 0.88 1.84 2.632(4) 149.0 . yes
O1S H1S F2 0.84 2.99 3.585(9) 130.0 . yes
O2S H2S F11 0.84 3.26 3.425(13) 93.9 2_564 yes

_refine_diff_density_max         1.339
_refine_diff_density_min         -0.772
_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_lb2209
_database_code_depnum_ccdc_archive 'CCDC 2172381'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C90 H72 Fe2 N18, 4(Cl O4), 9.667(C H4 O), 2(H2 O)'
_chemical_formula_sum            'C99.67 H114.67 Cl4 Fe2 N18 O27.67'
_chemical_formula_weight         2260.95

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'
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'
Cl Cl 0.1551 0.1682
'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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   23.217(5)
_cell_length_b                   17.634(3)
_cell_length_c                   27.292(5)
_cell_angle_alpha                90
_cell_angle_beta                 95.498(3)
_cell_angle_gamma                90
_cell_volume                     11122(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    36353
_cell_measurement_theta_min      1.04
_cell_measurement_theta_max      33.19

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_F_000             4684
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.473
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.986
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_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 at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27023
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         1.130
_diffrn_reflns_theta_max         29.137
_diffrn_reflns_theta_full        29.090
_diffrn_measured_fraction_theta_max 0.978
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.978
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.978
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             27023
_reflns_number_gt                22075
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_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-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
 Refined as a 2-component twin. TwinRotMat found was used to find the twinning
 law and to generate the HKLF 5 file.
 All non-hydrogens were refined anisotropically. The guest ClO4 ion is disordered
 over two flipped positions (CL1-O4:CL1B-O4B) with relative occupancies 2/3:1/3 
 (fixed, after letting it refine to 0.66:0.34). Associated with this disorder 
 one of the lattice methanol molecule (O3S-C3S) has a partial 2/3 occupancy as 
 it shares space of the minor component of the ClO4 disorder (O4B). Another ClO4 
 ion (Cl4:Cl4B) is disordered over two positions with relative occupancies 0.388:0.612.
 Both disordered ClO4 ion were refined with 1,2 and 1,3 distance restraints as well
 as displacement parameters restraints. Displacement parameters restraints were also
 used for oxygens of another ClO4 ion (O4-O8) and lattice methanol molecules (O5S-O9S).
 Hydrogens on the lattice water molecules and methanol oxygens O1S to O5S were
 found in a difference Fourier map and first refined with distance restraints,
 based on the presence of H-bond acceptors. Hydrogens on the rest of lattice
 methanol molecules are omitted in the structural model as no clear acceptor was
 found for the OH moieties and fixing it using HFIX 147 did not converge 
 satisfactorilly. 
;

_vrf_PLAT417_lb2209              
;
PROBLEM: Short Inter D-H..H-D       H1S      ..H15A     .       1.72 Ang.      
RESPONSE: This short contact is likely due to the vicinity of the lattice
methanol O1S-C1S with the main residue, resulting from hydrogen bonding with
guest ClO4 ion, and O1S acting as an acceptor for H15A.
;

_vrf_PLAT315_lb2209              
;
PROBLEM: Singly Bonded Carbon Detected (H-atoms Missing).      
RESPONSE: Hydrogens on the lattice methanol molecules for which no clear 
acceptor was found for the OH moieties and fixing it using HFIX 147 did 
not converge satisfactorily (O6S, O7S, O8S, O9S) are omitted in the 
structural model, resulting in this alert.
;

_vrf_PLAT601_lb2209              
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of .        160 Ang**3      
RESPONSE: PLATON/SQUEEZE was used to analyze the remaining void space and
indeed recovered a total of 154 electron, mainly over four voids of 150,
150, 164 and 166 cubic angstrom. These figures would agree with four
additional diffuse methanol molecules per cell, one per void/formula unit.
This was therefore reflected in the formula, even though the hkl file was
not modified, because of the incompatibility of SQUEEZE and TwinRotMat
treatments.
;

_vrf_PLAT043_lb2209              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..      48.19 Check       
RESPONSE: Hydrogens on the lattice methanol molecules for which no clear 
acceptor was found for the OH moieties and fixing it using HFIX 147 did 
not converge satisfactorily (O6S, O7S, O8S, O9S) are omitted in the 
structural model.
In addition, one additional lattice methanol molecule has been to the 
on basis of analysis by PLATON/SQUEEZE of remaining void space.
All this results in a discrepancy between the reported formula and that
calculated from the atomic sites list.
;

_vrf_PLAT041_lb2209              
;
PROBLEM: Calc. and Reported SumFormula    Strings  Differ     Please Check        
RESPONSE: Hydrogens on the lattice methanol molecules for which no clear 
acceptor was found for the OH moieties and fixing it using HFIX 147 did 
not converge satisfactorily (O6S, O7S, O8S, O9S) are omitted in the 
structural model.
In addition, one additional lattice methanol molecule has been to the 
on basis of analysis by PLATON/SQUEEZE of remaining void space.
All this results in a discrepancy between the reported formula and that
calculated from the atomic sites list.
;

_vrf_FORMU01_lb2209              
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.        
RESPONSE: Hydrogens on the lattice methanol molecules for which no clear 
acceptor was found for the OH moieties and fixing it using HFIX 147 did 
not converge satisfactorily (O6S, O7S, O8S, O9S) are omitted in the 
structural model.
In addition, one additional lattice methanol molecule has been to the 
on basis of analysis by PLATON/SQUEEZE of remaining void space.
All this results in a discrepancy between the reported formula and that
calculated from the atomic sites list.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2325P)²+29.0700P] 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-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0055(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         27023
_refine_ls_number_parameters     1436
_refine_ls_number_restraints     418
_refine_ls_R_factor_all          0.1389
_refine_ls_R_factor_gt           0.1285
_refine_ls_wR_factor_ref         0.4114
_refine_ls_wR_factor_gt          0.4025
_refine_ls_goodness_of_fit_ref   1.043
_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 0.25849(3) 0.32042(5) 0.33423(3) 0.0392(2) Uani 1 1 d . . . . .
Fe2 Fe 0.74941(4) 0.31588(5) 0.34217(4) 0.0502(3) Uani 1 1 d . . . . .
N1 N 0.21195(19) 0.2302(3) 0.34999(19) 0.0422(10) Uani 1 1 d . . . . .
N2 N 0.30740(19) 0.2812(3) 0.39130(19) 0.0421(10) Uani 1 1 d . . . . .
N3 N 0.35627(19) 0.3013(3) 0.41957(19) 0.0422(10) Uani 1 1 d . . . . .
H3A H 0.380095 0.337164 0.411776 0.051 Uiso 1 1 calc R U . . .
N4 N 0.6725(2) 0.3683(3) 0.4212(2) 0.0466(11) Uani 1 1 d . . . . .
H4B H 0.653985 0.325657 0.425594 0.056 Uiso 1 1 calc R U . . .
N5 N 0.7122(2) 0.3775(3) 0.3889(2) 0.0506(12) Uani 1 1 d . . . . .
N6 N 0.7942(2) 0.4117(4) 0.3368(3) 0.0595(14) Uani 1 1 d . . . . .
N7 N 0.20666(19) 0.3474(3) 0.27404(19) 0.0428(10) Uani 1 1 d . . . . .
N8 N 0.29734(19) 0.2640(3) 0.28492(18) 0.0403(10) Uani 1 1 d . . . . .
N9 N 0.34209(19) 0.2151(3) 0.28365(19) 0.0423(10) Uani 1 1 d . . . . .
H9A H 0.366437 0.203471 0.309255 0.051 Uiso 1 1 calc R U . . .
N10 N 0.6606(2) 0.1864(3) 0.3296(2) 0.0480(12) Uani 1 1 d . . . . .
H10B H 0.635931 0.206999 0.306983 0.058 Uiso 1 1 calc R U . . .
N11 N 0.7068(2) 0.2229(3) 0.3524(2) 0.0489(12) Uani 1 1 d . . . . .
N12 N 0.8019(2) 0.2701(3) 0.3960(2) 0.0558(13) Uani 1 1 d . . . . .
N13 N 0.2153(2) 0.3851(3) 0.37976(19) 0.0435(10) Uani 1 1 d . . . . .
N14 N 0.30117(19) 0.4170(3) 0.32998(19) 0.0421(10) Uani 1 1 d . . . . .
N15 N 0.34297(19) 0.4462(3) 0.30466(19) 0.0409(10) Uani 1 1 d . . . . .
H15A H 0.361831 0.420653 0.283594 0.049 Uiso 1 1 calc R U . . .
N16 N 0.6577(2) 0.4044(3) 0.2767(2) 0.0509(12) Uani 1 1 d . . . . .
H16B H 0.639576 0.426421 0.299737 0.061 Uiso 1 1 calc R U . . .
N17 N 0.6998(2) 0.3516(3) 0.2856(2) 0.0520(12) Uani 1 1 d . . . . .
N18 N 0.7866(2) 0.2639(4) 0.2885(3) 0.0571(14) Uani 1 1 d . . . . .
C1 C 0.1630(2) 0.2050(4) 0.3252(3) 0.0482(13) Uani 1 1 d . . . . .
H1A H 0.149946 0.227762 0.294573 0.058 Uiso 1 1 calc R U . . .
C2 C 0.1311(3) 0.1470(5) 0.3429(3) 0.0588(17) Uani 1 1 d . . . . .
H2A H 0.097247 0.129808 0.323890 0.071 Uiso 1 1 calc R U . . .
C3 C 0.1475(3) 0.1129(5) 0.3882(3) 0.067(2) Uani 1 1 d . . . . .
C4 C 0.1984(3) 0.1388(5) 0.4134(3) 0.0596(18) Uani 1 1 d . . . . .
H4A H 0.211736 0.117284 0.444328 0.072 Uiso 1 1 calc R U . . .
C5 C 0.2298(3) 0.1960(4) 0.3935(2) 0.0492(14) Uani 1 1 d . . . . .
C6 C 0.2836(2) 0.2258(4) 0.4169(2) 0.0475(13) Uani 1 1 d . . . . .
C7 C 0.3173(3) 0.2109(4) 0.4605(3) 0.0537(15) Uani 1 1 d . . . . .
H7A H 0.309687 0.174795 0.484910 0.064 Uiso 1 1 calc R U . . .
C8 C 0.3639(2) 0.2593(4) 0.4613(2) 0.0465(13) Uani 1 1 d . . . . .
C9 C 0.4119(3) 0.2713(4) 0.5002(2) 0.0494(14) Uani 1 1 d . . . . .
C10 C 0.4091(3) 0.2330(5) 0.5450(3) 0.067(2) Uani 1 1 d . . . . .
H10A H 0.377848 0.199808 0.549416 0.080 Uiso 1 1 calc R U . . .
C11 C 0.4528(4) 0.2444(6) 0.5829(3) 0.079(3) Uani 1 1 d . . . . .
H11A H 0.452669 0.216466 0.612610 0.094 Uiso 1 1 calc R U . . .
C12 C 0.4969(3) 0.2966(6) 0.5774(3) 0.069(2) Uani 1 1 d . . . . .
H12A H 0.525396 0.306039 0.604030 0.083 Uiso 1 1 calc R U . . .
C13 C 0.4994(3) 0.3349(4) 0.5333(2) 0.0493(14) Uani 1 1 d . . . . .
C14 C 0.4574(2) 0.3205(4) 0.4942(2) 0.0467(13) Uani 1 1 d . . . . .
H14A H 0.459984 0.344547 0.463339 0.056 Uiso 1 1 calc R U . . .
C15 C 0.5463(2) 0.3909(4) 0.5275(2) 0.0480(13) Uani 1 1 d . . . . .
C16 C 0.5570(3) 0.4484(4) 0.5621(3) 0.0567(16) Uani 1 1 d . . . . .
H16A H 0.534501 0.450930 0.589384 0.068 Uiso 1 1 calc R U . . .
C17 C 0.5995(3) 0.5016(4) 0.5576(3) 0.0583(16) Uani 1 1 d . . . . .
H17A H 0.605278 0.541128 0.581184 0.070 Uiso 1 1 calc R U . . .
C18 C 0.6333(3) 0.4979(4) 0.5195(3) 0.0532(15) Uani 1 1 d . . . . .
H18A H 0.662284 0.535191 0.516356 0.064 Uiso 1 1 calc R U . . .
C19 C 0.6254(3) 0.4394(4) 0.4849(2) 0.0476(13) Uani 1 1 d . . . . .
C20 C 0.5803(3) 0.3868(4) 0.4888(2) 0.0473(13) Uani 1 1 d . . . . .
H20A H 0.573365 0.348264 0.464582 0.057 Uiso 1 1 calc R U . . .
C21 C 0.6649(3) 0.4342(4) 0.4463(3) 0.0523(14) Uani 1 1 d . . . . .
C22 C 0.7009(3) 0.4881(4) 0.4285(3) 0.0642(19) Uani 1 1 d . . . . .
H22A H 0.705388 0.539517 0.438524 0.077 Uiso 1 1 calc R U . . .
C23 C 0.7291(3) 0.4508(4) 0.3928(3) 0.0584(16) Uani 1 1 d . . . . .
C24 C 0.7737(3) 0.4724(4) 0.3612(3) 0.0607(17) Uani 1 1 d . . . . .
C25 C 0.7947(4) 0.5456(5) 0.3576(4) 0.074(2) Uani 1 1 d . . . . .
H25A H 0.779560 0.585812 0.375625 0.089 Uiso 1 1 calc R U . . .
C26 C 0.8385(4) 0.5594(6) 0.3271(4) 0.080(3) Uani 1 1 d . . . . .
C27 C 0.8606(3) 0.4975(5) 0.3037(4) 0.076(2) Uani 1 1 d . . . . .
H27A H 0.892129 0.504379 0.284391 0.092 Uiso 1 1 calc R U . . .
C28 C 0.8373(3) 0.4255(5) 0.3082(4) 0.068(2) Uani 1 1 d . . . . .
H28A H 0.852258 0.384700 0.290555 0.081 Uiso 1 1 calc R U . . .
C29 C 0.1126(4) 0.0514(7) 0.4090(4) 0.091(3) Uani 1 1 d . . . . .
H29A H 0.078345 0.040745 0.386214 0.137 Uiso 1 1 calc R U . . .
H29B H 0.136147 0.005447 0.413784 0.137 Uiso 1 1 calc R U . . .
H29C H 0.100405 0.067929 0.440746 0.137 Uiso 1 1 calc R U . . .
C30 C 0.8607(5) 0.6390(6) 0.3204(5) 0.103(4) Uani 1 1 d . . . . .
H30A H 0.839654 0.674468 0.339833 0.155 Uiso 1 1 calc R U . . .
H30B H 0.902053 0.641152 0.331387 0.155 Uiso 1 1 calc R U . . .
H30C H 0.854603 0.652994 0.285503 0.155 Uiso 1 1 calc R U . . .
C31 C 0.1601(2) 0.3926(4) 0.2711(2) 0.0454(12) Uani 1 1 d . . . . .
H31A H 0.149410 0.415729 0.300323 0.054 Uiso 1 1 calc R U . . .
C32 C 0.1265(3) 0.4071(4) 0.2266(3) 0.0505(14) Uani 1 1 d . . . . .
H32A H 0.094141 0.440161 0.226107 0.061 Uiso 1 1 calc R U . . .
C33 C 0.1404(2) 0.3737(4) 0.1837(2) 0.0481(13) Uani 1 1 d . . . . .
C34 C 0.1889(3) 0.3267(4) 0.1863(2) 0.0459(12) Uani 1 1 d . . . . .
H34A H 0.200146 0.302882 0.157456 0.055 Uiso 1 1 calc R U . . .
C35 C 0.2208(2) 0.3150(3) 0.2319(2) 0.0416(11) Uani 1 1 d . . . . .
C36 C 0.2717(2) 0.2657(3) 0.2388(2) 0.0419(11) Uani 1 1 d . . . . .
C37 C 0.2994(2) 0.2189(4) 0.2079(2) 0.0458(12) Uani 1 1 d . . . . .
H37A H 0.289612 0.210693 0.173743 0.055 Uiso 1 1 calc R U . . .
C38 C 0.3446(2) 0.1865(3) 0.2379(2) 0.0438(12) Uani 1 1 d . . . . .
C39 C 0.3874(2) 0.1303(3) 0.2246(2) 0.0445(12) Uani 1 1 d . . . . .
C40 C 0.3777(3) 0.0953(4) 0.1787(3) 0.0561(16) Uani 1 1 d . . . . .
H40A H 0.345023 0.109134 0.156889 0.067 Uiso 1 1 calc R U . . .
C41 C 0.4154(3) 0.0407(5) 0.1648(3) 0.0604(17) Uani 1 1 d . . . . .
H41A H 0.408415 0.017199 0.133487 0.073 Uiso 1 1 calc R U . . .
C42 C 0.4635(3) 0.0196(4) 0.1962(3) 0.0560(15) Uani 1 1 d . . . . .
H42A H 0.489410 -0.017953 0.186417 0.067 Uiso 1 1 calc R U . . .
C43 C 0.4734(2) 0.0543(3) 0.2425(3) 0.0474(13) Uani 1 1 d . . . . .
C44 C 0.4356(2) 0.1097(3) 0.2561(2) 0.0437(12) Uani 1 1 d . . . . .
H44A H 0.442673 0.133865 0.287236 0.052 Uiso 1 1 calc R U . . .
C45 C 0.5245(2) 0.0288(3) 0.2760(3) 0.0481(13) Uani 1 1 d . . . . .
C46 C 0.5372(3) -0.0487(4) 0.2821(3) 0.0586(17) Uani 1 1 d . . . . .
H46A H 0.511709 -0.085742 0.266826 0.070 Uiso 1 1 calc R U . . .
C47 C 0.5872(3) -0.0709(4) 0.3104(4) 0.069(2) Uani 1 1 d . . . . .
H47A H 0.595123 -0.123474 0.314746 0.083 Uiso 1 1 calc R U . . .
C48 C 0.6252(3) -0.0193(4) 0.3322(3) 0.066(2) Uani 1 1 d . . . . .
H48A H 0.658900 -0.036191 0.351590 0.079 Uiso 1 1 calc R U . . .
C49 C 0.6145(3) 0.0600(4) 0.3259(3) 0.0537(15) Uani 1 1 d . . . . .
C50 C 0.5617(2) 0.0820(4) 0.2989(3) 0.0499(14) Uani 1 1 d . . . . .
H50A H 0.551859 0.134267 0.296533 0.060 Uiso 1 1 calc R U . . .
C51 C 0.6571(3) 0.1137(4) 0.3461(3) 0.0542(15) Uani 1 1 d . . . . .
C52 C 0.7041(3) 0.1034(4) 0.3817(3) 0.0557(16) Uani 1 1 d . . . . .
H52A H 0.713965 0.059081 0.400353 0.067 Uiso 1 1 calc R U . . .
C53 C 0.7329(3) 0.1724(4) 0.3836(3) 0.0523(15) Uani 1 1 d . . . . .
C54 C 0.7861(3) 0.2001(4) 0.4112(3) 0.0528(15) Uani 1 1 d . . . . .
C55 C 0.8174(3) 0.1612(5) 0.4483(3) 0.0600(17) Uani 1 1 d . . . . .
H55A H 0.804416 0.113069 0.458426 0.072 Uiso 1 1 calc R U . . .
C56 C 0.8681(3) 0.1925(6) 0.4710(3) 0.072(2) Uani 1 1 d . . . . .
C57 C 0.8843(3) 0.2628(6) 0.4556(3) 0.071(2) Uani 1 1 d . . . . .
H57A H 0.918631 0.285708 0.470642 0.086 Uiso 1 1 calc R U . . .
C58 C 0.8514(3) 0.3002(5) 0.4188(3) 0.0642(19) Uani 1 1 d . . . . .
H58A H 0.863631 0.348695 0.408778 0.077 Uiso 1 1 calc R U . . .
C59 C 0.1040(3) 0.3854(5) 0.1355(3) 0.0628(18) Uani 1 1 d . . . . .
H59A H 0.120859 0.357125 0.109511 0.094 Uiso 1 1 calc R U . . .
H59B H 0.064591 0.367235 0.138472 0.094 Uiso 1 1 calc R U . . .
H59C H 0.102892 0.439540 0.127314 0.094 Uiso 1 1 calc R U . . .
C60 C 0.9019(4) 0.1499(8) 0.5125(4) 0.100(4) Uani 1 1 d . . . . .
H60A H 0.883002 0.101168 0.517580 0.150 Uiso 1 1 calc R U . . .
H60B H 0.941386 0.140980 0.504104 0.150 Uiso 1 1 calc R U . . .
H60C H 0.903050 0.179989 0.542804 0.150 Uiso 1 1 calc R U . . .
C61 C 0.1699(2) 0.3662(4) 0.4042(3) 0.0498(14) Uani 1 1 d . . . . .
H61A H 0.152774 0.317734 0.398302 0.060 Uiso 1 1 calc R U . . .
C62 C 0.1470(3) 0.4137(4) 0.4373(3) 0.0521(14) Uani 1 1 d . . . . .
H62A H 0.114300 0.397824 0.452988 0.063 Uiso 1 1 calc R U . . .
C63 C 0.1715(3) 0.4857(4) 0.4483(3) 0.0534(15) Uani 1 1 d . . . . .
C64 C 0.2179(3) 0.5051(4) 0.4224(2) 0.0490(13) Uani 1 1 d . . . . .
H64A H 0.236561 0.552656 0.428183 0.059 Uiso 1 1 calc R U . . .
C65 C 0.2373(2) 0.4553(4) 0.3882(2) 0.0437(12) Uani 1 1 d . . . . .
C66 C 0.2837(2) 0.4735(3) 0.3578(2) 0.0415(11) Uani 1 1 d . . . . .
C67 C 0.3142(2) 0.5399(4) 0.3497(2) 0.0466(13) Uani 1 1 d . . . . .
H67A H 0.309619 0.588068 0.364461 0.056 Uiso 1 1 calc R U . . .
C68 C 0.3522(2) 0.5210(3) 0.3161(2) 0.0432(12) Uani 1 1 d . . . . .
C69 C 0.3953(2) 0.5695(3) 0.2956(2) 0.0411(11) Uani 1 1 d . . . . .
C70 C 0.3935(2) 0.6477(3) 0.3039(2) 0.0455(12) Uani 1 1 d . . . . .
H70A H 0.364743 0.667953 0.322607 0.055 Uiso 1 1 calc R U . . .
C71 C 0.4328(2) 0.6959(3) 0.2853(2) 0.0449(12) Uani 1 1 d . . . . .
H71A H 0.431129 0.748818 0.291391 0.054 Uiso 1 1 calc R U . . .
C72 C 0.4746(2) 0.6670(3) 0.2578(2) 0.0452(12) Uani 1 1 d . . . . .
H72A H 0.501008 0.700457 0.244437 0.054 Uiso 1 1 calc R U . . .
C73 C 0.4785(2) 0.5891(3) 0.2494(2) 0.0431(12) Uani 1 1 d . . . . .
C74 C 0.4389(2) 0.5409(3) 0.2690(2) 0.0440(12) Uani 1 1 d . . . . .
H74A H 0.441659 0.487679 0.264172 0.053 Uiso 1 1 calc R U . . .
C75 C 0.5226(2) 0.5596(3) 0.2186(2) 0.0461(13) Uani 1 1 d . . . . .
C76 C 0.5316(3) 0.5938(4) 0.1736(3) 0.0512(14) Uani 1 1 d . . . . .
H76A H 0.507111 0.634300 0.161660 0.061 Uiso 1 1 calc R U . . .
C77 C 0.5751(3) 0.5700(4) 0.1463(3) 0.0601(17) Uani 1 1 d . . . . .
H77A H 0.579534 0.593145 0.115439 0.072 Uiso 1 1 calc R U . . .
C78 C 0.6127(3) 0.5120(4) 0.1637(3) 0.0570(16) Uani 1 1 d . . . . .
H78A H 0.643335 0.496590 0.145195 0.068 Uiso 1 1 calc R U . . .
C79 C 0.6047(3) 0.4765(4) 0.2087(3) 0.0510(14) Uani 1 1 d . . . . .
C80 C 0.5593(2) 0.4998(3) 0.2351(2) 0.0456(13) Uani 1 1 d . . . . .
H80A H 0.553131 0.474720 0.264971 0.055 Uiso 1 1 calc R U . . .
C81 C 0.6467(3) 0.4190(4) 0.2278(3) 0.0524(14) Uani 1 1 d . . . . .
C82 C 0.6832(3) 0.3737(4) 0.2039(3) 0.0578(16) Uani 1 1 d . . . . .
H82A H 0.685883 0.370468 0.169461 0.069 Uiso 1 1 calc R U . . .
C83 C 0.7151(3) 0.3337(4) 0.2407(3) 0.0543(15) Uani 1 1 d . . . . .
C84 C 0.7629(3) 0.2791(4) 0.2422(3) 0.0570(16) Uani 1 1 d . . . . .
C85 C 0.7823(3) 0.2461(5) 0.2006(3) 0.068(2) Uani 1 1 d . . . . .
H85A H 0.764937 0.258405 0.168670 0.082 Uiso 1 1 calc R U . . .
C86 C 0.8289(3) 0.1934(5) 0.2070(4) 0.068(2) Uani 1 1 d . . . . .
C87 C 0.8509(3) 0.1776(5) 0.2545(4) 0.072(2) Uani 1 1 d . . . . .
H87A H 0.880881 0.141065 0.260118 0.087 Uiso 1 1 calc R U . . .
C88 C 0.8306(3) 0.2135(5) 0.2935(3) 0.0644(19) Uani 1 1 d . . . . .
H88A H 0.848131 0.202628 0.325628 0.077 Uiso 1 1 calc R U . . .
C89 C 0.1502(3) 0.5377(5) 0.4859(3) 0.068(2) Uani 1 1 d . . . . .
H89A H 0.117308 0.514271 0.500092 0.102 Uiso 1 1 calc R U . . .
H89B H 0.181355 0.547174 0.512026 0.102 Uiso 1 1 calc R U . . .
H89C H 0.137930 0.585881 0.470268 0.102 Uiso 1 1 calc R U . . .
C90 C 0.8506(5) 0.1546(7) 0.1631(5) 0.096(3) Uani 1 1 d . . . . .
H90A H 0.829273 0.173744 0.132854 0.144 Uiso 1 1 calc R U . . .
H90B H 0.891911 0.165087 0.162326 0.144 Uiso 1 1 calc R U . . .
H90C H 0.844570 0.099751 0.165483 0.144 Uiso 1 1 calc R U . . .
Cl1 Cl 0.48340(13) 0.32172(17) 0.34612(10) 0.0589(6) Uani 0.6667 1 d D U P A 1
Cl1B Cl 0.5081(3) 0.3557(4) 0.3462(2) 0.0741(13) Uani 0.3333 1 d D U P A 2
O1 O 0.4512(2) 0.3742(3) 0.3676(2) 0.0697(12) Uani 1 1 d D U . . .
O2 O 0.4887(3) 0.3401(5) 0.2966(2) 0.0955(18) Uani 1 1 d D U . . .
O3 O 0.5383(3) 0.3065(4) 0.3716(3) 0.0998(19) Uani 1 1 d D U . . .
O4 O 0.4560(4) 0.2484(5) 0.3490(4) 0.094(3) Uani 0.6667 1 d D U P A 1
O4B O 0.5385(7) 0.4261(8) 0.3476(6) 0.121(5) Uani 0.3333 1 d D U P A 2
Cl2 Cl 0.74335(9) 0.26231(11) 0.55879(6) 0.0613(4) Uani 1 1 d . . . . .
O5 O 0.7528(3) 0.3037(4) 0.5160(2) 0.0821(18) Uani 1 1 d . . . . .
O6 O 0.7277(5) 0.3090(4) 0.5968(2) 0.109(3) Uani 1 1 d . . . . .
O7 O 0.7906(4) 0.2163(7) 0.5761(3) 0.129(4) Uani 1 1 d . . . . .
O8 O 0.6958(5) 0.2107(5) 0.5471(3) 0.126(4) Uani 1 1 d . . . . .
Cl3 Cl 0.49842(9) 0.81596(10) 0.14832(9) 0.0656(5) Uani 1 1 d . . . . .
O9 O 0.5085(4) 0.8812(4) 0.1208(3) 0.108(3) Uani 1 1 d . . . . .
O10 O 0.4776(4) 0.7557(4) 0.1156(3) 0.098(2) Uani 1 1 d D . . . .
O11 O 0.4545(3) 0.8319(4) 0.1799(3) 0.090(2) Uani 1 1 d . . . . .
O12 O 0.5485(3) 0.7934(5) 0.1770(4) 0.101(2) Uani 1 1 d . . . . .
Cl4 Cl 0.7756(6) -0.1034(8) 0.4320(5) 0.102(3) Uani 0.388(10) 1 d D U P B 1
O13 O 0.7710(9) -0.0501(11) 0.3929(7) 0.094(4) Uani 0.388(10) 1 d D U P B 1
O14 O 0.7182(8) -0.1269(13) 0.4401(8) 0.129(4) Uani 0.388(10) 1 d D U P B 1
O15 O 0.8035(10) -0.0713(13) 0.4743(7) 0.137(5) Uani 0.388(10) 1 d D U P B 1
O16 O 0.8056(10) -0.1677(10) 0.4164(8) 0.125(5) Uani 0.388(10) 1 d D U P B 1
Cl4B Cl 0.7596(4) -0.1015(4) 0.4347(3) 0.0889(17) Uani 0.612(10) 1 d D U P B 2
O13B O 0.7873(6) -0.0453(8) 0.4104(5) 0.106(4) Uani 0.612(10) 1 d D U P B 2
O14B O 0.7096(6) -0.0691(8) 0.4551(5) 0.121(4) Uani 0.612(10) 1 d D U P B 2
O15B O 0.7932(6) -0.1398(8) 0.4712(4) 0.119(4) Uani 0.612(10) 1 d D U P B 2
O16B O 0.7343(7) -0.1558(8) 0.3986(5) 0.142(4) Uani 0.612(10) 1 d D U P B 2
O1S O 0.3871(4) 0.3703(5) 0.2288(3) 0.114(3) Uani 1 1 d D . . . .
H1S H 0.415(5) 0.375(8) 0.255(4) 0.171 Uiso 1 1 d D U . . .
C1S C 0.3877(10) 0.3776(12) 0.1835(5) 0.177(10) Uani 1 1 d . . . . .
H1S1 H 0.356903 0.412626 0.170993 0.266 Uiso 1 1 calc R U . . .
H1S2 H 0.381294 0.328110 0.167528 0.266 Uiso 1 1 calc R U . . .
H1S3 H 0.425222 0.397826 0.176172 0.266 Uiso 1 1 calc R U . . .
O2S O 0.3773(4) 0.1294(4) 0.3645(3) 0.091(2) Uani 1 1 d D . . . .
H2S H 0.351(4) 0.092(6) 0.355(5) 0.136 Uiso 1 1 d D U . . .
C2S C 0.4257(6) 0.1043(8) 0.3950(5) 0.113(4) Uani 1 1 d . . . . .
H2S1 H 0.451090 0.147434 0.404033 0.170 Uiso 1 1 calc R U . . .
H2S2 H 0.446798 0.066522 0.377376 0.170 Uiso 1 1 calc R U . . .
H2S3 H 0.412857 0.081416 0.424807 0.170 Uiso 1 1 calc R U . . .
O3S O 0.5926(3) 0.4550(5) 0.3503(3) 0.069(2) Uani 0.6667 1 d D . P C 1
H3S H 0.560108 0.412022 0.344921 0.103 Uiso 0.6667 1 d DR U P C 1
C3S C 0.5604(6) 0.5124(9) 0.3714(6) 0.080(4) Uani 0.6667 1 d . . P C 1
H3S1 H 0.536952 0.489902 0.395560 0.119 Uiso 0.6667 1 calc R U P C 1
H3S2 H 0.535080 0.537410 0.345472 0.119 Uiso 0.6667 1 calc R U P C 1
H3S3 H 0.587006 0.549813 0.387663 0.119 Uiso 0.6667 1 calc R U P C 1
O4S O 0.6389(2) 0.2276(3) 0.4519(2) 0.0659(13) Uani 1 1 d . . . . .
H4S H 0.654806 0.231226 0.480751 0.099 Uiso 1 1 calc R U . . .
C4S C 0.5890(4) 0.1801(5) 0.4515(4) 0.081(3) Uani 1 1 d . . . . .
H4S1 H 0.600465 0.127027 0.448044 0.122 Uiso 1 1 calc R U . . .
H4S2 H 0.561026 0.194210 0.423881 0.122 Uiso 1 1 calc R U . . .
H4S3 H 0.571354 0.186471 0.482489 0.122 Uiso 1 1 calc R U . . .
O5S O 0.2885(5) 0.0301(6) 0.3409(4) 0.132(3) Uani 1 1 d D U . . .
H5S H 0.267936 0.013237 0.362176 0.198 Uiso 1 1 d R U . . .
C5S C 0.2544(5) 0.0377(7) 0.2953(5) 0.099(3) Uani 1 1 d . U . . .
H5S1 H 0.220241 0.005105 0.295053 0.148 Uiso 1 1 calc R U . . .
H5S2 H 0.277323 0.022681 0.268512 0.148 Uiso 1 1 calc R U . . .
H5S3 H 0.242199 0.090641 0.290662 0.148 Uiso 1 1 calc R U . . .
O6S O 0.2524(6) -0.0542(6) 0.4126(4) 0.144(4) Uani 1 1 d . U . . .
C6S C 0.2783(12) -0.0315(10) 0.4564(7) 0.166(6) Uani 1 1 d . U . . .
O7S O 0.5373(7) 0.2846(8) 0.1594(5) 0.187(6) Uani 1 1 d . U . . .
C7S C 0.4928(10) 0.2321(12) 0.1437(9) 0.183(7) Uani 1 1 d . U . . .
O8S O 0.4802(8) 0.9319(11) -0.0270(7) 0.215(6) Uani 1 1 d D U . . .
C8S C 0.4603(12) 0.9585(15) -0.0708(9) 0.193(8) Uani 1 1 d . U . . .
O9S O 0.7494(7) 0.1852(6) 0.0707(4) 0.165(5) Uani 1 1 d . U . . .
C9S C 0.7178(10) 0.1701(10) 0.0312(7) 0.161(7) Uani 1 1 d . U . . .
O1W O 0.5811(2) 0.2590(3) 0.2580(2) 0.0660(13) Uani 1 1 d D . . . .
H1W H 0.554(3) 0.279(6) 0.276(3) 0.099 Uiso 1 1 d D U . . .
H2W H 0.564(4) 0.266(6) 0.2267(14) 0.099 Uiso 1 1 d D U . . .
O2W O 0.4587(5) 0.7867(8) 0.0114(4) 0.167(5) Uani 1 1 d D U . . .
H3W H 0.467766 0.769362 0.044076 0.250 Uiso 1 1 d DR U . . .
H4W H 0.479146 0.835522 0.011156 0.250 Uiso 1 1 d DR U . . .


_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 N8 1.961(5) . ?
Fe1 N2 1.964(5) . ?
Fe1 N14 1.979(5) . ?
Fe1 N1 1.993(5) . ?
Fe1 N7 1.999(5) . ?
Fe1 N13 2.022(5) . ?
Fe2 N17 1.941(6) . ?
Fe2 N5 1.941(6) . ?
Fe2 N11 1.949(6) . ?
Fe2 N12 1.989(6) . ?
Fe2 N18 1.993(6) . ?
Fe2 N6 1.997(6) . ?
N1 C1 1.342(7) . ?
N1 C5 1.360(8) . ?
N2 C6 1.348(8) . ?
N2 N3 1.357(6) . ?
N3 C8 1.355(8) . ?
N3 H3A 0.8800 . ?
N4 N5 1.344(8) . ?
N4 C21 1.369(9) . ?
N4 H4B 0.8800 . ?
N5 C23 1.351(9) . ?
N6 C28 1.349(9) . ?
N6 C24 1.370(10) . ?
N7 C31 1.339(7) . ?
N7 C35 1.353(8) . ?
N8 C36 1.339(7) . ?
N8 N9 1.353(6) . ?
N9 C38 1.354(8) . ?
N9 H9A 0.8800 . ?
N10 N11 1.350(7) . ?
N10 C51 1.364(8) . ?
N10 H10B 0.8800 . ?
N11 C53 1.335(8) . ?
N12 C54 1.362(9) . ?
N12 C58 1.361(9) . ?
N13 C61 1.341(8) . ?
N13 C65 1.351(8) . ?
N14 C66 1.339(8) . ?
N14 N15 1.347(7) . ?
N15 C68 1.367(8) . ?
N15 H15A 0.8800 . ?
N16 N17 1.355(7) . ?
N16 C81 1.358(9) . ?
N16 H16B 0.8800 . ?
N17 C83 1.345(9) . ?
N18 C88 1.351(8) . ?
N18 C84 1.355(10) . ?
C1 C2 1.377(9) . ?
C1 H1A 0.9500 . ?
C2 C3 1.393(11) . ?
C2 H2A 0.9500 . ?
C3 C4 1.386(9) . ?
C3 C29 1.499(10) . ?
C4 C5 1.386(9) . ?
C4 H4A 0.9500 . ?
C5 C6 1.446(7) . ?
C6 C7 1.386(9) . ?
C7 C8 1.377(8) . ?
C7 H7A 0.9500 . ?
C8 C9 1.479(8) . ?
C9 C14 1.388(8) . ?
C9 C10 1.404(10) . ?
C10 C11 1.392(9) . ?
C10 H10A 0.9500 . ?
C11 C12 1.396(10) . ?
C11 H11A 0.9500 . ?
C12 C13 1.385(9) . ?
C12 H12A 0.9500 . ?
C13 C14 1.398(8) . ?
C13 C15 1.488(9) . ?
C14 H14A 0.9500 . ?
C15 C20 1.382(9) . ?
C15 C16 1.392(9) . ?
C16 C17 1.375(10) . ?
C16 H16A 0.9500 . ?
C17 C18 1.365(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.397(9) . ?
C18 H18A 0.9500 . ?
C19 C20 1.410(8) . ?
C19 C21 1.466(10) . ?
C20 H20A 0.9500 . ?
C21 C22 1.384(9) . ?
C22 C23 1.390(11) . ?
C22 H22A 0.9500 . ?
C23 C24 1.461(10) . ?
C24 C25 1.386(11) . ?
C25 C26 1.394(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.388(14) . ?
C26 C30 1.513(13) . ?
C27 C28 1.389(12) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.402(9) . ?
C31 H31A 0.9500 . ?
C32 C33 1.376(10) . ?
C32 H32A 0.9500 . ?
C33 C34 1.395(8) . ?
C33 C59 1.507(9) . ?
C34 C35 1.402(8) . ?
C34 H34A 0.9500 . ?
C35 C36 1.465(7) . ?
C36 C37 1.381(8) . ?
C37 C38 1.390(8) . ?
C37 H37A 0.9500 . ?
C38 C39 1.473(8) . ?
C39 C44 1.392(8) . ?
C39 C40 1.397(9) . ?
C40 C41 1.377(9) . ?
C40 H40A 0.9500 . ?
C41 C42 1.393(10) . ?
C41 H41A 0.9500 . ?
C42 C43 1.402(10) . ?
C42 H42A 0.9500 . ?
C43 C44 1.389(8) . ?
C43 C45 1.496(8) . ?
C44 H44A 0.9500 . ?
C45 C50 1.383(9) . ?
C45 C46 1.405(9) . ?
C46 C47 1.388(10) . ?
C46 H46A 0.9500 . ?
C47 C48 1.363(11) . ?
C47 H47A 0.9500 . ?
C48 C49 1.428(9) . ?
C48 H48A 0.9500 . ?
C49 C50 1.421(8) . ?
C49 C51 1.442(9) . ?
C50 H50A 0.9500 . ?
C51 C52 1.400(9) . ?
C52 C53 1.388(10) . ?
C52 H52A 0.9500 . ?
C53 C54 1.467(9) . ?
C54 C55 1.373(10) . ?
C55 C56 1.391(10) . ?
C55 H55A 0.9500 . ?
C56 C57 1.373(14) . ?
C56 C60 1.515(12) . ?
C57 C58 1.372(11) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.376(10) . ?
C61 H61A 0.9500 . ?
C62 C63 1.412(10) . ?
C62 H62A 0.9500 . ?
C63 C64 1.387(9) . ?
C63 C89 1.496(10) . ?
C64 C65 1.388(9) . ?
C64 H64A 0.9500 . ?
C65 C66 1.457(8) . ?
C66 C67 1.396(8) . ?
C67 C68 1.375(9) . ?
C67 H67A 0.9500 . ?
C68 C69 1.466(8) . ?
C69 C74 1.395(8) . ?
C69 C70 1.398(8) . ?
C70 C71 1.378(8) . ?
C70 H70A 0.9500 . ?
C71 C72 1.379(9) . ?
C71 H71A 0.9500 . ?
C72 C73 1.396(8) . ?
C72 H72A 0.9500 . ?
C73 C74 1.397(8) . ?
C73 C75 1.480(9) . ?
C74 H74A 0.9500 . ?
C75 C80 1.402(8) . ?
C75 C76 1.403(9) . ?
C76 C77 1.376(10) . ?
C76 H76A 0.9500 . ?
C77 C78 1.399(10) . ?
C77 H77A 0.9500 . ?
C78 C79 1.408(10) . ?
C78 H78A 0.9500 . ?
C79 C80 1.394(9) . ?
C79 C81 1.466(9) . ?
C80 H80A 0.9500 . ?
C81 C82 1.374(10) . ?
C82 C83 1.383(10) . ?
C82 H82A 0.9500 . ?
C83 C84 1.467(9) . ?
C84 C85 1.389(11) . ?
C85 C86 1.424(10) . ?
C85 H85A 0.9500 . ?
C86 C87 1.374(14) . ?
C86 C90 1.509(13) . ?
C87 C88 1.362(12) . ?
C87 H87A 0.9500 . ?
C88 H88A 0.9500 . ?
C89 H89A 0.9800 . ?
C89 H89B 0.9800 . ?
C89 H89C 0.9800 . ?
C90 H90A 0.9800 . ?
C90 H90B 0.9800 . ?
C90 H90C 0.9800 . ?
Cl1 O1 1.359(6) . ?
Cl1 O2 1.408(6) . ?
Cl1 O3 1.419(6) . ?
Cl1 O4 1.446(8) . ?
Cl1B O3 1.278(8) . ?
Cl1B O2 1.414(8) . ?
Cl1B O4B 1.426(11) . ?
Cl1B O1 1.532(8) . ?
Cl2 O6 1.399(7) . ?
Cl2 O7 1.410(7) . ?
Cl2 O5 1.413(6) . ?
Cl2 O8 1.442(8) . ?
Cl3 O12 1.395(7) . ?
Cl3 O9 1.407(7) . ?
Cl3 O11 1.425(7) . ?
Cl3 O10 1.441(8) . ?
Cl4 O15 1.389(14) . ?
Cl4 O13 1.419(14) . ?
Cl4 O16 1.420(14) . ?
Cl4 O14 1.431(14) . ?
Cl4B O15B 1.383(11) . ?
Cl4B O13B 1.384(10) . ?
Cl4B O14B 1.453(11) . ?
Cl4B O16B 1.458(12) . ?
O1S C1S 1.246(15) . ?
O1S H1S 0.92(2) . ?
C1S H1S1 0.9800 . ?
C1S H1S2 0.9800 . ?
C1S H1S3 0.9800 . ?
O2S C2S 1.404(13) . ?
O2S H2S 0.918(19) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
O3S C3S 1.413(16) . ?
O3S H3S 1.0687 . ?
C3S H3S1 0.9800 . ?
C3S H3S2 0.9800 . ?
C3S H3S3 0.9800 . ?
O4S C4S 1.429(10) . ?
O4S H4S 0.8400 . ?
C4S H4S1 0.9800 . ?
C4S H4S2 0.9800 . ?
C4S H4S3 0.9800 . ?
O5S C5S 1.417(15) . ?
O5S H5S 0.8399 . ?
C5S H5S1 0.9800 . ?
C5S H5S2 0.9800 . ?
C5S H5S3 0.9800 . ?
O6S C6S 1.35(2) . ?
O7S C7S 1.42(2) . ?
O8S C8S 1.33(3) . ?
O9S C9S 1.272(19) . ?
O1W H1W 0.92(2) . ?
O1W H2W 0.92(2) . ?
O2W H3W 0.9479 . ?
O2W H4W 0.9846 . ?

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
N8 Fe1 N2 95.5(2) . . ?
N8 Fe1 N14 97.5(2) . . ?
N2 Fe1 N14 95.4(2) . . ?
N8 Fe1 N1 92.1(2) . . ?
N2 Fe1 N1 80.32(19) . . ?
N14 Fe1 N1 169.8(2) . . ?
N8 Fe1 N7 80.6(2) . . ?
N2 Fe1 N7 173.1(2) . . ?
N14 Fe1 N7 90.7(2) . . ?
N1 Fe1 N7 94.1(2) . . ?
N8 Fe1 N13 174.5(2) . . ?
N2 Fe1 N13 89.7(2) . . ?
N14 Fe1 N13 80.3(2) . . ?
N1 Fe1 N13 90.4(2) . . ?
N7 Fe1 N13 94.3(2) . . ?
N17 Fe2 N5 94.2(2) . . ?
N17 Fe2 N11 96.7(2) . . ?
N5 Fe2 N11 96.5(2) . . ?
N17 Fe2 N12 174.2(3) . . ?
N5 Fe2 N12 91.2(3) . . ?
N11 Fe2 N12 80.5(2) . . ?
N17 Fe2 N18 80.3(2) . . ?
N5 Fe2 N18 172.7(2) . . ?
N11 Fe2 N18 88.9(2) . . ?
N12 Fe2 N18 94.5(3) . . ?
N17 Fe2 N6 86.6(3) . . ?
N5 Fe2 N6 80.9(2) . . ?
N11 Fe2 N6 176.0(3) . . ?
N12 Fe2 N6 96.4(3) . . ?
N18 Fe2 N6 94.0(3) . . ?
C1 N1 C5 117.8(5) . . ?
C1 N1 Fe1 127.3(4) . . ?
C5 N1 Fe1 114.5(4) . . ?
C6 N2 N3 104.9(5) . . ?
C6 N2 Fe1 115.5(4) . . ?
N3 N2 Fe1 138.4(4) . . ?
C8 N3 N2 111.7(5) . . ?
C8 N3 H3A 124.1 . . ?
N2 N3 H3A 124.1 . . ?
N5 N4 C21 110.7(5) . . ?
N5 N4 H4B 124.6 . . ?
C21 N4 H4B 124.6 . . ?
N4 N5 C23 106.1(6) . . ?
N4 N5 Fe2 137.6(4) . . ?
C23 N5 Fe2 116.3(5) . . ?
C28 N6 C24 116.8(7) . . ?
C28 N6 Fe2 128.0(6) . . ?
C24 N6 Fe2 114.7(4) . . ?
C31 N7 C35 117.5(5) . . ?
C31 N7 Fe1 127.6(4) . . ?
C35 N7 Fe1 114.9(4) . . ?
C36 N8 N9 105.2(5) . . ?
C36 N8 Fe1 116.2(4) . . ?
N9 N8 Fe1 138.2(4) . . ?
N8 N9 C38 111.2(5) . . ?
N8 N9 H9A 124.4 . . ?
C38 N9 H9A 124.4 . . ?
N11 N10 C51 111.5(5) . . ?
N11 N10 H10B 124.3 . . ?
C51 N10 H10B 124.3 . . ?
C53 N11 N10 105.6(5) . . ?
C53 N11 Fe2 116.5(4) . . ?
N10 N11 Fe2 136.6(4) . . ?
C54 N12 C58 117.1(6) . . ?
C54 N12 Fe2 115.4(4) . . ?
C58 N12 Fe2 127.6(5) . . ?
C61 N13 C65 116.5(5) . . ?
C61 N13 Fe1 128.6(4) . . ?
C65 N13 Fe1 114.8(4) . . ?
C66 N14 N15 106.1(5) . . ?
C66 N14 Fe1 115.3(4) . . ?
N15 N14 Fe1 138.5(4) . . ?
N14 N15 C68 111.0(5) . . ?
N14 N15 H15A 124.5 . . ?
C68 N15 H15A 124.5 . . ?
N17 N16 C81 111.8(6) . . ?
N17 N16 H16B 124.1 . . ?
C81 N16 H16B 124.1 . . ?
C83 N17 N16 104.3(6) . . ?
C83 N17 Fe2 117.4(4) . . ?
N16 N17 Fe2 136.8(5) . . ?
C88 N18 C84 117.3(7) . . ?
C88 N18 Fe2 127.2(6) . . ?
C84 N18 Fe2 115.4(4) . . ?
N1 C1 C2 121.7(6) . . ?
N1 C1 H1A 119.1 . . ?
C2 C1 H1A 119.1 . . ?
C1 C2 C3 121.5(6) . . ?
C1 C2 H2A 119.3 . . ?
C3 C2 H2A 119.3 . . ?
C4 C3 C2 116.5(6) . . ?
C4 C3 C29 121.1(7) . . ?
C2 C3 C29 122.5(7) . . ?
C3 C4 C5 120.0(7) . . ?
C3 C4 H4A 120.0 . . ?
C5 C4 H4A 120.0 . . ?
N1 C5 C4 122.4(5) . . ?
N1 C5 C6 113.7(5) . . ?
C4 C5 C6 123.8(6) . . ?
N2 C6 C7 110.9(5) . . ?
N2 C6 C5 114.5(5) . . ?
C7 C6 C5 134.6(6) . . ?
C8 C7 C6 105.9(6) . . ?
C8 C7 H7A 127.1 . . ?
C6 C7 H7A 127.1 . . ?
N3 C8 C7 106.6(5) . . ?
N3 C8 C9 123.6(5) . . ?
C7 C8 C9 129.6(6) . . ?
C14 C9 C10 120.1(6) . . ?
C14 C9 C8 122.4(6) . . ?
C10 C9 C8 117.5(6) . . ?
C11 C10 C9 119.1(7) . . ?
C11 C10 H10A 120.4 . . ?
C9 C10 H10A 120.4 . . ?
C10 C11 C12 120.3(7) . . ?
C10 C11 H11A 119.8 . . ?
C12 C11 H11A 119.8 . . ?
C13 C12 C11 120.5(6) . . ?
C13 C12 H12A 119.8 . . ?
C11 C12 H12A 119.8 . . ?
C12 C13 C14 119.3(6) . . ?
C12 C13 C15 120.4(5) . . ?
C14 C13 C15 120.3(6) . . ?
C9 C14 C13 120.5(6) . . ?
C9 C14 H14A 119.8 . . ?
C13 C14 H14A 119.8 . . ?
C20 C15 C16 118.6(6) . . ?
C20 C15 C13 121.6(6) . . ?
C16 C15 C13 119.8(6) . . ?
C17 C16 C15 121.3(7) . . ?
C17 C16 H16A 119.4 . . ?
C15 C16 H16A 119.4 . . ?
C18 C17 C16 120.4(7) . . ?
C18 C17 H17A 119.8 . . ?
C16 C17 H17A 119.8 . . ?
C17 C18 C19 120.1(6) . . ?
C17 C18 H18A 120.0 . . ?
C19 C18 H18A 120.0 . . ?
C18 C19 C20 119.1(6) . . ?
C18 C19 C21 118.8(6) . . ?
C20 C19 C21 122.1(6) . . ?
C15 C20 C19 120.4(6) . . ?
C15 C20 H20A 119.8 . . ?
C19 C20 H20A 119.8 . . ?
N4 C21 C22 107.2(6) . . ?
N4 C21 C19 122.2(6) . . ?
C22 C21 C19 130.5(7) . . ?
C21 C22 C23 105.1(6) . . ?
C21 C22 H22A 127.4 . . ?
C23 C22 H22A 127.4 . . ?
N5 C23 C22 110.8(6) . . ?
N5 C23 C24 114.9(7) . . ?
C22 C23 C24 134.3(7) . . ?
N6 C24 C25 123.5(7) . . ?
N6 C24 C23 112.4(6) . . ?
C25 C24 C23 124.0(8) . . ?
C24 C25 C26 119.1(9) . . ?
C24 C25 H25A 120.4 . . ?
C26 C25 H25A 120.4 . . ?
C27 C26 C25 117.4(8) . . ?
C27 C26 C30 121.9(8) . . ?
C25 C26 C30 120.7(10) . . ?
C26 C27 C28 120.9(8) . . ?
C26 C27 H27A 119.5 . . ?
C28 C27 H27A 119.5 . . ?
N6 C28 C27 122.2(8) . . ?
N6 C28 H28A 118.9 . . ?
C27 C28 H28A 118.9 . . ?
C3 C29 H29A 109.5 . . ?
C3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N7 C31 C32 122.7(6) . . ?
N7 C31 H31A 118.7 . . ?
C32 C31 H31A 118.7 . . ?
C33 C32 C31 120.2(6) . . ?
C33 C32 H32A 119.9 . . ?
C31 C32 H32A 119.9 . . ?
C32 C33 C34 117.7(6) . . ?
C32 C33 C59 121.8(6) . . ?
C34 C33 C59 120.5(6) . . ?
C33 C34 C35 119.2(6) . . ?
C33 C34 H34A 120.4 . . ?
C35 C34 H34A 120.4 . . ?
N7 C35 C34 122.8(5) . . ?
N7 C35 C36 113.6(5) . . ?
C34 C35 C36 123.6(6) . . ?
N8 C36 C37 111.7(5) . . ?
N8 C36 C35 114.5(5) . . ?
C37 C36 C35 133.8(5) . . ?
C36 C37 C38 104.8(5) . . ?
C36 C37 H37A 127.6 . . ?
C38 C37 H37A 127.6 . . ?
N9 C38 C37 107.0(5) . . ?
N9 C38 C39 124.5(5) . . ?
C37 C38 C39 128.5(6) . . ?
C44 C39 C40 119.4(6) . . ?
C44 C39 C38 123.0(6) . . ?
C40 C39 C38 117.6(5) . . ?
C41 C40 C39 120.2(6) . . ?
C41 C40 H40A 119.9 . . ?
C39 C40 H40A 119.9 . . ?
C40 C41 C42 120.7(7) . . ?
C40 C41 H41A 119.6 . . ?
C42 C41 H41A 119.6 . . ?
C41 C42 C43 119.4(6) . . ?
C41 C42 H42A 120.3 . . ?
C43 C42 H42A 120.3 . . ?
C44 C43 C42 119.7(6) . . ?
C44 C43 C45 122.1(6) . . ?
C42 C43 C45 118.2(6) . . ?
C43 C44 C39 120.6(6) . . ?
C43 C44 H44A 119.7 . . ?
C39 C44 H44A 119.7 . . ?
C50 C45 C46 119.5(6) . . ?
C50 C45 C43 119.8(5) . . ?
C46 C45 C43 120.6(6) . . ?
C47 C46 C45 119.6(7) . . ?
C47 C46 H46A 120.2 . . ?
C45 C46 H46A 120.2 . . ?
C48 C47 C46 121.7(7) . . ?
C48 C47 H47A 119.1 . . ?
C46 C47 H47A 119.1 . . ?
C47 C48 C49 120.2(6) . . ?
C47 C48 H48A 119.9 . . ?
C49 C48 H48A 119.9 . . ?
C50 C49 C48 117.5(6) . . ?
C50 C49 C51 123.0(6) . . ?
C48 C49 C51 119.4(6) . . ?
C45 C50 C49 121.2(6) . . ?
C45 C50 H50A 119.4 . . ?
C49 C50 H50A 119.4 . . ?
N10 C51 C52 106.4(6) . . ?
N10 C51 C49 123.5(6) . . ?
C52 C51 C49 129.9(6) . . ?
C53 C52 C51 104.7(6) . . ?
C53 C52 H52A 127.6 . . ?
C51 C52 H52A 127.6 . . ?
N11 C53 C52 111.8(5) . . ?
N11 C53 C54 114.4(6) . . ?
C52 C53 C54 133.7(6) . . ?
N12 C54 C55 122.6(6) . . ?
N12 C54 C53 112.5(6) . . ?
C55 C54 C53 124.9(7) . . ?
C54 C55 C56 119.7(8) . . ?
C54 C55 H55A 120.2 . . ?
C56 C55 H55A 120.2 . . ?
C57 C56 C55 117.9(7) . . ?
C57 C56 C60 122.5(8) . . ?
C55 C56 C60 119.5(9) . . ?
C58 C57 C56 120.5(7) . . ?
C58 C57 H57A 119.8 . . ?
C56 C57 H57A 119.8 . . ?
N12 C58 C57 122.3(8) . . ?
N12 C58 H58A 118.9 . . ?
C57 C58 H58A 118.9 . . ?
C33 C59 H59A 109.5 . . ?
C33 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C33 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C56 C60 H60A 109.5 . . ?
C56 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C56 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N13 C61 C62 123.1(6) . . ?
N13 C61 H61A 118.5 . . ?
C62 C61 H61A 118.5 . . ?
C61 C62 C63 121.0(6) . . ?
C61 C62 H62A 119.5 . . ?
C63 C62 H62A 119.5 . . ?
C64 C63 C62 115.4(6) . . ?
C64 C63 C89 121.5(7) . . ?
C62 C63 C89 123.0(6) . . ?
C63 C64 C65 120.4(6) . . ?
C63 C64 H64A 119.8 . . ?
C65 C64 H64A 119.8 . . ?
N13 C65 C64 123.5(5) . . ?
N13 C65 C66 113.1(5) . . ?
C64 C65 C66 123.4(5) . . ?
N14 C66 C67 110.5(5) . . ?
N14 C66 C65 116.1(5) . . ?
C67 C66 C65 133.4(6) . . ?
C68 C67 C66 105.6(5) . . ?
C68 C67 H67A 127.2 . . ?
C66 C67 H67A 127.2 . . ?
N15 C68 C67 106.8(5) . . ?
N15 C68 C69 125.0(5) . . ?
C67 C68 C69 128.2(6) . . ?
C74 C69 C70 118.3(5) . . ?
C74 C69 C68 122.8(5) . . ?
C70 C69 C68 118.8(5) . . ?
C71 C70 C69 121.2(6) . . ?
C71 C70 H70A 119.4 . . ?
C69 C70 H70A 119.4 . . ?
C70 C71 C72 119.8(6) . . ?
C70 C71 H71A 120.1 . . ?
C72 C71 H71A 120.1 . . ?
C71 C72 C73 120.9(6) . . ?
C71 C72 H72A 119.5 . . ?
C73 C72 H72A 119.5 . . ?
C72 C73 C74 118.7(6) . . ?
C72 C73 C75 119.9(5) . . ?
C74 C73 C75 121.3(5) . . ?
C69 C74 C73 121.0(5) . . ?
C69 C74 H74A 119.5 . . ?
C73 C74 H74A 119.5 . . ?
C80 C75 C76 117.9(6) . . ?
C80 C75 C73 121.0(6) . . ?
C76 C75 C73 121.0(5) . . ?
C77 C76 C75 121.4(6) . . ?
C77 C76 H76A 119.3 . . ?
C75 C76 H76A 119.3 . . ?
C76 C77 C78 120.4(7) . . ?
C76 C77 H77A 119.8 . . ?
C78 C77 H77A 119.8 . . ?
C77 C78 C79 119.4(7) . . ?
C77 C78 H78A 120.3 . . ?
C79 C78 H78A 120.3 . . ?
C80 C79 C78 119.3(6) . . ?
C80 C79 C81 122.0(6) . . ?
C78 C79 C81 118.6(6) . . ?
C79 C80 C75 121.5(6) . . ?
C79 C80 H80A 119.3 . . ?
C75 C80 H80A 119.3 . . ?
N16 C81 C82 106.8(6) . . ?
N16 C81 C79 122.4(6) . . ?
C82 C81 C79 130.7(7) . . ?
C81 C82 C83 105.3(7) . . ?
C81 C82 H82A 127.4 . . ?
C83 C82 H82A 127.4 . . ?
N17 C83 C82 111.8(6) . . ?
N17 C83 C84 113.2(6) . . ?
C82 C83 C84 134.9(7) . . ?
N18 C84 C85 123.0(6) . . ?
N18 C84 C83 113.2(7) . . ?
C85 C84 C83 123.8(7) . . ?
C84 C85 C86 118.3(8) . . ?
C84 C85 H85A 120.8 . . ?
C86 C85 H85A 120.8 . . ?
C87 C86 C85 117.3(8) . . ?
C87 C86 C90 122.3(8) . . ?
C85 C86 C90 120.3(9) . . ?
C88 C87 C86 121.2(7) . . ?
C88 C87 H87A 119.4 . . ?
C86 C87 H87A 119.4 . . ?
N18 C88 C87 122.8(8) . . ?
N18 C88 H88A 118.6 . . ?
C87 C88 H88A 118.6 . . ?
C63 C89 H89A 109.5 . . ?
C63 C89 H89B 109.5 . . ?
H89A C89 H89B 109.5 . . ?
C63 C89 H89C 109.5 . . ?
H89A C89 H89C 109.5 . . ?
H89B C89 H89C 109.5 . . ?
C86 C90 H90A 109.5 . . ?
C86 C90 H90B 109.5 . . ?
H90A C90 H90B 109.5 . . ?
C86 C90 H90C 109.5 . . ?
H90A C90 H90C 109.5 . . ?
H90B C90 H90C 109.5 . . ?
O1 Cl1 O2 111.2(4) . . ?
O1 Cl1 O3 115.1(4) . . ?
O2 Cl1 O3 110.9(5) . . ?
O1 Cl1 O4 108.8(5) . . ?
O2 Cl1 O4 109.7(5) . . ?
O3 Cl1 O4 100.5(5) . . ?
O3 Cl1B O2 119.6(7) . . ?
O3 Cl1B O4B 109.4(8) . . ?
O2 Cl1B O4B 107.9(8) . . ?
O3 Cl1B O1 112.8(6) . . ?
O2 Cl1B O1 101.5(5) . . ?
O4B Cl1B O1 104.3(8) . . ?
O6 Cl2 O7 109.8(5) . . ?
O6 Cl2 O5 112.4(5) . . ?
O7 Cl2 O5 113.4(5) . . ?
O6 Cl2 O8 106.7(7) . . ?
O7 Cl2 O8 105.4(7) . . ?
O5 Cl2 O8 108.7(4) . . ?
O12 Cl3 O9 111.1(5) . . ?
O12 Cl3 O11 108.9(5) . . ?
O9 Cl3 O11 109.1(5) . . ?
O12 Cl3 O10 110.4(5) . . ?
O9 Cl3 O10 109.6(5) . . ?
O11 Cl3 O10 107.7(5) . . ?
O15 Cl4 O13 110.5(11) . . ?
O15 Cl4 O16 111.8(11) . . ?
O13 Cl4 O16 107.9(10) . . ?
O15 Cl4 O14 110.9(11) . . ?
O13 Cl4 O14 107.7(11) . . ?
O16 Cl4 O14 107.8(11) . . ?
O15B Cl4B O13B 116.1(9) . . ?
O15B Cl4B O14B 109.4(8) . . ?
O13B Cl4B O14B 109.1(8) . . ?
O15B Cl4B O16B 109.2(8) . . ?
O13B Cl4B O16B 108.9(9) . . ?
O14B Cl4B O16B 103.4(9) . . ?
C1S O1S H1S 134(10) . . ?
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 . . ?
C2S O2S H2S 114(9) . . ?
O2S C2S H2S1 109.5 . . ?
O2S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
O2S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
C3S O3S H3S 99.8 . . ?
O3S C3S H3S1 109.5 . . ?
O3S C3S H3S2 109.5 . . ?
H3S1 C3S H3S2 109.5 . . ?
O3S C3S H3S3 109.5 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
C4S O4S H4S 109.5 . . ?
O4S C4S H4S1 109.5 . . ?
O4S C4S H4S2 109.5 . . ?
H4S1 C4S H4S2 109.5 . . ?
O4S C4S H4S3 109.5 . . ?
H4S1 C4S H4S3 109.5 . . ?
H4S2 C4S H4S3 109.5 . . ?
C5S O5S H5S 109.6 . . ?
O5S C5S H5S1 109.5 . . ?
O5S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
O5S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?
H1W O1W H2W 101(4) . . ?
H3W O2W H4W 102.9 . . ?

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 H3A O1 0.88 2.23 3.019(7) 148.8 . yes
N4 H4B O4S 0.88 1.92 2.755(7) 158.5 . yes
N9 H9A O4^a 0.88 2.39 3.102(11) 138.5 . yes
N9 H9A O2S 0.88 1.99 2.733(9) 141.1 . yes
N10 H10B O1W 0.88 1.98 2.859(7) 176.7 . yes
N15 H15A O1S 0.88 1.88 2.745(9) 167.0 . yes
N16 H16B O3S^a 0.88 1.91 2.774(10) 168.4 . yes
O1S H1S O2 0.92(2) 2.06(4) 2.904(13) 153(8) . yes
O2S H2S O5S 0.918(19) 1.83(3) 2.733(13) 169(12) . yes
O3S^a H3S^a O3 1.07 2.08 2.987(12) 141.1 . yes
O1W H1W O2 0.92(2) 1.98(4) 2.860(9) 161(9) . yes
O1W H2W O7S 0.92(2) 1.91(3) 2.821(15) 173(10) . yes
O2W H3W O10 0.95 1.96 2.889(13) 166.5 . yes
O2W H4W O8S 0.98 1.99 2.83(2) 141.1 . yes
O5S H5S O6S 0.84 1.88 2.656(17) 153.0 . yes

_refine_diff_density_max         1.560
_refine_diff_density_min         -0.945
_refine_diff_density_rms         0.163



####################################################################### 
# 
# 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_nc46
_database_code_depnum_ccdc_archive 'CCDC 2172377'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C78 H56 Fe2 N18, 2(B F4), F6 Si, C H4 O'
_chemical_formula_sum            'C79 H60 B2 F14 Fe2 N18 O Si'
_chemical_formula_weight         1704.85

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'
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'
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'
Si Si 0.0866 0.0751
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   17.310(3)
_cell_length_b                   25.070(5)
_cell_length_c                   18.781(4)
_cell_angle_alpha                90
_cell_angle_beta                 105.202(5)
_cell_angle_gamma                90
_cell_volume                     7865(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    19922
_cell_measurement_theta_min      1.15
_cell_measurement_theta_max      30.01

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_F_000             3473
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    0.514
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.995
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_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 at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            80998
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.251
_diffrn_reflns_theta_max         24.781
_diffrn_reflns_theta_full        24.780
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             12463
_reflns_number_gt                9299
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
 All non-hydrogens were refined anisotropically. One of the BF4 anion is
 disorder over two positions with the same B1 pivot site, with relative
 occupancies refining to 0.633:0.367. Both BF4 anions were refined with
 1,2 and 1,3 distance restraints and displacement parameters restraints due
 to disorder. Hydrogens were placed geometrically on their carrier atom
 and refined with a riding model, including those on the pyrazole N atoms.
 At the end of the refinement there remained empty portions
 of the cell with only weak electron density. This was analyzed and
 taken into account by PLATON/SQUEEZE that recovered a total of 80 electrons
 per cell over two voids of 518 cubic angstrom each. These figures would
 agree with 4 diffuse lattice methanol molecules per cell, 1 per formula
 unit. This have been included in the formula, and taken into account 
 for the density, mu and F000.
;

_vrf_PLAT027_nc46                
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      24.78 Degree       
RESPONSE: Crystals were tiny and relatively poorly diffracting. 
Even using a synchrotron source significant diffraction with reasonable
completeness was only up to ca. 0.85 angstrom. The present data were cut
at 0.87 angstrom resolution as then Rsigma>0.29. This results in poor 
theta_full and theta_max values.
;

_vrf_THETM01_nc46                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5747     
RESPONSE: Crystals were tiny and relatively poorly diffracting. 
Even using a synchrotron source significant diffraction with reasonable
completeness was only up to ca. 0.85 angstrom. The present data were cut
at 0.87 angstrom resolution as then Rsigma>0.29. This results in poor 
theta_full and theta_max values.
;

_vrf_PLAT094_nc46                
;
PROBLEM: Ratio of Maximum / Minimum Residual Density ....       4.32 Report       
RESPONSE: There remains one relatively strong residual electron density peak
in the close vicinity of the B1 site (0.03 angstrom). This could be associated
with the disorder shown by the corresponding BF4 anion, although the model does
not include disorder at the B site. Thus, another origin could be the
presence of twinning, although we were unable to spot it.
;

_vrf_PLAT097_nc46                
;
PROBLEM: Large Reported Max.  (Positive) Residual Density       3.22 eA-3       
RESPONSE: There remains one relatively strong residual electron density peak
in the close vicinity of the B1 site (0.03 angstrom). This could be associated
with the disorder shown by the corresponding BF4 anion, although the model does
not include disorder at the B site. Thus, another origin could be the
presence of twinning, although we were unable to spot it.
;

_vrf_DIFMX02_nc46                
;
PROBLEM: The maximum difference density is > 0.1*ZMAX*0.75
            The relevant atom site should be identified.       
RESPONSE: There remains one relatively strong residual electron density peak
in the close vicinity of the B1 site (0.03 angstrom). This could be associated
with the disorder shown by the corresponding BF4 anion, although the model does
not include disorder at the B site. Thus, another origin could be the
presence of twinning, although we were unable to spot it. 
;

_vrf_FORMU01_nc46                
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.       
RESPONSE: At the end of the refinement there remained empty portions
 of the cell with only weak electron density. This was analyzed and
 taken into account by PLATON/SQUEEZE that recovered a total of 80 electrons
 per cell over two voids of 518 cubic angstrom each. These figures would
 agree with 4 diffuse lattice methanol molecules per cell, 1 per formula
 unit. This has been included in the formula, resulting in this
 discrepancy.
;

_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+32.5600P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12463
_refine_ls_number_parameters     1073
_refine_ls_number_restraints     257
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.1137
_refine_ls_wR_factor_ref         0.2921
_refine_ls_wR_factor_gt          0.2796
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.141
_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 0.07179(6) 0.67676(5) 0.73245(7) 0.0905(4) Uani 1 1 d . . . . .
Fe2 Fe 0.49409(6) 0.67365(4) 0.44240(7) 0.0835(4) Uani 1 1 d . . . . .
N1 N -0.0284(4) 0.7304(3) 0.6776(5) 0.104(2) Uani 1 1 d . . . . .
N2 N 0.0370(4) 0.6496(3) 0.6204(4) 0.095(2) Uani 1 1 d . . . . .
N3 N 0.0515(4) 0.6086(3) 0.5790(4) 0.095(2) Uani 1 1 d . . . . .
H3B H 0.089604 0.584924 0.595320 0.114 Uiso 1 1 calc R U . . .
N4 N 0.3688(3) 0.5785(3) 0.4263(4) 0.093(2) Uani 1 1 d . . . . .
H4B H 0.327557 0.596233 0.433453 0.112 Uiso 1 1 calc R U . . .
N5 N 0.4422(3) 0.6007(3) 0.4311(4) 0.0874(18) Uani 1 1 d . . . . .
N6 N 0.5879(3) 0.6257(3) 0.4362(4) 0.0861(18) Uani 1 1 d . . . . .
N7 N 0.0003(4) 0.6267(3) 0.7856(4) 0.0933(19) Uani 1 1 d . . . . .
N8 N 0.1449(3) 0.6084(3) 0.7689(4) 0.0883(18) Uani 1 1 d . . . . .
N9 N 0.2161(3) 0.5873(3) 0.7637(4) 0.0870(18) Uani 1 1 d . . . . .
H9A H 0.247979 0.602807 0.740382 0.104 Uiso 1 1 calc R U . . .
N10 N 0.5125(4) 0.6363(3) 0.6045(4) 0.094(2) Uani 1 1 d . . . . .
H10B H 0.477004 0.610384 0.595872 0.112 Uiso 1 1 calc R U . . .
N11 N 0.5199(3) 0.6727(3) 0.5519(5) 0.098(2) Uani 1 1 d . . . . .
N12 N 0.5670(4) 0.7415(3) 0.4717(5) 0.099(2) Uani 1 1 d . . . . .
N13 N 0.1003(4) 0.7289(3) 0.8303(4) 0.097(2) Uani 1 1 d . . . . .
N14 N 0.1543(4) 0.7356(3) 0.7128(4) 0.0934(19) Uani 1 1 d . . . . .
N15 N 0.1753(4) 0.7503(3) 0.6516(4) 0.095(2) Uani 1 1 d . . . . .
H15A H 0.177967 0.728013 0.616078 0.115 Uiso 1 1 calc R U . . .
N16 N 0.3575(4) 0.7410(3) 0.4724(4) 0.0932(19) Uani 1 1 d . . . . .
H16B H 0.360245 0.729544 0.517264 0.112 Uiso 1 1 calc R U . . .
N17 N 0.3945(4) 0.7177(3) 0.4260(4) 0.0886(18) Uani 1 1 d . . . . .
N18 N 0.4700(3) 0.6923(3) 0.3313(4) 0.0897(19) Uani 1 1 d . . . . .
C1 C -0.0547(5) 0.7737(4) 0.7090(7) 0.116(3) Uani 1 1 d . . . . .
H1A H -0.038063 0.778927 0.760908 0.139 Uiso 1 1 calc R U . . .
C2 C -0.1069(6) 0.8106(4) 0.6635(8) 0.125(4) Uani 1 1 d . . . . .
H2A H -0.125079 0.841057 0.684478 0.150 Uiso 1 1 calc R U . . .
C3 C -0.1314(7) 0.8020(5) 0.5880(9) 0.140(4) Uani 1 1 d . . . . .
H3A H -0.165106 0.827378 0.557207 0.168 Uiso 1 1 calc R U . . .
C4 C -0.1083(5) 0.7584(4) 0.5576(7) 0.117(3) Uani 1 1 d . . . . .
H4A H -0.126925 0.751911 0.506141 0.140 Uiso 1 1 calc R U . . .
C5 C -0.0560(5) 0.7228(4) 0.6040(6) 0.100(3) Uani 1 1 d . . . . .
C6 C -0.0251(4) 0.6757(3) 0.5750(6) 0.090(2) Uani 1 1 d . . . . .
C7 C -0.0493(4) 0.6512(4) 0.5075(5) 0.093(2) Uani 1 1 d . . . . .
H7A H -0.092207 0.661729 0.467067 0.112 Uiso 1 1 calc R U . . .
C8 C 0.0019(4) 0.6075(4) 0.5103(6) 0.094(2) Uani 1 1 d . . . . .
C9 C 0.0040(4) 0.5689(4) 0.4541(5) 0.096(2) Uani 1 1 d . . . . .
C10 C -0.0642(5) 0.5575(5) 0.3997(6) 0.121(3) Uani 1 1 d . . . . .
H10A H -0.112520 0.575203 0.400338 0.145 Uiso 1 1 calc R U . . .
C11 C -0.0648(5) 0.5217(5) 0.3450(7) 0.136(4) Uani 1 1 d . . . . .
H11A H -0.113119 0.513790 0.308767 0.163 Uiso 1 1 calc R U . . .
C12 C 0.0067(5) 0.4970(5) 0.3431(6) 0.121(3) Uani 1 1 d . . . . .
H12A H 0.007324 0.472347 0.304846 0.145 Uiso 1 1 calc R U . . .
C13 C 0.0773(4) 0.5081(4) 0.3966(5) 0.096(2) Uani 1 1 d . . . . .
C14 C 0.0751(4) 0.5431(4) 0.4518(5) 0.094(2) Uani 1 1 d . . . . .
H14A H 0.122661 0.550048 0.489424 0.113 Uiso 1 1 calc R U . . .
C15 C 0.1540(4) 0.4829(4) 0.3940(5) 0.092(2) Uani 1 1 d . . . . .
C16 C 0.1595(5) 0.4301(4) 0.3785(5) 0.106(3) Uani 1 1 d . . . . .
H16A H 0.113133 0.408280 0.370324 0.127 Uiso 1 1 calc R U . . .
C17 C 0.2311(5) 0.4077(4) 0.3743(5) 0.106(3) Uani 1 1 d . . . . .
H17A H 0.233517 0.370959 0.362449 0.127 Uiso 1 1 calc R U . . .
C18 C 0.2996(5) 0.4390(4) 0.3875(5) 0.096(2) Uani 1 1 d . . . . .
H18A H 0.349493 0.423371 0.387072 0.116 Uiso 1 1 calc R U . . .
C19 C 0.2950(4) 0.4931(4) 0.4015(5) 0.087(2) Uani 1 1 d . . . . .
C20 C 0.2229(4) 0.5145(4) 0.4058(4) 0.091(2) Uani 1 1 d . . . . .
H20A H 0.219970 0.551278 0.416994 0.109 Uiso 1 1 calc R U . . .
C21 C 0.3672(4) 0.5271(3) 0.4097(5) 0.083(2) Uani 1 1 d . . . . .
C22 C 0.4428(4) 0.5136(3) 0.4034(4) 0.084(2) Uani 1 1 d . . . . .
H22A H 0.460778 0.479621 0.392312 0.101 Uiso 1 1 calc R U . . .
C23 C 0.4862(4) 0.5606(3) 0.4169(4) 0.080(2) Uani 1 1 d . . . . .
C24 C 0.5699(4) 0.5736(3) 0.4196(5) 0.082(2) Uani 1 1 d . . . . .
C25 C 0.6239(4) 0.5380(3) 0.4072(5) 0.090(2) Uani 1 1 d . . . . .
H25A H 0.608422 0.502160 0.394416 0.108 Uiso 1 1 calc R U . . .
C26 C 0.7014(5) 0.5543(4) 0.4134(5) 0.102(3) Uani 1 1 d . . . . .
H26A H 0.740536 0.529605 0.406773 0.123 Uiso 1 1 calc R U . . .
C27 C 0.7208(5) 0.6061(4) 0.4293(6) 0.110(3) Uani 1 1 d . . . . .
H27A H 0.773501 0.618338 0.432356 0.132 Uiso 1 1 calc R U . . .
C28 C 0.6641(4) 0.6409(4) 0.4408(5) 0.099(3) Uani 1 1 d . . . . .
H28A H 0.678846 0.677033 0.452464 0.118 Uiso 1 1 calc R U . . .
C31 C -0.0711(5) 0.6404(4) 0.7960(5) 0.103(3) Uani 1 1 d . . . . .
H31A H -0.098585 0.670265 0.770125 0.123 Uiso 1 1 calc R U . . .
C32 C -0.1048(6) 0.6131(5) 0.8418(6) 0.122(3) Uani 1 1 d . . . . .
H32A H -0.155978 0.623185 0.846915 0.146 Uiso 1 1 calc R U . . .
C33 C -0.0651(6) 0.5707(5) 0.8811(7) 0.131(4) Uani 1 1 d . . . . .
H33A H -0.087999 0.551647 0.914288 0.157 Uiso 1 1 calc R U . . .
C34 C 0.0086(6) 0.5560(4) 0.8717(6) 0.117(3) Uani 1 1 d . . . . .
H34A H 0.037382 0.526561 0.897710 0.141 Uiso 1 1 calc R U . . .
C35 C 0.0390(5) 0.5857(4) 0.8231(5) 0.092(2) Uani 1 1 d . . . . .
C36 C 0.1176(4) 0.5739(3) 0.8098(5) 0.087(2) Uani 1 1 d . . . . .
C37 C 0.1687(5) 0.5300(4) 0.8296(5) 0.096(2) Uani 1 1 d . . . . .
H37A H 0.162163 0.499748 0.858028 0.115 Uiso 1 1 calc R U . . .
C38 C 0.2315(5) 0.5408(4) 0.7979(5) 0.092(2) Uani 1 1 d . . . . .
C39 C 0.3041(5) 0.5098(4) 0.7995(5) 0.098(3) Uani 1 1 d . . . . .
C40 C 0.3033(6) 0.4544(4) 0.8042(7) 0.125(4) Uani 1 1 d . . . . .
H40A H 0.255663 0.436089 0.805477 0.150 Uiso 1 1 calc R U . . .
C41 C 0.3727(6) 0.4264(4) 0.8070(7) 0.141(4) Uani 1 1 d . . . . .
H41A H 0.372600 0.388630 0.811279 0.169 Uiso 1 1 calc R U . . .
C42 C 0.4424(6) 0.4521(4) 0.8036(7) 0.124(4) Uani 1 1 d . . . . .
H42A H 0.489189 0.431942 0.804797 0.149 Uiso 1 1 calc R U . . .
C43 C 0.4442(5) 0.5074(4) 0.7986(5) 0.101(3) Uani 1 1 d . . . . .
C44 C 0.3741(4) 0.5362(4) 0.7972(5) 0.095(2) Uani 1 1 d . . . . .
H44A H 0.374604 0.574022 0.794724 0.114 Uiso 1 1 calc R U . . .
C45 C 0.5162(5) 0.5387(4) 0.7930(5) 0.100(3) Uani 1 1 d . . . . .
C46 C 0.5931(5) 0.5252(5) 0.8349(6) 0.124(3) Uani 1 1 d . . . . .
H46A H 0.600426 0.495510 0.867382 0.149 Uiso 1 1 calc R U . . .
C47 C 0.6594(6) 0.5553(5) 0.8291(6) 0.129(4) Uani 1 1 d . . . . .
H47A H 0.710932 0.548042 0.860642 0.155 Uiso 1 1 calc R U . . .
C48 C 0.6499(5) 0.5942(4) 0.7792(6) 0.109(3) Uani 1 1 d . . . . .
H48A H 0.695474 0.613679 0.774800 0.131 Uiso 1 1 calc R U . . .
C49 C 0.5740(4) 0.6075(4) 0.7327(5) 0.092(2) Uani 1 1 d . . . . .
C50 C 0.5080(4) 0.5786(3) 0.7429(5) 0.091(2) Uani 1 1 d . . . . .
H50A H 0.455971 0.587426 0.713598 0.109 Uiso 1 1 calc R U . . .
C51 C 0.5657(4) 0.6446(4) 0.6715(6) 0.094(2) Uani 1 1 d . . . . .
C52 C 0.6103(5) 0.6891(3) 0.6618(6) 0.093(2) Uani 1 1 d . . . . .
H52A H 0.652807 0.705326 0.697769 0.112 Uiso 1 1 calc R U . . .
C53 C 0.5800(5) 0.7046(3) 0.5894(6) 0.094(2) Uani 1 1 d . . . . .
C54 C 0.6004(5) 0.7465(3) 0.5448(6) 0.094(2) Uani 1 1 d . . . . .
C55 C 0.6489(5) 0.7903(4) 0.5734(7) 0.123(3) Uani 1 1 d . U . . .
H55A H 0.673040 0.793410 0.624894 0.147 Uiso 1 1 calc R U . . .
C56 C 0.6605(6) 0.8285(4) 0.5250(8) 0.129(3) Uani 1 1 d . U . . .
H56A H 0.692373 0.858791 0.543766 0.155 Uiso 1 1 calc R U . . .
C57 C 0.6275(6) 0.8243(4) 0.4502(8) 0.132(3) Uani 1 1 d . U . . .
H57A H 0.635907 0.851073 0.417139 0.158 Uiso 1 1 calc R U . . .
C58 C 0.5812(5) 0.7796(4) 0.4247(7) 0.115(3) Uani 1 1 d . . . . .
H58A H 0.558887 0.775268 0.373180 0.138 Uiso 1 1 calc R U . . .
C61 C 0.0750(5) 0.7215(4) 0.8922(6) 0.108(3) Uani 1 1 d . . . . .
H61A H 0.052967 0.688094 0.900420 0.130 Uiso 1 1 calc R U . . .
C62 C 0.0809(5) 0.7623(5) 0.9437(6) 0.112(3) Uani 1 1 d . . . . .
H62A H 0.063403 0.756546 0.986951 0.134 Uiso 1 1 calc R U . . .
C63 C 0.1126(5) 0.8114(5) 0.9315(6) 0.114(3) Uani 1 1 d . . . . .
H63A H 0.116108 0.839472 0.966164 0.137 Uiso 1 1 calc R U . . .
C64 C 0.1392(5) 0.8192(4) 0.8685(5) 0.104(3) Uani 1 1 d . . . . .
H64A H 0.161247 0.852297 0.859033 0.125 Uiso 1 1 calc R U . . .
C65 C 0.1321(5) 0.7767(4) 0.8202(5) 0.099(3) Uani 1 1 d . . . . .
C66 C 0.1568(5) 0.7802(4) 0.7516(5) 0.101(3) Uani 1 1 d . . . . .
C67 C 0.1793(6) 0.8234(4) 0.7147(6) 0.113(3) Uani 1 1 d . . . . .
H67A H 0.184977 0.859530 0.730702 0.136 Uiso 1 1 calc R U . . .
C68 C 0.1917(6) 0.8031(4) 0.6503(6) 0.105(3) Uani 1 1 d . . . . .
C69 C 0.2151(6) 0.8265(4) 0.5882(6) 0.110(3) Uani 1 1 d . . . . .
C70 C 0.1975(9) 0.8804(5) 0.5706(8) 0.158(4) Uani 1 1 d . U . . .
H70A H 0.173523 0.902054 0.600333 0.190 Uiso 1 1 calc R U . . .
C71 C 0.2169(9) 0.9018(4) 0.5062(8) 0.159(4) Uani 1 1 d . U . . .
H71A H 0.203776 0.937703 0.491729 0.191 Uiso 1 1 calc R U . . .
C72 C 0.2550(7) 0.8697(4) 0.4650(7) 0.128(4) Uani 1 1 d . . . . .
H72A H 0.268755 0.884004 0.423152 0.154 Uiso 1 1 calc R U . . .
C73 C 0.2729(5) 0.8173(3) 0.4849(5) 0.097(2) Uani 1 1 d . . . . .
C74 C 0.2526(5) 0.7967(3) 0.5461(5) 0.098(3) Uani 1 1 d . . . . .
H74A H 0.265206 0.760503 0.559315 0.118 Uiso 1 1 calc R U . . .
C75 C 0.3153(5) 0.7845(3) 0.4410(5) 0.089(2) Uani 1 1 d . . . . .
C76 C 0.3253(5) 0.7890(3) 0.3726(5) 0.092(2) Uani 1 1 d . . . . .
H76A H 0.302789 0.815443 0.336998 0.110 Uiso 1 1 calc R U . . .
C77 C 0.3751(4) 0.7471(3) 0.3644(5) 0.083(2) Uani 1 1 d . . . . .
C78 C 0.4148(4) 0.7304(3) 0.3083(5) 0.089(2) Uani 1 1 d . . . . .
C79 C 0.3986(5) 0.7525(4) 0.2384(6) 0.106(3) Uani 1 1 d . . . . .
H79A H 0.359904 0.780006 0.223901 0.127 Uiso 1 1 calc R U . . .
C80 C 0.4405(5) 0.7333(4) 0.1900(6) 0.110(3) Uani 1 1 d . . . . .
H80A H 0.430378 0.747010 0.141241 0.133 Uiso 1 1 calc R U . . .
C81 C 0.4964(5) 0.6945(4) 0.2134(6) 0.107(3) Uani 1 1 d . . . . .
H81A H 0.526190 0.681570 0.181134 0.129 Uiso 1 1 calc R U . . .
C82 C 0.5100(5) 0.6738(4) 0.2832(6) 0.101(3) Uani 1 1 d . . . . .
H82A H 0.548064 0.645982 0.298093 0.121 Uiso 1 1 calc R U . . .
Si1 Si 0.28529(11) 0.62518(9) 0.58837(14) 0.0821(6) Uani 1 1 d . . . . .
F1 F 0.2633(2) 0.62317(18) 0.4950(2) 0.0889(12) Uani 1 1 d . . . . .
F2 F 0.3657(2) 0.58660(16) 0.5929(3) 0.0902(12) Uani 1 1 d . . . . .
F3 F 0.3435(2) 0.68008(16) 0.5883(3) 0.0874(12) Uani 1 1 d . . . . .
F4 F 0.2286(2) 0.57201(17) 0.5930(3) 0.0925(13) Uani 1 1 d . . . . .
F5 F 0.3090(2) 0.63016(18) 0.6819(3) 0.0950(13) Uani 1 1 d . . . . .
F6 F 0.2053(2) 0.66489(17) 0.5829(3) 0.0913(12) Uani 1 1 d . . . . .
B1 B 0.7817(3) 0.7242(2) 0.3176(3) 0.0484(11) Uani 1 1 d D U . . .
F7 F 0.7963(6) 0.7708(4) 0.2837(6) 0.123(3) Uani 0.599(7) 1 d D U P A 1
F8 F 0.7759(6) 0.7266(4) 0.3974(4) 0.125(3) Uani 0.599(7) 1 d D U P A 1
F9 F 0.6951(4) 0.7072(3) 0.2732(5) 0.124(3) Uani 0.599(7) 1 d D U P A 1
F10 F 0.8253(7) 0.6721(4) 0.3159(6) 0.146(3) Uani 0.599(7) 1 d D U P A 1
F7B F 0.7219(8) 0.7366(6) 0.3576(9) 0.149(4) Uani 0.401(7) 1 d D U P A 2
F8B F 0.8743(5) 0.7352(5) 0.3615(5) 0.100(3) Uani 0.401(7) 1 d D U P A 2
F9B F 0.7762(10) 0.6705(5) 0.2801(9) 0.142(4) Uani 0.401(7) 1 d D U P A 2
F10B F 0.7780(7) 0.7698(6) 0.2513(7) 0.104(4) Uani 0.401(7) 1 d D U P A 2
B2 B 0.8050(7) 0.9404(4) 0.5154(7) 0.148(3) Uani 1 1 d D U . . .
F11 F 0.8013(4) 0.8993(2) 0.4671(4) 0.144(2) Uani 1 1 d D U . . .
F12 F 0.8617(5) 0.9743(3) 0.5134(5) 0.209(4) Uani 1 1 d D U . . .
F13 F 0.8139(6) 0.9202(3) 0.5853(4) 0.196(3) Uani 1 1 d D U . . .
F14 F 0.7334(5) 0.9669(4) 0.5046(5) 0.212(3) Uani 1 1 d D U . . .


_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 N8 2.133(7) . ?
Fe1 N2 2.143(8) . ?
Fe1 N14 2.151(7) . ?
Fe1 N7 2.180(7) . ?
Fe1 N13 2.203(8) . ?
Fe1 N1 2.224(7) . ?
Fe2 N11 1.988(9) . ?
Fe2 N17 2.002(6) . ?
Fe2 N5 2.023(6) . ?
Fe2 N6 2.048(6) . ?
Fe2 N18 2.071(7) . ?
Fe2 N12 2.104(7) . ?
N1 C5 1.351(11) . ?
N1 C1 1.370(11) . ?
N2 N3 1.352(9) . ?
N2 C6 1.352(10) . ?
N3 C8 1.351(11) . ?
N3 H3B 0.8800 . ?
N4 C21 1.324(10) . ?
N4 N5 1.370(8) . ?
N4 H4B 0.8800 . ?
N5 C23 1.329(9) . ?
N6 C28 1.354(9) . ?
N6 C24 1.359(10) . ?
N7 C35 1.325(10) . ?
N7 C31 1.344(9) . ?
N8 C36 1.325(10) . ?
N8 N9 1.369(8) . ?
N9 C38 1.323(10) . ?
N9 H9A 0.8800 . ?
N10 C51 1.366(11) . ?
N10 N11 1.374(9) . ?
N10 H10B 0.8800 . ?
N11 C53 1.353(10) . ?
N12 C54 1.347(11) . ?
N12 C58 1.365(11) . ?
N13 C65 1.354(11) . ?
N13 C61 1.357(11) . ?
N14 C66 1.330(11) . ?
N14 N15 1.344(9) . ?
N15 C68 1.355(11) . ?
N15 H15A 0.8800 . ?
N16 N17 1.342(8) . ?
N16 C75 1.358(10) . ?
N16 H16B 0.8800 . ?
N17 C77 1.338(10) . ?
N18 C78 1.339(10) . ?
N18 C82 1.357(10) . ?
C1 C2 1.413(14) . ?
C1 H1A 0.9500 . ?
C2 C3 1.387(16) . ?
C2 H2A 0.9500 . ?
C3 C4 1.339(15) . ?
C3 H3A 0.9500 . ?
C4 C5 1.402(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.460(12) . ?
C6 C7 1.371(12) . ?
C7 C8 1.402(12) . ?
C7 H7A 0.9500 . ?
C8 C9 1.440(12) . ?
C9 C10 1.373(12) . ?
C9 C14 1.400(11) . ?
C10 C11 1.363(13) . ?
C10 H10A 0.9500 . ?
C11 C12 1.393(13) . ?
C11 H11A 0.9500 . ?
C12 C13 1.391(12) . ?
C12 H12A 0.9500 . ?
C13 C14 1.367(11) . ?
C13 C15 1.483(11) . ?
C14 H14A 0.9500 . ?
C15 C16 1.364(12) . ?
C15 C20 1.401(10) . ?
C16 C17 1.382(12) . ?
C16 H16A 0.9500 . ?
C17 C18 1.388(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.389(11) . ?
C18 H18A 0.9500 . ?
C19 C20 1.380(10) . ?
C19 C21 1.487(10) . ?
C20 H20A 0.9500 . ?
C21 C22 1.385(9) . ?
C22 C23 1.385(10) . ?
C22 H22A 0.9500 . ?
C23 C24 1.472(9) . ?
C24 C25 1.356(10) . ?
C25 C26 1.377(10) . ?
C25 H25A 0.9500 . ?
C26 C27 1.356(12) . ?
C26 H26A 0.9500 . ?
C27 C28 1.372(11) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C31 C32 1.347(13) . ?
C31 H31A 0.9500 . ?
C32 C33 1.371(14) . ?
C32 H32A 0.9500 . ?
C33 C34 1.384(12) . ?
C33 H33A 0.9500 . ?
C34 C35 1.384(12) . ?
C34 H34A 0.9500 . ?
C35 C36 1.475(10) . ?
C36 C37 1.400(11) . ?
C37 C38 1.397(10) . ?
C37 H37A 0.9500 . ?
C38 C39 1.471(11) . ?
C39 C44 1.391(11) . ?
C39 C40 1.393(12) . ?
C40 C41 1.380(12) . ?
C40 H40A 0.9500 . ?
C41 C42 1.385(13) . ?
C41 H41A 0.9500 . ?
C42 C43 1.389(13) . ?
C42 H42A 0.9500 . ?
C43 C44 1.407(11) . ?
C43 C45 1.499(12) . ?
C44 H44A 0.9500 . ?
C45 C50 1.357(11) . ?
C45 C46 1.398(12) . ?
C46 C47 1.402(14) . ?
C46 H46A 0.9500 . ?
C47 C48 1.332(13) . ?
C47 H47A 0.9500 . ?
C48 C49 1.413(12) . ?
C48 H48A 0.9500 . ?
C49 C50 1.406(11) . ?
C49 C51 1.456(12) . ?
C50 H50A 0.9500 . ?
C51 C52 1.395(11) . ?
C52 C53 1.380(12) . ?
C52 H52A 0.9500 . ?
C53 C54 1.444(12) . ?
C54 C55 1.401(12) . ?
C55 C56 1.372(15) . ?
C55 H55A 0.9500 . ?
C56 C57 1.376(16) . ?
C56 H56A 0.9500 . ?
C57 C58 1.389(14) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C61 C62 1.392(13) . ?
C61 H61A 0.9500 . ?
C62 C63 1.390(14) . ?
C62 H62A 0.9500 . ?
C63 C64 1.392(13) . ?
C63 H63A 0.9500 . ?
C64 C65 1.382(12) . ?
C64 H64A 0.9500 . ?
C65 C66 1.463(12) . ?
C66 C67 1.396(13) . ?
C67 C68 1.382(13) . ?
C67 H67A 0.9500 . ?
C68 C69 1.455(13) . ?
C69 C74 1.369(12) . ?
C69 C70 1.404(13) . ?
C70 C71 1.442(15) . ?
C70 H70A 0.9500 . ?
C71 C72 1.395(13) . ?
C71 H71A 0.9500 . ?
C72 C73 1.378(12) . ?
C72 H72A 0.9500 . ?
C73 C74 1.386(12) . ?
C73 C75 1.488(12) . ?
C74 H74A 0.9500 . ?
C75 C76 1.345(11) . ?
C76 C77 1.394(10) . ?
C76 H76A 0.9500 . ?
C77 C78 1.460(11) . ?
C78 C79 1.385(12) . ?
C79 C80 1.390(12) . ?
C79 H79A 0.9500 . ?
C80 C81 1.360(12) . ?
C80 H80A 0.9500 . ?
C81 C82 1.371(12) . ?
C81 H81A 0.9500 . ?
C82 H82A 0.9500 . ?
Si1 F4 1.671(4) . ?
Si1 F2 1.678(4) . ?
Si1 F6 1.687(4) . ?
Si1 F1 1.694(5) . ?
Si1 F5 1.700(5) . ?
Si1 F3 1.706(4) . ?
B1 F7 1.384(8) . ?
B1 F7B 1.464(9) . ?
B1 F9B 1.512(10) . ?
B1 F10 1.514(8) . ?
B1 F8 1.530(8) . ?
B1 F9 1.573(7) . ?
B1 F8B 1.621(8) . ?
B1 F10B 1.679(10) . ?
B2 F12 1.306(10) . ?
B2 F11 1.363(10) . ?
B2 F14 1.373(11) . ?
B2 F13 1.378(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
N8 Fe1 N2 92.9(3) . . ?
N8 Fe1 N14 103.9(2) . . ?
N2 Fe1 N14 94.4(3) . . ?
N8 Fe1 N7 75.6(3) . . ?
N2 Fe1 N7 102.7(3) . . ?
N14 Fe1 N7 162.9(3) . . ?
N8 Fe1 N13 103.0(3) . . ?
N2 Fe1 N13 162.1(3) . . ?
N14 Fe1 N13 73.9(3) . . ?
N7 Fe1 N13 89.4(3) . . ?
N8 Fe1 N1 163.7(3) . . ?
N2 Fe1 N1 75.7(3) . . ?
N14 Fe1 N1 88.8(3) . . ?
N7 Fe1 N1 95.3(3) . . ?
N13 Fe1 N1 90.3(3) . . ?
N11 Fe2 N17 96.7(3) . . ?
N11 Fe2 N5 94.1(3) . . ?
N17 Fe2 N5 98.1(2) . . ?
N11 Fe2 N6 94.9(3) . . ?
N17 Fe2 N6 168.1(3) . . ?
N5 Fe2 N6 78.5(2) . . ?
N11 Fe2 N18 167.6(3) . . ?
N17 Fe2 N18 77.4(3) . . ?
N5 Fe2 N18 97.6(3) . . ?
N6 Fe2 N18 91.7(3) . . ?
N11 Fe2 N12 77.4(3) . . ?
N17 Fe2 N12 91.6(3) . . ?
N5 Fe2 N12 167.8(3) . . ?
N6 Fe2 N12 93.4(2) . . ?
N18 Fe2 N12 91.7(3) . . ?
C5 N1 C1 119.0(9) . . ?
C5 N1 Fe1 114.3(6) . . ?
C1 N1 Fe1 125.9(8) . . ?
N3 N2 C6 104.1(7) . . ?
N3 N2 Fe1 139.4(6) . . ?
C6 N2 Fe1 116.0(6) . . ?
C8 N3 N2 113.4(7) . . ?
C8 N3 H3B 123.3 . . ?
N2 N3 H3B 123.3 . . ?
C21 N4 N5 111.8(6) . . ?
C21 N4 H4B 124.1 . . ?
N5 N4 H4B 124.1 . . ?
C23 N5 N4 104.5(6) . . ?
C23 N5 Fe2 116.3(4) . . ?
N4 N5 Fe2 138.9(5) . . ?
C28 N6 C24 116.6(7) . . ?
C28 N6 Fe2 127.1(6) . . ?
C24 N6 Fe2 116.1(4) . . ?
C35 N7 C31 118.5(8) . . ?
C35 N7 Fe1 114.9(5) . . ?
C31 N7 Fe1 124.9(7) . . ?
C36 N8 N9 104.7(6) . . ?
C36 N8 Fe1 116.1(5) . . ?
N9 N8 Fe1 139.2(5) . . ?
C38 N9 N8 112.1(6) . . ?
C38 N9 H9A 123.9 . . ?
N8 N9 H9A 123.9 . . ?
C51 N10 N11 113.2(7) . . ?
C51 N10 H10B 123.4 . . ?
N11 N10 H10B 123.4 . . ?
C53 N11 N10 102.9(8) . . ?
C53 N11 Fe2 117.7(6) . . ?
N10 N11 Fe2 135.5(5) . . ?
C54 N12 C58 119.4(9) . . ?
C54 N12 Fe2 114.2(6) . . ?
C58 N12 Fe2 126.4(8) . . ?
C65 N13 C61 118.3(8) . . ?
C65 N13 Fe1 114.8(6) . . ?
C61 N13 Fe1 125.6(7) . . ?
C66 N14 N15 105.1(7) . . ?
C66 N14 Fe1 114.1(6) . . ?
N15 N14 Fe1 132.5(6) . . ?
N14 N15 C68 112.9(7) . . ?
N14 N15 H15A 123.6 . . ?
C68 N15 H15A 123.6 . . ?
N17 N16 C75 111.2(7) . . ?
N17 N16 H16B 124.4 . . ?
C75 N16 H16B 124.4 . . ?
C77 N17 N16 105.5(7) . . ?
C77 N17 Fe2 116.5(5) . . ?
N16 N17 Fe2 132.7(6) . . ?
C78 N18 C82 118.4(8) . . ?
C78 N18 Fe2 115.1(6) . . ?
C82 N18 Fe2 126.2(6) . . ?
N1 C1 C2 119.3(11) . . ?
N1 C1 H1A 120.3 . . ?
C2 C1 H1A 120.3 . . ?
C3 C2 C1 119.5(10) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C4 C3 C2 121.1(12) . . ?
C4 C3 H3A 119.5 . . ?
C2 C3 H3A 119.5 . . ?
C3 C4 C5 118.1(12) . . ?
C3 C4 H4A 120.9 . . ?
C5 C4 H4A 120.9 . . ?
N1 C5 C4 122.9(9) . . ?
N1 C5 C6 115.5(9) . . ?
C4 C5 C6 121.6(10) . . ?
N2 C6 C7 111.5(8) . . ?
N2 C6 C5 117.6(9) . . ?
C7 C6 C5 130.9(9) . . ?
C6 C7 C8 106.2(8) . . ?
C6 C7 H7A 126.9 . . ?
C8 C7 H7A 126.9 . . ?
N3 C8 C7 104.9(8) . . ?
N3 C8 C9 125.6(8) . . ?
C7 C8 C9 129.5(9) . . ?
C10 C9 C14 118.2(9) . . ?
C10 C9 C8 120.2(8) . . ?
C14 C9 C8 121.6(8) . . ?
C11 C10 C9 122.2(9) . . ?
C11 C10 H10A 118.9 . . ?
C9 C10 H10A 118.9 . . ?
C10 C11 C12 118.7(9) . . ?
C10 C11 H11A 120.7 . . ?
C12 C11 H11A 120.7 . . ?
C13 C12 C11 120.7(10) . . ?
C13 C12 H12A 119.7 . . ?
C11 C12 H12A 119.7 . . ?
C14 C13 C12 118.9(8) . . ?
C14 C13 C15 120.1(7) . . ?
C12 C13 C15 121.0(9) . . ?
C13 C14 C9 121.3(8) . . ?
C13 C14 H14A 119.4 . . ?
C9 C14 H14A 119.4 . . ?
C16 C15 C20 118.6(8) . . ?
C16 C15 C13 122.3(7) . . ?
C20 C15 C13 119.1(8) . . ?
C15 C16 C17 121.4(8) . . ?
C15 C16 H16A 119.3 . . ?
C17 C16 H16A 119.3 . . ?
C16 C17 C18 119.7(9) . . ?
C16 C17 H17A 120.1 . . ?
C18 C17 H17A 120.1 . . ?
C17 C18 C19 119.9(8) . . ?
C17 C18 H18A 120.1 . . ?
C19 C18 H18A 120.1 . . ?
C20 C19 C18 119.2(7) . . ?
C20 C19 C21 121.3(8) . . ?
C18 C19 C21 119.4(7) . . ?
C19 C20 C15 121.1(8) . . ?
C19 C20 H20A 119.4 . . ?
C15 C20 H20A 119.4 . . ?
N4 C21 C22 107.3(7) . . ?
N4 C21 C19 123.1(7) . . ?
C22 C21 C19 129.6(8) . . ?
C21 C22 C23 104.9(7) . . ?
C21 C22 H22A 127.6 . . ?
C23 C22 H22A 127.6 . . ?
N5 C23 C22 111.6(6) . . ?
N5 C23 C24 115.9(7) . . ?
C22 C23 C24 132.6(7) . . ?
C25 C24 N6 123.0(7) . . ?
C25 C24 C23 124.4(7) . . ?
N6 C24 C23 112.6(6) . . ?
C24 C25 C26 119.3(8) . . ?
C24 C25 H25A 120.3 . . ?
C26 C25 H25A 120.3 . . ?
C27 C26 C25 118.8(8) . . ?
C27 C26 H26A 120.6 . . ?
C25 C26 H26A 120.6 . . ?
C26 C27 C28 119.9(7) . . ?
C26 C27 H27A 120.1 . . ?
C28 C27 H27A 120.1 . . ?
N6 C28 C27 122.3(8) . . ?
N6 C28 H28A 118.8 . . ?
C27 C28 H28A 118.8 . . ?
N7 C31 C32 122.1(10) . . ?
N7 C31 H31A 118.9 . . ?
C32 C31 H31A 118.9 . . ?
C31 C32 C33 119.9(9) . . ?
C31 C32 H32A 120.1 . . ?
C33 C32 H32A 120.1 . . ?
C32 C33 C34 119.1(10) . . ?
C32 C33 H33A 120.4 . . ?
C34 C33 H33A 120.4 . . ?
C35 C34 C33 117.6(10) . . ?
C35 C34 H34A 121.2 . . ?
C33 C34 H34A 121.2 . . ?
N7 C35 C34 122.8(8) . . ?
N7 C35 C36 115.2(7) . . ?
C34 C35 C36 122.0(8) . . ?
N8 C36 C37 111.8(7) . . ?
N8 C36 C35 116.9(7) . . ?
C37 C36 C35 131.3(8) . . ?
C38 C37 C36 104.0(8) . . ?
C38 C37 H37A 128.0 . . ?
C36 C37 H37A 128.0 . . ?
N9 C38 C37 107.4(7) . . ?
N9 C38 C39 122.5(7) . . ?
C37 C38 C39 130.1(8) . . ?
C44 C39 C40 119.9(8) . . ?
C44 C39 C38 119.7(8) . . ?
C40 C39 C38 120.4(8) . . ?
C41 C40 C39 119.2(9) . . ?
C41 C40 H40A 120.4 . . ?
C39 C40 H40A 120.4 . . ?
C40 C41 C42 121.4(10) . . ?
C40 C41 H41A 119.3 . . ?
C42 C41 H41A 119.3 . . ?
C41 C42 C43 120.2(9) . . ?
C41 C42 H42A 119.9 . . ?
C43 C42 H42A 119.9 . . ?
C42 C43 C44 118.6(8) . . ?
C42 C43 C45 124.1(8) . . ?
C44 C43 C45 117.3(8) . . ?
C39 C44 C43 120.7(8) . . ?
C39 C44 H44A 119.7 . . ?
C43 C44 H44A 119.7 . . ?
C50 C45 C46 118.6(9) . . ?
C50 C45 C43 119.9(8) . . ?
C46 C45 C43 121.4(9) . . ?
C45 C46 C47 120.3(10) . . ?
C45 C46 H46A 119.8 . . ?
C47 C46 H46A 119.8 . . ?
C48 C47 C46 119.7(9) . . ?
C48 C47 H47A 120.1 . . ?
C46 C47 H47A 120.1 . . ?
C47 C48 C49 122.0(9) . . ?
C47 C48 H48A 119.0 . . ?
C49 C48 H48A 119.0 . . ?
C50 C49 C48 116.9(9) . . ?
C50 C49 C51 121.3(7) . . ?
C48 C49 C51 121.4(8) . . ?
C45 C50 C49 122.2(8) . . ?
C45 C50 H50A 118.9 . . ?
C49 C50 H50A 118.9 . . ?
N10 C51 C52 105.3(9) . . ?
N10 C51 C49 122.3(8) . . ?
C52 C51 C49 132.0(9) . . ?
C53 C52 C51 105.8(8) . . ?
C53 C52 H52A 127.1 . . ?
C51 C52 H52A 127.1 . . ?
N11 C53 C52 112.8(8) . . ?
N11 C53 C54 113.6(9) . . ?
C52 C53 C54 133.6(9) . . ?
N12 C54 C55 121.2(9) . . ?
N12 C54 C53 114.7(8) . . ?
C55 C54 C53 124.1(11) . . ?
C56 C55 C54 118.0(12) . . ?
C56 C55 H55A 121.0 . . ?
C54 C55 H55A 121.0 . . ?
C55 C56 C57 122.0(11) . . ?
C55 C56 H56A 119.0 . . ?
C57 C56 H56A 119.0 . . ?
C56 C57 C58 117.4(11) . . ?
C56 C57 H57A 121.3 . . ?
C58 C57 H57A 121.3 . . ?
N12 C58 C57 121.9(12) . . ?
N12 C58 H58A 119.1 . . ?
C57 C58 H58A 119.1 . . ?
N13 C61 C62 120.9(10) . . ?
N13 C61 H61A 119.6 . . ?
C62 C61 H61A 119.6 . . ?
C63 C62 C61 119.7(10) . . ?
C63 C62 H62A 120.1 . . ?
C61 C62 H62A 120.1 . . ?
C62 C63 C64 119.8(10) . . ?
C62 C63 H63A 120.1 . . ?
C64 C63 H63A 120.1 . . ?
C65 C64 C63 117.2(10) . . ?
C65 C64 H64A 121.4 . . ?
C63 C64 H64A 121.4 . . ?
N13 C65 C64 124.0(9) . . ?
N13 C65 C66 113.5(9) . . ?
C64 C65 C66 122.4(9) . . ?
N14 C66 C67 110.7(8) . . ?
N14 C66 C65 117.3(9) . . ?
C67 C66 C65 131.8(9) . . ?
C68 C67 C66 106.0(9) . . ?
C68 C67 H67A 127.0 . . ?
C66 C67 H67A 127.0 . . ?
N15 C68 C67 105.3(9) . . ?
N15 C68 C69 120.8(9) . . ?
C67 C68 C69 133.8(9) . . ?
C74 C69 C70 119.8(10) . . ?
C74 C69 C68 121.0(8) . . ?
C70 C69 C68 119.2(9) . . ?
C69 C70 C71 118.2(10) . . ?
C69 C70 H70A 120.9 . . ?
C71 C70 H70A 120.9 . . ?
C72 C71 C70 119.8(10) . . ?
C72 C71 H71A 120.1 . . ?
C70 C71 H71A 120.1 . . ?
C73 C72 C71 120.3(10) . . ?
C73 C72 H72A 119.8 . . ?
C71 C72 H72A 119.8 . . ?
C72 C73 C74 119.5(8) . . ?
C72 C73 C75 119.0(8) . . ?
C74 C73 C75 121.5(8) . . ?
C69 C74 C73 122.4(8) . . ?
C69 C74 H74A 118.8 . . ?
C73 C74 H74A 118.8 . . ?
C76 C75 N16 107.0(7) . . ?
C76 C75 C73 133.5(8) . . ?
N16 C75 C73 119.4(8) . . ?
C75 C76 C77 106.3(8) . . ?
C75 C76 H76A 126.8 . . ?
C77 C76 H76A 126.8 . . ?
N17 C77 C76 109.9(8) . . ?
N17 C77 C78 114.1(7) . . ?
C76 C77 C78 135.8(8) . . ?
N18 C78 C79 122.7(8) . . ?
N18 C78 C77 113.7(8) . . ?
C79 C78 C77 123.6(8) . . ?
C78 C79 C80 118.1(8) . . ?
C78 C79 H79A 120.9 . . ?
C80 C79 H79A 120.9 . . ?
C81 C80 C79 119.0(9) . . ?
C81 C80 H80A 120.5 . . ?
C79 C80 H80A 120.5 . . ?
C80 C81 C82 120.6(9) . . ?
C80 C81 H81A 119.7 . . ?
C82 C81 H81A 119.7 . . ?
N18 C82 C81 121.2(8) . . ?
N18 C82 H82A 119.4 . . ?
C81 C82 H82A 119.4 . . ?
F4 Si1 F2 91.6(2) . . ?
F4 Si1 F6 89.4(2) . . ?
F2 Si1 F6 178.8(3) . . ?
F4 Si1 F1 93.1(2) . . ?
F2 Si1 F1 89.6(2) . . ?
F6 Si1 F1 89.8(2) . . ?
F4 Si1 F5 89.5(2) . . ?
F2 Si1 F5 91.0(2) . . ?
F6 Si1 F5 89.5(2) . . ?
F1 Si1 F5 177.3(3) . . ?
F4 Si1 F3 177.1(3) . . ?
F2 Si1 F3 89.0(2) . . ?
F6 Si1 F3 90.0(2) . . ?
F1 Si1 F3 89.8(2) . . ?
F5 Si1 F3 87.7(2) . . ?
F7B B1 F9B 117.5(8) . . ?
F7 B1 F10 124.5(7) . . ?
F7 B1 F8 119.0(7) . . ?
F10 B1 F8 102.4(6) . . ?
F7 B1 F9 104.4(5) . . ?
F10 B1 F9 99.5(6) . . ?
F8 B1 F9 103.4(5) . . ?
F7B B1 F8B 116.2(8) . . ?
F9B B1 F8B 108.7(7) . . ?
F7B B1 F10B 110.0(8) . . ?
F9B B1 F10B 106.0(7) . . ?
F8B B1 F10B 95.9(5) . . ?
F12 B2 F11 112.2(8) . . ?
F12 B2 F14 109.7(9) . . ?
F11 B2 F14 112.6(9) . . ?
F12 B2 F13 111.7(10) . . ?
F11 B2 F13 109.3(9) . . ?
F14 B2 F13 100.8(8) . . ?

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 H3B F4 0.88 2.44 3.144(7) 137.3 . yes
N4 H4B F1 0.88 1.92 2.736(7) 152.6 . yes
N9 H9A F5 0.88 1.84 2.720(7) 173.1 . yes
N10 H10B F2 0.88 2.00 2.787(7) 147.6 . yes
N15 H15A F6 0.88 1.81 2.621(8) 152.5 . yes
N16 H16B F3 0.88 1.90 2.722(8) 155.0 . yes

_refine_diff_density_max         3.217
_refine_diff_density_min         -0.745
_refine_diff_density_rms         0.115




####################################################################### 
# 
# 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_nc33c
_database_code_depnum_ccdc_archive 'CCDC 2172379'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Ciencia de Materiales de Aragon (ICMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2022-07-29 deposited with the CCDC.	2022-09-05 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         
'C82 H64 Fe2 N18, F6 Si, 2(B F4), 4(C3 H7 N O), C H4 O'
_chemical_formula_sum            'C95 H96 B2 F14 Fe2 N22 O5 Si'
_chemical_formula_weight         2053.34

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'
Si Si 0.0866 0.0751
'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      tetragonal
_space_group_IT_number           92
_space_group_name_H-M_alt        'P 41 21 2'
_space_group_name_Hall           'P 4abw 2nw'

_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, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'

_cell_length_a                   30.215(4)
_cell_length_b                   30.215(4)
_cell_length_c                   21.126(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     19287(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    62660
_cell_measurement_theta_min      0.98
_cell_measurement_theta_max      29.24

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.415
_exptl_crystal_F_000             8445
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.461
_shelx_estimated_absorpt_T_min   0.967
_shelx_estimated_absorpt_T_max   0.975
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.72932
_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 at various κ'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            204178
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_av_R_equivalents  0.0523
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         0.978
_diffrn_reflns_theta_max         24.776
_diffrn_reflns_theta_full        24.776
_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             15347
_reflns_number_gt                13967
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.814
_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.
 
 Structure factors included contributions from the .fab file.
 
 _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    'XP (Bruker, Sheldrick), PLATON (Spek, 2015)'
_computing_publication_material  'Mercury (CCDC), PLATON (Spek, 2015)'
_refine_special_details          
;
Likely due the overall poor quality of the available crystals, most non-hydrogens
showed relatively large thermal parameters. All non-hydrogens were nevertheless
refined anisotropically, except those of the partial and disordered BF4 anions
(B2-B4, F9-F16). These were in addition refined using 1,2 and 1,3-distance restraints. 
Displacement parameters restraints (SIMU/DELU) were used for the refinement of
two lattice dmf molecules, which also required 1,2 and 1,3 distance restraints.
Hydrogens were placed geometrically on their carrier atom and refined with a riding
model, including those on the pyrazole N atom (AFIX 43), as free refinement was
not satisfactory. At the end of the refinement, there remained portions of the
cell with only weak electron density peaks. These were analyzed and taken into
account with PLATON/SQUEEZE that recovered a total of 957 electrons per cell,
distributed over four large voids of 633 cubic angstroms (183 electrons each) and
eight small voids of 93 cubic angstroms (28 electrons each). These figures would
agree with 1 diffuse lattice methanol molecule per small void and 4 diffuse dmf
molecules per large voids, giving a total of 8 methanol and 16 dmf diffuse
molecules per cell, respectively 1 and 2 per formula unit. These have been
included in the formula, and taken into account for the density, mu and F000.
We note that such large diffuse electron density areas (17% of the cell) may
be the origin of the poor diffraction shown by the crystals.
;

_vrf_THETM01_nc33c               
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
Calculated sin(theta_max)/wavelength = 0.5746       
RESPONSE: Crystals were poorly diffracting. Even using a synchrotron source
significant diffraction was only up to ca. 0.85 angstrom. The present data
were cut at 0.87 angstrom resolution as then Rsigma>0.27. This results in
a relatively poor theta_max value.
;

_vrf_PLAT413_nc33c               
;
PROBLEM: Short Inter XH3 .. XHn      
RESPONSE: These shot contacts all involve one of the methyl groups of one of
the two lattice dmf molecules. These were heavily disordered and refined with
1,2 and 1,3-distance restraints. Hydrogens were placed geometrically on their
carrier carbon atoms, which given the disorder of these latter likely results
in ill-defined positions, and to these abnormally short H H contacts.
;

_vrf_PLAT260_nc33c               
;
PROBLEM: Large Average Ueq of Residue Including       O1S/O2S     
RESPONSE: Although clearly distinguished among residual electron peaks,
both lattice dfm molecules showed strong disorder and required 1,2 and
1,3 distance restraints combined with displacement parameters restraints
to refine satisfactorilly.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1956P)²+2.3423P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 5786 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.064(4)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         15347
_refine_ls_number_parameters     1165
_refine_ls_number_restraints     377
_refine_ls_R_factor_all          0.0838
_refine_ls_R_factor_gt           0.0799
_refine_ls_wR_factor_ref         0.2422
_refine_ls_wR_factor_gt          0.2312
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.047
_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 0.57259(4) 0.75936(4) 0.69897(6) 0.1011(3) Uani 1 1 d . . . . .
Fe2 Fe 0.74253(4) 1.00982(3) 0.47564(5) 0.0959(3) Uani 1 1 d . . . . .
N1 N 0.5235(2) 0.7057(2) 0.6783(4) 0.1102(19) Uani 1 1 d . . . . .
N2 N 0.5901(2) 0.7347(2) 0.6066(3) 0.0960(15) Uani 1 1 d . . . . .
N3 N 0.6196(2) 0.74312(18) 0.5601(3) 0.0906(14) Uani 1 1 d . . . . .
H3A H 0.638228 0.765468 0.560826 0.109 Uiso 1 1 calc R U . . .
N4 N 0.7607(2) 0.90321(17) 0.4571(3) 0.0960(15) Uani 1 1 d . . . . .
H4B H 0.733329 0.893920 0.452026 0.115 Uiso 1 1 calc R U . . .
N5 N 0.7718(2) 0.94386(19) 0.4779(3) 0.0997(16) Uani 1 1 d . . . . .
N6 N 0.8096(2) 1.01921(18) 0.5130(3) 0.0945(15) Uani 1 1 d . . . . .
N7 N 0.5289(3) 0.7800(3) 0.7794(4) 0.122(2) Uani 1 1 d . . . . .
N8 N 0.5362(2) 0.8164(2) 0.6635(4) 0.1091(19) Uani 1 1 d . . . . .
N9 N 0.5319(2) 0.8388(2) 0.6090(4) 0.1047(18) Uani 1 1 d . . . . .
H9A H 0.551037 0.837467 0.577648 0.126 Uiso 1 1 calc R U . . .
N10 N 0.6539(3) 0.9663(2) 0.4133(4) 0.112(2) Uani 1 1 d . . . . .
H10B H 0.643042 0.953446 0.447310 0.135 Uiso 1 1 calc R U . . .
N11 N 0.6920(3) 0.9901(2) 0.4121(4) 0.111(2) Uani 1 1 d . . . . .
N12 N 0.7675(3) 1.0298(2) 0.3819(3) 0.114(2) Uani 1 1 d . . . . .
N13 N 0.6099(2) 0.7121(2) 0.7623(3) 0.0985(15) Uani 1 1 d . . . . .
N14 N 0.63270(19) 0.79310(19) 0.7248(3) 0.0911(13) Uani 1 1 d . . . . .
N15 N 0.6473(2) 0.83534(19) 0.7178(3) 0.0926(14) Uani 1 1 d . . . . .
H15A H 0.638083 0.853864 0.688521 0.111 Uiso 1 1 calc R U . . .
N16 N 0.7133(2) 0.9748(2) 0.6082(3) 0.0949(15) Uani 1 1 d . . . . .
H16B H 0.715725 0.946464 0.599412 0.114 Uiso 1 1 calc R U . . .
N17 N 0.7115(2) 1.00599(18) 0.5646(3) 0.0944(15) Uani 1 1 d . . . . .
N18 N 0.7210(2) 1.0798(2) 0.5002(4) 0.1091(19) Uani 1 1 d . . . . .
C1 C 0.4891(3) 0.6907(4) 0.7164(6) 0.124(3) Uani 1 1 d . . . . .
H1A H 0.482802 0.707543 0.753227 0.148 Uiso 1 1 calc R U . . .
C2 C 0.4651(4) 0.6562(4) 0.7068(6) 0.127(3) Uani 1 1 d . . . . .
H2A H 0.441643 0.648722 0.734774 0.153 Uiso 1 1 calc R U . . .
C3 C 0.4749(3) 0.6292(4) 0.6519(8) 0.141(4) Uani 1 1 d . . . . .
C4 C 0.5096(3) 0.6440(3) 0.6129(6) 0.127(3) Uani 1 1 d . . . . .
H4A H 0.516867 0.628231 0.575491 0.152 Uiso 1 1 calc R U . . .
C5 C 0.5326(2) 0.6808(3) 0.6287(5) 0.104(2) Uani 1 1 d . . . . .
C6 C 0.5686(3) 0.6982(3) 0.5872(4) 0.105(2) Uani 1 1 d . . . . .
C7 C 0.5851(3) 0.6841(2) 0.5299(4) 0.099(2) Uani 1 1 d . . . . .
H7A H 0.575951 0.658731 0.506837 0.119 Uiso 1 1 calc R U . . .
C8 C 0.6172(3) 0.7135(2) 0.5126(4) 0.0944(19) Uani 1 1 d . . . . .
C9 C 0.6458(3) 0.7148(2) 0.4571(4) 0.0941(18) Uani 1 1 d . . . . .
C10 C 0.6368(3) 0.6849(2) 0.4065(4) 0.102(2) Uani 1 1 d . . . . .
H10A H 0.611491 0.666295 0.408213 0.122 Uiso 1 1 calc R U . . .
C11 C 0.6638(3) 0.6830(3) 0.3570(4) 0.107(2) Uani 1 1 d . . . . .
H11A H 0.657149 0.662812 0.323915 0.128 Uiso 1 1 calc R U . . .
C12 C 0.7022(3) 0.7097(2) 0.3513(4) 0.0975(19) Uani 1 1 d . . . . .
H12A H 0.720610 0.707827 0.315020 0.117 Uiso 1 1 calc R U . . .
C13 C 0.7120(3) 0.7387(2) 0.4005(3) 0.0934(17) Uani 1 1 d . . . . .
C14 C 0.6842(3) 0.7411(2) 0.4529(3) 0.0923(17) Uani 1 1 d . . . . .
H14A H 0.691264 0.760709 0.486540 0.111 Uiso 1 1 calc R U . . .
C15 C 0.7547(3) 0.7657(2) 0.3973(3) 0.0976(19) Uani 1 1 d . . . . .
C16 C 0.7918(3) 0.7478(2) 0.3699(4) 0.101(2) Uani 1 1 d . . . . .
H16A H 0.790607 0.719152 0.351552 0.121 Uiso 1 1 calc R U . . .
C17 C 0.8305(4) 0.7714(2) 0.3690(4) 0.111(2) Uani 1 1 d . . . . .
H17A H 0.856449 0.758339 0.351874 0.134 Uiso 1 1 calc R U . . .
C18 C 0.8324(3) 0.8154(2) 0.3935(4) 0.107(2) Uani 1 1 d . . . . .
H18A H 0.858890 0.832234 0.391522 0.129 Uiso 1 1 calc R U . . .
C19 C 0.7942(3) 0.8326(2) 0.4203(4) 0.100(2) Uani 1 1 d . . . . .
C20 C 0.7559(3) 0.8081(2) 0.4232(3) 0.099(2) Uani 1 1 d . . . . .
H20A H 0.730305 0.820036 0.442809 0.119 Uiso 1 1 calc R U . . .
C21 C 0.7971(3) 0.8785(2) 0.4449(4) 0.0986(19) Uani 1 1 d . . . . .
C22 C 0.8328(3) 0.9046(2) 0.4571(4) 0.1004(19) Uani 1 1 d . . . . .
H22A H 0.863079 0.896950 0.452115 0.120 Uiso 1 1 calc R U . . .
C23 C 0.8160(3) 0.9448(3) 0.4784(4) 0.1015(19) Uani 1 1 d . . . . .
C24 C 0.8377(3) 0.9852(2) 0.5000(4) 0.103(2) Uani 1 1 d . . . . .
C25 C 0.8818(3) 0.9880(3) 0.5093(6) 0.123(3) Uani 1 1 d . . . . .
H25A H 0.900392 0.963592 0.499307 0.147 Uiso 1 1 calc R U . . .
C26 C 0.9005(3) 1.0278(3) 0.5341(6) 0.127(3) Uani 1 1 d . . . . .
C27 C 0.8711(3) 1.0613(3) 0.5495(4) 0.107(2) Uani 1 1 d . . . . .
H27A H 0.881713 1.087515 0.569066 0.128 Uiso 1 1 calc R U . . .
C28 C 0.8266(3) 1.0569(2) 0.5368(4) 0.1004(19) Uani 1 1 d . . . . .
H28A H 0.807387 1.081093 0.544957 0.120 Uiso 1 1 calc R U . . .
C29 C 0.4491(5) 0.5889(6) 0.6368(11) 0.188(7) Uani 1 1 d . . . . .
H29A H 0.426561 0.584217 0.669463 0.282 Uiso 1 1 calc R U . . .
H29B H 0.434686 0.592528 0.595558 0.282 Uiso 1 1 calc R U . . .
H29C H 0.468990 0.563314 0.635374 0.282 Uiso 1 1 calc R U . . .
C30 C 0.9495(4) 1.0343(4) 0.5414(9) 0.161(5) Uani 1 1 d . . . . .
H30A H 0.965025 1.007305 0.528308 0.241 Uiso 1 1 calc R U . . .
H30B H 0.959151 1.059099 0.514877 0.241 Uiso 1 1 calc R U . . .
H30C H 0.956401 1.040697 0.585801 0.241 Uiso 1 1 calc R U . . .
C31 C 0.5267(4) 0.7590(5) 0.8358(5) 0.141(4) Uani 1 1 d . . . . .
H31A H 0.549423 0.738630 0.846478 0.169 Uiso 1 1 calc R U . . .
C32 C 0.4929(5) 0.7659(5) 0.8787(7) 0.157(4) Uani 1 1 d . . . . .
H32A H 0.493554 0.752126 0.919088 0.188 Uiso 1 1 calc R U . . .
C33 C 0.4576(6) 0.7936(7) 0.8616(9) 0.184(6) Uani 1 1 d . . . . .
C34 C 0.4622(5) 0.8159(6) 0.8047(10) 0.178(6) Uani 1 1 d . . . . .
H34A H 0.441108 0.837870 0.793738 0.213 Uiso 1 1 calc R U . . .
C35 C 0.4969(3) 0.8070(4) 0.7626(6) 0.130(3) Uani 1 1 d . . . . .
C36 C 0.5014(3) 0.8277(3) 0.6986(5) 0.113(2) Uani 1 1 d . . . . .
C37 C 0.4741(4) 0.8577(3) 0.6651(8) 0.141(4) Uani 1 1 d . . . . .
H37A H 0.447243 0.870742 0.679252 0.169 Uiso 1 1 calc R U . . .
C38 C 0.4946(3) 0.8639(3) 0.6079(6) 0.115(3) Uani 1 1 d . . . . .
C39 C 0.4800(4) 0.8880(3) 0.5512(7) 0.136(2) Uani 1 1 d . U . . .
C40 C 0.4359(4) 0.9035(3) 0.5499(8) 0.150(3) Uani 1 1 d . U . . .
H40A H 0.418277 0.900752 0.586913 0.180 Uiso 1 1 calc R U . . .
C41 C 0.4181(5) 0.9218(3) 0.4984(10) 0.169(3) Uani 1 1 d . U . . .
H41A H 0.387945 0.930681 0.497970 0.203 Uiso 1 1 calc R U . . .
C42 C 0.4441(5) 0.9275(3) 0.4467(9) 0.164(3) Uani 1 1 d . U . . .
H42A H 0.431913 0.941590 0.410478 0.196 Uiso 1 1 calc R U . . .
C43 C 0.4909(4) 0.9125(3) 0.4444(8) 0.152(2) Uani 1 1 d . U . . .
C44 C 0.5067(4) 0.8940(3) 0.5020(7) 0.136(2) Uani 1 1 d . U . . .
H44A H 0.536950 0.885761 0.505317 0.164 Uiso 1 1 calc R U . . .
C45 C 0.5210(5) 0.9171(3) 0.3876(8) 0.154(2) Uani 1 1 d . U . . .
C46 C 0.5101(5) 0.9036(3) 0.3269(8) 0.165(3) Uani 1 1 d . U . . .
H46A H 0.482824 0.888678 0.320134 0.198 Uiso 1 1 calc R U . . .
C47 C 0.5352(6) 0.9104(5) 0.2808(9) 0.175(3) Uani 1 1 d . U . . .
H47A H 0.524484 0.903150 0.239780 0.210 Uiso 1 1 calc R U . . .
C48 C 0.5788(5) 0.9284(4) 0.2857(7) 0.160(3) Uani 1 1 d . U . . .
H48A H 0.597891 0.930996 0.250171 0.193 Uiso 1 1 calc R U . . .
C49 C 0.5917(5) 0.9421(3) 0.3474(7) 0.145(3) Uani 1 1 d . U . . .
C50 C 0.5637(4) 0.9365(3) 0.3970(7) 0.143(3) Uani 1 1 d . U . . .
H50A H 0.572524 0.945401 0.438184 0.171 Uiso 1 1 calc R U . . .
C51 C 0.6349(5) 0.9649(3) 0.3558(6) 0.146(5) Uani 1 1 d . . . . .
C52 C 0.6608(5) 0.9897(3) 0.3152(6) 0.142(4) Uani 1 1 d . . . . .
H52A H 0.655676 0.995177 0.271499 0.171 Uiso 1 1 calc R U . . .
C53 C 0.6952(4) 1.0045(3) 0.3507(5) 0.124(3) Uani 1 1 d . . . . .
C54 C 0.7362(5) 1.0292(3) 0.3375(5) 0.128(3) Uani 1 1 d . . . . .
C55 C 0.7434(6) 1.0502(4) 0.2791(5) 0.150(4) Uani 1 1 d . . . . .
H55A H 0.721564 1.048799 0.246830 0.180 Uiso 1 1 calc R U . . .
C56 C 0.7818(7) 1.0727(4) 0.2690(6) 0.164(6) Uani 1 1 d . . . . .
C57 C 0.8142(5) 1.0699(4) 0.3119(5) 0.150(5) Uani 1 1 d . . . . .
H57A H 0.842460 1.082281 0.302931 0.180 Uiso 1 1 calc R U . . .
C58 C 0.8068(5) 1.0491(3) 0.3693(5) 0.131(3) Uani 1 1 d . . . . .
H58A H 0.829693 1.048424 0.400176 0.157 Uiso 1 1 calc R U . . .
C59 C 0.4175(8) 0.8073(10) 0.9042(12) 0.257(13) Uani 1 1 d . U . . .
H59A H 0.417613 0.789487 0.942939 0.386 Uiso 1 1 calc R U . . .
H59B H 0.419941 0.838704 0.915147 0.386 Uiso 1 1 calc R U . . .
H59C H 0.389844 0.802217 0.881056 0.386 Uiso 1 1 calc R U . . .
C60 C 0.7855(9) 1.1008(5) 0.2054(6) 0.211(10) Uani 1 1 d . U . . .
H60A H 0.757885 1.097988 0.181291 0.317 Uiso 1 1 calc R U . . .
H60B H 0.790602 1.131954 0.215770 0.317 Uiso 1 1 calc R U . . .
H60C H 0.810175 1.089612 0.179891 0.317 Uiso 1 1 calc R U . . .
C61 C 0.5999(3) 0.6697(3) 0.7769(4) 0.113(2) Uani 1 1 d . . . . .
H61A H 0.574410 0.656859 0.757944 0.136 Uiso 1 1 calc R U . . .
C62 C 0.6242(3) 0.6443(3) 0.8169(4) 0.114(2) Uani 1 1 d . . . . .
H62A H 0.615261 0.615084 0.827375 0.137 Uiso 1 1 calc R U . . .
C63 C 0.6628(4) 0.6626(4) 0.8424(5) 0.125(3) Uani 1 1 d . . . . .
H63A H 0.681352 0.644997 0.868548 0.150 Uiso 1 1 calc R U . . .
C64 C 0.6744(3) 0.7068(3) 0.8295(4) 0.109(2) Uani 1 1 d . . . . .
H64A H 0.699906 0.720235 0.847340 0.131 Uiso 1 1 calc R U . . .
C65 C 0.6459(3) 0.7298(3) 0.7885(3) 0.100(2) Uani 1 1 d . . . . .
C66 C 0.6550(3) 0.7757(3) 0.7722(3) 0.0950(17) Uani 1 1 d . . . . .
C67 C 0.6849(2) 0.8062(3) 0.7971(4) 0.0996(19) Uani 1 1 d . . . . .
H67A H 0.705510 0.801560 0.830463 0.120 Uiso 1 1 calc R U . . .
C68 C 0.6782(2) 0.8449(3) 0.7628(3) 0.0935(17) Uani 1 1 d . . . . .
C69 C 0.6991(2) 0.8892(3) 0.7660(4) 0.102(2) Uani 1 1 d . . . . .
C70 C 0.7210(3) 0.9010(3) 0.8218(4) 0.110(2) Uani 1 1 d . . . . .
H70A H 0.724421 0.880093 0.855036 0.132 Uiso 1 1 calc R U . . .
C71 C 0.7377(3) 0.9436(4) 0.8281(5) 0.118(3) Uani 1 1 d . . . . .
H71A H 0.751268 0.952443 0.866600 0.141 Uiso 1 1 calc R U . . .
C72 C 0.7346(3) 0.9734(3) 0.7775(5) 0.110(2) Uani 1 1 d . . . . .
H72A H 0.747096 1.002190 0.780869 0.133 Uiso 1 1 calc R U . . .
C73 C 0.7133(2) 0.9608(3) 0.7232(4) 0.0956(19) Uani 1 1 d . . . . .
C74 C 0.6952(2) 0.9188(2) 0.7177(4) 0.0946(18) Uani 1 1 d . . . . .
H74A H 0.680138 0.910649 0.680004 0.113 Uiso 1 1 calc R U . . .
C75 C 0.7113(2) 0.9910(3) 0.6678(4) 0.098(2) Uani 1 1 d . . . . .
C76 C 0.7082(2) 1.0367(2) 0.6624(4) 0.097(2) Uani 1 1 d . . . . .
H76A H 0.706382 1.057831 0.695618 0.117 Uiso 1 1 calc R U . . .
C77 C 0.7083(2) 1.0445(2) 0.5976(5) 0.100(2) Uani 1 1 d . . . . .
C78 C 0.7073(3) 1.0852(3) 0.5586(5) 0.106(2) Uani 1 1 d . . . . .
C79 C 0.6909(3) 1.1255(3) 0.5830(5) 0.114(3) Uani 1 1 d . . . . .
H79A H 0.681222 1.127745 0.625612 0.137 Uiso 1 1 calc R U . . .
C80 C 0.6894(3) 1.1602(3) 0.5442(7) 0.129(3) Uani 1 1 d . . . . .
H80A H 0.679119 1.188092 0.558788 0.155 Uiso 1 1 calc R U . . .
C81 C 0.7035(5) 1.1548(3) 0.4812(8) 0.149(5) Uani 1 1 d . . . . .
H81A H 0.701825 1.179093 0.452814 0.179 Uiso 1 1 calc R U . . .
C82 C 0.7192(4) 1.1158(3) 0.4606(6) 0.126(3) Uani 1 1 d . . . . .
H82A H 0.729118 1.113102 0.418084 0.151 Uiso 1 1 calc R U . . .
Si1 Si 0.64787(7) 0.86908(6) 0.53696(10) 0.0904(5) Uani 1 1 d . . . . .
F1 F 0.62523(13) 0.87546(12) 0.6099(2) 0.0948(10) Uani 1 1 d . . . . .
F2 F 0.67004(16) 0.86423(13) 0.46425(19) 0.1021(11) Uani 1 1 d . . . . .
F3 F 0.62740(16) 0.91862(12) 0.5171(2) 0.1059(12) Uani 1 1 d . . . . .
F4 F 0.69525(13) 0.89301(12) 0.56260(19) 0.0938(10) Uani 1 1 d . . . . .
F5 F 0.66817(14) 0.81928(11) 0.55871(19) 0.0933(10) Uani 1 1 d . . . . .
F6 F 0.60105(15) 0.84407(12) 0.5130(2) 0.1026(12) Uani 1 1 d . . . . .
B1 B 0.5532(4) 0.5532(4) 0.500000 0.179(5) Uani 1 2 d DS TU P . .
F7 F 0.5657(4) 0.5870(4) 0.4527(6) 0.222(4) Uani 1 1 d D U . . .
F8 F 0.5198(7) 0.5470(9) 0.5503(13) 0.222(7) Uani 0.5 1 d D U P A 1
F8B F 0.5094(6) 0.5760(8) 0.5000(16) 0.220(7) Uani 0.5 1 d D U P A 2
B2 B 0.2603(13) 0.8293(12) 0.8016(17) 0.346(14) Uiso 0.5 1 d D U P B 1
F9 F 0.2966(16) 0.8515(15) 0.834(2) 0.397(19) Uiso 0.5 1 d D U P B 1
F10 F 0.2636(14) 0.7817(11) 0.8125(18) 0.294(12) Uiso 0.5 1 d D U P B 1
F11 F 0.2634(19) 0.8378(16) 0.7330(18) 0.407(18) Uiso 0.5 1 d D U P B 1
F12 F 0.2180(14) 0.8453(16) 0.825(2) 0.42(2) Uiso 0.5 1 d D U P B 1
B3 B 0.2554(11) 0.7855(12) 0.7584(16) 0.329(12) Uiso 0.5 1 d D U P C 2
F13 F 0.2565(14) 0.8100(14) 0.8196(17) 0.330(14) Uiso 0.5 1 d D U P C 2
F14 F 0.2701(15) 0.7386(13) 0.768(2) 0.339(14) Uiso 0.5 1 d D U P C 2
F15 F 0.2866(15) 0.8077(17) 0.713(2) 0.40(2) Uiso 0.5 1 d D U P C 2
F16 F 0.2099(11) 0.7871(13) 0.7303(16) 0.286(12) Uiso 0.5 1 d D U P C 2
B4 B 0.9434(14) 1.0614(12) 0.1927(16) 0.39(2) Uiso 0.5 1 d D U P D -1
F17 F 0.9439(15) 1.0767(14) 0.1304(16) 0.315(17) Uiso 0.5 1 d D U P D -1
F18 F 0.936(2) 1.0158(15) 0.194(3) 0.43(3) Uiso 0.5 1 d D U P D -1
F19 F 0.9088(18) 1.0833(17) 0.225(2) 0.38(2) Uiso 0.5 1 d D U P D -1
F20 F 0.9838(17) 1.071(2) 0.222(2) 0.44(3) Uiso 0.5 1 d D U P D -1
O1S O 0.5125(12) 0.8678(13) 0.9242(13) 0.412(14) Uani 1 1 d D U . . .
C1S C 0.4970(17) 0.8935(15) 0.881(2) 0.392(14) Uani 1 1 d D U . . .
H1S H 0.484353 0.880636 0.844015 0.470 Uiso 1 1 calc R U . . .
N1S N 0.4984(14) 0.9424(13) 0.8863(17) 0.388(13) Uani 1 1 d D U . . .
C2S C 0.5162(14) 0.9654(16) 0.9435(19) 0.389(15) Uani 1 1 d D U . . .
H2S1 H 0.534336 0.944740 0.968146 0.584 Uiso 1 1 calc R U . . .
H2S2 H 0.534442 0.990612 0.930279 0.584 Uiso 1 1 calc R U . . .
H2S3 H 0.491608 0.976020 0.969646 0.584 Uiso 1 1 calc R U . . .
C3S C 0.4700(14) 0.9677(17) 0.842(2) 0.398(16) Uani 1 1 d D U . . .
H3S1 H 0.478849 0.998942 0.841935 0.597 Uiso 1 1 d R U . . .
H3S2 H 0.438889 0.965442 0.855165 0.597 Uiso 1 1 d R U . . .
H3S3 H 0.473599 0.955202 0.799865 0.597 Uiso 1 1 d R U . . .
O2S O 0.4245(11) 0.5572(13) 1.1276(14) 0.382(13) Uani 1 1 d D U . . .
C4S C 0.4015(12) 0.5805(13) 1.0891(17) 0.316(10) Uani 1 1 d D U . . .
H4S H 0.410023 0.610366 1.082402 0.379 Uiso 1 1 calc R U . . .
N2S N 0.3630(10) 0.5638(11) 1.0548(12) 0.304(9) Uani 1 1 d D U . . .
C5S C 0.3322(9) 0.5321(10) 1.0832(12) 0.251(9) Uani 1 1 d D U . . .
H5S1 H 0.308743 0.525051 1.052853 0.377 Uiso 1 1 calc R U . . .
H5S2 H 0.348244 0.504973 1.094351 0.377 Uiso 1 1 calc R U . . .
H5S3 H 0.319171 0.544994 1.121427 0.377 Uiso 1 1 calc R U . . .
C6S C 0.3630(14) 0.5510(16) 0.9866(14) 0.353(14) Uani 1 1 d D U . . .
H6S1 H 0.338010 0.531208 0.978330 0.529 Uiso 1 1 d R U . . .
H6S2 H 0.390800 0.535348 0.977990 0.529 Uiso 1 1 d R U . . .
H6S3 H 0.360910 0.577038 0.959150 0.529 Uiso 1 1 d R U . . .


_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 N14 2.153(6) . ?
Fe1 N2 2.155(7) . ?
Fe1 N8 2.176(7) . ?
Fe1 N7 2.240(9) . ?
Fe1 N1 2.241(7) . ?
Fe1 N13 2.258(6) . ?
Fe2 N17 2.104(7) . ?
Fe2 N11 2.119(7) . ?
Fe2 N5 2.181(6) . ?
Fe2 N6 2.194(6) . ?
Fe2 N12 2.203(8) . ?
Fe2 N18 2.273(6) . ?
N1 C5 1.319(12) . ?
N1 C1 1.390(14) . ?
N2 C6 1.342(10) . ?
N2 N3 1.350(9) . ?
N3 C8 1.347(9) . ?
N3 H3A 0.8800 . ?
N4 N5 1.348(8) . ?
N4 C21 1.352(10) . ?
N4 H4B 0.8800 . ?
N5 C23 1.337(11) . ?
N6 C28 1.346(9) . ?
N6 C24 1.360(10) . ?
N7 C35 1.313(15) . ?
N7 C31 1.352(15) . ?
N8 C36 1.332(12) . ?
N8 N9 1.343(11) . ?
N9 C38 1.359(11) . ?
N9 H9A 0.8800 . ?
N10 C51 1.345(13) . ?
N10 N11 1.357(11) . ?
N10 H10B 0.8800 . ?
N11 C53 1.373(13) . ?
N12 C54 1.333(13) . ?
N12 C58 1.351(15) . ?
N13 C65 1.332(11) . ?
N13 C61 1.354(12) . ?
N14 C66 1.317(10) . ?
N14 N15 1.358(9) . ?
N15 C68 1.363(9) . ?
N15 H15A 0.8800 . ?
N16 N17 1.318(10) . ?
N16 C75 1.352(10) . ?
N16 H16B 0.8800 . ?
N17 C77 1.360(9) . ?
N18 C78 1.311(13) . ?
N18 C82 1.374(13) . ?
C1 C2 1.286(15) . ?
C1 H1A 0.9500 . ?
C2 C3 1.449(19) . ?
C2 H2A 0.9500 . ?
C3 C4 1.406(18) . ?
C3 C29 1.480(19) . ?
C4 C5 1.351(13) . ?
C4 H4A 0.9500 . ?
C5 C6 1.494(14) . ?
C6 C7 1.377(13) . ?
C7 C8 1.365(12) . ?
C7 H7A 0.9500 . ?
C8 C9 1.457(12) . ?
C9 C14 1.407(11) . ?
C9 C10 1.426(10) . ?
C10 C11 1.327(13) . ?
C10 H10A 0.9500 . ?
C11 C12 1.416(13) . ?
C11 H11A 0.9500 . ?
C12 C13 1.391(10) . ?
C12 H12A 0.9500 . ?
C13 C14 1.392(11) . ?
C13 C15 1.528(12) . ?
C14 H14A 0.9500 . ?
C15 C16 1.370(12) . ?
C15 C20 1.393(9) . ?
C16 C17 1.371(14) . ?
C16 H16A 0.9500 . ?
C17 C18 1.425(11) . ?
C17 H17A 0.9500 . ?
C18 C19 1.387(13) . ?
C18 H18A 0.9500 . ?
C19 C20 1.374(13) . ?
C19 C21 1.486(9) . ?
C20 H20A 0.9500 . ?
C21 C22 1.362(12) . ?
C22 C23 1.390(11) . ?
C22 H22A 0.9500 . ?
C23 C24 1.458(11) . ?
C24 C25 1.351(13) . ?
C25 C26 1.428(12) . ?
C25 H25A 0.9500 . ?
C26 C27 1.385(12) . ?
C26 C30 1.502(15) . ?
C27 C28 1.377(12) . ?
C27 H27A 0.9500 . ?
C28 H28A 0.9500 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.380(18) . ?
C31 H31A 0.9500 . ?
C32 C33 1.40(2) . ?
C32 H32A 0.9500 . ?
C33 C34 1.38(3) . ?
C33 C59 1.56(2) . ?
C34 C35 1.40(2) . ?
C34 H34A 0.9500 . ?
C35 C36 1.496(17) . ?
C36 C37 1.415(15) . ?
C37 C38 1.370(19) . ?
C37 H37A 0.9500 . ?
C38 C39 1.469(17) . ?
C39 C44 1.328(19) . ?
C39 C40 1.414(15) . ?
C40 C41 1.33(2) . ?
C40 H40A 0.9500 . ?
C41 C42 1.36(2) . ?
C41 H41A 0.9500 . ?
C42 C43 1.49(2) . ?
C42 H42A 0.9500 . ?
C43 C44 1.422(18) . ?
C43 C45 1.51(2) . ?
C44 H44A 0.9500 . ?
C45 C46 1.38(2) . ?
C45 C50 1.432(17) . ?
C46 C47 1.25(3) . ?
C46 H46A 0.9500 . ?
C47 C48 1.43(2) . ?
C47 H47A 0.9500 . ?
C48 C49 1.422(17) . ?
C48 H48A 0.9500 . ?
C49 C50 1.36(2) . ?
C49 C51 1.48(2) . ?
C50 H50A 0.9500 . ?
C51 C52 1.38(2) . ?
C52 C53 1.358(16) . ?
C52 H52A 0.9500 . ?
C53 C54 1.470(18) . ?
C54 C55 1.405(16) . ?
C55 C56 1.36(2) . ?
C55 H55A 0.9500 . ?
C56 C57 1.34(2) . ?
C56 C60 1.593(18) . ?
C57 C58 1.384(16) . ?
C57 H57A 0.9500 . ?
C58 H58A 0.9500 . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 C62 1.357(13) . ?
C61 H61A 0.9500 . ?
C62 C63 1.397(16) . ?
C62 H62A 0.9500 . ?
C63 C64 1.408(15) . ?
C63 H63A 0.9500 . ?
C64 C65 1.405(11) . ?
C64 H64A 0.9500 . ?
C65 C66 1.453(12) . ?
C66 C67 1.396(12) . ?
C67 C68 1.392(12) . ?
C67 H67A 0.9500 . ?
C68 C69 1.479(12) . ?
C69 C74 1.364(12) . ?
C69 C70 1.398(12) . ?
C70 C71 1.389(15) . ?
C70 H70A 0.9500 . ?
C71 C72 1.402(16) . ?
C71 H71A 0.9500 . ?
C72 C73 1.368(11) . ?
C72 H72A 0.9500 . ?
C73 C74 1.387(11) . ?
C73 C75 1.485(13) . ?
C74 H74A 0.9500 . ?
C75 C76 1.389(12) . ?
C76 C77 1.391(13) . ?
C76 H76A 0.9500 . ?
C77 C78 1.479(13) . ?
C78 C79 1.411(11) . ?
C79 C80 1.332(17) . ?
C79 H79A 0.9500 . ?
C80 C81 1.41(2) . ?
C80 H80A 0.9500 . ?
C81 C82 1.342(17) . ?
C81 H81A 0.9500 . ?
C82 H82A 0.9500 . ?
Si1 F3 1.673(4) . ?
Si1 F6 1.682(5) . ?
Si1 F2 1.682(5) . ?
Si1 F5 1.689(4) . ?
Si1 F4 1.693(4) . ?
Si1 F1 1.697(5) . ?
B1 F8 1.476(17) . ?
B1 F8 1.476(17) 7_556 ?
B1 F7 1.478(14) . ?
B1 F7 1.478(14) 7_556 ?
B1 F8B 1.491(16) 7_556 ?
B1 F8B 1.491(16) . ?
B2 F12 1.45(2) . ?
B2 F9 1.46(2) . ?
B2 F10 1.46(2) . ?
B2 F11 1.48(2) . ?
B3 F16 1.31(5) 8_666 ?
B3 F13 1.49(2) . ?
B3 F16 1.50(2) . ?
B3 F14 1.50(2) . ?
B3 F15 1.50(2) . ?
B3 F14 1.77(6) 8_666 ?
B3 B3 1.78(7) 8_666 ?
F14 F14 0.83(9) 8_666 ?
F16 F16 0.84(7) 8_666 ?
B4 F18 1.40(3) . ?
B4 F17 1.40(3) . ?
B4 F20 1.40(3) . ?
B4 F19 1.41(3) . ?
O1S C1S 1.29(3) . ?
C1S N1S 1.48(3) . ?
C1S H1S 0.9500 . ?
N1S C3S 1.48(3) . ?
N1S C2S 1.50(3) . ?
C2S H2S1 0.9800 . ?
C2S H2S2 0.9800 . ?
C2S H2S3 0.9800 . ?
C3S H3S1 0.9802 . ?
C3S H3S2 0.9799 . ?
C3S H3S3 0.9799 . ?
O2S C4S 1.28(3) . ?
C4S N2S 1.46(2) . ?
C4S H4S 0.9500 . ?
N2S C5S 1.46(2) . ?
N2S C6S 1.49(3) . ?
C5S H5S1 0.9800 . ?
C5S H5S2 0.9800 . ?
C5S H5S3 0.9800 . ?
C6S H6S1 0.9797 . ?
C6S H6S2 0.9798 . ?
C6S H6S3 0.9800 . ?

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
N14 Fe1 N2 100.7(2) . . ?
N14 Fe1 N8 97.9(2) . . ?
N2 Fe1 N8 94.9(3) . . ?
N14 Fe1 N7 100.0(3) . . ?
N2 Fe1 N7 158.1(3) . . ?
N8 Fe1 N7 75.1(3) . . ?
N14 Fe1 N1 161.9(3) . . ?
N2 Fe1 N1 74.7(3) . . ?
N8 Fe1 N1 99.9(3) . . ?
N7 Fe1 N1 87.6(3) . . ?
N14 Fe1 N13 74.2(2) . . ?
N2 Fe1 N13 101.3(2) . . ?
N8 Fe1 N13 163.0(3) . . ?
N7 Fe1 N13 91.2(3) . . ?
N1 Fe1 N13 89.4(3) . . ?
N17 Fe2 N11 103.2(3) . . ?
N17 Fe2 N5 96.4(2) . . ?
N11 Fe2 N5 92.9(2) . . ?
N17 Fe2 N6 95.6(2) . . ?
N11 Fe2 N6 158.5(3) . . ?
N5 Fe2 N6 74.6(2) . . ?
N17 Fe2 N12 166.0(3) . . ?
N11 Fe2 N12 75.8(3) . . ?
N5 Fe2 N12 97.6(3) . . ?
N6 Fe2 N12 88.4(3) . . ?
N17 Fe2 N18 73.7(3) . . ?
N11 Fe2 N18 101.5(3) . . ?
N5 Fe2 N18 164.0(3) . . ?
N6 Fe2 N18 93.6(2) . . ?
N12 Fe2 N18 92.7(3) . . ?
C5 N1 C1 115.4(8) . . ?
C5 N1 Fe1 115.5(6) . . ?
C1 N1 Fe1 128.1(7) . . ?
C6 N2 N3 104.5(7) . . ?
C6 N2 Fe1 116.2(6) . . ?
N3 N2 Fe1 139.1(4) . . ?
C8 N3 N2 112.5(6) . . ?
C8 N3 H3A 123.7 . . ?
N2 N3 H3A 123.7 . . ?
N5 N4 C21 111.2(7) . . ?
N5 N4 H4B 124.4 . . ?
C21 N4 H4B 124.4 . . ?
C23 N5 N4 105.7(6) . . ?
C23 N5 Fe2 112.7(5) . . ?
N4 N5 Fe2 136.4(5) . . ?
C28 N6 C24 118.4(7) . . ?
C28 N6 Fe2 126.6(5) . . ?
C24 N6 Fe2 114.0(5) . . ?
C35 N7 C31 119.5(10) . . ?
C35 N7 Fe1 113.7(8) . . ?
C31 N7 Fe1 124.6(8) . . ?
C36 N8 N9 105.7(7) . . ?
C36 N8 Fe1 114.3(7) . . ?
N9 N8 Fe1 138.1(6) . . ?
N8 N9 C38 112.1(9) . . ?
N8 N9 H9A 123.9 . . ?
C38 N9 H9A 123.9 . . ?
C51 N10 N11 111.2(10) . . ?
C51 N10 H10B 124.4 . . ?
N11 N10 H10B 124.4 . . ?
N10 N11 C53 104.3(7) . . ?
N10 N11 Fe2 138.5(6) . . ?
C53 N11 Fe2 117.3(7) . . ?
C54 N12 C58 119.5(9) . . ?
C54 N12 Fe2 112.7(7) . . ?
C58 N12 Fe2 126.6(6) . . ?
C65 N13 C61 117.9(7) . . ?
C65 N13 Fe1 113.6(5) . . ?
C61 N13 Fe1 128.5(6) . . ?
C66 N14 N15 107.0(6) . . ?
C66 N14 Fe1 115.7(5) . . ?
N15 N14 Fe1 133.7(4) . . ?
N14 N15 C68 110.3(6) . . ?
N14 N15 H15A 124.9 . . ?
C68 N15 H15A 124.9 . . ?
N17 N16 C75 113.0(6) . . ?
N17 N16 H16B 123.5 . . ?
C75 N16 H16B 123.5 . . ?
N16 N17 C77 104.9(7) . . ?
N16 N17 Fe2 130.1(4) . . ?
C77 N17 Fe2 116.2(6) . . ?
C78 N18 C82 117.6(8) . . ?
C78 N18 Fe2 114.8(6) . . ?
C82 N18 Fe2 127.5(7) . . ?
C2 C1 N1 126.5(12) . . ?
C2 C1 H1A 116.7 . . ?
N1 C1 H1A 116.7 . . ?
C1 C2 C3 117.8(11) . . ?
C1 C2 H2A 121.1 . . ?
C3 C2 H2A 121.1 . . ?
C4 C3 C2 116.2(10) . . ?
C4 C3 C29 121.9(15) . . ?
C2 C3 C29 121.9(13) . . ?
C5 C4 C3 120.1(12) . . ?
C5 C4 H4A 119.9 . . ?
C3 C4 H4A 119.9 . . ?
N1 C5 C4 123.8(9) . . ?
N1 C5 C6 114.6(7) . . ?
C4 C5 C6 121.4(10) . . ?
N2 C6 C7 110.4(8) . . ?
N2 C6 C5 117.6(8) . . ?
C7 C6 C5 132.1(8) . . ?
C8 C7 C6 106.9(7) . . ?
C8 C7 H7A 126.5 . . ?
C6 C7 H7A 126.5 . . ?
N3 C8 C7 105.6(7) . . ?
N3 C8 C9 123.5(7) . . ?
C7 C8 C9 130.9(7) . . ?
C14 C9 C10 117.9(8) . . ?
C14 C9 C8 123.6(6) . . ?
C10 C9 C8 118.2(7) . . ?
C11 C10 C9 120.0(8) . . ?
C11 C10 H10A 120.0 . . ?
C9 C10 H10A 120.0 . . ?
C10 C11 C12 123.0(7) . . ?
C10 C11 H11A 118.5 . . ?
C12 C11 H11A 118.5 . . ?
C13 C12 C11 118.1(8) . . ?
C13 C12 H12A 121.0 . . ?
C11 C12 H12A 121.0 . . ?
C12 C13 C14 119.8(8) . . ?
C12 C13 C15 118.9(7) . . ?
C14 C13 C15 121.2(6) . . ?
C13 C14 C9 121.2(6) . . ?
C13 C14 H14A 119.4 . . ?
C9 C14 H14A 119.4 . . ?
C16 C15 C20 120.4(8) . . ?
C16 C15 C13 119.9(6) . . ?
C20 C15 C13 119.6(8) . . ?
C15 C16 C17 119.9(7) . . ?
C15 C16 H16A 120.1 . . ?
C17 C16 H16A 120.1 . . ?
C16 C17 C18 120.9(9) . . ?
C16 C17 H17A 119.5 . . ?
C18 C17 H17A 119.5 . . ?
C19 C18 C17 117.6(9) . . ?
C19 C18 H18A 121.2 . . ?
C17 C18 H18A 121.2 . . ?
C20 C19 C18 121.1(6) . . ?
C20 C19 C21 122.5(8) . . ?
C18 C19 C21 116.4(8) . . ?
C19 C20 C15 120.0(8) . . ?
C19 C20 H20A 120.0 . . ?
C15 C20 H20A 120.0 . . ?
N4 C21 C22 106.8(6) . . ?
N4 C21 C19 122.3(8) . . ?
C22 C21 C19 130.9(8) . . ?
C21 C22 C23 106.2(7) . . ?
C21 C22 H22A 126.9 . . ?
C23 C22 H22A 126.9 . . ?
N5 C23 C22 110.1(7) . . ?
N5 C23 C24 118.0(7) . . ?
C22 C23 C24 132.0(8) . . ?
C25 C24 N6 122.7(7) . . ?
C25 C24 C23 122.7(7) . . ?
N6 C24 C23 114.5(7) . . ?
C24 C25 C26 119.7(8) . . ?
C24 C25 H25A 120.1 . . ?
C26 C25 H25A 120.1 . . ?
C27 C26 C25 116.6(8) . . ?
C27 C26 C30 120.9(8) . . ?
C25 C26 C30 122.5(8) . . ?
C28 C27 C26 120.6(7) . . ?
C28 C27 H27A 119.7 . . ?
C26 C27 H27A 119.7 . . ?
N6 C28 C27 121.8(7) . . ?
N6 C28 H28A 119.1 . . ?
C27 C28 H28A 119.1 . . ?
C3 C29 H29A 109.5 . . ?
C3 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C3 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C26 C30 H30A 109.5 . . ?
C26 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C26 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N7 C31 C32 123.0(13) . . ?
N7 C31 H31A 118.5 . . ?
C32 C31 H31A 118.5 . . ?
C31 C32 C33 118.9(15) . . ?
C31 C32 H32A 120.5 . . ?
C33 C32 H32A 120.5 . . ?
C34 C33 C32 115.9(14) . . ?
C34 C33 C59 116.7(19) . . ?
C32 C33 C59 126.8(19) . . ?
C33 C34 C35 122.3(15) . . ?
C33 C34 H34A 118.9 . . ?
C35 C34 H34A 118.9 . . ?
N7 C35 C34 119.9(14) . . ?
N7 C35 C36 116.0(9) . . ?
C34 C35 C36 124.1(12) . . ?
N8 C36 C37 110.3(11) . . ?
N8 C36 C35 117.8(8) . . ?
C37 C36 C35 131.8(11) . . ?
C38 C37 C36 105.4(10) . . ?
C38 C37 H37A 127.3 . . ?
C36 C37 H37A 127.3 . . ?
N9 C38 C37 106.5(10) . . ?
N9 C38 C39 122.6(11) . . ?
C37 C38 C39 130.7(10) . . ?
C44 C39 C40 120.7(12) . . ?
C44 C39 C38 121.7(9) . . ?
C40 C39 C38 117.6(14) . . ?
C41 C40 C39 122.3(17) . . ?
C41 C40 H40A 118.9 . . ?
C39 C40 H40A 118.9 . . ?
C40 C41 C42 118.4(13) . . ?
C40 C41 H41A 120.8 . . ?
C42 C41 H41A 120.8 . . ?
C41 C42 C43 122.6(13) . . ?
C41 C42 H42A 118.7 . . ?
C43 C42 H42A 118.7 . . ?
C44 C43 C42 114.2(16) . . ?
C44 C43 C45 121.0(11) . . ?
C42 C43 C45 124.8(12) . . ?
C39 C44 C43 121.4(11) . . ?
C39 C44 H44A 119.3 . . ?
C43 C44 H44A 119.3 . . ?
C46 C45 C50 117.5(17) . . ?
C46 C45 C43 124.5(12) . . ?
C50 C45 C43 118.0(12) . . ?
C47 C46 C45 121.9(13) . . ?
C47 C46 H46A 119.0 . . ?
C45 C46 H46A 119.0 . . ?
C46 C47 C48 124.3(14) . . ?
C46 C47 H47A 117.8 . . ?
C48 C47 H47A 117.8 . . ?
C49 C48 C47 115.5(17) . . ?
C49 C48 H48A 122.2 . . ?
C47 C48 H48A 122.2 . . ?
C50 C49 C48 119.9(13) . . ?
C50 C49 C51 121.0(11) . . ?
C48 C49 C51 119.0(15) . . ?
C49 C50 C45 120.5(12) . . ?
C49 C50 H50A 119.7 . . ?
C45 C50 H50A 119.7 . . ?
N10 C51 C52 107.5(11) . . ?
N10 C51 C49 119.8(13) . . ?
C52 C51 C49 132.4(10) . . ?
C53 C52 C51 105.7(10) . . ?
C53 C52 H52A 127.2 . . ?
C51 C52 H52A 127.2 . . ?
C52 C53 N11 111.3(11) . . ?
C52 C53 C54 134.9(11) . . ?
N11 C53 C54 113.6(8) . . ?
N12 C54 C55 120.0(11) . . ?
N12 C54 C53 118.1(9) . . ?
C55 C54 C53 121.8(10) . . ?
C56 C55 C54 119.8(12) . . ?
C56 C55 H55A 120.1 . . ?
C54 C55 H55A 120.1 . . ?
C57 C56 C55 119.1(12) . . ?
C57 C56 C60 123.7(15) . . ?
C55 C56 C60 117.2(16) . . ?
C56 C57 C58 120.3(12) . . ?
C56 C57 H57A 119.9 . . ?
C58 C57 H57A 119.9 . . ?
N12 C58 C57 120.7(11) . . ?
N12 C58 H58A 119.6 . . ?
C57 C58 H58A 119.6 . . ?
C33 C59 H59A 109.5 . . ?
C33 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C33 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C56 C60 H60A 109.5 . . ?
C56 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C56 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
N13 C61 C62 123.8(10) . . ?
N13 C61 H61A 118.1 . . ?
C62 C61 H61A 118.1 . . ?
C61 C62 C63 118.0(9) . . ?
C61 C62 H62A 121.0 . . ?
C63 C62 H62A 121.0 . . ?
C62 C63 C64 120.5(8) . . ?
C62 C63 H63A 119.7 . . ?
C64 C63 H63A 119.7 . . ?
C65 C64 C63 115.9(9) . . ?
C65 C64 H64A 122.1 . . ?
C63 C64 H64A 122.1 . . ?
N13 C65 C64 123.9(8) . . ?
N13 C65 C66 116.0(7) . . ?
C64 C65 C66 120.1(8) . . ?
N14 C66 C67 110.7(7) . . ?
N14 C66 C65 117.7(7) . . ?
C67 C66 C65 131.6(7) . . ?
C68 C67 C66 105.4(6) . . ?
C68 C67 H67A 127.3 . . ?
C66 C67 H67A 127.3 . . ?
N15 C68 C67 106.5(7) . . ?
N15 C68 C69 121.1(7) . . ?
C67 C68 C69 132.3(7) . . ?
C74 C69 C70 120.2(8) . . ?
C74 C69 C68 121.5(7) . . ?
C70 C69 C68 118.2(9) . . ?
C71 C70 C69 119.3(10) . . ?
C71 C70 H70A 120.3 . . ?
C69 C70 H70A 120.3 . . ?
C70 C71 C72 120.0(7) . . ?
C70 C71 H71A 120.0 . . ?
C72 C71 H71A 120.0 . . ?
C73 C72 C71 119.4(8) . . ?
C73 C72 H72A 120.3 . . ?
C71 C72 H72A 120.3 . . ?
C72 C73 C74 120.7(9) . . ?
C72 C73 C75 120.6(8) . . ?
C74 C73 C75 118.6(7) . . ?
C69 C74 C73 120.3(7) . . ?
C69 C74 H74A 119.8 . . ?
C73 C74 H74A 119.8 . . ?
N16 C75 C76 106.6(8) . . ?
N16 C75 C73 120.8(6) . . ?
C76 C75 C73 132.6(7) . . ?
C75 C76 C77 104.5(6) . . ?
C75 C76 H76A 127.8 . . ?
C77 C76 H76A 127.8 . . ?
N17 C77 C76 111.1(8) . . ?
N17 C77 C78 115.3(8) . . ?
C76 C77 C78 133.6(7) . . ?
N18 C78 C79 124.0(10) . . ?
N18 C78 C77 114.5(7) . . ?
C79 C78 C77 121.4(9) . . ?
C80 C79 C78 117.9(11) . . ?
C80 C79 H79A 121.1 . . ?
C78 C79 H79A 121.1 . . ?
C79 C80 C81 118.7(9) . . ?
C79 C80 H80A 120.7 . . ?
C81 C80 H80A 120.7 . . ?
C82 C81 C80 121.1(11) . . ?
C82 C81 H81A 119.4 . . ?
C80 C81 H81A 119.4 . . ?
C81 C82 N18 120.7(12) . . ?
C81 C82 H82A 119.7 . . ?
N18 C82 H82A 119.7 . . ?
F3 Si1 F6 90.9(2) . . ?
F3 Si1 F2 89.8(2) . . ?
F6 Si1 F2 91.2(2) . . ?
F3 Si1 F5 178.7(3) . . ?
F6 Si1 F5 89.3(2) . . ?
F2 Si1 F5 91.5(2) . . ?
F3 Si1 F4 90.6(2) . . ?
F6 Si1 F4 178.3(2) . . ?
F2 Si1 F4 89.6(2) . . ?
F5 Si1 F4 89.2(2) . . ?
F3 Si1 F1 88.7(2) . . ?
F6 Si1 F1 89.2(2) . . ?
F2 Si1 F1 178.4(2) . . ?
F5 Si1 F1 90.0(2) . . ?
F4 Si1 F1 90.1(2) . . ?
F8 B1 F8 110(2) . 7_556 ?
F8 B1 F7 138.5(12) . . ?
F8 B1 F7 91.0(12) 7_556 . ?
F8 B1 F7 91.0(12) . 7_556 ?
F8 B1 F7 138.5(12) 7_556 7_556 ?
F7 B1 F7 95.8(14) . 7_556 ?
F8 B1 F8B 101.9(16) . 7_556 ?
F8 B1 F8B 56.8(15) 7_556 7_556 ?
F7 B1 F8B 119.5(13) . 7_556 ?
F7 B1 F8B 84.7(14) 7_556 7_556 ?
F7 B1 F8B 84.7(14) . . ?
F7 B1 F8B 119.5(13) 7_556 . ?
F8B B1 F8B 145(2) 7_556 . ?
F12 B2 F9 110.2(17) . . ?
F12 B2 F10 109.6(17) . . ?
F9 B2 F10 109.2(17) . . ?
F12 B2 F11 109.6(17) . . ?
F9 B2 F11 109.5(17) . . ?
F10 B2 F11 108.8(17) . . ?
F16 B3 F13 79(3) 8_666 . ?
F16 B3 F16 34(3) 8_666 . ?
F13 B3 F16 110.4(16) . . ?
F16 B3 F14 111(3) 8_666 . ?
F13 B3 F14 110.6(16) . . ?
F16 B3 F14 110.8(16) . . ?
F16 B3 F15 133(3) 8_666 . ?
F13 B3 F15 108.4(16) . . ?
F16 B3 F15 108.0(16) . . ?
F14 B3 F15 108.6(16) . . ?
F16 B3 F14 105(4) 8_666 8_666 ?
F13 B3 F14 137(3) . 8_666 ?
F16 B3 F14 90(3) . 8_666 ?
F14 B3 F14 28(3) . 8_666 ?
F15 B3 F14 99(3) . 8_666 ?
F16 B3 B3 55(2) 8_666 8_666 ?
F13 B3 B3 122(3) . 8_666 ?
F16 B3 B3 46.3(17) . 8_666 ?
F14 B3 B3 64.9(17) . 8_666 ?
F15 B3 B3 128(3) . 8_666 ?
F14 B3 B3 49.8(18) 8_666 8_666 ?
F14 F14 B3 95(4) 8_666 . ?
F14 F14 B3 57(3) 8_666 8_666 ?
B3 F14 B3 65(2) . 8_666 ?
F16 F16 B3 85(4) 8_666 8_666 ?
F16 F16 B3 61(3) 8_666 . ?
B3 F16 B3 78(3) 8_666 . ?
F18 B4 F17 110.7(18) . . ?
F18 B4 F20 109.7(18) . . ?
F17 B4 F20 109.8(18) . . ?
F18 B4 F19 109.3(18) . . ?
F17 B4 F19 108.1(17) . . ?
F20 B4 F19 109.3(18) . . ?
O1S C1S N1S 122(4) . . ?
O1S C1S H1S 118.8 . . ?
N1S C1S H1S 118.8 . . ?
C3S N1S C1S 117(4) . . ?
C3S N1S C2S 118(3) . . ?
C1S N1S C2S 122(3) . . ?
N1S C2S H2S1 109.5 . . ?
N1S C2S H2S2 109.5 . . ?
H2S1 C2S H2S2 109.5 . . ?
N1S C2S H2S3 109.5 . . ?
H2S1 C2S H2S3 109.5 . . ?
H2S2 C2S H2S3 109.5 . . ?
N1S C3S H3S1 110.2 . . ?
N1S C3S H3S2 110.2 . . ?
H3S1 C3S H3S2 109.4 . . ?
N1S C3S H3S3 108.0 . . ?
H3S1 C3S H3S3 109.5 . . ?
H3S2 C3S H3S3 109.5 . . ?
O2S C4S N2S 124(3) . . ?
O2S C4S H4S 118.0 . . ?
N2S C4S H4S 118.0 . . ?
C4S N2S C5S 122(2) . . ?
C4S N2S C6S 125(3) . . ?
C5S N2S C6S 103(3) . . ?
N2S C5S H5S1 109.5 . . ?
N2S C5S H5S2 109.5 . . ?
H5S1 C5S H5S2 109.5 . . ?
N2S C5S H5S3 109.5 . . ?
H5S1 C5S H5S3 109.5 . . ?
H5S2 C5S H5S3 109.5 . . ?
N2S C6S H6S1 109.3 . . ?
N2S C6S H6S2 107.8 . . ?
H6S1 C6S H6S2 109.5 . . ?
N2S C6S H6S3 111.3 . . ?
H6S1 C6S H6S3 109.5 . . ?
H6S2 C6S H6S3 109.5 . . ?

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 H3A F5 0.88 1.86 2.730(7) 169.0 . yes
N4 H4B F2 0.88 2.13 2.986(9) 164.7 . yes
N9 H9A F6 0.88 2.05 2.916(10) 169.3 . yes
N10 H10B F3 0.88 1.87 2.743(10) 170.1 . yes
N15 H15A F1 0.88 1.83 2.667(8) 159.2 . yes
N16 H16B F4 0.88 1.90 2.709(6) 152.8 . yes

_refine_diff_density_max         0.580
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.079


