# Electronic Supplementary Material (ESI) for Chemical Science.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_ar25
_database_code_depnum_ccdc_archive 'CCDC 2279862'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-06 deposited with the CCDC.	2024-05-24 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         '2(C90 H60 Fe N18), 3(F6 P), Cl, 4(C3 H6 O)'
_chemical_formula_sum            'C192 H144 Cl F18 Fe2 N36 O4 P3'
_chemical_formula_weight         3601.48

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0034 0.0017
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
H H 0.0000 0.0000
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
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'
P P 0.1071 0.1002
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Cl Cl 0.1549 0.1679
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'
Fe Fe 0.3511 0.8892
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

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

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

_cell_length_a                   26.5187(5)
_cell_length_b                   26.5187(5)
_cell_length_c                   26.5187(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18649.0(11)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9478
_cell_measurement_theta_min      2.490
_cell_measurement_theta_max      23.779

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_F_000             7424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.294
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.971
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.702
_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            307605
_diffrn_reflns_av_unetI/netI     0.0175
_diffrn_reflns_av_R_equivalents  0.0541
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.929
_diffrn_reflns_theta_max         24.201
_diffrn_reflns_theta_full        24.201
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9289
_reflns_number_gt                8821
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.863
_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       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;All non-hydrogens were refined anisotropically. 
 Hydrogens were placed geometrically on their carrier atom and refined with 
 a riding model, including those on the pyrazole N (AFIX 43). The PF6 anion
 is disordered over two positions with relative occupancies refining to
 0.599:0.401. Both were refined with 1,2 and 1,3 distance restraints as well
 as displacement parameters restraints. 
 At the end of the refinement there remained void spaces with only
 weak electron density peaks that could not be modelled as lattice solvent
 molecules (acetone or ether). Analysis with PLATON/SQUEEZE (see below) gave 
 a four voids of 510 cubic angstrom and four voids of 310 cubic angstroms
 per cell, with 90 and 53 electrons respectively. These figures would agree
 with respectively 2.5 and 1.5 diffuse acetone molecules per void, for a total
 of 16 per cell, 4 per formula unit. This agrees well with results from
 elemental analysis, and was therefore reflected in the reported formula,
 calculated density, mu etc. Refinement with the squeezed data resulted in an
 improvement in R1 of ca. 2%.

# SQUEEZE RESULTS (Version = 180518)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.609 -0.109  0.109       510        90 ' '
   2  0.891  0.109  0.609       510        90 ' '
   3  0.447  0.053  0.947         8         1 ' '
   4  0.290  0.210  0.790       310        53 ' '
   5  0.790  0.290  0.210       310        53 ' '
   6  0.391  0.391  0.391       510        90 ' '
   7  0.109  0.609 -0.109       510        90 ' '
   8  0.947  0.447  0.053         8         1 ' '
   9  0.553  0.553  0.553         8         1 ' '
  10  0.710  0.710  0.710       311        52 ' '
  11  0.210  0.790  0.290       310        53 ' '
  12  0.053  0.947  0.447         8         1 ' ',SQUEEZE
;

_vrf_PLAT027_ar25                
;
PROBLEM: _diffrn_reflns_theta_full value (too) Low ......      25.81 Degree      
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.85 angstrom resolution. Altogether resulting in relatively
poor values of theta_full, theta_max and data over parameter ratio. 
;

_vrf_THETM01_ar25                
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.575
            Calculated sin(theta_max)/wavelength =    0.5625      
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.85 angstrom resolution. Altogether resulting in relatively
poor values of theta_full, theta_max and data over parameter ratio. 
;

_vrf_PLAT090_ar25                
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       6.30 Note      
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.85 angstrom resolution. Altogether resulting in relatively
poor values of theta_full, theta_max and data over parameter ratio. 
;

_vrf_FORMU01_ar25                
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.      
RESPONSE: PLATON/SQUEEZE has been used to analyse and take into account
the diffuse solvent content, for a total of 4 acetone molecules per formula
unit. This has been reflected in the formula, giving rise to this
discrepancy between the formula from the atom list and that reported.
;


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1127P)²+4.4548P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 3956 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         9289
_refine_ls_number_parameters     791
_refine_ls_number_restraints     152
_refine_ls_R_factor_all          0.0526
_refine_ls_R_factor_gt           0.0503
_refine_ls_wR_factor_ref         0.1500
_refine_ls_wR_factor_gt          0.1469
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_restrained_S_all      1.115
_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 0.83056(2) 0.66944(2) 0.33056(2) 0.0395(3) Uani 1 3 d S T P . .
N1 N 0.85366(14) 0.75370(14) 0.32739(15) 0.0468(9) Uani 1 1 d . . . . .
N2 N 0.85171(12) 0.68922(12) 0.40604(13) 0.0384(7) Uani 1 1 d . . . . .
N3 N 0.85342(13) 0.66621(13) 0.45156(13) 0.0368(7) Uani 1 1 d D . . . .
H3B H 0.845(2) 0.6353(12) 0.457(2) 0.055 Uiso 1 1 d D U . . .
N4 N 0.92660(14) 0.53593(14) 0.58518(13) 0.0434(8) Uani 1 1 d . . . . .
H4B H 0.934619 0.544463 0.554131 0.052 Uiso 1 1 calc R U . . .
N5 N 0.93588(15) 0.49001(15) 0.60472(14) 0.0482(9) Uani 1 1 d . . . . .
N6 N 0.93058(17) 0.40508(19) 0.66458(17) 0.0648(12) Uani 1 1 d . . . . .
C1 C 0.85610(18) 0.78529(18) 0.2858(2) 0.0527(12) Uani 1 1 d . . . . .
C2 C 0.8379(2) 0.7703(2) 0.2394(2) 0.0623(13) Uani 1 1 d . . . . .
H2A H 0.823543 0.737610 0.235902 0.075 Uiso 1 1 calc R U . . .
C3 C 0.8401(3) 0.8017(2) 0.1983(2) 0.0747(17) Uani 1 1 d . . . . .
H3A H 0.827043 0.790817 0.166713 0.090 Uiso 1 1 calc R U . . .
C4 C 0.8610(3) 0.8488(3) 0.2026(3) 0.0813(18) Uani 1 1 d . . . . .
H4A H 0.862346 0.869995 0.173762 0.098 Uiso 1 1 calc R U . . .
C5 C 0.8800(3) 0.8663(2) 0.2473(3) 0.0749(17) Uani 1 1 d . . . . .
H5A H 0.894850 0.898815 0.249322 0.090 Uiso 1 1 calc R U . . .
C6 C 0.8772(2) 0.83501(19) 0.2905(2) 0.0592(13) Uani 1 1 d . . . . .
C7 C 0.8926(2) 0.85169(19) 0.3387(2) 0.0610(13) Uani 1 1 d . . . . .
H7A H 0.906253 0.884551 0.342969 0.073 Uiso 1 1 calc R U . . .
C8 C 0.88794(18) 0.82076(18) 0.3785(2) 0.0540(12) Uani 1 1 d . . . . .
H8A H 0.897446 0.831990 0.411130 0.065 Uiso 1 1 calc R U . . .
C9 C 0.86879(16) 0.77130(17) 0.37174(18) 0.0458(10) Uani 1 1 d . . . . .
C10 C 0.86559(16) 0.73703(16) 0.41452(16) 0.0411(9) Uani 1 1 d . . . . .
C11 C 0.87571(16) 0.74489(16) 0.46554(18) 0.0443(10) Uani 1 1 d . . . . .
H11A H 0.886376 0.775227 0.481331 0.053 Uiso 1 1 calc R U . . .
C12 C 0.86663(16) 0.69806(16) 0.48834(17) 0.0424(10) Uani 1 1 d . . . . .
C13 C 0.87070(17) 0.68295(17) 0.54100(18) 0.0464(10) Uani 1 1 d . . . . .
C14 C 0.8606(3) 0.7174(2) 0.5789(2) 0.0698(16) Uani 1 1 d . . . . .
H14A H 0.851652 0.751148 0.570790 0.084 Uiso 1 1 calc R U . . .
C15 C 0.8637(3) 0.7023(3) 0.6286(2) 0.091(2) Uani 1 1 d . . . . .
H15A H 0.856613 0.726063 0.654451 0.109 Uiso 1 1 calc R U . . .
C16 C 0.8769(3) 0.6538(2) 0.6419(2) 0.0705(16) Uani 1 1 d . . . . .
H16A H 0.878064 0.644092 0.676324 0.085 Uiso 1 1 calc R U . . .
C17 C 0.88846(18) 0.61917(18) 0.60390(17) 0.0495(11) Uani 1 1 d . . . . .
C18 C 0.88493(16) 0.63458(17) 0.55385(16) 0.0416(9) Uani 1 1 d . . . . .
H18A H 0.892522 0.611162 0.527829 0.050 Uiso 1 1 calc R U . . .
C19 C 0.90412(17) 0.56717(18) 0.61736(16) 0.0458(10) Uani 1 1 d . . . . .
C20 C 0.8978(2) 0.5406(2) 0.66129(17) 0.0566(12) Uani 1 1 d . . . . .
H20A H 0.882861 0.552224 0.691686 0.068 Uiso 1 1 calc R U . . .
C21 C 0.91796(18) 0.4933(2) 0.65200(17) 0.0517(11) Uani 1 1 d . . . . .
C22 C 0.91970(19) 0.4482(2) 0.68519(19) 0.0589(13) Uani 1 1 d . . . . .
C23 C 0.9107(3) 0.4545(3) 0.7377(2) 0.0829(19) Uani 1 1 d . . . . .
H23A H 0.903726 0.486800 0.751479 0.099 Uiso 1 1 calc R U . . .
C24 C 0.9124(3) 0.4124(4) 0.7678(2) 0.100(2) Uani 1 1 d . . . . .
H24A H 0.907432 0.415409 0.803156 0.120 Uiso 1 1 calc R U . . .
C25 C 0.9215(3) 0.3650(3) 0.7462(3) 0.084(2) Uani 1 1 d . . . . .
C26 C 0.9218(3) 0.3200(4) 0.7744(3) 0.109(3) Uani 1 1 d . . . . .
H26A H 0.916244 0.320715 0.809736 0.131 Uiso 1 1 calc R U . . .
C27 C 0.9302(3) 0.2744(4) 0.7499(4) 0.116(3) Uani 1 1 d . . . . .
H27A H 0.928567 0.243693 0.768309 0.139 Uiso 1 1 calc R U . . .
C28 C 0.9406(3) 0.2736(4) 0.7009(4) 0.117(3) Uani 1 1 d . . . . .
H28A H 0.947688 0.241992 0.685635 0.140 Uiso 1 1 calc R U . . .
C29 C 0.9417(3) 0.3159(3) 0.6710(3) 0.096(2) Uani 1 1 d . . . . .
H29A H 0.948513 0.313671 0.635922 0.115 Uiso 1 1 calc R U . . .
C30 C 0.9322(2) 0.3635(3) 0.6947(3) 0.0795(19) Uani 1 1 d . . . . .
Fe2 Fe 1.09501(2) 0.40499(2) 0.59501(2) 0.0621(4) Uani 1 3 d S T P . .
N7 N 1.1107(2) 0.32404(19) 0.56678(19) 0.0732(14) Uani 1 1 d . . . . .
N8 N 1.02442(16) 0.37944(15) 0.56614(15) 0.0526(10) Uani 1 1 d . . . . .
N9 N 0.97776(15) 0.39825(15) 0.55935(15) 0.0488(9) Uani 1 1 d D . . . .
H9A H 0.971(2) 0.4281(14) 0.571(2) 0.073 Uiso 1 1 d D U . . .
N10 N 0.83958(13) 0.52299(13) 0.48377(13) 0.0386(8) Uani 1 1 d . . . . .
H10A H 0.871572 0.518649 0.476105 0.046 Uiso 1 1 calc R U . . .
N11 N 0.81579(13) 0.56820(13) 0.48102(13) 0.0384(8) Uani 1 1 d . . . . .
N12 N 0.74860(14) 0.64555(15) 0.49255(14) 0.0467(9) Uani 1 1 d . . . . .
C31 C 1.1547(3) 0.2958(2) 0.5695(3) 0.0825(19) Uani 1 1 d . . . . .
C32 C 1.2008(3) 0.3175(3) 0.5815(5) 0.133(4) Uani 1 1 d . . . . .
H32A H 1.201989 0.353028 0.585983 0.159 Uiso 1 1 calc R U . . .
C33 C 1.2433(4) 0.2918(4) 0.5872(5) 0.146(5) Uani 1 1 d . . . . .
H33A H 1.273260 0.308251 0.597890 0.175 Uiso 1 1 calc R U . . .
C34 C 1.2434(4) 0.2418(4) 0.5774(4) 0.117(3) Uani 1 1 d . . . . .
H34A H 1.274153 0.223545 0.580206 0.141 Uiso 1 1 calc R U . . .
C35 C 1.2023(4) 0.2177(3) 0.5642(3) 0.104(3) Uani 1 1 d . . . . .
H35A H 1.203302 0.182426 0.557743 0.125 Uiso 1 1 calc R U . . .
C36 C 1.1552(3) 0.2452(3) 0.5594(3) 0.0836(19) Uani 1 1 d . . . . .
C37 C 1.1107(4) 0.2224(3) 0.5449(4) 0.111(3) Uani 1 1 d . . . . .
H37A H 1.110263 0.187250 0.538192 0.133 Uiso 1 1 calc R U . . .
C38 C 1.0667(3) 0.2499(2) 0.5402(3) 0.0810(18) Uani 1 1 d . . . . .
H38A H 1.036178 0.234601 0.529243 0.097 Uiso 1 1 calc R U . . .
C39 C 1.0690(3) 0.3013(2) 0.5521(2) 0.0656(15) Uani 1 1 d . . . . .
C40 C 1.0231(2) 0.33170(18) 0.54899(19) 0.0566(12) Uani 1 1 d . . . . .
C41 C 0.9753(2) 0.32039(18) 0.5320(2) 0.0602(13) Uani 1 1 d . . . . .
H41A H 0.964355 0.289156 0.518254 0.072 Uiso 1 1 calc R U . . .
C42 C 0.94611(19) 0.36330(17) 0.53879(19) 0.0508(11) Uani 1 1 d . . . . .
C43 C 0.89379(19) 0.37459(18) 0.52660(19) 0.0509(11) Uani 1 1 d . . . . .
C44 C 0.8591(2) 0.3348(2) 0.5207(2) 0.0650(14) Uani 1 1 d . . . . .
H44A H 0.869901 0.301006 0.525558 0.078 Uiso 1 1 calc R U . . .
C45 C 0.8104(2) 0.3445(2) 0.5082(3) 0.0720(16) Uani 1 1 d . . . . .
H45A H 0.787776 0.317078 0.503725 0.086 Uiso 1 1 calc R U . . .
C46 C 0.7927(2) 0.3940(2) 0.5017(2) 0.0619(13) Uani 1 1 d . . . . .
H46A H 0.758342 0.400377 0.493779 0.074 Uiso 1 1 calc R U . . .
C47 C 0.82688(17) 0.43330(17) 0.50717(16) 0.0447(10) Uani 1 1 d . . . . .
C48 C 0.87666(18) 0.42347(17) 0.51950(16) 0.0445(10) Uani 1 1 d . . . . .
H48A H 0.899548 0.450781 0.523179 0.053 Uiso 1 1 calc R U . . .
C49 C 0.80921(16) 0.48545(16) 0.49945(16) 0.0418(9) Uani 1 1 d . . . . .
C50 C 0.76281(16) 0.50732(17) 0.50760(16) 0.0439(10) Uani 1 1 d . . . . .
H50A H 0.732991 0.490891 0.518738 0.053 Uiso 1 1 calc R U . . .
C51 C 0.76832(15) 0.55845(17) 0.49623(15) 0.0416(9) Uani 1 1 d . . . . .
C52 C 0.73176(16) 0.59979(18) 0.50194(16) 0.0448(10) Uani 1 1 d . . . . .
C53 C 0.68137(18) 0.5892(2) 0.51638(19) 0.0547(12) Uani 1 1 d . . . . .
H53A H 0.670435 0.555464 0.521300 0.066 Uiso 1 1 calc R U . . .
C54 C 0.64938(19) 0.6280(2) 0.5229(2) 0.0610(14) Uani 1 1 d . . . . .
H54A H 0.615718 0.621643 0.533408 0.073 Uiso 1 1 calc R U . . .
C55 C 0.66514(19) 0.6779(2) 0.5145(2) 0.0600(13) Uani 1 1 d . . . . .
C56 C 0.6340(2) 0.7212(2) 0.5201(3) 0.0729(16) Uani 1 1 d . . . . .
H56A H 0.600355 0.717444 0.531745 0.087 Uiso 1 1 calc R U . . .
C57 C 0.6515(2) 0.7672(2) 0.5092(3) 0.0746(17) Uani 1 1 d . . . . .
H57A H 0.630145 0.795662 0.513204 0.090 Uiso 1 1 calc R U . . .
C58 C 0.7009(2) 0.7739(2) 0.4919(3) 0.0706(15) Uani 1 1 d . . . . .
H58A H 0.712250 0.806843 0.483580 0.085 Uiso 1 1 calc R U . . .
C59 C 0.7329(2) 0.73409(19) 0.4868(2) 0.0580(12) Uani 1 1 d . . . . .
H59A H 0.766463 0.739427 0.475546 0.070 Uiso 1 1 calc R U . . .
C60 C 0.71626(18) 0.6853(2) 0.49821(19) 0.0539(12) Uani 1 1 d . . . . .
Cl1 Cl 0.96317(4) 0.53683(4) 0.46317(4) 0.0359(4) Uani 1 3 d S T P . .
P1 P 0.62410(12) 0.43195(13) 0.49471(15) 0.0943(11) Uani 0.599(5) 1 d D U P A 1
F1 F 0.6489(3) 0.4599(3) 0.5374(3) 0.111(2) Uani 0.599(5) 1 d D U P A 1
F2 F 0.6506(6) 0.4688(6) 0.4561(3) 0.195(5) Uani 0.599(5) 1 d D U P A 1
F4 F 0.5949(5) 0.3962(5) 0.5312(5) 0.186(4) Uani 0.599(5) 1 d D U P A 1
F5 F 0.5839(5) 0.4707(5) 0.4939(7) 0.198(4) Uani 0.599(5) 1 d D U P A 1
F3 F 0.5963(6) 0.4049(5) 0.4499(5) 0.195(5) Uani 0.599(5) 1 d D U P A 1
F6 F 0.6675(5) 0.3966(6) 0.4928(8) 0.228(5) Uani 0.599(5) 1 d D U P A 1
P2 P 0.8174(5) 0.8721(5) 0.5973(5) 0.208(5) Uani 0.401(5) 1 d D U P A 2
F7 F 0.7732(7) 0.8974(7) 0.6270(8) 0.196(6) Uani 0.401(5) 1 d D U P A 2
F8 F 0.8542(9) 0.9110(11) 0.6243(11) 0.241(8) Uani 0.401(5) 1 d D U P A 2
F9 F 0.8283(9) 0.8359(8) 0.6406(7) 0.216(7) Uani 0.401(5) 1 d D U P A 2
F10 F 0.8155(11) 0.9169(11) 0.5574(10) 0.286(9) Uani 0.401(5) 1 d D U P A 2
F11 F 0.7829(11) 0.8383(8) 0.5656(10) 0.237(8) Uani 0.401(5) 1 d D U P A 2
F12 F 0.8653(13) 0.8518(13) 0.5658(12) 0.315(10) Uani 0.401(5) 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.144(4) 6_566 ?
Fe1 N2 2.144(4) 12_664 ?
Fe1 N2 2.144(4) . ?
Fe1 N1 2.319(4) 12_664 ?
Fe1 N1 2.319(4) 6_566 ?
Fe1 N1 2.319(4) . ?
N1 C9 1.327(6) . ?
N1 C1 1.386(6) . ?
N2 C10 1.339(6) . ?
N2 N3 1.353(5) . ?
N3 C12 1.337(6) . ?
N3 H3B 0.86(3) . ?
N4 C19 1.330(6) . ?
N4 N5 1.346(5) . ?
N4 H4B 0.8800 . ?
N5 C21 1.344(6) . ?
N6 C22 1.300(8) . ?
N6 C30 1.361(7) . ?
C1 C2 1.381(8) . ?
C1 C6 1.437(7) . ?
C2 C3 1.376(8) . ?
C2 H2A 0.9500 . ?
C3 C4 1.372(10) . ?
C3 H3A 0.9500 . ?
C4 C5 1.368(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.417(8) . ?
C5 H5A 0.9500 . ?
C6 C7 1.414(8) . ?
C7 C8 1.341(8) . ?
C7 H7A 0.9500 . ?
C8 C9 1.418(7) . ?
C8 H8A 0.9500 . ?
C9 C10 1.456(6) . ?
C10 C11 1.395(7) . ?
C11 C12 1.402(6) . ?
C11 H11A 0.9500 . ?
C12 C13 1.457(7) . ?
C13 C18 1.380(7) . ?
C13 C14 1.385(7) . ?
C14 C15 1.380(9) . ?
C14 H14A 0.9500 . ?
C15 C16 1.378(9) . ?
C15 H15A 0.9500 . ?
C16 C17 1.397(7) . ?
C16 H16A 0.9500 . ?
C17 C18 1.392(6) . ?
C17 C19 1.484(7) . ?
C18 H18A 0.9500 . ?
C19 C20 1.371(7) . ?
C20 C21 1.386(8) . ?
C20 H20A 0.9500 . ?
C21 C22 1.485(7) . ?
C22 C23 1.422(8) . ?
C23 C24 1.373(11) . ?
C23 H23A 0.9500 . ?
C24 C25 1.402(12) . ?
C24 H24A 0.9500 . ?
C25 C30 1.397(10) . ?
C25 C26 1.409(11) . ?
C26 C27 1.389(14) . ?
C26 H26A 0.9500 . ?
C27 C28 1.329(14) . ?
C27 H27A 0.9500 . ?
C28 C29 1.374(10) . ?
C28 H28A 0.9500 . ?
C29 C30 1.432(11) . ?
C29 H29A 0.9500 . ?
Fe2 N8 2.133(4) 6_566 ?
Fe2 N8 2.133(4) 12_664 ?
Fe2 N8 2.133(4) . ?
Fe2 N7 2.311(5) 12_664 ?
Fe2 N7 2.311(5) 6_566 ?
Fe2 N7 2.311(5) . ?
N7 C39 1.319(9) . ?
N7 C31 1.387(8) . ?
N8 C40 1.346(7) . ?
N8 N9 1.346(6) . ?
N9 C42 1.364(7) . ?
N9 H9A 0.87(3) . ?
N10 C49 1.346(6) . ?
N10 N11 1.357(5) . ?
N10 H10A 0.8800 . ?
N11 C51 1.347(5) . ?
N12 C52 1.317(6) . ?
N12 C60 1.366(6) . ?
C31 C36 1.368(10) . ?
C31 C32 1.389(12) . ?
C32 C33 1.326(11) . ?
C32 H32A 0.9500 . ?
C33 C34 1.351(14) . ?
C33 H33A 0.9500 . ?
C34 C35 1.312(13) . ?
C34 H34A 0.9500 . ?
C35 C36 1.452(11) . ?
C35 H35A 0.9500 . ?
C36 C37 1.381(13) . ?
C37 C38 1.381(11) . ?
C37 H37A 0.9500 . ?
C38 C39 1.400(9) . ?
C38 H38A 0.9500 . ?
C39 C40 1.464(8) . ?
C40 C41 1.378(8) . ?
C41 C42 1.388(7) . ?
C41 H41A 0.9500 . ?
C42 C43 1.456(7) . ?
C43 C48 1.386(7) . ?
C43 C44 1.407(7) . ?
C44 C45 1.358(9) . ?
C44 H44A 0.9500 . ?
C45 C46 1.405(8) . ?
C45 H45A 0.9500 . ?
C46 C47 1.389(7) . ?
C46 H46A 0.9500 . ?
C47 C48 1.385(7) . ?
C47 C49 1.475(6) . ?
C48 H48A 0.9500 . ?
C49 C50 1.377(6) . ?
C50 C51 1.397(7) . ?
C50 H50A 0.9500 . ?
C51 C52 1.471(6) . ?
C52 C53 1.418(7) . ?
C53 C54 1.345(8) . ?
C53 H53A 0.9500 . ?
C54 C55 1.404(8) . ?
C54 H54A 0.9500 . ?
C55 C56 1.423(8) . ?
C55 C60 1.436(7) . ?
C56 C57 1.336(9) . ?
C56 H56A 0.9500 . ?
C57 C58 1.398(9) . ?
C57 H57A 0.9500 . ?
C58 C59 1.362(8) . ?
C58 H58A 0.9500 . ?
C59 C60 1.401(7) . ?
C59 H59A 0.9500 . ?
P1 F5 1.481(11) . ?
P1 F6 1.486(11) . ?
P1 F1 1.505(8) . ?
P1 F4 1.560(10) . ?
P1 F3 1.571(10) . ?
P1 F2 1.579(10) . ?
P2 F9 1.525(18) . ?
P2 F11 1.534(18) . ?
P2 F7 1.565(18) . ?
P2 F8 1.590(19) . ?
P2 F10 1.59(2) . ?
P2 F12 1.61(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 92.76(13) 6_566 12_664 ?
N2 Fe1 N2 92.76(13) 6_566 . ?
N2 Fe1 N2 92.76(13) 12_664 . ?
N2 Fe1 N1 166.90(14) 6_566 12_664 ?
N2 Fe1 N1 74.27(13) 12_664 12_664 ?
N2 Fe1 N1 89.80(13) . 12_664 ?
N2 Fe1 N1 74.27(13) 6_566 6_566 ?
N2 Fe1 N1 89.80(13) 12_664 6_566 ?
N2 Fe1 N1 166.90(14) . 6_566 ?
N1 Fe1 N1 103.25(11) 12_664 6_566 ?
N2 Fe1 N1 89.80(13) 6_566 . ?
N2 Fe1 N1 166.90(13) 12_664 . ?
N2 Fe1 N1 74.27(13) . . ?
N1 Fe1 N1 103.25(11) 12_664 . ?
N1 Fe1 N1 103.25(11) 6_566 . ?
C9 N1 C1 118.5(4) . . ?
C9 N1 Fe1 112.7(3) . . ?
C1 N1 Fe1 128.6(3) . . ?
C10 N2 N3 105.5(3) . . ?
C10 N2 Fe1 117.4(3) . . ?
N3 N2 Fe1 137.0(3) . . ?
C12 N3 N2 112.0(3) . . ?
C12 N3 H3B 124(4) . . ?
N2 N3 H3B 124(4) . . ?
C19 N4 N5 113.5(4) . . ?
C19 N4 H4B 123.3 . . ?
N5 N4 H4B 123.3 . . ?
C21 N5 N4 103.7(4) . . ?
C22 N6 C30 118.2(5) . . ?
C2 C1 N1 121.2(4) . . ?
C2 C1 C6 118.6(5) . . ?
N1 C1 C6 120.3(5) . . ?
C3 C2 C1 121.2(6) . . ?
C3 C2 H2A 119.4 . . ?
C1 C2 H2A 119.4 . . ?
C4 C3 C2 120.1(6) . . ?
C4 C3 H3A 119.9 . . ?
C2 C3 H3A 119.9 . . ?
C5 C4 C3 122.0(6) . . ?
C5 C4 H4A 119.0 . . ?
C3 C4 H4A 119.0 . . ?
C4 C5 C6 118.9(6) . . ?
C4 C5 H5A 120.6 . . ?
C6 C5 H5A 120.6 . . ?
C7 C6 C5 122.2(5) . . ?
C7 C6 C1 118.6(5) . . ?
C5 C6 C1 119.2(5) . . ?
C8 C7 C6 119.5(5) . . ?
C8 C7 H7A 120.3 . . ?
C6 C7 H7A 120.3 . . ?
C7 C8 C9 120.0(5) . . ?
C7 C8 H8A 120.0 . . ?
C9 C8 H8A 120.0 . . ?
N1 C9 C8 123.0(4) . . ?
N1 C9 C10 116.9(4) . . ?
C8 C9 C10 120.0(4) . . ?
N2 C10 C11 110.9(4) . . ?
N2 C10 C9 118.4(4) . . ?
C11 C10 C9 130.6(4) . . ?
C10 C11 C12 104.6(4) . . ?
C10 C11 H11A 127.7 . . ?
C12 C11 H11A 127.7 . . ?
N3 C12 C11 106.9(4) . . ?
N3 C12 C13 123.0(4) . . ?
C11 C12 C13 130.1(4) . . ?
C18 C13 C14 119.2(5) . . ?
C18 C13 C12 120.8(4) . . ?
C14 C13 C12 120.0(4) . . ?
C15 C14 C13 119.3(5) . . ?
C15 C14 H14A 120.3 . . ?
C13 C14 H14A 120.3 . . ?
C16 C15 C14 122.0(5) . . ?
C16 C15 H15A 119.0 . . ?
C14 C15 H15A 119.0 . . ?
C15 C16 C17 119.0(5) . . ?
C15 C16 H16A 120.5 . . ?
C17 C16 H16A 120.5 . . ?
C18 C17 C16 118.6(5) . . ?
C18 C17 C19 121.4(4) . . ?
C16 C17 C19 120.0(4) . . ?
C13 C18 C17 121.8(4) . . ?
C13 C18 H18A 119.1 . . ?
C17 C18 H18A 119.1 . . ?
N4 C19 C20 106.2(4) . . ?
N4 C19 C17 123.4(4) . . ?
C20 C19 C17 130.4(4) . . ?
C19 C20 C21 105.5(4) . . ?
C19 C20 H20A 127.2 . . ?
C21 C20 H20A 127.2 . . ?
N5 C21 C20 111.1(4) . . ?
N5 C21 C22 119.3(5) . . ?
C20 C21 C22 129.5(4) . . ?
N6 C22 C23 123.5(5) . . ?
N6 C22 C21 117.8(4) . . ?
C23 C22 C21 118.7(6) . . ?
C24 C23 C22 118.0(7) . . ?
C24 C23 H23A 121.0 . . ?
C22 C23 H23A 121.0 . . ?
C23 C24 C25 119.8(6) . . ?
C23 C24 H24A 120.1 . . ?
C25 C24 H24A 120.1 . . ?
C30 C25 C24 117.3(6) . . ?
C30 C25 C26 119.6(8) . . ?
C24 C25 C26 123.0(7) . . ?
C27 C26 C25 119.5(8) . . ?
C27 C26 H26A 120.3 . . ?
C25 C26 H26A 120.3 . . ?
C28 C27 C26 120.2(8) . . ?
C28 C27 H27A 119.9 . . ?
C26 C27 H27A 119.9 . . ?
C27 C28 C29 123.8(10) . . ?
C27 C28 H28A 118.1 . . ?
C29 C28 H28A 118.1 . . ?
C28 C29 C30 117.6(8) . . ?
C28 C29 H29A 121.2 . . ?
C30 C29 H29A 121.2 . . ?
N6 C30 C25 123.0(7) . . ?
N6 C30 C29 117.6(6) . . ?
C25 C30 C29 119.3(6) . . ?
N8 Fe2 N8 94.47(14) 6_566 12_664 ?
N8 Fe2 N8 94.47(14) 6_566 . ?
N8 Fe2 N8 94.47(14) 12_664 . ?
N8 Fe2 N7 89.53(17) 6_566 12_664 ?
N8 Fe2 N7 75.35(18) 12_664 12_664 ?
N8 Fe2 N7 169.34(19) . 12_664 ?
N8 Fe2 N7 75.35(17) 6_566 6_566 ?
N8 Fe2 N7 169.34(19) 12_664 6_566 ?
N8 Fe2 N7 89.53(17) . 6_566 ?
N7 Fe2 N7 101.05(15) 12_664 6_566 ?
N8 Fe2 N7 169.34(19) 6_566 . ?
N8 Fe2 N7 89.53(17) 12_664 . ?
N8 Fe2 N7 75.35(18) . . ?
N7 Fe2 N7 101.05(15) 12_664 . ?
N7 Fe2 N7 101.05(15) 6_566 . ?
C39 N7 C31 118.2(5) . . ?
C39 N7 Fe2 111.7(4) . . ?
C31 N7 Fe2 129.5(5) . . ?
C40 N8 N9 106.2(4) . . ?
C40 N8 Fe2 116.3(3) . . ?
N9 N8 Fe2 137.5(3) . . ?
N8 N9 C42 111.5(4) . . ?
N8 N9 H9A 118(4) . . ?
C42 N9 H9A 130(4) . . ?
C49 N10 N11 113.1(3) . . ?
C49 N10 H10A 123.5 . . ?
N11 N10 H10A 123.5 . . ?
C51 N11 N10 104.4(3) . . ?
C52 N12 C60 118.5(4) . . ?
C36 C31 N7 121.8(7) . . ?
C36 C31 C32 116.2(6) . . ?
N7 C31 C32 121.9(6) . . ?
C33 C32 C31 124.1(9) . . ?
C33 C32 H32A 117.9 . . ?
C31 C32 H32A 117.9 . . ?
C32 C33 C34 119.0(10) . . ?
C32 C33 H33A 120.5 . . ?
C34 C33 H33A 120.5 . . ?
C35 C34 C33 121.8(8) . . ?
C35 C34 H34A 119.1 . . ?
C33 C34 H34A 119.1 . . ?
C34 C35 C36 119.5(7) . . ?
C34 C35 H35A 120.2 . . ?
C36 C35 H35A 120.2 . . ?
C31 C36 C37 118.3(6) . . ?
C31 C36 C35 119.0(8) . . ?
C37 C36 C35 122.6(7) . . ?
C38 C37 C36 121.1(7) . . ?
C38 C37 H37A 119.4 . . ?
C36 C37 H37A 119.4 . . ?
C37 C38 C39 117.1(8) . . ?
C37 C38 H38A 121.5 . . ?
C39 C38 H38A 121.5 . . ?
N7 C39 C38 123.4(6) . . ?
N7 C39 C40 117.5(5) . . ?
C38 C39 C40 119.1(6) . . ?
N8 C40 C41 109.9(4) . . ?
N8 C40 C39 118.5(5) . . ?
C41 C40 C39 131.6(5) . . ?
C40 C41 C42 106.9(5) . . ?
C40 C41 H41A 126.5 . . ?
C42 C41 H41A 126.5 . . ?
N9 C42 C41 105.4(4) . . ?
N9 C42 C43 122.4(4) . . ?
C41 C42 C43 132.1(5) . . ?
C48 C43 C44 118.1(5) . . ?
C48 C43 C42 122.3(4) . . ?
C44 C43 C42 119.5(4) . . ?
C45 C44 C43 120.5(5) . . ?
C45 C44 H44A 119.8 . . ?
C43 C44 H44A 119.8 . . ?
C44 C45 C46 121.6(5) . . ?
C44 C45 H45A 119.2 . . ?
C46 C45 H45A 119.2 . . ?
C47 C46 C45 118.0(5) . . ?
C47 C46 H46A 121.0 . . ?
C45 C46 H46A 121.0 . . ?
C48 C47 C46 120.4(4) . . ?
C48 C47 C49 120.8(4) . . ?
C46 C47 C49 118.8(4) . . ?
C47 C48 C43 121.4(4) . . ?
C47 C48 H48A 119.3 . . ?
C43 C48 H48A 119.3 . . ?
N10 C49 C50 105.8(4) . . ?
N10 C49 C47 123.1(4) . . ?
C50 C49 C47 131.1(4) . . ?
C49 C50 C51 106.3(4) . . ?
C49 C50 H50A 126.8 . . ?
C51 C50 H50A 126.8 . . ?
N11 C51 C50 110.4(4) . . ?
N11 C51 C52 120.3(4) . . ?
C50 C51 C52 129.2(4) . . ?
N12 C52 C53 123.6(4) . . ?
N12 C52 C51 116.3(4) . . ?
C53 C52 C51 120.1(4) . . ?
C54 C53 C52 118.6(5) . . ?
C54 C53 H53A 120.7 . . ?
C52 C53 H53A 120.7 . . ?
C53 C54 C55 120.8(5) . . ?
C53 C54 H54A 119.6 . . ?
C55 C54 H54A 119.6 . . ?
C54 C55 C56 124.9(5) . . ?
C54 C55 C60 117.2(4) . . ?
C56 C55 C60 117.9(5) . . ?
C57 C56 C55 120.9(5) . . ?
C57 C56 H56A 119.6 . . ?
C55 C56 H56A 119.6 . . ?
C56 C57 C58 120.8(5) . . ?
C56 C57 H57A 119.6 . . ?
C58 C57 H57A 119.6 . . ?
C59 C58 C57 121.2(6) . . ?
C59 C58 H58A 119.4 . . ?
C57 C58 H58A 119.4 . . ?
C58 C59 C60 120.0(5) . . ?
C58 C59 H59A 120.0 . . ?
C60 C59 H59A 120.0 . . ?
N12 C60 C59 119.4(4) . . ?
N12 C60 C55 121.4(5) . . ?
C59 C60 C55 119.2(5) . . ?
F5 P1 F6 174.5(11) . . ?
F5 P1 F1 89.1(8) . . ?
F6 P1 F1 89.9(7) . . ?
F5 P1 F4 94.2(9) . . ?
F6 P1 F4 91.3(11) . . ?
F1 P1 F4 92.8(5) . . ?
F5 P1 F3 88.1(9) . . ?
F6 P1 F3 92.9(9) . . ?
F1 P1 F3 177.2(8) . . ?
F4 P1 F3 87.6(7) . . ?
F5 P1 F2 83.2(10) . . ?
F6 P1 F2 91.3(11) . . ?
F1 P1 F2 89.4(5) . . ?
F4 P1 F2 176.5(8) . . ?
F3 P1 F2 90.1(7) . . ?
F9 P2 F11 99.0(15) . . ?
F9 P2 F7 91.8(10) . . ?
F11 P2 F7 94.5(15) . . ?
F9 P2 F8 87.3(16) . . ?
F11 P2 F8 173(2) . . ?
F7 P2 F8 87.4(14) . . ?
F9 P2 F10 167.7(17) . . ?
F11 P2 F10 93.1(16) . . ?
F7 P2 F10 89.5(10) . . ?
F8 P2 F10 80.5(17) . . ?
F9 P2 F12 91.8(10) . . ?
F11 P2 F12 90(2) . . ?
F7 P2 F12 174.1(17) . . ?
F8 P2 F12 88(2) . . ?
F10 P2 F12 86.0(10) . . ?

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 N11 0.86(3) 2.05(3) 2.892(5) 168(5) . yes
N9 H9A N5 0.87(3) 2.09(3) 2.933(6) 164(6) . yes
N4 H4B Cl1 0.88 2.54 3.378(3) 160.3 . yes
N10 H10A Cl1 0.88 2.50 3.343(3) 160.6 . yes

_refine_diff_density_max         0.494
_refine_diff_density_min         -0.240
_refine_diff_density_rms         0.061



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

data_lb2191
_database_code_depnum_ccdc_archive 'CCDC 2279863'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-06 deposited with the CCDC.	2024-05-24 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         '2(C90 H60 Fe N18), 3(F6 P), Br, 4(C3 H6 O)'
_chemical_formula_sum            'C192 H144 Br F18 Fe2 N36 O4 P3'
_chemical_formula_weight         3645.94

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'
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'
Br Br -0.4677 2.5495
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

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

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

_cell_length_a                   26.5373(7)
_cell_length_b                   26.5373(7)
_cell_length_c                   26.5373(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18688.3(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9946
_cell_measurement_theta_min      2.226
_cell_measurement_theta_max      24.284

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_F_000             7496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.110
_exptl_absorpt_coefficient_mu    0.505
_shelx_estimated_absorpt_T_min   0.888
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.678
_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            125109
_diffrn_reflns_av_unetI/netI     0.0590
_diffrn_reflns_av_R_equivalents  0.1008
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.760
_diffrn_reflns_theta_max         25.376
_diffrn_reflns_theta_full        25.376
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10649
_reflns_number_gt                9033
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_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       'Bruker APEX 3'
_computing_cell_refinement       'Bruker SAINT v8.40'
_computing_data_reduction        'Bruker SAINT v8.40'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;All non-hydrogens were refined anisotropically. 
 Hydrogens were placed geometrically on their carrier atom and refined with 
 a riding model, including those on the pyrazole N (AFIX 43). The PF6 anion
 is disordered over two positions with relative occupancies refining to
 0.571:0.429. Both were refined with 1,2 and 1,3 distance restraints as well
 as displacement parameters restraints. 
 At the end of the refinement there remained void spaces with only
 weak electron density peaks that could not be modelled as lattice solvent
 molecules (acetone or ether). Analysis with PLATON/SQUEEZE (see below) gave 
 four voids of 437 cubic angstrom and four voids of 317 cubic angstroms
 per cell, with 198 and 127 electrons respectively. Although high in
 terms of electron content, these figures could correspond to with 
 respectively 2.5 and 1.5 diffuse acetone molecules per void, for a total
 of 16 per cell, 4 per formula unit. This in line with results from
 elemental analysis, and was therefore reflected in the reported formula,
 calculated density, mu etc. Refinement with the squeezed data resulted in an
 improvement in R1 of ca. 2.5%.

# SQUEEZE RESULTS (Version = 301021)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
  _platon_squeeze_void_nr
  _platon_squeeze_void_average_x
  _platon_squeeze_void_average_y
  _platon_squeeze_void_average_z
  _platon_squeeze_void_volume
  _platon_squeeze_void_count_electrons
  _platon_squeeze_void_content
   1  0.386  0.114 -0.114       437       198 ' '
   2  0.114 -0.114  0.386       437       198 ' '
   3  0.902  0.016  0.389         9         1 ' '
   4  0.947  0.053  0.553         8         1 ' '
   5  0.111  0.098  0.516         9         2 ' '
   6  0.786  0.214  0.714       324       127 ' '
   7  0.516  0.111  0.098         9         2 ' '
   8  0.286  0.286  0.286       324       127 ' '
   9  0.886  0.386  0.114       437       198 ' '
  10  0.016  0.389  0.902         9         1 ' '
  11  0.610  0.405  0.485        10         2 ' '
  12  0.447  0.447  0.447         8         1 ' '
  13  0.614  0.615  0.615       436       198 ' '
  14  0.402  0.484  0.611         9         1 ' '
  15  0.098  0.516  0.111         9         2 ' '
  16  0.053  0.553  0.947         8         1 ' '
  17  0.889  0.598  0.984         9         1 ' '
  18  0.214  0.714  0.786       324       127 ' '
  19  0.484  0.611  0.402         9         1 ' '
  20  0.714  0.786  0.214       324       127 ' '
  21  0.984  0.889  0.598         9         1 ' '
  22  0.389  0.902  0.016         9         1 ' '
  23  0.553  0.947  0.053         8         1 ' '
  24  0.598  0.984  0.889         9         1 ' ',SQUEEZE
;

_vrf_FORMU01_lb2191              
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.      
RESPONSE: PLATON/SQUEEZE has been used to analyse and take into account
the diffuse solvent content, for a total of 4 acetone molecules per formula
unit. This has been reflected in the formula, giving rise to this
discrepancy between the formula from the atom list and that reported.
;

_vrf_PLAT090_lb2191              
;
PROBLEM: Poor Data / Parameter Ratio (Zmax > 18) ........       7.26 Note      
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.85 angstrom resolution. Altogether resulting in relatively
poor theta_max and data over parameter ratio. 
;

_vrf_THETM01_lb2191              
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.590
            Calculated sin(theta_max)/wavelength =    0.5880      
RESPONSE: Crystals were relatively poorly diffracting, probably a result of
a large portion of the cell contain diffuse lattice solvent. The present
data were cut at 0.85 angstrom resolution. Altogether resulting in relatively
poor theta_max and data over parameter ratio. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1544P)²+20.9710P] 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_abs_structure_details 
;
 Flack x determined using 3648 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         10649
_refine_ls_number_parameters     785
_refine_ls_number_restraints     240
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0742
_refine_ls_wR_factor_ref         0.2223
_refine_ls_wR_factor_gt          0.2073
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.105
_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
Br1 Br 0.03618(3) 0.46382(3) 0.53618(3) 0.0243(3) Uani 1 3 d S T P . .
Fe1 Fe 0.16864(4) 0.33136(4) 0.66864(4) 0.0268(4) Uani 1 3 d S T P . .
N1 N 0.1458(2) 0.2472(2) 0.6720(3) 0.0312(14) Uani 1 1 d . . . . .
N2 N 0.1481(2) 0.3119(2) 0.5927(2) 0.0279(14) Uani 1 1 d . . . . .
N3 N 0.1472(2) 0.3350(2) 0.5479(2) 0.0251(13) Uani 1 1 d . . . . .
H3B H 0.154510 0.366959 0.542910 0.030 Uiso 1 1 calc R U . . .
N4 N 0.0739(2) 0.4636(2) 0.4128(2) 0.0289(13) Uani 1 1 d . . . . .
H4B H 0.066058 0.455245 0.443903 0.035 Uiso 1 1 calc R U . . .
N5 N 0.0646(3) 0.5097(3) 0.3930(2) 0.0326(15) Uani 1 1 d . . . . .
N6 N 0.0700(3) 0.5931(3) 0.3335(3) 0.0412(17) Uani 1 1 d . . . . .
C1 C 0.1424(3) 0.2152(3) 0.7138(3) 0.0343(18) Uani 1 1 d . . . . .
C2 C 0.1622(4) 0.2305(3) 0.7602(3) 0.042(2) Uani 1 1 d . . . . .
H2A H 0.177398 0.262803 0.763099 0.050 Uiso 1 1 calc R U . . .
C3 C 0.1602(4) 0.1997(4) 0.8015(4) 0.054(3) Uani 1 1 d . . . . .
H3A H 0.173870 0.210437 0.832801 0.065 Uiso 1 1 calc R U . . .
C4 C 0.1372(4) 0.1511(4) 0.7971(4) 0.051(2) Uani 1 1 d . . . . .
H4A H 0.134798 0.129695 0.825681 0.061 Uiso 1 1 calc R U . . .
C5 C 0.1189(4) 0.1358(4) 0.7522(4) 0.054(3) Uani 1 1 d . . . . .
H5A H 0.103704 0.103513 0.749743 0.065 Uiso 1 1 calc R U . . .
C6 C 0.1215(3) 0.1660(3) 0.7091(4) 0.043(2) Uani 1 1 d . . . . .
C7 C 0.1054(4) 0.1488(4) 0.6604(4) 0.046(2) Uani 1 1 d . . . . .
H7A H 0.091576 0.116071 0.655896 0.055 Uiso 1 1 calc R U . . .
C8 C 0.1107(3) 0.1813(3) 0.6209(4) 0.0364(19) Uani 1 1 d . . . . .
H8A H 0.100590 0.170879 0.588149 0.044 Uiso 1 1 calc R U . . .
C9 C 0.1309(3) 0.2301(3) 0.6274(3) 0.0320(18) Uani 1 1 d . . . . .
C10 C 0.1338(3) 0.2638(3) 0.5845(3) 0.0273(16) Uani 1 1 d . . . . .
C11 C 0.1244(3) 0.2560(3) 0.5339(3) 0.0309(17) Uani 1 1 d . . . . .
H11A H 0.113974 0.225651 0.518146 0.037 Uiso 1 1 calc R U . . .
C12 C 0.1335(3) 0.3021(3) 0.5110(3) 0.0275(16) Uani 1 1 d . . . . .
C13 C 0.1304(3) 0.3170(3) 0.4581(3) 0.0287(16) Uani 1 1 d . . . . .
C14 C 0.1407(4) 0.2821(4) 0.4201(4) 0.048(2) Uani 1 1 d . . . . .
H14A H 0.150248 0.248712 0.428970 0.058 Uiso 1 1 calc R U . . .
C15 C 0.1373(5) 0.2952(4) 0.3704(4) 0.060(3) Uani 1 1 d . . . . .
H15A H 0.144489 0.271008 0.344949 0.072 Uiso 1 1 calc R U . . .
C16 C 0.1231(4) 0.3445(4) 0.3568(4) 0.050(2) Uani 1 1 d . . . . .
H16A H 0.121061 0.353698 0.322305 0.061 Uiso 1 1 calc R U . . .
C17 C 0.1121(3) 0.3800(3) 0.3941(3) 0.0313(17) Uani 1 1 d . . . . .
C18 C 0.1153(3) 0.3654(3) 0.4441(3) 0.0276(16) Uani 1 1 d . . . . .
H18A H 0.107022 0.389095 0.469641 0.033 Uiso 1 1 calc R U . . .
C19 C 0.0969(3) 0.4312(3) 0.3798(3) 0.0325(17) Uani 1 1 d . . . . .
C20 C 0.1029(3) 0.4584(3) 0.3363(3) 0.0356(18) Uani 1 1 d . . . . .
H20A H 0.117970 0.446946 0.305892 0.043 Uiso 1 1 calc R U . . .
C21 C 0.0827(3) 0.5056(3) 0.3451(3) 0.0353(19) Uani 1 1 d . . . . .
C22 C 0.0811(3) 0.5507(4) 0.3124(3) 0.039(2) Uani 1 1 d . . . . .
C23 C 0.0911(4) 0.5453(4) 0.2605(4) 0.056(3) Uani 1 1 d . . . . .
H23A H 0.099121 0.513087 0.247028 0.067 Uiso 1 1 calc R U . . .
C24 C 0.0893(5) 0.5863(5) 0.2299(4) 0.071(3) Uani 1 1 d . . . . .
H24A H 0.094217 0.583464 0.194562 0.085 Uiso 1 1 calc R U . . .
C25 C 0.0795(4) 0.6343(5) 0.2532(4) 0.061(3) Uani 1 1 d . . . . .
C26 C 0.0784(5) 0.6801(5) 0.2242(5) 0.074(4) Uani 1 1 d . . . . .
H26A H 0.082725 0.679148 0.188661 0.089 Uiso 1 1 calc R U . . .
C27 C 0.0712(6) 0.7233(6) 0.2475(6) 0.086(5) Uani 1 1 d . . . . .
H27A H 0.073800 0.753804 0.228895 0.103 Uiso 1 1 calc R U . . .
C28 C 0.0602(5) 0.7254(5) 0.2976(6) 0.076(4) Uani 1 1 d . . . . .
H28A H 0.052847 0.757004 0.312743 0.091 Uiso 1 1 calc R U . . .
C29 C 0.0596(4) 0.6823(4) 0.3269(5) 0.061(3) Uani 1 1 d . . . . .
H29A H 0.052557 0.683956 0.361962 0.073 Uiso 1 1 calc R U . . .
C30 C 0.0695(3) 0.6362(4) 0.3033(4) 0.051(3) Uani 1 1 d . . . . .
Fe2 Fe -0.09403(4) 0.59403(4) 0.40597(4) 0.0382(5) Uani 1 3 d S T P . .
N7 N -0.1099(3) 0.6750(3) 0.4346(3) 0.0468(19) Uani 1 1 d . . . . .
N8 N -0.0227(3) 0.6198(2) 0.4341(3) 0.0337(15) Uani 1 1 d . . . . .
N9 N 0.0238(3) 0.6007(2) 0.4400(2) 0.0332(15) Uani 1 1 d . . . . .
H9A H 0.032663 0.569884 0.431738 0.040 Uiso 1 1 calc R U . . .
N10 N 0.1622(2) 0.4776(2) 0.5159(2) 0.0278(14) Uani 1 1 d . . . . .
H10A H 0.130433 0.482244 0.524115 0.033 Uiso 1 1 calc R U . . .
N11 N 0.1853(2) 0.4322(2) 0.5179(2) 0.0265(13) Uani 1 1 d . . . . .
N12 N 0.2513(2) 0.3543(3) 0.5065(3) 0.0329(15) Uani 1 1 d . . . . .
C31 C -0.1530(4) 0.7033(4) 0.4314(4) 0.049(2) Uani 1 1 d . . . . .
C32 C -0.1978(4) 0.6802(5) 0.4170(6) 0.077(4) Uani 1 1 d . . . . .
H32A H -0.198484 0.645121 0.409744 0.092 Uiso 1 1 calc R U . . .
C33 C -0.2421(5) 0.7088(5) 0.4131(6) 0.081(4) Uani 1 1 d . . . . .
H33A H -0.272402 0.692872 0.402740 0.097 Uiso 1 1 calc R U . . .
C34 C -0.2427(5) 0.7589(5) 0.4239(6) 0.073(4) Uani 1 1 d . . . . .
H34A H -0.273539 0.777099 0.423108 0.088 Uiso 1 1 calc R U . . .
C35 C -0.1996(5) 0.7827(5) 0.4358(6) 0.077(4) Uani 1 1 d . . . . .
H35A H -0.199523 0.818315 0.439856 0.093 Uiso 1 1 calc R U . . .
C36 C -0.1534(4) 0.7549(4) 0.4424(5) 0.063(3) Uani 1 1 d . . . . .
C37 C -0.1080(5) 0.7761(4) 0.4573(5) 0.070(3) Uani 1 1 d . . . . .
H37A H -0.106751 0.810971 0.465050 0.085 Uiso 1 1 calc R U . . .
C38 C -0.0659(4) 0.7486(4) 0.4609(5) 0.061(3) Uani 1 1 d . . . . .
H38A H -0.035233 0.763828 0.471449 0.073 Uiso 1 1 calc R U . . .
C39 C -0.0674(4) 0.6987(4) 0.4492(3) 0.044(2) Uani 1 1 d . . . . .
C40 C -0.0211(3) 0.6677(3) 0.4514(3) 0.0328(18) Uani 1 1 d . . . . .
C41 C 0.0271(3) 0.6792(3) 0.4685(3) 0.040(2) Uani 1 1 d . . . . .
H41A H 0.038331 0.710202 0.482474 0.048 Uiso 1 1 calc R U . . .
C42 C 0.0555(3) 0.6357(3) 0.4608(3) 0.0358(18) Uani 1 1 d . . . . .
C43 C 0.1075(3) 0.6255(3) 0.4734(3) 0.0320(18) Uani 1 1 d . . . . .
C44 C 0.1413(3) 0.6652(3) 0.4796(4) 0.042(2) Uani 1 1 d . . . . .
H44A H 0.130189 0.698939 0.475200 0.050 Uiso 1 1 calc R U . . .
C45 C 0.1903(4) 0.6559(3) 0.4920(4) 0.050(2) Uani 1 1 d . . . . .
H45A H 0.212797 0.683479 0.495847 0.060 Uiso 1 1 calc R U . . .
C46 C 0.2083(3) 0.6067(3) 0.4991(4) 0.041(2) Uani 1 1 d . . . . .
H46A H 0.242418 0.600750 0.508162 0.050 Uiso 1 1 calc R U . . .
C47 C 0.1747(3) 0.5667(3) 0.4925(3) 0.0315(17) Uani 1 1 d . . . . .
C48 C 0.1254(3) 0.5764(3) 0.4798(3) 0.0315(18) Uani 1 1 d . . . . .
H48A H 0.102881 0.548968 0.475205 0.038 Uiso 1 1 calc R U . . .
C49 C 0.1928(3) 0.5152(3) 0.5001(3) 0.0296(17) Uani 1 1 d . . . . .
C50 C 0.2392(3) 0.4930(3) 0.4919(3) 0.0296(17) Uani 1 1 d . . . . .
H50A H 0.269221 0.509209 0.481037 0.036 Uiso 1 1 calc R U . . .
C51 C 0.2327(3) 0.4414(3) 0.5030(3) 0.0266(16) Uani 1 1 d . . . . .
C52 C 0.2687(3) 0.4003(3) 0.4972(3) 0.0266(16) Uani 1 1 d . . . . .
C53 C 0.3199(3) 0.4098(3) 0.4816(3) 0.0362(19) Uani 1 1 d . . . . .
H53A H 0.331109 0.443360 0.476264 0.043 Uiso 1 1 calc R U . . .
C54 C 0.3514(3) 0.3712(4) 0.4749(3) 0.040(2) Uani 1 1 d . . . . .
H54A H 0.385159 0.376868 0.464414 0.048 Uiso 1 1 calc R U . . .
C55 C 0.3338(3) 0.3218(3) 0.4835(3) 0.0376(19) Uani 1 1 d . . . . .
C56 C 0.3644(3) 0.2774(4) 0.4773(4) 0.050(3) Uani 1 1 d . . . . .
H56A H 0.397580 0.281069 0.464426 0.060 Uiso 1 1 calc R U . . .
C57 C 0.3477(4) 0.2311(4) 0.4888(4) 0.051(2) Uani 1 1 d . . . . .
H57A H 0.369099 0.202645 0.485236 0.062 Uiso 1 1 calc R U . . .
C58 C 0.2981(3) 0.2252(4) 0.5064(4) 0.052(2) Uani 1 1 d . . . . .
H58A H 0.286404 0.192543 0.515107 0.062 Uiso 1 1 calc R U . . .
C59 C 0.2663(3) 0.2652(3) 0.5112(4) 0.043(2) Uani 1 1 d . . . . .
H59A H 0.232505 0.260315 0.521904 0.052 Uiso 1 1 calc R U . . .
C60 C 0.2845(3) 0.3145(3) 0.4999(3) 0.0358(19) Uani 1 1 d . . . . .
P1 P 0.3759(3) 0.5669(3) 0.5028(3) 0.103(2) Uani 0.607(6) 1 d D U P A 1
F1 F 0.3560(5) 0.5364(5) 0.4605(4) 0.115(5) Uani 0.607(6) 1 d D U P A 1
F2 F 0.3485(7) 0.5303(7) 0.5414(5) 0.154(6) Uani 0.607(6) 1 d D U P A 1
F4 F 0.4073(7) 0.6018(6) 0.4691(7) 0.181(7) Uani 0.607(6) 1 d D U P A 1
F5 F 0.4224(6) 0.5309(7) 0.5073(8) 0.189(7) Uani 0.607(6) 1 d D U P A 1
F3 F 0.3995(8) 0.5955(7) 0.5496(7) 0.198(8) Uani 0.607(6) 1 d D U P A 1
F6 F 0.3319(6) 0.6007(6) 0.5024(8) 0.182(7) Uani 0.607(6) 1 d D U P A 1
P2 P 0.1760(6) 0.0970(7) 0.4006(8) 0.206(7) Uani 0.393(6) 1 d D U P A 2
F7 F 0.2213(5) 0.0583(6) 0.3902(6) 0.074(4) Uani 0.393(6) 1 d D U P A 2
F8 F 0.1584(10) 0.0929(13) 0.3463(10) 0.229(11) Uani 0.393(6) 1 d D U P A 2
F9 F 0.2096(11) 0.1415(8) 0.3876(15) 0.231(11) Uani 0.393(6) 1 d D U P A 2
F10 F 0.1395(6) 0.0535(10) 0.4140(12) 0.184(9) Uani 0.393(6) 1 d D U P A 2
F11 F 0.1904(10) 0.0996(13) 0.4555(9) 0.211(10) Uani 0.393(6) 1 d D U P A 2
F12 F 0.1311(11) 0.1356(12) 0.4115(15) 0.306(14) Uani 0.393(6) 1 d D U P A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N2 2.150(6) . ?
Fe1 N2 2.150(6) 12_565 ?
Fe1 N2 2.150(6) 6_456 ?
Fe1 N1 2.316(7) 6_456 ?
Fe1 N1 2.316(7) 12_565 ?
Fe1 N1 2.316(7) . ?
N1 C9 1.327(11) . ?
N1 C1 1.401(10) . ?
N2 N3 1.339(9) . ?
N2 C10 1.352(10) . ?
N3 C12 1.360(10) . ?
N3 H3B 0.8800 . ?
N4 N5 1.354(10) . ?
N4 C19 1.370(10) . ?
N4 H4B 0.8800 . ?
N5 C21 1.362(11) . ?
N6 C22 1.292(12) . ?
N6 C30 1.397(11) . ?
C1 C2 1.399(13) . ?
C1 C6 1.423(13) . ?
C2 C3 1.368(13) . ?
C2 H2A 0.9500 . ?
C3 C4 1.431(15) . ?
C3 H3A 0.9500 . ?
C4 C5 1.350(15) . ?
C4 H4A 0.9500 . ?
C5 C6 1.397(14) . ?
C5 H5A 0.9500 . ?
C6 C7 1.436(14) . ?
C7 C8 1.367(13) . ?
C7 H7A 0.9500 . ?
C8 C9 1.411(12) . ?
C8 H8A 0.9500 . ?
C9 C10 1.450(11) . ?
C10 C11 1.380(12) . ?
C11 C12 1.387(11) . ?
C11 H11A 0.9500 . ?
C12 C13 1.459(11) . ?
C13 C18 1.396(11) . ?
C13 C14 1.396(12) . ?
C14 C15 1.369(14) . ?
C14 H14A 0.9500 . ?
C15 C16 1.409(15) . ?
C15 H15A 0.9500 . ?
C16 C17 1.396(12) . ?
C16 H16A 0.9500 . ?
C17 C18 1.385(11) . ?
C17 C19 1.467(12) . ?
C18 H18A 0.9500 . ?
C19 C20 1.370(12) . ?
C20 C21 1.384(13) . ?
C20 H20A 0.9500 . ?
C21 C22 1.478(12) . ?
C22 C23 1.409(13) . ?
C23 C24 1.361(16) . ?
C23 H23A 0.9500 . ?
C24 C25 1.438(19) . ?
C24 H24A 0.9500 . ?
C25 C30 1.358(16) . ?
C25 C26 1.440(15) . ?
C26 C27 1.32(2) . ?
C26 H26A 0.9500 . ?
C27 C28 1.36(2) . ?
C27 H27A 0.9500 . ?
C28 C29 1.382(15) . ?
C28 H28A 0.9500 . ?
C29 C30 1.399(16) . ?
C29 H29A 0.9500 . ?
Fe2 N8 2.146(7) . ?
Fe2 N8 2.146(7) 6_456 ?
Fe2 N8 2.146(7) 12_565 ?
Fe2 N7 2.317(8) 12_565 ?
Fe2 N7 2.317(8) 6_456 ?
Fe2 N7 2.317(8) . ?
N7 C39 1.349(13) . ?
N7 C31 1.370(11) . ?
N8 N9 1.342(10) . ?
N8 C40 1.353(11) . ?
N9 C42 1.368(11) . ?
N9 H9A 0.8800 . ?
N10 C49 1.351(10) . ?
N10 N11 1.353(9) . ?
N10 H10A 0.8800 . ?
N11 C51 1.341(10) . ?
N12 C52 1.329(10) . ?
N12 C60 1.386(10) . ?
C31 C32 1.393(16) . ?
C31 C36 1.402(15) . ?
C32 C33 1.403(15) . ?
C32 H32A 0.9500 . ?
C33 C34 1.360(18) . ?
C33 H33A 0.9500 . ?
C34 C35 1.345(19) . ?
C34 H34A 0.9500 . ?
C35 C36 1.440(16) . ?
C35 H35A 0.9500 . ?
C36 C37 1.386(17) . ?
C37 C38 1.337(16) . ?
C37 H37A 0.9500 . ?
C38 C39 1.362(14) . ?
C38 H38A 0.9500 . ?
C39 C40 1.480(12) . ?
C40 C41 1.392(13) . ?
C41 C42 1.394(12) . ?
C41 H41A 0.9500 . ?
C42 C43 1.446(12) . ?
C43 C44 1.393(12) . ?
C43 C48 1.397(11) . ?
C44 C45 1.362(14) . ?
C44 H44A 0.9500 . ?
C45 C46 1.404(13) . ?
C45 H45A 0.9500 . ?
C46 C47 1.396(12) . ?
C46 H46A 0.9500 . ?
C47 C48 1.377(12) . ?
C47 C49 1.464(11) . ?
C48 H48A 0.9500 . ?
C49 C50 1.382(11) . ?
C50 C51 1.412(11) . ?
C50 H50A 0.9500 . ?
C51 C52 1.456(11) . ?
C52 C53 1.441(11) . ?
C53 C54 1.336(12) . ?
C53 H53A 0.9500 . ?
C54 C55 1.408(13) . ?
C54 H54A 0.9500 . ?
C55 C60 1.393(12) . ?
C55 C56 1.439(12) . ?
C56 C57 1.343(14) . ?
C56 H56A 0.9500 . ?
C57 C58 1.404(14) . ?
C57 H57A 0.9500 . ?
C58 C59 1.360(13) . ?
C58 H58A 0.9500 . ?
C59 C60 1.427(12) . ?
C59 H59A 0.9500 . ?
P1 F6 1.469(15) . ?
P1 F1 1.484(12) . ?
P1 F4 1.534(14) . ?
P1 F5 1.566(16) . ?
P1 F3 1.584(14) . ?
P1 F2 1.588(13) . ?
P2 F11 1.508(18) . ?
P2 F9 1.518(18) . ?
P2 F8 1.519(18) . ?
P2 F10 1.548(18) . ?
P2 F12 1.595(17) . ?
P2 F7 1.607(16) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 92.8(2) . 12_565 ?
N2 Fe1 N2 92.8(2) . 6_456 ?
N2 Fe1 N2 92.8(2) 12_565 6_456 ?
N2 Fe1 N1 167.5(2) . 6_456 ?
N2 Fe1 N1 89.4(2) 12_565 6_456 ?
N2 Fe1 N1 74.8(2) 6_456 6_456 ?
N2 Fe1 N1 89.4(2) . 12_565 ?
N2 Fe1 N1 74.8(2) 12_565 12_565 ?
N2 Fe1 N1 167.5(2) 6_456 12_565 ?
N1 Fe1 N1 103.1(2) 6_456 12_565 ?
N2 Fe1 N1 74.8(2) . . ?
N2 Fe1 N1 167.5(2) 12_565 . ?
N2 Fe1 N1 89.4(2) 6_456 . ?
N1 Fe1 N1 103.0(2) 6_456 . ?
N1 Fe1 N1 103.1(2) 12_565 . ?
C9 N1 C1 118.7(7) . . ?
C9 N1 Fe1 112.0(5) . . ?
C1 N1 Fe1 129.1(5) . . ?
N3 N2 C10 106.4(6) . . ?
N3 N2 Fe1 136.7(5) . . ?
C10 N2 Fe1 116.8(5) . . ?
N2 N3 C12 110.6(6) . . ?
N2 N3 H3B 124.7 . . ?
C12 N3 H3B 124.7 . . ?
N5 N4 C19 113.5(6) . . ?
N5 N4 H4B 123.2 . . ?
C19 N4 H4B 123.2 . . ?
N4 N5 C21 103.1(7) . . ?
C22 N6 C30 117.9(8) . . ?
C2 C1 N1 119.9(7) . . ?
C2 C1 C6 119.3(8) . . ?
N1 C1 C6 120.7(8) . . ?
C3 C2 C1 121.1(9) . . ?
C3 C2 H2A 119.5 . . ?
C1 C2 H2A 119.5 . . ?
C2 C3 C4 119.3(10) . . ?
C2 C3 H3A 120.3 . . ?
C4 C3 H3A 120.3 . . ?
C5 C4 C3 119.8(9) . . ?
C5 C4 H4A 120.1 . . ?
C3 C4 H4A 120.1 . . ?
C4 C5 C6 122.2(9) . . ?
C4 C5 H5A 118.9 . . ?
C6 C5 H5A 118.9 . . ?
C5 C6 C1 118.2(9) . . ?
C5 C6 C7 122.6(9) . . ?
C1 C6 C7 119.2(8) . . ?
C8 C7 C6 117.3(8) . . ?
C8 C7 H7A 121.3 . . ?
C6 C7 H7A 121.3 . . ?
C7 C8 C9 121.6(9) . . ?
C7 C8 H8A 119.2 . . ?
C9 C8 H8A 119.2 . . ?
N1 C9 C8 122.4(8) . . ?
N1 C9 C10 118.3(7) . . ?
C8 C9 C10 119.2(8) . . ?
N2 C10 C11 110.4(7) . . ?
N2 C10 C9 118.0(7) . . ?
C11 C10 C9 131.6(7) . . ?
C10 C11 C12 105.3(7) . . ?
C10 C11 H11A 127.3 . . ?
C12 C11 H11A 127.3 . . ?
N3 C12 C11 107.2(7) . . ?
N3 C12 C13 122.2(7) . . ?
C11 C12 C13 130.6(7) . . ?
C18 C13 C14 118.4(7) . . ?
C18 C13 C12 121.4(7) . . ?
C14 C13 C12 120.2(7) . . ?
C15 C14 C13 121.0(9) . . ?
C15 C14 H14A 119.5 . . ?
C13 C14 H14A 119.5 . . ?
C14 C15 C16 120.0(9) . . ?
C14 C15 H15A 120.0 . . ?
C16 C15 H15A 120.0 . . ?
C17 C16 C15 120.2(8) . . ?
C17 C16 H16A 119.9 . . ?
C15 C16 H16A 119.9 . . ?
C18 C17 C16 118.5(8) . . ?
C18 C17 C19 121.6(7) . . ?
C16 C17 C19 119.9(7) . . ?
C17 C18 C13 122.0(7) . . ?
C17 C18 H18A 119.0 . . ?
C13 C18 H18A 119.0 . . ?
N4 C19 C20 105.1(7) . . ?
N4 C19 C17 122.5(7) . . ?
C20 C19 C17 132.4(7) . . ?
C19 C20 C21 106.8(7) . . ?
C19 C20 H20A 126.6 . . ?
C21 C20 H20A 126.6 . . ?
N5 C21 C20 111.4(7) . . ?
N5 C21 C22 118.3(8) . . ?
C20 C21 C22 130.1(8) . . ?
N6 C22 C23 123.8(9) . . ?
N6 C22 C21 117.1(8) . . ?
C23 C22 C21 119.1(9) . . ?
C24 C23 C22 119.7(11) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C25 117.3(10) . . ?
C23 C24 H24A 121.4 . . ?
C25 C24 H24A 121.4 . . ?
C30 C25 C24 119.4(10) . . ?
C30 C25 C26 119.2(12) . . ?
C24 C25 C26 121.4(11) . . ?
C27 C26 C25 119.2(12) . . ?
C27 C26 H26A 120.4 . . ?
C25 C26 H26A 120.4 . . ?
C26 C27 C28 121.6(12) . . ?
C26 C27 H27A 119.2 . . ?
C28 C27 H27A 119.2 . . ?
C27 C28 C29 121.2(14) . . ?
C27 C28 H28A 119.4 . . ?
C29 C28 H28A 119.4 . . ?
C28 C29 C30 118.0(12) . . ?
C28 C29 H29A 121.0 . . ?
C30 C29 H29A 121.0 . . ?
C25 C30 N6 121.9(11) . . ?
C25 C30 C29 120.6(9) . . ?
N6 C30 C29 117.5(9) . . ?
N8 Fe2 N8 94.9(2) . 6_456 ?
N8 Fe2 N8 94.9(2) . 12_565 ?
N8 Fe2 N8 94.9(2) 6_456 12_565 ?
N8 Fe2 N7 170.2(3) . 12_565 ?
N8 Fe2 N7 88.5(3) 6_456 12_565 ?
N8 Fe2 N7 75.6(3) 12_565 12_565 ?
N8 Fe2 N7 88.5(3) . 6_456 ?
N8 Fe2 N7 75.6(3) 6_456 6_456 ?
N8 Fe2 N7 170.2(3) 12_565 6_456 ?
N7 Fe2 N7 101.2(2) 12_565 6_456 ?
N8 Fe2 N7 75.6(3) . . ?
N8 Fe2 N7 170.2(3) 6_456 . ?
N8 Fe2 N7 88.5(3) 12_565 . ?
N7 Fe2 N7 101.2(2) 12_565 . ?
N7 Fe2 N7 101.2(2) 6_456 . ?
C39 N7 C31 117.4(8) . . ?
C39 N7 Fe2 112.0(6) . . ?
C31 N7 Fe2 129.8(7) . . ?
N9 N8 C40 106.5(7) . . ?
N9 N8 Fe2 137.1(5) . . ?
C40 N8 Fe2 116.4(5) . . ?
N8 N9 C42 111.0(7) . . ?
N8 N9 H9A 124.5 . . ?
C42 N9 H9A 124.5 . . ?
C49 N10 N11 113.4(6) . . ?
C49 N10 H10A 123.3 . . ?
N11 N10 H10A 123.3 . . ?
C51 N11 N10 104.6(6) . . ?
C52 N12 C60 117.1(7) . . ?
N7 C31 C32 119.2(9) . . ?
N7 C31 C36 122.0(10) . . ?
C32 C31 C36 118.7(9) . . ?
C31 C32 C33 119.8(11) . . ?
C31 C32 H32A 120.1 . . ?
C33 C32 H32A 120.1 . . ?
C34 C33 C32 121.6(13) . . ?
C34 C33 H33A 119.2 . . ?
C32 C33 H33A 119.2 . . ?
C35 C34 C33 119.9(11) . . ?
C35 C34 H34A 120.0 . . ?
C33 C34 H34A 120.0 . . ?
C34 C35 C36 120.8(11) . . ?
C34 C35 H35A 119.6 . . ?
C36 C35 H35A 119.6 . . ?
C37 C36 C31 116.6(10) . . ?
C37 C36 C35 124.5(10) . . ?
C31 C36 C35 118.9(11) . . ?
C38 C37 C36 121.8(10) . . ?
C38 C37 H37A 119.1 . . ?
C36 C37 H37A 119.1 . . ?
C37 C38 C39 119.2(11) . . ?
C37 C38 H38A 120.4 . . ?
C39 C38 H38A 120.4 . . ?
N7 C39 C38 123.0(9) . . ?
N7 C39 C40 116.5(8) . . ?
C38 C39 C40 120.5(10) . . ?
N8 C40 C41 110.3(7) . . ?
N8 C40 C39 118.9(8) . . ?
C41 C40 C39 130.8(8) . . ?
C40 C41 C42 105.5(8) . . ?
C40 C41 H41A 127.3 . . ?
C42 C41 H41A 127.3 . . ?
N9 C42 C41 106.8(8) . . ?
N9 C42 C43 123.7(7) . . ?
C41 C42 C43 129.5(8) . . ?
C44 C43 C48 118.2(8) . . ?
C44 C43 C42 120.1(7) . . ?
C48 C43 C42 121.7(7) . . ?
C45 C44 C43 120.4(8) . . ?
C45 C44 H44A 119.8 . . ?
C43 C44 H44A 119.8 . . ?
C44 C45 C46 121.7(8) . . ?
C44 C45 H45A 119.1 . . ?
C46 C45 H45A 119.1 . . ?
C47 C46 C45 118.2(8) . . ?
C47 C46 H46A 120.9 . . ?
C45 C46 H46A 120.9 . . ?
C48 C47 C46 119.7(8) . . ?
C48 C47 C49 121.3(7) . . ?
C46 C47 C49 119.0(7) . . ?
C47 C48 C43 121.8(8) . . ?
C47 C48 H48A 119.1 . . ?
C43 C48 H48A 119.1 . . ?
N10 C49 C50 105.7(7) . . ?
N10 C49 C47 122.4(7) . . ?
C50 C49 C47 131.8(7) . . ?
C49 C50 C51 105.8(7) . . ?
C49 C50 H50A 127.1 . . ?
C51 C50 H50A 127.1 . . ?
N11 C51 C50 110.6(7) . . ?
N11 C51 C52 120.7(7) . . ?
C50 C51 C52 128.6(7) . . ?
N12 C52 C53 122.7(7) . . ?
N12 C52 C51 116.1(6) . . ?
C53 C52 C51 121.2(7) . . ?
C54 C53 C52 119.7(8) . . ?
C54 C53 H53A 120.2 . . ?
C52 C53 H53A 120.2 . . ?
C53 C54 C55 119.0(8) . . ?
C53 C54 H54A 120.5 . . ?
C55 C54 H54A 120.5 . . ?
C60 C55 C54 119.4(8) . . ?
C60 C55 C56 116.8(8) . . ?
C54 C55 C56 123.8(8) . . ?
C57 C56 C55 122.5(8) . . ?
C57 C56 H56A 118.7 . . ?
C55 C56 H56A 118.7 . . ?
C56 C57 C58 119.1(9) . . ?
C56 C57 H57A 120.5 . . ?
C58 C57 H57A 120.5 . . ?
C59 C58 C57 121.7(9) . . ?
C59 C58 H58A 119.1 . . ?
C57 C58 H58A 119.1 . . ?
C58 C59 C60 119.1(8) . . ?
C58 C59 H59A 120.5 . . ?
C60 C59 H59A 120.5 . . ?
N12 C60 C55 122.1(8) . . ?
N12 C60 C59 117.2(7) . . ?
C55 C60 C59 120.7(7) . . ?
F6 P1 F1 92.6(9) . . ?
F6 P1 F4 93.4(9) . . ?
F1 P1 F4 94.7(8) . . ?
F6 P1 F5 176.1(11) . . ?
F1 P1 F5 90.2(9) . . ?
F4 P1 F5 89.1(9) . . ?
F6 P1 F3 91.7(9) . . ?
F1 P1 F3 175.1(11) . . ?
F4 P1 F3 87.3(8) . . ?
F5 P1 F3 85.4(9) . . ?
F6 P1 F2 90.9(9) . . ?
F1 P1 F2 89.5(7) . . ?
F4 P1 F2 173.8(10) . . ?
F5 P1 F2 86.4(9) . . ?
F3 P1 F2 88.2(8) . . ?
F11 P2 F9 92.1(11) . . ?
F11 P2 F8 176.5(13) . . ?
F9 P2 F8 91.1(11) . . ?
F11 P2 F10 88.3(11) . . ?
F9 P2 F10 177.2(12) . . ?
F8 P2 F10 88.4(11) . . ?
F11 P2 F12 89.2(11) . . ?
F9 P2 F12 88.9(11) . . ?
F8 P2 F12 89.3(10) . . ?
F10 P2 F12 88.3(10) . . ?
F11 P2 F7 90.3(10) . . ?
F9 P2 F7 91.0(10) . . ?
F8 P2 F7 91.1(10) . . ?
F10 P2 F7 91.7(10) . . ?
F12 P2 F7 179.5(14) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N3 H3B N11 0.88 2.03 2.883(9) 164.0 . yes
N9 H9A N5 0.88 2.08 2.929(10) 161.3 . yes
N4 H4B Br1 0.88 2.58 3.424(6) 160.0 . yes
N10 H10A Br1 0.88 2.57 3.408(6) 159.7 . yes

_refine_diff_density_max         1.434
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.105



####################################################################### 
# 
# 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_ar34
_database_code_depnum_ccdc_archive 'CCDC 2279864'
loop_
_audit_author_name
_audit_author_address
'Olivier Roubeau'
;Instituto de Nanociencia y Materiales de Aragon (INMA), CSIC and Universidad de Zaragoza
Spain
;
_audit_update_record             
;
2023-07-06 deposited with the CCDC.	2024-05-24 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         
'2(C90 H60 Fe N18), 2.611(F6 P), (I), 0.389(I3), H2 O, 5 (C3 H6 O)'
_chemical_formula_sum            'C195 H152 F15.66 Fe2 I2.17 N36 O6 P2.61'
_chemical_formula_weight         3878.72

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'
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'
I I -0.3982 1.9061
'XDisp Program in WinGX L.J. Farrugia, J.Appl.Cryst. 2012,45,849-854'

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

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

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

_cell_length_a                   26.532(3)
_cell_length_b                   26.532(3)
_cell_length_c                   26.532(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     18677(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12011
_cell_measurement_theta_min      1.11
_cell_measurement_theta_max      34.18

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.379
_exptl_crystal_F_000             7857
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    0.703
_shelx_estimated_absorpt_T_min   0.968
_shelx_estimated_absorpt_T_max   0.984
_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_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            347834
_diffrn_reflns_av_unetI/netI     0.0305
_diffrn_reflns_av_R_equivalents  0.1011
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_k_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         1.114
_diffrn_reflns_theta_max         30.899
_diffrn_reflns_theta_full        30.899
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             18241
_reflns_number_gt                17922
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.889
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    1.000

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 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       'Global Phasing autoPROC package'
_computing_data_reduction        
;
autoPROC (Acta Cryst. 2011, D67, 293-302)
XDS (Kabsch, W. Acta Cryst. 2010, D66, 125-132)
;
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;All non hydrogens were refined anisotropically. Three strong residual
 electron peaks in the vicinity of the (PF6)- anion were assigned to a
 partial (I3)- anion, considering that their peak to peak separation was
 reasonable for I-I bonds. Due to their vicinity and for charge compensation,
 both anions were refined to have an overall occupancy of 1, converging to
 PF6:I3 0.87018:0.12982. These atoms were refined with displacement parameters
 restraints (SIMU/DELU). The PF6 anion was in addition refined with 1,2
 distances restraints (SADI). Hydrogens were placed geometrically on their
 carrier atoms, including those on the pyrazole N, as free refinement of these
 later did not converge satisfactorily. Hydrogens on the lattice O1W water
 oxygen could not be found nor fixed and are omitted in the structural model,
 but included in the formula.
 At the end of the refinement, there remained a number weak electron density
 peaks in the area of the disordered PF6 and I3 anion, that could not be
 modelled as lattice solvent (acetone). The corresponding void spaces were
 analysed and taken into account with PLATON/SQUEEZE that recovered a total
 of 886 electrons per cell, mostly over 4 voids of 301 cubic angstroms 
 (103 electrons), 4 voids of 205 cubic angstroms (82 electrons) and 4 voids 
 of 71 cubic angstroms (30 electrons). These figures are reasonable for a
 diffuse solvent content of 3 and 2 acetone molecules and 1 molecule of water, 
 respectively for each 301/205/71 cubic angstroms void. This was reflected in 
 the formula, density etc.,SQUEEZE
;

_vrf_PLAT306_ar34                
;
PROBLEM: Isolated Oxygen Atom (H-atoms Missing ?) .......        O1W Check        
RESPONSE: Hydrogens on the lattice O1W water oxygen could not be found nor
fixed and are omitted in the structural model, but included in the formula.
;

_vrf_CHEMW01_ar34                
;
PROBLEM: The difference between the given and expected weight for
            compound is greater 1 mass unit. Check that all hydrogen
            atoms have been taken into account.        
RESPONSE: The diffuse solvent content derived from PLATON/SQUEEZE analysis
of 5 acetone and 1 water molecules per formula unit has been included in the
formula. In addition, hydrogens on the lattice O1W water oxygen could not 
be found nor fixed and are omitted in the structural model, but included in 
the formula. This results in a discrepancy between the figures derived from
the atom site list and those reported for formula, weight, density, mu, F000.
;

_vrf_FORMU01_ar34                
;
PROBLEM: There is a discrepancy between the atom counts in the
            _chemical_formula_sum and the formula from the _atom_site* data.        
RESPONSE: The diffuse solvent content derived from PLATON/SQUEEZE analysis
of 5 acetone and 1 water molecules per formula unit has been included in the
formula. In addition, hydrogens on the lattice O1W water oxygen could not 
be found nor fixed and are omitted in the structural model, but included in 
the formula. This results in a discrepancy between the figures derived from
the atom site list and those reported for formula, weight, density, mu, F000.
;

_vrf_CELLZ01_ar34                
;
PROBLEM: Difference between formula and atom_site contents detected.        
RESPONSE: The diffuse solvent content derived from PLATON/SQUEEZE analysis
of 5 acetone and 1 water molecules per formula unit has been included in the
formula. In addition, hydrogens on the lattice O1W water oxygen could not 
be found nor fixed and are omitted in the structural model, but included in 
the formula. This results in a discrepancy between the figures derived from
the atom site list and those reported for formula, weight, density, mu, F000.
;



_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1217P)²+4.8088P] 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     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0100(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_abs_structure_details 
;
 Flack x determined using 8290 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.031(3)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         18241
_refine_ls_number_parameters     753
_refine_ls_number_restraints     132
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0542
_refine_ls_wR_factor_ref         0.1604
_refine_ls_wR_factor_gt          0.1597
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_restrained_S_all      1.120
_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
I1 I 0.96606(2) 0.53394(2) 0.46606(2) 0.02748(10) Uani 1 3 d S T P . .
P1 P 1.06976(10) 0.49913(15) 0.12243(11) 0.1050(9) Uani 0.8702 1 d D U P A 1
F1 F 1.0388(3) 0.4612(3) 0.1436(4) 0.142(3) Uani 0.8702 1 d D U P A 1
F2 F 1.0281(6) 0.5435(4) 0.1436(7) 0.221(5) Uani 0.8702 1 d D U P A 1
F3 F 1.1070(5) 0.4666(6) 0.0942(6) 0.230(5) Uani 0.8702 1 d D U P A 1
F5 F 1.0295(6) 0.5121(7) 0.0804(6) 0.228(5) Uani 0.8702 1 d D U P A 1
F4 F 1.0993(5) 0.5437(6) 0.0915(7) 0.237(5) Uani 0.8702 1 d D U P A 1
F6 F 1.1004(6) 0.5037(8) 0.1671(5) 0.239(5) Uani 0.8702 1 d D U P A 1
I2 I 1.10607(13) 0.69104(15) 0.14067(13) 0.0772(9) Uani 0.1298 1 d . U P B 2
I3 I 1.10219(12) 0.69168(10) 0.03080(12) 0.0625(6) Uani 0.1298 1 d . U P B 2
I4 I 1.10049(16) 0.69591(12) -0.07802(12) 0.0724(8) Uani 0.1298 1 d . U P B 2
Fe2 Fe 1.09347(2) 0.40653(2) 0.59347(2) 0.0451(2) Uani 1 3 d S T P . .
N7 N 1.06548(17) 0.39143(18) 0.67466(15) 0.0543(9) Uani 1 1 d . . . . .
N8 N 1.06718(13) 0.47833(13) 0.61893(12) 0.0407(6) Uani 1 1 d . . . . .
N9 N 1.06123(12) 0.52563(12) 0.60042(12) 0.0382(6) Uani 1 1 d . . . . .
H9A H 1.069355 0.534698 0.569572 0.046 Uiso 1 1 calc R U . . .
N10 N 0.98528(10) 0.66489(10) 0.47835(10) 0.0297(5) Uani 1 1 d . . . . .
H10A H 0.977057 0.633141 0.483272 0.036 Uiso 1 1 calc R U . . .
N11 N 0.98340(10) 0.68761(10) 0.43285(11) 0.0296(5) Uani 1 1 d . . . . .
N12 N 0.99556(11) 0.75271(10) 0.35440(12) 0.0345(5) Uani 1 1 d . . . . .
C31 C 1.0682(2) 0.3479(2) 0.7030(2) 0.0583(12) Uani 1 1 d . . . . .
C32 C 1.0833(4) 0.3030(3) 0.6816(3) 0.096(3) Uani 1 1 d . . . . .
H32A H 1.091844 0.302686 0.646809 0.115 Uiso 1 1 calc R U . . .
C33 C 1.0864(4) 0.2582(3) 0.7085(3) 0.093(3) Uani 1 1 d . . . . .
H33A H 1.095419 0.227684 0.692085 0.112 Uiso 1 1 calc R U . . .
C34 C 1.0763(4) 0.2587(3) 0.7595(3) 0.091(3) Uani 1 1 d . . . . .
H34A H 1.079203 0.228586 0.778652 0.110 Uiso 1 1 calc R U . . .
C35 C 1.0620(4) 0.3028(3) 0.7826(3) 0.092(2) Uani 1 1 d . . . . .
H35A H 1.055523 0.302979 0.817860 0.110 Uiso 1 1 calc R U . . .
C36 C 1.0569(3) 0.3476(3) 0.7550(2) 0.0700(16) Uani 1 1 d . . . . .
C37 C 1.0416(3) 0.3935(3) 0.7765(2) 0.082(2) Uani 1 1 d . . . . .
H37A H 1.032675 0.394462 0.811189 0.098 Uiso 1 1 calc R U . . .
C38 C 1.0391(3) 0.4378(3) 0.74823(19) 0.0665(14) Uani 1 1 d . . . . .
H38A H 1.029737 0.468968 0.763128 0.080 Uiso 1 1 calc R U . . .
C39 C 1.05108(18) 0.4344(2) 0.69728(16) 0.0495(9) Uani 1 1 d . . . . .
C40 C 1.04974(16) 0.47991(17) 0.66660(14) 0.0448(8) Uani 1 1 d . . . . .
C41 C 1.03321(17) 0.52836(18) 0.67854(14) 0.0460(8) Uani 1 1 d . . . . .
H41A H 1.019364 0.539474 0.709635 0.055 Uiso 1 1 calc R U . . .
C42 C 1.04131(15) 0.55711(15) 0.63516(13) 0.0399(7) Uani 1 1 d . . . . .
C43 C 1.02896(15) 0.61018(15) 0.62541(12) 0.0388(7) Uani 1 1 d . . . . .
C44 C 1.0223(2) 0.64303(19) 0.66561(16) 0.0532(10) Uani 1 1 d . . . . .
H44A H 1.027494 0.631569 0.699129 0.064 Uiso 1 1 calc R U . . .
C45 C 1.0081(2) 0.6921(2) 0.65696(18) 0.0584(12) Uani 1 1 d . . . . .
H45A H 1.002586 0.713931 0.684807 0.070 Uiso 1 1 calc R U . . .
C46 C 1.00151(18) 0.71061(16) 0.60789(16) 0.0473(9) Uani 1 1 d . . . . .
H46A H 0.992400 0.744796 0.602394 0.057 Uiso 1 1 calc R U . . .
C47 C 1.00855(13) 0.67809(13) 0.56742(13) 0.0345(6) Uani 1 1 d . . . . .
C48 C 1.02263(12) 0.62795(13) 0.57638(12) 0.0332(6) Uani 1 1 d . . . . .
H48A H 1.027904 0.605835 0.548721 0.040 Uiso 1 1 calc R U . . .
C49 C 1.00117(12) 0.69607(12) 0.51576(13) 0.0316(6) Uani 1 1 d . . . . .
C50 C 1.00930(13) 0.74229(12) 0.49369(14) 0.0337(6) Uani 1 1 d . . . . .
H50A H 1.019910 0.772462 0.509791 0.040 Uiso 1 1 calc R U . . .
C51 C 0.99850(12) 0.73536(11) 0.44202(13) 0.0303(5) Uani 1 1 d . . . . .
C52 C 1.00435(12) 0.77054(12) 0.39980(14) 0.0328(6) Uani 1 1 d . . . . .
C53 C 1.01944(14) 0.82112(13) 0.40942(16) 0.0394(7) Uani 1 1 d . . . . .
H53A H 1.024154 0.832785 0.442942 0.047 Uiso 1 1 calc R U . . .
C54 C 1.02696(16) 0.85239(13) 0.36940(17) 0.0436(8) Uani 1 1 d . . . . .
H54A H 1.037791 0.886089 0.374820 0.052 Uiso 1 1 calc R U . . .
C55 C 1.01868(16) 0.83483(14) 0.32004(17) 0.0438(8) Uani 1 1 d . . . . .
C56 C 1.0256(2) 0.86460(16) 0.27632(19) 0.0555(11) Uani 1 1 d . . . . .
H56A H 1.038900 0.897686 0.279450 0.067 Uiso 1 1 calc R U . . .
C57 C 1.0133(3) 0.84638(19) 0.2294(2) 0.0620(13) Uani 1 1 d . . . . .
H57A H 1.016547 0.867252 0.200455 0.074 Uiso 1 1 calc R U . . .
C58 C 0.9957(3) 0.79641(18) 0.22454(19) 0.0579(12) Uani 1 1 d . . . . .
H58A H 0.987715 0.783665 0.192059 0.069 Uiso 1 1 calc R U . . .
C59 C 0.99011(18) 0.76606(15) 0.26567(16) 0.0463(8) Uani 1 1 d . . . . .
H59A H 0.978000 0.732609 0.261602 0.056 Uiso 1 1 calc R U . . .
C60 C 1.00217(14) 0.78407(13) 0.31412(14) 0.0372(7) Uani 1 1 d . . . . .
Fe1 Fe 0.83329(2) 0.66671(2) 0.33329(2) 0.03101(16) Uani 1 3 d S T P . .
N1 N 0.82977(12) 0.64416(12) 0.24913(11) 0.0361(6) Uani 1 1 d . . . . .
N2 N 0.90945(10) 0.64726(10) 0.31314(10) 0.0293(5) Uani 1 1 d . . . . .
N3 N 0.95476(10) 0.64675(9) 0.33536(10) 0.0291(5) Uani 1 1 d . . . . .
H3B H 0.959860 0.654217 0.367267 0.035 Uiso 1 1 calc R U . . .
N4 N 1.09193(10) 0.57538(12) 0.46234(12) 0.0359(5) Uani 1 1 d . . . . .
H4B H 1.060757 0.567695 0.454007 0.043 Uiso 1 1 calc R U . . .
N5 N 1.11120(11) 0.56627(13) 0.50840(13) 0.0378(6) Uani 1 1 d . . . . .
N6 N 1.16989(15) 0.57014(15) 0.59322(18) 0.0536(9) Uani 1 1 d . . . . .
C1 C 0.78836(17) 0.64043(16) 0.21743(15) 0.0428(8) Uani 1 1 d . . . . .
C2 C 0.74186(18) 0.6606(2) 0.23259(17) 0.0522(10) Uani 1 1 d . . . . .
H2A H 0.738911 0.676410 0.264577 0.063 Uiso 1 1 calc R U . . .
C3 C 0.7001(2) 0.6576(3) 0.2011(2) 0.0653(14) Uani 1 1 d . . . . .
H3A H 0.668762 0.671169 0.211774 0.078 Uiso 1 1 calc R U . . .
C4 C 0.7041(2) 0.6343(3) 0.1535(2) 0.0688(15) Uani 1 1 d . . . . .
H4A H 0.675053 0.631158 0.132803 0.083 Uiso 1 1 calc R U . . .
C5 C 0.7495(2) 0.6163(2) 0.13677(19) 0.0605(13) Uani 1 1 d . . . . .
H5A H 0.751724 0.601600 0.104217 0.073 Uiso 1 1 calc R U . . .
C6 C 0.79356(19) 0.61945(17) 0.16763(16) 0.0483(9) Uani 1 1 d . . . . .
C7 C 0.8406(2) 0.60329(18) 0.15141(15) 0.0497(9) Uani 1 1 d . . . . .
H7A H 0.844281 0.588262 0.119122 0.060 Uiso 1 1 calc R U . . .
C8 C 0.88155(18) 0.60912(15) 0.18214(14) 0.0433(8) Uani 1 1 d . . . . .
H8A H 0.914285 0.600014 0.170862 0.052 Uiso 1 1 calc R U . . .
C9 C 0.87409(15) 0.62920(13) 0.23161(13) 0.0363(6) Uani 1 1 d . . . . .
C10 C 0.91733(13) 0.63334(12) 0.26528(12) 0.0317(6) Uani 1 1 d . . . . .
C11 C 0.96850(14) 0.62428(12) 0.25655(12) 0.0348(6) Uani 1 1 d . . . . .
H11A H 0.984088 0.614157 0.225942 0.042 Uiso 1 1 calc R U . . .
C12 C 0.99158(12) 0.63348(12) 0.30310(12) 0.0313(5) Uani 1 1 d . . . . .
C13 C 1.04454(12) 0.63084(14) 0.31707(14) 0.0361(6) Uani 1 1 d . . . . .
C14 C 1.08169(18) 0.6418(2) 0.2814(2) 0.0583(12) Uani 1 1 d . . . . .
H14A H 1.072343 0.651045 0.248150 0.070 Uiso 1 1 calc R U . . .
C15 C 1.13190(19) 0.6391(3) 0.2945(3) 0.076(2) Uani 1 1 d . . . . .
H15A H 1.156842 0.647106 0.270058 0.091 Uiso 1 1 calc R U . . .
C16 C 1.14675(16) 0.6249(3) 0.3428(2) 0.0656(15) Uani 1 1 d . . . . .
H16A H 1.181485 0.623337 0.351337 0.079 Uiso 1 1 calc R U . . .
C17 C 1.10968(13) 0.61280(15) 0.37885(16) 0.0392(7) Uani 1 1 d . . . . .
C18 C 1.05898(12) 0.61606(13) 0.36537(13) 0.0333(6) Uani 1 1 d . . . . .
H18A H 1.033818 0.608051 0.389550 0.040 Uiso 1 1 calc R U . . .
C19 C 1.12468(12) 0.59740(14) 0.42992(15) 0.0379(7) Uani 1 1 d . . . . .
C20 C 1.16926(13) 0.60250(16) 0.45688(19) 0.0453(8) Uani 1 1 d . . . . .
H20A H 1.200178 0.616214 0.445139 0.054 Uiso 1 1 calc R U . . .
C21 C 1.15916(13) 0.58323(15) 0.50499(17) 0.0422(8) Uani 1 1 d . . . . .
C22 C 1.19164(16) 0.58110(17) 0.5500(2) 0.0498(10) Uani 1 1 d . . . . .
C23 C 1.24436(18) 0.5906(2) 0.5439(3) 0.0694(17) Uani 1 1 d . . . . .
H23A H 1.258456 0.597537 0.511682 0.083 Uiso 1 1 calc R U . . .
C24 C 1.2738(2) 0.5894(3) 0.5865(3) 0.0821(17) Uani 1 1 d . U . . .
H24A H 1.309082 0.594871 0.584127 0.099 Uiso 1 1 calc R U . . .
C25 C 1.2513(3) 0.5799(2) 0.6343(3) 0.0779(16) Uani 1 1 d . U . . .
C26 C 1.2783(3) 0.5811(3) 0.6803(4) 0.097(2) Uani 1 1 d . U . . .
H26A H 1.313543 0.587646 0.680166 0.116 Uiso 1 1 calc R U . . .
C27 C 1.2534(4) 0.5729(4) 0.7260(4) 0.106(2) Uani 1 1 d . U . . .
H27A H 1.271405 0.575090 0.756878 0.127 Uiso 1 1 calc R U . . .
C28 C 1.2018(4) 0.5613(4) 0.7263(3) 0.097(2) Uani 1 1 d . U . . .
H28A H 1.185793 0.553563 0.757339 0.117 Uiso 1 1 calc R U . . .
C29 C 1.1740(3) 0.5611(3) 0.6829(3) 0.081(2) Uani 1 1 d . U . . .
H29A H 1.138772 0.554976 0.683946 0.097 Uiso 1 1 calc R U . . .
C30 C 1.1990(2) 0.5701(2) 0.6354(2) 0.0641(15) Uani 1 1 d . . . . .
O1W O 1.0481(8) 0.9519(8) 0.4519(8) 0.244(11) Uani 1 3 d S TU P . .


_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
P1 F1 1.415(7) . ?
P1 F6 1.443(11) . ?
P1 F3 1.510(10) . ?
P1 F5 1.582(11) . ?
P1 F4 1.640(11) . ?
P1 F2 1.710(12) . ?
I2 I3 2.917(5) . ?
I3 I4 2.890(5) . ?
Fe2 N8 2.138(4) . ?
Fe2 N8 2.138(4) 12_664 ?
Fe2 N8 2.138(4) 6_566 ?
Fe2 N7 2.313(4) 6_566 ?
Fe2 N7 2.313(4) 12_664 ?
Fe2 N7 2.313(4) . ?
N7 C39 1.343(7) . ?
N7 C31 1.380(6) . ?
N8 C40 1.347(5) . ?
N8 N9 1.357(4) . ?
N9 C42 1.352(5) . ?
N9 H9A 0.8800 . ?
N10 N11 1.350(4) . ?
N10 C49 1.359(4) . ?
N10 H10A 0.8800 . ?
N11 C51 1.351(4) . ?
N12 C52 1.315(5) . ?
N12 C60 1.366(4) . ?
C31 C32 1.380(10) . ?
C31 C36 1.410(8) . ?
C32 C33 1.390(8) . ?
C32 H32A 0.9500 . ?
C33 C34 1.379(12) . ?
C33 H33A 0.9500 . ?
C34 C35 1.374(13) . ?
C34 H34A 0.9500 . ?
C35 C36 1.404(8) . ?
C35 H35A 0.9500 . ?
C36 C37 1.407(11) . ?
C37 C38 1.395(9) . ?
C37 H37A 0.9500 . ?
C38 C39 1.391(7) . ?
C38 H38A 0.9500 . ?
C39 C40 1.457(6) . ?
C40 C41 1.395(7) . ?
C41 C42 1.398(5) . ?
C41 H41A 0.9500 . ?
C42 C43 1.469(6) . ?
C43 C44 1.389(5) . ?
C43 C48 1.394(5) . ?
C44 C45 1.375(8) . ?
C44 H44A 0.9500 . ?
C45 C46 1.402(7) . ?
C45 H45A 0.9500 . ?
C46 C47 1.390(5) . ?
C46 H46A 0.9500 . ?
C47 C48 1.402(5) . ?
C47 C49 1.464(5) . ?
C48 H48A 0.9500 . ?
C49 C50 1.376(4) . ?
C50 C51 1.413(5) . ?
C50 H50A 0.9500 . ?
C51 C52 1.466(4) . ?
C52 C53 1.424(4) . ?
C53 C54 1.362(5) . ?
C53 H53A 0.9500 . ?
C54 C55 1.407(6) . ?
C54 H54A 0.9500 . ?
C55 C56 1.415(6) . ?
C55 C60 1.425(5) . ?
C56 C57 1.376(8) . ?
C56 H56A 0.9500 . ?
C57 C58 1.411(7) . ?
C57 H57A 0.9500 . ?
C58 C59 1.364(6) . ?
C58 H58A 0.9500 . ?
C59 C60 1.408(6) . ?
C59 H59A 0.9500 . ?
Fe1 N2 2.153(3) 12_664 ?
Fe1 N2 2.153(3) 6_566 ?
Fe1 N2 2.153(3) . ?
Fe1 N1 2.314(3) 12_664 ?
Fe1 N1 2.314(3) 6_566 ?
Fe1 N1 2.314(3) . ?
N1 C9 1.325(5) . ?
N1 C1 1.387(4) . ?
N2 C10 1.339(4) . ?
N2 N3 1.339(4) . ?
N3 C12 1.346(4) . ?
N3 H3B 0.8800 . ?
N4 N5 1.347(4) . ?
N4 C19 1.355(5) . ?
N4 H4B 0.8800 . ?
N5 C21 1.353(5) . ?
N6 C22 1.316(7) . ?
N6 C30 1.360(5) . ?
C1 C2 1.404(7) . ?
C1 C6 1.440(6) . ?
C2 C3 1.389(6) . ?
C2 H2A 0.9500 . ?
C3 C4 1.411(9) . ?
C3 H3A 0.9500 . ?
C4 C5 1.369(10) . ?
C4 H4A 0.9500 . ?
C5 C6 1.430(6) . ?
C5 H5A 0.9500 . ?
C6 C7 1.387(8) . ?
C7 C8 1.368(6) . ?
C7 H7A 0.9500 . ?
C8 C9 1.430(5) . ?
C8 H8A 0.9500 . ?
C9 C10 1.458(5) . ?
C10 C11 1.398(5) . ?
C11 C12 1.400(5) . ?
C11 H11A 0.9500 . ?
C12 C13 1.455(5) . ?
C13 C18 1.394(5) . ?
C13 C14 1.396(5) . ?
C14 C15 1.378(7) . ?
C14 H14A 0.9500 . ?
C15 C16 1.393(9) . ?
C15 H15A 0.9500 . ?
C16 C17 1.409(5) . ?
C16 H16A 0.9500 . ?
C17 C18 1.395(5) . ?
C17 C19 1.470(6) . ?
C18 H18A 0.9500 . ?
C19 C20 1.389(5) . ?
C20 C21 1.401(7) . ?
C20 H20A 0.9500 . ?
C21 C22 1.474(6) . ?
C22 C23 1.431(6) . ?
C23 C24 1.376(9) . ?
C23 H23A 0.9500 . ?
C24 C25 1.423(13) . ?
C24 H24A 0.9500 . ?
C25 C30 1.413(9) . ?
C25 C26 1.417(9) . ?
C26 C27 1.398(15) . ?
C26 H26A 0.9500 . ?
C27 C28 1.403(13) . ?
C27 H27A 0.9500 . ?
C28 C29 1.367(7) . ?
C28 H28A 0.9500 . ?
C29 C30 1.442(11) . ?
C29 H29A 0.9500 . ?

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
F1 P1 F6 93.5(9) . . ?
F1 P1 F3 99.7(7) . . ?
F6 P1 F3 94.9(11) . . ?
F1 P1 F5 92.5(8) . . ?
F6 P1 F5 160.3(12) . . ?
F3 P1 F5 102.5(11) . . ?
F1 P1 F4 171.6(8) . . ?
F6 P1 F4 94.7(10) . . ?
F3 P1 F4 81.5(9) . . ?
F5 P1 F4 79.2(9) . . ?
F1 P1 F2 89.1(6) . . ?
F6 P1 F2 92.1(11) . . ?
F3 P1 F2 168.4(8) . . ?
F5 P1 F2 69.3(10) . . ?
F4 P1 F2 88.7(8) . . ?
I4 I3 I2 177.80(17) . . ?
N8 Fe2 N8 95.39(11) . 12_664 ?
N8 Fe2 N8 95.39(11) . 6_566 ?
N8 Fe2 N8 95.39(11) 12_664 6_566 ?
N8 Fe2 N7 87.88(15) . 6_566 ?
N8 Fe2 N7 170.92(15) 12_664 6_566 ?
N8 Fe2 N7 75.84(14) 6_566 6_566 ?
N8 Fe2 N7 170.92(15) . 12_664 ?
N8 Fe2 N7 75.84(14) 12_664 12_664 ?
N8 Fe2 N7 87.88(14) 6_566 12_664 ?
N7 Fe2 N7 101.14(13) 6_566 12_664 ?
N8 Fe2 N7 75.84(14) . . ?
N8 Fe2 N7 87.88(15) 12_664 . ?
N8 Fe2 N7 170.92(15) 6_566 . ?
N7 Fe2 N7 101.14(12) 6_566 . ?
N7 Fe2 N7 101.14(13) 12_664 . ?
C39 N7 C31 118.7(4) . . ?
C39 N7 Fe2 111.1(3) . . ?
C31 N7 Fe2 129.5(4) . . ?
C40 N8 N9 105.7(3) . . ?
C40 N8 Fe2 115.9(3) . . ?
N9 N8 Fe2 138.4(3) . . ?
C42 N9 N8 111.7(3) . . ?
C42 N9 H9A 124.1 . . ?
N8 N9 H9A 124.1 . . ?
N11 N10 C49 113.1(3) . . ?
N11 N10 H10A 123.4 . . ?
C49 N10 H10A 123.4 . . ?
N10 N11 C51 104.3(3) . . ?
C52 N12 C60 118.4(3) . . ?
C32 C31 N7 120.8(5) . . ?
C32 C31 C36 117.4(5) . . ?
N7 C31 C36 121.8(6) . . ?
C31 C32 C33 122.9(7) . . ?
C31 C32 H32A 118.5 . . ?
C33 C32 H32A 118.5 . . ?
C34 C33 C32 119.0(8) . . ?
C34 C33 H33A 120.5 . . ?
C32 C33 H33A 120.5 . . ?
C35 C34 C33 120.0(6) . . ?
C35 C34 H34A 120.0 . . ?
C33 C34 H34A 120.0 . . ?
C34 C35 C36 120.9(7) . . ?
C34 C35 H35A 119.5 . . ?
C36 C35 H35A 119.5 . . ?
C35 C36 C37 123.3(6) . . ?
C35 C36 C31 119.7(7) . . ?
C37 C36 C31 117.0(5) . . ?
C38 C37 C36 121.6(5) . . ?
C38 C37 H37A 119.2 . . ?
C36 C37 H37A 119.2 . . ?
C39 C38 C37 117.2(6) . . ?
C39 C38 H38A 121.4 . . ?
C37 C38 H38A 121.4 . . ?
N7 C39 C38 123.7(5) . . ?
N7 C39 C40 117.4(4) . . ?
C38 C39 C40 118.9(5) . . ?
N8 C40 C41 110.5(4) . . ?
N8 C40 C39 119.3(4) . . ?
C41 C40 C39 130.2(4) . . ?
C40 C41 C42 105.5(4) . . ?
C40 C41 H41A 127.2 . . ?
C42 C41 H41A 127.2 . . ?
N9 C42 C41 106.5(4) . . ?
N9 C42 C43 124.0(3) . . ?
C41 C42 C43 129.4(4) . . ?
C44 C43 C48 119.3(4) . . ?
C44 C43 C42 119.7(3) . . ?
C48 C43 C42 121.0(3) . . ?
C45 C44 C43 120.1(4) . . ?
C45 C44 H44A 120.0 . . ?
C43 C44 H44A 120.0 . . ?
C44 C45 C46 121.4(4) . . ?
C44 C45 H45A 119.3 . . ?
C46 C45 H45A 119.3 . . ?
C47 C46 C45 118.9(4) . . ?
C47 C46 H46A 120.6 . . ?
C45 C46 H46A 120.6 . . ?
C46 C47 C48 119.6(4) . . ?
C46 C47 C49 120.2(3) . . ?
C48 C47 C49 120.2(3) . . ?
C43 C48 C47 120.8(3) . . ?
C43 C48 H48A 119.6 . . ?
C47 C48 H48A 119.6 . . ?
N10 C49 C50 106.3(3) . . ?
N10 C49 C47 121.8(3) . . ?
C50 C49 C47 131.9(3) . . ?
C49 C50 C51 105.4(3) . . ?
C49 C50 H50A 127.3 . . ?
C51 C50 H50A 127.3 . . ?
N11 C51 C50 110.9(3) . . ?
N11 C51 C52 119.4(3) . . ?
C50 C51 C52 129.6(3) . . ?
N12 C52 C53 123.6(3) . . ?
N12 C52 C51 116.9(3) . . ?
C53 C52 C51 119.5(3) . . ?
C54 C53 C52 118.4(4) . . ?
C54 C53 H53A 120.8 . . ?
C52 C53 H53A 120.8 . . ?
C53 C54 C55 120.0(3) . . ?
C53 C54 H54A 120.0 . . ?
C55 C54 H54A 120.0 . . ?
C54 C55 C56 123.9(4) . . ?
C54 C55 C60 117.6(3) . . ?
C56 C55 C60 118.5(4) . . ?
C57 C56 C55 121.0(4) . . ?
C57 C56 H56A 119.5 . . ?
C55 C56 H56A 119.5 . . ?
C56 C57 C58 119.4(4) . . ?
C56 C57 H57A 120.3 . . ?
C58 C57 H57A 120.3 . . ?
C59 C58 C57 121.2(5) . . ?
C59 C58 H58A 119.4 . . ?
C57 C58 H58A 119.4 . . ?
C58 C59 C60 120.3(4) . . ?
C58 C59 H59A 119.8 . . ?
C60 C59 H59A 119.8 . . ?
N12 C60 C59 118.6(3) . . ?
N12 C60 C55 121.9(4) . . ?
C59 C60 C55 119.4(3) . . ?
N2 Fe1 N2 93.87(10) 12_664 6_566 ?
N2 Fe1 N2 93.87(10) 12_664 . ?
N2 Fe1 N2 93.87(10) 6_566 . ?
N2 Fe1 N1 74.71(11) 12_664 12_664 ?
N2 Fe1 N1 168.44(11) 6_566 12_664 ?
N2 Fe1 N1 88.78(10) . 12_664 ?
N2 Fe1 N1 88.78(10) 12_664 6_566 ?
N2 Fe1 N1 74.71(11) 6_566 6_566 ?
N2 Fe1 N1 168.44(11) . 6_566 ?
N1 Fe1 N1 102.77(10) 12_664 6_566 ?
N2 Fe1 N1 168.44(11) 12_664 . ?
N2 Fe1 N1 88.78(10) 6_566 . ?
N2 Fe1 N1 74.71(11) . . ?
N1 Fe1 N1 102.77(10) 12_664 . ?
N1 Fe1 N1 102.77(10) 6_566 . ?
C9 N1 C1 118.0(3) . . ?
C9 N1 Fe1 112.3(2) . . ?
C1 N1 Fe1 129.5(3) . . ?
C10 N2 N3 105.9(3) . . ?
C10 N2 Fe1 116.6(2) . . ?
N3 N2 Fe1 137.4(2) . . ?
N2 N3 C12 112.0(3) . . ?
N2 N3 H3B 124.0 . . ?
C12 N3 H3B 124.0 . . ?
N5 N4 C19 114.2(3) . . ?
N5 N4 H4B 122.9 . . ?
C19 N4 H4B 122.9 . . ?
N4 N5 C21 103.7(3) . . ?
C22 N6 C30 118.0(5) . . ?
N1 C1 C2 119.7(4) . . ?
N1 C1 C6 120.5(4) . . ?
C2 C1 C6 119.6(4) . . ?
C3 C2 C1 120.4(5) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 120.3(6) . . ?
C2 C3 H3A 119.9 . . ?
C4 C3 H3A 119.9 . . ?
C5 C4 C3 120.6(5) . . ?
C5 C4 H4A 119.7 . . ?
C3 C4 H4A 119.7 . . ?
C4 C5 C6 120.9(5) . . ?
C4 C5 H5A 119.5 . . ?
C6 C5 H5A 119.5 . . ?
C7 C6 C5 122.7(5) . . ?
C7 C6 C1 119.3(4) . . ?
C5 C6 C1 118.0(5) . . ?
C8 C7 C6 119.6(4) . . ?
C8 C7 H7A 120.2 . . ?
C6 C7 H7A 120.2 . . ?
C7 C8 C9 118.6(4) . . ?
C7 C8 H8A 120.7 . . ?
C9 C8 H8A 120.7 . . ?
N1 C9 C8 123.8(4) . . ?
N1 C9 C10 117.4(3) . . ?
C8 C9 C10 118.8(4) . . ?
N2 C10 C11 110.9(3) . . ?
N2 C10 C9 118.6(3) . . ?
C11 C10 C9 130.5(3) . . ?
C10 C11 C12 104.4(3) . . ?
C10 C11 H11A 127.8 . . ?
C12 C11 H11A 127.8 . . ?
N3 C12 C11 106.8(3) . . ?
N3 C12 C13 123.5(3) . . ?
C11 C12 C13 129.7(3) . . ?
C18 C13 C14 119.1(4) . . ?
C18 C13 C12 120.9(3) . . ?
C14 C13 C12 120.0(4) . . ?
C15 C14 C13 120.1(5) . . ?
C15 C14 H14A 119.9 . . ?
C13 C14 H14A 119.9 . . ?
C14 C15 C16 121.2(4) . . ?
C14 C15 H15A 119.4 . . ?
C16 C15 H15A 119.4 . . ?
C15 C16 C17 119.3(4) . . ?
C15 C16 H16A 120.4 . . ?
C17 C16 H16A 120.4 . . ?
C18 C17 C16 119.0(4) . . ?
C18 C17 C19 121.0(3) . . ?
C16 C17 C19 120.0(4) . . ?
C13 C18 C17 121.2(3) . . ?
C13 C18 H18A 119.4 . . ?
C17 C18 H18A 119.4 . . ?
N4 C19 C20 105.1(4) . . ?
N4 C19 C17 122.1(3) . . ?
C20 C19 C17 132.7(4) . . ?
C19 C20 C21 105.7(3) . . ?
C19 C20 H20A 127.1 . . ?
C21 C20 H20A 127.1 . . ?
N5 C21 C20 111.2(3) . . ?
N5 C21 C22 118.9(4) . . ?
C20 C21 C22 129.8(4) . . ?
N6 C22 C23 124.5(5) . . ?
N6 C22 C21 117.3(4) . . ?
C23 C22 C21 118.2(5) . . ?
C24 C23 C22 117.2(7) . . ?
C24 C23 H23A 121.4 . . ?
C22 C23 H23A 121.4 . . ?
C23 C24 C25 119.9(6) . . ?
C23 C24 H24A 120.0 . . ?
C25 C24 H24A 120.0 . . ?
C30 C25 C26 118.9(9) . . ?
C30 C25 C24 117.6(5) . . ?
C26 C25 C24 123.5(7) . . ?
C27 C26 C25 120.3(7) . . ?
C27 C26 H26A 119.9 . . ?
C25 C26 H26A 119.9 . . ?
C26 C27 C28 120.0(6) . . ?
C26 C27 H27A 120.0 . . ?
C28 C27 H27A 120.0 . . ?
C29 C28 C27 121.5(9) . . ?
C29 C28 H28A 119.2 . . ?
C27 C28 H28A 119.2 . . ?
C28 C29 C30 119.2(7) . . ?
C28 C29 H29A 120.4 . . ?
C30 C29 H29A 120.4 . . ?
N6 C30 C25 122.7(7) . . ?
N6 C30 C29 117.3(5) . . ?
C25 C30 C29 120.0(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
N4 H4B I1 0.88 2.69 3.517(3) 157.9 . yes
N10 H10A I1 0.88 2.69 3.527(3) 159.9 . yes
N3 H3B N11 0.88 2.05 2.906(4) 163.9 . yes
N9 H9A N5 0.88 2.14 2.980(5) 160.2 . yes

_refine_diff_density_max         1.034
_refine_diff_density_min         -0.542
_refine_diff_density_rms         0.105



