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

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_shelx
_database_code_depnum_ccdc_archive 'CCDC 2247017'
loop_
_audit_author_name
_audit_author_address
'Sankar Rath'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-05-29 downloaded from the CCDC.
;
_audit_creation_date             2023-05-02
_audit_creation_method           
;
Olex2 1.5-dev
(compiled 2023.03.24 svn.rc9df729e for OlexSys, GUI svn.r6758)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C47 H27 Br8 Fe N4 O, 1.5(C6 H6)'
_chemical_formula_sum            'C56 H36 Br8 Fe N4 O'
_chemical_formula_weight         1476.02
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   19.930(2)
_cell_length_b                   23.340(2)
_cell_length_c                   22.690(2)
_cell_angle_alpha                90
_cell_angle_beta                 99.864(3)
_cell_angle_gamma                90
_cell_volume                     10398.3(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    999
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.5
_shelx_estimated_absorpt_T_max   0.563
_shelx_estimated_absorpt_T_min   0.464
_exptl_absorpt_coefficient_mu    6.483
_exptl_absorpt_correction_T_max  0.523
_exptl_absorpt_correction_T_min  0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.886
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5712
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0842
_diffrn_reflns_av_unetI/netI     0.1068
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            26683
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.531
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5423
_reflns_number_total             9143
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-dev (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.612
_refine_diff_density_rms         0.143
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     663
_refine_ls_number_reflns         9143
_refine_ls_number_restraints     70
_refine_ls_R_factor_all          0.1038
_refine_ls_R_factor_gt           0.0471
_refine_ls_restrained_S_all      0.956
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0454P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0922
_refine_ls_wR_factor_ref         0.1126
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Fe1-O1 \\sim Fe1A-O1A
 with sigma of 0.02
 Fe1-N1 \\sim Fe1A-N1
 with sigma of 0.02
 Fe1-N2 \\sim Fe1A-N2
 with sigma of 0.02
 Fe1-N3 \\sim Fe1A-N3
 with sigma of 0.02
 Fe1-N4 \\sim Fe1A-N4
 with sigma of 0.02
 O1-C45 \\sim O1A-C45A
 with sigma of 0.02
 C45-C46 \\sim C45A-C46A
 with sigma of 0.02
 C45-C47 \\sim C45A-C47A
 with sigma of 0.02
 C1S-C2S \\sim C1T-C2T
 with sigma of 0.02
 C1S-C6S \\sim C1T-C6T
 with sigma of 0.02
 C2S-C3S \\sim C2T-C3T
 with sigma of 0.02
 C3S-C4S \\sim C3T-C4T
 with sigma of 0.02
 C4S-C5S \\sim C4T-C5T
 with sigma of 0.02
 C5S-C6S \\sim C5T-C6T
 with sigma of 0.02
 Fe1-C45 \\sim Fe1A-C45A
 with sigma of 0.04
 O1-N1 \\sim O1A-N1
 with sigma of 0.04
 O1-N2 \\sim O1A-N2
 with sigma of 0.04
 O1-N3 \\sim O1A-N3
 with sigma of 0.04
 O1-N4 \\sim O1A-N4
 with sigma of 0.04
 O1-C46 \\sim O1A-C46A
 with sigma of 0.04
 O1-C47 \\sim O1A-C47A
 with sigma of 0.04
 C46-C47 \\sim C46A-C47A
 with sigma of 0.04
 C1S-C3S \\sim C1T-C3T
 with sigma of 0.04
 C1S-C5S \\sim C1T-C5T
 with sigma of 0.04
 C2S-C4S \\sim C2T-C4T
 with sigma of 0.04
 C2S-C6S \\sim C2T-C6T
 with sigma of 0.04
 C3S-C5S \\sim C3T-C5T
 with sigma of 0.04
 C4S-C6S \\sim C4T-C6T
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
Uanis(C47) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04
4. Rigid body (RIGU) restrains
 C1S, C2S, C6S, C3S, C5S, C4S
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(C6T)=Sof(H6T)=Sof(C1T)=Sof(H1T)=Sof(C2T)=Sof(H2T)=Sof(C3T)=Sof(H3T)=
 Sof(C4T)=Sof(H4T)=Sof(C5T)=Sof(H5T)=Sof(O1A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=
 Sof(H46D)=Sof(H46E)=Sof(H46F)=Sof(C47A)=Sof(H47D)=Sof(H47E)=Sof(H47F)=
 Sof(Fe1A)=1-FVAR(1)
 Sof(Fe1)=Sof(O1)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46A)=Sof(H46B)=Sof(H46C)=
 Sof(C47)=Sof(H47A)=Sof(H47B)=Sof(H47C)=Sof(C1S)=Sof(H1S)=Sof(C2S)=Sof(H2S)=
 Sof(C3S)=Sof(H3S)=Sof(C4S)=Sof(H4S)=Sof(C5S)=Sof(H5S)=Sof(C6S)=Sof(H6S)=FVAR(1)
 Fixed Uiso: C6T(0.05) C1T(0.05) C2T(0.05) C3T(0.05) C4T(0.05) C5T(0.05)
 O1A(0.05) C45A(0.05) C46A(0.05) C47A(0.05)
6.a Ternary CH refined with riding coordinates:
 C45(H45), C45A(H45A)
6.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C28(H28),
 C29(H29), C30(H30), C31(H31), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38),
  C40(H40), C41(H41), C42(H42), C43(H43), C44(H44), C1S(H1S), C2S(H2S),
 C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C8S(H8S), C9S(H9S), C6T(H6T),
  C1T(H1T), C2T(H2T), C3T(H3T), C4T(H4T), C5T(H5T)
6.c Fitted hexagon refined as free rotating group:
 C6T(C1T,C2T,C3T,C4T,C5T)
6.d Idealised Me refined as rotating group:
 C46(H46A,H46B,H46C), C47(H47A,H47B,H47C), C46A(H46D,H46E,H46F), C47A(H47D,
 H47E,H47F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.26414(5) 0.04507(5) 0.57786(5) 0.0243(4) Uani 0.930(3) 1 d D . P A 1
Br1 Br 0.10582(4) -0.07333(3) 0.72374(3) 0.0349(2) Uani 1 1 d . . . . .
Br2 Br 0.01982(4) 0.04938(3) 0.67037(3) 0.0390(2) Uani 1 1 d . . . . .
Br3 Br 0.02867(4) 0.11905(4) 0.39554(3) 0.0373(2) Uani 1 1 d . . . . .
Br4 Br 0.17441(4) 0.16211(4) 0.34435(3) 0.0393(2) Uani 1 1 d . . . . .
Br5 Br 0.43973(4) 0.22476(3) 0.54408(3) 0.0384(2) Uani 1 1 d . . . . .
Br6 Br 0.53636(4) 0.11809(3) 0.62229(4) 0.0483(2) Uani 1 1 d . . . . .
Br7 Br 0.45584(4) -0.14463(3) 0.55252(4) 0.0385(2) Uani 1 1 d . . . . .
Br8 Br 0.30164(4) -0.20735(3) 0.56990(3) 0.0339(2) Uani 1 1 d . . . . .
O1 O 0.2781(3) 0.0862(2) 0.6451(2) 0.0346(14) Uani 0.930(3) 1 d D . P A 1
N1 N 0.1739(3) 0.0015(2) 0.5811(2) 0.0228(13) Uani 1 1 d D . . . .
N2 N 0.2058(3) 0.0966(2) 0.5139(2) 0.0253(14) Uani 1 1 d D . . . .
N3 N 0.3461(3) 0.0679(2) 0.5372(2) 0.0291(15) Uani 1 1 d D . . . .
N4 N 0.3111(3) -0.0332(2) 0.5920(2) 0.0244(14) Uani 1 1 d D . . . .
C1 C 0.1749(3) -0.0433(3) 0.6211(3) 0.0259(17) Uani 1 1 d . . . . .
C2 C 0.1214(4) -0.0340(3) 0.6556(3) 0.0277(17) Uani 1 1 d . . . . .
C3 C 0.0870(4) 0.0140(3) 0.6347(3) 0.0293(18) Uani 1 1 d . . . . .
C4 C 0.1170(3) 0.0353(3) 0.5846(3) 0.0256(17) Uani 1 1 d . . . . .
C5 C 0.0951(3) 0.0760(3) 0.5420(3) 0.0239(16) Uani 1 1 d . . . . .
C6 C 0.1355(3) 0.0959(3) 0.5008(3) 0.0240(16) Uani 1 1 d . . . . .
C7 C 0.1147(3) 0.1206(3) 0.4428(3) 0.0279(17) Uani 1 1 d . . . . .
C8 C 0.1722(4) 0.1379(3) 0.4236(3) 0.0281(18) Uani 1 1 d . . . . .
C9 C 0.2293(4) 0.1265(3) 0.4695(3) 0.0252(17) Uani 1 1 d . . . . .
C10 C 0.2959(4) 0.1475(3) 0.4753(3) 0.0271(17) Uani 1 1 d . . . . .
C11 C 0.3489(4) 0.1238(3) 0.5173(3) 0.0275(17) Uani 1 1 d . . . . .
C12 C 0.4139(4) 0.1481(3) 0.5432(3) 0.0268(17) Uani 1 1 d . . . . .
C13 C 0.4514(4) 0.1056(3) 0.5747(3) 0.0299(18) Uani 1 1 d . . . . .
C14 C 0.4099(4) 0.0544(3) 0.5689(3) 0.0251(17) Uani 1 1 d . . . . .
C15 C 0.4275(4) -0.0017(3) 0.5860(3) 0.0295(18) Uani 1 1 d . . . . .
C16 C 0.3772(4) -0.0452(3) 0.5852(3) 0.0264(17) Uani 1 1 d . . . . .
C17 C 0.3841(4) -0.1057(3) 0.5787(3) 0.0281(17) Uani 1 1 d . . . . .
C18 C 0.3241(3) -0.1308(3) 0.5856(3) 0.0255(17) Uani 1 1 d . . . . .
C19 C 0.2803(3) -0.0844(3) 0.5984(3) 0.0229(16) Uani 1 1 d . . . . .
C20 C 0.2187(4) -0.0895(3) 0.6219(3) 0.0268(17) Uani 1 1 d . . . . .
C21 C 0.0247(3) 0.1011(3) 0.5365(3) 0.0245(17) Uani 1 1 d . . . . .
C22 C -0.0335(4) 0.0666(3) 0.5295(3) 0.0308(18) Uani 1 1 d . . . . .
H22 H -0.029239 0.026093 0.528018 0.037 Uiso 1 1 calc R U . . .
C23 C -0.0970(4) 0.0913(3) 0.5246(3) 0.0315(18) Uani 1 1 d . . . . .
H23 H -0.136419 0.067668 0.517869 0.038 Uiso 1 1 calc R U . . .
C24 C -0.1043(4) 0.1494(3) 0.5294(3) 0.0341(19) Uani 1 1 d . . . . .
H24 H -0.148379 0.165794 0.526770 0.041 Uiso 1 1 calc R U . . .
C25 C -0.0471(4) 0.1843(3) 0.5381(3) 0.0343(19) Uani 1 1 d . . . . .
H25 H -0.051516 0.224493 0.542475 0.041 Uiso 1 1 calc R U . . .
C26 C 0.0169(4) 0.1595(3) 0.5404(3) 0.0282(18) Uani 1 1 d . . . . .
H26 H 0.055941 0.183477 0.544824 0.034 Uiso 1 1 calc R U . . .
C27 C 0.2745(4) 0.2447(3) 0.4283(3) 0.0312(18) Uani 1 1 d . . . . .
H27 H 0.237238 0.249096 0.448943 0.037 Uiso 1 1 calc R U . . .
C28 C 0.2892(4) 0.2884(3) 0.3912(3) 0.0345(19) Uani 1 1 d . . . . .
H28 H 0.262525 0.322368 0.386878 0.041 Uiso 1 1 calc R U . . .
C29 C 0.3427(4) 0.2822(3) 0.3605(3) 0.039(2) Uani 1 1 d . . . . .
H29 H 0.353077 0.312084 0.335067 0.046 Uiso 1 1 calc R U . . .
C30 C 0.3816(4) 0.2327(3) 0.3667(3) 0.0338(19) Uani 1 1 d . . . . .
H30 H 0.417959 0.227949 0.344901 0.041 Uiso 1 1 calc R U . . .
C31 C 0.3667(3) 0.1899(3) 0.4053(3) 0.0275(17) Uani 1 1 d . . . . .
H31 H 0.394253 0.156427 0.410660 0.033 Uiso 1 1 calc R U . . .
C32 C 0.3122(3) 0.1950(3) 0.4361(3) 0.0245(17) Uani 1 1 d . . . . .
C33 C 0.4998(4) -0.0197(3) 0.6096(3) 0.0297(18) Uani 1 1 d . . . . .
C34 C 0.5519(4) -0.0107(3) 0.5770(3) 0.0350(19) Uani 1 1 d . . . . .
H34 H 0.542744 0.008442 0.539513 0.042 Uiso 1 1 calc R U . . .
C35 C 0.6166(4) -0.0294(3) 0.5989(4) 0.042(2) Uani 1 1 d . . . . .
H35 H 0.651679 -0.024520 0.575805 0.050 Uiso 1 1 calc R U . . .
C36 C 0.6312(4) -0.0554(3) 0.6544(4) 0.041(2) Uani 1 1 d . . . . .
H36 H 0.676225 -0.067564 0.669833 0.049 Uiso 1 1 calc R U . . .
C37 C 0.5802(4) -0.0633(3) 0.6870(4) 0.043(2) Uani 1 1 d . . . . .
H37 H 0.589935 -0.080975 0.725198 0.051 Uiso 1 1 calc R U . . .
C38 C 0.5150(4) -0.0458(3) 0.6646(3) 0.0349(19) Uani 1 1 d . . . . .
H38 H 0.479889 -0.051912 0.687400 0.042 Uiso 1 1 calc R U . . .
C39 C 0.2040(4) -0.1446(3) 0.6499(3) 0.0263(17) Uani 1 1 d . . . . .
C40 C 0.2483(4) -0.1675(3) 0.6978(3) 0.0350(19) Uani 1 1 d . . . . .
H40 H 0.289108 -0.147600 0.713384 0.042 Uiso 1 1 calc R U . . .
C41 C 0.2343(4) -0.2183(3) 0.7231(3) 0.040(2) Uani 1 1 d . . . . .
H41 H 0.265802 -0.233852 0.755276 0.048 Uiso 1 1 calc R U . . .
C42 C 0.1742(4) -0.2472(3) 0.7020(4) 0.044(2) Uani 1 1 d . . . . .
H42 H 0.163767 -0.281889 0.720496 0.053 Uiso 1 1 calc R U . . .
C43 C 0.1293(4) -0.2253(3) 0.6537(4) 0.045(2) Uani 1 1 d . . . . .
H43 H 0.088638 -0.245249 0.637979 0.054 Uiso 1 1 calc R U . . .
C44 C 0.1447(4) -0.1739(3) 0.6290(3) 0.0310(18) Uani 1 1 d . . . . .
H44 H 0.113485 -0.158284 0.596664 0.037 Uiso 1 1 calc R U . . .
C45 C 0.3049(5) 0.0895(5) 0.7060(4) 0.057(3) Uani 0.930(3) 1 d D . P A 1
H45 H 0.283968 0.123637 0.722417 0.069 Uiso 0.930(3) 1 calc R U P A 1
C46 C 0.2850(8) 0.0393(5) 0.7368(5) 0.112(6) Uani 0.930(3) 1 d D . P A 1
H46A H 0.303384 0.004816 0.720717 0.168 Uiso 0.930(3) 1 calc R U P A 1
H46B H 0.235214 0.036807 0.730748 0.168 Uiso 0.930(3) 1 calc R U P A 1
H46C H 0.303025 0.042397 0.779656 0.168 Uiso 0.930(3) 1 calc R U P A 1
C47 C 0.3773(7) 0.0996(9) 0.7134(5) 0.180(9) Uani 0.930(3) 1 d D U P A 1
H47A H 0.397020 0.098501 0.756058 0.270 Uiso 0.930(3) 1 calc R U P A 1
H47B H 0.385652 0.137300 0.697033 0.270 Uiso 0.930(3) 1 calc R U P A 1
H47C H 0.398511 0.069914 0.692187 0.270 Uiso 0.930(3) 1 calc R U P A 1
C1S C 0.2563(5) -0.1318(4) 0.3908(5) 0.063(3) Uani 0.930(3) 1 d D . P A 1
H1S H 0.284665 -0.163852 0.402707 0.076 Uiso 0.930(3) 1 calc R U P A 1
C2S C 0.2056(5) -0.1352(5) 0.3412(5) 0.073(3) Uani 0.930(3) 1 d D . P A 1
H2S H 0.198223 -0.169699 0.318865 0.087 Uiso 0.930(3) 1 calc R U P A 1
C3S C 0.1662(5) -0.0879(5) 0.3247(4) 0.068(3) Uani 0.930(3) 1 d D . P A 1
H3S H 0.132391 -0.089879 0.289721 0.082 Uiso 0.930(3) 1 calc R U P A 1
C4S C 0.1734(5) -0.0380(5) 0.3564(4) 0.060(3) Uani 0.930(3) 1 d D . P A 1
H4S H 0.143732 -0.006600 0.344915 0.072 Uiso 0.930(3) 1 calc R U P A 1
C5S C 0.2247(5) -0.0338(4) 0.4056(4) 0.053(3) Uani 0.930(3) 1 d D . P A 1
H5S H 0.232128 0.001003 0.427461 0.064 Uiso 0.930(3) 1 calc R U P A 1
C6S C 0.2653(5) -0.0817(5) 0.4226(4) 0.058(3) Uani 0.930(3) 1 d D . P A 1
H6S H 0.299907 -0.079485 0.457001 0.070 Uiso 0.930(3) 1 calc R U P A 1
C7S C 0.5252(6) 0.2964(5) 0.2734(6) 0.115(6) Uani 1 1 d . . . . .
H7S H 0.542137 0.331853 0.290458 0.138 Uiso 1 1 calc R U . . .
C8S C 0.5518(6) 0.2486(7) 0.2963(5) 0.094(5) Uani 1 1 d . . . . .
H8S H 0.589381 0.248887 0.328317 0.113 Uiso 1 1 calc R U . . .
C9S C 0.5255(7) 0.2000(5) 0.2740(5) 0.108(7) Uani 1 1 d . . . . .
H9S H 0.542272 0.164696 0.291552 0.129 Uiso 1 1 calc R U . . .
C6T C 0.262(4) 0.074(4) 0.666(3) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H6T H 0.226195 0.056105 0.639294 0.060 Uiso 0.070(3) 1 calc R U P A 2
C1T C 0.262(4) 0.072(4) 0.727(4) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H1T H 0.226214 0.052437 0.742357 0.060 Uiso 0.070(3) 1 calc R U P A 2
C2T C 0.314(4) 0.098(3) 0.767(3) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H2T H 0.314103 0.096103 0.808813 0.060 Uiso 0.070(3) 1 calc R U P A 2
C3T C 0.366(4) 0.126(3) 0.745(3) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H3T H 0.401973 0.143437 0.772207 0.060 Uiso 0.070(3) 1 calc R U P A 2
C4T C 0.366(4) 0.128(4) 0.684(4) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H4T H 0.401955 0.147106 0.669144 0.060 Uiso 0.070(3) 1 calc R U P A 2
C5T C 0.314(5) 0.102(4) 0.645(3) 0.050 Uiso 0.070(3) 1 d DG U P A 2
H5T H 0.314066 0.103440 0.602687 0.060 Uiso 0.070(3) 1 calc R U P A 2
O1A O 0.237(2) -0.0168(15) 0.4628(11) 0.050 Uiso 0.070(3) 1 d D U P A 2
C45A C 0.250(4) -0.049(3) 0.415(2) 0.050 Uiso 0.070(3) 1 d D U P A 2
H45A H 0.295593 -0.036165 0.406372 0.060 Uiso 0.070(3) 1 calc R U P A 2
C46A C 0.256(7) -0.110(3) 0.428(5) 0.050 Uiso 0.070(3) 1 d D U P A 2
H46D H 0.300918 -0.123248 0.422660 0.075 Uiso 0.070(3) 1 calc R U P A 2
H46E H 0.220558 -0.130519 0.401478 0.075 Uiso 0.070(3) 1 calc R U P A 2
H46F H 0.250358 -0.115781 0.469835 0.075 Uiso 0.070(3) 1 calc R U P A 2
C47A C 0.201(7) -0.034(5) 0.362(2) 0.050 Uiso 0.070(3) 1 d D U P A 2
H47D H 0.154975 -0.037935 0.371446 0.075 Uiso 0.070(3) 1 calc R U P A 2
H47E H 0.206448 -0.059997 0.329437 0.075 Uiso 0.070(3) 1 calc R U P A 2
H47F H 0.208537 0.005468 0.350645 0.075 Uiso 0.070(3) 1 calc R U P A 2
Fe1A Fe 0.2533(5) 0.0220(5) 0.5301(6) 0.030(5) Uani 0.070(3) 1 d D . 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 O1 1.784(5) . y
Fe1 N1 2.078(5) . y
Fe1 N2 2.080(6) . y
Fe1 N3 2.079(6) . y
Fe1 N4 2.053(6) . y
Br1 C2 1.870(7) . ?
Br2 C3 1.871(7) . ?
Br3 C7 1.861(7) . ?
Br4 C8 1.892(7) . ?
Br5 C12 1.860(7) . ?
Br6 C13 1.868(7) . ?
Br7 C17 1.875(7) . ?
Br8 C18 1.862(7) . ?
O1 C45 1.397(9) . ?
N1 C1 1.383(8) . ?
N1 C4 1.394(8) . ?
N1 Fe1A 2.169(12) . y
N2 C6 1.382(8) . ?
N2 C9 1.373(8) . ?
N2 Fe1A 1.986(12) . y
N3 C11 1.385(8) . ?
N3 C14 1.386(8) . ?
N3 Fe1A 2.120(12) . y
N4 C16 1.382(8) . ?
N4 C19 1.362(8) . ?
N4 Fe1A 2.099(12) . y
C1 C2 1.442(9) . ?
C1 C20 1.385(9) . ?
C2 C3 1.356(9) . ?
C3 C4 1.459(9) . ?
C4 C5 1.373(9) . ?
C5 C6 1.413(9) . ?
C5 C21 1.504(9) . ?
C6 C7 1.432(9) . ?
C7 C8 1.356(9) . ?
C8 C9 1.429(9) . ?
C9 C10 1.401(10) . ?
C10 C11 1.409(9) . ?
C10 C32 1.492(9) . ?
C11 C12 1.443(10) . ?
C12 C13 1.368(9) . ?
C13 C14 1.447(9) . ?
C14 C15 1.393(9) . ?
C15 C16 1.424(9) . ?
C15 C33 1.509(10) . ?
C16 C17 1.428(9) . ?
C17 C18 1.364(9) . ?
C18 C19 1.451(9) . ?
C19 C20 1.425(9) . ?
C20 C39 1.484(9) . ?
C21 C22 1.399(9) . ?
C21 C26 1.377(9) . ?
C22 H22 0.9500 . ?
C22 C23 1.379(9) . ?
C23 H23 0.9500 . ?
C23 C24 1.371(10) . ?
C24 H24 0.9500 . ?
C24 C25 1.386(10) . ?
C25 H25 0.9500 . ?
C25 C26 1.392(9) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
C27 C28 1.386(9) . ?
C27 C32 1.375(9) . ?
C28 H28 0.9500 . ?
C28 C29 1.377(10) . ?
C29 H29 0.9500 . ?
C29 C30 1.386(10) . ?
C30 H30 0.9500 . ?
C30 C31 1.394(9) . ?
C31 H31 0.9500 . ?
C31 C32 1.394(9) . ?
C33 C34 1.392(9) . ?
C33 C38 1.374(9) . ?
C34 H34 0.9500 . ?
C34 C35 1.371(10) . ?
C35 H35 0.9500 . ?
C35 C36 1.383(10) . ?
C36 H36 0.9500 . ?
C36 C37 1.366(10) . ?
C37 H37 0.9500 . ?
C37 C38 1.374(10) . ?
C38 H38 0.9500 . ?
C39 C40 1.386(9) . ?
C39 C44 1.377(9) . ?
C40 H40 0.9500 . ?
C40 C41 1.367(10) . ?
C41 H41 0.9500 . ?
C41 C42 1.387(10) . ?
C42 H42 0.9500 . ?
C42 C43 1.388(11) . ?
C43 H43 0.9500 . ?
C43 C44 1.381(10) . ?
C44 H44 0.9500 . ?
C45 H45 1.0000 . ?
C45 C46 1.453(14) . ?
C45 C47 1.444(16) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C1S H1S 0.9500 . ?
C1S C2S 1.379(12) . ?
C1S C6S 1.370(12) . ?
C2S H2S 0.9500 . ?
C2S C3S 1.370(12) . ?
C3S H3S 0.9500 . ?
C3S C4S 1.364(12) . ?
C4S H4S 0.9500 . ?
C4S C5S 1.381(11) . ?
C5S H5S 0.9500 . ?
C5S C6S 1.394(11) . ?
C6S H6S 0.9500 . ?
C7S C7S 1.33(2) 2_655 ?
C7S H7S 0.9500 . ?
C7S C8S 1.305(15) . ?
C8S H8S 0.9500 . ?
C8S C9S 1.314(16) . ?
C9S C9S 1.36(3) 2_655 ?
C9S H9S 0.9500 . ?
C6T H6T 0.9500 . ?
C6T C1T 1.3900 . ?
C6T C5T 1.3900 . ?
C1T H1T 0.9500 . ?
C1T C2T 1.3900 . ?
C2T H2T 0.9500 . ?
C2T C3T 1.3900 . ?
C3T H3T 0.9500 . ?
C3T C4T 1.3900 . ?
C4T H4T 0.9500 . ?
C4T C5T 1.3900 . ?
C5T H5T 0.9500 . ?
O1A C45A 1.38(2) . ?
O1A Fe1A 1.757(17) . y
C45A H45A 1.0000 . ?
C45A C46A 1.45(2) . ?
C45A C47A 1.44(3) . ?
C46A H46D 0.9800 . ?
C46A H46E 0.9800 . ?
C46A H46F 0.9800 . ?
C47A H47D 0.9800 . ?
C47A H47E 0.9800 . ?
C47A H47F 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N1 104.0(2) . . y
O1 Fe1 N2 105.8(2) . . y
O1 Fe1 N3 102.8(2) . . y
O1 Fe1 N4 110.3(2) . . y
N1 Fe1 N2 85.6(2) . . y
N1 Fe1 N3 153.1(2) . . y
N3 Fe1 N2 86.0(2) . . y
N4 Fe1 N1 86.2(2) . . y
N4 Fe1 N2 144.0(2) . . y
N4 Fe1 N3 85.8(2) . . y
C45 O1 Fe1 148.6(6) . . ?
C1 N1 Fe1 118.6(4) . . ?
C1 N1 C4 108.1(5) . . ?
C1 N1 Fe1A 125.9(5) . . ?
C4 N1 Fe1 116.3(4) . . ?
C4 N1 Fe1A 125.5(5) . . ?
C6 N2 Fe1 124.6(4) . . ?
C6 N2 Fe1A 117.6(5) . . ?
C9 N2 Fe1 125.9(5) . . ?
C9 N2 C6 108.0(6) . . ?
C9 N2 Fe1A 111.6(5) . . ?
C11 N3 Fe1 117.7(4) . . ?
C11 N3 C14 107.4(6) . . ?
C11 N3 Fe1A 122.3(5) . . ?
C14 N3 Fe1 115.6(4) . . ?
C14 N3 Fe1A 129.4(5) . . ?
C16 N4 Fe1 125.5(4) . . ?
C16 N4 Fe1A 118.3(5) . . ?
C19 N4 Fe1 126.5(4) . . ?
C19 N4 C16 106.9(5) . . ?
C19 N4 Fe1A 113.9(5) . . ?
N1 C1 C2 108.2(6) . . ?
C20 C1 N1 122.5(6) . . ?
C20 C1 C2 129.2(6) . . ?
C1 C2 Br1 128.2(5) . . ?
C3 C2 Br1 123.2(5) . . ?
C3 C2 C1 108.2(6) . . ?
C2 C3 Br2 124.8(5) . . ?
C2 C3 C4 107.6(6) . . ?
C4 C3 Br2 127.2(5) . . ?
N1 C4 C3 107.3(6) . . ?
C5 C4 N1 121.0(6) . . ?
C5 C4 C3 131.3(6) . . ?
C4 C5 C6 123.0(6) . . ?
C4 C5 C21 120.5(6) . . ?
C6 C5 C21 116.5(6) . . ?
N2 C6 C5 122.2(6) . . ?
N2 C6 C7 108.4(6) . . ?
C5 C6 C7 129.3(6) . . ?
C6 C7 Br3 127.9(5) . . ?
C8 C7 Br3 124.5(5) . . ?
C8 C7 C6 106.8(6) . . ?
C7 C8 Br4 123.6(6) . . ?
C7 C8 C9 108.7(6) . . ?
C9 C8 Br4 127.1(5) . . ?
N2 C9 C8 107.6(6) . . ?
N2 C9 C10 123.1(6) . . ?
C10 C9 C8 128.8(6) . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 C32 120.3(6) . . ?
C11 C10 C32 118.7(6) . . ?
N3 C11 C10 121.5(6) . . ?
N3 C11 C12 108.7(6) . . ?
C10 C11 C12 129.6(7) . . ?
C11 C12 Br5 127.5(5) . . ?
C13 C12 Br5 124.5(6) . . ?
C13 C12 C11 107.4(6) . . ?
C12 C13 Br6 123.3(6) . . ?
C12 C13 C14 107.4(6) . . ?
C14 C13 Br6 128.9(5) . . ?
N3 C14 C13 108.5(6) . . ?
N3 C14 C15 121.6(6) . . ?
C15 C14 C13 129.7(7) . . ?
C14 C15 C16 121.6(7) . . ?
C14 C15 C33 122.7(6) . . ?
C16 C15 C33 115.6(6) . . ?
N4 C16 C15 122.4(6) . . ?
N4 C16 C17 108.7(6) . . ?
C15 C16 C17 128.9(7) . . ?
C16 C17 Br7 127.1(5) . . ?
C18 C17 Br7 124.0(5) . . ?
C18 C17 C16 108.1(6) . . ?
C17 C18 Br8 125.2(5) . . ?
C17 C18 C19 105.8(6) . . ?
C19 C18 Br8 128.4(5) . . ?
N4 C19 C18 109.5(6) . . ?
N4 C19 C20 123.2(6) . . ?
C20 C19 C18 126.8(6) . . ?
C1 C20 C19 120.7(6) . . ?
C1 C20 C39 120.7(6) . . ?
C19 C20 C39 118.6(6) . . ?
C22 C21 C5 121.9(6) . . ?
C26 C21 C5 119.6(6) . . ?
C26 C21 C22 118.4(7) . . ?
C21 C22 H22 120.0 . . ?
C23 C22 C21 120.1(7) . . ?
C23 C22 H22 120.0 . . ?
C22 C23 H23 119.5 . . ?
C24 C23 C22 121.1(7) . . ?
C24 C23 H23 119.5 . . ?
C23 C24 H24 120.1 . . ?
C23 C24 C25 119.7(7) . . ?
C25 C24 H24 120.1 . . ?
C24 C25 H25 120.4 . . ?
C24 C25 C26 119.2(7) . . ?
C26 C25 H25 120.4 . . ?
C21 C26 C25 121.5(7) . . ?
C21 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C28 C27 H27 119.0 . . ?
C32 C27 H27 119.0 . . ?
C32 C27 C28 122.1(7) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 C27 119.5(7) . . ?
C29 C28 H28 120.3 . . ?
C28 C29 H29 119.8 . . ?
C28 C29 C30 120.3(7) . . ?
C30 C29 H29 119.8 . . ?
C29 C30 H30 120.5 . . ?
C29 C30 C31 119.0(7) . . ?
C31 C30 H30 120.5 . . ?
C30 C31 H31 119.3 . . ?
C32 C31 C30 121.4(7) . . ?
C32 C31 H31 119.3 . . ?
C27 C32 C10 122.2(6) . . ?
C27 C32 C31 117.6(6) . . ?
C31 C32 C10 120.1(6) . . ?
C34 C33 C15 121.6(6) . . ?
C38 C33 C15 119.6(6) . . ?
C38 C33 C34 118.8(7) . . ?
C33 C34 H34 120.0 . . ?
C35 C34 C33 120.0(7) . . ?
C35 C34 H34 120.0 . . ?
C34 C35 H35 119.7 . . ?
C34 C35 C36 120.5(7) . . ?
C36 C35 H35 119.7 . . ?
C35 C36 H36 120.3 . . ?
C37 C36 C35 119.5(7) . . ?
C37 C36 H36 120.3 . . ?
C36 C37 H37 119.9 . . ?
C36 C37 C38 120.2(8) . . ?
C38 C37 H37 119.9 . . ?
C33 C38 C37 121.0(7) . . ?
C33 C38 H38 119.5 . . ?
C37 C38 H38 119.5 . . ?
C40 C39 C20 121.6(7) . . ?
C44 C39 C20 120.3(6) . . ?
C44 C39 C40 118.1(7) . . ?
C39 C40 H40 119.5 . . ?
C41 C40 C39 121.0(8) . . ?
C41 C40 H40 119.5 . . ?
C40 C41 H41 119.8 . . ?
C40 C41 C42 120.3(7) . . ?
C42 C41 H41 119.8 . . ?
C41 C42 H42 120.2 . . ?
C41 C42 C43 119.6(7) . . ?
C43 C42 H42 120.2 . . ?
C42 C43 H43 120.6 . . ?
C44 C43 C42 118.9(8) . . ?
C44 C43 H43 120.6 . . ?
C39 C44 C43 122.0(7) . . ?
C39 C44 H44 119.0 . . ?
C43 C44 H44 119.0 . . ?
O1 C45 H45 107.4 . . ?
O1 C45 C46 110.0(9) . . ?
O1 C45 C47 109.2(9) . . ?
C46 C45 H45 107.4 . . ?
C47 C45 H45 107.4 . . ?
C47 C45 C46 115.2(12) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46B 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 H47A 109.5 . . ?
C45 C47 H47B 109.5 . . ?
C45 C47 H47C 109.5 . . ?
H47A C47 H47B 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C2S C1S H1S 120.3 . . ?
C6S C1S H1S 120.3 . . ?
C6S C1S C2S 119.4(10) . . ?
C1S C2S H2S 120.6 . . ?
C3S C2S C1S 118.8(10) . . ?
C3S C2S H2S 120.6 . . ?
C2S C3S H3S 118.7 . . ?
C4S C3S C2S 122.7(10) . . ?
C4S C3S H3S 118.7 . . ?
C3S C4S H4S 120.5 . . ?
C3S C4S C5S 118.9(10) . . ?
C5S C4S H4S 120.5 . . ?
C4S C5S H5S 120.6 . . ?
C4S C5S C6S 118.7(9) . . ?
C6S C5S H5S 120.6 . . ?
C1S C6S C5S 121.3(10) . . ?
C1S C6S H6S 119.3 . . ?
C5S C6S H6S 119.3 . . ?
C7S C7S H7S 119.4 2_655 . ?
C8S C7S C7S 121.1(8) . 2_655 ?
C8S C7S H7S 119.4 . . ?
C7S C8S H8S 120.7 . . ?
C7S C8S C9S 118.5(12) . . ?
C9S C8S H8S 120.7 . . ?
C8S C9S C9S 120.2(8) . 2_655 ?
C8S C9S H9S 119.9 . . ?
C9S C9S H9S 119.9 2_655 . ?
C1T C6T H6T 120.0 . . ?
C1T C6T C5T 120.0 . . ?
C5T C6T H6T 120.0 . . ?
C6T C1T H1T 120.0 . . ?
C2T C1T C6T 120.0 . . ?
C2T C1T H1T 120.0 . . ?
C1T C2T H2T 120.0 . . ?
C1T C2T C3T 120.0 . . ?
C3T C2T H2T 120.0 . . ?
C2T C3T H3T 120.0 . . ?
C4T C3T C2T 120.0 . . ?
C4T C3T H3T 120.0 . . ?
C3T C4T H4T 120.0 . . ?
C5T C4T C3T 120.0 . . ?
C5T C4T H4T 120.0 . . ?
C6T C5T H5T 120.0 . . ?
C4T C5T C6T 120.0 . . ?
C4T C5T H5T 120.0 . . ?
C45A O1A Fe1A 159(4) . . ?
O1A C45A H45A 106.6 . . ?
O1A C45A C46A 112(3) . . ?
O1A C45A C47A 109(3) . . ?
C46A C45A H45A 106.6 . . ?
C47A C45A H45A 106.6 . . ?
C47A C45A C46A 115(4) . . ?
C45A C46A H46D 109.5 . . ?
C45A C46A H46E 109.5 . . ?
C45A C46A H46F 109.5 . . ?
H46D C46A H46E 109.5 . . ?
H46D C46A H46F 109.5 . . ?
H46E C46A H46F 109.5 . . ?
C45A C47A H47D 109.5 . . ?
C45A C47A H47E 109.5 . . ?
C45A C47A H47F 109.5 . . ?
H47D C47A H47E 109.5 . . ?
H47D C47A H47F 109.5 . . ?
H47E C47A H47F 109.5 . . ?
N2 Fe1A N1 85.6(4) . . y
N2 Fe1A N3 87.3(5) . . y
N2 Fe1A N4 148.4(8) . . y
N3 Fe1A N1 141.1(7) . . y
N4 Fe1A N1 82.8(4) . . y
N4 Fe1A N3 83.6(5) . . y
O1A Fe1A N1 108.0(14) . . y
O1A Fe1A N2 106.3(14) . . y
O1A Fe1A N3 110.7(14) . . y
O1A Fe1A N4 105.2(14) . . y

_olex2_submission_special_instructions 'No special instructions were received'
# start Validation Reply Form
_vrf_PLAT331_shelx               
;
PROBLEM: Small Aver Phenyl C-C Dist C7S      --C7S_a    .       1.32 Ang.  
RESPONSE: a mirror plane is passing through C7S and C9S of a benzene ring
which results in such behaviour.
;
_vrf_PLAT220_shelx               
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        7.8 Ratio 
RESPONSE: The crystal was weakly diffracting and thus the quality of
data is relatively poor. The methyl groups of the axial (Me)2CHOH ligand 
have orientation disorder due to free rotations.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2247020'
loop_
_audit_author_name
_audit_author_address
'Sankar Rath'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2023-05-23 deposited with the CCDC.	2023-05-29 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         ?
_chemical_formula_sum            'C52 H34 Br8 Cl Fe N4 O6'
_chemical_formula_weight         1541.41

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

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

_cell_length_a                   14.639(5)
_cell_length_b                   16.495(5)
_cell_length_c                   21.095(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     5094(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.25

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.010
_exptl_crystal_F_000             2980
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    6.680
_shelx_estimated_absorpt_T_min   0.455
_shelx_estimated_absorpt_T_max   0.555
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.408
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_process_details   'SADABS 2.05 (Sheldrick, 2002)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            26131
_diffrn_reflns_av_unetI/netI     0.1116
_diffrn_reflns_av_R_equivalents  0.0883
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.860
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_full        24.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             8917
_reflns_number_gt                6897
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_max     0.992
_reflns_Friedel_fraction_full    0.992

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

_computing_data_collection       'Bruker APEX'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0149P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Flack x determined using 2301 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.025(12)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         8917
_refine_ls_number_parameters     659
_refine_ls_number_restraints     14
_refine_ls_R_factor_all          0.0727
_refine_ls_R_factor_gt           0.0499
_refine_ls_wR_factor_ref         0.0887
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.961
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.57481(13) 0.83462(10) 0.16262(8) 0.0149(4) Uani 1 1 d . . . . .
N1 N 0.5817(6) 0.7826(5) 0.2500(4) 0.011(2) Uani 1 1 d . . . . .
N2 N 0.7125(7) 0.8234(5) 0.1544(4) 0.016(2) Uani 1 1 d . . . . .
N3 N 0.5676(7) 0.8903(5) 0.0764(4) 0.014(2) Uani 1 1 d . . . . .
N4 N 0.4374(7) 0.8414(5) 0.1698(4) 0.012(2) Uani 1 1 d . U . . .
O1 O 0.5942(6) 0.9515(5) 0.2008(4) 0.018(2) Uani 1 1 d D . . . .
O2 O 0.5612(6) 0.7139(5) 0.1255(4) 0.018(2) Uani 1 1 d D . . . .
Br1 Br 0.48309(9) 0.78970(8) 0.43268(5) 0.0224(3) Uani 1 1 d . . . . .
Br2 Br 0.71304(9) 0.75759(7) 0.42245(6) 0.0227(3) Uani 1 1 d . . . . .
Br3 Br 0.93878(10) 0.67736(8) 0.17842(6) 0.0264(3) Uani 1 1 d . . . . .
Br4 Br 0.92978(9) 0.77238(7) 0.03563(6) 0.0235(3) Uani 1 1 d . . . . .
Br5 Br 0.68321(10) 1.06305(7) -0.04174(6) 0.0261(3) Uani 1 1 d . . . . .
Br6 Br 0.46024(10) 1.09306(8) -0.00878(6) 0.0287(4) Uani 1 1 d . . . . .
Br7 Br 0.18797(9) 0.81954(8) 0.07806(6) 0.0254(3) Uani 1 1 d . . . . .
Br8 Br 0.20511(9) 0.70988(8) 0.21428(6) 0.0236(3) Uani 1 1 d . . . . .
C1 C 0.5093(9) 0.7808(7) 0.2913(5) 0.014(3) Uani 1 1 d . . . . .
C2 C 0.5448(9) 0.7744(7) 0.3552(5) 0.019(3) Uani 1 1 d . . . . .
C3 C 0.6377(9) 0.7660(7) 0.3515(5) 0.016(3) Uani 1 1 d . . . . .
C4 C 0.6622(8) 0.7689(7) 0.2850(5) 0.015(3) Uani 1 1 d . . . . .
C5 C 0.7480(9) 0.7572(7) 0.2566(6) 0.019(3) Uani 1 1 d . . . . .
C6 C 0.7677(9) 0.7743(7) 0.1922(5) 0.018(3) Uani 1 1 d . . . . .
C7 C 0.8471(8) 0.7519(7) 0.1577(6) 0.018(3) Uani 1 1 d . . . . .
C8 C 0.8443(9) 0.7897(7) 0.1002(5) 0.017(3) Uani 1 1 d . . . . .
C9 C 0.7591(9) 0.8360(6) 0.0980(5) 0.015(3) Uani 1 1 d . . . . .
C10 C 0.7317(8) 0.8905(7) 0.0501(5) 0.015(3) Uani 1 1 d . . . . .
C11 C 0.6442(9) 0.9217(6) 0.0454(5) 0.013(3) Uani 1 1 d . . . . .
C12 C 0.6135(10) 0.9899(7) 0.0069(6) 0.022(3) Uani 1 1 d . . . . .
C13 C 0.5240(9) 0.9995(7) 0.0163(6) 0.020(3) Uani 1 1 d . . . . .
C14 C 0.4932(9) 0.9360(7) 0.0574(5) 0.015(3) Uani 1 1 d . . . . .
C15 C 0.4011(8) 0.9157(6) 0.0715(5) 0.011(3) Uani 1 1 d . . . . .
C16 C 0.3780(9) 0.8619(7) 0.1191(5) 0.017(3) Uani 1 1 d . . . . .
C17 C 0.2904(9) 0.8222(7) 0.1314(5) 0.018(3) Uani 1 1 d . . . . .
C18 C 0.2968(9) 0.7819(7) 0.1863(5) 0.018(3) Uani 1 1 d . . . . .
C19 C 0.3857(9) 0.7949(7) 0.2135(5) 0.016(3) Uani 1 1 d . . . . .
C20 C 0.4182(9) 0.7756(6) 0.2732(5) 0.014(3) Uani 1 1 d . . . . .
C21 C 0.8231(8) 0.7247(7) 0.2961(5) 0.011(3) Uani 1 1 d . U . . .
C22 C 0.8256(9) 0.6435(7) 0.3147(6) 0.020(3) Uani 1 1 d . . . . .
H22A H 0.775443 0.609071 0.305270 0.024 Uiso 1 1 calc R U . . .
C23 C 0.8998(10) 0.6131(8) 0.3466(6) 0.027(4) Uani 1 1 d . . . . .
H23A H 0.902104 0.556949 0.356586 0.033 Uiso 1 1 calc R U . . .
C24 C 0.9708(10) 0.6629(8) 0.3641(6) 0.029(4) Uani 1 1 d . . . . .
H24A H 1.021654 0.641564 0.386569 0.035 Uiso 1 1 calc R U . . .
C25 C 0.9675(10) 0.7431(8) 0.3490(6) 0.031(4) Uani 1 1 d . . . . .
H25A H 1.015332 0.777899 0.362694 0.038 Uiso 1 1 calc R U . . .
C26 C 0.8958(9) 0.7752(8) 0.3141(6) 0.023(3) Uani 1 1 d . . . . .
H26A H 0.895825 0.830851 0.302558 0.028 Uiso 1 1 calc R U . . .
C27 C 0.8054(9) 0.9189(7) 0.0051(6) 0.017(3) Uani 1 1 d . . . . .
C28 C 0.8732(8) 0.9692(7) 0.0266(6) 0.019(3) Uani 1 1 d . . . . .
H28A H 0.874433 0.985182 0.069846 0.022 Uiso 1 1 calc R U . . .
C29 C 0.9392(10) 0.9966(7) -0.0142(6) 0.027(3) Uani 1 1 d . . . . .
H29A H 0.985147 1.032433 0.000869 0.032 Uiso 1 1 calc R U . . .
C30 C 0.9397(10) 0.9724(7) -0.0774(6) 0.028(3) Uani 1 1 d . . . . .
H30A H 0.986349 0.990773 -0.105172 0.034 Uiso 1 1 calc R U . . .
C31 C 0.8719(10) 0.9214(8) -0.0994(6) 0.030(4) Uani 1 1 d . . . . .
H31A H 0.872707 0.904395 -0.142422 0.036 Uiso 1 1 calc R U . . .
C32 C 0.8027(10) 0.8945(7) -0.0596(5) 0.023(3) Uani 1 1 d . . . . .
H32A H 0.755021 0.860907 -0.075079 0.027 Uiso 1 1 calc R U . . .
C33 C 0.3295(9) 0.9516(7) 0.0297(5) 0.016(3) Uani 1 1 d . . . . .
C34 C 0.2653(9) 1.0060(7) 0.0548(6) 0.021(3) Uani 1 1 d . . . . .
H34A H 0.263993 1.017085 0.099009 0.026 Uiso 1 1 calc R U . . .
C35 C 0.2039(9) 1.0434(7) 0.0142(6) 0.022(3) Uani 1 1 d . . . . .
H35A H 0.161237 1.081170 0.030986 0.026 Uiso 1 1 calc R U . . .
C36 C 0.2031(10) 1.0273(7) -0.0494(6) 0.023(3) Uani 1 1 d . . . . .
H36A H 0.160033 1.052877 -0.076476 0.027 Uiso 1 1 calc R U . . .
C37 C 0.2670(9) 0.9724(7) -0.0738(6) 0.024(3) Uani 1 1 d . . . . .
H37A H 0.267380 0.960514 -0.117871 0.028 Uiso 1 1 calc R U . . .
C38 C 0.3290(9) 0.9356(7) -0.0345(6) 0.018(3) Uani 1 1 d . . . . .
H38A H 0.372088 0.898558 -0.051659 0.022 Uiso 1 1 calc R U . . .
C39 C 0.3500(9) 0.7460(7) 0.3213(5) 0.019(3) Uani 1 1 d . . . . .
C40 C 0.2828(8) 0.7963(7) 0.3442(5) 0.018(3) Uani 1 1 d . . . . .
H40A H 0.278604 0.850237 0.328793 0.022 Uiso 1 1 calc R U . . .
C41 C 0.2206(9) 0.7694(8) 0.3898(6) 0.025(3) Uani 1 1 d . . . . .
H41A H 0.178414 0.805956 0.408669 0.030 Uiso 1 1 calc R U . . .
C42 C 0.2219(9) 0.6873(8) 0.4072(6) 0.024(3) Uani 1 1 d . . . . .
H42A H 0.176677 0.666547 0.435146 0.029 Uiso 1 1 calc R U . . .
C43 C 0.2876(10) 0.6377(7) 0.3842(6) 0.026(3) Uani 1 1 d . . . . .
H43A H 0.289038 0.582692 0.397534 0.031 Uiso 1 1 calc R U . . .
C44 C 0.3532(10) 0.6652(7) 0.3414(6) 0.026(3) Uani 1 1 d . . . . .
H44A H 0.399294 0.629709 0.326199 0.031 Uiso 1 1 calc R U . . .
C45 C 0.6541(10) 0.9690(7) 0.2533(6) 0.027(4) Uani 1 1 d . . . . .
H45A H 0.664379 1.027632 0.255871 0.041 Uiso 1 1 calc R U . . .
H45B H 0.712560 0.941274 0.247055 0.041 Uiso 1 1 calc R U . . .
H45C H 0.625909 0.950059 0.292795 0.041 Uiso 1 1 calc R U . . .
C46 C 0.6080(9) 0.6898(7) 0.0686(5) 0.024(3) Uani 1 1 d . . . . .
H46A H 0.580422 0.639992 0.052059 0.036 Uiso 1 1 calc R U . . .
H46B H 0.672570 0.680073 0.078210 0.036 Uiso 1 1 calc R U . . .
H46C H 0.602890 0.732936 0.036876 0.036 Uiso 1 1 calc R U . . .
C47 C 0.9806(11) 0.9883(8) 0.3175(7) 0.031(4) Uani 1 1 d . . . . .
H47A H 0.979286 1.009084 0.359475 0.038 Uiso 1 1 calc R U . . .
C48 C 1.0562(10) 0.9477(8) 0.2956(6) 0.030(4) Uani 1 1 d . . . . .
H48A H 1.106508 0.940840 0.323511 0.036 Uiso 1 1 calc R U . . .
C49 C 1.0625(11) 0.9170(8) 0.2360(7) 0.033(4) Uani 1 1 d . . . . .
H49A H 1.116029 0.889559 0.222340 0.039 Uiso 1 1 calc R U . . .
C50 C 0.9876(12) 0.9270(8) 0.1953(7) 0.037(4) Uani 1 1 d . . . . .
H50A H 0.989490 0.905516 0.153545 0.044 Uiso 1 1 calc R U . . .
C51 C 0.9114(10) 0.9681(8) 0.2160(6) 0.027(3) Uani 1 1 d . . . . .
H51A H 0.861417 0.975974 0.187866 0.032 Uiso 1 1 calc R U . . .
C52 C 0.9064(11) 0.9985(7) 0.2777(7) 0.033(4) Uani 1 1 d . . . . .
H52A H 0.853044 1.025582 0.292052 0.040 Uiso 1 1 calc R U . . .
Cl1 Cl 0.3844(3) 1.02333(19) 0.26231(15) 0.0243(8) Uani 1 1 d . . . . .
O3 O 0.3029(7) 0.9843(5) 0.2390(4) 0.039(3) Uani 1 1 d . . . . .
O4 O 0.4328(7) 0.9672(5) 0.3016(4) 0.032(2) Uani 1 1 d . . . . .
O5 O 0.3579(7) 1.0932(5) 0.2980(4) 0.030(2) Uani 1 1 d . . . . .
O6 O 0.4406(7) 1.0468(5) 0.2089(4) 0.036(3) Uani 1 1 d . . . . .
H2A H 0.572(11) 0.709(9) 0.163(2) 0.06(5) Uiso 1 1 d D . . . .
H1A H 0.553(5) 0.983(5) 0.203(5) 0.01(4) Uiso 1 1 d D . . . .


_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 N4 2.020(10) . ?
Fe1 N2 2.032(10) . ?
Fe1 N1 2.036(9) . ?
Fe1 N3 2.041(9) . ?
Fe1 O1 2.109(8) . ?
Fe1 O2 2.149(8) . ?
N1 C1 1.372(14) . ?
N1 C4 1.410(14) . ?
N2 C9 1.387(14) . ?
N2 C6 1.395(14) . ?
N3 C14 1.383(14) . ?
N3 C11 1.398(14) . ?
N4 C19 1.419(14) . ?
N4 C16 1.420(14) . ?
O1 C45 1.442(14) . ?
O2 C46 1.438(13) . ?
Br1 C2 1.884(12) . ?
Br2 C3 1.865(12) . ?
Br3 C7 1.872(12) . ?
Br4 C8 1.872(12) . ?
Br5 C12 1.884(12) . ?
Br6 C13 1.880(12) . ?
Br7 C17 1.875(12) . ?
Br8 C18 1.888(12) . ?
C1 C20 1.389(16) . ?
C1 C2 1.448(15) . ?
C2 C3 1.368(17) . ?
C3 C4 1.448(15) . ?
C4 C5 1.405(16) . ?
C5 C6 1.416(16) . ?
C5 C21 1.481(15) . ?
C6 C7 1.420(16) . ?
C7 C8 1.364(15) . ?
C8 C9 1.462(17) . ?
C9 C10 1.411(15) . ?
C10 C11 1.383(16) . ?
C10 C27 1.512(16) . ?
C11 C12 1.460(15) . ?
C12 C13 1.334(17) . ?
C13 C14 1.432(16) . ?
C14 C15 1.421(16) . ?
C15 C16 1.381(16) . ?
C15 C33 1.492(15) . ?
C16 C17 1.463(17) . ?
C17 C18 1.338(15) . ?
C18 C19 1.439(16) . ?
C19 C20 1.384(15) . ?
C20 C39 1.505(16) . ?
C21 C22 1.396(15) . ?
C21 C26 1.403(16) . ?
C22 C23 1.372(17) . ?
C23 C24 1.377(18) . ?
C24 C25 1.362(17) . ?
C25 C26 1.387(17) . ?
C27 C28 1.371(16) . ?
C27 C32 1.423(15) . ?
C28 C29 1.370(16) . ?
C29 C30 1.392(17) . ?
C30 C31 1.381(18) . ?
C31 C32 1.388(17) . ?
C33 C38 1.380(16) . ?
C33 C34 1.403(16) . ?
C34 C35 1.387(16) . ?
C35 C36 1.367(16) . ?
C36 C37 1.400(17) . ?
C37 C38 1.371(16) . ?
C39 C40 1.374(16) . ?
C39 C44 1.399(16) . ?
C40 C41 1.396(16) . ?
C41 C42 1.404(16) . ?
C42 C43 1.352(17) . ?
C43 C44 1.393(17) . ?
C47 C48 1.372(19) . ?
C47 C52 1.383(19) . ?
C48 C49 1.359(18) . ?
C49 C50 1.402(19) . ?
C50 C51 1.377(19) . ?
C51 C52 1.396(18) . ?
Cl1 O5 1.430(8) . ?
Cl1 O4 1.431(9) . ?
Cl1 O3 1.441(10) . ?
Cl1 O6 1.448(9) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N4 Fe1 N2 177.8(4) . . ?
N4 Fe1 N1 90.3(4) . . ?
N2 Fe1 N1 89.4(4) . . ?
N4 Fe1 N3 89.4(4) . . ?
N2 Fe1 N3 90.9(4) . . ?
N1 Fe1 N3 178.2(4) . . ?
N4 Fe1 O1 93.1(4) . . ?
N2 Fe1 O1 89.0(4) . . ?
N1 Fe1 O1 91.9(3) . . ?
N3 Fe1 O1 86.3(3) . . ?
N4 Fe1 O2 89.2(3) . . ?
N2 Fe1 O2 88.7(4) . . ?
N1 Fe1 O2 86.8(3) . . ?
N3 Fe1 O2 95.0(3) . . ?
O1 Fe1 O2 177.3(4) . . ?
C1 N1 C4 108.0(9) . . ?
C1 N1 Fe1 123.1(7) . . ?
C4 N1 Fe1 125.7(7) . . ?
C9 N2 C6 107.0(10) . . ?
C9 N2 Fe1 123.2(8) . . ?
C6 N2 Fe1 125.3(8) . . ?
C14 N3 C11 107.2(8) . . ?
C14 N3 Fe1 123.0(8) . . ?
C11 N3 Fe1 122.8(8) . . ?
C19 N4 C16 107.0(10) . . ?
C19 N4 Fe1 123.3(8) . . ?
C16 N4 Fe1 124.5(7) . . ?
C45 O1 Fe1 124.0(7) . . ?
C46 O2 Fe1 121.1(7) . . ?
N1 C1 C20 124.6(10) . . ?
N1 C1 C2 108.4(11) . . ?
C20 C1 C2 126.6(11) . . ?
C3 C2 C1 108.1(11) . . ?
C3 C2 Br1 122.7(9) . . ?
C1 C2 Br1 128.7(10) . . ?
C2 C3 C4 107.4(11) . . ?
C2 C3 Br2 123.3(9) . . ?
C4 C3 Br2 129.2(10) . . ?
C5 C4 N1 123.0(10) . . ?
C5 C4 C3 129.1(11) . . ?
N1 C4 C3 107.8(10) . . ?
C4 C5 C6 124.4(12) . . ?
C4 C5 C21 118.2(10) . . ?
C6 C5 C21 117.4(11) . . ?
N2 C6 C5 123.1(11) . . ?
N2 C6 C7 109.3(10) . . ?
C5 C6 C7 127.4(12) . . ?
C8 C7 C6 108.2(11) . . ?
C8 C7 Br3 122.0(10) . . ?
C6 C7 Br3 129.6(9) . . ?
C7 C8 C9 107.1(11) . . ?
C7 C8 Br4 123.8(10) . . ?
C9 C8 Br4 128.8(8) . . ?
N2 C9 C10 124.7(11) . . ?
N2 C9 C8 108.3(10) . . ?
C10 C9 C8 126.8(11) . . ?
C11 C10 C9 123.5(11) . . ?
C11 C10 C27 120.1(10) . . ?
C9 C10 C27 116.3(11) . . ?
C10 C11 N3 124.9(10) . . ?
C10 C11 C12 127.7(11) . . ?
N3 C11 C12 107.3(11) . . ?
C13 C12 C11 108.1(11) . . ?
C13 C12 Br5 122.5(10) . . ?
C11 C12 Br5 129.0(10) . . ?
C12 C13 C14 108.3(11) . . ?
C12 C13 Br6 122.8(10) . . ?
C14 C13 Br6 127.9(10) . . ?
N3 C14 C15 123.9(10) . . ?
N3 C14 C13 109.0(10) . . ?
C15 C14 C13 126.7(11) . . ?
C16 C15 C14 122.4(11) . . ?
C16 C15 C33 120.8(11) . . ?
C14 C15 C33 116.7(10) . . ?
C15 C16 N4 123.4(11) . . ?
C15 C16 C17 129.2(12) . . ?
N4 C16 C17 107.2(10) . . ?
C18 C17 C16 108.4(11) . . ?
C18 C17 Br7 124.3(10) . . ?
C16 C17 Br7 127.2(9) . . ?
C17 C18 C19 109.6(11) . . ?
C17 C18 Br8 122.3(10) . . ?
C19 C18 Br8 127.7(9) . . ?
C20 C19 N4 122.2(11) . . ?
C20 C19 C18 129.8(11) . . ?
N4 C19 C18 107.6(9) . . ?
C19 C20 C1 124.5(12) . . ?
C19 C20 C39 117.4(11) . . ?
C1 C20 C39 118.2(10) . . ?
C22 C21 C26 118.2(11) . . ?
C22 C21 C5 121.7(11) . . ?
C26 C21 C5 120.1(10) . . ?
C23 C22 C21 120.7(12) . . ?
C22 C23 C24 120.7(12) . . ?
C25 C24 C23 119.4(13) . . ?
C24 C25 C26 121.4(14) . . ?
C25 C26 C21 119.4(12) . . ?
C28 C27 C32 120.5(12) . . ?
C28 C27 C10 119.8(11) . . ?
C32 C27 C10 119.7(11) . . ?
C29 C28 C27 120.2(12) . . ?
C28 C29 C30 120.7(13) . . ?
C31 C30 C29 119.6(13) . . ?
C30 C31 C32 121.0(13) . . ?
C31 C32 C27 118.0(13) . . ?
C38 C33 C34 119.3(12) . . ?
C38 C33 C15 120.6(11) . . ?
C34 C33 C15 120.0(10) . . ?
C35 C34 C33 119.1(11) . . ?
C36 C35 C34 121.6(12) . . ?
C35 C36 C37 118.8(12) . . ?
C38 C37 C36 120.4(12) . . ?
C37 C38 C33 120.9(12) . . ?
C40 C39 C44 119.4(12) . . ?
C40 C39 C20 121.1(11) . . ?
C44 C39 C20 119.4(12) . . ?
C39 C40 C41 121.2(12) . . ?
C40 C41 C42 118.5(12) . . ?
C43 C42 C41 120.0(12) . . ?
C42 C43 C44 121.7(12) . . ?
C43 C44 C39 118.9(12) . . ?
C48 C47 C52 119.2(13) . . ?
C49 C48 C47 123.2(14) . . ?
C48 C49 C50 118.0(14) . . ?
C51 C50 C49 119.9(13) . . ?
C50 C51 C52 120.9(14) . . ?
C47 C52 C51 118.8(14) . . ?
O5 Cl1 O4 110.5(5) . . ?
O5 Cl1 O3 108.4(6) . . ?
O4 Cl1 O3 108.6(6) . . ?
O5 Cl1 O6 110.4(5) . . ?
O4 Cl1 O6 110.0(6) . . ?
O3 Cl1 O6 108.9(6) . . ?

_refine_diff_density_max         0.672
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.138


# start Validation Reply Form
_vrf_PLAT341_shelx               
;
PROBLEM: Low Bond Precision on  C-C Bonds ...............    0.01737 Ang.  
RESPONSE: The crystal was weakly diffracting and thus the quality of
data is relatively poor.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2247019'
loop_
_audit_author_name
_audit_author_address
'Sankar Rath'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2023-05-01 deposited with the CCDC.	2023-05-29 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         ?
_chemical_formula_sum            'C52 H40 Br8 Cl Fe N4 O8'
_chemical_formula_weight         1579.46

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   26.344(10)
_cell_length_b                   10.225(4)
_cell_length_c                   28.292(10)
_cell_angle_alpha                90
_cell_angle_beta                 115.931(7)
_cell_angle_gamma                90
_cell_volume                     6854(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.0

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_F_000             3068
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    4.968
_shelx_estimated_absorpt_T_min   0.523
_shelx_estimated_absorpt_T_max   0.636
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.480
_exptl_absorpt_correction_T_max  0.609
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   'SADABS 2.05 (Sheldrick, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            17748
_diffrn_reflns_av_unetI/netI     0.0912
_diffrn_reflns_av_R_equivalents  0.0697
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_theta_min         2.178
_diffrn_reflns_theta_max         25.498
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             6340
_reflns_number_gt                3540
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
The unit cell contains eight THF molecules which
have been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON.
 
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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1107P)²+3.8093P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6340
_refine_ls_number_parameters     302
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1180
_refine_ls_R_factor_gt           0.0696
_refine_ls_wR_factor_ref         0.2219
_refine_ls_wR_factor_gt          0.1943
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.500000 2.76730(16) 0.250000 0.0459(4) Uani 1 2 d S T P . .
N1 N 0.5303(3) 2.7720(7) 0.1955(2) 0.0528(18) Uani 1 1 d . . . . .
N2 N 0.4209(3) 2.7657(7) 0.1916(2) 0.0477(17) Uani 1 1 d . . . . .
O1 O 0.500000 2.5621(7) 0.250000 0.056(2) Uani 1 2 d DS T P . .
O2 O 0.500000 2.9748(9) 0.250000 0.082(3) Uani 1 2 d DS T P . .
Br1 Br 0.64183(4) 3.00172(10) 0.16899(4) 0.0712(4) Uani 1 1 d . . . . .
Br2 Br 0.50782(5) 2.98882(11) 0.06655(4) 0.0765(4) Uani 1 1 d . . . . .
Br3 Br 0.32773(5) 2.54754(12) 0.05935(4) 0.0802(4) Uani 1 1 d . . . . .
Br4 Br 0.27807(4) 2.54948(10) 0.15517(4) 0.0627(3) Uani 1 1 d . . . . .
C1 C 0.5847(4) 2.8143(8) 0.2094(3) 0.050(2) Uani 1 1 d . . . . .
C2 C 0.5835(4) 2.8918(9) 0.1672(3) 0.059(2) Uani 1 1 d . . . . .
C3 C 0.5315(3) 2.8869(9) 0.1274(3) 0.054(2) Uani 1 1 d . . . . .
C4 C 0.4973(4) 2.8086(8) 0.1447(3) 0.053(2) Uani 1 1 d . . . . .
C5 C 0.4424(4) 2.7637(9) 0.1162(3) 0.054(2) Uani 1 1 d . . . . .
C6 C 0.4089(3) 2.7231(8) 0.1414(3) 0.050(2) Uani 1 1 d . . . . .
C7 C 0.3584(3) 2.6477(8) 0.1218(3) 0.050(2) Uani 1 1 d . . . . .
C8 C 0.3371(3) 2.6529(8) 0.1573(3) 0.051(2) Uani 1 1 d . . . . .
C9 C 0.3766(4) 2.7267(8) 0.2010(3) 0.047(2) Uani 1 1 d . . . . .
C10 C 0.3692(4) 2.7732(8) 0.2439(3) 0.046(2) Uani 1 1 d . . . . .
C11 C 0.4178(3) 2.7637(8) 0.05795(19) 0.077(3) Uani 1 1 d G . . . .
C12 C 0.4466(3) 2.7021(8) 0.0331(3) 0.098(4) Uani 1 1 d G . . . .
H12A H 0.481311 2.658835 0.053395 0.118 Uiso 1 1 calc R U . . .
C13 C 0.4246(4) 2.7039(9) -0.0214(3) 0.135(5) Uani 1 1 d G U . . .
H13A H 0.444310 2.661864 -0.038350 0.162 Uiso 1 1 calc R U . . .
C14 C 0.3738(4) 2.7673(9) -0.05104(19) 0.131(6) Uani 1 1 d G U . . .
H14A H 0.358804 2.768491 -0.088291 0.157 Uiso 1 1 calc R U . . .
C15 C 0.3450(3) 2.8288(9) -0.0262(3) 0.139(6) Uani 1 1 d G U . . .
H15A H 0.310298 2.872091 -0.046487 0.167 Uiso 1 1 calc R U . . .
C16 C 0.3670(3) 2.8270(8) 0.0283(3) 0.110(5) Uani 1 1 d G . . . .
H16A H 0.347298 2.869065 0.045259 0.132 Uiso 1 1 calc R U . . .
C17 C 0.3114(4) 2.7787(8) 0.2423(3) 0.054(2) Uani 1 1 d . . . . .
C18 C 0.2991(4) 2.7169(9) 0.2788(4) 0.058(2) Uani 1 1 d . . . . .
H18A H 0.327204 2.667196 0.306094 0.070 Uiso 1 1 calc R U . . .
C19 C 0.2463(5) 2.7268(12) 0.2759(4) 0.079(3) Uani 1 1 d . . . . .
H19A H 0.237622 2.683797 0.301208 0.095 Uiso 1 1 calc R U . . .
C20 C 0.2055(4) 2.7984(10) 0.2367(4) 0.069(3) Uani 1 1 d . . . . .
H20A H 0.169086 2.807084 0.235519 0.083 Uiso 1 1 calc R U . . .
C21 C 0.2175(4) 2.8570(11) 0.1996(4) 0.069(3) Uani 1 1 d . . . . .
H21A H 0.188756 2.904789 0.172040 0.083 Uiso 1 1 calc R U . . .
C22 C 0.2691(3) 2.8486(9) 0.2011(3) 0.053(2) Uani 1 1 d . . . . .
H22A H 0.276811 2.889267 0.174815 0.063 Uiso 1 1 calc R U . . .
Cl1 Cl 0.4496(2) 3.4432(5) 0.3434(2) 0.0621(12) Uani 0.5 1 d . . P . .
O1S O 0.4382(7) 3.4254(17) 0.2915(6) 0.104(6) Uani 0.5 1 d . . P . .
O2S O 0.5088(6) 3.4662(14) 0.3640(8) 0.100(5) Uani 0.5 1 d . . P . .
O3S O 0.4419(7) 3.3145(15) 0.3573(6) 0.092(5) Uani 0.5 1 d . . P . .
O4S O 0.4219(8) 3.530(2) 0.3577(9) 0.137(8) Uani 0.5 1 d . . P . .
H1A H 0.518700 2.519200 0.243000 0.050 Uiso 1 1 d D . . . .
H2A H 0.469000 3.020200 0.232300 0.050 Uiso 1 1 d D . . . .


_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 2.015(6) 2_655 ?
Fe1 N2 2.015(6) . ?
Fe1 N1 2.024(7) . ?
Fe1 N1 2.024(7) 2_655 ?
Fe1 O1 2.098(8) . ?
Fe1 O2 2.122(9) . ?
N1 C4 1.366(10) . ?
N1 C1 1.378(10) . ?
N2 C9 1.362(10) . ?
N2 C6 1.386(10) . ?
Br1 C2 1.886(9) . ?
Br2 C3 1.871(8) . ?
Br3 C7 1.891(8) . ?
Br4 C8 1.859(8) . ?
C1 C10 1.413(11) 2_655 ?
C1 C2 1.422(11) . ?
C2 C3 1.340(11) . ?
C3 C4 1.442(11) . ?
C4 C5 1.390(11) . ?
C5 C6 1.416(12) . ?
C5 C11 1.485(9) . ?
C6 C7 1.424(11) . ?
C7 C8 1.349(12) . ?
C8 C9 1.434(11) . ?
C9 C10 1.396(11) . ?
C10 C17 1.503(12) . ?
C11 C12 1.3900 . ?
C11 C16 1.3900 . ?
C12 C13 1.3900 . ?
C13 C14 1.3900 . ?
C14 C15 1.3900 . ?
C15 C16 1.3900 . ?
C17 C18 1.365(12) . ?
C17 C22 1.406(11) . ?
C18 C19 1.360(13) . ?
C19 C20 1.369(15) . ?
C20 C21 1.360(14) . ?
C21 C22 1.344(12) . ?
Cl1 O4S 1.32(3) . ?
Cl1 O1S 1.376(14) . ?
Cl1 O3S 1.413(14) . ?
Cl1 O2S 1.426(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Fe1 N2 179.1(4) 2_655 . ?
N2 Fe1 N1 90.8(3) 2_655 . ?
N2 Fe1 N1 89.3(3) . . ?
N2 Fe1 N1 89.3(3) 2_655 2_655 ?
N2 Fe1 N1 90.8(3) . 2_655 ?
N1 Fe1 N1 177.3(4) . 2_655 ?
N2 Fe1 O1 89.53(19) 2_655 . ?
N2 Fe1 O1 89.53(19) . . ?
N1 Fe1 O1 91.3(2) . . ?
N1 Fe1 O1 91.3(2) 2_655 . ?
N2 Fe1 O2 90.47(19) 2_655 . ?
N2 Fe1 O2 90.47(19) . . ?
N1 Fe1 O2 88.7(2) . . ?
N1 Fe1 O2 88.7(2) 2_655 . ?
O1 Fe1 O2 180.0 . . ?
C4 N1 C1 108.6(7) . . ?
C4 N1 Fe1 121.7(6) . . ?
C1 N1 Fe1 119.8(5) . . ?
C9 N2 C6 106.1(7) . . ?
C9 N2 Fe1 120.7(5) . . ?
C6 N2 Fe1 122.2(6) . . ?
N1 C1 C10 122.4(7) . 2_655 ?
N1 C1 C2 107.3(7) . . ?
C10 C1 C2 130.2(8) 2_655 . ?
C3 C2 C1 108.8(8) . . ?
C3 C2 Br1 124.5(7) . . ?
C1 C2 Br1 126.2(6) . . ?
C2 C3 C4 107.3(8) . . ?
C2 C3 Br2 124.0(7) . . ?
C4 C3 Br2 127.9(6) . . ?
N1 C4 C5 122.8(7) . . ?
N1 C4 C3 107.7(7) . . ?
C5 C4 C3 129.3(8) . . ?
C4 C5 C6 121.6(7) . . ?
C4 C5 C11 118.9(7) . . ?
C6 C5 C11 119.4(7) . . ?
N2 C6 C5 120.7(7) . . ?
N2 C6 C7 108.8(7) . . ?
C5 C6 C7 130.2(7) . . ?
C8 C7 C6 108.2(7) . . ?
C8 C7 Br3 124.7(6) . . ?
C6 C7 Br3 126.9(6) . . ?
C7 C8 C9 106.2(7) . . ?
C7 C8 Br4 124.6(6) . . ?
C9 C8 Br4 127.6(7) . . ?
N2 C9 C10 121.8(7) . . ?
N2 C9 C8 110.4(7) . . ?
C10 C9 C8 127.1(8) . . ?
C9 C10 C1 121.6(8) . 2_655 ?
C9 C10 C17 120.9(7) . . ?
C1 C10 C17 117.5(7) 2_655 . ?
C12 C11 C16 120.0 . . ?
C12 C11 C5 119.4(6) . . ?
C16 C11 C5 120.6(6) . . ?
C13 C12 C11 120.0 . . ?
C14 C13 C12 120.0 . . ?
C13 C14 C15 120.0 . . ?
C16 C15 C14 120.0 . . ?
C15 C16 C11 120.0 . . ?
C18 C17 C22 119.8(9) . . ?
C18 C17 C10 122.2(8) . . ?
C22 C17 C10 118.0(8) . . ?
C19 C18 C17 119.6(10) . . ?
C18 C19 C20 120.6(11) . . ?
C21 C20 C19 119.7(10) . . ?
C22 C21 C20 121.2(9) . . ?
C21 C22 C17 119.0(9) . . ?
O4S Cl1 O1S 121.5(14) . . ?
O4S Cl1 O3S 112.2(12) . . ?
O1S Cl1 O3S 100.5(10) . . ?
O4S Cl1 O2S 114.5(12) . . ?
O1S Cl1 O2S 98.4(10) . . ?
O3S Cl1 O2S 107.7(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
O1 H1A O1S 0.75 2.03 2.768(13) 167.1 2_645 yes

_refine_diff_density_max         0.847
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.144



# start Validation Reply Form
_vrf_PLAT420_shelx               
;
PROBLEM: D-H Bond Without Acceptor  O2       --H2A      .     Please Check 
RESPONSE: The oxygen atom of the unbound THF solvent molecule has been 
the acceptor. However, the THF was removed using SQUEEZE routine of PLATON 
since the solvent molecule was highly disordered.  
;
# end Validation Reply Form
####################################################################### 
# 
# 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_shelx_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 2247018'
loop_
_audit_author_name
_audit_author_address
'Sankar Rath'
;Indian Institute of Technology Kanpur
India
;
_audit_update_record             
;
2023-05-01 deposited with the CCDC.	2023-05-29 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         ?
_chemical_formula_sum            'C64 H44 Br8 Fe N8'
_chemical_formula_weight         1620.20

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   13.733(5)
_cell_length_b                   15.553(6)
_cell_length_c                   15.799(6)
_cell_angle_alpha                86.173(7)
_cell_angle_beta                 73.994(7)
_cell_angle_gamma                77.696(8)
_cell_volume                     3169(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    999
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      27.5

_exptl_crystal_description       block
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_F_000             1580
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    5.327
_shelx_estimated_absorpt_T_min   0.483
_shelx_estimated_absorpt_T_max   0.618
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.430
_exptl_absorpt_correction_T_max  0.587
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   'SADABS 2.05 (Sheldrick, 2002)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16764
_diffrn_reflns_av_unetI/netI     0.1474
_diffrn_reflns_av_R_equivalents  0.0610
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.014
_diffrn_reflns_theta_max         25.500
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.977
_reflns_number_total             11498
_reflns_number_gt                6293
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
The unit cell contains four C6H6 molecules which
have been treated as a diffuse contribution to the overall
scattering without specific atom positions by SQUEEZE/PLATON. 

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'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'SHELXL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL-97
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1214P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11498
_refine_ls_number_parameters     558
_refine_ls_number_restraints     40
_refine_ls_R_factor_all          0.1303
_refine_ls_R_factor_gt           0.0758
_refine_ls_wR_factor_ref         0.2328
_refine_ls_wR_factor_gt          0.1962
_refine_ls_goodness_of_fit_ref   0.961
_refine_ls_restrained_S_all      0.963
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br -0.32651(8) 0.32347(7) 0.99978(8) 0.0384(3) Uani 1 1 d . . . . .
Br2 Br -0.24827(8) 0.23406(8) 0.79424(9) 0.0483(4) Uani 1 1 d . . . . .
Br3 Br 0.16883(8) -0.04170(7) 0.65807(9) 0.0438(4) Uani 1 1 d . . . . .
Br4 Br 0.41062(8) 0.00169(7) 0.62639(8) 0.0434(3) Uani 1 1 d . . . . .
Br5 Br 0.49704(8) 0.36506(7) 0.71180(7) 0.0375(3) Uani 1 1 d . . . . .
Br6 Br 0.43003(8) 0.44397(7) 0.92145(8) 0.0396(3) Uani 1 1 d . . . . .
Br7 Br 0.17043(9) 0.27675(8) 1.26023(8) 0.0424(3) Uani 1 1 d . . . . .
Br8 Br -0.07467(9) 0.24592(7) 1.28794(8) 0.0407(3) Uani 1 1 d . . . . .
Fe1 Fe 0.12938(10) 0.23174(8) 0.90439(10) 0.0247(4) Uani 1 1 d . . . . .
N1 N -0.0130(6) 0.2176(5) 0.9160(6) 0.0254(19) Uani 1 1 d . . . . .
N2 N 0.1761(5) 0.1776(5) 0.7857(5) 0.0236(19) Uani 1 1 d . . . . .
N3 N 0.2687(6) 0.2595(5) 0.8882(5) 0.028(2) Uani 1 1 d . . . . .
N4 N 0.0888(6) 0.2719(5) 1.0270(6) 0.028(2) Uani 1 1 d . . . . .
C1 C -0.0993(7) 0.2545(6) 0.9831(7) 0.029(2) Uani 1 1 d . . . . .
C2 C -0.1901(7) 0.2638(6) 0.9490(8) 0.033(3) Uani 1 1 d . . . . .
C3 C -0.1594(7) 0.2262(6) 0.8665(8) 0.031(3) Uani 1 1 d . . . . .
C4 C -0.0489(7) 0.1957(6) 0.8487(7) 0.029(3) Uani 1 1 d . . . . .
C5 C 0.0126(7) 0.1408(6) 0.7795(7) 0.024(2) Uani 1 1 d . U . . .
C6 C 0.1213(7) 0.1255(6) 0.7589(7) 0.028(2) Uani 1 1 d . . . . .
C7 C 0.1941(7) 0.0592(6) 0.6991(8) 0.032(3) Uani 1 1 d . U . . .
C8 C 0.2895(7) 0.0762(6) 0.6878(7) 0.029(2) Uani 1 1 d . . . . .
C9 C 0.2775(7) 0.1526(6) 0.7391(7) 0.025(2) Uani 1 1 d . . . . .
C10 C 0.3540(7) 0.2006(6) 0.7387(7) 0.029(2) Uani 1 1 d . . . . .
C11 C 0.3412(7) 0.2580(6) 0.8071(7) 0.025(2) Uani 1 1 d . . . . .
C12 C 0.4046(7) 0.3209(6) 0.8100(7) 0.028(2) Uani 1 1 d . . . . .
C13 C 0.3743(7) 0.3536(6) 0.8883(7) 0.031(3) Uani 1 1 d . . . . .
C14 C 0.2905(7) 0.3143(6) 0.9415(7) 0.031(3) Uani 1 1 d . . . . .
C15 C 0.2478(7) 0.3166(6) 1.0321(6) 0.026(2) Uani 1 1 d . . . . .
C16 C 0.1563(8) 0.2873(6) 1.0739(7) 0.030(2) Uani 1 1 d . . . . .
C17 C 0.1096(8) 0.2799(6) 1.1680(7) 0.031(2) Uani 1 1 d . . . . .
C18 C 0.0127(8) 0.2654(6) 1.1766(7) 0.031(3) Uani 1 1 d . . . . .
C19 C -0.0039(7) 0.2640(6) 1.0897(7) 0.033(3) Uani 1 1 d . . . . .
C20 C -0.0951(7) 0.2665(6) 1.0696(7) 0.027(2) Uani 1 1 d . . . . .
C21 C -0.1948(4) 0.2858(4) 1.1412(4) 0.035(3) Uani 1 1 d G . . . .
C22 C -0.2361(5) 0.3711(4) 1.1720(5) 0.039(3) Uani 1 1 d G . . . .
H22A H -0.203244 0.417894 1.145865 0.047 Uiso 1 1 calc R U . . .
C23 C -0.3256(5) 0.3878(4) 1.2411(5) 0.045(3) Uani 1 1 d G . . . .
H23A H -0.353897 0.446125 1.262217 0.054 Uiso 1 1 calc R U . . .
C24 C -0.3738(4) 0.3193(5) 1.2794(4) 0.057(4) Uani 1 1 d G . . . .
H24A H -0.434934 0.330779 1.326652 0.068 Uiso 1 1 calc R U . . .
C25 C -0.3324(5) 0.2340(5) 1.2486(5) 0.054(4) Uani 1 1 d G . . . .
H25A H -0.365316 0.187202 1.274736 0.065 Uiso 1 1 calc R U . . .
C26 C -0.2429(5) 0.2173(4) 1.1795(5) 0.045(3) Uani 1 1 d G . . . .
H26A H -0.214662 0.158970 1.158384 0.054 Uiso 1 1 calc R U . . .
C27 C -0.0380(5) 0.0964(4) 0.7265(5) 0.043(3) Uani 1 1 d G . . . .
C28 C -0.0852(6) 0.0270(5) 0.7634(5) 0.050(4) Uani 1 1 d G . . . .
H28A H -0.091250 0.011463 0.823594 0.060 Uiso 1 1 calc R U . . .
C29 C -0.1236(6) -0.0198(4) 0.7124(7) 0.072(5) Uani 1 1 d G . . . .
H29A H -0.155914 -0.067194 0.737707 0.086 Uiso 1 1 calc R U . . .
C30 C -0.1148(6) 0.0029(6) 0.6244(6) 0.094(7) Uani 1 1 d G . . . .
H30A H -0.141096 -0.029021 0.589556 0.112 Uiso 1 1 calc R U . . .
C31 C -0.0676(6) 0.0723(6) 0.5874(5) 0.075(5) Uani 1 1 d G . . . .
H31A H -0.061615 0.087811 0.527291 0.090 Uiso 1 1 calc R U . . .
C32 C -0.0292(5) 0.1190(4) 0.6385(5) 0.049(3) Uani 1 1 d G . . . .
H32A H 0.003050 0.166469 0.613177 0.059 Uiso 1 1 calc R U . . .
C33 C 0.4543(4) 0.1826(5) 0.6715(5) 0.040(3) Uani 1 1 d G . . . .
C34 C 0.4612(6) 0.1995(6) 0.5827(5) 0.068(5) Uani 1 1 d G . . . .
H34A H 0.400250 0.221008 0.564135 0.082 Uiso 1 1 calc R U . . .
C35 C 0.5573(9) 0.1847(7) 0.5212(5) 0.081(6) Uani 1 1 d G . . . .
H35A H 0.561989 0.196237 0.460536 0.097 Uiso 1 1 calc R U . . .
C36 C 0.6465(6) 0.1532(7) 0.5484(7) 0.098(7) Uani 1 1 d G . . . .
H36A H 0.712142 0.143163 0.506356 0.117 Uiso 1 1 calc R U . . .
C37 C 0.6396(5) 0.1364(6) 0.6372(8) 0.096(6) Uani 1 1 d G U . . .
H37A H 0.700558 0.114859 0.655774 0.115 Uiso 1 1 calc R U . . .
C38 C 0.5435(6) 0.1511(5) 0.6987(5) 0.058(4) Uani 1 1 d G . . . .
H38A H 0.538819 0.139629 0.759374 0.070 Uiso 1 1 calc R U . . .
C39 C 0.2964(5) 0.3601(5) 1.0882(5) 0.036(3) Uani 1 1 d G . . . .
C40 C 0.3887(5) 0.3169(5) 1.1053(5) 0.047(3) Uani 1 1 d G . . . .
H40A H 0.421557 0.260325 1.081260 0.056 Uiso 1 1 calc R U . . .
C41 C 0.4329(5) 0.3563(7) 1.1577(5) 0.066(5) Uani 1 1 d G . . . .
H41A H 0.495906 0.326797 1.169381 0.079 Uiso 1 1 calc R U . . .
C42 C 0.3848(7) 0.4391(7) 1.1929(5) 0.074(5) Uani 1 1 d G . . . .
H42A H 0.414942 0.466055 1.228697 0.089 Uiso 1 1 calc R U . . .
C43 C 0.2925(7) 0.4823(5) 1.1758(5) 0.058(4) Uani 1 1 d G . . . .
H43A H 0.259628 0.538841 1.199892 0.070 Uiso 1 1 calc R U . . .
C44 C 0.2483(5) 0.4428(5) 1.1235(5) 0.048(3) Uani 1 1 d G . . . .
H44A H 0.185276 0.472370 1.111773 0.057 Uiso 1 1 calc R U . . .
N5 N 0.1706(6) 0.1107(4) 0.9468(6) 0.046(3) Uani 1 1 d G U . . .
C45 C 0.1036(6) 0.0524(5) 0.9859(8) 0.083(5) Uani 1 1 d G U . . .
H45A H 0.030506 0.067972 1.007619 0.100 Uiso 1 1 calc R U . . .
C46 C 0.1652(9) -0.0333(4) 0.9869(8) 0.102(7) Uani 1 1 d G U . . .
H46A H 0.140492 -0.085146 1.009422 0.123 Uiso 1 1 calc R U . . .
N6 N 0.2702(7) -0.0280(5) 0.9484(9) 0.131(7) Uani 1 1 d G U . . .
C47 C 0.2735(5) 0.0610(6) 0.9236(9) 0.110(7) Uani 1 1 d G U . . .
H47A H 0.334001 0.083364 0.896351 0.131 Uiso 1 1 calc R U . . .
C48 C 0.3561(17) -0.0944(11) 0.9279(17) 0.146(10) Uani 1 1 d . . . . .
H48A H 0.417884 -0.069056 0.905102 0.219 Uiso 1 1 calc R U . . .
H48B H 0.350090 -0.132048 0.883061 0.219 Uiso 1 1 calc R U . . .
H48C H 0.361635 -0.129443 0.980876 0.219 Uiso 1 1 calc R U . . .
N7 N 0.0914(5) 0.3491(3) 0.8571(4) 0.0256(19) Uani 1 1 d G . . . .
C49 C 0.0420(6) 0.4268(4) 0.9066(4) 0.049(3) Uani 1 1 d G U . . .
H49A H 0.018269 0.430371 0.968917 0.059 Uiso 1 1 calc R U . . .
C50 C 0.0343(6) 0.4983(3) 0.8464(5) 0.041(3) Uani 1 1 d G . . . .
H50A H 0.004487 0.558136 0.861420 0.050 Uiso 1 1 calc R U . . .
N8 N 0.0789(7) 0.4648(4) 0.7598(4) 0.067(3) Uani 1 1 d G . . . .
C51 C 0.1142(7) 0.3725(4) 0.7664(4) 0.067(4) Uani 1 1 d G . . . .
H51A H 0.147212 0.333371 0.718593 0.080 Uiso 1 1 calc R U . . .
C52 C 0.0934(19) 0.5142(10) 0.6823(11) 0.125(8) Uani 1 1 d . U . . .
H52A H 0.085653 0.576162 0.696268 0.188 Uiso 1 1 calc R U . . .
H52B H 0.041878 0.508501 0.651887 0.188 Uiso 1 1 calc R U . . .
H52C H 0.163005 0.492742 0.644230 0.188 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 C2 1.882(10) . ?
Br2 C3 1.868(11) . ?
Br3 C7 1.869(9) . ?
Br4 C8 1.867(9) . ?
Br5 C12 1.906(9) . ?
Br6 C13 1.901(10) . ?
Br7 C17 1.862(11) . ?
Br8 C18 1.883(10) . ?
Fe1 N7 1.946(5) . ?
Fe1 N4 1.968(9) . ?
Fe1 N1 1.971(7) . ?
Fe1 N5 1.975(6) . ?
Fe1 N2 1.989(8) . ?
Fe1 N3 1.995(8) . ?
N1 C4 1.377(13) . ?
N1 C1 1.399(12) . ?
N2 C9 1.369(11) . ?
N2 C6 1.374(11) . ?
N3 C14 1.367(12) . ?
N3 C11 1.387(12) . ?
N4 C16 1.400(13) . ?
N4 C19 1.405(12) . ?
C1 C20 1.410(15) . ?
C1 C2 1.466(14) . ?
C2 C3 1.384(14) . ?
C3 C4 1.444(12) . ?
C4 C5 1.395(13) . ?
C5 C6 1.408(13) . ?
C5 C27 1.505(10) . ?
C6 C7 1.458(13) . ?
C7 C8 1.353(13) . ?
C8 C9 1.437(12) . ?
C9 C10 1.411(12) . ?
C10 C11 1.398(13) . ?
C10 C33 1.474(11) . ?
C11 C12 1.453(12) . ?
C12 C13 1.293(14) . ?
C13 C14 1.449(13) . ?
C14 C15 1.389(14) . ?
C15 C16 1.403(13) . ?
C15 C39 1.512(11) . ?
C16 C17 1.456(14) . ?
C17 C18 1.366(14) . ?
C18 C19 1.454(15) . ?
C19 C20 1.367(14) . ?
C20 C21 1.504(11) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22A 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23A 0.9500 . ?
C24 C25 1.3900 . ?
C24 H24A 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25A 0.9500 . ?
C26 H26A 0.9500 . ?
C27 C28 1.3900 . ?
C27 C32 1.3900 . ?
C28 C29 1.3900 . ?
C28 H28A 0.9500 . ?
C29 C30 1.3900 . ?
C29 H29A 0.9500 . ?
C30 C31 1.3900 . ?
C30 H30A 0.9500 . ?
C31 C32 1.3900 . ?
C31 H31A 0.9500 . ?
C32 H32A 0.9500 . ?
C33 C34 1.3900 . ?
C33 C38 1.3900 . ?
C34 C35 1.3900 . ?
C34 H34A 0.9500 . ?
C35 C36 1.3900 . ?
C35 H35A 0.9500 . ?
C36 C37 1.3900 . ?
C36 H36A 0.9500 . ?
C37 C38 1.3900 . ?
C37 H37A 0.9500 . ?
C38 H38A 0.9500 . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C40 C41 1.3900 . ?
C40 H40A 0.9500 . ?
C41 C42 1.3900 . ?
C41 H41A 0.9500 . ?
C42 C43 1.3900 . ?
C42 H42A 0.9500 . ?
C43 C44 1.3900 . ?
C43 H43A 0.9500 . ?
C44 H44A 0.9500 . ?
N5 C47 1.4200 . ?
N5 C45 1.4200 . ?
C45 C46 1.4200 . ?
C45 H45A 0.9500 . ?
C46 N6 1.4200 . ?
C46 H46A 0.9500 . ?
N6 C48 1.369(18) . ?
N6 C47 1.4200 . ?
C47 H47A 0.9500 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N7 C49 1.4200 . ?
N7 C51 1.4200 . ?
C49 C50 1.4200 . ?
C49 H49A 0.9500 . ?
C50 N8 1.4200 . ?
C50 H50A 0.9500 . ?
N8 C52 1.390(16) . ?
N8 C51 1.4200 . ?
C51 H51A 0.9500 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N7 Fe1 N4 93.9(3) . . ?
N7 Fe1 N1 87.7(3) . . ?
N4 Fe1 N1 90.3(3) . . ?
N7 Fe1 N5 177.4(3) . . ?
N4 Fe1 N5 88.7(4) . . ?
N1 Fe1 N5 92.6(3) . . ?
N7 Fe1 N2 92.6(3) . . ?
N4 Fe1 N2 173.5(3) . . ?
N1 Fe1 N2 90.5(3) . . ?
N5 Fe1 N2 84.8(3) . . ?
N7 Fe1 N3 86.1(3) . . ?
N4 Fe1 N3 89.7(3) . . ?
N1 Fe1 N3 173.8(3) . . ?
N5 Fe1 N3 93.7(3) . . ?
N2 Fe1 N3 90.2(3) . . ?
C4 N1 C1 107.3(8) . . ?
C4 N1 Fe1 125.3(6) . . ?
C1 N1 Fe1 124.5(6) . . ?
C9 N2 C6 107.3(7) . . ?
C9 N2 Fe1 124.4(6) . . ?
C6 N2 Fe1 122.2(6) . . ?
C14 N3 C11 107.5(8) . . ?
C14 N3 Fe1 124.2(6) . . ?
C11 N3 Fe1 123.3(6) . . ?
C16 N4 C19 106.6(9) . . ?
C16 N4 Fe1 125.7(6) . . ?
C19 N4 Fe1 125.1(7) . . ?
N1 C1 C20 123.3(9) . . ?
N1 C1 C2 107.1(9) . . ?
C20 C1 C2 129.0(9) . . ?
C3 C2 C1 108.8(8) . . ?
C3 C2 Br1 122.7(8) . . ?
C1 C2 Br1 128.3(8) . . ?
C2 C3 C4 105.2(9) . . ?
C2 C3 Br2 122.9(7) . . ?
C4 C3 Br2 131.2(8) . . ?
N1 C4 C5 123.2(9) . . ?
N1 C4 C3 111.2(9) . . ?
C5 C4 C3 125.1(9) . . ?
C4 C5 C6 121.1(8) . . ?
C4 C5 C27 119.6(8) . . ?
C6 C5 C27 119.3(8) . . ?
N2 C6 C5 124.5(8) . . ?
N2 C6 C7 108.5(8) . . ?
C5 C6 C7 126.7(9) . . ?
C8 C7 C6 107.1(8) . . ?
C8 C7 Br3 124.2(7) . . ?
C6 C7 Br3 128.1(7) . . ?
C7 C8 C9 107.2(8) . . ?
C7 C8 Br4 123.1(7) . . ?
C9 C8 Br4 129.3(7) . . ?
N2 C9 C10 123.2(8) . . ?
N2 C9 C8 109.6(7) . . ?
C10 C9 C8 127.1(9) . . ?
C11 C10 C9 120.9(9) . . ?
C11 C10 C33 118.6(8) . . ?
C9 C10 C33 120.0(8) . . ?
N3 C11 C10 124.9(8) . . ?
N3 C11 C12 107.6(8) . . ?
C10 C11 C12 127.3(9) . . ?
C13 C12 C11 107.7(8) . . ?
C13 C12 Br5 124.9(7) . . ?
C11 C12 Br5 126.4(8) . . ?
C12 C13 C14 109.6(9) . . ?
C12 C13 Br6 122.9(7) . . ?
C14 C13 Br6 127.4(8) . . ?
N3 C14 C15 122.5(9) . . ?
N3 C14 C13 107.3(9) . . ?
C15 C14 C13 129.4(9) . . ?
C14 C15 C16 123.2(9) . . ?
C14 C15 C39 118.7(8) . . ?
C16 C15 C39 117.8(8) . . ?
N4 C16 C15 122.0(9) . . ?
N4 C16 C17 109.8(8) . . ?
C15 C16 C17 127.7(9) . . ?
C18 C17 C16 106.1(9) . . ?
C18 C17 Br7 124.9(8) . . ?
C16 C17 Br7 128.6(7) . . ?
C17 C18 C19 109.2(9) . . ?
C17 C18 Br8 121.1(8) . . ?
C19 C18 Br8 129.6(7) . . ?
C20 C19 N4 124.0(10) . . ?
C20 C19 C18 127.7(9) . . ?
N4 C19 C18 107.9(9) . . ?
C19 C20 C1 122.2(9) . . ?
C19 C20 C21 119.2(9) . . ?
C1 C20 C21 118.6(8) . . ?
C22 C21 C26 120.0 . . ?
C22 C21 C20 120.2(5) . . ?
C26 C21 C20 119.7(5) . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22A 120.0 . . ?
C23 C22 H22A 120.0 . . ?
C22 C23 C24 120.0 . . ?
C22 C23 H23A 120.0 . . ?
C24 C23 H23A 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24A 120.0 . . ?
C23 C24 H24A 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25A 120.0 . . ?
C26 C25 H25A 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26A 120.0 . . ?
C21 C26 H26A 120.0 . . ?
C28 C27 C32 120.0 . . ?
C28 C27 C5 119.6(6) . . ?
C32 C27 C5 120.1(6) . . ?
C27 C28 C29 120.0 . . ?
C27 C28 H28A 120.0 . . ?
C29 C28 H28A 120.0 . . ?
C28 C29 C30 120.0 . . ?
C28 C29 H29A 120.0 . . ?
C30 C29 H29A 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30A 120.0 . . ?
C31 C30 H30A 120.0 . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31A 120.0 . . ?
C30 C31 H31A 120.0 . . ?
C31 C32 C27 120.0 . . ?
C31 C32 H32A 120.0 . . ?
C27 C32 H32A 120.0 . . ?
C34 C33 C38 120.0 . . ?
C34 C33 C10 121.3(7) . . ?
C38 C33 C10 118.7(7) . . ?
C33 C34 C35 120.0 . . ?
C33 C34 H34A 120.0 . . ?
C35 C34 H34A 120.0 . . ?
C34 C35 C36 120.0 . . ?
C34 C35 H35A 120.0 . . ?
C36 C35 H35A 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36A 120.0 . . ?
C35 C36 H36A 120.0 . . ?
C36 C37 C38 120.0 . . ?
C36 C37 H37A 120.0 . . ?
C38 C37 H37A 120.0 . . ?
C37 C38 C33 120.0 . . ?
C37 C38 H38A 120.0 . . ?
C33 C38 H38A 120.0 . . ?
C40 C39 C44 120.0 . . ?
C40 C39 C15 119.9(6) . . ?
C44 C39 C15 120.1(6) . . ?
C39 C40 C41 120.0 . . ?
C39 C40 H40A 120.0 . . ?
C41 C40 H40A 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 H41A 120.0 . . ?
C40 C41 H41A 120.0 . . ?
C41 C42 C43 120.0 . . ?
C41 C42 H42A 120.0 . . ?
C43 C42 H42A 120.0 . . ?
C42 C43 C44 120.0 . . ?
C42 C43 H43A 120.0 . . ?
C44 C43 H43A 120.0 . . ?
C43 C44 C39 120.0 . . ?
C43 C44 H44A 120.0 . . ?
C39 C44 H44A 120.0 . . ?
C47 N5 C45 108.0 . . ?
C47 N5 Fe1 123.9(5) . . ?
C45 N5 Fe1 126.5(5) . . ?
N5 C45 C46 108.0 . . ?
N5 C45 H45A 126.0 . . ?
C46 C45 H45A 126.0 . . ?
N6 C46 C45 108.0 . . ?
N6 C46 H46A 126.0 . . ?
C45 C46 H46A 126.0 . . ?
C48 N6 C46 129.2(12) . . ?
C48 N6 C47 122.5(12) . . ?
C46 N6 C47 108.0 . . ?
N5 C47 N6 108.0 . . ?
N5 C47 H47A 126.0 . . ?
N6 C47 H47A 126.0 . . ?
N6 C48 H48A 109.5 . . ?
N6 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
N6 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C49 N7 C51 108.0 . . ?
C49 N7 Fe1 126.5(4) . . ?
C51 N7 Fe1 125.4(4) . . ?
C50 C49 N7 108.0 . . ?
C50 C49 H49A 126.0 . . ?
N7 C49 H49A 126.0 . . ?
C49 C50 N8 108.0 . . ?
C49 C50 H50A 126.0 . . ?
N8 C50 H50A 126.0 . . ?
C52 N8 C50 126.1(9) . . ?
C52 N8 C51 125.7(9) . . ?
C50 N8 C51 108.0 . . ?
N8 C51 N7 108.0 . . ?
N8 C51 H51A 126.0 . . ?
N7 C51 H51A 126.0 . . ?
N8 C52 H52A 109.5 . . ?
N8 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N8 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?

_refine_diff_density_max         1.464
_refine_diff_density_min         -1.143
_refine_diff_density_rms         0.205



# start Validation Reply Form
_vrf_PLAT220_shelx               
;
PROBLEM: NonSolvent   Resd 1  C   Ueq(max)/Ueq(min) Range        6.1 Ratio 
RESPONSE: The crystal was weakly diffracting and thus the quality of
data is relatively poor. The terminal methyl group attached to the 
imidazole ring can rotate freely and thus has positional disorder which 
could not be resolved properly.
;
# end Validation Reply Form
