# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_2a
_database_code_depnum_ccdc_archive 'CCDC 1547031'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_shelx               
;
PROBLEM: Atom F4AA            has ADP max/min Ratio .....        4.2 prolat
RESPONSE: These fluorine atoms belong to the CF3 groups in the
BARF ion, which are very disordered. The regular disorder modeling did
not improve the situation.
;
# end Validation Reply Form 
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C65 H38 B F24 Fe N2 O3 P S'
_chemical_formula_sum            'C65 H38 B F24 Fe N2 O3 P S'
_chemical_formula_weight         1480.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0090 0.0039 '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                   12.3336(6)
_cell_length_b                   13.7435(6)
_cell_length_c                   19.1836(8)
_cell_angle_alpha                82.349(4)
_cell_angle_beta                 76.412(4)
_cell_angle_gamma                86.564(4)
_cell_volume                     3131.2(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    6749
_cell_measurement_theta_min      3.9050
_cell_measurement_theta_max      73.8420

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.570
_exptl_crystal_F_000             1488
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.115
_exptl_crystal_size_mid          0.077
_exptl_crystal_size_min          0.056
_exptl_absorpt_coefficient_mu    3.575
_shelx_estimated_absorpt_T_min   0.684
_shelx_estimated_absorpt_T_max   0.825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.70516
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22438
_diffrn_reflns_av_unetI/netI     0.0700
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         3.689
_diffrn_reflns_theta_max         74.304
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12346
_reflns_number_gt                9266
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_structure_solution    
;
SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_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)+(0.0510P)²+0.4400P] 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         12344
_refine_ls_number_parameters     935
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0505
_refine_ls_wR_factor_ref         0.1348
_refine_ls_wR_factor_gt          0.1190
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_restrained_S_all      1.067
_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
C1 C 0.4926(3) 0.4435(2) 0.16587(17) 0.0346(7) Uani 1 1 d . . . . .
C2 C 0.5161(3) 0.5234(2) 0.19751(19) 0.0387(7) Uani 1 1 d . . . . .
H2 H 0.5357 0.5848 0.1694 0.046 Uiso 1 1 calc R U . . .
C3 C 0.5100(3) 0.5102(3) 0.27004(19) 0.0414(8) Uani 1 1 d . . . . .
H3 H 0.5311 0.5610 0.2928 0.050 Uiso 1 1 calc R U . . .
C4 C 0.4726(3) 0.4218(2) 0.31063(18) 0.0364(7) Uani 1 1 d . . . . .
H4 H 0.4687 0.4122 0.3611 0.044 Uiso 1 1 calc R U . . .
C5 C 0.4409(2) 0.3479(2) 0.27759(16) 0.0292(6) Uani 1 1 d . . . . .
C6 C 0.3752(2) 0.2662(2) 0.32385(16) 0.0297(6) Uani 1 1 d . . . . .
C7 C 0.3046(3) 0.2892(2) 0.38917(16) 0.0345(7) Uani 1 1 d . . . . .
H7 H 0.3033 0.3540 0.4016 0.041 Uiso 1 1 calc R U . . .
C8 C 0.2375(3) 0.2200(3) 0.43555(18) 0.0417(8) Uani 1 1 d . . . . .
H8 H 0.1922 0.2373 0.4797 0.050 Uiso 1 1 calc R U . . .
C9 C 0.2355(3) 0.1259(3) 0.41830(19) 0.0440(8) Uani 1 1 d . . . . .
H9 H 0.1887 0.0787 0.4502 0.053 Uiso 1 1 calc R U . . .
C10 C 0.3019(3) 0.1011(3) 0.35448(18) 0.0404(7) Uani 1 1 d . . . . .
H10 H 0.3001 0.0367 0.3419 0.048 Uiso 1 1 calc R U . . .
C11 C 0.3717(3) 0.1701(2) 0.30813(16) 0.0315(6) Uani 1 1 d . . . . .
C12 C 0.5919(3) 0.1209(3) 0.2583(2) 0.0497(9) Uani 1 1 d . . . . .
H12A H 0.6091 0.1861 0.2674 0.075 Uiso 1 1 calc R U . . .
H12B H 0.6515 0.0981 0.2199 0.075 Uiso 1 1 calc R U . . .
H12C H 0.5861 0.0748 0.3025 0.075 Uiso 1 1 calc R U . . .
C13 C 0.4823(3) 0.3670(2) 0.06297(17) 0.0353(7) Uani 1 1 d . . . . .
C14 C 0.6125(3) 0.2527(2) 0.11568(18) 0.0400(7) Uani 1 1 d . . . . .
C15 C 0.4652(3) 0.1719(2) 0.07144(17) 0.0358(7) Uani 1 1 d . . . . .
C16 C 0.1955(2) 0.3462(2) 0.22064(15) 0.0279(6) Uani 1 1 d . . . . .
C17 C 0.2210(3) 0.4437(2) 0.22124(17) 0.0330(6) Uani 1 1 d . . . . .
H17 H 0.2757 0.4750 0.1827 0.040 Uiso 1 1 calc R U . . .
C18 C 0.1673(3) 0.4954(2) 0.27763(19) 0.0396(7) Uani 1 1 d . . . . .
H18 H 0.1843 0.5620 0.2771 0.048 Uiso 1 1 calc R U . . .
C19 C 0.0888(3) 0.4500(3) 0.33465(18) 0.0413(8) Uani 1 1 d . . . . .
H19 H 0.0523 0.4852 0.3734 0.050 Uiso 1 1 calc R U . . .
C20 C 0.0638(3) 0.3531(3) 0.33489(17) 0.0381(7) Uani 1 1 d . . . . .
H20 H 0.0099 0.3218 0.3740 0.046 Uiso 1 1 calc R U . . .
C21 C 0.1168(3) 0.3013(2) 0.27838(16) 0.0318(6) Uani 1 1 d . . . . .
H21 H 0.0994 0.2347 0.2792 0.038 Uiso 1 1 calc R U . . .
C22 C 0.2351(3) 0.3444(2) 0.06480(16) 0.0337(7) Uani 1 1 d D . . . .
C23B C 0.1625(8) 0.4272(7) 0.0656(7) 0.041(2) Uani 0.5 1 d D . P A 2
H23B H 0.1351 0.4541 0.1097 0.049 Uiso 0.5 1 calc R U P A 2
C24B C 0.1293(9) 0.4713(8) 0.0038(6) 0.055(3) Uani 0.5 1 d D . P A 2
H24B H 0.0835 0.5295 0.0051 0.066 Uiso 0.5 1 calc R U P A 2
C25B C 0.1647(8) 0.4281(9) -0.0604(7) 0.044(2) Uani 0.5 1 d D . P A 2
H25B H 0.1407 0.4542 -0.1029 0.053 Uiso 0.5 1 calc R U P A 2
C26B C 0.2360(18) 0.3461(13) -0.0599(8) 0.063(7) Uani 0.5 1 d D . P A 2
H26B H 0.2681 0.3218 -0.1045 0.075 Uiso 0.5 1 calc R U P A 2
C27 C 0.2629(3) 0.2980(2) 0.00202(17) 0.0376(7) Uani 1 1 d D . . . .
H27A H 0.2994 0.2351 0.0020 0.045 Uiso 0.5 1 calc R U P A 2
H27 H 0.2981 0.2347 0.0044 0.045 Uiso 0.5 1 calc R U P A 1
C28 C 0.1820(3) 0.1712(2) 0.15747(15) 0.0298(6) Uani 1 1 d D . . . .
C29 C 0.0712(3) 0.1865(2) 0.15005(18) 0.0387(7) Uani 1 1 d D . . . .
H29 H 0.0439 0.2515 0.1390 0.046 Uiso 1 1 calc R U . . .
C30 C 0.0017(3) 0.1087(3) 0.1586(2) 0.0450(8) Uani 1 1 d . . . . .
H30 H -0.0728 0.1204 0.1534 0.054 Uiso 1 1 calc R U . . .
C31 C 0.0400(3) 0.0138(3) 0.17478(19) 0.0454(8) Uani 1 1 d . . . . .
H31 H -0.0086 -0.0395 0.1814 0.055 Uiso 1 1 calc R U . . .
C32 C 0.1491(3) -0.0036(2) 0.1812(2) 0.0459(8) Uani 1 1 d . . . . .
H32 H 0.1759 -0.0691 0.1913 0.055 Uiso 1 1 calc R U . . .
C33 C 0.2197(3) 0.0742(2) 0.17305(17) 0.0363(7) Uani 1 1 d D . . . .
H33 H 0.2942 0.0617 0.1781 0.044 Uiso 1 1 calc R U . . .
C34 C 0.6313(3) 0.7915(2) 0.33424(16) 0.0305(6) Uani 1 1 d . . . . .
C35 C 0.5924(3) 0.8192(2) 0.40384(17) 0.0326(6) Uani 1 1 d . . . . .
H35 H 0.6448 0.8241 0.4324 0.039 Uiso 1 1 calc R U . . .
C36 C 0.4802(3) 0.8399(2) 0.43272(18) 0.0369(7) Uani 1 1 d D . . . .
C37B C 0.4348(17) 0.8589(18) 0.5083(9) 0.0475(9) Uani 0.2 1 d D . P B 2
C38 C 0.4022(3) 0.8385(2) 0.3913(2) 0.0403(7) Uani 1 1 d . . . . .
H38 H 0.3258 0.8547 0.4100 0.048 Uiso 1 1 calc R U . . .
C39 C 0.4384(3) 0.8130(2) 0.32195(19) 0.0377(7) Uani 1 1 d . . . . .
C40 C 0.3592(3) 0.8113(3) 0.2735(2) 0.0478(9) Uani 1 1 d . . . . .
C41 C 0.5502(3) 0.7881(2) 0.29488(18) 0.0344(7) Uani 1 1 d . . . . .
H41 H 0.5719 0.7682 0.2479 0.041 Uiso 1 1 calc R U . . .
C42 C 0.8123(3) 0.7882(2) 0.21921(16) 0.0302(6) Uani 1 1 d . . . . .
C43 C 0.7662(3) 0.8635(2) 0.17729(16) 0.0310(6) Uani 1 1 d . . . . .
H43 H 0.6969 0.8935 0.1983 0.037 Uiso 1 1 calc R U . . .
C44 C 0.8178(3) 0.8959(2) 0.10639(17) 0.0354(7) Uani 1 1 d . . . . .
C45 C 0.7651(4) 0.9767(3) 0.06383(18) 0.0462(9) Uani 1 1 d . . . . .
C46 C 0.9191(3) 0.8545(2) 0.07321(18) 0.0412(8) Uani 1 1 d . . . . .
H46 H 0.9540 0.8755 0.0243 0.049 Uiso 1 1 calc R U . . .
C47 C 0.9677(3) 0.7812(2) 0.11411(18) 0.0390(7) Uani 1 1 d . . . . .
C48 C 1.0791(4) 0.7382(3) 0.0819(2) 0.0590(11) Uani 1 1 d . . . . .
C49 C 0.9164(3) 0.7496(2) 0.18483(17) 0.0330(6) Uani 1 1 d . . . . .
H49 H 0.9528 0.7000 0.2113 0.040 Uiso 1 1 calc R U . . .
C50 C 0.7561(2) 0.6323(2) 0.32535(16) 0.0267(6) Uani 1 1 d . . . . .
C51 C 0.7866(2) 0.5611(2) 0.27742(16) 0.0284(6) Uani 1 1 d . . . . .
H51 H 0.8115 0.5818 0.2272 0.034 Uiso 1 1 calc R U . . .
C52 C 0.7812(2) 0.4606(2) 0.30168(16) 0.0297(6) Uani 1 1 d . . . . .
C53 C 0.8149(3) 0.3880(2) 0.24775(18) 0.0371(7) Uani 1 1 d . . . . .
C54 C 0.7449(3) 0.4267(2) 0.37403(17) 0.0317(6) Uani 1 1 d . . . . .
H54 H 0.7416 0.3583 0.3904 0.038 Uiso 1 1 calc R U . . .
C55 C 0.7131(3) 0.4961(2) 0.42231(16) 0.0324(6) Uani 1 1 d . . . . .
C56 C 0.6773(3) 0.4658(2) 0.50169(18) 0.0419(8) Uani 1 1 d . . . . .
C57 C 0.7189(2) 0.5955(2) 0.39761(16) 0.0295(6) Uani 1 1 d . . . . .
H57 H 0.6962 0.6410 0.4319 0.035 Uiso 1 1 calc R U . . .
C58 C 0.8446(2) 0.7962(2) 0.34629(15) 0.0279(6) Uani 1 1 d . . . . .
C59 C 0.9237(2) 0.7390(2) 0.37520(15) 0.0279(6) Uani 1 1 d . . . . .
H59 H 0.9270 0.6701 0.3736 0.034 Uiso 1 1 calc R U . . .
C60 C 0.9992(2) 0.7802(2) 0.40684(16) 0.0308(6) Uani 1 1 d . . . . .
C61 C 1.0795(3) 0.7116(3) 0.43755(18) 0.0370(7) Uani 1 1 d . . . . .
C62 C 0.9985(3) 0.8798(2) 0.40911(16) 0.0327(6) Uani 1 1 d . . . . .
H62 H 1.0495 0.9075 0.4306 0.039 Uiso 1 1 calc R U . . .
C63 C 0.9215(3) 0.9388(2) 0.37926(16) 0.0320(6) Uani 1 1 d . . . . .
C64 C 0.9212(3) 1.0471(2) 0.38143(18) 0.0414(8) Uani 1 1 d . . . . .
C65 C 0.8459(3) 0.8978(2) 0.34893(16) 0.0303(6) Uani 1 1 d . . . . .
H65 H 0.7936 0.9398 0.3294 0.036 Uiso 1 1 calc R U . . .
F1 F 0.5186(6) 0.9009(4) 0.5343(5) 0.0565(16) Uani 0.8 1 d D . P B 1
F2 F 0.4222(4) 0.7747(3) 0.55562(18) 0.0794(12) Uani 0.8 1 d D . P B 1
F3 F 0.3517(3) 0.9189(4) 0.5227(3) 0.0814(15) Uani 0.8 1 d D . P B 1
F4 F 0.25688(18) 0.84807(18) 0.30195(14) 0.0603(6) Uani 1 1 d . . . . .
F5 F 0.3446(2) 0.72060(18) 0.26051(15) 0.0644(7) Uani 1 1 d . . . . .
F6 F 0.3944(2) 0.8643(2) 0.20894(14) 0.0689(7) Uani 1 1 d . . . . .
F7 F 0.8235(6) 1.0583(3) 0.0509(5) 0.109(2) Uani 0.64 1 d . . P C 1
F8 F 0.6626(5) 1.0072(5) 0.0979(2) 0.0951(17) Uani 0.64 1 d . . P C 1
F9 F 0.7530(6) 0.9590(4) 0.0022(3) 0.0766(13) Uani 0.64 1 d . . P C 1
F10 F 1.0911(3) 0.7319(2) 0.01064(15) 0.0903(10) Uani 1 1 d . . . . .
F11 F 1.1628(2) 0.7909(2) 0.0861(2) 0.0962(11) Uani 1 1 d . . . . .
F12 F 1.0967(2) 0.64759(18) 0.11139(15) 0.0796(9) Uani 1 1 d . . . . .
F13 F 0.7536(2) 0.48751(16) 0.53680(11) 0.0553(6) Uani 1 1 d . . . . .
F14 F 0.58386(19) 0.51528(19) 0.53189(11) 0.0570(6) Uani 1 1 d . . . . .
F15 F 0.6593(3) 0.37091(17) 0.51962(13) 0.0804(9) Uani 1 1 d . . . . .
F16 F 0.73690(19) 0.38310(18) 0.20970(13) 0.0591(6) Uani 1 1 d . . . . .
F17 F 0.8311(2) 0.29670(14) 0.27807(12) 0.0563(6) Uani 1 1 d . . . . .
F18 F 0.90930(18) 0.41161(14) 0.19876(11) 0.0472(5) Uani 1 1 d . . . . .
F19 F 1.15424(17) 0.67062(16) 0.38663(11) 0.0475(5) Uani 1 1 d . . . . .
F20 F 1.02853(18) 0.63706(17) 0.48325(12) 0.0540(5) Uani 1 1 d . . . . .
F21 F 1.13760(19) 0.75554(18) 0.47475(13) 0.0596(6) Uani 1 1 d . . . . .
F22 F 1.0224(2) 1.08332(17) 0.35324(16) 0.0697(7) Uani 1 1 d . . . . .
F23 F 0.8922(2) 1.06993(15) 0.44970(11) 0.0584(6) Uani 1 1 d . . . . .
F24 F 0.8514(2) 1.09800(14) 0.34691(13) 0.0569(6) Uani 1 1 d . . . . .
Fe1 Fe 0.46096(4) 0.25406(3) 0.13721(2) 0.02849(12) Uani 1 1 d . . . . .
N1 N 0.4593(2) 0.35579(17) 0.20413(13) 0.0286(5) Uani 1 1 d . . . . .
N2 N 0.4999(2) 0.44983(19) 0.09285(14) 0.0384(6) Uani 1 1 d . . . . .
H2A H 0.5155 0.5059 0.0652 0.046 Uiso 1 1 calc R U . . .
O1 O 0.4890(2) 0.37207(16) -0.00202(11) 0.0398(5) Uani 1 1 d . . . . .
O2 O 0.7066(2) 0.2553(2) 0.09950(16) 0.0548(7) Uani 1 1 d . . . . .
O3 O 0.4717(2) 0.11986(19) 0.02911(14) 0.0514(6) Uani 1 1 d . . . . .
P1 P 0.26765(6) 0.27726(5) 0.14685(4) 0.02645(15) Uani 1 1 d D . . . .
S1 S 0.45948(7) 0.12789(5) 0.23037(4) 0.03365(16) Uani 1 1 d . . . . .
B1 B 0.7597(3) 0.7522(2) 0.30495(18) 0.0285(7) Uani 1 1 d . . . . .
F2AA F 0.7491(12) 1.0534(7) 0.0916(5) 0.0766(13) Uani 0.36 1 d . . P C 2
F1AA F 0.8261(9) 0.9954(9) -0.0022(5) 0.0951(17) Uani 0.36 1 d . . P C 2
F0AA F 0.6721(11) 0.9464(6) 0.0566(9) 0.109(2) Uani 0.36 1 d . . P C 2
F3AA F 0.3495(11) 0.8027(10) 0.5411(7) 0.060(3) Uani 0.2 1 d D . P B 2
F4AA F 0.515(2) 0.869(2) 0.5409(16) 0.085(11) Uani 0.2 1 d D . P B 2
F5AA F 0.3844(17) 0.946(2) 0.5053(14) 0.0814(15) Uani 0.2 1 d D . P B 2
C37A C 0.4430(5) 0.8595(5) 0.5100(3) 0.0475(9) Uani 0.8 1 d D . P B 1
C25A C 0.2122(8) 0.4380(8) -0.0679(7) 0.044(2) Uani 0.5 1 d D . P A 1
H25A H 0.2082 0.4727 -0.1136 0.053 Uiso 0.5 1 calc R U P A 1
C24A C 0.1883(8) 0.4869(8) -0.0080(6) 0.055(3) Uani 0.5 1 d D . P A 1
H24A H 0.1610 0.5531 -0.0123 0.066 Uiso 0.5 1 calc R U P A 1
C23A C 0.2026(9) 0.4431(7) 0.0581(7) 0.041(2) Uani 0.5 1 d D . P A 1
H23A H 0.1905 0.4794 0.0982 0.049 Uiso 0.5 1 calc R U P A 1
C26A C 0.2417(12) 0.3400(10) -0.0632(7) 0.031(4) Uani 0.5 1 d D . P A 1
H26A H 0.2473 0.3031 -0.1025 0.037 Uiso 0.5 1 calc R U P A 1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.358(4) . ?
C1 N2 1.374(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.364(5) . ?
C3 C4 1.393(5) . ?
C4 C5 1.386(4) . ?
C5 N1 1.364(4) . ?
C5 C6 1.487(4) . ?
C6 C11 1.399(4) . ?
C6 C7 1.410(4) . ?
C7 C8 1.381(5) . ?
C8 C9 1.379(5) . ?
C9 C10 1.376(5) . ?
C10 C11 1.395(4) . ?
C11 S1 1.769(3) . ?
C12 S1 1.828(4) . ?
C13 O1 1.223(4) . ?
C13 N2 1.391(4) . ?
C13 Fe1 1.947(3) . ?
C14 O2 1.130(4) . ?
C14 Fe1 1.817(4) . ?
C15 O3 1.138(4) . ?
C15 Fe1 1.792(3) . ?
C16 C21 1.391(4) . ?
C16 C17 1.397(4) . ?
C16 P1 1.833(3) . ?
C17 C18 1.387(4) . ?
C18 C19 1.384(5) . ?
C19 C20 1.385(5) . ?
C20 C21 1.388(4) . ?
C22 C23A 1.389(10) . ?
C22 C27 1.399(4) . ?
C22 C23B 1.405(10) . ?
C22 P1 1.832(3) . ?
C23B C24B 1.396(10) . ?
C24B C25B 1.404(11) . ?
C25B C26B 1.387(12) . ?
C26B C27 1.381(11) . ?
C27 C26A 1.382(9) . ?
C28 C33 1.402(4) . ?
C28 C29 1.407(4) . ?
C28 P1 1.813(3) . ?
C29 C30 1.379(5) . ?
C30 C31 1.381(5) . ?
C31 C32 1.385(5) . ?
C32 C33 1.389(4) . ?
C34 C41 1.393(4) . ?
C34 C35 1.404(4) . ?
C34 B1 1.636(5) . ?
C35 C36 1.392(4) . ?
C36 C38 1.387(5) . ?
C36 C37B 1.479(16) . ?
C36 C37A 1.500(6) . ?
C37B F5AA 1.320(15) . ?
C37B F4AA 1.318(14) . ?
C37B F3AA 1.325(14) . ?
C38 C39 1.385(5) . ?
C39 C41 1.394(5) . ?
C39 C40 1.501(5) . ?
C40 F5 1.334(4) . ?
C40 F6 1.341(4) . ?
C40 F4 1.348(4) . ?
C42 C43 1.402(4) . ?
C42 C49 1.407(4) . ?
C42 B1 1.641(4) . ?
C43 C44 1.385(4) . ?
C44 C46 1.388(5) . ?
C44 C45 1.498(5) . ?
C45 F2AA 1.228(8) . ?
C45 F9 1.282(5) . ?
C45 F0AA 1.287(10) . ?
C45 F1AA 1.313(9) . ?
C45 F7 1.334(6) . ?
C45 F8 1.350(6) . ?
C46 C47 1.388(5) . ?
C47 C49 1.379(4) . ?
C47 C48 1.490(5) . ?
C48 F11 1.318(5) . ?
C48 F12 1.325(5) . ?
C48 F10 1.355(5) . ?
C50 C57 1.389(4) . ?
C50 C51 1.406(4) . ?
C50 B1 1.643(4) . ?
C51 C52 1.398(4) . ?
C52 C54 1.380(4) . ?
C52 C53 1.504(4) . ?
C53 F17 1.335(4) . ?
C53 F18 1.340(4) . ?
C53 F16 1.346(4) . ?
C54 C55 1.394(4) . ?
C55 C57 1.386(4) . ?
C55 C56 1.491(4) . ?
C56 F15 1.323(4) . ?
C56 F13 1.346(4) . ?
C56 F14 1.350(4) . ?
C58 C59 1.387(4) . ?
C58 C65 1.406(4) . ?
C58 B1 1.639(4) . ?
C59 C60 1.406(4) . ?
C60 C62 1.375(4) . ?
C60 C61 1.493(5) . ?
C61 F19 1.335(4) . ?
C61 F21 1.339(4) . ?
C61 F20 1.339(4) . ?
C62 C63 1.389(5) . ?
C63 C65 1.388(4) . ?
C63 C64 1.494(4) . ?
C64 F24 1.320(4) . ?
C64 F22 1.335(4) . ?
C64 F23 1.348(4) . ?
F1 C37A 1.322(7) . ?
F2 C37A 1.359(7) . ?
F3 C37A 1.346(6) . ?
Fe1 N1 2.016(2) . ?
Fe1 S1 2.3161(9) . ?
Fe1 P1 2.3532(9) . ?
C25A C26A 1.371(11) . ?
C25A C24A 1.373(11) . ?
C24A C23A 1.375(11) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 C1 N2 115.2(3) . . ?
N1 C1 C2 123.4(3) . . ?
N2 C1 C2 121.4(3) . . ?
C3 C2 C1 117.7(3) . . ?
C2 C3 C4 119.7(3) . . ?
C5 C4 C3 120.2(3) . . ?
N1 C5 C4 120.4(3) . . ?
N1 C5 C6 120.7(2) . . ?
C4 C5 C6 118.5(3) . . ?
C11 C6 C7 116.3(3) . . ?
C11 C6 C5 127.1(3) . . ?
C7 C6 C5 116.5(3) . . ?
C8 C7 C6 121.7(3) . . ?
C9 C8 C7 120.6(3) . . ?
C10 C9 C8 119.4(3) . . ?
C9 C10 C11 120.2(3) . . ?
C10 C11 C6 121.7(3) . . ?
C10 C11 S1 116.3(2) . . ?
C6 C11 S1 121.9(2) . . ?
O1 C13 N2 119.8(3) . . ?
O1 C13 Fe1 130.3(2) . . ?
N2 C13 Fe1 109.7(2) . . ?
O2 C14 Fe1 176.6(4) . . ?
O3 C15 Fe1 177.8(3) . . ?
C21 C16 C17 118.7(3) . . ?
C21 C16 P1 120.5(2) . . ?
C17 C16 P1 120.7(2) . . ?
C18 C17 C16 120.6(3) . . ?
C19 C18 C17 120.1(3) . . ?
C18 C19 C20 119.7(3) . . ?
C19 C20 C21 120.4(3) . . ?
C20 C21 C16 120.4(3) . . ?
C23A C22 C27 117.8(6) . . ?
C27 C22 C23B 118.0(6) . . ?
C23A C22 P1 123.9(6) . . ?
C27 C22 P1 117.3(2) . . ?
C23B C22 P1 123.0(6) . . ?
C24B C23B C22 122.3(11) . . ?
C23B C24B C25B 118.7(11) . . ?
C26B C25B C24B 117.9(12) . . ?
C27 C26B C25B 123.5(13) . . ?
C26B C27 C22 118.2(8) . . ?
C26A C27 C22 123.2(6) . . ?
C33 C28 C29 117.9(3) . . ?
C33 C28 P1 123.7(2) . . ?
C29 C28 P1 118.4(2) . . ?
C30 C29 C28 121.0(3) . . ?
C29 C30 C31 120.3(3) . . ?
C30 C31 C32 120.0(3) . . ?
C31 C32 C33 120.2(3) . . ?
C32 C33 C28 120.7(3) . . ?
C41 C34 C35 115.6(3) . . ?
C41 C34 B1 121.7(3) . . ?
C35 C34 B1 122.3(3) . . ?
C36 C35 C34 122.6(3) . . ?
C38 C36 C35 120.3(3) . . ?
C38 C36 C37B 115.6(9) . . ?
C35 C36 C37B 124.0(9) . . ?
C38 C36 C37A 120.0(4) . . ?
C35 C36 C37A 119.7(4) . . ?
F5AA C37B F4AA 104(2) . . ?
F5AA C37B F3AA 100.9(19) . . ?
F4AA C37B F3AA 120(2) . . ?
F5AA C37B C36 106.5(17) . . ?
F4AA C37B C36 111.2(19) . . ?
F3AA C37B C36 112.2(14) . . ?
C39 C38 C36 118.3(3) . . ?
C38 C39 C41 120.8(3) . . ?
C38 C39 C40 121.4(3) . . ?
C41 C39 C40 117.8(3) . . ?
F5 C40 F6 106.5(3) . . ?
F5 C40 F4 106.3(3) . . ?
F6 C40 F4 106.2(3) . . ?
F5 C40 C39 112.4(3) . . ?
F6 C40 C39 112.5(3) . . ?
F4 C40 C39 112.5(3) . . ?
C34 C41 C39 122.4(3) . . ?
C43 C42 C49 115.2(3) . . ?
C43 C42 B1 124.6(3) . . ?
C49 C42 B1 119.9(3) . . ?
C44 C43 C42 122.4(3) . . ?
C43 C44 C46 121.0(3) . . ?
C43 C44 C45 120.4(3) . . ?
C46 C44 C45 118.5(3) . . ?
F2AA C45 F0AA 110.0(8) . . ?
F2AA C45 F1AA 108.6(8) . . ?
F0AA C45 F1AA 105.4(8) . . ?
F9 C45 F7 105.9(5) . . ?
F9 C45 F8 104.4(4) . . ?
F7 C45 F8 102.8(5) . . ?
F2AA C45 C44 113.4(4) . . ?
F9 C45 C44 116.4(3) . . ?
F0AA C45 C44 108.2(4) . . ?
F1AA C45 C44 111.0(5) . . ?
F7 C45 C44 111.3(3) . . ?
F8 C45 C44 114.7(3) . . ?
C47 C46 C44 117.6(3) . . ?
C49 C47 C46 121.2(3) . . ?
C49 C47 C48 119.3(3) . . ?
C46 C47 C48 119.5(3) . . ?
F11 C48 F12 107.3(4) . . ?
F11 C48 F10 105.6(3) . . ?
F12 C48 F10 105.3(3) . . ?
F11 C48 C47 113.3(3) . . ?
F12 C48 C47 113.4(3) . . ?
F10 C48 C47 111.4(4) . . ?
C47 C49 C42 122.4(3) . . ?
C57 C50 C51 115.3(3) . . ?
C57 C50 B1 117.5(3) . . ?
C51 C50 B1 127.2(3) . . ?
C52 C51 C50 121.8(3) . . ?
C54 C52 C51 121.3(3) . . ?
C54 C52 C53 119.4(3) . . ?
C51 C52 C53 119.3(3) . . ?
F17 C53 F18 106.5(3) . . ?
F17 C53 F16 106.5(3) . . ?
F18 C53 F16 105.8(3) . . ?
F17 C53 C52 113.3(3) . . ?
F18 C53 C52 112.6(3) . . ?
F16 C53 C52 111.6(3) . . ?
C52 C54 C55 117.8(3) . . ?
C57 C55 C54 120.4(3) . . ?
C57 C55 C56 118.4(3) . . ?
C54 C55 C56 121.2(3) . . ?
F15 C56 F13 106.5(3) . . ?
F15 C56 F14 107.7(3) . . ?
F13 C56 F14 104.1(3) . . ?
F15 C56 C55 114.1(3) . . ?
F13 C56 C55 111.8(3) . . ?
F14 C56 C55 111.9(3) . . ?
C55 C57 C50 123.4(3) . . ?
C59 C58 C65 116.2(3) . . ?
C59 C58 B1 123.4(2) . . ?
C65 C58 B1 120.2(3) . . ?
C58 C59 C60 121.8(3) . . ?
C62 C60 C59 120.9(3) . . ?
C62 C60 C61 121.7(3) . . ?
C59 C60 C61 117.4(3) . . ?
F19 C61 F21 106.6(3) . . ?
F19 C61 F20 106.0(3) . . ?
F21 C61 F20 106.0(3) . . ?
F19 C61 C60 112.5(3) . . ?
F21 C61 C60 112.9(3) . . ?
F20 C61 C60 112.3(3) . . ?
C60 C62 C63 118.4(3) . . ?
C65 C63 C62 120.6(3) . . ?
C65 C63 C64 121.0(3) . . ?
C62 C63 C64 118.3(3) . . ?
F24 C64 F22 107.2(3) . . ?
F24 C64 F23 105.8(3) . . ?
F22 C64 F23 105.9(3) . . ?
F24 C64 C63 114.0(3) . . ?
F22 C64 C63 111.6(3) . . ?
F23 C64 C63 111.8(3) . . ?
C63 C65 C58 122.0(3) . . ?
C15 Fe1 C14 89.63(15) . . ?
C15 Fe1 C13 91.60(14) . . ?
C14 Fe1 C13 82.04(15) . . ?
C15 Fe1 N1 175.11(12) . . ?
C14 Fe1 N1 89.27(12) . . ?
C13 Fe1 N1 83.54(12) . . ?
C15 Fe1 S1 93.46(10) . . ?
C14 Fe1 S1 90.76(12) . . ?
C13 Fe1 S1 171.17(10) . . ?
N1 Fe1 S1 91.31(7) . . ?
C15 Fe1 P1 89.04(11) . . ?
C14 Fe1 P1 169.72(12) . . ?
C13 Fe1 P1 87.80(10) . . ?
N1 Fe1 P1 91.20(7) . . ?
S1 Fe1 P1 99.50(3) . . ?
C1 N1 C5 117.8(2) . . ?
C1 N1 Fe1 110.65(19) . . ?
C5 N1 Fe1 131.2(2) . . ?
C1 N2 C13 119.6(3) . . ?
C28 P1 C22 99.75(13) . . ?
C28 P1 C16 103.55(13) . . ?
C22 P1 C16 105.49(14) . . ?
C28 P1 Fe1 119.36(10) . . ?
C22 P1 Fe1 112.39(11) . . ?
C16 P1 Fe1 114.47(9) . . ?
C11 S1 C12 98.95(16) . . ?
C11 S1 Fe1 105.93(10) . . ?
C12 S1 Fe1 110.18(14) . . ?
C34 B1 C58 111.1(2) . . ?
C34 B1 C42 114.0(2) . . ?
C58 B1 C42 103.7(2) . . ?
C34 B1 C50 104.9(2) . . ?
C58 B1 C50 109.4(2) . . ?
C42 B1 C50 113.9(2) . . ?
F3 C37A F1 105.1(6) . . ?
F3 C37A F2 108.2(5) . . ?
F1 C37A F2 103.2(5) . . ?
F3 C37A C36 113.6(5) . . ?
F1 C37A C36 114.4(6) . . ?
F2 C37A C36 111.5(5) . . ?
C26A C25A C24A 121.3(12) . . ?
C25A C24A C23A 122.0(11) . . ?
C24A C23A C22 118.4(11) . . ?
C25A C26A C27 116.0(12) . . ?

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
N2 H2A O1 0.88 1.94 2.800(4) 165.3 2_665
C21 H21 F22 0.95 2.46 3.298(4) 146.7 1_445
C33 H33 S1 0.95 2.72 3.537(3) 144.0 .
C4 H4 F14 0.95 2.34 3.161(4) 144.6 2_666

_refine_diff_density_max         0.386
_refine_diff_density_min         -0.547
_refine_diff_density_rms         0.060

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_3a
_database_code_depnum_ccdc_archive 'CCDC 1547036'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H34 Br Cl4 Fe N2 O2 P S'
_chemical_formula_sum            'C36 H34 Br Cl4 Fe N2 O2 P S'
_chemical_formula_weight         867.24

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/n'
_space_group_name_Hall           '-P 2yac'

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

_cell_length_a                   14.1110(9)
_cell_length_b                   13.7420(8)
_cell_length_c                   19.9776(12)
_cell_angle_alpha                90
_cell_angle_beta                 104.537(6)
_cell_angle_gamma                90
_cell_volume                     3749.9(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7737
_cell_measurement_theta_min      3.2610
_cell_measurement_theta_max      73.4950

_exptl_crystal_description       Prism
_exptl_crystal_colour            Orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_F_000             1760
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.070
_exptl_absorpt_coefficient_mu    8.301
_shelx_estimated_absorpt_T_min   0.288
_shelx_estimated_absorpt_T_max   0.594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.50138
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15223
_diffrn_reflns_av_unetI/netI     0.0367
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.216
_diffrn_reflns_theta_max         74.463
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             7395
_reflns_number_gt                6961
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_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)+(0.0704P)²+5.7052P] 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         7395
_refine_ls_number_parameters     450
_refine_ls_number_restraints     393
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1280
_refine_ls_wR_factor_gt          0.1255
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.013
_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
C13 C 0.3571(2) 0.4722(2) 0.50680(16) 0.0217(6) Uani 1 1 d . U . . .
C1 C 0.4260(2) 0.3696(2) 0.60251(15) 0.0186(5) Uani 1 1 d . U . . .
C2 C 0.5059(2) 0.3322(2) 0.65222(16) 0.0219(6) Uani 1 1 d . U . . .
H2 H 0.5711 0.3469 0.6508 0.026 Uiso 1 1 calc R U . . .
C3 C 0.4871(2) 0.2738(2) 0.70299(16) 0.0244(6) Uani 1 1 d . U . . .
H3 H 0.5394 0.2506 0.7393 0.029 Uiso 1 1 calc R U . . .
C4 C 0.3910(2) 0.2487(2) 0.70095(15) 0.0222(6) Uani 1 1 d . U . . .
H4 H 0.3776 0.2070 0.7354 0.027 Uiso 1 1 calc R U . . .
C5 C 0.3142(2) 0.2846(2) 0.64852(14) 0.0171(5) Uani 1 1 d . U . . .
C6 C 0.2153(2) 0.2406(2) 0.64120(14) 0.0179(5) Uani 1 1 d . U . . .
C7 C 0.2125(2) 0.1410(2) 0.65736(15) 0.0201(6) Uani 1 1 d . U . . .
H7 H 0.2723 0.1059 0.6709 0.024 Uiso 1 1 calc R U . . .
C8 C 0.1252(2) 0.0926(2) 0.65414(15) 0.0216(6) Uani 1 1 d . U . . .
H8 H 0.1258 0.0254 0.6654 0.026 Uiso 1 1 calc R U . . .
C9 C 0.0367(2) 0.1425(2) 0.63449(15) 0.0219(6) Uani 1 1 d . U . . .
H9 H -0.0231 0.1104 0.6338 0.026 Uiso 1 1 calc R U . . .
C10 C 0.0370(2) 0.2394(2) 0.61595(15) 0.0205(6) Uani 1 1 d . U . . .
H10 H -0.0233 0.2735 0.6016 0.025 Uiso 1 1 calc R U . . .
C11 C 0.1248(2) 0.2880(2) 0.61805(14) 0.0186(5) Uani 1 1 d . U . . .
C12 C 0.1214(3) 0.4719(3) 0.67100(18) 0.0327(7) Uani 1 1 d . U . . .
H12A H 0.0669 0.4508 0.6897 0.049 Uiso 1 1 calc R U . . .
H12B H 0.1179 0.5425 0.6637 0.049 Uiso 1 1 calc R U . . .
H12C H 0.1835 0.4554 0.7038 0.049 Uiso 1 1 calc R U . . .
C14 C 0.1759(2) 0.5356(2) 0.48523(16) 0.0205(6) Uani 1 1 d . U . . .
C15 C 0.3041(2) 0.2525(2) 0.45011(17) 0.0255(6) Uani 1 1 d . U . . .
C16 C 0.3551(3) 0.2635(3) 0.3997(2) 0.0420(9) Uani 1 1 d . U . . .
H16 H 0.3337 0.3094 0.3635 0.050 Uiso 1 1 calc R U . . .
C17 C 0.4385(3) 0.2066(4) 0.4026(3) 0.0592(14) Uani 1 1 d . U . . .
H17 H 0.4735 0.2145 0.3680 0.071 Uiso 1 1 calc R U . . .
C18 C 0.4704(3) 0.1401(3) 0.4542(3) 0.0466(10) Uani 1 1 d . U . . .
H18 H 0.5269 0.1019 0.4554 0.056 Uiso 1 1 calc R U . . .
C19 C 0.4203(2) 0.1286(3) 0.5045(2) 0.0347(8) Uani 1 1 d . U . . .
H19 H 0.4425 0.0828 0.5406 0.042 Uiso 1 1 calc R U . . .
C20 C 0.3374(2) 0.1837(2) 0.50249(17) 0.0259(6) Uani 1 1 d . U . . .
H20 H 0.3027 0.1747 0.5371 0.031 Uiso 1 1 calc R U . . .
C21 C 0.0977(2) 0.2534(2) 0.45330(15) 0.0205(6) Uani 1 1 d . U . . .
C22 C 0.0069(2) 0.2995(2) 0.44526(15) 0.0227(6) Uani 1 1 d . U . . .
H22 H 0.0036 0.3685 0.4457 0.027 Uiso 1 1 calc R U . . .
C23 C -0.0782(2) 0.2451(3) 0.43661(16) 0.0260(6) Uani 1 1 d . U . . .
H23 H -0.1397 0.2769 0.4301 0.031 Uiso 1 1 calc R U . . .
C24 C -0.0734(2) 0.1443(3) 0.43745(17) 0.0290(7) Uani 1 1 d . U . . .
H24 H -0.1315 0.1068 0.4318 0.035 Uiso 1 1 calc R U . . .
C25 C 0.0165(2) 0.0983(2) 0.44651(17) 0.0265(6) Uani 1 1 d . U . . .
H25 H 0.0198 0.0293 0.4478 0.032 Uiso 1 1 calc R U . . .
C26 C 0.1017(2) 0.1521(2) 0.45367(15) 0.0229(6) Uani 1 1 d . U . . .
H26 H 0.1627 0.1199 0.4588 0.027 Uiso 1 1 calc R U . . .
C27 C 0.1588(2) 0.3765(3) 0.36238(16) 0.0256(6) Uani 1 1 d . U . . .
C28 C 0.0923(3) 0.3194(3) 0.31359(18) 0.0353(8) Uani 1 1 d . U . . .
H28 H 0.0748 0.2565 0.3262 0.042 Uiso 1 1 calc R U . . .
C29 C 0.0525(3) 0.3540(3) 0.24777(19) 0.0445(9) Uani 1 1 d . U . . .
H29 H 0.0071 0.3152 0.2156 0.053 Uiso 1 1 calc R U . . .
C30 C 0.0780(3) 0.4445(3) 0.22829(19) 0.0395(9) Uani 1 1 d . U . . .
H30 H 0.0496 0.4683 0.1831 0.047 Uiso 1 1 calc R U . . .
C31 C 0.1456(3) 0.5008(3) 0.27517(18) 0.0344(8) Uani 1 1 d . U . . .
H31 H 0.1642 0.5627 0.2616 0.041 Uiso 1 1 calc R U . . .
C32 C 0.1861(2) 0.4668(3) 0.34179(17) 0.0269(6) Uani 1 1 d . U . . .
H32 H 0.2326 0.5053 0.3734 0.032 Uiso 1 1 calc R U . . .
N2 N 0.43862(18) 0.42866(19) 0.55060(14) 0.0212(5) Uani 1 1 d . U . . .
H1 H 0.4976 0.4392 0.5448 0.025 Uiso 1 1 calc R U . . .
N1 N 0.33161(16) 0.35069(17) 0.60213(12) 0.0162(5) Uani 1 1 d . U . . .
O2 O 0.13640(16) 0.59964(17) 0.45336(13) 0.0295(5) Uani 1 1 d . U . . .
O1 O 0.37171(15) 0.52599(17) 0.46035(12) 0.0256(5) Uani 1 1 d . U . . .
P1 P 0.20148(5) 0.33306(5) 0.45224(4) 0.01831(16) Uani 1 1 d . U . . .
S1 S 0.11421(5) 0.41091(5) 0.58930(4) 0.01820(15) Uani 1 1 d . U . . .
Fe1 Fe 0.24157(3) 0.44272(3) 0.53736(2) 0.01571(12) Uani 1 1 d . U . . .
Br1 Br 0.30506(2) 0.57638(3) 0.62128(2) 0.03250(12) Uani 1 1 d . U . . .
Cl1 Cl 0.75674(7) 0.24119(9) 0.65931(6) 0.0499(3) Uani 1 1 d . U . . .
Cl2 Cl 0.74015(8) 0.06764(7) 0.53546(7) 0.0516(3) Uani 1 1 d . U . . .
C33 C 0.6867(3) 0.2469(3) 0.5711(2) 0.0350(8) Uani 1 1 d . U . . .
H33A H 0.6222 0.2161 0.5671 0.042 Uiso 1 1 calc R U . . .
H33B H 0.6754 0.3159 0.5571 0.042 Uiso 1 1 calc R U . . .
C34 C 0.7370(3) 0.1972(3) 0.5236(2) 0.0397(9) Uani 1 1 d . U . . .
H34A H 0.8047 0.2221 0.5318 0.048 Uiso 1 1 calc R U . . .
H34B H 0.7024 0.2125 0.4751 0.048 Uiso 1 1 calc R U . . .
Cl4 Cl -0.3275(4) 0.1194(4) 0.3159(2) 0.0533(9) Uani 0.5 1 d . U P A -1
Cl4B Cl -0.1765(5) 0.1318(5) 0.2081(3) 0.0662(12) Uani 0.5 1 d . U P A -1
C36 C -0.3219(9) 0.2150(7) 0.2558(6) 0.045(2) Uani 0.5 1 d . U P A -1
H36A H -0.3642 0.1977 0.2098 0.054 Uiso 0.5 1 calc R U P A -1
H36B H -0.3479 0.2757 0.2712 0.054 Uiso 0.5 1 calc R U P A -1
C36B C -0.2217(8) 0.2328(8) 0.2492(6) 0.050(3) Uani 0.5 1 d . U P A -1
H36C H -0.1777 0.2434 0.2957 0.060 Uiso 0.5 1 calc R U P A -1
H36D H -0.2210 0.2925 0.2216 0.060 Uiso 0.5 1 calc R U P A -1
Cl3 Cl -0.1041(2) -0.0376(2) 0.73426(17) 0.0667(7) Uiso 0.5 1 d . . P B -1
Cl3A Cl -0.4012(13) -0.0211(13) 0.7454(9) 0.322(8) Uiso 0.5 1 d . . P B -1
C35 C -0.2449(14) -0.0248(15) 0.7172(9) 0.097(5) Uiso 0.5 1 d . . P B -1
H35A H -0.2631 0.0447 0.7102 0.117 Uiso 0.5 1 calc R U P B -1
H35B H -0.2768 -0.0604 0.6744 0.117 Uiso 0.5 1 calc R U P B -1
C35A C -0.280(2) -0.0629(18) 0.7744(13) 0.133(9) Uiso 0.5 1 d . . P B -1
H35C H -0.2455 -0.0338 0.8193 0.160 Uiso 0.5 1 calc R U P B -1
H35D H -0.2759 -0.1348 0.7774 0.160 Uiso 0.5 1 calc R U P B -1


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C13 O1 1.243(4) . ?
C13 N2 1.394(4) . ?
C13 Fe1 1.922(3) . ?
C1 N1 1.355(4) . ?
C1 N2 1.363(4) . ?
C1 C2 1.399(4) . ?
C2 C3 1.371(5) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.395(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.363(4) . ?
C5 C6 1.494(4) . ?
C6 C11 1.405(4) . ?
C6 C7 1.408(4) . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.392(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.398(4) . ?
C10 H10 0.9500 . ?
C11 S1 1.779(3) . ?
C12 S1 1.815(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 O2 1.145(4) . ?
C14 Fe1 1.757(3) . ?
C15 C16 1.385(5) . ?
C15 C20 1.401(5) . ?
C15 P1 1.832(3) . ?
C16 C17 1.402(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.368(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.374(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.385(5) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C21 C26 1.394(4) . ?
C21 C22 1.401(4) . ?
C21 P1 1.833(3) . ?
C22 C23 1.388(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(5) . ?
C23 H23 0.9500 . ?
C24 C25 1.388(5) . ?
C24 H24 0.9500 . ?
C25 C26 1.388(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.391(5) . ?
C27 C28 1.410(5) . ?
C27 P1 1.844(3) . ?
C28 C29 1.379(5) . ?
C28 H28 0.9500 . ?
C29 C30 1.377(6) . ?
C29 H29 0.9500 . ?
C30 C31 1.392(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.391(5) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
N2 H1 0.8800 . ?
N1 Fe1 2.016(2) . ?
P1 Fe1 2.2360(9) . ?
S1 Fe1 2.3311(8) . ?
Fe1 Br1 2.4965(6) . ?
Cl1 C33 1.793(4) . ?
Cl2 C34 1.795(4) . ?
C33 C34 1.485(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
Cl4 C36 1.795(12) . ?
Cl4B C36B 1.808(13) . ?
C36 C36B 1.473(18) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C36B H36C 0.9900 . ?
C36B H36D 0.9900 . ?
Cl3 C35 1.94(2) . ?
Cl3A C35A 1.76(3) . ?
C35 C35A 1.45(2) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35A H35C 0.9900 . ?
C35A H35D 0.9900 . ?

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 C13 N2 117.3(3) . . ?
O1 C13 Fe1 132.5(2) . . ?
N2 C13 Fe1 110.0(2) . . ?
N1 C1 N2 115.2(2) . . ?
N1 C1 C2 123.3(3) . . ?
N2 C1 C2 121.5(3) . . ?
C3 C2 C1 118.0(3) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C2 C3 C4 119.5(3) . . ?
C2 C3 H3 120.3 . . ?
C4 C3 H3 120.3 . . ?
C3 C4 C5 120.2(3) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 120.5(3) . . ?
N1 C5 C6 121.8(2) . . ?
C4 C5 C6 117.4(3) . . ?
C11 C6 C7 116.8(3) . . ?
C11 C6 C5 126.4(3) . . ?
C7 C6 C5 116.8(3) . . ?
C8 C7 C6 122.1(3) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 120.0(3) . . ?
C7 C8 H8 120.0 . . ?
C9 C8 H8 120.0 . . ?
C10 C9 C8 119.1(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 120.9(3) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C6 120.9(3) . . ?
C10 C11 S1 116.2(2) . . ?
C6 C11 S1 122.8(2) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C14 Fe1 176.4(3) . . ?
C16 C15 C20 118.6(3) . . ?
C16 C15 P1 120.6(3) . . ?
C20 C15 P1 120.6(3) . . ?
C15 C16 C17 119.6(4) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
C18 C17 C16 121.1(4) . . ?
C18 C17 H17 119.4 . . ?
C16 C17 H17 119.4 . . ?
C17 C18 C19 119.8(4) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 H18 120.1 . . ?
C18 C19 C20 120.1(4) . . ?
C18 C19 H19 119.9 . . ?
C20 C19 H19 119.9 . . ?
C19 C20 C15 120.8(3) . . ?
C19 C20 H20 119.6 . . ?
C15 C20 H20 119.6 . . ?
C26 C21 C22 119.1(3) . . ?
C26 C21 P1 124.4(2) . . ?
C22 C21 P1 116.1(2) . . ?
C23 C22 C21 120.6(3) . . ?
C23 C22 H22 119.7 . . ?
C21 C22 H22 119.7 . . ?
C24 C23 C22 119.9(3) . . ?
C24 C23 H23 120.1 . . ?
C22 C23 H23 120.1 . . ?
C23 C24 C25 119.8(3) . . ?
C23 C24 H24 120.1 . . ?
C25 C24 H24 120.1 . . ?
C24 C25 C26 120.8(3) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 119.8(3) . . ?
C25 C26 H26 120.1 . . ?
C21 C26 H26 120.1 . . ?
C32 C27 C28 118.6(3) . . ?
C32 C27 P1 122.0(3) . . ?
C28 C27 P1 119.4(3) . . ?
C29 C28 C27 120.5(4) . . ?
C29 C28 H28 119.7 . . ?
C27 C28 H28 119.7 . . ?
C30 C29 C28 120.6(4) . . ?
C30 C29 H29 119.7 . . ?
C28 C29 H29 119.7 . . ?
C29 C30 C31 119.7(3) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C32 C31 C30 120.3(4) . . ?
C32 C31 H31 119.9 . . ?
C30 C31 H31 119.9 . . ?
C27 C32 C31 120.3(3) . . ?
C27 C32 H32 119.8 . . ?
C31 C32 H32 119.8 . . ?
C1 N2 C13 119.2(2) . . ?
C1 N2 H1 120.4 . . ?
C13 N2 H1 120.4 . . ?
C1 N1 C5 117.9(2) . . ?
C1 N1 Fe1 110.10(19) . . ?
C5 N1 Fe1 131.47(19) . . ?
C15 P1 C21 106.16(15) . . ?
C15 P1 C27 103.90(15) . . ?
C21 P1 C27 97.92(14) . . ?
C15 P1 Fe1 111.99(11) . . ?
C21 P1 Fe1 116.36(10) . . ?
C27 P1 Fe1 118.71(11) . . ?
C11 S1 C12 99.62(15) . . ?
C11 S1 Fe1 108.09(10) . . ?
C12 S1 Fe1 115.98(13) . . ?
C14 Fe1 C13 91.24(13) . . ?
C14 Fe1 N1 171.83(12) . . ?
C13 Fe1 N1 83.58(11) . . ?
C14 Fe1 P1 92.51(10) . . ?
C13 Fe1 P1 88.48(10) . . ?
N1 Fe1 P1 93.65(7) . . ?
C14 Fe1 S1 92.82(10) . . ?
C13 Fe1 S1 172.35(9) . . ?
N1 Fe1 S1 91.65(7) . . ?
P1 Fe1 S1 97.81(3) . . ?
C14 Fe1 Br1 84.86(10) . . ?
C13 Fe1 Br1 82.42(9) . . ?
N1 Fe1 Br1 88.19(7) . . ?
P1 Fe1 Br1 170.46(3) . . ?
S1 Fe1 Br1 91.48(3) . . ?
C34 C33 Cl1 112.0(3) . . ?
C34 C33 H33A 109.2 . . ?
Cl1 C33 H33A 109.2 . . ?
C34 C33 H33B 109.2 . . ?
Cl1 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 Cl2 111.8(3) . . ?
C33 C34 H34A 109.3 . . ?
Cl2 C34 H34A 109.3 . . ?
C33 C34 H34B 109.3 . . ?
Cl2 C34 H34B 109.3 . . ?
H34A C34 H34B 107.9 . . ?
C36B C36 Cl4 112.6(9) . . ?
C36B C36 H36A 109.1 . . ?
Cl4 C36 H36A 109.1 . . ?
C36B C36 H36B 109.1 . . ?
Cl4 C36 H36B 109.1 . . ?
H36A C36 H36B 107.8 . . ?
C36 C36B Cl4B 111.7(9) . . ?
C36 C36B H36C 109.3 . . ?
Cl4B C36B H36C 109.3 . . ?
C36 C36B H36D 109.3 . . ?
Cl4B C36B H36D 109.3 . . ?
H36C C36B H36D 108.0 . . ?
C35A C35 Cl3 111.4(15) . . ?
C35A C35 H35A 109.3 . . ?
Cl3 C35 H35A 109.3 . . ?
C35A C35 H35B 109.3 . . ?
Cl3 C35 H35B 109.3 . . ?
H35A C35 H35B 108.0 . . ?
C35 C35A Cl3A 96.7(16) . . ?
C35 C35A H35C 112.4 . . ?
Cl3A C35A H35C 112.4 . . ?
C35 C35A H35D 112.4 . . ?
Cl3A C35A H35D 112.4 . . ?
H35C C35A H35D 110.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.1(5) . . . . ?
N2 C1 C2 C3 179.6(3) . . . . ?
C1 C2 C3 C4 4.1(5) . . . . ?
C2 C3 C4 C5 -1.5(5) . . . . ?
C3 C4 C5 N1 -5.3(5) . . . . ?
C3 C4 C5 C6 168.6(3) . . . . ?
N1 C5 C6 C11 -37.7(4) . . . . ?
C4 C5 C6 C11 148.5(3) . . . . ?
N1 C5 C6 C7 140.5(3) . . . . ?
C4 C5 C6 C7 -33.3(4) . . . . ?
C11 C6 C7 C8 -3.2(4) . . . . ?
C5 C6 C7 C8 178.4(3) . . . . ?
C6 C7 C8 C9 0.0(5) . . . . ?
C7 C8 C9 C10 2.3(4) . . . . ?
C8 C9 C10 C11 -1.3(4) . . . . ?
C9 C10 C11 C6 -2.1(4) . . . . ?
C9 C10 C11 S1 177.4(2) . . . . ?
C7 C6 C11 C10 4.2(4) . . . . ?
C5 C6 C11 C10 -177.6(3) . . . . ?
C7 C6 C11 S1 -175.2(2) . . . . ?
C5 C6 C11 S1 3.0(4) . . . . ?
C20 C15 C16 C17 -0.5(6) . . . . ?
P1 C15 C16 C17 174.5(4) . . . . ?
C15 C16 C17 C18 0.2(8) . . . . ?
C16 C17 C18 C19 -0.2(8) . . . . ?
C17 C18 C19 C20 0.5(7) . . . . ?
C18 C19 C20 C15 -0.8(5) . . . . ?
C16 C15 C20 C19 0.8(5) . . . . ?
P1 C15 C20 C19 -174.2(3) . . . . ?
C26 C21 C22 C23 -1.1(4) . . . . ?
P1 C21 C22 C23 171.9(2) . . . . ?
C21 C22 C23 C24 1.4(5) . . . . ?
C22 C23 C24 C25 -0.4(5) . . . . ?
C23 C24 C25 C26 -1.0(5) . . . . ?
C24 C25 C26 C21 1.4(5) . . . . ?
C22 C21 C26 C25 -0.4(5) . . . . ?
P1 C21 C26 C25 -172.7(2) . . . . ?
C32 C27 C28 C29 -2.5(6) . . . . ?
P1 C27 C28 C29 174.2(3) . . . . ?
C27 C28 C29 C30 0.9(7) . . . . ?
C28 C29 C30 C31 0.9(7) . . . . ?
C29 C30 C31 C32 -1.1(6) . . . . ?
C28 C27 C32 C31 2.3(5) . . . . ?
P1 C27 C32 C31 -174.3(3) . . . . ?
C30 C31 C32 C27 -0.6(5) . . . . ?
N1 C1 N2 C13 6.5(4) . . . . ?
C2 C1 N2 C13 -173.3(3) . . . . ?
O1 C13 N2 C1 179.6(3) . . . . ?
Fe1 C13 N2 C1 4.3(4) . . . . ?
N2 C1 N1 C5 173.7(3) . . . . ?
C2 C1 N1 C5 -6.5(4) . . . . ?
N2 C1 N1 Fe1 -13.4(3) . . . . ?
C2 C1 N1 Fe1 166.4(2) . . . . ?
C4 C5 N1 C1 9.1(4) . . . . ?
C6 C5 N1 C1 -164.5(3) . . . . ?
C4 C5 N1 Fe1 -161.9(2) . . . . ?
C6 C5 N1 Fe1 24.4(4) . . . . ?
Cl1 C33 C34 Cl2 69.5(3) . . . . ?
Cl4 C36 C36B Cl4B 68.0(8) . . . . ?
Cl3 C35 C35A Cl3A 171.4(13) . . . . ?

_refine_diff_density_max         1.157
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.091

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2b
_database_code_depnum_ccdc_archive 'CCDC 1547032'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_shelx               
;
PROBLEM: Atom F19             has ADP max/min Ratio .....        4.4 prolat
RESPONSE: These fluorine atoms belong to the CF3 groups in the
BARF ion, which are very disordered. The regular disorder modeling did
not improve the situation.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          36 Note  
RESPONSE: These few reflections were blocked by the beam stop
and omitted by the data set.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C101 H66 B2 Cl2 F48 Fe2 N4 O6 P2 S2'
_chemical_formula_sum            'C101 H66 B2 Cl2 F48 Fe2 N4 O6 P2 S2'
_chemical_formula_weight         2673.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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'

_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                   12.2647(13)
_cell_length_b                   18.6289(19)
_cell_length_c                   24.731(3)
_cell_angle_alpha                90.896(3)
_cell_angle_beta                 95.597(2)
_cell_angle_gamma                95.427(3)
_cell_volume                     5596.6(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    107287
_cell_measurement_theta_min      0.663864
_cell_measurement_theta_max      1.000000

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_F_000             2676
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.507
_shelx_estimated_absorpt_T_min   0.928
_shelx_estimated_absorpt_T_max   0.956
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9279
_exptl_absorpt_correction_T_max  0.9558
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            107287
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_av_R_equivalents  0.1102
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.023
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             19749
_reflns_number_gt                13260
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'BRUKER SHELXTL'
_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)+(0.0578P)²+20.0693P] 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         19749
_refine_ls_number_parameters     1566
_refine_ls_number_restraints     1065
_refine_ls_R_factor_all          0.1265
_refine_ls_R_factor_gt           0.0831
_refine_ls_wR_factor_ref         0.1917
_refine_ls_wR_factor_gt          0.1697
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.082
_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
C1 C -0.0530(4) 0.9000(3) 0.33565(19) 0.0202(11) Uani 1 1 d . U . . .
C2 C -0.1428(4) 0.9188(3) 0.3623(2) 0.0241(12) Uani 1 1 d . U . . .
H2 H -0.1767 0.9616 0.3536 0.029 Uiso 1 1 calc R U . . .
C3 C -0.1799(4) 0.8737(3) 0.4009(2) 0.0274(12) Uani 1 1 d . U . . .
H3 H -0.2366 0.8866 0.4217 0.033 Uiso 1 1 calc R U . . .
C4 C -0.1344(4) 0.8088(3) 0.4097(2) 0.0243(12) Uani 1 1 d . U . . .
H4 H -0.1627 0.7762 0.4352 0.029 Uiso 1 1 calc R U . . .
C5 C -0.0479(4) 0.7914(3) 0.3815(2) 0.0251(12) Uani 1 1 d . U . . .
C6 C -0.0122(4) 0.7178(3) 0.3853(2) 0.0258(12) Uani 1 1 d . U . . .
C7 C -0.0944(5) 0.6605(3) 0.3872(2) 0.0316(13) Uani 1 1 d . U . . .
H7 H -0.1690 0.6706 0.3864 0.038 Uiso 1 1 calc R U . . .
C8 C -0.0695(5) 0.5899(3) 0.3900(2) 0.0399(15) Uani 1 1 d . U . . .
H8 H -0.1271 0.5523 0.3908 0.048 Uiso 1 1 calc R U . . .
C9 C 0.0378(6) 0.5733(3) 0.3915(2) 0.0422(16) Uani 1 1 d . U . . .
H9 H 0.0544 0.5246 0.3942 0.051 Uiso 1 1 calc R U . . .
C10 C 0.1214(5) 0.6284(3) 0.3891(2) 0.0372(15) Uani 1 1 d . U . . .
H10 H 0.1956 0.6175 0.3899 0.045 Uiso 1 1 calc R U . . .
C11 C 0.0966(5) 0.6991(3) 0.3855(2) 0.0305(13) Uani 1 1 d . U . . .
C12 C 0.2254(5) 0.8053(4) 0.4465(2) 0.0390(15) Uani 1 1 d . U . . .
H12A H 0.1574 0.8261 0.4533 0.058 Uiso 1 1 calc R U . . .
H12B H 0.2866 0.8435 0.4493 0.058 Uiso 1 1 calc R U . . .
H12C H 0.2407 0.7686 0.4734 0.058 Uiso 1 1 calc R U . . .
C13 C 0.0813(4) 0.9199(3) 0.2723(2) 0.0218(11) Uani 1 1 d . U . . .
C14 C 0.1943(4) 0.9233(3) 0.3621(2) 0.0273(12) Uani 1 1 d . U . . .
C15 C 0.2699(4) 0.8569(3) 0.2861(2) 0.0275(12) Uani 1 1 d . U . . .
C16 C -0.0671(5) 0.7793(3) 0.2229(3) 0.0399(15) Uani 1 1 d . U . . .
H16A H -0.0729 0.8287 0.2105 0.060 Uiso 1 1 calc R U . . .
H16B H -0.1133 0.7699 0.2526 0.060 Uiso 1 1 calc R U . . .
H16C H -0.0918 0.7451 0.1927 0.060 Uiso 1 1 calc R U . . .
C17 C 0.1473(5) 0.7841(3) 0.1861(2) 0.0397(15) Uani 1 1 d . U . . .
H17A H 0.1054 0.7577 0.1550 0.060 Uiso 1 1 calc R U . . .
H17B H 0.2207 0.7671 0.1920 0.060 Uiso 1 1 calc R U . . .
H17C H 0.1544 0.8358 0.1787 0.060 Uiso 1 1 calc R U . . .
C18 C 0.0748(5) 0.6718(3) 0.2551(2) 0.0363(14) Uani 1 1 d . U . . .
H18A H 0.0516 0.6469 0.2201 0.054 Uiso 1 1 calc R U . . .
H18B H 0.0235 0.6561 0.2815 0.054 Uiso 1 1 calc R U . . .
H18C H 0.1490 0.6603 0.2682 0.054 Uiso 1 1 calc R U . . .
C19 C 0.5906(4) 0.6753(3) 0.1259(2) 0.0296(13) Uani 1 1 d . U . . .
C20 C 0.4813(5) 0.6522(3) 0.1341(2) 0.0356(14) Uani 1 1 d . U . . .
H20 H 0.4236 0.6718 0.1125 0.043 Uiso 1 1 calc R U . . .
C21 C 0.4540(5) 0.6018(3) 0.1727(2) 0.0359(14) Uani 1 1 d . U . . .
C22 C 0.3357(6) 0.5810(4) 0.1798(3) 0.0542(18) Uani 1 1 d . U . . .
C23 C 0.5355(5) 0.5724(3) 0.2060(2) 0.0357(14) Uani 1 1 d . U . . .
H23 H 0.5171 0.5375 0.2320 0.043 Uiso 1 1 calc R U . . .
C24 C 0.6440(5) 0.5953(3) 0.2001(2) 0.0339(14) Uani 1 1 d . U . . .
C25 C 0.7335(5) 0.5653(4) 0.2342(3) 0.0444(16) Uani 1 1 d . U . . .
C26 C 0.6698(5) 0.6450(3) 0.1604(2) 0.0306(13) Uani 1 1 d . U . . .
H26 H 0.7452 0.6588 0.1566 0.037 Uiso 1 1 calc R U . . .
C27 C 0.7456(4) 0.7538(3) 0.0735(2) 0.0275(12) Uani 1 1 d . U . . .
C28 C 0.8118(5) 0.6974(3) 0.0649(2) 0.0301(13) Uani 1 1 d . U . . .
H28 H 0.7789 0.6491 0.0630 0.036 Uiso 1 1 calc R U . . .
C29 C 0.9226(5) 0.7102(3) 0.0591(2) 0.0336(14) Uani 1 1 d . U . . .
C30 C 0.9901(6) 0.6477(4) 0.0569(3) 0.0462(17) Uani 1 1 d . U . . .
C31 C 0.9733(5) 0.7792(4) 0.0583(2) 0.0371(15) Uani 1 1 d . U . . .
H31 H 1.0495 0.7874 0.0538 0.045 Uiso 1 1 calc R U . . .
C32 C 0.9098(4) 0.8371(3) 0.0642(2) 0.0315(13) Uani 1 1 d . U . . .
C33 C 0.9612(5) 0.9127(4) 0.0644(2) 0.0391(15) Uani 1 1 d . U . . .
C34 C 0.7990(4) 0.8232(3) 0.0723(2) 0.0267(12) Uani 1 1 d . U . . .
H34 H 0.7578 0.8630 0.0773 0.032 Uiso 1 1 calc R U . . .
C35 C 0.5536(5) 0.7134(3) 0.0206(2) 0.0317(13) Uani 1 1 d . U . . .
C36 C 0.5556(5) 0.7637(4) -0.0211(2) 0.0395(15) Uani 1 1 d . U . . .
H36 H 0.5922 0.8105 -0.0132 0.047 Uiso 1 1 calc R U . . .
C37 C 0.5057(5) 0.7477(4) -0.0740(3) 0.0450(16) Uani 1 1 d . U . . .
C38 C 0.5086(7) 0.8020(6) -0.1165(3) 0.069(2) Uani 1 1 d . U . . .
C39 C 0.4537(6) 0.6793(4) -0.0864(3) 0.0552(19) Uani 1 1 d . U . . .
H39 H 0.4203 0.6675 -0.1221 0.066 Uiso 1 1 calc R U . . .
C40 C 0.4511(6) 0.6288(4) -0.0467(3) 0.0548(19) Uani 1 1 d . U . . .
C41 C 0.3928(10) 0.5543(5) -0.0597(4) 0.095(3) Uani 1 1 d . U . . .
C42 C 0.5011(5) 0.6451(3) 0.0060(3) 0.0463(17) Uani 1 1 d . U . . .
H42 H 0.4992 0.6088 0.0325 0.056 Uiso 1 1 calc R U . . .
C43 C 0.5660(4) 0.8090(3) 0.1050(2) 0.0264(12) Uani 1 1 d . U . . .
C44 C 0.4695(5) 0.8349(3) 0.0836(2) 0.0336(14) Uani 1 1 d . U . . .
H44 H 0.4298 0.8110 0.0525 0.040 Uiso 1 1 calc R U . . .
C45 C 0.4279(5) 0.8944(3) 0.1055(3) 0.0391(15) Uani 1 1 d . U . . .
C46 C 0.3224(6) 0.9185(5) 0.0808(4) 0.066(2) Uani 1 1 d . U . . .
C47 C 0.4833(5) 0.9317(3) 0.1506(3) 0.0389(15) Uani 1 1 d . U . . .
H47 H 0.4555 0.9728 0.1656 0.047 Uiso 1 1 calc R U . . .
C48 C 0.5801(4) 0.9073(3) 0.1730(2) 0.0298(13) Uani 1 1 d . U . . .
C49 C 0.6409(5) 0.9451(3) 0.2226(2) 0.0380(15) Uani 1 1 d . U . . .
C50 C 0.6188(4) 0.8466(3) 0.1514(2) 0.0291(13) Uani 1 1 d . U . . .
H50 H 0.6838 0.8297 0.1688 0.035 Uiso 1 1 calc R U . . .
C51 C 1.0756(4) 0.1140(3) 0.1507(2) 0.0258(12) Uani 1 1 d . U . . .
C52 C 1.1515(4) 0.0848(3) 0.1200(2) 0.0288(13) Uani 1 1 d . U . . .
H52 H 1.1767 0.0391 0.1281 0.035 Uiso 1 1 calc R U . . .
C53 C 1.1881(4) 0.1238(3) 0.0780(2) 0.0298(13) Uani 1 1 d . U . . .
H53 H 1.2346 0.1040 0.0543 0.036 Uiso 1 1 calc R U . . .
C54 C 1.1567(4) 0.1929(3) 0.0702(2) 0.0300(13) Uani 1 1 d . U . . .
H54 H 1.1845 0.2209 0.0419 0.036 Uiso 1 1 calc R U . . .
C55 C 1.0860(4) 0.2213(3) 0.1028(2) 0.0269(12) Uani 1 1 d . U . . .
C56 C 1.0733(5) 0.2995(3) 0.1015(2) 0.0309(13) Uani 1 1 d . U . . .
C57 C 1.1668(6) 0.3453(3) 0.0907(2) 0.0405(15) Uani 1 1 d . U . . .
H57 H 1.2318 0.3245 0.0833 0.049 Uiso 1 1 calc R U . . .
C58 C 1.1663(6) 0.4193(4) 0.0906(3) 0.0520(18) Uani 1 1 d . U . . .
H58 H 1.2303 0.4488 0.0830 0.062 Uiso 1 1 calc R U . . .
C59 C 1.0735(7) 0.4505(4) 0.1015(3) 0.0561(19) Uani 1 1 d . U . . .
H59 H 1.0737 0.5015 0.1021 0.067 Uiso 1 1 calc R U . . .
C60 C 0.9796(6) 0.4076(3) 0.1117(3) 0.0483(17) Uani 1 1 d . U . . .
H60 H 0.9153 0.4294 0.1187 0.058 Uiso 1 1 calc R U . . .
C61 C 0.9784(5) 0.3324(3) 0.1119(2) 0.0368(14) Uani 1 1 d . U . . .
C62 C 0.8040(5) 0.2460(4) 0.0595(2) 0.0423(16) Uani 1 1 d . U . . .
H62A H 0.7903 0.2854 0.0347 0.063 Uiso 1 1 calc R U . . .
H62B H 0.7353 0.2152 0.0617 0.063 Uiso 1 1 calc R U . . .
H62C H 0.8591 0.2174 0.0459 0.063 Uiso 1 1 calc R U . . .
C63 C 0.9521(4) 0.1068(3) 0.2202(2) 0.0277(12) Uani 1 1 d . U . . .
C64 C 0.8227(5) 0.1231(4) 0.1374(2) 0.0371(15) Uani 1 1 d . U . . .
C65 C 0.7965(5) 0.1954(3) 0.2230(2) 0.0332(14) Uani 1 1 d . U . . .
C66 C 1.1507(6) 0.2898(4) 0.2364(3) 0.060(2) Uani 1 1 d . U . . .
H66A H 1.1894 0.3123 0.2699 0.091 Uiso 1 1 calc R U . . .
H66B H 1.1537 0.3242 0.2069 0.091 Uiso 1 1 calc R U . . .
H66C H 1.1861 0.2470 0.2267 0.091 Uiso 1 1 calc R U . . .
C67 C 1.0226(5) 0.2248(3) 0.3132(2) 0.0382(15) Uani 1 1 d . U . . .
H67A H 1.0607 0.1810 0.3115 0.057 Uiso 1 1 calc R U . . .
H67B H 0.9493 0.2126 0.3250 0.057 Uiso 1 1 calc R U . . .
H67C H 1.0650 0.2595 0.3392 0.057 Uiso 1 1 calc R U . . .
C68 C 0.9542(7) 0.3486(4) 0.2608(3) 0.069(2) Uani 1 1 d . U . . .
H68A H 1.0049 0.3772 0.2878 0.103 Uiso 1 1 calc R U . . .
H68B H 0.8825 0.3389 0.2749 0.103 Uiso 1 1 calc R U . . .
H68C H 0.9456 0.3756 0.2272 0.103 Uiso 1 1 calc R U . . .
C69 C 0.4302(4) 0.3372(3) 0.4422(2) 0.0203(11) Uani 1 1 d . U . . .
C70 C 0.5277(4) 0.3728(3) 0.4671(2) 0.0221(11) Uani 1 1 d . U . . .
H70 H 0.5672 0.3499 0.4958 0.026 Uiso 1 1 calc R U . . .
C71 C 0.5697(4) 0.4408(3) 0.4515(2) 0.0224(11) Uani 1 1 d . U . . .
C72 C 0.6792(4) 0.4749(3) 0.4765(2) 0.0311(13) Uani 1 1 d . U . . .
C73 C 0.5129(4) 0.4769(3) 0.4106(2) 0.0284(13) Uani 1 1 d . U . . .
H73 H 0.5403 0.5235 0.4002 0.034 Uiso 1 1 calc R U . . .
C74 C 0.4145(4) 0.4427(3) 0.3852(2) 0.0286(13) Uani 1 1 d . U . . .
C75 C 0.3515(5) 0.4789(3) 0.3415(2) 0.0401(15) Uani 1 1 d D U . . .
C76 C 0.3769(4) 0.3740(3) 0.3998(2) 0.0244(12) Uani 1 1 d . U . . .
H76 H 0.3122 0.3508 0.3803 0.029 Uiso 1 1 calc R U . . .
C77 C 0.4281(4) 0.2053(3) 0.40809(19) 0.0190(11) Uani 1 1 d . U . . .
C78 C 0.5402(4) 0.1940(3) 0.4119(2) 0.0211(11) Uani 1 1 d . U . . .
H78 H 0.5875 0.2148 0.4419 0.025 Uiso 1 1 calc R U . . .
C79 C 0.5846(4) 0.1533(3) 0.3729(2) 0.0207(11) Uani 1 1 d . U . . .
C80 C 0.7047(4) 0.1427(3) 0.3818(2) 0.0285(13) Uani 1 1 d . U . . .
C81 C 0.5197(4) 0.1219(3) 0.3283(2) 0.0243(12) Uani 1 1 d . U . . .
H81 H 0.5501 0.0937 0.3023 0.029 Uiso 1 1 calc R U . . .
C82 C 0.4086(4) 0.1328(3) 0.3228(2) 0.0235(12) Uani 1 1 d . U . . .
C83 C 0.3347(5) 0.0997(4) 0.2756(2) 0.0376(15) Uani 1 1 d . U . . .
C84 C 0.3642(4) 0.1743(3) 0.36168(19) 0.0210(11) Uani 1 1 d . U . . .
H84 H 0.2884 0.1818 0.3564 0.025 Uiso 1 1 calc R U . . .
C85 C 0.4243(4) 0.2285(3) 0.5162(2) 0.0209(11) Uani 1 1 d . U . . .
C86 C 0.4504(4) 0.1588(3) 0.5261(2) 0.0209(11) Uani 1 1 d . U . . .
H86 H 0.4536 0.1271 0.4960 0.025 Uiso 1 1 calc R U . . .
C87 C 0.4722(4) 0.1334(3) 0.5785(2) 0.0204(11) Uani 1 1 d . U . . .
C88 C 0.4928(4) 0.0564(3) 0.5864(2) 0.0289(13) Uani 1 1 d . U . . .
C89 C 0.4680(4) 0.1782(3) 0.6236(2) 0.0255(12) Uani 1 1 d . U . . .
H89 H 0.4832 0.1614 0.6594 0.031 Uiso 1 1 calc R U . . .
C90 C 0.4412(4) 0.2482(3) 0.6149(2) 0.0241(12) Uani 1 1 d . U . . .
C91 C 0.4335(5) 0.2949(3) 0.6642(2) 0.0395(15) Uani 1 1 d . U . . .
C92 C 0.4206(4) 0.2726(3) 0.5626(2) 0.0235(12) Uani 1 1 d . U . . .
H92 H 0.4033 0.3209 0.5579 0.028 Uiso 1 1 calc R U . . .
C93 C 0.2482(4) 0.2448(3) 0.45277(19) 0.0196(11) Uani 1 1 d . U . . .
C94 C 0.1923(4) 0.1753(3) 0.45018(19) 0.0202(11) Uani 1 1 d . U . . .
H94 H 0.2337 0.1349 0.4481 0.024 Uiso 1 1 calc R U . . .
C95 C 0.0784(4) 0.1631(3) 0.4505(2) 0.0238(12) Uani 1 1 d . U . . .
C96 C 0.0246(5) 0.0873(3) 0.4448(3) 0.0422(16) Uani 1 1 d . U . . .
C97 C 0.0144(4) 0.2205(3) 0.4533(2) 0.0248(12) Uani 1 1 d . U . . .
H97 H -0.0633 0.2125 0.4527 0.030 Uiso 1 1 calc R U . . .
C98 C 0.0672(4) 0.2897(3) 0.45692(19) 0.0221(11) Uani 1 1 d . U . . .
C99 C -0.0005(5) 0.3522(3) 0.4562(2) 0.0310(13) Uani 1 1 d . U . . .
C100 C 0.1810(4) 0.3018(3) 0.45721(19) 0.0197(11) Uani 1 1 d . U . . .
H100 H 0.2146 0.3500 0.4605 0.024 Uiso 1 1 calc R U . . .
C101 C 0.5491(9) 0.3160(5) 0.2906(4) 0.097(3) Uani 1 1 d . U . . .
H10A H 0.5600 0.2658 0.2804 0.116 Uiso 1 1 calc R U . . .
H10B H 0.4859 0.3145 0.3128 0.116 Uiso 1 1 calc R U . . .
F1 F 0.2670(3) 0.5944(3) 0.1372(2) 0.0959(19) Uani 1 1 d . U . . .
F2 F 0.3035(4) 0.6138(4) 0.2227(3) 0.117(2) Uani 1 1 d . U . . .
F3 F 0.3143(3) 0.5109(3) 0.18888(18) 0.0732(13) Uani 1 1 d . U . . .
F4 F 0.7004(3) 0.5290(3) 0.27662(18) 0.0775(14) Uani 1 1 d . U . . .
F5 F 0.7913(5) 0.5243(3) 0.20754(19) 0.113(2) Uani 1 1 d . U . . .
F6 F 0.8064(4) 0.6170(3) 0.25763(19) 0.0811(15) Uani 1 1 d . U . . .
F7 F 0.9339(4) 0.5866(3) 0.03492(19) 0.0905(17) Uani 1 1 d . U . . .
F8 F 1.0257(3) 0.62821(19) 0.10646(14) 0.0537(10) Uani 1 1 d . U . . .
F9 F 1.0764(5) 0.6590(3) 0.0306(3) 0.131(3) Uani 1 1 d . U . . .
F10 F 1.0448(3) 0.9216(2) 0.03383(18) 0.0649(12) Uani 1 1 d . U . . .
F11 F 1.0004(4) 0.9361(2) 0.11487(16) 0.0736(14) Uani 1 1 d . U . . .
F12 F 0.8907(3) 0.9593(2) 0.04588(17) 0.0571(10) Uani 1 1 d . U . . .
F13 F 0.5827(5) 0.7909(4) -0.1506(2) 0.132(2) Uani 1 1 d . U . . .
F14 F 0.5382(5) 0.8684(3) -0.0986(2) 0.108(2) Uani 1 1 d . U . . .
F15 F 0.4134(4) 0.8017(4) -0.1469(2) 0.121(2) Uani 1 1 d . U . . .
F16 F 0.4659(8) 0.5133(3) -0.0808(3) 0.165(3) Uani 1 1 d . U . . .
F17 F 0.3680(5) 0.5165(3) -0.0193(3) 0.117(2) Uani 1 1 d . U . . .
F18 F 0.3164(8) 0.5531(3) -0.0985(4) 0.217(5) Uani 1 1 d . U . . .
F19 F 0.2684(5) 0.8741(4) 0.0445(3) 0.184(4) Uani 1 1 d . U . . .
F20 F 0.3300(4) 0.9806(3) 0.0603(2) 0.112(2) Uani 1 1 d . U . . .
F21 F 0.2511(4) 0.9279(3) 0.1188(2) 0.0991(18) Uani 1 1 d . U . . .
F22 F 0.7480(3) 0.9401(2) 0.22632(18) 0.0730(14) Uani 1 1 d . U . . .
F23 F 0.6062(5) 0.9254(3) 0.26786(17) 0.113(2) Uani 1 1 d . U . . .
F24 F 0.6355(4) 1.0170(2) 0.2218(2) 0.0868(16) Uani 1 1 d . U . . .
F25 F 0.6996(3) 0.4579(2) 0.52879(15) 0.0569(11) Uani 1 1 d . U . . .
F26 F 0.7622(3) 0.45327(19) 0.45130(15) 0.0479(9) Uani 1 1 d . U . . .
F27 F 0.6887(3) 0.54658(18) 0.47513(17) 0.0529(10) Uani 1 1 d . U . . .
F28A F 0.3581(8) 0.4516(5) 0.2927(2) 0.110(3) Uani 0.75 1 d D U P A 1
F29A F 0.3702(6) 0.5504(3) 0.3434(3) 0.090(2) Uani 0.75 1 d D U P A 1
F30A F 0.2415(4) 0.4703(3) 0.3463(3) 0.0667(17) Uani 0.75 1 d D U P A 1
F28B F 0.2879(19) 0.4349(12) 0.3059(8) 0.110(3) Uani 0.25 1 d D U P A 2
F29B F 0.4140(14) 0.5154(11) 0.3076(9) 0.090(2) Uani 0.25 1 d D U P A 2
F30B F 0.2737(13) 0.5150(10) 0.3558(8) 0.0667(17) Uani 0.25 1 d D U P A 2
F31 F 0.7348(2) 0.12526(19) 0.43360(13) 0.0397(8) Uani 1 1 d . U . . .
F32 F 0.7345(3) 0.09126(19) 0.34960(13) 0.0421(9) Uani 1 1 d . U . . .
F33 F 0.7694(2) 0.20338(19) 0.37316(15) 0.0443(9) Uani 1 1 d . U . . .
F34A F 0.3594(6) 0.0342(4) 0.2621(3) 0.079(2) Uani 0.75 1 d . U P B 1
F35A F 0.3292(9) 0.1397(6) 0.2334(3) 0.108(4) Uani 0.75 1 d . U P B 1
F36A F 0.2289(5) 0.0873(4) 0.2871(3) 0.059(2) Uani 0.75 1 d . U P B 1
F34B F 0.3891(13) 0.0792(13) 0.2347(6) 0.047(4) Uani 0.25 1 d . U P B 2
F35B F 0.2782(18) 0.1472(12) 0.2512(8) 0.056(7) Uani 0.25 1 d . U P B 2
F36B F 0.267(2) 0.0495(14) 0.2874(9) 0.082(7) Uani 0.25 1 d . U P B 2
F37 F 0.5585(3) 0.03284(18) 0.55110(13) 0.0406(8) Uani 1 1 d . U . . .
F38 F 0.3987(3) 0.01205(18) 0.57824(17) 0.0540(10) Uani 1 1 d . U . . .
F39 F 0.5389(3) 0.04349(18) 0.63600(12) 0.0388(8) Uani 1 1 d . U . . .
F40 F 0.5271(4) 0.3053(3) 0.69591(16) 0.0777(14) Uani 1 1 d . U . . .
F41 F 0.4033(3) 0.36043(19) 0.65209(13) 0.0494(10) Uani 1 1 d . U . . .
F42 F 0.3577(4) 0.2663(2) 0.69519(17) 0.0777(15) Uani 1 1 d . U . . .
F43 F -0.0044(5) 0.0676(2) 0.3929(2) 0.100(2) Uani 1 1 d . U . . .
F44 F 0.0888(3) 0.03867(17) 0.46452(16) 0.0470(10) Uani 1 1 d . U . . .
F45 F -0.0653(3) 0.0793(2) 0.4708(2) 0.0855(17) Uani 1 1 d . U . . .
F46 F 0.0529(3) 0.41246(18) 0.47916(14) 0.0411(8) Uani 1 1 d . U . . .
F47 F -0.0922(3) 0.33857(19) 0.48200(15) 0.0463(9) Uani 1 1 d . U . . .
F48 F -0.0361(3) 0.36939(19) 0.40494(13) 0.0466(9) Uani 1 1 d . U . . .
Fe1 Fe 0.14542(6) 0.84655(4) 0.31700(3) 0.02142(18) Uani 1 1 d . U . . .
Fe2 Fe 0.90544(6) 0.19066(4) 0.18181(3) 0.0267(2) Uani 1 1 d . U . . .
N1 N -0.0015(3) 0.8402(2) 0.34704(16) 0.0218(9) Uani 1 1 d . U . . .
N2 N -0.0098(3) 0.9411(2) 0.29562(17) 0.0239(10) Uani 1 1 d . U . . .
H2A H -0.0395 0.9803 0.2849 0.029 Uiso 1 1 calc R U . . .
N3 N 1.0383(4) 0.1788(2) 0.14115(16) 0.0239(10) Uani 1 1 d . U . . .
N4 N 1.0324(4) 0.0781(2) 0.19250(17) 0.0268(10) Uani 1 1 d . U . . .
H4A H 1.0554 0.0364 0.2021 0.032 Uiso 1 1 calc R U . . .
O1 O 0.1119(3) 0.94995(18) 0.23201(13) 0.0239(8) Uani 1 1 d . U . . .
O2 O 0.2249(3) 0.9739(2) 0.38832(17) 0.0412(10) Uani 1 1 d . U . . .
O3 O 0.3490(3) 0.8649(2) 0.26473(15) 0.0340(9) Uani 1 1 d . U . . .
O4 O 0.9183(3) 0.0758(2) 0.25949(15) 0.0308(9) Uani 1 1 d . U . . .
O5 O 0.7692(4) 0.0771(3) 0.11375(19) 0.0526(12) Uani 1 1 d . U . . .
O6 O 0.7259(3) 0.1967(2) 0.25053(17) 0.0436(11) Uani 1 1 d . U . . .
P1 P 0.07547(12) 0.76867(8) 0.24667(6) 0.0260(3) Uani 1 1 d . U . . .
P2 P 1.00950(14) 0.26381(9) 0.24692(6) 0.0341(4) Uani 1 1 d . U . . .
S1 S 0.21002(11) 0.76427(8) 0.37893(6) 0.0298(3) Uani 1 1 d . U . . .
S2 S 0.85448(13) 0.28331(9) 0.12667(6) 0.0372(4) Uani 1 1 d . U . . .
B1 B 0.6155(5) 0.7377(4) 0.0813(3) 0.0296(15) Uani 1 1 d . U . . .
B2 B 0.3833(4) 0.2545(3) 0.4546(2) 0.0202(13) Uani 1 1 d . U . . .
Cl1 Cl 0.5203(6) 0.3623(2) 0.23402(15) 0.218(3) Uani 1 1 d . U . . .
Cl2 Cl 0.6701(4) 0.35619(16) 0.33017(15) 0.1410(14) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.352(6) . ?
C1 N2 1.376(6) . ?
C1 C2 1.406(7) . ?
C2 C3 1.365(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(7) . ?
C4 H4 0.9500 . ?
C5 N1 1.377(6) . ?
C5 C6 1.480(7) . ?
C6 C7 1.401(8) . ?
C6 C11 1.411(7) . ?
C7 C8 1.379(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.378(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.386(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.381(8) . ?
C10 H10 0.9500 . ?
C11 S1 1.780(6) . ?
C12 S1 1.812(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O1 1.225(6) . ?
C13 N2 1.392(6) . ?
C13 Fe1 1.946(5) . ?
C14 O2 1.148(6) . ?
C14 Fe1 1.818(6) . ?
C15 O3 1.148(6) . ?
C15 Fe1 1.768(5) . ?
C16 P1 1.820(6) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 P1 1.824(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 P1 1.819(6) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C26 1.395(8) . ?
C19 C20 1.404(8) . ?
C19 B1 1.644(9) . ?
C20 C21 1.391(8) . ?
C20 H20 0.9500 . ?
C21 C23 1.390(8) . ?
C21 C22 1.493(9) . ?
C22 F1 1.325(8) . ?
C22 F2 1.327(8) . ?
C22 F3 1.333(8) . ?
C23 C24 1.380(8) . ?
C23 H23 0.9500 . ?
C24 C26 1.398(8) . ?
C24 C25 1.476(8) . ?
C25 F5 1.301(8) . ?
C25 F4 1.333(7) . ?
C25 F6 1.335(7) . ?
C26 H26 0.9500 . ?
C27 C34 1.395(8) . ?
C27 C28 1.413(7) . ?
C27 B1 1.626(8) . ?
C28 C29 1.379(8) . ?
C28 H28 0.9500 . ?
C29 C31 1.374(9) . ?
C29 C30 1.496(8) . ?
C30 F9 1.298(8) . ?
C30 F8 1.329(7) . ?
C30 F7 1.350(8) . ?
C31 C32 1.404(8) . ?
C31 H31 0.9500 . ?
C32 C34 1.393(7) . ?
C32 C33 1.487(8) . ?
C33 F10 1.331(7) . ?
C33 F12 1.336(7) . ?
C33 F11 1.345(7) . ?
C34 H34 0.9500 . ?
C35 C42 1.396(8) . ?
C35 C36 1.403(8) . ?
C35 B1 1.651(8) . ?
C36 C37 1.404(8) . ?
C36 H36 0.9500 . ?
C37 C39 1.386(10) . ?
C37 C38 1.471(10) . ?
C38 F14 1.314(10) . ?
C38 F13 1.326(10) . ?
C38 F15 1.326(8) . ?
C39 C40 1.371(10) . ?
C39 H39 0.9500 . ?
C40 C42 1.402(8) . ?
C40 C41 1.515(12) . ?
C41 F18 1.272(10) . ?
C41 F17 1.276(11) . ?
C41 F16 1.367(13) . ?
C42 H42 0.9500 . ?
C43 C44 1.382(7) . ?
C43 C50 1.405(7) . ?
C43 B1 1.634(8) . ?
C44 C45 1.387(8) . ?
C44 H44 0.9500 . ?
C45 C47 1.389(8) . ?
C45 C46 1.487(9) . ?
C46 F20 1.270(10) . ?
C46 F19 1.298(9) . ?
C46 F21 1.363(9) . ?
C47 C48 1.380(8) . ?
C47 H47 0.9500 . ?
C48 C50 1.386(7) . ?
C48 C49 1.500(8) . ?
C49 F23 1.283(7) . ?
C49 F22 1.320(7) . ?
C49 F24 1.348(7) . ?
C50 H50 0.9500 . ?
C51 N3 1.347(6) . ?
C51 N4 1.363(7) . ?
C51 C52 1.401(7) . ?
C52 C53 1.365(7) . ?
C52 H52 0.9500 . ?
C53 C54 1.387(8) . ?
C53 H53 0.9500 . ?
C54 C55 1.376(7) . ?
C54 H54 0.9500 . ?
C55 N3 1.383(7) . ?
C55 C56 1.481(8) . ?
C56 C61 1.409(8) . ?
C56 C57 1.412(8) . ?
C57 C58 1.380(9) . ?
C57 H57 0.9500 . ?
C58 C59 1.373(10) . ?
C58 H58 0.9500 . ?
C59 C60 1.385(10) . ?
C59 H59 0.9500 . ?
C60 C61 1.399(8) . ?
C60 H60 0.9500 . ?
C61 S2 1.771(7) . ?
C62 S2 1.819(6) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 O4 1.225(6) . ?
C63 N4 1.395(7) . ?
C63 Fe2 1.943(6) . ?
C64 O5 1.146(7) . ?
C64 Fe2 1.821(6) . ?
C65 O6 1.154(6) . ?
C65 Fe2 1.765(6) . ?
C66 P2 1.799(7) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 P2 1.804(6) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 P2 1.818(7) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 C70 1.394(7) . ?
C69 C76 1.404(7) . ?
C69 B2 1.638(8) . ?
C70 C71 1.396(7) . ?
C70 H70 0.9500 . ?
C71 C73 1.390(7) . ?
C71 C72 1.502(7) . ?
C72 F27 1.330(6) . ?
C72 F26 1.333(6) . ?
C72 F25 1.343(7) . ?
C73 C74 1.396(8) . ?
C73 H73 0.9500 . ?
C74 C76 1.385(7) . ?
C74 C75 1.476(8) . ?
C75 F30B 1.293(13) . ?
C75 F28A 1.313(8) . ?
C75 F29A 1.331(7) . ?
C75 F28B 1.331(15) . ?
C75 F29B 1.341(14) . ?
C75 F30A 1.361(7) . ?
C76 H76 0.9500 . ?
C77 C78 1.405(7) . ?
C77 C84 1.408(7) . ?
C77 B2 1.628(7) . ?
C78 C79 1.400(7) . ?
C78 H78 0.9500 . ?
C79 C81 1.382(7) . ?
C79 C80 1.499(7) . ?
C80 F32 1.336(6) . ?
C80 F31 1.351(6) . ?
C80 F33 1.352(6) . ?
C81 C82 1.391(7) . ?
C81 H81 0.9500 . ?
C82 C84 1.406(7) . ?
C82 C83 1.494(7) . ?
C83 F36B 1.25(2) . ?
C83 F35A 1.292(10) . ?
C83 F35B 1.295(19) . ?
C83 F34A 1.330(9) . ?
C83 F34B 1.336(15) . ?
C83 F36A 1.354(8) . ?
C84 H84 0.9500 . ?
C85 C86 1.385(7) . ?
C85 C92 1.409(7) . ?
C85 B2 1.651(8) . ?
C86 C87 1.397(7) . ?
C86 H86 0.9500 . ?
C87 C89 1.391(7) . ?
C87 C88 1.491(7) . ?
C88 F39 1.336(6) . ?
C88 F37 1.340(6) . ?
C88 F38 1.351(6) . ?
C89 C90 1.390(7) . ?
C89 H89 0.9500 . ?
C90 C92 1.385(7) . ?
C90 C91 1.501(8) . ?
C91 F40 1.322(7) . ?
C91 F41 1.339(7) . ?
C91 F42 1.340(7) . ?
C92 H92 0.9500 . ?
C93 C94 1.404(7) . ?
C93 C100 1.414(7) . ?
C93 B2 1.646(7) . ?
C94 C95 1.394(7) . ?
C94 H94 0.9500 . ?
C95 C97 1.390(7) . ?
C95 C96 1.500(8) . ?
C96 F44 1.324(7) . ?
C96 F45 1.327(7) . ?
C96 F43 1.335(8) . ?
C97 C98 1.384(7) . ?
C97 H97 0.9500 . ?
C98 C100 1.391(7) . ?
C98 C99 1.493(7) . ?
C99 F46 1.333(7) . ?
C99 F47 1.351(6) . ?
C99 F48 1.354(6) . ?
C100 H100 0.9500 . ?
C101 Cl1 1.682(10) . ?
C101 Cl2 1.791(12) . ?
C101 H10A 0.9900 . ?
C101 H10B 0.9900 . ?
Fe1 N1 2.009(4) . ?
Fe1 P1 2.2937(16) . ?
Fe1 S1 2.3216(15) . ?
Fe2 N3 2.024(4) . ?
Fe2 P2 2.2979(17) . ?
Fe2 S2 2.3109(16) . ?
N2 H2A 0.8800 . ?
N4 H4A 0.8800 . ?

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
N1 C1 N2 114.1(4) . . ?
N1 C1 C2 123.1(4) . . ?
N2 C1 C2 122.8(5) . . ?
C3 C2 C1 117.9(5) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 119.8(5) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.8 . . ?
C3 C4 H4 119.8 . . ?
N1 C5 C4 120.3(5) . . ?
N1 C5 C6 120.4(4) . . ?
C4 C5 C6 119.1(5) . . ?
C7 C6 C11 116.3(5) . . ?
C7 C6 C5 117.2(5) . . ?
C11 C6 C5 126.4(5) . . ?
C8 C7 C6 121.6(5) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 C7 120.9(6) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
C8 C9 C10 119.2(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 120.0(6) . . ?
C11 C10 H10 120.0 . . ?
C9 C10 H10 120.0 . . ?
C10 C11 C6 121.9(5) . . ?
C10 C11 S1 115.7(4) . . ?
C6 C11 S1 122.3(4) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 N2 120.2(5) . . ?
O1 C13 Fe1 130.8(4) . . ?
N2 C13 Fe1 108.8(3) . . ?
O2 C14 Fe1 176.5(5) . . ?
O3 C15 Fe1 177.7(5) . . ?
P1 C16 H16A 109.5 . . ?
P1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
P1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
P1 C17 H17A 109.5 . . ?
P1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
P1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
P1 C18 H18A 109.5 . . ?
P1 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
P1 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C26 C19 C20 114.6(5) . . ?
C26 C19 B1 125.7(5) . . ?
C20 C19 B1 119.5(5) . . ?
C21 C20 C19 122.8(5) . . ?
C21 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C23 C21 C20 120.7(5) . . ?
C23 C21 C22 119.6(6) . . ?
C20 C21 C22 119.6(6) . . ?
F1 C22 F2 107.2(7) . . ?
F1 C22 F3 105.4(6) . . ?
F2 C22 F3 104.3(6) . . ?
F1 C22 C21 113.9(6) . . ?
F2 C22 C21 112.3(6) . . ?
F3 C22 C21 113.0(6) . . ?
C24 C23 C21 118.2(6) . . ?
C24 C23 H23 120.9 . . ?
C21 C23 H23 120.9 . . ?
C23 C24 C26 120.1(5) . . ?
C23 C24 C25 120.2(5) . . ?
C26 C24 C25 119.6(5) . . ?
F5 C25 F4 108.2(6) . . ?
F5 C25 F6 105.0(6) . . ?
F4 C25 F6 102.6(5) . . ?
F5 C25 C24 114.1(6) . . ?
F4 C25 C24 114.1(5) . . ?
F6 C25 C24 111.9(5) . . ?
C19 C26 C24 123.5(5) . . ?
C19 C26 H26 118.3 . . ?
C24 C26 H26 118.3 . . ?
C34 C27 C28 115.0(5) . . ?
C34 C27 B1 123.4(5) . . ?
C28 C27 B1 121.6(5) . . ?
C29 C28 C27 122.2(6) . . ?
C29 C28 H28 118.9 . . ?
C27 C28 H28 118.9 . . ?
C31 C29 C28 121.5(5) . . ?
C31 C29 C30 119.4(6) . . ?
C28 C29 C30 119.1(6) . . ?
F9 C30 F8 106.5(6) . . ?
F9 C30 F7 106.2(6) . . ?
F8 C30 F7 103.1(6) . . ?
F9 C30 C29 114.8(6) . . ?
F8 C30 C29 111.1(5) . . ?
F7 C30 C29 114.2(5) . . ?
C29 C31 C32 118.4(5) . . ?
C29 C31 H31 120.8 . . ?
C32 C31 H31 120.8 . . ?
C34 C32 C31 119.3(6) . . ?
C34 C32 C33 120.2(5) . . ?
C31 C32 C33 120.4(5) . . ?
F10 C33 F12 105.5(5) . . ?
F10 C33 F11 106.7(5) . . ?
F12 C33 F11 106.1(5) . . ?
F10 C33 C32 113.6(5) . . ?
F12 C33 C32 113.0(5) . . ?
F11 C33 C32 111.4(5) . . ?
C32 C34 C27 123.5(5) . . ?
C32 C34 H34 118.3 . . ?
C27 C34 H34 118.3 . . ?
C42 C35 C36 116.0(5) . . ?
C42 C35 B1 125.3(5) . . ?
C36 C35 B1 118.8(5) . . ?
C35 C36 C37 122.7(6) . . ?
C35 C36 H36 118.7 . . ?
C37 C36 H36 118.7 . . ?
C39 C37 C36 119.4(6) . . ?
C39 C37 C38 119.5(6) . . ?
C36 C37 C38 121.2(7) . . ?
F14 C38 F13 103.0(7) . . ?
F14 C38 F15 107.9(8) . . ?
F13 C38 F15 105.9(7) . . ?
F14 C38 C37 114.7(7) . . ?
F13 C38 C37 112.0(8) . . ?
F15 C38 C37 112.6(7) . . ?
C40 C39 C37 119.3(6) . . ?
C40 C39 H39 120.3 . . ?
C37 C39 H39 120.3 . . ?
C39 C40 C42 121.1(7) . . ?
C39 C40 C41 119.7(7) . . ?
C42 C40 C41 119.2(7) . . ?
F18 C41 F17 114.3(12) . . ?
F18 C41 F16 102.1(9) . . ?
F17 C41 F16 100.4(8) . . ?
F18 C41 C40 113.4(8) . . ?
F17 C41 C40 116.6(8) . . ?
F16 C41 C40 107.8(10) . . ?
C35 C42 C40 121.6(6) . . ?
C35 C42 H42 119.2 . . ?
C40 C42 H42 119.2 . . ?
C44 C43 C50 115.1(5) . . ?
C44 C43 B1 124.2(5) . . ?
C50 C43 B1 120.6(5) . . ?
C43 C44 C45 122.9(5) . . ?
C43 C44 H44 118.5 . . ?
C45 C44 H44 118.5 . . ?
C44 C45 C47 120.8(5) . . ?
C44 C45 C46 119.9(6) . . ?
C47 C45 C46 119.4(5) . . ?
F20 C46 F19 107.5(9) . . ?
F20 C46 F21 100.9(6) . . ?
F19 C46 F21 105.4(8) . . ?
F20 C46 C45 115.1(7) . . ?
F19 C46 C45 114.7(6) . . ?
F21 C46 C45 112.0(7) . . ?
C48 C47 C45 117.8(5) . . ?
C48 C47 H47 121.1 . . ?
C45 C47 H47 121.1 . . ?
C47 C48 C50 120.6(5) . . ?
C47 C48 C49 119.4(5) . . ?
C50 C48 C49 120.0(5) . . ?
F23 C49 F22 107.7(6) . . ?
F23 C49 F24 105.0(5) . . ?
F22 C49 F24 102.3(5) . . ?
F23 C49 C48 115.1(5) . . ?
F22 C49 C48 113.3(5) . . ?
F24 C49 C48 112.3(5) . . ?
C48 C50 C43 122.7(5) . . ?
C48 C50 H50 118.6 . . ?
C43 C50 H50 118.6 . . ?
N3 C51 N4 114.7(5) . . ?
N3 C51 C52 123.2(5) . . ?
N4 C51 C52 122.1(5) . . ?
C53 C52 C51 118.0(5) . . ?
C53 C52 H52 121.0 . . ?
C51 C52 H52 121.0 . . ?
C52 C53 C54 119.4(5) . . ?
C52 C53 H53 120.3 . . ?
C54 C53 H53 120.3 . . ?
C55 C54 C53 121.0(5) . . ?
C55 C54 H54 119.5 . . ?
C53 C54 H54 119.5 . . ?
C54 C55 N3 119.8(5) . . ?
C54 C55 C56 119.4(5) . . ?
N3 C55 C56 120.3(5) . . ?
C61 C56 C57 117.3(5) . . ?
C61 C56 C55 126.1(5) . . ?
C57 C56 C55 116.5(5) . . ?
C58 C57 C56 121.8(6) . . ?
C58 C57 H57 119.1 . . ?
C56 C57 H57 119.1 . . ?
C59 C58 C57 120.1(7) . . ?
C59 C58 H58 120.0 . . ?
C57 C58 H58 120.0 . . ?
C58 C59 C60 120.0(7) . . ?
C58 C59 H59 120.0 . . ?
C60 C59 H59 120.0 . . ?
C59 C60 C61 120.7(7) . . ?
C59 C60 H60 119.6 . . ?
C61 C60 H60 119.6 . . ?
C60 C61 C56 120.0(6) . . ?
C60 C61 S2 116.6(5) . . ?
C56 C61 S2 123.3(5) . . ?
S2 C62 H62A 109.5 . . ?
S2 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
S2 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O4 C63 N4 119.9(5) . . ?
O4 C63 Fe2 131.4(4) . . ?
N4 C63 Fe2 108.5(4) . . ?
O5 C64 Fe2 173.7(6) . . ?
O6 C65 Fe2 178.1(5) . . ?
P2 C66 H66A 109.5 . . ?
P2 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
P2 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
P2 C67 H67A 109.5 . . ?
P2 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
P2 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
P2 C68 H68A 109.5 . . ?
P2 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
P2 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C70 C69 C76 115.5(5) . . ?
C70 C69 B2 124.8(5) . . ?
C76 C69 B2 119.4(4) . . ?
C69 C70 C71 122.6(5) . . ?
C69 C70 H70 118.7 . . ?
C71 C70 H70 118.7 . . ?
C73 C71 C70 120.4(5) . . ?
C73 C71 C72 118.6(5) . . ?
C70 C71 C72 120.9(5) . . ?
F27 C72 F26 106.4(4) . . ?
F27 C72 F25 106.5(5) . . ?
F26 C72 F25 105.9(5) . . ?
F27 C72 C71 113.3(5) . . ?
F26 C72 C71 111.9(5) . . ?
F25 C72 C71 112.3(4) . . ?
C71 C73 C74 118.2(5) . . ?
C71 C73 H73 120.9 . . ?
C74 C73 H73 120.9 . . ?
C76 C74 C73 120.3(5) . . ?
C76 C74 C75 119.5(5) . . ?
C73 C74 C75 120.1(5) . . ?
F28A C75 F29A 112.4(7) . . ?
F30B C75 F28B 96.1(14) . . ?
F30B C75 F29B 112.2(13) . . ?
F28B C75 F29B 100.0(14) . . ?
F28A C75 F30A 102.9(7) . . ?
F29A C75 F30A 100.9(6) . . ?
F30B C75 C74 116.5(9) . . ?
F28A C75 C74 113.7(6) . . ?
F29A C75 C74 114.1(5) . . ?
F28B C75 C74 115.3(11) . . ?
F29B C75 C74 114.2(9) . . ?
F30A C75 C74 111.7(5) . . ?
C74 C76 C69 122.8(5) . . ?
C74 C76 H76 118.6 . . ?
C69 C76 H76 118.6 . . ?
C78 C77 C84 115.3(4) . . ?
C78 C77 B2 119.2(4) . . ?
C84 C77 B2 125.4(4) . . ?
C79 C78 C77 122.2(5) . . ?
C79 C78 H78 118.9 . . ?
C77 C78 H78 118.9 . . ?
C81 C79 C78 121.4(5) . . ?
C81 C79 C80 120.7(5) . . ?
C78 C79 C80 117.9(5) . . ?
F32 C80 F31 107.1(4) . . ?
F32 C80 F33 106.4(4) . . ?
F31 C80 F33 105.2(4) . . ?
F32 C80 C79 113.5(4) . . ?
F31 C80 C79 111.9(4) . . ?
F33 C80 C79 112.2(4) . . ?
C79 C81 C82 118.0(5) . . ?
C79 C81 H81 121.0 . . ?
C82 C81 H81 121.0 . . ?
C81 C82 C84 120.7(5) . . ?
C81 C82 C83 120.1(5) . . ?
C84 C82 C83 119.2(5) . . ?
F36B C83 F35B 106.7(18) . . ?
F35A C83 F34A 110.4(8) . . ?
F36B C83 F34B 110.3(16) . . ?
F35B C83 F34B 99.7(12) . . ?
F35A C83 F36A 104.2(7) . . ?
F34A C83 F36A 102.7(6) . . ?
F36B C83 C82 114.5(11) . . ?
F35A C83 C82 113.9(6) . . ?
F35B C83 C82 111.2(10) . . ?
F34A C83 C82 112.5(5) . . ?
F34B C83 C82 113.3(8) . . ?
F36A C83 C82 112.2(5) . . ?
C82 C84 C77 122.4(4) . . ?
C82 C84 H84 118.8 . . ?
C77 C84 H84 118.8 . . ?
C86 C85 C92 115.7(5) . . ?
C86 C85 B2 122.0(4) . . ?
C92 C85 B2 121.8(4) . . ?
C85 C86 C87 122.7(5) . . ?
C85 C86 H86 118.6 . . ?
C87 C86 H86 118.6 . . ?
C89 C87 C86 120.3(5) . . ?
C89 C87 C88 119.6(5) . . ?
C86 C87 C88 120.0(5) . . ?
F39 C88 F37 106.6(4) . . ?
F39 C88 F38 106.7(4) . . ?
F37 C88 F38 105.1(4) . . ?
F39 C88 C87 113.6(4) . . ?
F37 C88 C87 112.7(4) . . ?
F38 C88 C87 111.6(4) . . ?
C90 C89 C87 118.2(5) . . ?
C90 C89 H89 120.9 . . ?
C87 C89 H89 120.9 . . ?
C92 C90 C89 120.6(5) . . ?
C92 C90 C91 122.1(5) . . ?
C89 C90 C91 117.3(5) . . ?
F40 C91 F41 106.4(5) . . ?
F40 C91 F42 106.5(5) . . ?
F41 C91 F42 105.0(5) . . ?
F40 C91 C90 113.2(5) . . ?
F41 C91 C90 113.3(5) . . ?
F42 C91 C90 111.8(5) . . ?
C90 C92 C85 122.4(5) . . ?
C90 C92 H92 118.8 . . ?
C85 C92 H92 118.8 . . ?
C94 C93 C100 115.1(4) . . ?
C94 C93 B2 119.6(4) . . ?
C100 C93 B2 125.1(4) . . ?
C95 C94 C93 122.6(5) . . ?
C95 C94 H94 118.7 . . ?
C93 C94 H94 118.7 . . ?
C97 C95 C94 120.7(5) . . ?
C97 C95 C96 120.0(5) . . ?
C94 C95 C96 119.2(5) . . ?
F44 C96 F45 106.2(5) . . ?
F44 C96 F43 105.6(6) . . ?
F45 C96 F43 107.6(6) . . ?
F44 C96 C95 113.5(5) . . ?
F45 C96 C95 111.6(5) . . ?
F43 C96 C95 111.9(5) . . ?
C98 C97 C95 118.1(5) . . ?
C98 C97 H97 121.0 . . ?
C95 C97 H97 121.0 . . ?
C97 C98 C100 121.2(5) . . ?
C97 C98 C99 118.9(5) . . ?
C100 C98 C99 119.7(5) . . ?
F46 C99 F47 106.5(4) . . ?
F46 C99 F48 105.9(4) . . ?
F47 C99 F48 105.7(4) . . ?
F46 C99 C98 113.9(5) . . ?
F47 C99 C98 112.4(4) . . ?
F48 C99 C98 111.8(4) . . ?
C98 C100 C93 122.1(5) . . ?
C98 C100 H100 118.9 . . ?
C93 C100 H100 118.9 . . ?
Cl1 C101 Cl2 111.5(6) . . ?
Cl1 C101 H10A 109.3 . . ?
Cl2 C101 H10A 109.3 . . ?
Cl1 C101 H10B 109.3 . . ?
Cl2 C101 H10B 109.3 . . ?
H10A C101 H10B 108.0 . . ?
C15 Fe1 C14 89.8(2) . . ?
C15 Fe1 C13 92.5(2) . . ?
C14 Fe1 C13 83.1(2) . . ?
C15 Fe1 N1 175.0(2) . . ?
C14 Fe1 N1 90.5(2) . . ?
C13 Fe1 N1 82.58(19) . . ?
C15 Fe1 P1 87.90(18) . . ?
C14 Fe1 P1 167.53(18) . . ?
C13 Fe1 P1 84.82(15) . . ?
N1 Fe1 P1 90.77(13) . . ?
C15 Fe1 S1 93.36(18) . . ?
C14 Fe1 S1 92.85(18) . . ?
C13 Fe1 S1 172.81(15) . . ?
N1 Fe1 S1 91.58(12) . . ?
P1 Fe1 S1 99.51(6) . . ?
C65 Fe2 C64 90.8(3) . . ?
C65 Fe2 C63 90.8(2) . . ?
C64 Fe2 C63 83.4(3) . . ?
C65 Fe2 N3 173.7(2) . . ?
C64 Fe2 N3 90.8(2) . . ?
C63 Fe2 N3 83.3(2) . . ?
C65 Fe2 P2 86.1(2) . . ?
C64 Fe2 P2 172.0(2) . . ?
C63 Fe2 P2 89.29(16) . . ?
N3 Fe2 P2 91.57(13) . . ?
C65 Fe2 S2 94.47(19) . . ?
C64 Fe2 S2 92.0(2) . . ?
C63 Fe2 S2 173.05(17) . . ?
N3 Fe2 S2 91.58(12) . . ?
P2 Fe2 S2 95.58(6) . . ?
C1 N1 C5 117.8(4) . . ?
C1 N1 Fe1 110.8(3) . . ?
C5 N1 Fe1 130.8(3) . . ?
C1 N2 C13 119.3(4) . . ?
C1 N2 H2A 120.4 . . ?
C13 N2 H2A 120.4 . . ?
C51 N3 C55 117.9(4) . . ?
C51 N3 Fe2 110.6(3) . . ?
C55 N3 Fe2 131.1(3) . . ?
C51 N4 C63 120.7(5) . . ?
C51 N4 H4A 119.7 . . ?
C63 N4 H4A 119.7 . . ?
C18 P1 C16 103.0(3) . . ?
C18 P1 C17 103.0(3) . . ?
C16 P1 C17 103.4(3) . . ?
C18 P1 Fe1 120.0(2) . . ?
C16 P1 Fe1 113.4(2) . . ?
C17 P1 Fe1 112.1(2) . . ?
C66 P2 C67 102.0(3) . . ?
C66 P2 C68 104.1(4) . . ?
C67 P2 C68 102.3(3) . . ?
C66 P2 Fe2 117.7(2) . . ?
C67 P2 Fe2 113.9(2) . . ?
C68 P2 Fe2 114.8(3) . . ?
C11 S1 C12 99.7(3) . . ?
C11 S1 Fe1 105.82(18) . . ?
C12 S1 Fe1 109.0(2) . . ?
C61 S2 C62 100.2(3) . . ?
C61 S2 Fe2 106.2(2) . . ?
C62 S2 Fe2 108.9(2) . . ?
C27 B1 C43 111.3(5) . . ?
C27 B1 C19 113.1(5) . . ?
C43 B1 C19 104.4(4) . . ?
C27 B1 C35 106.1(4) . . ?
C43 B1 C35 110.8(4) . . ?
C19 B1 C35 111.1(5) . . ?
C77 B2 C69 104.6(4) . . ?
C77 B2 C93 112.2(4) . . ?
C69 B2 C93 112.0(4) . . ?
C77 B2 C85 111.3(4) . . ?
C69 B2 C85 113.6(4) . . ?
C93 B2 C85 103.4(4) . . ?

_refine_diff_density_max         1.002
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.090

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2g
_database_code_depnum_ccdc_archive 'CCDC 1547035'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C25 H24 N2 Fe Cl4 O3 S2'
_chemical_formula_sum            'C16.33 H15.33 Cl2 Fe0.67 N1.33 O2 S1.33'
_chemical_formula_weight         413.18

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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        'I 2/a'
_space_group_name_Hall           '-I 2ya'

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

_cell_length_a                   17.0361(6)
_cell_length_b                   14.2521(5)
_cell_length_c                   26.0871(9)
_cell_angle_alpha                90
_cell_angle_beta                 90.091(3)
_cell_angle_gamma                90
_cell_volume                     6333.9(4)
_cell_formula_units_Z            12
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    4591
_cell_measurement_theta_min      3.3540
_cell_measurement_theta_max      70.7280

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_F_000             2536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.510
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    7.595
_shelx_estimated_absorpt_T_min   0.113
_shelx_estimated_absorpt_T_max   0.804
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.29408
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            22169
_diffrn_reflns_av_unetI/netI     0.0806
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_theta_min         3.388
_diffrn_reflns_theta_max         74.182
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measured_fraction_theta_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_point_group_measured_fraction_full 0.989
_reflns_number_total             6220
_reflns_number_gt                4551
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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


_computing_data_collection       'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.27t (Agilent, 2015)'
_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'

_refine_special_details          
;
 ?
;

# SQUEEZE RESULTS (Version = 230916)
# 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 -0.003 0.000 0.000 1222 470 ' '
2 0.058 0.500 0.500 1221 470 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0970P)²+17.2923P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6220
_refine_ls_number_parameters     341
_refine_ls_number_restraints     4
_refine_ls_R_factor_all          0.0960
_refine_ls_R_factor_gt           0.0719
_refine_ls_wR_factor_ref         0.2048
_refine_ls_wR_factor_gt          0.1838
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.024
_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 0.53856(4) 0.64377(5) 0.12922(3) 0.0274(2) Uani 1 1 d . . . . .
S1 S 0.59397(7) 0.67448(8) 0.20806(4) 0.0294(3) Uani 1 1 d . . . . .
S2 S 0.49658(7) 0.49413(9) 0.16152(5) 0.0325(3) Uani 1 1 d . . . . .
O1 O 0.4461(2) 0.5874(3) 0.04066(14) 0.0344(8) Uani 1 1 d . . . . .
N1 N 0.6451(2) 0.5944(3) 0.10986(15) 0.0264(8) Uani 1 1 d . . . . .
O3 O 0.3765(3) 0.6983(3) 0.14748(19) 0.0553(11) Uani 1 1 d . . . . .
N2 N 0.5671(2) 0.5242(3) 0.04936(15) 0.0281(8) Uani 1 1 d D . . . .
O2 O 0.5705(3) 0.8230(3) 0.07907(17) 0.0510(10) Uani 1 1 d . . . . .
C1 C 0.6385(3) 0.5276(3) 0.07297(18) 0.0297(10) Uani 1 1 d . . . . .
C13 C 0.5076(3) 0.5839(3) 0.0659(2) 0.0310(10) Uani 1 1 d . . . . .
C3 C 0.7723(3) 0.4823(4) 0.0831(2) 0.0372(12) Uani 1 1 d . . . . .
H3 H 0.8141 0.4422 0.0762 0.045 Uiso 1 1 calc R U . . .
C4 C 0.7816(3) 0.5559(4) 0.1170(2) 0.0349(11) Uani 1 1 d . . . . .
H4 H 0.8302 0.5669 0.1320 0.042 Uiso 1 1 calc R U . . .
C14 C 0.5590(3) 0.7536(4) 0.0991(2) 0.0352(11) Uani 1 1 d . . . . .
C6 C 0.7305(3) 0.7033(4) 0.1574(2) 0.0322(11) Uani 1 1 d . . . . .
C5 C 0.7181(3) 0.6138(4) 0.1286(2) 0.0338(11) Uani 1 1 d . . . . .
C2 C 0.7003(3) 0.4684(4) 0.05943(19) 0.0321(11) Uani 1 1 d . . . . .
H2 H 0.6935 0.4211 0.0353 0.039 Uiso 1 1 calc R U . . .
C10 C 0.6920(3) 0.8299(4) 0.2146(2) 0.0373(12) Uani 1 1 d . . . . .
H10 H 0.6555 0.8556 0.2371 0.045 Uiso 1 1 calc R U . . .
C7 C 0.8001(3) 0.7531(4) 0.1466(2) 0.0408(12) Uani 1 1 d . . . . .
H7 H 0.8367 0.7282 0.1240 0.049 Uiso 1 1 calc R U . . .
C8 C 0.8140(3) 0.8399(4) 0.1698(2) 0.0432(14) Uani 1 1 d . . . . .
H8 H 0.8597 0.8726 0.1623 0.052 Uiso 1 1 calc R U . . .
C11 C 0.6777(3) 0.7430(4) 0.1917(2) 0.0332(11) Uani 1 1 d . . . . .
C16 C 0.5173(4) 0.4826(4) 0.2280(2) 0.0392(12) Uani 1 1 d . . . . .
C12 C 0.5350(3) 0.7528(4) 0.2456(2) 0.0374(12) Uani 1 1 d . . . . .
H12A H 0.5627 0.7692 0.2764 0.056 Uiso 1 1 calc R U . . .
H12B H 0.4865 0.7225 0.2543 0.056 Uiso 1 1 calc R U . . .
H12C H 0.5242 0.8085 0.2261 0.056 Uiso 1 1 calc R U . . .
C15 C 0.4395(3) 0.6781(4) 0.1420(2) 0.0350(11) Uani 1 1 d . . . . .
C9 C 0.7610(3) 0.8774(4) 0.2035(2) 0.0415(13) Uani 1 1 d . . . . .
H9 H 0.7713 0.9348 0.2190 0.050 Uiso 1 1 calc R U . . .
C21 C 0.5882(4) 0.4397(4) 0.2430(2) 0.0434(13) Uani 1 1 d . . . . .
C18 C 0.4781(4) 0.4940(4) 0.3171(2) 0.0493(16) Uani 1 1 d . . . . .
H18 H 0.4422 0.5127 0.3419 0.059 Uiso 1 1 calc R U . . .
C22 C 0.6494(4) 0.4069(5) 0.2051(3) 0.0510(15) Uani 1 1 d . . . . .
H22A H 0.6278 0.3582 0.1840 0.077 Uiso 1 1 calc R U . . .
H22B H 0.6942 0.3832 0.2233 0.077 Uiso 1 1 calc R U . . .
H22C H 0.6652 0.4587 0.1839 0.077 Uiso 1 1 calc R U . . .
C17 C 0.4613(4) 0.5090(4) 0.2650(2) 0.0477(15) Uani 1 1 d . . . . .
C20 C 0.6023(4) 0.4257(4) 0.2954(2) 0.0526(17) Uani 1 1 d . . . . .
H20 H 0.6493 0.3986 0.3060 0.063 Uiso 1 1 calc R U . . .
C23 C 0.3840(4) 0.5519(4) 0.2504(3) 0.0502(15) Uani 1 1 d . . . . .
H23A H 0.3528 0.5611 0.2806 0.075 Uiso 1 1 calc R U . . .
H23B H 0.3568 0.5109 0.2272 0.075 Uiso 1 1 calc R U . . .
H23C H 0.3929 0.6113 0.2340 0.075 Uiso 1 1 calc R U . . .
C19 C 0.5469(5) 0.4519(5) 0.3317(2) 0.0594(19) Uani 1 1 d . . . . .
H19 H 0.5567 0.4409 0.3663 0.071 Uiso 1 1 calc R U . . .
Cl1 Cl 0.43919(13) 0.30637(18) 0.04443(8) 0.0813(6) Uani 1 1 d D . . . .
Cl2 Cl 0.53121(15) 0.20407(14) 0.11996(8) 0.0814(6) Uani 1 1 d D . . . .
C1A C 0.5272(4) 0.2957(4) 0.0768(3) 0.0562(17) Uani 1 1 d D . . . .
H1AA H 0.5373 0.3538 0.0950 0.067 Uiso 1 1 calc R U . . .
H1AB H 0.5688 0.2876 0.0518 0.067 Uiso 1 1 calc R U . . .
Cl3 Cl 0.2547(14) 0.2942(2) 0.9995(6) 0.0622(19) Uani 0.5 1 d D . P A -1
Cl4 Cl 0.2394(5) 0.0982(3) 0.9720(2) 0.124(2) Uani 0.5 1 d D . P A -1
C2A C 0.2653(11) 0.1786(6) 1.0190(5) 0.070(4) Uani 0.5 1 d D . P A -1
H2A1 H 0.2330 0.1681 1.0490 0.084 Uiso 0.5 1 calc R U P A -1
H2A2 H 0.3195 0.1680 1.0288 0.084 Uiso 0.5 1 calc R U P A -1
H2N H 0.561(4) 0.484(3) 0.0229(14) 0.055(19) 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 C14 1.787(6) . ?
Fe1 C15 1.789(5) . ?
Fe1 C13 1.931(5) . ?
Fe1 N1 2.012(4) . ?
Fe1 S1 2.3035(13) . ?
Fe1 S2 2.4023(15) . ?
S1 C11 1.781(5) . ?
S1 C12 1.793(5) . ?
S2 C16 1.776(6) . ?
O1 C13 1.237(6) . ?
N1 C1 1.359(6) . ?
N1 C5 1.364(6) . ?
O3 C15 1.120(6) . ?
N2 C1 1.363(6) . ?
N2 C13 1.394(6) . ?
N2 H2N 0.900(2) . ?
O2 C14 1.135(7) . ?
C1 C2 1.396(7) . ?
C3 C4 1.381(8) . ?
C3 C2 1.386(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.393(7) . ?
C4 H4 0.9300 . ?
C6 C11 1.389(8) . ?
C6 C7 1.411(7) . ?
C6 C5 1.495(7) . ?
C2 H2 0.9300 . ?
C10 C9 1.388(8) . ?
C10 C11 1.396(7) . ?
C10 H10 0.9300 . ?
C7 C8 1.397(8) . ?
C7 H7 0.9300 . ?
C8 C9 1.370(9) . ?
C8 H8 0.9300 . ?
C16 C21 1.409(8) . ?
C16 C17 1.409(9) . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C9 H9 0.9300 . ?
C21 C20 1.402(8) . ?
C21 C22 1.513(9) . ?
C18 C19 1.371(10) . ?
C18 C17 1.405(9) . ?
C18 H18 0.9300 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C17 C23 1.502(9) . ?
C20 C19 1.389(11) . ?
C20 H20 0.9300 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C19 H19 0.9300 . ?
Cl1 C1A 1.725(7) . ?
Cl2 C1A 1.727(6) . ?
C1A H1AA 0.9700 . ?
C1A H1AB 0.9700 . ?
Cl3 C2A 1.732(9) . ?
Cl4 C2A 1.734(9) . ?
C2A H2A1 0.9700 . ?
C2A H2A2 0.9700 . ?

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
C14 Fe1 C15 91.6(2) . . ?
C14 Fe1 C13 93.7(2) . . ?
C15 Fe1 C13 91.4(2) . . ?
C14 Fe1 N1 91.1(2) . . ?
C15 Fe1 N1 173.8(2) . . ?
C13 Fe1 N1 82.91(18) . . ?
C14 Fe1 S1 98.43(16) . . ?
C15 Fe1 S1 99.58(17) . . ?
C13 Fe1 S1 163.41(16) . . ?
N1 Fe1 S1 85.52(12) . . ?
C14 Fe1 S2 172.18(17) . . ?
C15 Fe1 S2 84.03(18) . . ?
C13 Fe1 S2 80.03(15) . . ?
N1 Fe1 S2 92.69(12) . . ?
S1 Fe1 S2 88.70(5) . . ?
C11 S1 C12 103.9(3) . . ?
C11 S1 Fe1 102.54(17) . . ?
C12 S1 Fe1 112.12(19) . . ?
C16 S2 Fe1 111.48(17) . . ?
C1 N1 C5 118.1(4) . . ?
C1 N1 Fe1 110.4(3) . . ?
C5 N1 Fe1 131.4(3) . . ?
C1 N2 C13 119.2(4) . . ?
C1 N2 H2N 118(4) . . ?
C13 N2 H2N 123(4) . . ?
N1 C1 N2 114.7(4) . . ?
N1 C1 C2 122.7(4) . . ?
N2 C1 C2 122.5(4) . . ?
O1 C13 N2 118.3(4) . . ?
O1 C13 Fe1 131.9(4) . . ?
N2 C13 Fe1 109.7(3) . . ?
C4 C3 C2 119.6(5) . . ?
C4 C3 H3 120.2 . . ?
C2 C3 H3 120.2 . . ?
C3 C4 C5 120.1(5) . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
O2 C14 Fe1 178.2(5) . . ?
C11 C6 C7 118.0(5) . . ?
C11 C6 C5 125.5(5) . . ?
C7 C6 C5 116.5(5) . . ?
N1 C5 C4 120.6(5) . . ?
N1 C5 C6 118.7(5) . . ?
C4 C5 C6 120.4(5) . . ?
C3 C2 C1 118.0(5) . . ?
C3 C2 H2 121.0 . . ?
C1 C2 H2 121.0 . . ?
C9 C10 C11 119.4(5) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C8 C7 C6 120.0(5) . . ?
C8 C7 H7 120.0 . . ?
C6 C7 H7 120.0 . . ?
C9 C8 C7 120.8(5) . . ?
C9 C8 H8 119.6 . . ?
C7 C8 H8 119.6 . . ?
C6 C11 C10 121.6(5) . . ?
C6 C11 S1 116.8(4) . . ?
C10 C11 S1 121.5(4) . . ?
C21 C16 C17 120.4(5) . . ?
C21 C16 S2 118.7(4) . . ?
C17 C16 S2 120.7(5) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O3 C15 Fe1 176.3(5) . . ?
C8 C9 C10 120.2(5) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C20 C21 C16 118.6(6) . . ?
C20 C21 C22 118.5(6) . . ?
C16 C21 C22 122.9(5) . . ?
C19 C18 C17 120.6(6) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C17 C16 119.1(6) . . ?
C18 C17 C23 119.0(6) . . ?
C16 C17 C23 121.9(6) . . ?
C19 C20 C21 120.7(7) . . ?
C19 C20 H20 119.6 . . ?
C21 C20 H20 119.6 . . ?
C17 C23 H23A 109.5 . . ?
C17 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C17 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C18 C19 C20 120.6(6) . . ?
C18 C19 H19 119.7 . . ?
C20 C19 H19 119.7 . . ?
Cl1 C1A Cl2 114.8(4) . . ?
Cl1 C1A H1AA 108.6 . . ?
Cl2 C1A H1AA 108.6 . . ?
Cl1 C1A H1AB 108.6 . . ?
Cl2 C1A H1AB 108.6 . . ?
H1AA C1A H1AB 107.5 . . ?
Cl3 C2A Cl4 113.3(8) . . ?
Cl3 C2A H2A1 108.9 . . ?
Cl4 C2A H2A1 108.9 . . ?
Cl3 C2A H2A2 108.9 . . ?
Cl4 C2A H2A2 108.9 . . ?
H2A1 C2A H2A2 107.7 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C5 N1 C1 N2 -168.3(4) . . . . ?
Fe1 N1 C1 N2 14.4(5) . . . . ?
C5 N1 C1 C2 10.3(7) . . . . ?
Fe1 N1 C1 C2 -167.0(4) . . . . ?
C13 N2 C1 N1 -3.1(7) . . . . ?
C13 N2 C1 C2 178.4(5) . . . . ?
C1 N2 C13 O1 172.3(5) . . . . ?
C1 N2 C13 Fe1 -10.4(6) . . . . ?
C2 C3 C4 C5 2.3(8) . . . . ?
C1 N1 C5 C4 -11.0(7) . . . . ?
Fe1 N1 C5 C4 165.7(4) . . . . ?
C1 N1 C5 C6 162.8(4) . . . . ?
Fe1 N1 C5 C6 -20.5(7) . . . . ?
C3 C4 C5 N1 4.9(8) . . . . ?
C3 C4 C5 C6 -168.8(5) . . . . ?
C11 C6 C5 N1 39.0(7) . . . . ?
C7 C6 C5 N1 -137.9(5) . . . . ?
C11 C6 C5 C4 -147.2(5) . . . . ?
C7 C6 C5 C4 36.0(7) . . . . ?
C4 C3 C2 C1 -3.1(8) . . . . ?
N1 C1 C2 C3 -3.3(8) . . . . ?
N2 C1 C2 C3 175.2(5) . . . . ?
C11 C6 C7 C8 -0.5(8) . . . . ?
C5 C6 C7 C8 176.6(5) . . . . ?
C6 C7 C8 C9 0.5(9) . . . . ?
C7 C6 C11 C10 0.7(8) . . . . ?
C5 C6 C11 C10 -176.1(5) . . . . ?
C7 C6 C11 S1 -175.5(4) . . . . ?
C5 C6 C11 S1 7.7(7) . . . . ?
C9 C10 C11 C6 -0.9(8) . . . . ?
C9 C10 C11 S1 175.1(4) . . . . ?
C7 C8 C9 C10 -0.8(9) . . . . ?
C11 C10 C9 C8 1.0(8) . . . . ?
C17 C16 C21 C20 -1.2(8) . . . . ?
S2 C16 C21 C20 -176.3(4) . . . . ?
C17 C16 C21 C22 178.0(5) . . . . ?
S2 C16 C21 C22 2.9(7) . . . . ?
C19 C18 C17 C16 -1.7(8) . . . . ?
C19 C18 C17 C23 177.7(5) . . . . ?
C21 C16 C17 C18 1.5(8) . . . . ?
S2 C16 C17 C18 176.5(4) . . . . ?
C21 C16 C17 C23 -178.0(5) . . . . ?
S2 C16 C17 C23 -2.9(7) . . . . ?
C16 C21 C20 C19 1.2(8) . . . . ?
C22 C21 C20 C19 -178.1(5) . . . . ?
C17 C18 C19 C20 1.7(9) . . . . ?
C21 C20 C19 C18 -1.5(9) . . . . ?

_refine_diff_density_max         0.638
_refine_diff_density_min         -1.055
_refine_diff_density_rms         0.099

_shelxl_version_number           2013-4


####################################################################### 
# 
# 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_3c
_database_code_depnum_ccdc_archive 'CCDC 1547038'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C62 H38 B F25 Fe N4 O2 S'
_chemical_formula_sum            'C62 H38 B F25 Fe N4 O2 S'
_chemical_formula_weight         1444.68

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 '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                   12.6230(4)
_cell_length_b                   13.1564(3)
_cell_length_c                   19.2160(4)
_cell_angle_alpha                98.635(2)
_cell_angle_beta                 98.815(2)
_cell_angle_gamma                99.964(2)
_cell_volume                     3054.41(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    7814
_cell_measurement_theta_min      3.6130
_cell_measurement_theta_max      74.1400

_exptl_crystal_description       prism
_exptl_crystal_colour            orenge
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.571
_exptl_crystal_F_000             1452
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    3.428
_shelx_estimated_absorpt_T_min   0.279
_shelx_estimated_absorpt_T_max   0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.84368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
(compiled Feb  9 2015,16:26:32)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21026
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_av_R_equivalents  0.0388
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.366
_diffrn_reflns_theta_max         74.417
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.966
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.966
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.966
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12052
_reflns_number_gt                8516
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'

_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'


_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)+(0.0667P)²+1.4337P] 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         12052
_refine_ls_number_parameters     866
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0790
_refine_ls_R_factor_gt           0.0524
_refine_ls_wR_factor_ref         0.1429
_refine_ls_wR_factor_gt          0.1307
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
C11 C 0.8413(3) 0.0014(3) 0.31669(17) 0.0291(7) Uani 1 1 d . . . . .
C10 C 0.8865(4) -0.0470(3) 0.3709(2) 0.0410(9) Uani 1 1 d . . . . .
H10 H 0.9459 -0.0809 0.3647 0.049 Uiso 1 1 calc R U . . .
C9 C 0.8444(4) -0.0453(4) 0.4337(2) 0.0509(11) Uani 1 1 d . . . . .
H9 H 0.8752 -0.0772 0.4710 0.061 Uiso 1 1 calc R U . . .
C8 C 0.7577(4) 0.0031(4) 0.4412(2) 0.0491(11) Uani 1 1 d . . . . .
H8 H 0.7281 0.0039 0.4838 0.059 Uiso 1 1 calc R U . . .
C7 C 0.7127(3) 0.0507(3) 0.38750(19) 0.0369(8) Uani 1 1 d . . . . .
H7 H 0.6526 0.0834 0.3939 0.044 Uiso 1 1 calc R U . . .
C6 C 0.7541(3) 0.0516(3) 0.32382(17) 0.0265(7) Uani 1 1 d . . . . .
C5 C 0.7001(3) 0.1061(2) 0.27012(17) 0.0232(6) Uani 1 1 d . . . . .
C4 C 0.6606(3) 0.1948(3) 0.29495(18) 0.0291(7) Uani 1 1 d . . . . .
H4 H 0.6788 0.2258 0.3443 0.035 Uiso 1 1 calc R U . . .
C3 C 0.5942(3) 0.2378(3) 0.24722(19) 0.0295(7) Uani 1 1 d . . . . .
H3 H 0.5697 0.3000 0.2636 0.035 Uiso 1 1 calc R U . . .
C2 C 0.5644(3) 0.1902(3) 0.17688(18) 0.0278(7) Uani 1 1 d . . . . .
H2 H 0.5156 0.2156 0.1442 0.033 Uiso 1 1 calc R U . . .
C1 C 0.6079(3) 0.1032(3) 0.15474(17) 0.0245(6) Uani 1 1 d . . . . .
C13 C 0.6199(3) -0.0445(3) 0.07088(17) 0.0259(7) Uani 1 1 d . . . . .
C20 C 0.9067(3) -0.1449(3) 0.08241(18) 0.0268(7) Uani 1 1 d . . . . .
H20 H 0.9555 -0.0824 0.1075 0.032 Uiso 1 1 calc R U . . .
C21 C 0.9490(3) -0.2201(3) 0.0420(2) 0.0313(7) Uani 1 1 d . . . . .
H21 H 1.0246 -0.2087 0.0393 0.038 Uiso 1 1 calc R U . . .
C22 C 0.8785(3) -0.3117(3) 0.00604(19) 0.0316(7) Uani 1 1 d . . . . .
H22 H 0.9050 -0.3653 -0.0209 0.038 Uiso 1 1 calc R U . . .
C23 C 0.7689(3) -0.3238(3) 0.01001(18) 0.0291(7) Uani 1 1 d . . . . .
H23 H 0.7190 -0.3856 -0.0150 0.035 Uiso 1 1 calc R U . . .
C24 C 0.7317(3) -0.2451(2) 0.05087(17) 0.0254(6) Uani 1 1 d . . . . .
H24 H 0.6560 -0.2545 0.0528 0.030 Uiso 1 1 calc R U . . .
C19 C 0.7071(3) -0.2224(3) 0.22144(18) 0.0316(7) Uani 1 1 d . . . . .
H19 H 0.7781 -0.2289 0.2132 0.038 Uiso 1 1 calc R U . . .
C18 C 0.6575(4) -0.2864(3) 0.2630(2) 0.0402(9) Uani 1 1 d . . . . .
H18 H 0.6940 -0.3357 0.2829 0.048 Uiso 1 1 calc R U . . .
C17 C 0.5543(4) -0.2776(3) 0.2753(2) 0.0435(10) Uani 1 1 d . . . . .
H17 H 0.5189 -0.3202 0.3040 0.052 Uiso 1 1 calc R U . . .
C16 C 0.5036(3) -0.2061(3) 0.2452(2) 0.0389(9) Uani 1 1 d . . . . .
H16 H 0.4327 -0.1983 0.2530 0.047 Uiso 1 1 calc R U . . .
C15 C 0.5574(3) -0.1455(3) 0.20319(19) 0.0295(7) Uani 1 1 d . . . . .
H15 H 0.5209 -0.0978 0.1813 0.035 Uiso 1 1 calc R U . . .
C14 C 0.8111(3) 0.0480(3) 0.09840(18) 0.0269(7) Uani 1 1 d . . . . .
C12 C 0.9717(3) 0.1209(3) 0.2438(2) 0.0382(8) Uani 1 1 d . . . . .
H12A H 0.9211 0.1695 0.2460 0.057 Uiso 1 1 calc R U . . .
H12B H 1.0063 0.1256 0.2018 0.057 Uiso 1 1 calc R U . . .
H12C H 1.0282 0.1395 0.2873 0.057 Uiso 1 1 calc R U . . .
C25 C 0.3123(2) 0.4777(2) 0.20215(15) 0.0197(6) Uani 1 1 d . . . . .
C26 C 0.2693(3) 0.5558(3) 0.17209(17) 0.0243(6) Uani 1 1 d . . . . .
H26 H 0.2066 0.5765 0.1869 0.029 Uiso 1 1 calc R U . . .
C27 C 0.3156(3) 0.6041(3) 0.12113(17) 0.0271(7) Uani 1 1 d . . . . .
C28 C 0.4096(3) 0.5802(2) 0.09968(17) 0.0260(7) Uani 1 1 d . . . . .
H28 H 0.4423 0.6147 0.0659 0.031 Uiso 1 1 calc R U . . .
C29 C 0.4544(3) 0.5037(2) 0.12959(16) 0.0229(6) Uani 1 1 d . . . . .
C30 C 0.4061(2) 0.4536(2) 0.17883(16) 0.0208(6) Uani 1 1 d . . . . .
H30 H 0.4381 0.4008 0.1975 0.025 Uiso 1 1 calc R U . . .
C31 C 0.2632(4) 0.6850(3) 0.0896(2) 0.0419(9) Uani 1 1 d . . . . .
C32 C 0.5555(3) 0.4721(3) 0.1093(2) 0.0319(8) Uani 1 1 d . . . . .
C33 C 0.3515(2) 0.4976(2) 0.33885(16) 0.0195(6) Uani 1 1 d . . . . .
C34 C 0.3303(3) 0.5895(3) 0.37702(18) 0.0259(7) Uani 1 1 d . . . . .
H34 H 0.2613 0.6080 0.3645 0.031 Uiso 1 1 calc R U . . .
C35 C 0.4072(3) 0.6539(3) 0.43247(19) 0.0296(7) Uani 1 1 d . . . . .
C36 C 0.5109(3) 0.6326(3) 0.45189(18) 0.0308(7) Uani 1 1 d . . . . .
H36 H 0.5638 0.6776 0.4893 0.037 Uiso 1 1 calc R U . . .
C37 C 0.5337(3) 0.5428(3) 0.41434(16) 0.0232(6) Uani 1 1 d . . . . .
C38 C 0.4557(2) 0.4771(2) 0.36018(16) 0.0200(6) Uani 1 1 d . . . . .
H38 H 0.4737 0.4154 0.3365 0.024 Uiso 1 1 calc R U . . .
C39 C 0.6459(3) 0.5196(3) 0.42950(19) 0.0322(8) Uani 1 1 d . . . . .
C40 C 0.3810(4) 0.7511(3) 0.4720(2) 0.0458(10) Uani 1 1 d . . . . .
C41 C 0.2779(2) 0.3016(2) 0.26085(16) 0.0219(6) Uani 1 1 d . . . . .
C42 C 0.2850(3) 0.2550(3) 0.32193(17) 0.0261(7) Uani 1 1 d . . . . .
H42 H 0.2961 0.2982 0.3677 0.031 Uiso 1 1 calc R U . . .
C43 C 0.2761(3) 0.1475(3) 0.31742(18) 0.0318(8) Uani 1 1 d . . . . .
C44 C 0.2627(3) 0.0815(3) 0.2520(2) 0.0331(8) Uani 1 1 d . . . . .
H44 H 0.2585 0.0081 0.2491 0.040 Uiso 1 1 calc R U . . .
C45 C 0.2556(3) 0.1257(3) 0.19075(18) 0.0288(7) Uani 1 1 d . . . . .
C46 C 0.2623(3) 0.2337(2) 0.19512(17) 0.0236(6) Uani 1 1 d . . . . .
H46 H 0.2561 0.2617 0.1523 0.028 Uiso 1 1 calc R U . . .
C47 C 0.2742(4) 0.0992(3) 0.3836(2) 0.0426(10) Uani 1 1 d . . . . .
C48 C 0.2397(3) 0.0540(3) 0.1199(2) 0.0361(8) Uani 1 1 d . . . . .
C49 C 0.1405(3) 0.4220(2) 0.26944(17) 0.0231(6) Uani 1 1 d . . . . .
C50 C 0.0626(3) 0.4075(3) 0.20675(18) 0.0264(7) Uani 1 1 d . . . . .
H50 H 0.0867 0.4114 0.1626 0.032 Uiso 1 1 calc R U . . .
C51 C -0.0495(3) 0.3875(3) 0.20720(19) 0.0277(7) Uani 1 1 d . . . . .
C52 C -0.0879(3) 0.3791(3) 0.27054(19) 0.0291(7) Uani 1 1 d . . . . .
H52 H -0.1642 0.3652 0.2710 0.035 Uiso 1 1 calc R U . . .
C53 C -0.0121(3) 0.3916(3) 0.33290(18) 0.0277(7) Uani 1 1 d . . . . .
C54 C 0.0994(3) 0.4141(3) 0.33289(18) 0.0259(7) Uani 1 1 d . . . . .
H54 H 0.1493 0.4244 0.3769 0.031 Uiso 1 1 calc R U . . .
C55 C -0.0518(3) 0.3736(3) 0.4007(2) 0.0339(8) Uani 1 1 d . . . . .
C56 C -0.1276(3) 0.3752(3) 0.1381(2) 0.0344(8) Uani 1 1 d . . . . .
C57 C 0.0930(6) 0.7716(4) 0.2835(4) 0.0777(19) Uani 1 1 d . . . . .
C58 C -0.0009(7) 0.7004(5) 0.2408(4) 0.095(2) Uani 1 1 d . . . . .
H58 H -0.0158 0.6895 0.1900 0.114 Uiso 1 1 calc R U . . .
C59 C -0.0699(5) 0.6476(4) 0.2816(4) 0.0772(18) Uani 1 1 d . . . . .
H59 H -0.1351 0.5993 0.2582 0.093 Uiso 1 1 calc R U . . .
C60 C -0.0425(4) 0.6663(4) 0.3545(4) 0.0748(18) Uani 1 1 d . . . . .
H60 H -0.0890 0.6289 0.3805 0.090 Uiso 1 1 calc R U . . .
C61 C 0.0463(5) 0.7345(4) 0.3909(4) 0.0691(15) Uani 1 1 d . . . . .
H61 H 0.0612 0.7460 0.4418 0.083 Uiso 1 1 calc R U . . .
C62 C 0.1151(5) 0.7870(4) 0.3552(4) 0.0677(15) Uani 1 1 d . . . . .
H62 H 0.1791 0.8350 0.3809 0.081 Uiso 1 1 calc R U . . .
B1 B 0.2697(3) 0.4260(3) 0.26791(18) 0.0202(7) Uani 1 1 d . . . . .
N1 N 0.6803(2) 0.0651(2) 0.19879(13) 0.0207(5) Uani 1 1 d . . . . .
N2 N 0.5781(2) 0.0464(2) 0.08663(14) 0.0268(6) Uani 1 1 d . . . . .
H2A H 0.5340 0.0665 0.0537 0.032 Uiso 1 1 calc R U . . .
N3 N 0.6588(2) -0.1512(2) 0.19202(14) 0.0237(5) Uani 1 1 d . . . . .
N4 N 0.7992(2) -0.1562(2) 0.08772(14) 0.0225(5) Uani 1 1 d . . . . .
O1 O 0.5791(2) -0.10539(19) 0.01406(12) 0.0314(5) Uani 1 1 d . . . . .
O2 O 0.8536(2) 0.1028(2) 0.06545(15) 0.0394(6) Uani 1 1 d . . . . .
F1 F 0.6070(2) 0.53807(18) 0.07299(15) 0.0505(7) Uani 1 1 d . . . . .
F2 F 0.5328(2) 0.37683(16) 0.06695(12) 0.0427(5) Uani 1 1 d . . . . .
F3 F 0.62765(18) 0.4651(2) 0.16642(13) 0.0453(6) Uani 1 1 d . . . . .
F4 F 0.2985(2) 0.7090(3) 0.03198(16) 0.0691(9) Uani 1 1 d . . . . .
F5 F 0.2778(3) 0.7743(2) 0.13634(18) 0.0853(11) Uani 1 1 d . . . . .
F6 F 0.1548(2) 0.6542(3) 0.07083(18) 0.0739(10) Uani 1 1 d . . . . .
F7 F 0.70793(19) 0.5560(3) 0.38480(15) 0.0629(8) Uani 1 1 d . . . . .
F8 F 0.64490(18) 0.41644(18) 0.42168(13) 0.0417(5) Uani 1 1 d . . . . .
F9 F 0.69976(19) 0.5613(2) 0.49573(13) 0.0506(6) Uani 1 1 d . . . . .
F10 F 0.4490(2) 0.7895(2) 0.53515(16) 0.0692(9) Uani 1 1 d . . . . .
F11 F 0.3849(3) 0.8282(2) 0.43437(19) 0.0737(9) Uani 1 1 d . . . . .
F12 F 0.2800(2) 0.7341(2) 0.48802(13) 0.0489(6) Uani 1 1 d . . . . .
F13 F 0.3019(2) 0.16851(18) 0.44408(12) 0.0533(7) Uani 1 1 d . . . . .
F14 F 0.3389(3) 0.0305(2) 0.38778(15) 0.0688(9) Uani 1 1 d . . . . .
F15 F 0.1724(2) 0.0456(2) 0.38423(13) 0.0594(7) Uani 1 1 d . . . . .
F16 F 0.1601(2) -0.0296(2) 0.11356(13) 0.0557(7) Uani 1 1 d . . . . .
F17 F 0.2242(3) 0.10035(19) 0.06470(12) 0.0605(8) Uani 1 1 d . . . . .
F18 F 0.3280(2) 0.0096(2) 0.11216(15) 0.0576(7) Uani 1 1 d . . . . .
F19 F -0.0862(2) 0.2705(2) 0.39999(13) 0.0576(7) Uani 1 1 d . . . . .
F20 F -0.1345(2) 0.4179(3) 0.41149(15) 0.0627(8) Uani 1 1 d . . . . .
F21 F 0.02620(19) 0.4062(2) 0.45950(12) 0.0494(6) Uani 1 1 d . . . . .
F22 F -0.08715(18) 0.3365(2) 0.08141(12) 0.0482(6) Uani 1 1 d . . . . .
F23 F -0.22286(17) 0.3103(2) 0.13616(13) 0.0453(6) Uani 1 1 d . . . . .
F24 F -0.1529(2) 0.4663(2) 0.12559(14) 0.0518(6) Uani 1 1 d . . . . .
F25 F 0.1625(6) 0.8258(4) 0.2500(4) 0.191(3) Uani 1 1 d . . . . .
S1 S 0.89694(6) -0.01201(6) 0.23714(4) 0.02629(17) Uani 1 1 d . . . . .
Fe1 Fe 0.74340(4) -0.04290(4) 0.14444(3) 0.01961(12) Uani 1 1 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
C11 C6 1.393(5) . ?
C11 C10 1.398(5) . ?
C11 S1 1.775(3) . ?
C10 C9 1.390(6) . ?
C10 H10 0.9500 . ?
C9 C8 1.374(6) . ?
C9 H9 0.9500 . ?
C8 C7 1.384(5) . ?
C8 H8 0.9500 . ?
C7 C6 1.403(5) . ?
C7 H7 0.9500 . ?
C6 C5 1.489(4) . ?
C5 N1 1.363(4) . ?
C5 C4 1.394(5) . ?
C4 C3 1.396(5) . ?
C4 H4 0.9500 . ?
C3 C2 1.367(5) . ?
C3 H3 0.9500 . ?
C2 C1 1.390(5) . ?
C2 H2 0.9500 . ?
C1 N1 1.361(4) . ?
C1 N2 1.368(4) . ?
C13 O1 1.234(4) . ?
C13 N2 1.400(4) . ?
C13 Fe1 1.932(3) . ?
C20 N4 1.360(4) . ?
C20 C21 1.395(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.383(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.396(5) . ?
C23 H23 0.9500 . ?
C24 N4 1.348(4) . ?
C24 H24 0.9500 . ?
C19 N3 1.349(4) . ?
C19 C18 1.382(5) . ?
C19 H19 0.9500 . ?
C18 C17 1.381(6) . ?
C18 H18 0.9500 . ?
C17 C16 1.373(6) . ?
C17 H17 0.9500 . ?
C16 C15 1.386(5) . ?
C16 H16 0.9500 . ?
C15 N3 1.343(4) . ?
C15 H15 0.9500 . ?
C14 O2 1.147(4) . ?
C14 Fe1 1.772(3) . ?
C12 S1 1.814(4) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C25 C30 1.397(4) . ?
C25 C26 1.400(4) . ?
C25 B1 1.640(4) . ?
C26 C27 1.391(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.385(5) . ?
C27 C31 1.500(5) . ?
C28 C29 1.391(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(4) . ?
C29 C32 1.496(5) . ?
C30 H30 0.9500 . ?
C31 F4 1.317(5) . ?
C31 F5 1.333(5) . ?
C31 F6 1.334(5) . ?
C32 F1 1.337(4) . ?
C32 F3 1.340(4) . ?
C32 F2 1.347(4) . ?
C33 C38 1.400(4) . ?
C33 C34 1.407(4) . ?
C33 B1 1.630(5) . ?
C34 C35 1.387(5) . ?
C34 H34 0.9500 . ?
C35 C36 1.393(5) . ?
C35 C40 1.500(5) . ?
C36 C37 1.387(5) . ?
C36 H36 0.9500 . ?
C37 C38 1.386(4) . ?
C37 C39 1.495(4) . ?
C38 H38 0.9500 . ?
C39 F9 1.334(4) . ?
C39 F7 1.335(4) . ?
C39 F8 1.340(4) . ?
C40 F11 1.330(5) . ?
C40 F10 1.347(5) . ?
C40 F12 1.347(5) . ?
C41 C46 1.399(4) . ?
C41 C42 1.402(4) . ?
C41 B1 1.645(5) . ?
C42 C43 1.387(5) . ?
C42 H42 0.9500 . ?
C43 C44 1.386(5) . ?
C43 C47 1.506(5) . ?
C44 C45 1.386(5) . ?
C44 H44 0.9500 . ?
C45 C46 1.397(5) . ?
C45 C48 1.499(5) . ?
C46 H46 0.9500 . ?
C47 F14 1.323(5) . ?
C47 F13 1.323(5) . ?
C47 F15 1.357(5) . ?
C48 F17 1.307(4) . ?
C48 F16 1.332(4) . ?
C48 F18 1.364(5) . ?
C49 C50 1.399(4) . ?
C49 C54 1.407(4) . ?
C49 B1 1.628(4) . ?
C50 C51 1.395(4) . ?
C50 H50 0.9500 . ?
C51 C52 1.390(5) . ?
C51 C56 1.497(5) . ?
C52 C53 1.383(5) . ?
C52 H52 0.9500 . ?
C53 C54 1.388(5) . ?
C53 C55 1.502(5) . ?
C54 H54 0.9500 . ?
C55 F20 1.308(4) . ?
C55 F21 1.341(4) . ?
C55 F19 1.348(5) . ?
C56 F24 1.339(4) . ?
C56 F23 1.341(4) . ?
C56 F22 1.341(4) . ?
C57 F25 1.337(7) . ?
C57 C62 1.341(9) . ?
C57 C58 1.428(10) . ?
C58 C59 1.421(10) . ?
C58 H58 0.9500 . ?
C59 C60 1.363(9) . ?
C59 H59 0.9500 . ?
C60 C61 1.332(8) . ?
C60 H60 0.9500 . ?
C61 C62 1.348(8) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
N1 Fe1 1.987(3) . ?
N2 H2A 0.8800 . ?
N3 Fe1 2.042(3) . ?
N4 Fe1 2.004(3) . ?
S1 Fe1 2.3550(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
C6 C11 C10 121.5(3) . . ?
C6 C11 S1 122.5(3) . . ?
C10 C11 S1 115.8(3) . . ?
C9 C10 C11 119.9(4) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C8 C9 C10 119.2(4) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C9 C8 C7 120.9(4) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.6 . . ?
C8 C7 C6 121.4(4) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C11 C6 C7 117.0(3) . . ?
C11 C6 C5 126.2(3) . . ?
C7 C6 C5 116.8(3) . . ?
N1 C5 C4 120.4(3) . . ?
N1 C5 C6 121.1(3) . . ?
C4 C5 C6 118.2(3) . . ?
C5 C4 C3 119.9(3) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C2 C3 C4 119.8(3) . . ?
C2 C3 H3 120.1 . . ?
C4 C3 H3 120.1 . . ?
C3 C2 C1 117.9(3) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
N1 C1 N2 114.2(3) . . ?
N1 C1 C2 123.5(3) . . ?
N2 C1 C2 122.3(3) . . ?
O1 C13 N2 118.2(3) . . ?
O1 C13 Fe1 132.2(3) . . ?
N2 C13 Fe1 109.5(2) . . ?
N4 C20 C21 123.5(3) . . ?
N4 C20 H20 118.2 . . ?
C21 C20 H20 118.2 . . ?
C22 C21 C20 118.5(3) . . ?
C22 C21 H21 120.8 . . ?
C20 C21 H21 120.8 . . ?
C23 C22 C21 118.8(3) . . ?
C23 C22 H22 120.6 . . ?
C21 C22 H22 120.6 . . ?
C22 C23 C24 119.8(3) . . ?
C22 C23 H23 120.1 . . ?
C24 C23 H23 120.1 . . ?
N4 C24 C23 122.5(3) . . ?
N4 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
N3 C19 C18 122.8(4) . . ?
N3 C19 H19 118.6 . . ?
C18 C19 H19 118.6 . . ?
C17 C18 C19 119.0(4) . . ?
C17 C18 H18 120.5 . . ?
C19 C18 H18 120.5 . . ?
C16 C17 C18 118.9(3) . . ?
C16 C17 H17 120.6 . . ?
C18 C17 H17 120.6 . . ?
C17 C16 C15 119.0(4) . . ?
C17 C16 H16 120.5 . . ?
C15 C16 H16 120.5 . . ?
N3 C15 C16 123.0(3) . . ?
N3 C15 H15 118.5 . . ?
C16 C15 H15 118.5 . . ?
O2 C14 Fe1 176.4(3) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C30 C25 C26 115.4(3) . . ?
C30 C25 B1 119.6(3) . . ?
C26 C25 B1 124.5(3) . . ?
C27 C26 C25 122.0(3) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 C26 121.5(3) . . ?
C28 C27 C31 119.4(3) . . ?
C26 C27 C31 119.1(3) . . ?
C27 C28 C29 117.3(3) . . ?
C27 C28 H28 121.3 . . ?
C29 C28 H28 121.3 . . ?
C30 C29 C28 120.9(3) . . ?
C30 C29 C32 117.9(3) . . ?
C28 C29 C32 121.1(3) . . ?
C29 C30 C25 122.7(3) . . ?
C29 C30 H30 118.6 . . ?
C25 C30 H30 118.6 . . ?
F4 C31 F5 107.2(4) . . ?
F4 C31 F6 106.1(3) . . ?
F5 C31 F6 104.5(4) . . ?
F4 C31 C27 114.0(3) . . ?
F5 C31 C27 112.2(3) . . ?
F6 C31 C27 112.2(3) . . ?
F1 C32 F3 107.7(3) . . ?
F1 C32 F2 106.0(3) . . ?
F3 C32 F2 105.7(3) . . ?
F1 C32 C29 112.9(3) . . ?
F3 C32 C29 112.3(3) . . ?
F2 C32 C29 111.7(3) . . ?
C38 C33 C34 115.3(3) . . ?
C38 C33 B1 120.4(3) . . ?
C34 C33 B1 123.8(3) . . ?
C35 C34 C33 121.9(3) . . ?
C35 C34 H34 119.1 . . ?
C33 C34 H34 119.1 . . ?
C34 C35 C36 121.7(3) . . ?
C34 C35 C40 120.1(3) . . ?
C36 C35 C40 118.2(3) . . ?
C37 C36 C35 117.2(3) . . ?
C37 C36 H36 121.4 . . ?
C35 C36 H36 121.4 . . ?
C38 C37 C36 121.0(3) . . ?
C38 C37 C39 119.3(3) . . ?
C36 C37 C39 119.6(3) . . ?
C37 C38 C33 122.9(3) . . ?
C37 C38 H38 118.5 . . ?
C33 C38 H38 118.5 . . ?
F9 C39 F7 106.7(3) . . ?
F9 C39 F8 106.1(3) . . ?
F7 C39 F8 106.0(3) . . ?
F9 C39 C37 113.5(3) . . ?
F7 C39 C37 111.4(3) . . ?
F8 C39 C37 112.6(3) . . ?
F11 C40 F10 106.9(4) . . ?
F11 C40 F12 106.2(4) . . ?
F10 C40 F12 105.1(3) . . ?
F11 C40 C35 112.4(4) . . ?
F10 C40 C35 113.2(4) . . ?
F12 C40 C35 112.4(3) . . ?
C46 C41 C42 116.2(3) . . ?
C46 C41 B1 123.3(3) . . ?
C42 C41 B1 119.9(3) . . ?
C43 C42 C41 121.9(3) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C44 C43 C42 121.2(3) . . ?
C44 C43 C47 118.4(3) . . ?
C42 C43 C47 120.3(3) . . ?
C45 C44 C43 118.0(3) . . ?
C45 C44 H44 121.0 . . ?
C43 C44 H44 121.0 . . ?
C44 C45 C46 120.9(3) . . ?
C44 C45 C48 117.9(3) . . ?
C46 C45 C48 121.2(3) . . ?
C45 C46 C41 121.8(3) . . ?
C45 C46 H46 119.1 . . ?
C41 C46 H46 119.1 . . ?
F14 C47 F13 107.4(3) . . ?
F14 C47 F15 105.8(3) . . ?
F13 C47 F15 105.6(4) . . ?
F14 C47 C43 112.6(4) . . ?
F13 C47 C43 113.9(3) . . ?
F15 C47 C43 111.1(3) . . ?
F17 C48 F16 110.4(3) . . ?
F17 C48 F18 104.8(3) . . ?
F16 C48 F18 102.3(3) . . ?
F17 C48 C45 114.1(3) . . ?
F16 C48 C45 112.0(3) . . ?
F18 C48 C45 112.4(3) . . ?
C50 C49 C54 116.2(3) . . ?
C50 C49 B1 122.1(3) . . ?
C54 C49 B1 120.7(3) . . ?
C51 C50 C49 121.9(3) . . ?
C51 C50 H50 119.0 . . ?
C49 C50 H50 119.0 . . ?
C52 C51 C50 120.7(3) . . ?
C52 C51 C56 120.6(3) . . ?
C50 C51 C56 118.7(3) . . ?
C53 C52 C51 118.2(3) . . ?
C53 C52 H52 120.9 . . ?
C51 C52 H52 120.9 . . ?
C52 C53 C54 121.2(3) . . ?
C52 C53 C55 119.0(3) . . ?
C54 C53 C55 119.7(3) . . ?
C53 C54 C49 121.7(3) . . ?
C53 C54 H54 119.1 . . ?
C49 C54 H54 119.1 . . ?
F20 C55 F21 107.5(3) . . ?
F20 C55 F19 106.0(3) . . ?
F21 C55 F19 104.5(3) . . ?
F20 C55 C53 113.4(3) . . ?
F21 C55 C53 113.4(3) . . ?
F19 C55 C53 111.3(3) . . ?
F24 C56 F23 106.1(3) . . ?
F24 C56 F22 106.2(3) . . ?
F23 C56 F22 106.5(3) . . ?
F24 C56 C51 112.5(3) . . ?
F23 C56 C51 112.6(3) . . ?
F22 C56 C51 112.4(3) . . ?
F25 C57 C62 118.3(7) . . ?
F25 C57 C58 118.2(7) . . ?
C62 C57 C58 123.5(6) . . ?
C59 C58 C57 113.7(6) . . ?
C59 C58 H58 123.2 . . ?
C57 C58 H58 123.2 . . ?
C60 C59 C58 119.9(6) . . ?
C60 C59 H59 120.1 . . ?
C58 C59 H59 120.1 . . ?
C61 C60 C59 123.2(6) . . ?
C61 C60 H60 118.4 . . ?
C59 C60 H60 118.4 . . ?
C60 C61 C62 119.6(7) . . ?
C60 C61 H61 120.2 . . ?
C62 C61 H61 120.2 . . ?
C57 C62 C61 120.0(6) . . ?
C57 C62 H62 120.0 . . ?
C61 C62 H62 120.0 . . ?
C49 B1 C33 113.9(3) . . ?
C49 B1 C25 114.0(2) . . ?
C33 B1 C25 103.2(2) . . ?
C49 B1 C41 102.4(2) . . ?
C33 B1 C41 111.7(2) . . ?
C25 B1 C41 112.0(2) . . ?
C1 N1 C5 117.8(3) . . ?
C1 N1 Fe1 111.6(2) . . ?
C5 N1 Fe1 130.6(2) . . ?
C1 N2 C13 118.1(3) . . ?
C1 N2 H2A 121.0 . . ?
C13 N2 H2A 121.0 . . ?
C15 N3 C19 117.2(3) . . ?
C15 N3 Fe1 120.8(2) . . ?
C19 N3 Fe1 121.4(2) . . ?
C24 N4 C20 116.9(3) . . ?
C24 N4 Fe1 121.8(2) . . ?
C20 N4 Fe1 121.3(2) . . ?
C11 S1 C12 100.50(17) . . ?
C11 S1 Fe1 104.15(12) . . ?
C12 S1 Fe1 108.35(13) . . ?
C14 Fe1 C13 82.56(15) . . ?
C14 Fe1 N1 93.17(13) . . ?
C13 Fe1 N1 82.54(12) . . ?
C14 Fe1 N4 88.46(13) . . ?
C13 Fe1 N4 95.23(13) . . ?
N1 Fe1 N4 177.04(11) . . ?
C14 Fe1 N3 176.61(14) . . ?
C13 Fe1 N3 94.34(12) . . ?
N1 Fe1 N3 87.77(11) . . ?
N4 Fe1 N3 90.46(11) . . ?
C14 Fe1 S1 91.79(11) . . ?
C13 Fe1 S1 170.97(11) . . ?
N1 Fe1 S1 90.78(8) . . ?
N4 Fe1 S1 91.63(8) . . ?
N3 Fe1 S1 91.45(8) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C20 H20 F16 0.95 2.53 3.217(4) 128.9 1_655
C20 H20 S1 0.95 2.78 3.246(3) 111.3 .
C24 H24 O1 0.95 2.49 2.964(4) 110.6 .
C18 H18 F7 0.95 2.59 3.411(4) 144.7 1_545
N2 H2A O1 0.88 1.97 2.844(3) 173.1 2_655

_refine_diff_density_max         1.157
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.068

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2c
_database_code_depnum_ccdc_archive 'CCDC 1547033'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT213_shelx               
;
PROBLEM: Atom F7 has ADP max/min Ratio ..... 5.2 prolat
RESPONSE: These fluorine atoms belong to the CF3 groups in the BARF
ion, which are very disordered. The regular disorder
modeling did not improve the situation.
;
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Th(Min) ... 17 Report
RESPONSE: These few reflections were blocked by the beam stop and 
omitted by the data set.
;
# end Validation Reply Form
_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C55 H34 B Cl3 F24 Fe N3 O3 S'
_chemical_formula_sum            'C55 H34 B Cl3 F24 Fe N3 O3 S'
_chemical_formula_weight         1445.92

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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'

_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                   13.0380(10)
_cell_length_b                   14.2685(11)
_cell_length_c                   16.8688(13)
_cell_angle_alpha                89.575(2)
_cell_angle_beta                 71.762(2)
_cell_angle_gamma                79.118(2)
_cell_volume                     2922.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    46185
_cell_measurement_theta_min      3.0
_cell_measurement_theta_max      25.0

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.643
_exptl_crystal_F_000             1446
_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    0.555
_shelx_estimated_absorpt_T_min   0.926
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.9264
_exptl_absorpt_correction_T_max  0.9466
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            46185
_diffrn_reflns_av_unetI/netI     0.1480
_diffrn_reflns_av_R_equivalents  0.1512
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.003
_diffrn_reflns_theta_max         25.026
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             10308
_reflns_number_gt                5819
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'BRUKER SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0385P)²+9.1565P] 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         10308
_refine_ls_number_parameters     821
_refine_ls_number_restraints     546
_refine_ls_R_factor_all          0.1600
_refine_ls_R_factor_gt           0.0838
_refine_ls_wR_factor_ref         0.1761
_refine_ls_wR_factor_gt          0.1446
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.028
_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
C1 C 0.8484(5) 0.0295(4) 0.1821(4) 0.0206(15) Uani 1 1 d . U . . .
C2 C 0.7537(5) 0.0989(4) 0.1889(4) 0.0226(15) Uani 1 1 d . U . . .
H2 H 0.7406 0.1275 0.1411 0.027 Uiso 1 1 calc R U . . .
C3 C 0.6809(5) 0.1235(4) 0.2676(4) 0.0252(16) Uani 1 1 d . U . . .
H3 H 0.6141 0.1681 0.2748 0.030 Uiso 1 1 calc R U . . .
C4 C 0.7039(5) 0.0839(4) 0.3363(4) 0.0214(15) Uani 1 1 d . U . . .
H4 H 0.6539 0.1023 0.3907 0.026 Uiso 1 1 calc R U . . .
C5 C 0.7997(5) 0.0175(4) 0.3261(4) 0.0184(14) Uani 1 1 d . U . . .
C6 C 0.8314(5) -0.0133(4) 0.4017(4) 0.0194(14) Uani 1 1 d . U . . .
C7 C 0.8025(5) 0.0574(4) 0.4676(4) 0.0221(15) Uani 1 1 d . U . . .
H7 H 0.7678 0.1202 0.4603 0.026 Uiso 1 1 calc R U . . .
C8 C 0.8226(5) 0.0382(5) 0.5408(4) 0.0300(17) Uani 1 1 d . U . . .
H8 H 0.8004 0.0869 0.5842 0.036 Uiso 1 1 calc R U . . .
C9 C 0.8755(6) -0.0522(5) 0.5526(4) 0.0344(18) Uani 1 1 d . U . . .
H9 H 0.8895 -0.0655 0.6040 0.041 Uiso 1 1 calc R U . . .
C10 C 0.9075(5) -0.1223(5) 0.4892(4) 0.0306(17) Uani 1 1 d . U . . .
H10 H 0.9440 -0.1842 0.4972 0.037 Uiso 1 1 calc R U . . .
C11 C 0.8873(5) -0.1039(4) 0.4138(4) 0.0206(15) Uani 1 1 d . U . . .
C12 C 1.0369(5) -0.2777(5) 0.3566(4) 0.0328(18) Uani 1 1 d . U . . .
H12A H 1.0931 -0.2421 0.3596 0.049 Uiso 1 1 calc R U . . .
H12B H 1.0696 -0.3282 0.3119 0.049 Uiso 1 1 calc R U . . .
H12C H 1.0088 -0.3065 0.4100 0.049 Uiso 1 1 calc R U . . .
C13 C 1.0204(5) -0.0646(4) 0.1057(4) 0.0207(15) Uani 1 1 d . U . . .
C14 C 1.0825(5) -0.0670(5) 0.2419(4) 0.0245(16) Uani 1 1 d . U . . .
C15 C 1.1088(6) -0.2198(5) 0.1664(4) 0.0271(16) Uani 1 1 d . U . . .
C16 C 0.7920(5) -0.1949(4) 0.2048(4) 0.0280(16) Uani 1 1 d . U . . .
H16 H 0.7603 -0.1615 0.2580 0.034 Uiso 1 1 calc R U . . .
C17 C 0.7270(6) -0.2427(5) 0.1752(5) 0.0389(19) Uani 1 1 d . U . . .
H17 H 0.6523 -0.2414 0.2069 0.047 Uiso 1 1 calc R U . . .
C18 C 0.7739(7) -0.2925(5) 0.0978(5) 0.046(2) Uani 1 1 d . U . . .
H18 H 0.7325 -0.3277 0.0763 0.055 Uiso 1 1 calc R U . . .
C19 C 0.8807(6) -0.2898(5) 0.0532(5) 0.0400(19) Uani 1 1 d . U . . .
H19 H 0.9134 -0.3213 -0.0008 0.048 Uiso 1 1 calc R U . . .
C20 C 0.9403(6) -0.2414(4) 0.0865(4) 0.0278(16) Uani 1 1 d . U . . .
H20 H 1.0149 -0.2414 0.0552 0.033 Uiso 1 1 calc R U . . .
C21 C 0.6394(4) 0.7521(4) 0.6822(4) 0.0159(14) Uani 1 1 d . U . . .
C22 C 0.6285(5) 0.7500(4) 0.6028(4) 0.0169(14) Uani 1 1 d . U . . .
H22 H 0.6398 0.6898 0.5744 0.020 Uiso 1 1 calc R U . . .
C23 C 0.6014(5) 0.8335(4) 0.5630(4) 0.0171(14) Uani 1 1 d . U . . .
C24 C 0.5916(5) 0.8265(4) 0.4776(4) 0.0201(14) Uani 1 1 d . U . . .
C25 C 0.5808(4) 0.9217(4) 0.6039(4) 0.0197(14) Uani 1 1 d . U . . .
H25 H 0.5628 0.9786 0.5775 0.024 Uiso 1 1 calc R U . . .
C26 C 0.5868(5) 0.9254(4) 0.6839(4) 0.0152(13) Uani 1 1 d . U . . .
C27 C 0.5577(5) 1.0205(4) 0.7313(4) 0.0235(15) Uani 1 1 d . U . . .
C28 C 0.6158(4) 0.8422(4) 0.7223(4) 0.0186(14) Uani 1 1 d . U . . .
H28 H 0.6195 0.8471 0.7774 0.022 Uiso 1 1 calc R U . . .
C29 C 0.7860(4) 0.6540(4) 0.7524(3) 0.0124(13) Uani 1 1 d . U . . .
C30 C 0.8570(5) 0.7196(4) 0.7259(4) 0.0151(13) Uani 1 1 d . U . . .
H30 H 0.8358 0.7725 0.6961 0.018 Uiso 1 1 calc R U . . .
C31 C 0.9562(5) 0.7095(4) 0.7417(4) 0.0180(14) Uani 1 1 d . U . . .
C32 C 1.0301(6) 0.7775(5) 0.7095(5) 0.0330(18) Uani 1 1 d . U . . .
C33 C 0.9896(5) 0.6341(4) 0.7862(4) 0.0210(15) Uani 1 1 d . U . . .
H33 H 1.0570 0.6278 0.7981 0.025 Uiso 1 1 calc R U . . .
C34 C 0.9222(5) 0.5685(4) 0.8126(4) 0.0178(14) Uani 1 1 d . U . . .
C35 C 0.9595(5) 0.4839(5) 0.8568(4) 0.0279(16) Uani 1 1 d . U . . .
C36 C 0.8240(5) 0.5782(4) 0.7954(4) 0.0185(14) Uani 1 1 d . U . . .
H36 H 0.7802 0.5312 0.8137 0.022 Uiso 1 1 calc R U . . .
C37 C 0.5671(4) 0.6531(4) 0.8155(4) 0.0132(13) Uani 1 1 d . U . . .
C38 C 0.5717(5) 0.6547(4) 0.8975(4) 0.0204(15) Uani 1 1 d . U . . .
H38 H 0.6384 0.6621 0.9061 0.024 Uiso 1 1 calc R U . . .
C39 C 0.4829(5) 0.6459(4) 0.9661(4) 0.0219(15) Uani 1 1 d . U . . .
C40 C 0.4929(6) 0.6475(5) 1.0510(4) 0.0310(17) Uani 1 1 d . U . . .
C41 C 0.3839(5) 0.6363(4) 0.9560(4) 0.0217(15) Uani 1 1 d . U . . .
H41 H 0.3228 0.6298 1.0030 0.026 Uiso 1 1 calc R U . . .
C42 C 0.3753(5) 0.6364(4) 0.8762(4) 0.0188(14) Uani 1 1 d . U . . .
C43 C 0.2684(5) 0.6236(5) 0.8658(4) 0.0304(17) Uani 1 1 d . U . . .
C44 C 0.4649(5) 0.6448(4) 0.8072(4) 0.0155(13) Uani 1 1 d . U . . .
H44 H 0.4570 0.6449 0.7531 0.019 Uiso 1 1 calc R U . . .
C45 C 0.6982(5) 0.5581(4) 0.6703(4) 0.0171(14) Uani 1 1 d . U . . .
C46 C 0.6505(5) 0.4777(4) 0.6924(4) 0.0156(13) Uani 1 1 d . U . . .
H46 H 0.5971 0.4785 0.7459 0.019 Uiso 1 1 calc R U . . .
C47 C 0.6788(5) 0.3958(4) 0.6380(4) 0.0187(14) Uani 1 1 d . U . . .
C48 C 0.6284(6) 0.3113(5) 0.6678(4) 0.0302(17) Uani 1 1 d . U . . .
C49 C 0.7551(5) 0.3925(4) 0.5595(4) 0.0219(15) Uani 1 1 d . U . . .
H49 H 0.7727 0.3382 0.5221 0.026 Uiso 1 1 calc R U . . .
C50 C 0.8055(5) 0.4702(4) 0.5365(4) 0.0192(14) Uani 1 1 d . U . . .
C51 C 0.8859(6) 0.4670(5) 0.4512(4) 0.0332(17) Uani 1 1 d . U . . .
C52 C 0.7782(5) 0.5498(4) 0.5905(4) 0.0182(14) Uani 1 1 d . U . . .
H52 H 0.8151 0.6015 0.5732 0.022 Uiso 1 1 calc R U . . .
C54 C 0.4850(6) 0.4535(5) 0.4953(5) 0.0372(19) Uani 1 1 d . U . . .
H54A H 0.4153 0.4638 0.4816 0.045 Uiso 1 1 calc R U . . .
H54B H 0.4733 0.4212 0.5486 0.045 Uiso 1 1 calc R U . . .
C55 C 0.6555(6) 0.0260(5) 0.9713(5) 0.042(2) Uani 1 1 d . U . . .
H55A H 0.6165 0.0230 0.9298 0.050 Uiso 1 1 calc R U . . .
H55B H 0.7239 0.0498 0.9437 0.050 Uiso 1 1 calc R U . . .
C56 C 0.6829(7) -0.0706(5) 1.0013(5) 0.052(2) Uani 1 1 d . U . . .
H56A H 0.6145 -0.0937 1.0305 0.062 Uiso 1 1 calc R U . . .
H56B H 0.7246 -0.0683 1.0410 0.062 Uiso 1 1 calc R U . . .
B1 B 0.6715(5) 0.6552(5) 0.7305(4) 0.0167(16) Uani 1 1 d . U . . .
F1 F 0.6457(4) 0.7445(3) 0.4347(2) 0.0492(12) Uani 1 1 d . U . . .
F2 F 0.4864(3) 0.8338(3) 0.4794(2) 0.0398(10) Uani 1 1 d . U . . .
F3 F 0.6262(3) 0.8967(3) 0.4299(2) 0.0388(10) Uani 1 1 d . U . . .
F4 F 0.4518(3) 1.0399(3) 0.7799(3) 0.0524(13) Uani 1 1 d . U . . .
F5 F 0.5672(4) 1.0938(3) 0.6822(3) 0.0522(12) Uani 1 1 d . U . . .
F6 F 0.6163(4) 1.0279(3) 0.7810(3) 0.0539(13) Uani 1 1 d . U . . .
F7 F 1.0234(5) 0.8156(5) 0.6421(5) 0.130(3) Uani 1 1 d . U . . .
F8 F 1.0110(6) 0.8495(5) 0.7615(5) 0.160(4) Uani 1 1 d . U . . .
F9 F 1.1340(3) 0.7444(3) 0.6953(4) 0.0801(18) Uani 1 1 d . U . . .
F10 F 1.0313(4) 0.4976(3) 0.8941(3) 0.0553(13) Uani 1 1 d . U . . .
F11 F 1.0071(4) 0.4063(3) 0.8045(3) 0.0575(13) Uani 1 1 d . U . . .
F12 F 0.8772(3) 0.4569(3) 0.9162(3) 0.0549(13) Uani 1 1 d . U . . .
F13 F 0.4888(4) 0.7337(3) 1.0814(3) 0.0678(15) Uani 1 1 d . U . . .
F14 F 0.5900(3) 0.5962(3) 1.0536(2) 0.0436(11) Uani 1 1 d . U . . .
F15 F 0.4171(3) 0.6098(3) 1.1083(2) 0.0513(12) Uani 1 1 d . U . . .
F16 F 0.1823(3) 0.6814(4) 0.9178(3) 0.0766(17) Uani 1 1 d . U . . .
F17 F 0.2492(4) 0.5385(4) 0.8800(4) 0.092(2) Uani 1 1 d . U . . .
F18 F 0.2614(3) 0.6438(4) 0.7910(3) 0.0714(16) Uani 1 1 d . U . . .
F19 F 0.6828(4) 0.2549(3) 0.7113(3) 0.0487(12) Uani 1 1 d . U . . .
F20 F 0.5251(3) 0.3334(3) 0.7168(3) 0.0666(15) Uani 1 1 d . U . . .
F21 F 0.6304(4) 0.2547(3) 0.6039(3) 0.0610(14) Uani 1 1 d . U . . .
F22 F 0.8419(3) 0.4585(3) 0.3912(2) 0.0512(12) Uani 1 1 d . U . . .
F23 F 0.9688(3) 0.3897(3) 0.4378(3) 0.0604(14) Uani 1 1 d . U . . .
F24 F 0.9361(4) 0.5406(3) 0.4363(3) 0.0620(14) Uani 1 1 d . U . . .
Fe1 Fe 0.99357(7) -0.12640(6) 0.20972(5) 0.0188(2) Uani 1 1 d . U . . .
N1 N 0.8684(4) -0.0149(3) 0.2478(3) 0.0160(11) Uani 1 1 d . U . . .
N2 N 0.9295(4) 0.0043(4) 0.1071(3) 0.0229(13) Uani 1 1 d . U . . .
H2A H 0.9241 0.0313 0.0611 0.027 Uiso 1 1 calc R U . . .
N3 N 0.8971(4) -0.1937(3) 0.1622(3) 0.0218(12) Uani 1 1 d . U . . .
O1 O 1.0983(3) -0.0836(3) 0.0389(3) 0.0260(11) Uani 1 1 d . U . . .
O2 O 1.1448(4) -0.0328(4) 0.2606(3) 0.0416(13) Uani 1 1 d . U . . .
O3 O 1.1876(4) -0.2764(3) 0.1397(3) 0.0425(13) Uani 1 1 d . U . . .
S1 S 0.92475(13) -0.19705(11) 0.33497(10) 0.0223(4) Uani 1 1 d . U . . .
Cl2 Cl 0.59098(16) 0.37924(15) 0.41441(13) 0.0479(5) Uani 1 1 d . U . . .
Cl3 Cl 0.56979(16) 0.10556(13) 1.05826(12) 0.0434(5) Uani 1 1 d . U . . .
Cl4 Cl 0.7643(2) -0.14947(17) 0.91258(14) 0.0703(8) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.344(7) . ?
C1 N2 1.368(7) . ?
C1 C2 1.404(8) . ?
C2 C3 1.370(8) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.382(8) . ?
C4 H4 0.9500 . ?
C5 N1 1.369(7) . ?
C5 C6 1.497(8) . ?
C6 C11 1.407(8) . ?
C6 C7 1.417(8) . ?
C7 C8 1.355(8) . ?
C7 H7 0.9500 . ?
C8 C9 1.387(9) . ?
C8 H8 0.9500 . ?
C9 C10 1.378(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.392(8) . ?
C10 H10 0.9500 . ?
C11 S1 1.774(6) . ?
C12 S1 1.813(6) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O1 1.249(7) . ?
C13 N2 1.383(7) . ?
C13 Fe1 1.920(6) . ?
C14 O2 1.146(7) . ?
C14 Fe1 1.769(7) . ?
C15 O3 1.145(7) . ?
C15 Fe1 1.772(7) . ?
C16 N3 1.336(8) . ?
C16 C17 1.386(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.390(10) . ?
C17 H17 0.9500 . ?
C18 C19 1.368(10) . ?
C18 H18 0.9500 . ?
C19 C20 1.371(9) . ?
C19 H19 0.9500 . ?
C20 N3 1.354(8) . ?
C20 H20 0.9500 . ?
C21 C22 1.391(8) . ?
C21 C28 1.393(8) . ?
C21 B1 1.652(9) . ?
C22 C23 1.404(8) . ?
C22 H22 0.9500 . ?
C23 C25 1.378(8) . ?
C23 C24 1.491(8) . ?
C24 F1 1.331(7) . ?
C24 F3 1.337(7) . ?
C24 F2 1.347(7) . ?
C25 C26 1.378(8) . ?
C25 H25 0.9500 . ?
C26 C28 1.395(8) . ?
C26 C27 1.502(8) . ?
C27 F6 1.315(7) . ?
C27 F5 1.329(7) . ?
C27 F4 1.344(7) . ?
C28 H28 0.9500 . ?
C29 C36 1.397(8) . ?
C29 C30 1.413(8) . ?
C29 B1 1.643(9) . ?
C30 C31 1.382(8) . ?
C30 H30 0.9500 . ?
C31 C33 1.387(8) . ?
C31 C32 1.478(8) . ?
C32 F7 1.277(8) . ?
C32 F8 1.292(9) . ?
C32 F9 1.293(7) . ?
C33 C34 1.380(8) . ?
C33 H33 0.9500 . ?
C34 C36 1.381(8) . ?
C34 C35 1.497(8) . ?
C35 F10 1.324(7) . ?
C35 F12 1.335(7) . ?
C35 F11 1.342(8) . ?
C36 H36 0.9500 . ?
C37 C38 1.404(8) . ?
C37 C44 1.409(8) . ?
C37 B1 1.644(9) . ?
C38 C39 1.383(8) . ?
C38 H38 0.9500 . ?
C39 C41 1.386(8) . ?
C39 C40 1.478(9) . ?
C40 F13 1.322(8) . ?
C40 F15 1.339(7) . ?
C40 F14 1.351(7) . ?
C41 C42 1.384(8) . ?
C41 H41 0.9500 . ?
C42 C44 1.390(8) . ?
C42 C43 1.502(8) . ?
C43 F17 1.291(8) . ?
C43 F18 1.319(8) . ?
C43 F16 1.324(7) . ?
C44 H44 0.9500 . ?
C45 C46 1.400(8) . ?
C45 C52 1.410(8) . ?
C45 B1 1.641(9) . ?
C46 C47 1.409(8) . ?
C46 H46 0.9500 . ?
C47 C49 1.380(8) . ?
C47 C48 1.492(8) . ?
C48 F20 1.321(8) . ?
C48 F19 1.340(7) . ?
C48 F21 1.342(7) . ?
C49 C50 1.386(8) . ?
C49 H49 0.9500 . ?
C50 C52 1.381(8) . ?
C50 C51 1.486(9) . ?
C51 F24 1.323(8) . ?
C51 F22 1.327(7) . ?
C51 F23 1.354(8) . ?
C52 H52 0.9500 . ?
C54 C54 1.476(13) 2_666 ?
C54 Cl2 1.783(7) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C55 C56 1.484(10) . ?
C55 Cl3 1.792(7) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 Cl4 1.792(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
Fe1 N1 1.996(5) . ?
Fe1 N3 2.061(5) . ?
Fe1 S1 2.3257(18) . ?
N2 H2A 0.8800 . ?

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
N1 C1 N2 115.0(5) . . ?
N1 C1 C2 123.3(6) . . ?
N2 C1 C2 121.7(6) . . ?
C3 C2 C1 117.1(6) . . ?
C3 C2 H2 121.4 . . ?
C1 C2 H2 121.4 . . ?
C2 C3 C4 120.3(6) . . ?
C2 C3 H3 119.8 . . ?
C4 C3 H3 119.8 . . ?
C3 C4 C5 120.1(6) . . ?
C3 C4 H4 119.9 . . ?
C5 C4 H4 119.9 . . ?
N1 C5 C4 120.5(6) . . ?
N1 C5 C6 120.3(5) . . ?
C4 C5 C6 119.1(5) . . ?
C11 C6 C7 116.9(6) . . ?
C11 C6 C5 127.2(5) . . ?
C7 C6 C5 115.9(5) . . ?
C8 C7 C6 122.1(6) . . ?
C8 C7 H7 119.0 . . ?
C6 C7 H7 119.0 . . ?
C7 C8 C9 120.4(6) . . ?
C7 C8 H8 119.8 . . ?
C9 C8 H8 119.8 . . ?
C10 C9 C8 119.3(6) . . ?
C10 C9 H9 120.3 . . ?
C8 C9 H9 120.3 . . ?
C9 C10 C11 121.0(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C10 C11 C6 120.2(6) . . ?
C10 C11 S1 119.9(5) . . ?
C6 C11 S1 119.8(5) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 N2 118.7(5) . . ?
O1 C13 Fe1 130.6(5) . . ?
N2 C13 Fe1 110.3(4) . . ?
O2 C14 Fe1 176.1(6) . . ?
O3 C15 Fe1 175.5(6) . . ?
N3 C16 C17 123.1(7) . . ?
N3 C16 H16 118.4 . . ?
C17 C16 H16 118.4 . . ?
C16 C17 C18 118.3(7) . . ?
C16 C17 H17 120.8 . . ?
C18 C17 H17 120.8 . . ?
C19 C18 C17 118.7(7) . . ?
C19 C18 H18 120.6 . . ?
C17 C18 H18 120.6 . . ?
C18 C19 C20 119.8(7) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
N3 C20 C19 122.5(7) . . ?
N3 C20 H20 118.8 . . ?
C19 C20 H20 118.8 . . ?
C22 C21 C28 115.9(5) . . ?
C22 C21 B1 123.6(5) . . ?
C28 C21 B1 120.3(5) . . ?
C21 C22 C23 122.5(6) . . ?
C21 C22 H22 118.8 . . ?
C23 C22 H22 118.8 . . ?
C25 C23 C22 120.0(6) . . ?
C25 C23 C24 120.1(5) . . ?
C22 C23 C24 119.9(5) . . ?
F1 C24 F3 106.9(5) . . ?
F1 C24 F2 105.4(5) . . ?
F3 C24 F2 104.1(5) . . ?
F1 C24 C23 114.1(5) . . ?
F3 C24 C23 113.3(5) . . ?
F2 C24 C23 112.3(5) . . ?
C23 C25 C26 118.6(6) . . ?
C23 C25 H25 120.7 . . ?
C26 C25 H25 120.7 . . ?
C25 C26 C28 121.0(5) . . ?
C25 C26 C27 119.3(5) . . ?
C28 C26 C27 119.7(5) . . ?
F6 C27 F5 106.4(5) . . ?
F6 C27 F4 106.1(5) . . ?
F5 C27 F4 104.1(5) . . ?
F6 C27 C26 114.2(5) . . ?
F5 C27 C26 113.4(5) . . ?
F4 C27 C26 111.8(5) . . ?
C21 C28 C26 121.9(6) . . ?
C21 C28 H28 119.1 . . ?
C26 C28 H28 119.1 . . ?
C36 C29 C30 114.8(5) . . ?
C36 C29 B1 119.0(5) . . ?
C30 C29 B1 125.9(5) . . ?
C31 C30 C29 122.4(5) . . ?
C31 C30 H30 118.8 . . ?
C29 C30 H30 118.8 . . ?
C30 C31 C33 120.7(5) . . ?
C30 C31 C32 120.5(5) . . ?
C33 C31 C32 118.8(5) . . ?
F7 C32 F8 104.0(7) . . ?
F7 C32 F9 105.0(7) . . ?
F8 C32 F9 102.5(7) . . ?
F7 C32 C31 115.3(6) . . ?
F8 C32 C31 112.5(6) . . ?
F9 C32 C31 116.0(6) . . ?
C34 C33 C31 118.3(5) . . ?
C34 C33 H33 120.9 . . ?
C31 C33 H33 120.9 . . ?
C33 C34 C36 120.7(5) . . ?
C33 C34 C35 119.0(5) . . ?
C36 C34 C35 120.2(5) . . ?
F10 C35 F12 105.5(5) . . ?
F10 C35 F11 106.6(5) . . ?
F12 C35 F11 104.9(6) . . ?
F10 C35 C34 113.9(5) . . ?
F12 C35 C34 113.3(5) . . ?
F11 C35 C34 111.9(5) . . ?
C34 C36 C29 123.1(5) . . ?
C34 C36 H36 118.5 . . ?
C29 C36 H36 118.5 . . ?
C38 C37 C44 115.9(5) . . ?
C38 C37 B1 125.2(5) . . ?
C44 C37 B1 118.8(5) . . ?
C39 C38 C37 122.5(6) . . ?
C39 C38 H38 118.8 . . ?
C37 C38 H38 118.8 . . ?
C38 C39 C41 120.3(6) . . ?
C38 C39 C40 120.0(6) . . ?
C41 C39 C40 119.6(6) . . ?
F13 C40 F15 106.5(6) . . ?
F13 C40 F14 104.4(6) . . ?
F15 C40 F14 104.2(5) . . ?
F13 C40 C39 114.0(6) . . ?
F15 C40 C39 114.4(6) . . ?
F14 C40 C39 112.4(5) . . ?
C42 C41 C39 118.9(6) . . ?
C42 C41 H41 120.5 . . ?
C39 C41 H41 120.5 . . ?
C41 C42 C44 120.6(6) . . ?
C41 C42 C43 118.5(5) . . ?
C44 C42 C43 120.9(5) . . ?
F17 C43 F18 107.7(6) . . ?
F17 C43 F16 105.3(6) . . ?
F18 C43 F16 104.2(6) . . ?
F17 C43 C42 113.3(6) . . ?
F18 C43 C42 113.2(6) . . ?
F16 C43 C42 112.4(6) . . ?
C42 C44 C37 121.7(5) . . ?
C42 C44 H44 119.1 . . ?
C37 C44 H44 119.1 . . ?
C46 C45 C52 115.0(5) . . ?
C46 C45 B1 125.2(5) . . ?
C52 C45 B1 119.8(5) . . ?
C45 C46 C47 122.2(6) . . ?
C45 C46 H46 118.9 . . ?
C47 C46 H46 118.9 . . ?
C49 C47 C46 120.6(6) . . ?
C49 C47 C48 120.4(6) . . ?
C46 C47 C48 119.0(6) . . ?
F20 C48 F19 105.9(6) . . ?
F20 C48 F21 107.2(6) . . ?
F19 C48 F21 105.1(5) . . ?
F20 C48 C47 113.9(5) . . ?
F19 C48 C47 112.4(6) . . ?
F21 C48 C47 111.8(6) . . ?
C47 C49 C50 118.6(6) . . ?
C47 C49 H49 120.7 . . ?
C50 C49 H49 120.7 . . ?
C52 C50 C49 120.5(6) . . ?
C52 C50 C51 121.2(6) . . ?
C49 C50 C51 118.2(6) . . ?
F24 C51 F22 108.1(6) . . ?
F24 C51 F23 104.4(6) . . ?
F22 C51 F23 104.7(6) . . ?
F24 C51 C50 114.4(6) . . ?
F22 C51 C50 113.0(6) . . ?
F23 C51 C50 111.4(6) . . ?
C50 C52 C45 123.1(6) . . ?
C50 C52 H52 118.4 . . ?
C45 C52 H52 118.4 . . ?
C54 C54 Cl2 110.7(7) 2_666 . ?
C54 C54 H54A 109.5 2_666 . ?
Cl2 C54 H54A 109.5 . . ?
C54 C54 H54B 109.5 2_666 . ?
Cl2 C54 H54B 109.5 . . ?
H54A C54 H54B 108.1 . . ?
C56 C55 Cl3 109.2(5) . . ?
C56 C55 H55A 109.8 . . ?
Cl3 C55 H55A 109.8 . . ?
C56 C55 H55B 109.8 . . ?
Cl3 C55 H55B 109.8 . . ?
H55A C55 H55B 108.3 . . ?
C55 C56 Cl4 108.2(5) . . ?
C55 C56 H56A 110.1 . . ?
Cl4 C56 H56A 110.1 . . ?
C55 C56 H56B 110.1 . . ?
Cl4 C56 H56B 110.1 . . ?
H56A C56 H56B 108.4 . . ?
C45 B1 C29 104.2(5) . . ?
C45 B1 C37 110.9(5) . . ?
C29 B1 C37 111.6(5) . . ?
C45 B1 C21 111.4(5) . . ?
C29 B1 C21 111.3(5) . . ?
C37 B1 C21 107.5(5) . . ?
C14 Fe1 C15 87.4(3) . . ?
C14 Fe1 C13 92.3(3) . . ?
C15 Fe1 C13 91.7(3) . . ?
C14 Fe1 N1 92.3(2) . . ?
C15 Fe1 N1 174.3(3) . . ?
C13 Fe1 N1 82.7(2) . . ?
C14 Fe1 N3 175.3(3) . . ?
C15 Fe1 N3 90.9(3) . . ?
C13 Fe1 N3 83.4(2) . . ?
N1 Fe1 N3 89.02(19) . . ?
C14 Fe1 S1 96.8(2) . . ?
C15 Fe1 S1 95.9(2) . . ?
C13 Fe1 S1 168.39(19) . . ?
N1 Fe1 S1 89.77(14) . . ?
N3 Fe1 S1 87.71(15) . . ?
C1 N1 C5 118.0(5) . . ?
C1 N1 Fe1 110.8(4) . . ?
C5 N1 Fe1 131.1(4) . . ?
C1 N2 C13 118.1(5) . . ?
C1 N2 H2A 120.9 . . ?
C13 N2 H2A 120.9 . . ?
C16 N3 C20 117.5(6) . . ?
C16 N3 Fe1 122.3(4) . . ?
C20 N3 Fe1 120.2(4) . . ?
C11 S1 C12 103.3(3) . . ?
C11 S1 Fe1 105.3(2) . . ?
C12 S1 Fe1 109.1(2) . . ?

_refine_diff_density_max         0.989
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.102

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_3b
_database_code_depnum_ccdc_archive 'CCDC 1547037'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT910_shelx               
;
PROBLEM: Missing # of FCF Reflection(s) Below Theta(Min)          27 Note  
RESPONSE: These few reflections were blocked by the beam stop
and omitted by the data set.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C82 H53 B F24 Fe N2 O2 P2 S'
_chemical_formula_sum            'C82 H53 B F24 Fe N2 O2 P2 S'
_chemical_formula_weight         1714.92

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'
F F 0.0171 0.0103 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 '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                   14.5766(10)
_cell_length_b                   17.7215(13)
_cell_length_c                   18.8505(13)
_cell_angle_alpha                87.007(2)
_cell_angle_beta                 70.413(2)
_cell_angle_gamma                68.967(2)
_cell_volume                     4269.1(5)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13783
_cell_measurement_theta_min      1.7122
_cell_measurement_theta_max      31.4244

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.334
_exptl_crystal_F_000             1736
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.336
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8049
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Sealed Tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            60121
_diffrn_reflns_av_unetI/netI     0.0495
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         2.995
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             19294
_reflns_number_gt                14935
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'

_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_refine_special_details          
;
The BArF anion contains several highly anisotropic trifluoromethyl groups.  Three of these 
were best refined as a disordered group, while the others were allowed to refine in a 
single conformation, albeit with expected highly anisotropic displacement parameters.  
All these groups were refined with displacement parameter restraints.  The 
disorder was modeled separately for the three groups but in essentially the same manner.  
The variable x was assigned to the site occupancy for one component of the disordered 
CF3 group, while (1-x) was assigned to the alternate component.  A common isotropic 
displacement parameter was refined for all six F atoms while refining x.  The geometry 
of the CF3 groups was restrained throughout the refinement process.  Upon convergence of 
the variable x, the site occupancies for the atoms were fixed during subsequent refinement 
cycles.

A region of disordered solvent centered at 0,0,0 and extending along the a-axis was 
observed.  The solvent in this region could not be effectively modeled.  The program, 
SQUEEZE, was used to remove the contribution to the scattering due to the disordered 
solvent. The formula is calculated without the masked solvent.


# SQUEEZE RESULTS
# 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 -0.005  0.000  0.005       759        80 ' '
   2  0.093  0.561  0.665        11         1 ' '
   3  0.907  0.439  0.335        11         1 ' '
_platon_squeeze_details                           ?
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0649P)²+3.8687P] 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         19294
_refine_ls_number_parameters     1124
_refine_ls_number_restraints     801
_refine_ls_R_factor_all          0.0716
_refine_ls_R_factor_gt           0.0537
_refine_ls_wR_factor_ref         0.1423
_refine_ls_wR_factor_gt          0.1320
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.119
_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
C13 C 0.38997(17) 0.47105(14) 0.46300(12) 0.0155(4) Uani 1 1 d . . . . .
C1 C 0.52518(17) 0.43322(14) 0.34130(12) 0.0170(4) Uani 1 1 d . . . . .
C2 C 0.62663(18) 0.42276(15) 0.29419(13) 0.0207(5) Uani 1 1 d . . . . .
H2 H 0.6741 0.4330 0.3131 0.025 Uiso 1 1 calc R U . . .
C3 C 0.65568(19) 0.39734(16) 0.22011(14) 0.0245(5) Uani 1 1 d . . . . .
H3 H 0.7222 0.3934 0.1855 0.029 Uiso 1 1 calc R U . . .
C4 C 0.58624(19) 0.37722(16) 0.19594(13) 0.0234(5) Uani 1 1 d . . . . .
H4 H 0.6057 0.3592 0.1446 0.028 Uiso 1 1 calc R U . . .
C5 C 0.48872(18) 0.38325(15) 0.24643(12) 0.0187(5) Uani 1 1 d . . . . .
C6 C 0.42921(19) 0.34206(15) 0.22226(12) 0.0211(5) Uani 1 1 d . . . . .
C7 C 0.4883(2) 0.27063(16) 0.17434(13) 0.0264(5) Uani 1 1 d . . . . .
H7 H 0.5624 0.2519 0.1585 0.032 Uiso 1 1 calc R U . . .
C8 C 0.4416(2) 0.22694(17) 0.14960(14) 0.0300(6) Uani 1 1 d . . . . .
H8 H 0.4832 0.1790 0.1170 0.036 Uiso 1 1 calc R U . . .
C9 C 0.3340(2) 0.25354(17) 0.17257(15) 0.0310(6) Uani 1 1 d . . . . .
H9 H 0.3017 0.2241 0.1550 0.037 Uiso 1 1 calc R U . . .
C10 C 0.2730(2) 0.32222(17) 0.22063(14) 0.0267(6) Uani 1 1 d . . . . .
H10 H 0.1990 0.3397 0.2365 0.032 Uiso 1 1 calc R U . . .
C11 C 0.3199(2) 0.36652(15) 0.24624(12) 0.0211(5) Uani 1 1 d . . . . .
C12 C 0.1131(2) 0.46354(19) 0.32695(15) 0.0319(6) Uani 1 1 d . . . . .
H12A H 0.0935 0.4727 0.2815 0.048 Uiso 1 1 calc R U . . .
H12B H 0.0664 0.5085 0.3653 0.048 Uiso 1 1 calc R U . . .
H12C H 0.1072 0.4126 0.3467 0.048 Uiso 1 1 calc R U . . .
C14 C 0.18637(19) 0.48868(15) 0.47233(13) 0.0202(5) Uani 1 1 d . . . . .
C15 C 0.44896(18) 0.63888(15) 0.36036(13) 0.0205(5) Uani 1 1 d . . . . .
H15 H 0.4196 0.6536 0.4131 0.025 Uiso 1 1 calc R U . . .
C16 C 0.54417(19) 0.64477(16) 0.31948(14) 0.0245(5) Uani 1 1 d . . . . .
H16 H 0.5806 0.6625 0.3444 0.029 Uiso 1 1 calc R U . . .
C17 C 0.58643(19) 0.62505(16) 0.24260(14) 0.0252(5) Uani 1 1 d . . . . .
H17 H 0.6512 0.6303 0.2146 0.030 Uiso 1 1 calc R U . . .
C18 C 0.53472(19) 0.59763(16) 0.20599(14) 0.0254(5) Uani 1 1 d . . . . .
H18 H 0.5639 0.5844 0.1530 0.030 Uiso 1 1 calc R U . . .
C19 C 0.44010(19) 0.58949(15) 0.24692(13) 0.0204(5) Uani 1 1 d . . . . .
H19 H 0.4058 0.5690 0.2222 0.024 Uiso 1 1 calc R U . . .
C20 C 0.39566(17) 0.61151(14) 0.32461(12) 0.0170(4) Uani 1 1 d . . . . .
C21 C 0.22078(17) 0.67114(15) 0.46214(13) 0.0197(5) Uani 1 1 d . . . . .
C22 C 0.19140(19) 0.75301(16) 0.44644(14) 0.0243(5) Uani 1 1 d . . . . .
H22 H 0.2101 0.7667 0.3955 0.029 Uiso 1 1 calc R U . . .
C23 C 0.1356(2) 0.81384(17) 0.50421(16) 0.0294(6) Uani 1 1 d . . . . .
H23 H 0.1151 0.8690 0.4929 0.035 Uiso 1 1 calc R U . . .
C24 C 0.10950(19) 0.79439(17) 0.57880(15) 0.0279(6) Uani 1 1 d . . . . .
H24 H 0.0700 0.8361 0.6186 0.034 Uiso 1 1 calc R U . . .
C25 C 0.1412(2) 0.71433(18) 0.59481(14) 0.0285(6) Uani 1 1 d . . . . .
H25 H 0.1255 0.7012 0.6459 0.034 Uiso 1 1 calc R U . . .
C26 C 0.19644(18) 0.65202(16) 0.53679(13) 0.0221(5) Uani 1 1 d . . . . .
H26 H 0.2171 0.5970 0.5485 0.026 Uiso 1 1 calc R U . . .
C27 C 0.17770(18) 0.64598(15) 0.33780(13) 0.0206(5) Uani 1 1 d . . . . .
C28 C 0.1951(2) 0.68751(17) 0.27275(14) 0.0260(5) Uani 1 1 d . . . . .
H28 H 0.2641 0.6839 0.2438 0.031 Uiso 1 1 calc R U . . .
C29 C 0.1121(2) 0.73404(19) 0.25011(16) 0.0345(6) Uani 1 1 d . . . . .
H29 H 0.1244 0.7628 0.2061 0.041 Uiso 1 1 calc R U . . .
C30 C 0.0111(2) 0.7390(2) 0.29109(17) 0.0370(7) Uani 1 1 d . . . . .
H30 H -0.0452 0.7698 0.2745 0.044 Uiso 1 1 calc R U . . .
C31 C -0.0073(2) 0.69865(18) 0.35658(16) 0.0326(6) Uani 1 1 d . . . . .
H31 H -0.0764 0.7024 0.3853 0.039 Uiso 1 1 calc R U . . .
C32 C 0.07540(19) 0.65302(17) 0.37993(14) 0.0261(5) Uani 1 1 d . . . . .
H32 H 0.0624 0.6262 0.4251 0.031 Uiso 1 1 calc R U . . .
C33 C 0.47989(18) 0.26774(15) 0.41615(13) 0.0198(5) Uani 1 1 d . . . . .
C34 C 0.52921(19) 0.26147(17) 0.46952(14) 0.0265(5) Uani 1 1 d . . . . .
H34 H 0.4890 0.2848 0.5196 0.032 Uiso 1 1 calc R U . . .
C35 C 0.6363(2) 0.2214(2) 0.44982(16) 0.0371(7) Uani 1 1 d . . . . .
H35 H 0.6692 0.2179 0.4863 0.045 Uiso 1 1 calc R U . . .
C36 C 0.6957(2) 0.18641(19) 0.37685(17) 0.0361(7) Uani 1 1 d . . . . .
H36 H 0.7689 0.1585 0.3636 0.043 Uiso 1 1 calc R U . . .
C37 C 0.6481(2) 0.19231(17) 0.32389(15) 0.0285(6) Uani 1 1 d . . . . .
H37 H 0.6886 0.1685 0.2739 0.034 Uiso 1 1 calc R U . . .
C38 C 0.54112(19) 0.23288(15) 0.34318(13) 0.0216(5) Uani 1 1 d . . . . .
H38 H 0.5091 0.2370 0.3060 0.026 Uiso 1 1 calc R U . . .
C39 C 0.29303(17) 0.31502(16) 0.54361(13) 0.0203(5) Uani 1 1 d . . . . .
C40 C 0.24530(19) 0.37829(17) 0.59910(13) 0.0252(5) Uani 1 1 d . . . . .
H40 H 0.2346 0.4324 0.5856 0.030 Uiso 1 1 calc R U . . .
C41 C 0.2125(2) 0.3626(2) 0.67552(14) 0.0314(6) Uani 1 1 d . . . . .
H41 H 0.1776 0.4063 0.7135 0.038 Uiso 1 1 calc R U . . .
C42 C 0.2310(2) 0.2839(2) 0.69559(14) 0.0341(7) Uani 1 1 d . . . . .
H42 H 0.2102 0.2735 0.7474 0.041 Uiso 1 1 calc R U . . .
C43 C 0.2795(2) 0.22038(19) 0.64057(15) 0.0331(6) Uani 1 1 d . . . . .
H43 H 0.2925 0.1662 0.6545 0.040 Uiso 1 1 calc R U . . .
C44 C 0.30937(19) 0.23544(17) 0.56465(15) 0.0276(6) Uani 1 1 d . . . . .
H44 H 0.3410 0.1916 0.5269 0.033 Uiso 1 1 calc R U . . .
C45 C 0.28025(19) 0.26854(15) 0.40862(13) 0.0210(5) Uani 1 1 d . . . . .
C46 C 0.1711(2) 0.30083(17) 0.43257(15) 0.0273(5) Uani 1 1 d . . . . .
H46 H 0.1341 0.3508 0.4627 0.033 Uiso 1 1 calc R U . . .
C47 C 0.1163(2) 0.26042(19) 0.41270(17) 0.0351(6) Uani 1 1 d . . . . .
H47 H 0.0421 0.2827 0.4295 0.042 Uiso 1 1 calc R U . . .
C48 C 0.1693(2) 0.18791(19) 0.36856(17) 0.0359(7) Uani 1 1 d . . . . .
H48 H 0.1318 0.1608 0.3543 0.043 Uiso 1 1 calc R U . . .
C49 C 0.2771(2) 0.15499(18) 0.34531(17) 0.0340(6) Uani 1 1 d . . . . .
H49 H 0.3136 0.1050 0.3152 0.041 Uiso 1 1 calc R U . . .
C50 C 0.3326(2) 0.19468(16) 0.36569(15) 0.0272(5) Uani 1 1 d . . . . .
H50 H 0.4066 0.1711 0.3501 0.033 Uiso 1 1 calc R U . . .
C51 C 0.63102(18) 0.71377(14) 0.03787(12) 0.0174(4) Uani 1 1 d . U . . .
C52 C 0.52344(18) 0.75368(15) 0.05476(13) 0.0212(5) Uani 1 1 d . U . . .
H52 H 0.4911 0.8062 0.0804 0.025 Uiso 1 1 calc R U . . .
C53 C 0.46172(19) 0.71947(16) 0.03551(15) 0.0258(5) Uani 1 1 d . U . . .
C54 C 0.3478(2) 0.76673(17) 0.05429(17) 0.0392(7) Uani 1 1 d D U . . .
F19 F 0.3241(7) 0.8233(4) 0.0091(4) 0.0612(19) Uani 0.57 1 d D U P A 1
F20 F 0.3063(5) 0.8079(4) 0.1245(2) 0.0531(14) Uani 0.57 1 d D U P A 1
F21 F 0.2907(4) 0.7212(3) 0.0624(3) 0.0747(18) Uani 0.57 1 d D U P A 1
F19A F 0.2935(7) 0.7818(6) 0.1244(3) 0.072(2) Uani 0.43 1 d D U P A 2
F20A F 0.3048(5) 0.7308(4) 0.0192(4) 0.071(2) Uani 0.43 1 d D U P A 2
F21A F 0.3321(9) 0.8389(4) 0.0233(5) 0.0475(19) Uani 0.43 1 d D U P A 2
C55 C 0.5058(2) 0.64333(16) -0.00266(15) 0.0260(5) Uani 1 1 d . U . . .
H55 H 0.4636 0.6191 -0.0144 0.031 Uiso 1 1 calc R U . . .
C56 C 0.61288(19) 0.60355(14) -0.02324(13) 0.0203(5) Uani 1 1 d . U . . .
C57 C 0.6630(2) 0.52084(16) -0.06288(15) 0.0274(5) Uani 1 1 d . U . . .
C58 C 0.67401(18) 0.63848(14) -0.00374(13) 0.0187(5) Uani 1 1 d . U . . .
H58 H 0.7474 0.6102 -0.0192 0.022 Uiso 1 1 calc R U . . .
C59 C 0.80637(18) 0.69283(14) 0.07496(12) 0.0167(4) Uani 1 1 d . U . . .
C60 C 0.82271(18) 0.61293(14) 0.09400(12) 0.0191(5) Uani 1 1 d . U . . .
H60 H 0.7711 0.5910 0.0966 0.023 Uiso 1 1 calc R U . . .
C61 C 0.91227(19) 0.56410(15) 0.10939(13) 0.0211(5) Uani 1 1 d . U . . .
C62 C 0.92386(18) 0.47928(15) 0.13004(13) 0.0278(5) Uani 1 1 d D U . . .
F13 F 0.8914(4) 0.4420(4) 0.0863(3) 0.0490(15) Uani 0.53 1 d D U P B 1
F14 F 0.8617(5) 0.4759(7) 0.1993(3) 0.0361(16) Uani 0.53 1 d D U P B 1
F15 F 1.0185(4) 0.4303(4) 0.1231(4) 0.064(2) Uani 0.53 1 d D U P B 1
F13A F 1.0055(4) 0.4467(5) 0.1553(4) 0.060(2) Uani 0.47 1 d D U P B 2
F14A F 0.9399(5) 0.4302(5) 0.0744(3) 0.063(2) Uani 0.47 1 d D U P B 2
F15A F 0.8425(5) 0.4763(8) 0.1871(3) 0.0356(18) Uani 0.47 1 d D U P B 2
C63 C 0.99088(19) 0.59235(16) 0.10449(14) 0.0245(5) Uani 1 1 d . U . . .
H63 H 1.0523 0.5588 0.1141 0.029 Uiso 1 1 calc R U . . .
C64 C 0.97707(19) 0.67158(16) 0.08504(14) 0.0235(5) Uani 1 1 d . U . . .
C65 C 1.0624(2) 0.70407(18) 0.07329(17) 0.0346(6) Uani 1 1 d . U . . .
C66 C 0.88696(18) 0.72011(15) 0.07188(12) 0.0200(5) Uani 1 1 d . U . . .
H66 H 0.8792 0.7744 0.0602 0.024 Uiso 1 1 calc R U . . .
C67 C 0.63886(19) 0.82295(14) 0.13158(13) 0.0208(5) Uani 1 1 d . U . . .
C68 C 0.5545(2) 0.81800(15) 0.19196(13) 0.0267(5) Uani 1 1 d . U . . .
H68 H 0.5304 0.7752 0.1899 0.032 Uiso 1 1 calc R U . . .
C69 C 0.5041(2) 0.87339(17) 0.25502(14) 0.0341(6) Uani 1 1 d . U . . .
C70 C 0.4104(3) 0.8676(2) 0.31670(18) 0.0576(10) Uani 1 1 d . U . . .
F10 F 0.3365(2) 0.94124(13) 0.34280(14) 0.0981(11) Uani 1 1 d . U . . .
F11 F 0.36550(16) 0.82324(13) 0.29596(11) 0.0598(6) Uani 1 1 d . U . . .
F12 F 0.4345(2) 0.83416(14) 0.37734(10) 0.0789(8) Uani 1 1 d . U . . .
C71 C 0.5382(2) 0.93513(18) 0.26166(16) 0.0383(7) Uani 1 1 d . U . . .
H71 H 0.5046 0.9724 0.3051 0.046 Uiso 1 1 calc R U . . .
C72 C 0.6222(2) 0.94114(18) 0.20369(17) 0.0376(7) Uani 1 1 d . U . . .
C73 C 0.6598(3) 1.0075(2) 0.2092(2) 0.0649(11) Uani 1 1 d D U . . .
F7 F 0.6848(6) 1.0416(3) 0.1414(3) 0.1044(19) Uani 0.57 1 d D U P C 1
F8 F 0.7428(4) 0.9871(4) 0.2263(4) 0.0992(19) Uani 0.57 1 d D U P C 1
F9 F 0.5868(5) 1.0715(4) 0.2527(4) 0.108(3) Uani 0.57 1 d D U P C 1
F7A F 0.6840(7) 1.0008(4) 0.2745(4) 0.106(2) Uani 0.43 1 d D U P C 2
F8A F 0.5934(6) 1.0800(4) 0.2179(4) 0.0644(19) Uani 0.43 1 d D U P C 2
F9A F 0.7472(6) 1.0045(5) 0.1566(5) 0.114(3) Uani 0.43 1 d D U P C 2
C74 C 0.6710(2) 0.88680(16) 0.13944(15) 0.0281(6) Uani 1 1 d . U . . .
H74 H 0.7279 0.8933 0.0998 0.034 Uiso 1 1 calc R U . . .
C75 C 0.74376(18) 0.80207(14) -0.01880(12) 0.0173(4) Uani 1 1 d . U . . .
C76 C 0.67906(19) 0.87727(15) -0.03297(14) 0.0208(5) Uani 1 1 d . U . . .
H76 H 0.6116 0.9033 0.0032 0.025 Uiso 1 1 calc R U . . .
C77 C 0.7112(2) 0.91477(15) -0.09865(14) 0.0243(5) Uani 1 1 d . U . . .
C78 C 0.6358(2) 0.99312(19) -0.11083(19) 0.0397(7) Uani 1 1 d . U . . .
F4 F 0.67943(17) 1.03092(13) -0.16743(14) 0.0768(8) Uani 1 1 d . U . . .
F5 F 0.55640(18) 0.98351(14) -0.12399(15) 0.0707(7) Uani 1 1 d . U . . .
F6 F 0.58960(16) 1.04586(11) -0.04993(13) 0.0586(5) Uani 1 1 d . U . . .
C79 C 0.8089(2) 0.87951(16) -0.15207(14) 0.0277(6) Uani 1 1 d . U . . .
H79 H 0.8315 0.9057 -0.1962 0.033 Uiso 1 1 calc R U . . .
C80 C 0.8728(2) 0.80500(16) -0.13938(14) 0.0269(5) Uani 1 1 d . U . . .
C81 C 0.9759(3) 0.76251(19) -0.19754(16) 0.0430(8) Uani 1 1 d . U . . .
F1 F 0.97188(18) 0.70554(13) -0.24160(11) 0.0664(6) Uani 1 1 d . U . . .
F2 F 1.04868(15) 0.72111(15) -0.16919(12) 0.0711(7) Uani 1 1 d . U . . .
F3 F 1.01367(15) 0.81237(11) -0.24407(10) 0.0525(5) Uani 1 1 d . U . . .
C82 C 0.8410(2) 0.76667(15) -0.07459(13) 0.0218(5) Uani 1 1 d . U . . .
H82 H 0.8868 0.7150 -0.0681 0.026 Uiso 1 1 calc R U . . .
F16 F 1.11252(18) 0.70589(17) 0.00023(12) 0.0730(7) Uani 1 1 d . U . . .
F17 F 1.02652(14) 0.77969(10) 0.10431(12) 0.0440(4) Uani 1 1 d . U . . .
F18 F 1.13410(14) 0.65961(11) 0.10313(13) 0.0547(5) Uani 1 1 d . U . . .
F22 F 0.67712(15) 0.46288(10) -0.01454(10) 0.0431(4) Uani 1 1 d . U . . .
F23 F 0.60552(15) 0.50500(11) -0.09888(11) 0.0471(5) Uani 1 1 d . U . . .
F24 F 0.75709(12) 0.50860(9) -0.11513(8) 0.0308(3) Uani 1 1 d . U . . .
Fe1 Fe 0.30954(2) 0.45752(2) 0.40274(2) 0.01495(8) Uani 1 1 d . . . . .
N2 N 0.49160(14) 0.45936(12) 0.41566(10) 0.0166(4) Uani 1 1 d . . . . .
H2A H 0.5348 0.4690 0.4340 0.020 Uiso 1 1 calc R U . . .
N1 N 0.45442(15) 0.41757(12) 0.31874(10) 0.0163(4) Uani 1 1 d . . . . .
O1 O 0.36819(12) 0.48997(10) 0.52989(8) 0.0188(3) Uani 1 1 d . . . . .
O2 O 0.10190(13) 0.50854(12) 0.51549(9) 0.0279(4) Uani 1 1 d . . . . .
P1 P 0.27760(4) 0.59508(4) 0.38172(3) 0.01582(12) Uani 1 1 d . . . . .
P2 P 0.34094(5) 0.32793(4) 0.44139(3) 0.01704(13) Uani 1 1 d . . . . .
S1 S 0.24627(5) 0.45785(4) 0.30382(3) 0.01962(13) Uani 1 1 d . . . . .
B1 B 0.7035(2) 0.75666(16) 0.05741(14) 0.0174(5) Uani 1 1 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
C13 O1 1.226(3) . ?
C13 N2 1.395(3) . ?
C13 Fe1 1.961(2) . ?
C1 N1 1.354(3) . ?
C1 N2 1.365(3) . ?
C1 C2 1.396(3) . ?
C2 C3 1.366(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.394(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 H4 0.9500 . ?
C5 N1 1.375(3) . ?
C5 C6 1.499(3) . ?
C6 C11 1.405(3) . ?
C6 C7 1.406(4) . ?
C7 C8 1.382(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.380(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.375(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.401(3) . ?
C10 H10 0.9500 . ?
C11 S1 1.762(3) . ?
C12 S1 1.807(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C14 O2 1.162(3) . ?
C14 Fe1 1.742(2) . ?
C15 C16 1.382(3) . ?
C15 C20 1.396(3) . ?
C15 H15 0.9500 . ?
C16 C17 1.379(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.388(4) . ?
C17 H17 0.9500 . ?
C18 C19 1.391(3) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(3) . ?
C19 H19 0.9500 . ?
C20 P1 1.814(2) . ?
C21 C26 1.386(3) . ?
C21 C22 1.404(4) . ?
C21 P1 1.836(2) . ?
C22 C23 1.382(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 C25 1.377(4) . ?
C24 H24 0.9500 . ?
C25 C26 1.401(4) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C28 1.393(3) . ?
C27 C32 1.397(3) . ?
C27 P1 1.846(2) . ?
C28 C29 1.386(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.387(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.389(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.385(4) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.393(3) . ?
C33 C34 1.399(3) . ?
C33 P2 1.823(2) . ?
C34 C35 1.386(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.390(4) . ?
C35 H35 0.9500 . ?
C36 C37 1.375(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.387(4) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C40 1.382(4) . ?
C39 C44 1.402(4) . ?
C39 P2 1.849(2) . ?
C40 C41 1.404(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.380(4) . ?
C41 H41 0.9500 . ?
C42 C43 1.379(4) . ?
C42 H42 0.9500 . ?
C43 C44 1.391(3) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C50 1.389(4) . ?
C45 C46 1.397(3) . ?
C45 P2 1.837(2) . ?
C46 C47 1.390(3) . ?
C46 H46 0.9500 . ?
C47 C48 1.381(4) . ?
C47 H47 0.9500 . ?
C48 C49 1.381(4) . ?
C48 H48 0.9500 . ?
C49 C50 1.393(3) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.398(3) . ?
C51 C58 1.403(3) . ?
C51 B1 1.642(3) . ?
C52 C53 1.393(3) . ?
C52 H52 0.9500 . ?
C53 C55 1.386(4) . ?
C53 C54 1.491(4) . ?
C54 F19A 1.276(5) . ?
C54 F19 1.308(5) . ?
C54 F21 1.323(4) . ?
C54 F21A 1.354(5) . ?
C54 F20A 1.357(5) . ?
C54 F20 1.377(5) . ?
C55 C56 1.384(4) . ?
C55 H55 0.9500 . ?
C56 C58 1.397(3) . ?
C56 C57 1.490(4) . ?
C57 F24 1.342(3) . ?
C57 F22 1.343(3) . ?
C57 F23 1.346(3) . ?
C58 H58 0.9500 . ?
C59 C60 1.397(3) . ?
C59 C66 1.406(3) . ?
C59 B1 1.647(3) . ?
C60 C61 1.398(3) . ?
C60 H60 0.9500 . ?
C61 C63 1.381(4) . ?
C61 C62 1.497(3) . ?
C62 F14A 1.302(5) . ?
C62 F15 1.306(5) . ?
C62 F15A 1.323(5) . ?
C62 F14 1.330(5) . ?
C62 F13A 1.354(5) . ?
C62 F13 1.373(5) . ?
C63 C64 1.393(4) . ?
C63 H63 0.9500 . ?
C64 C66 1.383(3) . ?
C64 C65 1.497(4) . ?
C65 F16 1.330(4) . ?
C65 F17 1.336(3) . ?
C65 F18 1.337(3) . ?
C66 H66 0.9500 . ?
C67 C68 1.395(3) . ?
C67 C74 1.403(4) . ?
C67 B1 1.648(3) . ?
C68 C69 1.391(4) . ?
C68 H68 0.9500 . ?
C69 C71 1.381(5) . ?
C69 C70 1.500(4) . ?
C70 F11 1.332(5) . ?
C70 F10 1.345(4) . ?
C70 F12 1.353(4) . ?
C71 C72 1.374(4) . ?
C71 H71 0.9500 . ?
C72 C74 1.397(4) . ?
C72 C73 1.486(5) . ?
C73 F8 1.278(5) . ?
C73 F8A 1.279(5) . ?
C73 F9A 1.311(5) . ?
C73 F9 1.317(5) . ?
C73 F7 1.377(5) . ?
C73 F7A 1.378(5) . ?
C74 H74 0.9500 . ?
C75 C82 1.393(3) . ?
C75 C76 1.402(3) . ?
C75 B1 1.646(3) . ?
C76 C77 1.394(3) . ?
C76 H76 0.9500 . ?
C77 C79 1.378(4) . ?
C77 C78 1.493(4) . ?
C78 F4 1.329(3) . ?
C78 F5 1.330(4) . ?
C78 F6 1.337(4) . ?
C79 C80 1.379(4) . ?
C79 H79 0.9500 . ?
C80 C82 1.388(3) . ?
C80 C81 1.482(4) . ?
C81 F2 1.315(4) . ?
C81 F3 1.341(3) . ?
C81 F1 1.369(4) . ?
C82 H82 0.9500 . ?
Fe1 N1 2.0664(19) . ?
Fe1 P2 2.3041(7) . ?
Fe1 S1 2.3400(6) . ?
Fe1 P1 2.3505(7) . ?
N2 H2A 0.8800 . ?

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 C13 N2 116.80(19) . . ?
O1 C13 Fe1 133.84(17) . . ?
N2 C13 Fe1 109.29(14) . . ?
N1 C1 N2 115.22(19) . . ?
N1 C1 C2 124.2(2) . . ?
N2 C1 C2 120.6(2) . . ?
C3 C2 C1 118.1(2) . . ?
C3 C2 H2 120.9 . . ?
C1 C2 H2 120.9 . . ?
C2 C3 C4 119.0(2) . . ?
C2 C3 H3 120.5 . . ?
C4 C3 H3 120.5 . . ?
C5 C4 C3 120.5(2) . . ?
C5 C4 H4 119.7 . . ?
C3 C4 H4 119.7 . . ?
N1 C5 C4 120.6(2) . . ?
N1 C5 C6 121.47(19) . . ?
C4 C5 C6 117.5(2) . . ?
C11 C6 C7 117.4(2) . . ?
C11 C6 C5 125.6(2) . . ?
C7 C6 C5 116.9(2) . . ?
C8 C7 C6 121.8(3) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C9 C8 C7 119.5(3) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C10 C9 C8 120.7(2) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.7 . . ?
C9 C10 C11 120.1(3) . . ?
C9 C10 H10 120.0 . . ?
C11 C10 H10 120.0 . . ?
C10 C11 C6 120.5(2) . . ?
C10 C11 S1 122.2(2) . . ?
C6 C11 S1 117.16(18) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O2 C14 Fe1 175.9(2) . . ?
C16 C15 C20 120.4(2) . . ?
C16 C15 H15 119.8 . . ?
C20 C15 H15 119.8 . . ?
C17 C16 C15 120.1(2) . . ?
C17 C16 H16 119.9 . . ?
C15 C16 H16 119.9 . . ?
C16 C17 C18 120.3(2) . . ?
C16 C17 H17 119.9 . . ?
C18 C17 H17 119.9 . . ?
C17 C18 C19 120.0(2) . . ?
C17 C18 H18 120.0 . . ?
C19 C18 H18 120.0 . . ?
C18 C19 C20 119.8(2) . . ?
C18 C19 H19 120.1 . . ?
C20 C19 H19 120.1 . . ?
C15 C20 C19 119.3(2) . . ?
C15 C20 P1 118.93(17) . . ?
C19 C20 P1 121.46(17) . . ?
C26 C21 C22 119.0(2) . . ?
C26 C21 P1 123.38(19) . . ?
C22 C21 P1 117.28(18) . . ?
C23 C22 C21 120.7(2) . . ?
C23 C22 H22 119.6 . . ?
C21 C22 H22 119.6 . . ?
C22 C23 C24 120.0(3) . . ?
C22 C23 H23 120.0 . . ?
C24 C23 H23 120.0 . . ?
C25 C24 C23 119.6(2) . . ?
C25 C24 H24 120.2 . . ?
C23 C24 H24 120.2 . . ?
C24 C25 C26 120.9(2) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
C21 C26 C25 119.6(2) . . ?
C21 C26 H26 120.2 . . ?
C25 C26 H26 120.2 . . ?
C28 C27 C32 118.9(2) . . ?
C28 C27 P1 124.18(18) . . ?
C32 C27 P1 116.15(18) . . ?
C29 C28 C27 120.1(2) . . ?
C29 C28 H28 119.9 . . ?
C27 C28 H28 119.9 . . ?
C28 C29 C30 120.6(2) . . ?
C28 C29 H29 119.7 . . ?
C30 C29 H29 119.7 . . ?
C29 C30 C31 119.6(2) . . ?
C29 C30 H30 120.2 . . ?
C31 C30 H30 120.2 . . ?
C32 C31 C30 119.9(2) . . ?
C32 C31 H31 120.1 . . ?
C30 C31 H31 120.1 . . ?
C31 C32 C27 120.8(2) . . ?
C31 C32 H32 119.6 . . ?
C27 C32 H32 119.6 . . ?
C38 C33 C34 118.3(2) . . ?
C38 C33 P2 122.02(18) . . ?
C34 C33 P2 119.48(18) . . ?
C35 C34 C33 120.5(2) . . ?
C35 C34 H34 119.8 . . ?
C33 C34 H34 119.8 . . ?
C34 C35 C36 120.2(3) . . ?
C34 C35 H35 119.9 . . ?
C36 C35 H35 119.9 . . ?
C37 C36 C35 119.8(3) . . ?
C37 C36 H36 120.1 . . ?
C35 C36 H36 120.1 . . ?
C36 C37 C38 120.2(2) . . ?
C36 C37 H37 119.9 . . ?
C38 C37 H37 119.9 . . ?
C37 C38 C33 121.0(2) . . ?
C37 C38 H38 119.5 . . ?
C33 C38 H38 119.5 . . ?
C40 C39 C44 119.2(2) . . ?
C40 C39 P2 123.94(19) . . ?
C44 C39 P2 116.79(19) . . ?
C39 C40 C41 120.0(3) . . ?
C39 C40 H40 120.0 . . ?
C41 C40 H40 120.0 . . ?
C42 C41 C40 120.2(3) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C43 C42 C41 120.1(2) . . ?
C43 C42 H42 119.9 . . ?
C41 C42 H42 119.9 . . ?
C42 C43 C44 120.1(3) . . ?
C42 C43 H43 119.9 . . ?
C44 C43 H43 119.9 . . ?
C43 C44 C39 120.3(3) . . ?
C43 C44 H44 119.9 . . ?
C39 C44 H44 119.9 . . ?
C50 C45 C46 118.7(2) . . ?
C50 C45 P2 125.97(19) . . ?
C46 C45 P2 115.30(19) . . ?
C47 C46 C45 120.6(3) . . ?
C47 C46 H46 119.7 . . ?
C45 C46 H46 119.7 . . ?
C48 C47 C46 120.2(3) . . ?
C48 C47 H47 119.9 . . ?
C46 C47 H47 119.9 . . ?
C49 C48 C47 119.7(2) . . ?
C49 C48 H48 120.2 . . ?
C47 C48 H48 120.2 . . ?
C48 C49 C50 120.4(3) . . ?
C48 C49 H49 119.8 . . ?
C50 C49 H49 119.8 . . ?
C45 C50 C49 120.4(3) . . ?
C45 C50 H50 119.8 . . ?
C49 C50 H50 119.8 . . ?
C52 C51 C58 115.3(2) . . ?
C52 C51 B1 122.0(2) . . ?
C58 C51 B1 122.4(2) . . ?
C53 C52 C51 122.7(2) . . ?
C53 C52 H52 118.7 . . ?
C51 C52 H52 118.7 . . ?
C55 C53 C52 120.6(2) . . ?
C55 C53 C54 120.0(2) . . ?
C52 C53 C54 119.3(2) . . ?
F19 C54 F21 109.9(4) . . ?
F19A C54 F21A 106.9(5) . . ?
F19A C54 F20A 109.7(4) . . ?
F21A C54 F20A 101.7(4) . . ?
F19 C54 F20 104.1(4) . . ?
F21 C54 F20 101.9(3) . . ?
F19A C54 C53 116.2(5) . . ?
F19 C54 C53 115.0(5) . . ?
F21 C54 C53 113.9(3) . . ?
F21A C54 C53 110.6(5) . . ?
F20A C54 C53 110.8(4) . . ?
F20 C54 C53 110.8(4) . . ?
C56 C55 C53 118.3(2) . . ?
C56 C55 H55 120.9 . . ?
C53 C55 H55 120.9 . . ?
C55 C56 C58 120.6(2) . . ?
C55 C56 C57 119.9(2) . . ?
C58 C56 C57 119.4(2) . . ?
F24 C57 F22 106.8(2) . . ?
F24 C57 F23 106.3(2) . . ?
F22 C57 F23 105.9(2) . . ?
F24 C57 C56 112.9(2) . . ?
F22 C57 C56 111.7(2) . . ?
F23 C57 C56 112.9(2) . . ?
C56 C58 C51 122.4(2) . . ?
C56 C58 H58 118.8 . . ?
C51 C58 H58 118.8 . . ?
C60 C59 C66 115.0(2) . . ?
C60 C59 B1 126.8(2) . . ?
C66 C59 B1 118.1(2) . . ?
C59 C60 C61 122.4(2) . . ?
C59 C60 H60 118.8 . . ?
C61 C60 H60 118.8 . . ?
C63 C61 C60 121.1(2) . . ?
C63 C61 C62 119.6(2) . . ?
C60 C61 C62 119.3(2) . . ?
F14A C62 F15A 108.2(5) . . ?
F15 C62 F14 107.8(5) . . ?
F14A C62 F13A 106.8(4) . . ?
F15A C62 F13A 104.2(5) . . ?
F15 C62 F13 105.2(4) . . ?
F14 C62 F13 102.1(4) . . ?
F14A C62 C61 114.1(4) . . ?
F15 C62 C61 115.9(4) . . ?
F15A C62 C61 112.4(6) . . ?
F14 C62 C61 113.1(5) . . ?
F13A C62 C61 110.5(4) . . ?
F13 C62 C61 111.4(3) . . ?
C61 C63 C64 117.8(2) . . ?
C61 C63 H63 121.1 . . ?
C64 C63 H63 121.1 . . ?
C66 C64 C63 120.7(2) . . ?
C66 C64 C65 118.7(2) . . ?
C63 C64 C65 120.5(2) . . ?
F16 C65 F17 106.6(3) . . ?
F16 C65 F18 106.9(3) . . ?
F17 C65 F18 106.3(2) . . ?
F16 C65 C64 111.4(2) . . ?
F17 C65 C64 112.6(2) . . ?
F18 C65 C64 112.6(2) . . ?
C64 C66 C59 123.0(2) . . ?
C64 C66 H66 118.5 . . ?
C59 C66 H66 118.5 . . ?
C68 C67 C74 115.4(2) . . ?
C68 C67 B1 124.0(2) . . ?
C74 C67 B1 120.5(2) . . ?
C69 C68 C67 122.5(3) . . ?
C69 C68 H68 118.8 . . ?
C67 C68 H68 118.8 . . ?
C71 C69 C68 120.9(3) . . ?
C71 C69 C70 118.8(3) . . ?
C68 C69 C70 120.3(3) . . ?
F11 C70 F10 107.1(4) . . ?
F11 C70 F12 106.2(3) . . ?
F10 C70 F12 105.6(3) . . ?
F11 C70 C69 113.9(3) . . ?
F10 C70 C69 111.6(3) . . ?
F12 C70 C69 112.0(4) . . ?
C72 C71 C69 118.2(3) . . ?
C72 C71 H71 120.9 . . ?
C69 C71 H71 120.9 . . ?
C71 C72 C74 120.9(3) . . ?
C71 C72 C73 119.2(3) . . ?
C74 C72 C73 119.9(3) . . ?
F8A C73 F9A 108.6(5) . . ?
F8 C73 F9 110.2(4) . . ?
F8 C73 F7 103.8(4) . . ?
F9 C73 F7 100.3(4) . . ?
F8A C73 F7A 102.7(4) . . ?
F9A C73 F7A 103.2(5) . . ?
F8 C73 C72 115.9(4) . . ?
F8A C73 C72 116.7(5) . . ?
F9A C73 C72 116.2(4) . . ?
F9 C73 C72 113.4(5) . . ?
F7 C73 C72 111.6(3) . . ?
F7A C73 C72 107.7(4) . . ?
C72 C74 C67 122.1(3) . . ?
C72 C74 H74 118.9 . . ?
C67 C74 H74 118.9 . . ?
C82 C75 C76 116.1(2) . . ?
C82 C75 B1 122.4(2) . . ?
C76 C75 B1 121.4(2) . . ?
C77 C76 C75 121.7(2) . . ?
C77 C76 H76 119.1 . . ?
C75 C76 H76 119.1 . . ?
C79 C77 C76 121.0(2) . . ?
C79 C77 C78 120.7(2) . . ?
C76 C77 C78 118.3(2) . . ?
F4 C78 F5 107.8(3) . . ?
F4 C78 F6 106.4(3) . . ?
F5 C78 F6 103.8(3) . . ?
F4 C78 C77 113.4(3) . . ?
F5 C78 C77 112.1(3) . . ?
F6 C78 C77 112.7(2) . . ?
C77 C79 C80 117.9(2) . . ?
C77 C79 H79 121.1 . . ?
C80 C79 H79 121.1 . . ?
C79 C80 C82 121.5(2) . . ?
C79 C80 C81 119.7(2) . . ?
C82 C80 C81 118.7(2) . . ?
F2 C81 F3 106.3(3) . . ?
F2 C81 F1 104.0(3) . . ?
F3 C81 F1 107.2(2) . . ?
F2 C81 C80 113.5(2) . . ?
F3 C81 C80 113.5(3) . . ?
F1 C81 C80 111.6(3) . . ?
C80 C82 C75 121.7(2) . . ?
C80 C82 H82 119.2 . . ?
C75 C82 H82 119.2 . . ?
C14 Fe1 C13 98.82(10) . . ?
C14 Fe1 N1 178.03(9) . . ?
C13 Fe1 N1 82.75(8) . . ?
C14 Fe1 P2 89.10(8) . . ?
C13 Fe1 P2 87.21(7) . . ?
N1 Fe1 P2 89.78(6) . . ?
C14 Fe1 S1 94.36(8) . . ?
C13 Fe1 S1 162.74(6) . . ?
N1 Fe1 S1 84.33(5) . . ?
P2 Fe1 S1 104.17(2) . . ?
C14 Fe1 P1 87.36(8) . . ?
C13 Fe1 P1 85.26(7) . . ?
N1 Fe1 P1 93.97(6) . . ?
P2 Fe1 P1 171.09(2) . . ?
S1 Fe1 P1 84.26(2) . . ?
C1 N2 C13 121.08(18) . . ?
C1 N2 H2A 119.5 . . ?
C13 N2 H2A 119.5 . . ?
C1 N1 C5 116.87(19) . . ?
C1 N1 Fe1 110.32(14) . . ?
C5 N1 Fe1 132.73(15) . . ?
C20 P1 C21 103.87(10) . . ?
C20 P1 C27 106.71(10) . . ?
C21 P1 C27 95.13(11) . . ?
C20 P1 Fe1 111.88(8) . . ?
C21 P1 Fe1 120.02(8) . . ?
C27 P1 Fe1 117.13(8) . . ?
C33 P2 C45 107.73(11) . . ?
C33 P2 C39 101.43(11) . . ?
C45 P2 C39 98.82(10) . . ?
C33 P2 Fe1 112.74(8) . . ?
C45 P2 Fe1 115.79(8) . . ?
C39 P2 Fe1 118.50(9) . . ?
C11 S1 C12 103.30(13) . . ?
C11 S1 Fe1 109.63(8) . . ?
C12 S1 Fe1 118.38(9) . . ?
C51 B1 C75 104.79(18) . . ?
C51 B1 C59 114.47(19) . . ?
C75 B1 C59 108.69(18) . . ?
C51 B1 C67 113.01(19) . . ?
C75 B1 C67 110.31(19) . . ?
C59 B1 C67 105.56(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.9(4) . . . . ?
N2 C1 C2 C3 -179.3(2) . . . . ?
C1 C2 C3 C4 -4.7(4) . . . . ?
C2 C3 C4 C5 0.3(4) . . . . ?
C3 C4 C5 N1 7.3(4) . . . . ?
C3 C4 C5 C6 -165.3(2) . . . . ?
N1 C5 C6 C11 36.2(3) . . . . ?
C4 C5 C6 C11 -151.3(2) . . . . ?
N1 C5 C6 C7 -140.5(2) . . . . ?
C4 C5 C6 C7 32.0(3) . . . . ?
C11 C6 C7 C8 1.9(4) . . . . ?
C5 C6 C7 C8 178.9(2) . . . . ?
C6 C7 C8 C9 -0.3(4) . . . . ?
C7 C8 C9 C10 -1.0(4) . . . . ?
C8 C9 C10 C11 0.7(4) . . . . ?
C9 C10 C11 C6 1.0(4) . . . . ?
C9 C10 C11 S1 176.59(19) . . . . ?
C7 C6 C11 C10 -2.2(3) . . . . ?
C5 C6 C11 C10 -178.9(2) . . . . ?
C7 C6 C11 S1 -178.00(17) . . . . ?
C5 C6 C11 S1 5.3(3) . . . . ?
C20 C15 C16 C17 1.2(4) . . . . ?
C15 C16 C17 C18 -1.3(4) . . . . ?
C16 C17 C18 C19 -0.4(4) . . . . ?
C17 C18 C19 C20 2.1(4) . . . . ?
C16 C15 C20 C19 0.5(4) . . . . ?
C16 C15 C20 P1 173.91(19) . . . . ?
C18 C19 C20 C15 -2.1(4) . . . . ?
C18 C19 C20 P1 -175.37(19) . . . . ?
C26 C21 C22 C23 -2.4(4) . . . . ?
P1 C21 C22 C23 171.30(19) . . . . ?
C21 C22 C23 C24 1.1(4) . . . . ?
C22 C23 C24 C25 1.2(4) . . . . ?
C23 C24 C25 C26 -2.2(4) . . . . ?
C22 C21 C26 C25 1.4(3) . . . . ?
P1 C21 C26 C25 -171.89(18) . . . . ?
C24 C25 C26 C21 0.9(4) . . . . ?
C32 C27 C28 C29 -0.8(4) . . . . ?
P1 C27 C28 C29 -170.3(2) . . . . ?
C27 C28 C29 C30 -0.9(5) . . . . ?
C28 C29 C30 C31 1.8(5) . . . . ?
C29 C30 C31 C32 -0.8(5) . . . . ?
C30 C31 C32 C27 -0.9(4) . . . . ?
C28 C27 C32 C31 1.8(4) . . . . ?
P1 C27 C32 C31 172.1(2) . . . . ?
C38 C33 C34 C35 -0.1(4) . . . . ?
P2 C33 C34 C35 -174.9(2) . . . . ?
C33 C34 C35 C36 -0.6(5) . . . . ?
C34 C35 C36 C37 0.7(5) . . . . ?
C35 C36 C37 C38 -0.2(5) . . . . ?
C36 C37 C38 C33 -0.5(4) . . . . ?
C34 C33 C38 C37 0.6(4) . . . . ?
P2 C33 C38 C37 175.3(2) . . . . ?
C44 C39 C40 C41 -0.8(3) . . . . ?
P2 C39 C40 C41 -179.20(18) . . . . ?
C39 C40 C41 C42 2.2(4) . . . . ?
C40 C41 C42 C43 -1.5(4) . . . . ?
C41 C42 C43 C44 -0.4(4) . . . . ?
C42 C43 C44 C39 1.8(4) . . . . ?
C40 C39 C44 C43 -1.1(4) . . . . ?
P2 C39 C44 C43 177.35(19) . . . . ?
C50 C45 C46 C47 -1.1(4) . . . . ?
P2 C45 C46 C47 -178.6(2) . . . . ?
C45 C46 C47 C48 -0.4(4) . . . . ?
C46 C47 C48 C49 1.1(4) . . . . ?
C47 C48 C49 C50 -0.4(4) . . . . ?
C46 C45 C50 C49 1.8(4) . . . . ?
P2 C45 C50 C49 179.1(2) . . . . ?
C48 C49 C50 C45 -1.1(4) . . . . ?
C58 C51 C52 C53 3.5(3) . . . . ?
B1 C51 C52 C53 177.1(2) . . . . ?
C51 C52 C53 C55 -0.7(4) . . . . ?
C51 C52 C53 C54 -178.8(2) . . . . ?
C55 C53 C54 F19A 116.4(5) . . . . ?
C52 C53 C54 F19A -65.4(5) . . . . ?
C55 C53 C54 F19 -100.5(4) . . . . ?
C52 C53 C54 F19 77.7(5) . . . . ?
C55 C53 C54 F21 27.6(4) . . . . ?
C52 C53 C54 F21 -154.3(4) . . . . ?
C55 C53 C54 F21A -121.5(5) . . . . ?
C52 C53 C54 F21A 56.6(5) . . . . ?
C55 C53 C54 F20A -9.6(5) . . . . ?
C52 C53 C54 F20A 168.5(4) . . . . ?
C55 C53 C54 F20 141.8(3) . . . . ?
C52 C53 C54 F20 -40.1(4) . . . . ?
C52 C53 C55 C56 -2.1(4) . . . . ?
C54 C53 C55 C56 176.0(2) . . . . ?
C53 C55 C56 C58 2.0(4) . . . . ?
C53 C55 C56 C57 178.7(2) . . . . ?
C55 C56 C57 F24 143.6(2) . . . . ?
C58 C56 C57 F24 -39.7(3) . . . . ?
C55 C56 C57 F22 -96.1(3) . . . . ?
C58 C56 C57 F22 80.6(3) . . . . ?
C55 C56 C57 F23 23.1(3) . . . . ?
C58 C56 C57 F23 -160.2(2) . . . . ?
C55 C56 C58 C51 0.9(3) . . . . ?
C57 C56 C58 C51 -175.8(2) . . . . ?
C52 C51 C58 C56 -3.5(3) . . . . ?
B1 C51 C58 C56 -177.1(2) . . . . ?
C66 C59 C60 C61 0.5(3) . . . . ?
B1 C59 C60 C61 -178.6(2) . . . . ?
C59 C60 C61 C63 -1.7(4) . . . . ?
C59 C60 C61 C62 179.5(2) . . . . ?
C63 C61 C62 F14A -108.6(4) . . . . ?
C60 C61 C62 F14A 70.2(4) . . . . ?
C63 C61 C62 F15 -17.2(4) . . . . ?
C60 C61 C62 F15 161.6(4) . . . . ?
C63 C61 C62 F15A 127.6(4) . . . . ?
C60 C61 C62 F15A -53.5(5) . . . . ?
C63 C61 C62 F14 108.1(4) . . . . ?
C60 C61 C62 F14 -73.1(4) . . . . ?
C63 C61 C62 F13A 11.7(4) . . . . ?
C60 C61 C62 F13A -169.5(4) . . . . ?
C63 C61 C62 F13 -137.5(3) . . . . ?
C60 C61 C62 F13 41.3(4) . . . . ?
C60 C61 C63 C64 1.1(4) . . . . ?
C62 C61 C63 C64 179.9(2) . . . . ?
C61 C63 C64 C66 0.6(4) . . . . ?
C61 C63 C64 C65 -175.6(2) . . . . ?
C66 C64 C65 F16 -73.5(3) . . . . ?
C63 C64 C65 F16 102.7(3) . . . . ?
C66 C64 C65 F17 46.2(3) . . . . ?
C63 C64 C65 F17 -137.5(3) . . . . ?
C66 C64 C65 F18 166.3(2) . . . . ?
C63 C64 C65 F18 -17.4(4) . . . . ?
C63 C64 C66 C59 -1.9(4) . . . . ?
C65 C64 C66 C59 174.4(2) . . . . ?
C60 C59 C66 C64 1.3(3) . . . . ?
B1 C59 C66 C64 -179.5(2) . . . . ?
C74 C67 C68 C69 1.2(4) . . . . ?
B1 C67 C68 C69 177.5(2) . . . . ?
C67 C68 C69 C71 -2.1(4) . . . . ?
C67 C68 C69 C70 177.0(3) . . . . ?
C71 C69 C70 F11 161.1(3) . . . . ?
C68 C69 C70 F11 -18.0(4) . . . . ?
C71 C69 C70 F10 39.7(5) . . . . ?
C68 C69 C70 F10 -139.5(3) . . . . ?
C71 C69 C70 F12 -78.4(3) . . . . ?
C68 C69 C70 F12 102.5(4) . . . . ?
C68 C69 C71 C72 1.0(4) . . . . ?
C70 C69 C71 C72 -178.1(3) . . . . ?
C69 C71 C72 C74 0.6(4) . . . . ?
C69 C71 C72 C73 179.5(3) . . . . ?
C71 C72 C73 F8 103.2(5) . . . . ?
C74 C72 C73 F8 -78.0(5) . . . . ?
C71 C72 C73 F8A -57.6(6) . . . . ?
C74 C72 C73 F8A 121.3(5) . . . . ?
C71 C72 C73 F9A 172.2(6) . . . . ?
C74 C72 C73 F9A -8.9(7) . . . . ?
C71 C72 C73 F9 -25.8(6) . . . . ?
C74 C72 C73 F9 153.0(5) . . . . ?
C71 C72 C73 F7 -138.3(4) . . . . ?
C74 C72 C73 F7 40.5(5) . . . . ?
C71 C72 C73 F7A 57.2(5) . . . . ?
C74 C72 C73 F7A -124.0(5) . . . . ?
C71 C72 C74 C67 -1.4(4) . . . . ?
C73 C72 C74 C67 179.7(3) . . . . ?
C68 C67 C74 C72 0.5(4) . . . . ?
B1 C67 C74 C72 -176.0(2) . . . . ?
C82 C75 C76 C77 -0.9(3) . . . . ?
B1 C75 C76 C77 -177.7(2) . . . . ?
C75 C76 C77 C79 -0.8(4) . . . . ?
C75 C76 C77 C78 177.5(2) . . . . ?
C79 C77 C78 F4 -13.2(4) . . . . ?
C76 C77 C78 F4 168.5(3) . . . . ?
C79 C77 C78 F5 109.1(3) . . . . ?
C76 C77 C78 F5 -69.1(4) . . . . ?
C79 C77 C78 F6 -134.2(3) . . . . ?
C76 C77 C78 F6 47.5(4) . . . . ?
C76 C77 C79 C80 1.6(4) . . . . ?
C78 C77 C79 C80 -176.6(3) . . . . ?
C77 C79 C80 C82 -0.8(4) . . . . ?
C77 C79 C80 C81 176.2(3) . . . . ?
C79 C80 C81 F2 145.1(3) . . . . ?
C82 C80 C81 F2 -37.9(4) . . . . ?
C79 C80 C81 F3 23.5(4) . . . . ?
C82 C80 C81 F3 -159.5(3) . . . . ?
C79 C80 C81 F1 -97.7(3) . . . . ?
C82 C80 C81 F1 79.3(3) . . . . ?
C79 C80 C82 C75 -1.0(4) . . . . ?
C81 C80 C82 C75 -177.9(3) . . . . ?
C76 C75 C82 C80 1.8(4) . . . . ?
B1 C75 C82 C80 178.5(2) . . . . ?
N1 C1 N2 C13 -2.0(3) . . . . ?
C2 C1 N2 C13 179.1(2) . . . . ?
O1 C13 N2 C1 175.8(2) . . . . ?
Fe1 C13 N2 C1 -6.9(3) . . . . ?
N2 C1 N1 C5 -173.5(2) . . . . ?
C2 C1 N1 C5 5.3(3) . . . . ?
N2 C1 N1 Fe1 9.4(2) . . . . ?
C2 C1 N1 Fe1 -171.77(19) . . . . ?
C4 C5 N1 C1 -9.8(3) . . . . ?
C6 C5 N1 C1 162.5(2) . . . . ?
C4 C5 N1 Fe1 166.49(18) . . . . ?
C6 C5 N1 Fe1 -21.2(3) . . . . ?
C52 C51 B1 C75 -90.7(2) . . . . ?
C58 C51 B1 C75 82.5(2) . . . . ?
C52 C51 B1 C59 150.3(2) . . . . ?
C58 C51 B1 C59 -36.5(3) . . . . ?
C52 C51 B1 C67 29.4(3) . . . . ?
C58 C51 B1 C67 -157.4(2) . . . . ?
C82 C75 B1 C51 -96.7(2) . . . . ?
C76 C75 B1 C51 79.8(3) . . . . ?
C82 C75 B1 C59 26.1(3) . . . . ?
C76 C75 B1 C59 -157.4(2) . . . . ?
C82 C75 B1 C67 141.4(2) . . . . ?
C76 C75 B1 C67 -42.1(3) . . . . ?
C60 C59 B1 C51 -17.9(3) . . . . ?
C66 C59 B1 C51 162.98(19) . . . . ?
C60 C59 B1 C75 -134.7(2) . . . . ?
C66 C59 B1 C75 46.2(3) . . . . ?
C60 C59 B1 C67 107.0(2) . . . . ?
C66 C59 B1 C67 -72.1(2) . . . . ?
C68 C67 B1 C51 29.4(3) . . . . ?
C74 C67 B1 C51 -154.5(2) . . . . ?
C68 C67 B1 C75 146.3(2) . . . . ?
C74 C67 B1 C75 -37.6(3) . . . . ?
C68 C67 B1 C59 -96.4(3) . . . . ?
C74 C67 B1 C59 79.7(3) . . . . ?

_refine_diff_density_max         0.977
_refine_diff_density_min         -0.674
_refine_diff_density_rms         0.072

_shelxl_version_number           2013-4


####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1547030'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H11 Br Fe N2 O3 S'
_chemical_formula_sum            'C15 H11 Br Fe N2 O3 S'
_chemical_formula_weight         435.08

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   9.7866(12)
_cell_length_b                   16.118(3)
_cell_length_c                   10.6175(17)
_cell_angle_alpha                90
_cell_angle_beta                 102.420(13)
_cell_angle_gamma                90
_cell_volume                     1635.6(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    153(2)
_cell_measurement_reflns_used    5748
_cell_measurement_theta_min      5.0340
_cell_measurement_theta_max      73.7800

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    11.588
_shelx_estimated_absorpt_T_min   0.390
_shelx_estimated_absorpt_T_max   0.654
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.11798
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 (release 14-01-2014 CrysAlis171 .NET)
(compiled Jan 14 2014,18:38:05)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      153(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'microfocus sealed tube'
_diffrn_measurement_device_type  'Agilent SuperNova Dual with AtlasS2 detector'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            5602
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_av_R_equivalents  0.0675
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         5.072
_diffrn_reflns_theta_max         74.141
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.993
_reflns_number_total             3186
_reflns_number_gt                2122
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _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       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_cell_refinement       
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction        
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_structure_solution    
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'

_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)+(0.0784P)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         3186
_refine_ls_number_parameters     209
_refine_ls_number_restraints     138
_refine_ls_R_factor_all          0.1093
_refine_ls_R_factor_gt           0.0690
_refine_ls_wR_factor_ref         0.1863
_refine_ls_wR_factor_gt          0.1577
_refine_ls_goodness_of_fit_ref   1.014
_refine_ls_restrained_S_all      1.006
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.9862(8) 0.0893(5) 0.2577(7) 0.0292(17) Uani 1 1 d . U . . .
C2 C 0.8486(10) 0.1113(6) 0.2619(9) 0.041(2) Uani 1 1 d . U . . .
H2 H 0.7723 0.0977 0.1933 0.049 Uiso 1 1 calc R U . . .
C3 C 0.8288(11) 0.1530(7) 0.3686(9) 0.046(2) Uani 1 1 d . U . . .
H3 H 0.7379 0.1718 0.3726 0.055 Uiso 1 1 calc R U . . .
C4 C 0.9396(10) 0.1680(6) 0.4704(8) 0.041(2) Uani 1 1 d . U . . .
H4 H 0.9245 0.1965 0.5445 0.049 Uiso 1 1 calc R U . . .
C5 C 1.0707(10) 0.1420(5) 0.4649(8) 0.0321(18) Uani 1 1 d . U . . .
C6 C 1.1858(10) 0.1419(5) 0.5825(7) 0.035(2) Uani 1 1 d . U . . .
C7 C 1.1473(12) 0.1202(6) 0.7000(8) 0.043(2) Uani 1 1 d . U . . .
H7 H 1.0522 0.1081 0.6995 0.052 Uiso 1 1 calc R U . . .
C8 C 1.2454(13) 0.1161(7) 0.8148(9) 0.055(3) Uani 1 1 d . U . . .
H8 H 1.2164 0.1038 0.8926 0.066 Uiso 1 1 calc R U . . .
C9 C 1.3847(13) 0.1297(7) 0.8174(8) 0.051(3) Uani 1 1 d . U . . .
H9 H 1.4520 0.1252 0.8962 0.061 Uiso 1 1 calc R U . . .
C10 C 1.4268(11) 0.1502(6) 0.7045(8) 0.045(2) Uani 1 1 d . U . . .
H10 H 1.5228 0.1603 0.7059 0.054 Uiso 1 1 calc R U . . .
C11 C 1.3280(10) 0.1558(6) 0.5897(7) 0.038(2) Uani 1 1 d . U . . .
C12 C 1.3309(11) 0.2901(6) 0.4301(8) 0.042(2) Uani 1 1 d . U . . .
H12A H 1.3630 0.3158 0.3579 0.063 Uiso 1 1 calc R U . . .
H12B H 1.3671 0.3216 0.5091 0.063 Uiso 1 1 calc R U . . .
H12C H 1.2284 0.2901 0.4120 0.063 Uiso 1 1 calc R U . . .
C13 C 1.1571(7) 0.0324(5) 0.1547(7) 0.0237(16) Uani 1 1 d . U . . .
C14 C 1.3172(8) 0.0019(7) 0.3908(7) 0.0329(19) Uani 1 1 d . U . . .
C15 C 1.4232(9) 0.0791(6) 0.2183(8) 0.036(2) Uani 1 1 d . U . . .
N1 N 1.0972(7) 0.1093(4) 0.3525(6) 0.0269(14) Uani 1 1 d . U . . .
N2 N 1.0199(7) 0.0456(4) 0.1588(6) 0.0275(14) Uani 1 1 d . U . . .
H2A H 0.9531 0.0257 0.0972 0.033 Uiso 1 1 calc R U . . .
S1 S 1.3944(2) 0.18411(14) 0.45069(17) 0.0321(5) Uani 1 1 d . U . . .
O1 O 1.1875(6) -0.0094(4) 0.0687(5) 0.0326(13) Uani 1 1 d . U . . .
O2 O 1.3419(8) -0.0523(5) 0.4484(7) 0.0510(18) Uani 1 1 d . U . . .
O3 O 1.5105(7) 0.0705(5) 0.1670(6) 0.0478(17) Uani 1 1 d . U . . .
Br1 Br 1.21404(10) 0.20907(6) 0.13940(8) 0.0351(3) Uani 1 1 d . U . . .
Fe1 Fe 1.27626(12) 0.09397(8) 0.29280(10) 0.0243(3) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.352(10) . ?
C1 N2 1.363(10) . ?
C1 C2 1.402(12) . ?
C2 C3 1.367(14) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.363(13) . ?
C4 H4 0.9500 . ?
C5 N1 1.379(10) . ?
C5 C6 1.491(11) . ?
C6 C11 1.396(14) . ?
C6 C7 1.422(12) . ?
C7 C8 1.381(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.376(17) . ?
C8 H8 0.9500 . ?
C9 C10 1.388(14) . ?
C9 H9 0.9500 . ?
C10 C11 1.386(12) . ?
C10 H10 0.9500 . ?
C11 S1 1.794(9) . ?
C12 S1 1.815(10) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O1 1.222(10) . ?
C13 N2 1.369(10) . ?
C13 Fe1 1.939(7) . ?
C14 O2 1.064(12) . ?
C14 Fe1 1.808(10) . ?
C15 O3 1.116(11) . ?
C15 Fe1 1.800(10) . ?
N1 Fe1 2.003(7) . ?
N2 H2A 0.8800 . ?
S1 Fe1 2.329(2) . ?
Br1 Fe1 2.4573(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
N1 C1 N2 114.1(7) . . ?
N1 C1 C2 122.7(8) . . ?
N2 C1 C2 123.3(7) . . ?
C3 C2 C1 117.3(9) . . ?
C3 C2 H2 121.3 . . ?
C1 C2 H2 121.3 . . ?
C2 C3 C4 120.6(9) . . ?
C2 C3 H3 119.7 . . ?
C4 C3 H3 119.7 . . ?
C5 C4 C3 120.1(8) . . ?
C5 C4 H4 120.0 . . ?
C3 C4 H4 120.0 . . ?
C4 C5 N1 120.6(8) . . ?
C4 C5 C6 120.9(8) . . ?
N1 C5 C6 118.4(8) . . ?
C11 C6 C7 116.1(8) . . ?
C11 C6 C5 127.6(8) . . ?
C7 C6 C5 116.1(9) . . ?
C8 C7 C6 121.4(10) . . ?
C8 C7 H7 119.3 . . ?
C6 C7 H7 119.3 . . ?
C9 C8 C7 120.5(9) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 119.8(9) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
C11 C10 C9 119.6(10) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C6 122.4(9) . . ?
C10 C11 S1 115.6(8) . . ?
C6 C11 S1 121.9(6) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 N2 120.5(7) . . ?
O1 C13 Fe1 130.1(6) . . ?
N2 C13 Fe1 109.3(5) . . ?
O2 C14 Fe1 179.7(9) . . ?
O3 C15 Fe1 176.9(7) . . ?
C1 N1 C5 117.7(7) . . ?
C1 N1 Fe1 110.7(5) . . ?
C5 N1 Fe1 131.4(6) . . ?
C1 N2 C13 120.4(6) . . ?
C1 N2 H2A 119.8 . . ?
C13 N2 H2A 119.8 . . ?
C11 S1 C12 99.4(4) . . ?
C11 S1 Fe1 102.8(3) . . ?
C12 S1 Fe1 113.3(3) . . ?
C15 Fe1 C14 92.6(4) . . ?
C15 Fe1 C13 90.4(4) . . ?
C14 Fe1 C13 92.2(3) . . ?
C15 Fe1 N1 172.5(3) . . ?
C14 Fe1 N1 91.1(3) . . ?
C13 Fe1 N1 83.0(3) . . ?
C15 Fe1 S1 94.6(3) . . ?
C14 Fe1 S1 94.8(3) . . ?
C13 Fe1 S1 171.2(2) . . ?
N1 Fe1 S1 91.6(2) . . ?
C15 Fe1 Br1 85.2(3) . . ?
C14 Fe1 Br1 173.8(3) . . ?
C13 Fe1 Br1 82.1(2) . . ?
N1 Fe1 Br1 90.46(19) . . ?
S1 Fe1 Br1 91.15(7) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -1.4(13) . . . . ?
N2 C1 C2 C3 178.0(8) . . . . ?
C1 C2 C3 C4 -3.8(14) . . . . ?
C2 C3 C4 C5 0.7(15) . . . . ?
C3 C4 C5 N1 7.6(14) . . . . ?
C3 C4 C5 C6 -167.5(9) . . . . ?
C4 C5 C6 C11 -147.3(10) . . . . ?
N1 C5 C6 C11 37.5(13) . . . . ?
C4 C5 C6 C7 36.9(13) . . . . ?
N1 C5 C6 C7 -138.3(9) . . . . ?
C11 C6 C7 C8 2.3(14) . . . . ?
C5 C6 C7 C8 178.5(9) . . . . ?
C6 C7 C8 C9 -2.8(17) . . . . ?
C7 C8 C9 C10 2.0(17) . . . . ?
C8 C9 C10 C11 -0.7(16) . . . . ?
C9 C10 C11 C6 0.3(15) . . . . ?
C9 C10 C11 S1 179.1(8) . . . . ?
C7 C6 C11 C10 -1.0(14) . . . . ?
C5 C6 C11 C10 -176.8(9) . . . . ?
C7 C6 C11 S1 -179.8(7) . . . . ?
C5 C6 C11 S1 4.4(13) . . . . ?
N2 C1 N1 C5 -170.1(7) . . . . ?
C2 C1 N1 C5 9.3(12) . . . . ?
N2 C1 N1 Fe1 15.1(9) . . . . ?
C2 C1 N1 Fe1 -165.4(7) . . . . ?
C4 C5 N1 C1 -12.4(12) . . . . ?
C6 C5 N1 C1 162.8(8) . . . . ?
C4 C5 N1 Fe1 161.1(7) . . . . ?
C6 C5 N1 Fe1 -23.8(11) . . . . ?
N1 C1 N2 C13 -6.4(11) . . . . ?
C2 C1 N2 C13 174.1(8) . . . . ?
O1 C13 N2 C1 177.2(7) . . . . ?
Fe1 C13 N2 C1 -6.1(9) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C4 H4 Br1 0.95 2.91 3.704(9) 141.9 4_566
C10 H10 Br1 0.95 3.00 3.789(11) 141.3 4_666
C2 H2 O3 0.95 2.56 3.312(11) 136.8 1_455
C2 H2 O3 0.95 2.56 3.312(11) 136.8 1_455
C4 H4 Br1 0.95 2.91 3.704(9) 141.9 4_566
C10 H10 Br1 0.95 3.00 3.789(11) 141.3 4_666

_refine_diff_density_max         1.268
_refine_diff_density_min         -0.673
_refine_diff_density_rms         0.175

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_2d
_database_code_depnum_ccdc_archive 'CCDC 1547034'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2017-06-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C17 H14 B F4 Fe N3 O3 S'
_chemical_formula_sum            'C17 H14 B F4 Fe N3 O3 S'
_chemical_formula_weight         483.03

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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                   7.8618(7)
_cell_length_b                   13.0402(11)
_cell_length_c                   19.3301(15)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1981.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    8046
_cell_measurement_theta_min      1.5632
_cell_measurement_theta_max      31.1143

_exptl_crystal_description       HEXAGONAL
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_F_000             976
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.928
_shelx_estimated_absorpt_T_min   0.905
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   MULTI-SCAN
_exptl_absorpt_correction_T_min  0.9049
_exptl_absorpt_correction_T_max  0.9551
_exptl_absorpt_process_details   
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;


_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25929
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.026
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.974
_reflns_number_total             3499
_reflns_number_gt                3425
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.735
_reflns_Friedel_fraction_max     1.000
_reflns_Friedel_fraction_full    0.974

_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       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_molecular_graphics    'XL SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'BRUKER SHELXTL'

_refine_special_details          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0253P)²+0.7572P] 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 1442 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.014(5)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         3499
_refine_ls_number_parameters     273
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.0226
_refine_ls_R_factor_gt           0.0219
_refine_ls_wR_factor_ref         0.0542
_refine_ls_wR_factor_gt          0.0539
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.097
_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
C1 C 0.5543(3) 1.0618(2) 0.16314(13) 0.0143(5) Uani 1 1 d . U . . .
C2 C 0.5728(4) 1.1381(2) 0.21341(14) 0.0177(6) Uani 1 1 d . U . . .
H2 H 0.5302 1.1288 0.2590 0.021 Uiso 1 1 calc R U . . .
C3 C 0.6541(4) 1.2266(2) 0.19489(15) 0.0193(6) Uani 1 1 d . U . . .
H3 H 0.6756 1.2780 0.2286 0.023 Uiso 1 1 calc R U . . .
C4 C 0.7056(4) 1.2418(2) 0.12670(15) 0.0179(6) Uani 1 1 d . U . . .
H4 H 0.7598 1.3039 0.1135 0.022 Uiso 1 1 calc R U . . .
C5 C 0.6770(4) 1.1651(2) 0.07806(14) 0.0133(6) Uani 1 1 d . U . . .
C6 C 0.7002(4) 1.1887(2) 0.00288(14) 0.0137(6) Uani 1 1 d . U . . .
C7 C 0.6507(3) 1.2871(2) -0.01856(15) 0.0171(6) Uani 1 1 d . U . . .
H7 H 0.6077 1.3340 0.0147 0.020 Uiso 1 1 calc R U . . .
C8 C 0.6631(4) 1.3174(2) -0.08694(15) 0.0199(6) Uani 1 1 d . U . . .
H8 H 0.6288 1.3845 -0.1002 0.024 Uiso 1 1 calc R U . . .
C9 C 0.7252(4) 1.2502(2) -0.13569(15) 0.0213(6) Uani 1 1 d . U . . .
H9 H 0.7344 1.2710 -0.1826 0.026 Uiso 1 1 calc R U . . .
C10 C 0.7744(4) 1.1520(2) -0.11638(15) 0.0186(6) Uani 1 1 d . U . . .
H10 H 0.8174 1.1059 -0.1502 0.022 Uiso 1 1 calc R U . . .
C11 C 0.7610(3) 1.1206(2) -0.04751(16) 0.0147(5) Uani 1 1 d . U . . .
C12 C 0.8528(4) 0.9270(2) -0.10006(14) 0.0204(6) Uani 1 1 d . U . . .
H12A H 0.7477 0.9333 -0.1270 0.031 Uiso 1 1 calc R U . . .
H12B H 0.8740 0.8545 -0.0896 0.031 Uiso 1 1 calc R U . . .
H12C H 0.9482 0.9546 -0.1269 0.031 Uiso 1 1 calc R U . . .
C13 C 0.4604(4) 0.8972(2) 0.12427(15) 0.0162(6) Uani 1 1 d . U . . .
C14 C 0.4272(4) 0.9760(2) -0.00042(14) 0.0164(6) Uani 1 1 d . U . . .
C15 C 0.5971(4) 0.8114(2) 0.01087(14) 0.0191(6) Uani 1 1 d . U . . .
C16 C 0.8852(4) 0.8621(2) 0.15200(14) 0.0162(6) Uani 1 1 d . U . . .
C17 C 1.0065(4) 0.8247(2) 0.20269(16) 0.0219(7) Uani 1 1 d . U . . .
H17A H 1.1213 0.8270 0.1831 0.033 Uiso 1 1 calc R U . . .
H17B H 0.9782 0.7538 0.2151 0.033 Uiso 1 1 calc R U . . .
H17C H 1.0018 0.8679 0.2441 0.033 Uiso 1 1 calc R U . . .
B1 B 0.3354(5) 0.9543(3) -0.19335(18) 0.0232(7) Uani 1 1 d . U . . .
F1 F 0.2010(2) 1.02652(13) -0.19253(9) 0.0266(4) Uani 1 1 d . U . . .
F2 F 0.4754(3) 0.9965(2) -0.16191(10) 0.0444(5) Uani 1 1 d . U . . .
F3 F 0.2811(3) 0.86738(15) -0.15884(13) 0.0482(6) Uani 1 1 d . U . . .
F4 F 0.3721(3) 0.93189(15) -0.26192(9) 0.0378(5) Uani 1 1 d . U . . .
Fe1 Fe 0.61021(5) 0.93728(3) 0.04847(2) 0.01201(11) Uani 1 1 d . U . . .
N1 N 0.6130(3) 1.07250(16) 0.09804(11) 0.0130(4) Uani 1 1 d . U . . .
N2 N 0.4724(3) 0.97057(17) 0.17602(12) 0.0166(5) Uani 1 1 d . U . . .
H2A H 0.4277 0.9588 0.2170 0.020 Uiso 1 1 calc R U . . .
N3 N 0.7899(3) 0.89157(17) 0.11219(12) 0.0158(5) Uani 1 1 d . U . . .
O1 O 0.3771(3) 0.81967(14) 0.13337(10) 0.0217(5) Uani 1 1 d . U . . .
O2 O 0.3043(3) 0.99827(18) -0.02693(11) 0.0281(5) Uani 1 1 d . U . . .
O3 O 0.5822(3) 0.73174(15) -0.01215(11) 0.0302(5) Uani 1 1 d . U . . .
S1 S 0.83167(8) 0.99787(5) -0.02029(3) 0.01376(15) Uani 1 1 d . U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.348(3) . ?
C1 N2 1.376(4) . ?
C1 C2 1.398(4) . ?
C2 C3 1.367(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.393(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(4) . ?
C4 H4 0.9500 . ?
C5 N1 1.364(3) . ?
C5 C6 1.496(4) . ?
C6 C11 1.402(4) . ?
C6 C7 1.403(4) . ?
C7 C8 1.383(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.377(4) . ?
C8 H8 0.9500 . ?
C9 C10 1.389(4) . ?
C9 H9 0.9500 . ?
C10 C11 1.397(4) . ?
C10 H10 0.9500 . ?
C11 S1 1.774(3) . ?
C12 S1 1.806(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C13 O1 1.218(3) . ?
C13 N2 1.387(4) . ?
C13 Fe1 1.951(3) . ?
C14 O2 1.131(4) . ?
C14 Fe1 1.794(3) . ?
C15 O3 1.136(3) . ?
C15 Fe1 1.799(3) . ?
C16 N3 1.140(4) . ?
C16 C17 1.452(4) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
B1 F2 1.372(4) . ?
B1 F3 1.383(4) . ?
B1 F4 1.388(4) . ?
B1 F1 1.416(4) . ?
Fe1 N3 1.967(2) . ?
Fe1 N1 2.007(2) . ?
Fe1 S1 2.3285(8) . ?
N2 H2A 0.8800 . ?

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
N1 C1 N2 114.8(2) . . ?
N1 C1 C2 122.7(3) . . ?
N2 C1 C2 122.6(2) . . ?
C3 C2 C1 117.9(3) . . ?
C3 C2 H2 121.1 . . ?
C1 C2 H2 121.1 . . ?
C2 C3 C4 120.2(3) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.4(3) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
N1 C5 C4 120.3(3) . . ?
N1 C5 C6 120.1(2) . . ?
C4 C5 C6 119.3(2) . . ?
C11 C6 C7 117.9(3) . . ?
C11 C6 C5 125.9(3) . . ?
C7 C6 C5 116.2(3) . . ?
C8 C7 C6 121.6(3) . . ?
C8 C7 H7 119.2 . . ?
C6 C7 H7 119.2 . . ?
C9 C8 C7 119.8(3) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 120.1(3) . . ?
C8 C9 H9 119.9 . . ?
C10 C9 H9 119.9 . . ?
C9 C10 C11 120.3(3) . . ?
C9 C10 H10 119.8 . . ?
C11 C10 H10 119.8 . . ?
C10 C11 C6 120.2(3) . . ?
C10 C11 S1 121.6(2) . . ?
C6 C11 S1 118.2(2) . . ?
S1 C12 H12A 109.5 . . ?
S1 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
S1 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 N2 120.3(3) . . ?
O1 C13 Fe1 130.9(2) . . ?
N2 C13 Fe1 108.43(19) . . ?
O2 C14 Fe1 174.7(2) . . ?
O3 C15 Fe1 177.3(3) . . ?
N3 C16 C17 180.0(4) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
F2 B1 F3 111.2(3) . . ?
F2 B1 F4 109.9(3) . . ?
F3 B1 F4 110.6(3) . . ?
F2 B1 F1 109.1(3) . . ?
F3 B1 F1 108.0(3) . . ?
F4 B1 F1 107.8(3) . . ?
C14 Fe1 C15 89.88(13) . . ?
C14 Fe1 C13 89.24(12) . . ?
C15 Fe1 C13 91.41(12) . . ?
C14 Fe1 N3 172.44(11) . . ?
C15 Fe1 N3 91.01(12) . . ?
C13 Fe1 N3 83.23(11) . . ?
C14 Fe1 N1 90.76(11) . . ?
C15 Fe1 N1 174.66(11) . . ?
C13 Fe1 N1 83.30(10) . . ?
N3 Fe1 N1 87.67(9) . . ?
C14 Fe1 S1 101.75(9) . . ?
C15 Fe1 S1 97.00(10) . . ?
C13 Fe1 S1 166.12(9) . . ?
N3 Fe1 S1 85.59(7) . . ?
N1 Fe1 S1 88.05(7) . . ?
C1 N1 C5 118.8(2) . . ?
C1 N1 Fe1 110.56(17) . . ?
C5 N1 Fe1 130.31(18) . . ?
C1 N2 C13 119.8(2) . . ?
C1 N2 H2A 120.1 . . ?
C13 N2 H2A 120.1 . . ?
C16 N3 Fe1 175.1(2) . . ?
C11 S1 C12 103.74(14) . . ?
C11 S1 Fe1 103.97(9) . . ?
C12 S1 Fe1 112.49(10) . . ?

_refine_diff_density_max         0.339
_refine_diff_density_min         -0.163
_refine_diff_density_rms         0.047

_shelxl_version_number           2013-4

