# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
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data_ylee94
_database_code_depnum_ccdc_archive 'CCDC 1483321'
# end Validation Reply Form



_audit_update_record             
;
2016-06-03 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT413_ylee94              
;
PROBLEM: Short Inter XH3 .. XHn H20A .. H48C .. 1.38 Ang.
RESPONSE: Those protons are part of the 47% thf molecule
located on an inversion center.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        C45H63N6Br2S1Fe3
_chemical_name_common            n/a
_chemical_melting_point          n/a
_chemical_formula_moiety         ' C45 H63 Br2 Fe3 N6 S1, O1 C4 H8'
_chemical_formula_sum            'C49 H71 Br2 Fe3 N6 O S'
_chemical_formula_weight         1119.54

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.9958(6)
_cell_length_b                   12.5852(7)
_cell_length_c                   17.0913(9)
_cell_angle_alpha                104.6972(10)
_cell_angle_beta                 102.6921(10)
_cell_angle_gamma                91.2459(10)
_cell_volume                     2426.6(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9979
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0

_exptl_crystal_description       plates
_exptl_crystal_colour            green
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.532
_exptl_crystal_F_000             1158
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.176
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.041
_exptl_absorpt_coefficient_mu    2.618
_shelx_estimated_absorpt_T_min   0.656
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.7776
_exptl_absorpt_correction_T_max  0.9418
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            54540
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  0.0539
_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       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.678
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11145
_reflns_number_gt                7854
_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       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2014 (Bruker, 2014)'
_computing_structure_refinement  'SHELXTL-2014 (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL-2014 (Bruker, 2014)'
_computing_publication_material  'SHELXTL-2014 (Bruker, 2014)'
_refine_special_details          
; 
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and 
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C). 
Methyl ones were allowed to rotate around the corresponding C---C. 

The asymmetric unit consists of the Fe3 complex and a thf solvent molecule. The
 latter is disordered and is refined in two positions with their site occupation
 factors refined but fixed at 0.85/0.15 ration in the last refinement cycles. 
 The core of the complex molecule is also disordered with two configurations of
 the Fe and Br atoms.  They were refined with an occupation ratio of 0.95/0.05
 for the major and minor products respectively.  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0507P)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         11145
_refine_ls_number_parameters     603
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0660
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0918
_refine_ls_wR_factor_gt          0.0840
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_restrained_S_all      0.959
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.27568(3) 0.50337(4) 0.43617(2) 0.01949(8) Uani 0.95 1 d . . P A 1
Br2 Br 0.34454(3) 0.90198(3) 0.27698(2) 0.02888(10) Uani 0.95 1 d . . P B 1
Fe1 Fe 0.32346(4) 0.67868(4) 0.39925(3) 0.02019(11) Uani 0.95 1 d . . P A 1
Fe3 Fe 0.23509(4) 0.73559(4) 0.19210(3) 0.01826(11) Uani 0.95 1 d . . P B 1
Br1' Br 0.2877(15) 0.5412(14) 0.4322(12) 0.093(7) Uiso 0.05 1 d . . P A 2
Br2' Br 0.3398(5) 0.8601(5) 0.3070(4) 0.0170(12) Uiso 0.05 1 d . . P A 2
Fe1' Fe 0.3211(7) 0.7228(8) 0.3690(6) 0.0188(19) Uiso 0.05 1 d . . P A 2
Fe3' Fe 0.2034(17) 0.6783(17) 0.1830(13) 0.087(6) Uiso 0.05 1 d . . P A 2
Fe2 Fe 0.17609(3) 0.45090(3) 0.28476(3) 0.02030(11) Uani 1 1 d . . . . .
S1 S 0.22849(6) 0.61489(6) 0.26236(4) 0.01759(16) Uani 1 1 d . . . . .
N1 N 0.4943(2) 0.7070(2) 0.43430(15) 0.0200(5) Uani 1 1 d . . . . .
N2 N 0.27479(19) 0.81414(19) 0.47050(14) 0.0186(5) Uani 1 1 d . . . . .
N3 N 0.2196(2) 0.3061(2) 0.22315(14) 0.0199(5) Uani 1 1 d . . . . .
N4 N 0.01397(19) 0.39840(19) 0.27838(14) 0.0185(5) Uani 1 1 d . . . . .
N5 N 0.3035(2) 0.6855(2) 0.09390(15) 0.0199(5) Uani 1 1 d . . . . .
N6 N 0.08316(19) 0.76516(19) 0.13002(14) 0.0184(5) Uani 1 1 d . . . . .
C1 C 0.5738(2) 0.6327(3) 0.39634(18) 0.0230(7) Uani 1 1 d . . . . .
H1A H 0.6001 0.5816 0.4309 0.028 Uiso 1 1 calc R U . . .
H1B H 0.6419 0.6769 0.3944 0.028 Uiso 1 1 calc R U . . .
C2 C 0.5385(2) 0.7885(2) 0.50150(18) 0.0218(7) Uani 1 1 d . . . . .
C3 C 0.4745(3) 0.8671(2) 0.54267(19) 0.0263(7) Uani 1 1 d . . . . .
H3A H 0.5198 0.9207 0.5890 0.032 Uiso 1 1 calc R U . . .
C4 C 0.3564(3) 0.8818(2) 0.52873(19) 0.0230(7) Uani 1 1 d . . . . .
C5 C 0.1544(2) 0.8445(2) 0.46644(18) 0.0212(6) Uani 1 1 d . . . . .
H5A H 0.1501 0.9229 0.4660 0.025 Uiso 1 1 calc R U . . .
H5B H 0.1300 0.8352 0.5162 0.025 Uiso 1 1 calc R U . . .
C6 C 0.6665(2) 0.8005(3) 0.5392(2) 0.0285(7) Uani 1 1 d . . . . .
H6A H 0.6849 0.8637 0.5884 0.043 Uiso 1 1 calc R U . . .
H6B H 0.7079 0.8122 0.4982 0.043 Uiso 1 1 calc R U . . .
H6C H 0.6895 0.7334 0.5552 0.043 Uiso 1 1 calc R U . . .
C7 C 0.3233(3) 0.9815(3) 0.5867(2) 0.0427(10) Uani 1 1 d . . . . .
H7A H 0.3923 1.0216 0.6263 0.064 Uiso 1 1 calc R U . . .
H7B H 0.2713 0.9578 0.6171 0.064 Uiso 1 1 calc R U . . .
H7C H 0.2848 1.0299 0.5543 0.064 Uiso 1 1 calc R U . . .
C8 C 0.3320(2) 0.2953(2) 0.20024(19) 0.0227(7) Uani 1 1 d . . . . .
H8A H 0.3200 0.2555 0.1407 0.027 Uiso 1 1 calc R U . . .
H8B H 0.3798 0.2516 0.2334 0.027 Uiso 1 1 calc R U . . .
C9 C 0.1539(3) 0.2126(2) 0.20656(18) 0.0221(7) Uani 1 1 d . . . . .
C10 C 0.0436(3) 0.2074(3) 0.2223(2) 0.0260(7) Uani 1 1 d . . . . .
H10A H 0.0073 0.1351 0.2084 0.031 Uiso 1 1 calc R U . . .
C11 C -0.0212(2) 0.2918(2) 0.25509(18) 0.0210(6) Uani 1 1 d . . . . .
C12 C -0.0654(2) 0.4776(2) 0.3111(2) 0.0231(7) Uani 1 1 d . . . . .
H12A H -0.0677 0.4740 0.3679 0.028 Uiso 1 1 calc R U . . .
H12B H -0.1437 0.4572 0.2753 0.028 Uiso 1 1 calc R U . . .
C13 C 0.1965(3) 0.1034(2) 0.1687(2) 0.0298(8) Uani 1 1 d . . . . .
H13A H 0.1370 0.0439 0.1590 0.045 Uiso 1 1 calc R U . . .
H13B H 0.2657 0.0907 0.2068 0.045 Uiso 1 1 calc R U . . .
H13C H 0.2144 0.1050 0.1157 0.045 Uiso 1 1 calc R U . . .
C14 C -0.1378(3) 0.2549(3) 0.2638(2) 0.0297(8) Uani 1 1 d . . . . .
H14A H -0.1482 0.1741 0.2471 0.045 Uiso 1 1 calc R U . . .
H14B H -0.1976 0.2843 0.2280 0.045 Uiso 1 1 calc R U . . .
H14C H -0.1430 0.2822 0.3218 0.045 Uiso 1 1 calc R U . . .
C15 C 0.4080(2) 0.6239(3) 0.09644(19) 0.0239(7) Uani 1 1 d . . . . .
H15A H 0.4750 0.6757 0.1036 0.029 Uiso 1 1 calc R U . . .
H15B H 0.3996 0.5680 0.0426 0.029 Uiso 1 1 calc R U . . .
C16 C 0.2682(2) 0.7276(2) 0.02973(18) 0.0221(7) Uani 1 1 d . . . . .
C17 C 0.1683(3) 0.7837(3) 0.01771(19) 0.0233(7) Uani 1 1 d . . . . .
H17A H 0.1595 0.8186 -0.0262 0.028 Uiso 1 1 calc R U . . .
C18 C 0.0801(2) 0.7963(2) 0.05993(18) 0.0196(6) Uani 1 1 d . . . . .
C19 C -0.0245(2) 0.7680(3) 0.16005(18) 0.0227(7) Uani 1 1 d . . . . .
H19A H -0.0855 0.7186 0.1166 0.027 Uiso 1 1 calc R U . . .
H19B H -0.0493 0.8438 0.1697 0.027 Uiso 1 1 calc R U . . .
C20 C 0.3355(3) 0.7133(3) -0.0373(2) 0.0305(8) Uani 1 1 d . . . . .
H20A H 0.3018 0.7538 -0.0775 0.046 Uiso 1 1 calc R U . . .
H20B H 0.3327 0.6349 -0.0658 0.046 Uiso 1 1 calc R U . . .
H20C H 0.4154 0.7420 -0.0118 0.046 Uiso 1 1 calc R U . . .
C21 C -0.0260(3) 0.8444(3) 0.0207(2) 0.0260(7) Uani 1 1 d . . . . .
H21A H -0.0119 0.8689 -0.0266 0.039 Uiso 1 1 calc R U . . .
H21B H -0.0438 0.9074 0.0619 0.039 Uiso 1 1 calc R U . . .
H21C H -0.0908 0.7881 0.0014 0.039 Uiso 1 1 calc R U . . .
C22 C 0.5141(2) 0.5669(2) 0.30879(18) 0.0201(6) Uani 1 1 d . . . . .
C23 C 0.4667(2) 0.4586(2) 0.29407(18) 0.0196(6) Uani 1 1 d . . . . .
C24 C 0.3945(2) 0.4081(2) 0.21587(19) 0.0206(6) Uani 1 1 d . . . . .
C25 C 0.3729(2) 0.4631(2) 0.15294(17) 0.0192(6) Uani 1 1 d . . . . .
C26 C 0.4305(2) 0.5671(2) 0.16583(18) 0.0202(6) Uani 1 1 d . . . . .
C27 C 0.5010(2) 0.6187(2) 0.24386(18) 0.0194(6) Uani 1 1 d . . . . .
C28 C 0.5002(2) 0.3937(3) 0.35825(19) 0.0229(7) Uani 1 1 d . . . . .
H28A H 0.4378 0.3367 0.3510 0.027 Uiso 1 1 calc R U . . .
H28B H 0.5119 0.4438 0.4149 0.027 Uiso 1 1 calc R U . . .
C29 C 0.6112(3) 0.3387(3) 0.3481(2) 0.0283(7) Uani 1 1 d . . . . .
H29A H 0.6317 0.2960 0.3891 0.043 Uiso 1 1 calc R U . . .
H29B H 0.6733 0.3954 0.3569 0.043 Uiso 1 1 calc R U . . .
H29C H 0.5994 0.2895 0.2920 0.043 Uiso 1 1 calc R U . . .
C30 C 0.2868(2) 0.4123(3) 0.07175(18) 0.0224(7) Uani 1 1 d . . . . .
H30A H 0.2518 0.4720 0.0491 0.027 Uiso 1 1 calc R U . . .
H30B H 0.2249 0.3689 0.0827 0.027 Uiso 1 1 calc R U . . .
C31 C 0.3404(3) 0.3374(3) 0.00668(19) 0.0290(7) Uani 1 1 d . . . . .
H31A H 0.2808 0.3049 -0.0438 0.043 Uiso 1 1 calc R U . . .
H31B H 0.3759 0.2785 0.0290 0.043 Uiso 1 1 calc R U . . .
H31C H 0.3989 0.3808 -0.0067 0.043 Uiso 1 1 calc R U . . .
C32 C 0.5663(2) 0.7304(3) 0.2598(2) 0.0246(7) Uani 1 1 d . . . . .
H32A H 0.5680 0.7748 0.3170 0.029 Uiso 1 1 calc R U . . .
H32B H 0.5259 0.7705 0.2205 0.029 Uiso 1 1 calc R U . . .
C33 C 0.6898(3) 0.7171(3) 0.2494(2) 0.0354(8) Uani 1 1 d . . . . .
H33A H 0.7311 0.7899 0.2635 0.053 Uiso 1 1 calc R U . . .
H33B H 0.6882 0.6784 0.1916 0.053 Uiso 1 1 calc R U . . .
H33C H 0.7287 0.6744 0.2864 0.053 Uiso 1 1 calc R U . . .
C34 C 0.0746(2) 0.7719(2) 0.38822(18) 0.0178(6) Uani 1 1 d . . . . .
C35 C 0.0322(2) 0.6667(2) 0.38806(18) 0.0183(6) Uani 1 1 d . . . . .
C36 C -0.0269(2) 0.5935(2) 0.31316(18) 0.0186(6) Uani 1 1 d . . . . .
C37 C -0.0451(2) 0.6254(2) 0.23829(18) 0.0185(6) Uani 1 1 d . . . . .
C38 C -0.0089(2) 0.7324(2) 0.23995(17) 0.0182(6) Uani 1 1 d . . . . .
C39 C 0.0487(2) 0.8076(2) 0.31511(18) 0.0176(6) Uani 1 1 d . . . . .
C40 C 0.0416(3) 0.6386(3) 0.47099(19) 0.0233(7) Uani 1 1 d . . . . .
H40A H 0.0444 0.5581 0.4627 0.028 Uiso 1 1 calc R U . . .
H40B H 0.1133 0.6755 0.5106 0.028 Uiso 1 1 calc R U . . .
C41 C -0.0613(3) 0.6765(3) 0.50667(19) 0.0264(7) Uani 1 1 d . . . . .
H41A H -0.0530 0.6610 0.5609 0.040 Uiso 1 1 calc R U . . .
H41B H -0.1318 0.6370 0.4687 0.040 Uiso 1 1 calc R U . . .
H41C H -0.0652 0.7559 0.5133 0.040 Uiso 1 1 calc R U . . .
C42 C -0.1048(3) 0.5440(3) 0.15613(19) 0.0250(7) Uani 1 1 d . . . . .
H42A H -0.1628 0.5822 0.1250 0.030 Uiso 1 1 calc R U . . .
H42B H -0.1461 0.4836 0.1685 0.030 Uiso 1 1 calc R U . . .
C43 C -0.0259(3) 0.4932(3) 0.09980(19) 0.0274(7) Uani 1 1 d . . . . .
H43A H -0.0724 0.4502 0.0459 0.041 Uiso 1 1 calc R U . . .
H43B H 0.0238 0.4449 0.1259 0.041 Uiso 1 1 calc R U . . .
H43C H 0.0214 0.5520 0.0915 0.041 Uiso 1 1 calc R U . . .
C44 C 0.0756(3) 0.9279(2) 0.3190(2) 0.0248(7) Uani 1 1 d . . . . .
H44A H 0.0821 0.9339 0.2635 0.030 Uiso 1 1 calc R U . . .
H44B H 0.1501 0.9556 0.3587 0.030 Uiso 1 1 calc R U . . .
C45 C -0.0181(3) 0.9980(3) 0.3464(2) 0.0334(8) Uani 1 1 d . . . . .
H45A H 0.0022 1.0754 0.3505 0.050 Uiso 1 1 calc R U . . .
H45B H -0.0257 0.9907 0.4008 0.050 Uiso 1 1 calc R U . . .
H45C H -0.0910 0.9729 0.3056 0.050 Uiso 1 1 calc R U . . .
O1 O 0.5552(4) 0.9044(4) 0.0705(4) 0.116(2) Uani 0.85 1 d D . P C 1
C46 C 0.6648(6) 0.9538(7) 0.1248(7) 0.111(3) Uani 0.85 1 d D . P C 1
H46A H 0.7037 1.0028 0.1002 0.134 Uiso 0.85 1 calc R U P C 1
H46B H 0.7162 0.8970 0.1378 0.134 Uiso 0.85 1 calc R U P C 1
C47 C 0.6289(6) 1.0157(6) 0.1980(4) 0.088(2) Uani 0.85 1 d D . P C 1
H47A H 0.6146 0.9667 0.2324 0.105 Uiso 0.85 1 calc R U P C 1
H47B H 0.6883 1.0751 0.2322 0.105 Uiso 0.85 1 calc R U P C 1
C48 C 0.5263(6) 1.0607(5) 0.1668(5) 0.097(2) Uani 0.85 1 d D . P C 1
H48A H 0.5427 1.1260 0.1476 0.116 Uiso 0.85 1 calc R U P C 1
H48B H 0.4808 1.0816 0.2094 0.116 Uiso 0.85 1 calc R U P C 1
C49 C 0.4677(6) 0.9702(5) 0.0980(5) 0.082(2) Uani 0.85 1 d D . P C 1
H49A H 0.4142 0.9259 0.1163 0.098 Uiso 0.85 1 calc R U P C 1
H49B H 0.4235 0.9983 0.0524 0.098 Uiso 0.85 1 calc R U P C 1
O1' O 0.571(4) 0.966(4) 0.138(3) 0.15(1) Uiso 0.15 1 d D . P D 2
C46' C 0.688(5) 0.935(6) 0.135(6) 0.15(1) Uiso 0.15 1 d D . P D 2
H46C H 0.7405 0.9575 0.1904 0.181 Uiso 0.15 1 calc R U P D 2
H46D H 0.6885 0.8551 0.1106 0.181 Uiso 0.15 1 calc R U P D 2
C47' C 0.718(4) 0.997(4) 0.081(3) 0.15(1) Uiso 0.15 1 d D . P D 2
H47C H 0.8013 1.0157 0.0945 0.181 Uiso 0.15 1 calc R U P D 2
H47D H 0.6927 0.9543 0.0219 0.181 Uiso 0.15 1 calc R U P D 2
C48' C 0.660(4) 1.091(3) 0.096(3) 0.15(1) Uiso 0.15 1 d D . P D 2
H48C H 0.6639 1.1349 0.0556 0.181 Uiso 0.15 1 calc R U P D 2
H48D H 0.6882 1.1385 0.1532 0.181 Uiso 0.15 1 calc R U P D 2
C49' C 0.549(3) 1.042(4) 0.083(3) 0.15(1) Uiso 0.15 1 d D . P D 2
H49C H 0.5181 1.0017 0.0245 0.181 Uiso 0.15 1 calc R U P D 2
H49D H 0.4960 1.0975 0.1013 0.181 Uiso 0.15 1 calc R U P D 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Br1 Fe2 2.5100(6) . ?
Br1 Fe1 2.5308(7) . ?
Br2 Fe3 2.3906(6) . ?
Fe1 N1 2.001(2) . ?
Fe1 N2 2.008(2) . ?
Fe1 S1 2.2918(8) . ?
Fe3 N6 1.992(2) . ?
Fe3 N5 1.994(2) . ?
Fe3 S1 2.1722(8) . ?
Br1' Fe2 2.536(18) . ?
Br1' Fe1' 2.821(19) . ?
Br2' Fe1' 2.274(13) . ?
Br2' Fe3' 2.87(2) . ?
Fe1' N2 2.020(9) . ?
Fe1' S1 2.046(8) . ?
Fe1' N1 2.172(9) . ?
Fe3' S1 1.72(2) . ?
Fe3' N6 2.02(2) . ?
Fe3' N5 2.15(2) . ?
Fe2 N3 2.003(2) . ?
Fe2 N4 2.011(2) . ?
Fe2 S1 2.2915(8) . ?
N1 C2 1.328(4) . ?
N1 C1 1.485(4) . ?
N2 C4 1.334(4) . ?
N2 C5 1.494(4) . ?
N3 C9 1.333(4) . ?
N3 C8 1.485(4) . ?
N4 C11 1.330(4) . ?
N4 C12 1.485(4) . ?
N5 C16 1.328(4) . ?
N5 C15 1.487(4) . ?
N6 C18 1.345(4) . ?
N6 C19 1.488(4) . ?
C1 C22 1.521(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.407(4) . ?
C2 C6 1.517(4) . ?
C3 C4 1.408(4) . ?
C3 H3A 0.9500 . ?
C4 C7 1.509(4) . ?
C5 C34 1.523(4) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C24 1.524(4) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.410(4) . ?
C9 C13 1.514(4) . ?
C10 C11 1.404(4) . ?
C10 H10A 0.9500 . ?
C11 C14 1.514(4) . ?
C12 C36 1.510(4) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 C26 1.513(4) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C16 C17 1.406(4) . ?
C16 C20 1.517(4) . ?
C17 C18 1.397(4) . ?
C17 H17A 0.9500 . ?
C18 C21 1.516(4) . ?
C19 C38 1.518(4) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.405(4) . ?
C22 C27 1.406(4) . ?
C23 C24 1.406(4) . ?
C23 C28 1.519(4) . ?
C24 C25 1.402(4) . ?
C25 C26 1.410(4) . ?
C25 C30 1.514(4) . ?
C26 C27 1.399(4) . ?
C27 C32 1.525(4) . ?
C28 C29 1.538(4) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C31 1.533(4) . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 C33 1.538(4) . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C35 1.407(4) . ?
C34 C39 1.408(4) . ?
C35 C36 1.402(4) . ?
C35 C40 1.527(4) . ?
C36 C37 1.410(4) . ?
C37 C38 1.397(4) . ?
C37 C42 1.527(4) . ?
C38 C39 1.410(4) . ?
C39 C44 1.522(4) . ?
C40 C41 1.527(4) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 C43 1.531(4) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 C45 1.526(4) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
O1 C49 1.437(8) . ?
O1 C46 1.454(9) . ?
C46 C47 1.454(13) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.419(10) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.448(9) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9900 . ?
C49 H49B 0.9900 . ?
O1' C46' 1.47(2) . ?
O1' C49' 1.49(2) . ?
C46' C47' 1.43(2) . ?
C46' H46C 0.9900 . ?
C46' H46D 0.9900 . ?
C47' C48' 1.39(2) . ?
C47' H47C 0.9900 . ?
C47' H47D 0.9900 . ?
C48' C49' 1.40(2) . ?
C48' H48C 0.9900 . ?
C48' H48D 0.9900 . ?
C49' H49C 0.9900 . ?
C49' H49D 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
Fe2 Br1 Fe1 80.397(18) . . ?
N1 Fe1 N2 101.08(10) . . ?
N1 Fe1 S1 122.15(7) . . ?
N2 Fe1 S1 119.35(7) . . ?
N1 Fe1 Br1 106.15(7) . . ?
N2 Fe1 Br1 113.44(7) . . ?
S1 Fe1 Br1 94.29(2) . . ?
N6 Fe3 N5 96.83(10) . . ?
N6 Fe3 S1 114.80(7) . . ?
N5 Fe3 S1 114.51(8) . . ?
N6 Fe3 Br2 111.79(7) . . ?
N5 Fe3 Br2 106.46(7) . . ?
S1 Fe3 Br2 111.41(3) . . ?
Fe2 Br1' Fe1' 84.2(5) . . ?
Fe1' Br2' Fe3' 72.5(5) . . ?
N2 Fe1' S1 132.0(4) . . ?
N2 Fe1' N1 95.1(4) . . ?
S1 Fe1' N1 126.1(4) . . ?
N2 Fe1' Br2' 97.9(4) . . ?
S1 Fe1' Br2' 94.4(4) . . ?
N1 Fe1' Br2' 104.7(4) . . ?
N2 Fe1' Br1' 85.7(5) . . ?
S1 Fe1' Br1' 80.7(5) . . ?
N1 Fe1' Br1' 78.3(5) . . ?
Br2' Fe1' Br1' 175.0(5) . . ?
S1 Fe3' N6 139.4(12) . . ?
S1 Fe3' N5 129.5(11) . . ?
N6 Fe3' N5 91.0(8) . . ?
S1 Fe3' Br2' 83.4(8) . . ?
N6 Fe3' Br2' 98.0(8) . . ?
N5 Fe3' Br2' 92.7(7) . . ?
N3 Fe2 N4 96.12(10) . . ?
N3 Fe2 S1 122.49(7) . . ?
N4 Fe2 S1 124.40(7) . . ?
N3 Fe2 Br1 112.37(7) . . ?
N4 Fe2 Br1 106.22(7) . . ?
S1 Fe2 Br1 94.86(3) . . ?
N3 Fe2 Br1' 119.4(4) . . ?
N4 Fe2 Br1' 113.1(4) . . ?
S1 Fe2 Br1' 83.1(4) . . ?
Fe3' S1 Fe1' 109.7(8) . . ?
Fe3' S1 Fe2 138.1(7) . . ?
Fe1' S1 Fe2 112.0(3) . . ?
Fe3 S1 Fe2 156.63(4) . . ?
Fe3 S1 Fe1 112.88(3) . . ?
Fe2 S1 Fe1 90.45(3) . . ?
C2 N1 C1 118.2(2) . . ?
C2 N1 Fe1 117.9(2) . . ?
C1 N1 Fe1 123.35(18) . . ?
C2 N1 Fe1' 115.6(3) . . ?
C1 N1 Fe1' 123.6(3) . . ?
C4 N2 C5 116.5(2) . . ?
C4 N2 Fe1 117.5(2) . . ?
C5 N2 Fe1 125.90(18) . . ?
C4 N2 Fe1' 117.2(3) . . ?
C5 N2 Fe1' 121.0(3) . . ?
C9 N3 C8 116.0(2) . . ?
C9 N3 Fe2 122.1(2) . . ?
C8 N3 Fe2 121.61(18) . . ?
C11 N4 C12 117.7(2) . . ?
C11 N4 Fe2 121.7(2) . . ?
C12 N4 Fe2 120.11(17) . . ?
C16 N5 C15 118.0(2) . . ?
C16 N5 Fe3 117.8(2) . . ?
C15 N5 Fe3 122.81(18) . . ?
C16 N5 Fe3' 123.4(6) . . ?
C15 N5 Fe3' 117.8(6) . . ?
C18 N6 C19 117.3(2) . . ?
C18 N6 Fe3 117.35(19) . . ?
C19 N6 Fe3 124.98(18) . . ?
C18 N6 Fe3' 126.4(6) . . ?
C19 N6 Fe3' 114.3(6) . . ?
N1 C1 C22 110.3(2) . . ?
N1 C1 H1A 109.6 . . ?
C22 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C22 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
N1 C2 C3 124.6(3) . . ?
N1 C2 C6 119.7(3) . . ?
C3 C2 C6 115.7(3) . . ?
C2 C3 C4 132.7(3) . . ?
C2 C3 H3A 113.7 . . ?
C4 C3 H3A 113.7 . . ?
N2 C4 C3 125.0(3) . . ?
N2 C4 C7 119.4(3) . . ?
C3 C4 C7 115.5(3) . . ?
N2 C5 C34 110.0(2) . . ?
N2 C5 H5A 109.7 . . ?
C34 C5 H5A 109.7 . . ?
N2 C5 H5B 109.7 . . ?
C34 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
C2 C6 H6A 109.5 . . ?
C2 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C2 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C24 110.9(2) . . ?
N3 C8 H8A 109.5 . . ?
C24 C8 H8A 109.5 . . ?
N3 C8 H8B 109.5 . . ?
C24 C8 H8B 109.5 . . ?
H8A C8 H8B 108.0 . . ?
N3 C9 C10 123.9(3) . . ?
N3 C9 C13 120.2(3) . . ?
C10 C9 C13 115.9(3) . . ?
C11 C10 C9 130.5(3) . . ?
C11 C10 H10A 114.8 . . ?
C9 C10 H10A 114.8 . . ?
N4 C11 C10 124.2(3) . . ?
N4 C11 C14 119.9(3) . . ?
C10 C11 C14 115.8(3) . . ?
N4 C12 C36 110.6(2) . . ?
N4 C12 H12A 109.5 . . ?
C36 C12 H12A 109.5 . . ?
N4 C12 H12B 109.5 . . ?
C36 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C11 C14 H14A 109.5 . . ?
C11 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C11 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N5 C15 C26 113.0(2) . . ?
N5 C15 H15A 109.0 . . ?
C26 C15 H15A 109.0 . . ?
N5 C15 H15B 109.0 . . ?
C26 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
N5 C16 C17 123.9(3) . . ?
N5 C16 C20 119.8(3) . . ?
C17 C16 C20 116.3(3) . . ?
C18 C17 C16 130.4(3) . . ?
C18 C17 H17A 114.8 . . ?
C16 C17 H17A 114.8 . . ?
N6 C18 C17 123.9(3) . . ?
N6 C18 C21 119.7(3) . . ?
C17 C18 C21 116.3(3) . . ?
N6 C19 C38 111.9(2) . . ?
N6 C19 H19A 109.2 . . ?
C38 C19 H19A 109.2 . . ?
N6 C19 H19B 109.2 . . ?
C38 C19 H19B 109.2 . . ?
H19A C19 H19B 107.9 . . ?
C16 C20 H20A 109.5 . . ?
C16 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C16 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C23 C22 C27 120.6(3) . . ?
C23 C22 C1 120.5(3) . . ?
C27 C22 C1 118.8(3) . . ?
C22 C23 C24 118.6(3) . . ?
C22 C23 C28 121.0(3) . . ?
C24 C23 C28 120.3(3) . . ?
C25 C24 C23 120.9(3) . . ?
C25 C24 C8 118.8(3) . . ?
C23 C24 C8 120.2(3) . . ?
C24 C25 C26 119.8(3) . . ?
C24 C25 C30 120.5(3) . . ?
C26 C25 C30 119.7(3) . . ?
C27 C26 C25 119.6(3) . . ?
C27 C26 C15 121.4(3) . . ?
C25 C26 C15 119.0(3) . . ?
C26 C27 C22 120.0(3) . . ?
C26 C27 C32 121.1(3) . . ?
C22 C27 C32 118.9(3) . . ?
C23 C28 C29 109.8(2) . . ?
C23 C28 H28A 109.7 . . ?
C29 C28 H28A 109.7 . . ?
C23 C28 H28B 109.7 . . ?
C29 C28 H28B 109.7 . . ?
H28A C28 H28B 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C25 C30 C31 112.8(2) . . ?
C25 C30 H30A 109.0 . . ?
C31 C30 H30A 109.0 . . ?
C25 C30 H30B 109.0 . . ?
C31 C30 H30B 109.0 . . ?
H30A C30 H30B 107.8 . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C27 C32 C33 111.2(3) . . ?
C27 C32 H32A 109.4 . . ?
C33 C32 H32A 109.4 . . ?
C27 C32 H32B 109.4 . . ?
C33 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C35 C34 C39 120.2(3) . . ?
C35 C34 C5 119.8(3) . . ?
C39 C34 C5 119.9(3) . . ?
C36 C35 C34 119.8(3) . . ?
C36 C35 C40 121.0(3) . . ?
C34 C35 C40 119.0(3) . . ?
C35 C36 C37 120.3(3) . . ?
C35 C36 C12 120.3(3) . . ?
C37 C36 C12 119.3(3) . . ?
C38 C37 C36 119.5(3) . . ?
C38 C37 C42 120.3(3) . . ?
C36 C37 C42 120.3(3) . . ?
C37 C38 C39 120.8(3) . . ?
C37 C38 C19 120.6(3) . . ?
C39 C38 C19 118.5(3) . . ?
C34 C39 C38 119.0(3) . . ?
C34 C39 C44 120.0(3) . . ?
C38 C39 C44 120.9(3) . . ?
C41 C40 C35 110.0(2) . . ?
C41 C40 H40A 109.7 . . ?
C35 C40 H40A 109.7 . . ?
C41 C40 H40B 109.7 . . ?
C35 C40 H40B 109.7 . . ?
H40A C40 H40B 108.2 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C42 C43 115.4(2) . . ?
C37 C42 H42A 108.4 . . ?
C43 C42 H42A 108.4 . . ?
C37 C42 H42B 108.4 . . ?
C43 C42 H42B 108.4 . . ?
H42A C42 H42B 107.5 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 C45 110.8(2) . . ?
C39 C44 H44A 109.5 . . ?
C45 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
C45 C44 H44B 109.5 . . ?
H44A C44 H44B 108.1 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C49 O1 C46 107.5(5) . . ?
O1 C46 C47 101.1(6) . . ?
O1 C46 H46A 111.5 . . ?
C47 C46 H46A 111.5 . . ?
O1 C46 H46B 111.5 . . ?
C47 C46 H46B 111.5 . . ?
H46A C46 H46B 109.4 . . ?
C48 C47 C46 105.3(7) . . ?
C48 C47 H47A 110.7 . . ?
C46 C47 H47A 110.7 . . ?
C48 C47 H47B 110.7 . . ?
C46 C47 H47B 110.7 . . ?
H47A C47 H47B 108.8 . . ?
C47 C48 C49 102.3(6) . . ?
C47 C48 H48A 111.3 . . ?
C49 C48 H48A 111.3 . . ?
C47 C48 H48B 111.3 . . ?
C49 C48 H48B 111.3 . . ?
H48A C48 H48B 109.2 . . ?
O1 C49 C48 106.4(5) . . ?
O1 C49 H49A 110.4 . . ?
C48 C49 H49A 110.4 . . ?
O1 C49 H49B 110.4 . . ?
C48 C49 H49B 110.4 . . ?
H49A C49 H49B 108.6 . . ?
C46' O1' C49' 103.5(19) . . ?
C47' C46' O1' 102.0(19) . . ?
C47' C46' H46C 111.4 . . ?
O1' C46' H46C 111.4 . . ?
C47' C46' H46D 111.4 . . ?
O1' C46' H46D 111.4 . . ?
H46C C46' H46D 109.2 . . ?
C48' C47' C46' 105(3) . . ?
C48' C47' H47C 110.8 . . ?
C46' C47' H47C 110.8 . . ?
C48' C47' H47D 110.8 . . ?
C46' C47' H47D 110.8 . . ?
H47C C47' H47D 108.9 . . ?
C47' C48' C49' 99(2) . . ?
C47' C48' H48C 112.0 . . ?
C49' C48' H48C 112.0 . . ?
C47' C48' H48D 112.0 . . ?
C49' C48' H48D 112.0 . . ?
H48C C48' H48D 109.7 . . ?
C48' C49' O1' 101(2) . . ?
C48' C49' H49C 111.6 . . ?
O1' C49' H49C 111.6 . . ?
C48' C49' H49D 111.5 . . ?
O1' C49' H49D 111.6 . . ?
H49C C49' H49D 109.4 . . ?

_refine_diff_density_max         0.839
_refine_diff_density_min         -0.968
_refine_diff_density_rms         0.088

_shelxl_version_number           2014/6


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'hexanes, tetrahydrofuran'
_chemical_compound_source        n/a
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# 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_ylee99
_database_code_depnum_ccdc_archive 'CCDC 1483322'

_audit_update_record             
;
2016-06-03 deposited with the CCDC.
2016-06-28 downloaded from the CCDC.
;
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        C47H67N6O0.5Br1S1Fe3
_chemical_name_common            n/a
_chemical_melting_point          n/a
_chemical_formula_moiety         
'C45 H63 Br1.03 Fe3 N6 S, 0.47 (O1 C4 H8), (O1 C4 H8)'
_chemical_formula_sum            'C50.88 H74.76 Br1.03 Fe3 N6 O1.47 S'
_chemical_formula_weight         1075.92

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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   11.6510(3)
_cell_length_b                   12.6465(4)
_cell_length_c                   17.0493(5)
_cell_angle_alpha                94.401(1)
_cell_angle_beta                 95.909(1)
_cell_angle_gamma                96.266(1)
_cell_volume                     2473.99(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9745
_cell_measurement_theta_min      2.0
_cell_measurement_theta_max      28.0

_exptl_crystal_description       plate
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_F_000             1128
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.237
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    1.787
_shelx_estimated_absorpt_T_min   0.677
_shelx_estimated_absorpt_T_max   0.900
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.2523
_exptl_absorpt_correction_T_max  0.3074
_exptl_absorpt_process_details   
'based on measured indexed crystal faces, Bruker SHELXTL2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II DUO'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            62395
_diffrn_reflns_av_unetI/netI     0.0245
_diffrn_reflns_av_R_equivalents  0.0313
_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       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.205
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             11378
_reflns_number_gt                9547
_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       'Bruker APEX2 (Bruker, 2014)'
_computing_cell_refinement       'Bruker APEX2 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT (Bruker, 2014)'
_computing_structure_solution    'SHELXTL-2014 (Bruker, 2014)'
_computing_structure_refinement  'SHELXTL-2014 (Bruker, 2014)'
_computing_molecular_graphics    'SHELXTL-2014 (Bruker, 2014)'
_computing_publication_material  'SHELXTL-2014 (Bruker, 2014)'
_refine_special_details          
; 
All H atoms were positioned geometrically ( C---H = 0.93/1.00 Å) and 
allowed to ride with Uiso(H)= 1.2/1.5Ueq(C). 
Methyl ones were allowed to rotate around the corresponding C---C.

The asymmetric unit consists of the Fe3 cluster, one thf molecule in general
 position and another one at an inversion center.  The latter half molecule is
 disordered with traces of Br that is part of the core.  One the other hand, we
 have a disorder in the core where the major part consists of a full Br, a 97%
 Fe1, a 100% Fe2 and a disorder of the third position as fe3/fe3? with
 occupancies refining to 0.93/0.07.  There is a thf molecule disordered around
 an inversion center and against traces (0.03%) of Br(2).  
 
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0464P)²+0.9317P] 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         11378
_refine_ls_number_parameters     588
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0294
_refine_ls_wR_factor_ref         0.0843
_refine_ls_wR_factor_gt          0.0796
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.07841(2) 0.99491(2) 0.26346(2) 0.01742(6) Uani 1 1 d . . . . .
Fe1 Fe 0.05731(2) 0.84371(3) 0.35162(2) 0.01588(7) Uani 0.97 1 d . . P A 1
Fe2 Fe 0.10899(2) 0.83359(2) 0.16724(2) 0.01616(7) Uani 1 1 d . . . . .
Fe3 Fe 0.09263(8) 0.54882(6) 0.29410(17) 0.0163(4) Uani 0.525(6) 1 d . . P A 1
Fe1' Fe 0.0589(9) 0.790(1) 0.3518(6) 0.018(2) Uiso 0.03 1 d . . P A 2
Fe3' Fe 0.10319(9) 0.54982(6) 0.2564(2) 0.0197(5) Uani 0.475(6) 1 d . . P A 2
Br2 Br 0.0554(8) 0.5933(9) 0.4333(6) 0.044(2) Uiso 0.03 1 d . . P B 2
S1 S 0.09031(4) 0.71554(4) 0.25890(3) 0.01675(10) Uani 1 1 d . . . . .
N1 N -0.09634(14) 0.82645(13) 0.39628(9) 0.0181(3) Uani 1 1 d . . . . .
N2 N 0.16656(14) 0.86637(13) 0.45205(9) 0.0164(3) Uani 1 1 d . . . . .
N3 N 0.00228(13) 0.82391(13) 0.06606(9) 0.0144(3) Uani 1 1 d . . . . .
N4 N 0.25891(13) 0.86484(12) 0.12108(9) 0.0140(3) Uani 1 1 d . . . . .
N5 N -0.02552(14) 0.43175(13) 0.23883(11) 0.0209(4) Uani 1 1 d . . . . .
N6 N 0.23338(13) 0.47123(13) 0.29255(10) 0.0177(3) Uani 1 1 d . . . . .
C1 C -0.20947(17) 0.79942(17) 0.34578(11) 0.0200(4) Uani 1 1 d . . . . .
H1A H -0.2423 0.8660 0.3336 0.024 Uiso 1 1 calc R U . . .
H1B H -0.2648 0.7574 0.3750 0.024 Uiso 1 1 calc R U . . .
C2 C -0.09743(17) 0.84331(16) 0.47449(11) 0.0195(4) Uani 1 1 d . . . . .
C3 C 0.00247(17) 0.86711(16) 0.52981(11) 0.0202(4) Uani 1 1 d . . . . .
H3A H -0.0139 0.8787 0.5830 0.024 Uiso 1 1 calc R U . . .
C4 C 0.12215(17) 0.87696(15) 0.52092(11) 0.0177(4) Uani 1 1 d . . . . .
C5 C 0.29565(16) 0.87827(16) 0.45348(11) 0.0184(4) Uani 1 1 d . . . . .
H5A H 0.3305 0.8505 0.5020 0.022 Uiso 1 1 calc R U . . .
H5B H 0.3251 0.9549 0.4549 0.022 Uiso 1 1 calc R U . . .
C6 C -0.21190(18) 0.83507(19) 0.51015(12) 0.0261(5) Uani 1 1 d . . . . .
H6A H -0.1968 0.8497 0.5678 0.039 Uiso 1 1 calc R U . . .
H6B H -0.2600 0.8872 0.4886 0.039 Uiso 1 1 calc R U . . .
H6C H -0.2527 0.7629 0.4971 0.039 Uiso 1 1 calc R U . . .
C7 C 0.20185(18) 0.90041(18) 0.59787(11) 0.0241(4) Uani 1 1 d . . . . .
H7A H 0.1551 0.9056 0.6423 0.036 Uiso 1 1 calc R U . . .
H7B H 0.2508 0.8427 0.6043 0.036 Uiso 1 1 calc R U . . .
H7C H 0.2512 0.9681 0.5967 0.036 Uiso 1 1 calc R U . . .
C8 C -0.12282(16) 0.78198(16) 0.06024(11) 0.0167(4) Uani 1 1 d . . . . .
H8A H -0.1430 0.7309 0.0126 0.020 Uiso 1 1 calc R U . . .
H8B H -0.1705 0.8417 0.0544 0.020 Uiso 1 1 calc R U . . .
C9 C 0.04080(16) 0.86029(15) 0.00105(11) 0.0158(4) Uani 1 1 d . . . . .
C10 C 0.15837(16) 0.89452(16) -0.00573(11) 0.0181(4) Uani 1 1 d . . . . .
H10A H 0.1720 0.9233 -0.0543 0.022 Uiso 1 1 calc R U . . .
C11 C 0.25903(16) 0.89316(15) 0.04744(11) 0.0160(4) Uani 1 1 d . . . . .
C12 C 0.37483(15) 0.86225(15) 0.16639(11) 0.0157(4) Uani 1 1 d . . . . .
H12A H 0.4134 0.9362 0.1788 0.019 Uiso 1 1 calc R U . . .
H12B H 0.4237 0.8229 0.1330 0.019 Uiso 1 1 calc R U . . .
C13 C -0.04387(17) 0.86556(18) -0.07178(11) 0.0214(4) Uani 1 1 d . . . . .
H13A H -0.0017 0.8939 -0.1139 0.032 Uiso 1 1 calc R U . . .
H13B H -0.0825 0.7938 -0.0897 0.032 Uiso 1 1 calc R U . . .
H13C H -0.1022 0.9124 -0.0588 0.032 Uiso 1 1 calc R U . . .
C14 C 0.37321(17) 0.92628(18) 0.01609(12) 0.0242(4) Uani 1 1 d . . . . .
H14A H 0.3582 0.9445 -0.0386 0.036 Uiso 1 1 calc R U . . .
H14B H 0.4143 0.9886 0.0491 0.036 Uiso 1 1 calc R U . . .
H14C H 0.4210 0.8672 0.0175 0.036 Uiso 1 1 calc R U . . .
C15 C -0.14523(17) 0.44852(16) 0.20663(14) 0.0249(5) Uani 1 1 d . . . . .
H15A H -0.2015 0.4162 0.2402 0.030 Uiso 1 1 calc R U . . .
H15B H -0.1632 0.4118 0.1526 0.030 Uiso 1 1 calc R U . . .
C16 C -0.00274(16) 0.33194(15) 0.24553(11) 0.0164(4) Uani 1 1 d . . . . .
C17 C 0.10794(17) 0.30288(15) 0.27044(12) 0.0193(4) Uani 1 1 d . . . . .
H17A H 0.1097 0.2285 0.2744 0.023 Uiso 1 1 calc R U . . .
C18 C 0.21641(17) 0.36538(16) 0.29049(12) 0.0183(4) Uani 1 1 d . . . . .
C19 C 0.35346(16) 0.52658(15) 0.30997(12) 0.0185(4) Uani 1 1 d . . . . .
H19A H 0.4013 0.5016 0.2691 0.022 Uiso 1 1 calc R U . . .
H19B H 0.3881 0.5081 0.3619 0.022 Uiso 1 1 calc R U . . .
C20 C -0.10012(17) 0.24149(15) 0.22565(14) 0.0239(4) Uani 1 1 d . . . . .
H20A H -0.0698 0.1733 0.2335 0.036 Uiso 1 1 calc R U . . .
H20B H -0.1610 0.2509 0.2603 0.036 Uiso 1 1 calc R U . . .
H20C H -0.1326 0.2416 0.1703 0.036 Uiso 1 1 calc R U . . .
C21 C 0.31820(19) 0.30456(19) 0.31274(18) 0.0377(6) Uani 1 1 d . . . . .
H21A H 0.2916 0.2279 0.3082 0.057 Uiso 1 1 calc R U . . .
H21B H 0.3777 0.3187 0.2770 0.057 Uiso 1 1 calc R U . . .
H21C H 0.3511 0.3277 0.3674 0.057 Uiso 1 1 calc R U . . .
C22 C -0.19462(15) 0.73558(15) 0.26908(11) 0.0150(4) Uani 1 1 d . . . . .
C23 C -0.18097(15) 0.78560(14) 0.19928(11) 0.0132(3) Uani 1 1 d . . . . .
C24 C -0.15081(15) 0.72652(15) 0.13293(11) 0.0138(4) Uani 1 1 d . . . . .
C25 C -0.13790(15) 0.61750(15) 0.13521(11) 0.0167(4) Uani 1 1 d . . . . .
C26 C -0.15937(16) 0.56652(15) 0.20342(12) 0.0186(4) Uani 1 1 d . . . . .
C27 C -0.18638(15) 0.62560(16) 0.27023(11) 0.0170(4) Uani 1 1 d . . . . .
C28 C -0.20131(16) 0.90177(15) 0.19547(11) 0.0161(4) Uani 1 1 d . . . . .
H28A H -0.1549 0.9337 0.1559 0.019 Uiso 1 1 calc R U . . .
H28B H -0.1748 0.9416 0.2476 0.019 Uiso 1 1 calc R U . . .
C29 C -0.32954(17) 0.91263(17) 0.17306(13) 0.0219(4) Uani 1 1 d . . . . .
H29A H -0.3398 0.9883 0.1711 0.033 Uiso 1 1 calc R U . . .
H29B H -0.3556 0.8743 0.1210 0.033 Uiso 1 1 calc R U . . .
H29C H -0.3755 0.8822 0.2127 0.033 Uiso 1 1 calc R U . . .
C30 C -0.09472(18) 0.55633(17) 0.06624(13) 0.0242(4) Uani 1 1 d . . . . .
H30A H -0.0481 0.5015 0.0869 0.029 Uiso 1 1 calc R U . . .
H30B H -0.0430 0.6063 0.0399 0.029 Uiso 1 1 calc R U . . .
C31 C -0.1926(2) 0.5014(2) 0.00461(14) 0.0345(6) Uani 1 1 d . . . . .
H31A H -0.1590 0.4635 -0.0381 0.052 Uiso 1 1 calc R U . . .
H31B H -0.2432 0.4504 0.0298 0.052 Uiso 1 1 calc R U . . .
H31C H -0.2381 0.5553 -0.0172 0.052 Uiso 1 1 calc R U . . .
C32 C -0.20428(19) 0.57208(18) 0.34549(13) 0.0275(5) Uani 1 1 d . . . . .
H32A H -0.1756 0.6236 0.3918 0.033 Uiso 1 1 calc R U . . .
H32B H -0.1579 0.5111 0.3479 0.033 Uiso 1 1 calc R U . . .
C33 C -0.3320(2) 0.5319(2) 0.35007(15) 0.0413(6) Uani 1 1 d . . . . .
H33A H -0.3393 0.4981 0.3994 0.062 Uiso 1 1 calc R U . . .
H33B H -0.3781 0.5922 0.3488 0.062 Uiso 1 1 calc R U . . .
H33C H -0.3604 0.4797 0.3049 0.062 Uiso 1 1 calc R U . . .
C34 C 0.33214(16) 0.81811(15) 0.38104(11) 0.0161(4) Uani 1 1 d . . . . .
C35 C 0.35253(15) 0.87037(15) 0.31292(11) 0.0146(4) Uani 1 1 d . . . . .
C36 C 0.36615(15) 0.80950(15) 0.24284(11) 0.0142(4) Uani 1 1 d . . . . .
C37 C 0.36474(15) 0.69778(15) 0.24133(11) 0.0148(4) Uani 1 1 d . . . . .
C38 C 0.35524(15) 0.64745(15) 0.31152(11) 0.0158(4) Uani 1 1 d . . . . .
C39 C 0.33856(16) 0.70758(16) 0.38114(11) 0.0167(4) Uani 1 1 d . . . . .
C40 C 0.36473(16) 0.99150(15) 0.31643(12) 0.0177(4) Uani 1 1 d . . . . .
H40A H 0.3107 1.0189 0.3521 0.021 Uiso 1 1 calc R U . . .
H40B H 0.3432 1.0137 0.2630 0.021 Uiso 1 1 calc R U . . .
C41 C 0.48915(18) 1.04004(17) 0.34629(13) 0.0257(5) Uani 1 1 d . . . . .
H41A H 0.4943 1.1181 0.3479 0.039 Uiso 1 1 calc R U . . .
H41B H 0.5102 1.0191 0.3996 0.039 Uiso 1 1 calc R U . . .
H41C H 0.5426 1.0140 0.3105 0.039 Uiso 1 1 calc R U . . .
C42 C 0.36892(17) 0.63180(16) 0.16347(11) 0.0199(4) Uani 1 1 d . . . . .
H42A H 0.3298 0.6670 0.1200 0.024 Uiso 1 1 calc R U . . .
H42B H 0.3248 0.5607 0.1652 0.024 Uiso 1 1 calc R U . . .
C43 C 0.49201(19) 0.61661(18) 0.14465(13) 0.0275(5) Uani 1 1 d . . . . .
H43A H 0.4880 0.5736 0.0939 0.041 Uiso 1 1 calc R U . . .
H43B H 0.5359 0.6865 0.1414 0.041 Uiso 1 1 calc R U . . .
H43C H 0.5309 0.5800 0.1866 0.041 Uiso 1 1 calc R U . . .
C44 C 0.33212(18) 0.65503(17) 0.45792(12) 0.0233(4) Uani 1 1 d . . . . .
H44A H 0.3012 0.5788 0.4461 0.028 Uiso 1 1 calc R U . . .
H44B H 0.2785 0.6899 0.4902 0.028 Uiso 1 1 calc R U . . .
C45 C 0.4533(2) 0.6644(2) 0.50477(13) 0.0316(5) Uani 1 1 d . . . . .
H45A H 0.4480 0.6302 0.5541 0.047 Uiso 1 1 calc R U . . .
H45B H 0.5060 0.6290 0.4730 0.047 Uiso 1 1 calc R U . . .
H45C H 0.4833 0.7400 0.5170 0.047 Uiso 1 1 calc R U . . .
O1 O 0.46871(17) 0.15445(17) 0.15132(13) 0.0537(5) Uani 1 1 d . . . . .
C46 C 0.5639(2) 0.2338(2) 0.1717(2) 0.0501(7) Uani 1 1 d . . . . .
H46A H 0.6377 0.2028 0.1675 0.060 Uiso 1 1 calc R U . . .
H46B H 0.5639 0.2648 0.2269 0.060 Uiso 1 1 calc R U . . .
C47 C 0.5520(3) 0.3181(2) 0.1155(2) 0.0663(10) Uani 1 1 d . . . . .
H47A H 0.5898 0.3018 0.0673 0.080 Uiso 1 1 calc R U . . .
H47B H 0.5860 0.3893 0.1407 0.080 Uiso 1 1 calc R U . . .
C48 C 0.4226(3) 0.3132(3) 0.0965(2) 0.0742(11) Uani 1 1 d . . . . .
H48A H 0.3905 0.3646 0.1325 0.089 Uiso 1 1 calc R U . . .
H48B H 0.4021 0.3289 0.0411 0.089 Uiso 1 1 calc R U . . .
C49 C 0.3780(3) 0.2006(3) 0.1085(2) 0.0705(11) Uani 1 1 d . . . . .
H49A H 0.3097 0.1999 0.1386 0.085 Uiso 1 1 calc R U . . .
H49B H 0.3541 0.1591 0.0567 0.085 Uiso 1 1 calc R U . . .
O2 O 0.0667(2) 0.5365(2) 0.42094(17) 0.0166(6) Uiso 0.47 1 d . . P A -1
C50 C 0.0674(4) 0.4333(4) 0.4506(3) 0.0206(9) Uiso 0.47 1 d . . P A -1
H50A H 0.1391 0.4303 0.4866 0.025 Uiso 0.47 1 calc R U P A -1
H50B H 0.0623 0.3766 0.4066 0.025 Uiso 0.47 1 calc R U P A -1
C51 C -0.0387(4) 0.4205(4) 0.4948(3) 0.0223(10) Uiso 0.47 1 d . . P A -1
H51A H -0.0271 0.3743 0.5385 0.027 Uiso 0.47 1 calc R U P A -1
H51B H -0.1085 0.3897 0.4588 0.027 Uiso 0.47 1 calc R U P A -1
C52 C -0.0499(4) 0.5369(4) 0.5270(3) 0.0207(9) Uiso 0.47 1 d . . P A -1
H52A H -0.0280 0.5478 0.5849 0.025 Uiso 0.47 1 calc R U P A -1
H52B H -0.1302 0.5546 0.5148 0.025 Uiso 0.47 1 calc R U P A -1
C53 C 0.0374(4) 0.6058(4) 0.4821(3) 0.0200(9) Uiso 0.47 1 d . . P A -1
H53A H 0.0007 0.6659 0.4602 0.024 Uiso 0.47 1 calc R U P A -1
H53B H 0.1075 0.6352 0.5182 0.024 Uiso 0.47 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
Br1 Fe1 2.5280(4) . ?
Br1 Fe2 2.5973(3) . ?
Fe1 N2 2.0076(16) . ?
Fe1 N1 2.0133(16) . ?
Fe1 S1 2.2677(6) . ?
Fe2 N4 2.0017(15) . ?
Fe2 N3 2.0074(15) . ?
Fe2 S1 2.2528(5) . ?
Fe3 N6 2.0023(18) . ?
Fe3 N5 2.0121(18) . ?
Fe3 O2 2.229(4) . ?
Fe3 S1 2.2381(14) . ?
Fe1' S1 1.870(11) . ?
Fe1' N1 2.114(11) . ?
Fe1' N2 2.113(11) . ?
Fe3' N6 1.9747(18) . ?
Fe3' N5 1.9794(18) . ?
Fe3' S1 2.1148(9) . ?
N1 C2 1.336(2) . ?
N1 C1 1.489(2) . ?
N2 C4 1.334(2) . ?
N2 C5 1.493(2) . ?
N3 C9 1.333(2) . ?
N3 C8 1.486(2) . ?
N4 C11 1.332(2) . ?
N4 C12 1.490(2) . ?
N5 C16 1.329(2) . ?
N5 C15 1.489(2) . ?
N6 C18 1.329(3) . ?
N6 C19 1.485(2) . ?
C1 C22 1.519(3) . ?
C2 C3 1.410(3) . ?
C2 C6 1.518(3) . ?
C3 C4 1.411(3) . ?
C4 C7 1.517(3) . ?
C5 C34 1.523(3) . ?
C8 C24 1.517(3) . ?
C9 C10 1.410(3) . ?
C9 C13 1.515(3) . ?
C10 C11 1.409(3) . ?
C11 C14 1.513(3) . ?
C12 C36 1.517(3) . ?
C15 C26 1.524(3) . ?
C16 C17 1.412(3) . ?
C16 C20 1.513(3) . ?
C17 C18 1.411(3) . ?
C18 C21 1.514(3) . ?
C19 C38 1.525(3) . ?
C22 C23 1.405(3) . ?
C22 C27 1.406(3) . ?
C23 C24 1.404(3) . ?
C23 C28 1.519(2) . ?
C24 C25 1.406(3) . ?
C25 C26 1.404(3) . ?
C25 C30 1.517(3) . ?
C26 C27 1.396(3) . ?
C27 C32 1.518(3) . ?
C28 C29 1.527(3) . ?
C30 C31 1.535(3) . ?
C32 C33 1.531(3) . ?
C34 C35 1.408(3) . ?
C34 C39 1.408(3) . ?
C35 C36 1.404(3) . ?
C35 C40 1.519(3) . ?
C36 C37 1.409(3) . ?
C37 C38 1.406(3) . ?
C37 C42 1.521(3) . ?
C38 C39 1.402(3) . ?
C39 C44 1.518(3) . ?
C40 C41 1.531(3) . ?
C42 C43 1.530(3) . ?
C44 C45 1.537(3) . ?
O1 C46 1.408(3) . ?
O1 C49 1.425(4) . ?
C46 C47 1.497(5) . ?
C47 C48 1.502(5) . ?
C48 C49 1.497(5) . ?
O2 C53 1.403(6) . ?
O2 C50 1.435(5) . ?
C50 C51 1.513(7) . ?
C51 C52 1.556(7) . ?
C52 C53 1.565(7) . ?

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
Fe1 Br1 Fe2 78.886(11) . . ?
N2 Fe1 N1 100.31(6) . . ?
N2 Fe1 S1 117.21(5) . . ?
N1 Fe1 S1 117.37(5) . . ?
N2 Fe1 Br1 113.83(5) . . ?
N1 Fe1 Br1 113.82(5) . . ?
S1 Fe1 Br1 95.215(16) . . ?
N4 Fe2 N3 97.59(6) . . ?
N4 Fe2 S1 121.29(5) . . ?
N3 Fe2 S1 123.10(5) . . ?
N4 Fe2 Br1 109.45(5) . . ?
N3 Fe2 Br1 111.76(5) . . ?
S1 Fe2 Br1 93.698(16) . . ?
N6 Fe3 N5 98.29(8) . . ?
N6 Fe3 O2 97.83(12) . . ?
N5 Fe3 O2 102.24(13) . . ?
N6 Fe3 S1 122.64(10) . . ?
N5 Fe3 S1 119.39(10) . . ?
O2 Fe3 S1 112.62(11) . . ?
S1 Fe1' N1 133.3(6) . . ?
S1 Fe1' N2 132.8(6) . . ?
N1 Fe1' N2 93.8(4) . . ?
N6 Fe3' N5 100.33(8) . . ?
N6 Fe3' S1 131.01(7) . . ?
N5 Fe3' S1 127.42(6) . . ?
Fe1' S1 Fe3' 119.8(4) . . ?
Fe1' S1 Fe2 107.6(4) . . ?
Fe3' S1 Fe2 132.60(11) . . ?
Fe3 S1 Fe2 149.95(8) . . ?
Fe3 S1 Fe1 117.86(8) . . ?
Fe2 S1 Fe1 92.17(2) . . ?
C2 N1 C1 118.37(16) . . ?
C2 N1 Fe1 118.65(13) . . ?
C1 N1 Fe1 122.94(12) . . ?
C2 N1 Fe1' 118.9(3) . . ?
C1 N1 Fe1' 119.8(3) . . ?
C4 N2 C5 118.08(15) . . ?
C4 N2 Fe1 118.58(13) . . ?
C5 N2 Fe1 123.24(12) . . ?
C4 N2 Fe1' 118.8(3) . . ?
C5 N2 Fe1' 120.6(3) . . ?
C9 N3 C8 116.77(15) . . ?
C9 N3 Fe2 120.41(12) . . ?
C8 N3 Fe2 122.75(11) . . ?
C11 N4 C12 116.40(15) . . ?
C11 N4 Fe2 120.41(12) . . ?
C12 N4 Fe2 123.15(11) . . ?
C16 N5 C15 117.79(16) . . ?
C16 N5 Fe3' 119.60(13) . . ?
C15 N5 Fe3' 121.98(13) . . ?
C16 N5 Fe3 116.97(13) . . ?
C15 N5 Fe3 123.87(13) . . ?
C18 N6 C19 119.15(16) . . ?
C18 N6 Fe3' 119.39(13) . . ?
C19 N6 Fe3' 120.77(12) . . ?
C18 N6 Fe3 117.02(13) . . ?
C19 N6 Fe3 122.60(12) . . ?
N1 C1 C22 111.10(15) . . ?
N1 C2 C3 124.82(18) . . ?
N1 C2 C6 120.22(18) . . ?
C3 C2 C6 114.95(17) . . ?
C2 C3 C4 132.06(18) . . ?
N2 C4 C3 125.09(17) . . ?
N2 C4 C7 120.27(18) . . ?
C3 C4 C7 114.64(17) . . ?
N2 C5 C34 111.11(15) . . ?
N3 C8 C24 111.37(14) . . ?
N3 C9 C10 124.13(17) . . ?
N3 C9 C13 119.85(17) . . ?
C10 C9 C13 116.02(16) . . ?
C11 C10 C9 130.77(17) . . ?
N4 C11 C10 124.52(17) . . ?
N4 C11 C14 119.68(17) . . ?
C10 C11 C14 115.80(16) . . ?
N4 C12 C36 112.36(15) . . ?
N5 C15 C26 112.11(16) . . ?
N5 C16 C17 124.42(17) . . ?
N5 C16 C20 119.20(17) . . ?
C17 C16 C20 116.38(17) . . ?
C16 C17 C18 131.02(18) . . ?
N6 C18 C17 124.79(17) . . ?
N6 C18 C21 119.39(18) . . ?
C17 C18 C21 115.81(18) . . ?
N6 C19 C38 111.54(15) . . ?
C23 C22 C27 119.97(17) . . ?
C23 C22 C1 121.25(17) . . ?
C27 C22 C1 118.63(17) . . ?
C24 C23 C22 119.34(17) . . ?
C24 C23 C28 120.58(16) . . ?
C22 C23 C28 120.07(16) . . ?
C23 C24 C25 120.53(17) . . ?
C23 C24 C8 120.00(17) . . ?
C25 C24 C8 119.31(17) . . ?
C26 C25 C24 119.68(17) . . ?
C26 C25 C30 119.86(18) . . ?
C24 C25 C30 120.38(18) . . ?
C27 C26 C25 119.89(17) . . ?
C27 C26 C15 119.87(18) . . ?
C25 C26 C15 120.11(19) . . ?
C26 C27 C22 120.38(17) . . ?
C26 C27 C32 120.22(18) . . ?
C22 C27 C32 119.39(18) . . ?
C23 C28 C29 111.45(15) . . ?
C25 C30 C31 113.60(17) . . ?
C27 C32 C33 112.38(17) . . ?
C35 C34 C39 120.05(17) . . ?
C35 C34 C5 120.78(17) . . ?
C39 C34 C5 119.06(17) . . ?
C36 C35 C34 119.24(17) . . ?
C36 C35 C40 120.50(17) . . ?
C34 C35 C40 120.20(17) . . ?
C35 C36 C37 120.57(17) . . ?
C35 C36 C12 120.32(17) . . ?
C37 C36 C12 118.99(16) . . ?
C38 C37 C36 119.71(17) . . ?
C38 C37 C42 120.29(17) . . ?
C36 C37 C42 119.96(17) . . ?
C39 C38 C37 119.77(17) . . ?
C39 C38 C19 120.27(17) . . ?
C37 C38 C19 119.78(17) . . ?
C38 C39 C34 120.21(17) . . ?
C38 C39 C44 120.32(18) . . ?
C34 C39 C44 119.42(17) . . ?
C35 C40 C41 111.33(16) . . ?
C37 C42 C43 113.96(16) . . ?
C39 C44 C45 110.29(17) . . ?
C46 O1 C49 108.4(2) . . ?
O1 C46 C47 107.3(2) . . ?
C46 C47 C48 102.7(3) . . ?
C49 C48 C47 104.1(3) . . ?
O1 C49 C48 108.2(2) . . ?
C53 O2 C50 106.8(4) . . ?
C53 O2 Fe3 135.2(3) . . ?
C50 O2 Fe3 117.7(3) . . ?
O2 C50 C51 104.7(4) . . ?
C50 C51 C52 103.1(4) . . ?
C51 C52 C53 103.3(4) . . ?
O2 C53 C52 105.9(4) . . ?

_refine_diff_density_max         0.931
_refine_diff_density_min         -0.544
_refine_diff_density_rms         0.071

_shelxl_version_number           2014/6


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'hexanes and tetrahydrofuran'
_chemical_compound_source        n/a
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
