# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_asb444
_database_code_depnum_ccdc_archive 'CCDC 1554806'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Fe(II)(Br)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H64 Br Cl2 Fe2 N6 O7 S3'
_chemical_formula_weight         1099.66

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   21.7773(13)
_cell_length_b                   13.2666(8)
_cell_length_c                   17.6201(11)
_cell_angle_alpha                90
_cell_angle_beta                 107.4513(8)
_cell_angle_gamma                90
_cell_volume                     4856.3(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9585
_cell_measurement_theta_min      2.33
_cell_measurement_theta_max      28.92

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.504
_exptl_crystal_F_000             2284
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.395
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.256
_exptl_absorpt_coefficient_mu    1.711
_shelx_estimated_absorpt_T_min   0.551
_shelx_estimated_absorpt_T_max   0.668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6676
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58750
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0266
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.821
_diffrn_reflns_theta_max         29.005
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12173
_reflns_number_gt                10639
_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 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;

A red crystal of approximate dimensions 0.395 x 0.298 x 0.256 mm was mounted in a cryoloop and transferred to a Bruker 
SMART APEX II diffractometer.  The APEX2 program package was used to determine the unit-cell parameters and for data 
collection (25 sec/frame scan time for a sphere of diffraction data).  The raw frame data was processed using SAINT 
and SADABS to yield the reflection data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent with the monoclinic space group P21/c 
that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix least-squares techniques.  The analytical 
scattering factors for neutral atoms were used throughout the analysis.  Hydrogen atom H1 was located from a 
difference-Fourier map and refined (x,y,z and Uiso). The remaining hydrogen atoms were included using a riding model. 
There was one molecule of dichloromethane present that was disordered over two positions (0.50:0.50). The 
tetramethylethylenediamine ligand was disordered over two positions (0.70:0.30).

At convergence, wR2 = 0.0745 and Goof = 1.039 for 613 variables refined against 12173 data (0.73 Å), R1 = 0.0290 for 
those 10639 data with I > 2.0sigma(I).  
  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0342P)²+4.4924P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12173
_refine_ls_number_parameters     613
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0361
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0745
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_restrained_S_all      1.039
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.22252(2) 0.45733(2) 0.57869(2) 0.01864(5) Uani 1 1 d . . . . .
Fe1 Fe 0.25155(2) 0.43163(2) 0.28191(2) 0.00981(5) Uani 1 1 d . . . . .
Fe2 Fe 0.28642(2) 0.47936(2) 0.48473(2) 0.01399(6) Uani 1 1 d . . . . .
S1 S 0.37837(2) 0.52753(3) 0.24268(2) 0.01278(8) Uani 1 1 d . . . . .
S2 S 0.26385(2) 0.23606(3) 0.39316(2) 0.01193(8) Uani 1 1 d . . . . .
S3 S 0.14565(2) 0.57559(3) 0.32442(2) 0.01177(8) Uani 1 1 d . . . . .
O1 O 0.30402(6) 0.48088(9) 0.38062(7) 0.0136(2) Uani 1 1 d D . . . .
H1 H 0.3387(10) 0.499(2) 0.3744(17) 0.01 Uiso 1 1 d D . . . .
O2 O 0.40390(6) 0.52719(10) 0.32904(7) 0.0176(3) Uani 1 1 d . . . . .
O3 O 0.37000(6) 0.62601(9) 0.20627(8) 0.0188(3) Uani 1 1 d . . . . .
O4 O 0.26475(6) 0.31468(9) 0.45112(7) 0.0156(2) Uani 1 1 d . . . . .
O5 O 0.32270(6) 0.17963(10) 0.40727(8) 0.0189(3) Uani 1 1 d . . . . .
O6 O 0.19960(6) 0.58590(9) 0.39595(7) 0.0162(2) Uani 1 1 d . . . . .
O7 O 0.08700(6) 0.53601(9) 0.33495(8) 0.0171(3) Uani 1 1 d . . . . .
N1 N 0.19627(7) 0.37152(11) 0.16133(8) 0.0125(3) Uani 1 1 d . . . . .
N2 N 0.31278(7) 0.46386(11) 0.21715(8) 0.0127(3) Uani 1 1 d . . . . .
N3 N 0.24148(7) 0.28694(10) 0.30711(8) 0.0125(3) Uani 1 1 d . . . . .
N4 N 0.16857(7) 0.50703(11) 0.26264(8) 0.0121(3) Uani 1 1 d . . . . .
N5 N 0.38392(8) 0.42295(13) 0.55938(9) 0.0212(3) Uani 1 1 d . . . . .
N6 N 0.33031(8) 0.62779(12) 0.53218(9) 0.0234(3) Uani 1 1 d . . . . .
C1 C 0.24006(8) 0.36759(14) 0.11121(10) 0.0150(3) Uani 1 1 d . . . . .
H1A H 0.2146 0.3684 0.0543 0.018 Uiso 1 1 calc R U . . .
H1B H 0.2653 0.3044 0.1219 0.018 Uiso 1 1 calc R U . . .
C2 C 0.28515(8) 0.45730(14) 0.12947(10) 0.0159(3) Uani 1 1 d . . . . .
H2A H 0.3199 0.4484 0.1045 0.019 Uiso 1 1 calc R U . . .
H2B H 0.2613 0.5198 0.1084 0.019 Uiso 1 1 calc R U . . .
C3 C 0.17352(8) 0.26863(13) 0.17296(10) 0.0149(3) Uani 1 1 d . . . . .
H3A H 0.1650 0.2294 0.1231 0.018 Uiso 1 1 calc R U . . .
H3B H 0.1330 0.2730 0.1874 0.018 Uiso 1 1 calc R U . . .
C4 C 0.22516(9) 0.21687(13) 0.23900(10) 0.0154(3) Uani 1 1 d . . . . .
H4A H 0.2088 0.1524 0.2537 0.019 Uiso 1 1 calc R U . . .
H4B H 0.2636 0.2028 0.2217 0.019 Uiso 1 1 calc R U . . .
C5 C 0.14245(8) 0.44249(13) 0.12785(10) 0.0154(3) Uani 1 1 d . . . . .
H5A H 0.1084 0.4086 0.0853 0.018 Uiso 1 1 calc R U . . .
H5B H 0.1581 0.5011 0.1042 0.018 Uiso 1 1 calc R U . . .
C6 C 0.11473(8) 0.47832(14) 0.19277(10) 0.0156(3) Uani 1 1 d . . . . .
H6A H 0.0861 0.5369 0.1738 0.019 Uiso 1 1 calc R U . . .
H6B H 0.0892 0.4238 0.2071 0.019 Uiso 1 1 calc R U . . .
C7 C 0.43556(8) 0.46042(13) 0.20688(10) 0.0131(3) Uani 1 1 d . . . . .
C8 C 0.45921(9) 0.50123(14) 0.14708(10) 0.0162(3) Uani 1 1 d . . . . .
C9 C 0.50943(9) 0.45061(15) 0.12947(12) 0.0218(4) Uani 1 1 d . . . . .
H9 H 0.5264 0.4780 0.0902 0.026 Uiso 1 1 calc R U . . .
C10 C 0.53550(10) 0.36172(16) 0.16710(12) 0.0242(4) Uani 1 1 d . . . . .
C11 C 0.50906(9) 0.32082(14) 0.22291(11) 0.0197(4) Uani 1 1 d . . . . .
H11 H 0.5257 0.2589 0.2478 0.024 Uiso 1 1 calc R U . . .
C12 C 0.45910(8) 0.36746(13) 0.24364(10) 0.0149(3) Uani 1 1 d . . . . .
C13 C 0.43369(9) 0.59377(14) 0.09755(11) 0.0208(4) Uani 1 1 d . . . . .
H13A H 0.3869 0.5882 0.0747 0.031 Uiso 1 1 calc R U . . .
H13B H 0.4535 0.5991 0.0546 0.031 Uiso 1 1 calc R U . . .
H13C H 0.4441 0.6539 0.1313 0.031 Uiso 1 1 calc R U . . .
C14 C 0.58931(13) 0.3095(2) 0.14588(17) 0.0442(7) Uani 1 1 d . . . . .
H14A H 0.5741 0.2869 0.0904 0.066 Uiso 1 1 calc R U . . .
H14B H 0.6036 0.2511 0.1808 0.066 Uiso 1 1 calc R U . . .
H14C H 0.6253 0.3564 0.1526 0.066 Uiso 1 1 calc R U . . .
C15 C 0.43320(9) 0.31446(14) 0.30361(11) 0.0192(4) Uani 1 1 d . . . . .
H15A H 0.4485 0.3491 0.3550 0.029 Uiso 1 1 calc R U . . .
H15B H 0.4483 0.2445 0.3097 0.029 Uiso 1 1 calc R U . . .
H15C H 0.3860 0.3155 0.2850 0.029 Uiso 1 1 calc R U . . .
C16 C 0.20107(8) 0.15082(12) 0.39712(9) 0.0122(3) Uani 1 1 d . . . . .
C17 C 0.21073(8) 0.04504(13) 0.40215(10) 0.0135(3) Uani 1 1 d . . . . .
C18 C 0.16120(9) -0.01523(13) 0.41244(10) 0.0156(3) Uani 1 1 d . . . . .
H18 H 0.1673 -0.0861 0.4168 0.019 Uiso 1 1 calc R U . . .
C19 C 0.10320(9) 0.02479(13) 0.41661(10) 0.0162(3) Uani 1 1 d . . . . .
C20 C 0.09432(8) 0.12845(13) 0.40844(10) 0.0151(3) Uani 1 1 d . . . . .
H20 H 0.0544 0.1562 0.4097 0.018 Uiso 1 1 calc R U . . .
C21 C 0.14174(8) 0.19313(13) 0.39846(9) 0.0136(3) Uani 1 1 d . . . . .
C22 C 0.27063(9) -0.00927(14) 0.39651(12) 0.0197(4) Uani 1 1 d . . . . .
H22A H 0.2803 0.0119 0.3480 0.029 Uiso 1 1 calc R U . . .
H22B H 0.2632 -0.0822 0.3948 0.029 Uiso 1 1 calc R U . . .
H22C H 0.3071 0.0074 0.4430 0.029 Uiso 1 1 calc R U . . .
C23 C 0.05095(9) -0.04198(15) 0.42897(12) 0.0222(4) Uani 1 1 d . . . . .
H23A H 0.0655 -0.0717 0.4823 0.033 Uiso 1 1 calc R U . . .
H23B H 0.0413 -0.0958 0.3890 0.033 Uiso 1 1 calc R U . . .
H23C H 0.0121 -0.0018 0.4236 0.033 Uiso 1 1 calc R U . . .
C24 C 0.12604(9) 0.30426(13) 0.39077(11) 0.0172(3) Uani 1 1 d . . . . .
H24A H 0.1485 0.3385 0.4407 0.026 Uiso 1 1 calc R U . . .
H24B H 0.0795 0.3135 0.3793 0.026 Uiso 1 1 calc R U . . .
H24C H 0.1400 0.3329 0.3474 0.026 Uiso 1 1 calc R U . . .
C25 C 0.12811(8) 0.69881(12) 0.28037(9) 0.0119(3) Uani 1 1 d . . . . .
C26 C 0.06785(8) 0.74638(13) 0.27092(10) 0.0132(3) Uani 1 1 d . . . . .
C27 C 0.05967(8) 0.84464(13) 0.24157(10) 0.0143(3) Uani 1 1 d . . . . .
H27 H 0.0194 0.8767 0.2347 0.017 Uiso 1 1 calc R U . . .
C28 C 0.10770(8) 0.89793(13) 0.22183(10) 0.0138(3) Uani 1 1 d . . . . .
C29 C 0.16548(8) 0.84822(13) 0.22896(10) 0.0144(3) Uani 1 1 d . . . . .
H29 H 0.1984 0.8827 0.2142 0.017 Uiso 1 1 calc R U . . .
C30 C 0.17673(8) 0.74956(13) 0.25698(10) 0.0129(3) Uani 1 1 d . . . . .
C31 C 0.01042(8) 0.70005(14) 0.28911(11) 0.0182(4) Uani 1 1 d . . . . .
H31A H -0.0006 0.6361 0.2604 0.027 Uiso 1 1 calc R U . . .
H31B H -0.0263 0.7462 0.2723 0.027 Uiso 1 1 calc R U . . .
H31C H 0.0209 0.6878 0.3464 0.027 Uiso 1 1 calc R U . . .
C32 C 0.09713(9) 1.00609(13) 0.19504(11) 0.0173(3) Uani 1 1 d . . . . .
H32A H 0.1033 1.0499 0.2415 0.026 Uiso 1 1 calc R U . . .
H32B H 0.0532 1.0142 0.1594 0.026 Uiso 1 1 calc R U . . .
H32C H 0.1280 1.0245 0.1668 0.026 Uiso 1 1 calc R U . . .
C33 C 0.24012(8) 0.70298(14) 0.25712(11) 0.0178(3) Uani 1 1 d . . . . .
H33A H 0.2571 0.6624 0.3054 0.027 Uiso 1 1 calc R U . . .
H33B H 0.2709 0.7565 0.2559 0.027 Uiso 1 1 calc R U . . .
H33C H 0.2335 0.6599 0.2102 0.027 Uiso 1 1 calc R U . . .
C40 C 0.41697(11) 0.5116(2) 0.60403(15) 0.0382(6) Uani 1 1 d . . . . .
H40A H 0.4039 0.5195 0.6529 0.046 Uiso 0.7 1 calc R U P A 1
H40B H 0.4640 0.4998 0.6204 0.046 Uiso 0.7 1 calc R U P A 1
H40C H 0.4507 0.5331 0.5802 0.046 Uiso 0.3 1 calc R U P B 2
H40D H 0.4391 0.4900 0.6592 0.046 Uiso 0.3 1 calc R U P B 2
C41 C 0.42287(9) 0.38117(17) 0.51131(13) 0.0274(4) Uani 1 1 d . . . . .
H41A H 0.4003 0.3237 0.4803 0.041 Uiso 1 1 calc R U . . .
H41B H 0.4646 0.3588 0.5465 0.041 Uiso 1 1 calc R U . . .
H41C H 0.4296 0.4332 0.4751 0.041 Uiso 1 1 calc R U . . .
C42 C 0.37827(12) 0.3425(2) 0.61545(15) 0.0445(7) Uani 1 1 d . . . . .
H42A H 0.3524 0.3671 0.6485 0.067 Uiso 1 1 calc R U . . .
H42B H 0.4213 0.3240 0.6495 0.067 Uiso 1 1 calc R U . . .
H42C H 0.3574 0.2833 0.5853 0.067 Uiso 1 1 calc R U . . .
C35 C 0.3210(2) 0.7052(3) 0.4698(3) 0.0246(8) Uani 0.7 1 d . . P C 1
H35A H 0.3354 0.6787 0.4260 0.037 Uiso 0.7 1 calc R U P C 1
H35B H 0.3462 0.7653 0.4920 0.037 Uiso 0.7 1 calc R U P C 1
H35C H 0.2753 0.7229 0.4498 0.037 Uiso 0.7 1 calc R U P C 1
C37 C 0.31293(17) 0.6669(2) 0.59891(19) 0.0285(7) Uani 0.7 1 d . . P C 1
H37A H 0.3217 0.6160 0.6411 0.043 Uiso 0.7 1 calc R U P C 1
H37B H 0.2670 0.6838 0.5823 0.043 Uiso 0.7 1 calc R U P C 1
H37C H 0.3382 0.7276 0.6189 0.043 Uiso 0.7 1 calc R U P C 1
C39 C 0.40304(13) 0.6026(2) 0.55903(17) 0.0245(6) Uani 0.7 1 d . . P C 1
H39A H 0.4181 0.5961 0.5115 0.029 Uiso 0.7 1 calc R U P C 1
H39B H 0.4270 0.6588 0.5917 0.029 Uiso 0.7 1 calc R U P C 1
C34 C 0.3485(5) 0.6850(7) 0.4762(6) 0.029(2) Uani 0.3 1 d . . P C 2
H34A H 0.3787 0.6462 0.4562 0.044 Uiso 0.3 1 calc R U P C 2
H34B H 0.3693 0.7472 0.5011 0.044 Uiso 0.3 1 calc R U P C 2
H34C H 0.3104 0.7017 0.4319 0.044 Uiso 0.3 1 calc R U P C 2
C36 C 0.2757(4) 0.7016(5) 0.5537(4) 0.0283(15) Uani 0.3 1 d . . P C 2
H36A H 0.2548 0.6645 0.5873 0.042 Uiso 0.3 1 calc R U P C 2
H36B H 0.2433 0.7220 0.5043 0.042 Uiso 0.3 1 calc R U P C 2
H36C H 0.2970 0.7617 0.5821 0.042 Uiso 0.3 1 calc R U P C 2
C38 C 0.3738(4) 0.6081(5) 0.6080(4) 0.0299(16) Uani 0.3 1 d . . P C 2
H38A H 0.3496 0.5956 0.6465 0.036 Uiso 0.3 1 calc R U P C 2
H38B H 0.4019 0.6674 0.6264 0.036 Uiso 0.3 1 calc R U P C 2
Cl1B Cl -0.0075(2) 0.6360(5) 0.5050(3) 0.0707(14) Uani 0.5 1 d . . P D 1
Cl2B Cl 0.1197(3) 0.7340(5) 0.5278(4) 0.1063(19) Uani 0.5 1 d . . P D 1
C43B C 0.0722(2) 0.6110(4) 0.5081(3) 0.0290(10) Uiso 0.5 1 d . . P D 1
H43A H 0.0733 0.5818 0.4568 0.035 Uiso 0.5 1 calc R U P D 1
H43B H 0.0916 0.5618 0.5508 0.035 Uiso 0.5 1 calc R U P D 1
Cl1 Cl 0.0096(2) 0.6619(5) 0.5112(3) 0.0567(10) Uani 0.5 1 d . . P E 2
Cl2 Cl 0.1321(3) 0.7372(3) 0.5165(3) 0.0561(6) Uani 0.5 1 d . . P E 2
C43 C 0.0909(2) 0.6371(4) 0.5158(3) 0.0247(9) Uiso 0.5 1 d . . P E 2
H43C H 0.1115 0.5977 0.5644 0.030 Uiso 0.5 1 calc R U P E 2
H43D H 0.0915 0.5954 0.4694 0.030 Uiso 0.5 1 calc R U P E 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 2.4789(3) . ?
Fe1 O1 1.8884(12) . ?
Fe1 N3 1.9971(14) . ?
Fe1 N4 2.0033(14) . ?
Fe1 N2 2.0434(14) . ?
Fe1 N1 2.2506(14) . ?
Fe2 O1 1.9834(12) . ?
Fe2 N6 2.2384(16) . ?
Fe2 N5 2.2634(16) . ?
Fe2 O4 2.2758(12) . ?
Fe2 O6 2.4990(12) . ?
S1 O3 1.4429(13) . ?
S1 O2 1.4551(13) . ?
S1 N2 1.6033(15) . ?
S1 C7 1.7924(17) . ?
S2 O5 1.4401(13) . ?
S2 O4 1.4557(12) . ?
S2 N3 1.5965(14) . ?
S2 C16 1.7916(17) . ?
S3 O7 1.4435(13) . ?
S3 O6 1.4490(13) . ?
S3 N4 1.6085(14) . ?
S3 C25 1.8007(17) . ?
N1 C5 1.481(2) . ?
N1 C1 1.482(2) . ?
N1 C3 1.487(2) . ?
N2 C2 1.483(2) . ?
N3 C4 1.475(2) . ?
N4 C6 1.473(2) . ?
N5 C41 1.475(3) . ?
N5 C40 1.477(3) . ?
N5 C42 1.484(3) . ?
N6 C34 1.393(11) . ?
N6 C38 1.411(7) . ?
N6 C37 1.436(3) . ?
N6 C35 1.473(5) . ?
N6 C39 1.547(3) . ?
N6 C36 1.669(7) . ?
C1 C2 1.515(2) . ?
C3 C4 1.518(2) . ?
C5 C6 1.521(2) . ?
C7 C8 1.412(2) . ?
C7 C12 1.416(2) . ?
C8 C9 1.395(3) . ?
C8 C13 1.512(2) . ?
C9 C10 1.388(3) . ?
C10 C11 1.390(3) . ?
C10 C14 1.502(3) . ?
C11 C12 1.392(2) . ?
C12 C15 1.512(2) . ?
C16 C21 1.415(2) . ?
C16 C17 1.418(2) . ?
C17 C18 1.397(2) . ?
C17 C22 1.519(2) . ?
C18 C19 1.392(3) . ?
C19 C20 1.390(2) . ?
C19 C23 1.508(2) . ?
C20 C21 1.394(2) . ?
C21 C24 1.510(2) . ?
C25 C30 1.416(2) . ?
C25 C26 1.420(2) . ?
C26 C27 1.394(2) . ?
C26 C31 1.512(2) . ?
C27 C28 1.390(2) . ?
C28 C29 1.393(2) . ?
C28 C32 1.507(2) . ?
C29 C30 1.394(2) . ?
C30 C33 1.512(2) . ?
C40 C39 1.426(4) . ?
C40 C38 1.601(8) . ?
Cl1B C43B 1.752(7) . ?
Cl2B C43B 1.907(9) . ?
Cl1 C43 1.778(7) . ?
Cl2 C43 1.600(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
O1 Fe1 N3 101.79(5) . . ?
O1 Fe1 N4 104.44(6) . . ?
N3 Fe1 N4 111.35(6) . . ?
O1 Fe1 N2 97.23(6) . . ?
N3 Fe1 N2 117.31(6) . . ?
N4 Fe1 N2 120.49(6) . . ?
O1 Fe1 N1 175.38(5) . . ?
N3 Fe1 N1 78.81(5) . . ?
N4 Fe1 N1 79.46(5) . . ?
N2 Fe1 N1 78.52(5) . . ?
O1 Fe2 N6 99.05(6) . . ?
O1 Fe2 N5 97.64(6) . . ?
N6 Fe2 N5 81.53(6) . . ?
O1 Fe2 O4 81.46(5) . . ?
N6 Fe2 O4 166.83(6) . . ?
N5 Fe2 O4 85.35(5) . . ?
O1 Fe2 Br1 157.19(4) . . ?
N6 Fe2 Br1 96.70(4) . . ?
N5 Fe2 Br1 100.93(4) . . ?
O4 Fe2 Br1 86.93(3) . . ?
O1 Fe2 O6 74.64(5) . . ?
N6 Fe2 O6 83.94(5) . . ?
N5 Fe2 O6 162.27(5) . . ?
O4 Fe2 O6 108.73(4) . . ?
Br1 Fe2 O6 90.80(3) . . ?
O3 S1 O2 115.18(8) . . ?
O3 S1 N2 111.66(8) . . ?
O2 S1 N2 108.70(7) . . ?
O3 S1 C7 107.57(8) . . ?
O2 S1 C7 106.18(8) . . ?
N2 S1 C7 107.11(8) . . ?
O5 S2 O4 115.30(8) . . ?
O5 S2 N3 112.70(8) . . ?
O4 S2 N3 107.42(7) . . ?
O5 S2 C16 108.37(8) . . ?
O4 S2 C16 105.96(8) . . ?
N3 S2 C16 106.54(8) . . ?
O7 S3 O6 116.14(8) . . ?
O7 S3 N4 110.33(8) . . ?
O6 S3 N4 107.86(7) . . ?
O7 S3 C25 107.71(8) . . ?
O6 S3 C25 107.52(8) . . ?
N4 S3 C25 106.88(7) . . ?
Fe1 O1 Fe2 128.09(7) . . ?
S2 O4 Fe2 145.95(8) . . ?
S3 O6 Fe2 139.03(8) . . ?
C5 N1 C1 111.02(13) . . ?
C5 N1 C3 112.45(13) . . ?
C1 N1 C3 110.50(13) . . ?
C5 N1 Fe1 106.62(10) . . ?
C1 N1 Fe1 108.50(10) . . ?
C3 N1 Fe1 107.53(10) . . ?
C2 N2 S1 111.85(11) . . ?
C2 N2 Fe1 116.14(10) . . ?
S1 N2 Fe1 128.99(8) . . ?
C4 N3 S2 115.90(11) . . ?
C4 N3 Fe1 116.14(10) . . ?
S2 N3 Fe1 126.51(8) . . ?
C6 N4 S3 112.40(11) . . ?
C6 N4 Fe1 117.64(10) . . ?
S3 N4 Fe1 127.95(8) . . ?
C41 N5 C40 109.44(17) . . ?
C41 N5 C42 106.79(18) . . ?
C40 N5 C42 110.03(19) . . ?
C41 N5 Fe2 113.04(12) . . ?
C40 N5 Fe2 105.57(13) . . ?
C42 N5 Fe2 111.96(13) . . ?
C34 N6 C38 121.2(6) . . ?
C37 N6 C35 110.4(3) . . ?
C37 N6 C39 108.9(2) . . ?
C35 N6 C39 106.1(2) . . ?
C34 N6 C36 102.4(5) . . ?
C38 N6 C36 102.5(4) . . ?
C34 N6 Fe2 113.3(4) . . ?
C38 N6 Fe2 106.3(3) . . ?
C37 N6 Fe2 115.84(15) . . ?
C35 N6 Fe2 112.74(19) . . ?
C39 N6 Fe2 101.97(14) . . ?
C36 N6 Fe2 110.3(3) . . ?
N1 C1 C2 109.74(14) . . ?
N2 C2 C1 107.58(13) . . ?
N1 C3 C4 108.66(13) . . ?
N3 C4 C3 106.32(14) . . ?
N1 C5 C6 110.14(14) . . ?
N4 C6 C5 108.27(14) . . ?
C8 C7 C12 120.82(15) . . ?
C8 C7 S1 121.30(13) . . ?
C12 C7 S1 117.79(13) . . ?
C9 C8 C7 117.84(16) . . ?
C9 C8 C13 116.07(16) . . ?
C7 C8 C13 126.06(16) . . ?
C10 C9 C8 122.56(17) . . ?
C9 C10 C11 118.20(17) . . ?
C9 C10 C14 120.72(18) . . ?
C11 C10 C14 121.04(18) . . ?
C10 C11 C12 122.28(17) . . ?
C11 C12 C7 118.13(16) . . ?
C11 C12 C15 117.47(16) . . ?
C7 C12 C15 124.40(16) . . ?
C21 C16 C17 120.70(15) . . ?
C21 C16 S2 117.47(12) . . ?
C17 C16 S2 121.77(13) . . ?
C18 C17 C16 117.94(16) . . ?
C18 C17 C22 116.65(15) . . ?
C16 C17 C22 125.41(16) . . ?
C19 C18 C17 122.44(16) . . ?
C20 C19 C18 118.17(16) . . ?
C20 C19 C23 120.54(17) . . ?
C18 C19 C23 121.28(16) . . ?
C19 C20 C21 122.46(16) . . ?
C20 C21 C16 118.20(15) . . ?
C20 C21 C24 117.12(15) . . ?
C16 C21 C24 124.68(15) . . ?
C30 C25 C26 119.98(15) . . ?
C30 C25 S3 118.46(12) . . ?
C26 C25 S3 121.54(13) . . ?
C27 C26 C25 118.02(15) . . ?
C27 C26 C31 115.92(15) . . ?
C25 C26 C31 126.06(15) . . ?
C28 C27 C26 123.12(16) . . ?
C27 C28 C29 117.63(16) . . ?
C27 C28 C32 120.47(15) . . ?
C29 C28 C32 121.90(16) . . ?
C28 C29 C30 122.32(16) . . ?
C29 C30 C25 118.81(15) . . ?
C29 C30 C33 116.59(15) . . ?
C25 C30 C33 124.55(15) . . ?
C39 C40 N5 112.9(2) . . ?
N5 C40 C38 117.4(3) . . ?
C40 C39 N6 112.4(2) . . ?
N6 C38 C40 110.1(5) . . ?
Cl1B C43B Cl2B 108.7(4) . . ?
Cl2 C43 Cl1 113.3(4) . . ?

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
N3 Fe1 O1 Fe2 -58.20(9) . . . . ?
N4 Fe1 O1 Fe2 57.75(9) . . . . ?
N2 Fe1 O1 Fe2 -178.14(8) . . . . ?
O5 S2 O4 Fe2 89.52(15) . . . . ?
N3 S2 O4 Fe2 -37.05(16) . . . . ?
C16 S2 O4 Fe2 -150.63(13) . . . . ?
O7 S3 O6 Fe2 81.57(12) . . . . ?
N4 S3 O6 Fe2 -42.81(13) . . . . ?
C25 S3 O6 Fe2 -157.76(10) . . . . ?
O3 S1 N2 C2 54.16(14) . . . . ?
O2 S1 N2 C2 -177.69(11) . . . . ?
C7 S1 N2 C2 -63.36(13) . . . . ?
O3 S1 N2 Fe1 -105.16(11) . . . . ?
O2 S1 N2 Fe1 22.99(13) . . . . ?
C7 S1 N2 Fe1 137.32(10) . . . . ?
O5 S2 N3 C4 63.44(14) . . . . ?
O4 S2 N3 C4 -168.48(12) . . . . ?
C16 S2 N3 C4 -55.29(14) . . . . ?
O5 S2 N3 Fe1 -102.22(11) . . . . ?
O4 S2 N3 Fe1 25.85(12) . . . . ?
C16 S2 N3 Fe1 139.04(10) . . . . ?
O7 S3 N4 C6 43.18(14) . . . . ?
O6 S3 N4 C6 170.98(12) . . . . ?
C25 S3 N4 C6 -73.66(13) . . . . ?
O7 S3 N4 Fe1 -120.10(10) . . . . ?
O6 S3 N4 Fe1 7.70(13) . . . . ?
C25 S3 N4 Fe1 123.06(10) . . . . ?
C5 N1 C1 C2 80.11(16) . . . . ?
C3 N1 C1 C2 -154.40(14) . . . . ?
Fe1 N1 C1 C2 -36.75(15) . . . . ?
S1 N2 C2 C1 159.22(12) . . . . ?
Fe1 N2 C2 C1 -38.59(17) . . . . ?
N1 C1 C2 N2 48.70(18) . . . . ?
C5 N1 C3 C4 -153.91(14) . . . . ?
C1 N1 C3 C4 81.42(16) . . . . ?
Fe1 N1 C3 C4 -36.83(15) . . . . ?
S2 N3 C4 C3 149.16(12) . . . . ?
Fe1 N3 C4 C3 -43.65(16) . . . . ?
N1 C3 C4 N3 51.57(17) . . . . ?
C1 N1 C5 C6 -157.04(14) . . . . ?
C3 N1 C5 C6 78.56(17) . . . . ?
Fe1 N1 C5 C6 -39.05(15) . . . . ?
S3 N4 C6 C5 163.09(12) . . . . ?
Fe1 N4 C6 C5 -31.75(18) . . . . ?
N1 C5 C6 N4 46.57(19) . . . . ?
O3 S1 C7 C8 -6.07(17) . . . . ?
O2 S1 C7 C8 -129.89(14) . . . . ?
N2 S1 C7 C8 114.10(15) . . . . ?
O3 S1 C7 C12 170.44(13) . . . . ?
O2 S1 C7 C12 46.63(15) . . . . ?
N2 S1 C7 C12 -69.39(15) . . . . ?
C12 C7 C8 C9 -4.3(3) . . . . ?
S1 C7 C8 C9 172.09(14) . . . . ?
C12 C7 C8 C13 173.45(17) . . . . ?
S1 C7 C8 C13 -10.1(3) . . . . ?
C7 C8 C9 C10 1.4(3) . . . . ?
C13 C8 C9 C10 -176.62(19) . . . . ?
C8 C9 C10 C11 1.7(3) . . . . ?
C8 C9 C10 C14 179.6(2) . . . . ?
C9 C10 C11 C12 -2.0(3) . . . . ?
C14 C10 C11 C12 -179.9(2) . . . . ?
C10 C11 C12 C7 -0.9(3) . . . . ?
C10 C11 C12 C15 178.53(18) . . . . ?
C8 C7 C12 C11 4.1(3) . . . . ?
S1 C7 C12 C11 -172.44(14) . . . . ?
C8 C7 C12 C15 -175.27(17) . . . . ?
S1 C7 C12 C15 8.2(2) . . . . ?
O5 S2 C16 C21 169.36(12) . . . . ?
O4 S2 C16 C21 45.08(14) . . . . ?
N3 S2 C16 C21 -69.11(14) . . . . ?
O5 S2 C16 C17 -8.01(16) . . . . ?
O4 S2 C16 C17 -132.29(14) . . . . ?
N3 S2 C16 C17 113.52(14) . . . . ?
C21 C16 C17 C18 -3.1(2) . . . . ?
S2 C16 C17 C18 174.15(12) . . . . ?
C21 C16 C17 C22 176.25(16) . . . . ?
S2 C16 C17 C22 -6.5(2) . . . . ?
C16 C17 C18 C19 1.0(3) . . . . ?
C22 C17 C18 C19 -178.45(16) . . . . ?
C17 C18 C19 C20 1.4(3) . . . . ?
C17 C18 C19 C23 -179.09(16) . . . . ?
C18 C19 C20 C21 -1.8(3) . . . . ?
C23 C19 C20 C21 178.74(16) . . . . ?
C19 C20 C21 C16 -0.3(2) . . . . ?
C19 C20 C21 C24 -179.65(16) . . . . ?
C17 C16 C21 C20 2.8(2) . . . . ?
S2 C16 C21 C20 -174.57(12) . . . . ?
C17 C16 C21 C24 -177.91(16) . . . . ?
S2 C16 C21 C24 4.7(2) . . . . ?
O7 S3 C25 C30 -173.99(13) . . . . ?
O6 S3 C25 C30 60.16(14) . . . . ?
N4 S3 C25 C30 -55.43(15) . . . . ?
O7 S3 C25 C26 7.79(16) . . . . ?
O6 S3 C25 C26 -118.06(14) . . . . ?
N4 S3 C25 C26 126.35(14) . . . . ?
C30 C25 C26 C27 -2.7(2) . . . . ?
S3 C25 C26 C27 175.49(12) . . . . ?
C30 C25 C26 C31 176.70(16) . . . . ?
S3 C25 C26 C31 -5.1(2) . . . . ?
C25 C26 C27 C28 -0.5(2) . . . . ?
C31 C26 C27 C28 -179.93(16) . . . . ?
C26 C27 C28 C29 2.7(2) . . . . ?
C26 C27 C28 C32 -176.32(16) . . . . ?
C27 C28 C29 C30 -1.9(2) . . . . ?
C32 C28 C29 C30 177.16(16) . . . . ?
C28 C29 C30 C25 -1.2(3) . . . . ?
C28 C29 C30 C33 176.58(16) . . . . ?
C26 C25 C30 C29 3.5(2) . . . . ?
S3 C25 C30 C29 -174.75(12) . . . . ?
C26 C25 C30 C33 -174.06(16) . . . . ?
S3 C25 C30 C33 7.7(2) . . . . ?
C41 N5 C40 C39 85.5(2) . . . . ?
C42 N5 C40 C39 -157.4(2) . . . . ?
Fe2 N5 C40 C39 -36.4(2) . . . . ?
C41 N5 C40 C38 137.6(4) . . . . ?
C42 N5 C40 C38 -105.3(4) . . . . ?
Fe2 N5 C40 C38 15.6(4) . . . . ?
N5 C40 C39 N6 59.7(3) . . . . ?
C37 N6 C39 C40 76.2(3) . . . . ?
C35 N6 C39 C40 -164.9(3) . . . . ?
Fe2 N6 C39 C40 -46.7(2) . . . . ?
C34 N6 C38 C40 -85.1(7) . . . . ?
C36 N6 C38 C40 161.9(4) . . . . ?
Fe2 N6 C38 C40 46.1(5) . . . . ?
N5 C40 C38 N6 -44.3(6) . . . . ?

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
O1 H1 O2 0.832(17) 1.863(19) 2.6683(17) 162(3) .

_refine_diff_density_max         0.771
_refine_diff_density_min         -0.669
_refine_diff_density_rms         0.069


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/Pentane'
####################################################################### 
# 
# 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_asb448
_database_code_depnum_ccdc_archive 'CCDC 1554809'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Fe(II)(N3)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C39 H62 Fe2 N9 O7 S3'
_chemical_formula_weight         976.85

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'
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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   34.1173(18)
_cell_length_b                   34.1173(18)
_cell_length_c                   21.0137(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     21183(2)
_cell_formula_units_Z            18
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9903
_cell_measurement_theta_min      2.38
_cell_measurement_theta_max      28.72

_exptl_crystal_description       irregular
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_F_000             9270
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.305
_exptl_crystal_size_mid          0.196
_exptl_crystal_size_min          0.152
_exptl_absorpt_coefficient_mu    0.804
_shelx_estimated_absorpt_T_min   0.791
_shelx_estimated_absorpt_T_max   0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6010
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            83277
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_av_R_equivalents  0.0620
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.685
_diffrn_reflns_theta_max         27.101
_diffrn_reflns_theta_full        25.500
_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             10386
_reflns_number_gt                8242
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
An orange crystal of approximate dimensions 0.152 x 0.196 x 0.305 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters 
and for data collection (25 sec/frame scan time for a sphere of diffraction 
data).  The raw frame data was processed using SAINT and SADABS to yield 
the reflection data file.  Subsequent calculations were carried out using the 
SHELXTL program.  The systematic absences were consistent with the hexagonal 
space groups R3 and R-3.  The centrosymmetric space group R-3 was assigned and 
later determined to be correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis. Hydrogen atoms H(1) was located from a 
difference-Fourier amp and refined (x,y,z and Uiso) with d(O-H) = 0.85Å.  The 
remaining hydrogen atoms were included using a riding model.  Atoms C(36) and 
C(37) were disordered and including using multiple components with partial 
site-occupancies-factors.

At convergence, wR2 = 0.0.0969 and Goof = 1.019 for 576 variables refined against 
10386 data (0.78 Å), R1 = 0.0358 for those 8242 data with I > 2.0sigma(I).

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that pentane and/or dichloromethane solvents were present.  The SQUEEZE 
routine in the PLATON program package was used to account for the electrons 
in the solvent accessible voids.  
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+56.3815P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10386
_refine_ls_number_parameters     576
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0358
_refine_ls_wR_factor_ref         0.0969
_refine_ls_wR_factor_gt          0.0879
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.019
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

# start Validation Reply Form
_vrf_PLAT412_asb448              
;
PROBLEM: Short Intra XH3 .. XHn     H34A   ..  H36C    ..       1.68 Ang.  
RESPONSE: ...The short contacts are due to disordered carbon atoms associated
with the hydrogens.
;
# end Validation Reply Form

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 0.20621(2) 0.40035(2) 0.53583(2) 0.01456(8) Uani 1 1 d . . . . .
Fe2 Fe 0.09998(2) 0.39105(2) 0.52633(2) 0.01785(8) Uani 1 1 d . . . . .
S1 S 0.24467(2) 0.43500(2) 0.39072(3) 0.02004(12) Uani 1 1 d . . . . .
S2 S 0.12123(2) 0.30117(2) 0.56943(3) 0.01718(11) Uani 1 1 d . . . . .
S3 S 0.19318(2) 0.46541(2) 0.63559(3) 0.01871(12) Uani 1 1 d . . . . .
O1 O 0.16025(5) 0.40555(5) 0.49347(7) 0.0180(3) Uani 1 1 d D . . . .
H1 H 0.1694(10) 0.4161(9) 0.4568(7) 0.040(9) Uiso 1 1 d D . . . .
O2 O 0.20590(5) 0.44203(6) 0.38906(7) 0.0246(4) Uani 1 1 d . . . . .
O3 O 0.24374(6) 0.40303(6) 0.34563(8) 0.0288(4) Uani 1 1 d . . . . .
O4 O 0.09801(5) 0.32396(5) 0.54571(8) 0.0231(3) Uani 1 1 d . . . . .
O5 O 0.10959(6) 0.28249(5) 0.63283(7) 0.0255(4) Uani 1 1 d . . . . .
O6 O 0.14780(5) 0.44078(6) 0.60883(7) 0.0223(3) Uani 1 1 d . . . . .
O7 O 0.21664(6) 0.51350(5) 0.62570(8) 0.0270(4) Uani 1 1 d . . . . .
N1 N 0.26437(6) 0.39668(6) 0.57780(9) 0.0184(4) Uani 1 1 d . . . . .
N2 N 0.25036(6) 0.42182(6) 0.46182(8) 0.0182(4) Uani 1 1 d . . . . .
N3 N 0.17438(6) 0.33518(6) 0.56444(9) 0.0180(4) Uani 1 1 d . . . . .
N4 N 0.22082(6) 0.44218(6) 0.60961(8) 0.0178(4) Uani 1 1 d . . . . .
N5 N 0.05935(8) 0.35593(8) 0.43984(11) 0.0364(5) Uani 1 1 d . . . . .
N6 N 0.09960(7) 0.45062(7) 0.47972(9) 0.0244(4) Uani 1 1 d . . . . .
N7 N 0.04827(7) 0.37292(7) 0.59076(10) 0.0258(4) Uani 1 1 d . . . . .
N8 N 0.01312(7) 0.36879(7) 0.59363(10) 0.0293(5) Uani 1 1 d . . . . .
N9 N -0.02299(8) 0.36435(10) 0.59875(14) 0.0540(7) Uani 1 1 d . . . . .
C1 C 0.30389(8) 0.42040(9) 0.53524(11) 0.0256(5) Uani 1 1 d . . . . .
H1A H 0.3249 0.4088 0.5424 0.031 Uiso 1 1 calc R U . . .
H1B H 0.3202 0.4532 0.5451 0.031 Uiso 1 1 calc R U . . .
C2 C 0.28896(8) 0.41328(8) 0.46680(11) 0.0230(5) Uani 1 1 d . . . . .
H2A H 0.3141 0.4344 0.4390 0.028 Uiso 1 1 calc R U . . .
H2B H 0.2794 0.3819 0.4535 0.028 Uiso 1 1 calc R U . . .
C3 C 0.25011(8) 0.34793(8) 0.58290(12) 0.0260(5) Uani 1 1 d . . . . .
H3A H 0.2693 0.3440 0.6145 0.031 Uiso 1 1 calc R U . . .
H3B H 0.2543 0.3369 0.5413 0.031 Uiso 1 1 calc R U . . .
C4 C 0.20131(8) 0.32064(8) 0.60272(11) 0.0243(5) Uani 1 1 d . . . . .
H4A H 0.1901 0.2880 0.5958 0.029 Uiso 1 1 calc R U . . .
H4B H 0.1983 0.3254 0.6485 0.029 Uiso 1 1 calc R U . . .
C5 C 0.27348(8) 0.41848(8) 0.64135(11) 0.0257(5) Uani 1 1 d . . . . .
H5A H 0.3051 0.4287 0.6542 0.031 Uiso 1 1 calc R U . . .
H5B H 0.2530 0.3965 0.6734 0.031 Uiso 1 1 calc R U . . .
C6 C 0.26593(7) 0.45854(8) 0.63829(11) 0.0225(5) Uani 1 1 d . . . . .
H6A H 0.2670 0.4706 0.6815 0.027 Uiso 1 1 calc R U . . .
H6B H 0.2896 0.4829 0.6119 0.027 Uiso 1 1 calc R U . . .
C7 C 0.29319(7) 0.48940(8) 0.37505(11) 0.0228(5) Uani 1 1 d . . . . .
C8 C 0.32463(8) 0.49536(9) 0.32659(11) 0.0272(5) Uani 1 1 d . . . . .
C9 C 0.35918(8) 0.53969(10) 0.31434(13) 0.0359(6) Uani 1 1 d . . . . .
H9 H 0.3803 0.5445 0.2815 0.043 Uiso 1 1 calc R U . . .
C10 C 0.36412(9) 0.57677(9) 0.34752(13) 0.0377(7) Uani 1 1 d . . . . .
C11 C 0.33346(9) 0.56966(9) 0.39550(13) 0.0319(6) Uani 1 1 d . . . . .
H11 H 0.3367 0.5949 0.4189 0.038 Uiso 1 1 calc R U . . .
C12 C 0.29808(8) 0.52678(8) 0.41060(11) 0.0265(5) Uani 1 1 d . . . . .
C13 C 0.32452(9) 0.45804(10) 0.28796(13) 0.0340(6) Uani 1 1 d . . . . .
H13A H 0.3261 0.4362 0.3166 0.051 Uiso 1 1 calc R U . . .
H13B H 0.3508 0.4710 0.2595 0.051 Uiso 1 1 calc R U . . .
H13C H 0.2967 0.4427 0.2627 0.051 Uiso 1 1 calc R U . . .
C14 C 0.40275(12) 0.62395(11) 0.33344(17) 0.0612(10) Uani 1 1 d . . . . .
H14A H 0.3952 0.6463 0.3495 0.092 Uiso 1 1 calc R U . . .
H14B H 0.4077 0.6277 0.2874 0.092 Uiso 1 1 calc R U . . .
H14C H 0.4303 0.6283 0.3544 0.092 Uiso 1 1 calc R U . . .
C15 C 0.26794(9) 0.52373(9) 0.46532(13) 0.0375(6) Uani 1 1 d . . . . .
H15A H 0.2374 0.5137 0.4494 0.056 Uiso 1 1 calc R U . . .
H15B H 0.2801 0.5535 0.4853 0.056 Uiso 1 1 calc R U . . .
H15C H 0.2668 0.5019 0.4967 0.056 Uiso 1 1 calc R U . . .
C16 C 0.10570(8) 0.25330(7) 0.51909(10) 0.0197(4) Uani 1 1 d . . . . .
C17 C 0.06589(9) 0.21296(8) 0.53571(12) 0.0285(5) Uani 1 1 d . . . . .
C18 C 0.05596(10) 0.17384(9) 0.50223(13) 0.0382(7) Uani 1 1 d . . . . .
H18 H 0.0294 0.1463 0.5130 0.046 Uiso 1 1 calc R U . . .
C19 C 0.08341(11) 0.17351(10) 0.45360(13) 0.0382(7) Uani 1 1 d . . . . .
C20 C 0.11977(9) 0.21433(10) 0.43534(12) 0.0327(6) Uani 1 1 d . . . . .
H20 H 0.1376 0.2148 0.4003 0.039 Uiso 1 1 calc R U . . .
C21 C 0.13152(8) 0.25496(9) 0.46613(11) 0.0251(5) Uani 1 1 d . . . . .
C22 C 0.03215(10) 0.20973(10) 0.58484(15) 0.0491(8) Uani 1 1 d . . . . .
H22A H 0.0422 0.2065 0.6272 0.074 Uiso 1 1 calc R U . . .
H22B H 0.0025 0.1834 0.5757 0.074 Uiso 1 1 calc R U . . .
H22C H 0.0299 0.2373 0.5835 0.074 Uiso 1 1 calc R U . . .
C23 C 0.07210(13) 0.13010(11) 0.41972(17) 0.0590(10) Uani 1 1 d . . . . .
H23A H 0.0886 0.1372 0.3793 0.089 Uiso 1 1 calc R U . . .
H23B H 0.0395 0.1127 0.4114 0.089 Uiso 1 1 calc R U . . .
H23C H 0.0809 0.1122 0.4464 0.089 Uiso 1 1 calc R U . . .
C24 C 0.16964(9) 0.29768(10) 0.43685(12) 0.0385(7) Uani 1 1 d . . . . .
H24A H 0.1629 0.3223 0.4409 0.058 Uiso 1 1 calc R U . . .
H24B H 0.1726 0.2924 0.3917 0.058 Uiso 1 1 calc R U . . .
H24C H 0.1980 0.3059 0.4590 0.058 Uiso 1 1 calc R U . . .
C25 C 0.18851(7) 0.45501(8) 0.71984(10) 0.0195(4) Uani 1 1 d . . . . .
C26 C 0.21470(8) 0.48924(8) 0.76445(11) 0.0233(5) Uani 1 1 d . . . . .
C27 C 0.21001(8) 0.47729(9) 0.82866(11) 0.0263(5) Uani 1 1 d . . . . .
H27 H 0.2270 0.5002 0.8591 0.032 Uiso 1 1 calc R U . . .
C28 C 0.18183(8) 0.43370(8) 0.85012(11) 0.0236(5) Uani 1 1 d . . . . .
C29 C 0.15670(8) 0.40076(8) 0.80525(11) 0.0221(5) Uani 1 1 d . . . . .
H29 H 0.1371 0.3707 0.8193 0.027 Uiso 1 1 calc R U . . .
C30 C 0.15913(7) 0.41012(8) 0.74067(11) 0.0205(5) Uani 1 1 d . . . . .
C31 C 0.24828(9) 0.53813(8) 0.74842(12) 0.0304(6) Uani 1 1 d . . . . .
H31A H 0.2714 0.5393 0.7196 0.046 Uiso 1 1 calc R U . . .
H31B H 0.2627 0.5547 0.7876 0.046 Uiso 1 1 calc R U . . .
H31C H 0.2324 0.5520 0.7278 0.046 Uiso 1 1 calc R U . . .
C32 C 0.17862(10) 0.42070(10) 0.91945(11) 0.0342(6) Uani 1 1 d . . . . .
H32A H 0.1482 0.4113 0.9353 0.051 Uiso 1 1 calc R U . . .
H32B H 0.2009 0.4467 0.9441 0.051 Uiso 1 1 calc R U . . .
H32C H 0.1847 0.3956 0.9239 0.051 Uiso 1 1 calc R U . . .
C33 C 0.13079(8) 0.37129(8) 0.69719(11) 0.0257(5) Uani 1 1 d . . . . .
H33A H 0.1050 0.3738 0.6819 0.039 Uiso 1 1 calc R U . . .
H33B H 0.1197 0.3427 0.7204 0.039 Uiso 1 1 calc R U . . .
H33C H 0.1491 0.3719 0.6609 0.039 Uiso 1 1 calc R U . . .
C34 C 0.08394(9) 0.34364(10) 0.39339(12) 0.0349(6) Uani 1 1 d . . . . .
H34A H 0.1120 0.3709 0.3807 0.052 Uiso 1 1 calc R U . . .
H34B H 0.0649 0.3299 0.3558 0.052 Uiso 1 1 calc R U . . .
H34C H 0.0912 0.3220 0.4128 0.052 Uiso 1 1 calc R U . . .
C35 C 0.01809(10) 0.31273(13) 0.45773(18) 0.0647(11) Uani 1 1 d . . . . .
H35A H 0.0270 0.2920 0.4762 0.097 Uiso 1 1 calc R U . . .
H35B H -0.0004 0.2989 0.4197 0.097 Uiso 1 1 calc R U . . .
H35C H 0.0005 0.3189 0.4890 0.097 Uiso 1 1 calc R U . . .
C36 C 0.04215(12) 0.38445(13) 0.41688(16) 0.0305(7) Uani 0.75 1 d . . P A 1
H36A H 0.0185 0.3826 0.4461 0.037 Uiso 0.75 1 calc R U P A 1
H36B H 0.0285 0.3742 0.3742 0.037 Uiso 0.75 1 calc R U P A 1
C37 C 0.08065(19) 0.43241(19) 0.4134(2) 0.0300(11) Uani 0.75 1 d . . P A 1
H37A H 0.0700 0.4517 0.3937 0.036 Uiso 0.75 1 calc R U P A 1
H37B H 0.1050 0.4337 0.3863 0.036 Uiso 0.75 1 calc R U P A 1
C36B C 0.0717(4) 0.4017(4) 0.3902(5) 0.031(2) Uani 0.25 1 d . . P A 2
H36C H 0.1025 0.4145 0.3723 0.037 Uiso 0.25 1 calc R U P A 2
H36D H 0.0497 0.3921 0.3547 0.037 Uiso 0.25 1 calc R U P A 2
C37B C 0.0686(6) 0.4360(6) 0.4304(7) 0.031(3) Uani 0.25 1 d . . P A 2
H37C H 0.0741 0.4622 0.4037 0.037 Uiso 0.25 1 calc R U P A 2
H37D H 0.0376 0.4226 0.4482 0.037 Uiso 0.25 1 calc R U P A 2
C38 C 0.07270(12) 0.46486(11) 0.51683(16) 0.0497(9) Uani 1 1 d . . . . .
H38A H 0.0424 0.4389 0.5239 0.075 Uiso 1 1 calc R U . A 2
H38B H 0.0702 0.4884 0.4936 0.075 Uiso 1 1 calc R U . A 2
H38C H 0.0874 0.4769 0.5579 0.075 Uiso 1 1 calc R U . A 2
C39 C 0.14461(9) 0.48997(9) 0.46936(14) 0.0355(6) Uani 1 1 d . . . . .
H39A H 0.1598 0.5011 0.5104 0.053 Uiso 1 1 calc R U . . .
H39B H 0.1416 0.5139 0.4481 0.053 Uiso 1 1 calc R U . . .
H39C H 0.1625 0.4812 0.4426 0.053 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.8871(15) . ?
Fe1 N4 1.9942(18) . ?
Fe1 N3 2.0174(18) . ?
Fe1 N2 2.0300(18) . ?
Fe1 N1 2.2315(18) . ?
Fe2 O1 1.9828(15) . ?
Fe2 N7 2.058(2) . ?
Fe2 N5 2.236(2) . ?
Fe2 N6 2.2619(19) . ?
Fe2 O4 2.2925(15) . ?
Fe2 O6 2.4038(16) . ?
S1 O3 1.4333(17) . ?
S1 O2 1.4578(16) . ?
S1 N2 1.5999(19) . ?
S1 C7 1.795(2) . ?
S2 O5 1.4442(16) . ?
S2 O4 1.4477(16) . ?
S2 N3 1.5941(18) . ?
S2 C16 1.790(2) . ?
S3 O7 1.4361(17) . ?
S3 O6 1.4554(16) . ?
S3 N4 1.6009(18) . ?
S3 C25 1.797(2) . ?
N1 C1 1.477(3) . ?
N1 C5 1.484(3) . ?
N1 C3 1.485(3) . ?
N2 C2 1.488(3) . ?
N3 C4 1.481(3) . ?
N4 C6 1.478(3) . ?
N5 C36 1.447(4) . ?
N5 C34 1.478(3) . ?
N5 C35 1.490(4) . ?
N5 C36B 1.746(11) . ?
N6 C37B 1.384(17) . ?
N6 C38 1.460(3) . ?
N6 C39 1.465(3) . ?
N6 C37 1.531(6) . ?
N7 N8 1.137(3) . ?
N8 N9 1.169(3) . ?
C1 C2 1.504(3) . ?
C3 C4 1.504(3) . ?
C5 C6 1.513(3) . ?
C7 C12 1.414(3) . ?
C7 C8 1.418(3) . ?
C8 C9 1.400(4) . ?
C8 C13 1.508(4) . ?
C9 C10 1.379(4) . ?
C10 C11 1.384(4) . ?
C10 C14 1.515(4) . ?
C11 C12 1.390(3) . ?
C12 C15 1.511(4) . ?
C16 C21 1.403(3) . ?
C16 C17 1.411(3) . ?
C17 C18 1.392(3) . ?
C17 C22 1.509(4) . ?
C18 C19 1.390(4) . ?
C19 C20 1.378(4) . ?
C19 C23 1.509(4) . ?
C20 C21 1.395(3) . ?
C21 C24 1.516(4) . ?
C25 C26 1.414(3) . ?
C25 C30 1.417(3) . ?
C26 C27 1.395(3) . ?
C26 C31 1.516(3) . ?
C27 C28 1.382(4) . ?
C28 C29 1.387(3) . ?
C28 C32 1.511(3) . ?
C29 C30 1.387(3) . ?
C30 C33 1.498(3) . ?
C36 C37 1.503(7) . ?
C36B C37B 1.487(16) . ?
C37B C38 2.037(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
O1 Fe1 N4 102.80(7) . . ?
O1 Fe1 N3 103.26(7) . . ?
N4 Fe1 N3 111.18(8) . . ?
O1 Fe1 N2 96.10(7) . . ?
N4 Fe1 N2 117.55(7) . . ?
N3 Fe1 N2 121.29(8) . . ?
O1 Fe1 N1 174.72(7) . . ?
N4 Fe1 N1 79.74(7) . . ?
N3 Fe1 N1 79.87(7) . . ?
N2 Fe1 N1 78.63(7) . . ?
O1 Fe2 N7 158.44(7) . . ?
O1 Fe2 N5 97.96(8) . . ?
N7 Fe2 N5 99.50(9) . . ?
O1 Fe2 N6 95.51(7) . . ?
N7 Fe2 N6 99.53(7) . . ?
N5 Fe2 N6 81.31(8) . . ?
O1 Fe2 O4 79.64(6) . . ?
N7 Fe2 O4 89.45(7) . . ?
N5 Fe2 O4 84.76(7) . . ?
N6 Fe2 O4 164.48(7) . . ?
O1 Fe2 O6 79.74(6) . . ?
N7 Fe2 O6 85.12(7) . . ?
N5 Fe2 O6 169.93(8) . . ?
N6 Fe2 O6 89.13(6) . . ?
O4 Fe2 O6 104.32(6) . . ?
O3 S1 O2 115.64(10) . . ?
O3 S1 N2 111.29(10) . . ?
O2 S1 N2 108.43(9) . . ?
O3 S1 C7 108.89(11) . . ?
O2 S1 C7 105.61(10) . . ?
N2 S1 C7 106.46(10) . . ?
O5 S2 O4 116.81(10) . . ?
O5 S2 N3 110.10(10) . . ?
O4 S2 N3 108.36(9) . . ?
O5 S2 C16 104.60(10) . . ?
O4 S2 C16 107.14(10) . . ?
N3 S2 C16 109.59(10) . . ?
O7 S3 O6 115.34(10) . . ?
O7 S3 N4 112.73(10) . . ?
O6 S3 N4 107.60(9) . . ?
O7 S3 C25 108.18(10) . . ?
O6 S3 C25 107.63(10) . . ?
N4 S3 C25 104.73(10) . . ?
Fe1 O1 Fe2 128.24(8) . . ?
S2 O4 Fe2 147.83(10) . . ?
S3 O6 Fe2 146.80(9) . . ?
C1 N1 C5 111.42(18) . . ?
C1 N1 C3 110.82(18) . . ?
C5 N1 C3 111.46(18) . . ?
C1 N1 Fe1 108.88(13) . . ?
C5 N1 Fe1 107.26(13) . . ?
C3 N1 Fe1 106.79(13) . . ?
C2 N2 S1 111.37(14) . . ?
C2 N2 Fe1 116.44(14) . . ?
S1 N2 Fe1 130.13(10) . . ?
C4 N3 S2 113.01(14) . . ?
C4 N3 Fe1 116.66(14) . . ?
S2 N3 Fe1 127.70(10) . . ?
C6 N4 S3 115.72(14) . . ?
C6 N4 Fe1 115.32(13) . . ?
S3 N4 Fe1 128.39(10) . . ?
C36 N5 C34 116.7(3) . . ?
C36 N5 C35 104.4(3) . . ?
C34 N5 C35 106.0(2) . . ?
C34 N5 C36B 86.7(4) . . ?
C35 N5 C36B 136.2(4) . . ?
C36 N5 Fe2 105.19(18) . . ?
C34 N5 Fe2 113.65(15) . . ?
C35 N5 Fe2 110.55(19) . . ?
C36B N5 Fe2 101.4(4) . . ?
C37B N6 C38 91.4(6) . . ?
C37B N6 C39 118.8(7) . . ?
C38 N6 C39 108.6(2) . . ?
C38 N6 C37 114.4(3) . . ?
C39 N6 C37 105.8(3) . . ?
C37B N6 Fe2 110.3(7) . . ?
C38 N6 Fe2 110.78(15) . . ?
C39 N6 Fe2 114.43(14) . . ?
C37 N6 Fe2 102.7(2) . . ?
N8 N7 Fe2 139.88(18) . . ?
N7 N8 N9 177.8(3) . . ?
N1 C1 C2 110.36(18) . . ?
N2 C2 C1 107.27(18) . . ?
N1 C3 C4 110.77(19) . . ?
N3 C4 C3 108.81(18) . . ?
N1 C5 C6 109.08(19) . . ?
N4 C6 C5 106.96(18) . . ?
C12 C7 C8 120.7(2) . . ?
C12 C7 S1 117.88(17) . . ?
C8 C7 S1 121.35(19) . . ?
C9 C8 C7 117.1(2) . . ?
C9 C8 C13 117.3(2) . . ?
C7 C8 C13 125.7(2) . . ?
C10 C9 C8 123.3(2) . . ?
C9 C10 C11 118.2(2) . . ?
C9 C10 C14 121.2(3) . . ?
C11 C10 C14 120.5(3) . . ?
C10 C11 C12 122.2(3) . . ?
C11 C12 C7 118.5(2) . . ?
C11 C12 C15 116.7(2) . . ?
C7 C12 C15 124.8(2) . . ?
C21 C16 C17 121.0(2) . . ?
C21 C16 S2 122.60(18) . . ?
C17 C16 S2 116.43(17) . . ?
C18 C17 C16 117.6(2) . . ?
C18 C17 C22 117.7(2) . . ?
C16 C17 C22 124.6(2) . . ?
C19 C18 C17 122.5(3) . . ?
C20 C19 C18 117.8(2) . . ?
C20 C19 C23 121.3(3) . . ?
C18 C19 C23 120.8(3) . . ?
C19 C20 C21 122.8(2) . . ?
C20 C21 C16 117.7(2) . . ?
C20 C21 C24 116.7(2) . . ?
C16 C21 C24 125.5(2) . . ?
C26 C25 C30 120.1(2) . . ?
C26 C25 S3 122.22(18) . . ?
C30 C25 S3 117.58(17) . . ?
C27 C26 C25 117.8(2) . . ?
C27 C26 C31 116.7(2) . . ?
C25 C26 C31 125.4(2) . . ?
C28 C27 C26 123.1(2) . . ?
C27 C28 C29 117.8(2) . . ?
C27 C28 C32 122.7(2) . . ?
C29 C28 C32 119.5(2) . . ?
C28 C29 C30 122.5(2) . . ?
C29 C30 C25 118.7(2) . . ?
C29 C30 C33 117.1(2) . . ?
C25 C30 C33 124.2(2) . . ?
N5 C36 C37 108.7(3) . . ?
C36 C37 N6 111.1(4) . . ?
C37B C36B N5 106.5(9) . . ?
N6 C37B C36B 111.5(11) . . ?
N6 C37B C38 45.8(5) . . ?
C36B C37B C38 150.6(11) . . ?
N6 C38 C37B 42.8(5) . . ?

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
N4 Fe1 O1 Fe2 -60.92(11) . . . . ?
N3 Fe1 O1 Fe2 54.81(11) . . . . ?
N2 Fe1 O1 Fe2 178.99(10) . . . . ?
O5 S2 O4 Fe2 100.54(19) . . . . ?
N3 S2 O4 Fe2 -24.5(2) . . . . ?
C16 S2 O4 Fe2 -142.63(18) . . . . ?
O7 S3 O6 Fe2 106.17(18) . . . . ?
N4 S3 O6 Fe2 -20.6(2) . . . . ?
C25 S3 O6 Fe2 -132.99(17) . . . . ?
O3 S1 N2 C2 50.68(18) . . . . ?
O2 S1 N2 C2 178.95(15) . . . . ?
C7 S1 N2 C2 -67.84(17) . . . . ?
O3 S1 N2 Fe1 -112.09(14) . . . . ?
O2 S1 N2 Fe1 16.17(17) . . . . ?
C7 S1 N2 Fe1 129.39(14) . . . . ?
O5 S2 N3 C4 35.54(18) . . . . ?
O4 S2 N3 C4 164.41(15) . . . . ?
C16 S2 N3 C4 -78.99(17) . . . . ?
O5 S2 N3 Fe1 -125.25(13) . . . . ?
O4 S2 N3 Fe1 3.62(16) . . . . ?
C16 S2 N3 Fe1 120.23(13) . . . . ?
O7 S3 N4 C6 59.61(18) . . . . ?
O6 S3 N4 C6 -172.10(15) . . . . ?
C25 S3 N4 C6 -57.77(18) . . . . ?
O7 S3 N4 Fe1 -111.26(14) . . . . ?
O6 S3 N4 Fe1 17.03(16) . . . . ?
C25 S3 N4 Fe1 131.36(13) . . . . ?
C5 N1 C1 C2 -153.83(19) . . . . ?
C3 N1 C1 C2 81.4(2) . . . . ?
Fe1 N1 C1 C2 -35.7(2) . . . . ?
S1 N2 C2 C1 156.92(16) . . . . ?
Fe1 N2 C2 C1 -37.7(2) . . . . ?
N1 C1 C2 N2 47.2(2) . . . . ?
C1 N1 C3 C4 -157.17(19) . . . . ?
C5 N1 C3 C4 78.1(2) . . . . ?
Fe1 N1 C3 C4 -38.7(2) . . . . ?
S2 N3 C4 C3 166.42(16) . . . . ?
Fe1 N3 C4 C3 -30.5(2) . . . . ?
N1 C3 C4 N3 45.7(3) . . . . ?
C1 N1 C5 C6 82.2(2) . . . . ?
C3 N1 C5 C6 -153.41(18) . . . . ?
Fe1 N1 C5 C6 -36.8(2) . . . . ?
S3 N4 C6 C5 145.99(16) . . . . ?
Fe1 N4 C6 C5 -41.9(2) . . . . ?
N1 C5 C6 N4 51.0(2) . . . . ?
O3 S1 C7 C12 174.19(18) . . . . ?
O2 S1 C7 C12 49.4(2) . . . . ?
N2 S1 C7 C12 -65.7(2) . . . . ?
O3 S1 C7 C8 -2.9(2) . . . . ?
O2 S1 C7 C8 -127.68(19) . . . . ?
N2 S1 C7 C8 117.18(19) . . . . ?
C12 C7 C8 C9 -2.4(3) . . . . ?
S1 C7 C8 C9 174.65(18) . . . . ?
C12 C7 C8 C13 176.5(2) . . . . ?
S1 C7 C8 C13 -6.5(3) . . . . ?
C7 C8 C9 C10 1.1(4) . . . . ?
C13 C8 C9 C10 -177.9(2) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C8 C9 C10 C14 178.6(3) . . . . ?
C9 C10 C11 C12 -0.5(4) . . . . ?
C14 C10 C11 C12 -178.8(3) . . . . ?
C10 C11 C12 C7 -0.7(4) . . . . ?
C10 C11 C12 C15 178.2(2) . . . . ?
C8 C7 C12 C11 2.2(3) . . . . ?
S1 C7 C12 C11 -174.92(18) . . . . ?
C8 C7 C12 C15 -176.7(2) . . . . ?
S1 C7 C12 C15 6.2(3) . . . . ?
O5 S2 C16 C21 -142.02(19) . . . . ?
O4 S2 C16 C21 93.4(2) . . . . ?
N3 S2 C16 C21 -24.0(2) . . . . ?
O5 S2 C16 C17 37.3(2) . . . . ?
O4 S2 C16 C17 -87.29(19) . . . . ?
N3 S2 C16 C17 155.34(18) . . . . ?
C21 C16 C17 C18 7.0(4) . . . . ?
S2 C16 C17 C18 -172.3(2) . . . . ?
C21 C16 C17 C22 -169.7(3) . . . . ?
S2 C16 C17 C22 11.0(4) . . . . ?
C16 C17 C18 C19 -0.5(4) . . . . ?
C22 C17 C18 C19 176.5(3) . . . . ?
C17 C18 C19 C20 -5.0(4) . . . . ?
C17 C18 C19 C23 178.3(3) . . . . ?
C18 C19 C20 C21 4.2(4) . . . . ?
C23 C19 C20 C21 -179.1(2) . . . . ?
C19 C20 C21 C16 2.1(4) . . . . ?
C19 C20 C21 C24 -174.4(2) . . . . ?
C17 C16 C21 C20 -7.8(3) . . . . ?
S2 C16 C21 C20 171.52(17) . . . . ?
C17 C16 C21 C24 168.4(2) . . . . ?
S2 C16 C21 C24 -12.3(3) . . . . ?
O7 S3 C25 C26 -15.3(2) . . . . ?
O6 S3 C25 C26 -140.52(18) . . . . ?
N4 S3 C25 C26 105.17(19) . . . . ?
O7 S3 C25 C30 168.19(17) . . . . ?
O6 S3 C25 C30 42.95(19) . . . . ?
N4 S3 C25 C30 -71.36(19) . . . . ?
C30 C25 C26 C27 -0.8(3) . . . . ?
S3 C25 C26 C27 -177.29(17) . . . . ?
C30 C25 C26 C31 178.2(2) . . . . ?
S3 C25 C26 C31 1.8(3) . . . . ?
C25 C26 C27 C28 1.3(3) . . . . ?
C31 C26 C27 C28 -177.8(2) . . . . ?
C26 C27 C28 C29 -1.0(3) . . . . ?
C26 C27 C28 C32 177.1(2) . . . . ?
C27 C28 C29 C30 0.2(3) . . . . ?
C32 C28 C29 C30 -177.9(2) . . . . ?
C28 C29 C30 C25 0.2(3) . . . . ?
C28 C29 C30 C33 179.0(2) . . . . ?
C26 C25 C30 C29 0.1(3) . . . . ?
S3 C25 C30 C29 176.74(16) . . . . ?
C26 C25 C30 C33 -178.6(2) . . . . ?
S3 C25 C30 C33 -2.0(3) . . . . ?
C34 N5 C36 C37 -77.9(3) . . . . ?
C35 N5 C36 C37 165.6(3) . . . . ?
Fe2 N5 C36 C37 49.1(3) . . . . ?
N5 C36 C37 N6 -64.8(4) . . . . ?
C38 N6 C37 C36 -78.8(4) . . . . ?
C39 N6 C37 C36 161.6(3) . . . . ?
Fe2 N6 C37 C36 41.3(4) . . . . ?
C34 N5 C36B C37B -158.0(9) . . . . ?
C35 N5 C36B C37B 92.2(10) . . . . ?
Fe2 N5 C36B C37B -44.6(9) . . . . ?
C38 N6 C37B C36B -157.4(11) . . . . ?
C39 N6 C37B C36B 90.3(12) . . . . ?
Fe2 N6 C37B C36B -44.6(13) . . . . ?
C39 N6 C37B C38 -112.2(4) . . . . ?
Fe2 N6 C37B C38 112.8(3) . . . . ?
N5 C36B C37B N6 61.2(13) . . . . ?
N5 C36B C37B C38 27(3) . . . . ?
C39 N6 C38 C37B 121.1(7) . . . . ?
Fe2 N6 C38 C37B -112.4(7) . . . . ?

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
O1 H1 O2 0.841(10) 1.805(14) 2.617(2) 162(3) .

_refine_diff_density_max         0.847
_refine_diff_density_min         -0.667
_refine_diff_density_rms         0.070



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/Pentane'
####################################################################### 
# 
# 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_asb462
_database_code_depnum_ccdc_archive 'CCDC 1554810'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Co(II)(OTf)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H62 Co F3 Fe N6 O10 S4'
_chemical_formula_weight         1086.97

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'
F F 0.0171 0.0103 '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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   39.277(5)
_cell_length_b                   16.972(2)
_cell_length_c                   18.844(2)
_cell_angle_alpha                90
_cell_angle_beta                 110.7870(15)
_cell_angle_gamma                90
_cell_volume                     11744(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9569
_cell_measurement_theta_min      2.40
_cell_measurement_theta_max      26.40

_exptl_crystal_description       rod
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             4544
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.177
_exptl_crystal_size_min          0.102
_exptl_absorpt_coefficient_mu    0.730
_shelx_estimated_absorpt_T_min   0.788
_shelx_estimated_absorpt_T_max   0.929
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4802
_exptl_absorpt_correction_T_max  0.6473
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            28661
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_av_R_equivalents  0.0360
_diffrn_reflns_limit_h_min       -49
_diffrn_reflns_limit_h_max       49
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.109
_diffrn_reflns_theta_max         26.442
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12057
_reflns_number_gt                9013
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
An orange crystal of approximate dimensions 0.102 x 0.177 x 0.342 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  
The APEX2 program package was used to determine the unit-cell parameters and 
for data collection (60 sec/frame scan time).  The raw frame data was processed 
using SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL4 program.  The diffraction 
symmetry was 2/m and the systematic absences were consistent with the monoclinic 
space groups Cc and C2/c.  It was later determined that space group C2/c was correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atom H(1) was located from a 
difference-Fourier map and refined (x,y,z and riding Uiso) with d(O-H) = 0.85Å.  
The remaining hydrogen atoms were included using a riding model.

At convergence, wR2 = 0.0974 and Goof = 1.032 for 603 variables refined against 
12057 data (0.80Å), R1 = 0.0396 for those 9013 data with I > 2.0sigma(I).

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that tetrahydrofuran and/or pentane solvents were present.  The SQUEEZE 
routine in the PLATON program package was used to account for the electrons in 
the solvent accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0448P)²+4.8939P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12057
_refine_ls_number_parameters     603
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.0974
_refine_ls_wR_factor_gt          0.0899
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_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
Co1 Co 0.35531(2) 0.68921(2) 0.49335(2) 0.01751(9) Uani 1 1 d . . . . .
Fe1 Fe 0.37209(2) 0.58805(2) 0.65924(2) 0.01568(9) Uani 1 1 d . . . . .
S1 S 0.30052(2) 0.63508(4) 0.70422(4) 0.02047(14) Uani 1 1 d . . . . .
S2 S 0.36842(2) 0.48787(4) 0.51340(3) 0.01772(14) Uani 1 1 d . . . . .
S3 S 0.43313(2) 0.71225(4) 0.65536(4) 0.01785(14) Uani 1 1 d . . . . .
S4 S 0.40859(2) 0.73537(4) 0.39143(4) 0.02326(15) Uani 1 1 d . . . . .
F1 F 0.36714(5) 0.83350(10) 0.28903(9) 0.0428(4) Uani 1 1 d . . . . .
F2 F 0.36335(5) 0.71263(9) 0.25179(9) 0.0376(4) Uani 1 1 d . . . . .
F3 F 0.41063(5) 0.78118(10) 0.26029(10) 0.0474(5) Uani 1 1 d . . . . .
O1 O 0.34223(4) 0.65067(10) 0.57900(9) 0.0203(4) Uani 1 1 d D . . . .
H1 H 0.3229(5) 0.6610(17) 0.5873(17) 0.042(9) Uiso 1 1 d D . . . .
O2 O 0.28779(4) 0.66626(10) 0.62744(10) 0.0237(4) Uani 1 1 d . . . . .
O3 O 0.30464(5) 0.69226(10) 0.76271(10) 0.0269(4) Uani 1 1 d . . . . .
O4 O 0.37370(4) 0.56657(10) 0.48802(9) 0.0203(4) Uani 1 1 d . . . . .
O5 O 0.33343(4) 0.45387(10) 0.47254(10) 0.0245(4) Uani 1 1 d . . . . .
O6 O 0.40594(4) 0.72228(10) 0.58014(9) 0.0211(4) Uani 1 1 d . . . . .
O7 O 0.46951(4) 0.69664(10) 0.65832(10) 0.0238(4) Uani 1 1 d . . . . .
O8 O 0.37666(5) 0.71722(10) 0.41084(10) 0.0239(4) Uani 1 1 d . . . . .
O9 O 0.42862(5) 0.80358(11) 0.42882(11) 0.0331(5) Uani 1 1 d . . . . .
O10 O 0.42910(5) 0.66739(11) 0.38588(10) 0.0286(4) Uani 1 1 d . . . . .
N1 N 0.40172(5) 0.50952(12) 0.75565(11) 0.0179(4) Uani 1 1 d . . . . .
N2 N 0.33748(5) 0.58773(12) 0.71799(11) 0.0183(4) Uani 1 1 d . . . . .
N3 N 0.37751(5) 0.49282(12) 0.60233(11) 0.0187(4) Uani 1 1 d . . . . .
N4 N 0.41975(5) 0.64423(12) 0.69754(11) 0.0182(4) Uani 1 1 d . . . . .
N6 N 0.33407(6) 0.81013(12) 0.49356(12) 0.0226(5) Uani 1 1 d . . . . .
N5 N 0.30259(5) 0.67163(12) 0.40191(12) 0.0212(5) Uani 1 1 d . . . . .
C1 C 0.37657(7) 0.48684(14) 0.79552(14) 0.0197(5) Uani 1 1 d . . . . .
H1A H 0.3907 0.4702 0.8481 0.024 Uiso 1 1 calc R U . . .
H1B H 0.3611 0.4422 0.7689 0.024 Uiso 1 1 calc R U . . .
C2 C 0.35302(7) 0.55716(15) 0.79652(14) 0.0210(6) Uani 1 1 d . . . . .
H2A H 0.3333 0.5412 0.8146 0.025 Uiso 1 1 calc R U . . .
H2B H 0.3678 0.5984 0.8309 0.025 Uiso 1 1 calc R U . . .
C3 C 0.41359(7) 0.43917(15) 0.72322(14) 0.0221(6) Uani 1 1 d . . . . .
H3A H 0.4172 0.3939 0.7583 0.026 Uiso 1 1 calc R U . . .
H3B H 0.4371 0.4503 0.7167 0.026 Uiso 1 1 calc R U . . .
C4 C 0.38497(7) 0.41918(15) 0.64734(14) 0.0222(6) Uani 1 1 d . . . . .
H4A H 0.3940 0.3778 0.6215 0.027 Uiso 1 1 calc R U . . .
H4B H 0.3625 0.3999 0.6541 0.027 Uiso 1 1 calc R U . . .
C5 C 0.43292(6) 0.55558(15) 0.80592(14) 0.0215(6) Uani 1 1 d . . . . .
H5A H 0.4516 0.5192 0.8388 0.026 Uiso 1 1 calc R U . . .
H5B H 0.4246 0.5900 0.8390 0.026 Uiso 1 1 calc R U . . .
C6 C 0.44967(6) 0.60581(16) 0.76019(15) 0.0243(6) Uani 1 1 d . . . . .
H6A H 0.4658 0.6463 0.7932 0.029 Uiso 1 1 calc R U . . .
H6B H 0.4645 0.5725 0.7390 0.029 Uiso 1 1 calc R U . . .
C7 C 0.26701(6) 0.56427(16) 0.70697(15) 0.0235(6) Uani 1 1 d . . . . .
C8 C 0.24938(7) 0.57018(17) 0.76051(16) 0.0302(7) Uani 1 1 d . . . . .
C9 C 0.22226(7) 0.51471(19) 0.75510(18) 0.0382(8) Uani 1 1 d . . . . .
H9A H 0.2100 0.5181 0.7903 0.046 Uiso 1 1 calc R U . . .
C10 C 0.21243(8) 0.45590(19) 0.7021(2) 0.0415(8) Uani 1 1 d . . . . .
C11 C 0.23069(8) 0.45133(17) 0.65113(18) 0.0366(7) Uani 1 1 d . . . . .
H11A H 0.2244 0.4105 0.6143 0.044 Uiso 1 1 calc R U . . .
C12 C 0.25773(7) 0.50407(16) 0.65206(16) 0.0290(6) Uani 1 1 d . . . . .
C13 C 0.25722(8) 0.6297(2) 0.82317(17) 0.0417(8) Uani 1 1 d . . . . .
H13A H 0.2404 0.6219 0.8505 0.063 Uiso 1 1 calc R U . . .
H13B H 0.2541 0.6829 0.8016 0.063 Uiso 1 1 calc R U . . .
H13C H 0.2823 0.6232 0.8584 0.063 Uiso 1 1 calc R U . . .
C14 C 0.18328(9) 0.3956(2) 0.6994(2) 0.0650(11) Uani 1 1 d . . . . .
H14A H 0.1727 0.4089 0.7377 0.097 Uiso 1 1 calc R U . . .
H14B H 0.1942 0.3430 0.7098 0.097 Uiso 1 1 calc R U . . .
H14C H 0.1642 0.3962 0.6490 0.097 Uiso 1 1 calc R U . . .
C15 C 0.27479(9) 0.49377(18) 0.59204(19) 0.0421(8) Uani 1 1 d . . . . .
H15A H 0.2641 0.4477 0.5607 0.063 Uiso 1 1 calc R U . . .
H15B H 0.3011 0.4861 0.6167 0.063 Uiso 1 1 calc R U . . .
H15C H 0.2702 0.5409 0.5599 0.063 Uiso 1 1 calc R U . . .
C16 C 0.40261(6) 0.42527(14) 0.50149(13) 0.0176(5) Uani 1 1 d . . . . .
C17 C 0.39474(7) 0.34686(15) 0.47738(14) 0.0198(5) Uani 1 1 d . . . . .
C18 C 0.42271(7) 0.30202(15) 0.46830(14) 0.0233(6) Uani 1 1 d . . . . .
H18A H 0.4177 0.2491 0.4514 0.028 Uiso 1 1 calc R U . . .
C19 C 0.45741(7) 0.33119(15) 0.48277(15) 0.0239(6) Uani 1 1 d . . . . .
C20 C 0.46467(7) 0.40693(15) 0.51013(14) 0.0212(6) Uani 1 1 d . . . . .
H20A H 0.4887 0.4268 0.5223 0.025 Uiso 1 1 calc R U . . .
C21 C 0.43832(7) 0.45584(15) 0.52076(14) 0.0194(5) Uani 1 1 d . . . . .
C22 C 0.35866(7) 0.30536(16) 0.46026(17) 0.0287(6) Uani 1 1 d . . . . .
H22A H 0.3622 0.2484 0.4579 0.043 Uiso 1 1 calc R U . . .
H22B H 0.3415 0.3238 0.4114 0.043 Uiso 1 1 calc R U . . .
H22C H 0.3490 0.3170 0.5004 0.043 Uiso 1 1 calc R U . . .
C23 C 0.48644(8) 0.28000(17) 0.47113(18) 0.0363(7) Uani 1 1 d . . . . .
H23A H 0.4989 0.3095 0.4428 0.054 Uiso 1 1 calc R U . . .
H23B H 0.4752 0.2328 0.4425 0.054 Uiso 1 1 calc R U . . .
H23C H 0.5041 0.2645 0.5206 0.054 Uiso 1 1 calc R U . . .
C24 C 0.45000(7) 0.53701(15) 0.55256(15) 0.0239(6) Uani 1 1 d . . . . .
H24A H 0.4766 0.5394 0.5744 0.036 Uiso 1 1 calc R U . . .
H24B H 0.4399 0.5484 0.5921 0.036 Uiso 1 1 calc R U . . .
H24C H 0.4411 0.5761 0.5118 0.036 Uiso 1 1 calc R U . . .
C25 C 0.43420(6) 0.80562(15) 0.70089(14) 0.0209(5) Uani 1 1 d . . . . .
C26 C 0.45348(7) 0.86648(16) 0.68029(16) 0.0285(6) Uani 1 1 d . . . . .
C27 C 0.45434(8) 0.94036(17) 0.71285(18) 0.0386(7) Uani 1 1 d . . . . .
H27A H 0.4668 0.9819 0.6987 0.046 Uiso 1 1 calc R U . . .
C28 C 0.43772(9) 0.95594(18) 0.76511(19) 0.0423(8) Uani 1 1 d . . . . .
C29 C 0.41826(8) 0.89588(17) 0.78245(17) 0.0346(7) Uani 1 1 d . . . . .
H29A H 0.4063 0.9064 0.8172 0.042 Uiso 1 1 calc R U . . .
C30 C 0.41540(7) 0.82060(15) 0.75137(15) 0.0235(6) Uani 1 1 d . . . . .
C31 C 0.47322(8) 0.85664(17) 0.62525(18) 0.0385(7) Uani 1 1 d . . . . .
H31A H 0.4788 0.9086 0.6096 0.058 Uiso 1 1 calc R U . . .
H31B H 0.4578 0.8274 0.5806 0.058 Uiso 1 1 calc R U . . .
H31C H 0.4959 0.8275 0.6499 0.058 Uiso 1 1 calc R U . . .
C32 C 0.44092(12) 1.0360(2) 0.8021(3) 0.0748(13) Uani 1 1 d . . . . .
H32A H 0.4194 1.0457 0.8158 0.112 Uiso 1 1 calc R U . . .
H32B H 0.4425 1.0767 0.7666 0.112 Uiso 1 1 calc R U . . .
H32C H 0.4628 1.0376 0.8479 0.112 Uiso 1 1 calc R U . . .
C33 C 0.39116(8) 0.76364(16) 0.77186(16) 0.0309(7) Uani 1 1 d . . . . .
H33A H 0.3792 0.7906 0.8027 0.046 Uiso 1 1 calc R U . . .
H33B H 0.4058 0.7198 0.8009 0.046 Uiso 1 1 calc R U . . .
H33C H 0.3727 0.7434 0.7254 0.046 Uiso 1 1 calc R U . . .
C34 C 0.27574(7) 0.63192(18) 0.42846(16) 0.0322(7) Uani 1 1 d . . . . .
H34A H 0.2522 0.6292 0.3867 0.048 Uiso 1 1 calc R U . . .
H34B H 0.2731 0.6618 0.4707 0.048 Uiso 1 1 calc R U . . .
H34C H 0.2842 0.5785 0.4456 0.048 Uiso 1 1 calc R U . . .
C35 C 0.30507(7) 0.62503(16) 0.33748(15) 0.0260(6) Uani 1 1 d . . . . .
H35A H 0.2812 0.6238 0.2966 0.039 Uiso 1 1 calc R U . . .
H35B H 0.3127 0.5712 0.3544 0.039 Uiso 1 1 calc R U . . .
H35C H 0.3229 0.6493 0.3188 0.039 Uiso 1 1 calc R U . . .
C36 C 0.29072(7) 0.75259(16) 0.37538(15) 0.0273(6) Uani 1 1 d . . . . .
H36A H 0.2648 0.7519 0.3418 0.033 Uiso 1 1 calc R U . . .
H36B H 0.3052 0.7726 0.3457 0.033 Uiso 1 1 calc R U . . .
C37 C 0.29553(7) 0.80708(17) 0.44242(16) 0.0308(7) Uani 1 1 d . . . . .
H37A H 0.2872 0.8607 0.4235 0.037 Uiso 1 1 calc R U . . .
H37B H 0.2803 0.7881 0.4710 0.037 Uiso 1 1 calc R U . . .
C38 C 0.33549(8) 0.83652(16) 0.56967(16) 0.0311(7) Uani 1 1 d . . . . .
H38A H 0.3234 0.8878 0.5652 0.047 Uiso 1 1 calc R U . . .
H38B H 0.3609 0.8412 0.6035 0.047 Uiso 1 1 calc R U . . .
H38D H 0.3230 0.7979 0.5905 0.047 Uiso 1 1 calc R U . . .
C39 C 0.35413(8) 0.86860(16) 0.46564(18) 0.0360(7) Uani 1 1 d . . . . .
H39A H 0.3446 0.9214 0.4683 0.054 Uiso 1 1 calc R U . . .
H39D H 0.3511 0.8565 0.4129 0.054 Uiso 1 1 calc R U . . .
H39B H 0.3800 0.8667 0.4972 0.054 Uiso 1 1 calc R U . . .
C40 C 0.38631(8) 0.76749(16) 0.29354(16) 0.0308(7) 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
Co1 O1 1.9712(17) . ?
Co1 O8 2.0670(17) . ?
Co1 O6 2.1530(17) . ?
Co1 N5 2.194(2) . ?
Co1 N6 2.216(2) . ?
Co1 O4 2.2171(16) . ?
Fe1 O1 1.8794(17) . ?
Fe1 N3 1.992(2) . ?
Fe1 N4 1.994(2) . ?
Fe1 N2 2.0353(19) . ?
Fe1 N1 2.221(2) . ?
S1 O3 1.4340(19) . ?
S1 O2 1.4526(18) . ?
S1 N2 1.598(2) . ?
S1 C7 1.797(3) . ?
S2 O5 1.4364(18) . ?
S2 O4 1.4582(17) . ?
S2 N3 1.587(2) . ?
S2 C16 1.788(2) . ?
S3 O7 1.4350(17) . ?
S3 O6 1.4507(17) . ?
S3 N4 1.593(2) . ?
S3 C25 1.795(3) . ?
S4 O10 1.4322(19) . ?
S4 O9 1.4361(19) . ?
S4 O8 1.4581(17) . ?
S4 C40 1.822(3) . ?
F1 C40 1.336(3) . ?
F2 C40 1.340(3) . ?
F3 C40 1.336(3) . ?
N1 C5 1.479(3) . ?
N1 C1 1.488(3) . ?
N1 C3 1.490(3) . ?
N2 C2 1.480(3) . ?
N3 C4 1.480(3) . ?
N4 C6 1.488(3) . ?
N6 C39 1.475(3) . ?
N6 C37 1.479(3) . ?
N6 C38 1.485(3) . ?
N5 C36 1.480(3) . ?
N5 C34 1.480(3) . ?
N5 C35 1.481(3) . ?
C1 C2 1.514(3) . ?
C3 C4 1.511(4) . ?
C5 C6 1.518(3) . ?
C7 C12 1.407(4) . ?
C7 C8 1.415(4) . ?
C8 C9 1.398(4) . ?
C8 C13 1.501(4) . ?
C9 C10 1.367(4) . ?
C10 C11 1.390(4) . ?
C10 C14 1.523(4) . ?
C11 C12 1.384(4) . ?
C12 C15 1.516(4) . ?
C16 C17 1.405(3) . ?
C16 C21 1.417(3) . ?
C17 C18 1.396(3) . ?
C17 C22 1.511(3) . ?
C18 C19 1.383(4) . ?
C19 C20 1.377(4) . ?
C19 C23 1.510(3) . ?
C20 C21 1.396(3) . ?
C21 C24 1.507(3) . ?
C25 C26 1.414(4) . ?
C25 C30 1.419(3) . ?
C26 C27 1.391(4) . ?
C26 C31 1.508(4) . ?
C27 C28 1.387(4) . ?
C28 C29 1.381(4) . ?
C28 C32 1.512(4) . ?
C29 C30 1.393(4) . ?
C30 C33 1.501(4) . ?
C36 C37 1.522(4) . ?

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 Co1 O8 170.23(7) . . ?
O1 Co1 O6 84.45(7) . . ?
O8 Co1 O6 89.97(7) . . ?
O1 Co1 N5 98.65(7) . . ?
O8 Co1 N5 87.84(7) . . ?
O6 Co1 N5 172.69(7) . . ?
O1 Co1 N6 95.64(7) . . ?
O8 Co1 N6 92.40(7) . . ?
O6 Co1 N6 90.23(7) . . ?
N5 Co1 N6 82.90(8) . . ?
O1 Co1 O4 84.79(7) . . ?
O8 Co1 O4 87.49(6) . . ?
O6 Co1 O4 92.94(6) . . ?
N5 Co1 O4 93.93(7) . . ?
N6 Co1 O4 176.83(7) . . ?
O1 Fe1 N3 100.43(8) . . ?
O1 Fe1 N4 104.98(8) . . ?
N3 Fe1 N4 108.48(8) . . ?
O1 Fe1 N2 95.31(8) . . ?
N3 Fe1 N2 120.67(8) . . ?
N4 Fe1 N2 121.80(8) . . ?
O1 Fe1 N1 173.62(7) . . ?
N3 Fe1 N1 80.12(8) . . ?
N4 Fe1 N1 80.72(8) . . ?
N2 Fe1 N1 79.08(7) . . ?
O3 S1 O2 115.10(11) . . ?
O3 S1 N2 111.56(11) . . ?
O2 S1 N2 108.47(10) . . ?
O3 S1 C7 108.32(12) . . ?
O2 S1 C7 106.00(11) . . ?
N2 S1 C7 106.94(11) . . ?
O5 S2 O4 114.35(10) . . ?
O5 S2 N3 113.66(11) . . ?
O4 S2 N3 107.03(10) . . ?
O5 S2 C16 108.20(11) . . ?
O4 S2 C16 107.62(10) . . ?
N3 S2 C16 105.46(11) . . ?
O7 S3 O6 115.93(10) . . ?
O7 S3 N4 110.31(10) . . ?
O6 S3 N4 108.29(10) . . ?
O7 S3 C25 106.88(11) . . ?
O6 S3 C25 104.34(11) . . ?
N4 S3 C25 110.93(11) . . ?
O10 S4 O9 117.43(11) . . ?
O10 S4 O8 113.84(11) . . ?
O9 S4 O8 114.68(11) . . ?
O10 S4 C40 104.34(12) . . ?
O9 S4 C40 103.78(12) . . ?
O8 S4 C40 99.81(12) . . ?
Fe1 O1 Co1 125.23(9) . . ?
S2 O4 Co1 139.35(10) . . ?
S3 O6 Co1 150.79(11) . . ?
S4 O8 Co1 148.41(11) . . ?
C5 N1 C1 111.16(19) . . ?
C5 N1 C3 112.19(19) . . ?
C1 N1 C3 111.13(19) . . ?
C5 N1 Fe1 106.34(14) . . ?
C1 N1 Fe1 108.62(14) . . ?
C3 N1 Fe1 107.15(14) . . ?
C2 N2 S1 111.54(15) . . ?
C2 N2 Fe1 115.27(14) . . ?
S1 N2 Fe1 130.85(12) . . ?
C4 N3 S2 119.01(16) . . ?
C4 N3 Fe1 114.45(15) . . ?
S2 N3 Fe1 125.76(12) . . ?
C6 N4 S3 113.95(16) . . ?
C6 N4 Fe1 116.96(15) . . ?
S3 N4 Fe1 126.83(12) . . ?
C39 N6 C37 110.1(2) . . ?
C39 N6 C38 107.5(2) . . ?
C37 N6 C38 108.6(2) . . ?
C39 N6 Co1 111.92(16) . . ?
C37 N6 Co1 105.39(15) . . ?
C38 N6 Co1 113.33(15) . . ?
C36 N5 C34 111.1(2) . . ?
C36 N5 C35 108.9(2) . . ?
C34 N5 C35 107.2(2) . . ?
C36 N5 Co1 103.63(15) . . ?
C34 N5 Co1 112.55(16) . . ?
C35 N5 Co1 113.47(15) . . ?
N1 C1 C2 108.68(19) . . ?
N2 C2 C1 107.50(19) . . ?
N1 C3 C4 109.40(19) . . ?
N3 C4 C3 106.4(2) . . ?
N1 C5 C6 111.2(2) . . ?
N4 C6 C5 108.48(19) . . ?
C12 C7 C8 120.7(2) . . ?
C12 C7 S1 117.76(19) . . ?
C8 C7 S1 121.5(2) . . ?
C9 C8 C7 117.0(3) . . ?
C9 C8 C13 116.7(3) . . ?
C7 C8 C13 126.4(2) . . ?
C10 C9 C8 123.7(3) . . ?
C9 C10 C11 117.7(3) . . ?
C9 C10 C14 121.9(3) . . ?
C11 C10 C14 120.4(3) . . ?
C12 C11 C10 122.5(3) . . ?
C11 C12 C7 118.4(3) . . ?
C11 C12 C15 117.2(3) . . ?
C7 C12 C15 124.4(2) . . ?
C17 C16 C21 120.9(2) . . ?
C17 C16 S2 120.99(18) . . ?
C21 C16 S2 118.01(18) . . ?
C18 C17 C16 117.6(2) . . ?
C18 C17 C22 116.0(2) . . ?
C16 C17 C22 126.3(2) . . ?
C19 C18 C17 123.0(2) . . ?
C20 C19 C18 117.8(2) . . ?
C20 C19 C23 121.7(2) . . ?
C18 C19 C23 120.5(2) . . ?
C19 C20 C21 122.9(2) . . ?
C20 C21 C16 117.5(2) . . ?
C20 C21 C24 117.7(2) . . ?
C16 C21 C24 124.8(2) . . ?
C26 C25 C30 120.7(2) . . ?
C26 C25 S3 115.94(19) . . ?
C30 C25 S3 123.30(19) . . ?
C27 C26 C25 118.0(3) . . ?
C27 C26 C31 117.7(3) . . ?
C25 C26 C31 124.3(2) . . ?
C28 C27 C26 122.8(3) . . ?
C29 C28 C27 117.8(3) . . ?
C29 C28 C32 121.1(3) . . ?
C27 C28 C32 121.1(3) . . ?
C28 C29 C30 123.1(3) . . ?
C29 C30 C25 117.6(2) . . ?
C29 C30 C33 116.5(2) . . ?
C25 C30 C33 125.9(2) . . ?
N5 C36 C37 110.6(2) . . ?
N6 C37 C36 111.0(2) . . ?
F1 C40 F3 107.8(2) . . ?
F1 C40 F2 107.4(2) . . ?
F3 C40 F2 106.8(2) . . ?
F1 C40 S4 111.89(19) . . ?
F3 C40 S4 111.1(2) . . ?
F2 C40 S4 111.58(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
N3 Fe1 O1 Co1 -61.40(12) . . . . ?
N4 Fe1 O1 Co1 51.12(13) . . . . ?
N2 Fe1 O1 Co1 176.05(11) . . . . ?
O5 S2 O4 Co1 72.70(18) . . . . ?
N3 S2 O4 Co1 -54.13(18) . . . . ?
C16 S2 O4 Co1 -167.08(15) . . . . ?
O7 S3 O6 Co1 122.9(2) . . . . ?
N4 S3 O6 Co1 -1.7(3) . . . . ?
C25 S3 O6 Co1 -119.9(2) . . . . ?
O10 S4 O8 Co1 79.7(2) . . . . ?
O9 S4 O8 Co1 -59.5(2) . . . . ?
C40 S4 O8 Co1 -169.7(2) . . . . ?
O3 S1 N2 C2 49.63(19) . . . . ?
O2 S1 N2 C2 177.43(16) . . . . ?
C7 S1 N2 C2 -68.64(19) . . . . ?
O3 S1 N2 Fe1 -111.79(16) . . . . ?
O2 S1 N2 Fe1 16.01(19) . . . . ?
C7 S1 N2 Fe1 129.94(16) . . . . ?
O5 S2 N3 C4 70.4(2) . . . . ?
O4 S2 N3 C4 -162.41(17) . . . . ?
C16 S2 N3 C4 -48.0(2) . . . . ?
O5 S2 N3 Fe1 -98.92(15) . . . . ?
O4 S2 N3 Fe1 28.31(16) . . . . ?
C16 S2 N3 Fe1 142.72(14) . . . . ?
O7 S3 N4 C6 29.3(2) . . . . ?
O6 S3 N4 C6 157.10(17) . . . . ?
C25 S3 N4 C6 -88.97(19) . . . . ?
O7 S3 N4 Fe1 -132.99(13) . . . . ?
O6 S3 N4 Fe1 -5.15(17) . . . . ?
C25 S3 N4 Fe1 108.78(15) . . . . ?
C5 N1 C1 C2 79.0(2) . . . . ?
C3 N1 C1 C2 -155.3(2) . . . . ?
Fe1 N1 C1 C2 -37.7(2) . . . . ?
S1 N2 C2 C1 155.60(17) . . . . ?
Fe1 N2 C2 C1 -39.9(2) . . . . ?
N1 C1 C2 N2 50.1(3) . . . . ?
C5 N1 C3 C4 -151.7(2) . . . . ?
C1 N1 C3 C4 83.2(2) . . . . ?
Fe1 N1 C3 C4 -35.3(2) . . . . ?
S2 N3 C4 C3 145.03(17) . . . . ?
Fe1 N3 C4 C3 -44.5(2) . . . . ?
N1 C3 C4 N3 51.6(2) . . . . ?
C1 N1 C5 C6 -157.0(2) . . . . ?
C3 N1 C5 C6 77.9(2) . . . . ?
Fe1 N1 C5 C6 -38.9(2) . . . . ?
S3 N4 C6 C5 167.97(17) . . . . ?
Fe1 N4 C6 C5 -27.9(3) . . . . ?
N1 C5 C6 N4 44.4(3) . . . . ?
O3 S1 C7 C12 177.70(19) . . . . ?
O2 S1 C7 C12 53.7(2) . . . . ?
N2 S1 C7 C12 -61.9(2) . . . . ?
O3 S1 C7 C8 0.1(2) . . . . ?
O2 S1 C7 C8 -123.9(2) . . . . ?
N2 S1 C7 C8 120.5(2) . . . . ?
C12 C7 C8 C9 -1.1(4) . . . . ?
S1 C7 C8 C9 176.5(2) . . . . ?
C12 C7 C8 C13 178.2(3) . . . . ?
S1 C7 C8 C13 -4.3(4) . . . . ?
C7 C8 C9 C10 0.6(4) . . . . ?
C13 C8 C9 C10 -178.8(3) . . . . ?
C8 C9 C10 C11 0.3(4) . . . . ?
C8 C9 C10 C14 178.6(3) . . . . ?
C9 C10 C11 C12 -0.7(4) . . . . ?
C14 C10 C11 C12 -179.1(3) . . . . ?
C10 C11 C12 C7 0.2(4) . . . . ?
C10 C11 C12 C15 -178.4(3) . . . . ?
C8 C7 C12 C11 0.7(4) . . . . ?
S1 C7 C12 C11 -176.9(2) . . . . ?
C8 C7 C12 C15 179.2(3) . . . . ?
S1 C7 C12 C15 1.6(4) . . . . ?
O5 S2 C16 C17 -18.2(2) . . . . ?
O4 S2 C16 C17 -142.29(19) . . . . ?
N3 S2 C16 C17 103.7(2) . . . . ?
O5 S2 C16 C21 164.88(18) . . . . ?
O4 S2 C16 C21 40.8(2) . . . . ?
N3 S2 C16 C21 -73.2(2) . . . . ?
C21 C16 C17 C18 -4.2(4) . . . . ?
S2 C16 C17 C18 179.06(19) . . . . ?
C21 C16 C17 C22 175.6(2) . . . . ?
S2 C16 C17 C22 -1.2(4) . . . . ?
C16 C17 C18 C19 0.8(4) . . . . ?
C22 C17 C18 C19 -179.0(2) . . . . ?
C17 C18 C19 C20 2.6(4) . . . . ?
C17 C18 C19 C23 -179.4(2) . . . . ?
C18 C19 C20 C21 -2.6(4) . . . . ?
C23 C19 C20 C21 179.4(2) . . . . ?
C19 C20 C21 C16 -0.6(4) . . . . ?
C19 C20 C21 C24 178.8(2) . . . . ?
C17 C16 C21 C20 4.1(3) . . . . ?
S2 C16 C21 C20 -179.02(18) . . . . ?
C17 C16 C21 C24 -175.3(2) . . . . ?
S2 C16 C21 C24 1.6(3) . . . . ?
O7 S3 C25 C26 45.4(2) . . . . ?
O6 S3 C25 C26 -77.9(2) . . . . ?
N4 S3 C25 C26 165.65(19) . . . . ?
O7 S3 C25 C30 -138.1(2) . . . . ?
O6 S3 C25 C30 98.6(2) . . . . ?
N4 S3 C25 C30 -17.8(2) . . . . ?
C30 C25 C26 C27 2.0(4) . . . . ?
S3 C25 C26 C27 178.6(2) . . . . ?
C30 C25 C26 C31 -178.0(3) . . . . ?
S3 C25 C26 C31 -1.4(4) . . . . ?
C25 C26 C27 C28 1.2(5) . . . . ?
C31 C26 C27 C28 -178.9(3) . . . . ?
C26 C27 C28 C29 -2.9(5) . . . . ?
C26 C27 C28 C32 176.9(3) . . . . ?
C27 C28 C29 C30 1.6(5) . . . . ?
C32 C28 C29 C30 -178.2(3) . . . . ?
C28 C29 C30 C25 1.4(4) . . . . ?
C28 C29 C30 C33 -175.9(3) . . . . ?
C26 C25 C30 C29 -3.2(4) . . . . ?
S3 C25 C30 C29 -179.5(2) . . . . ?
C26 C25 C30 C33 173.8(3) . . . . ?
S3 C25 C30 C33 -2.5(4) . . . . ?
C34 N5 C36 C37 74.2(3) . . . . ?
C35 N5 C36 C37 -167.9(2) . . . . ?
Co1 N5 C36 C37 -46.9(2) . . . . ?
C39 N6 C37 C36 84.4(3) . . . . ?
C38 N6 C37 C36 -158.2(2) . . . . ?
Co1 N6 C37 C36 -36.5(3) . . . . ?
N5 C36 C37 N6 59.7(3) . . . . ?
O10 S4 C40 F1 -177.07(18) . . . . ?
O9 S4 C40 F1 -53.5(2) . . . . ?
O8 S4 C40 F1 65.1(2) . . . . ?
O10 S4 C40 F3 -56.6(2) . . . . ?
O9 S4 C40 F3 67.0(2) . . . . ?
O8 S4 C40 F3 -174.44(18) . . . . ?
O10 S4 C40 F2 62.6(2) . . . . ?
O9 S4 C40 F2 -173.91(18) . . . . ?
O8 S4 C40 F2 -55.3(2) . . . . ?

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
O1 H1 O2 0.845(10) 1.796(13) 2.619(2) 164(3) .

_refine_diff_density_max         0.449
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.066



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Pentane'
####################################################################### 
# 
# 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_asb501
_database_code_depnum_ccdc_archive 'CCDC 1554812'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(en)2Fe(II)-(μ-OH)-Fe(III)MST]OTf'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C46 H78 Cl2 F3 Fe2 N8 O10 S4'
_chemical_formula_weight         1271.00

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'
F F 0.0171 0.0103 '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'
Fe Fe 0.3463 0.8444 '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                   9.0701(8)
_cell_length_b                   17.9865(15)
_cell_length_c                   18.8049(16)
_cell_angle_alpha                107.8561(11)
_cell_angle_beta                 94.8064(12)
_cell_angle_gamma                97.9985(10)
_cell_volume                     2865.5(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    8562
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      28.18

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_F_000             1334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.152
_exptl_absorpt_coefficient_mu    0.815
_shelx_estimated_absorpt_T_min   0.801
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7194
_exptl_absorpt_correction_T_max  0.8015
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            21437
_diffrn_reflns_av_unetI/netI     0.0347
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         1.208
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.906
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.906
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             12888
_reflns_number_gt                10581
_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 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.152 x 0.209 x 0.285 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (60 sec/frame scan time 
for a sphere of diffraction data).  The raw frame data was processed 
using SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  There were 
no systematic absences nor any diffraction symmetry other than the 
Friedel condition.  The centrosymmetric triclinic space group P-1 was 
assigned and later determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis. Hydrogen atoms were 
included using a riding model.  The hydrogen associated with O(1) was not
located or included in the refinement.  In addition to the triflate anion, 
there was one molecule of dichloromethane and one molecule of methyl
cyclohexane present per formula-unit.

At convergence, wR2 = 0.1326 and Goof = 1.029 for 686 variables refined 
against 12888 data (0.75 Å), R1 = 0.0474 for those 10581 data with I > 2.0sigma(I).
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0692P)²+4.5222P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12888
_refine_ls_number_parameters     686
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0474
_refine_ls_wR_factor_ref         0.1326
_refine_ls_wR_factor_gt          0.1229
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.60448(4) 0.73863(2) 0.65748(2) 0.01141(9) Uani 1 1 d . . . . .
Fe2 Fe 0.79220(4) 0.88952(2) 0.61298(2) 0.01398(9) Uani 1 1 d . . . . .
S1 S 0.88808(7) 0.63989(4) 0.63028(4) 0.01508(13) Uani 1 1 d . . . . .
S2 S 0.46857(8) 0.85653(4) 0.79515(4) 0.01911(15) Uani 1 1 d . . . . .
S3 S 0.48941(7) 0.77982(4) 0.50525(3) 0.01294(13) Uani 1 1 d . . . . .
O1 O 0.7456(2) 0.82186(11) 0.66480(10) 0.0161(4) Uani 1 1 d . . . . .
O2 O 0.9734(2) 0.71889(12) 0.64959(12) 0.0201(4) Uani 1 1 d . . . . .
O3 O 0.9058(2) 0.58600(13) 0.55826(11) 0.0227(4) Uani 1 1 d . . . . .
O4 O 0.5340(3) 0.91525(13) 0.76396(12) 0.0285(5) Uani 1 1 d . . . . .
O5 O 0.3065(2) 0.84227(15) 0.78903(12) 0.0287(5) Uani 1 1 d . . . . .
O6 O 0.6490(2) 0.81518(11) 0.51541(10) 0.0150(4) Uani 1 1 d . . . . .
O7 O 0.3902(2) 0.83676(12) 0.50797(11) 0.0184(4) Uani 1 1 d . . . . .
N1 N 0.4121(2) 0.63417(13) 0.64743(13) 0.0148(4) Uani 1 1 d . . . . .
N2 N 0.7141(2) 0.64510(13) 0.63627(13) 0.0157(4) Uani 1 1 d . . . . .
N3 N 0.5295(2) 0.77612(14) 0.75833(12) 0.0153(4) Uani 1 1 d . . . . .
N4 N 0.4655(2) 0.73592(14) 0.56541(12) 0.0146(4) Uani 1 1 d . . . . .
N5 N 0.8344(3) 0.97048(14) 0.54458(13) 0.0184(5) Uani 1 1 d . . . . .
H5A H 0.9174 1.0080 0.5667 0.022 Uiso 1 1 calc R U . . .
H5B H 0.8506 0.9424 0.4975 0.022 Uiso 1 1 calc R U . . .
N6 N 0.6245(3) 0.96444(14) 0.64263(13) 0.0184(5) Uani 1 1 d . . . . .
H6A H 0.5320 0.9360 0.6208 0.022 Uiso 1 1 calc R U . . .
H6B H 0.6250 0.9804 0.6935 0.022 Uiso 1 1 calc R U . . .
N7 N 0.9701(3) 0.96164(14) 0.70120(13) 0.0185(5) Uani 1 1 d . . . . .
H7A H 0.9946 1.0106 0.6966 0.022 Uiso 1 1 calc R U . . .
H7B H 0.9406 0.9673 0.7474 0.022 Uiso 1 1 calc R U . . .
N8 N 0.9782(3) 0.83785(14) 0.56678(13) 0.0187(5) Uani 1 1 d . . . . .
H8A H 0.9750 0.7888 0.5714 0.022 Uiso 1 1 calc R U . . .
H8B H 0.9733 0.8330 0.5170 0.022 Uiso 1 1 calc R U . . .
C1 C 0.4826(3) 0.56449(17) 0.64501(17) 0.0206(6) Uani 1 1 d . . . . .
H1A H 0.4093 0.5154 0.6188 0.025 Uiso 1 1 calc R U . . .
H1B H 0.5126 0.5650 0.6970 0.025 Uiso 1 1 calc R U . . .
C2 C 0.6189(3) 0.56526(16) 0.60429(17) 0.0207(6) Uani 1 1 d . . . . .
H2A H 0.6763 0.5243 0.6109 0.025 Uiso 1 1 calc R U . . .
H2B H 0.5876 0.5535 0.5497 0.025 Uiso 1 1 calc R U . . .
C3 C 0.3357(3) 0.65806(18) 0.71530(16) 0.0190(6) Uani 1 1 d . . . . .
H3A H 0.2888 0.6106 0.7266 0.023 Uiso 1 1 calc R U . . .
H3B H 0.2562 0.6882 0.7071 0.023 Uiso 1 1 calc R U . . .
C4 C 0.4543(3) 0.70967(18) 0.78038(16) 0.0200(6) Uani 1 1 d . . . . .
H4A H 0.4067 0.7304 0.8262 0.024 Uiso 1 1 calc R U . . .
H4B H 0.5288 0.6780 0.7914 0.024 Uiso 1 1 calc R U . . .
C5 C 0.3114(3) 0.62004(17) 0.57702(15) 0.0169(5) Uani 1 1 d . . . . .
H5C H 0.2089 0.5961 0.5815 0.020 Uiso 1 1 calc R U . . .
H5D H 0.3479 0.5827 0.5344 0.020 Uiso 1 1 calc R U . . .
C6 C 0.3074(3) 0.69796(16) 0.56222(15) 0.0158(5) Uani 1 1 d . . . . .
H6C H 0.2508 0.6885 0.5120 0.019 Uiso 1 1 calc R U . . .
H6D H 0.2574 0.7328 0.6008 0.019 Uiso 1 1 calc R U . . .
C7 C 0.9492(3) 0.59923(17) 0.70196(16) 0.0164(5) Uani 1 1 d . . . . .
C8 C 0.9818(3) 0.52137(17) 0.68334(17) 0.0200(6) Uani 1 1 d . . . . .
C9 C 1.0364(3) 0.4968(2) 0.7429(2) 0.0276(7) Uani 1 1 d . . . . .
H9 H 1.0601 0.4449 0.7315 0.033 Uiso 1 1 calc R U . . .
C10 C 1.0572(4) 0.5444(2) 0.8174(2) 0.0325(7) Uani 1 1 d . . . . .
C11 C 1.0216(3) 0.6203(2) 0.83366(18) 0.0295(7) Uani 1 1 d . . . . .
H11 H 1.0348 0.6535 0.8847 0.035 Uiso 1 1 calc R U . . .
C12 C 0.9674(3) 0.64896(18) 0.77780(16) 0.0211(6) Uani 1 1 d . . . . .
C13 C 0.9626(3) 0.46158(18) 0.60551(18) 0.0247(6) Uani 1 1 d . . . . .
H13A H 0.8604 0.4559 0.5807 0.037 Uiso 1 1 calc R U . . .
H13B H 0.9800 0.4103 0.6093 0.037 Uiso 1 1 calc R U . . .
H13C H 1.0351 0.4797 0.5759 0.037 Uiso 1 1 calc R U . . .
C14 C 1.1150(5) 0.5148(3) 0.8798(3) 0.0556(12) Uani 1 1 d . . . . .
H14A H 1.0301 0.4959 0.9025 0.083 Uiso 1 1 calc R U . . .
H14B H 1.1832 0.5582 0.9184 0.083 Uiso 1 1 calc R U . . .
H14C H 1.1690 0.4712 0.8589 0.083 Uiso 1 1 calc R U . . .
C15 C 0.9337(3) 0.73239(19) 0.80269(17) 0.0265(6) Uani 1 1 d . . . . .
H15A H 1.0100 0.7676 0.7887 0.040 Uiso 1 1 calc R U . . .
H15B H 0.9348 0.7509 0.8575 0.040 Uiso 1 1 calc R U . . .
H15C H 0.8344 0.7328 0.7780 0.040 Uiso 1 1 calc R U . . .
C16 C 0.5415(3) 0.88718(17) 0.89309(15) 0.0197(6) Uani 1 1 d . . . . .
C17 C 0.6968(3) 0.91625(18) 0.91302(16) 0.0238(6) Uani 1 1 d . . . . .
C18 C 0.7558(4) 0.9396(2) 0.98846(18) 0.0300(7) Uani 1 1 d . . . . .
H18 H 0.8602 0.9601 1.0025 0.036 Uiso 1 1 calc R U . . .
C19 C 0.6674(4) 0.9343(2) 1.04482(17) 0.0300(7) Uani 1 1 d . . . . .
C20 C 0.5164(4) 0.90496(19) 1.02318(17) 0.0276(7) Uani 1 1 d . . . . .
H20 H 0.4554 0.9010 1.0610 0.033 Uiso 1 1 calc R U . . .
C21 C 0.4486(4) 0.88090(19) 0.94876(17) 0.0248(6) Uani 1 1 d . . . . .
C22 C 0.8052(4) 0.9255(2) 0.85774(18) 0.0300(7) Uani 1 1 d . . . . .
H22A H 0.7793 0.8801 0.8112 0.045 Uiso 1 1 calc R U . . .
H22B H 0.9079 0.9277 0.8801 0.045 Uiso 1 1 calc R U . . .
H22C H 0.7983 0.9746 0.8462 0.045 Uiso 1 1 calc R U . . .
C23 C 0.7359(5) 0.9603(2) 1.12621(19) 0.0403(9) Uani 1 1 d . . . . .
H23A H 0.6572 0.9538 1.1576 0.060 Uiso 1 1 calc R U . . .
H23B H 0.7836 1.0162 1.1419 0.060 Uiso 1 1 calc R U . . .
H23C H 0.8115 0.9279 1.1321 0.060 Uiso 1 1 calc R U . . .
C24 C 0.2815(4) 0.8502(2) 0.93533(19) 0.0332(8) Uani 1 1 d . . . . .
H24A H 0.2292 0.8840 0.9136 0.050 Uiso 1 1 calc R U . . .
H24B H 0.2459 0.8510 0.9833 0.050 Uiso 1 1 calc R U . . .
H24C H 0.2609 0.7958 0.9003 0.050 Uiso 1 1 calc R U . . .
C25 C 0.4534(3) 0.70712(16) 0.41366(14) 0.0147(5) Uani 1 1 d . . . . .
C26 C 0.3190(3) 0.69761(16) 0.36555(15) 0.0169(5) Uani 1 1 d . . . . .
C27 C 0.2990(3) 0.63993(18) 0.29444(16) 0.0215(6) Uani 1 1 d . . . . .
H27 H 0.2080 0.6319 0.2620 0.026 Uiso 1 1 calc R U . . .
C28 C 0.4068(3) 0.59389(18) 0.26917(16) 0.0225(6) Uani 1 1 d . . . . .
C29 C 0.5388(3) 0.60600(17) 0.31745(16) 0.0207(6) Uani 1 1 d . . . . .
H29 H 0.6146 0.5759 0.3003 0.025 Uiso 1 1 calc R U . . .
C30 C 0.5645(3) 0.66080(16) 0.39034(15) 0.0160(5) Uani 1 1 d . . . . .
C31 C 0.1929(3) 0.74419(18) 0.38347(17) 0.0225(6) Uani 1 1 d . . . . .
H31A H 0.1636 0.7436 0.4323 0.034 Uiso 1 1 calc R U . . .
H31B H 0.1065 0.7202 0.3442 0.034 Uiso 1 1 calc R U . . .
H31C H 0.2268 0.7991 0.3856 0.034 Uiso 1 1 calc R U . . .
C32 C 0.3787(4) 0.5313(2) 0.19238(18) 0.0369(8) Uani 1 1 d . . . . .
H32A H 0.4725 0.5123 0.1799 0.055 Uiso 1 1 calc R U . . .
H32B H 0.3423 0.5541 0.1546 0.055 Uiso 1 1 calc R U . . .
H32C H 0.3031 0.4869 0.1928 0.055 Uiso 1 1 calc R U . . .
C33 C 0.7107(3) 0.66547(18) 0.43765(16) 0.0212(6) Uani 1 1 d . . . . .
H33A H 0.7823 0.7115 0.4375 0.032 Uiso 1 1 calc R U . . .
H33B H 0.7521 0.6170 0.4167 0.032 Uiso 1 1 calc R U . . .
H33C H 0.6925 0.6708 0.4895 0.032 Uiso 1 1 calc R U . . .
C34 C 0.7008(3) 1.00882(18) 0.53994(16) 0.0215(6) Uani 1 1 d . . . . .
H34A H 0.6181 0.9708 0.5037 0.026 Uiso 1 1 calc R U . . .
H34B H 0.7259 1.0551 0.5225 0.026 Uiso 1 1 calc R U . . .
C35 C 0.6532(3) 1.03500(17) 0.61763(16) 0.0205(6) Uani 1 1 d . . . . .
H35A H 0.7335 1.0755 0.6532 0.025 Uiso 1 1 calc R U . . .
H35B H 0.5610 1.0585 0.6161 0.025 Uiso 1 1 calc R U . . .
C36 C 1.1006(3) 0.91971(18) 0.69210(16) 0.0218(6) Uani 1 1 d . . . . .
H36A H 1.0840 0.8742 0.7113 0.026 Uiso 1 1 calc R U . . .
H36B H 1.1928 0.9561 0.7213 0.026 Uiso 1 1 calc R U . . .
C37 C 1.1189(3) 0.89061(18) 0.60892(16) 0.0216(6) Uani 1 1 d . . . . .
H37A H 1.1400 0.9363 0.5902 0.026 Uiso 1 1 calc R U . . .
H37B H 1.2041 0.8613 0.6017 0.026 Uiso 1 1 calc R U . . .
Cl1 Cl 1.23256(19) 0.69877(9) 0.11439(7) 0.0777(4) Uani 1 1 d . . . . .
Cl2 Cl 1.29807(14) 0.87244(8) 0.18058(6) 0.0567(3) Uani 1 1 d . . . . .
C39 C 1.2327(5) 0.7807(3) 0.1945(2) 0.0482(10) Uani 1 1 d . . . . .
H39A H 1.2975 0.7759 0.2373 0.058 Uiso 1 1 calc R U . . .
H39B H 1.1294 0.7804 0.2078 0.058 Uiso 1 1 calc R U . . .
S4 S 0.88103(8) 0.82821(5) 0.32437(4) 0.02472(16) Uani 1 1 d . . . . .
O8 O 0.9175(3) 0.8647(2) 0.40401(14) 0.0490(8) Uani 1 1 d . . . . .
O9 O 0.8582(3) 0.74244(14) 0.29882(15) 0.0368(6) Uani 1 1 d . . . . .
O10 O 0.9727(3) 0.86444(14) 0.28143(15) 0.0358(6) Uani 1 1 d . . . . .
C38 C 0.6953(4) 0.8492(2) 0.30284(19) 0.0295(7) Uani 1 1 d . . . . .
F1 F 0.6982(2) 0.92770(13) 0.32340(15) 0.0491(6) Uani 1 1 d . . . . .
F2 F 0.6476(3) 0.82032(17) 0.22958(13) 0.0564(7) Uani 1 1 d . . . . .
F3 F 0.5945(2) 0.81939(15) 0.33796(16) 0.0516(7) Uani 1 1 d . . . . .
C40 C 0.9227(5) 0.7840(3) 0.0378(3) 0.0569(12) Uani 1 1 d . . . . .
H40A H 0.9819 0.7449 0.0118 0.085 Uiso 1 1 calc R U . . .
H40B H 0.9727 0.8121 0.0893 0.085 Uiso 1 1 calc R U . . .
H40C H 0.9141 0.8221 0.0107 0.085 Uiso 1 1 calc R U . . .
C41 C 0.7692(5) 0.7426(3) 0.0405(2) 0.0472(10) Uani 1 1 d . . . . .
H41 H 0.7159 0.7833 0.0719 0.057 Uiso 1 1 calc R U . . .
C42 C 0.7752(5) 0.6787(3) 0.0786(3) 0.0496(10) Uani 1 1 d . . . . .
H42A H 0.8319 0.6388 0.0502 0.060 Uiso 1 1 calc R U . . .
H42B H 0.8295 0.7034 0.1303 0.060 Uiso 1 1 calc R U . . .
C43 C 0.6188(5) 0.6375(3) 0.0824(3) 0.0504(10) Uani 1 1 d . . . . .
H43A H 0.5660 0.6760 0.1159 0.060 Uiso 1 1 calc R U . . .
H43B H 0.6277 0.5943 0.1041 0.060 Uiso 1 1 calc R U . . .
C44 C 0.5273(5) 0.6030(3) 0.0040(2) 0.0504(10) Uani 1 1 d . . . . .
H44A H 0.5738 0.5597 -0.0273 0.060 Uiso 1 1 calc R U . . .
H44B H 0.4245 0.5797 0.0086 0.060 Uiso 1 1 calc R U . . .
C45 C 0.5178(5) 0.6629(3) -0.0348(2) 0.0483(10) Uani 1 1 d . . . . .
H45A H 0.4577 0.7019 -0.0079 0.058 Uiso 1 1 calc R U . . .
H45B H 0.4658 0.6364 -0.0868 0.058 Uiso 1 1 calc R U . . .
C46 C 0.6750(5) 0.7065(3) -0.0376(2) 0.0468(10) Uani 1 1 d . . . . .
H46A H 0.7290 0.6688 -0.0712 0.056 Uiso 1 1 calc R U . . .
H46B H 0.6638 0.7493 -0.0595 0.056 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 O1 1.7915(19) . ?
Fe1 N3 2.018(2) . ?
Fe1 N2 2.024(2) . ?
Fe1 N4 2.038(2) . ?
Fe1 N1 2.329(2) . ?
Fe2 O1 1.8061(19) . ?
Fe2 O6 2.1106(18) . ?
Fe2 N8 2.156(2) . ?
Fe2 N7 2.165(2) . ?
Fe2 N6 2.166(2) . ?
Fe2 N5 2.236(2) . ?
S1 O3 1.440(2) . ?
S1 O2 1.442(2) . ?
S1 N2 1.605(2) . ?
S1 C7 1.803(3) . ?
S2 O4 1.441(2) . ?
S2 O5 1.445(2) . ?
S2 N3 1.596(2) . ?
S2 C16 1.790(3) . ?
S3 O7 1.4470(19) . ?
S3 O6 1.4694(18) . ?
S3 N4 1.579(2) . ?
S3 C25 1.786(3) . ?
N1 C1 1.475(3) . ?
N1 C5 1.476(3) . ?
N1 C3 1.479(3) . ?
N2 C2 1.486(3) . ?
N3 C4 1.480(3) . ?
N4 C6 1.488(3) . ?
N5 C34 1.485(4) . ?
N6 C35 1.481(3) . ?
N7 C36 1.483(4) . ?
N8 C37 1.480(4) . ?
C1 C2 1.509(4) . ?
C3 C4 1.524(4) . ?
C5 C6 1.515(4) . ?
C7 C12 1.414(4) . ?
C7 C8 1.415(4) . ?
C8 C9 1.403(4) . ?
C8 C13 1.506(4) . ?
C9 C10 1.380(5) . ?
C10 C11 1.394(5) . ?
C10 C14 1.515(5) . ?
C11 C12 1.388(4) . ?
C12 C15 1.512(4) . ?
C16 C17 1.408(4) . ?
C16 C21 1.419(4) . ?
C17 C18 1.386(4) . ?
C17 C22 1.519(4) . ?
C18 C19 1.400(4) . ?
C19 C20 1.375(5) . ?
C19 C23 1.506(4) . ?
C20 C21 1.391(4) . ?
C21 C24 1.511(4) . ?
C25 C30 1.409(4) . ?
C25 C26 1.413(4) . ?
C26 C27 1.398(4) . ?
C26 C31 1.510(4) . ?
C27 C28 1.389(4) . ?
C28 C29 1.389(4) . ?
C28 C32 1.509(4) . ?
C29 C30 1.400(4) . ?
C30 C33 1.511(4) . ?
C34 C35 1.511(4) . ?
C36 C37 1.521(4) . ?
Cl1 C39 1.754(4) . ?
Cl2 C39 1.777(4) . ?
S4 O8 1.427(3) . ?
S4 O10 1.433(2) . ?
S4 O9 1.447(3) . ?
S4 C38 1.817(3) . ?
C38 F3 1.319(4) . ?
C38 F2 1.324(4) . ?
C38 F1 1.341(4) . ?
C40 C41 1.497(6) . ?
C41 C42 1.534(6) . ?
C41 C46 1.536(6) . ?
C42 C43 1.524(6) . ?
C43 C44 1.530(6) . ?
C44 C45 1.482(6) . ?
C45 C46 1.543(6) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N3 100.73(9) . . ?
O1 Fe1 N2 104.73(9) . . ?
N3 Fe1 N2 118.35(9) . . ?
O1 Fe1 N4 100.35(9) . . ?
N3 Fe1 N4 116.84(9) . . ?
N2 Fe1 N4 112.30(9) . . ?
O1 Fe1 N1 177.20(8) . . ?
N3 Fe1 N1 78.40(9) . . ?
N2 Fe1 N1 77.98(8) . . ?
N4 Fe1 N1 77.80(8) . . ?
O1 Fe2 O6 92.32(8) . . ?
O1 Fe2 N8 96.08(9) . . ?
O6 Fe2 N8 89.02(8) . . ?
O1 Fe2 N7 92.00(9) . . ?
O6 Fe2 N7 170.05(8) . . ?
N8 Fe2 N7 81.62(9) . . ?
O1 Fe2 N6 100.05(9) . . ?
O6 Fe2 N6 90.94(8) . . ?
N8 Fe2 N6 163.85(9) . . ?
N7 Fe2 N6 97.12(9) . . ?
O1 Fe2 N5 176.18(9) . . ?
O6 Fe2 N5 84.39(8) . . ?
N8 Fe2 N5 85.84(9) . . ?
N7 Fe2 N5 91.55(9) . . ?
N6 Fe2 N5 78.09(8) . . ?
O3 S1 O2 115.42(13) . . ?
O3 S1 N2 110.77(12) . . ?
O2 S1 N2 109.27(12) . . ?
O3 S1 C7 107.83(13) . . ?
O2 S1 C7 107.03(12) . . ?
N2 S1 C7 106.04(12) . . ?
O4 S2 O5 116.05(14) . . ?
O4 S2 N3 108.49(12) . . ?
O5 S2 N3 110.89(13) . . ?
O4 S2 C16 108.17(14) . . ?
O5 S2 C16 107.83(13) . . ?
N3 S2 C16 104.78(13) . . ?
O7 S3 O6 112.99(12) . . ?
O7 S3 N4 112.67(12) . . ?
O6 S3 N4 108.33(11) . . ?
O7 S3 C25 108.45(12) . . ?
O6 S3 C25 105.79(11) . . ?
N4 S3 C25 108.28(12) . . ?
Fe1 O1 Fe2 138.40(11) . . ?
S3 O6 Fe2 130.58(11) . . ?
C1 N1 C5 111.2(2) . . ?
C1 N1 C3 110.8(2) . . ?
C5 N1 C3 112.7(2) . . ?
C1 N1 Fe1 107.19(15) . . ?
C5 N1 Fe1 107.53(15) . . ?
C3 N1 Fe1 107.21(16) . . ?
C2 N2 S1 110.92(17) . . ?
C2 N2 Fe1 116.22(16) . . ?
S1 N2 Fe1 131.36(13) . . ?
C4 N3 S2 112.18(18) . . ?
C4 N3 Fe1 112.35(17) . . ?
S2 N3 Fe1 128.28(13) . . ?
C6 N4 S3 114.15(17) . . ?
C6 N4 Fe1 114.08(16) . . ?
S3 N4 Fe1 130.78(12) . . ?
C34 N5 Fe2 108.33(16) . . ?
C35 N6 Fe2 111.52(16) . . ?
C36 N7 Fe2 106.52(17) . . ?
C37 N8 Fe2 107.98(16) . . ?
N1 C1 C2 110.4(2) . . ?
N2 C2 C1 108.4(2) . . ?
N1 C3 C4 107.3(2) . . ?
N3 C4 C3 108.2(2) . . ?
N1 C5 C6 109.4(2) . . ?
N4 C6 C5 107.5(2) . . ?
C12 C7 C8 121.0(3) . . ?
C12 C7 S1 117.4(2) . . ?
C8 C7 S1 121.6(2) . . ?
C9 C8 C7 117.2(3) . . ?
C9 C8 C13 116.4(3) . . ?
C7 C8 C13 126.4(3) . . ?
C10 C9 C8 123.0(3) . . ?
C9 C10 C11 118.1(3) . . ?
C9 C10 C14 121.0(4) . . ?
C11 C10 C14 120.9(4) . . ?
C12 C11 C10 122.3(3) . . ?
C11 C12 C7 118.4(3) . . ?
C11 C12 C15 117.2(3) . . ?
C7 C12 C15 124.4(3) . . ?
C17 C16 C21 120.8(3) . . ?
C17 C16 S2 117.3(2) . . ?
C21 C16 S2 121.9(2) . . ?
C18 C17 C16 118.3(3) . . ?
C18 C17 C22 117.0(3) . . ?
C16 C17 C22 124.7(3) . . ?
C17 C18 C19 122.4(3) . . ?
C20 C19 C18 117.7(3) . . ?
C20 C19 C23 121.5(3) . . ?
C18 C19 C23 120.8(3) . . ?
C19 C20 C21 123.3(3) . . ?
C20 C21 C16 117.5(3) . . ?
C20 C21 C24 116.1(3) . . ?
C16 C21 C24 126.3(3) . . ?
C30 C25 C26 121.1(2) . . ?
C30 C25 S3 118.0(2) . . ?
C26 C25 S3 120.9(2) . . ?
C27 C26 C25 117.7(2) . . ?
C27 C26 C31 116.1(2) . . ?
C25 C26 C31 126.1(2) . . ?
C28 C27 C26 122.7(3) . . ?
C27 C28 C29 117.9(3) . . ?
C27 C28 C32 120.7(3) . . ?
C29 C28 C32 121.4(3) . . ?
C28 C29 C30 122.5(3) . . ?
C29 C30 C25 117.9(2) . . ?
C29 C30 C33 116.8(2) . . ?
C25 C30 C33 125.3(2) . . ?
N5 C34 C35 107.9(2) . . ?
N6 C35 C34 108.0(2) . . ?
N7 C36 C37 108.9(2) . . ?
N8 C37 C36 108.5(2) . . ?
Cl1 C39 Cl2 112.6(2) . . ?
O8 S4 O10 114.00(18) . . ?
O8 S4 O9 114.79(18) . . ?
O10 S4 O9 114.49(15) . . ?
O8 S4 C38 104.49(16) . . ?
O10 S4 C38 104.02(15) . . ?
O9 S4 C38 103.17(15) . . ?
F3 C38 F2 107.9(3) . . ?
F3 C38 F1 107.7(3) . . ?
F2 C38 F1 106.8(3) . . ?
F3 C38 S4 112.4(2) . . ?
F2 C38 S4 111.4(2) . . ?
F1 C38 S4 110.3(2) . . ?
C40 C41 C42 112.1(4) . . ?
C40 C41 C46 112.8(4) . . ?
C42 C41 C46 109.9(4) . . ?
C43 C42 C41 112.1(4) . . ?
C42 C43 C44 110.9(4) . . ?
C45 C44 C43 112.9(4) . . ?
C44 C45 C46 111.5(4) . . ?
C41 C46 C45 112.7(3) . . ?

_refine_diff_density_max         2.005
_refine_diff_density_min         -1.142
_refine_diff_density_rms         0.091


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Methylcyclohexane'
####################################################################### 
# 
# 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_asb457
_database_code_depnum_ccdc_archive 'CCDC 1554811'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Ni(II)(Br)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H64 Br Cl2 Fe N6 Ni O7 S3'
_chemical_formula_weight         1102.52

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   21.8160(18)
_cell_length_b                   13.1714(11)
_cell_length_c                   17.6057(14)
_cell_angle_alpha                90
_cell_angle_beta                 107.5355(10)
_cell_angle_gamma                90
_cell_volume                     4823.9(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9203
_cell_measurement_theta_min      2.43
_cell_measurement_theta_max      28.95

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.518
_exptl_crystal_F_000             2292
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.379
_exptl_crystal_size_mid          0.356
_exptl_crystal_size_min          0.227
_exptl_absorpt_coefficient_mu    1.812
_shelx_estimated_absorpt_T_min   0.547
_shelx_estimated_absorpt_T_max   0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6131
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            58560
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.830
_diffrn_reflns_theta_max         29.075
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.939
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.939
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.939
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12122
_reflns_number_gt                10529
_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 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.227 x 0.356 x 0.379 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (25 sec/frame scan time for 
a sphere of diffraction data).  The raw frame data was processed using 
SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The diffraction 
symmetry was 2/m and the systematic absences were consistent with the 
monoclinic space group P21/c that was later determined to be correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis.  Hydrogen atom H(1) 
was located from a difference-Fourier map and refined (x,y,z and Uiso) 
with d(O-H) = 0.85Å.  The remaining hydrogen atoms were included using a 
riding model.  There was one molecule of dichloromethane present that was 
disordered over two positions (0.55:0.45). At convergence, wR2 = 0.0833 and 
Goof = 1.036 for 584 variables refined against 12122 data (0.73 Å), 
R1 = 0.0307 for those 10529 data with I > 2.0sigma(I).  
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0416P)²+4.8685P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12122
_refine_ls_number_parameters     584
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0307
_refine_ls_wR_factor_ref         0.0833
_refine_ls_wR_factor_gt          0.0799
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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
Br1 Br 0.22871(2) 0.45567(2) 0.58207(2) 0.01837(5) Uani 1 1 d . . . . .
Fe1 Fe 0.25198(2) 0.43459(2) 0.28306(2) 0.00880(6) Uani 1 1 d . . . . .
Ni1 Ni 0.29137(2) 0.47548(2) 0.48850(2) 0.01262(6) Uani 1 1 d . . . . .
S1 S 0.37884(2) 0.53079(3) 0.24350(3) 0.01103(9) Uani 1 1 d . . . . .
S2 S 0.26233(2) 0.24044(3) 0.39503(3) 0.01090(9) Uani 1 1 d . . . . .
S3 S 0.14586(2) 0.57830(3) 0.32462(3) 0.01145(9) Uani 1 1 d . . . . .
O1 O 0.30578(6) 0.48165(10) 0.38242(8) 0.0119(3) Uani 1 1 d D . . . .
H1 H 0.3400(8) 0.501(2) 0.3748(17) 0.032(8) Uiso 1 1 d D . . . .
O2 O 0.40491(6) 0.53065(11) 0.33008(8) 0.0152(3) Uani 1 1 d . . . . .
O3 O 0.37017(7) 0.63009(10) 0.20708(8) 0.0163(3) Uani 1 1 d . . . . .
O4 O 0.26156(7) 0.32135(10) 0.45116(8) 0.0140(3) Uani 1 1 d . . . . .
O5 O 0.32163(7) 0.18436(11) 0.41228(8) 0.0175(3) Uani 1 1 d . . . . .
O6 O 0.19938(7) 0.58742(11) 0.39660(8) 0.0157(3) Uani 1 1 d . . . . .
O7 O 0.08696(7) 0.53849(10) 0.33395(9) 0.0167(3) Uani 1 1 d . . . . .
N1 N 0.19715(7) 0.37306(12) 0.16196(9) 0.0114(3) Uani 1 1 d . . . . .
N2 N 0.31354(7) 0.46634(12) 0.21837(9) 0.0114(3) Uani 1 1 d . . . . .
N3 N 0.24130(8) 0.28924(12) 0.30834(9) 0.0120(3) Uani 1 1 d . . . . .
N4 N 0.16909(7) 0.50991(12) 0.26270(9) 0.0118(3) Uani 1 1 d . . . . .
N5 N 0.38173(8) 0.41564(14) 0.55717(10) 0.0181(3) Uani 1 1 d . . . . .
N6 N 0.33219(9) 0.62059(13) 0.53055(10) 0.0188(3) Uani 1 1 d . . . . .
C1 C 0.24125(9) 0.36883(15) 0.11244(11) 0.0142(4) Uani 1 1 d . . . . .
H1A H 0.2161 0.3689 0.0553 0.017 Uiso 1 1 calc R U . . .
H1B H 0.2667 0.3054 0.1238 0.017 Uiso 1 1 calc R U . . .
C2 C 0.28580(9) 0.45935(15) 0.13040(11) 0.0150(4) Uani 1 1 d . . . . .
H2A H 0.3205 0.4507 0.1054 0.018 Uiso 1 1 calc R U . . .
H2B H 0.2617 0.5221 0.1091 0.018 Uiso 1 1 calc R U . . .
C3 C 0.17421(9) 0.26944(14) 0.17377(11) 0.0137(4) Uani 1 1 d . . . . .
H3A H 0.1659 0.2296 0.1240 0.016 Uiso 1 1 calc R U . . .
H3B H 0.1336 0.2740 0.1878 0.016 Uiso 1 1 calc R U . . .
C4 C 0.22571(9) 0.21782(14) 0.24058(11) 0.0140(4) Uani 1 1 d . . . . .
H4A H 0.2095 0.1529 0.2554 0.017 Uiso 1 1 calc R U . . .
H4B H 0.2643 0.2037 0.2239 0.017 Uiso 1 1 calc R U . . .
C5 C 0.14344(9) 0.44439(15) 0.12794(11) 0.0146(4) Uani 1 1 d . . . . .
H5A H 0.1095 0.4100 0.0854 0.018 Uiso 1 1 calc R U . . .
H5B H 0.1591 0.5032 0.1040 0.018 Uiso 1 1 calc R U . . .
C6 C 0.11555(9) 0.48117(15) 0.19257(11) 0.0157(4) Uani 1 1 d . . . . .
H6A H 0.0872 0.5404 0.1732 0.019 Uiso 1 1 calc R U . . .
H6B H 0.0898 0.4266 0.2068 0.019 Uiso 1 1 calc R U . . .
C7 C 0.43601(9) 0.46376(14) 0.20726(11) 0.0116(3) Uani 1 1 d . . . . .
C8 C 0.45869(9) 0.50492(15) 0.14672(11) 0.0143(4) Uani 1 1 d . . . . .
C9 C 0.50904(10) 0.45499(16) 0.12909(13) 0.0199(4) Uani 1 1 d . . . . .
H9A H 0.5254 0.4828 0.0893 0.024 Uiso 1 1 calc R U . . .
C10 C 0.53630(10) 0.36621(17) 0.16723(13) 0.0219(4) Uani 1 1 d . . . . .
C11 C 0.51048(9) 0.32457(15) 0.22364(12) 0.0168(4) Uani 1 1 d . . . . .
H11A H 0.5276 0.2625 0.2487 0.020 Uiso 1 1 calc R U . . .
C12 C 0.46048(9) 0.37087(14) 0.24443(11) 0.0127(3) Uani 1 1 d . . . . .
C13 C 0.43192(10) 0.59726(16) 0.09640(12) 0.0184(4) Uani 1 1 d . . . . .
H13A H 0.4504 0.6016 0.0522 0.028 Uiso 1 1 calc R U . . .
H13B H 0.4430 0.6585 0.1293 0.028 Uiso 1 1 calc R U . . .
H13C H 0.3851 0.5914 0.0752 0.028 Uiso 1 1 calc R U . . .
C14 C 0.59006(14) 0.3143(2) 0.14569(18) 0.0404(7) Uani 1 1 d . . . . .
H14A H 0.6036 0.2541 0.1792 0.061 Uiso 1 1 calc R U . . .
H14B H 0.6264 0.3611 0.1542 0.061 Uiso 1 1 calc R U . . .
H14C H 0.5752 0.2940 0.0896 0.061 Uiso 1 1 calc R U . . .
C15 C 0.43501(10) 0.31730(15) 0.30483(12) 0.0173(4) Uani 1 1 d . . . . .
H15A H 0.4501 0.2468 0.3108 0.026 Uiso 1 1 calc R U . . .
H15B H 0.3879 0.3182 0.2865 0.026 Uiso 1 1 calc R U . . .
H15C H 0.4505 0.3521 0.3563 0.026 Uiso 1 1 calc R U . . .
C16 C 0.19979(9) 0.15436(14) 0.39865(10) 0.0117(3) Uani 1 1 d . . . . .
C17 C 0.20956(9) 0.04790(14) 0.40271(11) 0.0129(4) Uani 1 1 d . . . . .
C18 C 0.15988(10) -0.01327(14) 0.41187(11) 0.0149(4) Uani 1 1 d . . . . .
H18A H 0.1659 -0.0847 0.4153 0.018 Uiso 1 1 calc R U . . .
C19 C 0.10175(10) 0.02657(15) 0.41620(11) 0.0156(4) Uani 1 1 d . . . . .
C20 C 0.09298(9) 0.13111(15) 0.40884(11) 0.0144(4) Uani 1 1 d . . . . .
H20A H 0.0531 0.1589 0.4099 0.017 Uiso 1 1 calc R U . . .
C21 C 0.14041(9) 0.19660(14) 0.39999(11) 0.0136(4) Uani 1 1 d . . . . .
C22 C 0.26948(10) -0.00617(15) 0.39702(13) 0.0183(4) Uani 1 1 d . . . . .
H22A H 0.2621 -0.0797 0.3945 0.027 Uiso 1 1 calc R U . . .
H22B H 0.3057 0.0101 0.4440 0.027 Uiso 1 1 calc R U . . .
H22C H 0.2793 0.0162 0.3489 0.027 Uiso 1 1 calc R U . . .
C23 C 0.04972(10) -0.04101(16) 0.42770(13) 0.0215(4) Uani 1 1 d . . . . .
H23A H 0.0107 -0.0010 0.4217 0.032 Uiso 1 1 calc R U . . .
H23B H 0.0639 -0.0708 0.4812 0.032 Uiso 1 1 calc R U . . .
H23C H 0.0406 -0.0953 0.3878 0.032 Uiso 1 1 calc R U . . .
C24 C 0.12465(10) 0.30873(14) 0.39241(12) 0.0167(4) Uani 1 1 d . . . . .
H24A H 0.0782 0.3180 0.3808 0.025 Uiso 1 1 calc R U . . .
H24B H 0.1386 0.3377 0.3491 0.025 Uiso 1 1 calc R U . . .
H24C H 0.1470 0.3431 0.4425 0.025 Uiso 1 1 calc R U . . .
C25 C 0.12856(9) 0.70247(14) 0.28055(11) 0.0117(3) Uani 1 1 d . . . . .
C26 C 0.06837(9) 0.75052(14) 0.27113(11) 0.0130(3) Uani 1 1 d . . . . .
C27 C 0.06012(9) 0.84923(14) 0.24077(11) 0.0142(4) Uani 1 1 d . . . . .
H27A H 0.0199 0.8817 0.2339 0.017 Uiso 1 1 calc R U . . .
C28 C 0.10775(9) 0.90213(14) 0.22015(11) 0.0139(4) Uani 1 1 d . . . . .
C29 C 0.16558(9) 0.85239(14) 0.22772(11) 0.0141(4) Uani 1 1 d . . . . .
H29A H 0.1984 0.8870 0.2128 0.017 Uiso 1 1 calc R U . . .
C30 C 0.17694(9) 0.75319(14) 0.25656(11) 0.0129(3) Uani 1 1 d . . . . .
C31 C 0.01126(9) 0.70450(15) 0.29003(12) 0.0175(4) Uani 1 1 d . . . . .
H31A H -0.0248 0.7523 0.2752 0.026 Uiso 1 1 calc R U . . .
H31B H 0.0227 0.6900 0.3472 0.026 Uiso 1 1 calc R U . . .
H31C H -0.0011 0.6413 0.2599 0.026 Uiso 1 1 calc R U . . .
C32 C 0.09689(10) 1.01065(15) 0.19200(12) 0.0173(4) Uani 1 1 d . . . . .
H32A H 0.0534 1.0177 0.1550 0.026 Uiso 1 1 calc R U . . .
H32B H 0.1285 1.0293 0.1649 0.026 Uiso 1 1 calc R U . . .
H32C H 0.1017 1.0555 0.2378 0.026 Uiso 1 1 calc R U . . .
C33 C 0.24013(9) 0.70624(15) 0.25681(12) 0.0171(4) Uani 1 1 d . . . . .
H33A H 0.2714 0.7601 0.2580 0.026 Uiso 1 1 calc R U . . .
H33B H 0.2338 0.6652 0.2086 0.026 Uiso 1 1 calc R U . . .
H33C H 0.2562 0.6630 0.3039 0.026 Uiso 1 1 calc R U . . .
C36 C 0.41434(12) 0.50092(19) 0.60818(14) 0.0299(5) Uani 1 1 d . . . . .
H36A H 0.4611 0.4874 0.6283 0.036 Uiso 1 1 calc R U . . .
H36B H 0.3978 0.5072 0.6545 0.036 Uiso 1 1 calc R U . . .
C34 C 0.42209(10) 0.37974(18) 0.50804(13) 0.0230(4) Uani 1 1 d . . . . .
H34A H 0.4633 0.3550 0.5430 0.034 Uiso 1 1 calc R U . . .
H34B H 0.4297 0.4360 0.4755 0.034 Uiso 1 1 calc R U . . .
H34C H 0.3999 0.3246 0.4732 0.034 Uiso 1 1 calc R U . . .
C35 C 0.37575(11) 0.32923(19) 0.60851(14) 0.0281(5) Uani 1 1 d . . . . .
H35A H 0.4184 0.3106 0.6435 0.042 Uiso 1 1 calc R U . . .
H35B H 0.3567 0.2710 0.5750 0.042 Uiso 1 1 calc R U . . .
H35C H 0.3482 0.3489 0.6409 0.042 Uiso 1 1 calc R U . . .
C38 C 0.32446(13) 0.69702(17) 0.46754(14) 0.0297(5) Uani 1 1 d . . . . .
H38A H 0.3494 0.7577 0.4898 0.045 Uiso 1 1 calc R U . . .
H38B H 0.2789 0.7151 0.4458 0.045 Uiso 1 1 calc R U . . .
H38C H 0.3399 0.6692 0.4250 0.045 Uiso 1 1 calc R U . . .
C39 C 0.31038(15) 0.6654(2) 0.59408(16) 0.0383(6) Uani 1 1 d . . . . .
H39A H 0.3353 0.7269 0.6140 0.057 Uiso 1 1 calc R U . . .
H39B H 0.3165 0.6164 0.6377 0.057 Uiso 1 1 calc R U . . .
H39C H 0.2647 0.6828 0.5731 0.057 Uiso 1 1 calc R U . . .
C37 C 0.40283(12) 0.59748(19) 0.56194(15) 0.0309(5) Uani 1 1 d . . . . .
H37A H 0.4209 0.5919 0.5169 0.037 Uiso 1 1 calc R U . . .
H37B H 0.4251 0.6538 0.5966 0.037 Uiso 1 1 calc R U . . .
C40 C 0.0955(2) 0.6390(4) 0.5166(3) 0.0257(11) Uiso 0.55 1 d . . P A 1
H40A H 0.1173 0.5983 0.5643 0.031 Uiso 0.55 1 calc R U P A 1
H40B H 0.0972 0.5999 0.4693 0.031 Uiso 0.55 1 calc R U P A 1
Cl1 Cl 0.0122(6) 0.6551(6) 0.5124(4) 0.0570(14) Uani 0.55 1 d . . P A 1
Cl2 Cl 0.1340(2) 0.7415(3) 0.5197(3) 0.0491(7) Uani 0.55 1 d . . P A 1
C40B C 0.0791(3) 0.6158(5) 0.5099(4) 0.0251(13) Uiso 0.45 1 d . . P B 2
H40C H 0.0790 0.5866 0.4581 0.030 Uiso 0.45 1 calc R U P B 2
H40D H 0.0969 0.5649 0.5522 0.030 Uiso 0.45 1 calc R U P B 2
Cl1B Cl 0.0026(7) 0.6502(8) 0.5081(5) 0.062(2) Uani 0.45 1 d . . P B 2
Cl2B Cl 0.1315(4) 0.7436(6) 0.5322(5) 0.095(2) Uani 0.45 1 d . . P B 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 Ni1 2.4510(3) . ?
Fe1 O1 1.8933(13) . ?
Fe1 N3 1.9949(16) . ?
Fe1 N4 1.9980(16) . ?
Fe1 N2 2.0487(16) . ?
Fe1 N1 2.2576(15) . ?
Ni1 O1 1.9868(13) . ?
Ni1 N5 2.1291(18) . ?
Ni1 N6 2.1440(17) . ?
Ni1 O4 2.1723(13) . ?
Ni1 O6 2.6197(14) . ?
S1 O3 1.4437(14) . ?
S1 O2 1.4576(14) . ?
S1 N2 1.6020(16) . ?
S1 C7 1.7949(19) . ?
S2 O5 1.4404(14) . ?
S2 O4 1.4568(13) . ?
S2 N3 1.5910(16) . ?
S2 C16 1.7899(19) . ?
S3 O7 1.4425(14) . ?
S3 O6 1.4463(14) . ?
S3 N4 1.6092(16) . ?
S3 C25 1.8008(19) . ?
N1 C5 1.480(2) . ?
N1 C1 1.481(2) . ?
N1 C3 1.490(2) . ?
N2 C2 1.486(2) . ?
N3 C4 1.476(2) . ?
N4 C6 1.471(2) . ?
N5 C36 1.480(3) . ?
N5 C35 1.483(3) . ?
N5 C34 1.485(3) . ?
N6 C39 1.465(3) . ?
N6 C38 1.470(3) . ?
N6 C37 1.503(3) . ?
C1 C2 1.510(3) . ?
C3 C4 1.520(3) . ?
C5 C6 1.522(3) . ?
C7 C8 1.412(3) . ?
C7 C12 1.414(3) . ?
C8 C9 1.393(3) . ?
C8 C13 1.514(3) . ?
C9 C10 1.390(3) . ?
C10 C11 1.393(3) . ?
C10 C14 1.501(3) . ?
C11 C12 1.392(3) . ?
C12 C15 1.514(3) . ?
C16 C21 1.417(3) . ?
C16 C17 1.417(3) . ?
C17 C18 1.398(3) . ?
C17 C22 1.518(3) . ?
C18 C19 1.395(3) . ?
C19 C20 1.391(3) . ?
C19 C23 1.504(3) . ?
C20 C21 1.392(3) . ?
C21 C24 1.513(3) . ?
C25 C30 1.417(3) . ?
C25 C26 1.422(3) . ?
C26 C27 1.397(3) . ?
C26 C31 1.510(3) . ?
C27 C28 1.387(3) . ?
C28 C29 1.392(3) . ?
C28 C32 1.508(3) . ?
C29 C30 1.397(3) . ?
C30 C33 1.510(3) . ?
C36 C37 1.490(4) . ?
C40 Cl2 1.582(7) . ?
C40 Cl1 1.810(12) . ?
C40B Cl1B 1.721(14) . ?
C40B Cl2B 2.004(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
O1 Fe1 N3 100.93(6) . . ?
O1 Fe1 N4 106.19(6) . . ?
N3 Fe1 N4 110.87(7) . . ?
O1 Fe1 N2 96.84(6) . . ?
N3 Fe1 N2 117.40(6) . . ?
N4 Fe1 N2 120.55(6) . . ?
O1 Fe1 N1 174.09(6) . . ?
N3 Fe1 N1 78.57(6) . . ?
N4 Fe1 N1 79.37(6) . . ?
N2 Fe1 N1 78.33(6) . . ?
O1 Ni1 N5 99.63(6) . . ?
O1 Ni1 N6 96.96(6) . . ?
N5 Ni1 N6 85.23(7) . . ?
O1 Ni1 O4 82.61(5) . . ?
N5 Ni1 O4 88.13(6) . . ?
N6 Ni1 O4 173.18(6) . . ?
O1 Ni1 Br1 156.12(4) . . ?
N5 Ni1 Br1 100.80(5) . . ?
N6 Ni1 Br1 96.93(5) . . ?
O4 Ni1 Br1 85.83(4) . . ?
O1 Ni1 O6 72.85(5) . . ?
N5 Ni1 O6 164.80(6) . . ?
N6 Ni1 O6 82.69(6) . . ?
O4 Ni1 O6 103.61(5) . . ?
Br1 Ni1 O6 89.80(3) . . ?
O3 S1 O2 115.04(8) . . ?
O3 S1 N2 111.76(8) . . ?
O2 S1 N2 108.81(8) . . ?
O3 S1 C7 107.45(8) . . ?
O2 S1 C7 106.09(8) . . ?
N2 S1 C7 107.25(8) . . ?
O5 S2 O4 115.17(8) . . ?
O5 S2 N3 112.99(9) . . ?
O4 S2 N3 107.23(8) . . ?
O5 S2 C16 108.27(9) . . ?
O4 S2 C16 105.94(8) . . ?
N3 S2 C16 106.71(8) . . ?
O7 S3 O6 116.23(8) . . ?
O7 S3 N4 110.30(8) . . ?
O6 S3 N4 107.71(8) . . ?
O7 S3 C25 107.51(8) . . ?
O6 S3 C25 108.13(8) . . ?
N4 S3 C25 106.53(8) . . ?
Fe1 O1 Ni1 128.72(7) . . ?
S2 O4 Ni1 145.63(8) . . ?
S3 O6 Ni1 139.50(8) . . ?
C5 N1 C1 111.17(15) . . ?
C5 N1 C3 112.31(15) . . ?
C1 N1 C3 110.66(14) . . ?
C5 N1 Fe1 106.49(11) . . ?
C1 N1 Fe1 108.43(11) . . ?
C3 N1 Fe1 107.56(11) . . ?
C2 N2 S1 111.69(12) . . ?
C2 N2 Fe1 115.94(11) . . ?
S1 N2 Fe1 129.20(9) . . ?
C4 N3 S2 116.58(12) . . ?
C4 N3 Fe1 116.44(11) . . ?
S2 N3 Fe1 125.62(9) . . ?
C6 N4 S3 112.34(12) . . ?
C6 N4 Fe1 118.02(12) . . ?
S3 N4 Fe1 127.53(9) . . ?
C36 N5 C35 109.10(17) . . ?
C36 N5 C34 109.53(17) . . ?
C35 N5 C34 106.68(17) . . ?
C36 N5 Ni1 104.90(14) . . ?
C35 N5 Ni1 113.18(13) . . ?
C34 N5 Ni1 113.40(12) . . ?
C39 N6 C38 108.11(19) . . ?
C39 N6 C37 109.49(19) . . ?
C38 N6 C37 106.74(18) . . ?
C39 N6 Ni1 115.20(14) . . ?
C38 N6 Ni1 114.13(13) . . ?
C37 N6 Ni1 102.68(13) . . ?
N1 C1 C2 109.76(15) . . ?
N2 C2 C1 107.54(15) . . ?
N1 C3 C4 108.46(15) . . ?
N3 C4 C3 106.06(15) . . ?
N1 C5 C6 110.22(15) . . ?
N4 C6 C5 108.31(15) . . ?
C8 C7 C12 120.82(17) . . ?
C8 C7 S1 121.24(14) . . ?
C12 C7 S1 117.84(14) . . ?
C9 C8 C7 117.79(18) . . ?
C9 C8 C13 116.10(17) . . ?
C7 C8 C13 126.08(17) . . ?
C10 C9 C8 122.74(19) . . ?
C9 C10 C11 118.01(18) . . ?
C9 C10 C14 120.92(19) . . ?
C11 C10 C14 121.01(19) . . ?
C12 C11 C10 122.16(18) . . ?
C11 C12 C7 118.30(17) . . ?
C11 C12 C15 117.58(17) . . ?
C7 C12 C15 124.11(17) . . ?
C21 C16 C17 120.82(17) . . ?
C21 C16 S2 117.55(14) . . ?
C17 C16 S2 121.60(14) . . ?
C18 C17 C16 117.78(17) . . ?
C18 C17 C22 116.75(17) . . ?
C16 C17 C22 125.47(17) . . ?
C19 C18 C17 122.56(18) . . ?
C20 C19 C18 117.98(18) . . ?
C20 C19 C23 120.68(18) . . ?
C18 C19 C23 121.34(18) . . ?
C19 C20 C21 122.55(18) . . ?
C20 C21 C16 118.23(17) . . ?
C20 C21 C24 117.26(17) . . ?
C16 C21 C24 124.51(17) . . ?
C30 C25 C26 120.01(17) . . ?
C30 C25 S3 118.58(14) . . ?
C26 C25 S3 121.40(14) . . ?
C27 C26 C25 117.84(17) . . ?
C27 C26 C31 115.99(17) . . ?
C25 C26 C31 126.16(17) . . ?
C28 C27 C26 123.19(17) . . ?
C27 C28 C29 117.86(17) . . ?
C27 C28 C32 120.41(17) . . ?
C29 C28 C32 121.72(17) . . ?
C28 C29 C30 122.11(17) . . ?
C29 C30 C25 118.88(17) . . ?
C29 C30 C33 116.49(16) . . ?
C25 C30 C33 124.59(17) . . ?
N5 C36 C37 110.21(18) . . ?
C36 C37 N6 111.04(19) . . ?
Cl2 C40 Cl1 114.7(4) . . ?
Cl1B C40B Cl2B 106.0(5) . . ?

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
N3 Fe1 O1 Ni1 -55.87(10) . . . . ?
N4 Fe1 O1 Ni1 59.84(10) . . . . ?
N2 Fe1 O1 Ni1 -175.55(9) . . . . ?
O5 S2 O4 Ni1 78.32(17) . . . . ?
N3 S2 O4 Ni1 -48.38(17) . . . . ?
C16 S2 O4 Ni1 -162.05(14) . . . . ?
O7 S3 O6 Ni1 83.30(13) . . . . ?
N4 S3 O6 Ni1 -40.99(14) . . . . ?
C25 S3 O6 Ni1 -155.75(11) . . . . ?
O3 S1 N2 C2 54.48(15) . . . . ?
O2 S1 N2 C2 -177.40(12) . . . . ?
C7 S1 N2 C2 -63.05(14) . . . . ?
O3 S1 N2 Fe1 -104.26(12) . . . . ?
O2 S1 N2 Fe1 23.86(14) . . . . ?
C7 S1 N2 Fe1 138.21(11) . . . . ?
O5 S2 N3 C4 64.26(16) . . . . ?
O4 S2 N3 C4 -167.78(13) . . . . ?
C16 S2 N3 C4 -54.62(15) . . . . ?
O5 S2 N3 Fe1 -101.86(12) . . . . ?
O4 S2 N3 Fe1 26.11(13) . . . . ?
C16 S2 N3 Fe1 139.26(11) . . . . ?
O7 S3 N4 C6 42.52(15) . . . . ?
O6 S3 N4 C6 170.32(13) . . . . ?
C25 S3 N4 C6 -73.86(15) . . . . ?
O7 S3 N4 Fe1 -120.45(11) . . . . ?
O6 S3 N4 Fe1 7.34(14) . . . . ?
C25 S3 N4 Fe1 123.16(11) . . . . ?
C5 N1 C1 C2 79.67(18) . . . . ?
C3 N1 C1 C2 -154.81(15) . . . . ?
Fe1 N1 C1 C2 -37.06(17) . . . . ?
S1 N2 C2 C1 159.05(13) . . . . ?
Fe1 N2 C2 C1 -39.16(18) . . . . ?
N1 C1 C2 N2 49.3(2) . . . . ?
C5 N1 C3 C4 -153.73(15) . . . . ?
C1 N1 C3 C4 81.39(17) . . . . ?
Fe1 N1 C3 C4 -36.88(16) . . . . ?
S2 N3 C4 C3 148.31(13) . . . . ?
Fe1 N3 C4 C3 -44.27(18) . . . . ?
N1 C3 C4 N3 51.78(18) . . . . ?
C1 N1 C5 C6 -156.74(15) . . . . ?
C3 N1 C5 C6 78.66(18) . . . . ?
Fe1 N1 C5 C6 -38.83(17) . . . . ?
S3 N4 C6 C5 163.88(13) . . . . ?
Fe1 N4 C6 C5 -31.4(2) . . . . ?
N1 C5 C6 N4 46.2(2) . . . . ?
O3 S1 C7 C8 -6.77(18) . . . . ?
O2 S1 C7 C8 -130.30(16) . . . . ?
N2 S1 C7 C8 113.54(16) . . . . ?
O3 S1 C7 C12 169.70(14) . . . . ?
O2 S1 C7 C12 46.17(16) . . . . ?
N2 S1 C7 C12 -70.00(16) . . . . ?
C12 C7 C8 C9 -4.6(3) . . . . ?
S1 C7 C8 C9 171.75(15) . . . . ?
C12 C7 C8 C13 173.18(19) . . . . ?
S1 C7 C8 C13 -10.5(3) . . . . ?
C7 C8 C9 C10 1.5(3) . . . . ?
C13 C8 C9 C10 -176.5(2) . . . . ?
C8 C9 C10 C11 1.9(3) . . . . ?
C8 C9 C10 C14 179.3(2) . . . . ?
C9 C10 C11 C12 -2.3(3) . . . . ?
C14 C10 C11 C12 -179.7(2) . . . . ?
C10 C11 C12 C7 -0.7(3) . . . . ?
C10 C11 C12 C15 178.37(19) . . . . ?
C8 C7 C12 C11 4.3(3) . . . . ?
S1 C7 C12 C11 -172.22(15) . . . . ?
C8 C7 C12 C15 -174.76(18) . . . . ?
S1 C7 C12 C15 8.8(3) . . . . ?
O5 S2 C16 C21 167.10(14) . . . . ?
O4 S2 C16 C21 43.04(16) . . . . ?
N3 S2 C16 C21 -71.00(15) . . . . ?
O5 S2 C16 C17 -10.85(17) . . . . ?
O4 S2 C16 C17 -134.90(15) . . . . ?
N3 S2 C16 C17 111.06(15) . . . . ?
C21 C16 C17 C18 -3.0(3) . . . . ?
S2 C16 C17 C18 174.91(14) . . . . ?
C21 C16 C17 C22 176.30(17) . . . . ?
S2 C16 C17 C22 -5.8(3) . . . . ?
C16 C17 C18 C19 0.7(3) . . . . ?
C22 C17 C18 C19 -178.64(18) . . . . ?
C17 C18 C19 C20 1.8(3) . . . . ?
C17 C18 C19 C23 -178.76(18) . . . . ?
C18 C19 C20 C21 -2.1(3) . . . . ?
C23 C19 C20 C21 178.46(18) . . . . ?
C19 C20 C21 C16 -0.1(3) . . . . ?
C19 C20 C21 C24 179.86(17) . . . . ?
C17 C16 C21 C20 2.7(3) . . . . ?
S2 C16 C21 C20 -175.25(14) . . . . ?
C17 C16 C21 C24 -177.27(17) . . . . ?
S2 C16 C21 C24 4.8(2) . . . . ?
O7 S3 C25 C30 -172.71(14) . . . . ?
O6 S3 C25 C30 61.06(16) . . . . ?
N4 S3 C25 C30 -54.48(16) . . . . ?
O7 S3 C25 C26 8.57(17) . . . . ?
O6 S3 C25 C26 -117.65(15) . . . . ?
N4 S3 C25 C26 126.81(15) . . . . ?
C30 C25 C26 C27 -2.4(3) . . . . ?
S3 C25 C26 C27 176.28(14) . . . . ?
C30 C25 C26 C31 176.83(18) . . . . ?
S3 C25 C26 C31 -4.5(3) . . . . ?
C25 C26 C27 C28 -0.4(3) . . . . ?
C31 C26 C27 C28 -179.77(18) . . . . ?
C26 C27 C28 C29 2.3(3) . . . . ?
C26 C27 C28 C32 -176.59(18) . . . . ?
C27 C28 C29 C30 -1.3(3) . . . . ?
C32 C28 C29 C30 177.56(18) . . . . ?
C28 C29 C30 C25 -1.5(3) . . . . ?
C28 C29 C30 C33 176.30(18) . . . . ?
C26 C25 C30 C29 3.3(3) . . . . ?
S3 C25 C30 C29 -175.39(14) . . . . ?
C26 C25 C30 C33 -174.23(17) . . . . ?
S3 C25 C30 C33 7.0(3) . . . . ?
C35 N5 C36 C37 -162.0(2) . . . . ?
C34 N5 C36 C37 81.5(2) . . . . ?
Ni1 N5 C36 C37 -40.5(2) . . . . ?
N5 C36 C37 N6 59.4(3) . . . . ?
C39 N6 C37 C36 80.0(2) . . . . ?
C38 N6 C37 C36 -163.25(19) . . . . ?
Ni1 N6 C37 C36 -42.9(2) . . . . ?

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
O1 H1 O2 0.836(10) 1.858(12) 2.6729(19) 164(3) .

_refine_diff_density_max         0.990
_refine_diff_density_min         -0.854
_refine_diff_density_rms         0.078


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/Pentane'
####################################################################### 
# 
# 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_asb445
_database_code_depnum_ccdc_archive 'CCDC 1554808'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Fe(II)(NCS)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H62 Fe2 N7 O7 S4'
_chemical_formula_weight         992.90

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'

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   34.669(3)
_cell_length_b                   34.669(3)
_cell_length_c                   20.8648(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     21718(4)
_cell_formula_units_Z            18
_cell_measurement_temperature    88(2)
_cell_measurement_reflns_used    9820
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      28.54

_exptl_crystal_description       irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_F_000             9414
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.352
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.158
_exptl_absorpt_coefficient_mu    0.826
_shelx_estimated_absorpt_T_min   0.760
_shelx_estimated_absorpt_T_max   0.881
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6828
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      88(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            85581
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_av_R_equivalents  0.0491
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.671
_diffrn_reflns_theta_max         27.102
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             10658
_reflns_number_gt                9003
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.158 x 0.159 x 0.352 mm was 
mounted in a cryoloop and transferred to a Bruker SMART APEX II 
diffractometer.  The APEX2 program package was used to determine the 
unit-cell parameters and for data collection (30 sec/frame scan time 
for a sphere of diffraction data).  The raw frame data was processed 
using SAINT and SADABS to yield the reflection data file.  Subsequent 
calculations were carried out using the SHELXTL program.  The systematic 
absences were consistent with the hexagonal space groups R3 and R-3.  The 
centrosymmetric space group R-3 was assigned and later determined to be 
correct.

The structure was solved by dual space methods and refined on F2 by 
full-matrix least-squares techniques.  The analytical scattering factors 
for neutral atoms were used throughout the analysis. Hydrogen atom H(1) 
was located from a difference-Fourier map and refined (x,y,z and Uiso).  
The  remaining hydrogen atoms were included using a riding model.  
Atoms C(34), C(36), C(37) and C(39) were disordered and included using 
multiple components with partial site-occupancy-factors.

At convergence, wR2 = 0.0781 and Goof = 1.041 for 596 variables refined 
against 10658 data (0.78 Å), R1 = 0.0290 for those 9003 data 
with I > 2.0sigma(I).

There were several high residuals present in the final difference-Fourier 
map.  It was not possible to determine the nature of the residuals although 
it was probable that pentane and/or dichloromethane was present. The SQUEEZE
routine in the PLATON program package was used to account for the electrons 
in the solvent accessible voids.  
;

# start Validation Reply Form
_vrf_PLAT412_asb445              
;
PROBLEM: Short Intra XH3 .. XHn     H38A   ..  H37C    ..       1.69 Ang.  
RESPONSE: ...The short contacts are due to disordered carbon atoms associated
with the hydrogens.
;
# end Validation Reply Form

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0386P)²+28.6379P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10658
_refine_ls_number_parameters     596
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0290
_refine_ls_wR_factor_ref         0.0781
_refine_ls_wR_factor_gt          0.0740
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_restrained_S_all      1.041
_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
Fe1 Fe 0.52809(2) 0.45814(2) 0.70088(2) 0.01088(6) Uani 1 1 d . . . . .
Fe2 Fe 0.62118(2) 0.56318(2) 0.69179(2) 0.01303(6) Uani 1 1 d . . . . .
S1 S 0.52752(2) 0.42252(2) 0.55356(2) 0.01549(9) Uani 1 1 d . . . . .
S2 S 0.60542(2) 0.47264(2) 0.80132(2) 0.01533(9) Uani 1 1 d . . . . .
S3 S 0.51145(2) 0.53945(2) 0.73771(2) 0.01278(9) Uani 1 1 d . . . . .
S4 S 0.72916(2) 0.69814(2) 0.77800(2) 0.02613(11) Uani 1 1 d . . . . .
O1 O 0.57773(4) 0.50428(4) 0.65830(6) 0.0148(2) Uani 1 1 d . . . . .
H1 H 0.5803(8) 0.4963(8) 0.6245(12) 0.030(6) Uiso 1 1 d . . . . .
O2 O 0.57212(4) 0.46159(4) 0.55245(6) 0.0194(3) Uani 1 1 d . . . . .
O3 O 0.49653(4) 0.42291(4) 0.50842(6) 0.0222(3) Uani 1 1 d . . . . .
O4 O 0.62459(4) 0.51755(4) 0.77572(6) 0.0194(3) Uani 1 1 d . . . . .
O5 O 0.63054(4) 0.45068(5) 0.78875(6) 0.0235(3) Uani 1 1 d . . . . .
O6 O 0.55689(4) 0.56356(4) 0.71390(6) 0.0169(3) Uani 1 1 d . . . . .
O7 O 0.50435(4) 0.54928(4) 0.80223(6) 0.0194(3) Uani 1 1 d . . . . .
N1 N 0.46795(5) 0.39955(4) 0.74065(6) 0.0131(3) Uani 1 1 d . . . . .
N2 N 0.50867(5) 0.41541(5) 0.62540(7) 0.0142(3) Uani 1 1 d . . . . .
N3 N 0.55510(5) 0.44494(5) 0.77624(7) 0.0147(3) Uani 1 1 d . . . . .
N4 N 0.49337(5) 0.48746(5) 0.72955(7) 0.0136(3) Uani 1 1 d . . . . .
N5 N 0.68233(5) 0.56738(5) 0.64441(7) 0.0197(3) Uani 1 1 d . . . . .
N6 N 0.62676(5) 0.60616(6) 0.60840(8) 0.0262(4) Uani 1 1 d . . . . .
N7 N 0.65557(5) 0.61442(5) 0.75431(7) 0.0191(3) Uani 1 1 d . . . . .
C1 C 0.45505(6) 0.36073(5) 0.69792(8) 0.0163(3) Uani 1 1 d . . . . .
H1A H 0.4232 0.3386 0.7041 0.020 Uiso 1 1 calc R U . . .
H1B H 0.4728 0.3464 0.7086 0.020 Uiso 1 1 calc R U . . .
C2 C 0.46321(6) 0.37611(6) 0.62908(8) 0.0167(4) Uani 1 1 d . . . . .
H2A H 0.4608 0.3521 0.6009 0.020 Uiso 1 1 calc R U . . .
H2B H 0.4409 0.3842 0.6151 0.020 Uiso 1 1 calc R U . . .
C3 C 0.47983(6) 0.39129(6) 0.80551(8) 0.0170(4) Uani 1 1 d . . . . .
H3A H 0.4593 0.3601 0.8183 0.020 Uiso 1 1 calc R U . . .
H3B H 0.4771 0.4111 0.8370 0.020 Uiso 1 1 calc R U . . .
C4 C 0.52738(6) 0.40014(6) 0.80458(8) 0.0179(4) Uani 1 1 d . . . . .
H4A H 0.5375 0.3993 0.8486 0.021 Uiso 1 1 calc R U . . .
H4B H 0.5294 0.3774 0.7784 0.021 Uiso 1 1 calc R U . . .
C5 C 0.43245(6) 0.41137(6) 0.74270(8) 0.0164(3) Uani 1 1 d . . . . .
H5A H 0.4087 0.3911 0.7725 0.020 Uiso 1 1 calc R U . . .
H5B H 0.4192 0.4077 0.6995 0.020 Uiso 1 1 calc R U . . .
C6 C 0.45121(6) 0.45925(6) 0.76479(9) 0.0179(4) Uani 1 1 d . . . . .
H6A H 0.4296 0.4694 0.7559 0.022 Uiso 1 1 calc R U . . .
H6B H 0.4570 0.4615 0.8115 0.022 Uiso 1 1 calc R U . . .
C7 C 0.53471(6) 0.37573(6) 0.53657(8) 0.0175(4) Uani 1 1 d . . . . .
C8 C 0.56685(6) 0.37146(6) 0.57291(9) 0.0215(4) Uani 1 1 d . . . . .
C9 C 0.57457(7) 0.33665(6) 0.55795(10) 0.0256(4) Uani 1 1 d . . . . .
H9 H 0.5962 0.3336 0.5819 0.031 Uiso 1 1 calc R U . . .
C10 C 0.55180(7) 0.30644(7) 0.50947(11) 0.0308(5) Uani 1 1 d . . . . .
C11 C 0.51998(7) 0.31106(6) 0.47551(10) 0.0283(5) Uani 1 1 d . . . . .
H11 H 0.5041 0.2902 0.4425 0.034 Uiso 1 1 calc R U . . .
C12 C 0.51020(6) 0.34483(6) 0.48752(9) 0.0215(4) Uani 1 1 d . . . . .
C13 C 0.59348(8) 0.40121(7) 0.62802(11) 0.0329(5) Uani 1 1 d . . . . .
H13A H 0.6142 0.4311 0.6118 0.049 Uiso 1 1 calc R U . . .
H13B H 0.6103 0.3889 0.6488 0.049 Uiso 1 1 calc R U . . .
H13C H 0.5732 0.4029 0.6592 0.049 Uiso 1 1 calc R U . . .
C14 C 0.56032(10) 0.26834(9) 0.49633(14) 0.0523(7) Uani 1 1 d . . . . .
H14A H 0.5864 0.2728 0.5209 0.078 Uiso 1 1 calc R U . . .
H14B H 0.5659 0.2674 0.4505 0.078 Uiso 1 1 calc R U . . .
H14C H 0.5342 0.2402 0.5092 0.078 Uiso 1 1 calc R U . . .
C15 C 0.47363(6) 0.34467(7) 0.44789(9) 0.0257(4) Uani 1 1 d . . . . .
H15A H 0.4502 0.3426 0.4763 0.039 Uiso 1 1 calc R U . . .
H15B H 0.4611 0.3191 0.4188 0.039 Uiso 1 1 calc R U . . .
H15C H 0.4859 0.3722 0.4229 0.039 Uiso 1 1 calc R U . . .
C16 C 0.60038(6) 0.47555(6) 0.88690(8) 0.0160(3) Uani 1 1 d . . . . .
C17 C 0.60881(6) 0.44869(6) 0.92910(9) 0.0194(4) Uani 1 1 d . . . . .
C18 C 0.60131(6) 0.45112(6) 0.99450(9) 0.0214(4) Uani 1 1 d . . . . .
H18 H 0.6074 0.4337 1.0234 0.026 Uiso 1 1 calc R U . . .
C19 C 0.58554(6) 0.47760(6) 1.01920(9) 0.0202(4) Uani 1 1 d . . . . .
C20 C 0.57759(6) 0.50361(6) 0.97640(8) 0.0188(4) Uani 1 1 d . . . . .
H20 H 0.5670 0.5222 0.9925 0.023 Uiso 1 1 calc R U . . .
C21 C 0.58466(6) 0.50333(6) 0.91073(8) 0.0170(4) Uani 1 1 d . . . . .
C22 C 0.62459(7) 0.41673(7) 0.90979(10) 0.0279(4) Uani 1 1 d . . . . .
H22A H 0.6034 0.3948 0.8794 0.042 Uiso 1 1 calc R U . . .
H22B H 0.6266 0.4013 0.9479 0.042 Uiso 1 1 calc R U . . .
H22C H 0.6540 0.4333 0.8895 0.042 Uiso 1 1 calc R U . . .
C23 C 0.57590(7) 0.47793(7) 1.08951(9) 0.0275(4) Uani 1 1 d . . . . .
H23A H 0.5732 0.4512 1.1099 0.041 Uiso 1 1 calc R U . . .
H23B H 0.5480 0.4783 1.0948 0.041 Uiso 1 1 calc R U . . .
H23C H 0.6003 0.5045 1.1096 0.041 Uiso 1 1 calc R U . . .
C24 C 0.57410(7) 0.53246(6) 0.86934(9) 0.0239(4) Uani 1 1 d . . . . .
H24A H 0.6019 0.5580 0.8540 0.036 Uiso 1 1 calc R U . . .
H24B H 0.5574 0.5432 0.8945 0.036 Uiso 1 1 calc R U . . .
H24C H 0.5561 0.5152 0.8326 0.036 Uiso 1 1 calc R U . . .
C25 C 0.47871(5) 0.55483(6) 0.68878(8) 0.0140(3) Uani 1 1 d . . . . .
C26 C 0.47687(6) 0.59304(6) 0.70790(9) 0.0190(4) Uani 1 1 d . . . . .
C27 C 0.44743(7) 0.60245(7) 0.67568(9) 0.0244(4) Uani 1 1 d . . . . .
H27 H 0.4458 0.6280 0.6880 0.029 Uiso 1 1 calc R U . . .
C28 C 0.42034(6) 0.57606(7) 0.62632(9) 0.0237(4) Uani 1 1 d . . . . .
C29 C 0.42540(6) 0.54090(6) 0.60583(9) 0.0222(4) Uani 1 1 d . . . . .
H29 H 0.4081 0.5235 0.5706 0.027 Uiso 1 1 calc R U . . .
C30 C 0.45500(6) 0.53007(6) 0.63495(8) 0.0176(4) Uani 1 1 d . . . . .
C31 C 0.50609(8) 0.62545(7) 0.75896(10) 0.0302(5) Uani 1 1 d . . . . .
H31A H 0.4932 0.6139 0.8013 0.045 Uiso 1 1 calc R U . . .
H31B H 0.5080 0.6543 0.7521 0.045 Uiso 1 1 calc R U . . .
H31C H 0.5360 0.6291 0.7566 0.045 Uiso 1 1 calc R U . . .
C32 C 0.38789(7) 0.58694(8) 0.59385(12) 0.0372(6) Uani 1 1 d . . . . .
H32A H 0.3744 0.5672 0.5569 0.056 Uiso 1 1 calc R U . . .
H32B H 0.4037 0.6180 0.5794 0.056 Uiso 1 1 calc R U . . .
H32C H 0.3645 0.5826 0.6243 0.056 Uiso 1 1 calc R U . . .
C33 C 0.46081(7) 0.49408(6) 0.60258(9) 0.0273(4) Uani 1 1 d . . . . .
H33A H 0.4921 0.5020 0.6049 0.041 Uiso 1 1 calc R U . . .
H33B H 0.4517 0.4915 0.5576 0.041 Uiso 1 1 calc R U . . .
H33C H 0.4423 0.4656 0.6244 0.041 Uiso 1 1 calc R U . . .
C34 C 0.72338(16) 0.59532(14) 0.6787(2) 0.0236(9) Uani 0.75 1 d . . P A 1
H34A H 0.7278 0.6254 0.6828 0.035 Uiso 0.75 1 calc R U P A 1
H34B H 0.7484 0.5966 0.6551 0.035 Uiso 0.75 1 calc R U P A 1
H34C H 0.7217 0.5829 0.7215 0.035 Uiso 0.75 1 calc R U P A 1
C34B C 0.7204(5) 0.5810(4) 0.6969(6) 0.025(3) Uani 0.25 1 d . . P A 2
H34D H 0.7269 0.6092 0.7169 0.038 Uiso 0.25 1 calc R U P A 2
H34E H 0.7474 0.5845 0.6764 0.038 Uiso 0.25 1 calc R U P A 2
H34F H 0.7103 0.5578 0.7297 0.038 Uiso 0.25 1 calc R U P A 2
C35 C 0.67715(7) 0.52354(7) 0.63075(11) 0.0282(4) Uani 1 1 d . . . . .
H35A H 0.6726 0.5072 0.6710 0.042 Uiso 1 1 calc R U . . .
H35B H 0.7040 0.5273 0.6094 0.042 Uiso 1 1 calc R U . . .
H35C H 0.6514 0.5068 0.6027 0.042 Uiso 1 1 calc R U . . .
C36 C 0.68337(12) 0.58748(11) 0.57937(16) 0.0210(7) Uani 0.75 1 d . . P A 1
H36A H 0.6615 0.5640 0.5506 0.025 Uiso 0.75 1 calc R U P A 1
H36B H 0.7133 0.5993 0.5601 0.025 Uiso 0.75 1 calc R U P A 1
C36B C 0.6986(4) 0.6019(4) 0.5986(6) 0.031(2) Uani 0.25 1 d . . P A 2
H36C H 0.7202 0.5997 0.5701 0.037 Uiso 0.25 1 calc R U P A 2
H36D H 0.7142 0.6311 0.6206 0.037 Uiso 0.25 1 calc R U P A 2
C37 C 0.67256(9) 0.62485(9) 0.58510(13) 0.0214(5) Uani 0.75 1 d . . P A 1
H37A H 0.6935 0.6478 0.6153 0.026 Uiso 0.75 1 calc R U P A 1
H37B H 0.6757 0.6390 0.5428 0.026 Uiso 0.75 1 calc R U P A 1
C37B C 0.6622(3) 0.5988(4) 0.5612(4) 0.033(2) Uani 0.25 1 d . . P A 2
H37C H 0.6460 0.5691 0.5405 0.040 Uiso 0.25 1 calc R U P A 2
H37D H 0.6739 0.6217 0.5271 0.040 Uiso 0.25 1 calc R U P A 2
C38 C 0.59110(7) 0.58194(7) 0.56098(9) 0.0290(5) Uani 1 1 d . . . . .
H38A H 0.5919 0.5555 0.5463 0.043 Uiso 1 1 calc R U . . .
H38B H 0.5955 0.6014 0.5243 0.043 Uiso 1 1 calc R U . . .
H38C H 0.5621 0.5728 0.5807 0.043 Uiso 1 1 calc R U . . .
C39 C 0.62137(12) 0.64598(12) 0.62992(19) 0.0227(7) Uani 0.75 1 d . . P A 1
H39A H 0.5914 0.6348 0.6476 0.034 Uiso 0.75 1 calc R U P A 1
H39B H 0.6256 0.6652 0.5930 0.034 Uiso 0.75 1 calc R U P A 1
H39C H 0.6436 0.6631 0.6628 0.034 Uiso 0.75 1 calc R U P A 1
C39B C 0.6381(4) 0.6454(4) 0.6146(5) 0.031(3) Uani 0.25 1 d . . P A 2
H39D H 0.6153 0.6481 0.6388 0.047 Uiso 0.25 1 calc R U P A 2
H39E H 0.6417 0.6590 0.5722 0.047 Uiso 0.25 1 calc R U P A 2
H39F H 0.6665 0.6607 0.6377 0.047 Uiso 0.25 1 calc R U P A 2
C40 C 0.68606(6) 0.64952(6) 0.76486(8) 0.0154(3) 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
Fe1 O1 1.8861(12) . ?
Fe1 N3 1.9969(14) . ?
Fe1 N4 2.0158(14) . ?
Fe1 N2 2.0324(14) . ?
Fe1 N1 2.2195(14) . ?
Fe2 O1 1.9624(12) . ?
Fe2 N7 2.0399(15) . ?
Fe2 N6 2.2355(16) . ?
Fe2 N5 2.2768(15) . ?
Fe2 O6 2.2825(12) . ?
Fe2 O4 2.4019(12) . ?
S1 O3 1.4337(13) . ?
S1 O2 1.4600(13) . ?
S1 N2 1.6043(14) . ?
S1 C7 1.7954(18) . ?
S2 O5 1.4387(13) . ?
S2 O4 1.4548(13) . ?
S2 N3 1.6012(14) . ?
S2 C16 1.8018(17) . ?
S3 O7 1.4398(12) . ?
S3 O6 1.4529(12) . ?
S3 N4 1.5942(14) . ?
S3 C25 1.7941(17) . ?
S4 C40 1.6219(18) . ?
N1 C5 1.479(2) . ?
N1 C3 1.484(2) . ?
N1 C1 1.485(2) . ?
N2 C2 1.483(2) . ?
N3 C4 1.481(2) . ?
N4 C6 1.484(2) . ?
N5 C36B 1.410(11) . ?
N5 C34 1.448(5) . ?
N5 C35 1.467(2) . ?
N5 C36 1.518(4) . ?
N5 C34B 1.594(14) . ?
N6 C39B 1.219(10) . ?
N6 C37 1.466(3) . ?
N6 C38 1.475(2) . ?
N6 C39 1.549(4) . ?
N6 C37B 1.691(9) . ?
N7 C40 1.166(2) . ?
C1 C2 1.509(2) . ?
C3 C4 1.519(2) . ?
C5 C6 1.520(2) . ?
C7 C8 1.415(3) . ?
C7 C12 1.417(2) . ?
C8 C9 1.396(3) . ?
C8 C13 1.512(3) . ?
C9 C10 1.384(3) . ?
C10 C11 1.386(3) . ?
C10 C14 1.516(3) . ?
C11 C12 1.395(3) . ?
C12 C15 1.511(3) . ?
C16 C21 1.413(2) . ?
C16 C17 1.414(2) . ?
C17 C18 1.400(3) . ?
C17 C22 1.515(3) . ?
C18 C19 1.382(3) . ?
C19 C20 1.391(3) . ?
C19 C23 1.506(3) . ?
C20 C21 1.393(2) . ?
C21 C24 1.507(2) . ?
C25 C30 1.403(2) . ?
C25 C26 1.415(2) . ?
C26 C27 1.390(3) . ?
C26 C31 1.512(3) . ?
C27 C28 1.386(3) . ?
C28 C29 1.383(3) . ?
C28 C32 1.514(3) . ?
C29 C30 1.396(3) . ?
C30 C33 1.518(3) . ?
C36 C37 1.523(4) . ?
C36B C37B 1.442(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N3 103.40(6) . . ?
O1 Fe1 N4 103.53(6) . . ?
N3 Fe1 N4 110.40(6) . . ?
O1 Fe1 N2 94.72(6) . . ?
N3 Fe1 N2 117.74(6) . . ?
N4 Fe1 N2 122.27(6) . . ?
O1 Fe1 N1 173.49(5) . . ?
N3 Fe1 N1 80.18(5) . . ?
N4 Fe1 N1 79.98(5) . . ?
N2 Fe1 N1 78.78(5) . . ?
O1 Fe2 N7 160.78(6) . . ?
O1 Fe2 N6 100.48(6) . . ?
N7 Fe2 N6 95.69(6) . . ?
O1 Fe2 N5 96.76(5) . . ?
N7 Fe2 N5 95.85(6) . . ?
N6 Fe2 N5 81.48(6) . . ?
O1 Fe2 O6 80.46(5) . . ?
N7 Fe2 O6 90.74(5) . . ?
N6 Fe2 O6 84.99(5) . . ?
N5 Fe2 O6 165.46(5) . . ?
O1 Fe2 O4 80.75(5) . . ?
N7 Fe2 O4 84.70(5) . . ?
N6 Fe2 O4 171.93(5) . . ?
N5 Fe2 O4 90.45(5) . . ?
O6 Fe2 O4 103.07(4) . . ?
O3 S1 O2 115.57(8) . . ?
O3 S1 N2 111.46(8) . . ?
O2 S1 N2 108.57(7) . . ?
O3 S1 C7 108.79(8) . . ?
O2 S1 C7 105.90(8) . . ?
N2 S1 C7 105.99(8) . . ?
O5 S2 O4 115.21(8) . . ?
O5 S2 N3 112.91(8) . . ?
O4 S2 N3 107.43(7) . . ?
O5 S2 C16 108.15(8) . . ?
O4 S2 C16 108.01(8) . . ?
N3 S2 C16 104.50(8) . . ?
O7 S3 O6 116.63(8) . . ?
O7 S3 N4 110.50(7) . . ?
O6 S3 N4 108.31(7) . . ?
O7 S3 C25 104.68(8) . . ?
O6 S3 C25 107.44(8) . . ?
N4 S3 C25 109.01(8) . . ?
Fe1 O1 Fe2 127.94(7) . . ?
S2 O4 Fe2 145.69(7) . . ?
S3 O6 Fe2 147.89(7) . . ?
C5 N1 C3 112.13(13) . . ?
C5 N1 C1 110.68(13) . . ?
C3 N1 C1 111.08(13) . . ?
C5 N1 Fe1 106.75(10) . . ?
C3 N1 Fe1 107.06(10) . . ?
C1 N1 Fe1 108.93(10) . . ?
C2 N2 S1 110.70(11) . . ?
C2 N2 Fe1 116.24(10) . . ?
S1 N2 Fe1 130.62(8) . . ?
C4 N3 S2 116.08(11) . . ?
C4 N3 Fe1 114.96(10) . . ?
S2 N3 Fe1 127.95(8) . . ?
C6 N4 S3 113.15(11) . . ?
C6 N4 Fe1 117.01(10) . . ?
S3 N4 Fe1 127.26(8) . . ?
C36B N5 C35 122.5(5) . . ?
C34 N5 C35 111.1(2) . . ?
C34 N5 C36 110.2(2) . . ?
C35 N5 C36 105.34(18) . . ?
C36B N5 C34B 107.0(6) . . ?
C35 N5 C34B 95.5(5) . . ?
C36B N5 Fe2 108.3(5) . . ?
C34 N5 Fe2 113.6(2) . . ?
C35 N5 Fe2 112.98(11) . . ?
C36 N5 Fe2 103.03(15) . . ?
C34B N5 Fe2 109.1(5) . . ?
C39B N6 C38 114.7(6) . . ?
C37 N6 C38 116.33(18) . . ?
C37 N6 C39 106.8(2) . . ?
C38 N6 C39 105.16(19) . . ?
C39B N6 C37B 112.1(7) . . ?
C38 N6 C37B 89.4(4) . . ?
C39B N6 Fe2 122.2(5) . . ?
C37 N6 Fe2 105.45(13) . . ?
C38 N6 Fe2 111.98(12) . . ?
C39 N6 Fe2 111.08(17) . . ?
C37B N6 Fe2 100.3(3) . . ?
C40 N7 Fe2 149.26(14) . . ?
N1 C1 C2 109.46(13) . . ?
N2 C2 C1 107.41(13) . . ?
N1 C3 C4 109.10(14) . . ?
N3 C4 C3 106.66(14) . . ?
N1 C5 C6 110.49(14) . . ?
N4 C6 C5 108.19(14) . . ?
C8 C7 C12 120.90(16) . . ?
C8 C7 S1 117.45(13) . . ?
C12 C7 S1 121.62(14) . . ?
C9 C8 C7 118.17(17) . . ?
C9 C8 C13 116.36(18) . . ?
C7 C8 C13 125.47(17) . . ?
C10 C9 C8 122.29(19) . . ?
C9 C10 C11 118.15(18) . . ?
C9 C10 C14 120.4(2) . . ?
C11 C10 C14 121.4(2) . . ?
C10 C11 C12 123.13(18) . . ?
C11 C12 C7 117.34(18) . . ?
C11 C12 C15 117.01(17) . . ?
C7 C12 C15 125.64(17) . . ?
C21 C16 C17 120.45(16) . . ?
C21 C16 S2 117.90(13) . . ?
C17 C16 S2 121.50(14) . . ?
C18 C17 C16 117.50(17) . . ?
C18 C17 C22 116.69(16) . . ?
C16 C17 C22 125.80(16) . . ?
C19 C18 C17 123.42(17) . . ?
C18 C19 C20 117.63(17) . . ?
C18 C19 C23 122.09(17) . . ?
C20 C19 C23 120.26(18) . . ?
C19 C20 C21 122.30(17) . . ?
C20 C21 C16 118.70(16) . . ?
C20 C21 C24 117.16(16) . . ?
C16 C21 C24 124.13(16) . . ?
C30 C25 C26 120.76(16) . . ?
C30 C25 S3 122.54(13) . . ?
C26 C25 S3 116.68(13) . . ?
C27 C26 C25 117.74(17) . . ?
C27 C26 C31 117.64(17) . . ?
C25 C26 C31 124.56(16) . . ?
C28 C27 C26 122.62(18) . . ?
C29 C28 C27 117.96(17) . . ?
C29 C28 C32 121.25(19) . . ?
C27 C28 C32 120.72(19) . . ?
C28 C29 C30 122.46(18) . . ?
C29 C30 C25 117.94(17) . . ?
C29 C30 C33 116.42(16) . . ?
C25 C30 C33 125.52(16) . . ?
N5 C36 C37 111.2(2) . . ?
N5 C36B C37B 109.8(8) . . ?
N6 C37 C36 108.8(2) . . ?
C36B C37B N6 110.4(7) . . ?
N7 C40 S4 178.50(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
N3 Fe1 O1 Fe2 -59.59(9) . . . . ?
N4 Fe1 O1 Fe2 55.62(9) . . . . ?
N2 Fe1 O1 Fe2 -179.57(8) . . . . ?
O5 S2 O4 Fe2 101.98(14) . . . . ?
N3 S2 O4 Fe2 -24.80(16) . . . . ?
C16 S2 O4 Fe2 -137.01(13) . . . . ?
O7 S3 O6 Fe2 101.36(15) . . . . ?
N4 S3 O6 Fe2 -23.98(17) . . . . ?
C25 S3 O6 Fe2 -141.60(14) . . . . ?
O3 S1 N2 C2 51.33(13) . . . . ?
O2 S1 N2 C2 179.74(11) . . . . ?
C7 S1 N2 C2 -66.87(13) . . . . ?
O3 S1 N2 Fe1 -109.91(11) . . . . ?
O2 S1 N2 Fe1 18.50(13) . . . . ?
C7 S1 N2 Fe1 131.89(11) . . . . ?
O5 S2 N3 C4 60.59(14) . . . . ?
O4 S2 N3 C4 -171.29(12) . . . . ?
C16 S2 N3 C4 -56.71(14) . . . . ?
O5 S2 N3 Fe1 -107.27(11) . . . . ?
O4 S2 N3 Fe1 20.85(13) . . . . ?
C16 S2 N3 Fe1 135.43(10) . . . . ?
O7 S3 N4 C6 38.57(14) . . . . ?
O6 S3 N4 C6 167.45(11) . . . . ?
C25 S3 N4 C6 -75.94(13) . . . . ?
O7 S3 N4 Fe1 -122.50(10) . . . . ?
O6 S3 N4 Fe1 6.38(12) . . . . ?
C25 S3 N4 Fe1 122.98(10) . . . . ?
C5 N1 C1 C2 80.00(17) . . . . ?
C3 N1 C1 C2 -154.75(14) . . . . ?
Fe1 N1 C1 C2 -37.07(15) . . . . ?
S1 N2 C2 C1 158.07(12) . . . . ?
Fe1 N2 C2 C1 -37.72(17) . . . . ?
N1 C1 C2 N2 48.05(18) . . . . ?
C5 N1 C3 C4 -154.56(14) . . . . ?
C1 N1 C3 C4 81.01(16) . . . . ?
Fe1 N1 C3 C4 -37.80(15) . . . . ?
S2 N3 C4 C3 149.06(12) . . . . ?
Fe1 N3 C4 C3 -41.49(16) . . . . ?
N1 C3 C4 N3 51.52(17) . . . . ?
C3 N1 C5 C6 76.26(17) . . . . ?
C1 N1 C5 C6 -159.09(14) . . . . ?
Fe1 N1 C5 C6 -40.69(15) . . . . ?
S3 N4 C6 C5 168.49(12) . . . . ?
Fe1 N4 C6 C5 -28.36(17) . . . . ?
N1 C5 C6 N4 45.62(18) . . . . ?
O3 S1 C7 C8 175.17(13) . . . . ?
O2 S1 C7 C8 50.35(15) . . . . ?
N2 S1 C7 C8 -64.87(15) . . . . ?
O3 S1 C7 C12 -3.08(17) . . . . ?
O2 S1 C7 C12 -127.90(14) . . . . ?
N2 S1 C7 C12 116.89(15) . . . . ?
C12 C7 C8 C9 1.7(3) . . . . ?
S1 C7 C8 C9 -176.58(14) . . . . ?
C12 C7 C8 C13 -177.29(19) . . . . ?
S1 C7 C8 C13 4.5(3) . . . . ?
C7 C8 C9 C10 -0.4(3) . . . . ?
C13 C8 C9 C10 178.67(19) . . . . ?
C8 C9 C10 C11 -0.7(3) . . . . ?
C8 C9 C10 C14 -178.1(2) . . . . ?
C9 C10 C11 C12 0.6(3) . . . . ?
C14 C10 C11 C12 178.0(2) . . . . ?
C10 C11 C12 C7 0.6(3) . . . . ?
C10 C11 C12 C15 -178.12(18) . . . . ?
C8 C7 C12 C11 -1.8(3) . . . . ?
S1 C7 C12 C11 176.40(14) . . . . ?
C8 C7 C12 C15 176.86(17) . . . . ?
S1 C7 C12 C15 -5.0(3) . . . . ?
O5 S2 C16 C21 167.82(13) . . . . ?
O4 S2 C16 C21 42.51(15) . . . . ?
N3 S2 C16 C21 -71.66(15) . . . . ?
O5 S2 C16 C17 -16.53(17) . . . . ?
O4 S2 C16 C17 -141.83(14) . . . . ?
N3 S2 C16 C17 103.99(15) . . . . ?
C21 C16 C17 C18 -0.5(3) . . . . ?
S2 C16 C17 C18 -176.01(13) . . . . ?
C21 C16 C17 C22 178.44(17) . . . . ?
S2 C16 C17 C22 2.9(3) . . . . ?
C16 C17 C18 C19 1.2(3) . . . . ?
C22 C17 C18 C19 -177.85(17) . . . . ?
C17 C18 C19 C20 -1.2(3) . . . . ?
C17 C18 C19 C23 177.23(17) . . . . ?
C18 C19 C20 C21 0.5(3) . . . . ?
C23 C19 C20 C21 -177.94(16) . . . . ?
C19 C20 C21 C16 0.1(3) . . . . ?
C19 C20 C21 C24 179.06(17) . . . . ?
C17 C16 C21 C20 -0.1(3) . . . . ?
S2 C16 C21 C20 175.55(13) . . . . ?
C17 C16 C21 C24 -178.99(17) . . . . ?
S2 C16 C21 C24 -3.3(2) . . . . ?
O7 S3 C25 C30 -141.68(14) . . . . ?
O6 S3 C25 C30 93.71(15) . . . . ?
N4 S3 C25 C30 -23.45(16) . . . . ?
O7 S3 C25 C26 36.83(15) . . . . ?
O6 S3 C25 C26 -87.78(14) . . . . ?
N4 S3 C25 C26 155.06(13) . . . . ?
C30 C25 C26 C27 6.4(3) . . . . ?
S3 C25 C26 C27 -172.15(14) . . . . ?
C30 C25 C26 C31 -170.83(18) . . . . ?
S3 C25 C26 C31 10.6(2) . . . . ?
C25 C26 C27 C28 0.0(3) . . . . ?
C31 C26 C27 C28 177.41(18) . . . . ?
C26 C27 C28 C29 -4.7(3) . . . . ?
C26 C27 C28 C32 178.32(18) . . . . ?
C27 C28 C29 C30 3.1(3) . . . . ?
C32 C28 C29 C30 -179.87(17) . . . . ?
C28 C29 C30 C25 3.0(3) . . . . ?
C28 C29 C30 C33 -173.24(17) . . . . ?
C26 C25 C30 C29 -7.8(2) . . . . ?
S3 C25 C30 C29 170.64(13) . . . . ?
C26 C25 C30 C33 168.04(17) . . . . ?
S3 C25 C30 C33 -13.5(2) . . . . ?
C34 N5 C36 C37 -79.8(3) . . . . ?
C35 N5 C36 C37 160.3(2) . . . . ?
Fe2 N5 C36 C37 41.7(3) . . . . ?
C35 N5 C36B C37B 88.9(9) . . . . ?
C34B N5 C36B C37B -162.8(9) . . . . ?
Fe2 N5 C36B C37B -45.3(10) . . . . ?
C38 N6 C37 C36 -77.2(3) . . . . ?
C39 N6 C37 C36 165.8(2) . . . . ?
Fe2 N6 C37 C36 47.5(2) . . . . ?
N5 C36 C37 N6 -63.9(3) . . . . ?
N5 C36B C37B N6 63.3(11) . . . . ?
C39B N6 C37B C36B 86.3(10) . . . . ?
C38 N6 C37B C36B -157.2(8) . . . . ?
Fe2 N6 C37B C36B -44.9(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
O1 H1 O2 0.78(2) 1.86(2) 2.6110(17) 163(2) .

_refine_diff_density_max         0.425
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.060



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: DCM/Pentane'
####################################################################### 
# 
# 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_asb484
_database_code_depnum_ccdc_archive 'CCDC 1554807'
_audit_update_record             
;
2017-06-08 deposited with the CCDC.
2018-08-01 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        '[(TMEDA)Fe(II)(OTf)-(μ-OH)-Fe(III)MST]'
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C40 H62 F3 Fe2 N6 O10 S4'
_chemical_formula_weight         1083.89

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'
F F 0.0171 0.0103 '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'

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

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

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

_cell_length_a                   39.226(3)
_cell_length_b                   16.9526(13)
_cell_length_c                   18.8719(14)
_cell_angle_alpha                90
_cell_angle_beta                 110.8868(9)
_cell_angle_gamma                90
_cell_volume                     11724.9(15)
_cell_formula_units_Z            8
_cell_measurement_temperature    133(2)
_cell_measurement_reflns_used    9884
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      27.33

_exptl_crystal_description       Irregular
_exptl_crystal_colour            red
_exptl_crystal_density_meas      not_measured
_exptl_crystal_density_method    not_measured
_exptl_crystal_density_diffrn    1.228
_exptl_crystal_F_000             4536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.399
_exptl_crystal_size_mid          0.203
_exptl_crystal_size_min          0.176
_exptl_absorpt_coefficient_mu    0.696
_shelx_estimated_absorpt_T_min   0.769
_shelx_estimated_absorpt_T_max   0.887
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6709
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_process_details   'Bruker SADABS 2014/5'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      133(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            68580
_diffrn_reflns_av_unetI/netI     0.0518
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.323
_diffrn_reflns_theta_max         28.753
_diffrn_reflns_theta_full        25.500
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.935
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.935
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14240
_reflns_number_gt                9978
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2 2014.11-0, 2014'
_computing_cell_refinement       'Bruker SAINT 8.34a, 2013'
_computing_data_reduction        'Bruker SAINT 8.34a, 2013'
_computing_structure_solution    'Bruker SHELXTL 2014/4'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
A red crystal of approximate dimensions 0.176 x 0.203 x 0.399 mm was mounted 
in a cryoloop and transferred to a Bruker SMART APEX II diffractometer.  The 
APEX21 program package was used to determine the unit-cell parameters and for 
data collection (30 sec/frame scan time for a sphere of diffraction data).  
The raw frame data was processed using SAINT and SADABS to yield the reflection 
data file.  Subsequent calculations were carried out using the SHELXTL program.  
The diffraction symmetry was 2/m and the systematic absences were consistent with 
the monoclinic space groups Cc and C2/c.  It was later determined that space 
group C2/c was correct.

The structure was solved by dual space methods and refined on F2 by full-matrix 
least-squares techniques.  The analytical scattering factors for neutral atoms 
were used throughout the analysis.  Hydrogen atom H(1) was located from a 
difference-Fourier map and refined (x,y,z and riding Uiso) with d(O-H) = 0.85Å.  
The remaining hydrogen atoms were included using a riding model.

At convergence, wR2 = 0.1302 and Goof = 1.025 for 602 variables refined against 
14240 data (0.74Å), R1 = 0.0459 for those 9978 data with I > 2.0sigma(I).

There were several high residuals present in the final difference-Fourier map.  
It was not possible to determine the nature of the residuals although it was 
probable that tetrahydrofuran and/or pentane solvents were present.  The SQUEEZE 
routine in the PLATON program package was used to account for the electrons in 
the solvent accessible voids.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0651P)²+12.5095P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         14240
_refine_ls_number_parameters     602
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0761
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1302
_refine_ls_wR_factor_gt          0.1150
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_restrained_S_all      1.025
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.37095(2) 0.58729(2) 0.65567(2) 0.01747(9) Uani 1 1 d . . . . .
Fe2 Fe 0.35592(2) 0.68766(2) 0.49275(2) 0.02069(10) Uani 1 1 d . . . . .
S1 S 0.29989(2) 0.63633(4) 0.70109(4) 0.02197(14) Uani 1 1 d . . . . .
S2 S 0.36697(2) 0.48587(4) 0.50920(3) 0.01909(14) Uani 1 1 d . . . . .
S3 S 0.43330(2) 0.71106(4) 0.65469(3) 0.01845(13) Uani 1 1 d . . . . .
S4 S 0.40861(2) 0.73731(4) 0.38936(4) 0.02900(16) Uani 1 1 d . . . . .
F1 F 0.36596(6) 0.83451(11) 0.28762(11) 0.0505(5) Uani 1 1 d . . . . .
F2 F 0.36251(5) 0.71448(11) 0.25020(10) 0.0426(5) Uani 1 1 d . . . . .
F3 F 0.40949(6) 0.78396(12) 0.25763(11) 0.0547(6) Uani 1 1 d . . . . .
O1 O 0.34283(5) 0.65078(11) 0.57631(10) 0.0223(4) Uani 1 1 d D . . . .
H1 H 0.3233(5) 0.6563(18) 0.5843(18) 0.033 Uiso 1 1 d D U . . .
O2 O 0.28768(5) 0.66972(12) 0.62542(11) 0.0288(4) Uani 1 1 d . . . . .
O3 O 0.30435(5) 0.69187(11) 0.76129(11) 0.0286(4) Uani 1 1 d . . . . .
O4 O 0.37170(5) 0.56444(11) 0.48239(10) 0.0228(4) Uani 1 1 d . . . . .
O5 O 0.33215(5) 0.45076(12) 0.46910(10) 0.0278(4) Uani 1 1 d . . . . .
O6 O 0.40669(5) 0.72174(11) 0.57813(9) 0.0232(4) Uani 1 1 d . . . . .
O7 O 0.47008(5) 0.69604(11) 0.65925(10) 0.0243(4) Uani 1 1 d . . . . .
O8 O 0.37738(5) 0.71682(12) 0.40967(10) 0.0281(4) Uani 1 1 d . . . . .
O9 O 0.42834(6) 0.80608(13) 0.42677(13) 0.0398(5) Uani 1 1 d . . . . .
O10 O 0.42952(6) 0.67019(13) 0.38317(12) 0.0366(5) Uani 1 1 d . . . . .
N1 N 0.40036(5) 0.50721(13) 0.75154(11) 0.0193(4) Uani 1 1 d . . . . .
N2 N 0.33647(6) 0.58755(13) 0.71439(12) 0.0203(4) Uani 1 1 d . . . . .
N3 N 0.37629(6) 0.49182(12) 0.59817(11) 0.0189(4) Uani 1 1 d . . . . .
N4 N 0.41937(5) 0.64221(12) 0.69479(11) 0.0190(4) Uani 1 1 d . . . . .
N5 N 0.30255(6) 0.67211(14) 0.40037(13) 0.0266(5) Uani 1 1 d . . . . .
N6 N 0.33536(6) 0.81024(14) 0.49368(13) 0.0272(5) Uani 1 1 d . . . . .
C1 C 0.37503(7) 0.48538(16) 0.79106(15) 0.0231(6) Uani 1 1 d . . . . .
H1A H 0.3891 0.4684 0.8436 0.028 Uiso 1 1 calc R U . . .
H1B H 0.3593 0.4410 0.7643 0.028 Uiso 1 1 calc R U . . .
C2 C 0.35183(7) 0.55559(17) 0.79237(14) 0.0247(6) Uani 1 1 d . . . . .
H2A H 0.3319 0.5396 0.8100 0.030 Uiso 1 1 calc R U . . .
H2B H 0.3668 0.5962 0.8274 0.030 Uiso 1 1 calc R U . . .
C3 C 0.41182(7) 0.43661(16) 0.71876(14) 0.0217(5) Uani 1 1 d . . . . .
H3A H 0.4149 0.3910 0.7532 0.026 Uiso 1 1 calc R U . . .
H3B H 0.4355 0.4469 0.7129 0.026 Uiso 1 1 calc R U . . .
C4 C 0.38298(7) 0.41809(15) 0.64197(14) 0.0223(5) Uani 1 1 d . . . . .
H4A H 0.3918 0.3765 0.6158 0.027 Uiso 1 1 calc R U . . .
H4B H 0.3603 0.3995 0.6481 0.027 Uiso 1 1 calc R U . . .
C5 C 0.43186(7) 0.55242(17) 0.80186(14) 0.0245(6) Uani 1 1 d . . . . .
H5A H 0.4503 0.5154 0.8348 0.029 Uiso 1 1 calc R U . . .
H5B H 0.4237 0.5872 0.8349 0.029 Uiso 1 1 calc R U . . .
C6 C 0.44910(7) 0.60197(17) 0.75695(15) 0.0248(6) Uani 1 1 d . . . . .
H6A H 0.4657 0.6416 0.7904 0.030 Uiso 1 1 calc R U . . .
H6B H 0.4635 0.5680 0.7354 0.030 Uiso 1 1 calc R U . . .
C7 C 0.26586(7) 0.56592(18) 0.70154(16) 0.0274(6) Uani 1 1 d . . . . .
C8 C 0.24801(8) 0.5704(2) 0.75467(17) 0.0345(7) Uani 1 1 d . . . . .
C9 C 0.22051(9) 0.5150(2) 0.7472(2) 0.0488(9) Uani 1 1 d . . . . .
H9 H 0.2079 0.5178 0.7817 0.059 Uiso 1 1 calc R U . . .
C10 C 0.21058(9) 0.4566(2) 0.6927(2) 0.0499(9) Uani 1 1 d . . . . .
C11 C 0.22852(9) 0.4543(2) 0.6413(2) 0.0463(9) Uani 1 1 d . . . . .
H11 H 0.2217 0.4154 0.6025 0.056 Uiso 1 1 calc R U . . .
C12 C 0.25618(8) 0.50734(19) 0.64477(17) 0.0338(7) Uani 1 1 d . . . . .
C13 C 0.25602(9) 0.6282(2) 0.81896(18) 0.0434(8) Uani 1 1 d . . . . .
H13A H 0.2816 0.6232 0.8523 0.065 Uiso 1 1 calc R U . . .
H13B H 0.2402 0.6172 0.8479 0.065 Uiso 1 1 calc R U . . .
H13C H 0.2515 0.6819 0.7986 0.065 Uiso 1 1 calc R U . . .
C14 C 0.18069(12) 0.3976(3) 0.6878(3) 0.0751(14) Uani 1 1 d . . . . .
H14A H 0.1737 0.4030 0.7325 0.113 Uiso 1 1 calc R U . . .
H14B H 0.1897 0.3439 0.6860 0.113 Uiso 1 1 calc R U . . .
H14C H 0.1594 0.4076 0.6419 0.113 Uiso 1 1 calc R U . . .
C15 C 0.27404(9) 0.4979(2) 0.5862(2) 0.0440(8) Uani 1 1 d . . . . .
H15A H 0.2722 0.5475 0.5584 0.066 Uiso 1 1 calc R U . . .
H15B H 0.2617 0.4558 0.5506 0.066 Uiso 1 1 calc R U . . .
H15C H 0.2998 0.4841 0.6116 0.066 Uiso 1 1 calc R U . . .
C16 C 0.40157(7) 0.42419(15) 0.49741(13) 0.0197(5) Uani 1 1 d . . . . .
C17 C 0.39412(7) 0.34536(16) 0.47355(14) 0.0217(5) Uani 1 1 d . . . . .
C18 C 0.42245(8) 0.30151(16) 0.46416(14) 0.0246(6) Uani 1 1 d . . . . .
H18 H 0.4178 0.2484 0.4474 0.029 Uiso 1 1 calc R U . . .
C19 C 0.45688(7) 0.33192(16) 0.47809(15) 0.0244(6) Uani 1 1 d . . . . .
C20 C 0.46378(7) 0.40848(16) 0.50476(14) 0.0234(6) Uani 1 1 d . . . . .
H20 H 0.4876 0.4293 0.5162 0.028 Uiso 1 1 calc R U . . .
C21 C 0.43709(7) 0.45624(16) 0.51552(13) 0.0209(5) Uani 1 1 d . . . . .
C22 C 0.35838(8) 0.30276(17) 0.45712(16) 0.0285(6) Uani 1 1 d . . . . .
H22A H 0.3490 0.3131 0.4980 0.043 Uiso 1 1 calc R U . . .
H22B H 0.3622 0.2459 0.4538 0.043 Uiso 1 1 calc R U . . .
H22C H 0.3407 0.3215 0.4089 0.043 Uiso 1 1 calc R U . . .
C23 C 0.48633(8) 0.28253(18) 0.46628(18) 0.0343(7) Uani 1 1 d . . . . .
H23A H 0.4981 0.3127 0.4371 0.051 Uiso 1 1 calc R U . . .
H23B H 0.4755 0.2345 0.4385 0.051 Uiso 1 1 calc R U . . .
H23C H 0.5045 0.2683 0.5156 0.051 Uiso 1 1 calc R U . . .
C24 C 0.44817(7) 0.53726(16) 0.54786(16) 0.0257(6) Uani 1 1 d . . . . .
H24A H 0.4387 0.5767 0.5076 0.039 Uiso 1 1 calc R U . . .
H24B H 0.4748 0.5407 0.5693 0.039 Uiso 1 1 calc R U . . .
H24C H 0.4382 0.5473 0.5878 0.039 Uiso 1 1 calc R U . . .
C25 C 0.43385(7) 0.80433(15) 0.70018(14) 0.0204(5) Uani 1 1 d . . . . .
C26 C 0.45317(7) 0.86589(17) 0.68082(16) 0.0269(6) Uani 1 1 d . . . . .
C27 C 0.45398(8) 0.93898(18) 0.71383(18) 0.0339(7) Uani 1 1 d . . . . .
H27 H 0.4664 0.9809 0.6999 0.041 Uiso 1 1 calc R U . . .
C28 C 0.43736(9) 0.95402(18) 0.76680(18) 0.0363(7) Uani 1 1 d . . . . .
C29 C 0.41796(8) 0.89310(18) 0.78291(17) 0.0316(7) Uani 1 1 d . . . . .
H29 H 0.4061 0.9025 0.8181 0.038 Uiso 1 1 calc R U . . .
C30 C 0.41481(7) 0.81867(16) 0.75028(14) 0.0225(5) Uani 1 1 d . . . . .
C31 C 0.47279(8) 0.85768(18) 0.62513(17) 0.0318(7) Uani 1 1 d . . . . .
H31A H 0.4958 0.8292 0.6493 0.048 Uiso 1 1 calc R U . . .
H31B H 0.4780 0.9102 0.6097 0.048 Uiso 1 1 calc R U . . .
H31C H 0.4574 0.8284 0.5804 0.048 Uiso 1 1 calc R U . . .
C32 C 0.44064(12) 1.0334(2) 0.8045(2) 0.0599(11) Uani 1 1 d . . . . .
H32A H 0.4170 1.0484 0.8071 0.090 Uiso 1 1 calc R U . . .
H32B H 0.4482 1.0728 0.7750 0.090 Uiso 1 1 calc R U . . .
H32C H 0.4589 1.0305 0.8559 0.090 Uiso 1 1 calc R U . . .
C33 C 0.39021(8) 0.76108(17) 0.76982(17) 0.0304(6) Uani 1 1 d . . . . .
H33A H 0.3713 0.7424 0.7231 0.046 Uiso 1 1 calc R U . . .
H33B H 0.3786 0.7873 0.8017 0.046 Uiso 1 1 calc R U . . .
H33C H 0.4046 0.7162 0.7973 0.046 Uiso 1 1 calc R U . . .
C34 C 0.27546(8) 0.6312(2) 0.42431(19) 0.0416(8) Uani 1 1 d . . . . .
H34A H 0.2836 0.5770 0.4391 0.062 Uiso 1 1 calc R U . . .
H34B H 0.2519 0.6303 0.3822 0.062 Uiso 1 1 calc R U . . .
H34C H 0.2728 0.6589 0.4676 0.062 Uiso 1 1 calc R U . . .
C35 C 0.30411(9) 0.6279(2) 0.33348(19) 0.0433(8) Uani 1 1 d . . . . .
H35A H 0.3219 0.6528 0.3151 0.065 Uiso 1 1 calc R U . . .
H35B H 0.2800 0.6286 0.2931 0.065 Uiso 1 1 calc R U . . .
H35C H 0.3114 0.5733 0.3481 0.065 Uiso 1 1 calc R U . . .
C36 C 0.29079(9) 0.7538(2) 0.37404(19) 0.0443(8) Uani 1 1 d . . . . .
H36A H 0.2648 0.7537 0.3403 0.053 Uiso 1 1 calc R U . . .
H36B H 0.3055 0.7742 0.3448 0.053 Uiso 1 1 calc R U . . .
C37 C 0.29587(9) 0.8076(2) 0.4429(2) 0.0481(9) Uani 1 1 d . . . . .
H37A H 0.2874 0.8616 0.4252 0.058 Uiso 1 1 calc R U . . .
H37B H 0.2810 0.7875 0.4718 0.058 Uiso 1 1 calc R U . . .
C38 C 0.33636(10) 0.8366(2) 0.56965(19) 0.0483(9) Uani 1 1 d . . . . .
H38A H 0.3252 0.7962 0.5915 0.072 Uiso 1 1 calc R U . . .
H38B H 0.3228 0.8862 0.5644 0.072 Uiso 1 1 calc R U . . .
H38C H 0.3617 0.8448 0.6030 0.072 Uiso 1 1 calc R U . . .
C39 C 0.35499(10) 0.8698(2) 0.4677(2) 0.0483(9) Uani 1 1 d . . . . .
H39A H 0.3808 0.8696 0.5006 0.072 Uiso 1 1 calc R U . . .
H39B H 0.3445 0.9219 0.4695 0.072 Uiso 1 1 calc R U . . .
H39C H 0.3529 0.8581 0.4155 0.072 Uiso 1 1 calc R U . . .
C40 C 0.38534(9) 0.76897(19) 0.29124(18) 0.0372(7) 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
Fe1 O1 1.8548(18) . ?
Fe1 N3 2.001(2) . ?
Fe1 N4 2.005(2) . ?
Fe1 N2 2.031(2) . ?
Fe1 N1 2.227(2) . ?
Fe2 O1 1.9284(18) . ?
Fe2 O8 2.0863(19) . ?
Fe2 O6 2.1468(17) . ?
Fe2 O4 2.2072(18) . ?
Fe2 N5 2.211(2) . ?
Fe2 N6 2.231(2) . ?
S1 O3 1.437(2) . ?
S1 O2 1.4496(19) . ?
S1 N2 1.596(2) . ?
S1 C7 1.793(3) . ?
S2 O5 1.4337(19) . ?
S2 O4 1.4600(19) . ?
S2 N3 1.589(2) . ?
S2 C16 1.789(3) . ?
S3 O7 1.4374(18) . ?
S3 O6 1.4609(18) . ?
S3 N4 1.590(2) . ?
S3 C25 1.796(3) . ?
S4 O10 1.431(2) . ?
S4 O9 1.438(2) . ?
S4 O8 1.450(2) . ?
S4 C40 1.829(3) . ?
F1 C40 1.334(4) . ?
F2 C40 1.327(4) . ?
F3 C40 1.339(4) . ?
N1 C5 1.476(3) . ?
N1 C1 1.486(3) . ?
N1 C3 1.489(3) . ?
N2 C2 1.480(3) . ?
N3 C4 1.470(3) . ?
N4 C6 1.492(3) . ?
N5 C34 1.469(4) . ?
N5 C35 1.488(4) . ?
N5 C36 1.489(4) . ?
N6 C39 1.457(4) . ?
N6 C38 1.489(4) . ?
N6 C37 1.504(4) . ?
C1 C2 1.504(4) . ?
C3 C4 1.520(4) . ?
C5 C6 1.513(4) . ?
C7 C12 1.410(4) . ?
C7 C8 1.415(4) . ?
C8 C9 1.399(4) . ?
C8 C13 1.503(5) . ?
C9 C10 1.380(5) . ?
C10 C11 1.387(5) . ?
C10 C14 1.519(5) . ?
C11 C12 1.392(4) . ?
C12 C15 1.514(4) . ?
C16 C17 1.407(4) . ?
C16 C21 1.419(4) . ?
C17 C18 1.400(4) . ?
C17 C22 1.507(4) . ?
C18 C19 1.380(4) . ?
C19 C20 1.384(4) . ?
C19 C23 1.506(4) . ?
C20 C21 1.395(4) . ?
C21 C24 1.503(4) . ?
C25 C26 1.412(4) . ?
C25 C30 1.419(4) . ?
C26 C27 1.382(4) . ?
C26 C31 1.514(4) . ?
C27 C28 1.398(4) . ?
C28 C29 1.379(4) . ?
C28 C32 1.505(4) . ?
C29 C30 1.390(4) . ?
C30 C33 1.508(4) . ?
C36 C37 1.542(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Fe1 N3 100.29(8) . . ?
O1 Fe1 N4 103.91(8) . . ?
N3 Fe1 N4 107.86(8) . . ?
O1 Fe1 N2 96.85(8) . . ?
N3 Fe1 N2 121.10(9) . . ?
N4 Fe1 N2 121.72(9) . . ?
O1 Fe1 N1 175.20(8) . . ?
N3 Fe1 N1 79.83(8) . . ?
N4 Fe1 N1 80.53(8) . . ?
N2 Fe1 N1 79.10(8) . . ?
O1 Fe2 O8 171.04(8) . . ?
O1 Fe2 O6 85.40(7) . . ?
O8 Fe2 O6 89.16(7) . . ?
O1 Fe2 O4 86.01(7) . . ?
O8 Fe2 O4 87.51(7) . . ?
O6 Fe2 O4 96.13(7) . . ?
O1 Fe2 N5 98.79(8) . . ?
O8 Fe2 N5 87.60(8) . . ?
O6 Fe2 N5 171.16(8) . . ?
O4 Fe2 N5 91.94(8) . . ?
O1 Fe2 N6 95.35(8) . . ?
O8 Fe2 N6 91.67(8) . . ?
O6 Fe2 N6 89.12(8) . . ?
O4 Fe2 N6 174.68(8) . . ?
N5 Fe2 N6 82.76(9) . . ?
O3 S1 O2 115.29(12) . . ?
O3 S1 N2 111.46(12) . . ?
O2 S1 N2 108.66(11) . . ?
O3 S1 C7 108.27(12) . . ?
O2 S1 C7 106.23(12) . . ?
N2 S1 C7 106.45(13) . . ?
O5 S2 O4 114.25(11) . . ?
O5 S2 N3 113.64(11) . . ?
O4 S2 N3 107.36(11) . . ?
O5 S2 C16 108.30(12) . . ?
O4 S2 C16 107.12(11) . . ?
N3 S2 C16 105.64(11) . . ?
O7 S3 O6 115.41(11) . . ?
O7 S3 N4 110.44(11) . . ?
O6 S3 N4 108.44(11) . . ?
O7 S3 C25 106.65(11) . . ?
O6 S3 C25 104.26(11) . . ?
N4 S3 C25 111.50(11) . . ?
O10 S4 O9 117.45(13) . . ?
O10 S4 O8 113.18(13) . . ?
O9 S4 O8 114.95(13) . . ?
O10 S4 C40 104.14(14) . . ?
O9 S4 C40 104.25(14) . . ?
O8 S4 C40 100.03(13) . . ?
Fe1 O1 Fe2 126.40(9) . . ?
S2 O4 Fe2 139.33(11) . . ?
S3 O6 Fe2 148.58(12) . . ?
S4 O8 Fe2 149.39(12) . . ?
C5 N1 C1 111.2(2) . . ?
C5 N1 C3 112.2(2) . . ?
C1 N1 C3 111.3(2) . . ?
C5 N1 Fe1 106.18(15) . . ?
C1 N1 Fe1 108.31(15) . . ?
C3 N1 Fe1 107.35(14) . . ?
C2 N2 S1 111.75(16) . . ?
C2 N2 Fe1 115.30(15) . . ?
S1 N2 Fe1 130.64(12) . . ?
C4 N3 S2 117.90(17) . . ?
C4 N3 Fe1 114.53(15) . . ?
S2 N3 Fe1 126.54(12) . . ?
C6 N4 S3 113.91(17) . . ?
C6 N4 Fe1 116.70(16) . . ?
S3 N4 Fe1 127.35(12) . . ?
C34 N5 C35 106.0(2) . . ?
C34 N5 C36 111.7(2) . . ?
C35 N5 C36 106.7(2) . . ?
C34 N5 Fe2 113.54(18) . . ?
C35 N5 Fe2 114.54(17) . . ?
C36 N5 Fe2 104.23(18) . . ?
C39 N6 C38 106.2(3) . . ?
C39 N6 C37 110.7(3) . . ?
C38 N6 C37 106.8(2) . . ?
C39 N6 Fe2 114.04(18) . . ?
C38 N6 Fe2 113.7(2) . . ?
C37 N6 Fe2 105.12(19) . . ?
N1 C1 C2 109.1(2) . . ?
N2 C2 C1 107.9(2) . . ?
N1 C3 C4 109.3(2) . . ?
N3 C4 C3 106.5(2) . . ?
N1 C5 C6 111.5(2) . . ?
N4 C6 C5 108.3(2) . . ?
C12 C7 C8 120.6(3) . . ?
C12 C7 S1 117.7(2) . . ?
C8 C7 S1 121.7(2) . . ?
C9 C8 C7 116.8(3) . . ?
C9 C8 C13 116.8(3) . . ?
C7 C8 C13 126.4(3) . . ?
C10 C9 C8 124.0(3) . . ?
C9 C10 C11 117.5(3) . . ?
C9 C10 C14 121.6(3) . . ?
C11 C10 C14 120.9(4) . . ?
C10 C11 C12 122.1(3) . . ?
C11 C12 C7 119.0(3) . . ?
C11 C12 C15 116.9(3) . . ?
C7 C12 C15 124.1(3) . . ?
C17 C16 C21 121.0(2) . . ?
C17 C16 S2 120.97(19) . . ?
C21 C16 S2 118.01(19) . . ?
C18 C17 C16 117.5(2) . . ?
C18 C17 C22 116.2(2) . . ?
C16 C17 C22 126.3(2) . . ?
C19 C18 C17 123.0(3) . . ?
C18 C19 C20 118.1(2) . . ?
C18 C19 C23 120.9(3) . . ?
C20 C19 C23 120.9(3) . . ?
C19 C20 C21 122.5(2) . . ?
C20 C21 C16 117.8(2) . . ?
C20 C21 C24 117.8(2) . . ?
C16 C21 C24 124.4(2) . . ?
C26 C25 C30 120.3(2) . . ?
C26 C25 S3 116.31(19) . . ?
C30 C25 S3 123.3(2) . . ?
C27 C26 C25 118.3(3) . . ?
C27 C26 C31 117.4(3) . . ?
C25 C26 C31 124.3(3) . . ?
C26 C27 C28 123.0(3) . . ?
C29 C28 C27 117.1(3) . . ?
C29 C28 C32 121.7(3) . . ?
C27 C28 C32 121.2(3) . . ?
C28 C29 C30 123.4(3) . . ?
C29 C30 C25 117.7(3) . . ?
C29 C30 C33 116.3(2) . . ?
C25 C30 C33 125.9(2) . . ?
N5 C36 C37 109.7(3) . . ?
N6 C37 C36 110.4(3) . . ?
F2 C40 F1 107.2(3) . . ?
F2 C40 F3 107.5(3) . . ?
F1 C40 F3 107.7(3) . . ?
F2 C40 S4 112.1(2) . . ?
F1 C40 S4 111.5(2) . . ?
F3 C40 S4 110.7(2) . . ?

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
O1 H1 O2 0.838(10) 1.838(12) 2.659(2) 166(3) .

_refine_diff_density_max         1.047
_refine_diff_density_min         -0.569
_refine_diff_density_rms         0.081



_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: THF/Pentane'
