#------------------------------------------------------------------------------
#$Date: 2019-11-10 07:37:43 +0200 (Sun, 10 Nov 2019) $
#$Revision: 225882 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/51/57/4515757.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4515757
loop_
_publ_author_name
'Brazzolotto, Deborah'
'Wang, Lianke'
'Tang, Hao'
'Gennari, Marcello'
'Queyriaux, Nicolas'
'Philouze, Christian'
'Demeshko, Serhiy'
'Meyer, Franc'
'Orio, Maylis'
'Artero, Vincent'
'Hall, Michael B.'
'Duboc, Carole'
_publ_section_title
;
 Tuning Reactivity of Bioinspired [NiFe]-Hydrogenase Models by Ligand
 Design and Modeling the CO Inhibition Process
;
_journal_issue                   11
_journal_name_full               'ACS Catalysis'
_journal_page_first              10658
_journal_paper_doi               10.1021/acscatal.8b02830
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety
'C49 H45 Fe N2 Ni O S2, 0.69(C H2 Cl2), 2(B0.5 F2), 0.15(C4 H10 O), 0.15(H2 O)'
_chemical_formula_sum            'C50.31 H48.22 B Cl1.39 F4 Fe N2 Ni O1.31 S2'
_chemical_formula_weight         1016.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-06-23
_audit_creation_method
;
Olex2 1.2
(compiled 2014.07.22 svn.r2960 for OlexSys, GUI svn.r4862)
;
_cell_angle_alpha                90
_cell_angle_beta                 127.48(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.286(5)
_cell_length_b                   23.295(5)
_cell_length_c                   20.693(4)
_cell_measurement_reflns_used    63311
_cell_measurement_temperature    200
_cell_measurement_theta_max      27.537
_cell_measurement_theta_min      2.210
_cell_volume                     9673(5)
_computing_cell_refinement       EvalCCD
_computing_data_collection       Collect
_computing_data_reduction        EvalCCD
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      200
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'APEX II'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Bruker-AXS-enraf-nonius KappaAPEXII'
_diffrn_measurement_method       'Phi and omega scans'
_diffrn_radiation_collimation    'Montel optic'
_diffrn_radiation_detector       CCD
_diffrn_radiation_monochromator  'Multilayer mirrors'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            63311
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.537
_diffrn_reflns_theta_min         2.210
_diffrn_source                   'Incoatec ISG250'
_diffrn_source_target            Mo
_diffrn_source_type              'Microfocus sealed tube'
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.711926
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.0603 before and 0.0366 after correction.
The Ratio of minimum to maximum transmission is 0.7119.
The λ/2 correction factor is 0.0015.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_description       needle
_exptl_crystal_F_000             4201
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.44
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.941
_refine_diff_density_min         -0.606
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.241
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         11046
_refine_ls_number_restraints     622
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.0868
_refine_ls_R_factor_gt           0.0666
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+84.9581P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1507
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9024
_reflns_number_total             11046
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            cs8b02830_si_001.cif
_cod_data_source_block           NiFeCpSTAR
_cod_database_code               4515757
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 C54-C53
 1.5 with sigma of 0.02
 C54-O2
 1.5 with sigma of 0.02
 O2-C55
 1.5 with sigma of 0.02
 C55-C56
 1.5 with sigma of 0.02
 C53-O2
 2.5 with sigma of 0.02
 C54-C55
 2.5 with sigma of 0.02
 O2-C56
 2.5 with sigma of 0.02
3. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1.7A with sigma of 0.04 and sigma
for terminal atoms of 0.08
Uanis(C53) = Uanis(C56) = Uanis(O3)
Uanis(C54) = Uanis(C55)
5. Others
 Sof(C53)=Sof(H53A)=Sof(H53B)=Sof(H53C)=Sof(O2)=Sof(C54)=Sof(H54A)=Sof(H54B)=
 Sof(C55)=Sof(H55A)=Sof(H55B)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=Sof(O3)=
 Sof(H3A)=Sof(H3B)=0.5*(1-FVAR(2))
 Sof(Cl1)=Sof(Cl2)=Sof(C52)=Sof(H52A)=Sof(H52B)=FVAR(1)
6.a Riding coordinates:
 O3(H3A,H3B)
6.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B), C52(H52A,H52B), C54(H54A,H54B), C55(H55A,H55B)
6.c Aromatic/amide H refined with riding coordinates:
 C34(H34), C3(H3), C35(H35), C15(H15), C2(H2), C32(H32), C19(H19), C28(H28),
 C30(H30), C7(H7), C4(H4), C36(H36), C21(H21), C29(H29), C8(H8), C37(H37),
 C23(H23), C18(H18), C16(H16), C38(H38), C22(H22), C25(H25), C9(H9), C17(H17),
 C31(H31), C24(H24)
6.d Idealised Me refined with riding coordinates:
 C53(H53A,H53B,H53C)
6.e Idealised Me refined as rotating group:
 C50(H50A,H50B,H50C), C51(H51A,H51B,H51C), C47(H47A,H47B,H47C), C49(H49A,H49B,
 H49C), C48(H48A,H48B,H48C), C56(H56A,H56B,H56C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
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'
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
Ni1 Ni 0.69159(3) 0.70442(2) 0.63567(3) 0.02734(13) Uani 1 1 d . U . . .
Fe1 Fe 0.56886(3) 0.64973(3) 0.63872(4) 0.03147(16) Uani 1 1 d . U . . .
S2 S 0.68099(5) 0.63957(5) 0.70230(6) 0.0285(2) Uani 1 1 d . U . . .
S1 S 0.60148(6) 0.73532(5) 0.61452(7) 0.0314(2) Uani 1 1 d . U . . .
N1 N 0.69779(18) 0.75922(16) 0.5722(2) 0.0298(7) Uani 1 1 d . U . . .
N2 N 0.78204(18) 0.68563(18) 0.6787(2) 0.0331(8) Uani 1 1 d . U . . .
C5 C 0.7617(2) 0.7704(2) 0.6023(3) 0.0323(9) Uani 1 1 d . U . . .
C13 C 0.5527(2) 0.7813(2) 0.5197(3) 0.0331(9) Uani 1 1 d . U . . .
C1 C 0.6475(2) 0.7870(2) 0.5059(3) 0.0332(9) Uani 1 1 d . U . . .
O1 O 0.50401(19) 0.57956(19) 0.4931(2) 0.0537(10) Uani 1 1 d . U . . .
C34 C 0.6514(2) 0.5957(2) 0.5362(3) 0.0311(9) Uani 1 1 d . U . . .
H34 H 0.6292 0.6263 0.5411 0.037 Uiso 1 1 calc R . . . .
Cl1 Cl 0.8567(2) 0.43033(19) 0.5135(3) 0.1203(17) Uani 0.695(6) 1 d . U . A 1
C27 C 0.7076(2) 0.5237(2) 0.7217(3) 0.0332(9) Uani 1 1 d . U . . .
C12 C 0.7960(2) 0.5933(2) 0.7489(3) 0.0385(10) Uani 1 1 d . U . . .
H12A H 0.8069 0.6023 0.8026 0.046 Uiso 1 1 calc R . . . .
H12B H 0.8218 0.5586 0.7563 0.046 Uiso 1 1 calc R . . . .
C14 C 0.4776(2) 0.7677(2) 0.4678(3) 0.0353(10) Uani 1 1 d . U . . .
C50 C 0.6356(3) 0.5803(3) 0.8095(3) 0.0499(14) Uani 1 1 d . U . . .
H50A H 0.6320 0.5418 0.7880 0.075 Uiso 1 1 calc GR . . . .
H50B H 0.6315 0.5777 0.8536 0.075 Uiso 1 1 calc GR . . . .
H50C H 0.6789 0.5969 0.8305 0.075 Uiso 1 1 calc GR . . . .
C26 C 0.7217(2) 0.5774(2) 0.6909(2) 0.0292(9) Uani 1 1 d . U . . .
C3 C 0.7253(3) 0.8443(2) 0.5040(3) 0.0467(12) Uani 1 1 d . U . . .
H3 H 0.7345 0.8747 0.4815 0.056 Uiso 1 1 calc R . . . .
C44 C 0.5815(3) 0.6172(2) 0.7434(3) 0.0409(11) Uani 1 1 d . U . . .
C10 C 0.8216(2) 0.6422(2) 0.7271(3) 0.0385(11) Uani 1 1 d . U . . .
C35 C 0.6331(3) 0.5817(2) 0.4592(3) 0.0413(11) Uani 1 1 d . U . . .
H35 H 0.5979 0.6019 0.4124 0.050 Uiso 1 1 calc R . . . .
C15 C 0.4513(3) 0.7197(2) 0.4184(3) 0.0436(11) Uani 1 1 d . U . . .
H15 H 0.4805 0.6933 0.4193 0.052 Uiso 1 1 calc R . . . .
C2 C 0.6599(3) 0.8307(2) 0.4707(3) 0.0409(11) Uani 1 1 d . U . . .
H2 H 0.6240 0.8509 0.4244 0.049 Uiso 1 1 calc R . . . .
C6 C 0.8101(2) 0.7295(2) 0.6645(3) 0.0355(10) Uani 1 1 d . U . . .
C33 C 0.7008(2) 0.5660(2) 0.6051(3) 0.0308(9) Uani 1 1 d . U . . .
C32 C 0.7522(3) 0.5040(2) 0.8019(3) 0.0429(12) Uani 1 1 d . U . . .
H32 H 0.7929 0.5239 0.8391 0.051 Uiso 1 1 calc R . . . .
C20 C 0.5658(2) 0.8451(2) 0.5451(3) 0.0404(11) Uani 1 1 d . U . . .
C11 C 0.5780(2) 0.7675(2) 0.4695(3) 0.0351(10) Uani 1 1 d . U . . .
H11A H 0.5757 0.7254 0.4614 0.042 Uiso 1 1 calc R . . . .
H11B H 0.5472 0.7853 0.4151 0.042 Uiso 1 1 calc R . . . .
C19 C 0.4332(3) 0.8055(2) 0.4650(3) 0.0457(12) Uani 1 1 d . U . . .
H19 H 0.4498 0.8391 0.4978 0.055 Uiso 1 1 calc R . . . .
C28 C 0.6482(2) 0.4937(2) 0.6694(3) 0.0372(10) Uani 1 1 d . U . . .
H28 H 0.6172 0.5060 0.6146 0.045 Uiso 1 1 calc R . . . .
C45 C 0.5810(3) 0.6785(2) 0.7443(3) 0.0453(12) Uani 1 1 d . U . . .
C30 C 0.6789(3) 0.4267(2) 0.7758(3) 0.0488(13) Uani 1 1 d . U . . .
H30 H 0.6691 0.3937 0.7939 0.059 Uiso 1 1 calc R . . . .
C7 C 0.8774(2) 0.7318(3) 0.7009(3) 0.0483(13) Uani 1 1 d . U . . .
H7 H 0.8958 0.7635 0.6918 0.058 Uiso 1 1 calc R . . . .
C42 C 0.4806(3) 0.6479(3) 0.6277(3) 0.0500(13) Uani 1 1 d . U . . .
C4 C 0.7765(3) 0.8141(2) 0.5691(3) 0.0404(11) Uani 1 1 d . U . . .
H4 H 0.8214 0.8225 0.5916 0.048 Uiso 1 1 calc R . . . .
C36 C 0.6658(3) 0.5394(3) 0.4512(3) 0.0489(13) Uani 1 1 d . U . . .
H36 H 0.6541 0.5305 0.3992 0.059 Uiso 1 1 calc R . . . .
C41 C 0.5174(3) 0.6974(3) 0.6734(4) 0.0512(13) Uani 1 1 d . U . . .
C46 C 0.5321(2) 0.6093(2) 0.5490(3) 0.0360(10) Uani 1 1 d . U . . .
C51 C 0.6359(4) 0.7161(3) 0.8097(4) 0.0619(17) Uani 1 1 d . U . . .
H51A H 0.6789 0.6974 0.8339 0.093 Uiso 1 1 calc GR . . . .
H51B H 0.6300 0.7224 0.8518 0.093 Uiso 1 1 calc GR . . . .
H51C H 0.6347 0.7530 0.7861 0.093 Uiso 1 1 calc GR . . . .
C21 C 0.5471(3) 0.8859(2) 0.4847(4) 0.0503(13) Uani 1 1 d . U . . .
H21 H 0.5300 0.8733 0.4316 0.060 Uiso 1 1 calc R . . . .
C47 C 0.4932(4) 0.7577(3) 0.6543(5) 0.075(2) Uani 1 1 d . U . . .
H47A H 0.5300 0.7833 0.6695 0.113 Uiso 1 1 calc GR . . . .
H47B H 0.4767 0.7682 0.6850 0.113 Uiso 1 1 calc GR . . . .
H47C H 0.4571 0.7613 0.5959 0.113 Uiso 1 1 calc GR . . . .
C29 C 0.6338(3) 0.4463(2) 0.6962(3) 0.0440(12) Uani 1 1 d . U . . .
H29 H 0.5926 0.4269 0.6599 0.053 Uiso 1 1 calc R . . . .
C8 C 0.9170(3) 0.6874(3) 0.7503(3) 0.0598(17) Uani 1 1 d . U . . .
H8 H 0.9635 0.6882 0.7765 0.072 Uiso 1 1 calc R . . . .
C49 C 0.4966(3) 0.5368(3) 0.6494(4) 0.0577(15) Uani 1 1 d . U . . .
H49A H 0.4653 0.5332 0.5900 0.087 Uiso 1 1 calc GR . . . .
H49B H 0.4743 0.5259 0.6731 0.087 Uiso 1 1 calc GR . . . .
H49C H 0.5349 0.5116 0.6705 0.087 Uiso 1 1 calc GR . . . .
C43 C 0.5201(3) 0.5979(2) 0.6717(3) 0.0446(11) Uani 1 1 d . U . . .
C37 C 0.7156(3) 0.5098(3) 0.5187(4) 0.0590(15) Uani 1 1 d . U . . .
H37 H 0.7385 0.4802 0.5133 0.071 Uiso 1 1 calc R . . . .
C23 C 0.5774(3) 0.9632(3) 0.5771(5) 0.072(2) Uani 1 1 d . U . . .
H23 H 0.5804 1.0032 0.5877 0.087 Uiso 1 1 calc R . . . .
C18 C 0.3651(3) 0.7946(3) 0.4149(4) 0.0554(14) Uani 1 1 d . U . . .
H18 H 0.3359 0.8200 0.4153 0.066 Uiso 1 1 calc R . . . .
C16 C 0.3829(3) 0.7092(3) 0.3671(4) 0.0535(14) Uani 1 1 d . U . . .
H16 H 0.3660 0.6760 0.3336 0.064 Uiso 1 1 calc R . . . .
C38 C 0.7332(3) 0.5225(3) 0.5955(3) 0.0483(13) Uani 1 1 d . U . . .
H38 H 0.7675 0.5012 0.6417 0.058 Uiso 1 1 calc R . . . .
C22 C 0.5531(3) 0.9439(3) 0.5012(5) 0.0640(17) Uani 1 1 d . U . . .
H22 H 0.5402 0.9707 0.4594 0.077 Uiso 1 1 calc R . . . .
C25 C 0.5914(3) 0.8652(3) 0.6218(4) 0.0578(15) Uani 1 1 d . U . . .
H25 H 0.6050 0.8386 0.6642 0.069 Uiso 1 1 calc R . . . .
C9 C 0.8893(2) 0.6418(3) 0.7620(3) 0.0559(15) Uani 1 1 d . U . . .
H9 H 0.9162 0.6099 0.7938 0.067 Uiso 1 1 calc R . . . .
C17 C 0.3395(3) 0.7471(3) 0.3648(4) 0.0563(15) Uani 1 1 d . U . . .
H17 H 0.2928 0.7405 0.3292 0.068 Uiso 1 1 calc R . . . .
C31 C 0.7376(3) 0.4557(3) 0.8276(3) 0.0520(14) Uani 1 1 d . U . . .
H31 H 0.7689 0.4426 0.8819 0.062 Uiso 1 1 calc R . . . .
C48 C 0.4103(3) 0.6480(4) 0.5510(4) 0.073(2) Uani 1 1 d . U . . .
H48A H 0.4020 0.6834 0.5206 0.110 Uiso 1 1 calc GR . . . .
H48B H 0.3795 0.6457 0.5648 0.110 Uiso 1 1 calc GR . . . .
H48C H 0.4035 0.6148 0.5175 0.110 Uiso 1 1 calc GR . . . .
C24 C 0.5975(3) 0.9244(3) 0.6379(5) 0.0734(19) Uani 1 1 d . U . . .
H24 H 0.6156 0.9375 0.6911 0.088 Uiso 1 1 calc R . . . .
F1 F 0.5286(2) 0.68673(19) 0.3180(2) 0.0755(12) Uani 1 1 d . U . . .
B1 B 0.5000 0.6529(4) 0.2500 0.0401(17) Uani 1 2 d S TU P . .
F2 F 0.4522(3) 0.6214(3) 0.2415(3) 0.131(2) Uani 1 1 d . U . . .
F4 F 1.0364(3) 0.5876(2) 0.8172(3) 0.1071(17) Uani 1 1 d . U . . .
F3 F 0.9600(4) 0.5201(3) 0.7583(4) 0.147(3) Uani 1 1 d . U . . .
B2 B 1.0000 0.5536(6) 0.7500 0.084(4) Uani 1 2 d S TU P . .
Cl2 Cl 0.8715(6) 0.3802(3) 0.6481(6) 0.276(5) Uani 0.695(6) 1 d . U . A 1
C52 C 0.9030(11) 0.4206(9) 0.6097(11) 0.155(7) Uani 0.695(6) 1 d . U . A 1
H52A H 0.9150 0.4587 0.6362 0.186 Uiso 0.695(6) 1 calc R . . A 1
H52B H 0.9449 0.4023 0.6261 0.186 Uiso 0.695(6) 1 calc R . . A 1
C53 C 0.825(2) 0.394(2) 0.581(5) 0.164(16) Uani 0.153(3) 1 d D U . A -2
H53A H 0.7917 0.3892 0.5215 0.246 Uiso 0.153(3) 1 calc R . . A -2
H53B H 0.8670 0.3768 0.5989 0.246 Uiso 0.153(3) 1 calc R . . A -2
H53C H 0.8309 0.4347 0.5945 0.246 Uiso 0.153(3) 1 calc R . . A -2
O2 O 0.758(3) 0.3118(17) 0.577(4) 0.192(19) Uani 0.153(3) 1 d D U . A -2
C54 C 0.799(5) 0.364(3) 0.623(4) 0.196(18) Uani 0.153(3) 1 d D U . A -2
H54A H 0.8381 0.3520 0.6781 0.235 Uiso 0.153(3) 1 calc R . . A -2
H54B H 0.7724 0.3909 0.6282 0.235 Uiso 0.153(3) 1 calc R . . A -2
C55 C 0.767(5) 0.2928(18) 0.514(4) 0.196(18) Uani 0.153(3) 1 d D U . A -2
H55A H 0.8137 0.2995 0.5357 0.235 Uiso 0.153(3) 1 calc R . . A -2
H55B H 0.7380 0.3165 0.4646 0.235 Uiso 0.153(3) 1 calc R . . A -2
C56 C 0.750(2) 0.2304(13) 0.4916(15) 0.164(16) Uani 0.153(3) 1 d D U . A -2
H56A H 0.7727 0.2163 0.4696 0.246 Uiso 0.153(3) 1 calc GR . . A -2
H56B H 0.7018 0.2262 0.4504 0.246 Uiso 0.153(3) 1 calc GR . . A -2
H56C H 0.7648 0.2082 0.5401 0.246 Uiso 0.153(3) 1 calc GR . . A -2
O3 O 0.7339(18) 0.1370(16) 0.360(4) 0.164(16) Uani 0.153(3) 1 d . U . A -3
H3A H 0.7708 0.1192 0.3893 0.246 Uiso 0.153(3) 1 d R . . A -3
H3B H 0.7273 0.1494 0.3173 0.246 Uiso 0.153(3) 1 d R . . A -3
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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'
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
S1 Ni1 S2 80.69(5) . .
N1 Ni1 S2 177.10(12) . .
N1 Ni1 S1 98.96(12) . .
N1 Ni1 N2 84.20(16) . .
N2 Ni1 S2 96.80(12) . .
N2 Ni1 S1 166.64(12) . .
S2 Fe1 S1 74.69(4) . .
C44 Fe1 S2 90.64(15) . .
C44 Fe1 S1 132.17(16) . .
C44 Fe1 C41 65.7(2) . .
C45 Fe1 S2 95.05(17) . .
C45 Fe1 S1 95.90(15) . .
C45 Fe1 C44 39.3(2) . .
C45 Fe1 C41 39.4(2) . .
C42 Fe1 S2 156.71(15) . .
C42 Fe1 S1 119.10(18) . .
C42 Fe1 C44 66.1(2) . .
C42 Fe1 C45 66.2(2) . .
C42 Fe1 C41 39.1(2) . .
C42 Fe1 C43 40.0(2) . .
C41 Fe1 S2 130.65(19) . .
C41 Fe1 S1 89.72(16) . .
C46 Fe1 S2 103.00(15) . .
C46 Fe1 S1 105.11(16) . .
C46 Fe1 C44 122.6(2) . .
C46 Fe1 C45 155.2(2) . .
C46 Fe1 C42 91.7(2) . .
C46 Fe1 C41 126.3(2) . .
C46 Fe1 C43 89.8(2) . .
C43 Fe1 S2 120.99(16) . .
C43 Fe1 S1 155.81(16) . .
C43 Fe1 C44 39.1(2) . .
C43 Fe1 C45 66.1(2) . .
C43 Fe1 C41 66.1(2) . .
Ni1 S2 Fe1 98.68(5) . .
C26 S2 Ni1 99.72(14) . .
C26 S2 Fe1 126.02(14) . .
Ni1 S1 Fe1 97.99(5) . .
C13 S1 Ni1 109.86(14) . .
C13 S1 Fe1 128.07(16) . .
C5 N1 Ni1 112.8(3) . .
C1 N1 Ni1 127.2(3) . .
C1 N1 C5 120.0(4) . .
C10 N2 Ni1 130.5(3) . .
C10 N2 C6 118.1(4) . .
C6 N2 Ni1 110.7(3) . .
N1 C5 C6 113.8(4) . .
N1 C5 C4 120.9(5) . .
C4 C5 C6 125.1(4) . .
C14 C13 S1 110.8(3) . .
C14 C13 C20 110.7(4) . .
C14 C13 C11 109.0(4) . .
C20 C13 S1 108.8(3) . .
C20 C13 C11 109.8(4) . .
C11 C13 S1 107.7(3) . .
N1 C1 C2 120.8(4) . .
N1 C1 C11 117.4(4) . .
C2 C1 C11 121.8(4) . .
C35 C34 H34 119.3 . .
C33 C34 H34 119.3 . .
C33 C34 C35 121.5(5) . .
C32 C27 C26 122.3(4) . .
C28 C27 C26 119.8(4) . .
C28 C27 C32 117.9(4) . .
H12A C12 H12B 107.0 . .
C26 C12 H12A 107.4 . .
C26 C12 H12B 107.4 . .
C10 C12 H12A 107.4 . .
C10 C12 H12B 107.4 . .
C10 C12 C26 119.5(4) . .
C15 C14 C13 121.0(4) . .
C15 C14 C19 117.8(5) . .
C19 C14 C13 121.1(5) . .
H50A C50 H50B 109.5 . .
H50A C50 H50C 109.5 . .
H50B C50 H50C 109.5 . .
C44 C50 H50A 109.5 . .
C44 C50 H50B 109.5 . .
C44 C50 H50C 109.5 . .
C27 C26 S2 107.0(3) . .
C12 C26 S2 102.6(3) . .
C12 C26 C27 110.7(4) . .
C33 C26 S2 116.7(3) . .
C33 C26 C27 109.6(4) . .
C33 C26 C12 109.9(4) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C4 C3 C2 120.0(5) . .
C50 C44 Fe1 129.0(3) . .
C45 C44 Fe1 70.2(3) . .
C45 C44 C50 125.3(5) . .
C43 C44 Fe1 69.9(3) . .
C43 C44 C50 126.1(5) . .
C43 C44 C45 108.5(5) . .
N2 C10 C12 122.0(4) . .
N2 C10 C9 120.9(5) . .
C9 C10 C12 117.1(5) . .
C34 C35 H35 119.9 . .
C36 C35 C34 120.2(5) . .
C36 C35 H35 119.9 . .
C14 C15 H15 119.4 . .
C14 C15 C16 121.2(5) . .
C16 C15 H15 119.4 . .
C1 C2 H2 120.4 . .
C3 C2 C1 119.1(5) . .
C3 C2 H2 120.4 . .
N2 C6 C5 114.1(4) . .
N2 C6 C7 122.6(5) . .
C7 C6 C5 123.1(5) . .
C34 C33 C26 124.4(4) . .
C34 C33 C38 117.4(4) . .
C38 C33 C26 118.1(4) . .
C27 C32 H32 119.7 . .
C31 C32 C27 120.7(5) . .
C31 C32 H32 119.7 . .
C21 C20 C13 117.5(5) . .
C25 C20 C13 124.8(5) . .
C25 C20 C21 117.6(5) . .
C13 C11 H11A 108.3 . .
C13 C11 H11B 108.3 . .
C1 C11 C13 115.8(4) . .
C1 C11 H11A 108.3 . .
C1 C11 H11B 108.3 . .
H11A C11 H11B 107.4 . .
C14 C19 H19 119.5 . .
C18 C19 C14 120.9(6) . .
C18 C19 H19 119.5 . .
C27 C28 H28 119.6 . .
C29 C28 C27 120.9(4) . .
C29 C28 H28 119.6 . .
C44 C45 Fe1 70.5(3) . .
C44 C45 C41 107.8(5) . .
C44 C45 C51 125.8(6) . .
C41 C45 Fe1 70.9(3) . .
C41 C45 C51 126.3(6) . .
C51 C45 Fe1 126.1(4) . .
C29 C30 H30 120.7 . .
C31 C30 H30 120.7 . .
C31 C30 C29 118.7(5) . .
C6 C7 H7 120.8 . .
C8 C7 C6 118.4(5) . .
C8 C7 H7 120.8 . .
C41 C42 Fe1 71.9(3) . .
C41 C42 C43 108.3(5) . .
C41 C42 C48 125.3(6) . .
C43 C42 Fe1 70.5(3) . .
C43 C42 C48 126.1(6) . .
C48 C42 Fe1 127.8(4) . .
C5 C4 H4 120.5 . .
C3 C4 C5 118.9(5) . .
C3 C4 H4 120.5 . .
C35 C36 H36 120.3 . .
C35 C36 C37 119.5(5) . .
C37 C36 H36 120.3 . .
C45 C41 Fe1 69.7(3) . .
C45 C41 C47 125.7(6) . .
C42 C41 Fe1 69.0(3) . .
C42 C41 C45 107.7(5) . .
C42 C41 C47 126.4(6) . .
C47 C41 Fe1 129.6(4) . .
O1 C46 Fe1 171.9(4) . .
C45 C51 H51A 109.5 . .
C45 C51 H51B 109.5 . .
C45 C51 H51C 109.5 . .
H51A C51 H51B 109.5 . .
H51A C51 H51C 109.5 . .
H51B C51 H51C 109.5 . .
C20 C21 H21 119.5 . .
C22 C21 C20 121.1(6) . .
C22 C21 H21 119.5 . .
C41 C47 H47A 109.5 . .
C41 C47 H47B 109.5 . .
C41 C47 H47C 109.5 . .
H47A C47 H47B 109.5 . .
H47A C47 H47C 109.5 . .
H47B C47 H47C 109.5 . .
C28 C29 C30 120.8(5) . .
C28 C29 H29 119.6 . .
C30 C29 H29 119.6 . .
C7 C8 H8 120.1 . .
C7 C8 C9 119.9(5) . .
C9 C8 H8 120.1 . .
H49A C49 H49B 109.5 . .
H49A C49 H49C 109.5 . .
H49B C49 H49C 109.5 . .
C43 C49 H49A 109.5 . .
C43 C49 H49B 109.5 . .
C43 C49 H49C 109.5 . .
C44 C43 Fe1 71.0(3) . .
C44 C43 C42 107.6(5) . .
C44 C43 C49 126.7(5) . .
C42 C43 Fe1 69.6(3) . .
C42 C43 C49 125.4(5) . .
C49 C43 Fe1 129.8(4) . .
C36 C37 H37 119.6 . .
C36 C37 C38 120.7(5) . .
C38 C37 H37 119.6 . .
C22 C23 H23 120.2 . .
C22 C23 C24 119.6(6) . .
C24 C23 H23 120.2 . .
C19 C18 H18 119.7 . .
C17 C18 C19 120.6(6) . .
C17 C18 H18 119.7 . .
C15 C16 H16 119.9 . .
C17 C16 C15 120.3(6) . .
C17 C16 H16 119.9 . .
C33 C38 C37 120.6(5) . .
C33 C38 H38 119.7 . .
C37 C38 H38 119.7 . .
C21 C22 H22 119.7 . .
C23 C22 C21 120.7(7) . .
C23 C22 H22 119.7 . .
C20 C25 H25 119.6 . .
C20 C25 C24 120.8(7) . .
C24 C25 H25 119.6 . .
C10 C9 H9 120.0 . .
C8 C9 C10 120.0(6) . .
C8 C9 H9 120.0 . .
C18 C17 C16 119.1(5) . .
C18 C17 H17 120.5 . .
C16 C17 H17 120.5 . .
C32 C31 H31 119.5 . .
C30 C31 C32 121.1(5) . .
C30 C31 H31 119.5 . .
C42 C48 H48A 109.5 . .
C42 C48 H48B 109.5 . .
C42 C48 H48C 109.5 . .
H48A C48 H48B 109.5 . .
H48A C48 H48C 109.5 . .
H48B C48 H48C 109.5 . .
C23 C24 C25 120.2(7) . .
C23 C24 H24 119.9 . .
C25 C24 H24 119.9 . .
F1 B1 F1 109.9(7) 2_655 .
F2 B1 F1 108.8(3) 2_655 2_655
F2 B1 F1 108.2(3) . 2_655
F2 B1 F1 108.2(3) 2_655 .
F2 B1 F1 108.8(3) . .
F2 B1 F2 113.0(9) . 2_655
F4 B2 F4 108.8(10) 2_756 .
F4 B2 F3 107.2(4) . .
F4 B2 F3 111.6(4) . 2_756
F4 B2 F3 107.2(4) 2_756 2_756
F4 B2 F3 111.6(4) 2_756 .
F3 B2 F3 110.3(11) . 2_756
Cl1 C52 Cl2 117.5(13) . .
Cl1 C52 H52A 107.9 . .
Cl1 C52 H52B 107.9 . .
Cl2 C52 H52A 107.9 . .
Cl2 C52 H52B 107.9 . .
H52A C52 H52B 107.2 . .
H53A C53 H53B 109.5 . .
H53A C53 H53C 109.5 . .
H53B C53 H53C 109.5 . .
C54 C53 H53A 109.5 . .
C54 C53 H53B 109.5 . .
C54 C53 H53C 109.5 . .
C54 O2 C55 112.0(19) . .
C53 C54 H54A 109.1 . .
C53 C54 H54B 109.1 . .
O2 C54 C53 112.3(19) . .
O2 C54 H54A 109.1 . .
O2 C54 H54B 109.1 . .
H54A C54 H54B 107.9 . .
O2 C55 H55A 109.0 . .
O2 C55 H55B 109.0 . .
O2 C55 C56 113(2) . .
H55A C55 H55B 107.8 . .
C56 C55 H55A 109.0 . .
C56 C55 H55B 109.0 . .
C55 C56 H56A 109.5 . .
C55 C56 H56B 109.5 . .
C55 C56 H56C 109.5 . .
H56A C56 H56B 109.5 . .
H56A C56 H56C 109.5 . .
H56B C56 H56C 109.5 . .
H3A O3 H3B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 S2 2.1691(12) .
Ni1 S1 2.1652(13) .
Ni1 N1 1.905(4) .
Ni1 N2 1.933(4) .
Fe1 S2 2.2994(15) .
Fe1 S1 2.3257(14) .
Fe1 C44 2.127(5) .
Fe1 C45 2.123(5) .
Fe1 C42 2.101(5) .
Fe1 C41 2.139(5) .
Fe1 C46 1.760(5) .
Fe1 C43 2.113(5) .
S2 C26 1.873(5) .
S1 C13 1.891(5) .
N1 C5 1.358(5) .
N1 C1 1.341(6) .
N2 C10 1.345(6) .
N2 C6 1.374(6) .
C5 C6 1.465(7) .
C5 C4 1.399(6) .
C13 C14 1.543(7) .
C13 C20 1.544(7) .
C13 C11 1.548(6) .
C1 C2 1.395(6) .
C1 C11 1.500(6) .
O1 C46 1.150(6) .
C34 H34 0.9500 .
C34 C35 1.402(6) .
C34 C33 1.379(6) .
Cl1 C52 1.597(17) .
C27 C26 1.541(6) .
C27 C32 1.400(6) .
C27 C28 1.390(7) .
C12 H12A 0.9900 .
C12 H12B 0.9900 .
C12 C26 1.539(6) .
C12 C10 1.508(7) .
C14 C15 1.383(7) .
C14 C19 1.400(7) .
C50 H50A 0.9800 .
C50 H50B 0.9800 .
C50 H50C 0.9800 .
C50 C44 1.484(7) .
C26 C33 1.537(6) .
C3 H3 0.9500 .
C3 C2 1.388(7) .
C3 C4 1.367(8) .
C44 C45 1.430(7) .
C44 C43 1.418(8) .
C10 C9 1.394(7) .
C35 H35 0.9500 .
C35 C36 1.358(8) .
C15 H15 0.9500 .
C15 C16 1.395(7) .
C2 H2 0.9500 .
C6 C7 1.381(6) .
C33 C38 1.390(7) .
C32 H32 0.9500 .
C32 C31 1.385(7) .
C20 C21 1.404(7) .
C20 C25 1.380(8) .
C11 H11A 0.9900 .
C11 H11B 0.9900 .
C19 H19 0.9500 .
C19 C18 1.390(8) .
C28 H28 0.9500 .
C28 C29 1.381(7) .
C45 C41 1.436(8) .
C45 C51 1.495(8) .
C30 H30 0.9500 .
C30 C29 1.392(7) .
C30 C31 1.370(8) .
C7 H7 0.9500 .
C7 C8 1.368(9) .
C42 C41 1.420(9) .
C42 C43 1.441(8) .
C42 C48 1.499(8) .
C4 H4 0.9500 .
C36 H36 0.9500 .
C36 C37 1.369(9) .
C41 C47 1.486(8) .
C51 H51A 0.9800 .
C51 H51B 0.9800 .
C51 H51C 0.9800 .
C21 H21 0.9500 .
C21 C22 1.378(8) .
C47 H47A 0.9800 .
C47 H47B 0.9800 .
C47 H47C 0.9800 .
C29 H29 0.9500 .
C8 H8 0.9500 .
C8 C9 1.373(8) .
C49 H49A 0.9800 .
C49 H49B 0.9800 .
C49 H49C 0.9800 .
C49 C43 1.502(8) .
C37 H37 0.9500 .
C37 C38 1.398(8) .
C23 H23 0.9500 .
C23 C22 1.369(10) .
C23 C24 1.371(11) .
C18 H18 0.9500 .
C18 C17 1.379(9) .
C16 H16 0.9500 .
C16 C17 1.386(9) .
C38 H38 0.9500 .
C22 H22 0.9500 .
C25 H25 0.9500 .
C25 C24 1.405(9) .
C9 H9 0.9500 .
C17 H17 0.9500 .
C31 H31 0.9500 .
C48 H48A 0.9800 .
C48 H48B 0.9800 .
C48 H48C 0.9800 .
C24 H24 0.9500 .
F1 B1 1.373(6) .
B1 F1 1.373(6) 2_655
B1 F2 1.330(6) .
B1 F2 1.330(6) 2_655
F4 B2 1.360(9) .
F3 B2 1.368(9) .
B2 F4 1.360(9) 2_756
B2 F3 1.368(9) 2_756
Cl2 C52 1.710(19) .
C52 H52A 0.9900 .
C52 H52B 0.9900 .
C53 H53A 0.9800 .
C53 H53B 0.9800 .
C53 H53C 0.9800 .
C53 C54 1.52(2) .
O2 C54 1.50(2) .
O2 C55 1.50(2) .
C54 H54A 0.9900 .
C54 H54B 0.9900 .
C55 H55A 0.9900 .
C55 H55B 0.9900 .
C55 C56 1.51(2) .
C56 H56A 0.9800 .
C56 H56B 0.9800 .
C56 H56C 0.9800 .
O3 H3A 0.8493 .
O3 H3B 0.8510 .
