Dithiolato-bridged nickel-iron complexes as models for the active site of [NiFe]-hydrogenases.
Song, Li-Cheng; Yang, Xi-Yue; Cao, Meng; Gao, Xiu-Yun; Liu, Bei-Bei; Zhu, Liang; Jiang, Feng; Chemical communications (Cambridge, England) 53 (2017) 3818–3821; doi:10.1039/c7cc00149e

data_7119751
_publ_section_title
;
 Dithiolato-bridged nickel-iron complexes as models for the active site of
 [NiFe]-hydrogenases.
;
_journal_issue                   27
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3818
_journal_page_last               3821
_journal_paper_doi               10.1039/c7cc00149e
_journal_volume                  53
_journal_year                    2017
_chemical_formula_moiety
'2(C62 H58 Fe N Ni O2 P4 S2), 2(B F4), 5(C3 H6 O), 0.5(H2 O)'
_chemical_formula_sum            'C139 H147 B2 F8 Fe2 N2 Ni2 O9.5 P8 S4'
_chemical_formula_weight         2776.33
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2016-06-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-07-14 deposited with the CCDC.
2017-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                72.238(6)
_cell_angle_beta                 88.640(6)
_cell_angle_gamma                81.428(6)
_cell_formula_units_Z            1
_cell_length_a                   12.8843(12)
_cell_length_b                   16.7478(12)
_cell_length_c                   17.1899(13)
_cell_measurement_reflns_used    10983
_cell_measurement_temperature    113
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     3492.1(5)
_computing_cell_refinement
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_collection
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_data_reduction
;
CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113
_diffrn_detector                 PILT
_diffrn_detector_area_resol_mean 5.8140
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_details
;
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 0.0000
                 XTD: 44.9575
              2theta: -15.0892
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 90.0000
                 XTD: 44.9575
              2theta: -15.0892
scan:
    Number of images: 360
               Slice: -105.0000 - 75.0000
         Image width: 0.5000
            Exp time: 5.0000
       Rotation axis: Omega
               Omega: 0.0000
                 Chi: 45.0000
                 Phi: 180.0000
                 XTD: 44.9575
              2theta: -15.0892
;
_diffrn_measurement_device
;
AFC10: Fixed Chi 2 circle
;
_diffrn_measurement_device_type
;
Rigaku Pilatus 200K
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support Fiber
_diffrn_orient_matrix_type       d*Trek
_diffrn_orient_matrix_UB_11      -0.033763
_diffrn_orient_matrix_UB_12      0.027790
_diffrn_orient_matrix_UB_13      0.065206
_diffrn_orient_matrix_UB_21      0.055366
_diffrn_orient_matrix_UB_22      -0.018131
_diffrn_orient_matrix_UB_23      0.025024
_diffrn_orient_matrix_UB_31      0.006334
_diffrn_orient_matrix_UB_32      0.057544
_diffrn_orient_matrix_UB_33      -0.019546
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0224
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            45162
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         3.13
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.687
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    "'not measured'"
_exptl_crystal_description       Prism
_exptl_crystal_F_000             1445
_exptl_crystal_preparation       Fiber
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.420
_refine_diff_density_min         -0.665
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     861
_refine_ls_number_reflns         15809
_refine_ls_number_restraints     269
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0432
_refine_ls_R_factor_gt           0.0378
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+2.8016P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1130
_refine_ls_wR_factor_ref         0.1164
_reflns_number_gt                13965
_reflns_number_total             15809
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7cc00149e2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas 

 Adding full bibliography for 7119749--7119751.cif.
;
_cod_original_formula_sum        'C139 H147 B2 F8 Fe2 N2 Ni2 O9.50 P8 S4'
_cod_database_code               7119751
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 B1-F1 = B1-F2 = B1-F3 = B1-F4 = B1-F1' = B1-F2' = B1-F3' = B1-F4'
 1.35 with sigma of 0.01
 O5-C70
 1.24 with sigma of 0.01
 C69-C70 = C70-C71
 1.54 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim F3 \\sim F4 \\sim F1' \\sim F2' \\sim F3' \\sim F4': within
1.7A with sigma of 0.01 and sigma for terminal atoms of 0.02
C69 \\sim C70 \\sim C71 \\sim C5: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
O3 \\sim C63 \\sim C64 \\sim C65 \\sim O4 \\sim C66 \\sim C67 \\sim C68 \\sim
O5 \\sim C69 \\sim C70 \\sim C71: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
C70 \\sim O5 \\sim C69 \\sim C71: within 3.8A with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(F1) \\sim Ueq, Uanis(F2) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F4) \\sim
Ueq, Uanis(F1') \\sim Ueq, Uanis(F2') \\sim Ueq, Uanis(F3') \\sim Ueq,
Uanis(F4') \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(C63) \\sim Ueq, Uanis(C64) \\sim Ueq, Uanis(C65)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C67) \\sim Ueq,
Uanis(C68) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C70)
\\sim Ueq, Uanis(C71) \\sim Ueq: with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(F1) \\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.005
Uanis(C69) \\sim Ueq, Uanis(C70) \\sim Ueq, Uanis(C71) \\sim Ueq, Uanis(O5)
\\sim Ueq, Uanis(O6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
4. Others
 Sof(F1')=Sof(F2')=Sof(F3')=Sof(F4')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
 Fixed Sof: O5(0.5) C69(0.5) H69A(0.5) H69B(0.5) H69C(0.5) C70(0.5) C71(0.5)
 H71A(0.5) H71B(0.5) H71C(0.5) O6(0.25) H6A(0.25) H6B(0.25)
5.a Riding coordinates:
 O2(H2), C69(H69A,H69B,H69C), C71(H71A,H71B,H71C), O6(H6A,H6B)
5.b Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C43(H43A,H43B), C44(H44A,H44B)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10), C11(H11), C12(H12),
 C13(H13), C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21),
  C23(H23), C24(H24), C25(H25), C26(H26), C27(H27), C32(H32), C33(H33),
 C34(H34), C35(H35), C36(H36), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42),
  C46(H46), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53),
 C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C61(H61), C62(H62)
5.d Idealised Me refined as rotating group:
 C63(H63A,H63B,H63C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C68(H68A,H68B,
 H68C)
;
_olex2_submission_special_instructions 'No special instructions were received'