Dithiolato- and halogenido-bridged nickel-iron complexes related to the active site of [NiFe]-H2ases: preparation, structures, and electrocatalytic H2 production
Song, Li-Cheng; Han, Xiao-Feng; Chen, Wei; Li, Jia-Peng; Wang, Xu-Yong; Dalton Trans.  (2017) –; doi:10.1039/C7DT02203D

data_7043637
_publ_section_title
;
 Dithiolato- and halogenido-bridged nickel-iron complexes related to the
 active site of [NiFe]-H2ases: preparation, structures, and
 electrocatalytic H2 production
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02203D
_journal_year                    2017
_chemical_formula_moiety         '0.5(C58 H55 Cl Fe N Ni O3 P4 S2), B F4'
_chemical_formula_sum            'C58 H55 B Cl F4 Fe N Ni O3 P4 S2'
_chemical_formula_weight         1238.85
_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
_audit_creation_date             2017-04-26
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5335)
;
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-07-14 downloaded from the CCDC.
;
_cell_angle_alpha                102.90(3)
_cell_angle_beta                 105.00(3)
_cell_angle_gamma                106.05(3)
_cell_formula_units_Z            4
_cell_length_a                   13.580(3)
_cell_length_b                   22.475(5)
_cell_length_c                   25.330(5)
_cell_measurement_reflns_used    19719
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8824
_cell_measurement_theta_min      1.6606
_cell_volume                     6805(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL-1997 (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'rigaku saturn 70 CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            48967
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        25.020
_diffrn_reflns_theta_max         25.020
_diffrn_reflns_theta_min         1.661
_exptl_absorpt_coefficient_mu    0.733
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   CrystalClear
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       Prism
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.917
_exptl_transmission_factor_min   0.867
_refine_diff_density_max         1.560
_refine_diff_density_min         -0.842
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1371
_refine_ls_number_reflns         23588
_refine_ls_number_restraints     135
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0517
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0758P)^2^+1.0038P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1462
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17352
_reflns_number_total             23588
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02203d2.cif
_cod_data_source_block           r130617b1_sq
_cod_original_cell_volume        6805(3)
_cod_database_code               7043637
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.867
_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
2. Restrained distances
 C57-C58
 1.54 with sigma of 0.01
3. Rigid bond restraints
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C58) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C57) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C35) \\sim Ueq, Uanis(C42) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F7)
\\sim Ueq, Uanis(F6) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
5.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C55(H55A,H55B), C57(H57A,H57B)
5.b 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),
  C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C50(H50), C51(H51),
 C52(H52), C53(H53), C54(H54)
5.c Idealised Me refined as rotating group:
 C58(H58A,H58B,H58C)
;
_shelx_res_checksum              49322
_shelx_fab_checksum              91440
_olex2_submission_special_instructions 'No special instructions were received'