Heterodinuclear nickel(ii)‒iron(ii) azadithiolates as structural and functional models for the active site of [NiFe]-hydrogenases
Song, Li-Cheng; Liu, Bei-Bei; Liu, Wen-Bo; Tan, Zheng-Lei; RSC Advances 10 (2020) 32069–32077; doi:10.1039/D0RA04344C

data_7241152
_publ_section_title
;
 Heterodinuclear nickel(ii)--iron(ii) azadithiolates as structural and
 functional models for the active site of [NiFe]-hydrogenases
;
_journal_issue                   53
_journal_name_full               'RSC Advances'
_journal_page_first              32069
_journal_page_last               32077
_journal_paper_doi               10.1039/D0RA04344C
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety         'C40 H35 Cl Fe N Ni O P2 S2, B F4'
_chemical_formula_sum            'C40 H35 B Cl F4 Fe N Ni O P2 S2'
_chemical_formula_weight         908.57
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-08-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.15(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.861(4)
_cell_length_b                   11.063(2)
_cell_length_c                   22.252(5)
_cell_measurement_reflns_used    9242
_cell_measurement_temperature    113.1500
_cell_measurement_theta_max      27.8704
_cell_measurement_theta_min      1.9262
_cell_volume                     4178.1(17)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113.1500
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1038
_diffrn_reflns_av_unetI/netI     0.0749
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            49278
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.863
_diffrn_reflns_theta_min         2.078
_exptl_absorpt_coefficient_mu    1.088
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             1856
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.127
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9958
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.127
_refine_ls_R_factor_all          0.0866
_refine_ls_R_factor_gt           0.0693
_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^)+(0.0700P)^2^+0.9964P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1538
_refine_ls_wR_factor_ref         0.1648
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8228
_reflns_number_total             9958
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04344c2.cif
_cod_data_source_block           6
_cod_depositor_comments
'Adding full bibliography for 7241152--7241154.cif.'
_cod_original_cell_volume        4178.2(16)
_cod_database_code               7241152
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.948
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C28(H28A,H28B), C27(H27A,H27B)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C20(H20), C10(H10), C12(H12), C33(H33), C22(H22), C13(H13),
 C11(H11), C8(H8), C2(H2), C30(H30), C37(H37), C34(H34), C31(H31), C38(H38),
 C16(H16), C9(H9), C3(H3), C26(H26), C19(H19), C6(H6), C18(H18), C36(H36),
 C17(H17), C4(H4), C23(H23), C25(H25), C24(H24), C5(H5), C35(H35), C39(H39)
;
_shelx_res_checksum              77022
_shelx_fab_checksum              70012
_olex2_submission_special_instructions 'No special instructions were received'