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_7241154
_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         'C41 H38 Fe N Ni O P2 S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C42 H40 B Cl2 F4 Fe N Ni O P2 S2'
_chemical_formula_weight         973.08
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-21
_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                 108.615(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.8793(11)
_cell_length_b                   11.0429(5)
_cell_length_c                   22.4895(10)
_cell_measurement_reflns_used    16134
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      32.4530
_cell_measurement_theta_min      1.8940
_cell_volume                     4208.0(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00   0.00  180
  2  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00  90.00  180
  3  \w   -115.00  65.00   1.00    2.00    --  -25.00  45.00 180.00  180
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0010090000
_diffrn_orient_matrix_UB_12      0.0082774000
_diffrn_orient_matrix_UB_13      -0.0309917000
_diffrn_orient_matrix_UB_21      0.0418749000
_diffrn_orient_matrix_UB_22      -0.0017844000
_diffrn_orient_matrix_UB_23      0.0112380000
_diffrn_orient_matrix_UB_31      -0.0010485000
_diffrn_orient_matrix_UB_32      -0.0636498000
_diffrn_orient_matrix_UB_33      -0.0043563000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0859
_diffrn_reflns_av_unetI/netI     0.0565
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            43090
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.905
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50793
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1992
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.000
_refine_diff_density_min         -1.039
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     528
_refine_ls_number_reflns         8586
_refine_ls_number_restraints     74
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0924
_refine_ls_R_factor_gt           0.0712
_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/[\s^2^(Fo^2^)+(0.0945P)^2^+12.9566P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1847
_refine_ls_wR_factor_ref         0.1987
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6564
_reflns_number_total             8586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04344c2.cif
_cod_data_source_block           7
_cod_depositor_comments
'Adding full bibliography for 7241152--7241154.cif.'
_cod_database_code               7241154
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C11 H10 N O'
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.934
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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
 F4A-B1 = F1-B1 = F3A-B1 = F3-B1 = F4-B1 = F2-B1
 1.35 with sigma of 0.005
 F2A-B1 = F1A-B1
 1.35 with sigma of 0.005
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F2-F3 \\sim F2-F4 \\sim F3-F4 \\sim
F1A-F2A \\sim F1A-F3A \\sim F1A-F4A ~
 F2A-F3A \\sim F2A-F4A \\sim F3A-F4A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(F3) = Uanis(F3A)
Uanis(F4) = Uanis(F4A)
Uanis(F2A) = Uanis(F2)
Uanis(F1A) = Uanis(F1)
4. Others
 Sof(F4A)=Sof(F3A)=Sof(F2A)=Sof(F1A)=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(F4)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C34(H34A,H34B), C42(H42A,H42B)
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), C28(H28), C29(H29),
 C30(H30), C31(H31), C32(H32), C36(H36), C37(H37), C39(H39), C40(H40)
5.c Idealised Me refined as rotating group:
 C41(H41A,H41B,H41C)
;
_shelx_res_checksum              4234
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.804
_oxdiff_exptl_absorpt_empirical_full_min 0.635