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_7241153
_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         'C42 H40 Fe N Ni O3 P2 S2, C H2 Cl2, B F4'
_chemical_formula_sum            'C43 H42 B Cl2 F4 Fe N Ni O3 P2 S2'
_chemical_formula_weight         1019.10
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2020-04-23
_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                75.55(3)
_cell_angle_beta                 87.96(3)
_cell_angle_gamma                77.76(3)
_cell_formula_units_Z            2
_cell_length_a                   10.113(2)
_cell_length_b                   12.365(3)
_cell_length_c                   18.383(4)
_cell_measurement_reflns_used    5822
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8944
_cell_measurement_theta_min      1.1440
_cell_volume                     2175.1(9)
_computing_cell_refinement       crystalclear
_computing_data_collection       crystalclear
_computing_data_reduction        crystalclear
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      113.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_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  0.0487
_diffrn_reflns_av_unetI/netI     0.0608
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            26271
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.834
_diffrn_reflns_theta_min         1.144
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8395
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       block
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.255
_refine_diff_density_rms         0.107
_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     648
_refine_ls_number_reflns         10291
_refine_ls_number_restraints     223
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0784P)^2^+1.7397P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7872
_reflns_number_total             10291
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ra04344c2.cif
_cod_data_source_block           8
_cod_depositor_comments
'Adding full bibliography for 7241152--7241154.cif.'
_cod_original_cell_volume        2175.1(8)
_cod_database_code               7241153
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.807
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Restrained distances
 N1-C35A \\sim N1-C35
 with sigma of 0.02
 O2-C35A \\sim O2A-C35
 with sigma of 0.02
 O3A-C35 \\sim O3-C35A
 with sigma of 0.02
 O3-C36 \\sim O3A-C36A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C38A) \\sim Ueq, Uanis(C39A) \\sim Ueq, Uanis(C40A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 N1, C35A, O2, O3, C36, C37, C38, C39, C40, C41, C42
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N1, C35, O2A, O3A, C36A, C37A, C42A, C41A, C39A, C38A, C40A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 B1, F2, F3, F1, F4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 F4, B1, F1', F2', F3'
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5. Others
 Sof(C35)=Sof(F1')=Sof(F2')=Sof(F3')=1-FVAR(1)
 Sof(F1)=Sof(F2)=Sof(F3)=Sof(C35A)=FVAR(1)
 Sof(O2A)=Sof(O3A)=Sof(C36A)=Sof(H36C)=Sof(H36D)=Sof(C37A)=Sof(C42A)=Sof(H42A)=
 Sof(C41A)=Sof(H41A)=Sof(C40A)=Sof(H40A)=Sof(C39A)=Sof(H39A)=Sof(C38A)=
 Sof(H38A)=1-FVAR(2)
 Sof(O2)=Sof(O3)=Sof(C36)=Sof(H36A)=Sof(H36B)=Sof(C37)=Sof(C38)=Sof(H38)=
 Sof(C39)=Sof(H39)=Sof(C40)=Sof(H40)=Sof(C41)=Sof(H41)=Sof(C42)=Sof(H42)=FVAR(2)
6.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C15(H15A,H15B), C33(H33A,H33B), C34(H34A,H34B), C36(H36A,
 H36B), C43(H43A,H43B), C36A(H36C,H36D)
6.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), 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), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42), C42A(H42A),
 C41A(H41A), C40A(H40A), C39A(H39A), C38A(H38A)
6.c Fitted hexagon refined as free rotating group:
 C37A(C42A,C41A,C40A,C39A,C38A)
;
_shelx_res_checksum              33652
_olex2_submission_special_instructions 'No special instructions were received'