H<sub>2</sub> Evolution from a Thiolate-Bound Ni(III) Hydride.
Gu, Nina X.; Oyala, Paul H.; Peters, Jonas C.; Journal of the American Chemical Society 142 (2020) 7827–7835; doi:10.1021/jacs.0c00712

data_4134745
_publ_section_title
;
 H<sub>2</sub> Evolution from a Thiolate-Bound Ni(III) Hydride.
;
_journal_issue                   17
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7827
_journal_page_last               7835
_journal_paper_doi               10.1021/jacs.0c00712
_journal_volume                  142
_journal_year                    2020
_chemical_formula_moiety         'C36 H45 K Ni P2 S Si'
_chemical_formula_sum            'C36 H45 K Ni P2 S Si'
_chemical_formula_weight         697.62
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-21
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 96.3290(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5790(4)
_cell_length_b                   26.7073(9)
_cell_length_c                   13.4850(5)
_cell_measurement_reflns_used    9337
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      35.07
_cell_measurement_theta_min      2.47
_cell_volume                     3786.8(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 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    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       41
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            172135
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.140
_diffrn_reflns_theta_min         2.448
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.816
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6842
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0979 before and 0.0491 after correction. The Ratio of minimum to maximum transmission is 0.9159. The \l/2 correction factor is Not present.'
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       block
_exptl_crystal_F_000             1472
_exptl_crystal_size_max          0.268
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.128
_refine_diff_density_max         1.063
_refine_diff_density_min         -1.111
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         14419
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0429
_refine_ls_R_factor_gt           0.0319
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0329P)^2^+1.9729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0782
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11997
_reflns_number_total             14419
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00712_si_002.cif
_cod_data_source_block           compound3
_cod_depositor_comments
'Adding full bibliography for 4134744--4134749.cif.'
_cod_database_code               4134745
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(C24)=Sof(H24A)=Sof(H24B)=Sof(H24C)=Sof(C23)=Sof(H23)=Sof(C22)=Sof(H22A)=
 Sof(H22B)=Sof(H22C)=1-FVAR(1)
 Sof(C26)=Sof(H26)=Sof(C25)=Sof(H25A)=Sof(H25B)=Sof(H25C)=Sof(C27)=Sof(H27A)=
 Sof(H27B)=Sof(H27C)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C35(H35), C20(H20), C38(H38), C26(H26), C23(H23)
3.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C17(H17), C10(H10), C8(H8), C9(H9), C15(H15), C32(H32), C31(H31),
 C1(H1), C5(H5), C2(H2), C29(H29), C30(H30), C4(H4), C3(H3), C16(H16)
3.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C36(H36A,H36B,
 H36C), C19(H19A,H19B,H19C), C34(H34A,H34B,H34C), C25(H25A,H25B,H25C), C27(H27A,
 H27B,H27C), C24(H24A,H24B,H24C), C22(H22A,H22B,H22C)
;
_shelx_res_checksum              61387
_shelx_hkl_checksum              85231
_shelx_fab_checksum              95860
_olex2_submission_special_instructions 'No special instructions were received'