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_4134746
_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 H44 N Ni P2 S Si, C4 H8 O'
_chemical_formula_sum            'C40 H52 N Ni O P2 S Si'
_chemical_formula_weight         743.62
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-18
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 108.276(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5609(17)
_cell_length_b                   19.0517(10)
_cell_length_c                   24.6555(18)
_cell_measurement_reflns_used    9888
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      40.35
_cell_measurement_theta_min      2.31
_cell_volume                     7386.7(10)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_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  0.0665
_diffrn_reflns_av_unetI/netI     0.0461
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_number            157479
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         41.038
_diffrn_reflns_theta_min         2.695
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.734
_exptl_absorpt_correction_T_max  0.9847
_exptl_absorpt_correction_T_min  0.9459
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0773 before and 0.0680 after correction. The Ratio of minimum to maximum transmission is 0.9606. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.337
_exptl_crystal_description       block
_exptl_crystal_F_000             3160
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.803
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     432
_refine_ls_number_reflns         23737
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0630
_refine_ls_R_factor_gt           0.0441
_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^)+(0.0336P)^2^+6.4277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0901
_refine_ls_wR_factor_ref         0.0972
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18893
_reflns_number_total             23737
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00712_si_002.cif
_cod_data_source_block           compound4'
_cod_depositor_comments
'Adding full bibliography for 4134744--4134749.cif.'
_cod_database_code               4134746
_shelx_shelxl_version_number     2014/7
_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.a Ternary CH refined with riding coordinates:
 C19(H19), C34(H34), C22(H22), C31(H31)
2.b Secondary CH2 refined with riding coordinates:
 C38(H38A,H38B), C39(H39A,H39B), C37(H37A,H37B), C40(H40A,H40B)
2.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C10(H10), C9(H9), C27(H27), C8(H8), C1(H1), C26(H26), C5(H5),
 C17(H17), C29(H29), C4(H4), C3(H3), C28(H28), C15(H15), C16(H16), C14(H14)
2.d Idealised Me refined as rotating group:
 C24(H24A,H24B,H24C), C33(H33A,H33B,H33C), C32(H32A,H32B,H32C), C23(H23A,H23B,
 H23C), C36(H36A,H36B,H36C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C35(H35A,
 H35B,H35C)
;
_shelx_res_checksum              26521
_shelx_hkl_checksum              16381
_olex2_submission_special_instructions 'No special instructions were received'