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_4134744
_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         'C38.88 H51.65 Ni P2 S Si'
_chemical_formula_sum            'C38.88 H51.66 Ni P2 S Si'
_chemical_formula_weight         699.88
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-07-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   19.6982(13)
_cell_length_b                   18.6978(13)
_cell_length_c                   20.3197(14)
_cell_measurement_reflns_used    9735
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      39.962
_cell_measurement_theta_min      2.256
_cell_volume                     7484.0(9)
_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      100.03
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_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  0.0610
_diffrn_reflns_av_unetI/netI     0.0311
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            215724
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         38.568
_diffrn_reflns_theta_min         2.256
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.7480
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0723 before and 0.0580 after correction. The Ratio of minimum to maximum transmission is 0.9376. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             2984
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         1.673
_refine_diff_density_min         -0.622
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         21177
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0355
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+3.0311P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0793
_refine_ls_wR_factor_ref         0.0866
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16514
_reflns_number_total             21177
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00712_si_002.cif
_cod_data_source_block           compound2
_cod_depositor_comments
'Adding full bibliography for 4134744--4134749.cif.'
_cod_database_code               4134744
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.792
_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(C14)=Sof(H14A)=Sof(H14B)=Sof(H14C)=Sof(C15)=Sof(H15A)=Sof(H15B)=Sof(H15C)=
 FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C22(H22), C37(H37), C25(H25), C13(H13), C34(H34)
3.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C20(H20), C32(H32), C17(H17), C29(H29), C18(H18), C19(H19), C1(H1),
 C9(H9), C5(H5), C8(H8), C31(H31), C2(H2), C30(H30), C4(H4), C3(H3)
3.c Idealised Me refined as rotating group:
 C23(H23A,H23B,H23C), C26(H26A,H26B,H26C), C24(H24A,H24B,H24C), C27(H27A,H27B,
 H27C), C39(H39A,H39B,H39C), C36(H36A,H36B,H36C), C35(H35A,H35B,H35C), C38(H38A,
 H38B,H38C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              99163
_shelx_hkl_checksum              58219
_olex2_submission_special_instructions 'No special instructions were received'