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_4134749
_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         'C36.87 H46.6 N0.26 Ni P2 S Si'
_chemical_formula_sum            'C36.87 H46.6 N0.26 Ni P2 S Si'
_chemical_formula_weight         674.26
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2019-06-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.473(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5356(8)
_cell_length_b                   17.6421(11)
_cell_length_c                   15.1447(16)
_cell_measurement_reflns_used    9958
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      80.30
_cell_measurement_theta_min      4.52
_cell_volume                     3348.2(5)
_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      100.02
_diffrn_detector                 'CMOS Area Detector'
_diffrn_detector_type            'Bruker PHOTON 100 CMOS'
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0524
_diffrn_reflns_av_unetI/netI     0.0312
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            44584
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.882
_diffrn_reflns_theta_min         3.847
_diffrn_source_current           1
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatech I\mS HB'
_diffrn_source_voltage           50
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.849
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0845 before and 0.0598 after correction.
The Ratio of minimum to maximum transmission is 0.8645.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       plate
_exptl_crystal_F_000             1431
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     407
_refine_ls_number_reflns         6960
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0352
_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^)+(0.0511P)^2^+1.4259P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0924
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5828
_reflns_number_total             6960
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00712_si_002.cif
_cod_data_source_block           compound9
_cod_depositor_comments
'Adding full bibliography for 4134744--4134749.cif.'
_cod_original_formula_sum        'C36.87 H46.60 N0.26 Ni P2 S Si'
_cod_database_code               4134749
_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(N2)=Sof(N1)=1-FVAR(1)
 Sof(C0AA)=Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=FVAR(1)
3.a Ternary CH refined with riding coordinates:
 C17(H17), C14(H14), C29(H29), C26(H26)
3.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C4(H4), C3(H3), C9(H9), C5(H5), C32(H32), C33(H33), C35(H35),
 C34(H34), C10(H10), C22(H22), C21(H21), C8(H8), C20(H20), C23(H23), C2(H2)
3.c Idealised Me refined as rotating group:
 C0AA(H0AA,H0AB,H0AC), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C30(H30A,H30B,
 H30C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C16(H16A,H16B,H16C), C18(H18A,
 H18B,H18C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              36156
_shelx_hkl_checksum              9792
_olex2_submission_special_instructions 'No special instructions were received'