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_4134748
_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         'C41 H57 Li Ni O P2 S Si'
_chemical_formula_sum            'C41 H57 Li Ni O P2 S Si'
_chemical_formula_weight         753.60
_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   geom
_atom_sites_solution_primary     dual
_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                 103.426(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.6307(6)
_cell_length_b                   24.5754(12)
_cell_length_c                   17.3135(7)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      36.26
_cell_measurement_theta_min      2.448
_cell_volume                     4813.5(4)
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.02
_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  0.0816
_diffrn_reflns_av_unetI/netI     0.0557
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            124005
_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         30.508
_diffrn_reflns_theta_min         2.419
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.563
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.7067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0919 before and 0.0568 after correction. The Ratio of minimum to maximum transmission is 0.9472. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.040
_exptl_crystal_description       needle
_exptl_crystal_F_000             1608
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.007
_refine_diff_density_min         -0.772
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         14687
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0927
_refine_ls_R_factor_gt           0.0665
_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^)+(0.0725P)^2^+2.6734P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1457
_refine_ls_wR_factor_ref         0.1564
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10477
_reflns_number_total             14687
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c00712_si_002.cif
_cod_data_source_block           compound8
_cod_depositor_comments
'Adding full bibliography for 4134744--4134749.cif.'
_cod_database_code               4134748
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.962
_shelx_estimated_absorpt_t_min   0.790
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 C40
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
C40: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C39: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
4. Others
 Sof(C37)=Sof(H37A)=Sof(H37B)=Sof(H37C)=Sof(O1)=Sof(C38)=Sof(H38A)=Sof(H38B)=
 Sof(H39C)=Sof(H39D)=1-FVAR(1)
 Sof(O2)=Sof(C42)=Sof(H42A)=Sof(H42B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=
 Sof(H39A)=Sof(H39B)=FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C35(H35), C23(H23), C32(H32), C20(H20)
5.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C38(H38A,H38B), C39(H39A,H39B), C39(H39C,H39D)
5.c Aromatic/amide H refined with riding coordinates:
 C14(H14), C1(H1), C12(H12), C17(H17), C11(H11), C10(H10), C16(H16), C15(H15),
 C29(H29), C2(H2), C28(H28), C5(H5), C27(H27), C26(H26), C3(H3), C4(H4)
5.d Idealised Me refined as rotating group:
 C00B(H00A,H00B,H00C), C24(H24A,H24B,H24C), C36(H36A,H36B,H36C), C34(H34A,H34B,
 H34C), C31(H31A,H31B,H31C), C21(H21A,H21B,H21C), C19(H19A,H19B,H19C), C33(H33A,
 H33B,H33C), C22(H22A,H22B,H22C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C37(H37A,H37B,H37C)
;
_shelx_res_checksum              87997
_shelx_hkl_checksum              53199
_shelx_fab_checksum              65261
_olex2_submission_special_instructions 'No special instructions were received'