Formation of [NiIII(κ1-S2CH)(P(o-C6H3-3-SiMe3-2-S)3)]-via CS2 Insertion into Nickel(III) Hydride Containing [NiIII(H)(P(o-C6H3-3-SiMe3-2-S)3)]-
Kuan-Ting Lai; Wei-Chieh Ho; Tzung-Wen Chiou; Wen-Feng Liaw; Inorganic Chemistry 52 (2013) 4151–4153; doi:10.1021/ic400293k

data_4334529
_publ_section_title
;
 Formation of [NiIII(\k1-S2CH)(P(o-C6H3-3-SiMe3-2-S)3)]-via CS2 Insertion
 into Nickel(III) Hydride Containing [NiIII(H)(P(o-C6H3-3-SiMe3-2-S)3)]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4151
_journal_page_last               4153
_journal_paper_doi               10.1021/ic400293k
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C64 H67 N Ni P3 S5 Si3'
_chemical_formula_weight         1246.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.452(2)
_cell_length_b                   17.5520(14)
_cell_length_c                   27.756(3)
_cell_measurement_reflns_used    9910
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.3965
_cell_measurement_theta_min      2.5446
_cell_volume                     13374(2)
_computing_cell_refinement       'SAINT V7.68A (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT V7.68A (Bruker AXS, 2009)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            103184
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.47
_exptl_absorpt_coefficient_mu    0.609
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.8723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008/1 (Bruker AXS)'
_exptl_crystal_colour            Black
_exptl_crystal_density_diffrn    1.238
_exptl_crystal_description       Lump
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
;
_refine_diff_density_max         0.853
_refine_diff_density_min         -0.513
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         13685
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0512
_refine_ls_R_factor_gt           0.0373
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0529P)^2^+4.0308P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0938
_refine_ls_wR_factor_ref         0.0992
_reflns_number_gt                10888
_reflns_number_total             13685
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic400293k_si_001.cif
_cod_data_source_block           120920lts
_cod_database_code               4334529