Mononuclear Nickel(III) Complexes [NiIII(OR)(P(C6H3-3-SiMe3-2-S)3)]- (R = Me, Ph) Containing the Terminal Alkoxide Ligand: Relevance to the Nickel Site of Oxidized-Form [NiFe] Hydrogenases
Tzung-Wen Chiou; Wen-Feng Liaw; Inorganic Chemistry 47 (2008) 7908–7913; doi:10.1021/ic801069t

data_4306157
_publ_section_title
;
Mononuclear Nickel(III) Complexes [NiIII(OR)(P(C6H3-3-SiMe3-2-S)3)]- (R =
Me, Ph) Containing the Terminal Alkoxide Ligand: Relevance to the Nickel
Site of Oxidized-Form [NiFe] Hydrogenases
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7908
_journal_page_last               7913
_journal_paper_doi               10.1021/ic801069t
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C66 H77 N Ni O3 P3 S3 Si3'
_chemical_formula_sum            'C66 H77 N Ni O3 P3 S3 Si3'
_chemical_formula_weight         1264.36
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                76.7230(10)
_cell_angle_beta                 77.5540(10)
_cell_angle_gamma                65.5870(10)
_cell_formula_units_Z            2
_cell_length_a                   15.0077(3)
_cell_length_b                   15.4326(3)
_cell_length_c                   16.8312(4)
_cell_measurement_reflns_used    98733
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      25.35
_cell_measurement_theta_min      2.037
_cell_volume                     3422.68(13)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 19'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'CCD rotation images, thick slices'
_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  0.0872
_diffrn_reflns_av_sigmaI/netI    0.0577
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            48263
_diffrn_reflns_theta_full        25.36
_diffrn_reflns_theta_max         25.36
_diffrn_reflns_theta_min         2.08
_exptl_absorpt_coefficient_mu    0.541
_exptl_absorpt_correction_T_max  1.0717
_exptl_absorpt_correction_T_min  0.6956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 ?
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1334
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.567
_refine_diff_density_min         -0.712
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    fixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         12495
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0741
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0971P)^2^+3.4970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1589
_refine_ls_wR_factor_ref         0.1774
_reflns_number_gt                10043
_reflns_number_total             12495
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic801069t-file003_3.cif
_cod_data_source_block           complex3
_cod_database_code               4306157