Mononuclear Ni(III) Complexes [NiIII(L)(P(C6H3-3-SiMe3-2-S)3)]0/1-(L = Thiolate, Selenolate, CH2CN, Cl, PPh3): Relevance to the Nickel Site of [NiFe] Hydrogenases
Lee, Chien-Ming; Chuang, Ya-Lan; Chiang, Chao-Yi; Lee, Gene-Hsiang; Liaw, Wen-Feng; Inorganic Chemistry 45 (2006) 10895–10904; doi:10.1021/ic061399g

data_4333092
_publ_section_title
;
 Mononuclear Ni(III) Complexes [NiIII(L)(P(C6H3-3-SiMe3-2-S)3)]0/1-(L =
 Thiolate, Selenolate, CH2CN, Cl, PPh3):&#x00A0; Relevance to the Nickel
 Site of [NiFe] Hydrogenases
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10895
_journal_page_last               10904
_journal_paper_doi               10.1021/ic061399g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C67 H69 N Ni P3 S5 Si3'
_chemical_formula_weight         1284.42
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 99.830(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.9933(9)
_cell_length_b                   27.3245(16)
_cell_length_c                   17.2121(10)
_cell_measurement_reflns_used    3811
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      2.5
_cell_measurement_theta_min      25
_cell_volume                     6484.6(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0916
_diffrn_reflns_av_sigmaI/netI    0.1578
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45764
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.920
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       column
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.878
_refine_diff_density_min         -0.594
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.773
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         14888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.773
_refine_ls_R_factor_all          0.1050
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0207P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0751
_refine_ls_wR_factor_ref         0.0851
_reflns_number_gt                8044
_reflns_number_total             14888
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061399gsup4.cif
_cod_data_source_block           nv51m
_cod_database_code               4333092