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_4333091
_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 N2 Ni P3 S4 Si3'
_chemical_formula_weight         1266.37
_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                   27.3739(8)
_cell_length_b                   17.4606(5)
_cell_length_c                   28.0152(8)
_cell_measurement_reflns_used    7853
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      21.32
_cell_measurement_theta_min      2.33
_cell_volume                     13390.3(7)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'BRUKER SMART APEXCCD area detector'
_diffrn_measurement_method       'omega 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  0.1063
_diffrn_reflns_av_sigmaI/netI    0.0592
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            100069
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    0.580
_exptl_absorpt_correction_T_max  0.8685
_exptl_absorpt_correction_T_min  0.8011
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5312
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.164
_refine_diff_density_min         -0.590
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       0.00128(11)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.183
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     759
_refine_ls_number_reflns         15380
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.185
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0896
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0855P)^2^+27.2217P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1983
_refine_ls_wR_factor_ref         0.2166
_reflns_number_gt                12026
_reflns_number_total             15380
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061399gsup3.cif
_cod_data_source_block           ic11195
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4333091