Mononuclear Nickel(III) and Nickel(II) Thiolate Complexes with Intramolecular S-H Proton Interacting with Both Sulfur and Nickel: Relevance to the [NiFe]/[NiFeSe] Hydrogenases
Chien-Ming Lee; Chien-Hong Chen; Shyue-Chu Ke; Gene-Hsiang Lee; Wen-Feng Liaw; Journal of the American Chemical Society 126 (2004) 8406–8412; doi:10.1021/ja048568l

data_4112744
_publ_section_title
;
 Mononuclear Nickel(III) and Nickel(II) Thiolate Complexes with
 Intramolecular S-H Proton Interacting with Both Sulfur and Nickel:
 Relevance to the [NiFe]/[NiFeSe] Hydrogenases
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8406
_journal_page_last               8412
_journal_paper_doi               10.1021/ja048568l
_journal_volume                  126
_journal_year                    2004
_chemical_formula_sum            'C60 H48 N Ni P3 S3 Se'
_chemical_formula_weight         1109.75
_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                87.7054(3)
_cell_angle_beta                 73.0004(3)
_cell_angle_gamma                74.6810(3)
_cell_formula_units_Z            2
_cell_length_a                   10.62590(10)
_cell_length_b                   15.55330(10)
_cell_length_c                   17.08170(10)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.50
_cell_measurement_theta_min      1.25
_cell_volume                     2601.67(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'NONIUS COLLECT'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'NONIUS KappaCCD'
_diffrn_measurement_method       '\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  0.0643
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            46562
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    1.326
_exptl_absorpt_correction_T_max  0.903
_exptl_absorpt_correction_T_min  0.787
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.417
_exptl_crystal_description       plate
_exptl_crystal_F_000             1140
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.151
_refine_diff_density_min         -0.983
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.0192(9)
_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   1.107
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         11932
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.107
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0459
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1069
_refine_ls_wR_factor_ref         0.1375
_reflns_number_gt                8751
_reflns_number_total             11932
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja048568lsi20040311_101119.cif
_cod_data_source_block           ic9850
_cod_database_code               4112744