Kinetic Evidence for Intramolecular Proton Transfer Between Nickel and Coordinated Thiolate
William Clegg; Inorganic Chemistry 41 (2002) 1128–1135; doi:10.1021/ic0104306

data_4317615
_publ_section_title
;
 Kinetic Evidence for Intramolecular Proton Transfer Between Nickel and
 Coordinated Thiolate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1128
_journal_page_last               1135
_journal_paper_doi               10.1021/ic0104306
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C64 H58 B Ni P3 S'
_chemical_formula_weight         1021.59
_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                111.050(2)
_cell_angle_beta                 101.407(2)
_cell_angle_gamma                96.042(2)
_cell_formula_units_Z            4
_cell_length_a                   14.6807(11)
_cell_length_b                   18.6897(14)
_cell_length_c                   20.9971(16)
_cell_measurement_reflns_used    6339
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.46
_cell_measurement_theta_min      2.20
_cell_volume                     5171.7(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 and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0365
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44882
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.63
_diffrn_reflns_theta_min         1.44
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.550
_exptl_absorpt_correction_T_max  0.984
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            burgundy
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.495
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1261
_refine_ls_number_reflns         23463
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0714
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0461P)^2^+0.4294P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0933
_refine_ls_wR_factor_ref         0.1044
_reflns_number_gt                16747
_reflns_number_total             23463
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic0104306.cif
_cod_data_source_block           rah2
_cod_database_code               4317615