Proton Transfer to Nickel-Thiolate Complexes. 1. Protonation of [Ni(SC6H4R-4)2(Ph2PCH2CH2PPh2)] (R = Me, MeO, H, Cl, or NO2)
Valerie Autissier; William Clegg; Ross W. Harrington; Richard A. Henderson; Inorganic Chemistry 43 (2004) 3098–3105; doi:10.1021/ic030322e

data_4310952
_publ_section_title
;
 Proton Transfer to Nickel-Thiolate Complexes. 1. Protonation of
 [Ni(SC6H4R-4)2(Ph2PCH2CH2PPh2)] (R = Me, MeO, H, Cl, or NO2)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3098
_journal_page_last               3105
_journal_paper_doi               10.1021/ic030322e
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C76.5 H65 Cl5 Ni2 P4 S4'
_chemical_formula_weight         1531.08
_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                65.2550(10)
_cell_angle_beta                 75.7480(10)
_cell_angle_gamma                71.4270(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6352(7)
_cell_length_b                   16.5127(8)
_cell_length_c                   18.9762(10)
_cell_measurement_reflns_used    18479
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.76
_cell_measurement_theta_min      2.26
_cell_volume                     3646.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0360
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            26364
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.40
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.944
_exptl_absorpt_correction_T_max  0.8336
_exptl_absorpt_correction_T_min  0.7038
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1578
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.228
_refine_diff_density_min         -0.941
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         12693
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0607P)^2^+4.7114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                9401
_reflns_number_total             12693
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic030322e_s_3.cif
_cod_data_source_block           rah47
_cod_original_formula_sum        'C76.50 H65 Cl5 Ni2 P4 S4'
_cod_database_code               4310952