Kinetic and Theoretical Studies on the Protonation of [Ni(2-SC6H4N){PhP(CH2CH2PPh2)2}]+: Nitrogen versus Sulfur as the Protonation Site
Athinoula L. Petrou; Andreas D. Koutselos; Hilal S. Wahab; William Clegg; Ross W. Harrington; Richard A. Henderson; Inorganic Chemistry 50 (2011) 847–857; doi:10.1021/ic101444d

data_4324290
_publ_section_title
;
 Kinetic and Theoretical Studies on the Protonation of
 [Ni(2-SC6H4N){PhP(CH2CH2PPh2)2}]+: Nitrogen versus Sulfur as the
 Protonation Site
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              847
_journal_page_last               857
_journal_paper_doi               10.1021/ic101444d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety
'C29 H37 N Ni P3 S +,C24 H20 B -,2 C H4 O,0.5 C4 H8 O'
_chemical_formula_sum            'C67 H69 B N Ni O2.5 P3 S'
_chemical_formula_weight         1122.72
_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                73.159(2)
_cell_angle_beta                 73.332(2)
_cell_angle_gamma                67.844(2)
_cell_formula_units_Z            2
_cell_length_a                   11.6661(6)
_cell_length_b                   14.3526(7)
_cell_length_c                   20.1381(10)
_cell_measurement_reflns_used    16189
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.38
_cell_volume                     2928.4(3)
_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 0.983
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_device_type  'Bruker SMART 1K CCD diffractometer'
_diffrn_measurement_method       'thin-slice \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0331
_diffrn_reflns_av_sigmaI/netI    0.0543
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            24838
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.495
_exptl_absorpt_correction_T_max  0.907
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_description       plate
_exptl_crystal_F_000             1184
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.556
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         13054
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0699
_refine_ls_R_factor_gt           0.0460
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0721P)^2^+0.9623P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1198
_refine_ls_wR_factor_ref         0.1334
_reflns_number_gt                9825
_reflns_number_total             13054
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic101444d_si_003_2.cif
_cod_data_source_block           rah9_S-4py_complex
_cod_database_code               4324290