Studies of Structural Effects on the Half-Wave Potentials of Mononuclear and Dinuclear Nickel(II) Diphosphine/Dithiolate Complexes
Kendra Redin; Aaron D. Wilson; Rachel Newell; M. Rakowski DuBois; Daniel L. DuBois; Inorganic Chemistry 46 (2007) 1268–1276; doi:10.1021/ic061740x

data_4307203
_publ_contact_author_address
'Division of Chemical Sciences, Pacific Northwest National Laboratory, Richland, WA 99352'
_publ_contact_author_name        'Daniel L. DuBois'
_publ_section_title
;
Studies of Structural Effects on the Half-Wave Potentials of Mononuclear
and Dinuclear Nickel(II) Diphosphine/Dithiolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1268
_journal_page_last               1276
_journal_paper_doi               10.1021/ic061740x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C57 H57 B2 F8 N Ni2 P4 S2'
_chemical_formula_weight         1235.06
_chemical_name_common            '[(SC3H6S)(Nidppe)2](BF4)2'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 107.9140(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.1836(5)
_cell_length_b                   47.750(2)
_cell_length_c                   10.3067(4)
_cell_measurement_reflns_used    4224
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      22.843
_cell_measurement_theta_min      2.310
_cell_volume                     5705.4(4)
_computing_cell_refinement       'SAINT, Bruker'
_computing_data_collection       'SMART, Bruker'
_computing_data_reduction        'SAINT, Bruker'
_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      143(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1750
_diffrn_reflns_av_sigmaI/netI    0.2054
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       54
_diffrn_reflns_limit_k_min       -62
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            45702
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_T_max  0.9145
_exptl_absorpt_correction_T_min  0.7412
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 absorption correction applied
 using SADABS (Blessing, R. H. Acta Crystallogr., Sect. A 1995, 51, 33-38)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'cut prism'
_exptl_crystal_F_000             2544
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.679
_refine_diff_density_min         -0.605
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.951
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         13090
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.951
_refine_ls_R_factor_all          0.1783
_refine_ls_R_factor_gt           0.0808
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0657P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1621
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                6015
_reflns_number_total             13090
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061740xsi20060913_033027_2.cif
_cod_data_source_block           p22
_cod_database_code               4307203