Relative Hydride, Proton, and Hydrogen Atom Transfer Abilities of [HM(diphosphine)2]PF6 Complexes (M = Pt, Ni)
Douglas E. Berning; Bruce C. Noll; Daniel L. DuBois; Journal of the American Chemical Society 121 (1999) 11432–11447; doi:10.1021/ja991888y

data_4116633
_publ_section_title
;
 Relative Hydride, Proton, and Hydrogen Atom Transfer Abilities of
 [HM(diphosphine)2]PF6 Complexes (M = Pt, Ni)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11432
_journal_page_last               11447
_journal_paper_doi               10.1021/ja991888y
_journal_volume                  121
_journal_year                    1999
_chemical_formula_sum            'C14 H36 B2 F8 Ni P4'
_chemical_formula_weight         560.64
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   refall
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.136(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.8371(13)
_cell_length_b                   16.764(3)
_cell_length_c                   14.8801(18)
_cell_measurement_reflns_used    7583
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      30.81
_cell_measurement_theta_min      1.85
_cell_volume                     2407.7(6)
_computing_cell_refinement       'Siemens SAINT'
_computing_data_collection       'Siemens SMART'
_computing_data_reduction        'Siemens SAINT'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.935
_diffrn_measured_fraction_theta_max 0.935
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       '\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  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0188
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            21377
_diffrn_reflns_theta_full        30.81
_diffrn_reflns_theta_max         30.81
_diffrn_reflns_theta_min         1.85
_exptl_absorpt_coefficient_mu    1.133
_exptl_absorpt_correction_T_max  0.71
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.491
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     436
_refine_ls_number_reflns         7057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0286
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0308P)^2^+1.7342P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0672
_refine_ls_wR_factor_ref         0.0716
_reflns_number_gt                6203
_reflns_number_total             7057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991888y_4.cif
_cod_data_source_block           '[Ni(dmpp)2](BF4)2'
_cod_database_code               4116633