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_4116630
_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 P4 Pt'
_chemical_formula_weight         523.40
_chemical_name_common            Pt(dmpp)~2~
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.879(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.481(6)
_cell_length_b                   9.892(3)
_cell_length_c                   14.524(5)
_cell_measurement_reflns_used    6120
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      31.14
_cell_measurement_theta_min      2.49
_cell_volume                     2085.1(12)
_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  0.039
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            12788
_diffrn_reflns_theta_full        31.14
_diffrn_reflns_theta_max         31.14
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    7.025
_exptl_absorpt_correction_T_max  0.32
_exptl_absorpt_correction_T_min  0.18
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.667
_exptl_crystal_density_meas      ?
_exptl_crystal_description       'rhombic bloc'
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.21
_refine_diff_density_max         1.432
_refine_diff_density_min         -3.053
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00009(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.113
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         3155
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.113
_refine_ls_R_factor_all          0.0223
_refine_ls_R_factor_gt           0.0218
_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^)+(0.0308P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0508
_refine_ls_wR_factor_ref         0.0510
_reflns_number_gt                3130
_reflns_number_total             3155
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991888y_1.cif
_cod_data_source_block           '[Pt(dmpp)2]'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measure' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2085.3(13)
_cod_database_code               4116630