Synthetic and Structural Studies of the Coordination Behavior of 2-Pyridylbis(diphenylphosphino)methane
Joel T. Mague; Jamin L. Krinsky; Inorganic Chemistry 40 (2001) 1962–1971; doi:10.1021/ic001266+

data_4327576
_publ_section_title
;
 Synthetic and Structural Studies of the Coordination Behavior of
 2-Pyridylbis(diphenylphosphino)methane
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1962
_journal_page_last               1971
_journal_paper_doi               10.1021/ic001266+
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '(((C6 H5)2 P)2 C (C5 H4 N))((C6 H5)3)P H Pt'
_chemical_formula_sum            'C48 H40 N P3 Pt'
_chemical_formula_weight         918.81
_chemical_name_systematic
; 
 Hydrido(\h^2^-(2-pyridylbis(diphenylphosphino)methanido))triphenylphosphine 
 platinum(II)
;
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.975(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.0878(11)
_cell_length_b                   12.8836(9)
_cell_length_c                   18.4228(17)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.23
_cell_measurement_theta_min      21.52
_cell_volume                     3952.6(6)
_computing_cell_refinement       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1987)'
_computing_molecular_graphics    'SHELXTL (Bruker AXS, 1997)'
_computing_publication_material  'SHELXTL (Bruker AXS, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\q/2\q scans'
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0566
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7270
_diffrn_reflns_theta_full        25.11
_diffrn_reflns_theta_max         25.11
_diffrn_reflns_theta_min         1.98
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  120
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    3.707
_exptl_absorpt_correction_T_max  0.7241
_exptl_absorpt_correction_T_min  0.4426
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '\y scan (Phillips, et al., 1968)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.544
_exptl_crystal_description       Plate
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.734
_refine_diff_density_min         -0.938
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     478
_refine_ls_number_reflns         7031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0688
_refine_ls_R_factor_gt           0.0292
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0427P)^2^+1.5430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0727
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                5069
_reflns_number_total             7031
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0012662B_10.cif
_cod_data_source_block           14
_cod_original_cell_volume        3952.6(5)
_cod_database_code               4327576