Structural investigation of homonuclear Pt~2~ and heteronuclear PdPt complexes containing a metal‒metal bond bridged by hydrido and sulfido ligands
Clegg, William; Capdevila, Mercè; González-Duarte, Pilar; Sola, Joan; Acta Crystallographica Section B 52 (1996) 270–276; doi:10.1107/S0108768195010640

data_2101487
_publ_section_title
;
 Structural investigation of homonuclear Pt~2~ and heteronuclear PdPt
 complexes containing a metal--metal bond bridged by hydrido and
 sulfido ligands
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              270
_journal_page_last               276
_journal_paper_doi               10.1107/S0108768195010640
_journal_volume                  52
_journal_year                    1996
_chemical_formula_sum            'C52 H49 F6 P5 Pt2 S'
_chemical_formula_weight         1365.00
_chemical_name_systematic
;
 ?
;
_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'
_cell_angle_alpha                90.00
_cell_angle_beta                 95.92(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.689(4)
_cell_length_b                   21.857(7)
_cell_length_c                   16.662(5)
_cell_measurement_reflns_used    32
_cell_measurement_temperature    160.0(10)
_cell_measurement_theta_max      12.25
_cell_measurement_theta_min      10.20
_cell_volume                     4959(3)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'SHELXL-93 and local programs'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      160.0(10)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method
'\w/\q scans with on-line profile fitting (Clegg, 1981)'
_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  0.0307
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -3
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10478
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         4
_exptl_absorpt_coefficient_mu    5.898
_exptl_absorpt_correction_T_max  0.225
_exptl_absorpt_correction_T_min  0.144
_exptl_absorpt_correction_type   '\y scans (SHELXTL)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.828
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         '2.097 e \%A^-3^ 1.1\%A from Pt'
_refine_diff_density_min         '-1.204 e \%A^-3^ 1.1\%A from Pt'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.099
_refine_ls_goodness_of_fit_obs   1.054
_refine_ls_hydrogen_treatment    'H-atom treatment: see text'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     599
_refine_ls_number_reflns         8679
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.124
_refine_ls_restrained_S_obs      1.054
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_obs          0.0385
_refine_ls_shift/esd_max         2.821
_refine_ls_shift/esd_mean        0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^)+(0.0254P)^2^+58.7745P] where
P = (F~o~^2^+2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.1163
_refine_ls_wR_factor_obs         0.0850
_reflns_number_observed          5497
_reflns_number_total             8708
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg0001.cif
_cod_data_source_block           pg11b
_cod_original_cell_volume        4959.(3)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2101487