Reactions of the Bis(dialkylphosphino)methane Complexes Pd2X2(μ-R2PCH2PR2)2 (X = halogen, R = Me or Et) with H2S, S8, COS, and CS2; Detection of Reaction Intermediates
Craig B. Pamplin; Steven J. Rettig; Brian O. Patrick; Brian R. James; Inorganic Chemistry 50 (2011) 8094–8105; doi:10.1021/ic200503d

data_4326012
_publ_section_title
;
 Reactions of the Bis(dialkylphosphino)methane Complexes
 Pd2X2(\m-R2PCH2PR2)2 (X = halogen, R = Me or Et) with H2S, S8, COS, and
 CS2; Detection of Reaction Intermediates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8094
_journal_page_last               8105
_journal_paper_doi               10.1021/ic200503d
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C11 H28 Cl2 O0 P4 Pd2 S2'
_chemical_formula_weight         632.03
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   27.7975(4)
_cell_length_b                   27.7975(4)
_cell_length_c                   17.7113(5)
_cell_measurement_reflns_used    26060
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.5
_cell_measurement_theta_min      2.0
_cell_volume                     11852.0(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Rigaku/ADSC CCD'
_diffrn_measurement_method       'area detector'
_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  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35236
_diffrn_reflns_theta_full        30.03
_diffrn_reflns_theta_max         30.03
_diffrn_reflns_theta_min         2.05
_exptl_absorpt_coefficient_mu    1.963
_exptl_absorpt_correction_T_max  0.555
_exptl_absorpt_correction_T_min  0.386
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.594
_exptl_crystal_description       irregular
_exptl_crystal_F_000             5616
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.30
_platon_squeeze_details
;
;
_refine_diff_density_max         0.807
_refine_diff_density_min         -0.880
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     198
_refine_ls_number_reflns         7381
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0274
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0738
_refine_ls_wR_factor_ref         0.0750
_reflns_number_gt                5884
_reflns_number_total             7381
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200503d_si_001_2.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4326012