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_4326011
_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            'C10 H28 Br2 P4 Pd2 S'
_chemical_formula_weight         676.88
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_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                 93.9050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2224(10)
_cell_length_b                   8.3638(14)
_cell_length_c                   15.8628(4)
_cell_measurement_reflns_used    8377
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      30.02
_cell_measurement_theta_min      2.48
_cell_volume                     1088.4(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.859
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_av_sigmaI/netI    0.0789
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9314
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         30.02
_diffrn_reflns_theta_min         2.48
_exptl_absorpt_coefficient_mu    5.701
_exptl_absorpt_correction_T_max  0.181
_exptl_absorpt_correction_T_min  0.103
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.065
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.881
_refine_diff_density_min         -1.773
_refine_diff_density_rms         0.210
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.111(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.151
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0364
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1.0732P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.0906
_reflns_number_gt                4575
_reflns_number_total             4613
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic200503d_si_001_1.cif
_cod_data_source_block           2b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4326011