Unexpected Reactivity of PdCl2 and PtCl2 Complexes of the Unsaturated Diphosphineo-Me2TTF(PPh2)2 toward Chloride Abstraction with Thallium Triflate
Thomas Devic; Patrick Batail; Marc Fourmigué; Narcis Avarvari; Inorganic Chemistry 43 (2004) 3136–3141; doi:10.1021/ic035447y

data_4311011
_publ_section_title
;
 Unexpected Reactivity of PdCl2 and PtCl2 Complexes of the Unsaturated
 Diphosphineo-Me2TTF(PPh2)2 toward Chloride Abstraction with Thallium
 Triflate
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3136
_journal_page_last               3141
_journal_paper_doi               10.1021/ic035447y
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         C34H28Cl8P2PdS4
_chemical_formula_sum            'C34 H28 Cl8 P2 Pd S4'
_chemical_formula_weight         1016.74
_chemical_name_common            'DM-TTF-(PPh2)2PdCl2, 2CHCl3'
_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'
_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                 118.152(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.0352(13)
_cell_length_b                   15.7744(11)
_cell_length_c                   17.8266(14)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.75
_cell_measurement_theta_min      1.85
_cell_volume                     4223.7(6)
_computing_cell_refinement       'CELL, Stoe-IPDS'
_computing_data_collection       'EXPOSE, Stoe-IPDS'
_computing_data_reduction        'INTEGRATE, Stoe-IPDS'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 1.3'
_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  0.1072
_diffrn_reflns_av_sigmaI/netI    0.0995
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            34575
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    1.244
_exptl_absorpt_correction_T_max  0.807
_exptl_absorpt_correction_T_min  0.663
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.599
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.22
_refine_diff_density_max         4.146
_refine_diff_density_min         -1.377
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.264
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     442
_refine_ls_number_reflns         8099
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.264
_refine_ls_R_factor_all          0.1328
_refine_ls_R_factor_gt           0.0892
_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^)+(0.1213P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2695
_refine_ls_wR_factor_ref         0.2806
_reflns_number_gt                4605
_reflns_number_total             8099
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035447ysi20040211_051635_1.cif
_cod_data_source_block           P2PdCl2
_cod_original_cell_volume        4223.7(5)
_cod_database_code               4311011