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_4311012
_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         C37H36Cl2F3O4P2PdS5Tl
_chemical_formula_sum            'C37 H36 Cl2 F3 O4 P2 Pd S5 Tl'
_chemical_formula_weight         1205.57
_chemical_name_common            'DM-TTF-(PPh2)2PdCl2, Tl(OTf), Et2O'
_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                 96.044(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.9545(5)
_cell_length_b                   18.5549(13)
_cell_length_c                   23.9138(13)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.7
_cell_measurement_theta_min      2.0
_cell_volume                     4392.4(5)
_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 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       'rotation, phi incr. 1.0'
_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  0.0668
_diffrn_reflns_av_sigmaI/netI    0.1132
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            36124
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    4.556
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.603
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT, Stoe-IPDS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2352
_exptl_crystal_size_max          0.77
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.675
_refine_diff_density_min         -0.580
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.696
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     471
_refine_ls_number_reflns         8198
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.709
_refine_ls_R_factor_all          0.0948
_refine_ls_R_factor_gt           0.0394
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0382P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0852
_refine_ls_wR_factor_ref         0.0945
_reflns_number_gt                3645
_reflns_number_total             8198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035447ysi20040211_051635_2.cif
_cod_data_source_block           P2PdCl2,Tl(OTf)
_cod_original_cell_volume        4392.4(4)
_cod_database_code               4311012