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_4311014
_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         C37H36Cl2F3O4P2PtS5Tl
_chemical_formula_sum            'C37 H36 Cl2 F3 O4 P2 Pt S5 Tl'
_chemical_formula_weight         1294.26
_chemical_name_common            'DM-TTF-(PPh2)2PtCl2, 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                 97.363(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0411(4)
_cell_length_b                   18.958(2)
_cell_length_c                   23.730(4)
_cell_measurement_reflns_used    276
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.0
_cell_volume                     4480.0(9)
_computing_cell_refinement
'Dirax/lsq (Duisenberg & Schreurs, 1989-2000)'
_computing_data_collection       KappaCCD
_computing_data_reduction        'Denzo and Scalepak'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  area_detector
_diffrn_measurement_method       CCD
_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  0.0579
_diffrn_reflns_av_sigmaI/netI    0.0683
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            47944
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         4.08
_exptl_absorpt_coefficient_mu    7.185
_exptl_absorpt_correction_T_max  0.71014
_exptl_absorpt_correction_T_min  0.32789
_exptl_absorpt_correction_type   semi-empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.919
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2480
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.914
_refine_diff_density_min         -0.775
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         10201
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1131
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+10.7648P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1156
_reflns_number_gt                5883
_reflns_number_total             10201
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035447ysi20040211_051635_4.cif
_cod_data_source_block           P2PtCl2,Tl(OTf)
_cod_original_cell_volume        4479.9(9)
_cod_database_code               4311014