Reactivity of TCNE or TCNQ Derivatives of Quinonoid Zwitterions: Platinum-Induced HCN Elimination vs Oxidative-Addition
Thomas Kauf; Pierre Braunstein; Inorganic Chemistry 50 (2011) 11472–11480; doi:10.1021/ic2013045

data_4326855
_publ_contact_author_address
;Laboratoire de Chimie de Coordination
CNRS-UMR 7177
Universit\'e de Strasbourg
Institut le Bel,
4, Rue Blaise Pascal,
67081 Strasbourg,
France
;
_publ_contact_author_email       braunstein@unistra.fr
_publ_contact_author_fax         (+33)0368851322
_publ_contact_author_name        'Dr. Pierre Braunstein'
_publ_contact_author_phone       (+33)0368851308
_publ_section_title
;
 Reactivity of TCNE or TCNQ Derivatives of Quinonoid Zwitterions:
 Platinum-Induced HCN Elimination vs Oxidative-Addition
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11472
_journal_page_last               11480
_journal_paper_doi               10.1021/ic2013045
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C62 H56 N6 O2 P2 Pt, 3(C H2 Cl2)'
_chemical_formula_sum            'C65 H62 Cl6 N6 O2 P2 Pt'
_chemical_formula_weight         1428.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                98.998(2)
_cell_angle_beta                 107.8050(10)
_cell_angle_gamma                96.889(2)
_cell_formula_units_Z            2
_cell_length_a                   13.4792(4)
_cell_length_b                   14.5565(3)
_cell_length_c                   19.5384(5)
_cell_measurement_reflns_used    40359
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     3547.25(16)
_computing_cell_refinement       'Denzo (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo (Nonius B.V., 1998)'
_computing_molecular_graphics    'PLATON 98 (Spek, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi and omega scans'
_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  0.0677
_diffrn_reflns_av_sigmaI/netI    0.0697
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            36000
_diffrn_reflns_theta_full        27.46
_diffrn_reflns_theta_max         27.46
_diffrn_reflns_theta_min         1.12
_exptl_absorpt_coefficient_mu    2.292
_exptl_absorpt_correction_T_max  0.59798
_exptl_absorpt_correction_T_min  0.42767
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON (Spek, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.15
_platon_squeeze_details
;
 The residual electron density was assigned to two molecules of the
 dichloromethane solvent [183/2 = 91 e per asymmetric unit; two molecules
 of CH2Cl2 would give 84 e].
;
_refine_diff_density_max         2.555
_refine_diff_density_min         -1.390
_refine_diff_density_rms         0.166
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     676
_refine_ls_number_reflns         16095
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0769
_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^)+(0.0934P)^2^+22.0693P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2055
_reflns_number_gt                12637
_reflns_number_total             16095
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            ic2013045_si_001_4.cif
_cod_data_source_block           kauf9
_cod_database_code               4326855