Formation of P-C Bond through Reductive Coupling between Bridging Phosphido and Benzoquinolinate Groups. Isolation of Complexes of the Pt(II)/Pt(IV)/Pt(II) Sequence
Andersson Arias; Juan Forniés; Consuelo Fortuño; Antonio Martín; Mario Latronico; Piero Mastrorilli; Stefano Todisco; Vito Gallo; Inorganic Chemistry 51 (2012) 12682–12696; doi:10.1021/ic301298p

data_4331131
_publ_section_title
;
 Formation of P-C Bond through Reductive Coupling between Bridging
 Phosphido and Benzoquinolinate Groups. Isolation of Complexes of the
 Pt(II)/Pt(IV)/Pt(II) Sequence
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12682
_journal_page_last               12696
_journal_paper_doi               10.1021/ic301298p
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C53.5 H38.5 F10 I N P2 Pd2'
_chemical_formula_weight         1286.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 97.294(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.1149(7)
_cell_length_b                   13.7727(4)
_cell_length_c                   22.9446(7)
_cell_measurement_reflns_used    23102
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8717
_cell_measurement_theta_min      3.8006
_cell_volume                     5364.7(3)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.910
_diffrn_measurement_details
;
  1 omega  -64.00  -18.15   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.8053  -77.0000   60.0000 131

  2 omega  -11.00   53.75   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  -37.0000   60.0000 185

  3 omega  -26.00   93.00   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271    0.0000  120.0000 340

  4 omega   47.00   75.70   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  179.0000  300.0000 82

  5 omega  -93.00   12.00   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.8053  -37.0000  180.0000 300

  6 omega   34.00  101.90   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  179.0000  120.0000 194

  7 omega  -11.00   66.70   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271   77.0000  330.0000 222

  8 omega  -50.00   48.00   0.3500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  -51.0000  264.0000 280

;
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      -0.0336836238
_diffrn_orient_matrix_UB_12      0.0300454246
_diffrn_orient_matrix_UB_13      0.0005746096
_diffrn_orient_matrix_UB_21      0.0131356204
_diffrn_orient_matrix_UB_22      0.0124999476
_diffrn_orient_matrix_UB_23      0.0296133286
_diffrn_orient_matrix_UB_31      0.0210112908
_diffrn_orient_matrix_UB_32      0.0399677912
_diffrn_orient_matrix_UB_33      -0.0098114457
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            58471
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.93
_diffrn_reflns_theta_min         3.81
_exptl_absorpt_coefficient_mu    1.375
_exptl_absorpt_correction_T_max  0.8100
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.31 (release 08-01-2009 CrysAlis171 .NET)
(compiled Jan  8 2009,16:24:04)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_description       block
_exptl_crystal_F_000             2526
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.571
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12899
_refine_ls_number_restraints     105
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.1095
_refine_ls_R_factor_gt           0.0795
_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^)+(0.1000P)^2^+61.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2136
_refine_ls_wR_factor_ref         0.2254
_reflns_number_gt                9323
_reflns_number_total             12899
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301298p_si_002_4.cif
_cod_data_source_block           8
_cod_original_formula_sum        'C53.50 H38.50 F10 I N P2 Pd2'
_cod_database_code               4331131