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_4331128
_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            'C89.5 H67.5 F10 I2 N2 O P4 Pt2'
_chemical_formula_weight         2144.82
_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                88.4788(15)
_cell_angle_beta                 81.7974(16)
_cell_angle_gamma                80.0805(17)
_cell_formula_units_Z            2
_cell_length_a                   10.3642(2)
_cell_length_b                   19.8014(4)
_cell_length_c                   20.3880(4)
_cell_measurement_reflns_used    41165
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9047
_cell_measurement_theta_min      4.1577
_cell_volume                     4079.42(14)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
;
_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 0.995
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details
;
  1 omega  -94.00  -16.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615    0.0000  120.0000 78

  2 omega   -9.00   92.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000  -90.0000 101

  3 omega  -40.00   47.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -77.0000  150.0000 87

  4 omega  -50.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -77.0000   60.0000 104

  5 omega   18.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -134.0000   37.0000 57

  6 omega -102.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000  -60.0000 70

  7 omega  -92.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000    0.0000 105

  8 omega -102.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000  150.0000 70

  9 omega  -93.00   12.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -37.0000   30.0000 105

 10 omega -102.00  -32.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000 -150.0000 70

 11 omega  -10.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000  -60.0000 106

 12 omega  -11.00   95.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000  150.0000 106

 13 omega    2.00   87.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -133.0000 -142.0000 85

 14 omega   34.00   59.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000  -30.0000 25

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      -0.0088288000
_diffrn_orient_matrix_UB_12      -0.0332864000
_diffrn_orient_matrix_UB_13      0.0113633000
_diffrn_orient_matrix_UB_21      -0.0072106000
_diffrn_orient_matrix_UB_22      0.0112707000
_diffrn_orient_matrix_UB_23      0.0332621000
_diffrn_orient_matrix_UB_31      -0.0692375000
_diffrn_orient_matrix_UB_32      0.0093461000
_diffrn_orient_matrix_UB_33      0.0000830000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0821
_diffrn_reflns_av_sigmaI/netI    0.0526
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            79857
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    4.332
_exptl_absorpt_correction_T_max  0.8458
_exptl_absorpt_correction_T_min  0.2460
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.55 (release 05-01-2010 CrysAlis171 .NET)
(compiled Jan  5 2010,16:28:46)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.746
_exptl_crystal_description       needle
_exptl_crystal_F_000             2077
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         3.603
_refine_diff_density_min         -2.296
_refine_diff_density_rms         0.215
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         15993
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.0620
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0900P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                12611
_reflns_number_total             15993
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301298p_si_002_1.cif
_cod_data_source_block           5
_cod_original_cell_volume        4079.44(14)
_cod_original_formula_sum        'C89.50 H67.50 F10 I2 N2 O P4 Pt2'
_cod_database_code               4331128