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_4331129
_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            'C49 H28 F10 I N P2 Pt2'
_chemical_formula_weight         1399.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   11.79970(10)
_cell_length_b                   20.9853(2)
_cell_length_c                   34.6859(3)
_cell_measurement_reflns_used    26571
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.9127
_cell_measurement_theta_min      3.7351
_cell_volume                     8588.93(13)
_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(1)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_details
;
  1 omega  -76.00  -32.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.8053  179.0000  120.0000 176

  2 omega   35.00   77.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  179.0000  210.0000 168

  3 omega  -15.00   48.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  -77.0000  330.0000 252

  4 omega  -15.00   38.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271   87.0000   29.0000 212

  5 omega  -10.00   22.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271   37.0000  300.0000 128

  6 omega  -49.00   47.00   0.2500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       22.2271  -52.0000  264.0000 384

;
_diffrn_measurement_device_type
'Goniometer KM4/Xcalibur, detector: Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0353586924
_diffrn_orient_matrix_UB_12      0.0262702436
_diffrn_orient_matrix_UB_13      0.0046425976
_diffrn_orient_matrix_UB_21      0.0153453925
_diffrn_orient_matrix_UB_22      -0.0150159015
_diffrn_orient_matrix_UB_23      0.0175611995
_diffrn_orient_matrix_UB_31      0.0461488426
_diffrn_orient_matrix_UB_32      -0.0151255388
_diffrn_orient_matrix_UB_33      -0.0093885330
_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  0.0267
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            50175
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    7.383
_exptl_absorpt_correction_T_max  0.3846
_exptl_absorpt_correction_T_min  0.1763
_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            'pale orange'
_exptl_crystal_density_diffrn    2.165
_exptl_crystal_description       block
_exptl_crystal_F_000             5264
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.654
_refine_diff_density_min         -5.606
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         10363
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0455
_refine_ls_R_factor_gt           0.0387
_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^)+(0.0685P)^2^+96.0598P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1211
_reflns_number_gt                9027
_reflns_number_total             10363
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301298p_si_002_2.cif
_cod_data_source_block           6
_cod_database_code               4331129