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_4331130
_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            'C55.75 H43.5 Cl1.5 F10 I N P2 Pd Pt'
_chemical_formula_weight         1460.92
_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                 96.7838(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.2984(3)
_cell_length_b                   13.6095(2)
_cell_length_c                   22.9239(4)
_cell_measurement_reflns_used    15889
_cell_measurement_temperature    373(2)
_cell_measurement_theta_max      28.9166
_cell_measurement_theta_min      3.6735
_cell_volume                     5359.02(15)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      373(2)
_diffrn_detector_area_resol_mean 16.0655
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.892
_diffrn_measurement_details
;
  1 omega  -57.00   11.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053  -77.0000   90.0000    0.0000    0.0000 86

  2 omega  -90.00  -56.40   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053  -57.0000  189.0000    0.0000    0.0000 42

  3 omega   39.00  101.40   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2271  179.0000  120.0000    0.0000    0.0000 78

  4 omega  -49.00   48.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2271  -37.0000  270.0000    0.0000    0.0000 122

  5 omega  -92.00   12.80   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053  -77.0000  270.0000    0.0000    0.0000 131

  6 omega -102.00  -77.20   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -      -19.8053  179.0000    0.0000    0.0000    0.0000 31

  7 omega  -48.00   45.60   0.8000   10.0000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
    -       22.2271  -57.0000  189.0000    0.0000    0.0000 117

;
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0309530767
_diffrn_orient_matrix_UB_12      -0.0058778431
_diffrn_orient_matrix_UB_13      0.0229677446
_diffrn_orient_matrix_UB_21      -0.0176542814
_diffrn_orient_matrix_UB_22      0.0349202616
_diffrn_orient_matrix_UB_23      0.0171883693
_diffrn_orient_matrix_UB_31      -0.0208956165
_diffrn_orient_matrix_UB_32      -0.0382025514
_diffrn_orient_matrix_UB_33      0.0121905815
_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  0.0594
_diffrn_reflns_av_sigmaI/netI    0.0826
_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       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            48264
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.97
_diffrn_reflns_theta_min         3.75
_exptl_absorpt_coefficient_mu    3.727
_exptl_absorpt_correction_T_max  0.7548
_exptl_absorpt_correction_T_min  0.3639
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale orange'
_exptl_crystal_density_diffrn    1.811
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2830
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.357
_refine_diff_density_min         -0.868
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     667
_refine_ls_number_reflns         12672
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0683
_refine_ls_R_factor_gt           0.0349
_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^)+(0.0170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0590
_refine_ls_wR_factor_ref         0.0621
_reflns_number_gt                8362
_reflns_number_total             12672
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301298p_si_002_3.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C55.75 H43.50 Cl1.50 F10 I N P2 Pd Pt'
_cod_database_code               4331130