Addition of Nucleophiles to Phosphanido Derivatives of Pt(III): Formation of P-C, P-N, and P-O Bonds
Andersson Arias; Juan Forniés; Consuelo Fortuño; Susana Ibáñez; Antonio Martín; Piero Mastrorilli; Vito Gallo; Stefano Todisco; Inorganic Chemistry 52 (2013) 11398–11408; doi:10.1021/ic401689c

data_4336258
_publ_section_title
;
 Addition of Nucleophiles to Phosphanido Derivatives of Pt(III): Formation
 of P-C, P-N, and P-O Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11398
_journal_page_last               11408
_journal_paper_doi               10.1021/ic401689c
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C72 H91 Cl2 F20 N5 P Pt2'
_chemical_formula_weight         1898.55
_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                102.0812(9)
_cell_angle_beta                 94.0890(8)
_cell_angle_gamma                107.7983(10)
_cell_formula_units_Z            2
_cell_length_a                   11.92684(12)
_cell_length_b                   15.87947(19)
_cell_length_c                   23.5241(2)
_cell_measurement_reflns_used    49250
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7968
_cell_measurement_theta_min      4.1095
_cell_volume                     4104.06(8)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_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 0.916
_diffrn_measurement_details
;
  1 omega -102.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000   60.0000 70

  2 omega   -7.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000   30.0000 103

  3 omega  -10.00   94.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000  -60.0000 104

  4 omega   -6.00   33.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -117.0000  149.0000 39

  5 omega   49.00   74.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -117.0000  149.0000 25

  6 omega   43.00   75.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490 -117.0000  -30.0000 32

  7 omega   35.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000  150.0000 67

  8 omega  -92.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000  -30.0000 105

  9 omega  -92.00   13.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000 -150.0000 105

 10 omega  -52.00   54.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   37.0000 -120.0000 106

 11 omega -102.00  -32.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000 -150.0000 70

 12 omega   34.00  102.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000  120.0000 68

 13 omega  -10.00   96.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000  150.0000 106

 14 omega  -50.00    8.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  -77.0000   90.0000 58

 15 omega  -11.00   95.00   1.0000   15.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000  150.0000 106

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      -0.0019892097
_diffrn_orient_matrix_UB_12      -0.0203416427
_diffrn_orient_matrix_UB_13      -0.0300848875
_diffrn_orient_matrix_UB_21      0.0074792945
_diffrn_orient_matrix_UB_22      0.0426328668
_diffrn_orient_matrix_UB_23      -0.0068044963
_diffrn_orient_matrix_UB_31      0.0626416601
_diffrn_orient_matrix_UB_32      0.0102600102
_diffrn_orient_matrix_UB_33      0.0044680710
_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  0.0393
_diffrn_reflns_av_sigmaI/netI    0.0399
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            89134
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.86
_diffrn_reflns_theta_min         4.14
_exptl_absorpt_coefficient_mu    3.576
_exptl_absorpt_correction_T_max  0.6944
_exptl_absorpt_correction_T_min  0.3288
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_description       block
_exptl_crystal_F_000             1886
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.11
_refine_diff_density_max         4.873
_refine_diff_density_min         -1.296
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         19725
_refine_ls_number_restraints     45
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0511
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0985
_reflns_number_gt                15348
_reflns_number_total             19725
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401689c_si_002_1.cif
_cod_data_source_block           4a
_cod_database_code               4336258