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_4336259
_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            'C73 H91 Cl2 F20 N3 O P Pt2'
_chemical_formula_weight         1898.54
_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                102.329(5)
_cell_angle_beta                 94.439(4)
_cell_angle_gamma                107.748(4)
_cell_formula_units_Z            2
_cell_length_a                   11.9169(5)
_cell_length_b                   15.8673(9)
_cell_length_c                   23.4522(13)
_cell_measurement_reflns_used    11479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.8811
_cell_measurement_theta_min      4.1066
_cell_volume                     4077.4(4)
_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 0.996
_diffrn_measurement_details
;
  1 omega  -50.00   48.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000 -150.0000 98

  2 omega   11.00   36.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000    0.0000 25

  3 omega  -51.00   49.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000  120.0000 100

  4 omega    3.00   50.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000 -120.0000 47

  5 omega  -52.00  -26.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   77.0000    0.0000 26

  6 omega  -10.00   38.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000   90.0000 48

  7 omega  -11.00   88.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   77.0000  -30.0000 99

  8 omega  -38.00   17.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -87.0000   70.0000 55

  9 omega  -52.00   54.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615   37.0000  -30.0000 106

 10 omega  -93.00   12.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -37.0000  150.0000 105

 11 omega   34.00   86.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000 -180.0000 52

 12 omega  -10.00   96.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490   37.0000  -30.0000 106

 13 omega   34.00  102.00   1.0000   35.0000
omega____ theta____ kappa____ phi______ frames
    -       22.1490  179.0000   90.0000 68

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0322271748
_diffrn_orient_matrix_UB_12      0.0271530586
_diffrn_orient_matrix_UB_13      -0.0176961205
_diffrn_orient_matrix_UB_21      -0.0060246034
_diffrn_orient_matrix_UB_22      -0.0402150755
_diffrn_orient_matrix_UB_23      -0.0220355123
_diffrn_orient_matrix_UB_31      -0.0542392790
_diffrn_orient_matrix_UB_32      0.0018820028
_diffrn_orient_matrix_UB_33      -0.0136411899
_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  0.0988
_diffrn_reflns_av_sigmaI/netI    0.1643
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            65427
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         4.12
_exptl_absorpt_coefficient_mu    3.600
_exptl_absorpt_correction_T_max  0.8997
_exptl_absorpt_correction_T_min  0.8130
_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    1.546
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1886
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.832
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.133
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.921
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     916
_refine_ls_number_reflns         15962
_refine_ls_number_restraints     51
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1025
_refine_ls_R_factor_gt           0.0456
_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^)+(0.0100P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0704
_reflns_number_gt                9031
_reflns_number_total             15962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401689c_si_002_2.cif
_cod_data_source_block           5a
_cod_database_code               4336259