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_4336261
_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            'C100 H78 F20 N O P5 Pt3'
_chemical_formula_weight         2429.75
_chemical_name_systematic
; 
 ? 
;
_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                 90.933(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.8959(4)
_cell_length_b                   20.0988(5)
_cell_length_c                   32.2459(10)
_cell_measurement_reflns_used    30223
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.7698
_cell_measurement_theta_min      4.1606
_cell_volume                     9004.8(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
;
_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 0.907
_diffrn_measurement_details
;
  1 omega -101.00  -61.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  179.0000 -150.0000 40

  2 omega  -67.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000 -180.0000 80

  3 omega  -28.00   84.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928    0.0000 -180.0000 112

  4 omega  -92.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000   30.0000 105

  5 omega  -92.00   13.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -19.9615  -77.0000 -120.0000 105

  6 omega   48.00   96.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  162.0000  148.0000 48

  7 omega  -52.00   54.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       21.9928  -37.0000   90.0000 106

;
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       'w scans'
_diffrn_orient_matrix_UB_11      0.0216441000
_diffrn_orient_matrix_UB_12      0.0245239000
_diffrn_orient_matrix_UB_13      -0.0125998000
_diffrn_orient_matrix_UB_21      -0.0292061000
_diffrn_orient_matrix_UB_22      0.0248229000
_diffrn_orient_matrix_UB_23      0.0090993000
_diffrn_orient_matrix_UB_31      0.0358068000
_diffrn_orient_matrix_UB_32      0.0053577000
_diffrn_orient_matrix_UB_33      0.0155749000
_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  0.0485
_diffrn_reflns_av_sigmaI/netI    0.0693
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            99028
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         4.17
_exptl_absorpt_coefficient_mu    4.830
_exptl_absorpt_correction_T_max  0.5949
_exptl_absorpt_correction_T_min  0.2198
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET)
(compiled May 16 2011,17:55:39)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.792
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             4728
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.12
_refine_diff_density_max         2.022
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1174
_refine_ls_number_reflns         21469
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0514
_refine_ls_R_factor_gt           0.0292
_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^)+(0.0170P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0504
_refine_ls_wR_factor_ref         0.0522
_reflns_number_gt                15274
_reflns_number_total             21469
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401689c_si_002_4.cif
_cod_data_source_block           7'
_cod_database_code               4336261