Synthesis, Structure, and Reactivity of Carbene-Stabilized Phosphorus(III)-Centered Trications [L3P]3+
Jekaterina Petuškova; Mahendra Patil; Sigrid Holle; Christian W. Lehmann; Walter Thiel; Manuel Alcarazo; Journal of the American Chemical Society 133 (2011) 20758–20760; doi:10.1021/ja210223s

data_4107270
_publ_section_title
;
 Synthesis, Structure, and Reactivity of Carbene-Stabilized
 Phosphorus(III)-Centered Trications [L3P]3+
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              20758
_journal_page_last               20760
_journal_paper_doi               10.1021/ja210223s
_journal_volume                  133
_journal_year                    2011
_chemical_compound_source        dichloromethane,dimethylsulfoxide
_chemical_formula_moiety         'C21 H36 Cl3 N6 P Pt, 2(Cl O4), 4(C H2 Cl2)'
_chemical_formula_sum            'C25 H44 Cl13 N6 O8 P Pt'
_chemical_formula_weight         1243.57
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_block_code                AVM-AC-068-01
_audit_creation_date             2011-10-13
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                80.587(2)
_cell_angle_beta                 87.289(2)
_cell_angle_gamma                85.177(2)
_cell_formula_units_Z            2
_cell_length_a                   11.1859(13)
_cell_length_b                   12.7423(15)
_cell_length_c                   16.686(2)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    200
_cell_measurement_theta_max      34.2325
_cell_measurement_theta_min      2.1726
_cell_volume                     2336.6(5)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'APEX2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      200
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker-AXS Kappa Mach3 APEX-II'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'Incoatec Helios mirrors'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_av_unetI/netI     0.0277
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            82022
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         34.42
_diffrn_reflns_theta_min         1.62
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.827
_exptl_absorpt_correction_T_max  0.75282
_exptl_absorpt_correction_T_min  0.33054
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_description       plate
_exptl_crystal_F_000             1228
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.048
_refine_diff_density_max         3.736
_refine_diff_density_min         -1.291
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         19600
_refine_ls_number_restraints     88
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0426
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0526P)^2^+2.7705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0963
_reflns_number_gt                17089
_reflns_number_total             19600
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210223s_si_003.cif
_cod_data_source_block           7576
_cod_original_cell_volume        2336.7(5)
_cod_database_code               4107270