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_4107269
_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_absolute_configuration rmad
_chemical_compound_source        dichloromethane,pentane
_chemical_formula_moiety         'C45 H84 N6 P, 3 (B F4), H2 O'
_chemical_formula_sum            'C45 H86 B3 F12 N6 O P'
_chemical_formula_weight         1018.60
_space_group_IT_number           14
_symmetry_Int_Tables_number      14
_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_block_code                PTA-PB-183-01
_audit_creation_date             2011-03-30
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.408(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2410(6)
_cell_length_b                   20.3202(9)
_cell_length_c                   21.5275(10)
_cell_measurement_reflns_used    9715
_cell_measurement_temperature    100
_cell_measurement_theta_max      66.2271
_cell_measurement_theta_min      3.4051
_cell_volume                     5677.8(4)
_computing_cell_refinement       'SAINT software (Bruker AXS, 2004)'
_computing_data_collection       'PROTEUM2 (Bruker AXS, 2008)'
_computing_data_reduction        'SAINT software (Bruker AXS, 2004)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_structure_refinement  'SHELXL-97 (G. M. Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (G. M. Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 66.67
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker AXS X8 Proteum'
_diffrn_measurement_method       'CCD \f- and \w-scans'
_diffrn_radiation_monochromator  'focusing multilayer optic'
_diffrn_radiation_source         '0.2 x 2mm^2^ focus rotating anode'
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0552
_diffrn_reflns_av_sigmaI/netI    0.0328
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            246109
_diffrn_reflns_theta_full        67.21
_diffrn_reflns_theta_max         67.21
_diffrn_reflns_theta_min         3.02
_exptl_absorpt_coefficient_mu    1.087
_exptl_absorpt_correction_T_max  0.87605
_exptl_absorpt_correction_T_min  0.71040
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   'SADABS (Bruker AXS, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.192
_exptl_crystal_description       prism
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.615
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     655
_refine_ls_number_reflns         10120
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0500
_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^)+(0.0468P)^2^+5.6982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1255
_refine_ls_wR_factor_ref         0.1279
_reflns_number_gt                9467
_reflns_number_total             10120
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja210223s_si_002.cif
_cod_data_source_block           7317sadabs
_cod_original_sg_symbol_Hall     '-p 2ybc'
_cod_database_code               4107269