Carbene-Stabilized Phosphorus(III)-Centered Cations [LPX~2~]^+^ and [L~2~PX]^2+^ (L = NHC; X = Cl, CN, N~3~)
Jan J. Weigand; Kai-Oliver Feldmann; Florian D. Henne; Journal of the American Chemical Society 132 (2010) 16321–16323; doi:10.1021/ja106172d

data_4103535
_publ_contact_author_address
;
Institut f\"ur Anorganische und Analytische Chemie
Corrensstra\&se 30
WWU M\"unster
D-48149 M\"unster
Germany
;
_publ_contact_author_email       jweigand@uni-muenster.de
_publ_contact_author_fax         +49-251-83-33108
_publ_contact_author_name        'Jan J. Weigand'
_publ_contact_author_phone       +49-251-83-36074
_publ_section_title
;
 Carbene-Stabilized Phosphorus(III)-Centered Cations [LPX~2~]^+^ and
 [L~2~PX]^2+^ (L = NHC; X = Cl, CN, N~3~)
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16321
_journal_page_last               16323
_journal_paper_doi               10.1021/ja106172d
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C23 H40 N5 P, 2(C F3 O3 S)'
_chemical_formula_sum            'C25 H40 F6 N5 O6 P S2'
_chemical_formula_weight         715.71
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2010-06-26 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.187(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.8923(9)
_cell_length_b                   9.1889(5)
_cell_length_c                   23.6454(11)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     3316.1(3)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement
;
SHELXL-97, G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_computing_structure_solution
;
SHELXS-97 , G. M. Sheldrick, Acta Cryst. (2008) A64, 112-122
;
_diffrn_ambient_temperature      153(1)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0358
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            17891
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    2.626
_exptl_absorpt_correction_T_max  0.9494
_exptl_absorpt_correction_T_min  0.8174
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax =  0.658340 

;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.945
_refine_diff_density_min         -0.642
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.572(18)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         9804
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0575
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1083P)^2^+0.6972P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1513
_refine_ls_wR_factor_ref         0.1562
_reflns_number_gt                8879
_reflns_number_total             9804
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106172d_si_005.cif
_cod_data_source_block           sad_asym
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4103535