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_4103536
_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         +49-251-83-363018
_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         'C22 H40 N7 P, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C25 H42 Cl2 F6 N7 O6 P S2'
_chemical_formula_weight         816.65
_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
_audit_update_record
;
2010-06-26 # Formatted by publCIF
;
_cell_angle_alpha                82.943(2)
_cell_angle_beta                 85.659(2)
_cell_angle_gamma                79.724(2)
_cell_formula_units_Z            2
_cell_length_a                   10.1689(3)
_cell_length_b                   10.5770(4)
_cell_length_c                   17.9056(5)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(1)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     1877.76(11)
_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 1.000
_diffrn_measured_fraction_theta_max 0.906
_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  0.0356
_diffrn_reflns_av_sigmaI/netI    0.0477
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9944
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         63.68
_diffrn_reflns_theta_min         2.49
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  0.8975
_exptl_absorpt_correction_T_min  0.6079
_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 =  0.546091 

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             848
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.736
_refine_diff_density_min         -0.386
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         5609
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.956
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0621
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1217P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1558
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                4028
_reflns_number_total             5609
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja106172d_si_006.cif
_cod_data_source_block           sad
_cod_original_cell_volume        1877.76(10)
_cod_database_code               4103536