Observation of a Chloride-Bridged P–P Bond in the Phosphorus Cation [L(Cl)P(μ-Cl)P(Cl)L]+(L = NHC)
Henne, Florian D.; Schnöckelborg, Eva-Maria; Feldmann, Kai-Oliver; Grunenberg, Jörg; Wolf, Robert; Weigand, Jan J.; Organometallics 32 (2013) 6674–; doi:10.1021/om4002268

data_4081728
_publ_section_title
;
 Observation of a Chloride-Bridged P--P Bond in the Phosphorus Cation
 [L(Cl)P(\m-Cl)P(Cl)L]+(L = NHC)
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              6674
_journal_paper_doi               10.1021/om4002268
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C27 H36 Cl2 N2 P, C F3 O3 S '
_chemical_formula_sum            'C28 H36 Cl2 F3 N2 O3 P S'
_chemical_formula_weight         639.52
_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
;
2012-05-07 # Formatted by publCIF
;
_cell_angle_alpha                90.00
_cell_angle_beta                 108.1620(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.6668(2)
_cell_length_b                   13.8796(3)
_cell_length_c                   12.3280(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     1571.66(6)
_computing_cell_refinement       'APEX2 Software Suit (v2012.2-0)'
_computing_data_collection       'APEX2 Software Suit (v2012.2-0)'
_computing_data_reduction        'APEX2 Software Suit (v2012.2-0)'
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0388
_diffrn_reflns_av_sigmaI/netI    0.0515
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            9505
_diffrn_reflns_theta_full        68.24
_diffrn_reflns_theta_max         68.24
_diffrn_reflns_theta_min         3.77
_exptl_absorpt_coefficient_mu    3.388
_exptl_absorpt_correction_T_max  0.7974
_exptl_absorpt_correction_T_min  0.5807
_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 =  0.8142

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             668
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.938
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.02(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.081
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         4855
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.081
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0873P)^2^+0.6632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1448
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                4327
_reflns_number_total             4855
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om4002268_si_001.cif
_cod_data_source_block           sad_1[OTf]
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4081728