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_4081729
_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_sum            'C61 H84 Cl3 F3 N4 O4.5 P2 S'
_chemical_formula_weight         1202.67
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 101.776(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9384(5)
_cell_length_b                   29.4375(11)
_cell_length_c                   18.4497(7)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     6879.1(5)
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w and \f 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  0.0370
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            19795
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         3.00
_exptl_absorpt_coefficient_mu    2.357
_exptl_absorpt_correction_T_max  0.8158
_exptl_absorpt_correction_T_min  0.4102
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2552
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.372
_refine_diff_density_rms         0.082
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.040(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     747
_refine_ls_number_reflns         10161
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0591
_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^)+(0.1330P)^2^+1.2274P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1579
_refine_ls_wR_factor_ref         0.1614
_reflns_number_gt                9746
_reflns_number_total             10161
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om4002268_si_001.cif
_cod_data_source_block           rw270311_2[OTf]
_cod_original_sg_symbol_H-M      Cc
_cod_original_formula_sum        'C61 H84 Cl3 F3 N4 O4.50 P2 S'
_cod_database_code               4081729