Solvate-free bis(triphenylphosphine)iminium chloride
Knapp, Carsten; Uzun, Rabiya; Acta Crystallographica Section E 66 (2010) o3185–; doi:10.1107/S1600536810046325

data_2228303
_publ_section_title
;
 Solvate-free bis(triphenylphosphine)iminium chloride
;
_journal_coeditor_code           FI2099
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o3185
_journal_paper_doi               10.1107/S1600536810046325
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          'C36 H30 N P2 +, Cl -'
_chemical_formula_moiety         'C36 H30 N P2 +, Cl -'
_chemical_formula_sum            'C36 H30 Cl N P2'
_chemical_formula_weight         574.00
_chemical_name_common
;
bis(triphenylphosphine)iminium chloride
;
_chemical_name_systematic
;
Bis(triphenylphosphanylidene)iminium chloride
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.06(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.094(3)
_cell_length_b                   10.499(2)
_cell_length_c                   18.615(4)
_cell_measurement_reflns_used    1435
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      27.49
_cell_measurement_theta_min      2.22
_cell_volume                     2913.2(10)
_computing_cell_refinement       'CrystalClear (Rigaku, 2007)'
_computing_data_collection       'CrystalClear (Rigaku, 2007)'
_computing_data_reduction        'CrystalClear (Rigaku, 2007)'
_computing_molecular_graphics    'DIAMOND (Brandenburg & Putz, 2010)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Rigaku R-AXIS Spider'
_diffrn_measurement_method       '\w scans and/or \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0586
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            7362
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9410
_exptl_absorpt_correction_T_min  0.9240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(ABSCOR; Higashi, 2001)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1200
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.413
_refine_diff_density_min         -0.416
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.239
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2551
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.239
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0487
_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^)+10.5312P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1059
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                2296
_reflns_number_total             2551
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            fi2099.cif
_cod_data_source_block           I
_cod_original_cell_volume        2913.0(10)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               2228303
_cod_database_fobs_code          2228303