Bis(trichlorophosphine)iminium salts, [Cl~3~P=N=PCl~3~]^+^, with transition metal halide counter-ions
Rivard, Eric; McWilliams, Andrew R.; Lough, Alan J.; Manners, Ian; Acta Crystallographica Section C 58 (2002) i114–i118; doi:10.1107/S0108270102012532

data_2012955
_publ_section_title
;
 Bis(trichlorophosphine)iminium salts, [Cl~3~P=N=PCl~3~]^+^, with
 transition metal halide counter-ions
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              i114
_journal_page_last               i118
_journal_paper_doi               10.1107/S0108270102012532
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac          '(Cl6 N P2) [Ti2 Cl9]'
_chemical_formula_moiety         'Cl6 N P2 1+, Cl9 Ti2 1-'
_chemical_formula_sum            'Cl15 N P2 Ti2'
_chemical_formula_weight         703.50
_chemical_name_systematic
;
Bis(trichlorophosphino)iminium tri-\m-chloro-bis[trichlorotitanium(IV)]
;
_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   none
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                91.770(2)
_cell_angle_beta                 105.714(3)
_cell_angle_gamma                107.973(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9436(4)
_cell_length_b                   9.0892(4)
_cell_length_c                   14.2963(6)
_cell_measurement_reflns_used    12979
_cell_measurement_temperature    250.0(10)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      4.3
_cell_volume                     1055.78(8)
_computing_cell_refinement       'DENZO--SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius BV, 2001)'
_computing_data_reduction        DENZO--SMN
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1999)'
_diffrn_ambient_temperature      250.0(10)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.039
_diffrn_reflns_av_sigmaI/netI    0.047
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12979
_diffrn_reflns_theta_full        26.33
_diffrn_reflns_theta_max         26.33
_diffrn_reflns_theta_min         4.31
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.790
_exptl_absorpt_correction_T_max  0.660
_exptl_absorpt_correction_T_min  0.526
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(DENZO--SMN; Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.213
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.509
_refine_diff_density_min         -0.535
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         4258
_refine_ls_number_restraints     57
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0363
_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^)+(0.0575P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0923
_refine_ls_wR_factor_ref         0.0989
_reflns_number_gt                3346
_reflns_number_total             4258
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk1570.cif
_cod_data_source_block           III
_cod_database_code               2012955
_cod_database_fobs_code          2012955