#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/29/2012955.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2012955
loop_
_publ_author_name
'Rivard, Eric'
'McWilliams, Andrew R.'
'Lough, Alan J.'
'Manners, Ian'
_publ_section_title
;
 Bis(trichlorophosphine)iminium salts, [Cl₃P=N=PCl₃]⁺, 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-μ-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       'φ scans and ω scans with κ 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/[σ²(Fo²)+(0.0575P)²] where P = (Fo²+2Fc²)/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>2σ(I)
_cod_data_source_file            sk1570.cif
_cod_data_source_block           III
_cod_database_code               2012955
_cod_database_fobs_code          2012955
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Ti1 0.35977(6) 0.20032(6) 0.07903(4) 0.03053(15) Uani d . 1 . . Ti
Ti2 0.54436(7) 0.18594(6) 0.32013(4) 0.03525(16) Uani d . 1 . . Ti
Cl10 0.81739(11) 0.27859(12) 0.37889(7) 0.0575(3) Uani d . 1 . . Cl
Cl11 0.50611(12) -0.04308(10) 0.37568(6) 0.0486(2) Uani d . 1 . . Cl
Cl12 0.48944(12) 0.30989(11) 0.43719(6) 0.0507(2) Uani d . 1 . . Cl
Cl13 0.51682(10) 0.29241(10) -0.01527(6) 0.0430(2) Uani d . 1 . . Cl
Cl14 0.19919(10) -0.02184(9) -0.01198(6) 0.0435(2) Uani d . 1 . . Cl
Cl15 0.19202(10) 0.33726(10) 0.03959(6) 0.0469(2) Uani d . 1 . . Cl
Cl16 0.25198(9) 0.11061(9) 0.21983(5) 0.03626(19) Uani d . 1 . . Cl
Cl17 0.55712(10) 0.07112(9) 0.16598(6) 0.03882(19) Uani d . 1 . . Cl
Cl18 0.54615(9) 0.40449(8) 0.21881(5) 0.03630(18) Uani d . 1 . . Cl
N1 1.0190(5) 0.6578(5) 0.3119(3) 0.0703(13) Uani d PD 0.852(6) A 1 N
P1 0.9470(2) 0.77731(19) 0.34034(16) 0.0394(10) Uani d PD 0.852(6) A 1 P
P2 1.0800(2) 0.57493(19) 0.24280(18) 0.0396(8) Uani d PD 0.852(6) A 1 P
Cl1 0.8195(2) 0.8451(3) 0.22815(15) 0.0813(6) Uani d PDU 0.852(6) A 1 Cl
Cl2 1.1151(3) 0.9636(3) 0.41932(16) 0.0594(6) Uani d PDU 0.852(6) A 1 Cl
Cl3 0.8014(3) 0.6936(3) 0.4199(2) 0.0558(5) Uani d PDU 0.852(6) A 1 Cl
Cl4 1.2374(2) 0.4844(3) 0.31688(14) 0.0664(5) Uani d PDU 0.852(6) A 1 Cl
Cl5 1.1869(4) 0.7110(3) 0.16047(19) 0.0633(6) Uani d PDU 0.852(6) A 1 Cl
Cl6 0.9013(3) 0.4073(3) 0.15365(16) 0.0582(5) Uani d PDU 0.852(6) A 1 Cl
N1A 0.9703(14) 0.6649(14) 0.2651(9) 0.072(9) Uiso d PD 0.148(6) A 2 N
P1A 0.9404(9) 0.7795(8) 0.3313(6) 0.032(5) Uiso d PD 0.148(6) A 2 P
P2A 1.0706(10) 0.5770(9) 0.2309(6) 0.029(4) Uiso d PD 0.148(6) A 2 P
Cl1A 0.8152(12) 0.9016(13) 0.2593(8) 0.0716(18) Uani d PDU 0.148(6) A 2 Cl
Cl2A 1.1438(12) 0.9262(14) 0.4175(8) 0.051(2) Uani d PDU 0.148(6) A 2 Cl
Cl3A 0.8185(18) 0.6721(19) 0.4178(11) 0.058(2) Uani d PDU 0.148(6) A 2 Cl
Cl4A 1.2195(11) 0.5296(14) 0.3422(7) 0.0622(19) Uani d PDU 0.148(6) A 2 Cl
Cl5A 1.203(2) 0.691(2) 0.1519(10) 0.059(2) Uani d PDU 0.148(6) A 2 Cl
Cl6A 0.9304(13) 0.3808(14) 0.1511(9) 0.0488(19) Uani d PDU 0.148(6) A 2 Cl
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_publ_flag
Cl15 Ti1 Cl13 98.57(4) ?
Cl15 Ti1 Cl14 98.77(4) ?
Cl13 Ti1 Cl14 99.31(4) y
Cl15 Ti1 Cl17 165.71(4) y
Cl13 Ti1 Cl17 90.38(3) ?
Cl14 Ti1 Cl17 90.69(4) ?
Cl15 Ti1 Cl18 90.80(3) ?
Cl13 Ti1 Cl18 91.66(3) ?
Cl14 Ti1 Cl18 164.15(4) y
Cl17 Ti1 Cl18 77.75(3) ?
Cl15 Ti1 Cl16 91.36(3) ?
Cl13 Ti1 Cl16 165.03(4) y
Cl14 Ti1 Cl16 90.15(3) ?
Cl17 Ti1 Cl16 77.84(3) ?
Cl18 Ti1 Cl16 76.94(3) y
Cl11 Ti2 Cl10 97.92(4) ?
Cl11 Ti2 Cl12 98.20(4) ?
Cl10 Ti2 Cl12 97.33(4) ?
Cl11 Ti2 Cl17 89.98(3) ?
Cl10 Ti2 Cl17 91.88(4) ?
Cl12 Ti2 Cl17 166.69(4) y
Cl11 Ti2 Cl16 92.26(4) ?
Cl10 Ti2 Cl16 166.44(4) ?
Cl12 Ti2 Cl16 90.02(4) ?
Cl17 Ti2 Cl16 79.14(3) ?
Cl11 Ti2 Cl18 166.04(4) y
Cl10 Ti2 Cl18 90.67(4) ?
Cl12 Ti2 Cl18 91.55(3) ?
Cl17 Ti2 Cl18 78.70(3) ?
Cl16 Ti2 Cl18 77.70(3) ?
Ti2 Cl16 Ti1 86.43(3) y
Ti2 Cl17 Ti1 87.45(3) y
Ti2 Cl18 Ti1 86.39(3) y
P1 N1 P2 154.3(3) y
N1 P1 Cl1 113.0(2) y
N1 P1 Cl2 112.55(19) y
Cl1 P1 Cl2 107.08(10) y
N1 P1 Cl3 111.23(19) y
Cl1 P1 Cl3 106.92(9) y
Cl2 P1 Cl3 105.66(9) y
N1 P2 Cl4 110.3(2) y
N1 P2 Cl6 111.82(18) y
Cl4 P2 Cl6 107.47(8) y
N1 P2 Cl5 113.88(18) y
Cl4 P2 Cl5 107.10(8) y
Cl6 P2 Cl5 105.92(10) y
P1A N1A P2A 155.8(4) ?
N1A P1A Cl1A 112.9(2) ?
N1A P1A Cl2A 112.7(2) ?
Cl1A P1A Cl2A 107.03(14) ?
N1A P1A Cl3A 111.2(2) ?
Cl1A P1A Cl3A 106.91(13) ?
Cl2A P1A Cl3A 105.62(12) ?
N1A P2A Cl4A 110.4(2) ?
N1A P2A Cl6A 111.7(2) ?
Cl4A P2A Cl6A 107.45(13) ?
N1A P2A Cl5A 113.9(2) ?
Cl4A P2A Cl5A 107.09(12) ?
Cl6A P2A Cl5A 105.92(13) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Ti1 Cl15 . 2.2036(10) y
Ti1 Cl13 . 2.2047(9) ?
Ti1 Cl14 . 2.2065(9) ?
Ti1 Cl17 . 2.4941(9) y
Ti1 Cl18 . 2.5047(9) y
Ti1 Cl16 . 2.5127(8) y
Ti2 Cl11 . 2.2115(10) ?
Ti2 Cl10 . 2.2256(11) ?
Ti2 Cl12 . 2.2319(10) y
Ti2 Cl17 . 2.4548(9) y
Ti2 Cl16 . 2.4832(9) y
Ti2 Cl18 . 2.4930(9) y
N1 P1 . 1.519(3) y
N1 P2 . 1.530(3) y
P1 Cl1 . 1.938(2) ?
P1 Cl2 . 1.9477(16) ?
P1 Cl3 . 1.9531(16) ?
P2 Cl4 . 1.934(2) ?
P2 Cl6 . 1.9426(16) ?
P2 Cl5 . 1.9488(18) ?
N1A P1A . 1.517(3) ?
N1A P2A . 1.528(3) ?
P1A Cl1A . 1.938(2) ?
P1A Cl2A . 1.9477(18) ?
P1A Cl3A . 1.9532(18) ?
P2A Cl4A . 1.934(2) ?
P2A Cl6A . 1.9429(18) ?
P2A Cl5A . 1.949(2) ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_publ_flag
Cl11 Ti2 Cl16 Ti1 -128.87(3) ?
Cl10 Ti2 Cl16 Ti1 9.87(18) ?
Cl12 Ti2 Cl16 Ti1 132.93(3) ?
Cl17 Ti2 Cl16 Ti1 -39.32(3) ?
Cl18 Ti2 Cl16 Ti1 41.34(3) ?
Cl15 Ti1 Cl16 Ti2 -131.76(3) ?
Cl13 Ti1 Cl16 Ti2 -0.01(15) ?
Cl14 Ti1 Cl16 Ti2 129.47(3) ?
Cl17 Ti1 Cl16 Ti2 38.79(3) ?
Cl18 Ti1 Cl16 Ti2 -41.26(3) ?
Cl11 Ti2 Cl17 Ti1 131.93(4) ?
Cl10 Ti2 Cl17 Ti1 -130.15(4) ?
Cl12 Ti2 Cl17 Ti1 3.73(18) ?
Cl16 Ti2 Cl17 Ti1 39.62(3) ?
Cl18 Ti2 Cl17 Ti1 -39.84(3) ?
Cl15 Ti1 Cl17 Ti2 2.38(16) ?
Cl13 Ti1 Cl17 Ti2 131.40(3) ?
Cl14 Ti1 Cl17 Ti2 -129.28(3) ?
Cl18 Ti1 Cl17 Ti2 39.78(3) ?
Cl16 Ti1 Cl17 Ti2 -39.28(3) ?
Cl11 Ti2 Cl18 Ti1 3.27(17) ?
Cl10 Ti2 Cl18 Ti1 131.46(4) ?
Cl12 Ti2 Cl18 Ti1 -131.18(4) ?
Cl17 Ti2 Cl18 Ti1 39.68(3) ?
Cl16 Ti2 Cl18 Ti1 -41.51(3) ?
Cl15 Ti1 Cl18 Ti2 132.27(3) ?
Cl13 Ti1 Cl18 Ti2 -129.13(3) ?
Cl14 Ti1 Cl18 Ti2 4.88(14) ?
Cl17 Ti1 Cl18 Ti2 -39.10(3) ?
Cl16 Ti1 Cl18 Ti2 41.06(3) ?
P2 N1 P1 Cl1 23.6(8) ?
P2 N1 P1 Cl2 -97.9(7) ?
P2 N1 P1 Cl3 143.8(7) y
P1 N1 P2 Cl4 155.0(7) y
P1 N1 P2 Cl6 -85.5(7) ?
P1 N1 P2 Cl5 34.5(8) ?
P2A N1A P1A Cl1A 138(2) ?
P2A N1A P1A Cl2A 16(2) ?
P2A N1A P1A Cl3A -102(2) ?
P1A N1A P2A Cl4A 36(2) ?
P1A N1A P2A Cl6A 156(2) ?
P1A N1A P2A Cl5A -84(2) ?
