#------------------------------------------------------------------------------
#$Date: 2016-02-18 14:25:00 +0200 (Thu, 18 Feb 2016) $
#$Revision: 176728 $
#$URL: svn://www.crystallography.net/cod/cif/8/10/19/8101908.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_8101908
loop_
_publ_author_name
'Li, M.-F.'
'Shan, Y.-K.'
_publ_section_title
;
Crystal structure of trans-bis(triphenylphospine oxide)-tetrachlorotitanum
(IV), TiCl₄[(C₆H₅)₃PO]₂
;
_journal_issue                   1
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              41
_journal_page_last               42
_journal_volume                  221
_journal_year                    2006
_chemical_formula_structural     TiCl4[(C6H5)3PO]2
_chemical_formula_sum            'C36 H30 Cl4 O2 P2 Ti'
_chemical_formula_weight         746.21
_chemical_name_systematic
; 
trans-bis(triphenylphospine oxide)tetrachlorotitanum(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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.100(2)
_cell_angle_beta                 108.657(2)
_cell_angle_gamma                92.652(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4920(13)
_cell_length_b                   9.6398(13)
_cell_length_c                   10.4285(13)
_cell_measurement_temperature    273(2)
_cell_volume                     877.3(2)
_computing_molecular_graphics    'SHELXS-97 (Sheldrick, 1990)'
_computing_publication_material  'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      273(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Siemens SMART CCD'
_diffrn_measurement_method       phi/omega
_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  0.0202
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6070
_diffrn_reflns_theta_full        28.30
_diffrn_reflns_theta_max         28.30
_diffrn_reflns_theta_min         2.12
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.671
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             382
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.264
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4207
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_R_factor_all          0.0846
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0448P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0914
_refine_ls_wR_factor_ref         0.1060
_reflns_number_gt                2709
_reflns_number_total             4207
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            1267-1701.cff
_cod_data_source_block           compound_1
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               8101908
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_Wyckoff_symbol
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.5000 1.0000 1.0000 0.02946(16) Uani 1 1 d d S . .
P1 P 0.26687(7) 0.73122(7) 0.74152(6) 0.03279(16) Uani 1 2 i d . . .
Cl1 Cl 0.32164(7) 1.14132(7) 0.90426(7) 0.04536(19) Uani 1 2 i d . . .
Cl2 Cl 0.36323(7) 0.94943(7) 1.13851(7) 0.04712(19) Uani 1 2 i d . . .
O1 O 0.39086(17) 0.83569(17) 0.85572(16) 0.0399(4) Uani 1 2 i d . . .
C1 C 0.1137(3) 0.6926(3) 0.7980(2) 0.0375(6) Uani 1 2 i d . . .
C2 C 0.0455(3) 0.8051(3) 0.8483(3) 0.0514(7) Uani 1 2 i d . . .
H2 H 0.0826 0.8984 0.8555 0.062 Uiso 1 2 i calc R . .
C3 C -0.0767(3) 0.7801(4) 0.8879(3) 0.0637(9) Uani 1 2 i d . . .
H3 H -0.1220 0.8561 0.9218 0.076 Uiso 1 2 i calc R . .
C4 C -0.1313(4) 0.6423(4) 0.8770(4) 0.0728(10) Uani 1 2 i d . . .
H4 H -0.2145 0.6251 0.9028 0.087 Uiso 1 2 i calc R . .
C5 C -0.0638(4) 0.5293(4) 0.8283(4) 0.0756(10) Uani 1 2 i d . . .
H5 H -0.1012 0.4363 0.8220 0.091 Uiso 1 2 i calc R . .
C6 C 0.0588(3) 0.5532(3) 0.7888(3) 0.0549(8) Uani 1 2 i d . . .
H6 H 0.1045 0.4767 0.7562 0.066 Uiso 1 2 i calc R . .
C7 C 0.3429(3) 0.5698(2) 0.6952(3) 0.0371(6) Uani 1 2 i d . . .
C8 C 0.4429(3) 0.5206(3) 0.8011(3) 0.0525(7) Uani 1 2 i d . . .
H8 H 0.4727 0.5741 0.8927 0.063 Uiso 1 2 i calc R . .
C9 C 0.4976(4) 0.3928(3) 0.7703(4) 0.0658(9) Uani 1 2 i d . . .
H9 H 0.5627 0.3591 0.8415 0.079 Uiso 1 2 i calc R . .
C10 C 0.4572(4) 0.3159(3) 0.6374(4) 0.0729(10) Uani 1 2 i d . . .
H10 H 0.4953 0.2298 0.6178 0.087 Uiso 1 2 i calc R . .
C11 C 0.3605(4) 0.3633(3) 0.5304(4) 0.0765(10) Uani 1 2 i d . . .
H11 H 0.3337 0.3097 0.4390 0.092 Uiso 1 2 i calc R . .
C12 C 0.3035(3) 0.4912(3) 0.5595(3) 0.0546(7) Uani 1 2 i d . . .
H12 H 0.2386 0.5242 0.4876 0.065 Uiso 1 2 i calc R . .
C13 C 0.1974(3) 0.8020(3) 0.5915(2) 0.0376(6) Uani 1 2 i d . . .
C14 C 0.0471(3) 0.7750(3) 0.5092(3) 0.0526(7) Uani 1 2 i d . . .
H14 H -0.0209 0.7245 0.5350 0.063 Uiso 1 2 i calc R . .
C15 C -0.0009(4) 0.8239(3) 0.3882(3) 0.0686(10) Uani 1 2 i d . . .
H15 H -0.1015 0.8061 0.3329 0.082 Uiso 1 2 i calc R . .
C16 C 0.0989(5) 0.8981(4) 0.3496(3) 0.0704(10) Uani 1 2 i d . . .
H16 H 0.0666 0.9278 0.2667 0.084 Uiso 1 2 i calc R . .
C17 C 0.2467(4) 0.9287(4) 0.4331(3) 0.0673(9) Uani 1 2 i d . . .
H17 H 0.3135 0.9817 0.4079 0.081 Uiso 1 2 i calc R . .
C18 C 0.2970(3) 0.8816(3) 0.5539(3) 0.0544(7) Uani 1 2 i d . . .
H18 H 0.3971 0.9029 0.6101 0.065 Uiso 1 2 i calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 '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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 180.00 . 2_677 ?
O1 Ti1 Cl1 90.10(5) . . ?
O1 Ti1 Cl1 89.90(5) 2_677 . ?
O1 Ti1 Cl1 89.90(5) . 2_677 ?
O1 Ti1 Cl1 90.10(5) 2_677 2_677 ?
Cl1 Ti1 Cl1 180.0 . 2_677 ?
O1 Ti1 Cl2 90.06(5) . 2_677 ?
O1 Ti1 Cl2 89.94(5) 2_677 2_677 ?
Cl1 Ti1 Cl2 89.88(2) . 2_677 ?
Cl1 Ti1 Cl2 90.12(2) 2_677 2_677 ?
O1 Ti1 Cl2 89.94(5) . . ?
O1 Ti1 Cl2 90.06(5) 2_677 . ?
Cl1 Ti1 Cl2 90.12(2) . . ?
Cl1 Ti1 Cl2 89.88(2) 2_677 . ?
Cl2 Ti1 Cl2 180.0 2_677 . ?
O1 P1 C13 110.71(11) . . ?
O1 P1 C7 108.14(11) . . ?
C13 P1 C7 108.97(12) . . ?
O1 P1 C1 111.54(11) . . ?
C13 P1 C1 108.17(12) . . ?
C7 P1 C1 109.28(12) . . ?
P1 O1 Ti1 163.24(11) . . ?
C6 C1 C2 119.5(2) . . ?
C6 C1 P1 122.0(2) . . ?
C2 C1 P1 118.6(2) . . ?
C3 C2 C1 120.6(3) . . ?
C2 C3 C4 119.6(3) . . ?
C3 C4 C5 120.5(3) . . ?
C6 C5 C4 120.4(3) . . ?
C5 C6 C1 119.5(3) . . ?
C12 C7 C8 119.2(2) . . ?
C12 C7 P1 122.5(2) . . ?
C8 C7 P1 118.3(2) . . ?
C9 C8 C7 120.0(3) . . ?
C10 C9 C8 120.4(3) . . ?
C9 C10 C11 120.9(3) . . ?
C10 C11 C12 119.6(3) . . ?
C7 C12 C11 120.0(3) . . ?
C18 C13 C14 119.5(2) . . ?
C18 C13 P1 119.13(19) . . ?
C14 C13 P1 121.3(2) . . ?
C15 C14 C13 119.6(3) . . ?
C16 C15 C14 120.4(3) . . ?
C15 C16 C17 120.1(3) . . ?
C18 C17 C16 120.6(3) . . ?
C17 C18 C13 119.8(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.9229(15) . ?
Ti1 O1 1.9229(15) 2_677 ?
Ti1 Cl1 2.3283(6) . ?
Ti1 Cl1 2.3283(6) 2_677 ?
Ti1 Cl2 2.3336(6) 2_677 ?
Ti1 Cl2 2.3336(6) . ?
P1 O1 1.5193(16) . ?
P1 C1 1.785(2) . ?
P1 C7 1.785(2) . ?
P1 C13 1.783(2) . ?
C1 C2 1.384(4) . ?
C1 C6 1.391(3) . ?
C2 C3 1.377(4) . ?
C3 C4 1.371(4) . ?
C4 C5 1.377(5) . ?
C5 C6 1.379(4) . ?
C7 C8 1.392(3) . ?
C7 C12 1.379(4) . ?
C8 C9 1.375(4) . ?
C9 C10 1.349(5) . ?
C10 C11 1.376(5) . ?
C11 C12 1.384(4) . ?
C13 C14 1.389(3) . ?
C13 C18 1.390(4) . ?
C14 C15 1.386(4) . ?
C15 C16 1.368(5) . ?
C16 C17 1.374(5) . ?
C17 C18 1.377(4) . ?
