#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/30/4323078.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_4323078
loop_
_publ_author_name
'Peihua Yu'
'Thomas Pape'
'Isabel Usón'
'Musa A. Said'
'Herbert W. Roesky'
'Mavis L. Montero'
'Hans-Georg Schmidt'
'Alojz Demsar'
_publ_contact_author
;
       Herbert W. Roesky
       Institut für Anorganische Chemie
       Universität Göttingen
       Tammannstr. 4
       37077 Göttingen
       Germany
;
_publ_contact_author_fax         '49 551 39 3373'
_publ_contact_author_phone       '49 551 39 3001'
_publ_section_title
;
 Reactions of Organotitanoxane Fluorides with AlR3 (R = Me, Et, CH2Ph) and
 Me3SiCl: X-ray Crystal Structures of [C5Me5Ti(μ-O)]4F[(μ-F)AlMe3]3,
 [C5Me5Ti(μ-O)]4F3[(μ-F)Al(CH2Ph)3], [C5Me5Ti(μ-O)Et]4, and
 (C5Me5)4Ti4O5X2 (X = Cl and F)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5117
_journal_page_last               5124
_journal_paper_doi               10.1021/ic980450g
_journal_volume                  37
_journal_year                    1998
_chemical_formula_sum            'C42 H64 Cl2 O5.5 Ti4'
_chemical_formula_weight         919.43
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 98.87(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.404(4)
_cell_length_b                   16.524(3)
_cell_length_c                   14.893(3)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     4474.9(16)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Siemens/STOE AED2'
_diffrn_measurement_method       '2thetaω scans'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0118
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            4304
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         3.58
_diffrn_standards_decay_%        <3%
_diffrn_standards_interval_count 180
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.849
_exptl_absorpt_correction_T_max  0.7848
_exptl_absorpt_correction_T_min  0.5154
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plates
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.538
_refine_diff_density_min         -0.978
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     389
_refine_ls_number_reflns         4096
_refine_ls_number_restraints     385
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0415
_refine_ls_R_factor_gt           0.0396
_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/[σ²(Fo²)+(0.0741P)²+4.6215P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1086
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                3858
_reflns_number_total             4096
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic980450g_1.cif
_cod_data_source_block           1a
_cod_original_cell_volume        4475.1(16)
_cod_original_formula_sum        'C42 H64 Cl2 O5.50 Ti4'
_cod_database_code               4323078
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.31725(2) 0.0000 0.33404(3) 0.01860(14) Uani 1 2 d S . .
Ti2 Ti 0.14190(2) 0.0000 0.33206(3) 0.02111(15) Uani 1 2 d S . .
Ti3 Ti 0.219324(18) 0.15496(2) 0.24442(2) 0.02416(13) Uani 1 1 d . . .
O1 O 0.23655(10) 0.0000 0.39310(12) 0.0222(4) Uani 1 2 d S . .
O2 O 0.14258(7) 0.08922(9) 0.25632(10) 0.0285(3) Uani 1 1 d . A .
O3 O 0.29907(7) 0.08930(8) 0.25794(9) 0.0261(3) Uani 1 1 d . A .
Cl1 Cl 0.23497(3) 0.22855(3) 0.37586(4) 0.03966(17) Uani 1 1 d . A .
C11 C 0.39278(10) 0.04298(14) 0.46967(14) 0.0311(4) Uani 1 1 d . . .
C11* C 0.36246(14) 0.0959(2) 0.53674(18) 0.0580(8) Uani 1 1 d . . .
H11A H 0.3982 0.0996 0.5927 0.087 Uiso 1 1 calc R . .
H11B H 0.3165 0.0726 0.5506 0.087 Uiso 1 1 calc R . .
H11C H 0.3529 0.1501 0.5108 0.087 Uiso 1 1 calc R . .
C12 C 0.42665(10) 0.06901(12) 0.39608(15) 0.0302(4) Uani 1 1 d . . .
C12* C 0.43950(15) 0.15560(15) 0.3723(2) 0.0556(8) Uani 1 1 d . . .
H12A H 0.4848 0.1752 0.4092 0.083 Uiso 1 1 calc R . .
H12B H 0.3979 0.1887 0.3844 0.083 Uiso 1 1 calc R . .
H12C H 0.4441 0.1594 0.3077 0.083 Uiso 1 1 calc R . .
C13 C 0.44720(14) 0.0000 0.3502(2) 0.0299(6) Uani 1 2 d S . .
C13* C 0.4828(2) 0.0000 0.2663(3) 0.0567(11) Uani 1 2 d S . .
H13A H 0.5327 0.0219 0.2807 0.085 Uiso 0.50 1 calc PR . .
H13B H 0.4540 0.0336 0.2195 0.085 Uiso 0.50 1 calc PR . .
H13C H 0.4851 -0.0555 0.2437 0.085 Uiso 0.50 1 calc PR . .
C21 C 0.01510(15) 0.0000 0.3440(2) 0.0348(7) Uani 1 2 d S . .
C21* C -0.0394(2) 0.0000 0.2583(3) 0.0606(11) Uani 1 2 d S . .
H21A H -0.0859 0.0233 0.2703 0.091 Uiso 0.50 1 calc PR . .
H21B H -0.0477 -0.0557 0.2364 0.091 Uiso 0.50 1 calc PR . .
H21C H -0.0202 0.0324 0.2121 0.091 Uiso 0.50 1 calc PR . .
C22 C 0.04642(11) 0.06903(13) 0.39096(17) 0.0356(5) Uani 1 1 d . . .
C22* C 0.02825(17) 0.15545(15) 0.3674(3) 0.0636(9) Uani 1 1 d . . .
H22A H 0.0069 0.1593 0.3031 0.095 Uiso 1 1 calc R . .
H22B H 0.0732 0.1881 0.3787 0.095 Uiso 1 1 calc R . .
H22C H -0.0072 0.1755 0.4050 0.095 Uiso 1 1 calc R . .
C23 C 0.09724(12) 0.04311(15) 0.46570(16) 0.0378(5) Uani 1 1 d . . .
C23* C 0.14311(16) 0.0956(2) 0.5343(2) 0.0659(9) Uani 1 1 d . . .
H23A H 0.1198 0.0996 0.5890 0.099 Uiso 1 1 calc R . .
H23B H 0.1473 0.1498 0.5087 0.099 Uiso 1 1 calc R . .
H23C H 0.1922 0.0719 0.5500 0.099 Uiso 1 1 calc R . .
C31 C 0.1689(5) 0.1710(6) 0.0912(10) 0.0417(17) Uani 0.60 1 d PDU A 1
C31* C 0.1250(5) 0.1033(4) 0.0408(4) 0.093(3) Uani 0.60 1 d PDU A 1
H31A H 0.1573 0.0707 0.0085 0.140 Uiso 0.60 1 calc PR A 1
H31B H 0.0851 0.1262 -0.0031 0.140 Uiso 0.60 1 calc PR A 1
H31C H 0.1042 0.0690 0.0841 0.140 Uiso 0.60 1 calc PR A 1
C32 C 0.2455(5) 0.1847(7) 0.0985(8) 0.0444(19) Uani 0.60 1 d PDU A 1
C32* C 0.2996(5) 0.1333(5) 0.0580(5) 0.097(3) Uani 0.60 1 d PDU A 1
H32A H 0.3359 0.1110 0.1068 0.145 Uiso 0.60 1 calc PR A 1
H32B H 0.3247 0.1665 0.0177 0.145 Uiso 0.60 1 calc PR A 1
H32C H 0.2736 0.0889 0.0232 0.145 Uiso 0.60 1 calc PR A 1
C33 C 0.2627(4) 0.2560(6) 0.1511(6) 0.0427(16) Uani 0.60 1 d PDU A 1
C33* C 0.3367(4) 0.2948(6) 0.1778(5) 0.103(3) Uani 0.60 1 d PDU A 1
H33A H 0.3364 0.3489 0.1507 0.154 Uiso 0.60 1 calc PR A 1
H33B H 0.3745 0.2616 0.1560 0.154 Uiso 0.60 1 calc PR A 1
H33C H 0.3475 0.2993 0.2442 0.154 Uiso 0.60 1 calc PR A 1
C34 C 0.1958(5) 0.2870(4) 0.1716(5) 0.0402(14) Uani 0.60 1 d PDU A 1
C34* C 0.1872(6) 0.3655(3) 0.2211(4) 0.087(2) Uani 0.60 1 d PDU A 1
H34A H 0.1776 0.4096 0.1770 0.130 Uiso 0.60 1 calc PR A 1
H34B H 0.2326 0.3769 0.2631 0.130 Uiso 0.60 1 calc PR A 1
H34C H 0.1461 0.3608 0.2555 0.130 Uiso 0.60 1 calc PR A 1
C35 C 0.1392(3) 0.2345(6) 0.1356(7) 0.0404(14) Uani 0.60 1 d PDU A 1
C35* C 0.0584(3) 0.2433(5) 0.1441(5) 0.084(2) Uani 0.60 1 d PDU A 1
H35A H 0.0534 0.2791 0.1952 0.126 Uiso 0.60 1 calc PR A 1
H35B H 0.0379 0.1900 0.1546 0.126 Uiso 0.60 1 calc PR A 1
H35C H 0.0318 0.2665 0.0879 0.126 Uiso 0.60 1 calc PR A 1
C31' C 0.1531(5) 0.1910(10) 0.1017(14) 0.042(3) Uani 0.40 1 d PDU A 2
C41 C 0.0835(5) 0.1447(7) 0.0670(7) 0.083(3) Uani 0.40 1 d PDU A 2
H41A H 0.0949 0.1008 0.0271 0.125 Uiso 0.40 1 calc PR A 2
H41B H 0.0475 0.1814 0.0330 0.125 Uiso 0.40 1 calc PR A 2
H41C H 0.0632 0.1219 0.1185 0.125 Uiso 0.40 1 calc PR A 2
C32' C 0.2238(7) 0.1667(9) 0.0884(15) 0.037(2) Uani 0.40 1 d PDU A 2
C42 C 0.2466(7) 0.0958(5) 0.0361(6) 0.073(3) Uani 0.40 1 d PDU A 2
H42A H 0.2053 0.0579 0.0228 0.110 Uiso 0.40 1 calc PR A 2
H42B H 0.2884 0.0683 0.0723 0.110 Uiso 0.40 1 calc PR A 2
H42C H 0.2609 0.1148 -0.0210 0.110 Uiso 0.40 1 calc PR A 2
C33' C 0.2740(5) 0.2263(8) 0.1298(9) 0.0361(19) Uani 0.40 1 d PDU A 2
C43 C 0.3553(4) 0.2276(7) 0.1317(6) 0.073(3) Uani 0.40 1 d PDU A 2
H43A H 0.3665 0.2514 0.0751 0.109 Uiso 0.40 1 calc PR A 2
H43B H 0.3744 0.1722 0.1377 0.109 Uiso 0.40 1 calc PR A 2
H43C H 0.3783 0.2601 0.1834 0.109 Uiso 0.40 1 calc PR A 2
C34' C 0.2334(8) 0.2834(5) 0.1715(7) 0.044(2) Uani 0.40 1 d PDU A 2
C44 C 0.2622(9) 0.3601(5) 0.2198(6) 0.095(4) Uani 0.40 1 d PDU A 2
H44A H 0.2535 0.4060 0.1778 0.143 Uiso 0.40 1 calc PR A 2
H44B H 0.3152 0.3546 0.2409 0.143 Uiso 0.40 1 calc PR A 2
H44C H 0.2368 0.3694 0.2720 0.143 Uiso 0.40 1 calc PR A 2
C35' C 0.1587(7) 0.2607(8) 0.1550(9) 0.047(3) Uani 0.40 1 d PDU A 2
C45 C 0.0957(6) 0.3035(7) 0.1891(7) 0.094(4) Uani 0.40 1 d PDU A 2
H45A H 0.1103 0.3591 0.2062 0.140 Uiso 0.40 1 calc PR A 2
H45B H 0.0831 0.2748 0.2421 0.140 Uiso 0.40 1 calc PR A 2
H45C H 0.0529 0.3044 0.1409 0.140 Uiso 0.40 1 calc PR A 2
C51 C 0.4562(9) 0.0700(10) -0.0235(10) 0.106(8) Uani 0.25 1 d PRDU A -1
H51A H 0.4322 0.1081 -0.0702 0.127 Uiso 0.25 1 calc PR A -1
H51B H 0.4409 0.0841 0.0354 0.127 Uiso 0.25 1 calc PR A -1
C52 C 0.5313(15) 0.0753(13) -0.0170(17) 0.077(5) Uani 0.25 1 d PDU A -1
H52A H 0.5513 0.1149 0.0304 0.092 Uiso 0.25 1 calc PR A -1
H52B H 0.5452 0.0925 -0.0757 0.092 Uiso 0.25 1 calc PR A -1
O53 O 0.5616(12) -0.0131(16) 0.0094(15) 0.128(8) Uani 0.25 1 d PDU A -1
C54 C 0.489(2) -0.0639(13) -0.003(4) 0.094(7) Uani 0.25 1 d PDU A -1
H54A H 0.4936 -0.1126 -0.0403 0.112 Uiso 0.25 1 calc PR A -1
H54B H 0.4766 -0.0808 0.0566 0.112 Uiso 0.25 1 calc PR A -1
C55 C 0.4353(15) -0.0103(16) -0.048(2) 0.105(7) Uani 0.25 1 d PDU A -1
H55A H 0.4311 -0.0173 -0.1143 0.126 Uiso 0.25 1 calc PR A -1
H55B H 0.3868 -0.0224 -0.0297 0.126 Uiso 0.25 1 calc PR A -1
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'
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 O3 102.06(6) . . ?
O1 Ti1 O3 102.06(6) . 6 ?
O3 Ti1 O3 105.06(9) . 6 ?
O1 Ti1 C13 146.04(9) . . ?
O3 Ti1 C13 98.39(6) . . ?
O3 Ti1 C13 98.39(6) 6 . ?
O1 Ti1 C12 120.86(7) . . ?
O3 Ti1 C12 85.30(7) . . ?
O3 Ti1 C12 132.90(7) 6 . ?
C13 Ti1 C12 34.63(7) . . ?
O1 Ti1 C12 120.85(7) . 6 ?
O3 Ti1 C12 132.90(7) . 6 ?
O3 Ti1 C12 85.30(7) 6 6 ?
C13 Ti1 C12 34.63(7) . 6 ?
C12 Ti1 C12 57.43(10) . 6 ?
O1 Ti1 C11 90.18(8) . . ?
O3 Ti1 C11 107.91(7) . . ?
O3 Ti1 C11 141.42(7) 6 . ?
C13 Ti1 C11 57.61(9) . . ?
C12 Ti1 C11 34.50(8) . . ?
C12 Ti1 C11 57.52(7) 6 . ?
O1 Ti1 C11 90.18(8) . 6 ?
O3 Ti1 C11 141.42(7) . 6 ?
O3 Ti1 C11 107.91(7) 6 6 ?
C13 Ti1 C11 57.61(9) . 6 ?
C12 Ti1 C11 57.52(7) . 6 ?
C12 Ti1 C11 34.50(8) 6 6 ?
C11 Ti1 C11 34.77(11) . 6 ?
O1 Ti1 Ti2 28.72(6) . . ?
O3 Ti1 Ti2 84.76(5) . . ?
O3 Ti1 Ti2 84.76(5) 6 . ?
C13 Ti1 Ti2 174.76(8) . . ?
C12 Ti1 Ti2 142.34(5) . . ?
C12 Ti1 Ti2 142.34(5) 6 . ?
C11 Ti1 Ti2 117.47(6) . . ?
C11 Ti1 Ti2 117.47(6) 6 . ?
O1 Ti1 Ti3 76.23(4) . . ?
O3 Ti1 Ti3 25.85(4) . . ?
O3 Ti1 Ti3 109.53(5) 6 . ?
C13 Ti1 Ti3 121.50(3) . . ?
C12 Ti1 Ti3 99.35(5) . . ?
C12 Ti1 Ti3 155.47(5) 6 . ?
C11 Ti1 Ti3 108.90(6) . . ?
C11 Ti1 Ti3 142.04(6) 6 . ?
Ti2 Ti1 Ti3 60.766(16) . . ?
O1 Ti1 Ti3 76.23(4) . 6 ?
O3 Ti1 Ti3 109.53(5) . 6 ?
O3 Ti1 Ti3 25.85(4) 6 6 ?
C13 Ti1 Ti3 121.50(3) . 6 ?
C12 Ti1 Ti3 155.46(5) . 6 ?
C12 Ti1 Ti3 99.35(5) 6 6 ?
C11 Ti1 Ti3 142.04(6) . 6 ?
C11 Ti1 Ti3 108.90(6) 6 6 ?
Ti2 Ti1 Ti3 60.767(16) . 6 ?
Ti3 Ti1 Ti3 102.08(3) . 6 ?
O1 Ti2 O2 101.88(6) . . ?
O1 Ti2 O2 101.88(6) . 6 ?
O2 Ti2 O2 105.06(9) . 6 ?
O1 Ti2 C21 146.45(10) . . ?
O2 Ti2 C21 98.32(7) . . ?
O2 Ti2 C21 98.32(7) 6 . ?
O1 Ti2 C22 121.12(8) . . ?
O2 Ti2 C22 85.28(7) . . ?
O2 Ti2 C22 132.88(7) 6 . ?
C21 Ti2 C22 34.69(7) . . ?
O1 Ti2 C22 121.12(8) . 6 ?
O2 Ti2 C22 132.88(7) . 6 ?
O2 Ti2 C22 85.28(7) 6 6 ?
C21 Ti2 C22 34.69(7) . 6 ?
C22 Ti2 C22 57.44(10) . 6 ?
O1 Ti2 C23 90.55(8) . . ?
O2 Ti2 C23 107.83(8) . . ?
O2 Ti2 C23 141.44(7) 6 . ?
C21 Ti2 C23 57.64(10) . . ?
C22 Ti2 C23 34.43(9) . . ?
C22 Ti2 C23 57.54(8) 6 . ?
O1 Ti2 C23 90.55(8) . 6 ?
O2 Ti2 C23 141.44(7) . 6 ?
O2 Ti2 C23 107.83(8) 6 6 ?
C21 Ti2 C23 57.64(10) . 6 ?
C22 Ti2 C23 57.54(8) . 6 ?
C22 Ti2 C23 34.43(9) 6 6 ?
C23 Ti2 C23 34.88(12) . 6 ?
O1 Ti2 Ti1 28.76(6) . . ?
O2 Ti2 Ti1 84.55(5) . . ?
O2 Ti2 Ti1 84.55(5) 6 . ?
C21 Ti2 Ti1 175.22(9) . . ?
C22 Ti2 Ti1 142.56(6) . . ?
C22 Ti2 Ti1 142.56(6) 6 . ?
C23 Ti2 Ti1 117.87(6) . . ?
C23 Ti2 Ti1 117.87(6) 6 . ?
O1 Ti2 Ti3 76.17(4) . . ?
O2 Ti2 Ti3 25.73(4) . . ?
O2 Ti2 Ti3 109.41(5) 6 . ?
C21 Ti2 Ti3 121.41(4) . . ?
C22 Ti2 Ti3 99.38(5) . . ?
C22 Ti2 Ti3 155.45(5) 6 . ?
C23 Ti2 Ti3 108.98(6) . . ?
C23 Ti2 Ti3 142.27(6) 6 . ?
Ti1 Ti2 Ti3 60.671(15) . . ?
O1 Ti2 Ti3 76.18(4) . 6 ?
O2 Ti2 Ti3 109.41(5) . 6 ?
O2 Ti2 Ti3 25.73(4) 6 6 ?
C21 Ti2 Ti3 121.41(4) . 6 ?
C22 Ti2 Ti3 155.44(5) . 6 ?
C22 Ti2 Ti3 99.38(5) 6 6 ?
C23 Ti2 Ti3 142.27(6) . 6 ?
C23 Ti2 Ti3 108.98(6) 6 6 ?
Ti1 Ti2 Ti3 60.672(16) . 6 ?
Ti3 Ti2 Ti3 101.95(3) . 6 ?
O3 Ti3 O2 105.10(7) . . ?
O3 Ti3 Cl1 103.34(5) . . ?
O2 Ti3 Cl1 103.44(5) . . ?
O3 Ti3 C31 111.6(2) . . ?
O2 Ti3 C31 88.0(3) . . ?
Cl1 Ti3 C31 138.9(2) . . ?
O3 Ti3 C32' 90.5(4) . . ?
O2 Ti3 C32' 107.1(3) . . ?
Cl1 Ti3 C32' 141.8(3) . . ?
C31 Ti3 C32' 25.1(4) . . ?
O3 Ti3 C32 87.1(2) . . ?
O2 Ti3 C32 119.3(3) . . ?
Cl1 Ti3 C32 131.7(3) . . ?
C31 Ti3 C32 35.1(3) . . ?
C32' Ti3 C32 12.3(3) . . ?
O3 Ti3 C31' 123.3(3) . . ?
O2 Ti3 C31' 86.4(3) . . ?
Cl1 Ti3 C31' 128.1(4) . . ?
C31 Ti3 C31' 11.8(3) . . ?
C32' Ti3 C31' 34.7(4) . . ?
C32 Ti3 C31' 42.6(4) . . ?
O3 Ti3 C35' 143.9(3) . . ?
O2 Ti3 C35' 101.0(4) . . ?
Cl1 Ti3 C35' 94.3(3) . . ?
C31 Ti3 C35' 44.5(3) . . ?
C32' Ti3 C35' 57.8(4) . . ?
C32 Ti3 C35' 58.1(3) . . ?
C31' Ti3 C35' 34.3(3) . . ?
O3 Ti3 C33 98.4(2) . . ?
O2 Ti3 C33 144.29(16) . . ?
Cl1 Ti3 C33 96.7(2) . . ?
C31 Ti3 C33 58.1(3) . . ?
C32' Ti3 C33 45.5(3) . . ?
C32 Ti3 C33 35.0(2) . . ?
C31' Ti3 C33 58.1(4) . . ?
C35' Ti3 C33 47.8(3) . . ?
O3 Ti3 C35 143.5(2) . . ?
O2 Ti3 C35 89.27(18) . . ?
Cl1 Ti3 C35 105.7(2) . . ?
C31 Ti3 C35 34.1(2) . . ?
C32' Ti3 C35 53.0(4) . . ?
C32 Ti3 C35 56.9(3) . . ?
C31' Ti3 C35 22.6(3) . . ?
C35' Ti3 C35 14.6(3) . . ?
C33 Ti3 C35 56.7(2) . . ?
O3 Ti3 C34' 115.8(4) . . ?
O2 Ti3 C34' 135.2(4) . . ?
Cl1 Ti3 C34' 84.8(2) . . ?
C31 Ti3 C34' 61.1(3) . . ?
C32' Ti3 C34' 57.3(4) . . ?
C32 Ti3 C34' 49.4(3) . . ?
C31' Ti3 C34' 56.6(4) . . ?
C35' Ti3 C34' 34.2(3) . . ?
C33 Ti3 C34' 19.1(3) . . ?
C35 Ti3 C34' 46.7(3) . . ?
O3 Ti3 C33' 87.2(3) . . ?
O2 Ti3 C33' 141.0(3) . . ?
Cl1 Ti3 C33' 109.5(3) . . ?
C31 Ti3 C33' 53.3(3) . . ?
C32' Ti3 C33' 34.7(3) . . ?
C32 Ti3 C33' 22.8(3) . . ?
C31' Ti3 C33' 56.9(4) . . ?
C35' Ti3 C33' 57.0(3) . . ?
C33 Ti3 C33' 15.21(19) . . ?
C35 Ti3 C33' 62.4(3) . . ?
C34' Ti3 C33' 33.8(3) . . ?
Ti2 O1 Ti1 122.52(10) . . ?
Ti3 O2 Ti2 127.84(8) . . ?
Ti3 O3 Ti1 127.57(7) . . ?
C12 C11 C11 107.78(12) . 6 ?
C12 C11 C11* 126.5(2) . . ?
C11 C11 C11* 125.70(17) 6 . ?
C12 C11 Ti1 72.61(11) . . ?
C11 C11 Ti1 72.62(6) 6 . ?
C11* C11 Ti1 120.78(14) . . ?
C11 C12 C13 108.29(19) . . ?
C11 C12 C12* 125.4(2) . . ?
C13 C12 C12* 126.3(2) . . ?
C11 C12 Ti1 72.88(11) . . ?
C13 C12 Ti1 72.41(13) . . ?
C12* C12 Ti1 121.39(15) . . ?
C12 C13 C12 107.9(3) . 6 ?
C12 C13 C13* 126.07(13) . . ?
C12 C13 C13* 126.07(13) 6 . ?
C12 C13 Ti1 72.96(13) . . ?
C12 C13 Ti1 72.96(13) 6 . ?
C13* C13 Ti1 118.7(2) . . ?
C22 C21 C22 107.6(3) . 6 ?
C22 C21 C21* 126.18(15) . . ?
C22 C21 C21* 126.17(15) 6 . ?
C22 C21 Ti2 72.88(13) . . ?
C22 C21 Ti2 72.88(13) 6 . ?
C21* C21 Ti2 118.3(2) . . ?
C23 C22 C21 108.5(2) . . ?
C23 C22 C22* 125.0(2) . . ?
C21 C22 C22* 126.5(3) . . ?
C23 C22 Ti2 72.91(11) . . ?
C21 C22 Ti2 72.43(13) . . ?
C22* C22 Ti2 121.57(16) . . ?
C22 C23 C23 107.73(13) . 6 ?
C22 C23 C23* 126.9(3) . . ?
C23 C23 C23* 125.40(19) 6 . ?
C22 C23 Ti2 72.66(12) . . ?
C23 C23 Ti2 72.56(6) 6 . ?
C23* C23 Ti2 120.90(15) . . ?
C35 C31 C32 107.6(6) . . ?
C35 C31 C31* 125.0(9) . . ?
C32 C31 C31* 127.3(9) . . ?
C35 C31 Ti3 75.5(7) . . ?
C32 C31 Ti3 72.8(7) . . ?
C31* C31 Ti3 120.1(8) . . ?
C31 C32 C33 108.0(5) . . ?
C31 C32 C32* 126.4(9) . . ?
C33 C32 C32* 125.6(9) . . ?
C31 C32 Ti3 72.2(7) . . ?
C33 C32 Ti3 73.9(5) . . ?
C32* C32 Ti3 119.7(7) . . ?
C34 C33 C32 106.9(5) . . ?
C34 C33 C33* 125.1(10) . . ?
C32 C33 C33* 128.0(9) . . ?
C34 C33 Ti3 75.3(4) . . ?
C32 C33 Ti3 71.1(5) . . ?
C33* C33 Ti3 121.0(5) . . ?
C35 C34 C33 108.4(6) . . ?
C35 C34 C34* 126.3(9) . . ?
C33 C34 C34* 125.2(9) . . ?
C35 C34 Ti3 71.8(5) . . ?
C33 C34 Ti3 70.8(4) . . ?
C34* C34 Ti3 125.0(4) . . ?
C31 C35 C34 109.0(6) . . ?
C31 C35 C35* 124.9(8) . . ?
C34 C35 C35* 126.1(9) . . ?
C31 C35 Ti3 70.4(7) . . ?
C34 C35 Ti3 74.8(5) . . ?
C35* C35 Ti3 120.2(6) . . ?
C35' C31' C32' 109.2(8) . . ?
C35' C31' C41 126.6(13) . . ?
C32' C31' C41 124.1(12) . . ?
C35' C31' Ti3 73.3(9) . . ?
C32' C31' Ti3 72.2(11) . . ?
C41 C31' Ti3 118.2(12) . . ?
C31' C32' C33' 107.2(8) . . ?
C31' C32' C42 129.4(11) . . ?
C33' C32' C42 123.3(12) . . ?
C31' C32' Ti3 73.1(11) . . ?
C33' C32' Ti3 75.4(10) . . ?
C42 C32' Ti3 120.3(13) . . ?
C34' C33' C32' 107.5(8) . . ?
C34' C33' C43 125.6(12) . . ?
C32' C33' C43 126.9(12) . . ?
C34' C33' Ti3 73.0(6) . . ?
C32' C33' Ti3 69.8(10) . . ?
C43 C33' Ti3 121.3(8) . . ?
C33' C34' C35' 108.4(7) . . ?
C33' C34' C44 126.9(14) . . ?
C35' C34' C44 124.6(14) . . ?
C33' C34' Ti3 73.2(7) . . ?
C35' C34' Ti3 71.0(6) . . ?
C44 C34' Ti3 125.2(6) . . ?
C31' C35' C34' 107.6(7) . . ?
C31' C35' C45 125.8(14) . . ?
C34' C35' C45 126.5(14) . . ?
C31' C35' Ti3 72.4(9) . . ?
C34' C35' Ti3 74.7(6) . . ?
C45 C35' Ti3 118.4(8) . . ?
C52 C51 C55 108.0(14) . . ?
C51 C52 O53 105.6(12) . . ?
C54 O53 C52 101.7(19) . . ?
C55 C54 O53 104.0(14) . . ?
C51 C55 C54 108.9(18) . . ?
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 1.8392(18) . ?
Ti1 O3 1.8593(14) . ?
Ti1 O3 1.8593(14) 6 ?
Ti1 C13 2.367(3) . ?
Ti1 C12 2.374(2) . ?
Ti1 C12 2.374(2) 6 ?
Ti1 C11 2.377(2) . ?
Ti1 C11 2.377(2) 6 ?
Ti1 Ti2 3.2227(9) . ?
Ti1 Ti3 3.2930(7) . ?
Ti1 Ti3 3.2931(7) 6 ?
Ti2 O1 1.8363(19) . ?
Ti2 O2 1.8576(14) . ?
Ti2 O2 1.8576(14) 6 ?
Ti2 C21 2.368(3) . ?
Ti2 C22 2.374(2) . ?
Ti2 C22 2.374(2) 6 ?
Ti2 C23 2.377(2) . ?
Ti2 C23 2.377(2) 6 ?
Ti2 Ti3 3.2961(7) . ?
Ti2 Ti3 3.2961(7) 6 ?
Ti3 O3 1.8113(14) . ?
Ti3 O2 1.8120(14) . ?
Ti3 Cl1 2.2847(7) . ?
Ti3 C31 2.342(14) . ?
Ti3 C32' 2.35(2) . ?
Ti3 C32 2.349(12) . ?
Ti3 C31' 2.36(2) . ?
Ti3 C35' 2.369(12) . ?
Ti3 C33 2.387(7) . ?
Ti3 C35 2.406(9) . ?
Ti3 C34' 2.416(9) . ?
Ti3 C33' 2.418(12) . ?
C11 C12 1.409(3) . ?
C11 C11 1.420(5) 6 ?
C11 C11* 1.499(3) . ?
C12 C13 1.411(3) . ?
C12 C12* 1.501(3) . ?
C13 C12 1.411(3) 6 ?
C13 C13* 1.498(4) . ?
C21 C22 1.413(3) . ?
C21 C22 1.413(3) 6 ?
C21 C21* 1.497(5) . ?
C22 C23 1.406(4) . ?
C22 C22* 1.496(3) . ?
C23 C23 1.425(5) 6 ?
C23 C23* 1.498(4) . ?
C31 C35 1.395(8) . ?
C31 C32 1.414(9) . ?
C31 C31* 1.511(8) . ?
C32 C33 1.424(9) . ?
C32 C32* 1.504(7) . ?
C33 C34 1.410(9) . ?
C33 C33* 1.503(7) . ?
C34 C35 1.397(8) . ?
C34 C34* 1.512(7) . ?
C35 C35* 1.519(7) . ?
C31' C35' 1.393(12) . ?
C31' C32' 1.404(12) . ?
C31' C41 1.513(10) . ?
C32' C33' 1.424(10) . ?
C32' C42 1.503(10) . ?
C33' C34' 1.407(11) . ?
C33' C43 1.492(9) . ?
C34' C35' 1.409(12) . ?
C34' C44 1.513(10) . ?
C35' C45 1.510(10) . ?
C51 C52 1.37(2) . ?
C51 C55 1.41(2) . ?
C52 O53 1.59(3) . ?
O53 C54 1.56(3) . ?
C54 C55 1.41(3) . ?
