#------------------------------------------------------------------------------
#$Date: 2017-07-25 07:47:51 +0300 (Tue, 25 Jul 2017) $
#$Revision: 199031 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/38/7043807.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_7043807
loop_
_publ_author_name
'Gao, Mei-Yan'
'Chen, Shumei'
'Hu, Lan-Xia'
'Zhang, Lei'
'Zhang, Jian'
_publ_section_title
;
 Synthesis and photocatalytic H2 evolution properties of four
 titanium-oxo-clusters based on a cyclohex-3-ene-1-carboxylate ligand.
;
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_paper_doi               10.1039/c7dt00627f
_journal_year                    2017
_chemical_formula_sum            'C32 H60 O12 Ti3'
_chemical_formula_weight         780.50
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-03-18 deposited with the CCDC.
2017-03-27 downloaded from the CCDC.
;
_cell_angle_alpha                96.961(3)
_cell_angle_beta                 108.693(4)
_cell_angle_gamma                109.373(4)
_cell_formula_units_Z            2
_cell_length_a                   11.3849(6)
_cell_length_b                   13.5963(5)
_cell_length_c                   15.4306(7)
_cell_measurement_reflns_used    5170
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      73.9490
_cell_measurement_theta_min      4.4350
_cell_volume                     2064.10(19)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0253
_diffrn_reflns_av_unetI/netI     0.0431
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14218
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         74.468
_diffrn_reflns_theta_min         3.563
_exptl_absorpt_coefficient_mu    5.258
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.56408
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_exptl_transmission_factor_max   0.207
_exptl_transmission_factor_min   0.141
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.343
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     441
_refine_ls_number_reflns         8159
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0755
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1086P)²+0.3512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1728
_refine_ls_wR_factor_ref         0.2052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6242
_reflns_number_total             8159
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7dt00627f2.cif
_cod_data_source_block           PTC91
_cod_original_cell_volume        2064.10(18)
_cod_database_code               7043807
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.56408
_shelx_estimated_absorpt_t_max   1.00000
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.69072(7) 0.83650(5) 0.23061(5) 0.0765(2) Uani 1 1 d . . . . .
Ti2 Ti 0.83204(7) 1.04268(4) 0.39403(4) 0.06776(19) Uani 1 1 d . . . . .
Ti3 Ti 0.82715(6) 0.82177(4) 0.43397(4) 0.06625(19) Uani 1 1 d . . . . .
O4 O 0.7776(3) 0.94398(18) 0.47421(17) 0.0720(6) Uani 1 1 d . . . . .
O5 O 0.8496(2) 0.91112(16) 0.34516(15) 0.0628(5) Uani 1 1 d . . . . .
O6 O 0.7506(3) 0.72552(18) 0.49117(19) 0.0808(7) Uani 1 1 d . . . . .
O7 O 0.8866(3) 1.0951(2) 0.2871(2) 0.0836(7) Uani 1 1 d . . . . .
O8 O 0.8763(3) 0.72050(19) 0.35397(19) 0.0786(6) Uani 1 1 d . . . . .
O9 O 0.7958(3) 0.7426(2) 0.20811(19) 0.0854(7) Uani 1 1 d . . . . .
O10 O 1.0033(3) 1.12177(17) 0.47825(17) 0.0734(6) Uani 1 1 d . . . . .
O2 O 0.6348(3) 0.74798(19) 0.30969(19) 0.0797(7) Uani 1 1 d . . . . .
O12 O 0.6414(3) 0.9491(2) 0.2767(2) 0.0825(7) Uani 1 1 d . . . . .
O11 O 0.7598(3) 1.1396(2) 0.4125(2) 0.0888(8) Uani 1 1 d . . . . .
O3 O 0.5577(3) 0.7675(3) 0.1179(2) 0.1023(9) Uani 1 1 d . U . . .
O1 O 0.7978(3) 0.9441(3) 0.1708(2) 0.0913(8) Uani 1 1 d . . . . .
C6 C 0.8618(5) 0.7065(3) 0.2682(3) 0.0820(10) Uani 1 1 d . . . . .
C7 C 0.8702(5) 1.0436(4) 0.2083(3) 0.0903(11) Uani 1 1 d . . . . .
C8 C 0.9058(7) 0.5374(4) 0.2611(4) 0.1062(15) Uani 1 1 d . . . . .
H8A H 0.8092 0.4952 0.2349 0.127 Uiso 1 1 calc R U . . .
H8B H 0.9373 0.5502 0.3294 0.127 Uiso 1 1 calc R U . . .
C9 C 0.9322(8) 0.6411(5) 0.2361(5) 0.125(2) Uani 1 1 d . . . . .
H9A H 1.0201 0.6801 0.2884 0.150 Uiso 0.74(7) 1 calc R U P A 1
H9B H 1.0196 0.6799 0.2889 0.150 Uiso 0.26(7) 1 calc R U P A 2
C10 C 0.9742(8) 0.4746(5) 0.2249(5) 0.124(2) Uani 1 1 d . . . . .
H10 H 0.9752 0.4131 0.2453 0.149 Uiso 1 1 calc R U . . .
C11 C 0.9423(6) 1.1063(6) 0.1529(4) 0.1187(18) Uani 1 1 d . . . . .
H11 H 0.9761 1.1802 0.1910 0.142 Uiso 1 1 calc R U . . .
C12 C 0.5178(6) 0.6497(4) 0.2849(5) 0.130(2) Uani 1 1 d . . . . .
C13 C 0.5304(6) 0.9805(5) 0.2405(5) 0.1139(16) Uani 1 1 d . . . . .
H13 H 0.5434 1.0402 0.2900 0.137 Uiso 1 1 calc R U . . .
C14 C 0.4000(6) 0.8929(6) 0.2236(6) 0.142(2) Uani 1 1 d . . . . .
H14A H 0.3884 0.8294 0.1813 0.213 Uiso 1 1 calc R U . . .
H14B H 0.3277 0.9151 0.1959 0.213 Uiso 1 1 calc R U . . .
H14C H 0.3993 0.8775 0.2826 0.213 Uiso 1 1 calc R U . . .
C15 C 0.7417(7) 0.9630(5) 0.5539(4) 0.126(2) Uani 1 1 d . . . . .
H15 H 0.7574 0.9048 0.5810 0.151 Uiso 1 1 calc R U . . .
C16 C 0.7875(6) 0.6751(4) 0.5641(4) 0.1088(16) Uani 1 1 d . . . . .
H16 H 0.8764 0.7232 0.6117 0.131 Uiso 1 1 calc R U . . .
C17 C 0.5358(8) 1.0244(7) 0.1563(5) 0.146(3) Uani 1 1 d . . . . .
H17A H 0.6237 1.0795 0.1726 0.219 Uiso 1 1 calc R U . . .
H17B H 0.4690 1.0544 0.1379 0.219 Uiso 1 1 calc R U . . .
H17C H 0.5183 0.9673 0.1048 0.219 Uiso 1 1 calc R U . . .
C18 C 0.8356(7) 1.0490(6) 0.6293(4) 0.142(3) Uani 1 1 d . . . . .
H18A H 0.9214 1.0430 0.6480 0.213 Uiso 1 1 calc R U . . .
H18B H 0.8069 1.0487 0.6814 0.213 Uiso 1 1 calc R U . . .
H18C H 0.8438 1.1152 0.6109 0.213 Uiso 1 1 calc R U . . .
C19 C 0.8037(8) 1.2515(4) 0.4498(6) 0.131(2) Uani 1 1 d . . . . .
H19 H 0.8970 1.2762 0.4951 0.157 Uiso 1 1 calc R U . . .
C20 C 0.6838(9) 0.6552(6) 0.6101(5) 0.161(3) Uani 1 1 d . . . . .
H20A H 0.6747 0.7215 0.6286 0.242 Uiso 1 1 calc R U . . .
H20B H 0.7133 0.6292 0.6648 0.242 Uiso 1 1 calc R U . . .
H20C H 0.5982 0.6026 0.5656 0.242 Uiso 1 1 calc R U . . .
C1 C 0.7277(9) 1.2739(5) 0.5028(6) 0.150(3) Uani 1 1 d . . . . .
H1A H 0.6448 1.2735 0.4602 0.225 Uiso 1 1 calc R U . . .
H1B H 0.7795 1.3433 0.5470 0.225 Uiso 1 1 calc R U . . .
H1C H 0.7081 1.2196 0.5365 0.225 Uiso 1 1 calc R U . . .
C2 C 0.5427(8) 0.5549(4) 0.2561(6) 0.150(3) Uani 1 1 d . . . . .
H2A H 0.5780 0.5638 0.2074 0.225 Uiso 1 1 calc R U . . .
H2B H 0.4598 0.4922 0.2322 0.225 Uiso 1 1 calc R U . . .
H2C H 0.6069 0.5463 0.3095 0.225 Uiso 1 1 calc R U . . .
C3 C 1.0328(9) 0.5026(6) 0.1655(5) 0.138(2) Uani 1 1 d . . . . .
H3 H 1.0666 0.4566 0.1420 0.166 Uiso 1 1 calc R U . . .
C4 C 0.7956(10) 0.5738(5) 0.5230(5) 0.157(3) Uani 1 1 d . . . . .
H4A H 0.7069 0.5230 0.4816 0.236 Uiso 1 1 calc R U . . .
H4B H 0.8326 0.5437 0.5730 0.236 Uiso 1 1 calc R U . . .
H4C H 0.8526 0.5894 0.4879 0.236 Uiso 1 1 calc R U . . .
C5 C 0.4312(8) 0.6529(6) 0.3284(8) 0.200(5) Uani 1 1 d . . . . .
H5A H 0.4420 0.7223 0.3624 0.240 Uiso 1 1 calc R U . . .
H5B H 0.3919 0.5913 0.3507 0.240 Uiso 1 1 calc R U . . .
C29 C 1.0472(10) 0.5988(7) 0.1358(6) 0.155(3) Uani 1 1 d . . . . .
H29A H 1.0129 0.5814 0.0673 0.186 Uiso 0.74(7) 1 calc R U P A 1
H29B H 1.1424 0.6450 0.1594 0.186 Uiso 0.74(7) 1 calc R U P A 1
H29C H 1.0151 0.5779 0.0674 0.186 Uiso 0.26(7) 1 calc R U P A 2
H29D H 1.1435 0.6410 0.1586 0.186 Uiso 0.26(7) 1 calc R U P A 2
C28 C 1.0660(7) 1.0938(9) 0.1648(6) 0.169(4) Uani 1 1 d . . . . .
H28A H 1.0471 1.0186 0.1409 0.203 Uiso 1 1 calc R U . . .
H28B H 1.1230 1.1155 0.2316 0.203 Uiso 1 1 calc R U . . .
C27 C 0.976(3) 0.658(2) 0.168(2) 0.194(6) Uani 0.74(7) 1 d . . P A 1
H27A H 1.0357 0.7336 0.1870 0.233 Uiso 0.74(7) 1 calc R U P A 1
H27B H 0.8988 0.6486 0.1132 0.233 Uiso 0.74(7) 1 calc R U P A 1
C26 C 1.0659(10) 1.1928(9) 0.0368(6) 0.187(4) Uani 1 1 d . . . . .
H26 H 1.1095 1.2276 0.0007 0.225 Uiso 1 1 calc R U . . .
C25 C 0.9387(10) 1.1754(10) 0.0139(7) 0.217(5) Uani 1 1 d . . . . .
H25 H 0.8964 1.2015 -0.0346 0.260 Uiso 1 1 calc R U . . .
C24 C 0.8585(9) 1.1123(10) 0.0663(7) 0.218(6) Uani 1 1 d . . . . .
H24A H 0.8008 1.1468 0.0775 0.261 Uiso 1 1 calc R U . . .
H24B H 0.8011 1.0399 0.0267 0.261 Uiso 1 1 calc R U . . .
C23 C 0.8081(14) 1.3071(6) 0.3752(8) 0.226(6) Uani 1 1 d . . . . .
H23A H 0.8459 1.2775 0.3366 0.339 Uiso 1 1 calc R U . . .
H23B H 0.8631 1.3825 0.4030 0.339 Uiso 1 1 calc R U . . .
H23C H 0.7184 1.2981 0.3368 0.339 Uiso 1 1 calc R U . . .
C22 C 0.6017(8) 0.9244(10) 0.5281(7) 0.221(6) Uani 1 1 d . . . . .
C21 C 1.1409(10) 1.1628(10) 0.1117(6) 0.212(5) Uani 1 1 d . . . . .
H21A H 1.2108 1.2281 0.1576 0.255 Uiso 1 1 calc R U . . .
H21B H 1.1857 1.1234 0.0876 0.255 Uiso 1 1 calc R U . . .
C30 C 0.4973(11) 0.7183(10) 0.0221(5) 0.173(4) Uani 0.843(12) 1 d . U P B 1
C31 C 0.5636(16) 0.7127(16) -0.0212(8) 0.380(15) Uani 1 1 d . . . . .
H31A H 0.5226 0.6786 -0.0855 0.456 Uiso 1 1 calc R U . B 1
H31B H 0.6571 0.7423 0.0086 0.456 Uiso 1 1 calc R U . B 1
C32 C 0.3647(14) 0.6789(17) -0.0141(8) 0.420(15) Uani 1 1 d . U . . .
H32A H 0.3322 0.6812 0.0361 0.630 Uiso 1 1 calc R U . B 1
H32B H 0.3306 0.6056 -0.0499 0.630 Uiso 1 1 calc R U . B 1
H32C H 0.3345 0.7211 -0.0548 0.630 Uiso 1 1 calc R U . B 1
C27A C 0.978(13) 0.686(6) 0.162(7) 0.194(6) Uani 0.26(7) 1 d . . P A 2
C30A C 0.591(5) 0.366(5) -0.211(3) 0.173(4) Uani 0.157(12) 1 d . . P B 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 '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
O3 Ti1 O2 101.96(15) . .
O3 Ti1 O5 173.05(14) . .
O2 Ti1 O5 82.53(10) . .
O3 Ti1 O12 103.34(15) . .
O2 Ti1 O12 94.28(12) . .
O5 Ti1 O12 81.43(11) . .
O3 Ti1 O1 91.02(15) . .
O2 Ti1 O1 165.97(12) . .
O5 Ti1 O1 84.07(11) . .
O12 Ti1 O1 87.80(13) . .
O3 Ti1 O9 91.37(15) . .
O2 Ti1 O9 87.72(12) . .
O5 Ti1 O9 83.46(11) . .
O12 Ti1 O9 164.36(12) . .
O1 Ti1 O9 86.65(13) . .
O3 Ti1 Ti2 145.90(13) . .
O2 Ti1 Ti2 92.41(8) . .
O5 Ti1 Ti2 37.73(7) . .
O12 Ti1 Ti2 44.22(9) . .
O1 Ti1 Ti2 79.42(9) . .
O9 Ti1 Ti2 120.26(9) . .
O3 Ti1 Ti3 145.55(12) . .
O2 Ti1 Ti3 45.18(8) . .
O5 Ti1 Ti3 37.80(6) . .
O12 Ti1 Ti3 91.22(9) . .
O1 Ti1 Ti3 120.98(9) . .
O9 Ti1 Ti3 79.19(8) . .
Ti2 Ti1 Ti3 60.857(19) . .
O11 Ti2 O10 97.97(13) . .
O11 Ti2 O5 161.29(13) . .
O10 Ti2 O5 100.74(11) . .
O11 Ti2 O4 102.20(12) . .
O10 Ti2 O4 96.59(11) . .
O5 Ti2 O4 75.56(9) . .
O11 Ti2 O7 95.70(13) . .
O10 Ti2 O7 89.62(12) . .
O5 Ti2 O7 84.62(11) . .
O4 Ti2 O7 160.00(11) . .
O11 Ti2 O12 86.34(13) . .
O10 Ti2 O12 170.95(12) . .
O5 Ti2 O12 75.16(10) . .
O4 Ti2 O12 90.23(11) . .
O7 Ti2 O12 82.01(12) . .
O11 Ti2 Ti1 124.63(11) . .
O10 Ti2 Ti1 136.05(9) . .
O5 Ti2 Ti1 37.20(7) . .
O4 Ti2 Ti1 85.44(7) . .
O7 Ti2 Ti1 77.01(9) . .
O12 Ti2 Ti1 38.43(7) . .
O11 Ti2 Ti3 140.46(10) . .
O10 Ti2 Ti3 95.51(7) . .
O5 Ti2 Ti3 37.08(6) . .
O4 Ti2 Ti3 39.16(7) . .
O7 Ti2 Ti3 121.44(9) . .
O12 Ti2 Ti3 86.01(7) . .
Ti1 Ti2 Ti3 59.66(2) . .
O10 Ti3 O6 98.26(12) 2_776 .
O10 Ti3 O5 99.92(10) 2_776 .
O6 Ti3 O5 161.63(12) . .
O10 Ti3 O4 95.75(11) 2_776 .
O6 Ti3 O4 100.20(11) . .
O5 Ti3 O4 75.40(9) . .
O10 Ti3 O8 90.73(12) 2_776 .
O6 Ti3 O8 97.42(11) . .
O5 Ti3 O8 84.99(10) . .
O4 Ti3 O8 160.13(10) . .
O10 Ti3 O2 170.47(11) 2_776 .
O6 Ti3 O2 87.48(12) . .
O5 Ti3 O2 74.87(10) . .
O4 Ti3 O2 90.68(11) . .
O8 Ti3 O2 80.95(11) . .
O10 Ti3 Ti1 135.33(8) 2_776 .
O6 Ti3 Ti1 125.61(10) . .
O5 Ti3 Ti1 37.12(7) . .
O4 Ti3 Ti1 85.27(8) . .
O8 Ti3 Ti1 76.99(8) . .
O2 Ti3 Ti1 38.15(7) . .
O10 Ti3 Ti2 94.47(7) 2_776 .
O6 Ti3 Ti2 138.60(10) . .
O5 Ti3 Ti2 36.94(6) . .
O4 Ti3 Ti2 39.15(7) . .
O8 Ti3 Ti2 121.71(7) . .
O2 Ti3 Ti2 86.08(7) . .
Ti1 Ti3 Ti2 59.48(2) . .
C15 O4 Ti2 130.2(3) . .
C15 O4 Ti3 126.8(3) . .
Ti2 O4 Ti3 101.69(11) . .
Ti1 O5 Ti2 105.06(11) . .
Ti1 O5 Ti3 105.08(10) . .
Ti2 O5 Ti3 105.98(10) . .
C16 O6 Ti3 140.1(3) . .
C7 O7 Ti2 130.8(3) . .
C6 O8 Ti3 130.2(3) . .
C6 O9 Ti1 126.8(3) . .
Ti3 O10 Ti2 170.02(14) 2_776 .
C12 O2 Ti1 129.5(4) . .
C12 O2 Ti3 132.2(4) . .
Ti1 O2 Ti3 96.67(10) . .
C13 O12 Ti1 134.5(3) . .
C13 O12 Ti2 127.1(3) . .
Ti1 O12 Ti2 97.35(11) . .
C19 O11 Ti2 138.6(4) . .
C30 O3 Ti1 157.9(6) . .
C7 O1 Ti1 126.5(3) . .
O9 C6 O8 125.9(4) . .
O9 C6 C9 117.6(4) . .
O8 C6 C9 116.5(4) . .
O7 C7 O1 125.6(4) . .
O7 C7 C11 116.8(5) . .
O1 C7 C11 117.5(5) . .
C9 C8 C10 112.1(5) . .
C9 C8 H8A 109.2 . .
C10 C8 H8A 109.2 . .
C9 C8 H8B 109.2 . .
C10 C8 H8B 109.2 . .
H8A C8 H8B 107.9 . .
C27 C9 C8 120.4(12) . .
C8 C9 C27A 134(2) . .
C27 C9 C6 122.1(12) . .
C8 C9 C6 114.3(4) . .
C27A C9 C6 108(2) . .
C27 C9 H9A 96.0 . .
C8 C9 H9A 96.0 . .
C6 C9 H9A 96.0 . .
C8 C9 H9B 95.6 . .
C27A C9 H9B 95.6 . .
C6 C9 H9B 95.6 . .
C3 C10 C8 123.0(5) . .
C3 C10 H10 118.5 . .
C8 C10 H10 118.5 . .
C24 C11 C28 122.1(7) . .
C24 C11 C7 115.5(6) . .
C28 C11 C7 111.8(5) . .
C24 C11 H11 101.0 . .
C28 C11 H11 101.0 . .
C7 C11 H11 101.0 . .
C30A C12 C5 80(2) 2_665 .
C30A C12 O2 118(3) 2_665 .
C5 C12 O2 115.8(5) . .
C30A C12 C2 100(3) 2_665 .
C5 C12 C2 125.4(6) . .
O2 C12 C2 111.9(5) . .
O12 C13 C14 111.8(5) . .
O12 C13 C17 109.9(5) . .
C14 C13 C17 114.6(6) . .
O12 C13 H13 106.7 . .
C14 C13 H13 106.7 . .
C17 C13 H13 106.7 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
H14A C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
C18 C15 C22 125.2(6) . .
C18 C15 O4 116.5(4) . .
C22 C15 O4 112.2(6) . .
C18 C15 H15 98.3 . .
C22 C15 H15 98.3 . .
O4 C15 H15 98.3 . .
O6 C16 C4 108.6(4) . .
O6 C16 C20 108.4(6) . .
C4 C16 C20 112.8(5) . .
O6 C16 H16 109.0 . .
C4 C16 H16 109.0 . .
C20 C16 H16 109.0 . .
C13 C17 H17A 109.5 . .
C13 C17 H17B 109.5 . .
H17A C17 H17B 109.5 . .
C13 C17 H17C 109.5 . .
H17A C17 H17C 109.5 . .
H17B C17 H17C 109.5 . .
C15 C18 H18A 109.5 . .
C15 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C15 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O11 C19 C1 111.5(5) . .
O11 C19 C23 109.8(6) . .
C1 C19 C23 115.6(6) . .
O11 C19 H19 106.5 . .
C1 C19 H19 106.5 . .
C23 C19 H19 106.5 . .
C16 C20 H20A 109.5 . .
C16 C20 H20B 109.5 . .
H20A C20 H20B 109.5 . .
C16 C20 H20C 109.5 . .
H20A C20 H20C 109.5 . .
H20B C20 H20C 109.5 . .
C19 C1 H1A 109.5 . .
C19 C1 H1B 109.5 . .
H1A C1 H1B 109.5 . .
C19 C1 H1C 109.5 . .
H1A C1 H1C 109.5 . .
H1B C1 H1C 109.5 . .
C12 C2 H2A 109.5 . .
C12 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C12 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C10 C3 C29 123.5(6) . .
C10 C3 H3 118.3 . .
C29 C3 H3 118.3 . .
C16 C4 H4A 109.5 . .
C16 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C16 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
C12 C5 C30A 49(2) . 2_665
C12 C5 H5A 118.8 . .
C30A C5 H5A 118.8 2_665 .
C12 C5 H5B 118.8 . .
C30A C5 H5B 118.8 2_665 .
H5A C5 H5B 116.2 . .
C3 C29 C27 113.2(11) . .
C3 C29 C27A 125(2) . .
C3 C29 H29A 108.9 . .
C27 C29 H29A 108.9 . .
C3 C29 H29B 108.9 . .
C27 C29 H29B 108.9 . .
H29A C29 H29B 107.8 . .
C3 C29 H29C 106.1 . .
C27A C29 H29C 106.1 . .
C3 C29 H29D 106.1 . .
C27A C29 H29D 106.1 . .
H29C C29 H29D 106.3 . .
C11 C28 C21 110.8(7) . .
C11 C28 H28A 109.5 . .
C21 C28 H28A 109.5 . .
C11 C28 H28B 109.5 . .
C21 C28 H28B 109.5 . .
H28A C28 H28B 108.1 . .
C9 C27 C29 124.5(19) . .
C9 C27 H27A 106.2 . .
C29 C27 H27A 106.2 . .
C9 C27 H27B 106.2 . .
C29 C27 H27B 106.2 . .
H27A C27 H27B 106.4 . .
C25 C26 C21 124.4(7) . .
C25 C26 H26 117.8 . .
C21 C26 H26 117.8 . .
C26 C25 C24 120.6(7) . .
C26 C25 H25 119.7 . .
C24 C25 H25 119.7 . .
C11 C24 C25 112.4(7) . .
C11 C24 H24A 109.1 . .
C25 C24 H24A 109.1 . .
C11 C24 H24B 109.1 . .
C25 C24 H24B 109.1 . .
H24A C24 H24B 107.9 . .
C19 C23 H23A 109.5 . .
C19 C23 H23B 109.5 . .
H23A C23 H23B 109.5 . .
C19 C23 H23C 109.5 . .
H23A C23 H23C 109.5 . .
H23B C23 H23C 109.5 . .
C26 C21 C28 118.2(8) . .
C26 C21 H21A 107.8 . .
C28 C21 H21A 107.8 . .
C26 C21 H21B 107.8 . .
C28 C21 H21B 107.8 . .
H21A C21 H21B 107.1 . .
C31 C30 C32 124.2(10) . .
C31 C30 O3 120.2(11) . .
C32 C30 O3 115.6(11) . .
C30 C31 H31A 120.0 . .
C30 C31 H31B 120.0 . .
H31A C31 H31B 120.0 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
C9 C27A C29 99(3) . .
C12 C30A C5 51.5(14) 2_665 2_665
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O3 1.781(3) .
Ti1 O2 1.920(3) .
Ti1 O5 1.930(2) .
Ti1 O12 1.931(3) .
Ti1 O1 2.084(3) .
Ti1 O9 2.086(3) .
Ti1 Ti2 3.0820(9) .
Ti1 Ti3 3.0877(9) .
Ti2 O11 1.809(3) .
Ti2 O10 1.814(3) .
Ti2 O5 1.953(2) .
Ti2 O4 2.015(2) .
Ti2 O7 2.065(3) .
Ti2 O12 2.167(3) .
Ti2 Ti3 3.1248(8) .
Ti3 O10 1.800(3) 2_776
Ti3 O6 1.808(2) .
Ti3 O5 1.960(2) .
Ti3 O4 2.015(2) .
Ti3 O8 2.068(3) .
Ti3 O2 2.205(3) .
O4 C15 1.435(5) .
O6 C16 1.411(5) .
O7 C7 1.251(6) .
O8 C6 1.261(5) .
O9 C6 1.255(5) .
O10 Ti3 1.800(3) 2_776
O2 C12 1.441(5) .
O12 C13 1.433(6) .
O11 C19 1.412(6) .
O3 C30 1.382(7) .
O1 C7 1.268(6) .
C6 C9 1.517(6) .
C7 C11 1.513(6) .
C8 C9 1.467(7) .
C8 C10 1.501(8) .
C8 H8A 0.9700 .
C8 H8B 0.9700 .
C9 C27 1.31(2) .
C9 C27A 1.51(6) .
C9 H9A 0.9800 .
C9 H9B 0.9800 .
C10 C3 1.318(9) .
C10 H10 0.9300 .
C11 C24 1.402(9) .
C11 C28 1.431(9) .
C11 H11 0.9800 .
C12 C30A 1.31(5) 2_665
C12 C5 1.367(10) .
C12 C2 1.458(9) .
C13 C14 1.481(9) .
C13 C17 1.504(9) .
C13 H13 0.9800 .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
C15 C18 1.381(8) .
C15 C22 1.401(10) .
C15 H15 0.9800 .
C16 C4 1.489(8) .
C16 C20 1.530(9) .
C16 H16 0.9800 .
C17 H17A 0.9600 .
C17 H17B 0.9600 .
C17 H17C 0.9600 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C19 C1 1.442(9) .
C19 C23 1.458(10) .
C19 H19 0.9800 .
C20 H20A 0.9600 .
C20 H20B 0.9600 .
C20 H20C 0.9600 .
C1 H1A 0.9600 .
C1 H1B 0.9600 .
C1 H1C 0.9600 .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C3 C29 1.415(10) .
C3 H3 0.9300 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C30A 1.72(4) 2_665
C5 H5A 0.9700 .
C5 H5B 0.9700 .
C29 C27 1.46(2) .
C29 C27A 1.70(6) .
C29 H29A 0.9700 .
C29 H29B 0.9700 .
C29 H29C 0.9700 .
C29 H29D 0.9700 .
C28 C21 1.543(9) .
C28 H28A 0.9700 .
C28 H28B 0.9700 .
C27 H27A 0.9700 .
C27 H27B 0.9700 .
C26 C25 1.305(12) .
C26 C21 1.395(13) .
C26 H26 0.9300 .
C25 C24 1.530(10) .
C25 H25 0.9300 .
C24 H24A 0.9700 .
C24 H24B 0.9700 .
C23 H23A 0.9600 .
C23 H23B 0.9600 .
C23 H23C 0.9600 .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C30 C31 1.171(16) .
C30 C32 1.315(17) .
C31 H31A 0.9300 .
C31 H31B 0.9300 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C30A C12 1.31(5) 2_665
C30A C5 1.72(4) 2_665
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_site_symmetry_1
_geom_torsion_site_symmetry_4
O10 Ti3 O6 C16 -15.8(5) 2_776 .
O5 Ti3 O6 C16 172.5(4) . .
O4 Ti3 O6 C16 -113.2(4) . .
O8 Ti3 O6 C16 76.0(4) . .
O2 Ti3 O6 C16 156.5(4) . .
Ti1 Ti3 O6 C16 155.3(4) . .
Ti2 Ti3 O6 C16 -122.3(4) . .
O10 Ti2 O11 C19 19.6(6) . .
O5 Ti2 O11 C19 -160.8(5) . .
O4 Ti2 O11 C19 118.2(6) . .
O7 Ti2 O11 C19 -70.8(6) . .
O12 Ti2 O11 C19 -152.4(6) . .
Ti1 Ti2 O11 C19 -148.9(5) . .
Ti3 Ti2 O11 C19 128.4(5) . .
O2 Ti1 O3 C30 -129.2(17) . .
O12 Ti1 O3 C30 133.4(17) . .
O1 Ti1 O3 C30 45.4(17) . .
O9 Ti1 O3 C30 -41.3(17) . .
Ti2 Ti1 O3 C30 117.8(16) . .
Ti3 Ti1 O3 C30 -114.0(16) . .
Ti1 O9 C6 O8 0.1(6) . .
Ti1 O9 C6 C9 -179.1(4) . .
Ti3 O8 C6 O9 -10.3(6) . .
Ti3 O8 C6 C9 169.0(4) . .
Ti2 O7 C7 O1 10.0(7) . .
Ti2 O7 C7 C11 -170.7(3) . .
Ti1 O1 C7 O7 -2.2(7) . .
Ti1 O1 C7 C11 178.4(3) . .
C10 C8 C9 C27 18(2) . .
C10 C8 C9 C27A 20(7) . .
C10 C8 C9 C6 178.1(5) . .
O9 C6 C9 C27 30(2) . .
O8 C6 C9 C27 -149(2) . .
O9 C6 C9 C8 -129.9(6) . .
O8 C6 C9 C8 50.8(8) . .
O9 C6 C9 C27A 33(5) . .
O8 C6 C9 C27A -146(5) . .
C9 C8 C10 C3 -9.8(10) . .
O7 C7 C11 C24 -116.8(8) . .
O1 C7 C11 C24 62.7(10) . .
O7 C7 C11 C28 97.7(8) . .
O1 C7 C11 C28 -82.8(8) . .
Ti1 O2 C12 C30A -27(3) . 2_665
Ti3 O2 C12 C30A 171(3) . 2_665
Ti1 O2 C12 C5 -119.4(8) . .
Ti3 O2 C12 C5 78.7(9) . .
Ti1 O2 C12 C2 88.0(7) . .
Ti3 O2 C12 C2 -73.9(7) . .
Ti1 O12 C13 C14 60.1(8) . .
Ti2 O12 C13 C14 -134.4(5) . .
Ti1 O12 C13 C17 -68.3(7) . .
Ti2 O12 C13 C17 97.2(6) . .
Ti2 O4 C15 C18 -56.3(9) . .
Ti3 O4 C15 C18 108.2(6) . .
Ti2 O4 C15 C22 97.6(8) . .
Ti3 O4 C15 C22 -97.9(9) . .
Ti3 O6 C16 C4 -89.6(6) . .
Ti3 O6 C16 C20 147.6(4) . .
Ti2 O11 C19 C1 -140.8(5) . .
Ti2 O11 C19 C23 89.8(9) . .
C8 C10 C3 C29 5.3(13) . .
O2 C12 C5 C30A 117(3) . 2_665
C2 C12 C5 C30A -95(3) . 2_665
C10 C3 C29 C27 -7(2) . .
C10 C3 C29 C27A -7(6) . .
C24 C11 C28 C21 39.9(13) . .
C7 C11 C28 C21 -177.2(7) . .
C8 C9 C27 C29 -23(4) . .
C6 C9 C27 C29 178.8(19) . .
C3 C29 C27 C9 16(4) . .
C21 C26 C25 C24 -4(2) . .
C28 C11 C24 C25 -37.5(15) . .
C7 C11 C24 C25 -179.1(8) . .
C26 C25 C24 C11 17.6(19) . .
C25 C26 C21 C28 7(2) . .
C11 C28 C21 C26 -22.6(15) . .
Ti1 O3 C30 C31 0(3) . .
Ti1 O3 C30 C32 179.4(14) . .
C8 C9 C27A C29 -20(10) . .
C6 C9 C27A C29 -178(4) . .
C3 C29 C27A C9 11(9) . .
