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#$Date: 2024-09-06 04:00:07 +0300 (Fri, 06 Sep 2024) $
#$Revision: 294591 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/68/7716805.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_7716805
loop_
_publ_author_name
'Kubiak, Barbara'
'Muzioł, Tadeusz'
'Jabłoński, Mirosław'
'Radtke, Aleksandra'
'Piszczek, Piotr'
_publ_section_title
;
 Investigation of titanium(IV)-oxo complexes stabilized with
 α-hydroxy carboxylate ligands: structural analysis and DFT studies.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              14457
_journal_page_last               14468
_journal_paper_doi               10.1039/d4dt01710b
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety
'(Ti 4+)4, (C14 H8 O3 2-)2, (C3 H7 O 1-)10 (O 2-)'
_chemical_formula_sum            'C58 H86 O17 Ti4'
_chemical_formula_weight         1246.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 106.0037(19)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4667(4)
_cell_length_b                   12.6262(2)
_cell_length_c                   23.0730(5)
_cell_measurement_reflns_used    13846
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      78.2820
_cell_measurement_theta_min      3.9750
_cell_volume                     6291.4(2)
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3, (Dolomanov, 2009)'
_computing_publication_material  ciftab
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'Olex2 1.3, (Dolomanov, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.0000
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29621
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_min         3.986
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.707
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.120a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       'tiny rhombus'
_exptl_crystal_F_000             2632
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.066
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6404
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0428
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0593P)²+7.5391P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1131
_refine_ls_wR_factor_ref         0.1169
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5499
_reflns_number_total             6404
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01710b7.cif
_cod_data_source_block           nbk19-3Dshape
_cod_depositor_comments
'Adding full bibliography for 7716804--7716805.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7716805
_shelx_shelxl_version_number     2018/1
_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   0.705
_shelx_estimated_absorpt_t_max   0.912
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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 0.50773(2) 0.40534(3) 0.67735(2) 0.01917(11) Uani 1 1 d . . . . .
Ti2 Ti 0.58633(2) 0.18495(3) 0.66475(2) 0.02515(12) Uani 1 1 d . . . . .
O16 O 0.500000 0.45191(16) 0.750000 0.0214(4) Uani 1 2 d S T P . .
O1 O 0.55746(6) 0.27143(12) 0.72800(6) 0.0215(3) Uani 1 1 d . . . . .
O2 O 0.57610(7) 0.30869(12) 0.82606(7) 0.0231(3) Uani 1 1 d . . . . .
C2 C 0.59152(9) 0.27048(16) 0.78354(9) 0.0201(4) Uani 1 1 d . . . . .
C3 C 0.65475(9) 0.21726(18) 0.78983(10) 0.0226(4) Uani 1 1 d . . . . .
O3 O 0.65343(7) 0.17331(13) 0.73410(7) 0.0274(3) Uani 1 1 d . . . . .
C4 C 0.70448(10) 0.30201(18) 0.81211(11) 0.0263(5) Uani 1 1 d . . . . .
C5 C 0.71631(11) 0.39047(19) 0.78155(12) 0.0316(5) Uani 1 1 d . . . . .
H5 H 0.692728 0.404014 0.741262 0.038 Uiso 1 1 calc R U . . .
C6 C 0.76354(12) 0.4593(2) 0.81110(13) 0.0382(6) Uani 1 1 d . . . . .
H6 H 0.773275 0.519242 0.790541 0.046 Uiso 1 1 calc R U . . .
C7 C 0.79633(11) 0.4401(2) 0.87067(13) 0.0397(6) Uani 1 1 d . . . . .
H7 H 0.827514 0.488688 0.890705 0.048 Uiso 1 1 calc R U . . .
C8 C 0.78469(11) 0.3518(2) 0.90161(12) 0.0361(6) Uani 1 1 d . . . . .
H8 H 0.807706 0.339291 0.942207 0.043 Uiso 1 1 calc R U . . .
C9 C 0.73819(10) 0.2817(2) 0.87152(11) 0.0289(5) Uani 1 1 d . . . . .
C10 C 0.71665(10) 0.18122(19) 0.89064(11) 0.0289(5) Uani 1 1 d . . . . .
C11 C 0.73651(11) 0.1253(2) 0.94430(12) 0.0352(6) Uani 1 1 d . . . . .
H11 H 0.768115 0.152822 0.977156 0.042 Uiso 1 1 calc R U . . .
C12 C 0.70922(13) 0.0288(2) 0.94879(13) 0.0414(6) Uani 1 1 d . . . . .
H12 H 0.722016 -0.009908 0.985450 0.050 Uiso 1 1 calc R U . . .
C13 C 0.66342(13) -0.0132(2) 0.90080(13) 0.0410(6) Uani 1 1 d . . . . .
H13 H 0.645883 -0.080323 0.904758 0.049 Uiso 1 1 calc R U . . .
C14 C 0.64311(11) 0.0433(2) 0.84678(12) 0.0333(5) Uani 1 1 d . . . . .
H14 H 0.611676 0.015458 0.813884 0.040 Uiso 1 1 calc R U . . .
C15 C 0.66963(10) 0.13970(18) 0.84240(10) 0.0264(5) Uani 1 1 d . . . . .
O21 O 0.52077(7) 0.28243(12) 0.62116(6) 0.0241(3) Uani 1 1 d . . . . .
C22 C 0.49472(11) 0.2667(2) 0.55696(10) 0.0303(5) Uani 1 1 d . . . . .
H22 H 0.515918 0.204503 0.544578 0.036 Uiso 1 1 calc R U . . .
C23 C 0.50722(14) 0.3627(2) 0.52295(12) 0.0417(6) Uani 1 1 d . . . . .
H23A H 0.490966 0.350331 0.479510 0.063 Uiso 1 1 calc R U . . .
H23B H 0.551952 0.375171 0.532863 0.063 Uiso 1 1 calc R U . . .
H23C H 0.486853 0.424732 0.534426 0.063 Uiso 1 1 calc R U . . .
C24 C 0.42644(12) 0.2414(3) 0.54327(12) 0.0452(7) Uani 1 1 d . . . . .
H24A H 0.404462 0.302356 0.553715 0.068 Uiso 1 1 calc R U . . .
H24B H 0.420689 0.179761 0.566984 0.068 Uiso 1 1 calc R U . . .
H24C H 0.409930 0.225609 0.500222 0.068 Uiso 1 1 calc R U . . .
O31 O 0.45488(7) 0.49207(13) 0.62666(7) 0.0266(3) Uani 1 1 d . . . . .
C32 C 0.40084(10) 0.54883(19) 0.62923(11) 0.0288(5) Uani 1 1 d . . . . .
H32 H 0.389158 0.526711 0.666244 0.035 Uiso 1 1 calc R U . . .
C33 C 0.34850(12) 0.5213(2) 0.57453(14) 0.0435(7) Uani 1 1 d . . . . .
H33A H 0.311505 0.561701 0.575350 0.065 Uiso 1 1 calc R U . . .
H33B H 0.339585 0.445334 0.574828 0.065 Uiso 1 1 calc R U . . .
H33C H 0.360434 0.538912 0.537909 0.065 Uiso 1 1 calc R U . . .
C34 C 0.41599(12) 0.6661(2) 0.63363(13) 0.0383(6) Uani 1 1 d . . . . .
H34A H 0.427519 0.688570 0.597535 0.057 Uiso 1 1 calc R U . . .
H34B H 0.450581 0.679223 0.669443 0.057 Uiso 1 1 calc R U . . .
H34C H 0.379655 0.706163 0.636753 0.057 Uiso 1 1 calc R U . . .
O41 O 0.57971(7) 0.46844(13) 0.67459(7) 0.0284(3) Uani 1 1 d . . . . .
C42 C 0.59506(11) 0.5724(2) 0.65876(11) 0.0314(5) Uani 1 1 d . . . . .
H42 H 0.556516 0.607192 0.633796 0.038 Uiso 1 1 calc R U . . .
C43 C 0.64087(13) 0.5647(2) 0.62173(14) 0.0449(7) Uani 1 1 d . . . . .
H43A H 0.649558 0.635755 0.609025 0.067 Uiso 1 1 calc R U . . .
H43B H 0.623399 0.520799 0.586066 0.067 Uiso 1 1 calc R U . . .
H43C H 0.679372 0.532581 0.646087 0.067 Uiso 1 1 calc R U . . .
C44 C 0.62002(17) 0.6366(2) 0.71579(15) 0.0525(8) Uani 1 1 d . . . . .
H44A H 0.655050 0.599107 0.742767 0.079 Uiso 1 1 calc R U . . .
H44B H 0.587340 0.646187 0.736018 0.079 Uiso 1 1 calc R U . . .
H44C H 0.633808 0.705943 0.705483 0.079 Uiso 1 1 calc R U . . .
O51 O 0.63204(9) 0.18953(17) 0.61278(8) 0.0417(5) Uani 1 1 d . . . . .
C52 C 0.67528(17) 0.2584(3) 0.59544(17) 0.0593(9) Uani 1 1 d . . . . .
H52 H 0.661088 0.333304 0.596163 0.071 Uiso 1 1 calc R U . . .
C53 C 0.6729(2) 0.2288(4) 0.53104(18) 0.0844(15) Uani 1 1 d . . . . .
H53A H 0.699458 0.276880 0.515998 0.127 Uiso 1 1 calc R U . . .
H53B H 0.630162 0.234537 0.505578 0.127 Uiso 1 1 calc R U . . .
H53C H 0.687440 0.155836 0.529997 0.127 Uiso 1 1 calc R U . . .
C54 C 0.73864(16) 0.2475(3) 0.63857(19) 0.0622(9) Uani 1 1 d . . . . .
H54A H 0.754243 0.175708 0.635956 0.093 Uiso 1 1 calc R U . . .
H54B H 0.736347 0.260802 0.679750 0.093 Uiso 1 1 calc R U . . .
H54C H 0.766696 0.298986 0.628172 0.093 Uiso 1 1 calc R U . . .
O61 O 0.54799(10) 0.06034(15) 0.65581(9) 0.0453(5) Uani 1 1 d . . . . .
C62 C 0.5160(3) -0.0342(5) 0.6371(3) 0.0442(13) Uani 0.5 1 d . . P A 1
H62 H 0.476099 -0.035357 0.648376 0.053 Uiso 0.5 1 calc R U P A 1
C63 C 0.5590(3) -0.1225(6) 0.6694(4) 0.0636(19) Uani 0.5 1 d . . P A 1
H63A H 0.537283 -0.190542 0.661394 0.095 Uiso 0.5 1 calc R U P A 1
H63B H 0.571370 -0.108759 0.712853 0.095 Uiso 0.5 1 calc R U P A 1
H63C H 0.595869 -0.124786 0.654561 0.095 Uiso 0.5 1 calc R U P A 1
C64 C 0.5043(5) -0.0455(7) 0.5696(4) 0.074(2) Uani 0.5 1 d . . P A 1
H64A H 0.542272 -0.029036 0.558482 0.111 Uiso 0.5 1 calc R U P A 1
H64B H 0.471387 0.003481 0.549054 0.111 Uiso 0.5 1 calc R U P A 1
H64C H 0.491515 -0.118358 0.557684 0.111 Uiso 0.5 1 calc R U P A 1
C65 C 0.5547(3) -0.0526(5) 0.6598(3) 0.0447(14) Uani 0.5 1 d . . P A 2
H65 H 0.599438 -0.069794 0.678034 0.054 Uiso 0.5 1 calc R U P A 2
C66 C 0.5183(3) -0.0932(5) 0.7011(3) 0.0510(15) Uani 0.5 1 d . . P A 2
H66A H 0.473950 -0.085074 0.681468 0.077 Uiso 0.5 1 calc R U P A 2
H66B H 0.529464 -0.052759 0.738776 0.077 Uiso 0.5 1 calc R U P A 2
H66C H 0.527862 -0.168255 0.709817 0.077 Uiso 0.5 1 calc R U P A 2
C67 C 0.5345(4) -0.1010(6) 0.5988(3) 0.0609(19) Uani 0.5 1 d . . P A 2
H67A H 0.543098 -0.177141 0.601771 0.091 Uiso 0.5 1 calc R U P A 2
H67B H 0.557017 -0.068062 0.572674 0.091 Uiso 0.5 1 calc R U P A 2
H67C H 0.489920 -0.089516 0.581660 0.091 Uiso 0.5 1 calc R U P A 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
_geom_angle_publ_flag
O31 Ti1 O41 98.34(7) . . ?
O31 Ti1 O16 100.86(7) . . ?
O41 Ti1 O16 101.60(6) . . ?
O31 Ti1 O21 103.26(7) . . ?
O41 Ti1 O21 91.45(7) . . ?
O16 Ti1 O21 150.51(8) . . ?
O31 Ti1 O1 166.71(7) . . ?
O41 Ti1 O1 91.67(6) . . ?
O16 Ti1 O1 85.54(6) . . ?
O21 Ti1 O1 67.58(6) . . ?
O31 Ti1 O2 84.84(7) . 2_656 ?
O41 Ti1 O2 171.77(7) . 2_656 ?
O16 Ti1 O2 85.16(5) . 2_656 ?
O21 Ti1 O2 80.41(6) . 2_656 ?
O1 Ti1 O2 84.12(6) . 2_656 ?
O31 Ti1 Ti2 136.14(5) . . ?
O41 Ti1 Ti2 82.29(5) . . ?
O16 Ti1 Ti2 122.13(5) . . ?
O21 Ti1 Ti2 33.26(4) . . ?
O1 Ti1 Ti2 36.68(4) . . ?
O2 Ti1 Ti2 90.15(4) 2_656 . ?
O61 Ti2 O51 107.54(10) . . ?
O61 Ti2 O3 106.21(8) . . ?
O51 Ti2 O3 95.72(8) . . ?
O61 Ti2 O21 102.92(8) . . ?
O51 Ti2 O21 97.16(8) . . ?
O3 Ti2 O21 142.74(7) . . ?
O61 Ti2 O1 108.26(9) . . ?
O51 Ti2 O1 144.09(8) . . ?
O3 Ti2 O1 76.93(6) . . ?
O21 Ti2 O1 72.19(6) . . ?
O61 Ti2 Ti1 119.65(7) . . ?
O51 Ti2 Ti1 116.53(7) . . ?
O3 Ti2 Ti1 108.03(5) . . ?
O21 Ti2 Ti1 35.67(4) . . ?
O1 Ti2 Ti1 39.10(4) . . ?
Ti1 O16 Ti1 142.49(12) 2_656 . ?
C2 O1 Ti2 118.55(13) . . ?
C2 O1 Ti1 127.69(13) . . ?
Ti2 O1 Ti1 104.22(6) . . ?
C2 O2 Ti1 127.60(13) . 2_656 ?
O2 C2 O1 124.49(19) . . ?
O2 C2 C3 123.55(18) . . ?
O1 C2 C3 111.95(18) . . ?
O3 C3 C15 115.03(18) . . ?
O3 C3 C4 114.62(18) . . ?
C15 C3 C4 101.68(18) . . ?
O3 C3 C2 107.58(16) . . ?
C15 C3 C2 110.46(17) . . ?
C4 C3 C2 107.17(17) . . ?
C3 O3 Ti2 124.28(13) . . ?
C5 C4 C9 121.3(2) . . ?
C5 C4 C3 128.1(2) . . ?
C9 C4 C3 110.5(2) . . ?
C4 C5 C6 118.7(2) . . ?
C4 C5 H5 120.6 . . ?
C6 C5 H5 120.6 . . ?
C7 C6 C5 119.9(3) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 C6 121.7(2) . . ?
C8 C7 H7 119.1 . . ?
C6 C7 H7 119.1 . . ?
C7 C8 C9 118.3(2) . . ?
C7 C8 H8 120.9 . . ?
C9 C8 H8 120.9 . . ?
C4 C9 C8 120.0(2) . . ?
C4 C9 C10 108.6(2) . . ?
C8 C9 C10 131.3(2) . . ?
C11 C10 C15 120.2(2) . . ?
C11 C10 C9 131.0(2) . . ?
C15 C10 C9 108.8(2) . . ?
C12 C11 C10 118.4(2) . . ?
C12 C11 H11 120.8 . . ?
C10 C11 H11 120.8 . . ?
C11 C12 C13 121.5(2) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C12 C13 C14 120.2(3) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 118.4(2) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C14 C15 C10 121.3(2) . . ?
C14 C15 C3 128.7(2) . . ?
C10 C15 C3 110.0(2) . . ?
C22 O21 Ti2 118.10(14) . . ?
C22 O21 Ti1 130.45(14) . . ?
Ti2 O21 Ti1 111.07(7) . . ?
O21 C22 C23 109.9(2) . . ?
O21 C22 C24 110.08(19) . . ?
C23 C22 C24 112.6(2) . . ?
O21 C22 H22 108.1 . . ?
C23 C22 H22 108.1 . . ?
C24 C22 H22 108.1 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C32 O31 Ti1 134.35(14) . . ?
O31 C32 C33 109.0(2) . . ?
O31 C32 C34 108.41(19) . . ?
C33 C32 C34 112.9(2) . . ?
O31 C32 H32 108.8 . . ?
C33 C32 H32 108.8 . . ?
C34 C32 H32 108.8 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C42 O41 Ti1 133.64(14) . . ?
O41 C42 C43 109.6(2) . . ?
O41 C42 C44 109.1(2) . . ?
C43 C42 C44 112.2(2) . . ?
O41 C42 H42 108.6 . . ?
C43 C42 H42 108.6 . . ?
C44 C42 H42 108.6 . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 H44A 109.5 . . ?
C42 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C42 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C52 O51 Ti2 139.9(2) . . ?
O51 C52 C54 110.5(3) . . ?
O51 C52 C53 106.2(3) . . ?
C54 C52 C53 113.4(3) . . ?
O51 C52 H52 108.9 . . ?
C54 C52 H52 108.9 . . ?
C53 C52 H52 108.9 . . ?
C52 C53 H53A 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C52 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 H54A 109.5 . . ?
C52 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C52 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C62 O61 Ti2 169.1(3) . . ?
C65 O61 Ti2 146.4(3) . . ?
O61 C62 C64 109.2(6) . . ?
O61 C62 C63 105.6(5) . . ?
C64 C62 C63 109.9(6) . . ?
O61 C62 H62 110.7 . . ?
C64 C62 H62 110.7 . . ?
C63 C62 H62 110.7 . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
O61 C65 C67 110.3(6) . . ?
O61 C65 C66 108.3(5) . . ?
C67 C65 C66 112.4(6) . . ?
O61 C65 H65 108.6 . . ?
C67 C65 H65 108.6 . . ?
C66 C65 H65 108.6 . . ?
C65 C66 H66A 109.5 . . ?
C65 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C65 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C65 C67 H67A 109.5 . . ?
C65 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C65 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
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 O31 1.7921(15) . ?
Ti1 O41 1.8195(16) . ?
Ti1 O16 1.8293(7) . ?
Ti1 O21 2.0940(15) . ?
Ti1 O1 2.1801(15) . ?
Ti1 O2 2.2274(15) 2_656 ?
Ti1 Ti2 3.3510(5) . ?
Ti2 O61 1.778(2) . ?
Ti2 O51 1.7819(19) . ?
Ti2 O3 1.8773(16) . ?
Ti2 O21 1.9695(16) . ?
Ti2 O1 2.0651(15) . ?
O1 C2 1.299(2) . ?
O2 C2 1.226(3) . ?
C2 C3 1.542(3) . ?
C3 O3 1.393(3) . ?
C3 C15 1.523(3) . ?
C3 C4 1.530(3) . ?
C4 C5 1.385(3) . ?
C4 C9 1.395(3) . ?
C5 C6 1.396(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.390(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.387(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.399(3) . ?
C8 H8 0.9500 . ?
C9 C10 1.468(3) . ?
C10 C11 1.387(3) . ?
C10 C15 1.408(3) . ?
C11 C12 1.382(4) . ?
C11 H11 0.9500 . ?
C12 C13 1.392(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.399(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.372(3) . ?
C14 H14 0.9500 . ?
O21 C22 1.448(3) . ?
C22 C23 1.512(4) . ?
C22 C24 1.513(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
O31 C32 1.425(3) . ?
C32 C33 1.509(3) . ?
C32 C34 1.516(4) . ?
C32 H32 1.0000 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
O41 C42 1.430(3) . ?
C42 C43 1.511(4) . ?
C42 C44 1.515(4) . ?
C42 H42 1.0000 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O51 C52 1.440(4) . ?
C52 C54 1.501(5) . ?
C52 C53 1.518(5) . ?
C52 H52 1.0000 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O61 C62 1.399(6) . ?
O61 C65 1.435(7) . ?
C62 C64 1.511(10) . ?
C62 C63 1.528(9) . ?
C62 H62 1.0000 . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 C67 1.487(9) . ?
C65 C66 1.505(9) . ?
C65 H65 1.0000 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O31 Ti1 O16 Ti1 136.24(5) . . . 2_656 ?
O41 Ti1 O16 Ti1 -122.80(5) . . . 2_656 ?
O21 Ti1 O16 Ti1 -8.23(9) . . . 2_656 ?
O1 Ti1 O16 Ti1 -32.00(4) . . . 2_656 ?
O2 Ti1 O16 Ti1 52.45(4) 2_656 . . 2_656 ?
Ti2 Ti1 O16 Ti1 -34.68(3) . . . 2_656 ?
Ti1 O2 C2 O1 -7.2(3) 2_656 . . . ?
Ti1 O2 C2 C3 171.56(14) 2_656 . . . ?
Ti2 O1 C2 O2 -171.56(16) . . . . ?
Ti1 O1 C2 O2 47.7(3) . . . . ?
Ti2 O1 C2 C3 9.6(2) . . . . ?
Ti1 O1 C2 C3 -131.12(15) . . . . ?
O2 C2 C3 O3 173.6(2) . . . . ?
O1 C2 C3 O3 -7.5(2) . . . . ?
O2 C2 C3 C15 47.3(3) . . . . ?
O1 C2 C3 C15 -133.80(19) . . . . ?
O2 C2 C3 C4 -62.6(3) . . . . ?
O1 C2 C3 C4 116.24(19) . . . . ?
C15 C3 O3 Ti2 125.93(17) . . . . ?
C4 C3 O3 Ti2 -116.69(18) . . . . ?
C2 C3 O3 Ti2 2.4(2) . . . . ?
O61 Ti2 O3 C3 -103.75(18) . . . . ?
O51 Ti2 O3 C3 146.09(18) . . . . ?
O21 Ti2 O3 C3 36.3(2) . . . . ?
O1 Ti2 O3 C3 1.76(16) . . . . ?
Ti1 Ti2 O3 C3 25.77(18) . . . . ?
O3 C3 C4 C5 51.2(3) . . . . ?
C15 C3 C4 C5 176.0(2) . . . . ?
C2 C3 C4 C5 -68.1(3) . . . . ?
O3 C3 C4 C9 -130.7(2) . . . . ?
C15 C3 C4 C9 -6.0(2) . . . . ?
C2 C3 C4 C9 110.0(2) . . . . ?
C9 C4 C5 C6 0.8(4) . . . . ?
C3 C4 C5 C6 178.6(2) . . . . ?
C4 C5 C6 C7 -2.0(4) . . . . ?
C5 C6 C7 C8 1.9(4) . . . . ?
C6 C7 C8 C9 -0.6(4) . . . . ?
C5 C4 C9 C8 0.6(4) . . . . ?
C3 C4 C9 C8 -177.7(2) . . . . ?
C5 C4 C9 C10 -178.0(2) . . . . ?
C3 C4 C9 C10 3.8(3) . . . . ?
C7 C8 C9 C4 -0.7(4) . . . . ?
C7 C8 C9 C10 177.5(2) . . . . ?
C4 C9 C10 C11 177.7(3) . . . . ?
C8 C9 C10 C11 -0.7(4) . . . . ?
C4 C9 C10 C15 0.3(3) . . . . ?
C8 C9 C10 C15 -178.1(2) . . . . ?
C15 C10 C11 C12 0.2(4) . . . . ?
C9 C10 C11 C12 -176.9(3) . . . . ?
C10 C11 C12 C13 0.8(4) . . . . ?
C11 C12 C13 C14 -1.1(4) . . . . ?
C12 C13 C14 C15 0.4(4) . . . . ?
C13 C14 C15 C10 0.6(4) . . . . ?
C13 C14 C15 C3 -178.2(2) . . . . ?
C11 C10 C15 C14 -0.9(4) . . . . ?
C9 C10 C15 C14 176.8(2) . . . . ?
C11 C10 C15 C3 178.0(2) . . . . ?
C9 C10 C15 C3 -4.3(3) . . . . ?
O3 C3 C15 C14 -50.5(3) . . . . ?
C4 C3 C15 C14 -175.0(2) . . . . ?
C2 C3 C15 C14 71.5(3) . . . . ?
O3 C3 C15 C10 130.6(2) . . . . ?
C4 C3 C15 C10 6.1(2) . . . . ?
C2 C3 C15 C10 -107.4(2) . . . . ?
Ti2 O21 C22 C23 -117.73(19) . . . . ?
Ti1 O21 C22 C23 54.5(3) . . . . ?
Ti2 O21 C22 C24 117.7(2) . . . . ?
Ti1 O21 C22 C24 -70.1(3) . . . . ?
O41 Ti1 O31 C32 -130.1(2) . . . . ?
O16 Ti1 O31 C32 -26.5(2) . . . . ?
O21 Ti1 O31 C32 136.4(2) . . . . ?
O1 Ti1 O31 C32 91.4(3) . . . . ?
O2 Ti1 O31 C32 57.6(2) 2_656 . . . ?
Ti2 Ti1 O31 C32 142.40(17) . . . . ?
Ti1 O31 C32 C33 -126.3(2) . . . . ?
Ti1 O31 C32 C34 110.4(2) . . . . ?
O31 Ti1 O41 C42 21.8(2) . . . . ?
O16 Ti1 O41 C42 -81.1(2) . . . . ?
O21 Ti1 O41 C42 125.5(2) . . . . ?
O1 Ti1 O41 C42 -166.9(2) . . . . ?
Ti2 Ti1 O41 C42 157.5(2) . . . . ?
Ti1 O41 C42 C43 -138.5(2) . . . . ?
Ti1 O41 C42 C44 98.2(3) . . . . ?
O61 Ti2 O51 C52 -177.3(3) . . . . ?
O3 Ti2 O51 C52 -68.3(3) . . . . ?
O21 Ti2 O51 C52 76.6(3) . . . . ?
O1 Ti2 O51 C52 7.3(4) . . . . ?
Ti1 Ti2 O51 C52 45.1(3) . . . . ?
Ti2 O51 C52 C54 80.5(4) . . . . ?
Ti2 O51 C52 C53 -156.1(2) . . . . ?
O51 Ti2 O61 C62 -42.1(16) . . . . ?
O3 Ti2 O61 C62 -143.7(16) . . . . ?
O21 Ti2 O61 C62 59.8(16) . . . . ?
O1 Ti2 O61 C62 135.0(16) . . . . ?
Ti1 Ti2 O61 C62 93.9(16) . . . . ?
O51 Ti2 O61 C65 62.3(6) . . . . ?
O3 Ti2 O61 C65 -39.3(6) . . . . ?
O21 Ti2 O61 C65 164.2(6) . . . . ?
O1 Ti2 O61 C65 -120.6(6) . . . . ?
Ti1 Ti2 O61 C65 -161.8(5) . . . . ?
Ti2 O61 C62 C64 6(2) . . . . ?
Ti2 O61 C62 C63 124.6(15) . . . . ?
Ti2 O61 C65 C67 -112.1(6) . . . . ?
Ti2 O61 C65 C66 124.5(5) . . . . ?
