#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:29:59 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179973 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/67/7026719.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_7026719
loop_
_publ_author_name
'Heinz, Philipp'
'Puchberger, Michael'
'Bendova, Maria'
'Baumann, Stefan O.'
'Schubert, Ulrich'
_publ_section_title
;
 Clusters for alkyne-azide click reactions.
;
_journal_issue                   33
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7640
_journal_page_last               7644
_journal_paper_doi               10.1039/c0dt00618a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C64 H96 O28 Ti6'
_chemical_formula_sum            'C64 H96 O28 Ti6'
_chemical_formula_weight         1600.81
_chemical_name_systematic
;
?
;
_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                109.084(1)
_cell_angle_beta                 110.319(1)
_cell_angle_gamma                102.308(1)
_cell_formula_units_Z            1
_cell_length_a                   11.5840(6)
_cell_length_b                   14.1246(7)
_cell_length_c                   14.1278(7)
_cell_measurement_reflns_used    4341
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.1835
_cell_measurement_theta_min      2.5605
_cell_volume                     1904.32(17)
_computing_cell_refinement       'Bruker-AXS SAINT Software'
_computing_data_collection       'Bruker-AXS SMART Software'
_computing_data_reduction        'Bruker-AXS SAINT Software'
_computing_molecular_graphics    'Bruker-AXS SHELXTL Software'
_computing_publication_material  'Bruker-AXS SHELXTL Software'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'Bruker-AXS APEX CCD Detector'
_diffrn_measurement_method       omega-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  0.0238
_diffrn_reflns_av_sigmaI/netI    0.0498
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12595
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.97
_diffrn_standards_interval_time  15
_exptl_absorpt_coefficient_mu    0.676
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.759
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.396
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     473
_refine_ls_number_reflns         8611
_refine_ls_number_restraints     91
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0442
_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)+(0.0683P)²+0.4533P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                6896
_reflns_number_total             8611
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            c0dt00618a.txt
_cod_data_source_block           mb049
_cod_database_code               7026719
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.47102(4) 0.62856(3) 0.41539(3) 0.01333(10) Uani 1 1 d . A .
Ti2 Ti 0.45048(4) 0.37041(3) 0.32696(3) 0.01284(10) Uani 1 1 d . . .
Ti3 Ti 0.40886(4) 0.14265(3) 0.31948(3) 0.01516(11) Uani 1 1 d . . .
O1 O 0.52985(15) 0.69384(12) 0.57226(13) 0.0141(3) Uani 1 1 d . . .
O2 O 0.52520(15) 0.51166(13) 0.41031(13) 0.0140(3) Uani 1 1 d . . .
O11 O 0.48402(17) 0.87816(13) 0.54602(14) 0.0205(4) Uani 1 1 d . . .
O12 O 0.36283(16) 0.72430(13) 0.38905(14) 0.0196(4) Uani 1 1 d . . .
C11 C 0.3938(2) 0.82315(19) 0.4462(2) 0.0185(5) Uani 1 1 d . . .
C12 C 0.3230(3) 0.8845(2) 0.3937(2) 0.0302(6) Uani 1 1 d . . .
H11 H 0.3887 0.9402 0.3912 0.036 Uiso 1 1 calc R . .
H12 H 0.2884 0.9224 0.4433 0.036 Uiso 1 1 calc R . .
C13 C 0.2085(3) 0.8179(2) 0.2755(2) 0.0264(6) Uani 1 1 d . . .
H13 H 0.1896 0.8666 0.2404 0.032 Uiso 1 1 calc R . .
H14 H 0.2360 0.7665 0.2299 0.032 Uiso 1 1 calc R . .
C14 C 0.0867(3) 0.7576(2) 0.2730(2) 0.0248(6) Uani 1 1 d . . .
C15 C -0.0127(3) 0.7088(2) 0.2687(2) 0.0314(6) Uani 1 1 d . . .
H15 H -0.0927 0.6695 0.2653 0.038 Uiso 1 1 calc R . .
O21 O 0.28769(15) 0.53630(13) 0.38923(13) 0.0164(3) Uani 1 1 d . . .
O22 O 0.26865(15) 0.36416(13) 0.30901(13) 0.0164(3) Uani 1 1 d . . .
C21 C 0.2215(2) 0.43648(19) 0.33400(19) 0.0155(5) Uani 1 1 d . . .
C22 C 0.0737(2) 0.4010(2) 0.2922(2) 0.0213(5) Uani 1 1 d . . .
H21 H 0.0536 0.4234 0.3569 0.026 Uiso 1 1 calc R . .
H22 H 0.0330 0.3215 0.2508 0.026 Uiso 1 1 calc R . .
C23 C 0.0149(3) 0.4507(2) 0.2149(2) 0.0316(6) Uani 1 1 d . . .
H23 H -0.0778 0.4391 0.2017 0.038 Uiso 1 1 calc R . .
H24 H 0.0652 0.5294 0.2530 0.038 Uiso 1 1 calc R . .
C24 C 0.0168(3) 0.4058(3) 0.1065(3) 0.0347(7) Uani 1 1 d . . .
C25 C 0.0174(3) 0.3690(3) 0.0193(3) 0.0464(9) Uani 1 1 d . . .
H25 H 0.0178 0.3392 -0.0513 0.056 Uiso 1 1 calc R . .
O31 O 0.37993(16) 0.55210(13) 0.23911(13) 0.0182(4) Uani 1 1 d . . .
O32 O 0.40166(16) 0.39166(13) 0.18467(13) 0.0169(3) Uani 1 1 d . . .
C31 C 0.3770(2) 0.46978(19) 0.16716(19) 0.0157(5) Uani 1 1 d . . .
C32 C 0.3459(2) 0.4611(2) 0.05088(19) 0.0187(5) Uani 1 1 d . . .
H31 H 0.2726 0.3916 -0.0049 0.022 Uiso 1 1 calc R . .
H32 H 0.4245 0.4606 0.0380 0.022 Uiso 1 1 calc R . .
C33 C 0.3070(3) 0.5523(2) 0.0314(2) 0.0227(5) Uani 1 1 d . . .
H33 H 0.2149 0.5401 0.0205 0.027 Uiso 1 1 calc R . .
H34 H 0.3657 0.6215 0.0986 0.027 Uiso 1 1 calc R . .
C34 C 0.3167(2) 0.5591(2) -0.0669(2) 0.0203(5) Uani 1 1 d . . .
C35 C 0.3291(3) 0.5667(2) -0.1442(2) 0.0266(6) Uani 1 1 d . . .
H35 H 0.3390 0.5728 -0.2061 0.032 Uiso 1 1 calc R . .
O41 O 0.61977(16) 0.35916(13) 0.32418(14) 0.0170(3) Uani 1 1 d . . .
O42 O 0.60497(16) 0.20222(13) 0.33441(14) 0.0190(4) Uani 1 1 d . . .
C41 C 0.6673(2) 0.2878(2) 0.33782(19) 0.0176(5) Uani 1 1 d . . .
C42 C 0.8120(2) 0.3139(2) 0.3654(2) 0.0205(5) Uani 1 1 d . . .
H41 H 0.8473 0.3813 0.3602 0.025 Uiso 1 1 calc R . .
H42 H 0.8223 0.2550 0.3112 0.025 Uiso 1 1 calc R . .
C43 C 0.8886(2) 0.3271(2) 0.4848(2) 0.0248(6) Uani 1 1 d . . .
H43 H 0.8665 0.3778 0.5366 0.030 Uiso 1 1 calc R . .
H44 H 0.8609 0.2566 0.4865 0.030 Uiso 1 1 calc R . .
C44 C 1.0322(3) 0.3676(2) 0.5234(2) 0.0251(6) Uani 1 1 d . . .
C45 C 1.1477(3) 0.4001(2) 0.5514(2) 0.0304(6) Uani 1 1 d . . .
H45 H 1.2401 0.4261 0.5737 0.036 Uiso 1 1 calc R . .
O51 O 0.60202(17) 0.71165(14) 0.40636(14) 0.0234(4) Uani 1 1 d DU . .
C51 C 0.6642(4) 0.7215(4) 0.3349(4) 0.0196(11) Uani 0.581(7) 1 d PDU A 1
H51 H 0.6309 0.6511 0.2695 0.023 Uiso 0.581(7) 1 calc PR A 1
H52 H 0.7613 0.7441 0.3773 0.023 Uiso 0.581(7) 1 calc PR A 1
C52 C 0.6322(4) 0.8046(4) 0.2954(4) 0.0202(11) Uani 0.581(7) 1 d PDU A 1
H53 H 0.6746 0.8769 0.3598 0.024 Uiso 0.581(7) 1 calc PR A 1
H54 H 0.5352 0.7866 0.2606 0.024 Uiso 0.581(7) 1 calc PR A 1
C53 C 0.6845(14) 0.8042(9) 0.2092(11) 0.030(3) Uani 0.581(7) 1 d PDU A 1
H55 H 0.6659 0.8583 0.1833 0.046 Uiso 0.581(7) 1 calc PR A 1
H56 H 0.6406 0.7328 0.1451 0.046 Uiso 0.581(7) 1 calc PR A 1
H57 H 0.7803 0.8214 0.2441 0.046 Uiso 0.581(7) 1 calc PR A 1
C51A C 0.6047(7) 0.7754(6) 0.3427(6) 0.0331(19) Uani 0.419(7) 1 d PDU A 2
H51A H 0.6439 0.8535 0.3936 0.040 Uiso 0.419(7) 1 calc PR A 2
H52A H 0.5141 0.7582 0.2863 0.040 Uiso 0.419(7) 1 calc PR A 2
C52A C 0.6896(8) 0.7444(8) 0.2859(8) 0.048(2) Uani 0.419(7) 1 d PDU A 2
H53A H 0.6533 0.6653 0.2405 0.058 Uiso 0.419(7) 1 calc PR A 2
H54A H 0.7809 0.7653 0.3435 0.058 Uiso 0.419(7) 1 calc PR A 2
C53A C 0.693(3) 0.801(2) 0.2095(18) 0.075(7) Uani 0.419(7) 1 d PDU A 2
H55A H 0.7497 0.7816 0.1751 0.112 Uiso 0.419(7) 1 calc PR A 2
H56A H 0.7275 0.8792 0.2544 0.112 Uiso 0.419(7) 1 calc PR A 2
H57A H 0.6027 0.7779 0.1506 0.112 Uiso 0.419(7) 1 calc PR A 2
O61 O 0.36152(16) 0.21001(13) 0.21737(13) 0.0164(3) Uani 1 1 d . . .
C61 C 0.1467(3) 0.1459(3) 0.0576(3) 0.0427(8) Uani 1 1 d . . .
H61 H 0.1413 0.2174 0.0905 0.051 Uiso 1 1 calc R . .
H62 H 0.1027 0.0983 0.0831 0.051 Uiso 1 1 calc R . .
C62 C 0.2907(3) 0.1574(2) 0.0974(2) 0.0293(6) Uani 1 1 d . . .
H63 H 0.2958 0.0851 0.0694 0.035 Uiso 1 1 calc R . .
H64 H 0.3323 0.1996 0.0661 0.035 Uiso 1 1 calc R . .
C63 C 0.0760(4) 0.0985(3) -0.0701(3) 0.0559(10) Uani 1 1 d . . .
H65 H 0.1096 0.1512 -0.0944 0.084 Uiso 1 1 calc R . .
H66 H -0.0194 0.0809 -0.0955 0.084 Uiso 1 1 calc R . .
H67 H 0.0923 0.0330 -0.1024 0.084 Uiso 1 1 calc R . .
O71 O 0.25534(16) 0.10327(14) 0.32357(14) 0.0206(4) Uani 1 1 d . . .
C71 C 0.1535(2) 0.1317(2) 0.3452(2) 0.0230(5) Uani 1 1 d . . .
H71 H 0.0892 0.1324 0.2778 0.028 Uiso 1 1 calc R . .
H72 H 0.1923 0.2049 0.4076 0.028 Uiso 1 1 calc R . .
C72 C 0.0827(3) 0.0516(2) 0.3759(2) 0.0281(6) Uani 1 1 d . . .
H73 H 0.1471 0.0522 0.4442 0.034 Uiso 1 1 calc R . .
H74 H 0.0464 -0.0218 0.3142 0.034 Uiso 1 1 calc R . .
C73 C -0.0296(3) 0.0783(3) 0.3970(3) 0.0405(8) Uani 1 1 d . . .
H75 H 0.0060 0.1513 0.4576 0.061 Uiso 1 1 calc R . .
H76 H -0.0711 0.0265 0.4187 0.061 Uiso 1 1 calc R . .
H77 H -0.0956 0.0744 0.3284 0.061 Uiso 1 1 calc R . .
O81 O 0.38884(17) 0.01558(14) 0.21767(14) 0.0222(4) Uani 1 1 d . . .
C81 C 0.4632(3) -0.0304(3) 0.1690(3) 0.0445(9) Uani 1 1 d . . .
H81 H 0.5365 -0.0353 0.2272 0.053 Uiso 1 1 calc R . .
H82 H 0.5028 0.0174 0.1415 0.053 Uiso 1 1 calc R . .
C82 C 0.3813(4) -0.1405(3) 0.0734(3) 0.0558(10) Uani 1 1 d . . .
H83 H 0.4404 -0.1694 0.0463 0.067 Uiso 1 1 calc R . .
H84 H 0.3448 -0.1882 0.1024 0.067 Uiso 1 1 calc R . .
C83 C 0.2702(4) -0.1464(3) -0.0236(3) 0.0543(10) Uani 1 1 d . . .
H85 H 0.2093 -0.1199 0.0013 0.082 Uiso 1 1 calc R . .
H86 H 0.2228 -0.2214 -0.0809 0.082 Uiso 1 1 calc R . .
H87 H 0.3049 -0.1019 -0.0554 0.082 Uiso 1 1 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'
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
O51 Ti1 O2 99.91(8) . .
O51 Ti1 O1 100.01(7) . .
O2 Ti1 O1 96.24(7) . .
O51 Ti1 O12 90.80(8) . .
O2 Ti1 O12 164.48(7) . .
O1 Ti1 O12 92.89(7) . .
O51 Ti1 O21 164.76(7) . .
O2 Ti1 O21 88.97(7) . .
O1 Ti1 O21 91.22(7) . .
O12 Ti1 O21 78.28(7) . .
O51 Ti1 O31 86.34(7) . .
O2 Ti1 O31 86.81(7) . .
O1 Ti1 O31 172.33(7) . .
O12 Ti1 O31 82.66(7) . .
O21 Ti1 O31 81.78(7) . .
O51 Ti1 Ti2 112.20(6) . .
O2 Ti1 Ti2 21.81(5) . .
O1 Ti1 Ti2 110.39(5) . .
O12 Ti1 Ti2 142.73(5) . .
O21 Ti1 Ti2 72.72(5) . .
O31 Ti1 Ti2 70.60(5) . .
O2 Ti2 O1 106.69(7) . 2_666
O2 Ti2 O22 94.01(7) . .
O1 Ti2 O22 92.05(7) 2_666 .
O2 Ti2 O41 92.80(7) . .
O1 Ti2 O41 89.73(7) 2_666 .
O22 Ti2 O41 172.16(7) . .
O2 Ti2 O32 90.66(7) . .
O1 Ti2 O32 162.64(7) 2_666 .
O22 Ti2 O32 86.56(7) . .
O41 Ti2 O32 89.47(7) . .
O2 Ti2 O61 174.47(7) . .
O1 Ti2 O61 78.82(7) 2_666 .
O22 Ti2 O61 86.23(7) . .
O41 Ti2 O61 86.63(7) . .
O32 Ti2 O61 83.83(7) . .
O2 Ti2 Ti3 147.11(5) . .
O1 Ti2 Ti3 41.37(5) 2_666 .
O22 Ti2 Ti3 94.74(5) . .
O41 Ti2 Ti3 81.58(5) . .
O32 Ti2 Ti3 121.47(5) . .
O61 Ti2 Ti3 38.21(5) . .
O2 Ti2 Ti1 23.18(5) . .
O1 Ti2 Ti1 119.47(5) 2_666 .
O22 Ti2 Ti1 74.82(5) . .
O41 Ti2 Ti1 110.84(5) . .
O32 Ti2 Ti1 76.85(5) . .
O61 Ti2 Ti1 153.52(5) . .
Ti3 Ti2 Ti1 158.926(17) . .
O71 Ti3 O81 98.85(8) . .
O71 Ti3 O61 98.28(8) . .
O81 Ti3 O61 97.43(7) . .
O71 Ti3 O11 96.35(8) . 2_666
O81 Ti3 O11 94.44(8) . 2_666
O61 Ti3 O11 159.48(7) . 2_666
O71 Ti3 O1 95.15(7) . 2_666
O81 Ti3 O1 165.34(7) . 2_666
O61 Ti3 O1 76.14(6) . 2_666
O11 Ti3 O1 88.30(6) 2_666 2_666
O71 Ti3 O42 173.55(7) . .
O81 Ti3 O42 86.44(7) . .
O61 Ti3 O42 84.62(7) . .
O11 Ti3 O42 79.47(7) 2_666 .
O1 Ti3 O42 79.90(6) 2_666 .
O71 Ti3 Ti2 104.16(6) . .
O81 Ti3 Ti2 133.67(6) . .
O61 Ti3 Ti2 40.16(5) . .
O11 Ti3 Ti2 121.72(5) 2_666 .
O1 Ti3 Ti2 36.71(4) 2_666 .
O42 Ti3 Ti2 74.34(5) . .
Ti1 O1 Ti2 129.34(9) . 2_666
Ti1 O1 Ti3 128.73(8) . 2_666
Ti2 O1 Ti3 101.92(7) 2_666 2_666
Ti2 O2 Ti1 135.02(9) . .
C11 O11 Ti3 139.93(16) . 2_666
C11 O12 Ti1 128.60(15) . .
O12 C11 O11 125.0(2) . .
O12 C11 C12 119.3(2) . .
O11 C11 C12 115.7(2) . .
C11 C12 C13 116.2(2) . .
C11 C12 H11 108.2 . .
C13 C12 H11 108.2 . .
C11 C12 H12 108.2 . .
C13 C12 H12 108.2 . .
H11 C12 H12 107.4 . .
C14 C13 C12 113.7(2) . .
C14 C13 H13 108.8 . .
C12 C13 H13 108.8 . .
C14 C13 H14 108.8 . .
C12 C13 H14 108.8 . .
H13 C13 H14 107.7 . .
C15 C14 C13 178.6(3) . .
C14 C15 H15 180.0 . .
C21 O21 Ti1 131.32(15) . .
C21 O22 Ti2 132.64(15) . .
O21 C21 O22 125.4(2) . .
O21 C21 C22 117.0(2) . .
O22 C21 C22 117.6(2) . .
C21 C22 C23 110.6(2) . .
C21 C22 H21 109.5 . .
C23 C22 H21 109.5 . .
C21 C22 H22 109.5 . .
C23 C22 H22 109.5 . .
H21 C22 H22 108.1 . .
C24 C23 C22 113.4(2) . .
C24 C23 H23 108.9 . .
C22 C23 H23 108.9 . .
C24 C23 H24 108.9 . .
C22 C23 H24 108.9 . .
H23 C23 H24 107.7 . .
C25 C24 C23 179.4(4) . .
C24 C25 H25 180.0 . .
C31 O31 Ti1 134.50(15) . .
C31 O32 Ti2 129.37(15) . .
O31 C31 O32 125.0(2) . .
O31 C31 C32 119.1(2) . .
O32 C31 C32 115.9(2) . .
C31 C32 C33 113.8(2) . .
C31 C32 H31 108.8 . .
C33 C32 H31 108.8 . .
C31 C32 H32 108.8 . .
C33 C32 H32 108.8 . .
H31 C32 H32 107.7 . .
C34 C33 C32 111.5(2) . .
C34 C33 H33 109.3 . .
C32 C33 H33 109.3 . .
C34 C33 H34 109.3 . .
C32 C33 H34 109.3 . .
H33 C33 H34 108.0 . .
C35 C34 C33 177.8(3) . .
C34 C35 H35 180.0 . .
C41 O41 Ti2 126.74(15) . .
C41 O42 Ti3 131.13(15) . .
O42 C41 O41 125.0(2) . .
O42 C41 C42 118.6(2) . .
O41 C41 C42 116.4(2) . .
C41 C42 C43 108.86(19) . .
C41 C42 H41 109.9 . .
C43 C42 H41 109.9 . .
C41 C42 H42 109.9 . .
C43 C42 H42 109.9 . .
H41 C42 H42 108.3 . .
C44 C43 C42 111.9(2) . .
C44 C43 H43 109.2 . .
C42 C43 H43 109.2 . .
C44 C43 H44 109.2 . .
C42 C43 H44 109.2 . .
H43 C43 H44 107.9 . .
C45 C44 C43 177.9(3) . .
C44 C45 H45 180.0 . .
C51 O51 C51A 45.7(3) . .
C51 O51 Ti1 144.9(2) . .
C51A O51 Ti1 132.8(3) . .
O51 C51 C52 108.9(3) . .
O51 C51 H51 109.9 . .
C52 C51 H51 109.9 . .
O51 C51 H52 109.9 . .
C52 C51 H52 109.9 . .
H51 C51 H52 108.3 . .
C51 C52 C53 108.1(5) . .
C51 C52 H53 110.1 . .
C53 C52 H53 110.1 . .
C51 C52 H54 110.1 . .
C53 C52 H54 110.1 . .
H53 C52 H54 108.4 . .
C52 C53 H55 109.5 . .
C52 C53 H56 109.5 . .
H55 C53 H56 109.5 . .
C52 C53 H57 109.5 . .
H55 C53 H57 109.5 . .
H56 C53 H57 109.5 . .
O51 C51A C52A 105.5(5) . .
O51 C51A H51A 110.6 . .
C52A C51A H51A 110.6 . .
O51 C51A H52A 110.6 . .
C52A C51A H52A 110.6 . .
H51A C51A H52A 108.8 . .
C51A C52A C53A 110.5(11) . .
C51A C52A H53A 109.6 . .
C53A C52A H53A 109.6 . .
C51A C52A H54A 109.6 . .
C53A C52A H54A 109.6 . .
H53A C52A H54A 108.1 . .
C52A C53A H55A 109.5 . .
C52A C53A H56A 109.5 . .
H55A C53A H56A 109.5 . .
C52A C53A H57A 109.5 . .
H55A C53A H57A 109.5 . .
H56A C53A H57A 109.5 . .
C62 O61 Ti3 127.46(15) . .
C62 O61 Ti2 130.79(15) . .
Ti3 O61 Ti2 101.63(7) . .
C62 C61 C63 110.2(3) . .
C62 C61 H61 109.6 . .
C63 C61 H61 109.6 . .
C62 C61 H62 109.6 . .
C63 C61 H62 109.6 . .
H61 C61 H62 108.1 . .
O61 C62 C61 111.1(2) . .
O61 C62 H63 109.4 . .
C61 C62 H63 109.4 . .
O61 C62 H64 109.4 . .
C61 C62 H64 109.4 . .
H63 C62 H64 108.0 . .
C61 C63 H65 109.5 . .
C61 C63 H66 109.5 . .
H65 C63 H66 109.5 . .
C61 C63 H67 109.5 . .
H65 C63 H67 109.5 . .
H66 C63 H67 109.5 . .
C71 O71 Ti3 149.23(16) . .
O71 C71 C72 110.4(2) . .
O71 C71 H71 109.6 . .
C72 C71 H71 109.6 . .
O71 C71 H72 109.6 . .
C72 C71 H72 109.6 . .
H71 C71 H72 108.1 . .
C71 C72 C73 111.7(2) . .
C71 C72 H73 109.3 . .
C73 C72 H73 109.3 . .
C71 C72 H74 109.3 . .
C73 C72 H74 109.3 . .
H73 C72 H74 107.9 . .
C72 C73 H75 109.5 . .
C72 C73 H76 109.5 . .
H75 C73 H76 109.5 . .
C72 C73 H77 109.5 . .
H75 C73 H77 109.5 . .
H76 C73 H77 109.5 . .
C81 O81 Ti3 138.94(18) . .
O81 C81 C82 112.7(3) . .
O81 C81 H81 109.1 . .
C82 C81 H81 109.1 . .
O81 C81 H82 109.1 . .
C82 C81 H82 109.1 . .
H81 C81 H82 107.8 . .
C83 C82 C81 115.9(3) . .
C83 C82 H83 108.3 . .
C81 C82 H83 108.3 . .
C83 C82 H84 108.3 . .
C81 C82 H84 108.3 . .
H83 C82 H84 107.4 . .
C82 C83 H85 109.5 . .
C82 C83 H86 109.5 . .
H85 C83 H86 109.5 . .
C82 C83 H87 109.5 . .
H85 C83 H87 109.5 . .
H86 C83 H87 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti1 O51 1.7803(17) .
Ti1 O2 1.8764(16) .
Ti1 O1 1.8904(16) .
Ti1 O12 2.0655(17) .
Ti1 O21 2.0748(16) .
Ti1 O31 2.1006(16) .
Ti1 Ti2 3.3701(6) .
Ti2 O2 1.7709(16) .
Ti2 O1 1.9001(16) 2_666
Ti2 O22 2.0109(16) .
Ti2 O41 2.0136(16) .
Ti2 O32 2.0317(16) .
Ti2 O61 2.0481(16) .
Ti2 Ti3 3.1103(6) .
Ti3 O71 1.7737(17) .
Ti3 O81 1.8019(17) .
Ti3 O61 1.9641(16) .
Ti3 O11 2.0297(17) 2_666
Ti3 O1 2.1010(16) 2_666
Ti3 O42 2.1562(17) .
O1 Ti2 1.9001(16) 2_666
O1 Ti3 2.1010(16) 2_666
O11 C11 1.265(3) .
O11 Ti3 2.0297(17) 2_666
O12 C11 1.256(3) .
C11 C12 1.508(3) .
C12 C13 1.528(4) .
C12 H11 0.9900 .
C12 H12 0.9900 .
C13 C14 1.466(4) .
C13 H13 0.9900 .
C13 H14 0.9900 .
C14 C15 1.179(4) .
C15 H15 0.9500 .
O21 C21 1.260(3) .
O22 C21 1.266(3) .
C21 C22 1.506(3) .
C22 C23 1.529(4) .
C22 H21 0.9900 .
C22 H22 0.9900 .
C23 C24 1.464(4) .
C23 H23 0.9900 .
C23 H24 0.9900 .
C24 C25 1.172(5) .
C25 H25 0.9500 .
O31 C31 1.254(3) .
O32 C31 1.275(3) .
C31 C32 1.511(3) .
C32 C33 1.527(3) .
C32 H31 0.9900 .
C32 H32 0.9900 .
C33 C34 1.464(3) .
C33 H33 0.9900 .
C33 H34 0.9900 .
C34 C35 1.184(4) .
C35 H35 0.9500 .
O41 C41 1.284(3) .
O42 C41 1.245(3) .
C41 C42 1.512(3) .
C42 C43 1.533(3) .
C42 H41 0.9900 .
C42 H42 0.9900 .
C43 C44 1.466(4) .
C43 H43 0.9900 .
C43 H44 0.9900 .
C44 C45 1.188(4) .
C45 H45 0.9500 .
O51 C51 1.454(4) .
O51 C51A 1.469(7) .
C51 C52 1.515(6) .
C51 H51 0.9900 .
C51 H52 0.9900 .
C52 C53 1.537(9) .
C52 H53 0.9900 .
C52 H54 0.9900 .
C53 H55 0.9800 .
C53 H56 0.9800 .
C53 H57 0.9800 .
C51A C52A 1.519(10) .
C51A H51A 0.9900 .
C51A H52A 0.9900 .
C52A C53A 1.543(14) .
C52A H53A 0.9900 .
C52A H54A 0.9900 .
C53A H55A 0.9800 .
C53A H56A 0.9800 .
C53A H57A 0.9800 .
O61 C62 1.432(3) .
C61 C62 1.516(4) .
C61 C63 1.524(4) .
C61 H61 0.9900 .
C61 H62 0.9900 .
C62 H63 0.9900 .
C62 H64 0.9900 .
C63 H65 0.9800 .
C63 H66 0.9800 .
C63 H67 0.9800 .
O71 C71 1.420(3) .
C71 C72 1.521(4) .
C71 H71 0.9900 .
C71 H72 0.9900 .
C72 C73 1.526(4) .
C72 H73 0.9900 .
C72 H74 0.9900 .
C73 H75 0.9800 .
C73 H76 0.9800 .
C73 H77 0.9800 .
O81 C81 1.413(3) .
C81 C82 1.500(4) .
C81 H81 0.9900 .
C81 H82 0.9900 .
C82 C83 1.482(5) .
C82 H83 0.9900 .
C82 H84 0.9900 .
C83 H85 0.9800 .
C83 H86 0.9800 .
C83 H87 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
C35 H35 O41 0.95 2.31 3.231(3) 163.1 2_665
C45 H45 O2 0.95 2.58 3.510(3) 167.6 2_766
C45 H45 O41 0.95 2.71 3.287(3) 120.0 2_766
C25 H25 C14 0.95 2.65 3.536(4) 155.9 2_565
C25 H25 C15 0.95 2.90 3.830(4) 167.4 2_565
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
O51 Ti1 Ti2 O2 58.70(14) . .
O1 Ti1 Ti2 O2 -51.91(14) . .
O12 Ti1 Ti2 O2 -177.16(15) . .
O21 Ti1 Ti2 O2 -136.64(14) . .
O31 Ti1 Ti2 O2 136.18(14) . .
O51 Ti1 Ti2 O1 119.92(8) . 2_666
O2 Ti1 Ti2 O1 61.22(14) . 2_666
O1 Ti1 Ti2 O1 9.31(11) . 2_666
O12 Ti1 Ti2 O1 -115.95(10) . 2_666
O21 Ti1 Ti2 O1 -75.42(7) . 2_666
O31 Ti1 Ti2 O1 -162.60(8) . 2_666
O51 Ti1 Ti2 O22 -156.44(8) . .
O2 Ti1 Ti2 O22 144.85(14) . .
O1 Ti1 Ti2 O22 92.95(7) . .
O12 Ti1 Ti2 O22 -32.31(10) . .
O21 Ti1 Ti2 O22 8.22(7) . .
O31 Ti1 Ti2 O22 -78.96(7) . .
O51 Ti1 Ti2 O41 17.84(8) . .
O2 Ti1 Ti2 O41 -40.86(14) . .
O1 Ti1 Ti2 O41 -92.77(7) . .
O12 Ti1 Ti2 O41 141.98(10) . .
O21 Ti1 Ti2 O41 -177.50(7) . .
O31 Ti1 Ti2 O41 95.32(7) . .
O51 Ti1 Ti2 O32 -66.47(8) . .
O2 Ti1 Ti2 O32 -125.17(14) . .
O1 Ti1 Ti2 O32 -177.08(7) . .
O12 Ti1 Ti2 O32 57.66(10) . .
O21 Ti1 Ti2 O32 98.19(7) . .
O31 Ti1 Ti2 O32 11.01(7) . .
O51 Ti1 Ti2 O61 -110.68(12) . .
O2 Ti1 Ti2 O61 -169.39(17) . .
O1 Ti1 Ti2 O61 138.71(12) . .
O12 Ti1 Ti2 O61 13.45(14) . .
O21 Ti1 Ti2 O61 53.98(12) . .
O31 Ti1 Ti2 O61 -33.20(12) . .
O51 Ti1 Ti2 Ti3 141.35(7) . .
O2 Ti1 Ti2 Ti3 82.64(13) . .
O1 Ti1 Ti2 Ti3 30.74(7) . .
O12 Ti1 Ti2 Ti3 -94.52(9) . .
O21 Ti1 Ti2 Ti3 -53.99(7) . .
O31 Ti1 Ti2 Ti3 -141.17(7) . .
O2 Ti2 Ti3 O71 96.60(11) . .
O1 Ti2 Ti3 O71 79.42(9) 2_666 .
O22 Ti2 Ti3 O71 -8.30(7) . .
O41 Ti2 Ti3 O71 178.67(8) . .
O32 Ti2 Ti3 O71 -97.16(8) . .
O61 Ti2 Ti3 O71 -86.06(9) . .
Ti1 Ti2 Ti3 O71 50.65(8) . .
O2 Ti2 Ti3 O81 -145.99(12) . .
O1 Ti2 Ti3 O81 -163.18(11) 2_666 .
O22 Ti2 Ti3 O81 109.10(9) . .
O41 Ti2 Ti3 O81 -63.93(9) . .
O32 Ti2 Ti3 O81 20.24(10) . .
O61 Ti2 Ti3 O81 31.34(11) . .
Ti1 Ti2 Ti3 O81 168.05(8) . .
O2 Ti2 Ti3 O61 -177.34(12) . .
O1 Ti2 Ti3 O61 165.48(10) 2_666 .
O22 Ti2 Ti3 O61 77.76(9) . .
O41 Ti2 Ti3 O61 -95.27(9) . .
O32 Ti2 Ti3 O61 -11.10(9) . .
Ti1 Ti2 Ti3 O61 136.71(9) . .
O2 Ti2 Ti3 O11 -10.26(12) . 2_666
O1 Ti2 Ti3 O11 -27.44(9) 2_666 2_666
O22 Ti2 Ti3 O11 -115.16(8) . 2_666
O41 Ti2 Ti3 O11 71.81(8) . 2_666
O32 Ti2 Ti3 O11 155.98(8) . 2_666
O61 Ti2 Ti3 O11 167.08(10) . 2_666
Ti1 Ti2 Ti3 O11 -56.21(8) . 2_666
O2 Ti2 Ti3 O1 17.18(12) . 2_666
O22 Ti2 Ti3 O1 -87.72(9) . 2_666
O41 Ti2 Ti3 O1 99.25(9) . 2_666
O32 Ti2 Ti3 O1 -176.58(9) . 2_666
O61 Ti2 Ti3 O1 -165.48(10) . 2_666
Ti1 Ti2 Ti3 O1 -28.77(8) . 2_666
O2 Ti2 Ti3 O42 -76.90(11) . .
O1 Ti2 Ti3 O42 -94.09(9) 2_666 .
O22 Ti2 Ti3 O42 178.19(7) . .
O41 Ti2 Ti3 O42 5.16(7) . .
O32 Ti2 Ti3 O42 89.34(7) . .
O61 Ti2 Ti3 O42 100.43(9) . .
Ti1 Ti2 Ti3 O42 -122.86(6) . .
O51 Ti1 O1 Ti2 -128.85(11) . 2_666
O2 Ti1 O1 Ti2 -27.60(12) . 2_666
O12 Ti1 O1 Ti2 139.83(11) . 2_666
O21 Ti1 O1 Ti2 61.50(11) . 2_666
O31 Ti1 O1 Ti2 85.5(5) . 2_666
Ti2 Ti1 O1 Ti2 -10.49(12) . 2_666
O51 Ti1 O1 Ti3 50.95(12) . 2_666
O2 Ti1 O1 Ti3 152.21(10) . 2_666
O12 Ti1 O1 Ti3 -40.37(11) . 2_666
O21 Ti1 O1 Ti3 -118.69(10) . 2_666
O31 Ti1 O1 Ti3 -94.7(5) . 2_666
Ti2 Ti1 O1 Ti3 169.31(8) . 2_666
O1 Ti2 O2 Ti1 -127.19(12) 2_666 .
O22 Ti2 O2 Ti1 -33.84(13) . .
O41 Ti2 O2 Ti1 142.25(12) . .
O32 Ti2 O2 Ti1 52.75(13) . .
O61 Ti2 O2 Ti1 58.4(8) . .
Ti3 Ti2 O2 Ti1 -138.95(8) . .
O51 Ti1 O2 Ti2 -126.57(13) . .
O1 Ti1 O2 Ti2 132.09(12) . .
O12 Ti1 O2 Ti2 6.4(3) . .
O21 Ti1 O2 Ti2 40.97(13) . .
O31 Ti1 O2 Ti2 -40.85(13) . .
O51 Ti1 O12 C11 -59.1(2) . .
O2 Ti1 O12 C11 167.0(2) . .
O1 Ti1 O12 C11 40.9(2) . .
O21 Ti1 O12 C11 131.6(2) . .
O31 Ti1 O12 C11 -145.4(2) . .
Ti2 Ti1 O12 C11 170.89(16) . .
Ti1 O12 C11 O11 -17.9(4) . .
Ti1 O12 C11 C12 160.17(19) . .
Ti3 O11 C11 O12 -19.2(4) 2_666 .
Ti3 O11 C11 C12 162.7(2) 2_666 .
O12 C11 C12 C13 5.1(4) . .
O11 C11 C12 C13 -176.6(2) . .
C11 C12 C13 C14 77.1(3) . .
C12 C13 C14 C15 164(13) . .
O51 Ti1 O21 C21 93.1(3) . .
O2 Ti1 O21 C21 -33.0(2) . .
O1 Ti1 O21 C21 -129.2(2) . .
O12 Ti1 O21 C21 138.1(2) . .
O31 Ti1 O21 C21 53.93(19) . .
Ti2 Ti1 O21 C21 -18.22(18) . .
O2 Ti2 O22 C21 9.1(2) . .
O1 Ti2 O22 C21 116.0(2) 2_666 .
O41 Ti2 O22 C21 -141.0(5) . .
O32 Ti2 O22 C21 -81.3(2) . .
O61 Ti2 O22 C21 -165.4(2) . .
Ti3 Ti2 O22 C21 157.34(19) . .
Ti1 Ti2 O22 C21 -4.04(18) . .
Ti1 O21 C21 O22 23.2(3) . .
Ti1 O21 C21 C22 -155.26(16) . .
Ti2 O22 C21 O21 -7.3(3) . .
Ti2 O22 C21 C22 171.13(15) . .
O21 C21 C22 C23 59.6(3) . .
O22 C21 C22 C23 -119.0(2) . .
C21 C22 C23 C24 70.5(3) . .
C22 C23 C24 C25 79(42) . .
O51 Ti1 O31 C31 94.6(2) . .
O2 Ti1 O31 C31 -5.6(2) . .
O1 Ti1 O31 C31 -119.3(5) . .
O12 Ti1 O31 C31 -174.2(2) . .
O21 Ti1 O31 C31 -95.0(2) . .
Ti2 Ti1 O31 C31 -20.5(2) . .
O2 Ti2 O32 C31 -29.1(2) . .
O1 Ti2 O32 C31 150.8(2) 2_666 .
O22 Ti2 O32 C31 64.92(19) . .
O41 Ti2 O32 C31 -121.85(19) . .
O61 Ti2 O32 C31 151.5(2) . .
Ti3 Ti2 O32 C31 158.37(17) . .
Ti1 Ti2 O32 C31 -10.29(18) . .
Ti1 O31 C31 O32 21.4(4) . .
Ti1 O31 C31 C32 -156.76(17) . .
Ti2 O32 C31 O31 0.7(3) . .
Ti2 O32 C31 C32 178.95(15) . .
O31 C31 C32 C33 -6.0(3) . .
O32 C31 C32 C33 175.7(2) . .
C31 C32 C33 C34 162.9(2) . .
C32 C33 C34 C35 -85(7) . .
O2 Ti2 O41 C41 136.10(19) . .
O1 Ti2 O41 C41 29.40(19) 2_666 .
O22 Ti2 O41 C41 -73.7(6) . .
O32 Ti2 O41 C41 -133.26(19) . .
O61 Ti2 O41 C41 -49.41(19) . .
Ti3 Ti2 O41 C41 -11.32(18) . .
Ti1 Ti2 O41 C41 151.04(17) . .
O71 Ti3 O42 C41 -79.5(7) . .
O81 Ti3 O42 C41 135.4(2) . .
O61 Ti3 O42 C41 37.5(2) . .
O11 Ti3 O42 C41 -129.4(2) 2_666 .
O1 Ti3 O42 C41 -39.3(2) 2_666 .
Ti2 Ti3 O42 C41 -2.03(19) . .
Ti3 O42 C41 O41 -5.6(4) . .
Ti3 O42 C41 C42 171.35(15) . .
Ti2 O41 C41 O42 14.1(3) . .
Ti2 O41 C41 C42 -162.89(15) . .
O42 C41 C42 C43 -63.3(3) . .
O41 C41 C42 C43 113.8(2) . .
C41 C42 C43 C44 -171.8(2) . .
C42 C43 C44 C45 -6(9) . .
O2 Ti1 O51 C51 66.7(4) . .
O1 Ti1 O51 C51 164.9(4) . .
O12 Ti1 O51 C51 -102.0(4) . .
O21 Ti1 O51 C51 -58.2(5) . .
O31 Ti1 O51 C51 -19.4(4) . .
Ti2 Ti1 O51 C51 47.9(4) . .
O2 Ti1 O51 C51A 137.1(4) . .
O1 Ti1 O51 C51A -124.7(4) . .
O12 Ti1 O51 C51A -31.6(4) . .
O21 Ti1 O51 C51A 12.2(6) . .
O31 Ti1 O51 C51A 51.0(4) . .
Ti2 Ti1 O51 C51A 118.3(4) . .
C51A O51 C51 C52 1.5(5) . .
Ti1 O51 C51 C52 106.8(4) . .
O51 C51 C52 C53 -173.4(7) . .
C51 O51 C51A C52A 0.4(5) . .
Ti1 O51 C51A C52A -130.5(5) . .
O51 C51A C52A C53A 176.3(12) . .
O71 Ti3 O61 C62 -81.5(2) . .
O81 Ti3 O61 C62 18.6(2) . .
O11 Ti3 O61 C62 143.4(2) 2_666 .
O1 Ti3 O61 C62 -174.8(2) 2_666 .
O42 Ti3 O61 C62 104.3(2) . .
Ti2 Ti3 O61 C62 176.3(2) . .
O71 Ti3 O61 Ti2 102.18(8) . .
O81 Ti3 O61 Ti2 -157.70(8) . .
O11 Ti3 O61 Ti2 -32.9(2) 2_666 .
O1 Ti3 O61 Ti2 8.88(6) 2_666 .
O42 Ti3 O61 Ti2 -72.02(7) . .
O2 Ti2 O61 C62 -11.3(8) . .
O1 Ti2 O61 C62 174.2(2) 2_666 .
O22 Ti2 O61 C62 81.3(2) . .
O41 Ti2 O61 C62 -95.5(2) . .
O32 Ti2 O61 C62 -5.6(2) . .
Ti3 Ti2 O61 C62 -176.1(2) . .
Ti1 Ti2 O61 C62 37.5(3) . .
O2 Ti2 O61 Ti3 164.8(7) . .
O1 Ti2 O61 Ti3 -9.73(7) 2_666 .
O22 Ti2 O61 Ti3 -102.57(8) . .
O41 Ti2 O61 Ti3 80.66(7) . .
O32 Ti2 O61 Ti3 170.49(8) . .
Ti1 Ti2 O61 Ti3 -146.43(7) . .
Ti3 O61 C62 C61 100.3(3) . .
Ti2 O61 C62 C61 -84.5(3) . .
C63 C61 C62 O61 175.2(3) . .
O81 Ti3 O71 C71 -155.4(3) . .
O61 Ti3 O71 C71 -56.5(3) . .
O11 Ti3 O71 C71 109.1(3) 2_666 .
O1 Ti3 O71 C71 20.2(3) 2_666 .
O42 Ti3 O71 C71 59.8(8) . .
Ti2 Ti3 O71 C71 -15.9(3) . .
Ti3 O71 C71 C72 -154.1(2) . .
O71 C71 C72 C73 -178.6(2) . .
O71 Ti3 O81 C81 -174.5(3) . .
O61 Ti3 O81 C81 85.9(3) . .
O11 Ti3 O81 C81 -77.3(3) 2_666 .
O1 Ti3 O81 C81 23.0(5) 2_666 .
O42 Ti3 O81 C81 1.8(3) . .
Ti2 Ti3 O81 C81 66.1(3) . .
Ti3 O81 C81 C82 -171.8(2) . .
O81 C81 C82 C83 61.3(5) . .
