#------------------------------------------------------------------------------
#$Date: 2021-07-25 07:21:25 +0300 (Sun, 25 Jul 2021) $
#$Revision: 267740 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/32/7243266.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_7243266
loop_
_publ_author_name
'Kazimierczuk, Katarzyna'
'Milanesio, Marco'
'Dołęga, Anna'
'Palin, Luca'
'Walencik, Maja'
'Jurkowski, Michał'
'Conterosito, Eleonora'
_publ_section_title
;
 Solvothermal synthesis and structural characterization of three
 polyoxotitanium-organic acid clusters
;
_journal_issue                   40
_journal_name_full               'RSC Advances'
_journal_page_first              25068
_journal_page_last               25078
_journal_paper_doi               10.1039/D0RA09691A
_journal_volume                  11
_journal_year                    2021
_chemical_formula_moiety         'C96 H96 O24 Ti6'
_chemical_formula_sum            'C96 H96 O24 Ti6'
_chemical_formula_weight         1921.12
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_update_record
;
2020-10-09 deposited with the CCDC.	2021-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                107.574(13)
_cell_angle_beta                 92.097(13)
_cell_angle_gamma                105.434(11)
_cell_formula_units_Z            1
_cell_length_a                   12.1900(15)
_cell_length_b                   13.515(2)
_cell_length_c                   15.260(3)
_cell_measurement_reflns_used    20777
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      29.52
_cell_measurement_theta_min      2.5
_cell_measurement_wavelength     0.71073
_cell_volume                     2291.5(7)
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.98
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'parabolic x-ray mirror'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.023
_diffrn_reflns_av_unetI/netI     0.0223
_diffrn_reflns_Laue_measured_fraction_full 0.98
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16107
_diffrn_reflns_point_group_measured_fraction_full 0.98
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.5
_diffrn_reflns_theta_min         2.706
_diffrn_source                   'GeniX Mo, 0.05 x 0.05 mm2 microfocus'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.9317
_exptl_absorpt_correction_T_min  0.8644
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details
;
        Numerical  absorption  correction was  performed
        after the  optimization of  the  crystal-shape
        description due to Herrendorf?s method
        [Herrendorf, 1994]
        Herrendorf,  W. (1994).HABITUS, a program for the
        optimization  of  the  crystal description for
 the numerical absorption correction by means of
        suitable, psi scanned reflections;dissertation
        1994,Karlsruhe;extension 1998,Gießen
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       prism
_exptl_crystal_F_000             996
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.844
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         8379
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0448
_refine_ls_R_factor_gt           0.0384
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0494P)²+2.7446P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0
_reflns_number_gt                7358
_reflns_number_total             8379
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ra09691a2.cif
_cod_data_source_block           III
_cod_original_cell_volume        2291.4(7)
_cod_database_code               7243266
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_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
C1 C 0.23387(18) 0.24359(18) 0.29953(15) 0.0186(4) Uani 1 1 d . . . . .
C2 C 0.15286(18) 0.15938(18) 0.21495(15) 0.0196(4) Uani 1 1 d . . . . .
H2 H 0.072915 0.154332 0.230273 0.024 Uiso 1 1 calc R U . . .
C3 C 0.16779(19) 0.04724(18) 0.19731(16) 0.0222(5) Uani 1 1 d . . . . .
C4 C 0.1256(2) -0.0111(2) 0.25583(19) 0.0323(6) Uani 1 1 d . . . . .
H4 H 0.0854 0.018548 0.304385 0.039 Uiso 1 1 calc R U . . .
C5 C 0.1413(3) -0.1124(2) 0.2447(2) 0.0427(7) Uani 1 1 d . . . . .
H5 H 0.112576 -0.150659 0.285922 0.051 Uiso 1 1 calc R U . . .
C6 C 0.1978(3) -0.1570(2) 0.1744(2) 0.0435(7) Uani 1 1 d . . . . .
H6 H 0.208047 -0.226292 0.166493 0.052 Uiso 1 1 calc R U . . .
C7 C 0.2398(3) -0.1005(2) 0.1153(2) 0.0441(7) Uani 1 1 d . . . . .
H7 H 0.278852 -0.131371 0.066325 0.053 Uiso 1 1 calc R U . . .
C8 C 0.2254(2) 0.0016(2) 0.12665(18) 0.0326(6) Uani 1 1 d . . . . .
H8 H 0.255308 0.039936 0.085739 0.039 Uiso 1 1 calc R U . . .
C9 C 0.1642(2) 0.19937(18) 0.13120(15) 0.0222(5) Uani 1 1 d . . . . .
C10 C 0.2615(2) 0.2769(2) 0.12424(18) 0.0316(6) Uani 1 1 d . . . . .
H10 H 0.324452 0.30571 0.172087 0.038 Uiso 1 1 calc R U . . .
C11 C 0.2670(3) 0.3125(3) 0.0473(2) 0.0423(7) Uani 1 1 d . . . . .
H11 H 0.333716 0.365692 0.043234 0.051 Uiso 1 1 calc R U . . .
C12 C 0.1762(3) 0.2710(3) -0.02309(19) 0.0433(7) Uani 1 1 d . . . . .
H12 H 0.179963 0.296358 -0.074905 0.052 Uiso 1 1 calc R U . . .
C13 C 0.0797(3) 0.1922(2) -0.01751(18) 0.0385(7) Uani 1 1 d . . . . .
H13 H 0.017607 0.162601 -0.066165 0.046 Uiso 1 1 calc R U . . .
C14 C 0.0734(2) 0.1563(2) 0.05909(17) 0.0290(5) Uani 1 1 d . . . . .
H14 H 0.006983 0.102215 0.062424 0.035 Uiso 1 1 calc R U . . .
C15 C 0.5754(2) 0.2953(2) 0.24492(17) 0.0288(6) Uani 1 1 d . . . . .
C16 C 0.5883(2) 0.2163(2) 0.15121(19) 0.0206(9) Uani 0.798(8) 1 d . . P A 1
H16 H 0.512423 0.160235 0.126822 0.025 Uiso 0.798(8) 1 calc R U P A 1
C16A C 0.6749(10) 0.2679(10) 0.1736(7) 0.022(4) Uani 0.202(8) 1 d . . P A 2
H16A H 0.7524 0.321495 0.197092 0.027 Uiso 0.202(8) 1 calc R U P A 2
C17 C 0.6191(2) 0.2763(2) 0.07972(16) 0.0317(6) Uani 1 1 d . . . . .
C18 C 0.5320(3) 0.2410(3) 0.0069(3) 0.0594(9) Uani 1 1 d . . . . .
H18 H 0.464741 0.184191 0.003475 0.071 Uiso 1 1 calc R U . . .
C19 C 0.5457(4) 0.2919(5) -0.0627(3) 0.0876(16) Uani 1 1 d . . . . .
H19 H 0.488133 0.27013 -0.114002 0.105 Uiso 1 1 calc R U . . .
C20 C 0.6490(4) 0.3769(4) -0.0528(3) 0.0707(12) Uani 1 1 d . . . . .
H20 H 0.658559 0.417164 -0.09483 0.085 Uiso 1 1 calc R U . . .
C21 C 0.7314(4) 0.3992(3) 0.0154(3) 0.0659(11) Uani 1 1 d . . . . .
H21 H 0.802888 0.450733 0.018095 0.079 Uiso 1 1 calc R U . . .
C22 C 0.7163(3) 0.3504(3) 0.0809(2) 0.0551(9) Uani 1 1 d . . . . .
H22 H 0.776894 0.369585 0.129348 0.066 Uiso 1 1 calc R U . . .
C23 C 0.6749(2) 0.15871(19) 0.16628(16) 0.0221(5) Uani 1 1 d . . . . .
C25 C 0.7460(3) 0.0026(2) 0.1258(2) 0.0440(7) Uani 1 1 d . . . . .
H25 H 0.739142 -0.068495 0.085676 0.053 Uiso 0.797(4) 1 calc R U P A 1
H25A H 0.807011 -0.023889 0.10113 0.053 Uiso 0.203(4) 1 calc R U P A 2
C24 C 0.6649(3) 0.0553(3) 0.1108(2) 0.0332(8) Uani 0.797(4) 1 d . . P A 1
H24 H 0.603159 0.018853 0.062066 0.04 Uiso 0.797(4) 1 calc R U P A 1
C26 C 0.8318(3) 0.0502(3) 0.1946(2) 0.0323(8) Uani 0.797(4) 1 d . . P A 1
H26 H 0.88438 0.012614 0.204192 0.039 Uiso 0.797(4) 1 calc R U P A 1
C27 C 0.8446(3) 0.1549(3) 0.2526(2) 0.0336(8) Uani 0.797(4) 1 d . . P A 1
H27 H 0.906111 0.189072 0.301683 0.04 Uiso 0.797(4) 1 calc R U P A 1
C28 C 0.7674(3) 0.2096(3) 0.2387(2) 0.0291(7) Uani 0.797(4) 1 d . . P A 1
H28 H 0.776776 0.281543 0.278062 0.035 Uiso 0.797(4) 1 calc R U P A 1
C24A C 0.5645(12) 0.0717(12) 0.1544(9) 0.036(3) Uani 0.203(4) 1 d . . P A 2
H24A H 0.494048 0.089374 0.156603 0.044 Uiso 0.203(4) 1 calc R U P A 2
C26A C 0.6648(16) -0.0646(13) 0.1316(12) 0.052(5) Uani 0.203(4) 1 d . . P A 2
H26A H 0.668404 -0.134251 0.130704 0.063 Uiso 0.203(4) 1 calc R U P A 2
C27A C 0.7686(13) 0.1224(12) 0.1507(9) 0.036(3) Uani 0.203(4) 1 d . . P A 2
H27A H 0.843266 0.169977 0.15532 0.044 Uiso 0.203(4) 1 calc R U P A 2
C28A C 0.5643(14) -0.0360(11) 0.1400(11) 0.044(4) Uani 0.203(4) 1 d . . P A 2
H28A H 0.494072 -0.089762 0.135883 0.053 Uiso 0.203(4) 1 calc R U P A 2
C29 C 0.4226(4) 0.0989(3) 0.4524(3) 0.0703(13) Uani 1 1 d . . . . .
H29A H 0.339038 0.084697 0.454994 0.084 Uiso 1 1 calc R U . . .
H29B H 0.456267 0.083956 0.505332 0.084 Uiso 1 1 calc R U . . .
C30 C 0.4426(5) 0.0254(3) 0.3650(3) 0.0908(18) Uani 1 1 d . . . . .
H30A H 0.40842 0.039316 0.312386 0.136 Uiso 1 1 calc R U . . .
H30B H 0.407222 -0.050038 0.361585 0.136 Uiso 1 1 calc R U . . .
H30C H 0.525248 0.038084 0.362828 0.136 Uiso 1 1 calc R U . . .
C31 C 0.85244(18) 0.55700(18) 0.43812(15) 0.0188(4) Uani 1 1 d . . . . .
C32 C 0.97789(18) 0.58588(18) 0.42028(15) 0.0190(4) Uani 1 1 d . . . . .
H32 H 1.016846 0.544502 0.448749 0.023 Uiso 1 1 calc R U . . .
C33 C 1.0355(2) 0.7063(2) 0.47084(17) 0.0320(6) Uani 1 1 d . . . . .
C34 C 0.9761(3) 0.7823(3) 0.4924(2) 0.0417(7) Uani 1 1 d . . . . .
H34 H 0.894691 0.757296 0.480859 0.05 Uiso 0.748(11) 1 calc R U P B 1
C35 C 1.0278(9) 0.8929(6) 0.5300(5) 0.0537(19) Uani 0.748(11) 1 d . . P B 1
H35 H 0.98296 0.942007 0.544754 0.064 Uiso 0.748(11) 1 calc R U P B 1
C36 C 1.1437(7) 0.9295(4) 0.5452(4) 0.068(2) Uani 0.748(11) 1 d . . P B 1
H36 H 1.181018 1.005192 0.569973 0.082 Uiso 0.748(11) 1 calc R U P B 1
C37 C 1.2084(5) 0.8564(4) 0.5245(4) 0.065(2) Uani 0.748(11) 1 d . . P B 1
H37 H 1.289746 0.881496 0.536702 0.078 Uiso 0.748(11) 1 calc R U P B 1
C38 C 1.1522(4) 0.7462(4) 0.4857(4) 0.0389(12) Uani 0.748(11) 1 d . . P B 1
H38 H 1.196723 0.696948 0.46903 0.047 Uiso 0.748(11) 1 calc R U P B 1
C35A C 1.056(3) 0.886(2) 0.5531(17) 0.0537(19) Uani 0.252(11) 1 d . . P B 2
H35A H 1.028319 0.947748 0.565636 0.064 Uiso 0.252(11) 1 calc R U P B 2
C36A C 1.1636(13) 0.9035(12) 0.5930(15) 0.058(5) Uani 0.252(11) 1 d . . P B 2
H36A H 1.206608 0.975212 0.628847 0.069 Uiso 0.252(11) 1 calc R U P B 2
C37A C 1.2134(13) 0.8197(12) 0.5831(13) 0.061(6) Uani 0.252(11) 1 d . . P B 2
H37A H 1.286567 0.832944 0.615516 0.073 Uiso 0.252(11) 1 calc R U P B 2
C38A C 1.1548(10) 0.7182(11) 0.5257(12) 0.033(3) Uani 0.252(11) 1 d . . P B 2
H38A H 1.183545 0.657891 0.518807 0.04 Uiso 0.252(11) 1 calc R U P B 2
C39 C 0.99127(17) 0.55224(18) 0.31732(15) 0.0176(4) Uani 1 1 d . . . . .
C40 C 0.9820(2) 0.6166(2) 0.26292(16) 0.0250(5) Uani 1 1 d . . . . .
H40 H 0.965137 0.683163 0.289772 0.03 Uiso 1 1 calc R U . . .
C41 C 0.9971(2) 0.5844(2) 0.16977(17) 0.0296(5) Uani 1 1 d . . . . .
H41 H 0.991637 0.629424 0.133518 0.036 Uiso 1 1 calc R U . . .
C42 C 1.0203(2) 0.4866(2) 0.12980(17) 0.0298(5) Uani 1 1 d . . . . .
H42 H 1.030523 0.464293 0.066124 0.036 Uiso 1 1 calc R U . . .
C43 C 1.0284(2) 0.4217(2) 0.18307(17) 0.0292(5) Uani 1 1 d . . . . .
H43 H 1.043348 0.354261 0.155651 0.035 Uiso 1 1 calc R U . . .
C44 C 1.01472(18) 0.45440(19) 0.27638(16) 0.0212(5) Uani 1 1 d . . . . .
H44 H 1.021453 0.409634 0.312564 0.025 Uiso 1 1 calc R U . . .
C45 C 0.6856(2) 0.4016(2) 0.71216(16) 0.0259(5) Uani 1 1 d . . . . .
H45A H 0.632038 0.435771 0.748577 0.031 Uiso 1 1 calc R U . . .
H45B H 0.758522 0.422135 0.753047 0.031 Uiso 1 1 calc R U . . .
C46 C 0.6353(3) 0.2804(2) 0.6797(2) 0.0498(8) Uani 1 1 d . . . . .
H46A H 0.563369 0.260054 0.6389 0.075 Uiso 1 1 calc R U . . .
H46B H 0.620074 0.255693 0.733406 0.075 Uiso 1 1 calc R U . . .
H46C H 0.689571 0.246493 0.645746 0.075 Uiso 1 1 calc R U . . .
C47 C 0.3455(3) 0.3534(3) 0.7581(2) 0.0576(9) Uani 1 1 d . . . . .
H47A H 0.289135 0.393151 0.780549 0.069 Uiso 1 1 calc R U . . .
H47B H 0.402289 0.366856 0.811609 0.069 Uiso 1 1 calc R U . . .
C48 C 0.2867(4) 0.2376(3) 0.7197(3) 0.0700(11) Uani 1 1 d . . . . .
H48A H 0.222043 0.225492 0.673795 0.105 Uiso 1 1 calc R U . . .
H48B H 0.258278 0.209948 0.769534 0.105 Uiso 1 1 calc R U . . .
H48C H 0.340337 0.199369 0.689813 0.105 Uiso 1 1 calc R U . . .
O1 O 0.31553(14) 0.21867(13) 0.33042(11) 0.0259(4) Uani 1 1 d . . . . .
O2 O 0.21323(12) 0.33356(12) 0.33185(10) 0.0180(3) Uani 1 1 d . . . . .
O3 O 0.52260(16) 0.24965(14) 0.29632(11) 0.0281(4) Uani 1 1 d . . . . .
O4 O 0.61407(14) 0.39758(15) 0.26205(11) 0.0261(4) Uani 1 1 d . . . . .
O5 O 0.47148(14) 0.20873(13) 0.46039(11) 0.0244(3) Uani 1 1 d . . . . .
O6 O 0.60989(12) 0.41748(12) 0.45812(10) 0.0157(3) Uani 1 1 d . . . . .
O7 O 0.83373(12) 0.54252(13) 0.51522(10) 0.0183(3) Uani 1 1 d . . . . .
O8 O 0.77656(13) 0.55186(15) 0.37753(11) 0.0250(4) Uani 1 1 d . . . . .
O9 O 0.70638(12) 0.44059(12) 0.63602(10) 0.0184(3) Uani 1 1 d . . . . .
O10 O 0.55582(12) 0.55713(12) 0.63347(9) 0.0154(3) Uani 1 1 d . . . . .
O11 O 0.40241(14) 0.39259(15) 0.68996(12) 0.0273(4) Uani 1 1 d . . . . .
O12 O 0.37092(12) 0.38069(12) 0.50098(10) 0.0164(3) Uani 1 1 d . . . . .
Ti1 Ti 0.46367(3) 0.31519(3) 0.41815(3) 0.01610(10) Uani 1 1 d . . . . .
Ti2 Ti 0.68311(3) 0.52454(3) 0.57316(2) 0.01314(10) Uani 1 1 d . . . . .
Ti3 Ti 0.40008(3) 0.47942(3) 0.62353(3) 0.01584(10) Uani 1 1 d . . . . .
H34A H 0.925(9) 0.769(10) 0.466(8) 0.019 Uiso 0.252(11) 1 d . U 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 -5 2 0.082
-4 1 -1 0.135
0 2 -1 0.085
4 -1 1 0.221
0 0 1 0.091
-2 1 1 0.136
-2 1 -1 0.138
0 0 -1 0.105
4 -2 1 0.212
3 -2 -2 0.185
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 C1 O2 125.1(2) . . ?
O1 C1 C2 117.94(19) . . ?
O2 C1 C2 116.96(18) . . ?
C3 C2 C9 114.20(19) . . ?
C3 C2 C1 111.77(18) . . ?
C9 C2 C1 110.29(18) . . ?
C3 C2 H2 106.7 . . ?
C9 C2 H2 106.7 . . ?
C1 C2 H2 106.7 . . ?
C8 C3 C4 118.1(2) . . ?
C8 C3 C2 122.7(2) . . ?
C4 C3 C2 119.1(2) . . ?
C3 C4 C5 121.2(3) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
C6 C5 C4 120.2(3) . . ?
C6 C5 H5 119.9 . . ?
C4 C5 H5 119.9 . . ?
C5 C6 C7 119.5(3) . . ?
C5 C6 H6 120.3 . . ?
C7 C6 H6 120.3 . . ?
C6 C7 C8 120.6(3) . . ?
C6 C7 H7 119.7 . . ?
C8 C7 H7 119.7 . . ?
C3 C8 C7 120.3(3) . . ?
C3 C8 H8 119.8 . . ?
C7 C8 H8 119.8 . . ?
C10 C9 C14 119.0(2) . . ?
C10 C9 C2 122.3(2) . . ?
C14 C9 C2 118.7(2) . . ?
C9 C10 C11 120.3(2) . . ?
C9 C10 H10 119.9 . . ?
C11 C10 H10 119.9 . . ?
C12 C11 C10 120.6(3) . . ?
C12 C11 H11 119.7 . . ?
C10 C11 H11 119.7 . . ?
C11 C12 C13 119.5(3) . . ?
C11 C12 H12 120.2 . . ?
C13 C12 H12 120.2 . . ?
C12 C13 C14 120.3(2) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C13 C14 C9 120.4(3) . . ?
C13 C14 H14 119.8 . . ?
C9 C14 H14 119.8 . . ?
O3 C15 O4 125.8(2) . . ?
O3 C15 C16 113.9(2) . . ?
O4 C15 C16 120.3(2) . . ?
O3 C15 C16A 133.5(4) . . ?
O4 C15 C16A 93.5(5) . . ?
C23 C16 C17 112.8(2) . . ?
C23 C16 C15 109.7(2) . . ?
C17 C16 C15 110.9(2) . . ?
C23 C16 H16 107.7 . . ?
C17 C16 H16 107.7 . . ?
C15 C16 H16 107.7 . . ?
C23 C16A C17 113.0(7) . . ?
C23 C16A C15 105.4(7) . . ?
C17 C16A C15 100.6(6) . . ?
C23 C16A H16A 112.4 . . ?
C17 C16A H16A 112.4 . . ?
C15 C16A H16A 112.4 . . ?
C22 C17 C18 120.6(3) . . ?
C22 C17 C16 127.7(3) . . ?
C18 C17 C16 111.7(3) . . ?
C22 C17 C16A 87.9(5) . . ?
C18 C17 C16A 151.3(5) . . ?
C17 C18 C19 118.4(3) . . ?
C17 C18 H18 120.8 . . ?
C19 C18 H18 120.8 . . ?
C18 C19 C20 117.7(3) . . ?
C18 C19 H19 121.2 . . ?
C20 C19 H19 121.2 . . ?
C21 C20 C19 119.5(3) . . ?
C21 C20 H20 120.3 . . ?
C19 C20 H20 120.3 . . ?
C20 C21 C22 121.5(4) . . ?
C20 C21 H21 119.2 . . ?
C22 C21 H21 119.2 . . ?
C17 C22 C21 122.0(3) . . ?
C17 C22 H22 119 . . ?
C21 C22 H22 119 . . ?
C24 C23 C28 118.0(2) . . ?
C27A C23 C16A 123.3(8) . . ?
C27A C23 C24A 114.7(9) . . ?
C16A C23 C24A 120.6(7) . . ?
C24 C23 C16 120.9(2) . . ?
C28 C23 C16 121.1(2) . . ?
C26 C25 C24 121.4(3) . . ?
C26A C25 C27A 130.5(9) . . ?
C26 C25 H25 119.3 . . ?
C24 C25 H25 119.3 . . ?
C26A C25 H25A 114.7 . . ?
C27A C25 H25A 114.7 . . ?
C23 C24 C25 120.2(3) . . ?
C23 C24 H24 119.9 . . ?
C25 C24 H24 119.9 . . ?
C25 C26 C27 120.1(3) . . ?
C25 C26 H26 120 . . ?
C27 C26 H26 120 . . ?
C26 C27 C28 119.9(3) . . ?
C26 C27 H27 120.1 . . ?
C28 C27 H27 120.1 . . ?
C27 C28 C23 120.3(3) . . ?
C27 C28 H28 119.8 . . ?
C23 C28 H28 119.8 . . ?
C28A C24A C23 120.5(12) . . ?
C28A C24A H24A 119.8 . . ?
C23 C24A H24A 119.8 . . ?
C25 C26A C28A 116.0(13) . . ?
C25 C26A H26A 122 . . ?
C28A C26A H26A 122 . . ?
C23 C27A C25 115.3(11) . . ?
C23 C27A H27A 122.4 . . ?
C25 C27A H27A 122.4 . . ?
C26A C28A C24A 120.8(15) . . ?
C26A C28A H28A 119.6 . . ?
C24A C28A H28A 119.6 . . ?
O5 C29 C30 111.7(3) . . ?
O5 C29 H29A 109.3 . . ?
C30 C29 H29A 109.3 . . ?
O5 C29 H29B 109.3 . . ?
C30 C29 H29B 109.3 . . ?
H29A C29 H29B 107.9 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O8 C31 O7 125.0(2) . . ?
O8 C31 C32 118.57(19) . . ?
O7 C31 C32 116.46(18) . . ?
C39 C32 C33 112.99(18) . . ?
C39 C32 C31 112.81(17) . . ?
C33 C32 C31 109.27(18) . . ?
C39 C32 H32 107.1 . . ?
C33 C32 H32 107.1 . . ?
C31 C32 H32 107.1 . . ?
C38 C33 C34 115.9(3) . . ?
C38 C33 C32 120.4(3) . . ?
C34 C33 C32 123.1(2) . . ?
C34 C33 C38A 124.6(5) . . ?
C32 C33 C38A 108.2(5) . . ?
C33 C34 C35 123.9(5) . . ?
C33 C34 C35A 108.0(12) . . ?
C33 C34 H34 118 . . ?
C35 C34 H34 118 . . ?
C33 C34 H34A 116(10) . . ?
C35A C34 H34A 134(10) . . ?
C36 C35 C34 118.5(7) . . ?
C36 C35 H35 120.7 . . ?
C34 C35 H35 120.7 . . ?
C35 C36 C37 120.1(5) . . ?
C35 C36 H36 119.9 . . ?
C37 C36 H36 119.9 . . ?
C38 C37 C36 119.1(5) . . ?
C38 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C33 C38 C37 122.4(5) . . ?
C33 C38 H38 118.8 . . ?
C37 C38 H38 118.8 . . ?
C36A C35A C34 128(2) . . ?
C36A C35A H35A 116.1 . . ?
C34 C35A H35A 116.1 . . ?
C35A C36A C37A 122.2(16) . . ?
C35A C36A H36A 118.9 . . ?
C37A C36A H36A 118.9 . . ?
C38A C37A C36A 118.6(13) . . ?
C38A C37A H37A 120.7 . . ?
C36A C37A H37A 120.7 . . ?
C37A C38A C33 116.6(11) . . ?
C37A C38A H38A 121.7 . . ?
C33 C38A H38A 121.7 . . ?
C44 C39 C40 118.7(2) . . ?
C44 C39 C32 119.0(2) . . ?
C40 C39 C32 122.3(2) . . ?
C41 C40 C39 120.8(2) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C42 C41 C40 119.9(2) . . ?
C42 C41 H41 120 . . ?
C40 C41 H41 120 . . ?
C43 C42 C41 119.7(2) . . ?
C43 C42 H42 120.2 . . ?
C41 C42 H42 120.2 . . ?
C42 C43 C44 120.4(2) . . ?
C42 C43 H43 119.8 . . ?
C44 C43 H43 119.8 . . ?
C43 C44 C39 120.5(2) . . ?
C43 C44 H44 119.7 . . ?
C39 C44 H44 119.7 . . ?
O9 C45 C46 111.0(2) . . ?
O9 C45 H45A 109.4 . . ?
C46 C45 H45A 109.4 . . ?
O9 C45 H45B 109.4 . . ?
C46 C45 H45B 109.4 . . ?
H45A C45 H45B 108 . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
O11 C47 C48 110.7(3) . . ?
O11 C47 H47A 109.5 . . ?
C48 C47 H47A 109.5 . . ?
O11 C47 H47B 109.5 . . ?
C48 C47 H47B 109.5 . . ?
H47A C47 H47B 108.1 . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C1 O1 Ti1 130.40(15) . . ?
C1 O2 Ti2 128.39(14) . 2_666 ?
C15 O3 Ti1 129.43(16) . . ?
C15 O4 Ti3 128.49(15) . 2_666 ?
C29 O5 Ti1 145.78(19) . . ?
Ti1 O6 Ti2 134.32(8) . . ?
Ti1 O6 Ti3 99.65(6) . 2_666 ?
Ti2 O6 Ti3 99.95(7) . 2_666 ?
C31 O7 Ti2 128.45(13) . . ?
C31 O8 Ti3 130.58(14) . 2_666 ?
C45 O9 Ti2 149.52(15) . . ?
Ti3 O10 Ti2 133.80(8) . . ?
Ti3 O10 Ti1 99.36(6) . 2_666 ?
Ti2 O10 Ti1 100.18(6) . 2_666 ?
C47 O11 Ti3 142.3(2) . . ?
Ti3 O12 Ti1 134.13(8) . . ?
Ti3 O12 Ti2 100.39(7) . 2_666 ?
Ti1 O12 Ti2 101.08(6) . 2_666 ?
O5 Ti1 O6 104.36(7) . . ?
O5 Ti1 O12 100.67(7) . . ?
O6 Ti1 O12 102.42(6) . . ?
O5 Ti1 O3 93.22(7) . . ?
O6 Ti1 O3 88.19(7) . . ?
O12 Ti1 O3 159.70(7) . . ?
O5 Ti1 O1 91.52(7) . . ?
O6 Ti1 O1 158.56(7) . . ?
O12 Ti1 O1 88.38(7) . . ?
O3 Ti1 O1 76.44(7) . . ?
O5 Ti1 O10 176.90(7) . 2_666 ?
O6 Ti1 O10 78.43(6) . 2_666 ?
O12 Ti1 O10 77.29(6) . 2_666 ?
O3 Ti1 O10 88.17(6) . 2_666 ?
O1 Ti1 O10 86.11(6) . 2_666 ?
O5 Ti1 Ti3 146.08(6) . 2_666 ?
O6 Ti1 Ti3 43.36(4) . 2_666 ?
O12 Ti1 Ti3 97.55(5) . 2_666 ?
O3 Ti1 Ti3 78.20(5) . 2_666 ?
O1 Ti1 Ti3 117.48(5) . 2_666 ?
O10 Ti1 Ti3 36.97(4) 2_666 2_666 ?
O5 Ti1 Ti2 140.35(6) . 2_666 ?
O6 Ti1 Ti2 98.81(5) . 2_666 ?
O12 Ti1 Ti2 42.34(4) . 2_666 ?
O3 Ti1 Ti2 119.49(5) . 2_666 ?
O1 Ti1 Ti2 76.63(5) . 2_666 ?
O10 Ti1 Ti2 37.01(4) 2_666 2_666 ?
Ti3 Ti1 Ti2 68.338(16) 2_666 2_666 ?
O9 Ti2 O6 100.10(7) . . ?
O9 Ti2 O10 95.55(7) . . ?
O6 Ti2 O10 102.56(6) . . ?
O9 Ti2 O7 97.87(7) . . ?
O6 Ti2 O7 87.69(6) . . ?
O10 Ti2 O7 161.41(6) . . ?
O9 Ti2 O2 94.87(7) . 2_666 ?
O6 Ti2 O2 161.00(6) . 2_666 ?
O10 Ti2 O2 87.46(6) . 2_666 ?
O7 Ti2 O2 78.67(6) . 2_666 ?
O9 Ti2 O12 171.73(6) . 2_666 ?
O6 Ti2 O12 77.65(6) . 2_666 ?
O10 Ti2 O12 77.34(6) . 2_666 ?
O7 Ti2 O12 90.02(6) . 2_666 ?
O2 Ti2 O12 89.08(6) 2_666 2_666 ?
O9 Ti2 Ti3 142.64(5) . 2_666 ?
O6 Ti2 Ti3 42.94(5) . 2_666 ?
O10 Ti2 Ti3 98.08(5) . 2_666 ?
O7 Ti2 Ti3 78.78(4) . 2_666 ?
O2 Ti2 Ti3 120.29(5) 2_666 2_666 ?
O12 Ti2 Ti3 36.81(4) 2_666 2_666 ?
O9 Ti2 Ti1 137.46(5) . 2_666 ?
O6 Ti2 Ti1 98.17(5) . 2_666 ?
O10 Ti2 Ti1 42.81(4) . 2_666 ?
O7 Ti2 Ti1 121.01(5) . 2_666 ?
O2 Ti2 Ti1 78.12(4) 2_666 2_666 ?
O12 Ti2 Ti1 36.59(4) 2_666 2_666 ?
Ti3 Ti2 Ti1 68.133(17) 2_666 2_666 ?
O11 Ti3 O10 103.47(7) . . ?
O11 Ti3 O12 101.67(8) . . ?
O10 Ti3 O12 102.94(7) . . ?
O11 Ti3 O4 92.15(8) . 2_666 ?
O10 Ti3 O4 87.92(7) . 2_666 ?
O12 Ti3 O4 159.73(7) . 2_666 ?
O11 Ti3 O8 90.73(7) . 2_666 ?
O10 Ti3 O8 159.94(7) . 2_666 ?
O12 Ti3 O8 87.64(7) . 2_666 ?
O4 Ti3 O8 77.33(7) 2_666 2_666 ?
O11 Ti3 O6 177.78(7) . 2_666 ?
O10 Ti3 O6 78.75(6) . 2_666 ?
O12 Ti3 O6 77.80(6) . 2_666 ?
O4 Ti3 O6 87.81(6) 2_666 2_666 ?
O8 Ti3 O6 87.09(6) 2_666 2_666 ?
O11 Ti3 Ti1 145.11(6) . 2_666 ?
O10 Ti3 Ti1 43.67(4) . 2_666 ?
O12 Ti3 Ti1 98.20(5) . 2_666 ?
O4 Ti3 Ti1 77.74(5) 2_666 2_666 ?
O8 Ti3 Ti1 118.61(5) 2_666 2_666 ?
O6 Ti3 Ti1 36.99(4) 2_666 2_666 ?
O11 Ti3 Ti2 141.74(6) . 2_666 ?
O10 Ti3 Ti2 99.40(5) . 2_666 ?
O12 Ti3 Ti2 42.80(5) . 2_666 ?
O4 Ti3 Ti2 119.12(5) 2_666 2_666 ?
O8 Ti3 Ti2 76.70(5) 2_666 2_666 ?
O6 Ti3 Ti2 37.11(4) 2_666 2_666 ?
Ti1 Ti3 Ti2 68.592(19) 2_666 2_666 ?
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
C1 O1 1.251(3) . ?
C1 O2 1.263(3) . ?
C1 C2 1.536(3) . ?
C2 C3 1.519(3) . ?
C2 C9 1.528(3) . ?
C2 H2 1 . ?
C3 C8 1.386(3) . ?
C3 C4 1.388(4) . ?
C4 C5 1.392(4) . ?
C4 H4 0.95 . ?
C5 C6 1.368(5) . ?
C5 H5 0.95 . ?
C6 C7 1.379(5) . ?
C6 H6 0.95 . ?
C7 C8 1.397(4) . ?
C7 H7 0.95 . ?
C8 H8 0.95 . ?
C9 C10 1.389(4) . ?
C9 C14 1.399(3) . ?
C10 C11 1.394(4) . ?
C10 H10 0.95 . ?
C11 C12 1.383(4) . ?
C11 H11 0.95 . ?
C12 C13 1.386(5) . ?
C12 H12 0.95 . ?
C13 C14 1.392(4) . ?
C13 H13 0.95 . ?
C14 H14 0.95 . ?
C15 O3 1.236(3) . ?
C15 O4 1.276(3) . ?
C15 C16 1.547(3) . ?
C15 C16A 1.699(11) . ?
C16 C23 1.517(4) . ?
C16 C17 1.545(4) . ?
C16 H16 1 . ?
C16A C23 1.446(12) . ?
C16A C17 1.610(11) . ?
C16A H16A 1 . ?
C17 C22 1.328(4) . ?
C17 C18 1.383(4) . ?
C18 C19 1.422(6) . ?
C18 H18 0.95 . ?
C19 C20 1.428(7) . ?
C19 H19 0.95 . ?
C20 C21 1.325(6) . ?
C20 H20 0.95 . ?
C21 C22 1.347(5) . ?
C21 H21 0.95 . ?
C22 H22 0.95 . ?
C23 C27A 1.361(13) . ?
C23 C24 1.368(4) . ?
C23 C28 1.416(4) . ?
C23 C24A 1.496(14) . ?
C25 C26A 1.179(17) . ?
C25 C26 1.328(5) . ?
C25 C24 1.413(4) . ?
C25 C27A 1.491(15) . ?
C25 H25 0.95 . ?
C25 H25A 0.95 . ?
C24 H24 0.95 . ?
C26 C27 1.387(5) . ?
C26 H26 0.95 . ?
C27 C28 1.388(4) . ?
C27 H27 0.95 . ?
C28 H28 0.95 . ?
C24A C28A 1.40(2) . ?
C24A H24A 0.95 . ?
C26A C28A 1.38(2) . ?
C26A H26A 0.95 . ?
C27A H27A 0.95 . ?
C28A H28A 0.95 . ?
C29 O5 1.410(3) . ?
C29 C30 1.476(6) . ?
C29 H29A 0.99 . ?
C29 H29B 0.99 . ?
C30 H30A 0.98 . ?
C30 H30B 0.98 . ?
C30 H30C 0.98 . ?
C31 O8 1.257(3) . ?
C31 O7 1.269(3) . ?
C31 C32 1.530(3) . ?
C32 C39 1.526(3) . ?
C32 C33 1.526(3) . ?
C32 H32 1 . ?
C33 C38 1.364(5) . ?
C33 C34 1.378(4) . ?
C33 C38A 1.595(13) . ?
C34 C35 1.384(9) . ?
C34 C35A 1.48(3) . ?
C34 H34 0.95 . ?
C34 H34A 0.68(11) . ?
C35 C36 1.352(12) . ?
C35 H35 0.95 . ?
C36 C37 1.394(9) . ?
C36 H36 0.95 . ?
C37 C38 1.390(7) . ?
C37 H37 0.95 . ?
C38 H38 0.95 . ?
C35A C36A 1.36(3) . ?
C35A H35A 0.95 . ?
C36A C37A 1.39(2) . ?
C36A H36A 0.95 . ?
C37A C38A 1.366(18) . ?
C37A H37A 0.95 . ?
C38A H38A 0.95 . ?
C39 C44 1.391(3) . ?
C39 C40 1.392(3) . ?
C40 C41 1.390(3) . ?
C40 H40 0.95 . ?
C41 C42 1.387(4) . ?
C41 H41 0.95 . ?
C42 C43 1.382(4) . ?
C42 H42 0.95 . ?
C43 C44 1.388(3) . ?
C43 H43 0.95 . ?
C44 H44 0.95 . ?
C45 O9 1.418(3) . ?
C45 C46 1.503(4) . ?
C45 H45A 0.99 . ?
C45 H45B 0.99 . ?
C46 H46A 0.98 . ?
C46 H46B 0.98 . ?
C46 H46C 0.98 . ?
C47 O11 1.426(3) . ?
C47 C48 1.458(5) . ?
C47 H47A 0.99 . ?
C47 H47B 0.99 . ?
C48 H48A 0.98 . ?
C48 H48B 0.98 . ?
C48 H48C 0.98 . ?
O1 Ti1 2.0663(17) . ?
O2 Ti2 2.0672(16) 2_666 ?
O3 Ti1 2.0490(17) . ?
O4 Ti3 2.0648(17) 2_666 ?
O5 Ti1 1.7672(16) . ?
O6 Ti1 1.8868(15) . ?
O6 Ti2 1.9068(15) . ?
O6 Ti3 2.1530(15) 2_666 ?
O7 Ti2 2.0550(15) . ?
O8 Ti3 2.0795(16) 2_666 ?
O9 Ti2 1.7596(15) . ?
O10 Ti3 1.8845(15) . ?
O10 Ti2 1.9163(15) . ?
O10 Ti1 2.1633(15) 2_666 ?
O11 Ti3 1.7719(16) . ?
O12 Ti3 1.8963(15) . ?
O12 Ti1 1.9030(15) . ?
O12 Ti2 2.1503(15) 2_666 ?
Ti1 Ti3 3.0915(7) 2_666 ?
Ti1 Ti2 3.1333(6) 2_666 ?
Ti2 Ti3 3.1130(8) 2_666 ?
