# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nbk25-3Dfull
_database_code_depnum_ccdc_archive 'CCDC 2284900'
loop_
_audit_author_name
_audit_author_address
'Tadeusz Muziol'
;Nicolaus Copernicus University in Torun, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2023-07-27 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         
'(Ti 4+)6, (O 2-)4, (C14 H8 O3 2-)4, (C3 H5 O2 1-)6, (C3 H7 O 1-)2'
_chemical_formula_sum            'C80 H76 O30 Ti6'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1804.80

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 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.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.4059(10)
_cell_length_b                   12.5243(11)
_cell_length_c                   17.3816(13)
_cell_angle_alpha                77.520(7)
_cell_angle_beta                 69.528(8)
_cell_angle_gamma                63.331(9)
_cell_volume                     2255.3(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5570
_cell_measurement_theta_min      3.9320
_cell_measurement_theta_max      69.9040
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.329
_exptl_crystal_F_000             928
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    4.956
_shelx_estimated_absorpt_T_min   0.588
_shelx_estimated_absorpt_T_max   0.826
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.65108
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.55a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            27429
_diffrn_reflns_av_unetI/netI     0.0862
_diffrn_reflns_av_R_equivalents  0.0968
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         3.960
_diffrn_reflns_theta_max         74.443
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measured_fraction_theta_full 0.978
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_Laue_measured_fraction_full 0.978
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_point_group_measured_fraction_full 0.978
_reflns_number_total             8652
_reflns_number_gt                4656
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_cell_refinement       'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.55a (Rigaku OD, 2022)'
_computing_structure_solution    'Olex2-1.3 (Dolomanow, 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'WinGX v1.80.03 (Farrugia, 1999)'
_computing_publication_material  ciftab
_refine_special_details          'bypass in OLEX2'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1831P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8652
_refine_ls_number_parameters     531
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.1461
_refine_ls_R_factor_gt           0.0941
_refine_ls_wR_factor_ref         0.2977
_refine_ls_wR_factor_gt          0.2558
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_restrained_S_all      1.021
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.57305(12) 0.98174(10) 0.34729(6) 0.0591(4) Uani 1 1 d . . . . .
Ti2 Ti 0.36623(13) 1.22048(10) 0.48926(6) 0.0604(4) Uani 1 1 d . . . . .
Ti3 Ti 0.42800(14) 1.25090(11) 0.29792(7) 0.0661(4) Uani 1 1 d . . . . .
O16 O 0.4644(4) 1.1276(4) 0.3968(2) 0.0588(10) Uani 1 1 d . . . . .
O17 O 0.6485(5) 0.8835(4) 0.4224(3) 0.0642(11) Uani 1 1 d . . . . .
O1 O 0.2801(5) 1.3705(4) 0.5414(3) 0.0724(13) Uani 1 1 d . . . . .
O2 O 0.2337(6) 1.5656(5) 0.5341(3) 0.0907(17) Uani 1 1 d . . . . .
C2 C 0.2732(8) 1.4747(7) 0.5010(5) 0.075(2) Uani 1 1 d . . . . .
C3 C 0.3183(8) 1.4713(6) 0.4062(4) 0.0696(18) Uani 1 1 d . . . . .
O3 O 0.3703(5) 1.3479(4) 0.3892(3) 0.0646(12) Uani 1 1 d . . . . .
C4 C 0.2096(9) 1.5521(7) 0.3722(4) 0.076(2) Uani 1 1 d . . . . .
C5 C 0.0940(8) 1.5504(8) 0.3869(5) 0.080(2) Uani 1 1 d . . . . .
H5 H 0.075123 1.486751 0.420523 0.096 Uiso 1 1 calc R U . . .
C6 C 0.0046(9) 1.6428(9) 0.3523(5) 0.092(3) Uani 1 1 d . . . . .
H6 H -0.074849 1.641415 0.361450 0.111 Uiso 1 1 calc R U . . .
C7 C 0.0315(12) 1.7360(9) 0.3047(6) 0.103(3) Uani 1 1 d . . . . .
H7 H -0.030569 1.799446 0.282320 0.124 Uiso 1 1 calc R U . . .
C8 C 0.1467(11) 1.7387(8) 0.2892(5) 0.091(3) Uani 1 1 d . . . . .
H8 H 0.164622 1.802760 0.255535 0.109 Uiso 1 1 calc R U . . .
C9 C 0.2350(9) 1.6489(7) 0.3224(4) 0.078(2) Uani 1 1 d . . . . .
C10 C 0.3661(9) 1.6277(7) 0.3183(4) 0.079(2) Uani 1 1 d . . . . .
C11 C 0.4394(11) 1.6919(8) 0.2752(5) 0.095(3) Uani 1 1 d . . . . .
H11 H 0.408688 1.761611 0.240629 0.114 Uiso 1 1 calc R U . . .
C12 C 0.5601(11) 1.6498(8) 0.2847(5) 0.092(3) Uani 1 1 d . . . . .
H12 H 0.611317 1.692268 0.256027 0.110 Uiso 1 1 calc R U . . .
C13 C 0.6059(9) 1.5494(8) 0.3340(5) 0.086(2) Uani 1 1 d . . . . .
H13 H 0.687790 1.523357 0.339333 0.104 Uiso 1 1 calc R U . . .
C14 C 0.5327(9) 1.4853(7) 0.3764(5) 0.077(2) Uani 1 1 d . . . . .
H14 H 0.563489 1.415669 0.410975 0.092 Uiso 1 1 calc R U . . .
C15 C 0.4158(8) 1.5249(6) 0.3671(4) 0.072(2) Uani 1 1 d . . . . .
O21 O 0.6450(5) 0.8793(4) 0.2579(3) 0.0684(12) Uani 1 1 d . . . . .
O22 O 0.6570(6) 0.8458(5) 0.1331(3) 0.0829(15) Uani 1 1 d . . . . .
C22 C 0.6152(7) 0.9133(7) 0.1881(4) 0.0668(17) Uani 1 1 d . . . . .
O23 O 0.4983(5) 1.0949(4) 0.2539(2) 0.0641(11) Uani 1 1 d . . . . .
C23 C 0.5198(8) 1.0438(7) 0.1823(4) 0.073(2) Uani 1 1 d . . . . .
C24 C 0.5673(8) 1.1074(6) 0.1008(4) 0.0672(18) Uani 1 1 d . . . . .
C25 C 0.6729(8) 1.1326(7) 0.0765(5) 0.0746(19) Uani 1 1 d . . . . .
H25 H 0.724814 1.111616 0.111279 0.090 Uiso 1 1 calc R U . . .
C26 C 0.6993(9) 1.1901(7) -0.0016(5) 0.081(2) Uani 1 1 d . . . . .
H26 H 0.767934 1.213183 -0.019205 0.097 Uiso 1 1 calc R U . . .
C27 C 0.6274(9) 1.2143(7) -0.0541(4) 0.082(2) Uani 1 1 d . . . . .
H27 H 0.650717 1.249316 -0.108090 0.098 Uiso 1 1 calc R U . . .
C28 C 0.5198(8) 1.1877(7) -0.0288(4) 0.073(2) Uani 1 1 d . . . . .
H28 H 0.468951 1.206421 -0.064026 0.088 Uiso 1 1 calc R U . . .
C29 C 0.4919(8) 1.1331(6) 0.0498(4) 0.0682(18) Uani 1 1 d . . . . .
C30 C 0.3853(7) 1.1008(6) 0.0943(4) 0.0674(18) Uani 1 1 d . . . . .
C31 C 0.2828(8) 1.1134(7) 0.0737(5) 0.077(2) Uani 1 1 d . . . . .
H31 H 0.273747 1.146158 0.020488 0.092 Uiso 1 1 calc R U . . .
C32 C 0.1926(8) 1.0777(7) 0.1314(5) 0.081(2) Uani 1 1 d . . . . .
H32 H 0.121602 1.086289 0.117249 0.098 Uiso 1 1 calc R U . . .
C33 C 0.2042(8) 1.0306(7) 0.2080(5) 0.078(2) Uani 1 1 d . . . . .
H33 H 0.141169 1.007132 0.246744 0.094 Uiso 1 1 calc R U . . .
C34 C 0.3081(7) 1.0166(7) 0.2299(4) 0.0708(19) Uani 1 1 d . . . . .
H34 H 0.316684 0.983773 0.283175 0.085 Uiso 1 1 calc R U . . .
C35 C 0.3972(8) 1.0512(7) 0.1730(4) 0.074(2) Uani 1 1 d . . . . .
O41 O 0.2096(5) 1.2330(4) 0.4710(3) 0.0710(12) Uani 1 1 d . . . . .
O42 O 0.2570(5) 1.2488(4) 0.3333(3) 0.0765(14) Uani 1 1 d . . . . .
C42 C 0.1839(8) 1.2413(6) 0.4041(5) 0.0715(19) Uani 1 1 d . . . . .
C43 C 0.0583(9) 1.2467(10) 0.4106(7) 0.108(3) Uani 1 1 d . . . . .
H43A H -0.005134 1.295374 0.457051 0.129 Uiso 1 1 calc R U . . .
H43B H 0.061526 1.164580 0.424416 0.129 Uiso 1 1 calc R U . . .
C44 C 0.0124(11) 1.2992(12) 0.3330(7) 0.128(4) Uani 1 1 d . . . . .
H44A H -0.070558 1.299122 0.343719 0.192 Uiso 1 1 calc R U . . .
H44B H 0.072475 1.250212 0.286791 0.192 Uiso 1 1 calc R U . . .
H44C H 0.006221 1.381474 0.319297 0.192 Uiso 1 1 calc R U . . .
O51 O 0.6043(6) 1.2363(5) 0.2735(3) 0.0690(13) Uani 1 1 d . . . . .
O52 O 0.7127(5) 1.0408(4) 0.3012(3) 0.0648(12) Uani 1 1 d . . . . .
C52 C 0.7066(9) 1.1457(8) 0.2756(4) 0.073(2) Uani 1 1 d . . . . .
C53 C 0.8297(9) 1.1595(8) 0.2453(6) 0.092(3) Uani 1 1 d . . . . .
H53A H 0.859354 1.149737 0.293406 0.110 Uiso 1 1 calc R U . . .
H53B H 0.892695 1.093602 0.209621 0.110 Uiso 1 1 calc R U . . .
C54 C 0.8264(10) 1.2740(10) 0.1991(7) 0.114(3) Uani 1 1 d . . . . .
H54A H 0.784469 1.337432 0.237347 0.171 Uiso 1 1 calc R U . . .
H54B H 0.779913 1.294043 0.158869 0.171 Uiso 1 1 calc R U . . .
H54C H 0.912711 1.266431 0.170299 0.171 Uiso 1 1 calc R U . . .
O61 O 0.4328(5) 0.9260(4) 0.3923(3) 0.0650(12) Uani 1 1 d . . . . .
O62 O 0.4717(5) 0.7927(4) 0.4989(2) 0.0652(12) Uani 1 1 d . . . . .
C62 C 0.4053(8) 0.8523(6) 0.4507(4) 0.0657(18) Uani 1 1 d . . . . .
C63 C 0.2828(9) 0.8411(9) 0.4672(5) 0.087(2) Uani 1 1 d . U . . .
H63A H 0.239419 0.894178 0.426274 0.104 Uiso 0.5 1 calc R U P A 1
H63B H 0.301264 0.757708 0.460099 0.104 Uiso 0.5 1 calc R U P A 1
H63C H 0.286508 0.763600 0.497734 0.104 Uiso 0.5 1 calc R U P B 2
H63D H 0.265378 0.846016 0.414862 0.104 Uiso 0.5 1 calc R U P B 2
C64 C 0.199(3) 0.872(3) 0.550(2) 0.135(9) Uani 0.5 1 d . U P C 1
H64A H 0.188197 0.801133 0.581809 0.202 Uiso 0.5 1 calc R U P C 1
H64B H 0.116344 0.934200 0.546232 0.202 Uiso 0.5 1 calc R U P C 1
H64C H 0.234917 0.903019 0.577427 0.202 Uiso 0.5 1 calc R U P C 1
C65 C 0.178(3) 0.948(3) 0.520(2) 0.135(9) Uani 0.5 1 d . U P C 2
H65A H 0.190618 1.021117 0.496330 0.202 Uiso 0.5 1 calc R U P C 2
H65B H 0.183269 0.930384 0.576497 0.202 Uiso 0.5 1 calc R U P C 2
H65C H 0.095214 0.957841 0.519602 0.202 Uiso 0.5 1 calc R U P C 2
O71 O 0.4033(6) 1.3509(5) 0.2136(3) 0.0851(15) Uani 1 1 d . . . . .
C72 C 0.4063(15) 1.4228(14) 0.1374(8) 0.139(5) Uani 1 1 d D . . . .
H72 H 0.445298 1.361666 0.095981 0.166 Uiso 1 1 calc R U . . .
C73 C 0.5041(14) 1.4705(10) 0.1189(7) 0.129(4) Uani 1 1 d . . . . .
H73A H 0.586389 1.403711 0.115834 0.194 Uiso 1 1 calc R U . . .
H73B H 0.482530 1.520906 0.162617 0.194 Uiso 1 1 calc R U . . .
H73C H 0.507451 1.518374 0.066124 0.194 Uiso 1 1 calc R U . . .
C74 C 0.2792(16) 1.4855(18) 0.1322(10) 0.202(8) Uani 1 1 d D . . . .
H74A H 0.232497 1.550486 0.169514 0.303 Uiso 1 1 calc R U . . .
H74B H 0.238133 1.429840 0.147911 0.303 Uiso 1 1 calc R U . . .
H74C H 0.280468 1.519033 0.075617 0.303 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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 O17 1.794(5) . ?
Ti1 O16 1.884(4) . ?
Ti1 O21 1.929(4) . ?
Ti1 O61 2.008(5) . ?
Ti1 O52 2.028(4) . ?
Ti1 O23 2.093(5) . ?
Ti1 Ti3 3.1182(18) . ?
Ti2 O17 1.800(4) 2_676 ?
Ti2 O16 1.894(4) . ?
Ti2 O1 1.936(5) . ?
Ti2 O41 2.010(5) . ?
Ti2 O62 2.022(5) 2_676 ?
Ti2 O3 2.094(4) . ?
Ti2 Ti3 3.1185(15) . ?
Ti3 O71 1.728(5) . ?
Ti3 O3 1.940(4) . ?
Ti3 O23 1.953(4) . ?
Ti3 O42 2.002(6) . ?
Ti3 O51 2.006(6) . ?
Ti3 O16 2.077(4) . ?
O1 C2 1.323(9) . ?
O2 C2 1.205(8) . ?
C2 C3 1.547(10) . ?
C3 O3 1.435(8) . ?
C3 C4 1.506(12) . ?
C3 C15 1.527(10) . ?
C4 C5 1.375(12) . ?
C4 C9 1.421(11) . ?
C5 C6 1.395(13) . ?
C5 H5 0.9500 . ?
C6 C7 1.377(13) . ?
C6 H6 0.9500 . ?
C7 C8 1.373(14) . ?
C7 H7 0.9500 . ?
C8 C9 1.361(13) . ?
C8 H8 0.9500 . ?
C9 C10 1.503(13) . ?
C10 C15 1.392(11) . ?
C10 C11 1.399(12) . ?
C11 C12 1.404(14) . ?
C11 H11 0.9500 . ?
C12 C13 1.368(13) . ?
C12 H12 0.9500 . ?
C13 C14 1.394(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.364(12) . ?
C14 H14 0.9500 . ?
O21 C22 1.318(8) . ?
O22 C22 1.227(8) . ?
C22 C23 1.536(11) . ?
O23 C23 1.410(7) . ?
C23 C24 1.529(9) . ?
C23 C35 1.545(12) . ?
C24 C25 1.385(11) . ?
C24 C29 1.398(10) . ?
C25 C26 1.395(11) . ?
C25 H25 0.9500 . ?
C26 C27 1.389(12) . ?
C26 H26 0.9500 . ?
C27 C28 1.418(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.390(10) . ?
C28 H28 0.9500 . ?
C29 C30 1.463(11) . ?
C30 C31 1.373(11) . ?
C30 C35 1.403(10) . ?
C31 C32 1.389(11) . ?
C31 H31 0.9500 . ?
C32 C33 1.365(12) . ?
C32 H32 0.9500 . ?
C33 C34 1.396(11) . ?
C33 H33 0.9500 . ?
C34 C35 1.367(10) . ?
C34 H34 0.9500 . ?
O41 C42 1.281(9) . ?
O42 C42 1.261(9) . ?
C42 C43 1.494(12) . ?
C43 C44 1.547(16) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
O51 C52 1.273(10) . ?
O52 C52 1.270(9) . ?
C52 C53 1.508(11) . ?
C53 C54 1.475(13) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
O61 C62 1.279(8) . ?
O62 C62 1.264(9) . ?
C62 C63 1.510(11) . ?
C63 C64 1.46(3) . ?
C63 C65 1.56(3) . ?
C63 H63A 0.9900 . ?
C63 H63B 0.9900 . ?
C63 H63C 0.9900 . ?
C63 H63D 0.9900 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
O71 C72 1.430(12) . ?
C72 C74 1.438(15) . ?
C72 C73 1.493(17) . ?
C72 H72 1.0000 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?

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
O17 Ti1 O16 105.82(19) . . ?
O17 Ti1 O21 101.6(2) . . ?
O16 Ti1 O21 152.6(2) . . ?
O17 Ti1 O61 90.4(2) . . ?
O16 Ti1 O61 89.64(19) . . ?
O21 Ti1 O61 89.14(19) . . ?
O17 Ti1 O52 90.5(2) . . ?
O16 Ti1 O52 89.70(19) . . ?
O21 Ti1 O52 91.11(19) . . ?
O61 Ti1 O52 179.0(2) . . ?
O17 Ti1 O23 175.8(2) . . ?
O16 Ti1 O23 76.33(18) . . ?
O21 Ti1 O23 76.37(19) . . ?
O61 Ti1 O23 93.29(19) . . ?
O52 Ti1 O23 85.85(18) . . ?
O17 Ti1 Ti3 142.97(14) . . ?
O16 Ti1 Ti3 40.32(13) . . ?
O21 Ti1 Ti3 113.44(14) . . ?
O61 Ti1 Ti3 101.36(15) . . ?
O52 Ti1 Ti3 77.67(14) . . ?
O23 Ti1 Ti3 37.97(12) . . ?
O17 Ti2 O16 106.52(19) 2_676 . ?
O17 Ti2 O1 100.76(19) 2_676 . ?
O16 Ti2 O1 152.5(2) . . ?
O17 Ti2 O41 91.5(2) 2_676 . ?
O16 Ti2 O41 89.34(19) . . ?
O1 Ti2 O41 93.4(2) . . ?
O17 Ti2 O62 90.7(2) 2_676 2_676 ?
O16 Ti2 O62 88.01(18) . 2_676 ?
O1 Ti2 O62 88.3(2) . 2_676 ?
O41 Ti2 O62 176.96(19) . 2_676 ?
O17 Ti2 O3 176.2(2) 2_676 . ?
O16 Ti2 O3 76.00(18) . . ?
O1 Ti2 O3 76.94(18) . . ?
O41 Ti2 O3 85.6(2) . . ?
O62 Ti2 O3 92.33(18) 2_676 . ?
O17 Ti2 Ti3 143.93(14) 2_676 . ?
O16 Ti2 Ti3 40.38(13) . . ?
O1 Ti2 Ti3 113.89(15) . . ?
O41 Ti2 Ti3 77.24(14) . . ?
O62 Ti2 Ti3 99.76(13) 2_676 . ?
O3 Ti2 Ti3 37.60(11) . . ?
O71 Ti3 O3 105.8(2) . . ?
O71 Ti3 O23 103.5(2) . . ?
O3 Ti3 O23 150.71(19) . . ?
O71 Ti3 O42 94.6(3) . . ?
O3 Ti3 O42 88.0(2) . . ?
O23 Ti3 O42 88.81(19) . . ?
O71 Ti3 O51 92.6(3) . . ?
O3 Ti3 O51 90.9(2) . . ?
O23 Ti3 O51 88.6(2) . . ?
O42 Ti3 O51 172.8(2) . . ?
O71 Ti3 O16 177.9(3) . . ?
O3 Ti3 O16 75.47(17) . . ?
O23 Ti3 O16 75.29(17) . . ?
O42 Ti3 O16 87.09(19) . . ?
O51 Ti3 O16 85.71(19) . . ?
O71 Ti3 Ti1 142.43(19) . . ?
O3 Ti3 Ti1 110.37(14) . . ?
O23 Ti3 Ti1 41.27(13) . . ?
O42 Ti3 Ti1 96.57(15) . . ?
O51 Ti3 Ti1 77.09(15) . . ?
O16 Ti3 Ti1 35.94(12) . . ?
O71 Ti3 Ti2 145.41(19) . . ?
O3 Ti3 Ti2 41.21(13) . . ?
O23 Ti3 Ti2 109.84(13) . . ?
O42 Ti3 Ti2 77.49(14) . . ?
O51 Ti3 Ti2 97.02(13) . . ?
O16 Ti3 Ti2 36.21(12) . . ?
Ti1 Ti3 Ti2 72.15(4) . . ?
Ti1 O16 Ti2 152.8(2) . . ?
Ti1 O16 Ti3 103.74(18) . . ?
Ti2 O16 Ti3 103.4(2) . . ?
Ti1 O17 Ti2 144.6(3) . 2_676 ?
C2 O1 Ti2 123.5(4) . . ?
O2 C2 O1 123.7(7) . . ?
O2 C2 C3 122.1(7) . . ?
O1 C2 C3 114.1(6) . . ?
O3 C3 C4 114.3(6) . . ?
O3 C3 C15 111.3(6) . . ?
C4 C3 C15 104.3(6) . . ?
O3 C3 C2 106.7(5) . . ?
C4 C3 C2 109.1(6) . . ?
C15 C3 C2 111.1(6) . . ?
C3 O3 Ti3 140.1(4) . . ?
C3 O3 Ti2 118.0(4) . . ?
Ti3 O3 Ti2 101.19(18) . . ?
C5 C4 C9 119.1(8) . . ?
C5 C4 C3 131.0(7) . . ?
C9 C4 C3 109.7(8) . . ?
C4 C5 C6 119.6(8) . . ?
C4 C5 H5 120.2 . . ?
C6 C5 H5 120.2 . . ?
C7 C6 C5 120.1(10) . . ?
C7 C6 H6 120.0 . . ?
C5 C6 H6 120.0 . . ?
C8 C7 C6 121.0(10) . . ?
C8 C7 H7 119.5 . . ?
C6 C7 H7 119.5 . . ?
C9 C8 C7 119.6(9) . . ?
C9 C8 H8 120.2 . . ?
C7 C8 H8 120.2 . . ?
C8 C9 C4 120.7(9) . . ?
C8 C9 C10 132.2(8) . . ?
C4 C9 C10 107.2(7) . . ?
C15 C10 C11 119.2(9) . . ?
C15 C10 C9 109.8(7) . . ?
C11 C10 C9 131.0(9) . . ?
C10 C11 C12 117.7(9) . . ?
C10 C11 H11 121.1 . . ?
C12 C11 H11 121.1 . . ?
C13 C12 C11 121.9(8) . . ?
C13 C12 H12 119.0 . . ?
C11 C12 H12 119.0 . . ?
C12 C13 C14 120.1(9) . . ?
C12 C13 H13 119.9 . . ?
C14 C13 H13 119.9 . . ?
C15 C14 C13 118.4(8) . . ?
C15 C14 H14 120.8 . . ?
C13 C14 H14 120.8 . . ?
C14 C15 C10 122.7(7) . . ?
C14 C15 C3 128.5(7) . . ?
C10 C15 C3 108.8(8) . . ?
C22 O21 Ti1 123.7(5) . . ?
O22 C22 O21 123.1(7) . . ?
O22 C22 C23 122.5(7) . . ?
O21 C22 C23 114.3(6) . . ?
C23 O23 Ti3 140.7(4) . . ?
C23 O23 Ti1 118.3(4) . . ?
Ti3 O23 Ti1 100.76(17) . . ?
O23 C23 C24 115.5(5) . . ?
O23 C23 C22 106.7(6) . . ?
C24 C23 C22 110.0(6) . . ?
O23 C23 C35 112.4(6) . . ?
C24 C23 C35 101.0(6) . . ?
C22 C23 C35 111.4(6) . . ?
C25 C24 C29 122.8(6) . . ?
C25 C24 C23 126.8(7) . . ?
C29 C24 C23 110.3(6) . . ?
C24 C25 C26 116.8(7) . . ?
C24 C25 H25 121.6 . . ?
C26 C25 H25 121.6 . . ?
C27 C26 C25 121.3(8) . . ?
C27 C26 H26 119.3 . . ?
C25 C26 H26 119.3 . . ?
C26 C27 C28 121.3(7) . . ?
C26 C27 H27 119.3 . . ?
C28 C27 H27 119.3 . . ?
C29 C28 C27 117.1(7) . . ?
C29 C28 H28 121.4 . . ?
C27 C28 H28 121.4 . . ?
C28 C29 C24 120.4(7) . . ?
C28 C29 C30 129.8(7) . . ?
C24 C29 C30 109.6(6) . . ?
C31 C30 C35 119.3(7) . . ?
C31 C30 C29 132.5(7) . . ?
C35 C30 C29 108.2(6) . . ?
C30 C31 C32 119.2(8) . . ?
C30 C31 H31 120.4 . . ?
C32 C31 H31 120.4 . . ?
C33 C32 C31 121.1(8) . . ?
C33 C32 H32 119.4 . . ?
C31 C32 H32 119.4 . . ?
C32 C33 C34 120.4(8) . . ?
C32 C33 H33 119.8 . . ?
C34 C33 H33 119.8 . . ?
C35 C34 C33 118.5(7) . . ?
C35 C34 H34 120.8 . . ?
C33 C34 H34 120.8 . . ?
C34 C35 C30 121.5(8) . . ?
C34 C35 C23 128.0(7) . . ?
C30 C35 C23 110.5(6) . . ?
C42 O41 Ti2 130.5(5) . . ?
C42 O42 Ti3 131.0(5) . . ?
O42 C42 O41 123.7(7) . . ?
O42 C42 C43 118.3(8) . . ?
O41 C42 C43 117.9(8) . . ?
C42 C43 C44 116.0(10) . . ?
C42 C43 H43A 108.3 . . ?
C44 C43 H43A 108.3 . . ?
C42 C43 H43B 108.3 . . ?
C44 C43 H43B 108.3 . . ?
H43A C43 H43B 107.4 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C52 O51 Ti3 131.5(4) . . ?
C52 O52 Ti1 129.8(6) . . ?
O52 C52 O51 123.6(7) . . ?
O52 C52 C53 116.4(8) . . ?
O51 C52 C53 120.0(7) . . ?
C54 C53 C52 116.0(9) . . ?
C54 C53 H53A 108.3 . . ?
C52 C53 H53A 108.3 . . ?
C54 C53 H53B 108.3 . . ?
C52 C53 H53B 108.3 . . ?
H53A C53 H53B 107.4 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C62 O61 Ti1 135.7(5) . . ?
C62 O62 Ti2 134.9(4) . 2_676 ?
O62 C62 O61 123.6(6) . . ?
O62 C62 C63 117.6(6) . . ?
O61 C62 C63 118.7(7) . . ?
C64 C63 C62 112.7(16) . . ?
C62 C63 C65 106.2(14) . . ?
C64 C63 H63A 109.0 . . ?
C62 C63 H63A 109.0 . . ?
C64 C63 H63B 109.0 . . ?
C62 C63 H63B 109.0 . . ?
H63A C63 H63B 107.8 . . ?
C62 C63 H63C 110.5 . . ?
C65 C63 H63C 110.5 . . ?
C62 C63 H63D 110.5 . . ?
C65 C63 H63D 110.5 . . ?
H63C C63 H63D 108.7 . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C72 O71 Ti3 169.9(8) . . ?
C74 C72 O71 107.9(12) . . ?
C74 C72 C73 128.5(15) . . ?
O71 C72 C73 109.4(9) . . ?
C74 C72 H72 102.6 . . ?
O71 C72 H72 102.6 . . ?
C73 C72 H72 102.6 . . ?
C72 C73 H73A 109.5 . . ?
C72 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C72 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C72 C74 H74A 109.5 . . ?
C72 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C72 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?

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
O17 Ti1 O16 Ti2 -22.5(6) . . . . ?
O21 Ti1 O16 Ti2 155.2(5) . . . . ?
O61 Ti1 O16 Ti2 67.8(5) . . . . ?
O52 Ti1 O16 Ti2 -113.0(5) . . . . ?
O23 Ti1 O16 Ti2 161.2(6) . . . . ?
Ti3 Ti1 O16 Ti2 175.9(7) . . . . ?
O17 Ti1 O16 Ti3 161.5(2) . . . . ?
O21 Ti1 O16 Ti3 -20.8(5) . . . . ?
O61 Ti1 O16 Ti3 -108.2(2) . . . . ?
O52 Ti1 O16 Ti3 71.1(2) . . . . ?
O23 Ti1 O16 Ti3 -14.71(18) . . . . ?
O17 Ti2 O16 Ti1 -13.7(6) 2_676 . . . ?
O1 Ti2 O16 Ti1 158.9(5) . . . . ?
O41 Ti2 O16 Ti1 -105.1(5) . . . . ?
O62 Ti2 O16 Ti1 76.4(5) 2_676 . . . ?
O3 Ti2 O16 Ti1 169.3(6) . . . . ?
Ti3 Ti2 O16 Ti1 -175.9(7) . . . . ?
O17 Ti2 O16 Ti3 162.3(2) 2_676 . . . ?
O1 Ti2 O16 Ti3 -25.1(5) . . . . ?
O41 Ti2 O16 Ti3 70.9(2) . . . . ?
O62 Ti2 O16 Ti3 -107.6(2) 2_676 . . . ?
O3 Ti2 O16 Ti3 -14.73(19) . . . . ?
O16 Ti1 O17 Ti2 84.9(4) . . . 2_676 ?
O21 Ti1 O17 Ti2 -94.0(4) . . . 2_676 ?
O61 Ti1 O17 Ti2 -4.8(4) . . . 2_676 ?
O52 Ti1 O17 Ti2 174.8(4) . . . 2_676 ?
Ti3 Ti1 O17 Ti2 104.8(4) . . . 2_676 ?
Ti2 O1 C2 O2 -170.4(6) . . . . ?
Ti2 O1 C2 C3 10.6(9) . . . . ?
O2 C2 C3 O3 174.3(8) . . . . ?
O1 C2 C3 O3 -6.8(9) . . . . ?
O2 C2 C3 C4 -61.7(10) . . . . ?
O1 C2 C3 C4 117.2(7) . . . . ?
O2 C2 C3 C15 52.8(11) . . . . ?
O1 C2 C3 C15 -128.3(7) . . . . ?
C4 C3 O3 Ti3 48.3(9) . . . . ?
C15 C3 O3 Ti3 -69.6(9) . . . . ?
C2 C3 O3 Ti3 169.0(5) . . . . ?
C4 C3 O3 Ti2 -119.5(6) . . . . ?
C15 C3 O3 Ti2 122.6(5) . . . . ?
C2 C3 O3 Ti2 1.2(7) . . . . ?
O3 C3 C4 C5 60.1(10) . . . . ?
C15 C3 C4 C5 -178.1(7) . . . . ?
C2 C3 C4 C5 -59.2(9) . . . . ?
O3 C3 C4 C9 -125.5(6) . . . . ?
C15 C3 C4 C9 -3.7(7) . . . . ?
C2 C3 C4 C9 115.2(6) . . . . ?
C9 C4 C5 C6 0.6(11) . . . . ?
C3 C4 C5 C6 174.6(7) . . . . ?
C4 C5 C6 C7 -1.1(12) . . . . ?
C5 C6 C7 C8 1.3(14) . . . . ?
C6 C7 C8 C9 -1.1(13) . . . . ?
C7 C8 C9 C4 0.6(12) . . . . ?
C7 C8 C9 C10 -178.8(8) . . . . ?
C5 C4 C9 C8 -0.4(10) . . . . ?
C3 C4 C9 C8 -175.5(7) . . . . ?
C5 C4 C9 C10 179.2(6) . . . . ?
C3 C4 C9 C10 4.0(7) . . . . ?
C8 C9 C10 C15 176.7(8) . . . . ?
C4 C9 C10 C15 -2.8(8) . . . . ?
C8 C9 C10 C11 -3.7(13) . . . . ?
C4 C9 C10 C11 176.9(8) . . . . ?
C15 C10 C11 C12 -1.1(11) . . . . ?
C9 C10 C11 C12 179.2(7) . . . . ?
C10 C11 C12 C13 0.2(13) . . . . ?
C11 C12 C13 C14 0.3(13) . . . . ?
C12 C13 C14 C15 0.3(11) . . . . ?
C13 C14 C15 C10 -1.2(10) . . . . ?
C13 C14 C15 C3 179.9(6) . . . . ?
C11 C10 C15 C14 1.7(11) . . . . ?
C9 C10 C15 C14 -178.6(6) . . . . ?
C11 C10 C15 C3 -179.3(6) . . . . ?
C9 C10 C15 C3 0.5(7) . . . . ?
O3 C3 C15 C14 -55.4(9) . . . . ?
C4 C3 C15 C14 -179.2(7) . . . . ?
C2 C3 C15 C14 63.4(9) . . . . ?
O3 C3 C15 C10 125.7(6) . . . . ?
C4 C3 C15 C10 1.9(7) . . . . ?
C2 C3 C15 C10 -115.5(7) . . . . ?
Ti1 O21 C22 O22 -176.4(5) . . . . ?
Ti1 O21 C22 C23 1.4(8) . . . . ?
Ti3 O23 C23 C24 41.2(11) . . . . ?
Ti1 O23 C23 C24 -131.4(6) . . . . ?
Ti3 O23 C23 C22 163.8(5) . . . . ?
Ti1 O23 C23 C22 -8.8(7) . . . . ?
Ti3 O23 C23 C35 -73.9(8) . . . . ?
Ti1 O23 C23 C35 113.5(6) . . . . ?
O22 C22 C23 O23 -177.2(6) . . . . ?
O21 C22 C23 O23 4.9(8) . . . . ?
O22 C22 C23 C24 -51.3(9) . . . . ?
O21 C22 C23 C24 130.9(6) . . . . ?
O22 C22 C23 C35 59.8(9) . . . . ?
O21 C22 C23 C35 -118.0(6) . . . . ?
O23 C23 C24 C25 55.3(11) . . . . ?
C22 C23 C24 C25 -65.5(9) . . . . ?
C35 C23 C24 C25 176.8(7) . . . . ?
O23 C23 C24 C29 -127.8(7) . . . . ?
C22 C23 C24 C29 111.4(7) . . . . ?
C35 C23 C24 C29 -6.4(7) . . . . ?
C29 C24 C25 C26 2.5(11) . . . . ?
C23 C24 C25 C26 179.0(7) . . . . ?
C24 C25 C26 C27 -3.8(11) . . . . ?
C25 C26 C27 C28 3.7(12) . . . . ?
C26 C27 C28 C29 -2.0(11) . . . . ?
C27 C28 C29 C24 0.6(10) . . . . ?
C27 C28 C29 C30 176.5(7) . . . . ?
C25 C24 C29 C28 -1.0(11) . . . . ?
C23 C24 C29 C28 -178.0(6) . . . . ?
C25 C24 C29 C30 -177.6(6) . . . . ?
C23 C24 C29 C30 5.4(8) . . . . ?
C28 C29 C30 C31 0.1(13) . . . . ?
C24 C29 C30 C31 176.3(7) . . . . ?
C28 C29 C30 C35 -178.0(7) . . . . ?
C24 C29 C30 C35 -1.8(8) . . . . ?
C35 C30 C31 C32 0.5(11) . . . . ?
C29 C30 C31 C32 -177.4(7) . . . . ?
C30 C31 C32 C33 0.0(12) . . . . ?
C31 C32 C33 C34 -0.4(12) . . . . ?
C32 C33 C34 C35 0.1(12) . . . . ?
C33 C34 C35 C30 0.6(11) . . . . ?
C33 C34 C35 C23 -179.5(7) . . . . ?
C31 C30 C35 C34 -0.9(11) . . . . ?
C29 C30 C35 C34 177.5(6) . . . . ?
C31 C30 C35 C23 179.2(6) . . . . ?
C29 C30 C35 C23 -2.5(8) . . . . ?
O23 C23 C35 C34 -51.1(10) . . . . ?
C24 C23 C35 C34 -174.7(7) . . . . ?
C22 C23 C35 C34 68.6(9) . . . . ?
O23 C23 C35 C30 128.9(6) . . . . ?
C24 C23 C35 C30 5.3(7) . . . . ?
C22 C23 C35 C30 -111.5(7) . . . . ?
Ti3 O42 C42 O41 0.0(11) . . . . ?
Ti3 O42 C42 C43 177.7(6) . . . . ?
Ti2 O41 C42 O42 -3.5(10) . . . . ?
Ti2 O41 C42 C43 178.8(6) . . . . ?
O42 C42 C43 C44 -18.1(12) . . . . ?
O41 C42 C43 C44 159.8(8) . . . . ?
Ti1 O52 C52 O51 -1.5(9) . . . . ?
Ti1 O52 C52 C53 179.6(5) . . . . ?
Ti3 O51 C52 O52 -5.3(10) . . . . ?
Ti3 O51 C52 C53 173.6(5) . . . . ?
O52 C52 C53 C54 166.8(8) . . . . ?
O51 C52 C53 C54 -12.1(11) . . . . ?
Ti2 O62 C62 O61 -0.1(10) 2_676 . . . ?
Ti2 O62 C62 C63 -176.0(5) 2_676 . . . ?
Ti1 O61 C62 O62 0.9(10) . . . . ?
Ti1 O61 C62 C63 176.7(5) . . . . ?
O62 C62 C63 C64 56.9(17) . . . . ?
O61 C62 C63 C64 -119.2(16) . . . . ?
O62 C62 C63 C65 94.7(16) . . . . ?
O61 C62 C63 C65 -81.3(16) . . . . ?
O3 Ti3 O71 C72 122(4) . . . . ?
O23 Ti3 O71 C72 -59(4) . . . . ?
O42 Ti3 O71 C72 -149(4) . . . . ?
O51 Ti3 O71 C72 30(4) . . . . ?
Ti1 Ti3 O71 C72 -42(4) . . . . ?
Ti2 Ti3 O71 C72 137(4) . . . . ?
Ti3 O71 C72 C74 163(3) . . . . ?
Ti3 O71 C72 C73 -53(4) . . . . ?

_refine_diff_density_max         0.851
_refine_diff_density_min         -0.953
_refine_diff_density_rms         0.099



_symmetry_cell_setting           triclinic
_symmetry_space_group_name_h-m   'P -1'
_symmetry_int_tables_number      2
_chemical_absolute_configuration .

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_nbk19-3Dshape
_database_code_depnum_ccdc_archive 'CCDC 2284906'
loop_
_audit_author_name
_audit_author_address
'Tadeusz Muziol'
;Nicolaus Copernicus University in Torun, Faculty of Chemistry
Poland
;
_audit_update_record             
;
2023-07-27 deposited with the CCDC.	2024-07-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/1
_shelx_SHELXL_version_number     2018/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_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_melting_point          ?

_exptl_crystal_description       'tiny rhombus'
_exptl_crystal_colour            colourless
_diffrn_ambient_temperature      100(2)
_chemical_formula_weight         1246.86

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

_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.
;

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'

_cell_length_a                   22.4667(4)
_cell_length_b                   12.6262(2)
_cell_length_c                   23.0730(5)
_cell_angle_alpha                90
_cell_angle_beta                 106.0037(19)
_cell_angle_gamma                90
_cell_volume                     6291.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    13846
_cell_measurement_theta_min      3.9750
_cell_measurement_theta_max      78.2820
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_F_000             2632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.707
_shelx_estimated_absorpt_T_min   0.705
_shelx_estimated_absorpt_T_max   0.912
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_correction_T_min  0.746
_exptl_absorpt_correction_T_max  1.000
_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_absorpt_special_details   ?
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_reflns_number            29621
_diffrn_reflns_av_unetI/netI     0.0380
_diffrn_reflns_av_R_equivalents  0.0474
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.986
_diffrn_reflns_theta_max         74.492
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6404
_reflns_number_gt                5499
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.120a (Rigaku OD, 2021)'
_computing_structure_solution    'Olex2 1.3, (Dolomanov, 2009)'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2 1.3, (Dolomanov, 2009)'
_computing_publication_material  ciftab
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0593P)²+7.5391P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.00009(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         6404
_refine_ls_number_parameters     397
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0498
_refine_ls_R_factor_gt           0.0428
_refine_ls_wR_factor_ref         0.1169
_refine_ls_wR_factor_gt          0.1131
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

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_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_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) . . . . ?

_refine_diff_density_max         0.470
_refine_diff_density_min         -0.630
_refine_diff_density_rms         0.066


_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_h-m   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration .

