# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 2018

####################################################################### 
# 
# 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_Ti6cyclobutanA
_database_code_depnum_ccdc_archive 'CCDC 1826634'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H82 O28 Ti6'
_chemical_formula_weight         1490.62

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.6136(4)
_cell_length_b                   12.9095(7)
_cell_length_c                   13.5706(7)
_cell_angle_alpha                95.160(2)
_cell_angle_beta                 96.711(2)
_cell_angle_gamma                105.180(2)
_cell_volume                     1601.48(14)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    12883
_cell_measurement_theta_min      2.373
_cell_measurement_theta_max      24.540

_exptl_crystal_description       brick
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             774
_exptl_absorpt_coefficient_mu    0.797
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5693
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            12864
_diffrn_reflns_av_R_equivalents  0.0561
_diffrn_reflns_av_sigmaI/netI    0.0934
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.52
_diffrn_reflns_theta_max         25.01
_reflns_number_total             5603
_reflns_number_gt                3421
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0657P)²+0.7700P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5603
_refine_ls_number_parameters     436
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1097
_refine_ls_R_factor_gt           0.0568
_refine_ls_wR_factor_ref         0.1450
_refine_ls_wR_factor_gt          0.1250
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_restrained_S_all      1.004
_refine_ls_shift/su_max          0.000
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.68156(10) 0.29463(7) 0.24958(7) 0.0301(3) Uani 1 1 d . . .
Ti2 Ti 0.79860(10) 0.33409(7) 0.45669(6) 0.0281(3) Uani 1 1 d . . .
Ti3 Ti 1.01152(10) 0.46777(7) 0.67232(6) 0.0273(2) Uani 1 1 d . . .
O1 O 0.8635(3) 0.3945(2) 0.3447(2) 0.0242(7) Uani 1 1 d . . .
O2 O 0.6313(3) 0.2683(2) 0.3733(2) 0.0295(8) Uani 1 1 d . . .
O3 O 0.9821(3) 0.4040(2) 0.5517(2) 0.0288(8) Uani 1 1 d . . .
O4 O 0.5246(4) 0.2139(3) 0.1706(2) 0.0331(9) Uani 1 1 d . . .
C1 C 0.4211(6) 0.1791(6) 0.0845(4) 0.0589(18) Uani 1 1 d . . .
H1 H 0.3849 0.2423 0.0679 0.071 Uiso 1 1 calc R . .
C2 C 0.2936(6) 0.0926(5) 0.1028(5) 0.0608(19) Uani 1 1 d . . .
H2A H 0.3232 0.0268 0.1126 0.091 Uiso 1 1 calc R . .
H2B H 0.2166 0.0776 0.0451 0.091 Uiso 1 1 calc R . .
H2C H 0.2570 0.1166 0.1627 0.091 Uiso 1 1 calc R . .
C3 C 0.4926(9) 0.1500(9) 0.0026(6) 0.157(5) Uani 1 1 d . . .
H3A H 0.5653 0.2142 -0.0108 0.236 Uiso 1 1 calc R . .
H3B H 0.4203 0.1214 -0.0573 0.236 Uiso 1 1 calc R . .
H3C H 0.5410 0.0948 0.0202 0.236 Uiso 1 1 calc R . .
O5 O 0.7911(4) 0.1790(3) 0.2573(2) 0.0330(8) Uani 1 1 d . . .
O6 O 0.8770(3) 0.2056(2) 0.4215(3) 0.0324(8) Uani 1 1 d . . .
C4 C 0.8594(5) 0.1549(4) 0.3335(4) 0.0345(13) Uani 1 1 d . . .
C5 C 0.9208(6) 0.0609(4) 0.3210(5) 0.0455(16) Uani 1 1 d . . .
H5 H 1.0293 0.0866 0.3377 0.055 Uiso 1 1 calc R . .
C6 C 0.8650(10) -0.0344(5) 0.3746(6) 0.097(3) Uani 1 1 d . . .
H6A H 0.7642 -0.0432 0.3888 0.116 Uiso 1 1 calc R . .
H6B H 0.9308 -0.0370 0.4356 0.116 Uiso 1 1 calc R . .
C7 C 0.8756(8) -0.1082(5) 0.2859(6) 0.086(3) Uani 1 1 d . . .
H7A H 0.9658 -0.1319 0.2918 0.103 Uiso 1 1 calc R . .
H7B H 0.7883 -0.1704 0.2654 0.103 Uiso 1 1 calc R . .
C8 C 0.8805(9) -0.0165(6) 0.2255(5) 0.076(2) Uani 1 1 d . . .
H8A H 0.7851 -0.0190 0.1874 0.092 Uiso 1 1 calc R . .
H8B H 0.9574 -0.0061 0.1818 0.092 Uiso 1 1 calc R . .
O7 O 0.7923(4) 0.3371(3) 0.1360(2) 0.0383(9) Uani 1 1 d . . .
O8 O 1.0034(4) 0.5290(3) 0.8238(2) 0.0316(8) Uani 1 1 d . . .
C9 C 1.0851(6) 0.6095(4) 0.8803(4) 0.0310(12) Uani 1 1 d . . .
C10 C 1.0404(6) 0.6469(4) 0.9775(4) 0.0399(14) Uani 1 1 d . . .
H10 H 1.0822 0.6117 1.0318 0.048 Uiso 1 1 calc R . .
C11 C 1.0734(9) 0.7644(6) 1.0122(5) 0.075(2) Uani 1 1 d . . .
H11A H 1.1613 0.7920 1.0631 0.090 Uiso 1 1 calc R . .
H11B H 1.0779 0.8098 0.9570 0.090 Uiso 1 1 calc R . .
C12 C 0.9383(8) 0.7467(6) 1.0537(6) 0.081(3) Uani 1 1 d . . .
H12A H 0.8815 0.7981 1.0368 0.098 Uiso 1 1 calc R . .
H12B H 0.9492 0.7411 1.1264 0.098 Uiso 1 1 calc R . .
C13 C 0.8850(7) 0.6357(6) 0.9867(6) 0.079(2) Uani 1 1 d . . .
H13A H 0.8399 0.5744 1.0220 0.095 Uiso 1 1 calc R . .
H13B H 0.8235 0.6363 0.9231 0.095 Uiso 1 1 calc R . .
O9 O 0.6173(4) 0.4303(3) 0.2420(2) 0.0349(9) Uani 1 1 d . . .
O10 O 1.1884(4) 0.4244(3) 0.7283(2) 0.0313(8) Uani 1 1 d . . .
C14 C 1.3237(6) 0.4690(4) 0.7546(3) 0.0281(12) Uani 1 1 d . . .
C15 C 1.4171(5) 0.3986(4) 0.7834(4) 0.0330(13) Uani 1 1 d . . .
C16A C 1.5854(15) 0.4529(14) 0.8238(16) 0.058(5) Uani 0.505(11) 1 d P A 1
H16A H 1.6503 0.4445 0.7739 0.069 Uiso 0.505(11) 1 calc PR A 1
H16B H 1.6072 0.5295 0.8529 0.069 Uiso 0.505(11) 1 calc PR A 1
C17A C 1.5814(13) 0.3755(10) 0.9015(10) 0.041(4) Uani 0.505(11) 1 d P A 1
H17A H 1.6273 0.4105 0.9697 0.050 Uiso 0.505(11) 1 calc PR A 1
H17B H 1.6160 0.3119 0.8818 0.050 Uiso 0.505(11) 1 calc PR A 1
C18A C 1.4100(13) 0.3540(11) 0.8818(8) 0.042(4) Uani 0.505(11) 1 d P A 1
H18A H 1.3564 0.2764 0.8751 0.051 Uiso 0.505(11) 1 calc PR A 1
H18B H 1.3724 0.3967 0.9313 0.051 Uiso 0.505(11) 1 calc PR A 1
C16B C 1.5419(15) 0.4067(11) 0.7332(12) 0.058(5) Uani 0.495(11) 1 d P A 2
H16C H 1.5746 0.4759 0.7053 0.069 Uiso 0.495(11) 1 calc PR A 2
H16D H 1.5323 0.3441 0.6826 0.069 Uiso 0.495(11) 1 calc PR A 2
C17B C 1.6257(15) 0.4028(13) 0.8285(13) 0.051(5) Uani 0.495(11) 1 d P A 2
H17C H 1.7224 0.4567 0.8418 0.062 Uiso 0.495(11) 1 calc PR A 2
H17D H 1.6347 0.3296 0.8383 0.062 Uiso 0.495(11) 1 calc PR A 2
C18B C 1.5108(18) 0.4358(13) 0.8853(10) 0.056(5) Uani 0.495(11) 1 d P A 2
H18C H 1.4793 0.3911 0.9385 0.067 Uiso 0.495(11) 1 calc PR A 2
H18D H 1.5329 0.5141 0.9082 0.067 Uiso 0.495(11) 1 calc PR A 2
O11 O 0.7277(4) 0.2616(3) 0.5754(2) 0.0351(9) Uani 1 1 d . . .
O12 O 0.8802(4) 0.3321(3) 0.7175(2) 0.0340(9) Uani 1 1 d . . .
C19 C 0.7775(6) 0.2583(4) 0.6646(4) 0.0354(13) Uani 1 1 d . . .
C20 C 0.7078(7) 0.1611(5) 0.7098(4) 0.0583(19) Uani 1 1 d . . .
H20 H 0.7490 0.1662 0.7819 0.070 Uiso 1 1 calc R . .
C21 C 0.7027(7) 0.0516(4) 0.6511(5) 0.0612(19) Uani 1 1 d . . .
H21A H 0.7246 0.0570 0.5820 0.073 Uiso 1 1 calc R . .
H21B H 0.7619 0.0106 0.6870 0.073 Uiso 1 1 calc R . .
C22 C 0.5385(7) 0.0118(6) 0.6578(7) 0.093(3) Uani 1 1 d . . .
H22A H 0.4773 -0.0178 0.5923 0.111 Uiso 1 1 calc R . .
H22B H 0.5154 -0.0392 0.7077 0.111 Uiso 1 1 calc R . .
C23 C 0.5378(7) 0.1250(4) 0.6935(5) 0.0581(19) Uani 1 1 d . . .
H23A H 0.4950 0.1311 0.7560 0.070 Uiso 1 1 calc R . .
H23B H 0.4934 0.1607 0.6416 0.070 Uiso 1 1 calc R . .
O13 O 0.7195(3) 0.4580(3) 0.4993(2) 0.0300(8) Uani 1 1 d . . .
O14 O 0.8422(3) 0.5317(3) 0.6510(2) 0.0322(9) Uani 1 1 d . . .
C24 C 0.7489(6) 0.5291(4) 0.5758(4) 0.0339(13) Uani 1 1 d . . .
C25 C 0.6693(6) 0.6134(4) 0.5742(4) 0.0392(14) Uani 1 1 d . . .
H25 H 0.5635 0.5790 0.5753 0.047 Uiso 1 1 calc R . .
C26 C 0.6855(11) 0.6847(6) 0.4910(5) 0.102(3) Uani 1 1 d . . .
H26A H 0.7753 0.6890 0.4607 0.123 Uiso 1 1 calc R . .
H26B H 0.5989 0.6664 0.4387 0.123 Uiso 1 1 calc R . .
C27 C 0.6953(6) 0.7805(4) 0.5631(4) 0.0484(16) Uani 1 1 d . . .
H27A H 0.6037 0.8023 0.5607 0.058 Uiso 1 1 calc R . .
H27B H 0.7790 0.8432 0.5596 0.058 Uiso 1 1 calc R . .
C28 C 0.7208(6) 0.7150(4) 0.6502(4) 0.0453(15) Uani 1 1 d . . .
H28A H 0.8240 0.7312 0.6808 0.054 Uiso 1 1 calc R . .
H28B H 0.6566 0.7175 0.7018 0.054 Uiso 1 1 calc R . .


_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 O4 1.764(3) . ?
Ti1 O2 1.837(3) . ?
Ti1 O7 2.010(4) . ?
Ti1 O9 2.011(4) . ?
Ti1 O5 2.042(3) . ?
Ti1 O1 2.093(3) . ?
Ti1 Ti2 2.8509(12) . ?
Ti2 O2 1.810(3) . ?
Ti2 O1 1.867(3) . ?
Ti2 O3 2.003(3) . ?
Ti2 O13 2.011(3) . ?
Ti2 O11 2.031(3) . ?
Ti2 O6 2.035(3) . ?
Ti3 O3 1.722(3) . ?
Ti3 O1 1.918(3) 2_766 ?
Ti3 O14 2.013(3) . ?
Ti3 O10 2.013(3) . ?
Ti3 O12 2.063(3) . ?
Ti3 O8 2.152(3) . ?
O1 Ti3 1.918(3) 2_766 ?
O4 C1 1.399(6) . ?
C1 C3 1.445(10) . ?
C1 C2 1.488(8) . ?
O5 C4 1.266(6) . ?
O6 C4 1.280(6) . ?
C4 C5 1.487(7) . ?
C5 C6 1.495(8) . ?
C5 C8 1.509(8) . ?
C6 C7 1.496(10) . ?
C7 C8 1.493(9) . ?
O7 C9 1.255(6) 2_766 ?
O8 C9 1.255(5) . ?
C9 O7 1.255(6) 2_766 ?
C9 C10 1.511(7) . ?
C10 C13 1.483(8) . ?
C10 C11 1.486(8) . ?
C11 C12 1.448(9) . ?
C12 C13 1.554(9) . ?
O9 C14 1.269(5) 2_766 ?
O10 C14 1.270(6) . ?
C14 O9 1.269(5) 2_766 ?
C14 C15 1.481(7) . ?
C15 C16B 1.433(13) . ?
C15 C18A 1.503(11) . ?
C15 C18B 1.522(13) . ?
C15 C16A 1.593(15) . ?
C15 C17B 2.012(16) . ?
C16A C17A 1.51(2) . ?
C17A C18A 1.584(16) . ?
C16B C17B 1.45(2) . ?
C17B C18B 1.54(2) . ?
O11 C19 1.258(6) . ?
O12 C19 1.271(6) . ?
C19 C20 1.481(7) . ?
C20 C21 1.545(8) . ?
C20 C23 1.561(9) . ?
C21 C22 1.543(9) . ?
C22 C23 1.501(9) . ?
O13 C24 1.274(6) . ?
O14 C24 1.269(6) . ?
C24 C25 1.486(7) . ?
C25 C26 1.517(8) . ?
C25 C28 1.524(7) . ?
C26 C27 1.483(8) . ?
C27 C28 1.547(7) . ?

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
O4 Ti1 O2 101.09(15) . . ?
O4 Ti1 O7 94.01(15) . . ?
O2 Ti1 O7 164.07(14) . . ?
O4 Ti1 O9 93.16(14) . . ?
O2 Ti1 O9 97.07(14) . . ?
O7 Ti1 O9 87.02(15) . . ?
O4 Ti1 O5 96.88(15) . . ?
O2 Ti1 O5 88.37(14) . . ?
O7 Ti1 O5 84.82(15) . . ?
O9 Ti1 O5 167.47(13) . . ?
O4 Ti1 O1 177.88(15) . . ?
O2 Ti1 O1 78.32(13) . . ?
O7 Ti1 O1 86.76(13) . . ?
O9 Ti1 O1 84.91(12) . . ?
O5 Ti1 O1 85.15(12) . . ?
O4 Ti1 Ti2 138.84(12) . . ?
O2 Ti1 Ti2 38.23(10) . . ?
O7 Ti1 Ti2 126.06(10) . . ?
O9 Ti1 Ti2 97.48(10) . . ?
O5 Ti1 Ti2 79.81(10) . . ?
O1 Ti1 Ti2 40.88(8) . . ?
O2 Ti2 O1 85.24(14) . . ?
O2 Ti2 O3 178.39(14) . . ?
O1 Ti2 O3 96.30(13) . . ?
O2 Ti2 O13 91.11(14) . . ?
O1 Ti2 O13 93.23(14) . . ?
O3 Ti2 O13 89.27(13) . . ?
O2 Ti2 O11 93.69(14) . . ?
O1 Ti2 O11 177.38(14) . . ?
O3 Ti2 O11 84.75(13) . . ?
O13 Ti2 O11 89.17(14) . . ?
O2 Ti2 O6 89.84(14) . . ?
O1 Ti2 O6 90.07(14) . . ?
O3 Ti2 O6 89.69(13) . . ?
O13 Ti2 O6 176.63(14) . . ?
O11 Ti2 O6 87.53(14) . . ?
O2 Ti2 Ti1 38.92(10) . . ?
O1 Ti2 Ti1 47.20(9) . . ?
O3 Ti2 Ti1 142.50(10) . . ?
O13 Ti2 Ti1 99.63(10) . . ?
O11 Ti2 Ti1 131.33(10) . . ?
O6 Ti2 Ti1 83.13(10) . . ?
O3 Ti3 O1 99.89(14) . 2_766 ?
O3 Ti3 O14 94.23(15) . . ?
O1 Ti3 O14 87.98(13) 2_766 . ?
O3 Ti3 O10 100.21(15) . . ?
O1 Ti3 O10 89.07(13) 2_766 . ?
O14 Ti3 O10 165.55(14) . . ?
O3 Ti3 O12 90.64(14) . . ?
O1 Ti3 O12 169.45(14) 2_766 . ?
O14 Ti3 O12 90.80(14) . . ?
O10 Ti3 O12 89.51(13) . . ?
O3 Ti3 O8 168.36(14) . . ?
O1 Ti3 O8 89.71(13) 2_766 . ?
O14 Ti3 O8 79.43(13) . . ?
O10 Ti3 O8 86.41(13) . . ?
O12 Ti3 O8 79.78(13) . . ?
Ti2 O1 Ti3 132.99(17) . 2_766 ?
Ti2 O1 Ti1 91.92(13) . . ?
Ti3 O1 Ti1 129.64(15) 2_766 . ?
Ti2 O2 Ti1 102.84(16) . . ?
Ti3 O3 Ti2 131.75(19) . . ?
C1 O4 Ti1 158.2(4) . . ?
O4 C1 C3 108.6(6) . . ?
O4 C1 C2 111.1(5) . . ?
C3 C1 C2 114.8(7) . . ?
C4 O5 Ti1 128.6(3) . . ?
C4 O6 Ti2 124.4(3) . . ?
O5 C4 O6 123.9(5) . . ?
O5 C4 C5 118.5(5) . . ?
O6 C4 C5 117.6(5) . . ?
C4 C5 C6 118.9(5) . . ?
C4 C5 C8 121.1(5) . . ?
C6 C5 C8 87.4(5) . . ?
C5 C6 C7 89.6(6) . . ?
C8 C7 C6 88.0(5) . . ?
C7 C8 C5 89.2(5) . . ?
C9 O7 Ti1 141.0(3) 2_766 . ?
C9 O8 Ti3 130.9(3) . . ?
O8 C9 O7 124.7(5) . 2_766 ?
O8 C9 C10 120.2(5) . . ?
O7 C9 C10 115.0(4) 2_766 . ?
C13 C10 C11 89.0(5) . . ?
C13 C10 C9 121.1(5) . . ?
C11 C10 C9 120.0(5) . . ?
C12 C11 C10 90.6(5) . . ?
C11 C12 C13 87.8(5) . . ?
C10 C13 C12 86.7(5) . . ?
C14 O9 Ti1 137.6(3) 2_766 . ?
C14 O10 Ti3 137.6(3) . . ?
O9 C14 O10 123.9(5) 2_766 . ?
O9 C14 C15 118.5(4) 2_766 . ?
O10 C14 C15 117.6(4) . . ?
C16B C15 C14 116.1(6) . . ?
C16B C15 C18A 121.0(8) . . ?
C14 C15 C18A 119.5(6) . . ?
C16B C15 C18B 92.4(9) . . ?
C14 C15 C18B 114.2(7) . . ?
C18A C15 C18B 47.8(8) . . ?
C16B C15 C16A 50.1(9) . . ?
C14 C15 C16A 118.9(7) . . ?
C18A C15 C16A 85.9(8) . . ?
C18B C15 C16A 43.7(8) . . ?
C16B C15 C17B 46.2(8) . . ?
C14 C15 C17B 142.0(6) . . ?
C18A C15 C17B 77.2(7) . . ?
C18B C15 C17B 49.4(8) . . ?
C16A C15 C17B 23.5(6) . . ?
C17A C16A C15 90.8(9) . . ?
C16A C17A C18A 85.9(9) . . ?
C15 C18A C17A 91.5(8) . . ?
C15 C16B C17B 88.4(10) . . ?
C16B C17B C18B 90.7(12) . . ?
C16B C17B C15 45.4(7) . . ?
C18B C17B C15 48.5(7) . . ?
C15 C18B C17B 82.1(10) . . ?
C19 O11 Ti2 137.7(3) . . ?
C19 O12 Ti3 127.9(3) . . ?
O11 C19 O12 124.8(5) . . ?
O11 C19 C20 116.3(5) . . ?
O12 C19 C20 118.9(5) . . ?
C19 C20 C21 115.4(5) . . ?
C19 C20 C23 116.3(5) . . ?
C21 C20 C23 87.9(4) . . ?
C22 C21 C20 89.3(5) . . ?
C23 C22 C21 90.2(5) . . ?
C22 C23 C20 90.2(5) . . ?
C24 O13 Ti2 134.4(3) . . ?
C24 O14 Ti3 133.5(4) . . ?
O14 C24 O13 123.6(5) . . ?
O14 C24 C25 119.4(5) . . ?
O13 C24 C25 117.0(4) . . ?
C24 C25 C26 118.0(5) . . ?
C24 C25 C28 120.3(4) . . ?
C26 C25 C28 89.0(5) . . ?
C27 C26 C25 90.3(5) . . ?
C26 C27 C28 89.4(4) . . ?
C25 C28 C27 87.7(4) . . ?

_diffrn_measured_fraction_theta_max 0.991
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.991
_refine_diff_density_max         0.912
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.084
####################################################################### 
# 
# 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_Ti6prop
_database_code_depnum_ccdc_archive 'CCDC 1826635'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C36 H64 O28 Ti6'
_chemical_formula_weight         1232.27

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'

_symmetry_cell_setting           ?
_symmetry_space_group_name_H-M   ?

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3628(14)
_cell_length_b                   11.467(2)
_cell_length_c                   12.838(2)
_cell_angle_alpha                73.427(8)
_cell_angle_beta                 89.342(7)
_cell_angle_gamma                75.625(7)
_cell_volume                     1277.0(4)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3071
_cell_measurement_theta_min      2.250
_cell_measurement_theta_max      25.213

_exptl_crystal_description       brick
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.29
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             636
_exptl_absorpt_coefficient_mu    0.981
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5699
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            27774
_diffrn_reflns_av_R_equivalents  0.1313
_diffrn_reflns_av_sigmaI/netI    0.1638
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         28.15
_reflns_number_total             6202
_reflns_number_gt                3413
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'JANA2006 (Petricek, 2006)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0352P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6202
_refine_ls_number_parameters     323
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1345
_refine_ls_R_factor_gt           0.0529
_refine_ls_wR_factor_ref         0.0994
_refine_ls_wR_factor_gt          0.0821
_refine_ls_goodness_of_fit_ref   0.952
_refine_ls_restrained_S_all      0.952
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.28506(7) 0.69112(6) 0.44654(5) 0.00958(16) Uani 1 1 d . . .
Ti2 Ti 0.18486(7) 0.74896(6) 0.22425(5) 0.01003(16) Uani 1 1 d . . .
Ti3 Ti 0.49699(7) 0.47868(6) 0.32471(5) 0.00908(16) Uani 1 1 d . . .
O1 O 0.3624(2) 0.6333(2) 0.33018(18) 0.0093(6) Uani 1 1 d . . .
O2 O 0.5289(2) 0.3938(2) 0.45879(19) 0.0099(6) Uani 1 1 d . . .
O3 O 0.1201(2) 0.7654(2) 0.35768(18) 0.0101(6) Uani 1 1 d . . .
O4 O 0.3576(2) 0.8495(2) 0.38846(19) 0.0108(6) Uani 1 1 d . . .
O5 O 0.2812(2) 0.8911(2) 0.21388(19) 0.0133(6) Uani 1 1 d . . .
C1 C 0.3410(4) 0.9164(3) 0.2902(3) 0.0119(8) Uani 1 1 d . . .
C2 C 0.3942(4) 1.0344(4) 0.2601(3) 0.0193(9) Uani 1 1 d . . .
H2A H 0.4868 1.0189 0.2224 0.023 Uiso 1 1 calc R . .
H2B H 0.3197 1.1017 0.2078 0.023 Uiso 1 1 calc R . .
C3 C 0.4221(4) 1.0808(4) 0.3542(3) 0.0244(10) Uani 1 1 d . . .
H3A H 0.3353 1.0865 0.3976 0.037 Uiso 1 1 calc R . .
H3B H 0.4411 1.1642 0.3266 0.037 Uiso 1 1 calc R . .
H3C H 0.5081 1.0221 0.3997 0.037 Uiso 1 1 calc R . .
O6 O 0.2108(2) 0.7617(2) 0.57206(19) 0.0138(6) Uani 1 1 d . . .
O7 O 0.6307(3) 0.3317(2) 0.28131(19) 0.0121(6) Uani 1 1 d . . .
C4 C 0.2634(4) 0.7558(3) 0.6639(3) 0.0121(8) Uani 1 1 d . . .
C5 C 0.1964(4) 0.8603(4) 0.7130(3) 0.0182(9) Uani 1 1 d . . .
H5A H 0.1942 0.8232 0.7926 0.022 Uiso 1 1 calc R . .
H5B H 0.2617 0.9182 0.7016 0.022 Uiso 1 1 calc R . .
C6 C 0.0435(4) 0.9357(4) 0.6686(3) 0.0284(11) Uani 1 1 d . . .
H6A H 0.0450 0.9778 0.5907 0.043 Uiso 1 1 calc R . .
H6B H 0.0079 0.9989 0.7070 0.043 Uiso 1 1 calc R . .
H6C H -0.0226 0.8796 0.6789 0.043 Uiso 1 1 calc R . .
O8 O 0.2078(2) 0.5407(2) 0.51440(19) 0.0120(6) Uani 1 1 d . . .
O9 O 0.6652(2) 0.5602(2) 0.32502(19) 0.0132(6) Uani 1 1 d . . .
C7 C 0.7603(4) 0.5506(4) 0.3990(3) 0.0114(8) Uani 1 1 d . . .
C8 C 0.8390(4) 0.6518(3) 0.3843(3) 0.0150(9) Uani 1 1 d . . .
H8A H 0.8604 0.6810 0.3068 0.018 Uiso 1 1 calc R . .
H8B H 0.9343 0.6172 0.4281 0.018 Uiso 1 1 calc R . .
C9 C 0.7490(5) 0.7619(4) 0.4182(4) 0.0404(13) Uani 1 1 d . . .
H9A H 0.6609 0.8036 0.3683 0.061 Uiso 1 1 calc R . .
H9B H 0.8086 0.8217 0.4158 0.061 Uiso 1 1 calc R . .
H9C H 0.7190 0.7320 0.4924 0.061 Uiso 1 1 calc R . .
O10 O 0.3083(3) 0.7224(2) 0.09961(19) 0.0150(6) Uani 1 1 d . . .
O11 O 0.5034(3) 0.5572(2) 0.15341(19) 0.0132(6) Uani 1 1 d . . .
C10 C 0.4301(4) 0.6533(4) 0.0839(3) 0.0115(8) Uani 1 1 d . . .
C11 C 0.4859(4) 0.6893(4) -0.0278(3) 0.0168(9) Uani 1 1 d . . .
H11A H 0.4646 0.7822 -0.0546 0.020 Uiso 1 1 calc R . .
H11B H 0.4301 0.6617 -0.0773 0.020 Uiso 1 1 calc R . .
C12 C 0.6487(4) 0.6351(4) -0.0346(3) 0.0219(10) Uani 1 1 d . . .
H12A H 0.7056 0.6653 0.0109 0.033 Uiso 1 1 calc R . .
H12B H 0.6748 0.6617 -0.1103 0.033 Uiso 1 1 calc R . .
H12C H 0.6714 0.5430 -0.0088 0.033 Uiso 1 1 calc R . .
O12 O 0.1276(2) 0.5874(2) 0.2344(2) 0.0130(6) Uani 1 1 d . . .
O13 O 0.3206(2) 0.4196(2) 0.29320(19) 0.0118(6) Uani 1 1 d . . .
C13 C 0.1855(4) 0.4704(4) 0.2643(3) 0.0126(8) Uani 1 1 d . . .
C14 C 0.0852(4) 0.3852(4) 0.2668(3) 0.0165(9) Uani 1 1 d . . .
H14A H 0.0410 0.3686 0.3383 0.020 Uiso 1 1 calc R . .
H14B H 0.1451 0.3037 0.2601 0.020 Uiso 1 1 calc R . .
C15 C -0.0376(4) 0.4384(4) 0.1778(3) 0.0206(10) Uani 1 1 d . . .
H15A H -0.1009 0.5169 0.1861 0.031 Uiso 1 1 calc R . .
H15B H -0.0966 0.3776 0.1830 0.031 Uiso 1 1 calc R . .
H15C H 0.0050 0.4554 0.1066 0.031 Uiso 1 1 calc R . .
O14 O 0.0232(2) 0.8348(2) 0.13940(19) 0.0128(6) Uani 1 1 d . . .
C16 C -0.0911(5) 0.8337(5) 0.0695(4) 0.0476(15) Uani 1 1 d . . .
H16 H -0.1134 0.7512 0.1054 0.057 Uiso 1 1 calc R . .
C17 C -0.0415(4) 0.8198(4) -0.0344(3) 0.0322(11) Uani 1 1 d . . .
H17A H -0.0206 0.8982 -0.0783 0.048 Uiso 1 1 calc R . .
H17B H -0.1188 0.8008 -0.0727 0.048 Uiso 1 1 calc R . .
H17C H 0.0484 0.7509 -0.0226 0.048 Uiso 1 1 calc R . .
C18 C -0.2299(4) 0.9248(5) 0.0748(4) 0.0357(12) Uani 1 1 d . . .
H18A H -0.2534 0.9137 0.1511 0.054 Uiso 1 1 calc R . .
H18B H -0.3096 0.9113 0.0346 0.054 Uiso 1 1 calc R . .
H18C H -0.2194 1.0104 0.0424 0.054 Uiso 1 1 calc R . .


_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 O3 1.801(2) . ?
Ti1 O1 1.870(2) . ?
Ti1 O2 1.998(2) 2_666 ?
Ti1 O8 2.002(2) . ?
Ti1 O4 2.035(2) . ?
Ti1 O6 2.043(2) . ?
Ti1 Ti2 2.8525(10) . ?
Ti1 Ti3 3.3884(11) 2_666 ?
Ti2 O14 1.770(2) . ?
Ti2 O3 1.855(2) . ?
Ti2 O10 2.012(2) . ?
Ti2 O12 2.022(2) . ?
Ti2 O5 2.023(2) . ?
Ti2 O1 2.074(2) . ?
Ti3 O2 1.706(2) . ?
Ti3 O1 1.922(2) . ?
Ti3 O13 2.019(2) . ?
Ti3 O9 2.021(2) . ?
Ti3 O7 2.047(2) . ?
Ti3 O11 2.132(3) . ?
Ti3 Ti1 3.3884(11) 2_666 ?
O2 Ti1 1.998(2) 2_666 ?
O4 C1 1.263(4) . ?
O5 C1 1.270(4) . ?
C1 C2 1.504(5) . ?
C2 C3 1.501(5) . ?
O6 C4 1.260(4) . ?
O7 C4 1.267(4) 2_666 ?
C4 O7 1.267(4) 2_666 ?
C4 C5 1.509(5) . ?
C5 C6 1.499(5) . ?
O8 C7 1.268(4) 2_666 ?
O9 C7 1.272(4) . ?
C7 O8 1.268(4) 2_666 ?
C7 C8 1.490(5) . ?
C8 C9 1.507(5) . ?
O10 C10 1.267(4) . ?
O11 C10 1.248(4) . ?
C10 C11 1.501(5) . ?
C11 C12 1.507(5) . ?
O12 C13 1.261(4) . ?
O13 C13 1.265(4) . ?
C13 C14 1.508(5) . ?
C14 C15 1.511(5) . ?
O14 C16 1.409(4) . ?
C16 C17 1.445(6) . ?
C16 C18 1.466(6) . ?

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
O3 Ti1 O1 84.92(10) . . ?
O3 Ti1 O2 178.05(10) . 2_666 ?
O1 Ti1 O2 93.13(10) . 2_666 ?
O3 Ti1 O8 91.11(10) . . ?
O1 Ti1 O8 94.33(10) . . ?
O2 Ti1 O8 88.92(10) 2_666 . ?
O3 Ti1 O4 89.57(10) . . ?
O1 Ti1 O4 90.52(10) . . ?
O2 Ti1 O4 90.56(9) 2_666 . ?
O8 Ti1 O4 175.15(10) . . ?
O3 Ti1 O6 96.62(10) . . ?
O1 Ti1 O6 176.06(10) . . ?
O2 Ti1 O6 85.33(10) 2_666 . ?
O8 Ti1 O6 89.28(10) . . ?
O4 Ti1 O6 85.87(10) . . ?
O3 Ti1 Ti2 39.40(7) . . ?
O1 Ti1 Ti2 46.58(7) . . ?
O2 Ti1 Ti2 138.71(7) 2_666 . ?
O8 Ti1 Ti2 100.96(7) . . ?
O4 Ti1 Ti2 82.57(7) . . ?
O6 Ti1 Ti2 134.18(8) . . ?
O3 Ti1 Ti3 159.40(7) . 2_666 ?
O1 Ti1 Ti3 108.78(8) . 2_666 ?
O2 Ti1 Ti3 21.90(6) 2_666 2_666 ?
O8 Ti1 Ti3 72.99(7) . 2_666 ?
O4 Ti1 Ti3 105.20(7) . 2_666 ?
O6 Ti1 Ti3 70.76(7) . 2_666 ?
Ti2 Ti1 Ti3 154.93(3) . 2_666 ?
O14 Ti2 O3 100.21(11) . . ?
O14 Ti2 O10 94.04(11) . . ?
O3 Ti2 O10 164.67(10) . . ?
O14 Ti2 O12 89.54(10) . . ?
O3 Ti2 O12 96.99(10) . . ?
O10 Ti2 O12 88.70(10) . . ?
O14 Ti2 O5 99.01(11) . . ?
O3 Ti2 O5 87.92(10) . . ?
O10 Ti2 O5 84.26(9) . . ?
O12 Ti2 O5 169.26(10) . . ?
O14 Ti2 O1 173.80(10) . . ?
O3 Ti2 O1 78.03(10) . . ?
O10 Ti2 O1 88.38(10) . . ?
O12 Ti2 O1 84.80(9) . . ?
O5 Ti2 O1 86.90(9) . . ?
O14 Ti2 Ti1 138.08(8) . . ?
O3 Ti2 Ti1 38.05(7) . . ?
O10 Ti2 Ti1 127.14(8) . . ?
O12 Ti2 Ti1 97.93(7) . . ?
O5 Ti2 Ti1 80.05(7) . . ?
O1 Ti2 Ti1 40.92(6) . . ?
O2 Ti3 O1 102.65(11) . . ?
O2 Ti3 O13 97.26(10) . . ?
O1 Ti3 O13 88.20(9) . . ?
O2 Ti3 O9 94.24(10) . . ?
O1 Ti3 O9 88.59(10) . . ?
O13 Ti3 O9 168.48(10) . . ?
O2 Ti3 O7 90.38(11) . . ?
O1 Ti3 O7 166.90(10) . . ?
O13 Ti3 O7 88.78(9) . . ?
O9 Ti3 O7 91.87(9) . . ?
O2 Ti3 O11 167.11(11) . . ?
O1 Ti3 O11 89.31(10) . . ?
O13 Ti3 O11 87.81(9) . . ?
O9 Ti3 O11 81.09(9) . . ?
O7 Ti3 O11 77.84(10) . . ?
O2 Ti3 Ti1 25.90(7) . 2_666 ?
O1 Ti3 Ti1 116.48(7) . 2_666 ?
O13 Ti3 Ti1 117.80(8) . 2_666 ?
O9 Ti3 Ti1 73.45(7) . 2_666 ?
O7 Ti3 Ti1 76.09(7) . 2_666 ?
O11 Ti3 Ti1 142.57(7) . 2_666 ?
Ti1 O1 Ti3 132.17(13) . . ?
Ti1 O1 Ti2 92.50(10) . . ?
Ti3 O1 Ti2 129.97(12) . . ?
Ti3 O2 Ti1 132.20(12) . 2_666 ?
Ti1 O3 Ti2 102.55(11) . . ?
C1 O4 Ti1 124.6(2) . . ?
C1 O5 Ti2 128.3(2) . . ?
O4 C1 O5 124.3(3) . . ?
O4 C1 C2 118.7(3) . . ?
O5 C1 C2 116.9(3) . . ?
C3 C2 C1 114.9(3) . . ?
C4 O6 Ti1 136.1(2) . . ?
C4 O7 Ti3 129.2(2) 2_666 . ?
O6 C4 O7 124.9(3) . 2_666 ?
O6 C4 C5 118.2(3) . . ?
O7 C4 C5 117.0(3) 2_666 . ?
C6 C5 C4 115.3(3) . . ?
C7 O8 Ti1 135.3(2) 2_666 . ?
C7 O9 Ti3 132.5(2) . . ?
O8 C7 O9 123.6(3) 2_666 . ?
O8 C7 C8 117.6(3) 2_666 . ?
O9 C7 C8 118.7(3) . . ?
C7 C8 C9 111.8(3) . . ?
C10 O10 Ti2 139.0(2) . . ?
C10 O11 Ti3 134.7(2) . . ?
O11 C10 O10 124.7(3) . . ?
O11 C10 C11 118.7(3) . . ?
O10 C10 C11 116.6(3) . . ?
C10 C11 C12 115.1(3) . . ?
C13 O12 Ti2 138.8(2) . . ?
C13 O13 Ti3 135.9(2) . . ?
O12 C13 O13 124.9(3) . . ?
O12 C13 C14 117.3(3) . . ?
O13 C13 C14 117.8(3) . . ?
C13 C14 C15 113.8(3) . . ?
C16 O14 Ti2 147.7(3) . . ?
O14 C16 C17 113.2(4) . . ?
O14 C16 C18 112.4(4) . . ?
C17 C16 C18 120.3(4) . . ?


_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        28.15
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.904
_refine_diff_density_min         -0.914
_refine_diff_density_rms         0.115
####################################################################### 
# 
# 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_aaa
_database_code_depnum_ccdc_archive 'CCDC 1826636'
_audit_update_record             
;
2018-02-28 deposited with the CCDC.
2018-06-19 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C50 H102 O25 Ti6'
_chemical_formula_weight         1390.72

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'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5972(3)
_cell_length_b                   15.6563(3)
_cell_length_c                   19.9053(4)
_cell_angle_alpha                73.2380(10)
_cell_angle_beta                 76.7970(10)
_cell_angle_gamma                83.5880(10)
_cell_volume                     3655.25(13)
_cell_formula_units_Z            2
_cell_measurement_temperature    295(2)
_cell_measurement_reflns_used    9350
_cell_measurement_theta_min      2.199
_cell_measurement_theta_max      24.309

_exptl_crystal_description       fragment
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.2
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.264
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1468
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6138
_exptl_absorpt_correction_T_max  0.7366
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      295(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       'ω- and φ-scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            102190
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0228
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.09
_diffrn_reflns_theta_max         24.82
_reflns_number_total             12570
_reflns_number_gt                9709
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2008)'
_computing_cell_refinement       APEX2
_computing_data_reduction        APEX2
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'DIAMOND (Crystal Impact GbR, 2005)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0886P)²+2.9622P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12570
_refine_ls_number_parameters     758
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0470
_refine_ls_wR_factor_ref         0.1584
_refine_ls_wR_factor_gt          0.1371
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_restrained_S_all      1.074
_refine_ls_shift/su_max          0.117
_refine_ls_shift/su_mean         0.002

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
C1 C 0.4207(3) 0.4083(2) 0.31596(18) 0.0434(8) Uani 1 1 d . . .
C2 C 0.5107(3) 0.4708(2) 0.2751(2) 0.0505(9) Uani 1 1 d . . .
H2 H 0.5798 0.4538 0.2877 0.061 Uiso 1 1 calc R . .
C3 C 0.5062(3) 0.5453(3) 0.2247(2) 0.0545(9) Uani 1 1 d . . .
H3 H 0.5712 0.5768 0.2047 0.065 Uiso 1 1 calc R . .
C4 C 0.4071(3) 0.5842(2) 0.19649(19) 0.0484(8) Uani 1 1 d . . .
C5 C 0.0590(3) 0.4604(2) 0.39653(16) 0.0383(7) Uani 1 1 d . . .
C6 C -0.0159(3) 0.5386(3) 0.40618(18) 0.0490(9) Uani 1 1 d . . .
H6 H -0.0649 0.5323 0.4512 0.059 Uiso 1 1 calc R . .
C7 C -0.0197(3) 0.6155(2) 0.35764(19) 0.0513(9) Uani 1 1 d . . .
H7 H -0.0681 0.6621 0.3701 0.062 Uiso 1 1 calc R . .
C8 C 0.0481(3) 0.6326(2) 0.28446(19) 0.0466(8) Uani 1 1 d . . .
C9 C 0.4480(3) 0.2053(3) 0.4769(2) 0.0629(11) Uani 1 1 d . . .
H9 H 0.4792 0.1518 0.4599 0.075 Uiso 1 1 calc R . .
C10 C 0.4021(5) 0.1736(4) 0.5559(3) 0.0985(18) Uani 1 1 d . . .
H10A H 0.3463 0.1306 0.5645 0.148 Uiso 1 1 calc R . .
H10B H 0.3693 0.2246 0.5738 0.148 Uiso 1 1 calc R . .
H10C H 0.4608 0.1448 0.5808 0.148 Uiso 1 1 calc R . .
C11 C 0.5379(4) 0.2695(4) 0.4575(3) 0.0858(15) Uani 1 1 d . . .
H11A H 0.5651 0.2861 0.4055 0.129 Uiso 1 1 calc R . .
H11B H 0.5976 0.2410 0.4815 0.129 Uiso 1 1 calc R . .
H11C H 0.5093 0.3232 0.4729 0.129 Uiso 1 1 calc R . .
C12 C 0.2871(5) 0.2333(3) 0.2008(2) 0.0940(17) Uani 1 1 d D . .
H12 H 0.2200 0.2652 0.1850 0.113 Uiso 1 1 calc R . .
C13 C 0.3595(6) 0.3016(4) 0.1479(3) 0.136(3) Uani 1 1 d D . .
H13A H 0.3388 0.3600 0.1572 0.204 Uiso 1 1 calc R . .
H13B H 0.3518 0.3047 0.0993 0.204 Uiso 1 1 calc R . .
H13C H 0.4355 0.2851 0.1522 0.204 Uiso 1 1 calc R . .
C14 C 0.2514(11) 0.1466(7) 0.2042(6) 0.291(10) Uani 1 1 d D . .
H14A H 0.2474 0.1071 0.2528 0.437 Uiso 1 1 calc R . .
H14B H 0.3037 0.1203 0.1701 0.437 Uiso 1 1 calc R . .
H14C H 0.1793 0.1540 0.1921 0.437 Uiso 1 1 calc R . .
C15 C -0.0506(4) 0.5511(3) 0.1477(3) 0.0703(12) Uani 1 1 d . . .
H15 H -0.0976 0.5978 0.1205 0.084 Uiso 1 1 calc R . .
C16 C -0.1158(4) 0.5154(4) 0.2225(3) 0.0982(17) Uani 1 1 d . . .
H16A H -0.1310 0.5630 0.2468 0.147 Uiso 1 1 calc R . .
H16B H -0.0739 0.4659 0.2492 0.147 Uiso 1 1 calc R . .
H16C H -0.1847 0.4941 0.2201 0.147 Uiso 1 1 calc R . .
C17 C -0.0172(5) 0.4815(5) 0.1082(4) 0.110(2) Uani 1 1 d . . .
H17A H 0.0302 0.5073 0.0618 0.165 Uiso 1 1 calc R . .
H17B H -0.0823 0.4598 0.1005 0.165 Uiso 1 1 calc R . .
H17C H 0.0224 0.4316 0.1364 0.165 Uiso 1 1 calc R . .
C18 C 0.1065(5) 0.9202(3) 0.1205(3) 0.0856(15) Uani 1 1 d . . .
H18 H 0.0403 0.9332 0.0988 0.103 Uiso 1 1 calc R . .
C19 C 0.1926(7) 0.9826(4) 0.0749(5) 0.148(3) Uani 1 1 d . . .
H19A H 0.2069 0.9780 0.0256 0.222 Uiso 1 1 calc R . .
H19B H 0.2598 0.9669 0.0937 0.222 Uiso 1 1 calc R . .
H19C H 0.1677 1.0440 0.0757 0.222 Uiso 1 1 calc R . .
C20 C 0.0757(7) 0.9307(5) 0.1953(4) 0.130(3) Uani 1 1 d . . .
H20A H 0.0125 0.8953 0.2221 0.194 Uiso 1 1 calc R . .
H20B H 0.0573 0.9937 0.1933 0.194 Uiso 1 1 calc R . .
H20C H 0.1373 0.9099 0.2194 0.194 Uiso 1 1 calc R . .
C21 C 0.3527(4) 0.4578(3) 0.5227(2) 0.0719(13) Uani 1 1 d D . .
H21 H 0.4265 0.4603 0.4903 0.086 Uiso 1 1 calc R . .
C22 C 0.2948(6) 0.5473(3) 0.5018(4) 0.127(3) Uani 1 1 d D . .
H22A H 0.2815 0.5582 0.4533 0.190 Uiso 1 1 calc R . .
H22B H 0.3399 0.5938 0.5028 0.190 Uiso 1 1 calc R . .
H22C H 0.2249 0.5484 0.5356 0.190 Uiso 1 1 calc R . .
C23 C 0.3684(7) 0.4296(5) 0.5985(3) 0.146(3) Uani 1 1 d D . .
H23A H 0.4068 0.3707 0.6078 0.219 Uiso 1 1 calc R . .
H23B H 0.2971 0.4264 0.6314 0.219 Uiso 1 1 calc R . .
H23C H 0.4117 0.4731 0.6059 0.219 Uiso 1 1 calc R . .
C24 C 0.0765(4) 0.2062(3) 0.5305(2) 0.0751(13) Uani 1 1 d . . .
H24 H 0.1009 0.1777 0.4902 0.090 Uiso 1 1 calc R . .
C25 C -0.0360(5) 0.2486(4) 0.5282(4) 0.112(2) Uani 1 1 d . . .
H25A H -0.0337 0.2966 0.4837 0.168 Uiso 1 1 calc R . .
H25B H -0.0621 0.2732 0.5694 0.168 Uiso 1 1 calc R . .
H25C H -0.0855 0.2035 0.5300 0.168 Uiso 1 1 calc R . .
C26 C 0.0827(6) 0.1361(4) 0.6012(4) 0.130(3) Uani 1 1 d . . .
H26A H 0.1593 0.1184 0.6032 0.195 Uiso 1 1 calc R . .
H26B H 0.0439 0.0836 0.6046 0.195 Uiso 1 1 calc R . .
H26C H 0.0488 0.1611 0.6413 0.195 Uiso 1 1 calc R . .
C27 C 0.2788(5) 0.0265(3) 0.4093(4) 0.1001(19) Uani 1 1 d . . .
H27 H 0.3363 0.0147 0.3687 0.120 Uiso 1 1 calc R . .
C28 C 0.1757(9) -0.0082(6) 0.4080(8) 0.228(6) Uani 1 1 d . . .
H28A H 0.1460 0.0301 0.3674 0.342 Uiso 1 1 calc R . .
H28B H 0.1232 -0.0087 0.4528 0.342 Uiso 1 1 calc R . .
H28C H 0.1891 -0.0691 0.4029 0.342 Uiso 1 1 calc R . .
C29 C 0.3144(9) -0.0161(5) 0.4766(6) 0.198(5) Uani 1 1 d . . .
H29A H 0.3799 0.0118 0.4773 0.298 Uiso 1 1 calc R . .
H29B H 0.3311 -0.0798 0.4809 0.298 Uiso 1 1 calc R . .
H29C H 0.2562 -0.0088 0.5169 0.298 Uiso 1 1 calc R . .
C30 C 0.5666(5) 0.1529(4) 0.2865(5) 0.140(3) Uani 1 1 d D . .
H30 H 0.5959 0.1704 0.3230 0.168 Uiso 1 1 calc R . .
C31 C 0.6191(8) 0.2232(6) 0.2259(6) 0.231(6) Uani 1 1 d D . .
H31A H 0.6089 0.2798 0.2389 0.346 Uiso 1 1 calc R . .
H31B H 0.5864 0.2293 0.1845 0.346 Uiso 1 1 calc R . .
H31C H 0.6973 0.2075 0.2138 0.346 Uiso 1 1 calc R . .
C32 C 0.6093(8) 0.0599(5) 0.3054(8) 0.303(10) Uani 1 1 d D . .
H32A H 0.5489 0.0207 0.3305 0.455 Uiso 1 1 calc R . .
H32B H 0.6611 0.0536 0.3368 0.455 Uiso 1 1 calc R . .
H32C H 0.6464 0.0433 0.2617 0.455 Uiso 1 1 calc R . .
C33 C -0.0640(5) 0.2227(6) 0.3291(6) 0.165(4) Uani 1 1 d D . .
H33 H -0.0434 0.1888 0.3756 0.198 Uiso 1 1 calc R . .
C34 C -0.1655(5) 0.2659(6) 0.3604(6) 0.175(4) Uani 1 1 d D . .
H34A H -0.1489 0.3014 0.3897 0.262 Uiso 1 1 calc R . .
H34B H -0.2161 0.2201 0.3905 0.262 Uiso 1 1 calc R . .
H34C H -0.1990 0.3049 0.3219 0.262 Uiso 1 1 calc R . .
C35 C -0.0619(8) 0.1455(6) 0.3011(7) 0.211(6) Uani 1 1 d D . .
H35A H 0.0073 0.1419 0.2673 0.317 Uiso 1 1 calc R . .
H35B H -0.1226 0.1521 0.2765 0.317 Uiso 1 1 calc R . .
H35C H -0.0689 0.0908 0.3409 0.317 Uiso 1 1 calc R . .
C36 C 0.2759(7) 0.5532(5) 0.0148(3) 0.127(3) Uani 1 1 d . . .
H36 H 0.2112 0.5916 0.0008 0.153 Uiso 1 1 calc R . .
C37 C 0.3643(8) 0.6131(6) -0.0085(4) 0.185(5) Uani 1 1 d . . .
H37A H 0.3431 0.6642 0.0116 0.278 Uiso 1 1 calc R . .
H37B H 0.3807 0.6341 -0.0609 0.278 Uiso 1 1 calc R . .
H37C H 0.4292 0.5815 0.0082 0.278 Uiso 1 1 calc R . .
C38 C 0.2831(6) 0.4800(6) -0.0186(3) 0.135(3) Uani 1 1 d . . .
H38A H 0.2177 0.4452 0.0020 0.202 Uiso 1 1 calc R . .
H38B H 0.3479 0.4412 -0.0096 0.202 Uiso 1 1 calc R . .
H38C H 0.2887 0.5046 -0.0704 0.202 Uiso 1 1 calc R . .
C39 C 0.0398(6) 0.7958(4) -0.0281(3) 0.119(2) Uani 1 1 d D . .
H39 H -0.0117 0.8404 -0.0086 0.143 Uiso 1 1 calc R . .
C40 C 0.1247(8) 0.8506(8) -0.0825(4) 0.228(6) Uani 1 1 d D . .
H40A H 0.1504 0.8920 -0.0617 0.342 Uiso 1 1 calc R . .
H40B H 0.0938 0.8845 -0.1239 0.342 Uiso 1 1 calc R . .
H40C H 0.1860 0.8114 -0.0979 0.342 Uiso 1 1 calc R . .
C41 C -0.0311(12) 0.7436(7) -0.0497(6) 0.274(9) Uani 1 1 d D . .
H41A H -0.0558 0.6920 -0.0095 0.411 Uiso 1 1 calc R . .
H41B H 0.0100 0.7230 -0.0907 0.411 Uiso 1 1 calc R . .
H41C H -0.0946 0.7814 -0.0631 0.411 Uiso 1 1 calc R . .
C42 C -0.1740(5) 0.7991(6) 0.1789(5) 0.137(3) Uani 1 1 d . . .
H42 H -0.1598 0.7923 0.2277 0.164 Uiso 1 1 calc R . .
C43 C -0.2111(9) 0.8897(7) 0.1500(8) 0.254(8) Uani 1 1 d . . .
H43A H -0.1484 0.9278 0.1318 0.381 Uiso 1 1 calc R . .
H43B H -0.2626 0.9104 0.1877 0.381 Uiso 1 1 calc R . .
H43C H -0.2474 0.8925 0.1107 0.381 Uiso 1 1 calc R . .
C44 C -0.2584(9) 0.7427(9) 0.1850(12) 0.369(14) Uani 1 1 d . . .
H44A H -0.2289 0.6809 0.1918 0.553 Uiso 1 1 calc R . .
H44B H -0.2878 0.7616 0.1412 0.553 Uiso 1 1 calc R . .
H44C H -0.3167 0.7468 0.2262 0.553 Uiso 1 1 calc R . .
C45 C 0.4629(6) 0.8533(7) 0.0112(4) 0.183(4) Uani 1 1 d D . .
H45 H 0.4585 0.9084 0.0278 0.219 Uiso 1 1 calc R . .
C46 C 0.4476(8) 0.8987(7) -0.0622(4) 0.181(4) Uani 1 1 d D . .
H46A H 0.3852 0.9420 -0.0602 0.272 Uiso 1 1 calc R . .
H46B H 0.4338 0.8545 -0.0850 0.272 Uiso 1 1 calc R . .
H46C H 0.5135 0.9299 -0.0901 0.272 Uiso 1 1 calc R . .
C47 C 0.5691(6) 0.8178(8) 0.0292(5) 0.201(5) Uani 1 1 d D . .
H47A H 0.5709 0.8233 0.0768 0.301 Uiso 1 1 calc R . .
H47B H 0.6276 0.8517 -0.0065 0.301 Uiso 1 1 calc R . .
H47C H 0.5797 0.7548 0.0294 0.301 Uiso 1 1 calc R . .
C48 C 0.3347(9) 0.8086(6) 0.2690(5) 0.184(5) Uani 1 1 d D . .
H48 H 0.2716 0.8468 0.2868 0.221 Uiso 1 1 calc R . .
C49 C 0.3176(11) 0.7293(7) 0.3307(5) 0.229(6) Uani 1 1 d D . .
H49A H 0.2538 0.6992 0.3302 0.344 Uiso 1 1 calc R . .
H49B H 0.3054 0.7474 0.3752 0.344 Uiso 1 1 calc R . .
H49C H 0.3823 0.6884 0.3280 0.344 Uiso 1 1 calc R . .
C50 C 0.4214(9) 0.8709(8) 0.2564(6) 0.228(6) Uani 1 1 d D . .
H50A H 0.3965 0.9314 0.2330 0.342 Uiso 1 1 calc R . .
H50B H 0.4871 0.8526 0.2255 0.342 Uiso 1 1 calc R . .
H50C H 0.4383 0.8699 0.3023 0.342 Uiso 1 1 calc R . .
O1 O 0.21206(17) 0.30369(14) 0.37626(11) 0.0372(5) Uani 1 1 d . . .
O2 O 0.2084(2) 0.67341(16) 0.13746(13) 0.0498(6) Uani 1 1 d . . .
O3 O 0.15597(18) 0.42717(15) 0.22594(12) 0.0426(5) Uani 1 1 d . . .
O4 O 0.4223(2) 0.33946(16) 0.29593(13) 0.0501(6) Uani 1 1 d . . .
O5 O 0.35893(19) 0.42716(15) 0.36892(12) 0.0448(5) Uani 1 1 d . . .
O6 O 0.33153(19) 0.53345(16) 0.20691(13) 0.0481(6) Uani 1 1 d . . .
O7 O 0.4066(2) 0.66621(18) 0.16519(17) 0.0686(8) Uani 1 1 d . . .
O8 O 0.03581(18) 0.41200(16) 0.36172(12) 0.0443(5) Uani 1 1 d . . .
O9 O 0.13710(18) 0.44646(15) 0.42889(12) 0.0435(5) Uani 1 1 d . . .
O10 O 0.12236(19) 0.57529(15) 0.27160(12) 0.0443(5) Uani 1 1 d . . .
O11 O 0.0236(2) 0.70282(17) 0.23894(14) 0.0594(7) Uani 1 1 d . . .
O12 O 0.36266(18) 0.24568(15) 0.43906(12) 0.0452(5) Uani 1 1 d . . .
O13 O 0.2563(2) 0.25291(16) 0.26893(12) 0.0483(6) Uani 1 1 d . . .
O14 O 0.0436(2) 0.59355(17) 0.15007(13) 0.0535(6) Uani 1 1 d . . .
O15 O 0.1466(2) 0.82856(17) 0.12378(15) 0.0633(7) Uani 1 1 d . . .
O16 O 0.2955(2) 0.39139(16) 0.51217(13) 0.0499(6) Uani 1 1 d . . .
O17 O 0.1500(2) 0.27311(16) 0.52253(12) 0.0503(6) Uani 1 1 d . . .
O18 O 0.2639(2) 0.11868(16) 0.39987(15) 0.0573(7) Uani 1 1 d . . .
O19 O 0.4587(2) 0.16413(17) 0.31814(15) 0.0593(7) Uani 1 1 d . . .
O20 O 0.0231(2) 0.27328(19) 0.30398(15) 0.0621(7) Uani 1 1 d . . .
O21 O 0.2476(2) 0.52186(17) 0.09071(13) 0.0564(6) Uani 1 1 d . . .
O22 O 0.0822(3) 0.7445(2) 0.02996(15) 0.0765(9) Uani 1 1 d . . .
O23 O -0.0773(3) 0.7762(2) 0.13441(17) 0.0763(9) Uani 1 1 d . . .
O24 O 0.3737(3) 0.8170(2) 0.0570(2) 0.0963(12) Uani 1 1 d . . .
O25 O 0.3004(4) 0.8019(3) 0.2107(2) 0.1052(13) Uani 1 1 d . . .
Ti1 Ti 0.24737(5) 0.34269(4) 0.45445(3) 0.03732(15) Uani 1 1 d . . .
Ti2 Ti 0.33396(5) 0.21927(4) 0.35153(3) 0.04262(16) Uani 1 1 d . . .
Ti3 Ti 0.13419(5) 0.33392(4) 0.30307(3) 0.03835(16) Uani 1 1 d . . .
Ti4 Ti 0.18841(5) 0.54318(4) 0.17426(3) 0.04188(16) Uani 1 1 d . . .
Ti5 Ti 0.05935(6) 0.72667(5) 0.12515(4) 0.0567(2) Uani 1 1 d . . .
Ti6 Ti 0.28860(6) 0.76449(5) 0.13836(4) 0.0586(2) Uani 1 1 d . . .


_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
C1 O5 1.248(4) . ?
C1 O4 1.249(4) . ?
C1 C2 1.507(5) . ?
C2 C3 1.306(5) . ?
C3 C4 1.482(5) . ?
C4 O6 1.251(4) . ?
C4 O7 1.255(4) . ?
C5 O8 1.258(4) . ?
C5 O9 1.261(4) . ?
C5 C6 1.491(5) . ?
C6 C7 1.313(5) . ?
C7 C8 1.477(5) . ?
C8 O10 1.257(4) . ?
C8 O11 1.266(4) . ?
C9 O12 1.437(4) . ?
C9 C10 1.501(7) . ?
C9 C11 1.507(6) . ?
C12 O13 1.433(5) . ?
C12 C14 1.456(5) . ?
C12 C13 1.488(4) . ?
C15 O14 1.439(5) . ?
C15 C17 1.492(7) . ?
C15 C16 1.506(7) . ?
C18 O15 1.456(5) . ?
C18 C19 1.494(8) . ?
C18 C20 1.502(8) . ?
C21 O16 1.417(4) . ?
C21 C22 1.497(6) . ?
C21 C23 1.498(6) . ?
C24 O17 1.426(5) . ?
C24 C25 1.501(8) . ?
C24 C26 1.527(8) . ?
C27 O18 1.398(5) . ?
C27 C29 1.462(11) . ?
C27 C28 1.470(10) . ?
C30 O19 1.377(6) . ?
C30 C31 1.461(5) . ?
C30 C32 1.468(5) . ?
C33 O20 1.340(6) . ?
C33 C35 1.466(5) . ?
C33 C34 1.471(5) . ?
C36 O21 1.420(6) . ?
C36 C37 1.442(10) . ?
C36 C38 1.467(9) . ?
C39 O22 1.385(6) . ?
C39 C41 1.480(5) . ?
C39 C40 1.480(5) . ?
C42 O23 1.412(7) . ?
C42 C44 1.419(15) . ?
C42 C43 1.436(12) . ?
C45 O24 1.338(7) . ?
C45 C47 1.471(5) . ?
C45 C46 1.476(5) . ?
C48 O25 1.362(8) . ?
C48 C49 1.468(5) . ?
C48 C50 1.476(5) . ?
O1 Ti3 1.860(2) . ?
O1 Ti1 1.979(2) . ?
O1 Ti2 1.981(2) . ?
O2 Ti6 1.844(3) . ?
O2 Ti4 1.981(2) . ?
O2 Ti5 2.005(3) . ?
O3 Ti3 1.780(2) . ?
O3 Ti4 1.849(2) . ?
O4 Ti2 2.170(2) . ?
O5 Ti1 2.156(2) . ?
O6 Ti4 2.028(2) . ?
O7 Ti6 2.059(3) . ?
O8 Ti3 2.054(2) . ?
O9 Ti1 2.042(2) . ?
O10 Ti4 2.105(2) . ?
O11 Ti5 2.135(3) . ?
O12 Ti2 2.018(2) . ?
O12 Ti1 2.021(2) . ?
O13 Ti3 2.006(2) . ?
O13 Ti2 2.014(2) . ?
O14 Ti4 2.010(2) . ?
O14 Ti5 2.020(3) . ?
O15 Ti6 1.990(3) . ?
O15 Ti5 2.027(3) . ?
O16 Ti1 1.787(2) . ?
O17 Ti1 1.793(2) . ?
O18 Ti2 1.798(2) . ?
O19 Ti2 1.791(2) . ?
O20 Ti3 1.771(2) . ?
O21 Ti4 1.770(2) . ?
O22 Ti5 1.793(3) . ?
O23 Ti5 1.799(3) . ?
O24 Ti6 1.757(3) . ?
O25 Ti6 1.745(4) . ?
Ti1 Ti2 3.1484(8) . ?
Ti2 Ti3 3.0962(9) . ?
Ti4 Ti5 3.1487(9) . ?
Ti5 Ti6 3.0949(11) . ?

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
O5 C1 O4 127.4(3) . . ?
O5 C1 C2 116.9(3) . . ?
O4 C1 C2 115.5(3) . . ?
C3 C2 C1 128.6(3) . . ?
C2 C3 C4 124.9(3) . . ?
O6 C4 O7 126.1(3) . . ?
O6 C4 C3 117.7(3) . . ?
O7 C4 C3 116.3(3) . . ?
O8 C5 O9 126.4(3) . . ?
O8 C5 C6 118.5(3) . . ?
O9 C5 C6 115.0(3) . . ?
C7 C6 C5 125.4(3) . . ?
C6 C7 C8 122.8(3) . . ?
O10 C8 O11 125.3(3) . . ?
O10 C8 C7 118.0(3) . . ?
O11 C8 C7 116.7(3) . . ?
O12 C9 C10 110.3(4) . . ?
O12 C9 C11 109.4(3) . . ?
C10 C9 C11 114.0(4) . . ?
O13 C12 C14 111.9(5) . . ?
O13 C12 C13 111.1(4) . . ?
C14 C12 C13 136.4(5) . . ?
O14 C15 C17 110.5(4) . . ?
O14 C15 C16 109.9(4) . . ?
C17 C15 C16 113.1(5) . . ?
O15 C18 C19 109.5(4) . . ?
O15 C18 C20 109.0(4) . . ?
C19 C18 C20 111.1(6) . . ?
O16 C21 C22 110.0(4) . . ?
O16 C21 C23 108.4(4) . . ?
C22 C21 C23 114.6(5) . . ?
O17 C24 C25 109.3(4) . . ?
O17 C24 C26 107.0(4) . . ?
C25 C24 C26 113.0(5) . . ?
O18 C27 C29 109.8(6) . . ?
O18 C27 C28 108.7(6) . . ?
C29 C27 C28 111.6(8) . . ?
O19 C30 C31 120.2(5) . . ?
O19 C30 C32 113.4(5) . . ?
C31 C30 C32 124.3(7) . . ?
O20 C33 C35 116.9(6) . . ?
O20 C33 C34 116.0(6) . . ?
C35 C33 C34 123.3(7) . . ?
O21 C36 C37 111.7(7) . . ?
O21 C36 C38 111.2(6) . . ?
C37 C36 C38 118.3(6) . . ?
O22 C39 C41 111.4(6) . . ?
O22 C39 C40 110.8(6) . . ?
C41 C39 C40 120.4(9) . . ?
O23 C42 C44 110.5(9) . . ?
O23 C42 C43 110.9(7) . . ?
C44 C42 C43 107.8(9) . . ?
O24 C45 C47 117.0(6) . . ?
O24 C45 C46 115.0(7) . . ?
C47 C45 C46 124.0(8) . . ?
O25 C48 C49 114.4(7) . . ?
O25 C48 C50 117.4(8) . . ?
C49 C48 C50 122.8(8) . . ?
Ti3 O1 Ti1 144.54(12) . . ?
Ti3 O1 Ti2 107.39(10) . . ?
Ti1 O1 Ti2 105.31(10) . . ?
Ti6 O2 Ti4 144.11(14) . . ?
Ti6 O2 Ti5 106.95(12) . . ?
Ti4 O2 Ti5 104.33(11) . . ?
Ti3 O3 Ti4 156.58(13) . . ?
C1 O4 Ti2 128.1(2) . . ?
C1 O5 Ti1 128.3(2) . . ?
C4 O6 Ti4 135.8(2) . . ?
C4 O7 Ti6 135.5(2) . . ?
C5 O8 Ti3 130.8(2) . . ?
C5 O9 Ti1 135.0(2) . . ?
C8 O10 Ti4 129.0(2) . . ?
C8 O11 Ti5 126.7(2) . . ?
C9 O12 Ti2 126.5(2) . . ?
C9 O12 Ti1 131.1(2) . . ?
Ti2 O12 Ti1 102.43(10) . . ?
C12 O13 Ti3 129.2(3) . . ?
C12 O13 Ti2 129.6(3) . . ?
Ti3 O13 Ti2 100.76(10) . . ?
C15 O14 Ti4 131.7(3) . . ?
C15 O14 Ti5 125.5(2) . . ?
Ti4 O14 Ti5 102.75(11) . . ?
C18 O15 Ti6 132.1(3) . . ?
C18 O15 Ti5 126.8(3) . . ?
Ti6 O15 Ti5 100.82(11) . . ?
C21 O16 Ti1 150.8(3) . . ?
C24 O17 Ti1 140.0(2) . . ?
C27 O18 Ti2 139.7(3) . . ?
C30 O19 Ti2 159.1(3) . . ?
C33 O20 Ti3 160.0(5) . . ?
C36 O21 Ti4 149.3(4) . . ?
C39 O22 Ti5 139.7(4) . . ?
C42 O23 Ti5 149.3(4) . . ?
C45 O24 Ti6 159.2(5) . . ?
C48 O25 Ti6 161.1(6) . . ?
O16 Ti1 O17 97.03(11) . . ?
O16 Ti1 O1 169.53(10) . . ?
O17 Ti1 O1 93.42(10) . . ?
O16 Ti1 O12 103.47(11) . . ?
O17 Ti1 O12 97.49(11) . . ?
O1 Ti1 O12 75.74(9) . . ?
O16 Ti1 O9 93.21(10) . . ?
O17 Ti1 O9 94.73(11) . . ?
O1 Ti1 O9 85.21(9) . . ?
O12 Ti1 O9 157.88(9) . . ?
O16 Ti1 O5 85.39(10) . . ?
O17 Ti1 O5 177.10(10) . . ?
O1 Ti1 O5 84.15(9) . . ?
O12 Ti1 O5 83.46(9) . . ?
O9 Ti1 O5 83.51(9) . . ?
O16 Ti1 Ti2 139.70(9) . . ?
O17 Ti1 Ti2 101.00(8) . . ?
O1 Ti1 Ti2 37.36(6) . . ?
O12 Ti1 Ti2 38.76(7) . . ?
O9 Ti1 Ti2 120.55(6) . . ?
O5 Ti1 Ti2 78.02(6) . . ?
O19 Ti2 O18 95.63(12) . . ?
O19 Ti2 O1 167.81(11) . . ?
O18 Ti2 O1 96.55(10) . . ?
O19 Ti2 O13 103.54(12) . . ?
O18 Ti2 O13 96.64(12) . . ?
O1 Ti2 O13 74.47(9) . . ?
O19 Ti2 O12 103.64(12) . . ?
O18 Ti2 O12 95.48(11) . . ?
O1 Ti2 O12 75.76(9) . . ?
O13 Ti2 O12 148.89(10) . . ?
O19 Ti2 O4 83.63(11) . . ?
O18 Ti2 O4 177.95(12) . . ?
O1 Ti2 O4 84.22(9) . . ?
O13 Ti2 O4 85.39(10) . . ?
O12 Ti2 O4 82.86(9) . . ?
O19 Ti2 Ti3 142.06(10) . . ?
O18 Ti2 Ti3 97.13(9) . . ?
O1 Ti2 Ti3 34.98(6) . . ?
O13 Ti2 Ti3 39.52(7) . . ?
O12 Ti2 Ti3 110.48(7) . . ?
O4 Ti2 Ti3 84.59(7) . . ?
O19 Ti2 Ti1 139.38(10) . . ?
O18 Ti2 Ti1 101.77(9) . . ?
O1 Ti2 Ti1 37.33(6) . . ?
O13 Ti2 Ti1 110.42(7) . . ?
O12 Ti2 Ti1 38.81(6) . . ?
O4 Ti2 Ti1 77.69(7) . . ?
Ti3 Ti2 Ti1 71.697(19) . . ?
O20 Ti3 O3 111.11(12) . . ?
O20 Ti3 O1 122.92(12) . . ?
O3 Ti3 O1 125.93(10) . . ?
O20 Ti3 O13 98.48(12) . . ?
O3 Ti3 O13 97.74(10) . . ?
O1 Ti3 O13 77.32(9) . . ?
O20 Ti3 O8 92.46(11) . . ?
O3 Ti3 O8 90.85(10) . . ?
O1 Ti3 O8 85.35(9) . . ?
O13 Ti3 O8 162.57(10) . . ?
O20 Ti3 Ti2 115.48(10) . . ?
O3 Ti3 Ti2 119.06(8) . . ?
O1 Ti3 Ti2 37.63(7) . . ?
O13 Ti3 Ti2 39.72(7) . . ?
O8 Ti3 Ti2 122.98(7) . . ?
O21 Ti4 O3 97.78(11) . . ?
O21 Ti4 O2 93.95(11) . . ?
O3 Ti4 O2 168.25(10) . . ?
O21 Ti4 O14 96.63(12) . . ?
O3 Ti4 O14 101.57(10) . . ?
O2 Ti4 O14 76.40(10) . . ?
O21 Ti4 O6 95.25(12) . . ?
O3 Ti4 O6 92.64(10) . . ?
O2 Ti4 O6 86.82(10) . . ?
O14 Ti4 O6 160.02(11) . . ?
O21 Ti4 O10 176.81(11) . . ?
O3 Ti4 O10 85.23(9) . . ?
O2 Ti4 O10 83.05(10) . . ?
O14 Ti4 O10 83.75(10) . . ?
O6 Ti4 O10 83.52(10) . . ?
O21 Ti4 Ti5 101.16(9) . . ?
O3 Ti4 Ti5 137.41(8) . . ?
O2 Ti4 Ti5 38.10(7) . . ?
O14 Ti4 Ti5 38.73(7) . . ?
O6 Ti4 Ti5 122.81(7) . . ?
O10 Ti4 Ti5 77.15(6) . . ?
O22 Ti5 O23 95.50(15) . . ?
O22 Ti5 O2 97.12(13) . . ?
O23 Ti5 O2 167.04(13) . . ?
O22 Ti5 O14 95.60(13) . . ?
O23 Ti5 O14 106.04(13) . . ?
O2 Ti5 O14 75.65(10) . . ?
O22 Ti5 O15 97.17(14) . . ?
O23 Ti5 O15 101.62(14) . . ?
O2 Ti5 O15 73.89(11) . . ?
O14 Ti5 O15 148.15(11) . . ?
O22 Ti5 O11 176.84(14) . . ?
O23 Ti5 O11 82.31(13) . . ?
O2 Ti5 O11 85.19(10) . . ?
O14 Ti5 O11 82.86(10) . . ?
O15 Ti5 O11 85.53(11) . . ?
O22 Ti5 Ti6 99.63(12) . . ?
O23 Ti5 Ti6 139.23(12) . . ?
O2 Ti5 Ti6 34.75(7) . . ?
O14 Ti5 Ti6 109.82(7) . . ?
O15 Ti5 Ti6 39.15(8) . . ?
O11 Ti5 Ti6 83.50(8) . . ?
O22 Ti5 Ti4 102.45(10) . . ?
O23 Ti5 Ti4 141.02(11) . . ?
O2 Ti5 Ti4 37.57(7) . . ?
O14 Ti5 Ti4 38.52(7) . . ?
O15 Ti5 Ti4 109.96(8) . . ?
O11 Ti5 Ti4 78.07(7) . . ?
Ti6 Ti5 Ti4 71.31(2) . . ?
O25 Ti6 O24 113.9(2) . . ?
O25 Ti6 O2 129.12(17) . . ?
O24 Ti6 O2 116.77(17) . . ?
O25 Ti6 O15 97.05(16) . . ?
O24 Ti6 O15 100.12(15) . . ?
O2 Ti6 O15 78.32(11) . . ?
O25 Ti6 O7 88.13(16) . . ?
O24 Ti6 O7 92.50(14) . . ?
O2 Ti6 O7 85.80(11) . . ?
O15 Ti6 O7 162.95(11) . . ?
O25 Ti6 Ti5 118.80(15) . . ?
O24 Ti6 Ti5 114.73(14) . . ?
O2 Ti6 Ti5 38.30(8) . . ?
O15 Ti6 Ti5 40.03(8) . . ?
O7 Ti6 Ti5 123.74(8) . . ?

_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        24.82
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         0.969
_refine_diff_density_min         -0.406
_refine_diff_density_rms         0.101
