# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1946007'
loop_
_audit_author_name
_audit_author_address
'Qin-Yu Zhu'
;Soochow University
China
;
_audit_update_record             
;
2019-08-08 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C64 H86 N2 O20 Ti4'
_chemical_formula_weight         1394.94

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'
N N 0.0061 0.0033 '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'

_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                   12.740(3)
_cell_length_b                   12.982(3)
_cell_length_c                   13.026(3)
_cell_angle_alpha                64.27(3)
_cell_angle_beta                 79.31(3)
_cell_angle_gamma                78.76(3)
_cell_volume                     1891.1(9)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9004
_cell_measurement_theta_min      1.7
_cell_measurement_theta_max      34.9

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.225
_exptl_crystal_F_000             732
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.472
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8690
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            14406
_diffrn_reflns_av_unetI/netI     0.0722
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         3.198
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_full        25.000
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measured_fraction_theta_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_point_group_measured_fraction_full 0.975
_reflns_number_total             6507
_reflns_number_gt                5076
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0903P)²+1.2039P] 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         6507
_refine_ls_number_parameters     397
_refine_ls_number_restraints     47
_refine_ls_R_factor_all          0.1074
_refine_ls_R_factor_gt           0.0871
_refine_ls_wR_factor_ref         0.2157
_refine_ls_wR_factor_gt          0.2014
_refine_ls_goodness_of_fit_ref   1.119
_refine_ls_restrained_S_all      1.136
_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_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 0.40642(6) -0.04742(6) 1.08801(6) 0.0406(3) Uani 1 1 d . . . . .
Ti2 Ti 0.37492(6) 0.09538(7) 0.82337(7) 0.0456(3) Uani 1 1 d . . . . .
O1 O 0.1201(4) 0.1231(5) 1.2459(5) 0.1090(17) Uani 1 1 d . . . . .
O2 O -0.0098(3) 0.2618(4) 1.1764(4) 0.0764(11) Uani 1 1 d . . . . .
O3 O 0.2704(2) 0.0625(3) 1.0945(3) 0.0502(8) Uani 1 1 d . . . . .
O4 O 0.2391(2) 0.1499(3) 0.9101(3) 0.0543(8) Uani 1 1 d . . . . .
O5 O 0.4469(2) 0.0949(2) 0.9456(2) 0.0381(6) Uani 1 1 d . . . . .
O6 O 0.3475(2) -0.1746(3) 1.1832(3) 0.0519(8) Uani 1 1 d . . . . .
O7 O 0.3560(2) -0.0676(2) 0.9621(2) 0.0441(7) Uani 1 1 d . . . . .
O8 O 0.3020(3) 0.0468(3) 0.7508(3) 0.0560(8) Uani 1 1 d . . . . .
O9 O 0.4706(2) -0.0290(3) 1.2071(2) 0.0463(7) Uani 1 1 d . . . . .
O10 O 0.3821(3) 0.2377(3) 0.7114(3) 0.0660(10) Uani 1 1 d . . . . .
N1 N -0.2899(5) 0.5732(6) 1.0588(9) 0.126(3) Uani 1 1 d . . . . .
C1 C 0.0833(4) 0.1896(6) 1.1607(6) 0.0707(15) Uani 1 1 d . . . . .
C2 C 0.1187(4) 0.2059(4) 1.0419(5) 0.0534(12) Uani 1 1 d . . . . .
C3 C 0.0657(4) 0.2890(5) 0.9563(5) 0.0629(14) Uani 1 1 d . . . . .
H3 H 0.089668 0.298077 0.881328 0.075 Uiso 1 1 calc R U . . .
C4 C -0.0253(4) 0.3630(5) 0.9764(6) 0.0711(16) Uani 1 1 d . . . . .
C5 C -0.0611(4) 0.3468(5) 1.0870(7) 0.0728(17) Uani 1 1 d . . . . .
C6 C -0.1495(5) 0.4116(6) 1.1206(8) 0.091(2) Uani 1 1 d . . . . .
H6 H -0.171582 0.395433 1.197562 0.109 Uiso 1 1 calc R U . . .
C7 C -0.2053(5) 0.5044(6) 1.0314(10) 0.099(3) Uani 1 1 d . . . . .
C8 C -0.1701(5) 0.5217(6) 0.9168(10) 0.104(3) Uani 1 1 d . . . . .
H8 H -0.207039 0.580153 0.858620 0.124 Uiso 1 1 calc R U . . .
C9 C -0.0816(5) 0.4536(5) 0.8882(7) 0.086(2) Uani 1 1 d . . . . .
H9 H -0.059312 0.467203 0.811730 0.103 Uiso 1 1 calc R U . . .
C10 C -0.3487(6) 0.6676(7) 0.9668(11) 0.148(4) Uani 1 1 d . . . . .
H10A H -0.296890 0.706470 0.903252 0.178 Uiso 1 1 calc R U . . .
H10B H -0.387632 0.723438 0.995844 0.178 Uiso 1 1 calc R U . . .
C11 C -0.4288(7) 0.6264(8) 0.9224(13) 0.174(5) Uani 1 1 d . . . . .
H11A H -0.390403 0.574761 0.889227 0.261 Uiso 1 1 calc R U . . .
H11B H -0.465871 0.691700 0.865314 0.261 Uiso 1 1 calc R U . . .
H11C H -0.479998 0.587144 0.984937 0.261 Uiso 1 1 calc R U . . .
C12 C -0.3263(8) 0.5533(10) 1.1761(13) 0.157(5) Uani 1 1 d . . . . .
H12A H -0.367685 0.623423 1.178600 0.188 Uiso 1 1 calc R U . . .
H12B H -0.264125 0.535467 1.216848 0.188 Uiso 1 1 calc R U . . .
C13 C -0.3943(8) 0.4568(11) 1.2363(11) 0.173(5) Uani 1 1 d . . . . .
H13A H -0.467612 0.485628 1.220536 0.259 Uiso 1 1 calc R U . . .
H13B H -0.391074 0.425703 1.317438 0.259 Uiso 1 1 calc R U . . .
H13C H -0.367867 0.397359 1.209364 0.259 Uiso 1 1 calc R U . . .
C14 C 0.2766(4) -0.2471(4) 1.1826(5) 0.0631(13) Uani 1 1 d . U . . .
C15 C 0.2992(7) -0.2537(6) 1.0683(6) 0.105(2) Uani 1 1 d . U . . .
H15A H 0.268336 -0.314672 1.072041 0.126 Uiso 1 1 calc R U . . .
H15B H 0.325229 -0.258645 1.132669 0.126 Uiso 1 1 calc R U . . .
C16 C 0.3064(4) -0.1539(4) 0.9654(4) 0.0546(12) Uani 1 1 d . U . . .
C17 C 0.2688(7) -0.1481(6) 0.8742(6) 0.108(3) Uani 1 1 d . U . . .
H17 H 0.262672 -0.217470 0.872397 0.130 Uiso 1 1 calc R U . . .
C18 C 0.2357(5) -0.0401(6) 0.7746(5) 0.0726(16) Uani 1 1 d . . . . .
C19 C 0.3029(6) -0.3658(5) 1.2780(6) 0.098(2) Uani 1 1 d . . . . .
H19A H 0.376125 -0.396098 1.262702 0.147 Uiso 1 1 calc R U . . .
H19B H 0.255482 -0.416696 1.281498 0.147 Uiso 1 1 calc R U . . .
H19C H 0.293478 -0.359521 1.350022 0.147 Uiso 1 1 calc R U . . .
C20 C 0.1621(5) -0.1974(7) 1.2047(8) 0.121(3) Uani 1 1 d . . . . .
H20A H 0.151012 -0.194885 1.278538 0.182 Uiso 1 1 calc R U . . .
H20B H 0.113829 -0.244982 1.203187 0.182 Uiso 1 1 calc R U . . .
H20C H 0.148280 -0.120835 1.146484 0.182 Uiso 1 1 calc R U . . .
C21 C 0.1192(5) 0.0108(8) 0.8028(8) 0.114(3) Uani 1 1 d . . . . .
H21A H 0.115666 0.026914 0.868737 0.171 Uiso 1 1 calc R U . . .
H21B H 0.070824 -0.043838 0.818692 0.171 Uiso 1 1 calc R U . . .
H21C H 0.099056 0.080768 0.738491 0.171 Uiso 1 1 calc R U . . .
C22 C 0.2428(6) -0.0584(7) 0.6662(6) 0.100(2) Uani 1 1 d . . . . .
H22A H 0.235077 0.015045 0.601823 0.150 Uiso 1 1 calc R U . . .
H22B H 0.186363 -0.101146 0.673093 0.150 Uiso 1 1 calc R U . . .
H22C H 0.311419 -0.100602 0.655014 0.150 Uiso 1 1 calc R U . . .
C23 C 0.4195(6) -0.0226(7) 1.3130(5) 0.093(2) Uani 1 1 d D . . . .
H23 H 0.482173 -0.064277 1.354572 0.112 Uiso 1 1 calc R U . . .
C24 C 0.4240(11) 0.0790(9) 1.3230(9) 0.190(6) Uani 1 1 d D . . . .
H24A H 0.366452 0.088984 1.378327 0.285 Uiso 1 1 calc R U . . .
H24B H 0.416691 0.143211 1.249965 0.285 Uiso 1 1 calc R U . . .
H24C H 0.491817 0.074948 1.347470 0.285 Uiso 1 1 calc R U . . .
C25 C 0.3519(9) -0.1065(9) 1.3845(7) 0.158(4) Uani 1 1 d D . . . .
H25A H 0.297639 -0.075407 1.428893 0.237 Uiso 1 1 calc R U . . .
H25B H 0.393856 -0.173009 1.434996 0.237 Uiso 1 1 calc R U . . .
H25C H 0.318065 -0.128346 1.338180 0.237 Uiso 1 1 calc R U . . .
C26 C 0.3404(8) 0.3076(9) 0.6079(7) 0.131(3) Uani 1 1 d . U . . .
C27 C 0.2258(10) 0.3548(11) 0.6201(10) 0.187(5) Uani 1 1 d . U . . .
H27A H 0.199166 0.388942 0.546653 0.281 Uiso 1 1 calc R U . . .
H27B H 0.218846 0.412346 0.649499 0.281 Uiso 1 1 calc R U . . .
H27C H 0.184972 0.293808 0.672252 0.281 Uiso 1 1 calc R U . . .
C28 C 0.4192(18) 0.3995(17) 0.5408(15) 0.142(7) Uani 0.5 1 d . U P . .
C28' C 0.394(2) 0.315(3) 0.502(2) 0.195(10) Uani 0.5 1 d . U P . .
C29 C 0.2159(3) 0.1341(4) 1.0153(4) 0.0489(11) 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
Ti1 O6 1.786(3) . ?
Ti1 O5 1.883(3) 2_657 ?
Ti1 O9 2.000(3) . ?
Ti1 O7 2.001(3) . ?
Ti1 O3 2.033(3) . ?
Ti1 O5 2.040(3) . ?
Ti1 Ti1 3.0205(19) 2_657 ?
Ti1 Ti2 3.0617(14) 2_657 ?
Ti1 Ti2 3.1868(16) . ?
Ti2 O10 1.796(3) . ?
Ti2 O8 1.796(3) . ?
Ti2 O5 1.977(3) . ?
Ti2 O9 2.029(3) 2_657 ?
Ti2 O4 2.064(3) . ?
Ti2 O7 2.126(3) . ?
O1 C1 1.183(7) . ?
O2 C5 1.373(7) . ?
O2 C1 1.403(6) . ?
O3 C29 1.262(5) . ?
O4 C29 1.279(6) . ?
O6 C14 1.428(6) . ?
O7 C16 1.371(5) . ?
O8 C18 1.433(6) . ?
O9 C23 1.442(6) . ?
O10 C26 1.393(8) . ?
N1 C7 1.358(8) . ?
N1 C12 1.434(14) . ?
N1 C10 1.483(12) . ?
C1 C2 1.462(8) . ?
C2 C3 1.347(7) . ?
C2 C29 1.481(6) . ?
C3 C4 1.417(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.363(9) . ?
C4 C9 1.422(9) . ?
C5 C6 1.391(8) . ?
C6 C7 1.437(11) . ?
C6 H6 0.9300 . ?
C7 C8 1.408(12) . ?
C8 C9 1.391(9) . ?
C8 H8 0.9300 . ?
C9 H9 0.9300 . ?
C10 C11 1.536(11) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C13 1.501(13) . ?
C12 H12A 0.9700 . ?
C12 H12B 0.9700 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 C20 1.506(9) . ?
C14 C15 1.500(9) . ?
C14 C19 1.524(8) . ?
C15 C16 1.406(8) . ?
C15 H15A 0.9300 . ?
C15 H15B 0.9300 . ?
C16 C17 1.328(8) . ?
C17 C18 1.490(9) . ?
C17 H17 0.9300 . ?
C18 C22 1.514(8) . ?
C18 C21 1.549(9) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C24 1.393(9) . ?
C23 C25 1.409(9) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C28' 1.39(3) . ?
C26 C27 1.477(13) . ?
C26 C28 1.56(2) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C28' 1.49(3) . ?

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
O6 Ti1 O5 106.70(14) . 2_657 ?
O6 Ti1 O9 96.35(14) . . ?
O5 Ti1 O9 79.28(12) 2_657 . ?
O6 Ti1 O7 86.10(13) . . ?
O5 Ti1 O7 95.57(12) 2_657 . ?
O9 Ti1 O7 174.74(12) . . ?
O6 Ti1 O3 94.81(14) . . ?
O5 Ti1 O3 158.07(13) 2_657 . ?
O9 Ti1 O3 94.42(13) . . ?
O7 Ti1 O3 90.00(13) . . ?
O6 Ti1 O5 162.49(13) . . ?
O5 Ti1 O5 79.37(13) 2_657 . ?
O9 Ti1 O5 100.96(12) . . ?
O7 Ti1 O5 76.87(11) . . ?
O3 Ti1 O5 81.29(12) . . ?
O6 Ti1 Ti1 145.41(11) . 2_657 ?
O5 Ti1 Ti1 41.59(9) 2_657 2_657 ?
O9 Ti1 Ti1 90.71(9) . 2_657 ?
O7 Ti1 Ti1 84.67(9) . 2_657 ?
O3 Ti1 Ti1 118.42(10) . 2_657 ?
O5 Ti1 Ti1 37.78(8) . 2_657 ?
O6 Ti1 Ti2 101.83(11) . 2_657 ?
O5 Ti1 Ti2 38.61(8) 2_657 2_657 ?
O9 Ti1 Ti2 40.91(9) . 2_657 ?
O7 Ti1 Ti2 134.04(9) . 2_657 ?
O3 Ti1 Ti2 133.28(9) . 2_657 ?
O5 Ti1 Ti2 93.06(9) . 2_657 ?
Ti1 Ti1 Ti2 63.19(4) 2_657 2_657 ?
O6 Ti1 Ti2 125.68(11) . . ?
O5 Ti1 Ti2 92.40(9) 2_657 . ?
O9 Ti1 Ti2 137.56(9) . . ?
O7 Ti1 Ti2 40.89(8) . . ?
O3 Ti1 Ti2 78.02(10) . . ?
O5 Ti1 Ti2 36.82(8) . . ?
Ti1 Ti1 Ti2 59.03(4) 2_657 . ?
Ti2 Ti1 Ti2 122.22(4) 2_657 . ?
O10 Ti2 O8 96.07(16) . . ?
O10 Ti2 O5 104.00(15) . . ?
O8 Ti2 O5 159.87(14) . . ?
O10 Ti2 O9 97.10(15) . 2_657 ?
O8 Ti2 O9 102.86(14) . 2_657 ?
O5 Ti2 O9 76.43(11) . 2_657 ?
O10 Ti2 O4 92.53(16) . . ?
O8 Ti2 O4 94.83(14) . . ?
O5 Ti2 O4 82.91(12) . . ?
O9 Ti2 O4 158.77(13) 2_657 . ?
O10 Ti2 O7 175.62(14) . . ?
O8 Ti2 O7 84.47(13) . . ?
O5 Ti2 O7 75.41(11) . . ?
O9 Ti2 O7 87.00(12) 2_657 . ?
O4 Ti2 O7 83.10(13) . . ?
O10 Ti2 Ti1 100.48(12) . 2_657 ?
O8 Ti2 Ti1 140.87(11) . 2_657 ?
O5 Ti2 Ti1 36.45(8) . 2_657 ?
O9 Ti2 Ti1 40.20(8) 2_657 2_657 ?
O4 Ti2 Ti1 119.36(10) . 2_657 ?
O7 Ti2 Ti1 81.66(9) . 2_657 ?
O10 Ti2 Ti1 140.49(12) . . ?
O8 Ti2 Ti1 121.88(11) . . ?
O5 Ti2 Ti1 38.20(8) . . ?
O9 Ti2 Ti1 85.58(9) 2_657 . ?
O4 Ti2 Ti1 75.06(10) . . ?
O7 Ti2 Ti1 38.04(8) . . ?
Ti1 Ti2 Ti1 57.77(4) 2_657 . ?
C5 O2 C1 123.1(5) . . ?
C29 O3 Ti1 130.0(3) . . ?
C29 O4 Ti2 131.8(3) . . ?
Ti1 O5 Ti2 104.94(13) 2_657 . ?
Ti1 O5 Ti1 100.63(13) 2_657 . ?
Ti2 O5 Ti1 104.97(12) . . ?
C14 O6 Ti1 139.6(3) . . ?
C16 O7 Ti1 130.5(3) . . ?
C16 O7 Ti2 127.7(3) . . ?
Ti1 O7 Ti2 101.07(12) . . ?
C18 O8 Ti2 140.5(3) . . ?
C23 O9 Ti1 129.4(4) . . ?
C23 O9 Ti2 126.4(4) . 2_657 ?
Ti1 O9 Ti2 98.89(12) . 2_657 ?
C26 O10 Ti2 138.9(5) . . ?
C7 N1 C12 121.0(9) . . ?
C7 N1 C10 119.9(10) . . ?
C12 N1 C10 119.1(7) . . ?
O1 C1 O2 115.2(6) . . ?
O1 C1 C2 129.7(5) . . ?
O2 C1 C2 115.1(6) . . ?
C3 C2 C1 120.2(5) . . ?
C3 C2 C29 119.9(5) . . ?
C1 C2 C29 119.8(5) . . ?
C2 C3 C4 122.4(6) . . ?
C2 C3 H3 118.8 . . ?
C4 C3 H3 118.8 . . ?
C5 C4 C3 118.1(6) . . ?
C5 C4 C9 117.9(6) . . ?
C3 C4 C9 124.0(7) . . ?
C4 C5 O2 120.9(5) . . ?
C4 C5 C6 124.9(7) . . ?
O2 C5 C6 114.2(7) . . ?
C5 C6 C7 117.3(7) . . ?
C5 C6 H6 121.3 . . ?
C7 C6 H6 121.3 . . ?
N1 C7 C8 121.6(9) . . ?
N1 C7 C6 120.0(9) . . ?
C8 C7 C6 118.5(6) . . ?
C9 C8 C7 121.7(8) . . ?
C9 C8 H8 119.1 . . ?
C7 C8 H8 119.1 . . ?
C8 C9 C4 119.6(8) . . ?
C8 C9 H9 120.2 . . ?
C4 C9 H9 120.2 . . ?
N1 C10 C11 113.6(6) . . ?
N1 C10 H10A 108.8 . . ?
C11 C10 H10A 108.8 . . ?
N1 C10 H10B 108.8 . . ?
C11 C10 H10B 108.8 . . ?
H10A C10 H10B 107.7 . . ?
C10 C11 H11A 109.5 . . ?
C10 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C10 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C13 113.2(8) . . ?
N1 C12 H12A 108.9 . . ?
C13 C12 H12A 108.9 . . ?
N1 C12 H12B 108.9 . . ?
C13 C12 H12B 108.9 . . ?
H12A C12 H12B 107.7 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
O6 C14 C20 108.9(5) . . ?
O6 C14 C15 107.7(4) . . ?
C20 C14 C15 112.2(6) . . ?
O6 C14 C19 107.0(5) . . ?
C20 C14 C19 110.6(6) . . ?
C15 C14 C19 110.2(5) . . ?
C16 C15 C14 121.4(5) . . ?
C16 C15 H15A 120.0 . . ?
C14 C15 H15A 109.5 . . ?
C16 C15 H15B 120.0 . . ?
C14 C15 H15B 31.2 . . ?
H15A C15 H15B 120.0 . . ?
C17 C16 C15 119.3(5) . . ?
C17 C16 O7 122.4(5) . . ?
C15 C16 O7 118.3(5) . . ?
C16 C17 C18 125.7(6) . . ?
C16 C17 H17 117.1 . . ?
C18 C17 H17 117.1 . . ?
O8 C18 C22 107.7(5) . . ?
O8 C18 C17 110.9(4) . . ?
C22 C18 C17 112.7(6) . . ?
O8 C18 C21 105.8(5) . . ?
C22 C18 C21 109.4(5) . . ?
C17 C18 C21 110.2(6) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C23 C25 125.4(7) . . ?
C24 C23 O9 116.0(6) . . ?
C25 C23 O9 117.1(6) . . ?
C24 C23 H23 94.0 . . ?
C25 C23 H23 94.0 . . ?
O9 C23 H23 94.0 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28' C26 O10 123.2(13) . . ?
C28' C26 C27 121.3(14) . . ?
O10 C26 C27 114.4(8) . . ?
C28' C26 C28 60.7(15) . . ?
O10 C26 C28 105.3(10) . . ?
C27 C26 C28 115.1(12) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28' C28 C26 53.9(13) . . ?
C26 C28' C28 65.4(16) . . ?
O3 C29 O4 123.9(4) . . ?
O3 C29 C2 119.9(4) . . ?
O4 C29 C2 116.2(4) . . ?

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
O5 Ti1 O6 C14 -107.3(5) 2_657 . . . ?
O9 Ti1 O6 C14 172.0(5) . . . . ?
O7 Ti1 O6 C14 -12.7(5) . . . . ?
O3 Ti1 O6 C14 77.0(5) . . . . ?
O5 Ti1 O6 C14 0.8(8) . . . . ?
Ti1 Ti1 O6 C14 -87.4(5) 2_657 . . . ?
Ti2 Ti1 O6 C14 -146.9(5) 2_657 . . . ?
Ti2 Ti1 O6 C14 -1.7(5) . . . . ?
O10 Ti2 O8 C18 -160.1(5) . . . . ?
O5 Ti2 O8 C18 15.5(8) . . . . ?
O9 Ti2 O8 C18 101.2(5) 2_657 . . . ?
O4 Ti2 O8 C18 -67.0(5) . . . . ?
O7 Ti2 O8 C18 15.5(5) . . . . ?
Ti1 Ti2 O8 C18 85.0(6) 2_657 . . . ?
Ti1 Ti2 O8 C18 8.4(6) . . . . ?
O8 Ti2 O10 C26 8.4(7) . . . . ?
O5 Ti2 O10 C26 -170.1(7) . . . . ?
O9 Ti2 O10 C26 112.2(7) 2_657 . . . ?
O4 Ti2 O10 C26 -86.7(7) . . . . ?
Ti1 Ti2 O10 C26 152.8(7) 2_657 . . . ?
Ti1 Ti2 O10 C26 -156.1(7) . . . . ?
C5 O2 C1 O1 177.6(6) . . . . ?
C5 O2 C1 C2 -3.9(7) . . . . ?
O1 C1 C2 C3 -178.9(7) . . . . ?
O2 C1 C2 C3 2.8(7) . . . . ?
O1 C1 C2 C29 -1.5(10) . . . . ?
O2 C1 C2 C29 -179.8(4) . . . . ?
C1 C2 C3 C4 -0.2(7) . . . . ?
C29 C2 C3 C4 -177.6(4) . . . . ?
C2 C3 C4 C5 -1.6(8) . . . . ?
C2 C3 C4 C9 178.3(5) . . . . ?
C3 C4 C5 O2 0.6(8) . . . . ?
C9 C4 C5 O2 -179.3(4) . . . . ?
C3 C4 C5 C6 -179.4(5) . . . . ?
C9 C4 C5 C6 0.6(8) . . . . ?
C1 O2 C5 C4 2.3(8) . . . . ?
C1 O2 C5 C6 -177.7(5) . . . . ?
C4 C5 C6 C7 -1.7(8) . . . . ?
O2 C5 C6 C7 178.2(5) . . . . ?
C12 N1 C7 C8 178.8(7) . . . . ?
C10 N1 C7 C8 1.3(9) . . . . ?
C12 N1 C7 C6 -1.4(10) . . . . ?
C10 N1 C7 C6 -178.9(5) . . . . ?
C5 C6 C7 N1 -177.6(5) . . . . ?
C5 C6 C7 C8 2.2(8) . . . . ?
N1 C7 C8 C9 178.0(5) . . . . ?
C6 C7 C8 C9 -1.8(9) . . . . ?
C7 C8 C9 C4 0.7(9) . . . . ?
C5 C4 C9 C8 -0.1(8) . . . . ?
C3 C4 C9 C8 180.0(5) . . . . ?
C7 N1 C10 C11 78.7(10) . . . . ?
C12 N1 C10 C11 -98.9(10) . . . . ?
C7 N1 C12 C13 -78.8(10) . . . . ?
C10 N1 C12 C13 98.7(9) . . . . ?
Ti1 O6 C14 C20 -85.3(6) . . . . ?
Ti1 O6 C14 C15 36.6(7) . . . . ?
Ti1 O6 C14 C19 155.1(4) . . . . ?
O6 C14 C15 C16 -48.3(8) . . . . ?
C20 C14 C15 C16 71.6(8) . . . . ?
C19 C14 C15 C16 -164.7(6) . . . . ?
C14 C15 C16 C17 -143.6(7) . . . . ?
C14 C15 C16 O7 38.8(9) . . . . ?
Ti1 O7 C16 C17 173.4(5) . . . . ?
Ti2 O7 C16 C17 5.0(7) . . . . ?
Ti1 O7 C16 C15 -9.1(7) . . . . ?
Ti2 O7 C16 C15 -177.5(4) . . . . ?
C15 C16 C17 C18 157.9(7) . . . . ?
O7 C16 C17 C18 -24.6(11) . . . . ?
Ti2 O8 C18 C22 -155.8(4) . . . . ?
Ti2 O8 C18 C17 -32.1(8) . . . . ?
Ti2 O8 C18 C21 87.3(6) . . . . ?
C16 C17 C18 O8 34.4(10) . . . . ?
C16 C17 C18 C22 155.2(7) . . . . ?
C16 C17 C18 C21 -82.4(9) . . . . ?
Ti1 O9 C23 C24 -119.0(9) . . . . ?
Ti2 O9 C23 C24 92.2(10) 2_657 . . . ?
Ti1 O9 C23 C25 48.0(10) . . . . ?
Ti2 O9 C23 C25 -100.8(8) 2_657 . . . ?
Ti2 O10 C26 C28' -94(2) . . . . ?
Ti2 O10 C26 C27 74.1(12) . . . . ?
Ti2 O10 C26 C28 -158.6(10) . . . . ?
O10 C26 C28 C28' 119.9(15) . . . . ?
C27 C26 C28 C28' -113.2(16) . . . . ?
O10 C26 C28' C28 -89.6(17) . . . . ?
C27 C26 C28' C28 103.2(18) . . . . ?
Ti1 O3 C29 O4 0.2(6) . . . . ?
Ti1 O3 C29 C2 -179.7(3) . . . . ?
Ti2 O4 C29 O3 -11.7(7) . . . . ?
Ti2 O4 C29 C2 168.3(3) . . . . ?
C3 C2 C29 O3 174.4(4) . . . . ?
C1 C2 C29 O3 -3.0(7) . . . . ?
C3 C2 C29 O4 -5.5(6) . . . . ?
C1 C2 C29 O4 177.1(4) . . . . ?

_refine_diff_density_max         0.342
_refine_diff_density_min         -0.268
_refine_diff_density_rms         0.064



####################################################################### 
# 
# 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_2
_database_code_depnum_ccdc_archive 'CCDC 1946008'
loop_
_audit_author_name
_audit_author_address
'Qin-Yu Zhu'
;Soochow University
China
;
_audit_update_record             
;
2019-08-08 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C78 H100 N2 O18 Ti4'
_chemical_formula_weight         1545.19

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'
N N 0.0061 0.0033 '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'

_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                   11.383(2)
_cell_length_b                   12.183(2)
_cell_length_c                   14.906(3)
_cell_angle_alpha                90.01(3)
_cell_angle_beta                 98.41(3)
_cell_angle_gamma                95.11(3)
_cell_volume                     2036.5(7)
_cell_formula_units_Z            1
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    8966
_cell_measurement_theta_min      2.2
_cell_measurement_theta_max      34.9

_exptl_crystal_description       Prism
_exptl_crystal_colour            Yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_F_000             814
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.443
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.957
_exptl_absorpt_correction_type   Multi-scan
_exptl_absorpt_correction_T_min  0.8438
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            15793
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_av_R_equivalents  0.0294
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.678
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             7121
_reflns_number_gt                6306
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.1022P)²+1.9242P] 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         7121
_refine_ls_number_parameters     470
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0726
_refine_ls_R_factor_gt           0.0613
_refine_ls_wR_factor_ref         0.1868
_refine_ls_wR_factor_gt          0.1686
_refine_ls_goodness_of_fit_ref   1.108
_refine_ls_restrained_S_all      1.108
_refine_ls_shift/su_max          0.009
_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 0.61644(5) 0.20245(4) 1.04512(4) 0.02225(18) Uani 1 1 d . . . . .
Ti2 Ti 0.55233(5) -0.03738(5) 1.09294(4) 0.02372(18) Uani 1 1 d . . . . .
O1 O 0.4889(2) 0.29961(18) 0.98150(16) 0.0277(5) Uani 1 1 d . . . . .
O2 O 0.48255(19) 0.08600(17) 1.04020(14) 0.0219(5) Uani 1 1 d . . . . .
O3 O 0.6416(2) -0.17618(18) 1.10242(16) 0.0297(5) Uani 1 1 d . . . . .
O4 O 0.60101(19) 0.13304(18) 0.91324(15) 0.0244(5) Uani 1 1 d . . . . .
O5 O 0.7443(2) 0.28505(18) 1.01560(16) 0.0268(5) Uani 1 1 d . . . . .
O6 O 0.6088(2) 0.26443(18) 1.15258(15) 0.0274(5) Uani 1 1 d . . . . .
O7 O 0.69790(19) 0.06634(17) 1.08976(15) 0.0243(5) Uani 1 1 d . . . . .
O8 O 0.5509(2) -0.0295(2) 1.21307(16) 0.0338(6) Uani 1 1 d . . . . .
O9 O -0.1222(6) 0.1492(6) 0.6212(4) 0.155(3) Uani 1 1 d . . . . .
N1 N -0.1167(3) 0.6323(3) 0.6809(2) 0.0399(8) Uani 1 1 d . . . . .
C1 C -0.0327(3) 0.5606(3) 0.7186(2) 0.0325(8) Uani 1 1 d . . . . .
C2 C 0.0720(3) 0.6021(3) 0.7737(3) 0.0341(8) Uani 1 1 d . . . . .
H2 H 0.086449 0.677669 0.784027 0.041 Uiso 1 1 calc R U . . .
C3 C 0.1541(3) 0.5333(3) 0.8131(2) 0.0307(8) Uani 1 1 d . . . . .
H3 H 0.222234 0.562935 0.850389 0.037 Uiso 1 1 calc R U . . .
C4 C 0.1360(3) 0.4194(3) 0.7974(2) 0.0273(7) Uani 1 1 d . . . . .
C5 C 0.0323(3) 0.3791(3) 0.7411(2) 0.0310(8) Uani 1 1 d . . . . .
H5 H 0.019049 0.303684 0.729241 0.037 Uiso 1 1 calc R U . . .
C6 C -0.0511(3) 0.4469(3) 0.7025(2) 0.0331(8) Uani 1 1 d . . . . .
H6 H -0.119574 0.417057 0.665754 0.040 Uiso 1 1 calc R U . . .
C7 C -0.1444(3) 0.7211(3) 0.7361(3) 0.0332(8) Uani 1 1 d . . . . .
C8 C -0.1543(4) 0.8255(3) 0.6995(3) 0.0466(10) Uani 1 1 d . . . . .
H8 H -0.139275 0.839201 0.640678 0.056 Uiso 1 1 calc R U . . .
C9 C -0.1866(4) 0.9085(3) 0.7514(3) 0.0526(12) Uani 1 1 d . . . . .
H9 H -0.192857 0.978368 0.727110 0.063 Uiso 1 1 calc R U . . .
C10 C -0.2097(4) 0.8897(4) 0.8381(3) 0.0527(12) Uani 1 1 d . . . . .
H10 H -0.233451 0.945971 0.871614 0.063 Uiso 1 1 calc R U . . .
C11 C -0.1974(4) 0.7867(3) 0.8756(3) 0.0469(10) Uani 1 1 d . . . . .
H11 H -0.211207 0.773761 0.934863 0.056 Uiso 1 1 calc R U . . .
C12 C -0.1643(4) 0.7026(3) 0.8238(3) 0.0395(9) Uani 1 1 d . . . . .
H12 H -0.155582 0.633355 0.848842 0.047 Uiso 1 1 calc R U . . .
C13 C -0.1884(3) 0.6090(3) 0.5953(2) 0.0312(8) Uani 1 1 d . . . . .
C14 C -0.1398(4) 0.5665(3) 0.5246(3) 0.0391(9) Uani 1 1 d . . . . .
H14 H -0.059903 0.552741 0.532966 0.047 Uiso 1 1 calc R U . . .
C15 C -0.2095(4) 0.5441(3) 0.4412(3) 0.0469(10) Uani 1 1 d . . . . .
H15 H -0.176219 0.514916 0.394146 0.056 Uiso 1 1 calc R U . . .
C16 C -0.3266(4) 0.5647(3) 0.4277(3) 0.0500(11) Uani 1 1 d . . . . .
H16 H -0.372900 0.549854 0.371529 0.060 Uiso 1 1 calc R U . . .
C17 C -0.3759(4) 0.6074(4) 0.4977(3) 0.0500(11) Uani 1 1 d . . . . .
H17 H -0.455556 0.622167 0.488423 0.060 Uiso 1 1 calc R U . . .
C18 C -0.3078(3) 0.6286(3) 0.5816(3) 0.0416(9) Uani 1 1 d . . . . .
H18 H -0.342108 0.656024 0.628860 0.050 Uiso 1 1 calc R U . . .
C19 C 0.2189(3) 0.3424(3) 0.8368(2) 0.0286(7) Uani 1 1 d . . . . .
H19 H 0.201614 0.269623 0.816834 0.034 Uiso 1 1 calc R U . . .
C20 C 0.3170(3) 0.3626(3) 0.8980(2) 0.0292(7) Uani 1 1 d . . . . .
C21 C 0.3925(3) 0.2731(3) 0.9280(2) 0.0278(7) Uani 1 1 d . . . . .
C22 C 0.6674(3) 0.1614(3) 0.8454(2) 0.0261(7) Uani 1 1 d . . . . .
C23 C 0.7844(5) 0.2163(4) 0.8733(3) 0.0689(17) Uani 1 1 d . . . . .
H23A H 0.814329 0.242202 0.818688 0.083 Uiso 1 1 calc R U . . .
H23B H 0.834935 0.160559 0.898575 0.083 Uiso 1 1 calc R U . . .
C24 C 0.8046(3) 0.3111(3) 0.9393(3) 0.0339(8) Uani 1 1 d . . . . .
C25 C 0.6288(4) 0.1302(4) 0.7579(3) 0.0528(12) Uani 1 1 d . . . . .
H25 H 0.685283 0.133614 0.718520 0.063 Uiso 1 1 calc R U . . .
C26 C 0.7539(7) 0.4110(5) 0.8959(4) 0.098(3) Uani 1 1 d . . . . .
H26A H 0.668848 0.397442 0.881782 0.146 Uiso 1 1 calc R U . . .
H26B H 0.787022 0.426694 0.841095 0.146 Uiso 1 1 calc R U . . .
H26C H 0.773545 0.472881 0.936872 0.146 Uiso 1 1 calc R U . . .
C27 C 0.9352(4) 0.3336(6) 0.9739(4) 0.086(2) Uani 1 1 d . . . . .
H27A H 0.945719 0.382872 1.025306 0.128 Uiso 1 1 calc R U . . .
H27B H 0.975191 0.366760 0.926916 0.128 Uiso 1 1 calc R U . . .
H27C H 0.968104 0.265689 0.991596 0.128 Uiso 1 1 calc R U . . .
C28 C 0.5328(3) 0.2869(3) 1.2171(2) 0.0333(8) Uani 1 1 d . . . . .
H28 H 0.463756 0.231895 1.209905 0.040 Uiso 1 1 calc R U . . .
C29 C 0.4902(4) 0.4003(4) 1.1989(3) 0.0467(10) Uani 1 1 d . . . . .
H29A H 0.557323 0.454759 1.207998 0.070 Uiso 1 1 calc R U . . .
H29B H 0.435429 0.414786 1.239723 0.070 Uiso 1 1 calc R U . . .
H29C H 0.451021 0.403033 1.137495 0.070 Uiso 1 1 calc R U . . .
C30 C 0.6021(4) 0.2782(4) 1.3107(3) 0.0446(10) Uani 1 1 d . . . . .
H30A H 0.627250 0.205202 1.318777 0.067 Uiso 1 1 calc R U . . .
H30B H 0.552424 0.292820 1.355244 0.067 Uiso 1 1 calc R U . . .
H30C H 0.670838 0.330866 1.317554 0.067 Uiso 1 1 calc R U . . .
C31 C 0.8212(3) 0.0689(3) 1.1316(2) 0.0283(7) Uani 1 1 d . . . . .
H31 H 0.859777 0.142680 1.123658 0.034 Uiso 1 1 calc R U . . .
C32 C 0.8843(4) -0.0132(4) 1.0846(3) 0.0487(11) Uani 1 1 d . . . . .
H32A H 0.847441 -0.086116 1.091305 0.073 Uiso 1 1 calc R U . . .
H32B H 0.966586 -0.009394 1.111288 0.073 Uiso 1 1 calc R U . . .
H32C H 0.878887 0.003883 1.021339 0.073 Uiso 1 1 calc R U . . .
C33 C 0.8296(4) 0.0478(5) 1.2314(3) 0.0557(12) Uani 1 1 d . . . . .
H33A H 0.789478 0.101730 1.259146 0.084 Uiso 1 1 calc R U . . .
H33B H 0.911969 0.052592 1.258116 0.084 Uiso 1 1 calc R U . . .
H33C H 0.792899 -0.024543 1.240670 0.084 Uiso 1 1 calc R U . . .
C34 C 0.4968(3) -0.0906(3) 1.2808(2) 0.0338(8) Uani 1 1 d . . . . .
C35 C 0.4945(6) -0.0132(5) 1.3611(3) 0.082(2) Uani 1 1 d . . . . .
H35A H 0.574630 0.007928 1.389368 0.122 Uiso 1 1 calc R U . . .
H35B H 0.450576 -0.050123 1.404283 0.122 Uiso 1 1 calc R U . . .
H35C H 0.456841 0.051399 1.339999 0.122 Uiso 1 1 calc R U . . .
C36 C 0.5687(5) -0.1861(5) 1.3095(4) 0.082(2) Uani 1 1 d . . . . .
H36A H 0.568546 -0.233790 1.258196 0.123 Uiso 1 1 calc R U . . .
H36B H 0.534149 -0.226431 1.355948 0.123 Uiso 1 1 calc R U . . .
H36C H 0.649181 -0.158773 1.332511 0.123 Uiso 1 1 calc R U . . .
C37 C -0.1247(9) 0.2097(8) 0.4732(6) 0.137(3) Uani 1 1 d . . . . .
H37A H -0.139731 0.153504 0.426716 0.205 Uiso 1 1 calc R U . . .
H37B H -0.072008 0.268803 0.455072 0.205 Uiso 1 1 calc R U . . .
H37C H -0.198559 0.237295 0.482185 0.205 Uiso 1 1 calc R U . . .
C38 C -0.0710(9) 0.1644(7) 0.5555(5) 0.106(3) Uani 1 1 d . . . . .
C39 C 0.0605(9) 0.1461(7) 0.5626(6) 0.129(3) Uani 1 1 d . . . . .
H39A H 0.088854 0.122096 0.622581 0.193 Uiso 1 1 calc R U . . .
H39B H 0.105065 0.213727 0.550460 0.193 Uiso 1 1 calc R U . . .
H39C H 0.070673 0.090745 0.519161 0.193 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 O6 1.788(2) . ?
Ti1 O5 1.803(2) . ?
Ti1 O2 1.981(2) . ?
Ti1 O7 2.036(2) . ?
Ti1 O1 2.076(2) . ?
Ti1 O4 2.117(2) . ?
Ti1 Ti2 3.1818(14) 2_657 ?
Ti2 O8 1.796(2) . ?
Ti2 O2 1.881(2) . ?
Ti2 O4 2.001(2) 2_657 ?
Ti2 O7 1.999(2) . ?
Ti2 O2 2.043(2) 2_657 ?
Ti2 O3 2.043(2) . ?
Ti2 Ti2 3.0258(14) 2_657 ?
O1 C21 1.274(4) . ?
O3 C21 1.272(4) 2_657 ?
O4 C22 1.375(4) . ?
O5 C24 1.434(4) . ?
O6 C28 1.426(4) . ?
O7 C31 1.447(4) . ?
O8 C34 1.434(4) . ?
O9 C38 1.217(9) . ?
N1 C1 1.409(4) . ?
N1 C13 1.423(5) . ?
N1 C7 1.443(5) . ?
C1 C2 1.398(5) . ?
C1 C6 1.398(5) . ?
C2 C3 1.378(5) . ?
C3 C4 1.399(5) . ?
C4 C5 1.395(5) . ?
C4 C19 1.453(5) . ?
C5 C6 1.376(5) . ?
C7 C8 1.390(5) . ?
C7 C12 1.375(5) . ?
C8 C9 1.380(6) . ?
C9 C10 1.372(7) . ?
C10 C11 1.383(6) . ?
C11 C12 1.394(5) . ?
C13 C14 1.380(5) . ?
C13 C18 1.387(5) . ?
C14 C15 1.386(6) . ?
C15 C16 1.364(6) . ?
C16 C17 1.378(6) . ?
C17 C18 1.383(6) . ?
C19 C20 1.339(5) . ?
C20 C21 1.477(5) . ?
C22 C25 1.357(5) . ?
C22 C23 1.440(6) . ?
C23 C24 1.496(5) . ?
C24 C26 1.500(6) . ?
C24 C27 1.501(6) . ?
C25 C34 1.498(6) 2_657 ?
C28 C29 1.515(5) . ?
C28 C30 1.508(5) . ?
C31 C33 1.499(5) . ?
C31 C32 1.510(5) . ?
C34 C35 1.528(6) . ?
C34 C36 1.507(6) . ?
C37 C38 1.422(10) . ?
C38 C39 1.522(12) . ?

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
O6 Ti1 O5 99.07(11) . . ?
O6 Ti1 O2 99.90(10) . . ?
O5 Ti1 O2 160.95(10) . . ?
O6 Ti1 O7 98.70(10) . . ?
O5 Ti1 O7 98.82(10) . . ?
O2 Ti1 O7 76.50(9) . . ?
O6 Ti1 O1 91.00(10) . . ?
O5 Ti1 O1 96.42(10) . . ?
O2 Ti1 O1 85.08(9) . . ?
O7 Ti1 O1 160.38(9) . . ?
O6 Ti1 O4 172.27(10) . . ?
O5 Ti1 O4 85.62(10) . . ?
O2 Ti1 O4 75.73(9) . . ?
O7 Ti1 O4 86.56(9) . . ?
O1 Ti1 O4 82.34(9) . . ?
O6 Ti1 Ti2 136.27(8) . 2_657 ?
O5 Ti1 Ti2 123.50(8) . 2_657 ?
O2 Ti1 Ti2 38.44(7) . 2_657 ?
O7 Ti1 Ti2 85.29(7) . 2_657 ?
O1 Ti1 Ti2 75.99(7) . 2_657 ?
O4 Ti1 Ti2 38.10(6) . 2_657 ?
O8 Ti2 O2 107.85(11) . . ?
O8 Ti2 O4 86.48(11) . 2_657 ?
O2 Ti2 O4 95.38(10) . 2_657 ?
O8 Ti2 O7 96.98(11) . . ?
O2 Ti2 O7 79.68(9) . . ?
O4 Ti2 O7 174.64(9) 2_657 . ?
O8 Ti2 O2 162.68(10) . 2_657 ?
O2 Ti2 O2 79.19(10) . 2_657 ?
O4 Ti2 O2 76.98(9) 2_657 2_657 ?
O7 Ti2 O2 99.89(9) . 2_657 ?
O8 Ti2 O3 93.17(11) . . ?
O2 Ti2 O3 158.74(10) . . ?
O4 Ti2 O3 88.93(10) 2_657 . ?
O7 Ti2 O3 94.94(9) . . ?
O2 Ti2 O3 81.54(9) 2_657 . ?
O8 Ti2 Ti2 146.64(9) . 2_657 ?
O2 Ti2 Ti2 41.55(7) . 2_657 ?
O4 Ti2 Ti2 84.62(7) 2_657 2_657 ?
O7 Ti2 Ti2 90.27(7) . 2_657 ?
O2 Ti2 Ti2 37.64(6) 2_657 2_657 ?
O3 Ti2 Ti2 118.69(8) . 2_657 ?
O8 Ti2 Ti1 125.73(8) . 2_657 ?
O2 Ti2 Ti1 92.14(7) . 2_657 ?
O4 Ti2 Ti1 40.75(7) 2_657 2_657 ?
O7 Ti2 Ti1 136.70(7) . 2_657 ?
O2 Ti2 Ti1 37.06(6) 2_657 2_657 ?
O3 Ti2 Ti1 77.60(7) . 2_657 ?
Ti2 Ti2 Ti1 58.96(3) 2_657 2_657 ?
C21 O1 Ti1 130.5(2) . . ?
Ti2 O2 Ti1 104.69(10) . . ?
Ti2 O2 Ti2 100.81(10) . 2_657 ?
Ti1 O2 Ti2 104.50(10) . 2_657 ?
C21 O3 Ti2 129.7(2) 2_657 . ?
C22 O4 Ti2 129.4(2) . 2_657 ?
C22 O4 Ti1 128.62(19) . . ?
Ti2 O4 Ti1 101.15(10) 2_657 . ?
C24 O5 Ti1 140.8(2) . . ?
C28 O6 Ti1 145.3(2) . . ?
C31 O7 Ti2 134.6(2) . . ?
C31 O7 Ti1 124.01(19) . . ?
Ti2 O7 Ti1 98.55(10) . . ?
C34 O8 Ti2 138.0(2) . . ?
C1 N1 C13 121.3(3) . . ?
C1 N1 C7 119.1(3) . . ?
C13 N1 C7 118.8(3) . . ?
C2 C1 N1 120.4(3) . . ?
C2 C1 C6 118.1(3) . . ?
N1 C1 C6 121.5(3) . . ?
C3 C2 C1 121.5(3) . . ?
C2 C3 C4 120.6(3) . . ?
C3 C4 C5 117.5(3) . . ?
C3 C4 C19 123.4(3) . . ?
C5 C4 C19 119.1(3) . . ?
C6 C5 C4 122.3(3) . . ?
C5 C6 C1 120.0(3) . . ?
C8 C7 C12 119.7(4) . . ?
C8 C7 N1 119.8(4) . . ?
C12 C7 N1 120.5(3) . . ?
C7 C8 C9 119.3(4) . . ?
C10 C9 C8 121.2(4) . . ?
C9 C10 C11 119.8(4) . . ?
C10 C11 C12 119.4(4) . . ?
C7 C12 C11 120.6(4) . . ?
C14 C13 C18 118.9(3) . . ?
C14 C13 N1 120.4(3) . . ?
C18 C13 N1 120.7(3) . . ?
C13 C14 C15 120.4(4) . . ?
C16 C15 C14 120.5(4) . . ?
C15 C16 C17 119.6(4) . . ?
C18 C17 C16 120.4(4) . . ?
C13 C18 C17 120.1(4) . . ?
C20 C19 C4 128.5(3) . . ?
C19 C20 C21 120.5(3) . . ?
O1 C21 O3 124.7(3) . 2_657 ?
O1 C21 C20 117.1(3) . . ?
O3 C21 C20 118.1(3) 2_657 . ?
C25 C22 O4 121.5(3) . . ?
C25 C22 C23 121.8(3) . . ?
O4 C22 C23 116.4(3) . . ?
C22 C23 C24 121.7(4) . . ?
O5 C24 C23 110.0(3) . . ?
O5 C24 C26 107.2(3) . . ?
C23 C24 C26 110.2(5) . . ?
O5 C24 C27 107.8(3) . . ?
C23 C24 C27 110.2(4) . . ?
C26 C24 C27 111.3(5) . . ?
C22 C25 C34 125.7(4) . 2_657 ?
O6 C28 C29 108.6(3) . . ?
O6 C28 C30 108.1(3) . . ?
C29 C28 C30 112.6(3) . . ?
O7 C31 C33 110.9(3) . . ?
O7 C31 C32 109.8(3) . . ?
C33 C31 C32 111.7(4) . . ?
O8 C34 C25 108.9(3) . 2_657 ?
O8 C34 C35 108.2(3) . . ?
C25 C34 C35 108.9(4) 2_657 . ?
O8 C34 C36 108.9(3) . . ?
C25 C34 C36 111.0(4) 2_657 . ?
C35 C34 C36 110.9(4) . . ?
O9 C38 C37 123.2(10) . . ?
O9 C38 C39 119.7(8) . . ?
C37 C38 C39 116.8(8) . . ?

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
O8 Ti2 O2 Ti1 88.08(13) . . . . ?
O4 Ti2 O2 Ti1 176.10(10) 2_657 . . . ?
O7 Ti2 O2 Ti1 -6.00(9) . . . . ?
O2 Ti2 O2 Ti1 -108.28(13) 2_657 . . . ?
O3 Ti2 O2 Ti1 -82.9(3) . . . . ?
Ti2 Ti2 O2 Ti1 -108.27(13) 2_657 . . . ?
Ti1 Ti2 O2 Ti1 -143.18(8) 2_657 . . . ?
O8 Ti2 O2 Ti2 -163.65(10) . . . 2_657 ?
O4 Ti2 O2 Ti2 -75.62(10) 2_657 . . 2_657 ?
O7 Ti2 O2 Ti2 102.27(11) . . . 2_657 ?
O2 Ti2 O2 Ti2 0.0 2_657 . . 2_657 ?
O3 Ti2 O2 Ti2 25.3(3) . . . 2_657 ?
Ti1 Ti2 O2 Ti2 -34.90(8) 2_657 . . 2_657 ?
O6 Ti1 O5 C24 -165.4(3) . . . . ?
O2 Ti1 O5 C24 20.2(5) . . . . ?
O7 Ti1 O5 C24 94.3(3) . . . . ?
O1 Ti1 O5 C24 -73.3(4) . . . . ?
O4 Ti1 O5 C24 8.4(3) . . . . ?
Ti2 Ti1 O5 C24 4.1(4) 2_657 . . . ?
O5 Ti1 O6 C28 153.4(4) . . . . ?
O2 Ti1 O6 C28 -28.4(4) . . . . ?
O7 Ti1 O6 C28 -106.1(4) . . . . ?
O1 Ti1 O6 C28 56.8(4) . . . . ?
Ti2 Ti1 O6 C28 -13.8(4) 2_657 . . . ?
O2 Ti2 O8 C34 115.3(3) . . . . ?
O4 Ti2 O8 C34 20.8(3) 2_657 . . . ?
O7 Ti2 O8 C34 -163.3(3) . . . . ?
O2 Ti2 O8 C34 3.5(6) 2_657 . . . ?
O3 Ti2 O8 C34 -68.0(4) . . . . ?
Ti2 Ti2 O8 C34 95.4(4) 2_657 . . . ?
Ti1 Ti2 O8 C34 9.0(4) 2_657 . . . ?
C13 N1 C1 C2 148.6(4) . . . . ?
C7 N1 C1 C2 -41.6(5) . . . . ?
C13 N1 C1 C6 -31.5(6) . . . . ?
C7 N1 C1 C6 138.3(4) . . . . ?
N1 C1 C2 C3 178.5(3) . . . . ?
C6 C1 C2 C3 -1.4(6) . . . . ?
C1 C2 C3 C4 1.3(6) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
C2 C3 C4 C19 -180.0(3) . . . . ?
C3 C4 C5 C6 -0.8(5) . . . . ?
C19 C4 C5 C6 179.0(3) . . . . ?
C4 C5 C6 C1 0.6(6) . . . . ?
C2 C1 C6 C5 0.5(6) . . . . ?
N1 C1 C6 C5 -179.4(3) . . . . ?
C1 N1 C7 C8 136.8(4) . . . . ?
C13 N1 C7 C8 -53.1(5) . . . . ?
C1 N1 C7 C12 -45.0(5) . . . . ?
C13 N1 C7 C12 125.1(4) . . . . ?
C12 C7 C8 C9 -1.4(6) . . . . ?
N1 C7 C8 C9 176.8(4) . . . . ?
C7 C8 C9 C10 -0.3(7) . . . . ?
C8 C9 C10 C11 1.7(7) . . . . ?
C9 C10 C11 C12 -1.4(7) . . . . ?
C8 C7 C12 C11 1.8(6) . . . . ?
N1 C7 C12 C11 -176.5(4) . . . . ?
C10 C11 C12 C7 -0.3(6) . . . . ?
C1 N1 C13 C14 -40.6(5) . . . . ?
C7 N1 C13 C14 149.6(4) . . . . ?
C1 N1 C13 C18 139.5(4) . . . . ?
C7 N1 C13 C18 -30.4(5) . . . . ?
C18 C13 C14 C15 0.2(6) . . . . ?
N1 C13 C14 C15 -179.8(4) . . . . ?
C13 C14 C15 C16 0.5(6) . . . . ?
C14 C15 C16 C17 -0.3(7) . . . . ?
C15 C16 C17 C18 -0.6(7) . . . . ?
C14 C13 C18 C17 -1.1(6) . . . . ?
N1 C13 C18 C17 178.8(4) . . . . ?
C16 C17 C18 C13 1.3(7) . . . . ?
C3 C4 C19 C20 6.2(6) . . . . ?
C5 C4 C19 C20 -173.6(4) . . . . ?
C4 C19 C20 C21 -178.2(3) . . . . ?
Ti1 O1 C21 O3 -4.8(5) . . . 2_657 ?
Ti1 O1 C21 C20 176.7(2) . . . . ?
C19 C20 C21 O1 175.1(3) . . . . ?
C19 C20 C21 O3 -3.5(5) . . . 2_657 ?
Ti2 O4 C22 C25 4.5(5) 2_657 . . . ?
Ti1 O4 C22 C25 -162.7(3) . . . . ?
Ti2 O4 C22 C23 -169.7(3) 2_657 . . . ?
Ti1 O4 C22 C23 23.2(5) . . . . ?
C25 C22 C23 C24 138.6(5) . . . . ?
O4 C22 C23 C24 -47.3(6) . . . . ?
Ti1 O5 C24 C23 -28.2(5) . . . . ?
Ti1 O5 C24 C26 91.6(5) . . . . ?
Ti1 O5 C24 C27 -148.4(4) . . . . ?
C22 C23 C24 O5 47.0(6) . . . . ?
C22 C23 C24 C26 -71.0(6) . . . . ?
C22 C23 C24 C27 165.8(5) . . . . ?
O4 C22 C25 C34 17.3(7) . . . 2_657 ?
C23 C22 C25 C34 -168.9(5) . . . 2_657 ?
Ti1 O6 C28 C29 -93.7(4) . . . . ?
Ti1 O6 C28 C30 143.9(3) . . . . ?
Ti2 O7 C31 C33 -48.7(4) . . . . ?
Ti1 O7 C31 C33 107.8(3) . . . . ?
Ti2 O7 C31 C32 75.2(4) . . . . ?
Ti1 O7 C31 C32 -128.3(3) . . . . ?
Ti2 O8 C34 C25 -39.1(5) . . . 2_657 ?
Ti2 O8 C34 C35 -157.3(4) . . . . ?
Ti2 O8 C34 C36 82.1(5) . . . . ?

_refine_diff_density_max         0.733
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.154

####################################################################### 
# 
# 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_3
_database_code_depnum_ccdc_archive 'CCDC 1946009'
loop_
_audit_author_name
_audit_author_address
'Qin-Yu Zhu'
;Soochow University
China
;
_audit_update_record             
;
2019-08-08 deposited with the CCDC.	2019-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C56 H90 N2 O16 Ti4'
_chemical_formula_weight         1238.89

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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   15.836(2)
_cell_length_b                   11.5845(14)
_cell_length_c                   18.080(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.343(4)
_cell_angle_gamma                90
_cell_volume                     3240.1(7)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9511
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      23.4

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_F_000             1312
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.537
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.948
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            69449
_diffrn_reflns_av_unetI/netI     0.0388
_diffrn_reflns_av_R_equivalents  0.0966
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.608
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measured_fraction_theta_full 0.976
_diffrn_reflns_Laue_measured_fraction_max 0.976
_diffrn_reflns_Laue_measured_fraction_full 0.976
_diffrn_reflns_point_group_measured_fraction_max 0.976
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             5569
_reflns_number_gt                3703
_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       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_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)+(0.0938P)²+3.0201P] 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         5569
_refine_ls_number_parameters     370
_refine_ls_number_restraints     39
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0646
_refine_ls_wR_factor_ref         0.1979
_refine_ls_wR_factor_gt          0.1588
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.069
_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_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 -0.03566(5) 0.40658(6) 0.44496(4) 0.0546(3) Uani 1 1 d . . . . .
Ti2 Ti 0.16114(5) 0.43548(7) 0.48403(5) 0.0618(3) Uani 1 1 d . . . . .
O1 O 0.1171(2) 0.7126(3) 0.52484(17) 0.0656(8) Uani 1 1 d . . . . .
O2 O 0.2143(2) 0.5981(3) 0.48656(18) 0.0681(8) Uani 1 1 d . . . . .
O3 O 0.2556(2) 0.3654(3) 0.5392(2) 0.0752(9) Uani 1 1 d . . . . .
O4 O 0.13503(18) 0.4853(2) 0.58861(15) 0.0576(7) Uani 1 1 d . . . . .
O5 O 0.0533(2) 0.6405(3) 0.65118(16) 0.0708(9) Uani 1 1 d . . . . .
O6 O 0.05023(17) 0.5204(2) 0.45673(14) 0.0515(7) Uani 1 1 d . . . . .
O7 O 0.06971(19) 0.3120(2) 0.48236(16) 0.0611(8) Uani 1 1 d . . . . .
O8 O 0.1804(3) 0.4071(3) 0.3928(2) 0.0829(10) Uani 1 1 d . . . . .
N1 N 0.4894(4) 1.1681(6) 0.3655(4) 0.135(2) Uani 1 1 d . U . . .
C1 C 0.4404(4) 1.0776(6) 0.3851(4) 0.103(2) Uani 1 1 d . . . . .
C2 C 0.3637(5) 1.0968(5) 0.4063(4) 0.100(2) Uani 1 1 d . . . . .
H2 H 0.343253 1.171972 0.407128 0.120 Uiso 1 1 calc R U . . .
C3 C 0.3160(4) 1.0065(5) 0.4268(3) 0.0883(17) Uani 1 1 d . . . . .
H3 H 0.265230 1.022457 0.442796 0.106 Uiso 1 1 calc R U . . .
C4 C 0.3426(3) 0.8922(4) 0.4239(3) 0.0721(14) Uani 1 1 d . . . . .
C5 C 0.4177(4) 0.8744(6) 0.3993(4) 0.0983(19) Uani 1 1 d . . . . .
H5 H 0.436050 0.798865 0.395052 0.118 Uiso 1 1 calc R U . . .
C6 C 0.4669(5) 0.9624(7) 0.3807(5) 0.120(3) Uani 1 1 d . . . . .
H6 H 0.517927 0.946100 0.365178 0.144 Uiso 1 1 calc R U . . .
C7 C 0.4593(6) 1.2834(8) 0.3606(5) 0.154(4) Uani 1 1 d . . . . .
H7A H 0.397752 1.284364 0.338980 0.184 Uiso 1 1 calc R U . . .
H7B H 0.488079 1.326804 0.327192 0.184 Uiso 1 1 calc R U . . .
C8 C 0.4767(9) 1.3412(11) 0.4388(6) 0.228(7) Uani 1 1 d . . . . .
H8A H 0.442793 1.303984 0.470028 0.341 Uiso 1 1 calc R U . . .
H8B H 0.461151 1.421341 0.433251 0.341 Uiso 1 1 calc R U . . .
H8C H 0.536910 1.334428 0.462103 0.341 Uiso 1 1 calc R U . . .
C9 C 0.5782(6) 1.1545(9) 0.3621(5) 0.154(3) Uani 1 1 d . U . . .
H9A H 0.610158 1.224330 0.379383 0.185 Uiso 1 1 calc R U . . .
H9B H 0.603697 1.091062 0.394273 0.185 Uiso 1 1 calc R U . . .
C10 C 0.5815(6) 1.1309(10) 0.2835(5) 0.158(3) Uani 1 1 d . . . . .
H10A H 0.541933 1.069761 0.264306 0.237 Uiso 1 1 calc R U . . .
H10B H 0.639078 1.108184 0.280781 0.237 Uiso 1 1 calc R U . . .
H10C H 0.565720 1.199178 0.253663 0.237 Uiso 1 1 calc R U . . .
C11 C 0.2947(3) 0.7966(4) 0.4461(2) 0.0672(12) Uani 1 1 d . . . . .
H11 H 0.314447 0.723372 0.437179 0.081 Uiso 1 1 calc R U . . .
C12 C 0.2274(3) 0.7996(4) 0.4770(3) 0.0660(12) Uani 1 1 d . . . . .
H12 H 0.205939 0.871423 0.486860 0.079 Uiso 1 1 calc R U . . .
C13 C 0.1832(3) 0.6955(4) 0.4972(3) 0.0635(12) Uani 1 1 d . . . . .
C14 C 0.3054(4) 0.3633(6) 0.6122(4) 0.0965(18) Uani 1 1 d . . . . .
C15 C 0.2514(4) 0.3922(6) 0.6681(4) 0.106(2) Uani 1 1 d . . . . .
H15 H 0.269343 0.359928 0.715958 0.127 Uiso 1 1 calc R U . . .
C16 C 0.1817(3) 0.4573(5) 0.6584(3) 0.0726(13) Uani 1 1 d . . . . .
C17 C 0.1456(5) 0.4941(7) 0.7200(3) 0.122(3) Uani 1 1 d . . . . .
H17A H 0.187157 0.478707 0.766736 0.147 Uiso 1 1 calc R U . . .
H17B H 0.094682 0.447888 0.720537 0.147 Uiso 1 1 calc R U . . .
C18 C 0.1203(4) 0.6214(6) 0.7190(3) 0.0926(18) Uani 1 1 d . . . . .
C19 C 0.3439(5) 0.2412(7) 0.6260(4) 0.126(3) Uani 1 1 d . . . . .
H19A H 0.298078 0.185319 0.617415 0.189 Uiso 1 1 calc R U . . .
H19B H 0.376038 0.235114 0.677296 0.189 Uiso 1 1 calc R U . . .
H19C H 0.381654 0.226977 0.591930 0.189 Uiso 1 1 calc R U . . .
C20 C 0.3794(5) 0.4532(8) 0.6151(6) 0.161(4) Uani 1 1 d . . . . .
H20A H 0.428135 0.416195 0.601525 0.242 Uiso 1 1 calc R U . . .
H20B H 0.396116 0.484030 0.665376 0.242 Uiso 1 1 calc R U . . .
H20C H 0.359325 0.514643 0.580113 0.242 Uiso 1 1 calc R U . . .
C21 C 0.1940(5) 0.7018(9) 0.7160(4) 0.150(4) Uani 1 1 d . . . . .
H21A H 0.216500 0.685029 0.671871 0.225 Uiso 1 1 calc R U . . .
H21B H 0.238813 0.691495 0.760527 0.225 Uiso 1 1 calc R U . . .
H21C H 0.173863 0.780113 0.713643 0.225 Uiso 1 1 calc R U . . .
C22 C 0.0774(5) 0.6487(7) 0.7853(3) 0.118(2) Uani 1 1 d . . . . .
H22A H 0.059174 0.727922 0.782454 0.177 Uiso 1 1 calc R U . . .
H22B H 0.118001 0.635787 0.832193 0.177 Uiso 1 1 calc R U . . .
H22C H 0.028063 0.599500 0.782863 0.177 Uiso 1 1 calc R U . . .
C23 C 0.0824(6) 0.1899(5) 0.4881(4) 0.110(2) Uani 1 1 d . . . . .
H23 H 0.145505 0.188808 0.495285 0.133 Uiso 1 1 calc R U . . .
C24 C 0.0758(6) 0.1511(7) 0.5626(5) 0.151(3) Uani 1 1 d . . . . .
H24A H 0.016845 0.156560 0.567654 0.226 Uiso 1 1 calc R U . . .
H24B H 0.111590 0.198619 0.600229 0.226 Uiso 1 1 calc R U . . .
H24C H 0.094740 0.072330 0.569458 0.226 Uiso 1 1 calc R U . . .
C25 C 0.0625(9) 0.1314(7) 0.4206(6) 0.187(5) Uani 1 1 d . . . . .
H25A H 0.001867 0.139206 0.399036 0.280 Uiso 1 1 calc R U . . .
H25B H 0.076496 0.051181 0.429126 0.280 Uiso 1 1 calc R U . . .
H25C H 0.095194 0.162811 0.386298 0.280 Uiso 1 1 calc R U . . .
C26 C 0.1548(7) 0.4182(8) 0.3152(4) 0.136(3) Uani 1 1 d . U . . .
C27 C 0.1261(10) 0.5293(11) 0.2949(8) 0.218(6) Uani 1 1 d . U . . .
H27A H 0.174155 0.581645 0.305310 0.327 Uiso 1 1 calc R U . . .
H27B H 0.084212 0.551702 0.323505 0.327 Uiso 1 1 calc R U . . .
H27C H 0.100079 0.531293 0.241842 0.327 Uiso 1 1 calc R U . . .
C28 C 0.1689(16) 0.3166(18) 0.2774(10) 0.149(6) Uani 0.5 1 d . U P . .
C28' C 0.2239(13) 0.391(2) 0.2756(10) 0.146(6) Uani 0.5 1 d . U P . .


_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 O5 1.786(3) 3_566 ?
Ti1 O6 1.873(3) . ?
Ti1 O7 1.990(3) . ?
Ti1 O4 2.001(3) 3_566 ?
Ti1 O6 2.026(3) 3_566 ?
Ti1 O1 2.041(3) 3_566 ?
Ti1 Ti1 2.9934(14) 3_566 ?
Ti1 Ti2 3.0632(12) . ?
Ti1 Ti2 3.1678(12) 3_566 ?
Ti2 O8 1.772(3) . ?
Ti2 O3 1.804(3) . ?
Ti2 O6 1.981(3) . ?
Ti2 O7 2.031(3) . ?
Ti2 O2 2.060(3) . ?
Ti2 O4 2.101(3) . ?
O1 C13 1.269(6) . ?
O2 C13 1.262(6) . ?
O3 C14 1.386(7) . ?
O4 C16 1.358(5) . ?
O5 C18 1.456(6) . ?
O7 C23 1.429(6) . ?
O8 C26 1.380(8) . ?
N1 C1 1.395(7) . ?
N1 C7 1.415(11) . ?
N1 C9 1.428(11) . ?
C1 C2 1.368(10) . ?
C1 C6 1.405(10) . ?
C2 C3 1.387(8) . ?
C2 H2 0.9300 . ?
C3 C4 1.393(8) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(8) . ?
C4 C11 1.447(6) . ?
C5 C6 1.369(8) . ?
C5 H5 0.9300 . ?
C6 H6 0.9300 . ?
C7 C8 1.536(14) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.459(11) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 C12 1.306(7) . ?
C11 H11 0.9300 . ?
C12 C13 1.478(6) . ?
C12 H12 0.9300 . ?
C14 C15 1.493(9) . ?
C14 C20 1.560(9) . ?
C14 C19 1.540(9) . ?
C15 C16 1.317(8) . ?
C15 H15 0.9300 . ?
C16 C17 1.422(8) . ?
C17 C18 1.527(10) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C21 1.504(9) . ?
C18 C22 1.533(8) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 C25 1.373(10) . ?
C23 C24 1.446(10) . ?
C23 H23 0.9800 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.388(13) . ?
C26 C28 1.403(18) . ?
C26 C28' 1.464(17) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C28' 1.23(2) . ?

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 Ti1 O6 106.51(14) 3_566 . ?
O5 Ti1 O7 96.17(14) 3_566 . ?
O6 Ti1 O7 79.22(12) . . ?
O5 Ti1 O4 86.98(14) 3_566 3_566 ?
O6 Ti1 O4 95.67(12) . 3_566 ?
O7 Ti1 O4 174.58(12) . 3_566 ?
O5 Ti1 O6 163.38(14) 3_566 3_566 ?
O6 Ti1 O6 79.77(12) . 3_566 ?
O7 Ti1 O6 100.16(12) . 3_566 ?
O4 Ti1 O6 76.99(11) 3_566 3_566 ?
O5 Ti1 O1 94.45(14) 3_566 3_566 ?
O6 Ti1 O1 158.47(12) . 3_566 ?
O7 Ti1 O1 93.92(13) . 3_566 ?
O4 Ti1 O1 90.22(13) 3_566 3_566 ?
O6 Ti1 O1 81.43(12) 3_566 3_566 ?
O5 Ti1 Ti1 145.72(12) 3_566 3_566 ?
O6 Ti1 Ti1 41.76(8) . 3_566 ?
O7 Ti1 Ti1 90.13(9) . 3_566 ?
O4 Ti1 Ti1 84.81(9) 3_566 3_566 ?
O6 Ti1 Ti1 38.01(7) 3_566 3_566 ?
O1 Ti1 Ti1 118.76(10) 3_566 3_566 ?
O5 Ti1 Ti2 101.37(11) 3_566 . ?
O6 Ti1 Ti2 38.61(9) . . ?
O7 Ti1 Ti2 40.88(8) . . ?
O4 Ti1 Ti2 134.17(9) 3_566 . ?
O6 Ti1 Ti2 93.04(8) 3_566 . ?
O1 Ti1 Ti2 132.99(10) 3_566 . ?
Ti1 Ti1 Ti2 63.06(3) 3_566 . ?
O5 Ti1 Ti2 126.16(12) 3_566 3_566 ?
O6 Ti1 Ti2 92.91(9) . 3_566 ?
O7 Ti1 Ti2 137.17(9) . 3_566 ?
O4 Ti1 Ti2 40.60(8) 3_566 3_566 ?
O6 Ti1 Ti2 37.27(8) 3_566 3_566 ?
O1 Ti1 Ti2 78.20(10) 3_566 3_566 ?
Ti1 Ti1 Ti2 59.54(3) 3_566 3_566 ?
Ti2 Ti1 Ti2 122.61(3) . 3_566 ?
O8 Ti2 O3 98.30(17) . . ?
O8 Ti2 O6 100.38(15) . . ?
O3 Ti2 O6 161.31(14) . . ?
O8 Ti2 O7 96.89(15) . . ?
O3 Ti2 O7 101.27(14) . . ?
O6 Ti2 O7 75.79(11) . . ?
O8 Ti2 O2 92.25(15) . . ?
O3 Ti2 O2 96.49(15) . . ?
O6 Ti2 O2 83.56(12) . . ?
O7 Ti2 O2 158.59(13) . . ?
O8 Ti2 O4 174.50(14) . . ?
O3 Ti2 O4 85.70(14) . . ?
O6 Ti2 O4 75.72(11) . . ?
O7 Ti2 O4 85.98(11) . . ?
O2 Ti2 O4 83.51(12) . . ?
O8 Ti2 Ti1 97.73(13) . . ?
O3 Ti2 Ti1 139.53(11) . . ?
O6 Ti2 Ti1 36.16(8) . . ?
O7 Ti2 Ti1 39.88(8) . . ?
O2 Ti2 Ti1 119.72(10) . . ?
O4 Ti2 Ti1 81.44(8) . . ?
O8 Ti2 Ti1 137.09(13) . 3_566 ?
O3 Ti2 Ti1 123.60(12) . 3_566 ?
O6 Ti2 Ti1 38.26(7) . 3_566 ?
O7 Ti2 Ti1 84.59(9) . 3_566 ?
O2 Ti2 Ti1 75.60(10) . 3_566 ?
O4 Ti2 Ti1 38.32(8) . 3_566 ?
Ti1 Ti2 Ti1 57.39(3) . 3_566 ?
C13 O1 Ti1 128.5(3) . 3_566 ?
C13 O2 Ti2 130.6(3) . . ?
C14 O3 Ti2 140.4(4) . . ?
C16 O4 Ti1 131.9(3) . 3_566 ?
C16 O4 Ti2 126.7(3) . . ?
Ti1 O4 Ti2 101.08(12) 3_566 . ?
C18 O5 Ti1 134.9(4) . 3_566 ?
Ti1 O6 Ti2 105.23(13) . . ?
Ti1 O6 Ti1 100.23(12) . 3_566 ?
Ti2 O6 Ti1 104.47(12) . 3_566 ?
C23 O7 Ti1 131.6(4) . . ?
C23 O7 Ti2 127.4(4) . . ?
Ti1 O7 Ti2 99.25(12) . . ?
C26 O8 Ti2 149.0(5) . . ?
C1 N1 C7 121.8(7) . . ?
C1 N1 C9 122.3(7) . . ?
C7 N1 C9 115.0(6) . . ?
N1 C1 C2 121.6(7) . . ?
N1 C1 C6 120.6(7) . . ?
C2 C1 C6 117.7(6) . . ?
C3 C2 C1 121.2(7) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 121.4(6) . . ?
C2 C3 H3 119.3 . . ?
C4 C3 H3 119.3 . . ?
C5 C4 C3 116.4(5) . . ?
C5 C4 C11 121.1(5) . . ?
C3 C4 C11 122.4(5) . . ?
C4 C5 C6 123.1(7) . . ?
C4 C5 H5 118.5 . . ?
C6 C5 H5 118.5 . . ?
C5 C6 C1 120.1(7) . . ?
C5 C6 H6 120.0 . . ?
C1 C6 H6 120.0 . . ?
N1 C7 C8 111.2(8) . . ?
N1 C7 H7A 109.4 . . ?
C8 C7 H7A 109.4 . . ?
N1 C7 H7B 109.4 . . ?
C8 C7 H7B 109.4 . . ?
H7A C7 H7B 108.0 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 N1 107.7(7) . . ?
C10 C9 H9A 110.2 . . ?
N1 C9 H9A 110.2 . . ?
C10 C9 H9B 110.2 . . ?
N1 C9 H9B 110.2 . . ?
H9A C9 H9B 108.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C12 C11 C4 128.5(5) . . ?
C12 C11 H11 115.7 . . ?
C4 C11 H11 115.7 . . ?
C11 C12 C13 123.8(5) . . ?
C11 C12 H12 118.1 . . ?
C13 C12 H12 118.1 . . ?
O2 C13 O1 125.5(4) . . ?
O2 C13 C12 118.1(5) . . ?
O1 C13 C12 116.4(5) . . ?
O3 C14 C15 110.4(5) . . ?
O3 C14 C20 106.9(6) . . ?
C15 C14 C20 111.3(7) . . ?
O3 C14 C19 107.2(6) . . ?
C15 C14 C19 111.2(6) . . ?
C20 C14 C19 109.8(6) . . ?
C16 C15 C14 128.5(6) . . ?
C16 C15 H15 115.7 . . ?
C14 C15 H15 115.7 . . ?
C15 C16 O4 122.3(5) . . ?
C15 C16 C17 122.2(5) . . ?
O4 C16 C17 115.2(5) . . ?
C16 C17 C18 115.4(6) . . ?
C16 C17 H17A 108.4 . . ?
C18 C17 H17A 108.4 . . ?
C16 C17 H17B 108.4 . . ?
C18 C17 H17B 108.4 . . ?
H17A C17 H17B 107.5 . . ?
O5 C18 C21 107.9(5) . . ?
O5 C18 C17 107.5(4) . . ?
C21 C18 C17 113.2(7) . . ?
O5 C18 C22 105.2(5) . . ?
C21 C18 C22 112.2(5) . . ?
C17 C18 C22 110.4(6) . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C14 C20 H20A 109.5 . . ?
C14 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C14 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C25 C23 C24 128.8(7) . . ?
C25 C23 O7 115.0(6) . . ?
C24 C23 O7 109.8(6) . . ?
C25 C23 H23 98.4 . . ?
C24 C23 H23 98.4 . . ?
O7 C23 H23 98.4 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
O8 C26 C27 111.3(9) . . ?
O8 C26 C28 112.0(10) . . ?
C27 C26 C28 136.6(12) . . ?
O8 C26 C28' 112.8(10) . . ?
C27 C26 C28' 107.8(12) . . ?
C28 C26 C28' 50.9(11) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28' C28 C26 67.1(13) . . ?
C28 C28' C26 62.0(11) . . ?

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
O8 Ti2 O3 C14 161.1(5) . . . . ?
O6 Ti2 O3 C14 -21.2(8) . . . . ?
O7 Ti2 O3 C14 -100.1(5) . . . . ?
O2 Ti2 O3 C14 67.8(5) . . . . ?
O4 Ti2 O3 C14 -15.1(5) . . . . ?
Ti1 Ti2 O3 C14 -86.6(6) . . . . ?
Ti1 Ti2 O3 C14 -9.2(6) 3_566 . . . ?
O5 Ti1 O6 Ti2 -87.63(16) 3_566 . . . ?
O7 Ti1 O6 Ti2 5.68(12) . . . . ?
O4 Ti1 O6 Ti2 -176.14(12) 3_566 . . . ?
O6 Ti1 O6 Ti2 108.20(15) 3_566 . . . ?
O1 Ti1 O6 Ti2 78.7(4) 3_566 . . . ?
Ti1 Ti1 O6 Ti2 108.20(15) 3_566 . . . ?
Ti2 Ti1 O6 Ti2 143.23(9) 3_566 . . . ?
O5 Ti1 O6 Ti1 164.17(14) 3_566 . . 3_566 ?
O7 Ti1 O6 Ti1 -102.52(13) . . . 3_566 ?
O4 Ti1 O6 Ti1 75.66(12) 3_566 . . 3_566 ?
O6 Ti1 O6 Ti1 0.0 3_566 . . 3_566 ?
O1 Ti1 O6 Ti1 -29.5(4) 3_566 . . 3_566 ?
Ti2 Ti1 O6 Ti1 -108.20(15) . . . 3_566 ?
Ti2 Ti1 O6 Ti1 35.03(10) 3_566 . . 3_566 ?
O3 Ti2 O8 C26 -179.5(9) . . . . ?
O6 Ti2 O8 C26 1.2(10) . . . . ?
O7 Ti2 O8 C26 77.9(10) . . . . ?
O2 Ti2 O8 C26 -82.7(10) . . . . ?
Ti1 Ti2 O8 C26 37.7(10) . . . . ?
Ti1 Ti2 O8 C26 -11.5(10) 3_566 . . . ?
C7 N1 C1 C2 -5.3(11) . . . . ?
C9 N1 C1 C2 163.5(7) . . . . ?
C7 N1 C1 C6 172.3(8) . . . . ?
C9 N1 C1 C6 -18.9(11) . . . . ?
N1 C1 C2 C3 -179.0(6) . . . . ?
C6 C1 C2 C3 3.3(10) . . . . ?
C1 C2 C3 C4 -2.3(9) . . . . ?
C2 C3 C4 C5 -0.5(8) . . . . ?
C2 C3 C4 C11 179.0(5) . . . . ?
C3 C4 C5 C6 2.2(9) . . . . ?
C11 C4 C5 C6 -177.3(6) . . . . ?
C4 C5 C6 C1 -1.2(11) . . . . ?
N1 C1 C6 C5 -179.3(7) . . . . ?
C2 C1 C6 C5 -1.6(11) . . . . ?
C1 N1 C7 C8 82.9(9) . . . . ?
C9 N1 C7 C8 -86.7(10) . . . . ?
C1 N1 C9 C10 95.8(9) . . . . ?
C7 N1 C9 C10 -94.6(10) . . . . ?
C5 C4 C11 C12 173.1(5) . . . . ?
C3 C4 C11 C12 -6.4(8) . . . . ?
C4 C11 C12 C13 179.8(4) . . . . ?
Ti2 O2 C13 O1 16.1(7) . . . . ?
Ti2 O2 C13 C12 -164.8(3) . . . . ?
Ti1 O1 C13 O2 -4.0(7) 3_566 . . . ?
Ti1 O1 C13 C12 176.9(3) 3_566 . . . ?
C11 C12 C13 O2 2.8(6) . . . . ?
C11 C12 C13 O1 -178.1(4) . . . . ?
Ti2 O3 C14 C15 29.0(8) . . . . ?
Ti2 O3 C14 C20 -92.1(7) . . . . ?
Ti2 O3 C14 C19 150.2(5) . . . . ?
O3 C14 C15 C16 -28.6(10) . . . . ?
C20 C14 C15 C16 89.9(9) . . . . ?
C19 C14 C15 C16 -147.4(7) . . . . ?
C14 C15 C16 O4 17.5(11) . . . . ?
C14 C15 C16 C17 -168.5(7) . . . . ?
Ti1 O4 C16 C15 -172.6(5) 3_566 . . . ?
Ti2 O4 C16 C15 -0.4(7) . . . . ?
Ti1 O4 C16 C17 12.9(7) 3_566 . . . ?
Ti2 O4 C16 C17 -174.8(5) . . . . ?
C15 C16 C17 C18 134.6(7) . . . . ?
O4 C16 C17 C18 -51.0(8) . . . . ?
Ti1 O5 C18 C21 81.3(7) 3_566 . . . ?
Ti1 O5 C18 C17 -41.1(7) 3_566 . . . ?
Ti1 O5 C18 C22 -158.8(4) 3_566 . . . ?
C16 C17 C18 O5 62.3(7) . . . . ?
C16 C17 C18 C21 -56.7(7) . . . . ?
C16 C17 C18 C22 176.6(5) . . . . ?
Ti1 O7 C23 C25 61.1(10) . . . . ?
Ti2 O7 C23 C25 -100.6(9) . . . . ?
Ti1 O7 C23 C24 -93.4(7) . . . . ?
Ti2 O7 C23 C24 105.0(7) . . . . ?
Ti2 O8 C26 C27 43.3(15) . . . . ?
Ti2 O8 C26 C28 -140.0(13) . . . . ?
Ti2 O8 C26 C28' 164.7(12) . . . . ?
O8 C26 C28 C28' -102.2(14) . . . . ?
C27 C26 C28 C28' 73(2) . . . . ?
O8 C26 C28' C28 100.4(15) . . . . ?
C27 C26 C28' C28 -136.3(16) . . . . ?

_refine_diff_density_max         0.518
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.058

