# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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 1551804'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-08-01 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            'C36 H45 Br O11 Ti2'
_chemical_formula_weight         829.43

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'
Br Br -0.2901 2.4595 '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                   12.9644(12)
_cell_length_b                   13.1630(12)
_cell_length_c                   23.030(2)
_cell_angle_alpha                90
_cell_angle_beta                 104.724(3)
_cell_angle_gamma                90
_cell_volume                     3801.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9990
_cell_measurement_theta_min      2.3
_cell_measurement_theta_max      24.8

_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_F_000             1712
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.260
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    1.528
_shelx_estimated_absorpt_T_min   0.692
_shelx_estimated_absorpt_T_max   0.750
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.657
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(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            60996
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_av_R_equivalents  0.0987
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.624
_diffrn_reflns_theta_max         27.502
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             8698
_reflns_number_gt                5888
_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)+(0.0127P)²+16.4457P] 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         8698
_refine_ls_number_parameters     461
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0980
_refine_ls_R_factor_gt           0.0543
_refine_ls_wR_factor_ref         0.1345
_refine_ls_wR_factor_gt          0.0940
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_restrained_S_all      1.124
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Br1 Br 0.13519(4) 0.61232(4) 0.24127(2) 0.03461(14) Uani 1 1 d . . . . .
Ti1 Ti 0.21935(6) 0.36541(6) 0.61582(4) 0.02305(19) Uani 1 1 d . . . . .
Ti2 Ti 0.37780(6) 0.22197(6) 0.56245(4) 0.02168(19) Uani 1 1 d . . . . .
O1 O 0.3100(2) 0.1097(2) 0.50176(14) 0.0257(7) Uani 1 1 d . . . . .
O2 O -0.0868(3) -0.0160(3) 0.38923(16) 0.0446(10) Uani 1 1 d . . . . .
O3 O 0.2262(2) 0.2265(2) 0.57303(13) 0.0199(7) Uani 1 1 d . . . . .
O4 O 0.0677(2) 0.3278(2) 0.58623(14) 0.0260(7) Uani 1 1 d . . . . .
O5 O 0.3063(2) 0.3132(2) 0.48810(14) 0.0238(7) Uani 1 1 d . . . . .
O6 O 0.2018(2) 0.4191(2) 0.52447(14) 0.0236(7) Uani 1 1 d . . . . .
O7 O 0.2136(3) 0.4958(2) 0.63424(15) 0.0287(8) Uani 1 1 d . . . . .
O8 O 0.2423(3) 0.3175(3) 0.69117(14) 0.0293(8) Uani 1 1 d . . . . .
O9 O 0.3728(2) 0.3433(2) 0.61225(14) 0.0235(7) Uani 1 1 d . . . . .
O10 O 0.4201(2) 0.1331(2) 0.62244(14) 0.0266(7) Uani 1 1 d . . . . .
O11 O 0.4980(2) 0.2343(3) 0.53909(15) 0.0281(8) Uani 1 1 d . . . . .
C1 C 0.1237(4) 0.1278(3) 0.4905(2) 0.0227(10) Uani 1 1 d . . . . .
C2 C 0.1343(3) 0.1994(3) 0.5360(2) 0.0205(10) Uani 1 1 d . . . . .
C3 C 0.0453(4) 0.2537(4) 0.5465(2) 0.0245(10) Uani 1 1 d . . . . .
C4 C -0.0565(4) 0.2244(4) 0.5141(2) 0.0287(11) Uani 1 1 d . . . . .
H4 H -0.117680 0.257069 0.520984 0.034 Uiso 1 1 calc R U . . .
C5 C -0.0681(4) 0.1471(4) 0.4716(2) 0.0310(12) Uani 1 1 d . . . . .
H5 H -0.137977 0.126387 0.450909 0.037 Uiso 1 1 calc R U . . .
C6 C 0.0182(4) 0.0993(4) 0.4583(2) 0.0270(11) Uani 1 1 d . . . . .
C7 C 0.2018(4) 0.0075(4) 0.4274(2) 0.0305(11) Uani 1 1 d . . . . .
C8 C 0.2899(5) -0.0320(4) 0.4114(2) 0.0383(13) Uani 1 1 d . . . . .
H8 H 0.359495 -0.010695 0.432261 0.046 Uiso 1 1 calc R U . . .
C9 C 0.2775(5) -0.1019(4) 0.3654(3) 0.0463(15) Uani 1 1 d . . . . .
H9 H 0.338067 -0.128583 0.354499 0.056 Uiso 1 1 calc R U . . .
C10 C 0.1760(6) -0.1326(5) 0.3354(3) 0.0520(17) Uani 1 1 d . . . . .
H10 H 0.167292 -0.180648 0.303693 0.062 Uiso 1 1 calc R U . . .
C11 C 0.0881(6) -0.0951(4) 0.3505(2) 0.0470(16) Uani 1 1 d . . . . .
H11 H 0.019071 -0.117440 0.329292 0.056 Uiso 1 1 calc R U . . .
C12 C 0.0986(5) -0.0242(4) 0.3969(2) 0.0338(12) Uani 1 1 d . . . . .
C13 C 0.2167(4) 0.0836(3) 0.4762(2) 0.0241(10) Uani 1 1 d . . . . .
C14 C 0.0022(5) 0.0175(4) 0.4128(2) 0.0365(13) Uani 1 1 d . . . . .
C15 C 0.2109(3) 0.4400(3) 0.4235(2) 0.0212(10) Uani 1 1 d . . . . .
C16 C 0.2449(4) 0.4018(4) 0.3753(2) 0.0294(11) Uani 1 1 d . . . . .
H16 H 0.285697 0.340987 0.379859 0.035 Uiso 1 1 calc R U . . .
C17 C 0.2199(4) 0.4514(4) 0.3208(2) 0.0296(11) Uani 1 1 d . . . . .
H17 H 0.242000 0.424645 0.287572 0.036 Uiso 1 1 calc R U . . .
C18 C 0.1622(4) 0.5406(4) 0.3151(2) 0.0251(10) Uani 1 1 d . . . . .
C19 C 0.1247(4) 0.5785(4) 0.3614(2) 0.0285(11) Uani 1 1 d . . . . .
H19 H 0.082459 0.638468 0.356235 0.034 Uiso 1 1 calc R U . . .
C20 C 0.1498(4) 0.5273(4) 0.4159(2) 0.0258(10) Uani 1 1 d . . . . .
H20 H 0.124584 0.552630 0.448420 0.031 Uiso 1 1 calc R U . . .
C21 C 0.2415(3) 0.3871(4) 0.4832(2) 0.0220(10) Uani 1 1 d . . . . .
C22 C 0.1914(4) 0.6001(4) 0.6205(2) 0.0332(12) Uani 1 1 d . . . . .
H22 H 0.188339 0.612181 0.577259 0.040 Uiso 1 1 calc R U . . .
C23 C 0.0846(5) 0.6260(5) 0.6319(4) 0.066(2) Uani 1 1 d . . . . .
H23A H 0.028416 0.587183 0.604282 0.099 Uiso 1 1 calc R U . . .
H23B H 0.070839 0.698819 0.625316 0.099 Uiso 1 1 calc R U . . .
H23C H 0.085421 0.608724 0.673381 0.099 Uiso 1 1 calc R U . . .
C24 C 0.2781(5) 0.6646(4) 0.6589(3) 0.0518(17) Uani 1 1 d . . . . .
H24A H 0.276572 0.658306 0.701044 0.078 Uiso 1 1 calc R U . . .
H24B H 0.266830 0.735758 0.646350 0.078 Uiso 1 1 calc R U . . .
H24C H 0.347569 0.641817 0.654230 0.078 Uiso 1 1 calc R U . . .
C25 C 0.2501(5) 0.3617(6) 0.7486(3) 0.0553(18) Uani 1 1 d . . . . .
H25 H 0.253364 0.436923 0.743067 0.066 Uiso 1 1 calc R U . . .
C26 C 0.1491(5) 0.3414(6) 0.7671(3) 0.065(2) Uani 1 1 d . . . . .
H26A H 0.089209 0.374570 0.738865 0.098 Uiso 1 1 calc R U . . .
H26B H 0.155789 0.368456 0.807573 0.098 Uiso 1 1 calc R U . . .
H26C H 0.136460 0.268044 0.767069 0.098 Uiso 1 1 calc R U . . .
C27 C 0.3472(5) 0.3339(6) 0.7915(3) 0.070(2) Uani 1 1 d . . . . .
H27A H 0.347019 0.260721 0.799178 0.105 Uiso 1 1 calc R U . . .
H27B H 0.352554 0.371023 0.829041 0.105 Uiso 1 1 calc R U . . .
H27C H 0.408194 0.351096 0.775508 0.105 Uiso 1 1 calc R U . . .
C28 C 0.4565(4) 0.4121(4) 0.6423(2) 0.0278(11) Uani 1 1 d . . . . .
H28 H 0.430956 0.449416 0.673841 0.033 Uiso 1 1 calc R U . . .
C29 C 0.4755(4) 0.4889(4) 0.5975(3) 0.0397(14) Uani 1 1 d . . . . .
H29A H 0.502646 0.454166 0.566746 0.059 Uiso 1 1 calc R U . . .
H29B H 0.527861 0.539099 0.618142 0.059 Uiso 1 1 calc R U . . .
H29C H 0.408315 0.523162 0.578465 0.059 Uiso 1 1 calc R U . . .
C30 C 0.5559(4) 0.3541(4) 0.6730(2) 0.0364(13) Uani 1 1 d . . . . .
H30A H 0.538748 0.304896 0.701115 0.055 Uiso 1 1 calc R U . . .
H30B H 0.609996 0.401684 0.695072 0.055 Uiso 1 1 calc R U . . .
H30C H 0.583457 0.318195 0.642871 0.055 Uiso 1 1 calc R U . . .
C31 C 0.3776(4) 0.0825(4) 0.6664(2) 0.0336(12) Uani 1 1 d . . . . .
H31 H 0.308703 0.115496 0.667456 0.040 Uiso 1 1 calc R U . . .
C32 C 0.3567(5) -0.0266(4) 0.6489(3) 0.0469(15) Uani 1 1 d . . . . .
H32A H 0.311310 -0.030508 0.607807 0.070 Uiso 1 1 calc R U . . .
H32B H 0.320693 -0.059521 0.676438 0.070 Uiso 1 1 calc R U . . .
H32C H 0.424522 -0.061139 0.650892 0.070 Uiso 1 1 calc R U . . .
C33 C 0.4547(5) 0.0940(4) 0.7267(2) 0.0476(15) Uani 1 1 d . . . . .
H33A H 0.523442 0.063997 0.725714 0.071 Uiso 1 1 calc R U . . .
H33B H 0.426637 0.059186 0.757067 0.071 Uiso 1 1 calc R U . . .
H33C H 0.464462 0.166260 0.736801 0.071 Uiso 1 1 calc R U . . .
C34 C 0.5382(4) 0.2735(4) 0.4912(2) 0.0341(12) Uani 1 1 d . . . . .
H34 H 0.497898 0.336645 0.475315 0.041 Uiso 1 1 calc R U . . .
C35 C 0.5196(6) 0.1962(6) 0.4424(3) 0.070(2) Uani 1 1 d . . . . .
H35A H 0.555020 0.132490 0.458218 0.104 Uiso 1 1 calc R U . . .
H35B H 0.548828 0.220806 0.409694 0.104 Uiso 1 1 calc R U . . .
H35C H 0.442878 0.184272 0.427173 0.104 Uiso 1 1 calc R U . . .
C36 C 0.6539(4) 0.3001(6) 0.5160(3) 0.0588(19) Uani 1 1 d . . . . .
H36A H 0.660483 0.352216 0.547129 0.088 Uiso 1 1 calc R U . . .
H36B H 0.683147 0.326167 0.483627 0.088 Uiso 1 1 calc R U . . .
H36C H 0.693532 0.239309 0.533407 0.088 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
Br1 C18 1.898(5) . ?
Ti1 O7 1.774(3) . ?
Ti1 O8 1.799(3) . ?
Ti1 O4 1.974(3) . ?
Ti1 O9 2.033(3) . ?
Ti1 O3 2.090(3) . ?
Ti1 O6 2.176(3) . ?
Ti1 Ti2 3.2526(12) . ?
Ti2 O11 1.781(3) . ?
Ti2 O10 1.787(3) . ?
Ti2 O9 1.977(3) . ?
Ti2 O3 2.041(3) . ?
Ti2 O1 2.071(3) . ?
Ti2 O5 2.104(3) . ?
O1 C13 1.250(5) . ?
O2 C14 1.225(6) . ?
O3 C2 1.327(5) . ?
O4 C3 1.318(6) . ?
O5 C21 1.271(5) . ?
O6 C21 1.263(5) . ?
O7 C22 1.421(6) . ?
O8 C25 1.425(6) . ?
O9 C28 1.446(5) . ?
O10 C31 1.433(6) . ?
O11 C34 1.431(6) . ?
C1 C2 1.390(6) . ?
C1 C6 1.430(6) . ?
C1 C13 1.451(6) . ?
C2 C3 1.429(6) . ?
C3 C4 1.395(6) . ?
C4 C5 1.394(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(7) . ?
C5 H5 0.9500 . ?
C6 C14 1.480(7) . ?
C7 C8 1.388(7) . ?
C7 C12 1.408(7) . ?
C7 C13 1.480(7) . ?
C8 C9 1.382(7) . ?
C8 H8 0.9500 . ?
C9 C10 1.382(9) . ?
C9 H9 0.9500 . ?
C10 C11 1.367(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.399(7) . ?
C11 H11 0.9500 . ?
C12 C14 1.494(8) . ?
C15 C20 1.381(6) . ?
C15 C16 1.390(6) . ?
C15 C21 1.501(6) . ?
C16 C17 1.379(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.380(7) . ?
C17 H17 0.9500 . ?
C18 C19 1.374(6) . ?
C19 C20 1.389(7) . ?
C19 H19 0.9500 . ?
C20 H20 0.9500 . ?
C22 C23 1.512(7) . ?
C22 C24 1.504(7) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 C27 1.436(9) . ?
C25 C26 1.500(8) . ?
C25 H25 1.0000 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.509(7) . ?
C28 C30 1.510(7) . ?
C28 H28 1.0000 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.497(8) . ?
C31 C33 1.499(7) . ?
C31 H31 1.0000 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 C36 1.505(7) . ?
C34 C35 1.490(8) . ?
C34 H34 1.0000 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O7 Ti1 O8 96.62(15) . . ?
O7 Ti1 O4 103.10(15) . . ?
O8 Ti1 O4 98.69(15) . . ?
O7 Ti1 O9 104.42(14) . . ?
O8 Ti1 O9 93.75(14) . . ?
O4 Ti1 O9 148.16(13) . . ?
O7 Ti1 O3 165.62(14) . . ?
O8 Ti1 O3 97.57(14) . . ?
O4 Ti1 O3 77.04(12) . . ?
O9 Ti1 O3 72.32(12) . . ?
O7 Ti1 O6 85.21(14) . . ?
O8 Ti1 O6 176.18(14) . . ?
O4 Ti1 O6 84.12(13) . . ?
O9 Ti1 O6 82.54(12) . . ?
O3 Ti1 O6 80.49(12) . . ?
O7 Ti1 Ti2 136.14(11) . . ?
O8 Ti1 Ti2 101.28(11) . . ?
O4 Ti1 Ti2 113.15(10) . . ?
O9 Ti1 Ti2 35.23(9) . . ?
O3 Ti1 Ti2 37.54(8) . . ?
O6 Ti1 Ti2 75.17(8) . . ?
O11 Ti2 O10 99.95(15) . . ?
O11 Ti2 O9 105.18(14) . . ?
O10 Ti2 O9 97.43(14) . . ?
O11 Ti2 O3 167.51(14) . . ?
O10 Ti2 O3 92.44(13) . . ?
O9 Ti2 O3 74.51(12) . . ?
O11 Ti2 O1 96.62(14) . . ?
O10 Ti2 O1 92.81(14) . . ?
O9 Ti2 O1 153.83(13) . . ?
O3 Ti2 O1 81.07(12) . . ?
O11 Ti2 O5 86.61(14) . . ?
O10 Ti2 O5 171.16(14) . . ?
O9 Ti2 O5 86.45(13) . . ?
O3 Ti2 O5 80.91(12) . . ?
O1 Ti2 O5 80.48(13) . . ?
O11 Ti2 Ti1 138.31(12) . . ?
O10 Ti2 Ti1 100.78(11) . . ?
O9 Ti2 Ti1 36.38(9) . . ?
O3 Ti2 Ti1 38.59(9) . . ?
O1 Ti2 Ti1 117.96(9) . . ?
O5 Ti2 Ti1 77.65(9) . . ?
C13 O1 Ti2 135.1(3) . . ?
C2 O3 Ti2 130.6(3) . . ?
C2 O3 Ti1 113.5(3) . . ?
Ti2 O3 Ti1 103.87(13) . . ?
C3 O4 Ti1 116.7(3) . . ?
C21 O5 Ti2 130.9(3) . . ?
C21 O6 Ti1 131.1(3) . . ?
C22 O7 Ti1 154.1(3) . . ?
C25 O8 Ti1 135.0(4) . . ?
C28 O9 Ti2 130.7(3) . . ?
C28 O9 Ti1 120.9(3) . . ?
Ti2 O9 Ti1 108.39(14) . . ?
C31 O10 Ti2 138.8(3) . . ?
C34 O11 Ti2 141.6(3) . . ?
C2 C1 C6 117.8(4) . . ?
C2 C1 C13 121.0(4) . . ?
C6 C1 C13 121.2(4) . . ?
O3 C2 C1 124.6(4) . . ?
O3 C2 C3 112.9(4) . . ?
C1 C2 C3 122.5(4) . . ?
O4 C3 C4 125.9(4) . . ?
O4 C3 C2 116.3(4) . . ?
C4 C3 C2 117.8(5) . . ?
C5 C4 C3 119.7(5) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C6 C5 C4 122.6(4) . . ?
C6 C5 H5 118.7 . . ?
C4 C5 H5 118.7 . . ?
C5 C6 C1 119.1(5) . . ?
C5 C6 C14 120.7(5) . . ?
C1 C6 C14 120.1(5) . . ?
C8 C7 C12 119.8(5) . . ?
C8 C7 C13 119.9(5) . . ?
C12 C7 C13 120.3(5) . . ?
C9 C8 C7 120.7(6) . . ?
C9 C8 H8 119.7 . . ?
C7 C8 H8 119.7 . . ?
C8 C9 C10 119.3(6) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
C11 C10 C9 121.1(6) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C10 C11 C12 120.6(6) . . ?
C10 C11 H11 119.7 . . ?
C12 C11 H11 119.7 . . ?
C11 C12 C7 118.4(5) . . ?
C11 C12 C14 120.5(5) . . ?
C7 C12 C14 121.1(5) . . ?
O1 C13 C1 122.9(4) . . ?
O1 C13 C7 117.9(4) . . ?
C1 C13 C7 119.2(4) . . ?
O2 C14 C6 121.5(5) . . ?
O2 C14 C12 120.7(5) . . ?
C6 C14 C12 117.8(4) . . ?
C20 C15 C16 119.3(4) . . ?
C20 C15 C21 120.8(4) . . ?
C16 C15 C21 120.0(4) . . ?
C17 C16 C15 120.4(5) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.1(4) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C19 C18 C17 121.7(5) . . ?
C19 C18 Br1 119.6(4) . . ?
C17 C18 Br1 118.7(4) . . ?
C18 C19 C20 118.5(5) . . ?
C18 C19 H19 120.8 . . ?
C20 C19 H19 120.8 . . ?
C15 C20 C19 120.9(4) . . ?
C15 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
O6 C21 O5 125.0(4) . . ?
O6 C21 C15 118.1(4) . . ?
O5 C21 C15 116.9(4) . . ?
O7 C22 C23 108.8(4) . . ?
O7 C22 C24 109.7(4) . . ?
C23 C22 C24 110.6(5) . . ?
O7 C22 H22 109.3 . . ?
C23 C22 H22 109.3 . . ?
C24 C22 H22 109.3 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O8 C25 C27 112.1(5) . . ?
O8 C25 C26 109.3(5) . . ?
C27 C25 C26 115.8(6) . . ?
O8 C25 H25 106.3 . . ?
C27 C25 H25 106.3 . . ?
C26 C25 H25 106.3 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O9 C28 C29 108.9(4) . . ?
O9 C28 C30 110.8(4) . . ?
C29 C28 C30 113.0(4) . . ?
O9 C28 H28 108.0 . . ?
C29 C28 H28 108.0 . . ?
C30 C28 H28 108.0 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
O10 C31 C32 109.4(4) . . ?
O10 C31 C33 108.8(4) . . ?
C32 C31 C33 112.3(5) . . ?
O10 C31 H31 108.8 . . ?
C32 C31 H31 108.8 . . ?
C33 C31 H31 108.8 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O11 C34 C36 108.3(4) . . ?
O11 C34 C35 108.3(4) . . ?
C36 C34 C35 113.6(5) . . ?
O11 C34 H34 108.9 . . ?
C36 C34 H34 108.9 . . ?
C35 C34 H34 108.9 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O8 Ti1 O7 C22 -167.6(7) . . . . ?
O4 Ti1 O7 C22 -67.1(7) . . . . ?
O9 Ti1 O7 C22 96.7(7) . . . . ?
O3 Ti1 O7 C22 21.8(11) . . . . ?
O6 Ti1 O7 C22 15.7(7) . . . . ?
Ti2 Ti1 O7 C22 78.5(7) . . . . ?
O7 Ti1 O8 C25 2.4(5) . . . . ?
O4 Ti1 O8 C25 -102.0(5) . . . . ?
O9 Ti1 O8 C25 107.4(5) . . . . ?
O3 Ti1 O8 C25 -180.0(5) . . . . ?
Ti2 Ti1 O8 C25 142.1(5) . . . . ?
O11 Ti2 O10 C31 178.6(5) . . . . ?
O9 Ti2 O10 C31 71.6(5) . . . . ?
O3 Ti2 O10 C31 -3.0(5) . . . . ?
O1 Ti2 O10 C31 -84.2(5) . . . . ?
Ti1 Ti2 O10 C31 34.9(5) . . . . ?
O10 Ti2 O11 C34 167.3(5) . . . . ?
O9 Ti2 O11 C34 -92.1(5) . . . . ?
O3 Ti2 O11 C34 -5.3(10) . . . . ?
O1 Ti2 O11 C34 73.3(5) . . . . ?
O5 Ti2 O11 C34 -6.7(5) . . . . ?
Ti1 Ti2 O11 C34 -73.9(6) . . . . ?
Ti2 O3 C2 C1 25.3(6) . . . . ?
Ti1 O3 C2 C1 161.2(4) . . . . ?
Ti2 O3 C2 C3 -153.2(3) . . . . ?
Ti1 O3 C2 C3 -17.4(4) . . . . ?
C6 C1 C2 O3 173.8(4) . . . . ?
C13 C1 C2 O3 -6.4(7) . . . . ?
C6 C1 C2 C3 -7.8(7) . . . . ?
C13 C1 C2 C3 172.0(4) . . . . ?
Ti1 O4 C3 C4 -170.9(4) . . . . ?
Ti1 O4 C3 C2 8.8(5) . . . . ?
O3 C2 C3 O4 6.3(6) . . . . ?
C1 C2 C3 O4 -172.2(4) . . . . ?
O3 C2 C3 C4 -173.9(4) . . . . ?
C1 C2 C3 C4 7.5(7) . . . . ?
O4 C3 C4 C5 177.4(4) . . . . ?
C2 C3 C4 C5 -2.4(7) . . . . ?
C3 C4 C5 C6 -2.2(7) . . . . ?
C4 C5 C6 C1 2.0(7) . . . . ?
C4 C5 C6 C14 179.9(4) . . . . ?
C2 C1 C6 C5 2.9(6) . . . . ?
C13 C1 C6 C5 -176.9(4) . . . . ?
C2 C1 C6 C14 -175.0(4) . . . . ?
C13 C1 C6 C14 5.1(7) . . . . ?
C12 C7 C8 C9 0.4(8) . . . . ?
C13 C7 C8 C9 -179.0(5) . . . . ?
C7 C8 C9 C10 -0.2(8) . . . . ?
C8 C9 C10 C11 -0.1(9) . . . . ?
C9 C10 C11 C12 0.1(9) . . . . ?
C10 C11 C12 C7 0.1(8) . . . . ?
C10 C11 C12 C14 179.3(5) . . . . ?
C8 C7 C12 C11 -0.3(7) . . . . ?
C13 C7 C12 C11 179.1(4) . . . . ?
C8 C7 C12 C14 -179.6(5) . . . . ?
C13 C7 C12 C14 -0.2(7) . . . . ?
Ti2 O1 C13 C1 -7.0(7) . . . . ?
Ti2 O1 C13 C7 170.3(3) . . . . ?
C2 C1 C13 O1 -2.8(7) . . . . ?
C6 C1 C13 O1 177.0(4) . . . . ?
C2 C1 C13 C7 180.0(4) . . . . ?
C6 C1 C13 C7 -0.2(6) . . . . ?
C8 C7 C13 O1 -0.3(7) . . . . ?
C12 C7 C13 O1 -179.6(4) . . . . ?
C8 C7 C13 C1 177.1(4) . . . . ?
C12 C7 C13 C1 -2.3(7) . . . . ?
C5 C6 C14 O2 -6.0(7) . . . . ?
C1 C6 C14 O2 172.0(4) . . . . ?
C5 C6 C14 C12 174.6(4) . . . . ?
C1 C6 C14 C12 -7.4(7) . . . . ?
C11 C12 C14 O2 6.3(7) . . . . ?
C7 C12 C14 O2 -174.4(5) . . . . ?
C11 C12 C14 C6 -174.3(5) . . . . ?
C7 C12 C14 C6 5.0(7) . . . . ?
C20 C15 C16 C17 1.3(7) . . . . ?
C21 C15 C16 C17 -178.1(4) . . . . ?
C15 C16 C17 C18 1.2(7) . . . . ?
C16 C17 C18 C19 -3.3(7) . . . . ?
C16 C17 C18 Br1 176.5(4) . . . . ?
C17 C18 C19 C20 2.8(7) . . . . ?
Br1 C18 C19 C20 -177.0(4) . . . . ?
C16 C15 C20 C19 -1.8(7) . . . . ?
C21 C15 C20 C19 177.6(4) . . . . ?
C18 C19 C20 C15 -0.2(7) . . . . ?
Ti1 O6 C21 O5 -2.0(7) . . . . ?
Ti1 O6 C21 C15 178.3(3) . . . . ?
Ti2 O5 C21 O6 -3.2(6) . . . . ?
Ti2 O5 C21 C15 176.4(3) . . . . ?
C20 C15 C21 O6 6.4(6) . . . . ?
C16 C15 C21 O6 -174.2(4) . . . . ?
C20 C15 C21 O5 -173.3(4) . . . . ?
C16 C15 C21 O5 6.1(6) . . . . ?
Ti1 O7 C22 C23 99.2(8) . . . . ?
Ti1 O7 C22 C24 -139.7(6) . . . . ?
Ti1 O8 C25 C27 -126.3(6) . . . . ?
Ti1 O8 C25 C26 104.0(6) . . . . ?
Ti2 O9 C28 C29 81.8(5) . . . . ?
Ti1 O9 C28 C29 -96.9(4) . . . . ?
Ti2 O9 C28 C30 -43.0(6) . . . . ?
Ti1 O9 C28 C30 138.2(3) . . . . ?
Ti2 O10 C31 C32 105.9(5) . . . . ?
Ti2 O10 C31 C33 -131.1(4) . . . . ?
Ti2 O11 C34 C36 152.9(4) . . . . ?
Ti2 O11 C34 C35 -83.5(7) . . . . ?

_refine_diff_density_max         0.934
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.126
####################################################################### 
# 
# 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 1551803'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-08-01 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            'C36 H45 N O13 Ti2'
_chemical_formula_weight         795.53

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                   9.6859(3)
_cell_length_b                   21.7550(6)
_cell_length_c                   19.0222(5)
_cell_angle_alpha                90
_cell_angle_beta                 93.686(3)
_cell_angle_gamma                90
_cell_volume                     4000.0(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9866
_cell_measurement_theta_min      2.8
_cell_measurement_theta_max      27.5

_exptl_crystal_description       Prism
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             1664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.460
_shelx_estimated_absorpt_T_min   0.855
_shelx_estimated_absorpt_T_max   0.955
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5451
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication '
_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  'Xcalibur, Atlas, Gemini'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31104
_diffrn_reflns_av_unetI/netI     0.0516
_diffrn_reflns_av_R_equivalents  0.0421
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         2.819
_diffrn_reflns_theta_max         30.277
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.885
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.885
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.885
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             10589
_reflns_number_gt                6508
_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)+(0.0200P)²+6.0000P] 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         10589
_refine_ls_number_parameters     479
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.1144
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.1442
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.10273(6) 0.57035(3) 0.19878(3) 0.04146(15) Uani 1 1 d . . . . .
Ti2 Ti 0.02331(7) 0.62483(3) 0.35019(3) 0.04861(17) Uani 1 1 d . . . . .
O1 O -0.0249(2) 0.50132(9) 0.15315(10) 0.0415(5) Uani 1 1 d . . . . .
O2 O -0.4532(3) 0.36291(13) 0.22821(14) 0.0711(8) Uani 1 1 d . . . . .
O3 O -0.0582(2) 0.57488(9) 0.26328(10) 0.0400(5) Uani 1 1 d . . . . .
O4 O -0.1457(2) 0.58692(10) 0.38521(11) 0.0507(6) Uani 1 1 d . . . . .
O5 O 0.1126(2) 0.53357(10) 0.37309(11) 0.0486(5) Uani 1 1 d . . . . .
O6 O 0.1614(2) 0.49781(10) 0.26654(11) 0.0445(5) Uani 1 1 d . . . . .
O7 O 0.4128(4) 0.27228(15) 0.52104(17) 0.0990(11) Uani 1 1 d . . . . .
O8 O 0.4743(4) 0.24536(15) 0.42003(17) 0.0897(10) Uani 1 1 d . . . . .
O9 O 0.0213(2) 0.62444(10) 0.13903(11) 0.0507(6) Uani 1 1 d . . . . .
O10 O 0.2516(2) 0.55328(10) 0.15254(11) 0.0493(5) Uani 1 1 d . . . . .
O11 O 0.1671(2) 0.62598(10) 0.27669(12) 0.0505(6) Uani 1 1 d . . . . .
O12 O -0.0486(3) 0.69724(11) 0.32547(13) 0.0645(7) Uani 1 1 d . . . . .
O13 O 0.1097(3) 0.64577(12) 0.43194(13) 0.0636(7) Uani 1 1 d . . . . .
N1 N 0.4158(3) 0.27998(15) 0.45792(18) 0.0635(8) Uani 1 1 d . . . . .
C1 C -0.1975(3) 0.48576(13) 0.23508(14) 0.0355(6) Uani 1 1 d . . . . .
C2 C -0.1531(3) 0.53355(14) 0.27867(15) 0.0382(7) Uani 1 1 d . . . . .
C3 C -0.2066(3) 0.54319(15) 0.34602(15) 0.0435(7) Uani 1 1 d . . . . .
C4 C -0.3146(4) 0.50655(17) 0.36469(17) 0.0532(9) Uani 1 1 d . . . . .
H4 H -0.354640 0.513172 0.407168 0.064 Uiso 1 1 calc R U . . .
C5 C -0.3634(3) 0.45976(17) 0.32005(17) 0.0511(8) Uani 1 1 d . . . . .
H5 H -0.436514 0.435606 0.333400 0.061 Uiso 1 1 calc R U . . .
C6 C -0.3070(3) 0.44783(15) 0.25624(15) 0.0415(7) Uani 1 1 d . . . . .
C7 C -0.1930(3) 0.42726(13) 0.12127(14) 0.0361(6) Uani 1 1 d . . . . .
C8 C -0.1419(3) 0.41964(15) 0.05469(16) 0.0456(7) Uani 1 1 d . . . . .
H8 H -0.068801 0.443870 0.041460 0.055 Uiso 1 1 calc R U . . .
C9 C -0.1992(4) 0.37644(17) 0.00868(17) 0.0568(9) Uani 1 1 d . . . . .
H9 H -0.166172 0.372161 -0.035891 0.068 Uiso 1 1 calc R U . . .
C10 C -0.3057(4) 0.33950(18) 0.02861(19) 0.0608(10) Uani 1 1 d . . . . .
H10 H -0.343594 0.310094 -0.002445 0.073 Uiso 1 1 calc R U . . .
C11 C -0.3564(4) 0.34596(16) 0.09447(18) 0.0524(8) Uani 1 1 d . . . . .
H11 H -0.427706 0.320665 0.107602 0.063 Uiso 1 1 calc R U . . .
C12 C -0.3015(3) 0.38990(14) 0.14110(15) 0.0401(7) Uani 1 1 d . . . . .
C13 C -0.1319(3) 0.47364(13) 0.16984(14) 0.0348(6) Uani 1 1 d . . . . .
C14 C -0.3618(3) 0.39739(15) 0.21106(17) 0.0464(8) Uani 1 1 d . . . . .
C15 C 0.2232(3) 0.43697(14) 0.36627(16) 0.0415(7) Uani 1 1 d . . . . .
C16 C 0.2218(4) 0.42722(17) 0.43851(17) 0.0587(9) Uani 1 1 d . . . . .
H16 H 0.179186 0.455610 0.466590 0.070 Uiso 1 1 calc R U . . .
C17 C 0.2835(4) 0.37534(18) 0.46868(18) 0.0626(10) Uani 1 1 d . . . . .
H17 H 0.281837 0.368206 0.516821 0.075 Uiso 1 1 calc R U . . .
C18 C 0.3471(3) 0.33477(15) 0.42628(17) 0.0466(8) Uani 1 1 d . . . . .
C19 C 0.3499(3) 0.34292(15) 0.35486(17) 0.0474(8) Uani 1 1 d . . . . .
H19 H 0.393484 0.314537 0.327209 0.057 Uiso 1 1 calc R U . . .
C20 C 0.2863(3) 0.39429(15) 0.32509(17) 0.0444(7) Uani 1 1 d . . . . .
H20 H 0.285809 0.400273 0.276667 0.053 Uiso 1 1 calc R U . . .
C21 C 0.1602(3) 0.49421(15) 0.33333(16) 0.0426(7) Uani 1 1 d . . . . .
C22 C -0.1064(6) 0.6557(3) 0.1256(3) 0.1015(18) Uani 1 1 d . U . . .
H22 H -0.161574 0.651932 0.166757 0.122 Uiso 1 1 calc R U . . .
C23 C -0.1831(6) 0.6293(3) 0.0643(4) 0.156(3) Uani 1 1 d . U . . .
H23A H -0.171493 0.585473 0.064603 0.235 Uiso 1 1 calc R U . . .
H23B H -0.148717 0.645959 0.022074 0.235 Uiso 1 1 calc R U . . .
H23C H -0.279466 0.639076 0.065917 0.235 Uiso 1 1 calc R U . . .
C24 C -0.0760(10) 0.7190(3) 0.1144(6) 0.263(6) Uani 1 1 d . U . . .
H24A H 0.009310 0.729529 0.140086 0.394 Uiso 1 1 calc R U . . .
H24B H -0.149380 0.743926 0.130580 0.394 Uiso 1 1 calc R U . . .
H24C H -0.067492 0.726159 0.065087 0.394 Uiso 1 1 calc R U . . .
C25 C 0.3601(4) 0.51013(18) 0.1438(2) 0.0596(9) Uani 1 1 d . . . . .
H25 H 0.393518 0.494882 0.190261 0.072 Uiso 1 1 calc R U . . .
C26 C 0.3036(5) 0.4573(2) 0.1010(3) 0.0908(15) Uani 1 1 d . . . . .
H26A H 0.228554 0.438981 0.124052 0.136 Uiso 1 1 calc R U . . .
H26B H 0.375160 0.427369 0.096203 0.136 Uiso 1 1 calc R U . . .
H26C H 0.270809 0.471676 0.055202 0.136 Uiso 1 1 calc R U . . .
C27 C 0.4781(4) 0.5425(2) 0.1105(3) 0.0935(16) Uani 1 1 d . . . . .
H27A H 0.446483 0.557896 0.064973 0.140 Uiso 1 1 calc R U . . .
H27B H 0.552615 0.514115 0.105547 0.140 Uiso 1 1 calc R U . . .
H27C H 0.509873 0.576171 0.139969 0.140 Uiso 1 1 calc R U . . .
C28 C 0.2872(5) 0.6666(2) 0.2839(2) 0.0799(13) Uani 1 1 d . . . . .
H28 H 0.275552 0.692753 0.325018 0.096 Uiso 1 1 calc R U . . .
C29 C 0.2918(7) 0.7074(3) 0.2225(3) 0.133(2) Uani 1 1 d . . . . .
H29A H 0.303431 0.683203 0.181019 0.200 Uiso 1 1 calc R U . . .
H29B H 0.368034 0.735366 0.229559 0.200 Uiso 1 1 calc R U . . .
H29C H 0.206968 0.730146 0.216681 0.200 Uiso 1 1 calc R U . . .
C30 C 0.4146(5) 0.6281(3) 0.3002(3) 0.125(2) Uani 1 1 d . . . . .
H30A H 0.402882 0.604084 0.341696 0.187 Uiso 1 1 calc R U . . .
H30B H 0.493505 0.654502 0.307966 0.187 Uiso 1 1 calc R U . . .
H30C H 0.428467 0.601253 0.261217 0.187 Uiso 1 1 calc R U . . .
C31 C -0.1004(7) 0.7539(3) 0.3502(4) 0.121(2) Uani 1 1 d . . . . .
H31 H -0.082693 0.756271 0.401479 0.145 Uiso 1 1 calc R U . . .
C32 C -0.2530(7) 0.7567(4) 0.3324(5) 0.195(4) Uani 1 1 d . . . . .
H32A H -0.270466 0.755772 0.282113 0.292 Uiso 1 1 calc R U . . .
H32B H -0.289515 0.794092 0.350609 0.292 Uiso 1 1 calc R U . . .
H32C H -0.297029 0.722143 0.352871 0.292 Uiso 1 1 calc R U . . .
C33 C -0.0307(7) 0.8041(3) 0.3176(6) 0.216(5) Uani 1 1 d . . . . .
H33A H 0.066980 0.801266 0.329388 0.324 Uiso 1 1 calc R U . . .
H33B H -0.064875 0.842429 0.334381 0.324 Uiso 1 1 calc R U . . .
H33C H -0.047828 0.801807 0.267422 0.324 Uiso 1 1 calc R U . . .
C34 C 0.1733(6) 0.6233(3) 0.4973(2) 0.1009(17) Uani 1 1 d . U . . .
H34 H 0.136846 0.581800 0.503678 0.121 Uiso 1 1 calc R U . . .
C35 C 0.1330(11) 0.6578(6) 0.5535(4) 0.264(6) Uani 1 1 d . U . . .
H35A H 0.209323 0.682478 0.571758 0.395 Uiso 1 1 calc R U . . .
H35B H 0.104316 0.630872 0.589801 0.395 Uiso 1 1 calc R U . . .
H35C H 0.057361 0.684061 0.538042 0.395 Uiso 1 1 calc R U . . .
C36 C 0.3201(7) 0.6167(4) 0.4918(4) 0.184(4) Uani 1 1 d . U . . .
H36A H 0.336909 0.589178 0.453797 0.276 Uiso 1 1 calc R U . . .
H36B H 0.361365 0.600324 0.535065 0.276 Uiso 1 1 calc R U . . .
H36C H 0.359923 0.656088 0.482825 0.276 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 O10 1.776(2) . ?
Ti1 O9 1.784(2) . ?
Ti1 O11 1.983(2) . ?
Ti1 O3 2.047(2) . ?
Ti1 O6 2.093(2) . ?
Ti1 O1 2.097(2) . ?
Ti1 Ti2 3.2523(8) . ?
Ti2 O12 1.774(2) . ?
Ti2 O13 1.777(2) . ?
Ti2 O4 1.986(2) . ?
Ti2 O11 2.036(2) . ?
Ti2 O3 2.090(2) . ?
Ti2 O5 2.198(2) . ?
O1 C13 1.258(3) . ?
O2 C14 1.221(4) . ?
O3 C2 1.332(3) . ?
O4 C3 1.323(4) . ?
O5 C21 1.250(4) . ?
O6 C21 1.274(3) . ?
O7 N1 1.214(4) . ?
O8 N1 1.208(4) . ?
O9 C22 1.420(5) . ?
O10 C25 1.427(4) . ?
O11 C28 1.460(4) . ?
O12 C31 1.423(6) . ?
O13 C34 1.437(5) . ?
N1 C18 1.474(4) . ?
C1 C2 1.381(4) . ?
C1 C6 1.422(4) . ?
C1 C13 1.454(4) . ?
C2 C3 1.428(4) . ?
C3 C4 1.379(5) . ?
C4 C5 1.389(5) . ?
C5 C6 1.388(4) . ?
C6 C14 1.472(4) . ?
C7 C8 1.399(4) . ?
C7 C12 1.400(4) . ?
C7 C13 1.467(4) . ?
C8 C9 1.377(4) . ?
C9 C10 1.380(5) . ?
C10 C11 1.382(5) . ?
C11 C12 1.387(4) . ?
C12 C14 1.496(4) . ?
C15 C20 1.382(4) . ?
C15 C16 1.391(4) . ?
C15 C21 1.505(4) . ?
C16 C17 1.385(5) . ?
C17 C18 1.369(5) . ?
C18 C19 1.372(4) . ?
C19 C20 1.380(4) . ?
C22 C24 1.426(10) . ?
C22 C23 1.460(7) . ?
C25 C26 1.491(6) . ?
C25 C27 1.515(5) . ?
C28 C29 1.471(7) . ?
C28 C30 1.506(7) . ?
C31 C33 1.444(9) . ?
C31 C32 1.497(9) . ?
C34 C35 1.384(9) . ?
C34 C36 1.439(8) . ?

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
O10 Ti1 O9 99.34(10) . . ?
O10 Ti1 O11 105.75(10) . . ?
O9 Ti1 O11 100.28(10) . . ?
O10 Ti1 O3 168.71(10) . . ?
O9 Ti1 O3 91.58(9) . . ?
O11 Ti1 O3 74.78(9) . . ?
O10 Ti1 O6 87.15(9) . . ?
O9 Ti1 O6 168.81(10) . . ?
O11 Ti1 O6 86.56(9) . . ?
O3 Ti1 O6 81.62(8) . . ?
O10 Ti1 O1 96.95(9) . . ?
O9 Ti1 O1 89.08(10) . . ?
O11 Ti1 O1 153.52(9) . . ?
O3 Ti1 O1 80.29(8) . . ?
O6 Ti1 O1 81.05(8) . . ?
O10 Ti1 Ti2 139.51(8) . . ?
O9 Ti1 Ti2 101.76(8) . . ?
O11 Ti1 Ti2 36.53(7) . . ?
O3 Ti1 Ti2 38.65(6) . . ?
O6 Ti1 Ti2 78.44(6) . . ?
O1 Ti1 Ti2 117.44(6) . . ?
O12 Ti2 O13 99.15(12) . . ?
O12 Ti2 O4 98.02(12) . . ?
O13 Ti2 O4 99.49(11) . . ?
O12 Ti2 O11 94.66(11) . . ?
O13 Ti2 O11 107.07(11) . . ?
O4 Ti2 O11 148.26(9) . . ?
O12 Ti2 O3 97.48(10) . . ?
O13 Ti2 O3 163.32(11) . . ?
O4 Ti2 O3 76.81(8) . . ?
O11 Ti2 O3 72.75(8) . . ?
O12 Ti2 O5 176.06(10) . . ?
O13 Ti2 O5 84.32(10) . . ?
O4 Ti2 O5 83.16(9) . . ?
O11 Ti2 O5 82.49(9) . . ?
O3 Ti2 O5 79.10(8) . . ?
O12 Ti2 Ti1 101.54(9) . . ?
O13 Ti2 Ti1 138.03(9) . . ?
O4 Ti2 Ti1 113.12(6) . . ?
O11 Ti2 Ti1 35.43(6) . . ?
O3 Ti2 Ti1 37.71(6) . . ?
O5 Ti2 Ti1 74.56(6) . . ?
C13 O1 Ti1 135.40(19) . . ?
C2 O3 Ti1 131.47(18) . . ?
C2 O3 Ti2 114.08(17) . . ?
Ti1 O3 Ti2 103.63(9) . . ?
C3 O4 Ti2 117.16(19) . . ?
C21 O5 Ti2 130.9(2) . . ?
C21 O6 Ti1 129.9(2) . . ?
C22 O9 Ti1 140.8(3) . . ?
C25 O10 Ti1 145.4(2) . . ?
C28 O11 Ti1 130.5(2) . . ?
C28 O11 Ti2 121.3(2) . . ?
Ti1 O11 Ti2 108.04(10) . . ?
C31 O12 Ti2 145.4(3) . . ?
C34 O13 Ti2 145.2(3) . . ?
O8 N1 O7 123.1(3) . . ?
O8 N1 C18 118.5(3) . . ?
O7 N1 C18 118.5(3) . . ?
C2 C1 C6 118.4(3) . . ?
C2 C1 C13 120.9(3) . . ?
C6 C1 C13 120.7(3) . . ?
O3 C2 C1 124.7(3) . . ?
O3 C2 C3 113.2(3) . . ?
C1 C2 C3 122.2(3) . . ?
O4 C3 C4 126.0(3) . . ?
O4 C3 C2 115.9(3) . . ?
C4 C3 C2 118.1(3) . . ?
C3 C4 C5 120.0(3) . . ?
C6 C5 C4 122.3(3) . . ?
C5 C6 C1 118.8(3) . . ?
C5 C6 C14 120.2(3) . . ?
C1 C6 C14 121.0(3) . . ?
C8 C7 C12 119.4(3) . . ?
C8 C7 C13 120.0(3) . . ?
C12 C7 C13 120.6(3) . . ?
C9 C8 C7 120.3(3) . . ?
C8 C9 C10 120.1(3) . . ?
C9 C10 C11 120.3(3) . . ?
C10 C11 C12 120.4(3) . . ?
C11 C12 C7 119.4(3) . . ?
C11 C12 C14 119.3(3) . . ?
C7 C12 C14 121.3(3) . . ?
O1 C13 C1 122.8(3) . . ?
O1 C13 C7 118.4(2) . . ?
C1 C13 C7 118.8(3) . . ?
O2 C14 C6 122.9(3) . . ?
O2 C14 C12 120.1(3) . . ?
C6 C14 C12 117.0(3) . . ?
C20 C15 C16 119.4(3) . . ?
C20 C15 C21 120.1(3) . . ?
C16 C15 C21 120.5(3) . . ?
C17 C16 C15 120.1(3) . . ?
C18 C17 C16 118.7(3) . . ?
C17 C18 C19 122.6(3) . . ?
C17 C18 N1 119.3(3) . . ?
C19 C18 N1 118.1(3) . . ?
C18 C19 C20 118.3(3) . . ?
C19 C20 C15 120.9(3) . . ?
O5 C21 O6 126.0(3) . . ?
O5 C21 C15 118.1(3) . . ?
O6 C21 C15 115.9(3) . . ?
C24 C22 O9 107.7(6) . . ?
C24 C22 C23 111.1(6) . . ?
O9 C22 C23 110.3(4) . . ?
O10 C25 C26 108.9(3) . . ?
O10 C25 C27 108.9(3) . . ?
C26 C25 C27 113.0(4) . . ?
O11 C28 C29 110.8(4) . . ?
O11 C28 C30 108.7(4) . . ?
C29 C28 C30 115.6(5) . . ?
O12 C31 C33 109.1(6) . . ?
O12 C31 C32 108.9(6) . . ?
C33 C31 C32 110.7(6) . . ?
C35 C34 C36 116.1(7) . . ?
C35 C34 O13 110.9(6) . . ?
C36 C34 O13 110.0(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O10 Ti1 O9 C22 168.3(5) . . . . ?
O11 Ti1 O9 C22 -83.7(5) . . . . ?
O3 Ti1 O9 C22 -8.9(5) . . . . ?
O6 Ti1 O9 C22 43.4(8) . . . . ?
O1 Ti1 O9 C22 71.4(5) . . . . ?
Ti2 Ti1 O9 C22 -46.5(5) . . . . ?
O9 Ti1 O10 C25 -159.4(4) . . . . ?
O11 Ti1 O10 C25 97.1(4) . . . . ?
O3 Ti1 O10 C25 5.9(8) . . . . ?
O6 Ti1 O10 C25 11.4(4) . . . . ?
O1 Ti1 O10 C25 -69.2(4) . . . . ?
Ti2 Ti1 O10 C25 79.9(4) . . . . ?
O13 Ti2 O12 C31 -29.9(6) . . . . ?
O4 Ti2 O12 C31 71.1(6) . . . . ?
O11 Ti2 O12 C31 -138.0(6) . . . . ?
O3 Ti2 O12 C31 148.8(6) . . . . ?
Ti1 Ti2 O12 C31 -173.2(6) . . . . ?
O12 Ti2 O13 C34 163.5(5) . . . . ?
O4 Ti2 O13 C34 63.7(5) . . . . ?
O11 Ti2 O13 C34 -98.7(5) . . . . ?
O3 Ti2 O13 C34 -11.9(8) . . . . ?
O5 Ti2 O13 C34 -18.4(5) . . . . ?
Ti1 Ti2 O13 C34 -77.7(6) . . . . ?
Ti1 O3 C2 C1 -26.2(4) . . . . ?
Ti2 O3 C2 C1 -163.8(2) . . . . ?
Ti1 O3 C2 C3 153.9(2) . . . . ?
Ti2 O3 C2 C3 16.2(3) . . . . ?
C6 C1 C2 O3 -175.4(3) . . . . ?
C13 C1 C2 O3 5.9(4) . . . . ?
C6 C1 C2 C3 4.6(4) . . . . ?
C13 C1 C2 C3 -174.1(3) . . . . ?
Ti2 O4 C3 C4 172.1(3) . . . . ?
Ti2 O4 C3 C2 -7.4(4) . . . . ?
O3 C2 C3 O4 -6.3(4) . . . . ?
C1 C2 C3 O4 173.7(3) . . . . ?
O3 C2 C3 C4 174.2(3) . . . . ?
C1 C2 C3 C4 -5.8(5) . . . . ?
O4 C3 C4 C5 -176.2(3) . . . . ?
C2 C3 C4 C5 3.3(5) . . . . ?
C3 C4 C5 C6 0.2(5) . . . . ?
C4 C5 C6 C1 -1.5(5) . . . . ?
C4 C5 C6 C14 179.5(3) . . . . ?
C2 C1 C6 C5 -0.9(4) . . . . ?
C13 C1 C6 C5 177.8(3) . . . . ?
C2 C1 C6 C14 178.1(3) . . . . ?
C13 C1 C6 C14 -3.2(4) . . . . ?
C12 C7 C8 C9 1.0(5) . . . . ?
C13 C7 C8 C9 -179.6(3) . . . . ?
C7 C8 C9 C10 -1.4(5) . . . . ?
C8 C9 C10 C11 0.6(6) . . . . ?
C9 C10 C11 C12 0.5(6) . . . . ?
C10 C11 C12 C7 -0.8(5) . . . . ?
C10 C11 C12 C14 177.8(3) . . . . ?
C8 C7 C12 C11 0.1(4) . . . . ?
C13 C7 C12 C11 -179.3(3) . . . . ?
C8 C7 C12 C14 -178.5(3) . . . . ?
C13 C7 C12 C14 2.1(4) . . . . ?
Ti1 O1 C13 C1 -0.9(4) . . . . ?
Ti1 O1 C13 C7 179.09(19) . . . . ?
C2 C1 C13 O1 7.2(4) . . . . ?
C6 C1 C13 O1 -171.5(3) . . . . ?
C2 C1 C13 C7 -172.8(3) . . . . ?
C6 C1 C13 C7 8.6(4) . . . . ?
C8 C7 C13 O1 -7.3(4) . . . . ?
C12 C7 C13 O1 172.1(3) . . . . ?
C8 C7 C13 C1 172.6(3) . . . . ?
C12 C7 C13 C1 -8.0(4) . . . . ?
C5 C6 C14 O2 -3.0(5) . . . . ?
C1 C6 C14 O2 178.1(3) . . . . ?
C5 C6 C14 C12 176.3(3) . . . . ?
C1 C6 C14 C12 -2.6(4) . . . . ?
C11 C12 C14 O2 3.9(5) . . . . ?
C7 C12 C14 O2 -177.5(3) . . . . ?
C11 C12 C14 C6 -175.4(3) . . . . ?
C7 C12 C14 C6 3.2(4) . . . . ?
C20 C15 C16 C17 0.3(5) . . . . ?
C21 C15 C16 C17 -178.1(3) . . . . ?
C15 C16 C17 C18 0.9(6) . . . . ?
C16 C17 C18 C19 -1.2(6) . . . . ?
C16 C17 C18 N1 178.8(3) . . . . ?
O8 N1 C18 C17 -178.3(4) . . . . ?
O7 N1 C18 C17 0.5(5) . . . . ?
O8 N1 C18 C19 1.7(5) . . . . ?
O7 N1 C18 C19 -179.5(4) . . . . ?
C17 C18 C19 C20 0.3(5) . . . . ?
N1 C18 C19 C20 -179.7(3) . . . . ?
C18 C19 C20 C15 1.0(5) . . . . ?
C16 C15 C20 C19 -1.3(5) . . . . ?
C21 C15 C20 C19 177.1(3) . . . . ?
Ti2 O5 C21 O6 -3.6(5) . . . . ?
Ti2 O5 C21 C15 176.08(19) . . . . ?
Ti1 O6 C21 O5 5.5(5) . . . . ?
Ti1 O6 C21 C15 -174.13(19) . . . . ?
C20 C15 C21 O5 -175.2(3) . . . . ?
C16 C15 C21 O5 3.2(5) . . . . ?
C20 C15 C21 O6 4.4(4) . . . . ?
C16 C15 C21 O6 -177.2(3) . . . . ?
Ti1 O9 C22 C24 132.8(6) . . . . ?
Ti1 O9 C22 C23 -105.8(5) . . . . ?
Ti1 O10 C25 C26 77.5(5) . . . . ?
Ti1 O10 C25 C27 -158.9(3) . . . . ?
Ti1 O11 C28 C29 52.5(6) . . . . ?
Ti2 O11 C28 C29 -122.2(4) . . . . ?
Ti1 O11 C28 C30 -75.5(5) . . . . ?
Ti2 O11 C28 C30 109.7(4) . . . . ?
Ti2 O12 C31 C33 127.7(6) . . . . ?
Ti2 O12 C31 C32 -111.3(6) . . . . ?
Ti2 O13 C34 C35 -135.8(7) . . . . ?
Ti2 O13 C34 C36 94.4(7) . . . . ?

_refine_diff_density_max         1.201
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.065
####################################################################### 
# 
# 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 1547751'
_audit_update_record             
;
2017-05-23 deposited with the CCDC.
2017-08-01 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            'C36 H45 F O11 Ti2'
_chemical_formula_weight         768.52

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'
F F 0.0171 0.0103 '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                   9.6424(13)
_cell_length_b                   21.475(3)
_cell_length_c                   18.640(2)
_cell_angle_alpha                90
_cell_angle_beta                 96.606(4)
_cell_angle_gamma                90
_cell_volume                     3834.2(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9919
_cell_measurement_theta_min      2.19
_cell_measurement_theta_max      26.88

_exptl_crystal_description       Prism
_exptl_crystal_colour            Purple
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_F_000             1608
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.300
_exptl_absorpt_coefficient_mu    0.477
_shelx_estimated_absorpt_T_min   0.796
_shelx_estimated_absorpt_T_max   0.870
_exptl_absorpt_correction_type   'multi scan'
_exptl_absorpt_correction_T_min  0.574
_exptl_absorpt_correction_T_max  1.000
_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            20324
_diffrn_reflns_av_unetI/netI     0.1459
_diffrn_reflns_av_R_equivalents  0.1266
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.193
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_full        24.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             6748
_reflns_number_gt                3688
_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)+(0.0010P)²+12.0000P] 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         6748
_refine_ls_number_parameters     468
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.0902
_refine_ls_wR_factor_ref         0.1731
_refine_ls_wR_factor_gt          0.1451
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.47981(12) 0.37967(5) 0.15578(6) 0.0384(3) Uani 1 1 d . . . . .
Ti2 Ti 0.41181(11) 0.43665(5) 0.30888(6) 0.0323(3) Uani 1 1 d . . . . .
F1 F 0.0949(4) 0.72070(17) 0.0292(2) 0.0596(12) Uani 1 1 d . . . . .
O1 O 0.5444(4) 0.50701(18) 0.3556(2) 0.0316(10) Uani 1 1 d . . . . .
O2 O 0.9621(5) 0.6487(2) 0.2752(3) 0.0621(15) Uani 1 1 d . . . . .
O3 O 0.5688(4) 0.43130(18) 0.2442(2) 0.0311(10) Uani 1 1 d . . . . .
O4 O 0.6478(4) 0.4169(2) 0.1210(2) 0.0420(12) Uani 1 1 d . . . . .
O5 O 0.3456(4) 0.50894(18) 0.2375(2) 0.0336(10) Uani 1 1 d . . . . .
O6 O 0.3878(4) 0.47027(19) 0.1303(2) 0.0396(11) Uani 1 1 d . . . . .
O7 O 0.3412(4) 0.37932(19) 0.2297(2) 0.0400(11) Uani 1 1 d . . . . .
O8 O 0.5527(5) 0.3063(2) 0.1830(3) 0.0535(13) Uani 1 1 d . . . . .
O9 O 0.3891(5) 0.3566(2) 0.0715(2) 0.0506(13) Uani 1 1 d . . . . .
O10 O 0.4949(4) 0.38050(19) 0.3700(2) 0.0408(11) Uani 1 1 d . . . . .
O11 O 0.2663(4) 0.45511(18) 0.3554(2) 0.0367(11) Uani 1 1 d . . . . .
C1 C 0.7090(6) 0.5230(3) 0.2717(3) 0.0270(14) Uani 1 1 d . . . . .
C2 C 0.6613(6) 0.4733(3) 0.2278(3) 0.0306(15) Uani 1 1 d . . . . .
C3 C 0.7105(6) 0.4624(3) 0.1598(3) 0.0345(16) Uani 1 1 d . . . . .
C4 C 0.8180(7) 0.4992(3) 0.1399(3) 0.0419(17) Uani 1 1 d . . . . .
H4 H 0.855743 0.491484 0.097012 0.050 Uiso 1 1 calc R U . . .
C5 C 0.8684(7) 0.5476(3) 0.1849(4) 0.0417(17) Uani 1 1 d . . . . .
H5 H 0.939996 0.572250 0.170944 0.050 Uiso 1 1 calc R U . . .
C6 C 0.8172(6) 0.5609(3) 0.2493(3) 0.0332(15) Uani 1 1 d . . . . .
C7 C 0.7115(6) 0.5840(3) 0.3861(3) 0.0252(14) Uani 1 1 d . . . . .
C8 C 0.6667(6) 0.5933(3) 0.4531(3) 0.0337(15) Uani 1 1 d . . . . .
H8 H 0.595358 0.568534 0.467139 0.040 Uiso 1 1 calc R U . . .
C9 C 0.7254(7) 0.6382(3) 0.4995(4) 0.0436(18) Uani 1 1 d . . . . .
H9 H 0.694540 0.643766 0.544486 0.052 Uiso 1 1 calc R U . . .
C10 C 0.8312(7) 0.6751(3) 0.4782(4) 0.0479(18) Uani 1 1 d . . . . .
H10 H 0.871989 0.705318 0.509536 0.057 Uiso 1 1 calc R U . . .
C11 C 0.8773(7) 0.6677(3) 0.4111(4) 0.0453(18) Uani 1 1 d . . . . .
H11 H 0.946842 0.693491 0.397146 0.054 Uiso 1 1 calc R U . . .
C12 C 0.8198(6) 0.6219(3) 0.3648(3) 0.0343(15) Uani 1 1 d . . . . .
C13 C 0.6494(6) 0.5356(3) 0.3375(3) 0.0266(14) Uani 1 1 d . . . . .
C14 C 0.8733(6) 0.6132(3) 0.2938(4) 0.0386(16) Uani 1 1 d . . . . .
C15 C 0.2775(6) 0.5678(3) 0.1325(3) 0.0311(14) Uani 1 1 d . . . . .
C16 C 0.2149(6) 0.6123(3) 0.1708(4) 0.0376(16) Uani 1 1 d . . . . .
H16 H 0.215035 0.607783 0.220435 0.045 Uiso 1 1 calc R U . . .
C17 C 0.1513(7) 0.6640(3) 0.1361(4) 0.0422(17) Uani 1 1 d . . . . .
H17 H 0.106549 0.693728 0.161542 0.051 Uiso 1 1 calc R U . . .
C18 C 0.1569(7) 0.6697(3) 0.0639(4) 0.0396(17) Uani 1 1 d . . . . .
C19 C 0.2178(8) 0.6279(3) 0.0233(4) 0.055(2) Uani 1 1 d . . . . .
H19 H 0.218499 0.633480 -0.026134 0.066 Uiso 1 1 calc R U . . .
C20 C 0.2795(7) 0.5759(3) 0.0588(4) 0.0473(18) Uani 1 1 d . . . . .
H20 H 0.322587 0.546173 0.032569 0.057 Uiso 1 1 calc R U . . .
C21 C 0.3430(6) 0.5114(3) 0.1693(4) 0.0325(15) Uani 1 1 d . . . . .
C22 C 0.2208(8) 0.3374(4) 0.2217(5) 0.063(2) Uani 1 1 d . . . . .
H22 H 0.229130 0.310537 0.179873 0.076 Uiso 1 1 calc R U . . .
C23 C 0.2189(11) 0.2969(4) 0.2860(5) 0.110(4) Uani 1 1 d . . . . .
H23A H 0.308711 0.277731 0.297340 0.164 Uiso 1 1 calc R U . . .
H23B H 0.149124 0.265153 0.276078 0.164 Uiso 1 1 calc R U . . .
H23C H 0.197510 0.321472 0.326339 0.164 Uiso 1 1 calc R U . . .
C24 C 0.0897(8) 0.3764(5) 0.2052(6) 0.106(4) Uani 1 1 d . . . . .
H24A H 0.076109 0.401407 0.246517 0.159 Uiso 1 1 calc R U . . .
H24B H 0.010681 0.349526 0.193938 0.159 Uiso 1 1 calc R U . . .
H24C H 0.099398 0.403046 0.164677 0.159 Uiso 1 1 calc R U . . .
C25 C 0.5900(11) 0.2472(4) 0.1561(6) 0.092(3) Uani 1 1 d . . . . .
H25 H 0.546662 0.244593 0.106002 0.110 Uiso 1 1 calc R U . . .
C26 C 0.5287(10) 0.1981(4) 0.1959(7) 0.118(4) Uani 1 1 d . . . . .
H26A H 0.568828 0.199034 0.245481 0.177 Uiso 1 1 calc R U . . .
H26B H 0.547077 0.158457 0.175173 0.177 Uiso 1 1 calc R U . . .
H26C H 0.429667 0.204381 0.193362 0.177 Uiso 1 1 calc R U . . .
C27 C 0.7428(10) 0.2436(5) 0.1541(7) 0.122(4) Uani 1 1 d . . . . .
H27A H 0.770117 0.272781 0.119393 0.184 Uiso 1 1 calc R U . . .
H27B H 0.767471 0.202216 0.140731 0.184 Uiso 1 1 calc R U . . .
H27C H 0.789821 0.253333 0.200994 0.184 Uiso 1 1 calc R U . . .
C28 C 0.3236(9) 0.3795(4) 0.0038(4) 0.068(2) Uani 1 1 d . . . . .
H28 H 0.359590 0.421318 -0.004180 0.081 Uiso 1 1 calc R U . . .
C29 C 0.3557(13) 0.3393(5) -0.0547(5) 0.137(5) Uani 1 1 d . . . . .
H29A H 0.454718 0.332562 -0.051095 0.205 Uiso 1 1 calc R U . . .
H29B H 0.324812 0.358733 -0.100155 0.205 Uiso 1 1 calc R U . . .
H29C H 0.308947 0.300134 -0.051613 0.205 Uiso 1 1 calc R U . . .
C30 C 0.1698(9) 0.3838(6) 0.0074(5) 0.117(4) Uani 1 1 d . . . . .
H30A H 0.132753 0.342851 0.013335 0.176 Uiso 1 1 calc R U . . .
H30B H 0.125483 0.401864 -0.036462 0.176 Uiso 1 1 calc R U . . .
H30C H 0.152452 0.409368 0.047644 0.176 Uiso 1 1 calc R U . . .
C31 C 0.6047(9) 0.3357(4) 0.3826(5) 0.080(3) Uani 1 1 d . . . . .
C32 C 0.6027(19) 0.3118(10) 0.4626(9) 0.097(6) Uani 0.6 1 d . U P . .
C32' C 0.560(2) 0.2814(9) 0.4095(17) 0.081(8) Uani 0.4 1 d . . P . .
C33 C 0.7404(10) 0.3622(5) 0.3841(8) 0.140(5) Uani 1 1 d . . . . .
C34 C 0.1589(7) 0.5001(3) 0.3619(4) 0.0479(19) Uani 1 1 d . . . . .
H34 H 0.124442 0.515303 0.313508 0.057 Uiso 1 1 calc R U . . .
C35 C 0.2204(9) 0.5535(4) 0.4058(5) 0.086(3) Uani 1 1 d . . . . .
H35A H 0.249935 0.539622 0.454072 0.129 Uiso 1 1 calc R U . . .
H35B H 0.151525 0.585631 0.406909 0.129 Uiso 1 1 calc R U . . .
H35C H 0.299205 0.569503 0.384568 0.129 Uiso 1 1 calc R U . . .
C36 C 0.0408(7) 0.4693(4) 0.3939(5) 0.071(3) Uani 1 1 d . . . . .
H36A H 0.001418 0.437221 0.361930 0.106 Uiso 1 1 calc R U . . .
H36B H -0.029610 0.499647 0.400659 0.106 Uiso 1 1 calc R U . . .
H36C H 0.074967 0.451245 0.439681 0.106 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 O8 1.775(4) . ?
Ti1 O9 1.778(4) . ?
Ti1 O4 1.982(4) . ?
Ti1 O7 2.026(4) . ?
Ti1 O3 2.088(4) . ?
Ti1 O6 2.168(4) . ?
Ti1 Ti2 3.2406(16) . ?
Ti2 O11 1.778(4) . ?
Ti2 O10 1.784(4) . ?
Ti2 O7 1.982(4) . ?
Ti2 O3 2.044(4) . ?
Ti2 O5 2.096(4) . ?
Ti2 O1 2.102(4) . ?
F1 C18 1.374(7) . ?
O1 C13 1.263(6) . ?
O2 C14 1.226(7) . ?
O3 C2 1.329(6) . ?
O4 C3 1.321(7) . ?
O5 C21 1.270(7) . ?
O6 C21 1.252(7) . ?
O7 C22 1.463(8) . ?
O8 C25 1.426(9) . ?
O9 C28 1.432(8) . ?
O10 C31 1.430(8) . ?
O11 C34 1.431(7) . ?
C1 C2 1.390(8) . ?
C1 C6 1.422(8) . ?
C1 C13 1.439(8) . ?
C2 C3 1.425(8) . ?
C3 C4 1.386(8) . ?
C4 C5 1.389(9) . ?
C4 H4 0.9300 . ?
C5 C6 1.380(8) . ?
C5 H5 0.9300 . ?
C6 C14 1.463(9) . ?
C7 C8 1.382(8) . ?
C7 C12 1.417(8) . ?
C7 C13 1.461(8) . ?
C8 C9 1.372(8) . ?
C8 H8 0.9300 . ?
C9 C10 1.385(9) . ?
C9 H9 0.9300 . ?
C10 C11 1.384(9) . ?
C10 H10 0.9300 . ?
C11 C12 1.381(8) . ?
C11 H11 0.9300 . ?
C12 C14 1.486(8) . ?
C15 C16 1.374(8) . ?
C15 C20 1.387(8) . ?
C15 C21 1.496(8) . ?
C16 C17 1.392(8) . ?
C16 H16 0.9300 . ?
C17 C18 1.359(9) . ?
C17 H17 0.9300 . ?
C18 C19 1.351(9) . ?
C19 C20 1.395(9) . ?
C19 H19 0.9300 . ?
C20 H20 0.9300 . ?
C22 C23 1.485(11) . ?
C22 C24 1.518(11) . ?
C22 H22 0.9800 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.454(12) . ?
C25 C27 1.480(12) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.452(11) . ?
C28 C30 1.495(11) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32' 1.36(2) . ?
C31 C32 1.579(17) . ?
C31 C33 1.424(12) . ?
C32 C32' 1.22(3) . ?
C34 C35 1.491(10) . ?
C34 C36 1.500(9) . ?
C34 H34 0.9800 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?

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
O8 Ti1 O9 98.3(2) . . ?
O8 Ti1 O4 98.0(2) . . ?
O9 Ti1 O4 99.3(2) . . ?
O8 Ti1 O7 94.2(2) . . ?
O9 Ti1 O7 107.7(2) . . ?
O4 Ti1 O7 148.44(17) . . ?
O8 Ti1 O3 97.59(18) . . ?
O9 Ti1 O3 164.02(19) . . ?
O4 Ti1 O3 76.54(16) . . ?
O7 Ti1 O3 73.05(16) . . ?
O8 Ti1 O6 176.0(2) . . ?
O9 Ti1 O6 84.79(18) . . ?
O4 Ti1 O6 84.00(17) . . ?
O7 Ti1 O6 82.37(17) . . ?
O3 Ti1 O6 79.46(15) . . ?
O8 Ti1 Ti2 101.34(16) . . ?
O9 Ti1 Ti2 138.96(16) . . ?
O4 Ti1 Ti2 113.08(13) . . ?
O7 Ti1 Ti2 35.59(12) . . ?
O3 Ti1 Ti2 37.85(11) . . ?
O6 Ti1 Ti2 74.64(12) . . ?
O11 Ti2 O10 99.28(19) . . ?
O11 Ti2 O7 106.23(18) . . ?
O10 Ti2 O7 98.40(18) . . ?
O11 Ti2 O3 168.61(18) . . ?
O10 Ti2 O3 91.68(17) . . ?
O7 Ti2 O3 74.92(16) . . ?
O11 Ti2 O5 86.83(17) . . ?
O10 Ti2 O5 170.93(18) . . ?
O7 Ti2 O5 86.20(17) . . ?
O3 Ti2 O5 81.93(15) . . ?
O11 Ti2 O1 96.56(17) . . ?
O10 Ti2 O1 90.83(18) . . ?
O7 Ti2 O1 153.55(16) . . ?
O3 Ti2 O1 80.11(15) . . ?
O5 Ti2 O1 81.77(16) . . ?
O11 Ti2 Ti1 139.92(14) . . ?
O10 Ti2 Ti1 100.67(14) . . ?
O7 Ti2 Ti1 36.51(12) . . ?
O3 Ti2 Ti1 38.82(11) . . ?
O5 Ti2 Ti1 78.37(11) . . ?
O1 Ti2 Ti1 117.46(11) . . ?
C13 O1 Ti2 135.0(4) . . ?
C2 O3 Ti2 131.3(4) . . ?
C2 O3 Ti1 113.9(4) . . ?
Ti2 O3 Ti1 103.33(17) . . ?
C3 O4 Ti1 117.3(4) . . ?
C21 O5 Ti2 129.4(4) . . ?
C21 O6 Ti1 131.7(4) . . ?
C22 O7 Ti2 131.2(4) . . ?
C22 O7 Ti1 120.7(4) . . ?
Ti2 O7 Ti1 107.90(19) . . ?
C25 O8 Ti1 142.8(6) . . ?
C28 O9 Ti1 143.6(4) . . ?
C31 O10 Ti2 146.1(5) . . ?
C34 O11 Ti2 144.2(4) . . ?
C2 C1 C6 118.1(5) . . ?
C2 C1 C13 120.5(5) . . ?
C6 C1 C13 121.4(5) . . ?
O3 C2 C1 124.9(5) . . ?
O3 C2 C3 113.2(5) . . ?
C1 C2 C3 121.9(5) . . ?
O4 C3 C4 125.7(6) . . ?
O4 C3 C2 115.6(6) . . ?
C4 C3 C2 118.7(6) . . ?
C5 C4 C3 119.0(6) . . ?
C5 C4 H4 120.5 . . ?
C3 C4 H4 120.5 . . ?
C6 C5 C4 123.0(6) . . ?
C6 C5 H5 118.5 . . ?
C4 C5 H5 118.5 . . ?
C5 C6 C1 119.0(6) . . ?
C5 C6 C14 120.4(6) . . ?
C1 C6 C14 120.6(5) . . ?
C8 C7 C12 119.2(5) . . ?
C8 C7 C13 121.0(5) . . ?
C12 C7 C13 119.8(5) . . ?
C9 C8 C7 121.4(6) . . ?
C9 C8 H8 119.3 . . ?
C7 C8 H8 119.3 . . ?
C8 C9 C10 119.1(6) . . ?
C8 C9 H9 120.5 . . ?
C10 C9 H9 120.5 . . ?
C9 C10 C11 121.1(6) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 119.9(6) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C7 119.3(6) . . ?
C11 C12 C14 119.3(6) . . ?
C7 C12 C14 121.4(6) . . ?
O1 C13 C1 123.2(5) . . ?
O1 C13 C7 117.7(5) . . ?
C1 C13 C7 119.1(5) . . ?
O2 C14 C6 122.8(6) . . ?
O2 C14 C12 120.0(6) . . ?
C6 C14 C12 117.2(5) . . ?
C16 C15 C20 119.0(6) . . ?
C16 C15 C21 120.8(6) . . ?
C20 C15 C21 120.2(6) . . ?
C15 C16 C17 120.7(6) . . ?
C15 C16 H16 119.7 . . ?
C17 C16 H16 119.7 . . ?
C18 C17 C16 117.8(6) . . ?
C18 C17 H17 121.1 . . ?
C16 C17 H17 121.1 . . ?
C19 C18 C17 124.4(6) . . ?
C19 C18 F1 117.4(6) . . ?
C17 C18 F1 118.2(6) . . ?
C18 C19 C20 117.1(7) . . ?
C18 C19 H19 121.5 . . ?
C20 C19 H19 121.5 . . ?
C15 C20 C19 121.1(6) . . ?
C15 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
O6 C21 O5 125.8(6) . . ?
O6 C21 C15 117.4(6) . . ?
O5 C21 C15 116.8(6) . . ?
O7 C22 C23 111.2(7) . . ?
O7 C22 C24 108.3(6) . . ?
C23 C22 C24 113.5(8) . . ?
O7 C22 H22 107.9 . . ?
C23 C22 H22 107.9 . . ?
C24 C22 H22 107.9 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O8 C25 C26 109.4(8) . . ?
O8 C25 C27 110.4(8) . . ?
C26 C25 C27 116.0(9) . . ?
O8 C25 H25 106.9 . . ?
C26 C25 H25 106.9 . . ?
C27 C25 H25 106.9 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O9 C28 C29 110.3(7) . . ?
O9 C28 C30 108.7(7) . . ?
C29 C28 C30 111.6(8) . . ?
O9 C28 H28 108.7 . . ?
C29 C28 H28 108.7 . . ?
C30 C28 H28 108.7 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C28 C30 H30A 109.5 . . ?
C28 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C28 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32' C31 C32 48.3(12) . . ?
C32' C31 C33 131.9(12) . . ?
C32 C31 C33 102.8(11) . . ?
C32' C31 O10 112.0(11) . . ?
C32 C31 O10 106.5(8) . . ?
C33 C31 O10 113.2(8) . . ?
C32' C32 C31 56.4(12) . . ?
C32 C32' C31 75.3(15) . . ?
O11 C34 C35 108.6(6) . . ?
O11 C34 C36 109.0(5) . . ?
C35 C34 C36 113.1(7) . . ?
O11 C34 H34 108.7 . . ?
C35 C34 H34 108.7 . . ?
C36 C34 H34 108.7 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O9 Ti1 O8 C25 21.9(9) . . . . ?
O4 Ti1 O8 C25 -78.7(9) . . . . ?
O7 Ti1 O8 C25 130.4(9) . . . . ?
O3 Ti1 O8 C25 -156.1(9) . . . . ?
Ti2 Ti1 O8 C25 165.7(9) . . . . ?
O8 Ti1 O9 C28 -162.9(8) . . . . ?
O4 Ti1 O9 C28 -63.3(8) . . . . ?
O7 Ti1 O9 C28 100.0(8) . . . . ?
O3 Ti1 O9 C28 9.9(13) . . . . ?
O6 Ti1 O9 C28 19.7(8) . . . . ?
Ti2 Ti1 O9 C28 79.0(9) . . . . ?
O11 Ti2 O10 C31 173.2(9) . . . . ?
O7 Ti2 O10 C31 65.1(9) . . . . ?
O3 Ti2 O10 C31 -9.9(9) . . . . ?
O1 Ti2 O10 C31 -90.0(9) . . . . ?
Ti1 Ti2 O10 C31 28.1(9) . . . . ?
O10 Ti2 O11 C34 161.7(7) . . . . ?
O7 Ti2 O11 C34 -96.7(7) . . . . ?
O3 Ti2 O11 C34 -2.5(14) . . . . ?
O5 Ti2 O11 C34 -11.6(7) . . . . ?
O1 Ti2 O11 C34 69.7(7) . . . . ?
Ti1 Ti2 O11 C34 -79.3(7) . . . . ?
Ti2 O3 C2 C1 27.0(8) . . . . ?
Ti1 O3 C2 C1 163.4(5) . . . . ?
Ti2 O3 C2 C3 -153.8(4) . . . . ?
Ti1 O3 C2 C3 -17.4(6) . . . . ?
C6 C1 C2 O3 174.6(5) . . . . ?
C13 C1 C2 O3 -5.8(9) . . . . ?
C6 C1 C2 C3 -4.5(9) . . . . ?
C13 C1 C2 C3 175.1(5) . . . . ?
Ti1 O4 C3 C4 -171.6(5) . . . . ?
Ti1 O4 C3 C2 8.7(7) . . . . ?
O3 C2 C3 O4 6.4(7) . . . . ?
C1 C2 C3 O4 -174.4(5) . . . . ?
O3 C2 C3 C4 -173.3(5) . . . . ?
C1 C2 C3 C4 5.9(9) . . . . ?
O4 C3 C4 C5 176.6(6) . . . . ?
C2 C3 C4 C5 -3.8(9) . . . . ?
C3 C4 C5 C6 0.5(10) . . . . ?
C4 C5 C6 C1 0.9(10) . . . . ?
C4 C5 C6 C14 -179.0(6) . . . . ?
C2 C1 C6 C5 1.1(9) . . . . ?
C13 C1 C6 C5 -178.5(6) . . . . ?
C2 C1 C6 C14 -179.0(6) . . . . ?
C13 C1 C6 C14 1.4(9) . . . . ?
C12 C7 C8 C9 -0.3(9) . . . . ?
C13 C7 C8 C9 179.4(6) . . . . ?
C7 C8 C9 C10 0.3(10) . . . . ?
C8 C9 C10 C11 0.6(10) . . . . ?
C9 C10 C11 C12 -1.6(11) . . . . ?
C10 C11 C12 C7 1.6(10) . . . . ?
C10 C11 C12 C14 -178.2(6) . . . . ?
C8 C7 C12 C11 -0.7(9) . . . . ?
C13 C7 C12 C11 179.7(6) . . . . ?
C8 C7 C12 C14 179.1(6) . . . . ?
C13 C7 C12 C14 -0.6(8) . . . . ?
Ti2 O1 C13 C1 -1.1(8) . . . . ?
Ti2 O1 C13 C7 178.6(4) . . . . ?
C2 C1 C13 O1 -6.8(9) . . . . ?
C6 C1 C13 O1 172.8(5) . . . . ?
C2 C1 C13 C7 173.6(5) . . . . ?
C6 C1 C13 C7 -6.8(8) . . . . ?
C8 C7 C13 O1 7.0(8) . . . . ?
C12 C7 C13 O1 -173.3(5) . . . . ?
C8 C7 C13 C1 -173.3(5) . . . . ?
C12 C7 C13 C1 6.3(8) . . . . ?
C5 C6 C14 O2 3.1(10) . . . . ?
C1 C6 C14 O2 -176.8(6) . . . . ?
C5 C6 C14 C12 -175.9(6) . . . . ?
C1 C6 C14 C12 4.3(9) . . . . ?
C11 C12 C14 O2 -3.9(9) . . . . ?
C7 C12 C14 O2 176.3(6) . . . . ?
C11 C12 C14 C6 175.1(6) . . . . ?
C7 C12 C14 C6 -4.7(9) . . . . ?
C20 C15 C16 C17 1.5(9) . . . . ?
C21 C15 C16 C17 -178.6(6) . . . . ?
C15 C16 C17 C18 -1.8(9) . . . . ?
C16 C17 C18 C19 1.3(11) . . . . ?
C16 C17 C18 F1 -179.8(5) . . . . ?
C17 C18 C19 C20 -0.5(11) . . . . ?
F1 C18 C19 C20 -179.5(6) . . . . ?
C16 C15 C20 C19 -0.7(10) . . . . ?
C21 C15 C20 C19 179.4(6) . . . . ?
C18 C19 C20 C15 0.2(11) . . . . ?
Ti1 O6 C21 O5 2.0(9) . . . . ?
Ti1 O6 C21 C15 -176.4(4) . . . . ?
Ti2 O5 C21 O6 -3.8(9) . . . . ?
Ti2 O5 C21 C15 174.7(4) . . . . ?
C16 C15 C21 O6 174.2(5) . . . . ?
C20 C15 C21 O6 -5.9(9) . . . . ?
C16 C15 C21 O5 -4.4(8) . . . . ?
C20 C15 C21 O5 175.5(6) . . . . ?
Ti2 O7 C22 C23 -51.0(9) . . . . ?
Ti1 O7 C22 C23 123.1(7) . . . . ?
Ti2 O7 C22 C24 74.4(8) . . . . ?
Ti1 O7 C22 C24 -111.5(6) . . . . ?
Ti1 O8 C25 C26 -128.4(8) . . . . ?
Ti1 O8 C25 C27 102.8(10) . . . . ?
Ti1 O9 C28 C29 139.6(8) . . . . ?
Ti1 O9 C28 C30 -97.7(10) . . . . ?
Ti2 O10 C31 C32' -134.7(15) . . . . ?
Ti2 O10 C31 C32 174.2(10) . . . . ?
Ti2 O10 C31 C33 62.0(14) . . . . ?
C33 C31 C32 C32' -135.6(17) . . . . ?
O10 C31 C32 C32' 105.1(16) . . . . ?
C33 C31 C32' C32 66(2) . . . . ?
O10 C31 C32' C32 -92.9(15) . . . . ?
Ti2 O11 C34 C35 -79.0(9) . . . . ?
Ti2 O11 C34 C36 157.3(6) . . . . ?

_refine_diff_density_max         0.888
_refine_diff_density_min         -0.349
_refine_diff_density_rms         0.080
