# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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 2057320'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.169 0.731 -0.014 50 5 ' '
2 0.169 0.769 0.486 50 5 ' '
3 0.500 0.500 0.500 96 22 ' '
4 0.500 1.000 1.000 96 22 ' '
5 0.830 0.269 0.014 50 5 ' '
6 0.830 0.231 0.514 50 5 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Two sensible pockets each capable of containing 22e.  CH3CN is 22e electrons. 
As Z = 4 this equates to 0.5 MeCN per Ti2 complex. 
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C76 H99 N O10 Ti2, 3(C2 H3 N) [+ 0.5 MeCN]
;
_chemical_formula_sum            'C82 H108 N4 O10 Ti2'
_chemical_formula_weight         1405.52

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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                   12.0347(2)
_cell_length_b                   28.3198(4)
_cell_length_c                   24.5367(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.2370(10)
_cell_angle_gamma                90
_cell_volume                     8140.4(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    30751
_cell_measurement_theta_min      3.177
_cell_measurement_theta_max      70.028

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.147
_exptl_crystal_F_000             3008
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    2.112
_shelx_estimated_absorpt_T_min   0.677
_shelx_estimated_absorpt_T_max   0.920
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.69725
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            75678
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         2.420
_diffrn_reflns_theta_max         66.600
_diffrn_reflns_theta_full        66.600
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             14383
_reflns_number_gt                12259
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.2000P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         14383
_refine_ls_number_parameters     870
_refine_ls_number_restraints     58
_refine_ls_R_factor_all          0.1260
_refine_ls_R_factor_gt           0.1169
_refine_ls_wR_factor_ref         0.3681
_refine_ls_wR_factor_gt          0.3558
_refine_ls_goodness_of_fit_ref   1.675
_refine_ls_restrained_S_all      1.677
_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
C1 C 0.2912(3) 0.41421(16) 0.56057(17) 0.0420(9) Uani 1 1 d . . . . .
C2 C 0.1846(4) 0.43215(16) 0.53295(18) 0.0432(9) Uani 1 1 d . . . . .
C3 C 0.1555(4) 0.43107(16) 0.47531(18) 0.0465(10) Uani 1 1 d . . . . .
H3 H 0.082983 0.443118 0.456771 0.056 Uiso 1 1 calc R U . . .
C4 C 0.2267(4) 0.41323(17) 0.44273(18) 0.0448(9) Uani 1 1 d . . . . .
C5 C 0.3310(4) 0.39381(15) 0.47124(17) 0.0417(9) Uani 1 1 d . . . . .
H5 H 0.380492 0.380285 0.450425 0.050 Uiso 1 1 calc R U . . .
C6 C 0.3635(3) 0.39394(15) 0.52971(16) 0.0392(9) Uani 1 1 d . . . . .
C7 C 0.1886(4) 0.41544(19) 0.37904(18) 0.0510(11) Uani 1 1 d . . . . .
C8 C 0.1662(5) 0.4676(2) 0.3612(2) 0.0609(12) Uani 1 1 d . . . . .
H8A H 0.236271 0.485959 0.374247 0.091 Uiso 1 1 calc R U . . .
H8B H 0.142498 0.469482 0.320267 0.091 Uiso 1 1 calc R U . . .
H8C H 0.105718 0.480390 0.377675 0.091 Uiso 1 1 calc R U . . .
C9 C 0.2802(5) 0.3961(2) 0.3501(2) 0.0636(14) Uani 1 1 d . . . . .
H9A H 0.351407 0.413724 0.363110 0.095 Uiso 1 1 calc R U . . .
H9B H 0.293474 0.362601 0.359317 0.095 Uiso 1 1 calc R U . . .
H9C H 0.253885 0.399701 0.309449 0.095 Uiso 1 1 calc R U . . .
C10 C 0.0788(5) 0.3877(2) 0.3583(2) 0.0641(13) Uani 1 1 d . . . . .
H10A H 0.055918 0.389567 0.317392 0.096 Uiso 1 1 calc R U . . .
H10B H 0.091406 0.354580 0.369712 0.096 Uiso 1 1 calc R U . . .
H10C H 0.018425 0.401007 0.374493 0.096 Uiso 1 1 calc R U . . .
C11 C 0.4717(3) 0.37034(15) 0.56028(17) 0.0417(9) Uani 1 1 d . . . . .
H11A H 0.521922 0.363899 0.534343 0.050 Uiso 1 1 calc R U . . .
H11B H 0.513292 0.390827 0.590917 0.050 Uiso 1 1 calc R U . . .
C12 C 0.5229(3) 0.30872(15) 0.62829(17) 0.0408(9) Uani 1 1 d . . . . .
H12A H 0.558656 0.334533 0.653485 0.049 Uiso 1 1 calc R U . . .
H12B H 0.583236 0.291872 0.614595 0.049 Uiso 1 1 calc R U . . .
C13 C 0.3845(3) 0.29387(16) 0.68862(17) 0.0425(9) Uani 1 1 d . . . . .
C14 C 0.4607(3) 0.27504(15) 0.65889(17) 0.0416(9) Uani 1 1 d . . . . .
C15 C 0.4720(4) 0.22675(16) 0.65416(18) 0.0449(9) Uani 1 1 d . . . . .
H15 H 0.523741 0.214634 0.633645 0.054 Uiso 1 1 calc R U . . .
C16 C 0.4081(4) 0.19511(16) 0.67926(19) 0.0471(10) Uani 1 1 d . . . . .
C17 C 0.3292(3) 0.21539(17) 0.70657(18) 0.0463(10) Uani 1 1 d . . . . .
H17 H 0.282686 0.194875 0.722428 0.056 Uiso 1 1 calc R U . . .
C18 C 0.3155(3) 0.26360(16) 0.71170(17) 0.0424(9) Uani 1 1 d . . . . .
C19 C 0.4243(5) 0.14191(18) 0.6797(3) 0.0636(13) Uani 1 1 d . . . . .
C20 C 0.3084(6) 0.1179(2) 0.6658(6) 0.132(4) Uani 1 1 d . . . . .
H20A H 0.318865 0.083547 0.666087 0.198 Uiso 1 1 calc R U . . .
H20B H 0.265466 0.126634 0.693717 0.198 Uiso 1 1 calc R U . . .
H20C H 0.266159 0.127925 0.628591 0.198 Uiso 1 1 calc R U . . .
C21 C 0.4942(4) 0.12572(17) 0.6379(2) 0.0537(11) Uani 1 1 d . . . . .
H21A H 0.569030 0.141176 0.646776 0.081 Uiso 1 1 calc R U . . .
H21B H 0.504426 0.091391 0.640415 0.081 Uiso 1 1 calc R U . . .
H21C H 0.453659 0.134265 0.599817 0.081 Uiso 1 1 calc R U . . .
C22 C 0.4907(8) 0.1279(3) 0.7399(3) 0.101(2) Uani 1 1 d . . . . .
H22A H 0.565236 0.143575 0.748426 0.151 Uiso 1 1 calc R U . . .
H22B H 0.446935 0.137721 0.767046 0.151 Uiso 1 1 calc R U . . .
H22C H 0.501517 0.093592 0.741861 0.151 Uiso 1 1 calc R U . . .
C23 C 0.2269(4) 0.28283(16) 0.74074(18) 0.0450(9) Uani 1 1 d . . . . .
H23A H 0.179004 0.256426 0.748645 0.054 Uiso 1 1 calc R U . . .
H23B H 0.176672 0.305047 0.715229 0.054 Uiso 1 1 calc R U . . .
C24 C 0.2851(3) 0.35735(16) 0.79909(18) 0.0440(9) Uani 1 1 d . . . . .
C25 C 0.2788(4) 0.30808(16) 0.79507(18) 0.0463(10) Uani 1 1 d . . . . .
C26 C 0.3235(4) 0.28122(18) 0.84304(19) 0.0492(10) Uani 1 1 d . . . . .
H26 H 0.319994 0.247769 0.840336 0.059 Uiso 1 1 calc R U . . .
C27 C 0.3728(4) 0.30155(18) 0.8943(2) 0.0556(11) Uani 1 1 d . . . . .
C28 C 0.3804(4) 0.35023(17) 0.89621(19) 0.0509(11) Uani 1 1 d . . . . .
H28 H 0.417035 0.364885 0.930449 0.061 Uiso 1 1 calc R U . . .
C29 C 0.3367(4) 0.37868(16) 0.85004(18) 0.0458(10) Uani 1 1 d . . . . .
C30 C 0.4184(5) 0.2697(2) 0.9462(2) 0.0683(14) Uani 1 1 d D . . . .
C31A C 0.4984(10) 0.2324(4) 0.9312(5) 0.0754(9) Uiso 0.540(6) 1 d D U P A 1
H31A H 0.460733 0.216801 0.896167 0.113 Uiso 0.540(6) 1 calc R U P A 1
H31B H 0.568706 0.247655 0.926411 0.113 Uiso 0.540(6) 1 calc R U P A 1
H31C H 0.516946 0.208988 0.961236 0.113 Uiso 0.540(6) 1 calc R U P A 1
C32A C 0.3108(9) 0.2394(4) 0.9537(5) 0.0754(9) Uiso 0.540(6) 1 d D U P A 1
H32A H 0.278163 0.222630 0.918779 0.113 Uiso 0.540(6) 1 calc R U P A 1
H32B H 0.335142 0.216531 0.984037 0.113 Uiso 0.540(6) 1 calc R U P A 1
H32C H 0.253181 0.260532 0.962855 0.113 Uiso 0.540(6) 1 calc R U P A 1
C33A C 0.4671(10) 0.2946(4) 0.9973(5) 0.0754(9) Uiso 0.540(6) 1 d D U P A 1
H33A H 0.412208 0.317870 1.004736 0.113 Uiso 0.540(6) 1 calc R U P A 1
H33B H 0.485275 0.272042 1.028407 0.113 Uiso 0.540(6) 1 calc R U P A 1
H33C H 0.537035 0.310709 0.993582 0.113 Uiso 0.540(6) 1 calc R U P A 1
C31B C 0.3921(12) 0.2202(4) 0.9405(6) 0.0754(9) Uiso 0.460(6) 1 d D U P A 2
H31D H 0.421243 0.207170 0.909439 0.113 Uiso 0.460(6) 1 calc R U P A 2
H31E H 0.427942 0.203799 0.975218 0.113 Uiso 0.460(6) 1 calc R U P A 2
H31F H 0.309186 0.215833 0.932792 0.113 Uiso 0.460(6) 1 calc R U P A 2
C32B C 0.3743(12) 0.2922(5) 0.9947(6) 0.0754(9) Uiso 0.460(6) 1 d D U P A 2
H32D H 0.393757 0.325876 0.997353 0.113 Uiso 0.460(6) 1 calc R U P A 2
H32E H 0.291283 0.288535 0.987510 0.113 Uiso 0.460(6) 1 calc R U P A 2
H32F H 0.410039 0.276501 1.029936 0.113 Uiso 0.460(6) 1 calc R U P A 2
C33B C 0.5513(9) 0.2777(4) 0.9626(6) 0.0754(9) Uiso 0.460(6) 1 d D U P A 2
H33D H 0.567527 0.311573 0.966377 0.113 Uiso 0.460(6) 1 calc R U P A 2
H33E H 0.583367 0.261912 0.998345 0.113 Uiso 0.460(6) 1 calc R U P A 2
H33F H 0.585727 0.264464 0.933464 0.113 Uiso 0.460(6) 1 calc R U P A 2
C34 C 0.3486(4) 0.43165(16) 0.85574(19) 0.0481(10) Uani 1 1 d . . . . .
H34A H 0.343249 0.445360 0.818114 0.058 Uiso 1 1 calc R U . . .
H34B H 0.425525 0.439015 0.878744 0.058 Uiso 1 1 calc R U . . .
C35 C 0.1434(4) 0.44754(16) 0.86141(18) 0.0458(9) Uani 1 1 d . . . . .
C36 C 0.2599(4) 0.45556(16) 0.88208(18) 0.0451(9) Uani 1 1 d . . . . .
C37 C 0.2942(4) 0.48987(16) 0.92394(18) 0.0496(10) Uani 1 1 d . . . . .
H37 H 0.373443 0.495792 0.937568 0.060 Uiso 1 1 calc R U . . .
C38 C 0.2159(4) 0.51556(18) 0.94622(19) 0.0537(11) Uani 1 1 d . . . . .
C39 C 0.1005(4) 0.50574(18) 0.92563(18) 0.0517(11) Uani 1 1 d . . . . .
H39 H 0.045897 0.522615 0.940448 0.062 Uiso 1 1 calc R U . . .
C40 C 0.0622(4) 0.47219(17) 0.88425(18) 0.0479(10) Uani 1 1 d . . . . .
C41 C 0.2579(5) 0.5539(2) 0.9912(2) 0.0668(14) Uani 1 1 d . . . . .
C42 C 0.3465(9) 0.5842(3) 0.9740(4) 0.126(3) Uani 1 1 d . . . . .
H42A H 0.312862 0.599880 0.938481 0.190 Uiso 1 1 calc R U . . .
H42B H 0.373821 0.608031 1.002932 0.190 Uiso 1 1 calc R U . . .
H42C H 0.410606 0.564421 0.969487 0.190 Uiso 1 1 calc R U . . .
C43 C 0.3101(7) 0.5296(3) 1.0463(3) 0.098(2) Uani 1 1 d . . . . .
H43A H 0.252251 0.509779 1.057448 0.146 Uiso 1 1 calc R U . . .
H43B H 0.374168 0.509795 1.041719 0.146 Uiso 1 1 calc R U . . .
H43C H 0.337384 0.553405 1.075163 0.146 Uiso 1 1 calc R U . . .
C44 C 0.1579(7) 0.5845(3) 0.9993(3) 0.0870(19) Uani 1 1 d . . . . .
H44A H 0.100480 0.564472 1.010458 0.130 Uiso 1 1 calc R U . . .
H44B H 0.185634 0.608041 1.028515 0.130 Uiso 1 1 calc R U . . .
H44C H 0.123508 0.600580 0.964093 0.130 Uiso 1 1 calc R U . . .
C45 C -0.0632(4) 0.46390(18) 0.8627(2) 0.0524(11) Uani 1 1 d . . . . .
H45A H -0.074936 0.444474 0.828267 0.063 Uiso 1 1 calc R U . . .
H45B H -0.092422 0.445786 0.890926 0.063 Uiso 1 1 calc R U . . .
C46 C -0.1279(4) 0.52547(18) 0.79627(19) 0.0502(10) Uani 1 1 d . . . . .
H46A H -0.195378 0.546186 0.784484 0.060 Uiso 1 1 calc R U . . .
H46B H -0.136080 0.499076 0.769186 0.060 Uiso 1 1 calc R U . . .
C47 C 0.0664(3) 0.53317(17) 0.77314(17) 0.0447(9) Uani 1 1 d . . . . .
C48 C -0.0216(4) 0.55350(17) 0.79351(18) 0.0465(10) Uani 1 1 d . . . . .
C49 C -0.0096(4) 0.60021(18) 0.8119(2) 0.0538(11) Uani 1 1 d . . . . .
H49 H -0.069091 0.614060 0.826074 0.065 Uiso 1 1 calc R U . . .
C50 C 0.0849(4) 0.62711(18) 0.8103(2) 0.0536(11) Uani 1 1 d . . . . .
C51 C 0.1734(4) 0.60466(18) 0.7919(2) 0.0509(11) Uani 1 1 d . . . . .
H51 H 0.240663 0.622046 0.791472 0.061 Uiso 1 1 calc R U . . .
C52 C 0.1665(4) 0.55836(17) 0.77438(18) 0.0461(10) Uani 1 1 d . . . . .
C53 C 0.0903(5) 0.6807(2) 0.8212(3) 0.0726(16) Uani 1 1 d . . . . .
C54 C 0.2098(6) 0.6978(3) 0.8470(5) 0.114(3) Uani 1 1 d . . . . .
H54A H 0.261749 0.687468 0.823879 0.171 Uiso 1 1 calc R U . . .
H54B H 0.210071 0.732327 0.849131 0.171 Uiso 1 1 calc R U . . .
H54C H 0.235024 0.684597 0.884753 0.171 Uiso 1 1 calc R U . . .
C55 C 0.0077(5) 0.6960(2) 0.8560(3) 0.0772(17) Uani 1 1 d . . . . .
H55A H -0.069045 0.684611 0.838523 0.116 Uiso 1 1 calc R U . . .
H55B H 0.031888 0.682851 0.893762 0.116 Uiso 1 1 calc R U . . .
H55C H 0.006935 0.730581 0.858140 0.116 Uiso 1 1 calc R U . . .
C56 C 0.0508(8) 0.7061(3) 0.7625(4) 0.096(2) Uani 1 1 d . . . . .
H56A H -0.026641 0.695843 0.744415 0.145 Uiso 1 1 calc R U . . .
H56B H 0.051489 0.740374 0.768047 0.145 Uiso 1 1 calc R U . . .
H56C H 0.103098 0.697828 0.738696 0.145 Uiso 1 1 calc R U . . .
C57 C 0.2605(3) 0.53471(18) 0.75277(18) 0.0468(10) Uani 1 1 d . . . . .
H57A H 0.271784 0.502173 0.767767 0.056 Uiso 1 1 calc R U . . .
H57B H 0.332765 0.552268 0.766207 0.056 Uiso 1 1 calc R U . . .
C58 C 0.1908(3) 0.49244(16) 0.65936(17) 0.0427(9) Uani 1 1 d . . . . .
C59 C 0.2323(3) 0.53301(16) 0.68942(18) 0.0442(9) Uani 1 1 d . . . . .
C60 C 0.2404(4) 0.57421(18) 0.6611(2) 0.0501(11) Uani 1 1 d . . . . .
H60 H 0.266771 0.601803 0.682134 0.060 Uiso 1 1 calc R U . . .
C61 C 0.2114(4) 0.57736(18) 0.6024(2) 0.0534(11) Uani 1 1 d . . . . .
C62 C 0.1683(4) 0.53646(18) 0.57437(19) 0.0496(10) Uani 1 1 d . . . . .
H62 H 0.146718 0.537239 0.534635 0.060 Uiso 1 1 calc R U . . .
C63 C 0.1551(3) 0.49509(16) 0.60081(18) 0.0447(9) Uani 1 1 d . . . . .
C64 C 0.2272(4) 0.6230(2) 0.5715(2) 0.0637(13) Uani 1 1 d D . . . .
C65A C 0.2591(9) 0.6633(3) 0.6108(4) 0.0754(9) Uiso 0.621(6) 1 d D U P B 1
H65A H 0.198692 0.668497 0.631029 0.113 Uiso 0.621(6) 1 calc R U P B 1
H65B H 0.330850 0.656098 0.637643 0.113 Uiso 0.621(6) 1 calc R U P B 1
H65C H 0.268655 0.691810 0.589753 0.113 Uiso 0.621(6) 1 calc R U P B 1
C66A C 0.1131(8) 0.6341(4) 0.5302(4) 0.0754(9) Uiso 0.621(6) 1 d D U P B 1
H66A H 0.091886 0.607639 0.504148 0.113 Uiso 0.621(6) 1 calc R U P B 1
H66B H 0.053606 0.638949 0.550976 0.113 Uiso 0.621(6) 1 calc R U P B 1
H66C H 0.121370 0.662798 0.509094 0.113 Uiso 0.621(6) 1 calc R U P B 1
C67A C 0.3173(8) 0.6133(3) 0.5390(4) 0.0754(9) Uiso 0.621(6) 1 d D U P B 1
H67A H 0.293263 0.586601 0.513626 0.113 Uiso 0.621(6) 1 calc R U P B 1
H67B H 0.327458 0.641311 0.517245 0.113 Uiso 0.621(6) 1 calc R U P B 1
H67C H 0.389653 0.605599 0.565135 0.113 Uiso 0.621(6) 1 calc R U P B 1
C65B C 0.1789(14) 0.6686(5) 0.5933(7) 0.0754(9) Uiso 0.379(6) 1 d D U P B 2
H65D H 0.206010 0.670613 0.634026 0.113 Uiso 0.379(6) 1 calc R U P B 2
H65E H 0.204921 0.696416 0.575881 0.113 Uiso 0.379(6) 1 calc R U P B 2
H65F H 0.095245 0.667534 0.583579 0.113 Uiso 0.379(6) 1 calc R U P B 2
C66B C 0.1791(14) 0.6241(6) 0.5080(5) 0.0754(9) Uiso 0.379(6) 1 d D U P B 2
H66D H 0.194538 0.654965 0.493244 0.113 Uiso 0.379(6) 1 calc R U P B 2
H66E H 0.215519 0.599315 0.490294 0.113 Uiso 0.379(6) 1 calc R U P B 2
H66F H 0.096526 0.618688 0.499871 0.113 Uiso 0.379(6) 1 calc R U P B 2
C67B C 0.3581(10) 0.6331(6) 0.5803(7) 0.0754(9) Uiso 0.379(6) 1 d D U P B 2
H67D H 0.393817 0.632849 0.620383 0.113 Uiso 0.379(6) 1 calc R U P B 2
H67E H 0.392986 0.608619 0.561369 0.113 Uiso 0.379(6) 1 calc R U P B 2
H67F H 0.369302 0.664044 0.564520 0.113 Uiso 0.379(6) 1 calc R U P B 2
C68 C 0.1048(3) 0.45263(16) 0.56660(17) 0.0445(9) Uani 1 1 d . . . . .
H68A H 0.032267 0.461922 0.540713 0.053 Uiso 1 1 calc R U . . .
H68B H 0.087098 0.428011 0.591995 0.053 Uiso 1 1 calc R U . . .
C71 C 0.5405(4) 0.4464(2) 0.7305(2) 0.0678(14) Uani 1 1 d . . . . .
H71 H 0.578125 0.419013 0.716417 0.081 Uiso 1 1 calc R U . . .
C72 C 0.5442(6) 0.4879(3) 0.6919(3) 0.087(2) Uani 1 1 d . . . . .
H72A H 0.623830 0.496638 0.693824 0.131 Uiso 1 1 calc R U . . .
H72B H 0.507204 0.479152 0.653412 0.131 Uiso 1 1 calc R U . . .
H72C H 0.504009 0.514859 0.703581 0.131 Uiso 1 1 calc R U . . .
C73 C 0.5983(6) 0.4539(3) 0.7904(3) 0.099(2) Uani 1 1 d . . . . .
H73A H 0.678244 0.462537 0.793245 0.149 Uiso 1 1 calc R U . . .
H73B H 0.559803 0.479354 0.806007 0.149 Uiso 1 1 calc R U . . .
H73C H 0.594761 0.424743 0.811481 0.149 Uiso 1 1 calc R U . . .
C74A C -0.1348(9) 0.3950(4) 0.6896(4) 0.073(2) Uiso 0.600(10) 1 d D U P C 1
H74A H -0.168596 0.425511 0.698573 0.088 Uiso 0.600(10) 1 calc R U P C 1
C75A C -0.1680(14) 0.3844(5) 0.6272(5) 0.103(4) Uiso 0.600(10) 1 d D U P C 1
H75A H -0.251388 0.384069 0.614612 0.155 Uiso 0.600(10) 1 calc R U P C 1
H75B H -0.136604 0.408877 0.606751 0.155 Uiso 0.600(10) 1 calc R U P C 1
H75C H -0.137428 0.353571 0.620038 0.155 Uiso 0.600(10) 1 calc R U P C 1
C74B C -0.1092(11) 0.3698(5) 0.6766(5) 0.073(2) Uiso 0.400(10) 1 d D U P C 2
H74B H -0.084274 0.342411 0.656615 0.088 Uiso 0.400(10) 1 calc R U P C 2
C75B C -0.1851(19) 0.4036(7) 0.6360(8) 0.103(4) Uiso 0.400(10) 1 d D U P C 2
H75D H -0.251190 0.386420 0.614295 0.155 Uiso 0.400(10) 1 calc R U P C 2
H75E H -0.211271 0.429050 0.657115 0.155 Uiso 0.400(10) 1 calc R U P C 2
H75F H -0.141522 0.417119 0.610586 0.155 Uiso 0.400(10) 1 calc R U P C 2
C76 C -0.1743(8) 0.3533(4) 0.7210(5) 0.149(5) Uani 1 1 d D . . . .
H76A H -0.257747 0.351049 0.710479 0.224 Uiso 1 1 calc R U . C 1
H76B H -0.140884 0.323935 0.710901 0.224 Uiso 1 1 calc R U . C 1
H76C H -0.149373 0.358455 0.761426 0.224 Uiso 1 1 calc R U . C 1
C81 C 0.1518(4) 0.32635(19) 0.5944(2) 0.0549(11) Uani 1 1 d . . . . .
C82 C 0.1426(7) 0.2946(3) 0.5477(3) 0.094(2) Uani 1 1 d . . . . .
H82A H 0.173155 0.309861 0.518446 0.141 Uiso 1 1 calc R U . . .
H82B H 0.062241 0.286436 0.532796 0.141 Uiso 1 1 calc R U . . .
H82C H 0.186193 0.265759 0.560210 0.141 Uiso 1 1 calc R U . . .
C83 C 0.6846(10) 0.3293(4) 0.8409(4) 0.125(3) Uani 1 1 d . U . . .
C84 C 0.5942(7) 0.3091(4) 0.8052(3) 0.117(3) Uani 1 1 d . U . . .
H84A H 0.610999 0.275818 0.799675 0.176 Uiso 1 1 calc R U . . .
H84B H 0.579540 0.325582 0.769136 0.176 Uiso 1 1 calc R U . . .
H84C H 0.526589 0.311328 0.821017 0.176 Uiso 1 1 calc R U . . .
C85 C 0.1387(8) 0.1371(5) 0.5210(4) 0.123(3) Uani 1 1 d . . . . .
C86 C 0.1733(13) 0.0872(4) 0.5216(7) 0.178(6) Uani 1 1 d . . . . .
H86A H 0.256786 0.085219 0.529583 0.267 Uiso 1 1 calc R U . . .
H86B H 0.140878 0.072960 0.485081 0.267 Uiso 1 1 calc R U . . .
H86C H 0.145414 0.070328 0.550706 0.267 Uiso 1 1 calc R U . . .
C87 C 0.0401(12) 0.2756(4) 0.8914(5) 0.139(4) Uani 1 1 d . . . . .
N4 N 0.0396(17) 0.2367(5) 0.9046(6) 0.223(8) Uani 1 1 d . . . . .
N1 N 0.1666(3) 0.35210(14) 0.63170(16) 0.0494(9) Uani 1 1 d . . . . .
N2 N 0.7704(12) 0.3465(5) 0.8727(5) 0.183(5) Uani 1 1 d . U . . .
N3 N 0.1056(11) 0.1744(3) 0.5219(5) 0.156(4) Uani 1 1 d . . . . .
C88 C 0.0479(8) 0.3166(3) 0.8696(4) 0.116(3) Uani 1 1 d . . . . .
H88A H 0.118820 0.331912 0.889169 0.174 Uiso 1 1 calc R U . . .
H88B H -0.017411 0.336027 0.872991 0.174 Uiso 1 1 calc R U . . .
H88C H 0.048411 0.312819 0.829898 0.174 Uiso 1 1 calc R U . . .
O1 O 0.3249(2) 0.41604(11) 0.61672(12) 0.0437(6) Uani 1 1 d . . . . .
O2 O 0.4391(2) 0.32719(10) 0.58240(11) 0.0421(6) Uani 1 1 d . . . . .
O3 O 0.3824(2) 0.34077(10) 0.69639(12) 0.0435(6) Uani 1 1 d . . . . .
O4 O 0.2377(2) 0.38478(10) 0.75316(11) 0.0415(6) Uani 1 1 d . . . . .
O5 O 0.1085(2) 0.41592(11) 0.82005(12) 0.0455(7) Uani 1 1 d . . . . .
O6 O -0.1276(3) 0.50664(13) 0.85030(13) 0.0552(8) Uani 1 1 d . . . . .
O7 O 0.0541(2) 0.48911(11) 0.75095(12) 0.0450(7) Uani 1 1 d . . . . .
O8 O 0.1870(2) 0.44969(11) 0.68661(11) 0.0425(6) Uani 1 1 d . . . . .
O9 O 0.4263(2) 0.43415(10) 0.72762(12) 0.0428(6) Uani 1 1 d . . . . .
O10 O -0.0152(3) 0.39546(12) 0.70716(14) 0.0540(8) Uani 1 1 d D . . . .
Ti1 Ti 0.31261(6) 0.39913(3) 0.68698(3) 0.0396(2) Uani 1 1 d . . . . .
Ti2 Ti 0.10161(6) 0.42877(3) 0.74432(3) 0.0420(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.345(5) . ?
C1 C6 1.400(6) . ?
C1 C2 1.402(6) . ?
C2 C3 1.377(6) . ?
C2 C68 1.518(6) . ?
C3 C4 1.394(6) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(6) . ?
C4 C7 1.526(6) . ?
C5 C6 1.398(6) . ?
C5 H5 0.9500 . ?
C6 C11 1.503(6) . ?
C7 C10 1.521(7) . ?
C7 C9 1.542(7) . ?
C7 C8 1.547(8) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 O2 1.428(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.428(5) . ?
C12 C14 1.514(6) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 O3 1.343(5) . ?
C13 C18 1.400(6) . ?
C13 C14 1.401(6) . ?
C14 C15 1.382(6) . ?
C15 C16 1.411(6) . ?
C15 H15 0.9500 . ?
C16 C17 1.404(6) . ?
C16 C19 1.519(7) . ?
C17 C18 1.384(7) . ?
C17 H17 0.9500 . ?
C18 C23 1.513(6) . ?
C19 C20 1.519(8) . ?
C19 C21 1.539(7) . ?
C19 C22 1.560(10) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 C25 1.516(6) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C24 O4 1.380(5) . ?
C24 C29 1.399(6) . ?
C24 C25 1.400(7) . ?
C25 C26 1.401(7) . ?
C26 C27 1.387(7) . ?
C26 H26 0.9500 . ?
C27 C28 1.382(7) . ?
C27 C30 1.554(7) . ?
C28 C29 1.392(6) . ?
C28 H28 0.9500 . ?
C29 C34 1.510(7) . ?
C30 C31B 1.438(11) . ?
C30 C33A 1.440(10) . ?
C30 C31A 1.530(10) . ?
C30 C32B 1.546(12) . ?
C30 C33B 1.573(12) . ?
C30 C32A 1.599(11) . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C33A H33A 0.9800 . ?
C33A H33B 0.9800 . ?
C33A H33C 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33B H33D 0.9800 . ?
C33B H33E 0.9800 . ?
C33B H33F 0.9800 . ?
C34 C36 1.527(6) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O5 1.347(5) . ?
C35 C36 1.396(6) . ?
C35 C40 1.417(6) . ?
C36 C37 1.406(6) . ?
C37 C38 1.397(7) . ?
C37 H37 0.9500 . ?
C38 C39 1.393(7) . ?
C38 C41 1.547(7) . ?
C39 C40 1.390(7) . ?
C39 H39 0.9500 . ?
C40 C45 1.499(7) . ?
C41 C42 1.502(10) . ?
C41 C43 1.519(10) . ?
C41 C44 1.534(9) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 O6 1.432(6) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O6 1.428(6) . ?
C46 C48 1.520(6) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O7 1.356(5) . ?
C47 C52 1.394(6) . ?
C47 C48 1.395(6) . ?
C48 C49 1.394(7) . ?
C49 C50 1.377(7) . ?
C49 H49 0.9500 . ?
C50 C51 1.401(7) . ?
C50 C53 1.538(8) . ?
C51 C52 1.376(7) . ?
C51 H51 0.9500 . ?
C52 C57 1.512(6) . ?
C53 C54 1.513(9) . ?
C53 C55 1.515(8) . ?
C53 C56 1.582(11) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 C59 1.514(6) . ?
C57 H57A 0.9900 . ?
C57 H57B 0.9900 . ?
C58 O8 1.389(5) . ?
C58 C59 1.395(6) . ?
C58 C63 1.404(6) . ?
C59 C60 1.373(7) . ?
C60 C61 1.405(7) . ?
C60 H60 0.9500 . ?
C61 C62 1.386(7) . ?
C61 C64 1.533(7) . ?
C62 C63 1.366(7) . ?
C62 H62 0.9500 . ?
C63 C68 1.512(6) . ?
C64 C65A 1.486(10) . ?
C64 C67A 1.510(10) . ?
C64 C66B 1.533(12) . ?
C64 C66A 1.541(10) . ?
C64 C65B 1.560(12) . ?
C64 C67B 1.566(12) . ?
C65A H65A 0.9800 . ?
C65A H65B 0.9800 . ?
C65A H65C 0.9800 . ?
C66A H66A 0.9800 . ?
C66A H66B 0.9800 . ?
C66A H66C 0.9800 . ?
C67A H67A 0.9800 . ?
C67A H67B 0.9800 . ?
C67A H67C 0.9800 . ?
C65B H65D 0.9800 . ?
C65B H65E 0.9800 . ?
C65B H65F 0.9800 . ?
C66B H66D 0.9800 . ?
C66B H66E 0.9800 . ?
C66B H66F 0.9800 . ?
C67B H67D 0.9800 . ?
C67B H67E 0.9800 . ?
C67B H67F 0.9800 . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
C71 O9 1.404(6) . ?
C71 C73 1.491(9) . ?
C71 C72 1.516(9) . ?
C71 H71 1.0000 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74A O10 1.404(11) . ?
C74A C75A 1.522(13) . ?
C74A C76 1.543(11) . ?
C74A H74A 1.0000 . ?
C75A H75A 0.9800 . ?
C75A H75B 0.9800 . ?
C75A H75C 0.9800 . ?
C74B O10 1.407(13) . ?
C74B C75B 1.526(15) . ?
C74B C76 1.551(14) . ?
C74B H74B 1.0000 . ?
C75B H75D 0.9800 . ?
C75B H75E 0.9800 . ?
C75B H75F 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C81 N1 1.151(6) . ?
C81 C82 1.442(8) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C83 N2 1.242(14) . ?
C83 C84 1.357(13) . ?
C84 H84A 0.9800 . ?
C84 H84B 0.9800 . ?
C84 H84C 0.9800 . ?
C85 N3 1.132(12) . ?
C85 C86 1.471(17) . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 N4 1.151(14) . ?
C87 C88 1.289(14) . ?
N1 Ti1 2.368(4) . ?
C88 H88A 0.9800 . ?
C88 H88B 0.9800 . ?
C88 H88C 0.9800 . ?
O1 Ti1 1.828(3) . ?
O3 Ti1 1.844(3) . ?
O4 Ti2 2.029(3) . ?
O4 Ti1 2.070(3) . ?
O5 Ti2 1.877(3) . ?
O7 Ti2 1.821(3) . ?
O8 Ti2 2.019(3) . ?
O8 Ti1 2.081(3) . ?
O9 Ti1 1.796(3) . ?
O10 Ti2 1.764(3) . ?
Ti1 Ti2 3.2817(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C6 119.4(4) . . ?
O1 C1 C2 120.6(4) . . ?
C6 C1 C2 120.0(4) . . ?
C3 C2 C1 118.6(4) . . ?
C3 C2 C68 121.5(4) . . ?
C1 C2 C68 119.9(4) . . ?
C2 C3 C4 123.5(4) . . ?
C2 C3 H3 118.3 . . ?
C4 C3 H3 118.3 . . ?
C3 C4 C5 117.0(4) . . ?
C3 C4 C7 119.5(4) . . ?
C5 C4 C7 123.5(4) . . ?
C6 C5 C4 121.3(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 H5 119.4 . . ?
C5 C6 C1 119.6(4) . . ?
C5 C6 C11 121.2(4) . . ?
C1 C6 C11 119.1(4) . . ?
C10 C7 C4 110.8(4) . . ?
C10 C7 C9 108.7(4) . . ?
C4 C7 C9 112.2(4) . . ?
C10 C7 C8 108.5(4) . . ?
C4 C7 C8 108.7(4) . . ?
C9 C7 C8 107.7(4) . . ?
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 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O2 C11 C6 106.8(3) . . ?
O2 C11 H11A 110.4 . . ?
C6 C11 H11A 110.4 . . ?
O2 C11 H11B 110.4 . . ?
C6 C11 H11B 110.4 . . ?
H11A C11 H11B 108.6 . . ?
O2 C12 C14 106.4(3) . . ?
O2 C12 H12A 110.5 . . ?
C14 C12 H12A 110.5 . . ?
O2 C12 H12B 110.5 . . ?
C14 C12 H12B 110.5 . . ?
H12A C12 H12B 108.6 . . ?
O3 C13 C18 121.1(4) . . ?
O3 C13 C14 119.1(4) . . ?
C18 C13 C14 119.8(4) . . ?
C15 C14 C13 120.6(4) . . ?
C15 C14 C12 120.8(4) . . ?
C13 C14 C12 118.4(4) . . ?
C14 C15 C16 121.2(4) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 116.4(4) . . ?
C17 C16 C19 120.1(4) . . ?
C15 C16 C19 123.4(4) . . ?
C18 C17 C16 123.7(4) . . ?
C18 C17 H17 118.1 . . ?
C16 C17 H17 118.1 . . ?
C17 C18 C13 118.2(4) . . ?
C17 C18 C23 120.6(4) . . ?
C13 C18 C23 121.1(4) . . ?
C20 C19 C16 109.5(4) . . ?
C20 C19 C21 109.3(6) . . ?
C16 C19 C21 112.3(4) . . ?
C20 C19 C22 110.1(7) . . ?
C16 C19 C22 107.2(5) . . ?
C21 C19 C22 108.4(4) . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C19 C22 H22A 109.5 . . ?
C19 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C19 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 C25 113.0(3) . . ?
C18 C23 H23A 109.0 . . ?
C25 C23 H23A 109.0 . . ?
C18 C23 H23B 109.0 . . ?
C25 C23 H23B 109.0 . . ?
H23A C23 H23B 107.8 . . ?
O4 C24 C29 120.2(4) . . ?
O4 C24 C25 119.8(4) . . ?
C29 C24 C25 120.0(4) . . ?
C24 C25 C26 118.5(4) . . ?
C24 C25 C23 122.5(4) . . ?
C26 C25 C23 119.0(4) . . ?
C27 C26 C25 122.6(5) . . ?
C27 C26 H26 118.7 . . ?
C25 C26 H26 118.7 . . ?
C28 C27 C26 117.1(4) . . ?
C28 C27 C30 122.8(5) . . ?
C26 C27 C30 120.0(5) . . ?
C27 C28 C29 122.7(4) . . ?
C27 C28 H28 118.7 . . ?
C29 C28 H28 118.7 . . ?
C28 C29 C24 119.0(4) . . ?
C28 C29 C34 119.3(4) . . ?
C24 C29 C34 121.7(4) . . ?
C33A C30 C31A 113.2(7) . . ?
C31B C30 C32B 111.8(9) . . ?
C31B C30 C27 117.2(7) . . ?
C33A C30 C27 115.3(6) . . ?
C31A C30 C27 109.0(6) . . ?
C32B C30 C27 105.8(6) . . ?
C31B C30 C33B 110.7(8) . . ?
C32B C30 C33B 104.6(7) . . ?
C27 C30 C33B 106.0(6) . . ?
C33A C30 C32A 109.9(7) . . ?
C31A C30 C32A 103.2(6) . . ?
C27 C30 C32A 105.2(6) . . ?
C30 C31A H31A 109.5 . . ?
C30 C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C30 C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C30 C32A H32A 109.5 . . ?
C30 C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C30 C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C30 C33A H33A 109.5 . . ?
C30 C33A H33B 109.5 . . ?
H33A C33A H33B 109.5 . . ?
C30 C33A H33C 109.5 . . ?
H33A C33A H33C 109.5 . . ?
H33B C33A H33C 109.5 . . ?
C30 C31B H31D 109.5 . . ?
C30 C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C30 C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C30 C32B H32D 109.5 . . ?
C30 C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C30 C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
C30 C33B H33D 109.5 . . ?
C30 C33B H33E 109.5 . . ?
H33D C33B H33E 109.5 . . ?
C30 C33B H33F 109.5 . . ?
H33D C33B H33F 109.5 . . ?
H33E C33B H33F 109.5 . . ?
C29 C34 C36 114.8(4) . . ?
C29 C34 H34A 108.6 . . ?
C36 C34 H34A 108.6 . . ?
C29 C34 H34B 108.6 . . ?
C36 C34 H34B 108.6 . . ?
H34A C34 H34B 107.5 . . ?
O5 C35 C36 119.8(4) . . ?
O5 C35 C40 120.1(4) . . ?
C36 C35 C40 120.1(4) . . ?
C35 C36 C37 118.7(4) . . ?
C35 C36 C34 121.0(4) . . ?
C37 C36 C34 119.9(4) . . ?
C38 C37 C36 122.3(4) . . ?
C38 C37 H37 118.9 . . ?
C36 C37 H37 118.9 . . ?
C39 C38 C37 117.4(4) . . ?
C39 C38 C41 122.3(4) . . ?
C37 C38 C41 120.3(4) . . ?
C40 C39 C38 122.5(4) . . ?
C40 C39 H39 118.7 . . ?
C38 C39 H39 118.7 . . ?
C39 C40 C35 118.9(4) . . ?
C39 C40 C45 120.3(4) . . ?
C35 C40 C45 120.8(4) . . ?
C42 C41 C43 109.5(7) . . ?
C42 C41 C44 110.0(6) . . ?
C43 C41 C44 108.5(5) . . ?
C42 C41 C38 109.8(5) . . ?
C43 C41 C38 108.5(5) . . ?
C44 C41 C38 110.6(5) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
O6 C45 C40 113.3(4) . . ?
O6 C45 H45A 108.9 . . ?
C40 C45 H45A 108.9 . . ?
O6 C45 H45B 108.9 . . ?
C40 C45 H45B 108.9 . . ?
H45A C45 H45B 107.7 . . ?
O6 C46 C48 114.4(4) . . ?
O6 C46 H46A 108.7 . . ?
C48 C46 H46A 108.7 . . ?
O6 C46 H46B 108.7 . . ?
C48 C46 H46B 108.7 . . ?
H46A C46 H46B 107.6 . . ?
O7 C47 C52 119.6(4) . . ?
O7 C47 C48 120.1(4) . . ?
C52 C47 C48 120.3(4) . . ?
C49 C48 C47 118.4(4) . . ?
C49 C48 C46 120.5(4) . . ?
C47 C48 C46 121.1(4) . . ?
C50 C49 C48 122.8(4) . . ?
C50 C49 H49 118.6 . . ?
C48 C49 H49 118.6 . . ?
C49 C50 C51 116.8(4) . . ?
C49 C50 C53 122.9(4) . . ?
C51 C50 C53 119.9(4) . . ?
C52 C51 C50 122.5(4) . . ?
C52 C51 H51 118.7 . . ?
C50 C51 H51 118.7 . . ?
C51 C52 C47 119.0(4) . . ?
C51 C52 C57 122.3(4) . . ?
C47 C52 C57 118.5(4) . . ?
C54 C53 C55 110.8(6) . . ?
C54 C53 C50 112.7(5) . . ?
C55 C53 C50 111.9(5) . . ?
C54 C53 C56 107.1(7) . . ?
C55 C53 C56 106.4(5) . . ?
C50 C53 C56 107.4(6) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C53 C55 H55A 109.5 . . ?
C53 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C53 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C53 C56 H56A 109.5 . . ?
C53 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C53 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C52 C57 C59 111.4(3) . . ?
C52 C57 H57A 109.4 . . ?
C59 C57 H57A 109.4 . . ?
C52 C57 H57B 109.4 . . ?
C59 C57 H57B 109.4 . . ?
H57A C57 H57B 108.0 . . ?
O8 C58 C59 120.7(4) . . ?
O8 C58 C63 120.2(4) . . ?
C59 C58 C63 119.1(4) . . ?
C60 C59 C58 119.4(4) . . ?
C60 C59 C57 117.9(4) . . ?
C58 C59 C57 122.6(4) . . ?
C59 C60 C61 122.9(4) . . ?
C59 C60 H60 118.6 . . ?
C61 C60 H60 118.6 . . ?
C62 C61 C60 115.6(4) . . ?
C62 C61 C64 122.3(4) . . ?
C60 C61 C64 122.1(5) . . ?
C63 C62 C61 123.5(4) . . ?
C63 C62 H62 118.2 . . ?
C61 C62 H62 118.2 . . ?
C62 C63 C58 119.4(4) . . ?
C62 C63 C68 119.6(4) . . ?
C58 C63 C68 121.0(4) . . ?
C65A C64 C67A 111.9(6) . . ?
C65A C64 C61 111.6(5) . . ?
C67A C64 C61 107.0(5) . . ?
C66B C64 C61 117.3(7) . . ?
C65A C64 C66A 109.3(6) . . ?
C67A C64 C66A 109.2(6) . . ?
C61 C64 C66A 107.7(5) . . ?
C66B C64 C65B 104.4(8) . . ?
C61 C64 C65B 115.5(7) . . ?
C66B C64 C67B 105.7(9) . . ?
C61 C64 C67B 108.7(7) . . ?
C65B C64 C67B 104.2(8) . . ?
C64 C65A H65A 109.5 . . ?
C64 C65A H65B 109.5 . . ?
H65A C65A H65B 109.5 . . ?
C64 C65A H65C 109.5 . . ?
H65A C65A H65C 109.5 . . ?
H65B C65A H65C 109.5 . . ?
C64 C66A H66A 109.5 . . ?
C64 C66A H66B 109.5 . . ?
H66A C66A H66B 109.5 . . ?
C64 C66A H66C 109.5 . . ?
H66A C66A H66C 109.5 . . ?
H66B C66A H66C 109.5 . . ?
C64 C67A H67A 109.5 . . ?
C64 C67A H67B 109.5 . . ?
H67A C67A H67B 109.5 . . ?
C64 C67A H67C 109.5 . . ?
H67A C67A H67C 109.5 . . ?
H67B C67A H67C 109.5 . . ?
C64 C65B H65D 109.5 . . ?
C64 C65B H65E 109.5 . . ?
H65D C65B H65E 109.5 . . ?
C64 C65B H65F 109.5 . . ?
H65D C65B H65F 109.5 . . ?
H65E C65B H65F 109.5 . . ?
C64 C66B H66D 109.5 . . ?
C64 C66B H66E 109.5 . . ?
H66D C66B H66E 109.5 . . ?
C64 C66B H66F 109.5 . . ?
H66D C66B H66F 109.5 . . ?
H66E C66B H66F 109.5 . . ?
C64 C67B H67D 109.5 . . ?
C64 C67B H67E 109.5 . . ?
H67D C67B H67E 109.5 . . ?
C64 C67B H67F 109.5 . . ?
H67D C67B H67F 109.5 . . ?
H67E C67B H67F 109.5 . . ?
C63 C68 C2 112.5(3) . . ?
C63 C68 H68A 109.1 . . ?
C2 C68 H68A 109.1 . . ?
C63 C68 H68B 109.1 . . ?
C2 C68 H68B 109.1 . . ?
H68A C68 H68B 107.8 . . ?
O9 C71 C73 108.4(5) . . ?
O9 C71 C72 109.2(5) . . ?
C73 C71 C72 115.6(6) . . ?
O9 C71 H71 107.8 . . ?
C73 C71 H71 107.8 . . ?
C72 C71 H71 107.8 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
O10 C74A C75A 108.9(10) . . ?
O10 C74A C76 105.4(7) . . ?
C75A C74A C76 108.1(9) . . ?
O10 C74A H74A 111.4 . . ?
C75A C74A H74A 111.4 . . ?
C76 C74A H74A 111.4 . . ?
C74A C75A H75A 109.5 . . ?
C74A C75A H75B 109.5 . . ?
H75A C75A H75B 109.5 . . ?
C74A C75A H75C 109.5 . . ?
H75A C75A H75C 109.5 . . ?
H75B C75A H75C 109.5 . . ?
O10 C74B C75B 108.1(13) . . ?
O10 C74B C76 104.8(9) . . ?
C75B C74B C76 108.9(12) . . ?
O10 C74B H74B 111.6 . . ?
C75B C74B H74B 111.6 . . ?
C76 C74B H74B 111.6 . . ?
C74B C75B H75D 109.5 . . ?
C74B C75B H75E 109.5 . . ?
H75D C75B H75E 109.5 . . ?
C74B C75B H75F 109.5 . . ?
H75D C75B H75F 109.5 . . ?
H75E C75B H75F 109.5 . . ?
C74A C76 H76A 109.5 . . ?
C74A C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C74A C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N1 C81 C82 175.5(6) . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
N2 C83 C84 177.3(13) . . ?
C83 C84 H84A 109.5 . . ?
C83 C84 H84B 109.5 . . ?
H84A C84 H84B 109.5 . . ?
C83 C84 H84C 109.5 . . ?
H84A C84 H84C 109.5 . . ?
H84B C84 H84C 109.5 . . ?
N3 C85 C86 175.2(13) . . ?
C85 C86 H86A 109.5 . . ?
C85 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C85 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
N4 C87 C88 170.0(15) . . ?
C81 N1 Ti1 140.4(3) . . ?
C87 C88 H88A 109.5 . . ?
C87 C88 H88B 109.5 . . ?
H88A C88 H88B 109.5 . . ?
C87 C88 H88C 109.5 . . ?
H88A C88 H88C 109.5 . . ?
H88B C88 H88C 109.5 . . ?
C1 O1 Ti1 152.3(3) . . ?
C12 O2 C11 114.0(3) . . ?
C13 O3 Ti1 153.0(3) . . ?
C24 O4 Ti2 127.3(2) . . ?
C24 O4 Ti1 125.3(2) . . ?
Ti2 O4 Ti1 106.35(13) . . ?
C35 O5 Ti2 123.5(3) . . ?
C46 O6 C45 113.5(3) . . ?
C47 O7 Ti2 153.1(3) . . ?
C58 O8 Ti2 132.2(2) . . ?
C58 O8 Ti1 119.9(2) . . ?
Ti2 O8 Ti1 106.31(13) . . ?
C71 O9 Ti1 141.1(3) . . ?
C74A O10 Ti2 143.4(5) . . ?
C74B O10 Ti2 178.6(6) . . ?
O9 Ti1 O1 99.39(14) . . ?
O9 Ti1 O3 99.09(13) . . ?
O1 Ti1 O3 102.70(13) . . ?
O9 Ti1 O4 94.94(12) . . ?
O1 Ti1 O4 159.26(12) . . ?
O3 Ti1 O4 89.65(12) . . ?
O9 Ti1 O8 94.76(13) . . ?
O1 Ti1 O8 91.79(12) . . ?
O3 Ti1 O8 157.95(12) . . ?
O4 Ti1 O8 72.05(11) . . ?
O9 Ti1 N1 178.23(14) . . ?
O1 Ti1 N1 79.45(13) . . ?
O3 Ti1 N1 79.91(13) . . ?
O4 Ti1 N1 86.53(12) . . ?
O8 Ti1 N1 86.63(12) . . ?
O9 Ti1 Ti2 100.75(10) . . ?
O1 Ti1 Ti2 125.11(10) . . ?
O3 Ti1 Ti2 123.41(9) . . ?
O4 Ti1 Ti2 36.39(8) . . ?
O8 Ti1 Ti2 36.20(8) . . ?
N1 Ti1 Ti2 81.02(9) . . ?
O10 Ti2 O7 108.58(15) . . ?
O10 Ti2 O5 104.90(15) . . ?
O7 Ti2 O5 92.13(14) . . ?
O10 Ti2 O8 105.53(14) . . ?
O7 Ti2 O8 90.45(13) . . ?
O5 Ti2 O8 146.85(12) . . ?
O10 Ti2 O4 104.78(14) . . ?
O7 Ti2 O4 145.97(13) . . ?
O5 Ti2 O4 85.62(12) . . ?
O8 Ti2 O4 74.18(11) . . ?
O10 Ti2 Ti1 104.19(11) . . ?
O7 Ti2 Ti1 124.61(10) . . ?
O5 Ti2 Ti1 120.80(9) . . ?
O8 Ti2 Ti1 37.49(8) . . ?
O4 Ti2 Ti1 37.26(8) . . ?

_refine_diff_density_max         1.961
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.142




####################################################################### 
# 
# 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 2057322'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;   
 C54 H59 F14 N3 O6 Ti4 [+ solvent]
;
_chemical_formula_sum            'C54 H59 F14 N3 O6 Ti4'
_chemical_formula_weight         1303.64

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           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'

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.461 -0.035 821 140 ' '
2 0.181 0.637 0.036 9 1 ' '
3 0.181 0.863 0.536 9 1 ' '
4 0.334 0.641 0.050 13 1 ' '
5 0.334 0.859 0.550 14 1 ' '
6 0.678 0.141 0.451 16 1 ' '
7 0.679 0.359 0.951 17 1 ' '
8 0.833 0.137 0.466 7 0 ' '
9 0.833 0.363 0.966 7 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
140e per cell equates to about 6 MeCN per cell. 
Thus 1.5 per formula unit.
;


_cell_length_a                   16.1213(2)
_cell_length_b                   22.8130(2)
_cell_length_c                   17.0185(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.3810(10)
_cell_angle_gamma                90
_cell_volume                     6113.42(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    28774
_cell_measurement_theta_min      3.388
_cell_measurement_theta_max      70.168

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.416
_exptl_crystal_F_000             2664
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    5.091
_shelx_estimated_absorpt_T_min   0.516
_shelx_estimated_absorpt_T_max   0.785
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6143
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scan
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            55456
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         3.938
_diffrn_reflns_theta_max         70.413
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             11386
_reflns_number_gt                9819
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.1262P)²+4.0039P] 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         11386
_refine_ls_number_parameters     741
_refine_ls_number_restraints     3
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0637
_refine_ls_wR_factor_ref         0.1784
_refine_ls_wR_factor_gt          0.1701
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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 0.56081(4) 0.29990(2) 0.69342(3) 0.03454(15) Uani 1 1 d . . . . .
Ti2 Ti 0.40633(4) 0.37327(2) 0.80807(3) 0.03776(16) Uani 1 1 d . . . . .
Ti3 Ti 0.42430(4) 0.43334(2) 0.60026(3) 0.03291(15) Uani 1 1 d . . . . .
Ti4 Ti 0.31830(4) 0.28382(3) 0.61584(4) 0.04074(16) Uani 1 1 d . . . . .
O1 O 0.54672(15) 0.54334(10) 0.78137(13) 0.0418(5) Uani 1 1 d . . . . .
H1 H 0.540754 0.510556 0.758380 0.063 Uiso 1 1 calc DR U . . .
O2 O 0.65393(15) 0.33453(10) 0.74606(13) 0.0407(5) Uani 1 1 d . . . . .
O3 O 0.60817(14) 0.27261(9) 0.61245(13) 0.0379(5) Uani 1 1 d . . . . .
O4 O 0.43733(14) 0.42774(9) 0.49638(13) 0.0354(5) Uani 1 1 d . . . . .
O5 O 0.33454(14) 0.48210(10) 0.58490(13) 0.0389(5) Uani 1 1 d D . . . .
O6 O 0.35405(14) 0.55227(10) 0.73248(14) 0.0409(5) Uani 1 1 d . . . . .
H6 H 0.342832 0.526987 0.695852 0.061 Uiso 1 1 calc DR U . . .
F1 F 0.56801(13) 0.23212(8) 0.75246(11) 0.0445(4) Uani 1 1 d . . . . .
F2 F 0.44312(12) 0.27237(8) 0.63719(11) 0.0403(4) Uani 1 1 d . . . . .
F3 F 0.50106(12) 0.33355(8) 0.77699(10) 0.0397(4) Uani 1 1 d . . . . .
F4 F 0.40501(14) 0.32043(9) 0.88487(12) 0.0479(5) Uani 1 1 d . . . . .
F5 F 0.47645(14) 0.42286(9) 0.87040(12) 0.0489(5) Uani 1 1 d . . . . .
F6 F 0.30987(13) 0.40834(9) 0.81397(12) 0.0504(5) Uani 1 1 d . . . . .
F7 F 0.50661(11) 0.48718(8) 0.63903(10) 0.0374(4) Uani 1 1 d . . . . .
F8 F 0.41210(12) 0.42282(8) 0.71473(10) 0.0382(4) Uani 1 1 d . . . . .
F9 F 0.34884(12) 0.36277(8) 0.58240(11) 0.0390(4) Uani 1 1 d . . . . .
F10 F 0.21132(14) 0.30644(10) 0.60489(13) 0.0554(5) Uani 1 1 d . . . . .
F11 F 0.30809(15) 0.21416(9) 0.65848(13) 0.0532(5) Uani 1 1 d . . . . .
F12 F 0.34211(13) 0.31906(9) 0.72549(11) 0.0442(4) Uani 1 1 d . . . . .
F13 F 0.30879(14) 0.25887(9) 0.51548(12) 0.0507(5) Uani 1 1 d . . . . .
F14 F 0.51706(11) 0.37167(7) 0.63029(10) 0.0364(4) Uani 1 1 d . . . . .
C1 C 0.5332(2) 0.62608(14) 0.8910(2) 0.0420(7) Uani 1 1 d . . . . .
H1A H 0.536674 0.650945 0.844123 0.050 Uiso 1 1 calc R U . . .
H1B H 0.536735 0.651929 0.938321 0.050 Uiso 1 1 calc R U . . .
C2 C 0.6060(2) 0.58345(14) 0.9065(2) 0.0395(7) Uani 1 1 d . . . . .
C3 C 0.6100(2) 0.53994(14) 0.84952(19) 0.0370(7) Uani 1 1 d . . . . .
C4 C 0.6708(2) 0.49575(15) 0.8650(2) 0.0396(7) Uani 1 1 d . . . . .
C5 C 0.7308(2) 0.49883(16) 0.9380(2) 0.0424(7) Uani 1 1 d . . . . .
H5 H 0.772215 0.468721 0.950651 0.051 Uiso 1 1 calc R U . . .
C6 C 0.7318(2) 0.54404(16) 0.9922(2) 0.0426(7) Uani 1 1 d . . . . .
C7 C 0.6679(2) 0.58578(15) 0.9766(2) 0.0428(7) Uani 1 1 d . . . . .
H7 H 0.666547 0.616223 1.014416 0.051 Uiso 1 1 calc R U . . .
C8 C 0.8010(3) 0.5466(2) 1.0677(2) 0.0577(10) Uani 1 1 d . . . . .
H8A H 0.779939 0.529871 1.112728 0.087 Uiso 1 1 calc R U . . .
H8B H 0.817555 0.587551 1.079710 0.087 Uiso 1 1 calc R U . . .
H8C H 0.850320 0.524216 1.059610 0.087 Uiso 1 1 calc R U . . .
C9 C 0.6659(2) 0.44473(15) 0.8080(2) 0.0452(8) Uani 1 1 d . . . . .
H9A H 0.626424 0.415720 0.823181 0.054 Uiso 1 1 calc R U . . .
H9B H 0.639003 0.459189 0.753622 0.054 Uiso 1 1 calc DR U . . .
C10 C 0.7450(2) 0.41228(15) 0.8007(2) 0.0412(7) Uani 1 1 d . . . . .
C11 C 0.7341(2) 0.35659(15) 0.76590(19) 0.0388(7) Uani 1 1 d . . . . .
C12 C 0.8008(2) 0.32288(15) 0.75068(19) 0.0409(7) Uani 1 1 d . . . . .
C13 C 0.8823(2) 0.34670(16) 0.7705(2) 0.0445(8) Uani 1 1 d . . . . .
H13 H 0.929116 0.324436 0.761260 0.053 Uiso 1 1 calc R U . . .
C14 C 0.8962(2) 0.40259(17) 0.8036(2) 0.0460(8) Uani 1 1 d . . . . .
C15 C 0.9837(3) 0.4289(2) 0.8222(3) 0.0651(11) Uani 1 1 d . . . . .
H15A H 0.983833 0.465083 0.791275 0.098 Uiso 1 1 calc R U . . .
H15B H 1.024146 0.400979 0.807663 0.098 Uiso 1 1 calc R U . . .
H15C H 1.000176 0.437664 0.879817 0.098 Uiso 1 1 calc R U . . .
C16 C 0.8274(2) 0.43440(16) 0.8184(2) 0.0442(8) Uani 1 1 d . . . . .
H16 H 0.837047 0.472415 0.841381 0.053 Uiso 1 1 calc R U . . .
C17 C 0.7839(2) 0.26367(15) 0.7116(2) 0.0425(7) Uani 1 1 d . . . . .
H17A H 0.737182 0.244392 0.731163 0.051 Uiso 1 1 calc R U . . .
H17B H 0.835279 0.238991 0.727540 0.051 Uiso 1 1 calc R U . . .
C18 C 0.7601(2) 0.26777(14) 0.6202(2) 0.0392(7) Uani 1 1 d . . . . .
C19 C 0.6758(2) 0.27177(13) 0.57674(19) 0.0371(7) Uani 1 1 d . . . . .
C20 C 0.6582(2) 0.27159(14) 0.49195(19) 0.0392(7) Uani 1 1 d . . . . .
C21 C 0.7246(2) 0.26970(16) 0.4515(2) 0.0462(8) Uani 1 1 d . . . . .
H21 H 0.712268 0.269696 0.394354 0.055 Uiso 1 1 calc R U . . .
C22 C 0.8081(3) 0.26784(18) 0.4930(2) 0.0520(9) Uani 1 1 d . . . . .
C23 C 0.8240(2) 0.26627(16) 0.5768(2) 0.0471(8) Uani 1 1 d . . . . .
H23 H 0.881254 0.264058 0.605664 0.056 Uiso 1 1 calc R U . . .
C24 C 0.8796(3) 0.2663(3) 0.4486(3) 0.0704(13) Uani 1 1 d . . . . .
H24A H 0.872400 0.232395 0.412398 0.106 Uiso 1 1 calc R U . . .
H24B H 0.933930 0.263093 0.487411 0.106 Uiso 1 1 calc R U . . .
H24C H 0.878942 0.302352 0.417212 0.106 Uiso 1 1 calc R U . . .
C25 C 0.5681(2) 0.26961(14) 0.44758(19) 0.0390(7) Uani 1 1 d . . . . .
H25A H 0.536612 0.241827 0.475093 0.047 Uiso 1 1 calc R U . . .
H25B H 0.565865 0.254433 0.392674 0.047 Uiso 1 1 calc R U . . .
C26 C 0.4299(2) 0.31780(14) 0.4154(2) 0.0415(7) Uani 1 1 d . . . . .
H26A H 0.420916 0.286971 0.373513 0.050 Uiso 1 1 calc R U . . .
H26B H 0.409517 0.302040 0.462124 0.050 Uiso 1 1 calc R U . . .
C27 C 0.3760(2) 0.36932(14) 0.3834(2) 0.0383(7) Uani 1 1 d . . . . .
C28 C 0.3154(2) 0.36218(15) 0.3120(2) 0.0436(8) Uani 1 1 d . . . . .
H28 H 0.312860 0.326098 0.283700 0.052 Uiso 1 1 calc R U . . .
C29 C 0.2585(2) 0.40662(16) 0.2813(2) 0.0437(8) Uani 1 1 d . . . . .
C30 C 0.1909(3) 0.39696(18) 0.2058(2) 0.0521(9) Uani 1 1 d . . . . .
H30A H 0.212781 0.408970 0.158760 0.078 Uiso 1 1 calc R U . . .
H30B H 0.140605 0.420313 0.208533 0.078 Uiso 1 1 calc R U . . .
H30C H 0.175586 0.355346 0.201118 0.078 Uiso 1 1 calc R U . . .
C31 C 0.2669(2) 0.45982(15) 0.3217(2) 0.0421(7) Uani 1 1 d . . . . .
H31 H 0.229766 0.490970 0.300381 0.051 Uiso 1 1 calc R U . . .
C32 C 0.3277(2) 0.46956(14) 0.39243(19) 0.0367(7) Uani 1 1 d . . . . .
C33 C 0.38098(19) 0.42361(13) 0.42410(16) 0.0310(6) Uani 1 1 d . . . . .
C34 C 0.3347(2) 0.52921(14) 0.43198(19) 0.0371(7) Uani 1 1 d . . . . .
H34A H 0.333790 0.560053 0.390884 0.045 Uiso 1 1 calc R U . . .
H34B H 0.389173 0.532162 0.471818 0.045 Uiso 1 1 calc R U . . .
C35 C 0.2615(2) 0.53833(14) 0.47346(19) 0.0378(7) Uani 1 1 d . . . . .
C36 C 0.1890(2) 0.56861(15) 0.4367(2) 0.0416(7) Uani 1 1 d . . . . .
H36 H 0.187712 0.587528 0.386722 0.050 Uiso 1 1 calc R U . . .
C37 C 0.1186(2) 0.57208(16) 0.4707(2) 0.0455(8) Uani 1 1 d . . . . .
C38 C 0.0372(3) 0.6010(2) 0.4262(2) 0.0573(10) Uani 1 1 d . . . . .
H38A H 0.051125 0.633768 0.394002 0.086 Uiso 1 1 calc R U . . .
H38B H 0.005337 0.615676 0.465074 0.086 Uiso 1 1 calc R U . . .
H38C H 0.002640 0.572306 0.390658 0.086 Uiso 1 1 calc R U . . .
C39 C 0.1227(2) 0.54615(16) 0.5456(2) 0.0447(8) Uani 1 1 d . . . . .
H39 H 0.075127 0.548999 0.570111 0.054 Uiso 1 1 calc R U . . .
C40 C 0.1946(2) 0.51624(14) 0.5854(2) 0.0393(7) Uani 1 1 d . . . . .
C41 C 0.26310(19) 0.51214(13) 0.54839(19) 0.0360(7) Uani 1 1 d . . . . .
C42 C 0.1960(2) 0.48957(15) 0.6673(2) 0.0416(7) Uani 1 1 d . . . . .
H42A H 0.243915 0.461558 0.680568 0.050 Uiso 1 1 calc R U . . .
H42B H 0.142816 0.467355 0.664960 0.050 Uiso 1 1 calc R U . . .
C43 C 0.2052(2) 0.53507(15) 0.7337(2) 0.0408(7) Uani 1 1 d . . . . .
C44 C 0.1370(2) 0.55079(16) 0.7669(2) 0.0480(8) Uani 1 1 d . . . . .
H44 H 0.083346 0.533231 0.746290 0.058 Uiso 1 1 calc R U . . .
C45 C 0.1442(3) 0.59142(17) 0.8293(3) 0.0523(9) Uani 1 1 d . . . . .
C46 C 0.0687(3) 0.6069(2) 0.8645(3) 0.0706(12) Uani 1 1 d . . . . .
H46A H 0.088544 0.623256 0.918534 0.106 Uiso 1 1 calc R U . . .
H46B H 0.034979 0.571633 0.867683 0.106 Uiso 1 1 calc R U . . .
H46C H 0.033621 0.636030 0.830133 0.106 Uiso 1 1 calc R U . . .
C47 C 0.2229(2) 0.61641(16) 0.8585(2) 0.0482(8) Uani 1 1 d . . . . .
H47 H 0.229736 0.642833 0.902528 0.058 Uiso 1 1 calc R U . . .
C48 C 0.2923(2) 0.60376(14) 0.8247(2) 0.0414(7) Uani 1 1 d . . . . .
C49 C 0.2827(2) 0.56300(14) 0.7625(2) 0.0402(7) Uani 1 1 d . . . . .
C50 C 0.3750(2) 0.63460(14) 0.8533(2) 0.0439(8) Uani 1 1 d . . . . .
H50A H 0.371765 0.658446 0.901120 0.053 Uiso 1 1 calc R U . . .
H50B H 0.384716 0.661635 0.810622 0.053 Uiso 1 1 calc R U . . .
C51 C 0.4399(3) 0.55365(17) 0.9417(2) 0.0509(9) Uani 1 1 d . . . . .
H51A H 0.443589 0.576622 0.990959 0.076 Uiso 1 1 calc R U . . .
H51B H 0.485511 0.524409 0.950083 0.076 Uiso 1 1 calc DR U . . .
H51C H 0.384803 0.533782 0.928163 0.076 Uiso 1 1 calc R U . . .
C52 C 0.5583(2) 0.36970(15) 0.3870(2) 0.0425(7) Uani 1 1 d . . . . .
H52A H 0.543130 0.355125 0.331647 0.064 Uiso 1 1 calc R U . . .
H52B H 0.620266 0.371758 0.404338 0.064 Uiso 1 1 calc R U . . .
H52C H 0.534064 0.408857 0.389674 0.064 Uiso 1 1 calc R U . . .
C53 C 0.1515(3) 0.3804(2) 0.4467(3) 0.0676(12) Uani 1 1 d . . . . .
H53A H 0.209606 0.380584 0.437952 0.101 Uiso 1 1 calc R U . . .
H53B H 0.127962 0.340698 0.438032 0.101 Uiso 1 1 calc R U . . .
H53C H 0.151975 0.392703 0.501979 0.101 Uiso 1 1 calc R U . . .
C54 C 0.1000(3) 0.4201(2) 0.3913(3) 0.0679(12) Uani 1 1 d . . . . .
N1 N 0.44886(18) 0.59337(12) 0.87452(16) 0.0390(6) Uani 1 1 d . . . . .
H1C H 0.447806 0.568088 0.826317 0.047 Uiso 1 1 calc R U . . .
N2 N 0.52387(17) 0.32896(11) 0.44129(16) 0.0374(6) Uani 1 1 d . . . . .
H2 H 0.534942 0.346776 0.496236 0.045 Uiso 1 1 calc R U . . .
N3 N 0.0595(3) 0.4527(2) 0.3484(3) 0.0890(14) 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 O2 1.762(2) . ?
Ti1 O3 1.822(2) . ?
Ti1 F1 1.8342(19) . ?
Ti1 F14 2.0018(18) . ?
Ti1 F3 2.0316(19) . ?
Ti1 F2 2.0326(19) . ?
Ti2 F6 1.771(2) . ?
Ti2 F5 1.780(2) . ?
Ti2 F4 1.781(2) . ?
Ti2 F3 1.944(2) . ?
Ti2 F8 1.9680(18) . ?
Ti2 F12 1.988(2) . ?
Ti3 O5 1.799(2) . ?
Ti3 F7 1.8246(18) . ?
Ti3 O4 1.829(2) . ?
Ti3 F9 2.0014(19) . ?
Ti3 F8 2.0138(18) . ?
Ti3 F14 2.0369(18) . ?
Ti4 F11 1.769(2) . ?
Ti4 F10 1.771(2) . ?
Ti4 F13 1.776(2) . ?
Ti4 F9 1.9825(19) . ?
Ti4 F2 1.984(2) . ?
Ti4 F12 1.992(2) . ?
O1 C3 1.373(4) . ?
O1 H1 0.8400 . ?
O2 C11 1.361(4) . ?
O3 C19 1.357(4) . ?
O4 C33 1.367(3) . ?
O5 C41 1.369(4) . ?
O6 C49 1.376(4) . ?
O6 H6 0.8400 . ?
C1 C2 1.504(5) . ?
C1 N1 1.523(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.382(5) . ?
C2 C3 1.399(5) . ?
C3 C4 1.392(5) . ?
C4 C5 1.404(5) . ?
C4 C9 1.506(5) . ?
C5 C6 1.382(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.387(5) . ?
C6 C8 1.510(5) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 C10 1.503(5) . ?
C9 H9A 0.9900 . ?
C9 H9B 0.9900 . ?
C10 C16 1.392(5) . ?
C10 C11 1.397(5) . ?
C11 C12 1.390(5) . ?
C12 C13 1.396(5) . ?
C12 C17 1.504(5) . ?
C13 C14 1.393(5) . ?
C13 H13 0.9500 . ?
C14 C16 1.393(5) . ?
C14 C15 1.502(5) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16 0.9500 . ?
C17 C18 1.522(5) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C18 C23 1.390(5) . ?
C18 C19 1.405(5) . ?
C19 C20 1.410(4) . ?
C20 C21 1.392(5) . ?
C20 C25 1.488(5) . ?
C21 C22 1.380(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.395(5) . ?
C22 C24 1.507(6) . ?
C23 H23 0.9500 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 N2 1.523(4) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 C27 1.493(5) . ?
C26 N2 1.506(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C28 1.396(5) . ?
C27 C33 1.413(4) . ?
C28 C29 1.391(5) . ?
C28 H28 0.9500 . ?
C29 C31 1.387(5) . ?
C29 C30 1.512(5) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 C32 1.397(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(4) . ?
C32 C34 1.512(4) . ?
C34 C35 1.513(5) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 C36 1.386(5) . ?
C35 C41 1.404(5) . ?
C36 C37 1.383(5) . ?
C36 H36 0.9500 . ?
C37 C39 1.395(5) . ?
C37 C38 1.518(5) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C40 1.390(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.386(5) . ?
C40 C42 1.517(5) . ?
C42 C43 1.518(5) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C43 C44 1.385(5) . ?
C43 C49 1.395(5) . ?
C44 C45 1.396(6) . ?
C44 H44 0.9500 . ?
C45 C47 1.382(5) . ?
C45 C46 1.509(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.394(5) . ?
C47 H47 0.9500 . ?
C48 C49 1.393(5) . ?
C48 C50 1.494(5) . ?
C50 N1 1.499(4) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 N1 1.490(4) . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 N2 1.498(4) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 C54 1.438(7) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 N3 1.142(7) . ?
N1 H1C 1.0000 . ?
N2 H2 1.0000 . ?

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
O2 Ti1 O3 95.06(11) . . ?
O2 Ti1 F1 98.77(10) . . ?
O3 Ti1 F1 97.96(9) . . ?
O2 Ti1 F14 94.01(9) . . ?
O3 Ti1 F14 91.73(9) . . ?
F1 Ti1 F14 163.17(9) . . ?
O2 Ti1 F3 87.41(10) . . ?
O3 Ti1 F3 175.51(9) . . ?
F1 Ti1 F3 85.34(8) . . ?
F14 Ti1 F3 84.34(8) . . ?
O2 Ti1 F2 170.27(10) . . ?
O3 Ti1 F2 92.21(9) . . ?
F1 Ti1 F2 86.58(9) . . ?
F14 Ti1 F2 79.30(8) . . ?
F3 Ti1 F2 84.93(8) . . ?
F6 Ti2 F5 97.60(10) . . ?
F6 Ti2 F4 96.63(10) . . ?
F5 Ti2 F4 95.67(10) . . ?
F6 Ti2 F3 167.61(9) . . ?
F5 Ti2 F3 91.30(9) . . ?
F4 Ti2 F3 91.02(9) . . ?
F6 Ti2 F8 88.87(9) . . ?
F5 Ti2 F8 88.97(9) . . ?
F4 Ti2 F8 172.26(9) . . ?
F3 Ti2 F8 82.66(8) . . ?
F6 Ti2 F12 89.47(10) . . ?
F5 Ti2 F12 169.90(10) . . ?
F4 Ti2 F12 90.65(9) . . ?
F3 Ti2 F12 80.69(8) . . ?
F8 Ti2 F12 83.93(8) . . ?
O5 Ti3 F7 97.83(10) . . ?
O5 Ti3 O4 99.10(10) . . ?
F7 Ti3 O4 99.86(9) . . ?
O5 Ti3 F9 91.80(9) . . ?
F7 Ti3 F9 165.39(8) . . ?
O4 Ti3 F9 89.37(9) . . ?
O5 Ti3 F8 88.39(9) . . ?
F7 Ti3 F8 86.83(8) . . ?
O4 Ti3 F8 169.11(9) . . ?
F9 Ti3 F8 82.46(8) . . ?
O5 Ti3 F14 171.02(9) . . ?
F7 Ti3 F14 86.35(8) . . ?
O4 Ti3 F14 87.94(9) . . ?
F9 Ti3 F14 82.66(7) . . ?
F8 Ti3 F14 83.90(7) . . ?
F11 Ti4 F10 97.51(11) . . ?
F11 Ti4 F13 96.32(10) . . ?
F10 Ti4 F13 96.37(11) . . ?
F11 Ti4 F9 169.87(10) . . ?
F10 Ti4 F9 90.07(10) . . ?
F13 Ti4 F9 89.47(9) . . ?
F11 Ti4 F2 89.22(10) . . ?
F10 Ti4 F2 169.76(9) . . ?
F13 Ti4 F2 90.51(9) . . ?
F9 Ti4 F2 82.40(8) . . ?
F11 Ti4 F12 89.68(9) . . ?
F10 Ti4 F12 88.21(10) . . ?
F13 Ti4 F12 171.90(9) . . ?
F9 Ti4 F12 83.83(8) . . ?
F2 Ti4 F12 84.11(8) . . ?
C3 O1 H1 109.5 . . ?
C11 O2 Ti1 162.3(2) . . ?
C19 O3 Ti1 148.3(2) . . ?
C33 O4 Ti3 133.1(2) . . ?
C41 O5 Ti3 161.3(2) . . ?
C49 O6 H6 109.5 . . ?
Ti4 F2 Ti1 148.56(10) . . ?
Ti2 F3 Ti1 152.19(10) . . ?
Ti2 F8 Ti3 151.71(10) . . ?
Ti4 F9 Ti3 150.16(10) . . ?
Ti2 F12 Ti4 151.61(11) . . ?
Ti1 F14 Ti3 148.73(10) . . ?
C2 C1 N1 110.4(3) . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1B 109.6 . . ?
N1 C1 H1B 109.6 . . ?
H1A C1 H1B 108.1 . . ?
C7 C2 C3 119.6(3) . . ?
C7 C2 C1 121.2(3) . . ?
C3 C2 C1 119.1(3) . . ?
O1 C3 C4 124.5(3) . . ?
O1 C3 C2 114.2(3) . . ?
C4 C3 C2 121.2(3) . . ?
C3 C4 C5 117.0(3) . . ?
C3 C4 C9 120.0(3) . . ?
C5 C4 C9 122.7(3) . . ?
C6 C5 C4 122.4(3) . . ?
C6 C5 H5 118.8 . . ?
C4 C5 H5 118.8 . . ?
C5 C6 C7 118.8(3) . . ?
C5 C6 C8 119.9(3) . . ?
C7 C6 C8 121.3(3) . . ?
C2 C7 C6 120.6(3) . . ?
C2 C7 H7 119.7 . . ?
C6 C7 H7 119.7 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C10 C9 C4 120.3(3) . . ?
C10 C9 H9A 107.2 . . ?
C4 C9 H9A 107.2 . . ?
C10 C9 H9B 107.2 . . ?
C4 C9 H9B 107.2 . . ?
H9A C9 H9B 106.9 . . ?
C16 C10 C11 116.7(3) . . ?
C16 C10 C9 126.2(3) . . ?
C11 C10 C9 116.8(3) . . ?
O2 C11 C12 118.7(3) . . ?
O2 C11 C10 117.9(3) . . ?
C12 C11 C10 123.4(3) . . ?
C11 C12 C13 117.7(3) . . ?
C11 C12 C17 120.4(3) . . ?
C13 C12 C17 121.9(3) . . ?
C14 C13 C12 121.0(3) . . ?
C14 C13 H13 119.5 . . ?
C12 C13 H13 119.5 . . ?
C13 C14 C16 119.0(3) . . ?
C13 C14 C15 120.8(4) . . ?
C16 C14 C15 120.1(3) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C16 C14 122.1(3) . . ?
C10 C16 H16 118.9 . . ?
C14 C16 H16 118.9 . . ?
C12 C17 C18 112.3(3) . . ?
C12 C17 H17A 109.2 . . ?
C18 C17 H17A 109.2 . . ?
C12 C17 H17B 109.2 . . ?
C18 C17 H17B 109.2 . . ?
H17A C17 H17B 107.9 . . ?
C23 C18 C19 117.7(3) . . ?
C23 C18 C17 119.2(3) . . ?
C19 C18 C17 123.0(3) . . ?
O3 C19 C18 123.0(3) . . ?
O3 C19 C20 117.0(3) . . ?
C18 C19 C20 119.9(3) . . ?
C21 C20 C19 120.0(3) . . ?
C21 C20 C25 121.3(3) . . ?
C19 C20 C25 118.6(3) . . ?
C22 C21 C20 121.2(3) . . ?
C22 C21 H21 119.4 . . ?
C20 C21 H21 119.4 . . ?
C21 C22 C23 117.9(4) . . ?
C21 C22 C24 120.8(4) . . ?
C23 C22 C24 121.3(4) . . ?
C18 C23 C22 123.3(3) . . ?
C18 C23 H23 118.3 . . ?
C22 C23 H23 118.3 . . ?
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 . . ?
C20 C25 N2 113.6(3) . . ?
C20 C25 H25A 108.8 . . ?
N2 C25 H25A 108.8 . . ?
C20 C25 H25B 108.8 . . ?
N2 C25 H25B 108.8 . . ?
H25A C25 H25B 107.7 . . ?
C27 C26 N2 116.3(3) . . ?
C27 C26 H26A 108.2 . . ?
N2 C26 H26A 108.2 . . ?
C27 C26 H26B 108.2 . . ?
N2 C26 H26B 108.2 . . ?
H26A C26 H26B 107.4 . . ?
C28 C27 C33 119.0(3) . . ?
C28 C27 C26 118.0(3) . . ?
C33 C27 C26 122.9(3) . . ?
C29 C28 C27 121.6(3) . . ?
C29 C28 H28 119.2 . . ?
C27 C28 H28 119.2 . . ?
C31 C29 C28 117.7(3) . . ?
C31 C29 C30 121.7(3) . . ?
C28 C29 C30 120.6(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 C32 122.8(3) . . ?
C29 C31 H31 118.6 . . ?
C32 C31 H31 118.6 . . ?
C33 C32 C31 118.4(3) . . ?
C33 C32 C34 121.7(3) . . ?
C31 C32 C34 119.9(3) . . ?
O4 C33 C32 122.3(3) . . ?
O4 C33 C27 117.3(3) . . ?
C32 C33 C27 120.4(3) . . ?
C32 C34 C35 109.9(3) . . ?
C32 C34 H34A 109.7 . . ?
C35 C34 H34A 109.7 . . ?
C32 C34 H34B 109.7 . . ?
C35 C34 H34B 109.7 . . ?
H34A C34 H34B 108.2 . . ?
C36 C35 C41 118.1(3) . . ?
C36 C35 C34 121.6(3) . . ?
C41 C35 C34 120.1(3) . . ?
C37 C36 C35 121.9(3) . . ?
C37 C36 H36 119.0 . . ?
C35 C36 H36 119.0 . . ?
C36 C37 C39 118.4(3) . . ?
C36 C37 C38 121.0(3) . . ?
C39 C37 C38 120.5(3) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C37 121.6(3) . . ?
C40 C39 H39 119.2 . . ?
C37 C39 H39 119.2 . . ?
C41 C40 C39 118.3(3) . . ?
C41 C40 C42 122.3(3) . . ?
C39 C40 C42 119.4(3) . . ?
O5 C41 C40 120.1(3) . . ?
O5 C41 C35 118.3(3) . . ?
C40 C41 C35 121.5(3) . . ?
C40 C42 C43 113.0(3) . . ?
C40 C42 H42A 109.0 . . ?
C43 C42 H42A 109.0 . . ?
C40 C42 H42B 109.0 . . ?
C43 C42 H42B 109.0 . . ?
H42A C42 H42B 107.8 . . ?
C44 C43 C49 117.9(3) . . ?
C44 C43 C42 121.4(3) . . ?
C49 C43 C42 120.7(3) . . ?
C43 C44 C45 122.6(3) . . ?
C43 C44 H44 118.7 . . ?
C45 C44 H44 118.7 . . ?
C47 C45 C44 117.8(4) . . ?
C47 C45 C46 121.1(4) . . ?
C44 C45 C46 121.1(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C45 C47 C48 121.5(4) . . ?
C45 C47 H47 119.2 . . ?
C48 C47 H47 119.2 . . ?
C49 C48 C47 118.9(3) . . ?
C49 C48 C50 120.5(3) . . ?
C47 C48 C50 120.6(3) . . ?
O6 C49 C48 115.8(3) . . ?
O6 C49 C43 123.1(3) . . ?
C48 C49 C43 121.1(3) . . ?
C48 C50 N1 113.0(3) . . ?
C48 C50 H50A 109.0 . . ?
N1 C50 H50A 109.0 . . ?
C48 C50 H50B 109.0 . . ?
N1 C50 H50B 109.0 . . ?
H50A C50 H50B 107.8 . . ?
N1 C51 H51A 109.5 . . ?
N1 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
N1 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
N2 C52 H52A 109.5 . . ?
N2 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
N2 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C54 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C54 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N3 C54 C53 178.5(6) . . ?
C51 N1 C50 111.4(3) . . ?
C51 N1 C1 112.7(3) . . ?
C50 N1 C1 111.6(2) . . ?
C51 N1 H1C 106.9 . . ?
C50 N1 H1C 106.9 . . ?
C1 N1 H1C 106.9 . . ?
C52 N2 C26 114.0(3) . . ?
C52 N2 C25 111.4(3) . . ?
C26 N2 C25 107.3(2) . . ?
C52 N2 H2 108.0 . . ?
C26 N2 H2 108.0 . . ?
C25 N2 H2 108.0 . . ?

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
O3 Ti1 O2 C11 7.7(7) . . . . ?
F1 Ti1 O2 C11 106.5(7) . . . . ?
F14 Ti1 O2 C11 -84.4(7) . . . . ?
F3 Ti1 O2 C11 -168.6(7) . . . . ?
O2 Ti1 O3 C19 -7.5(4) . . . . ?
F1 Ti1 O3 C19 -107.1(4) . . . . ?
F14 Ti1 O3 C19 86.7(4) . . . . ?
F2 Ti1 O3 C19 166.1(4) . . . . ?
O5 Ti3 O4 C33 -39.7(3) . . . . ?
F7 Ti3 O4 C33 -139.4(2) . . . . ?
F9 Ti3 O4 C33 52.0(3) . . . . ?
F8 Ti3 O4 C33 93.3(5) . . . . ?
F14 Ti3 O4 C33 134.7(3) . . . . ?
F7 Ti3 O5 C41 123.2(7) . . . . ?
O4 Ti3 O5 C41 21.8(7) . . . . ?
F9 Ti3 O5 C41 -67.8(7) . . . . ?
F8 Ti3 O5 C41 -150.2(7) . . . . ?
N1 C1 C2 C7 -123.9(3) . . . . ?
N1 C1 C2 C3 54.7(4) . . . . ?
C7 C2 C3 O1 -177.9(3) . . . . ?
C1 C2 C3 O1 3.4(4) . . . . ?
C7 C2 C3 C4 5.7(5) . . . . ?
C1 C2 C3 C4 -173.0(3) . . . . ?
O1 C3 C4 C5 -179.7(3) . . . . ?
C2 C3 C4 C5 -3.7(5) . . . . ?
O1 C3 C4 C9 -4.9(5) . . . . ?
C2 C3 C4 C9 171.1(3) . . . . ?
C3 C4 C5 C6 -1.5(5) . . . . ?
C9 C4 C5 C6 -176.1(3) . . . . ?
C4 C5 C6 C7 4.5(5) . . . . ?
C4 C5 C6 C8 -176.6(4) . . . . ?
C3 C2 C7 C6 -2.5(5) . . . . ?
C1 C2 C7 C6 176.1(3) . . . . ?
C5 C6 C7 C2 -2.5(5) . . . . ?
C8 C6 C7 C2 178.7(4) . . . . ?
C3 C4 C9 C10 152.8(3) . . . . ?
C5 C4 C9 C10 -32.7(5) . . . . ?
C4 C9 C10 C16 -24.4(6) . . . . ?
C4 C9 C10 C11 162.0(3) . . . . ?
Ti1 O2 C11 C12 -43.9(8) . . . . ?
Ti1 O2 C11 C10 136.1(6) . . . . ?
C16 C10 C11 O2 -178.4(3) . . . . ?
C9 C10 C11 O2 -4.1(5) . . . . ?
C16 C10 C11 C12 1.7(5) . . . . ?
C9 C10 C11 C12 175.9(3) . . . . ?
O2 C11 C12 C13 179.2(3) . . . . ?
C10 C11 C12 C13 -0.9(5) . . . . ?
O2 C11 C12 C17 1.2(5) . . . . ?
C10 C11 C12 C17 -178.9(3) . . . . ?
C11 C12 C13 C14 -0.7(5) . . . . ?
C17 C12 C13 C14 177.3(3) . . . . ?
C12 C13 C14 C16 1.3(5) . . . . ?
C12 C13 C14 C15 -177.9(4) . . . . ?
C11 C10 C16 C14 -1.0(5) . . . . ?
C9 C10 C16 C14 -174.6(3) . . . . ?
C13 C14 C16 C10 -0.4(5) . . . . ?
C15 C14 C16 C10 178.7(4) . . . . ?
C11 C12 C17 C18 84.9(4) . . . . ?
C13 C12 C17 C18 -93.0(4) . . . . ?
C12 C17 C18 C23 89.2(4) . . . . ?
C12 C17 C18 C19 -92.3(4) . . . . ?
Ti1 O3 C19 C18 42.7(5) . . . . ?
Ti1 O3 C19 C20 -141.0(3) . . . . ?
C23 C18 C19 O3 178.9(3) . . . . ?
C17 C18 C19 O3 0.3(5) . . . . ?
C23 C18 C19 C20 2.7(5) . . . . ?
C17 C18 C19 C20 -175.9(3) . . . . ?
O3 C19 C20 C21 -178.9(3) . . . . ?
C18 C19 C20 C21 -2.4(5) . . . . ?
O3 C19 C20 C25 -2.7(4) . . . . ?
C18 C19 C20 C25 173.7(3) . . . . ?
C19 C20 C21 C22 0.2(5) . . . . ?
C25 C20 C21 C22 -175.9(3) . . . . ?
C20 C21 C22 C23 1.7(6) . . . . ?
C20 C21 C22 C24 -179.5(4) . . . . ?
C19 C18 C23 C22 -0.8(5) . . . . ?
C17 C18 C23 C22 177.9(3) . . . . ?
C21 C22 C23 C18 -1.4(6) . . . . ?
C24 C22 C23 C18 179.8(4) . . . . ?
C21 C20 C25 N2 -103.5(4) . . . . ?
C19 C20 C25 N2 80.4(4) . . . . ?
N2 C26 C27 C28 132.9(3) . . . . ?
N2 C26 C27 C33 -50.4(4) . . . . ?
C33 C27 C28 C29 -1.7(5) . . . . ?
C26 C27 C28 C29 175.2(3) . . . . ?
C27 C28 C29 C31 3.4(5) . . . . ?
C27 C28 C29 C30 -177.3(3) . . . . ?
C28 C29 C31 C32 -2.1(5) . . . . ?
C30 C29 C31 C32 178.7(3) . . . . ?
C29 C31 C32 C33 -1.0(5) . . . . ?
C29 C31 C32 C34 178.3(3) . . . . ?
Ti3 O4 C33 C32 68.0(4) . . . . ?
Ti3 O4 C33 C27 -109.4(3) . . . . ?
C31 C32 C33 O4 -174.5(3) . . . . ?
C34 C32 C33 O4 6.2(5) . . . . ?
C31 C32 C33 C27 2.9(5) . . . . ?
C34 C32 C33 C27 -176.5(3) . . . . ?
C28 C27 C33 O4 175.9(3) . . . . ?
C26 C27 C33 O4 -0.8(5) . . . . ?
C28 C27 C33 C32 -1.6(5) . . . . ?
C26 C27 C33 C32 -178.3(3) . . . . ?
C33 C32 C34 C35 -106.2(3) . . . . ?
C31 C32 C34 C35 74.5(4) . . . . ?
C32 C34 C35 C36 -96.7(3) . . . . ?
C32 C34 C35 C41 78.4(4) . . . . ?
C41 C35 C36 C37 -1.8(5) . . . . ?
C34 C35 C36 C37 173.4(3) . . . . ?
C35 C36 C37 C39 2.6(5) . . . . ?
C35 C36 C37 C38 -174.8(3) . . . . ?
C36 C37 C39 C40 -1.4(5) . . . . ?
C38 C37 C39 C40 176.0(3) . . . . ?
C37 C39 C40 C41 -0.5(5) . . . . ?
C37 C39 C40 C42 179.2(3) . . . . ?
Ti3 O5 C41 C40 134.5(6) . . . . ?
Ti3 O5 C41 C35 -45.6(8) . . . . ?
C39 C40 C41 O5 -178.8(3) . . . . ?
C42 C40 C41 O5 1.5(5) . . . . ?
C39 C40 C41 C35 1.3(5) . . . . ?
C42 C40 C41 C35 -178.4(3) . . . . ?
C36 C35 C41 O5 179.9(3) . . . . ?
C34 C35 C41 O5 4.6(4) . . . . ?
C36 C35 C41 C40 -0.2(5) . . . . ?
C34 C35 C41 C40 -175.5(3) . . . . ?
C41 C40 C42 C43 106.1(4) . . . . ?
C39 C40 C42 C43 -73.6(4) . . . . ?
C40 C42 C43 C44 105.5(4) . . . . ?
C40 C42 C43 C49 -73.6(4) . . . . ?
C49 C43 C44 C45 -2.5(6) . . . . ?
C42 C43 C44 C45 178.4(3) . . . . ?
C43 C44 C45 C47 -0.1(6) . . . . ?
C43 C44 C45 C46 -179.3(4) . . . . ?
C44 C45 C47 C48 2.8(6) . . . . ?
C46 C45 C47 C48 -178.0(4) . . . . ?
C45 C47 C48 C49 -2.8(6) . . . . ?
C45 C47 C48 C50 175.5(3) . . . . ?
C47 C48 C49 O6 -179.5(3) . . . . ?
C50 C48 C49 O6 2.2(5) . . . . ?
C47 C48 C49 C43 0.1(5) . . . . ?
C50 C48 C49 C43 -178.2(3) . . . . ?
C44 C43 C49 O6 -178.0(3) . . . . ?
C42 C43 C49 O6 1.1(5) . . . . ?
C44 C43 C49 C48 2.5(5) . . . . ?
C42 C43 C49 C48 -178.4(3) . . . . ?
C49 C48 C50 N1 -52.7(4) . . . . ?
C47 C48 C50 N1 129.0(3) . . . . ?
C48 C50 N1 C51 -61.8(4) . . . . ?
C48 C50 N1 C1 171.3(3) . . . . ?
C2 C1 N1 C51 57.7(4) . . . . ?
C2 C1 N1 C50 -176.1(3) . . . . ?
C27 C26 N2 C52 -39.6(4) . . . . ?
C27 C26 N2 C25 -163.4(3) . . . . ?
C20 C25 N2 C52 69.2(3) . . . . ?
C20 C25 N2 C26 -165.3(3) . . . . ?

_refine_diff_density_max         1.499
_refine_diff_density_min         -0.518
_refine_diff_density_rms         0.093




####################################################################### 
# 
# 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 2057321'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_vrf_PLAT201_2                   
;
RESPONSE: There is small-scale disorder in the ligand.
 This small-scale disorder was modelled using isotropic 
displacement parameters.     
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;  
C136 H164 O19 Ti4 [MeCN]
;
_chemical_formula_sum            'C136 H164 O19 Ti4'
_chemical_formula_weight         2294.26

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   28.1243(7)
_cell_length_b                   17.7721(4)
_cell_length_c                   31.2326(9)
_cell_angle_alpha                90
_cell_angle_beta                 113.009(3)
_cell_angle_gamma                90
_cell_volume                     14369.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    6769
_cell_measurement_theta_min      3.422
_cell_measurement_theta_max      62.826

_exptl_crystal_description       lath
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_F_000             4880
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.160
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.010
_exptl_absorpt_coefficient_mu    2.275
_shelx_estimated_absorpt_T_min   0.712
_shelx_estimated_absorpt_T_max   0.978
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.52429
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            46006
_diffrn_reflns_av_unetI/netI     0.0938
_diffrn_reflns_av_R_equivalents  0.0985
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         3.016
_diffrn_reflns_theta_max         66.594
_diffrn_reflns_theta_full        66.594
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measured_fraction_theta_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_reflns_number_total             12485
_reflns_number_gt                7979
_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.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.500 0.000 423 -4 ' '
2 0.000 0.862 0.250 107 24 ' '
3 0.000 0.500 0.500 423 -4 ' '
4 0.000 0.138 0.750 107 24 ' '
5 0.218 0.145 0.250 20 0 ' '
6 0.218 0.855 0.750 20 0 ' '
7 0.282 0.645 0.250 20 0 ' '
8 0.282 0.355 0.750 20 0 ' '
9 0.500 1.000 0.500 423 -4 ' '
10 0.500 0.000 1.000 423 -4 ' '
11 0.500 0.362 0.250 107 24 ' '
12 0.500 0.638 0.750 107 24 ' '
13 0.718 0.645 0.250 20 0 ' '
14 0.718 0.355 0.750 20 0 ' '
15 0.782 0.145 0.250 20 0 ' '
16 0.782 0.855 0.750 20 0 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Extra solvent modelled as one MeCN per pocket (22e)
;


_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.1274P)²+11.6039P] 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         12485
_refine_ls_number_parameters     697
_refine_ls_number_restraints     48
_refine_ls_R_factor_all          0.1277
_refine_ls_R_factor_gt           0.0848
_refine_ls_wR_factor_ref         0.2337
_refine_ls_wR_factor_gt          0.2076
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.027
_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
C1 C 0.4104(2) 0.1798(3) 0.74285(16) 0.0501(12) Uani 1 1 d . . . . .
C2 C 0.4439(2) 0.1273(3) 0.77261(16) 0.0616(15) Uani 1 1 d . . . . .
C6 C 0.3694(2) 0.1571(3) 0.70249(16) 0.0698(18) Uani 1 1 d . . . . .
O9 O 0.4941(2) 0.4553(3) 0.7704(2) 0.0485(15) Uani 0.5 1 d . . P . .
C3A C 0.4439(3) 0.0508(4) 0.7626(3) 0.054(2) Uiso 0.664(6) 1 d . U P A 1
H3A H 0.469960 0.018172 0.782467 0.065 Uiso 0.664(6) 1 calc R U P A 1
C4A C 0.4041(3) 0.0232(5) 0.7219(3) 0.060(2) Uiso 0.664(6) 1 d . U P A 1
C5A C 0.3708(3) 0.0761(4) 0.6928(3) 0.054(2) Uiso 0.664(6) 1 d . U P A 1
H5A H 0.346559 0.058399 0.663775 0.064 Uiso 0.664(6) 1 calc R U P A 1
C7A C 0.3970(4) -0.0605(6) 0.7086(4) 0.083(3) Uiso 0.664(6) 1 d . U P A 1
C8A C 0.3416(5) -0.0833(9) 0.6959(6) 0.119(4) Uiso 0.664(6) 1 d . U P A 1
H8A1 H 0.332194 -0.075705 0.722684 0.178 Uiso 0.664(6) 1 calc R U P A 1
H8A2 H 0.319105 -0.052556 0.669763 0.178 Uiso 0.664(6) 1 calc R U P A 1
H8A3 H 0.337307 -0.136509 0.686928 0.178 Uiso 0.664(6) 1 calc R U P A 1
C9A C 0.4109(5) -0.0722(7) 0.6677(4) 0.098(3) Uiso 0.664(6) 1 d . U P A 1
H9A1 H 0.390322 -0.038465 0.642430 0.147 Uiso 0.664(6) 1 calc R U P A 1
H9A2 H 0.447708 -0.061371 0.676531 0.147 Uiso 0.664(6) 1 calc R U P A 1
H9A3 H 0.403911 -0.124546 0.657182 0.147 Uiso 0.664(6) 1 calc R U P A 1
C10A C 0.4268(7) -0.1101(9) 0.7487(6) 0.140(5) Uiso 0.664(6) 1 d . U P A 1
H10A H 0.416233 -0.100246 0.774614 0.211 Uiso 0.664(6) 1 calc R U P A 1
H10B H 0.420022 -0.162948 0.739306 0.211 Uiso 0.664(6) 1 calc R U P A 1
H10C H 0.463819 -0.099773 0.758656 0.211 Uiso 0.664(6) 1 calc R U P A 1
C3B C 0.4150(5) 0.0563(7) 0.7628(4) 0.038(3) Uiso 0.336(6) 1 d . U P A 2
H3B H 0.430239 0.017397 0.784798 0.045 Uiso 0.336(6) 1 calc R U P A 2
C4B C 0.3682(6) 0.0365(8) 0.7259(5) 0.049(4) Uiso 0.336(6) 1 d . U P A 2
C5B C 0.3419(5) 0.0965(7) 0.6963(4) 0.039(3) Uiso 0.336(6) 1 d . U P A 2
H5B H 0.307405 0.092781 0.674091 0.046 Uiso 0.336(6) 1 calc R U P A 2
C7B C 0.3481(7) -0.0414(11) 0.7182(7) 0.072(5) Uiso 0.336(6) 1 d . U P A 2
C8B C 0.2922(7) -0.0440(11) 0.7160(7) 0.074(5) Uiso 0.336(6) 1 d . U P A 2
H8B1 H 0.279514 -0.095914 0.710902 0.111 Uiso 0.336(6) 1 calc R U P A 2
H8B2 H 0.291778 -0.025395 0.745418 0.111 Uiso 0.336(6) 1 calc R U P A 2
H8B3 H 0.269906 -0.012213 0.690385 0.111 Uiso 0.336(6) 1 calc R U P A 2
C9B C 0.3450(6) -0.0673(10) 0.6669(6) 0.063(4) Uiso 0.336(6) 1 d . U P A 2
H9B1 H 0.331761 -0.118921 0.660516 0.094 Uiso 0.336(6) 1 calc R U P A 2
H9B2 H 0.321804 -0.033455 0.643146 0.094 Uiso 0.336(6) 1 calc R U P A 2
H9B3 H 0.379556 -0.065188 0.666324 0.094 Uiso 0.336(6) 1 calc R U P A 2
C10B C 0.3840(8) -0.1012(11) 0.7501(7) 0.081(6) Uiso 0.336(6) 1 d . U P A 2
H10D H 0.367514 -0.150699 0.742439 0.121 Uiso 0.336(6) 1 calc R U P A 2
H10E H 0.416659 -0.102004 0.745648 0.121 Uiso 0.336(6) 1 calc R U P A 2
H10F H 0.390926 -0.089054 0.782593 0.121 Uiso 0.336(6) 1 calc R U P A 2
C11 C 0.3337(2) 0.2139(3) 0.66857(16) 0.0628(15) Uani 1 1 d . . . . .
H11A H 0.300152 0.214904 0.671900 0.075 Uiso 1 1 calc R U . . .
H11B H 0.349187 0.264796 0.675880 0.075 Uiso 1 1 calc R U . . .
C12 C 0.36667(18) 0.1997(3) 0.60536(16) 0.0498(12) Uani 1 1 d . . . . .
C13 C 0.32528(19) 0.1936(3) 0.61943(17) 0.0567(13) Uani 1 1 d . . . . .
C14 C 0.2794(2) 0.1604(3) 0.58904(17) 0.0634(15) Uani 1 1 d . . . . .
H14 H 0.250917 0.157125 0.598107 0.076 Uiso 1 1 calc R U . . .
C15 C 0.2742(2) 0.1320(3) 0.54589(17) 0.0615(15) Uani 1 1 d . . . . .
C16 C 0.3175(2) 0.1345(3) 0.53533(17) 0.0577(14) Uani 1 1 d . . . . .
H16 H 0.315268 0.113182 0.506734 0.069 Uiso 1 1 calc R U . . .
C17 C 0.3645(2) 0.1669(3) 0.56449(16) 0.0525(12) Uani 1 1 d . . . . .
C18 C 0.2230(2) 0.1005(3) 0.51094(18) 0.0697(17) Uani 1 1 d . . . . .
C19 C 0.1813(2) 0.0983(4) 0.5306(2) 0.084(2) Uani 1 1 d . . . . .
H19A H 0.175718 0.149159 0.539871 0.126 Uiso 1 1 calc R U . . .
H19B H 0.149076 0.079345 0.506835 0.126 Uiso 1 1 calc R U . . .
H19C H 0.192280 0.065038 0.557775 0.126 Uiso 1 1 calc R U . . .
C20 C 0.2307(3) 0.0208(3) 0.4969(2) 0.0807(19) Uani 1 1 d . . . . .
H20A H 0.257457 0.020904 0.484123 0.121 Uiso 1 1 calc R U . . .
H20B H 0.241413 -0.012081 0.524262 0.121 Uiso 1 1 calc R U . . .
H20C H 0.198209 0.002226 0.473322 0.121 Uiso 1 1 calc R U . . .
C21 C 0.2048(3) 0.1505(4) 0.4677(2) 0.093(2) Uani 1 1 d . . . . .
H21A H 0.231506 0.152159 0.454888 0.140 Uiso 1 1 calc R U . . .
H21B H 0.172854 0.129974 0.444383 0.140 Uiso 1 1 calc R U . . .
H21C H 0.198417 0.201511 0.476175 0.140 Uiso 1 1 calc R U . . .
C22 C 0.4121(2) 0.1591(3) 0.55304(17) 0.0552(12) Uani 1 1 d . . . . .
H22A H 0.442990 0.159660 0.582637 0.066 Uiso 1 1 calc R U . . .
H22B H 0.410872 0.109132 0.538604 0.066 Uiso 1 1 calc R U . . .
C23 C 0.44582(18) 0.2850(3) 0.53851(15) 0.0453(11) Uani 1 1 d . . . . .
C24 C 0.4197(2) 0.2181(3) 0.52111(16) 0.0540(12) Uani 1 1 d . . . . .
C28 C 0.45517(19) 0.3368(3) 0.50921(16) 0.0477(11) Uani 1 1 d . . . . .
C25A C 0.3934(5) 0.2104(6) 0.4719(4) 0.043(3) Uiso 0.480(12) 1 d . U P B 1
H25A H 0.369770 0.170025 0.459874 0.051 Uiso 0.480(12) 1 calc R U P B 1
C26A C 0.4013(5) 0.2605(7) 0.4409(4) 0.049(3) Uiso 0.480(12) 1 d . U P B 1
C27A C 0.4289(5) 0.3245(7) 0.4594(4) 0.047(3) Uiso 0.480(12) 1 d . U P B 1
H27A H 0.430980 0.362398 0.438734 0.056 Uiso 0.480(12) 1 calc R U P B 1
C29A C 0.3800(4) 0.2425(5) 0.3883(3) 0.047(3) Uiso 0.480(12) 1 d D U P B 1
C30A C 0.4062(8) 0.1701(9) 0.3790(8) 0.135(8) Uiso 0.480(12) 1 d D U P B 1
H30A H 0.405549 0.130217 0.400503 0.203 Uiso 0.480(12) 1 calc R U P B 1
H30B H 0.387349 0.153306 0.346924 0.203 Uiso 0.480(12) 1 calc R U P B 1
H30C H 0.442058 0.181299 0.383944 0.203 Uiso 0.480(12) 1 calc R U P B 1
C31A C 0.3769(8) 0.3092(8) 0.3598(7) 0.128(7) Uiso 0.480(12) 1 d D U P B 1
H31A H 0.363203 0.294883 0.326844 0.192 Uiso 0.480(12) 1 calc R U P B 1
H31B H 0.353909 0.346399 0.364886 0.192 Uiso 0.480(12) 1 calc R U P B 1
H31C H 0.411403 0.330972 0.368461 0.192 Uiso 0.480(12) 1 calc R U P B 1
C32A C 0.3221(6) 0.2135(11) 0.3731(7) 0.128(7) Uiso 0.480(12) 1 d D U P B 1
H32A H 0.321720 0.168519 0.391157 0.192 Uiso 0.480(12) 1 calc R U P B 1
H32B H 0.301073 0.252952 0.378953 0.192 Uiso 0.480(12) 1 calc R U P B 1
H32C H 0.307926 0.201001 0.339900 0.192 Uiso 0.480(12) 1 calc R U P B 1
C25B C 0.4121(5) 0.1998(6) 0.4751(4) 0.049(3) Uiso 0.520(12) 1 d . U P B 2
H25B H 0.400027 0.150729 0.464063 0.059 Uiso 0.520(12) 1 calc R U P B 2
C26B C 0.4213(5) 0.2494(7) 0.4451(4) 0.056(3) Uiso 0.520(12) 1 d . U P B 2
C27B C 0.4457(5) 0.3182(6) 0.4641(4) 0.045(3) Uiso 0.520(12) 1 d . U P B 2
H27B H 0.455625 0.351777 0.445356 0.054 Uiso 0.520(12) 1 calc R U P B 2
C29B C 0.4086(5) 0.2291(7) 0.3942(4) 0.075(4) Uiso 0.520(12) 1 d D U P B 2
C30B C 0.4503(7) 0.1645(9) 0.3960(7) 0.138(7) Uiso 0.520(12) 1 d D U P B 2
H30D H 0.448136 0.122935 0.415762 0.207 Uiso 0.520(12) 1 calc R U P B 2
H30E H 0.442649 0.145845 0.364487 0.207 Uiso 0.520(12) 1 calc R U P B 2
H30F H 0.485159 0.185942 0.408834 0.207 Uiso 0.520(12) 1 calc R U P B 2
C31B C 0.4148(6) 0.2877(7) 0.3643(5) 0.105(5) Uiso 0.520(12) 1 d D U P B 2
H31D H 0.405566 0.267769 0.332835 0.157 Uiso 0.520(12) 1 calc R U P B 2
H31E H 0.392283 0.330282 0.363358 0.157 Uiso 0.520(12) 1 calc R U P B 2
H31F H 0.450874 0.304630 0.376626 0.157 Uiso 0.520(12) 1 calc R U P B 2
C32B C 0.3566(5) 0.1860(7) 0.3735(5) 0.086(4) Uiso 0.520(12) 1 d D U P B 2
H32D H 0.355469 0.147734 0.395679 0.128 Uiso 0.520(12) 1 calc R U P B 2
H32E H 0.327957 0.221417 0.367352 0.128 Uiso 0.520(12) 1 calc R U P B 2
H32F H 0.353462 0.161629 0.344374 0.128 Uiso 0.520(12) 1 calc R U P B 2
C33 C 0.48277(18) 0.4083(3) 0.52909(17) 0.0483(11) Uani 1 1 d . . . . .
H33A H 0.514657 0.397528 0.556697 0.058 Uiso 1 1 calc R U . . .
H33B H 0.492492 0.434605 0.505741 0.058 Uiso 1 1 calc R U . . .
C34 C 0.47287(18) 0.4905(3) 0.58607(15) 0.0471(11) Uani 1 1 d . . . . .
H34A H 0.494162 0.533368 0.583646 0.057 Uiso 1 1 calc R U . . .
H34B H 0.495582 0.454596 0.609332 0.057 Uiso 1 1 calc R U . . .
C35 C 0.40565(16) 0.4684(3) 0.61969(14) 0.0433(11) Uani 1 1 d . . . . .
C36 C 0.43114(18) 0.5178(3) 0.60064(15) 0.0469(11) Uani 1 1 d . . . . .
C40 C 0.3642(2) 0.4931(4) 0.63032(16) 0.0630(15) Uani 1 1 d . . . . .
C37A C 0.4112(3) 0.5892(4) 0.5929(2) 0.0409(18) Uiso 0.675(9) 1 d . U P C 1
H37A H 0.426773 0.624315 0.579518 0.049 Uiso 0.675(9) 1 calc R U P C 1
C38A C 0.3698(3) 0.6146(4) 0.6032(3) 0.0460(18) Uiso 0.675(9) 1 d . U P C 1
C39A C 0.3459(3) 0.5614(5) 0.6214(3) 0.0482(19) Uiso 0.675(9) 1 d . U P C 1
H39A H 0.316329 0.575167 0.627197 0.058 Uiso 0.675(9) 1 calc R U P C 1
C41A C 0.3483(3) 0.6937(5) 0.5937(3) 0.060(2) Uiso 0.675(9) 1 d . U P C 1
C42A C 0.2953(3) 0.6922(5) 0.5536(3) 0.066(2) Uiso 0.675(9) 1 d . U P C 1
H42A H 0.281283 0.743359 0.547437 0.099 Uiso 0.675(9) 1 calc R U P C 1
H42B H 0.298661 0.672159 0.525686 0.099 Uiso 0.675(9) 1 calc R U P C 1
H42C H 0.271890 0.660036 0.561931 0.099 Uiso 0.675(9) 1 calc R U P C 1
C43A C 0.3827(4) 0.7469(5) 0.5791(4) 0.071(3) Uiso 0.675(9) 1 d . U P C 1
H43A H 0.367428 0.797357 0.573404 0.107 Uiso 0.675(9) 1 calc R U P C 1
H43B H 0.417260 0.749327 0.604082 0.107 Uiso 0.675(9) 1 calc R U P C 1
H43C H 0.385338 0.727863 0.550700 0.107 Uiso 0.675(9) 1 calc R U P C 1
C44A C 0.3423(4) 0.7278(6) 0.6372(4) 0.085(3) Uiso 0.675(9) 1 d . U P C 1
H44A H 0.328371 0.778862 0.630138 0.127 Uiso 0.675(9) 1 calc R U P C 1
H44B H 0.318719 0.696476 0.645813 0.127 Uiso 0.675(9) 1 calc R U P C 1
H44C H 0.376160 0.729393 0.663211 0.127 Uiso 0.675(9) 1 calc R U P C 1
C37B C 0.4322(8) 0.5997(10) 0.5997(6) 0.051(4) Uiso 0.325(9) 1 d . U P C 2
H37B H 0.455958 0.627926 0.591348 0.061 Uiso 0.325(9) 1 calc R U P C 2
C38B C 0.3946(8) 0.6320(11) 0.6126(6) 0.062(5) Uiso 0.325(9) 1 d . U P C 2
C39B C 0.3646(6) 0.5889(10) 0.6264(5) 0.046(4) Uiso 0.325(9) 1 d . U P C 2
H39B H 0.340262 0.614792 0.635175 0.056 Uiso 0.325(9) 1 calc R U P C 2
C41B C 0.3863(8) 0.7219(12) 0.6098(8) 0.081(6) Uiso 0.325(9) 1 d . U P C 2
C42B C 0.3306(11) 0.7358(19) 0.5834(10) 0.113(9) Uiso 0.325(9) 1 d . U P C 2
H42D H 0.310663 0.707788 0.597753 0.170 Uiso 0.325(9) 1 calc R U P C 2
H42E H 0.323522 0.789711 0.583872 0.170 Uiso 0.325(9) 1 calc R U P C 2
H42F H 0.320829 0.719106 0.551201 0.170 Uiso 0.325(9) 1 calc R U P C 2
C43B C 0.4208(10) 0.7604(14) 0.5922(9) 0.100(7) Uiso 0.325(9) 1 d . U P C 2
H43D H 0.456744 0.747871 0.611764 0.150 Uiso 0.325(9) 1 calc R U P C 2
H43E H 0.413135 0.744296 0.560154 0.150 Uiso 0.325(9) 1 calc R U P C 2
H43F H 0.415828 0.814901 0.592825 0.150 Uiso 0.325(9) 1 calc R U P C 2
C44B C 0.4058(12) 0.7455(19) 0.6637(11) 0.139(11) Uiso 0.325(9) 1 d . U P C 2
H44D H 0.383933 0.721242 0.677632 0.209 Uiso 0.325(9) 1 calc R U P C 2
H44E H 0.441680 0.729390 0.680264 0.209 Uiso 0.325(9) 1 calc R U P C 2
H44F H 0.403570 0.800282 0.666167 0.209 Uiso 0.325(9) 1 calc R U P C 2
C45 C 0.33426(19) 0.4390(4) 0.64804(17) 0.0716(18) Uani 1 1 d . . . . .
H45A H 0.299976 0.429330 0.623050 0.086 Uiso 1 1 calc R U . . .
H45B H 0.352990 0.390518 0.656217 0.086 Uiso 1 1 calc R U . . .
C46 C 0.36416(18) 0.4570(3) 0.73500(15) 0.0474(11) Uani 1 1 d . . . . .
C47 C 0.32711(19) 0.4701(4) 0.69038(18) 0.0750(19) Uani 1 1 d . . . . .
C51 C 0.36127(17) 0.4908(3) 0.77363(15) 0.0488(11) Uani 1 1 d . . . . .
C48A C 0.2817(3) 0.4982(5) 0.6855(3) 0.0481(19) Uiso 0.621(7) 1 d . U P D 1
H48A H 0.253147 0.494491 0.656455 0.058 Uiso 0.621(7) 1 calc R U P D 1
C49A C 0.2759(3) 0.5329(5) 0.7228(3) 0.0479(19) Uiso 0.621(7) 1 d . U P D 1
C50A C 0.3153(3) 0.5256(5) 0.7660(3) 0.0435(19) Uiso 0.621(7) 1 d . U P D 1
H50A H 0.310232 0.545912 0.792046 0.052 Uiso 0.621(7) 1 calc R U P D 1
C52A C 0.2278(4) 0.5806(5) 0.7154(3) 0.066(2) Uiso 0.621(7) 1 d . U P D 1
C53A C 0.2222(5) 0.6436(7) 0.6810(5) 0.097(4) Uiso 0.621(7) 1 d . U P D 1
H53A H 0.222360 0.622400 0.652052 0.145 Uiso 0.621(7) 1 calc R U P D 1
H53B H 0.189535 0.670113 0.674382 0.145 Uiso 0.621(7) 1 calc R U P D 1
H53C H 0.251024 0.678864 0.694214 0.145 Uiso 0.621(7) 1 calc R U P D 1
C54A C 0.2274(4) 0.6150(7) 0.7596(4) 0.088(3) Uiso 0.621(7) 1 d . U P D 1
H54A H 0.230984 0.575096 0.782320 0.131 Uiso 0.621(7) 1 calc R U P D 1
H54B H 0.256206 0.650403 0.772431 0.131 Uiso 0.621(7) 1 calc R U P D 1
H54C H 0.194717 0.641653 0.752598 0.131 Uiso 0.621(7) 1 calc R U P D 1
C55A C 0.1797(5) 0.5314(8) 0.6941(5) 0.109(4) Uiso 0.621(7) 1 d . U P D 1
H55A H 0.179080 0.508433 0.665392 0.163 Uiso 0.621(7) 1 calc R U P D 1
H55B H 0.180439 0.491840 0.716219 0.163 Uiso 0.621(7) 1 calc R U P D 1
H55C H 0.148786 0.562464 0.687128 0.163 Uiso 0.621(7) 1 calc R U P D 1
C48B C 0.2931(4) 0.5459(7) 0.6882(4) 0.042(3) Uiso 0.379(7) 1 d . U P D 2
H48B H 0.273414 0.567023 0.658565 0.051 Uiso 0.379(7) 1 calc R U P D 2
C49B C 0.2914(5) 0.5817(7) 0.7281(4) 0.044(3) Uiso 0.379(7) 1 d . U P D 2
C50B C 0.3273(4) 0.5586(7) 0.7709(4) 0.033(3) Uiso 0.379(7) 1 d . U P D 2
H50B H 0.330696 0.585045 0.798365 0.039 Uiso 0.379(7) 1 calc R U P D 2
C52B C 0.2545(5) 0.6492(8) 0.7216(5) 0.054(3) Uiso 0.379(7) 1 d . U P D 2
C53B C 0.2665(6) 0.7102(9) 0.6950(6) 0.069(4) Uiso 0.379(7) 1 d . U P D 2
H53D H 0.264651 0.690329 0.665073 0.104 Uiso 0.379(7) 1 calc R U P D 2
H53E H 0.241469 0.751099 0.689479 0.104 Uiso 0.379(7) 1 calc R U P D 2
H53F H 0.301396 0.729314 0.712731 0.104 Uiso 0.379(7) 1 calc R U P D 2
C54B C 0.2573(6) 0.6800(9) 0.7683(6) 0.072(4) Uiso 0.379(7) 1 d . U P D 2
H54D H 0.249366 0.639718 0.785820 0.109 Uiso 0.379(7) 1 calc R U P D 2
H54E H 0.292214 0.699152 0.786055 0.109 Uiso 0.379(7) 1 calc R U P D 2
H54F H 0.232286 0.720937 0.762803 0.109 Uiso 0.379(7) 1 calc R U P D 2
C55B C 0.1983(7) 0.6221(11) 0.6927(6) 0.078(5) Uiso 0.379(7) 1 d . U P D 2
H55D H 0.189254 0.581746 0.709489 0.117 Uiso 0.379(7) 1 calc R U P D 2
H55E H 0.174349 0.664287 0.687907 0.117 Uiso 0.379(7) 1 calc R U P D 2
H55F H 0.196129 0.603288 0.662485 0.117 Uiso 0.379(7) 1 calc R U P D 2
C56 C 0.40357(16) 0.4804(2) 0.82175(14) 0.0410(10) Uani 1 1 d . . . . .
H56A H 0.437459 0.482104 0.819020 0.049 Uiso 1 1 calc R U . . .
H56B H 0.402306 0.523255 0.841556 0.049 Uiso 1 1 calc R U . . .
C57 C 0.43024(15) 0.3457(3) 0.84526(14) 0.0378(9) Uani 1 1 d . . . . .
C58 C 0.40015(16) 0.4081(2) 0.84580(14) 0.0401(10) Uani 1 1 d . . . . .
C59 C 0.36874(17) 0.4021(3) 0.87084(15) 0.0453(11) Uani 1 1 d . . . . .
H59 H 0.348765 0.444525 0.872125 0.054 Uiso 1 1 calc R U . . .
C60 C 0.36540(17) 0.3374(3) 0.89381(15) 0.0448(10) Uani 1 1 d . . . . .
C61 C 0.39225(17) 0.2748(3) 0.88888(14) 0.0427(10) Uani 1 1 d . . . . .
H61 H 0.388890 0.228679 0.902856 0.051 Uiso 1 1 calc R U . . .
C62 C 0.42416(16) 0.2773(2) 0.86394(14) 0.0392(10) Uani 1 1 d . . . . .
C63 C 0.33648(18) 0.3376(3) 0.92648(17) 0.0510(12) Uani 1 1 d . . . . .
C64 C 0.2825(2) 0.3712(4) 0.9018(2) 0.0693(16) Uani 1 1 d . . . . .
H64A H 0.262637 0.340011 0.874849 0.104 Uiso 1 1 calc R U . . .
H64B H 0.264906 0.372691 0.923356 0.104 Uiso 1 1 calc R U . . .
H64C H 0.285483 0.422337 0.891401 0.104 Uiso 1 1 calc R U . . .
C65 C 0.3671(2) 0.3866(3) 0.96838(18) 0.0597(13) Uani 1 1 d . . . . .
H65A H 0.401732 0.365411 0.984385 0.090 Uiso 1 1 calc R U . . .
H65B H 0.369867 0.437720 0.957842 0.090 Uiso 1 1 calc R U . . .
H65C H 0.349290 0.388074 0.989797 0.090 Uiso 1 1 calc R U . . .
C66 C 0.3315(2) 0.2585(3) 0.9436(2) 0.0653(15) Uani 1 1 d . . . . .
H66A H 0.311930 0.226523 0.916924 0.098 Uiso 1 1 calc R U . . .
H66B H 0.366036 0.237042 0.960020 0.098 Uiso 1 1 calc R U . . .
H66C H 0.313475 0.261098 0.964762 0.098 Uiso 1 1 calc R U . . .
C67 C 0.44928(17) 0.2041(3) 0.85968(16) 0.0440(10) Uani 1 1 d . . . . .
H67A H 0.466477 0.181665 0.891009 0.053 Uiso 1 1 calc R U . . .
H67B H 0.422146 0.168673 0.840515 0.053 Uiso 1 1 calc R U . . .
C68 C 0.4920(2) 0.1485(3) 0.81336(16) 0.0523(12) Uani 1 1 d . . . . .
H68A H 0.503165 0.104984 0.834756 0.063 Uiso 1 1 calc R U . . .
H68B H 0.519685 0.158944 0.802031 0.063 Uiso 1 1 calc R U . . .
O1 O 0.41761(11) 0.25428(16) 0.75276(9) 0.0407(7) Uani 1 1 d . . . . .
O2 O 0.40994(11) 0.23701(18) 0.63434(10) 0.0487(8) Uani 1 1 d . . . . .
O3 O 0.46277(10) 0.30043(16) 0.58465(9) 0.0405(7) Uani 1 1 d . . . . .
O4 O 0.42013(11) 0.39546(18) 0.62685(10) 0.0465(7) Uani 1 1 d . . . . .
O5 O 0.40363(14) 0.41033(18) 0.73905(10) 0.0568(9) Uani 1 1 d . . . . .
O10 O 0.47310(11) 0.32236(18) 0.70881(10) 0.0473(8) Uani 1 1 d . . . . .
O6 O 0.46780(10) 0.35393(15) 0.82759(9) 0.0354(6) Uani 1 1 d . . . . .
O7 O 0.44888(11) 0.45431(18) 0.54190(10) 0.0479(8) Uani 1 1 d . . . . .
O8 O 0.48674(11) 0.21288(16) 0.83912(10) 0.0433(7) Uani 1 1 d . . . . .
Ti1 Ti 0.45286(3) 0.33988(4) 0.75896(2) 0.0369(2) Uani 1 1 d . . . . .
Ti2 Ti 0.45742(3) 0.30978(5) 0.64058(3) 0.0402(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.357(5) . ?
C1 C2 1.392(7) . ?
C1 C6 1.394(7) . ?
C2 C3A 1.396(9) . ?
C2 C3B 1.466(14) . ?
C2 C68 1.499(7) . ?
C6 C5B 1.295(13) . ?
C6 C5A 1.475(10) . ?
C6 C11 1.523(8) . ?
O9 O9 1.440(13) 2_656 ?
O9 Ti1 2.314(6) . ?
C3A C4A 1.412(11) . ?
C3A H3A 0.9500 . ?
C4A C5A 1.386(11) . ?
C4A C7A 1.536(13) . ?
C5A H5A 0.9500 . ?
C7A C9A 1.492(14) . ?
C7A C10A 1.494(18) . ?
C7A C8A 1.505(17) . ?
C8A H8A1 0.9800 . ?
C8A H8A2 0.9800 . ?
C8A H8A3 0.9800 . ?
C9A H9A1 0.9800 . ?
C9A H9A2 0.9800 . ?
C9A H9A3 0.9800 . ?
C10A H10A 0.9800 . ?
C10A H10B 0.9800 . ?
C10A H10C 0.9800 . ?
C3B C4B 1.415(19) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.416(19) . ?
C4B C7B 1.48(2) . ?
C5B H5B 0.9500 . ?
C7B C10B 1.54(3) . ?
C7B C8B 1.55(3) . ?
C7B C9B 1.64(3) . ?
C8B H8B1 0.9800 . ?
C8B H8B2 0.9800 . ?
C8B H8B3 0.9800 . ?
C9B H9B1 0.9800 . ?
C9B H9B2 0.9800 . ?
C9B H9B3 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C11 C13 1.502(7) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O2 1.370(5) . ?
C12 C17 1.383(7) . ?
C12 C13 1.400(7) . ?
C13 C14 1.399(6) . ?
C14 C15 1.393(8) . ?
C14 H14 0.9500 . ?
C15 C16 1.379(8) . ?
C15 C18 1.534(6) . ?
C16 C17 1.403(7) . ?
C16 H16 0.9500 . ?
C17 C22 1.522(7) . ?
C18 C19 1.522(9) . ?
C18 C20 1.523(9) . ?
C18 C21 1.528(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.518(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 O3 1.357(5) . ?
C23 C24 1.392(7) . ?
C23 C28 1.394(6) . ?
C24 C25B 1.406(11) . ?
C24 C25A 1.429(11) . ?
C28 C27B 1.369(11) . ?
C28 C27A 1.456(13) . ?
C28 C33 1.492(7) . ?
C25A C26A 1.395(15) . ?
C25A H25A 0.9500 . ?
C26A C27A 1.371(16) . ?
C26A C29A 1.547(14) . ?
C27A H27A 0.9500 . ?
C29A C31A 1.464(13) . ?
C29A C30A 1.565(14) . ?
C29A C32A 1.594(14) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C31A H31A 0.9800 . ?
C31A H31B 0.9800 . ?
C31A H31C 0.9800 . ?
C32A H32A 0.9800 . ?
C32A H32B 0.9800 . ?
C32A H32C 0.9800 . ?
C25B C26B 1.383(15) . ?
C25B H25B 0.9500 . ?
C26B C27B 1.414(15) . ?
C26B C29B 1.530(16) . ?
C27B H27B 0.9500 . ?
C29B C31B 1.455(13) . ?
C29B C32B 1.551(13) . ?
C29B C30B 1.625(15) . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31B H31D 0.9800 . ?
C31B H31E 0.9800 . ?
C31B H31F 0.9800 . ?
C32B H32D 0.9800 . ?
C32B H32E 0.9800 . ?
C32B H32F 0.9800 . ?
C33 O7 1.427(5) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 O7 1.430(5) . ?
C34 C36 1.496(7) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 O4 1.350(5) . ?
C35 C40 1.402(7) . ?
C35 C36 1.405(7) . ?
C36 C37A 1.370(8) . ?
C36 C37B 1.456(18) . ?
C40 C39A 1.306(9) . ?
C40 C45 1.518(8) . ?
C40 C39B 1.708(19) . ?
C37A C38A 1.397(11) . ?
C37A H37A 0.9500 . ?
C38A C39A 1.402(12) . ?
C38A C41A 1.513(12) . ?
C39A H39A 0.9500 . ?
C41A C42A 1.527(12) . ?
C41A C43A 1.545(13) . ?
C41A C44A 1.556(13) . ?
C42A H42A 0.9800 . ?
C42A H42B 0.9800 . ?
C42A H42C 0.9800 . ?
C43A H43A 0.9800 . ?
C43A H43B 0.9800 . ?
C43A H43C 0.9800 . ?
C44A H44A 0.9800 . ?
C44A H44B 0.9800 . ?
C44A H44C 0.9800 . ?
C37B C38B 1.39(3) . ?
C37B H37B 0.9500 . ?
C38B C39B 1.33(3) . ?
C38B C41B 1.61(3) . ?
C39B H39B 0.9500 . ?
C41B C43B 1.46(3) . ?
C41B C42B 1.48(3) . ?
C41B C44B 1.61(4) . ?
C42B H42D 0.9800 . ?
C42B H42E 0.9800 . ?
C42B H42F 0.9800 . ?
C43B H43D 0.9800 . ?
C43B H43E 0.9800 . ?
C43B H43F 0.9800 . ?
C44B H44D 0.9800 . ?
C44B H44E 0.9800 . ?
C44B H44F 0.9800 . ?
C45 C47 1.517(8) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 O5 1.351(6) . ?
C46 C51 1.379(7) . ?
C46 C47 1.395(7) . ?
C47 C48A 1.324(9) . ?
C47 C48B 1.639(14) . ?
C51 C50A 1.367(8) . ?
C51 C50B 1.518(12) . ?
C51 C56 1.520(6) . ?
C48A C49A 1.382(11) . ?
C48A H48A 0.9500 . ?
C49A C50A 1.378(10) . ?
C49A C52A 1.536(12) . ?
C50A H50A 0.9500 . ?
C52A C54A 1.513(14) . ?
C52A C53A 1.518(16) . ?
C52A C55A 1.526(16) . ?
C53A H53A 0.9800 . ?
C53A H53B 0.9800 . ?
C53A H53C 0.9800 . ?
C54A H54A 0.9800 . ?
C54A H54B 0.9800 . ?
C54A H54C 0.9800 . ?
C55A H55A 0.9800 . ?
C55A H55B 0.9800 . ?
C55A H55C 0.9800 . ?
C48B C49B 1.415(16) . ?
C48B H48B 0.9500 . ?
C49B C50B 1.386(15) . ?
C49B C52B 1.549(18) . ?
C50B H50B 0.9500 . ?
C52B C53B 1.48(2) . ?
C52B C54B 1.53(2) . ?
C52B C55B 1.56(2) . ?
C53B H53D 0.9800 . ?
C53B H53E 0.9800 . ?
C53B H53F 0.9800 . ?
C54B H54D 0.9800 . ?
C54B H54E 0.9800 . ?
C54B H54F 0.9800 . ?
C55B H55D 0.9800 . ?
C55B H55E 0.9800 . ?
C55B H55F 0.9800 . ?
C56 C58 1.511(6) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O6 1.378(5) . ?
C57 C62 1.386(6) . ?
C57 C58 1.399(6) . ?
C58 C59 1.394(6) . ?
C59 C60 1.378(7) . ?
C59 H59 0.9500 . ?
C60 C61 1.388(6) . ?
C60 C63 1.533(6) . ?
C61 C62 1.400(6) . ?
C61 H61 0.9500 . ?
C62 C67 1.512(6) . ?
C63 C65 1.527(7) . ?
C63 C64 1.529(7) . ?
C63 C66 1.530(8) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C67 O8 1.441(5) . ?
C67 H67A 0.9900 . ?
C67 H67B 0.9900 . ?
C68 O8 1.439(5) . ?
C68 H68A 0.9900 . ?
C68 H68B 0.9900 . ?
O1 Ti1 1.784(3) . ?
O2 Ti2 1.814(3) . ?
O3 Ti2 1.818(3) . ?
O4 Ti2 1.803(3) . ?
O5 Ti1 1.788(3) . ?
O10 Ti1 1.890(3) . ?
O10 Ti1 1.951(3) 2_656 ?
O10 Ti2 2.013(3) . ?
O6 Ti1 2.032(3) . ?
O6 Ti2 2.096(3) 2_656 ?
O8 Ti2 2.249(3) 2_656 ?
Ti1 Ti1 2.9164(15) 2_656 ?
Ti1 Ti2 3.2107(10) 2_656 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 120.0(4) . . ?
O1 C1 C6 119.1(5) . . ?
C2 C1 C6 120.9(5) . . ?
C1 C2 C3A 124.2(5) . . ?
C1 C2 C3B 105.2(7) . . ?
C1 C2 C68 123.3(4) . . ?
C3A C2 C68 110.9(6) . . ?
C3B C2 C68 129.5(6) . . ?
C5B C6 C1 127.6(7) . . ?
C1 C6 C5A 112.9(6) . . ?
C5B C6 C11 104.8(7) . . ?
C1 C6 C11 121.6(5) . . ?
C5A C6 C11 124.6(5) . . ?
O9 O9 Ti1 98.0(3) 2_656 . ?
C2 C3A C4A 118.1(7) . . ?
C2 C3A H3A 121.0 . . ?
C4A C3A H3A 121.0 . . ?
C5A C4A C3A 116.7(7) . . ?
C5A C4A C7A 119.7(8) . . ?
C3A C4A C7A 123.6(8) . . ?
C4A C5A C6 126.3(7) . . ?
C4A C5A H5A 116.8 . . ?
C6 C5A H5A 116.8 . . ?
C9A C7A C10A 112.7(11) . . ?
C9A C7A C8A 109.2(11) . . ?
C10A C7A C8A 104.3(11) . . ?
C9A C7A C4A 108.5(9) . . ?
C10A C7A C4A 111.9(10) . . ?
C8A C7A C4A 110.2(10) . . ?
C7A C8A H8A1 109.5 . . ?
C7A C8A H8A2 109.5 . . ?
H8A1 C8A H8A2 109.5 . . ?
C7A C8A H8A3 109.5 . . ?
H8A1 C8A H8A3 109.5 . . ?
H8A2 C8A H8A3 109.5 . . ?
C7A C9A H9A1 109.5 . . ?
C7A C9A H9A2 109.5 . . ?
H9A1 C9A H9A2 109.5 . . ?
C7A C9A H9A3 109.5 . . ?
H9A1 C9A H9A3 109.5 . . ?
H9A2 C9A H9A3 109.5 . . ?
C7A C10A H10A 109.5 . . ?
C7A C10A H10B 109.5 . . ?
H10A C10A H10B 109.5 . . ?
C7A C10A H10C 109.5 . . ?
H10A C10A H10C 109.5 . . ?
H10B C10A H10C 109.5 . . ?
C4B C3B C2 130.3(11) . . ?
C4B C3B H3B 114.8 . . ?
C2 C3B H3B 114.8 . . ?
C3B C4B C5B 115.2(12) . . ?
C3B C4B C7B 122.8(13) . . ?
C5B C4B C7B 122.0(13) . . ?
C6 C5B C4B 113.6(11) . . ?
C6 C5B H5B 123.2 . . ?
C4B C5B H5B 123.2 . . ?
C4B C7B C10B 115.4(16) . . ?
C4B C7B C8B 110.6(15) . . ?
C10B C7B C8B 114.1(16) . . ?
C4B C7B C9B 107.1(14) . . ?
C10B C7B C9B 102.2(15) . . ?
C8B C7B C9B 106.5(15) . . ?
C7B C8B H8B1 109.5 . . ?
C7B C8B H8B2 109.5 . . ?
H8B1 C8B H8B2 109.5 . . ?
C7B C8B H8B3 109.5 . . ?
H8B1 C8B H8B3 109.5 . . ?
H8B2 C8B H8B3 109.5 . . ?
C7B C9B H9B1 109.5 . . ?
C7B C9B H9B2 109.5 . . ?
H9B1 C9B H9B2 109.5 . . ?
C7B C9B H9B3 109.5 . . ?
H9B1 C9B H9B3 109.5 . . ?
H9B2 C9B H9B3 109.5 . . ?
C7B C10B H10D 109.5 . . ?
C7B C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C7B C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C13 C11 C6 110.4(5) . . ?
C13 C11 H11A 109.6 . . ?
C6 C11 H11A 109.6 . . ?
C13 C11 H11B 109.6 . . ?
C6 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
O2 C12 C17 121.4(4) . . ?
O2 C12 C13 117.6(4) . . ?
C17 C12 C13 121.0(4) . . ?
C14 C13 C12 118.6(5) . . ?
C14 C13 C11 122.0(5) . . ?
C12 C13 C11 118.9(4) . . ?
C15 C14 C13 121.9(5) . . ?
C15 C14 H14 119.0 . . ?
C13 C14 H14 119.0 . . ?
C16 C15 C14 116.8(4) . . ?
C16 C15 C18 120.8(5) . . ?
C14 C15 C18 122.3(5) . . ?
C15 C16 C17 123.6(5) . . ?
C15 C16 H16 118.2 . . ?
C17 C16 H16 118.2 . . ?
C12 C17 C16 117.5(5) . . ?
C12 C17 C22 122.0(4) . . ?
C16 C17 C22 120.2(5) . . ?
C19 C18 C20 108.1(5) . . ?
C19 C18 C21 109.1(6) . . ?
C20 C18 C21 108.9(5) . . ?
C19 C18 C15 112.3(5) . . ?
C20 C18 C15 110.1(5) . . ?
C21 C18 C15 108.3(4) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 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 . . ?
C24 C22 C17 116.9(4) . . ?
C24 C22 H22A 108.1 . . ?
C17 C22 H22A 108.1 . . ?
C24 C22 H22B 108.1 . . ?
C17 C22 H22B 108.1 . . ?
H22A C22 H22B 107.3 . . ?
O3 C23 C24 120.0(4) . . ?
O3 C23 C28 119.0(4) . . ?
C24 C23 C28 121.0(4) . . ?
C23 C24 C25B 116.3(6) . . ?
C23 C24 C25A 118.3(6) . . ?
C23 C24 C22 121.5(4) . . ?
C25B C24 C22 120.4(6) . . ?
C25A C24 C22 119.7(6) . . ?
C27B C28 C23 120.4(6) . . ?
C23 C28 C27A 117.1(6) . . ?
C27B C28 C33 119.6(6) . . ?
C23 C28 C33 119.4(4) . . ?
C27A C28 C33 122.5(6) . . ?
C26A C25A C24 122.0(9) . . ?
C26A C25A H25A 119.0 . . ?
C24 C25A H25A 119.0 . . ?
C27A C26A C25A 117.0(10) . . ?
C27A C26A C29A 122.6(10) . . ?
C25A C26A C29A 120.4(10) . . ?
C26A C27A C28 122.9(10) . . ?
C26A C27A H27A 118.6 . . ?
C28 C27A H27A 118.6 . . ?
C31A C29A C26A 112.7(11) . . ?
C31A C29A C30A 118.4(11) . . ?
C26A C29A C30A 110.5(11) . . ?
C31A C29A C32A 105.7(11) . . ?
C26A C29A C32A 108.0(11) . . ?
C30A C29A C32A 100.3(10) . . ?
C29A C30A H30A 109.5 . . ?
C29A C30A H30B 109.5 . . ?
H30A C30A H30B 109.5 . . ?
C29A C30A H30C 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29A C31A H31A 109.5 . . ?
C29A C31A H31B 109.5 . . ?
H31A C31A H31B 109.5 . . ?
C29A C31A H31C 109.5 . . ?
H31A C31A H31C 109.5 . . ?
H31B C31A H31C 109.5 . . ?
C29A C32A H32A 109.5 . . ?
C29A C32A H32B 109.5 . . ?
H32A C32A H32B 109.5 . . ?
C29A C32A H32C 109.5 . . ?
H32A C32A H32C 109.5 . . ?
H32B C32A H32C 109.5 . . ?
C26B C25B C24 123.4(9) . . ?
C26B C25B H25B 118.3 . . ?
C24 C25B H25B 118.3 . . ?
C25B C26B C27B 117.2(10) . . ?
C25B C26B C29B 121.6(10) . . ?
C27B C26B C29B 121.1(10) . . ?
C28 C27B C26B 120.5(10) . . ?
C28 C27B H27B 119.8 . . ?
C26B C27B H27B 119.8 . . ?
C31B C29B C26B 117.4(11) . . ?
C31B C29B C32B 114.6(10) . . ?
C26B C29B C32B 110.4(10) . . ?
C31B C29B C30B 105.1(10) . . ?
C26B C29B C30B 105.0(11) . . ?
C32B C29B C30B 102.4(10) . . ?
C29B C30B H30D 109.5 . . ?
C29B C30B H30E 109.5 . . ?
H30D C30B H30E 109.5 . . ?
C29B C30B H30F 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
C29B C31B H31D 109.5 . . ?
C29B C31B H31E 109.5 . . ?
H31D C31B H31E 109.5 . . ?
C29B C31B H31F 109.5 . . ?
H31D C31B H31F 109.5 . . ?
H31E C31B H31F 109.5 . . ?
C29B C32B H32D 109.5 . . ?
C29B C32B H32E 109.5 . . ?
H32D C32B H32E 109.5 . . ?
C29B C32B H32F 109.5 . . ?
H32D C32B H32F 109.5 . . ?
H32E C32B H32F 109.5 . . ?
O7 C33 C28 108.0(4) . . ?
O7 C33 H33A 110.1 . . ?
C28 C33 H33A 110.1 . . ?
O7 C33 H33B 110.1 . . ?
C28 C33 H33B 110.1 . . ?
H33A C33 H33B 108.4 . . ?
O7 C34 C36 108.0(4) . . ?
O7 C34 H34A 110.1 . . ?
C36 C34 H34A 110.1 . . ?
O7 C34 H34B 110.1 . . ?
C36 C34 H34B 110.1 . . ?
H34A C34 H34B 108.4 . . ?
O4 C35 C40 119.1(5) . . ?
O4 C35 C36 120.0(4) . . ?
C40 C35 C36 120.9(5) . . ?
C37A C36 C35 114.3(5) . . ?
C35 C36 C37B 130.6(8) . . ?
C37A C36 C34 124.3(5) . . ?
C35 C36 C34 121.1(4) . . ?
C37B C36 C34 107.1(8) . . ?
C39A C40 C35 122.4(6) . . ?
C39A C40 C45 116.0(6) . . ?
C35 C40 C45 121.2(5) . . ?
C35 C40 C39B 105.4(7) . . ?
C45 C40 C39B 132.7(7) . . ?
C36 C37A C38A 125.5(7) . . ?
C36 C37A H37A 117.3 . . ?
C38A C37A H37A 117.3 . . ?
C37A C38A C39A 116.7(7) . . ?
C37A C38A C41A 124.1(7) . . ?
C39A C38A C41A 119.1(7) . . ?
C40 C39A C38A 120.1(7) . . ?
C40 C39A H39A 119.9 . . ?
C38A C39A H39A 119.9 . . ?
C38A C41A C42A 109.3(7) . . ?
C38A C41A C43A 112.2(7) . . ?
C42A C41A C43A 107.0(7) . . ?
C38A C41A C44A 111.3(7) . . ?
C42A C41A C44A 108.7(7) . . ?
C43A C41A C44A 108.2(7) . . ?
C41A C42A H42A 109.5 . . ?
C41A C42A H42B 109.5 . . ?
H42A C42A H42B 109.5 . . ?
C41A C42A H42C 109.5 . . ?
H42A C42A H42C 109.5 . . ?
H42B C42A H42C 109.5 . . ?
C41A C43A H43A 109.5 . . ?
C41A C43A H43B 109.5 . . ?
H43A C43A H43B 109.5 . . ?
C41A C43A H43C 109.5 . . ?
H43A C43A H43C 109.5 . . ?
H43B C43A H43C 109.5 . . ?
C41A C44A H44A 109.5 . . ?
C41A C44A H44B 109.5 . . ?
H44A C44A H44B 109.5 . . ?
C41A C44A H44C 109.5 . . ?
H44A C44A H44C 109.5 . . ?
H44B C44A H44C 109.5 . . ?
C38B C37B C36 112.5(15) . . ?
C38B C37B H37B 123.8 . . ?
C36 C37B H37B 123.8 . . ?
C39B C38B C37B 120.3(17) . . ?
C39B C38B C41B 119.4(16) . . ?
C37B C38B C41B 120.2(17) . . ?
C38B C39B C40 128.3(13) . . ?
C38B C39B H39B 115.8 . . ?
C40 C39B H39B 115.8 . . ?
C43B C41B C42B 115(2) . . ?
C43B C41B C44B 106(2) . . ?
C42B C41B C44B 113(2) . . ?
C43B C41B C38B 112.4(18) . . ?
C42B C41B C38B 107(2) . . ?
C44B C41B C38B 102.6(19) . . ?
C41B C42B H42D 109.5 . . ?
C41B C42B H42E 109.5 . . ?
H42D C42B H42E 109.5 . . ?
C41B C42B H42F 109.5 . . ?
H42D C42B H42F 109.5 . . ?
H42E C42B H42F 109.5 . . ?
C41B C43B H43D 109.5 . . ?
C41B C43B H43E 109.5 . . ?
H43D C43B H43E 109.5 . . ?
C41B C43B H43F 109.5 . . ?
H43D C43B H43F 109.5 . . ?
H43E C43B H43F 109.5 . . ?
C41B C44B H44D 109.5 . . ?
C41B C44B H44E 109.5 . . ?
H44D C44B H44E 109.5 . . ?
C41B C44B H44F 109.5 . . ?
H44D C44B H44F 109.5 . . ?
H44E C44B H44F 109.5 . . ?
C47 C45 C40 111.6(5) . . ?
C47 C45 H45A 109.3 . . ?
C40 C45 H45A 109.3 . . ?
C47 C45 H45B 109.3 . . ?
C40 C45 H45B 109.3 . . ?
H45A C45 H45B 108.0 . . ?
O5 C46 C51 120.9(4) . . ?
O5 C46 C47 117.5(4) . . ?
C51 C46 C47 121.7(5) . . ?
C48A C47 C46 119.2(5) . . ?
C48A C47 C45 119.2(5) . . ?
C46 C47 C45 120.5(5) . . ?
C46 C47 C48B 112.0(6) . . ?
C45 C47 C48B 122.5(6) . . ?
C50A C51 C46 114.8(5) . . ?
C46 C51 C50B 123.2(5) . . ?
C50A C51 C56 123.3(5) . . ?
C46 C51 C56 121.4(4) . . ?
C50B C51 C56 112.6(5) . . ?
C47 C48A C49A 119.8(7) . . ?
C47 C48A H48A 120.1 . . ?
C49A C48A H48A 120.1 . . ?
C50A C49A C48A 118.0(7) . . ?
C50A C49A C52A 121.5(7) . . ?
C48A C49A C52A 120.5(7) . . ?
C51 C50A C49A 123.8(7) . . ?
C51 C50A H50A 118.1 . . ?
C49A C50A H50A 118.1 . . ?
C54A C52A C53A 108.2(9) . . ?
C54A C52A C55A 107.9(9) . . ?
C53A C52A C55A 106.5(10) . . ?
C54A C52A C49A 114.0(8) . . ?
C53A C52A C49A 110.8(8) . . ?
C55A C52A C49A 109.2(8) . . ?
C52A C53A H53A 109.5 . . ?
C52A C53A H53B 109.5 . . ?
H53A C53A H53B 109.5 . . ?
C52A C53A H53C 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
C52A C54A H54A 109.5 . . ?
C52A C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C52A C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C52A C55A H55A 109.5 . . ?
C52A C55A H55B 109.5 . . ?
H55A C55A H55B 109.5 . . ?
C52A C55A H55C 109.5 . . ?
H55A C55A H55C 109.5 . . ?
H55B C55A H55C 109.5 . . ?
C49B C48B C47 123.5(9) . . ?
C49B C48B H48B 118.2 . . ?
C47 C48B H48B 118.2 . . ?
C50B C49B C48B 117.0(11) . . ?
C50B C49B C52B 123.6(11) . . ?
C48B C49B C52B 119.0(10) . . ?
C49B C50B C51 119.6(10) . . ?
C49B C50B H50B 120.2 . . ?
C51 C50B H50B 120.2 . . ?
C53B C52B C54B 109.6(12) . . ?
C53B C52B C49B 110.4(11) . . ?
C54B C52B C49B 111.8(11) . . ?
C53B C52B C55B 107.6(13) . . ?
C54B C52B C55B 109.2(12) . . ?
C49B C52B C55B 108.2(12) . . ?
C52B C53B H53D 109.5 . . ?
C52B C53B H53E 109.5 . . ?
H53D C53B H53E 109.5 . . ?
C52B C53B H53F 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
C52B C54B H54D 109.5 . . ?
C52B C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C52B C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?
C52B C55B H55D 109.5 . . ?
C52B C55B H55E 109.5 . . ?
H55D C55B H55E 109.5 . . ?
C52B C55B H55F 109.5 . . ?
H55D C55B H55F 109.5 . . ?
H55E C55B H55F 109.5 . . ?
C58 C56 C51 114.7(4) . . ?
C58 C56 H56A 108.6 . . ?
C51 C56 H56A 108.6 . . ?
C58 C56 H56B 108.6 . . ?
C51 C56 H56B 108.6 . . ?
H56A C56 H56B 107.6 . . ?
O6 C57 C62 120.1(4) . . ?
O6 C57 C58 118.8(4) . . ?
C62 C57 C58 121.0(4) . . ?
C59 C58 C57 117.8(4) . . ?
C59 C58 C56 121.4(4) . . ?
C57 C58 C56 120.8(4) . . ?
C60 C59 C58 122.8(4) . . ?
C60 C59 H59 118.6 . . ?
C58 C59 H59 118.6 . . ?
C59 C60 C61 117.5(4) . . ?
C59 C60 C63 120.4(4) . . ?
C61 C60 C63 121.9(4) . . ?
C60 C61 C62 122.0(4) . . ?
C60 C61 H61 119.0 . . ?
C62 C61 H61 119.0 . . ?
C57 C62 C61 118.3(4) . . ?
C57 C62 C67 125.3(4) . . ?
C61 C62 C67 116.4(4) . . ?
C65 C63 C64 109.0(4) . . ?
C65 C63 C66 108.8(4) . . ?
C64 C63 C66 109.1(4) . . ?
C65 C63 C60 107.7(4) . . ?
C64 C63 C60 110.2(4) . . ?
C66 C63 C60 112.0(4) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
O8 C67 C62 113.2(3) . . ?
O8 C67 H67A 108.9 . . ?
C62 C67 H67A 108.9 . . ?
O8 C67 H67B 108.9 . . ?
C62 C67 H67B 108.9 . . ?
H67A C67 H67B 107.7 . . ?
O8 C68 C2 114.7(4) . . ?
O8 C68 H68A 108.6 . . ?
C2 C68 H68A 108.6 . . ?
O8 C68 H68B 108.6 . . ?
C2 C68 H68B 108.6 . . ?
H68A C68 H68B 107.6 . . ?
C1 O1 Ti1 152.1(3) . . ?
C12 O2 Ti2 147.4(3) . . ?
C23 O3 Ti2 155.8(3) . . ?
C35 O4 Ti2 163.6(3) . . ?
C46 O5 Ti1 163.4(3) . . ?
Ti1 O10 Ti1 98.78(13) . 2_656 ?
Ti1 O10 Ti2 152.07(17) . . ?
Ti1 O10 Ti2 108.17(14) 2_656 . ?
C57 O6 Ti1 122.3(2) . . ?
C57 O6 Ti2 123.7(2) . 2_656 ?
Ti1 O6 Ti2 102.12(12) . 2_656 ?
C33 O7 C34 114.4(3) . . ?
C68 O8 C67 114.6(3) . . ?
C68 O8 Ti2 123.6(3) . 2_656 ?
C67 O8 Ti2 120.6(2) . 2_656 ?
O1 Ti1 O5 103.73(15) . . ?
O1 Ti1 O10 95.97(14) . . ?
O5 Ti1 O10 105.67(14) . . ?
O1 Ti1 O10 110.83(14) . 2_656 ?
O5 Ti1 O10 144.69(16) . 2_656 ?
O10 Ti1 O10 78.16(14) . 2_656 ?
O1 Ti1 O6 95.53(12) . . ?
O5 Ti1 O6 95.37(13) . . ?
O10 Ti1 O6 152.80(12) . . ?
O10 Ti1 O6 74.72(12) 2_656 . ?
O1 Ti1 O9 174.79(19) . . ?
O5 Ti1 O9 72.90(19) . . ?
O10 Ti1 O9 88.83(19) . . ?
O10 Ti1 O9 72.11(18) 2_656 . ?
O6 Ti1 O9 80.98(17) . . ?
O1 Ti1 Ti1 119.17(9) . 2_656 ?
O5 Ti1 Ti1 124.86(12) . 2_656 ?
O10 Ti1 Ti1 41.40(9) . 2_656 ?
O10 Ti1 Ti1 39.83(9) 2_656 2_656 ?
O6 Ti1 Ti1 111.95(8) . 2_656 ?
O9 Ti1 Ti1 65.91(16) . 2_656 ?
O1 Ti1 Ti2 98.92(9) . 2_656 ?
O5 Ti1 Ti2 131.48(10) . 2_656 ?
O10 Ti1 Ti2 113.97(9) . 2_656 ?
O10 Ti1 Ti2 36.56(9) 2_656 2_656 ?
O6 Ti1 Ti2 39.66(8) . 2_656 ?
O9 Ti1 Ti2 80.89(14) . 2_656 ?
Ti1 Ti1 Ti2 76.19(3) 2_656 2_656 ?
O4 Ti2 O2 103.96(15) . . ?
O4 Ti2 O3 96.17(13) . . ?
O2 Ti2 O3 99.52(13) . . ?
O4 Ti2 O10 91.40(13) . . ?
O2 Ti2 O10 92.32(13) . . ?
O3 Ti2 O10 163.95(13) . . ?
O4 Ti2 O6 100.33(12) . 2_656 ?
O2 Ti2 O6 151.40(13) . 2_656 ?
O3 Ti2 O6 92.60(12) . 2_656 ?
O10 Ti2 O6 72.08(11) . 2_656 ?
O4 Ti2 O8 172.37(12) . 2_656 ?
O2 Ti2 O8 83.56(13) . 2_656 ?
O3 Ti2 O8 83.69(12) . 2_656 ?
O10 Ti2 O8 86.95(12) . 2_656 ?
O6 Ti2 O8 72.07(11) 2_656 2_656 ?
O4 Ti2 Ti1 104.70(10) . 2_656 ?
O2 Ti2 Ti1 119.22(10) . 2_656 ?
O3 Ti2 Ti1 128.71(9) . 2_656 ?
O10 Ti2 Ti1 35.27(8) . 2_656 ?
O6 Ti2 Ti1 38.23(7) 2_656 2_656 ?
O8 Ti2 Ti1 69.91(8) 2_656 2_656 ?

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
O1 C1 C2 C3A -171.2(6) . . . . ?
C6 C1 C2 C3A 8.3(9) . . . . ?
O1 C1 C2 C3B 158.5(6) . . . . ?
C6 C1 C2 C3B -22.1(8) . . . . ?
O1 C1 C2 C68 -6.9(8) . . . . ?
C6 C1 C2 C68 172.6(5) . . . . ?
O1 C1 C6 C5B -146.2(9) . . . . ?
C2 C1 C6 C5B 34.3(12) . . . . ?
O1 C1 C6 C5A 171.7(5) . . . . ?
C2 C1 C6 C5A -7.8(8) . . . . ?
O1 C1 C6 C11 2.0(8) . . . . ?
C2 C1 C6 C11 -177.5(5) . . . . ?
C1 C2 C3A C4A -7.0(11) . . . . ?
C68 C2 C3A C4A -173.0(7) . . . . ?
C2 C3A C4A C5A 6.0(12) . . . . ?
C2 C3A C4A C7A -175.1(8) . . . . ?
C3A C4A C5A C6 -7.1(13) . . . . ?
C7A C4A C5A C6 174.0(8) . . . . ?
C1 C6 C5A C4A 7.8(11) . . . . ?
C11 C6 C5A C4A 177.2(7) . . . . ?
C5A C4A C7A C9A 69.5(11) . . . . ?
C3A C4A C7A C9A -109.4(10) . . . . ?
C5A C4A C7A C10A -165.5(10) . . . . ?
C3A C4A C7A C10A 15.7(14) . . . . ?
C5A C4A C7A C8A -49.9(13) . . . . ?
C3A C4A C7A C8A 131.2(11) . . . . ?
C1 C2 C3B C4B 12.2(16) . . . . ?
C68 C2 C3B C4B 176.3(11) . . . . ?
C2 C3B C4B C5B -8(2) . . . . ?
C2 C3B C4B C7B 171.7(14) . . . . ?
C1 C6 C5B C4B -26.3(16) . . . . ?
C11 C6 C5B C4B -178.6(10) . . . . ?
C3B C4B C5B C6 12.2(18) . . . . ?
C7B C4B C5B C6 -167.3(13) . . . . ?
C3B C4B C7B C10B -6(2) . . . . ?
C5B C4B C7B C10B 173.6(15) . . . . ?
C3B C4B C7B C8B 125.6(16) . . . . ?
C5B C4B C7B C8B -55(2) . . . . ?
C3B C4B C7B C9B -118.7(15) . . . . ?
C5B C4B C7B C9B 60.7(19) . . . . ?
C5B C6 C11 C13 -71.5(8) . . . . ?
C1 C6 C11 C13 134.1(5) . . . . ?
C5A C6 C11 C13 -34.4(8) . . . . ?
O2 C12 C13 C14 175.7(5) . . . . ?
C17 C12 C13 C14 -6.6(8) . . . . ?
O2 C12 C13 C11 -11.9(7) . . . . ?
C17 C12 C13 C11 165.8(5) . . . . ?
C6 C11 C13 C14 103.8(6) . . . . ?
C6 C11 C13 C12 -68.4(6) . . . . ?
C12 C13 C14 C15 1.4(8) . . . . ?
C11 C13 C14 C15 -170.8(5) . . . . ?
C13 C14 C15 C16 3.3(8) . . . . ?
C13 C14 C15 C18 -175.6(5) . . . . ?
C14 C15 C16 C17 -3.1(8) . . . . ?
C18 C15 C16 C17 175.9(5) . . . . ?
O2 C12 C17 C16 -175.6(4) . . . . ?
C13 C12 C17 C16 6.8(7) . . . . ?
O2 C12 C17 C22 10.0(7) . . . . ?
C13 C12 C17 C22 -167.6(5) . . . . ?
C15 C16 C17 C12 -1.9(8) . . . . ?
C15 C16 C17 C22 172.7(5) . . . . ?
C16 C15 C18 C19 176.4(5) . . . . ?
C14 C15 C18 C19 -4.7(8) . . . . ?
C16 C15 C18 C20 55.8(7) . . . . ?
C14 C15 C18 C20 -125.3(6) . . . . ?
C16 C15 C18 C21 -63.1(8) . . . . ?
C14 C15 C18 C21 115.8(7) . . . . ?
C12 C17 C22 C24 -98.2(6) . . . . ?
C16 C17 C22 C24 87.5(6) . . . . ?
O3 C23 C24 C25B -168.4(7) . . . . ?
C28 C23 C24 C25B 11.5(9) . . . . ?
O3 C23 C24 C25A 167.4(7) . . . . ?
C28 C23 C24 C25A -12.7(9) . . . . ?
O3 C23 C24 C22 -3.7(7) . . . . ?
C28 C23 C24 C22 176.1(5) . . . . ?
C17 C22 C24 C23 88.1(6) . . . . ?
C17 C22 C24 C25B -107.9(8) . . . . ?
C17 C22 C24 C25A -83.0(8) . . . . ?
O3 C23 C28 C27B 170.1(7) . . . . ?
C24 C23 C28 C27B -9.8(9) . . . . ?
O3 C23 C28 C27A -169.7(7) . . . . ?
C24 C23 C28 C27A 10.5(9) . . . . ?
O3 C23 C28 C33 -1.0(7) . . . . ?
C24 C23 C28 C33 179.2(5) . . . . ?
C23 C24 C25A C26A 12.7(14) . . . . ?
C22 C24 C25A C26A -176.0(9) . . . . ?
C24 C25A C26A C27A -10.3(18) . . . . ?
C24 C25A C26A C29A 169.0(10) . . . . ?
C25A C26A C27A C28 8.1(18) . . . . ?
C29A C26A C27A C28 -171.1(10) . . . . ?
C23 C28 C27A C26A -8.3(15) . . . . ?
C33 C28 C27A C26A -176.6(10) . . . . ?
C27A C26A C29A C31A -19.2(17) . . . . ?
C25A C26A C29A C31A 161.5(13) . . . . ?
C27A C26A C29A C30A 115.7(14) . . . . ?
C25A C26A C29A C30A -63.6(15) . . . . ?
C27A C26A C29A C32A -135.6(13) . . . . ?
C25A C26A C29A C32A 45.1(15) . . . . ?
C23 C24 C25B C26B -11.1(14) . . . . ?
C22 C24 C25B C26B -175.9(10) . . . . ?
C24 C25B C26B C27B 8.3(18) . . . . ?
C24 C25B C26B C29B -175.3(11) . . . . ?
C23 C28 C27B C26B 6.7(14) . . . . ?
C33 C28 C27B C26B 177.7(9) . . . . ?
C25B C26B C27B C28 -5.9(17) . . . . ?
C29B C26B C27B C28 177.7(10) . . . . ?
C25B C26B C29B C31B 174.0(12) . . . . ?
C27B C26B C29B C31B -9.7(17) . . . . ?
C25B C26B C29B C32B 40.1(16) . . . . ?
C27B C26B C29B C32B -143.6(11) . . . . ?
C25B C26B C29B C30B -69.7(15) . . . . ?
C27B C26B C29B C30B 106.6(13) . . . . ?
C27B C28 C33 O7 118.3(7) . . . . ?
C23 C28 C33 O7 -70.6(5) . . . . ?
C27A C28 C33 O7 97.5(8) . . . . ?
O4 C35 C36 C37A 176.9(5) . . . . ?
C40 C35 C36 C37A -1.4(7) . . . . ?
O4 C35 C36 C37B -163.3(10) . . . . ?
C40 C35 C36 C37B 18.5(12) . . . . ?
O4 C35 C36 C34 2.6(6) . . . . ?
C40 C35 C36 C34 -175.6(4) . . . . ?
O7 C34 C36 C37A -94.9(6) . . . . ?
O7 C34 C36 C35 78.8(5) . . . . ?
O7 C34 C36 C37B -112.4(8) . . . . ?
O4 C35 C40 C39A -175.3(6) . . . . ?
C36 C35 C40 C39A 3.0(8) . . . . ?
O4 C35 C40 C45 -2.2(6) . . . . ?
C36 C35 C40 C45 176.1(4) . . . . ?
O4 C35 C40 C39B 170.0(6) . . . . ?
C36 C35 C40 C39B -11.8(7) . . . . ?
C35 C36 C37A C38A 1.2(9) . . . . ?
C34 C36 C37A C38A 175.2(6) . . . . ?
C36 C37A C38A C39A -2.2(11) . . . . ?
C36 C37A C38A C41A -179.3(7) . . . . ?
C35 C40 C39A C38A -4.1(10) . . . . ?
C45 C40 C39A C38A -177.5(6) . . . . ?
C37A C38A C39A C40 3.6(11) . . . . ?
C41A C38A C39A C40 -179.1(7) . . . . ?
C37A C38A C41A C42A 109.0(9) . . . . ?
C39A C38A C41A C42A -68.0(9) . . . . ?
C37A C38A C41A C43A -9.5(11) . . . . ?
C39A C38A C41A C43A 173.5(8) . . . . ?
C37A C38A C41A C44A -131.0(8) . . . . ?
C39A C38A C41A C44A 52.0(10) . . . . ?
C35 C36 C37B C38B -12.8(19) . . . . ?
C34 C36 C37B C38B 179.7(12) . . . . ?
C36 C37B C38B C39B 4(2) . . . . ?
C36 C37B C38B C41B -175.0(14) . . . . ?
C37B C38B C39B C40 -1(3) . . . . ?
C41B C38B C39B C40 177.6(13) . . . . ?
C35 C40 C39B C38B 5.0(19) . . . . ?
C45 C40 C39B C38B 175.8(14) . . . . ?
C39B C38B C41B C43B -178(2) . . . . ?
C37B C38B C41B C43B 1(3) . . . . ?
C39B C38B C41B C42B -50(3) . . . . ?
C37B C38B C41B C42B 129(2) . . . . ?
C39B C38B C41B C44B 69(2) . . . . ?
C37B C38B C41B C44B -112(2) . . . . ?
C39A C40 C45 C47 -54.2(7) . . . . ?
C35 C40 C45 C47 132.3(5) . . . . ?
C39B C40 C45 C47 -37.3(10) . . . . ?
O5 C46 C47 C48A 162.3(6) . . . . ?
C51 C46 C47 C48A -18.5(10) . . . . ?
O5 C46 C47 C45 -6.0(8) . . . . ?
C51 C46 C47 C45 173.3(5) . . . . ?
O5 C46 C47 C48B -161.6(6) . . . . ?
C51 C46 C47 C48B 17.6(8) . . . . ?
C40 C45 C47 C48A 103.3(7) . . . . ?
C40 C45 C47 C46 -88.4(7) . . . . ?
C40 C45 C47 C48B 64.6(8) . . . . ?
O5 C46 C51 C50A -168.9(6) . . . . ?
C47 C46 C51 C50A 11.9(8) . . . . ?
O5 C46 C51 C50B 162.9(7) . . . . ?
C47 C46 C51 C50B -16.3(9) . . . . ?
O5 C46 C51 C56 3.3(7) . . . . ?
C47 C46 C51 C56 -175.9(5) . . . . ?
C46 C47 C48A C49A 17.5(12) . . . . ?
C45 C47 C48A C49A -174.1(7) . . . . ?
C47 C48A C49A C50A -11.0(12) . . . . ?
C47 C48A C49A C52A 166.6(8) . . . . ?
C46 C51 C50A C49A -5.4(11) . . . . ?
C56 C51 C50A C49A -177.5(7) . . . . ?
C48A C49A C50A C51 5.0(13) . . . . ?
C52A C49A C50A C51 -172.6(8) . . . . ?
C50A C49A C52A C54A -2.2(12) . . . . ?
C48A C49A C52A C54A -179.8(8) . . . . ?
C50A C49A C52A C53A 120.1(10) . . . . ?
C48A C49A C52A C53A -57.4(11) . . . . ?
C50A C49A C52A C55A -122.9(10) . . . . ?
C48A C49A C52A C55A 59.6(11) . . . . ?
C46 C47 C48B C49B -16.2(13) . . . . ?
C45 C47 C48B C49B -171.3(9) . . . . ?
C47 C48B C49B C50B 11.5(17) . . . . ?
C47 C48B C49B C52B -175.0(10) . . . . ?
C48B C49B C50B C51 -7.9(17) . . . . ?
C52B C49B C50B C51 179.0(10) . . . . ?
C46 C51 C50B C49B 10.2(14) . . . . ?
C56 C51 C50B C49B 171.4(9) . . . . ?
C50B C49B C52B C53B 114.6(14) . . . . ?
C48B C49B C52B C53B -58.4(16) . . . . ?
C50B C49B C52B C54B -7.7(18) . . . . ?
C48B C49B C52B C54B 179.3(12) . . . . ?
C50B C49B C52B C55B -127.9(14) . . . . ?
C48B C49B C52B C55B 59.1(16) . . . . ?
C50A C51 C56 C58 90.2(7) . . . . ?
C46 C51 C56 C58 -81.3(6) . . . . ?
C50B C51 C56 C58 117.1(6) . . . . ?
O6 C57 C58 C59 -169.2(4) . . . . ?
C62 C57 C58 C59 8.0(6) . . . . ?
O6 C57 C58 C56 8.1(6) . . . . ?
C62 C57 C58 C56 -174.6(4) . . . . ?
C51 C56 C58 C59 -84.4(5) . . . . ?
C51 C56 C58 C57 98.4(5) . . . . ?
C57 C58 C59 C60 -1.5(6) . . . . ?
C56 C58 C59 C60 -178.9(4) . . . . ?
C58 C59 C60 C61 -4.2(7) . . . . ?
C58 C59 C60 C63 171.1(4) . . . . ?
C59 C60 C61 C62 3.7(6) . . . . ?
C63 C60 C61 C62 -171.5(4) . . . . ?
O6 C57 C62 C61 168.8(3) . . . . ?
C58 C57 C62 C61 -8.4(6) . . . . ?
O6 C57 C62 C67 -11.3(6) . . . . ?
C58 C57 C62 C67 171.5(4) . . . . ?
C60 C61 C62 C57 2.4(6) . . . . ?
C60 C61 C62 C67 -177.5(4) . . . . ?
C59 C60 C63 C65 -67.5(6) . . . . ?
C61 C60 C63 C65 107.5(5) . . . . ?
C59 C60 C63 C64 51.2(6) . . . . ?
C61 C60 C63 C64 -133.7(5) . . . . ?
C59 C60 C63 C66 172.9(4) . . . . ?
C61 C60 C63 C66 -12.1(6) . . . . ?
C57 C62 C67 O8 7.9(6) . . . . ?
C61 C62 C67 O8 -172.2(4) . . . . ?
C1 C2 C68 O8 40.2(7) . . . . ?
C3A C2 C68 O8 -153.6(5) . . . . ?
C3B C2 C68 O8 -121.4(9) . . . . ?
C2 C1 O1 Ti1 69.0(8) . . . . ?
C6 C1 O1 Ti1 -110.5(7) . . . . ?
C17 C12 O2 Ti2 53.6(8) . . . . ?
C13 C12 O2 Ti2 -128.7(5) . . . . ?
C24 C23 O3 Ti2 -49.2(9) . . . . ?
C28 C23 O3 Ti2 131.0(6) . . . . ?
C40 C35 O4 Ti2 -145.1(9) . . . . ?
C36 C35 O4 Ti2 36.7(12) . . . . ?
C51 C46 O5 Ti1 40.0(13) . . . . ?
C47 C46 O5 Ti1 -140.7(10) . . . . ?
C62 C57 O6 Ti1 94.6(4) . . . . ?
C58 C57 O6 Ti1 -88.1(4) . . . . ?
C62 C57 O6 Ti2 -41.4(5) . . . 2_656 ?
C58 C57 O6 Ti2 135.8(3) . . . 2_656 ?
C28 C33 O7 C34 136.6(4) . . . . ?
C36 C34 O7 C33 -164.2(4) . . . . ?
C2 C68 O8 C67 61.2(5) . . . . ?
C2 C68 O8 Ti2 -131.4(4) . . . 2_656 ?
C62 C67 O8 C68 -150.0(4) . . . . ?
C62 C67 O8 Ti2 42.2(4) . . . 2_656 ?
C1 O1 Ti1 O5 144.0(6) . . . . ?
C1 O1 Ti1 O10 36.2(6) . . . . ?
C1 O1 Ti1 O10 -43.3(6) . . . 2_656 ?
C1 O1 Ti1 O6 -119.1(6) . . . . ?
C1 O1 Ti1 Ti1 -0.1(6) . . . 2_656 ?
C1 O1 Ti1 Ti2 -79.2(6) . . . 2_656 ?
C46 O5 Ti1 O1 65.4(11) . . . . ?
C46 O5 Ti1 O10 165.8(11) . . . . ?
C46 O5 Ti1 O10 -102.6(11) . . . 2_656 ?
C46 O5 Ti1 O6 -31.6(11) . . . . ?
C46 O5 Ti1 O9 -110.4(11) . . . . ?
C46 O5 Ti1 Ti1 -153.1(11) . . . 2_656 ?
C46 O5 Ti1 Ti2 -50.0(12) . . . 2_656 ?
Ti1 O10 Ti1 O1 -128.48(14) 2_656 . . . ?
Ti2 O10 Ti1 O1 66.7(4) . . . . ?
Ti1 O10 Ti1 O5 125.42(16) 2_656 . . . ?
Ti2 O10 Ti1 O5 -39.4(4) . . . . ?
Ti1 O10 Ti1 O10 -18.4(2) 2_656 . . 2_656 ?
Ti2 O10 Ti1 O10 176.8(3) . . . 2_656 ?
Ti1 O10 Ti1 O6 -13.9(4) 2_656 . . . ?
Ti2 O10 Ti1 O6 -178.7(3) . . . . ?
Ti1 O10 Ti1 O9 53.56(18) 2_656 . . . ?
Ti2 O10 Ti1 O9 -111.2(4) . . . . ?
Ti2 O10 Ti1 Ti1 -164.8(5) . . . 2_656 ?
Ti1 O10 Ti1 Ti2 -25.94(16) 2_656 . . 2_656 ?
Ti2 O10 Ti1 Ti2 169.3(3) . . . 2_656 ?
C35 O4 Ti2 O2 177.1(10) . . . . ?
C35 O4 Ti2 O3 -81.5(10) . . . . ?
C35 O4 Ti2 O10 84.4(10) . . . . ?
C35 O4 Ti2 O6 12.3(10) . . . 2_656 ?
C35 O4 Ti2 Ti1 51.3(10) . . . 2_656 ?
C12 O2 Ti2 O4 63.2(6) . . . . ?
C12 O2 Ti2 O3 -35.6(6) . . . . ?
C12 O2 Ti2 O10 155.2(6) . . . . ?
C12 O2 Ti2 O6 -149.5(5) . . . 2_656 ?
C12 O2 Ti2 O8 -118.1(6) . . . 2_656 ?
C12 O2 Ti2 Ti1 179.2(5) . . . 2_656 ?
C23 O3 Ti2 O4 -74.4(7) . . . . ?
C23 O3 Ti2 O2 30.9(7) . . . . ?
C23 O3 Ti2 O10 167.9(6) . . . . ?
C23 O3 Ti2 O6 -175.1(7) . . . 2_656 ?
C23 O3 Ti2 O8 113.3(7) . . . 2_656 ?
C23 O3 Ti2 Ti1 171.2(6) . . . 2_656 ?

_refine_diff_density_max         0.771
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.080




####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2057326'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
C36 H40 F5 N2 O4 Ti2, F5 Si, 2(C2 H3 N)
;

_chemical_formula_sum            'C40 H46 F10 N4 O4 Si Ti2'
_chemical_formula_weight         960.70

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'
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'
Si Si 0.0817 0.0704 '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                   8.8857(4)
_cell_length_b                   13.0733(5)
_cell_length_c                   18.4231(11)
_cell_angle_alpha                84.872(4)
_cell_angle_beta                 82.208(4)
_cell_angle_gamma                73.277(4)
_cell_volume                     2027.83(18)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    5429
_cell_measurement_theta_min      2.141
_cell_measurement_theta_max      29.203

_exptl_crystal_description       plate
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.573
_exptl_crystal_F_000             988
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    0.517
_shelx_estimated_absorpt_T_min   0.950
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.20966
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71075
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            14106
_diffrn_reflns_av_unetI/netI     0.0562
_diffrn_reflns_av_R_equivalents  ?
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         2.235
_diffrn_reflns_theta_max         27.529
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             14106
_reflns_number_gt                10493
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 _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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;

_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_refine_special_details          
;
 Refined as a 2-component twin. 
 Twin law: 
 180.0 degree rotation about  -1.  3.  0. reciprocal lattice direction
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1876P)²+5.5805P] 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         14106
_refine_ls_number_parameters     547
_refine_ls_number_restraints     521
_refine_ls_R_factor_all          0.1332
_refine_ls_R_factor_gt           0.1050
_refine_ls_wR_factor_ref         0.2964
_refine_ls_wR_factor_gt          0.2732
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_restrained_S_all      1.009
_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
C1 C 0.9156(7) 0.6100(5) 0.1223(3) 0.0181(11) Uani 1 1 d . U . . .
C2 C 0.9321(7) 0.5060(5) 0.1508(3) 0.0174(11) Uani 1 1 d . . . . .
C3 C 0.8757(7) 0.4373(6) 0.1149(3) 0.0172(12) Uani 1 1 d . . . . .
H3 H 0.886523 0.366026 0.134239 0.021 Uiso 1 1 calc R U . . .
C4 C 0.8035(7) 0.4721(5) 0.0509(3) 0.0197(12) Uani 1 1 d . . . . .
C5 C 0.7904(7) 0.5761(5) 0.0232(3) 0.0190(12) Uani 1 1 d . U . . .
H5 H 0.742205 0.599851 -0.020572 0.023 Uiso 1 1 calc R U . . .
C6 C 0.8457(7) 0.6474(5) 0.0577(3) 0.0174(11) Uani 1 1 d . U . . .
C7 C 0.7412(9) 0.3980(6) 0.0126(4) 0.0253(14) Uani 1 1 d . . . . .
H7A H 0.760627 0.328343 0.039648 0.038 Uiso 1 1 calc R U . . .
H7B H 0.627292 0.428670 0.010670 0.038 Uiso 1 1 calc R U . . .
H7C H 0.795319 0.389010 -0.037428 0.038 Uiso 1 1 calc R U . . .
C8 C 0.8222(7) 0.7621(5) 0.0272(3) 0.0202(12) Uani 1 1 d . . . . .
H8A H 0.906351 0.789906 0.040982 0.024 Uiso 1 1 calc R U . . .
H8B H 0.831298 0.763870 -0.027062 0.024 Uiso 1 1 calc R U . . .
C9 C 0.6414(7) 0.8837(5) 0.1219(3) 0.0164(11) Uani 1 1 d . . . . .
C10 C 0.6626(7) 0.8329(5) 0.0560(3) 0.0182(12) Uani 1 1 d . . . . .
C11 C 0.5306(8) 0.8479(5) 0.0183(3) 0.0205(12) Uani 1 1 d . . . . .
H11 H 0.543344 0.813570 -0.026398 0.025 Uiso 1 1 calc R U . . .
C12 C 0.3824(8) 0.9108(5) 0.0438(3) 0.0210(12) Uani 1 1 d . . . . .
C13 C 0.3654(7) 0.9606(6) 0.1094(3) 0.0179(12) Uani 1 1 d . . . . .
H13 H 0.264102 1.004301 0.127307 0.021 Uiso 1 1 calc R U . . .
C14 C 0.4921(7) 0.9485(5) 0.1495(3) 0.0177(12) Uani 1 1 d . . . . .
C15 C 0.2430(8) 0.9237(7) 0.0020(3) 0.0240(14) Uani 1 1 d . . . . .
H15A H 0.148292 0.970770 0.027949 0.036 Uiso 1 1 calc R U . . .
H15B H 0.263896 0.955216 -0.047270 0.036 Uiso 1 1 calc R U . . .
H15C H 0.226261 0.853606 -0.001714 0.036 Uiso 1 1 calc R U . . .
C16 C 0.4759(7) 1.0044(5) 0.2187(3) 0.0150(11) Uani 1 1 d . . . . .
H16A H 0.386511 1.070304 0.217740 0.018 Uiso 1 1 calc R U . . .
H16B H 0.573274 1.026014 0.220555 0.018 Uiso 1 1 calc R U . . .
C17 C 0.2865(8) 0.9176(7) 0.2934(3) 0.0247(15) Uani 1 1 d . . . . .
H17A H 0.279923 0.880139 0.250727 0.037 Uiso 1 1 calc R U . . .
H17B H 0.269862 0.874143 0.338328 0.037 Uiso 1 1 calc R U . . .
H17C H 0.205097 0.986559 0.294829 0.037 Uiso 1 1 calc R U . . .
C18 C 0.4610(7) 0.9938(5) 0.3531(3) 0.0132(11) Uani 1 1 d . . . . .
H18A H 0.564337 1.010086 0.346210 0.016 Uiso 1 1 calc R U . . .
H18B H 0.377097 1.062708 0.355103 0.016 Uiso 1 1 calc R U . . .
C19 C 0.5829(7) 0.8639(5) 0.4526(3) 0.0146(11) Uani 1 1 d . . . . .
C20 C 0.4467(7) 0.9313(5) 0.4253(3) 0.0150(11) Uani 1 1 d . . . . .
C21 C 0.3012(6) 0.9411(5) 0.4679(3) 0.0114(10) Uani 1 1 d . . . . .
H21 H 0.207869 0.987135 0.450500 0.014 Uiso 1 1 calc R U . . .
C22 C 0.2899(7) 0.8845(5) 0.5359(3) 0.0163(11) Uani 1 1 d . . . . .
C23 C 0.4280(7) 0.8182(5) 0.5608(3) 0.0177(12) Uani 1 1 d . . . . .
H23 H 0.421119 0.780105 0.606904 0.021 Uiso 1 1 calc R U . . .
C24 C 0.5767(7) 0.8056(5) 0.5203(3) 0.0160(11) Uani 1 1 d . . . . .
C25 C 0.1311(7) 0.8943(6) 0.5797(4) 0.0216(13) Uani 1 1 d . . . . .
H25A H 0.048518 0.944265 0.553566 0.032 Uiso 1 1 calc R U . . .
H25B H 0.110916 0.824003 0.586229 0.032 Uiso 1 1 calc R U . . .
H25C H 0.130410 0.921005 0.627811 0.032 Uiso 1 1 calc R U . . .
C26 C 0.7237(7) 0.7298(5) 0.5477(3) 0.0176(11) Uani 1 1 d . . . . .
H26A H 0.815479 0.758000 0.531211 0.021 Uiso 1 1 calc R U . . .
H26B H 0.710079 0.724801 0.601977 0.021 Uiso 1 1 calc R U . . .
C27 C 0.8493(7) 0.5898(5) 0.4531(3) 0.0168(11) Uani 1 1 d . . . . .
C28 C 0.7554(7) 0.6200(5) 0.5194(3) 0.0160(11) Uani 1 1 d . . . . .
C29 C 0.6844(7) 0.5461(5) 0.5578(3) 0.0163(11) Uani 1 1 d . . . . .
H29 H 0.618890 0.565862 0.602452 0.020 Uiso 1 1 calc R U . . .
C30 C 0.7055(7) 0.4435(5) 0.5334(3) 0.0177(12) Uani 1 1 d . . . . .
C31 C 0.7992(7) 0.4186(5) 0.4674(3) 0.0159(11) Uani 1 1 d . . . . .
H31 H 0.813255 0.350497 0.448863 0.019 Uiso 1 1 calc R U . . .
C32 C 0.8736(7) 0.4893(5) 0.4270(3) 0.0182(12) Uani 1 1 d . . . . .
C33 C 0.6268(8) 0.3675(6) 0.5776(3) 0.0199(12) Uani 1 1 d . . . . .
H33A H 0.566699 0.401227 0.622000 0.030 Uiso 1 1 calc R U . . .
H33B H 0.554918 0.349198 0.548314 0.030 Uiso 1 1 calc R U . . .
H33C H 0.707315 0.302403 0.591255 0.030 Uiso 1 1 calc R U . . .
C34 C 0.9753(7) 0.4602(5) 0.3557(3) 0.0173(12) Uani 1 1 d . . . . .
H34A H 1.017631 0.381401 0.355576 0.021 Uiso 1 1 calc R U . . .
H34B H 1.066225 0.490495 0.352295 0.021 Uiso 1 1 calc R U . . .
C35 C 0.7512(8) 0.4549(7) 0.2908(4) 0.0261(16) Uani 1 1 d . . . . .
H35A H 0.697082 0.481600 0.247056 0.039 Uiso 1 1 calc R U . . .
H35B H 0.788929 0.376678 0.291732 0.039 Uiso 1 1 calc R U . . .
H35C H 0.677464 0.477148 0.334827 0.039 Uiso 1 1 calc R U . . .
C36 C 1.0051(7) 0.4688(5) 0.2212(3) 0.0170(12) Uani 1 1 d . . . . .
H36A H 1.093980 0.500040 0.221979 0.020 Uiso 1 1 calc R U . . .
H36B H 1.048756 0.390041 0.222456 0.020 Uiso 1 1 calc R U . . .
C41 C 0.4733(8) 0.6737(6) 0.2011(4) 0.0260(14) Uani 1 1 d . . . . .
C42 C 0.4027(9) 0.6371(7) 0.1462(4) 0.0301(15) Uani 1 1 d . . . . .
H42A H 0.360306 0.578199 0.167387 0.045 Uiso 1 1 calc R U . . .
H42B H 0.482992 0.612059 0.104757 0.045 Uiso 1 1 calc R U . . .
H42C H 0.316831 0.696069 0.128979 0.045 Uiso 1 1 calc R U . . .
C43 C 0.9849(9) 1.1572(6) 0.2113(4) 0.0300(15) Uani 1 1 d . . . . .
C44 C 0.9067(11) 1.1163(8) 0.1609(6) 0.048(2) Uani 1 1 d . . . . .
H44A H 0.797738 1.161569 0.160171 0.073 Uiso 1 1 calc R U . . .
H44B H 0.905920 1.042947 0.176908 0.073 Uiso 1 1 calc R U . . .
H44C H 0.963763 1.116887 0.111483 0.073 Uiso 1 1 calc R U . . .
N1 N 0.4479(6) 0.9361(4) 0.2879(3) 0.0159(10) Uani 1 1 d . . . . .
H1 H 0.530698 0.865657 0.286231 0.019 Uiso 1 1 calc R U . . .
N2 N 0.8885(6) 0.4997(4) 0.2889(3) 0.0171(10) Uani 1 1 d . . . . .
H2 H 0.848368 0.579447 0.288443 0.021 Uiso 1 1 calc R U . . .
N3 N 0.5238(9) 0.7059(7) 0.2450(4) 0.0402(18) Uani 1 1 d . . . . .
N4 N 1.0442(10) 1.1910(7) 0.2498(4) 0.0450(17) Uani 1 1 d . . . . .
O1 O 0.9747(5) 0.6760(4) 0.1577(2) 0.0188(9) Uani 1 1 d . . . . .
O2 O 0.7661(5) 0.8730(3) 0.1599(2) 0.0167(9) Uani 1 1 d . . . . .
O3 O 0.7251(5) 0.8578(4) 0.4124(2) 0.0179(9) Uani 1 1 d . . . . .
O4 O 0.9246(5) 0.6583(3) 0.4142(2) 0.0180(9) Uani 1 1 d . . . . .
F1 F 1.0890(4) 0.8518(3) 0.1578(2) 0.0217(8) Uani 1 1 d . . . . .
F2 F 0.7993(4) 0.7427(3) 0.28816(18) 0.0183(7) Uani 1 1 d . . . . .
F3 F 1.0774(4) 0.7240(3) 0.2837(2) 0.0196(7) Uani 1 1 d . . . . .
F4 F 0.8895(4) 0.9025(3) 0.2833(2) 0.0172(8) Uani 1 1 d . . . . .
F5 F 1.0461(4) 0.8330(3) 0.4102(2) 0.0224(8) Uani 1 1 d . . . . .
Si1 Si 0.4519(2) 0.31490(17) 0.20486(10) 0.0248(4) Uani 1 1 d D . . . .
F6 F 0.5152(7) 0.2146(4) 0.1519(3) 0.0506(14) Uani 1 1 d . . . . .
F10 F 0.3910(7) 0.4174(4) 0.2589(3) 0.0511(15) Uani 1 1 d . . . . .
F7A F 0.3594(12) 0.2544(7) 0.2655(5) 0.0482(11) Uiso 0.644(10) 1 d D U P A 1
F8A F 0.3645(11) 0.3946(7) 0.1428(5) 0.0482(11) Uiso 0.644(10) 1 d D U P A 1
F9A F 0.6343(10) 0.3123(7) 0.2102(5) 0.0482(11) Uiso 0.644(10) 1 d D U P A 1
F7B F 0.430(2) 0.2322(12) 0.2719(8) 0.0482(11) Uiso 0.356(10) 1 d D U P A 2
F8B F 0.323(2) 0.3674(14) 0.1481(9) 0.0482(11) Uiso 0.356(10) 1 d D U P A 2
F9B F 0.6037(18) 0.3487(14) 0.1771(9) 0.0482(11) Uiso 0.356(10) 1 d D U P A 2
Ti1 Ti 0.93529(12) 0.79716(9) 0.20437(6) 0.0126(3) Uani 1 1 d . . . . .
Ti2 Ti 0.91128(12) 0.78572(9) 0.36673(6) 0.0151(3) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 O1 1.379(8) . ?
C1 C2 1.388(9) . ?
C1 C6 1.402(9) . ?
C2 C3 1.397(9) . ?
C2 C36 1.507(8) . ?
C3 C4 1.397(9) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(9) . ?
C4 C7 1.510(9) . ?
C5 C6 1.402(9) . ?
C5 H5 0.9500 . ?
C6 C8 1.520(9) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.510(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 O2 1.357(7) . ?
C9 C10 1.400(9) . ?
C9 C14 1.409(9) . ?
C10 C11 1.401(9) . ?
C11 C12 1.382(9) . ?
C11 H11 0.9500 . ?
C12 C13 1.393(9) . ?
C12 C15 1.506(8) . ?
C13 C14 1.393(9) . ?
C13 H13 0.9500 . ?
C14 C16 1.495(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 N1 1.524(7) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 N1 1.510(7) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C20 1.508(8) . ?
C18 N1 1.510(7) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 O3 1.360(7) . ?
C19 C20 1.402(8) . ?
C19 C24 1.405(8) . ?
C20 C21 1.397(7) . ?
C21 C22 1.403(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.392(9) . ?
C22 C25 1.505(8) . ?
C23 C24 1.399(8) . ?
C23 H23 0.9500 . ?
C24 C26 1.512(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C28 1.507(8) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 O4 1.366(7) . ?
C27 C32 1.387(9) . ?
C27 C28 1.402(8) . ?
C28 C29 1.393(8) . ?
C29 C30 1.406(9) . ?
C29 H29 0.9500 . ?
C30 C31 1.386(8) . ?
C30 C33 1.496(8) . ?
C31 C32 1.393(9) . ?
C31 H31 0.9500 . ?
C32 C34 1.502(8) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 N2 1.513(8) . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 N2 1.492(8) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 N2 1.514(7) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C41 N3 1.140(10) . ?
C41 C42 1.443(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 N4 1.125(11) . ?
C43 C44 1.452(12) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
N1 H1 1.0000 . ?
N2 H2 1.0000 . ?
O1 Ti1 1.792(5) . ?
O2 Ti1 1.801(4) . ?
O3 Ti2 1.789(4) . ?
O4 Ti2 1.791(5) . ?
F1 Ti1 1.802(3) . ?
F2 Ti1 2.035(3) . ?
F2 Ti2 2.064(3) . ?
F3 Ti2 2.023(4) . ?
F3 Ti1 2.049(4) . ?
F4 Ti1 2.012(4) . ?
F4 Ti2 2.055(4) . ?
F5 Ti2 1.799(3) . ?
Si1 F9B 1.547(14) . ?
Si1 F7A 1.586(9) . ?
Si1 F7B 1.597(14) . ?
Si1 F8A 1.600(9) . ?
Si1 F8B 1.618(15) . ?
Si1 F6 1.625(6) . ?
Si1 F9A 1.627(8) . ?
Si1 F10 1.660(5) . ?
Ti1 Ti2 2.9632(14) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 118.5(6) . . ?
O1 C1 C6 120.0(6) . . ?
C2 C1 C6 121.5(6) . . ?
C1 C2 C3 119.3(6) . . ?
C1 C2 C36 120.3(5) . . ?
C3 C2 C36 120.4(6) . . ?
C2 C3 C4 120.8(6) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 118.7(6) . . ?
C5 C4 C7 120.7(6) . . ?
C3 C4 C7 120.6(6) . . ?
C4 C5 C6 122.2(6) . . ?
C4 C5 H5 118.9 . . ?
C6 C5 H5 118.9 . . ?
C5 C6 C1 117.5(6) . . ?
C5 C6 C8 120.4(6) . . ?
C1 C6 C8 122.0(6) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C6 111.3(5) . . ?
C10 C8 H8A 109.4 . . ?
C6 C8 H8A 109.4 . . ?
C10 C8 H8B 109.4 . . ?
C6 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O2 C9 C10 120.4(5) . . ?
O2 C9 C14 118.5(5) . . ?
C10 C9 C14 121.2(6) . . ?
C9 C10 C11 118.1(6) . . ?
C9 C10 C8 121.0(6) . . ?
C11 C10 C8 120.9(6) . . ?
C12 C11 C10 122.3(6) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 118.2(6) . . ?
C11 C12 C15 120.6(6) . . ?
C13 C12 C15 121.1(6) . . ?
C14 C13 C12 122.1(6) . . ?
C14 C13 H13 118.9 . . ?
C12 C13 H13 118.9 . . ?
C13 C14 C9 118.1(6) . . ?
C13 C14 C16 122.5(6) . . ?
C9 C14 C16 119.4(5) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 N1 113.4(5) . . ?
C14 C16 H16A 108.9 . . ?
N1 C16 H16A 108.9 . . ?
C14 C16 H16B 108.9 . . ?
N1 C16 H16B 108.9 . . ?
H16A C16 H16B 107.7 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C20 C18 N1 113.7(5) . . ?
C20 C18 H18A 108.8 . . ?
N1 C18 H18A 108.8 . . ?
C20 C18 H18B 108.8 . . ?
N1 C18 H18B 108.8 . . ?
H18A C18 H18B 107.7 . . ?
O3 C19 C20 118.1(5) . . ?
O3 C19 C24 119.7(5) . . ?
C20 C19 C24 122.2(5) . . ?
C21 C20 C19 118.2(5) . . ?
C21 C20 C18 121.9(5) . . ?
C19 C20 C18 119.8(5) . . ?
C20 C21 C22 121.4(5) . . ?
C20 C21 H21 119.3 . . ?
C22 C21 H21 119.3 . . ?
C23 C22 C21 118.4(5) . . ?
C23 C22 C25 121.3(5) . . ?
C21 C22 C25 120.3(6) . . ?
C22 C23 C24 122.4(6) . . ?
C22 C23 H23 118.8 . . ?
C24 C23 H23 118.8 . . ?
C23 C24 C19 117.3(5) . . ?
C23 C24 C26 121.1(5) . . ?
C19 C24 C26 121.6(5) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C28 C26 C24 111.0(4) . . ?
C28 C26 H26A 109.4 . . ?
C24 C26 H26A 109.4 . . ?
C28 C26 H26B 109.4 . . ?
C24 C26 H26B 109.4 . . ?
H26A C26 H26B 108.0 . . ?
O4 C27 C32 118.5(5) . . ?
O4 C27 C28 119.9(6) . . ?
C32 C27 C28 121.5(6) . . ?
C29 C28 C27 117.6(6) . . ?
C29 C28 C26 119.9(5) . . ?
C27 C28 C26 122.4(5) . . ?
C28 C29 C30 122.8(5) . . ?
C28 C29 H29 118.6 . . ?
C30 C29 H29 118.6 . . ?
C31 C30 C29 116.8(6) . . ?
C31 C30 C33 123.0(6) . . ?
C29 C30 C33 120.2(5) . . ?
C30 C31 C32 122.6(6) . . ?
C30 C31 H31 118.7 . . ?
C32 C31 H31 118.7 . . ?
C27 C32 C31 118.6(6) . . ?
C27 C32 C34 119.8(5) . . ?
C31 C32 C34 121.6(6) . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C32 C34 N2 113.6(5) . . ?
C32 C34 H34A 108.8 . . ?
N2 C34 H34A 108.8 . . ?
C32 C34 H34B 108.8 . . ?
N2 C34 H34B 108.8 . . ?
H34A C34 H34B 107.7 . . ?
N2 C35 H35A 109.5 . . ?
N2 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
N2 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C2 C36 N2 112.9(5) . . ?
C2 C36 H36A 109.0 . . ?
N2 C36 H36A 109.0 . . ?
C2 C36 H36B 109.0 . . ?
N2 C36 H36B 109.0 . . ?
H36A C36 H36B 107.8 . . ?
N3 C41 C42 177.3(9) . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N4 C43 C44 178.5(10) . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C17 N1 C18 110.5(5) . . ?
C17 N1 C16 110.4(5) . . ?
C18 N1 C16 108.1(4) . . ?
C17 N1 H1 109.3 . . ?
C18 N1 H1 109.3 . . ?
C16 N1 H1 109.3 . . ?
C35 N2 C34 111.0(5) . . ?
C35 N2 C36 111.5(5) . . ?
C34 N2 C36 108.2(4) . . ?
C35 N2 H2 108.7 . . ?
C34 N2 H2 108.7 . . ?
C36 N2 H2 108.7 . . ?
C1 O1 Ti1 147.6(4) . . ?
C9 O2 Ti1 153.9(4) . . ?
C19 O3 Ti2 152.9(4) . . ?
C27 O4 Ti2 148.5(4) . . ?
Ti1 F2 Ti2 92.60(13) . . ?
Ti2 F3 Ti1 93.38(15) . . ?
Ti1 F4 Ti2 93.52(15) . . ?
F9B Si1 F7B 126.8(9) . . ?
F7A Si1 F8A 121.8(5) . . ?
F9B Si1 F8B 107.9(9) . . ?
F7B Si1 F8B 125.0(8) . . ?
F9B Si1 F6 89.0(6) . . ?
F7A Si1 F6 94.5(4) . . ?
F7B Si1 F6 88.4(6) . . ?
F8A Si1 F6 93.7(4) . . ?
F8B Si1 F6 86.6(7) . . ?
F7A Si1 F9A 121.1(5) . . ?
F8A Si1 F9A 116.5(5) . . ?
F6 Si1 F9A 89.4(4) . . ?
F9B Si1 F10 90.0(6) . . ?
F7A Si1 F10 86.2(4) . . ?
F7B Si1 F10 91.8(6) . . ?
F8A Si1 F10 86.8(4) . . ?
F8B Si1 F10 94.1(7) . . ?
F6 Si1 F10 178.8(3) . . ?
F9A Si1 F10 89.5(4) . . ?
O1 Ti1 O2 97.67(19) . . ?
O1 Ti1 F1 100.70(19) . . ?
O2 Ti1 F1 101.88(19) . . ?
O1 Ti1 F4 162.69(19) . . ?
O2 Ti1 F4 92.36(18) . . ?
F1 Ti1 F4 90.92(16) . . ?
O1 Ti1 F2 91.46(18) . . ?
O2 Ti1 F2 92.85(17) . . ?
F1 Ti1 F2 159.36(16) . . ?
F4 Ti1 F2 73.92(15) . . ?
O1 Ti1 F3 92.85(18) . . ?
O2 Ti1 F3 161.85(18) . . ?
F1 Ti1 F3 90.58(16) . . ?
F4 Ti1 F3 74.09(15) . . ?
F2 Ti1 F3 72.06(14) . . ?
O1 Ti1 Ti2 118.95(15) . . ?
O2 Ti1 Ti2 118.95(14) . . ?
F1 Ti1 Ti2 115.35(13) . . ?
F4 Ti1 Ti2 43.80(11) . . ?
F2 Ti1 Ti2 44.08(10) . . ?
F3 Ti1 Ti2 42.96(10) . . ?
O3 Ti2 O4 97.88(19) . . ?
O3 Ti2 F5 101.16(18) . . ?
O4 Ti2 F5 101.76(19) . . ?
O3 Ti2 F3 159.21(18) . . ?
O4 Ti2 F3 93.79(17) . . ?
F5 Ti2 F3 93.18(15) . . ?
O3 Ti2 F4 90.11(18) . . ?
O4 Ti2 F4 160.31(18) . . ?
F5 Ti2 F4 94.24(17) . . ?
F3 Ti2 F4 73.75(14) . . ?
O3 Ti2 F2 90.91(17) . . ?
O4 Ti2 F2 89.38(17) . . ?
F5 Ti2 F2 162.17(15) . . ?
F3 Ti2 F2 72.01(14) . . ?
F4 Ti2 F2 72.45(15) . . ?
O3 Ti2 Ti1 115.59(15) . . ?
O4 Ti2 Ti1 118.14(14) . . ?
F5 Ti2 Ti1 118.90(12) . . ?
F3 Ti2 Ti1 43.66(11) . . ?
F4 Ti2 Ti1 42.68(11) . . ?
F2 Ti2 Ti1 43.32(9) . . ?

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
O1 C1 C2 C3 -178.8(5) . . . . ?
C6 C1 C2 C3 -1.0(9) . . . . ?
O1 C1 C2 C36 3.3(8) . . . . ?
C6 C1 C2 C36 -178.9(5) . . . . ?
C1 C2 C3 C4 0.1(9) . . . . ?
C36 C2 C3 C4 178.1(5) . . . . ?
C2 C3 C4 C5 0.6(9) . . . . ?
C2 C3 C4 C7 -179.4(6) . . . . ?
C3 C4 C5 C6 -0.6(9) . . . . ?
C7 C4 C5 C6 179.4(6) . . . . ?
C4 C5 C6 C1 -0.2(9) . . . . ?
C4 C5 C6 C8 -177.3(5) . . . . ?
O1 C1 C6 C5 178.8(5) . . . . ?
C2 C1 C6 C5 1.0(8) . . . . ?
O1 C1 C6 C8 -4.2(8) . . . . ?
C2 C1 C6 C8 178.0(5) . . . . ?
C5 C6 C8 C10 85.7(7) . . . . ?
C1 C6 C8 C10 -91.2(7) . . . . ?
O2 C9 C10 C11 -179.0(5) . . . . ?
C14 C9 C10 C11 -0.3(8) . . . . ?
O2 C9 C10 C8 2.3(8) . . . . ?
C14 C9 C10 C8 -179.0(5) . . . . ?
C6 C8 C10 C9 88.1(7) . . . . ?
C6 C8 C10 C11 -90.6(7) . . . . ?
C9 C10 C11 C12 0.3(9) . . . . ?
C8 C10 C11 C12 179.0(6) . . . . ?
C10 C11 C12 C13 0.0(9) . . . . ?
C10 C11 C12 C15 -179.2(6) . . . . ?
C11 C12 C13 C14 -0.2(9) . . . . ?
C15 C12 C13 C14 178.9(6) . . . . ?
C12 C13 C14 C9 0.2(9) . . . . ?
C12 C13 C14 C16 178.0(6) . . . . ?
O2 C9 C14 C13 178.8(5) . . . . ?
C10 C9 C14 C13 0.1(9) . . . . ?
O2 C9 C14 C16 0.9(8) . . . . ?
C10 C9 C14 C16 -177.8(5) . . . . ?
C13 C14 C16 N1 95.8(7) . . . . ?
C9 C14 C16 N1 -86.4(6) . . . . ?
O3 C19 C20 C21 -177.4(5) . . . . ?
C24 C19 C20 C21 0.9(9) . . . . ?
O3 C19 C20 C18 0.3(8) . . . . ?
C24 C19 C20 C18 178.6(5) . . . . ?
N1 C18 C20 C21 -91.2(7) . . . . ?
N1 C18 C20 C19 91.2(6) . . . . ?
C19 C20 C21 C22 -0.7(9) . . . . ?
C18 C20 C21 C22 -178.4(5) . . . . ?
C20 C21 C22 C23 0.5(9) . . . . ?
C20 C21 C22 C25 -178.3(5) . . . . ?
C21 C22 C23 C24 -0.4(9) . . . . ?
C25 C22 C23 C24 178.4(6) . . . . ?
C22 C23 C24 C19 0.6(9) . . . . ?
C22 C23 C24 C26 -177.7(5) . . . . ?
O3 C19 C24 C23 177.4(5) . . . . ?
C20 C19 C24 C23 -0.8(9) . . . . ?
O3 C19 C24 C26 -4.3(8) . . . . ?
C20 C19 C24 C26 177.5(5) . . . . ?
C23 C24 C26 C28 91.0(6) . . . . ?
C19 C24 C26 C28 -87.2(6) . . . . ?
O4 C27 C28 C29 -178.4(5) . . . . ?
C32 C27 C28 C29 -1.2(9) . . . . ?
O4 C27 C28 C26 4.6(9) . . . . ?
C32 C27 C28 C26 -178.2(5) . . . . ?
C24 C26 C28 C29 -86.9(6) . . . . ?
C24 C26 C28 C27 90.1(6) . . . . ?
C27 C28 C29 C30 1.1(9) . . . . ?
C26 C28 C29 C30 178.2(5) . . . . ?
C28 C29 C30 C31 -1.3(9) . . . . ?
C28 C29 C30 C33 179.5(6) . . . . ?
C29 C30 C31 C32 1.6(9) . . . . ?
C33 C30 C31 C32 -179.2(6) . . . . ?
O4 C27 C32 C31 178.8(5) . . . . ?
C28 C27 C32 C31 1.5(9) . . . . ?
O4 C27 C32 C34 -2.7(8) . . . . ?
C28 C27 C32 C34 -179.9(5) . . . . ?
C30 C31 C32 C27 -1.8(9) . . . . ?
C30 C31 C32 C34 179.7(5) . . . . ?
C27 C32 C34 N2 -82.8(7) . . . . ?
C31 C32 C34 N2 95.7(7) . . . . ?
C1 C2 C36 N2 82.5(7) . . . . ?
C3 C2 C36 N2 -95.4(7) . . . . ?
C20 C18 N1 C17 63.0(7) . . . . ?
C20 C18 N1 C16 -176.1(5) . . . . ?
C14 C16 N1 C17 -68.4(7) . . . . ?
C14 C16 N1 C18 170.7(5) . . . . ?
C32 C34 N2 C35 -59.4(7) . . . . ?
C32 C34 N2 C36 177.9(5) . . . . ?
C2 C36 N2 C35 58.6(7) . . . . ?
C2 C36 N2 C34 -179.0(5) . . . . ?
C2 C1 O1 Ti1 -120.1(7) . . . . ?
C6 C1 O1 Ti1 62.1(10) . . . . ?
C10 C9 O2 Ti1 -52.6(11) . . . . ?
C14 C9 O2 Ti1 128.7(8) . . . . ?
C20 C19 O3 Ti2 -127.1(8) . . . . ?
C24 C19 O3 Ti2 54.6(11) . . . . ?
C32 C27 O4 Ti2 122.9(7) . . . . ?
C28 C27 O4 Ti2 -59.8(10) . . . . ?
C1 O1 Ti1 O2 -27.8(8) . . . . ?
C1 O1 Ti1 F1 -131.5(7) . . . . ?
C1 O1 Ti1 F4 97.1(9) . . . . ?
C1 O1 Ti1 F2 65.3(8) . . . . ?
C1 O1 Ti1 F3 137.4(8) . . . . ?
C1 O1 Ti1 Ti2 101.5(7) . . . . ?
C9 O2 Ti1 O1 21.4(9) . . . . ?
C9 O2 Ti1 F1 124.1(9) . . . . ?
C9 O2 Ti1 F4 -144.5(9) . . . . ?
C9 O2 Ti1 F2 -70.5(9) . . . . ?
C9 O2 Ti1 F3 -103.5(10) . . . . ?
C9 O2 Ti1 Ti2 -107.9(9) . . . . ?
C19 O3 Ti2 O4 -20.7(9) . . . . ?
C19 O3 Ti2 F5 -124.4(8) . . . . ?
C19 O3 Ti2 F3 102.9(9) . . . . ?
C19 O3 Ti2 F4 141.3(8) . . . . ?
C19 O3 Ti2 F2 68.8(8) . . . . ?
C19 O3 Ti2 Ti1 105.8(8) . . . . ?
C27 O4 Ti2 O3 24.3(8) . . . . ?
C27 O4 Ti2 F5 127.5(7) . . . . ?
C27 O4 Ti2 F3 -138.5(7) . . . . ?
C27 O4 Ti2 F4 -88.8(9) . . . . ?
C27 O4 Ti2 F2 -66.5(8) . . . . ?
C27 O4 Ti2 Ti1 -100.3(7) . . . . ?

_refine_diff_density_max         2.991
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.198



####################################################################### 
# 
# 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_5
_database_code_depnum_ccdc_archive 'CCDC 2057324'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.007 0.000 527 109 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;

Solvent is MeCN (22 electrons) 110 electrons in the cell
equates to 5 MeCN and hence 2.5 per asym unit. 
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 C52 H60 Br4 N2 O9 Ti2, 2(C2 H3 N) [+ 2.5MeCN] 
;

_chemical_formula_sum            'C56 H66 Br4 N4 O9 Ti2'
_chemical_formula_weight         1354.56

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'
Br Br -0.2901 2.4595 '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                   12.8059(9)
_cell_length_b                   14.7294(9)
_cell_length_c                   18.6847(13)
_cell_angle_alpha                111.546(5)
_cell_angle_beta                 94.299(6)
_cell_angle_gamma                96.876(5)
_cell_volume                     3227.4(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18942
_cell_measurement_theta_min      1.50
_cell_measurement_theta_max      29.55

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_F_000             1372
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    2.775
_shelx_estimated_absorpt_T_min   0.435
_shelx_estimated_absorpt_T_max   0.607
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_correction_T_min  0.625
_exptl_absorpt_correction_T_max  0.825
_exptl_absorpt_process_details   
;
Face index absorption correction within 
Stoe X-AREA (Tompa method)
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-fosu sealed tube'
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 6.67
_diffrn_reflns_number            25790
_diffrn_reflns_av_unetI/netI     0.1022
_diffrn_reflns_av_R_equivalents  0.0792
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.520
_diffrn_reflns_theta_max         26.373
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             13079
_reflns_number_gt                8355
_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       'Stoe X-AREA'
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.0511P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13079
_refine_ls_number_parameters     699
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1066
_refine_ls_wR_factor_gt          0.0995
_refine_ls_goodness_of_fit_ref   0.859
_refine_ls_restrained_S_all      0.859
_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
C1 C 0.6836(3) 0.7545(3) 0.2064(2) 0.0256(9) Uani 1 1 d . . . . .
C2 C 0.6161(3) 0.8100(3) 0.2544(2) 0.0263(9) Uani 1 1 d . . . . .
C3 C 0.5607(4) 0.8706(3) 0.2286(3) 0.0323(10) Uani 1 1 d . . . . .
H3 H 0.515725 0.909074 0.261230 0.039 Uiso 1 1 calc R U . . .
C4 C 0.5693(4) 0.8765(3) 0.1571(3) 0.0373(12) Uani 1 1 d . . . . .
C5 C 0.6349(4) 0.8179(3) 0.1096(3) 0.0354(11) Uani 1 1 d . . . . .
H5 H 0.642008 0.821257 0.060333 0.042 Uiso 1 1 calc R U . . .
C6 C 0.6899(4) 0.7552(3) 0.1321(2) 0.0294(10) Uani 1 1 d . . . . .
C7 C 0.5121(5) 0.9455(4) 0.1314(3) 0.0539(16) Uani 1 1 d . . . . .
H7A H 0.559685 1.007937 0.143727 0.081 Uiso 1 1 calc R U . . .
H7B H 0.449472 0.958268 0.158425 0.081 Uiso 1 1 calc R U . . .
H7C H 0.489881 0.914905 0.075260 0.081 Uiso 1 1 calc R U . . .
C8 C 0.7549(3) 0.6893(3) 0.0770(2) 0.0294(10) Uani 1 1 d . . . . .
H8A H 0.813478 0.676353 0.107776 0.035 Uiso 1 1 calc R U . . .
H8B H 0.786955 0.725018 0.046305 0.035 Uiso 1 1 calc R U . . .
C10 C 0.6666(3) 0.5122(3) 0.0452(2) 0.0293(10) Uani 1 1 d . . . . .
C11 C 0.6926(3) 0.5910(3) 0.0216(3) 0.0299(10) Uani 1 1 d . . . . .
C12 C 0.6584(4) 0.5752(3) -0.0549(2) 0.0327(10) Uani 1 1 d . . . . .
H12 H 0.673192 0.628038 -0.072098 0.039 Uiso 1 1 calc R U . . .
C13 C 0.6031(4) 0.4850(4) -0.1077(3) 0.0380(12) Uani 1 1 d . . . . .
C14 C 0.5822(4) 0.4077(4) -0.0829(3) 0.0343(11) Uani 1 1 d . . . . .
H14 H 0.546281 0.345113 -0.118176 0.041 Uiso 1 1 calc R U . . .
C15 C 0.6138(3) 0.4219(3) -0.0062(2) 0.0279(10) Uani 1 1 d . . . . .
C17 C 0.5670(6) 0.4705(4) -0.1913(3) 0.0612(18) Uani 1 1 d . . . . .
H17A H 0.490555 0.471223 -0.197984 0.092 Uiso 1 1 calc R U . . .
H17B H 0.582578 0.406872 -0.226440 0.092 Uiso 1 1 calc R U . . .
H17C H 0.604800 0.524014 -0.203301 0.092 Uiso 1 1 calc R U . . .
C18 C 0.5891(3) 0.3387(3) 0.0220(3) 0.0298(10) Uani 1 1 d . . . . .
H18A H 0.551342 0.279322 -0.021643 0.036 Uiso 1 1 calc R U . . .
H18B H 0.541506 0.358064 0.062617 0.036 Uiso 1 1 calc R U . . .
C19 C 0.7637(4) 0.2863(4) -0.0035(3) 0.0403(12) Uani 1 1 d . . . . .
H19A H 0.729818 0.228485 -0.048943 0.060 Uiso 1 1 calc R U . . .
H19B H 0.827156 0.270635 0.019329 0.060 Uiso 1 1 calc R U . . .
H19C H 0.783991 0.341827 -0.019302 0.060 Uiso 1 1 calc R U . . .
C20 C 0.6664(3) 0.2330(3) 0.0860(2) 0.0270(9) Uani 1 1 d . . . . .
H20A H 0.650670 0.168344 0.041884 0.032 Uiso 1 1 calc R U . . .
H20B H 0.731295 0.232785 0.118284 0.032 Uiso 1 1 calc R U . . .
C21 C 0.5834(3) 0.3254(3) 0.2032(2) 0.0216(9) Uani 1 1 d . . . . .
C22 C 0.5765(3) 0.2435(3) 0.1335(2) 0.0244(9) Uani 1 1 d . . . . .
C23 C 0.4878(3) 0.1710(3) 0.1106(2) 0.0281(10) Uani 1 1 d . . . . .
H23 H 0.483170 0.115956 0.063006 0.034 Uiso 1 1 calc R U . . .
C24 C 0.4047(3) 0.1769(3) 0.1558(3) 0.0281(10) Uani 1 1 d . . . . .
C25 C 0.4138(3) 0.2605(3) 0.2237(2) 0.0257(9) Uani 1 1 d . . . . .
H25 H 0.357853 0.265919 0.254953 0.031 Uiso 1 1 calc R U . . .
C26 C 0.4997(3) 0.3363(3) 0.2486(2) 0.0240(9) Uani 1 1 d . . . . .
C27 C 0.3093(3) 0.0968(4) 0.1314(3) 0.0390(12) Uani 1 1 d . . . . .
H27A H 0.293214 0.079649 0.175754 0.058 Uiso 1 1 calc R U . . .
H27B H 0.324382 0.038259 0.089505 0.058 Uiso 1 1 calc R U . . .
H27C H 0.248371 0.120427 0.113064 0.058 Uiso 1 1 calc R U . . .
C28 C 0.5035(3) 0.4262(3) 0.3214(2) 0.0238(9) Uani 1 1 d . . . . .
H28A H 0.431089 0.442839 0.326893 0.029 Uiso 1 1 calc R U . . .
H28B H 0.548726 0.482749 0.316916 0.029 Uiso 1 1 calc R U . . .
C29 C 0.6551(3) 0.4380(3) 0.4220(2) 0.0221(9) Uani 1 1 d . . . . .
C30 C 0.5465(3) 0.4113(3) 0.3935(2) 0.0214(8) Uani 1 1 d . . . . .
C31 C 0.4796(3) 0.3721(3) 0.4330(2) 0.0255(9) Uani 1 1 d . . . . .
H31 H 0.406045 0.354264 0.414338 0.031 Uiso 1 1 calc R U . . .
C32 C 0.5168(3) 0.3578(3) 0.4995(2) 0.0256(9) Uani 1 1 d . . . . .
C33 C 0.6234(3) 0.3867(3) 0.5266(2) 0.0265(9) Uani 1 1 d . . . . .
H33 H 0.649452 0.377971 0.572237 0.032 Uiso 1 1 calc R U . . .
C34 C 0.6944(3) 0.4279(3) 0.4902(2) 0.0255(9) Uani 1 1 d . . . . .
C35 C 0.4421(3) 0.3125(4) 0.5400(3) 0.0341(11) Uani 1 1 d . . . . .
H35A H 0.370241 0.297008 0.512134 0.051 Uiso 1 1 calc R U . . .
H35B H 0.464791 0.251613 0.540856 0.051 Uiso 1 1 calc R U . . .
H35C H 0.442564 0.359199 0.593260 0.051 Uiso 1 1 calc R U . . .
C36 C 0.8093(3) 0.4624(3) 0.5250(2) 0.0242(9) Uani 1 1 d . . . . .
H36A H 0.853439 0.462632 0.483733 0.029 Uiso 1 1 calc R U . . .
H36B H 0.832997 0.415864 0.547465 0.029 Uiso 1 1 calc R U . . .
C37 C 0.8324(3) 0.6505(3) 0.5697(2) 0.0235(9) Uani 1 1 d . . . . .
C38 C 0.8246(3) 0.5658(3) 0.5879(2) 0.0254(9) Uani 1 1 d . . . . .
C39 C 0.8305(3) 0.5808(3) 0.6661(2) 0.0277(10) Uani 1 1 d . . . . .
H39 H 0.824359 0.524422 0.679753 0.033 Uiso 1 1 calc R U . . .
C40 C 0.8448(3) 0.6733(4) 0.7251(2) 0.0295(10) Uani 1 1 d . . . . .
C41 C 0.8557(3) 0.7555(4) 0.7041(3) 0.0311(10) Uani 1 1 d . . . . .
H41 H 0.868599 0.820028 0.743517 0.037 Uiso 1 1 calc R U . . .
C42 C 0.8481(3) 0.7446(3) 0.6270(3) 0.0277(10) Uani 1 1 d . . . . .
C43 C 0.8466(4) 0.6864(4) 0.8097(3) 0.0392(12) Uani 1 1 d . . . . .
H43A H 0.777094 0.699104 0.826110 0.059 Uiso 1 1 calc R U . . .
H43B H 0.900974 0.742466 0.841627 0.059 Uiso 1 1 calc R U . . .
H43C H 0.862933 0.626207 0.815863 0.059 Uiso 1 1 calc R U . . .
C44 C 0.8542(3) 0.8335(3) 0.6049(3) 0.0302(10) Uani 1 1 d . . . . .
H44A H 0.783471 0.835351 0.580589 0.036 Uiso 1 1 calc R U . . .
H44B H 0.873890 0.894342 0.652321 0.036 Uiso 1 1 calc R U . . .
C45 C 1.0429(3) 0.8333(4) 0.5844(3) 0.0349(11) Uani 1 1 d . . . . .
H45A H 1.065734 0.895853 0.628786 0.052 Uiso 1 1 calc R U . . .
H45B H 1.091903 0.826826 0.545595 0.052 Uiso 1 1 calc R U . . .
H45C H 1.042682 0.778136 0.601846 0.052 Uiso 1 1 calc R U . . .
C46 C 0.9358(3) 0.9170(3) 0.5221(3) 0.0265(9) Uani 1 1 d . . . . .
H46A H 0.970592 0.978241 0.565390 0.032 Uiso 1 1 calc R U . . .
H46B H 0.980146 0.905055 0.479380 0.032 Uiso 1 1 calc R U . . .
C47 C 0.7691(3) 0.8628(3) 0.4282(2) 0.0225(9) Uani 1 1 d . . . . .
C48 C 0.8297(3) 0.9337(3) 0.4945(2) 0.0232(9) Uani 1 1 d . . . . .
C49 C 0.7947(3) 1.0224(3) 0.5319(2) 0.0277(9) Uani 1 1 d . . . . .
H49 H 0.837017 1.070967 0.576544 0.033 Uiso 1 1 calc R U . . .
C50 C 0.6981(3) 1.0419(3) 0.5052(3) 0.0301(10) Uani 1 1 d . . . . .
C51 C 0.6380(3) 0.9683(3) 0.4405(2) 0.0271(9) Uani 1 1 d . . . . .
H51 H 0.571265 0.979863 0.422778 0.033 Uiso 1 1 calc R U . . .
C52 C 0.6702(3) 0.8792(3) 0.4006(2) 0.0226(9) Uani 1 1 d . . . . .
C53 C 0.6622(4) 1.1408(4) 0.5474(3) 0.0452(13) Uani 1 1 d . . . . .
H53A H 0.715816 1.181830 0.591270 0.068 Uiso 1 1 calc R U . . .
H53B H 0.653023 1.174670 0.511553 0.068 Uiso 1 1 calc R U . . .
H53C H 0.594636 1.129423 0.566610 0.068 Uiso 1 1 calc R U . . .
C54 C 0.6011(3) 0.8011(3) 0.3309(2) 0.0266(9) Uani 1 1 d . . . . .
H54A H 0.615554 0.735330 0.327820 0.032 Uiso 1 1 calc R U . . .
H54B H 0.525888 0.804213 0.339166 0.032 Uiso 1 1 calc R U . . .
C61 C 0.8036(6) 0.0291(4) 0.1263(4) 0.0656(19) Uani 1 1 d . . . . .
C62 C 0.8350(6) 0.0243(4) 0.2003(3) 0.0632(18) Uani 1 1 d . . . . .
H62A H 0.865853 -0.035906 0.192300 0.095 Uiso 1 1 calc R U . . .
H62B H 0.772778 0.023257 0.227701 0.095 Uiso 1 1 calc R U . . .
H62C H 0.887686 0.082284 0.231341 0.095 Uiso 1 1 calc R U . . .
C63 C 0.5805(4) 0.1524(4) 0.3375(3) 0.0461(13) Uani 1 1 d . . . . .
H63A H 0.623919 0.100280 0.331819 0.069 Uiso 1 1 calc R U . . .
H63B H 0.607705 0.209476 0.385421 0.069 Uiso 1 1 calc R U . . .
H63C H 0.583444 0.172345 0.293032 0.069 Uiso 1 1 calc R U . . .
C64 C 0.4722(4) 0.1156(4) 0.3408(3) 0.0450(12) Uani 1 1 d . . . . .
N1 N 0.6884(3) 0.3137(3) 0.0547(2) 0.0271(8) Uani 1 1 d . . . . .
H1 H 0.724170 0.374683 0.098967 0.032 Uiso 1 1 calc R U . . .
N2 N 0.9341(3) 0.8318(3) 0.5494(2) 0.0259(8) Uani 1 1 d . . . . .
H2 H 0.914068 0.768883 0.502812 0.031 Uiso 1 1 calc R U . . .
N3 N 0.7785(7) 0.0327(5) 0.0686(3) 0.113(3) Uani 1 1 d . . . . .
N4 N 0.3861(4) 0.0881(4) 0.3427(4) 0.0741(16) Uani 1 1 d . . . . .
O1 O 0.7383(2) 0.6950(2) 0.22990(16) 0.0276(7) Uani 1 1 d . . . . .
O2 O 0.6951(3) 0.5158(2) 0.11815(16) 0.0330(7) Uani 1 1 d . . . . .
H2A H 0.722685 0.573787 0.147047 0.050 Uiso 1 1 calc R U . . .
O3 O 0.6701(2) 0.3967(2) 0.22417(15) 0.0227(6) Uani 1 1 d . . . . .
O4 O 0.7229(2) 0.4796(2) 0.38555(15) 0.0242(6) Uani 1 1 d . . . . .
O5 O 0.8264(2) 0.6464(2) 0.49521(16) 0.0297(7) Uani 1 1 d . . . . .
H5A H 0.803274 0.588185 0.464334 0.045 Uiso 1 1 calc R U . . .
O6 O 0.8037(2) 0.7756(2) 0.39160(15) 0.0234(6) Uani 1 1 d . . . . .
O7 O 0.8116(2) 0.5778(2) 0.29986(15) 0.0218(6) Uani 1 1 d . . . . .
Br1 Br 1.03835(3) 0.70528(3) 0.37956(3) 0.03043(11) Uani 1 1 d . . . . .
Br2 Br 0.93998(4) 0.86380(4) 0.29109(3) 0.03535(12) Uani 1 1 d . . . . .
Br3 Br 0.81039(4) 0.28108(3) 0.29815(3) 0.03491(12) Uani 1 1 d . . . . .
Br4 Br 0.90993(3) 0.40720(4) 0.18148(3) 0.03278(12) Uani 1 1 d . . . . .
Ti1 Ti 0.85229(6) 0.70154(6) 0.30237(4) 0.02240(16) Uani 1 1 d . . . . .
Ti2 Ti 0.78827(5) 0.45158(6) 0.29535(4) 0.02106(16) Uani 1 1 d . . . . .
O9 O 0.9373(2) 0.4911(2) 0.36903(18) 0.0281(7) Uani 1 1 d D . . . .
O8 O 0.9298(2) 0.6332(2) 0.20359(18) 0.0322(7) Uani 1 1 d D . . . .
H8C H 0.932(4) 0.574(2) 0.196(3) 0.048 Uiso 1 1 d D U . . .
H8D H 0.993(3) 0.654(3) 0.203(3) 0.048 Uiso 1 1 d D U . . .
H9A H 0.966(4) 0.549(2) 0.382(3) 0.048 Uiso 1 1 d D U . . .
H9B H 0.977(3) 0.452(3) 0.353(3) 0.048 Uiso 1 1 d D 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
C1 O1 1.355(5) . ?
C1 C6 1.401(6) . ?
C1 C2 1.402(6) . ?
C2 C3 1.396(6) . ?
C2 C54 1.508(6) . ?
C3 C4 1.382(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.401(7) . ?
C4 C7 1.511(6) . ?
C5 C6 1.387(6) . ?
C5 H5 0.9500 . ?
C6 C8 1.511(6) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C11 1.518(6) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 O2 1.365(5) . ?
C10 C15 1.377(6) . ?
C10 C11 1.400(6) . ?
C11 C12 1.388(6) . ?
C12 C13 1.395(6) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(7) . ?
C13 C17 1.525(6) . ?
C14 C15 1.392(6) . ?
C14 H14 0.9500 . ?
C15 C18 1.511(6) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N1 1.512(5) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N1 1.485(6) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.494(6) . ?
C20 N1 1.514(5) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O3 1.358(5) . ?
C21 C22 1.401(6) . ?
C21 C26 1.404(6) . ?
C22 C23 1.384(6) . ?
C23 C24 1.399(6) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(6) . ?
C24 C27 1.506(6) . ?
C25 C26 1.385(6) . ?
C25 H25 0.9500 . ?
C26 C28 1.503(6) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.517(5) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O4 1.365(5) . ?
C29 C34 1.399(5) . ?
C29 C30 1.406(5) . ?
C30 C31 1.379(6) . ?
C31 C32 1.395(6) . ?
C31 H31 0.9500 . ?
C32 C33 1.378(6) . ?
C32 C35 1.502(6) . ?
C33 C34 1.386(6) . ?
C33 H33 0.9500 . ?
C34 C36 1.511(5) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.524(6) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O5 1.367(5) . ?
C37 C42 1.385(6) . ?
C37 C38 1.403(6) . ?
C38 C39 1.390(6) . ?
C39 C40 1.384(6) . ?
C39 H39 0.9500 . ?
C40 C41 1.398(6) . ?
C40 C43 1.518(6) . ?
C41 C42 1.384(6) . ?
C41 H41 0.9500 . ?
C42 C44 1.507(6) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N2 1.506(6) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N2 1.489(5) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.498(5) . ?
C46 N2 1.515(5) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O6 1.360(5) . ?
C47 C48 1.393(5) . ?
C47 C52 1.412(5) . ?
C48 C49 1.383(6) . ?
C49 C50 1.400(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.389(6) . ?
C50 C53 1.525(6) . ?
C51 C52 1.380(6) . ?
C51 H51 0.9500 . ?
C52 C54 1.512(6) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C61 N3 1.124(7) . ?
C61 C62 1.441(8) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.442(8) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 N4 1.136(7) . ?
N1 H1 1.0000 . ?
N2 H2 1.0000 . ?
O1 Ti1 1.883(3) . ?
O2 H2A 0.8400 . ?
O3 Ti2 1.825(3) . ?
O4 Ti2 1.869(3) . ?
O5 H5A 0.8400 . ?
O6 Ti1 1.828(3) . ?
O7 Ti2 1.817(3) . ?
O7 Ti1 1.817(3) . ?
Br1 Ti1 2.6748(8) . ?
Br2 Ti1 2.6040(9) . ?
Br3 Ti2 2.5796(9) . ?
Br4 Ti2 2.6647(9) . ?
Ti1 O8 2.134(3) . ?
Ti2 O9 2.152(3) . ?
O9 H9A 0.82(3) . ?
O9 H9B 0.81(3) . ?
O8 H8C 0.83(3) . ?
O8 H8D 0.83(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
O1 C1 C6 119.4(4) . . ?
O1 C1 C2 120.0(4) . . ?
C6 C1 C2 120.4(4) . . ?
C3 C2 C1 118.7(4) . . ?
C3 C2 C54 121.0(4) . . ?
C1 C2 C54 120.3(4) . . ?
C4 C3 C2 122.2(5) . . ?
C4 C3 H3 118.9 . . ?
C2 C3 H3 118.9 . . ?
C3 C4 C5 117.8(4) . . ?
C3 C4 C7 121.4(5) . . ?
C5 C4 C7 120.8(4) . . ?
C6 C5 C4 122.2(4) . . ?
C6 C5 H5 118.9 . . ?
C4 C5 H5 118.9 . . ?
C5 C6 C1 118.6(4) . . ?
C5 C6 C8 120.2(4) . . ?
C1 C6 C8 121.2(4) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 C11 114.4(4) . . ?
C6 C8 H8A 108.7 . . ?
C11 C8 H8A 108.7 . . ?
C6 C8 H8B 108.7 . . ?
C11 C8 H8B 108.7 . . ?
H8A C8 H8B 107.6 . . ?
O2 C10 C15 114.6(4) . . ?
O2 C10 C11 123.9(4) . . ?
C15 C10 C11 121.4(4) . . ?
C12 C11 C10 116.8(4) . . ?
C12 C11 C8 121.5(4) . . ?
C10 C11 C8 121.6(4) . . ?
C11 C12 C13 122.8(4) . . ?
C11 C12 H12 118.6 . . ?
C13 C12 H12 118.6 . . ?
C14 C13 C12 118.6(4) . . ?
C14 C13 C17 120.1(4) . . ?
C12 C13 C17 121.2(4) . . ?
C13 C14 C15 119.9(4) . . ?
C13 C14 H14 120.1 . . ?
C15 C14 H14 120.1 . . ?
C10 C15 C14 120.4(4) . . ?
C10 C15 C18 119.3(4) . . ?
C14 C15 C18 120.3(4) . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 N1 111.9(3) . . ?
C15 C18 H18A 109.2 . . ?
N1 C18 H18A 109.2 . . ?
C15 C18 H18B 109.2 . . ?
N1 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 N1 114.1(3) . . ?
C22 C20 H20A 108.7 . . ?
N1 C20 H20A 108.7 . . ?
C22 C20 H20B 108.7 . . ?
N1 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
O3 C21 C22 118.8(4) . . ?
O3 C21 C26 120.4(4) . . ?
C22 C21 C26 120.7(4) . . ?
C23 C22 C21 119.5(4) . . ?
C23 C22 C20 120.5(4) . . ?
C21 C22 C20 119.9(4) . . ?
C22 C23 C24 121.5(4) . . ?
C22 C23 H23 119.2 . . ?
C24 C23 H23 119.2 . . ?
C25 C24 C23 117.0(4) . . ?
C25 C24 C27 121.7(4) . . ?
C23 C24 C27 121.3(4) . . ?
C26 C25 C24 123.9(4) . . ?
C26 C25 H25 118.0 . . ?
C24 C25 H25 118.0 . . ?
C25 C26 C21 117.3(4) . . ?
C25 C26 C28 121.4(4) . . ?
C21 C26 C28 121.3(4) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 C30 112.6(3) . . ?
C26 C28 H28A 109.1 . . ?
C30 C28 H28A 109.1 . . ?
C26 C28 H28B 109.1 . . ?
C30 C28 H28B 109.1 . . ?
H28A C28 H28B 107.8 . . ?
O4 C29 C34 119.0(3) . . ?
O4 C29 C30 119.9(3) . . ?
C34 C29 C30 121.0(4) . . ?
C31 C30 C29 118.5(4) . . ?
C31 C30 C28 120.7(3) . . ?
C29 C30 C28 120.9(4) . . ?
C30 C31 C32 121.9(4) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 117.9(4) . . ?
C33 C32 C35 121.6(4) . . ?
C31 C32 C35 120.5(4) . . ?
C32 C33 C34 122.9(4) . . ?
C32 C33 H33 118.5 . . ?
C34 C33 H33 118.5 . . ?
C33 C34 C29 117.7(4) . . ?
C33 C34 C36 120.2(4) . . ?
C29 C34 C36 122.1(4) . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C34 C36 C38 111.0(3) . . ?
C34 C36 H36A 109.4 . . ?
C38 C36 H36A 109.4 . . ?
C34 C36 H36B 109.4 . . ?
C38 C36 H36B 109.4 . . ?
H36A C36 H36B 108.0 . . ?
O5 C37 C42 115.5(4) . . ?
O5 C37 C38 122.9(4) . . ?
C42 C37 C38 121.6(4) . . ?
C39 C38 C37 116.8(4) . . ?
C39 C38 C36 121.6(4) . . ?
C37 C38 C36 121.6(4) . . ?
C40 C39 C38 123.4(4) . . ?
C40 C39 H39 118.3 . . ?
C38 C39 H39 118.3 . . ?
C39 C40 C41 117.6(4) . . ?
C39 C40 C43 121.8(4) . . ?
C41 C40 C43 120.6(4) . . ?
C42 C41 C40 121.2(4) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C37 119.3(4) . . ?
C41 C42 C44 120.8(4) . . ?
C37 C42 C44 119.9(4) . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N2 C44 C42 111.9(4) . . ?
N2 C44 H44A 109.2 . . ?
C42 C44 H44A 109.2 . . ?
N2 C44 H44B 109.2 . . ?
C42 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C46 N2 115.5(3) . . ?
C48 C46 H46A 108.4 . . ?
N2 C46 H46A 108.4 . . ?
C48 C46 H46B 108.4 . . ?
N2 C46 H46B 108.4 . . ?
H46A C46 H46B 107.5 . . ?
O6 C47 C48 119.6(3) . . ?
O6 C47 C52 119.9(3) . . ?
C48 C47 C52 120.5(4) . . ?
C49 C48 C47 119.7(4) . . ?
C49 C48 C46 120.0(4) . . ?
C47 C48 C46 120.1(4) . . ?
C48 C49 C50 121.2(4) . . ?
C48 C49 H49 119.4 . . ?
C50 C49 H49 119.4 . . ?
C51 C50 C49 117.5(4) . . ?
C51 C50 C53 122.5(4) . . ?
C49 C50 C53 119.9(4) . . ?
C52 C51 C50 123.3(4) . . ?
C52 C51 H51 118.3 . . ?
C50 C51 H51 118.3 . . ?
C51 C52 C47 117.6(4) . . ?
C51 C52 C54 121.2(3) . . ?
C47 C52 C54 121.2(4) . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C2 C54 C52 115.0(4) . . ?
C2 C54 H54A 108.5 . . ?
C52 C54 H54A 108.5 . . ?
C2 C54 H54B 108.5 . . ?
C52 C54 H54B 108.5 . . ?
H54A C54 H54B 107.5 . . ?
N3 C61 C62 179.6(10) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C64 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N4 C64 C63 178.3(7) . . ?
C19 N1 C18 111.4(3) . . ?
C19 N1 C20 109.7(4) . . ?
C18 N1 C20 113.4(3) . . ?
C19 N1 H1 107.3 . . ?
C18 N1 H1 107.3 . . ?
C20 N1 H1 107.3 . . ?
C45 N2 C44 111.5(3) . . ?
C45 N2 C46 108.9(3) . . ?
C44 N2 C46 112.7(3) . . ?
C45 N2 H2 107.9 . . ?
C44 N2 H2 107.9 . . ?
C46 N2 H2 107.9 . . ?
C1 O1 Ti1 140.9(3) . . ?
C10 O2 H2A 109.5 . . ?
C21 O3 Ti2 142.6(2) . . ?
C29 O4 Ti2 142.8(3) . . ?
C37 O5 H5A 109.5 . . ?
C47 O6 Ti1 143.5(3) . . ?
Ti2 O7 Ti1 172.65(17) . . ?
O7 Ti1 O6 100.63(13) . . ?
O7 Ti1 O1 94.90(12) . . ?
O6 Ti1 O1 99.19(13) . . ?
O7 Ti1 O8 86.50(13) . . ?
O6 Ti1 O8 171.03(13) . . ?
O1 Ti1 O8 85.49(13) . . ?
O7 Ti1 Br2 168.80(9) . . ?
O6 Ti1 Br2 89.29(9) . . ?
O1 Ti1 Br2 88.59(9) . . ?
O8 Ti1 Br2 83.15(9) . . ?
O7 Ti1 Br1 88.29(8) . . ?
O6 Ti1 Br1 91.97(8) . . ?
O1 Ti1 Br1 167.59(10) . . ?
O8 Ti1 Br1 82.74(9) . . ?
Br2 Ti1 Br1 86.14(3) . . ?
O7 Ti2 O3 102.69(12) . . ?
O7 Ti2 O4 96.18(13) . . ?
O3 Ti2 O4 98.50(12) . . ?
O7 Ti2 O9 85.28(12) . . ?
O3 Ti2 O9 169.60(13) . . ?
O4 Ti2 O9 87.11(12) . . ?
O7 Ti2 Br3 164.40(9) . . ?
O3 Ti2 Br3 90.90(9) . . ?
O4 Ti2 Br3 89.25(9) . . ?
O9 Ti2 Br3 80.38(9) . . ?
O7 Ti2 Br4 86.94(9) . . ?
O3 Ti2 Br4 90.06(9) . . ?
O4 Ti2 Br4 169.98(8) . . ?
O9 Ti2 Br4 83.65(9) . . ?
Br3 Ti2 Br4 85.40(3) . . ?
Ti2 O9 H9A 115(4) . . ?
Ti2 O9 H9B 112(4) . . ?
H9A O9 H9B 112(4) . . ?
Ti1 O8 H8C 111(4) . . ?
Ti1 O8 H8D 120(4) . . ?
H8C O8 H8D 102(4) . . ?

_refine_diff_density_max         0.894
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.105




####################################################################### 
# 
# 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_4
_database_code_depnum_ccdc_archive 'CCDC 2057323'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 -0.006 0.000 522 139 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
Unit cell contains 139 electrons. MeCN is 22. This 
allows for 6 unresolved MeCN molecules in the cell. 
;


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
;
 C52 H60 Cl4 N2 O9 Ti2, 2(C2 H3 N) [+ 3MeCN]
;

_chemical_formula_sum            'C56 H66 Cl4 N4 O9 Ti2'
_chemical_formula_weight         1176.72

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.67497(8)
_cell_length_b                   14.54109(8)
_cell_length_c                   18.76966(10)
_cell_angle_alpha                111.9796(5)
_cell_angle_beta                 95.8292(5)
_cell_angle_gamma                96.1580(5)
_cell_volume                     3151.55(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    100.00(10)
_cell_measurement_reflns_used    98023
_cell_measurement_theta_min      2.5650
_cell_measurement_theta_max      70.3150

_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.240
_exptl_crystal_F_000             1228
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.090
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.142
_shelx_estimated_absorpt_T_min   0.707
_shelx_estimated_absorpt_T_max   0.922
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.67905
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       w-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            134309
_diffrn_reflns_av_unetI/netI     0.0102
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.313
_diffrn_reflns_theta_max         68.241
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             11490
_reflns_number_gt                11030
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.0549P)²+1.2930P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11490
_refine_ls_number_parameters     701
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0312
_refine_ls_wR_factor_ref         0.0915
_refine_ls_wR_factor_gt          0.0910
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_restrained_S_all      1.052
_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
C1 C 0.68690(13) 0.75635(11) 0.20909(9) 0.0288(3) Uani 1 1 d . . . . .
C2 C 0.61918(13) 0.81341(12) 0.25584(9) 0.0300(3) Uani 1 1 d . . . . .
C3 C 0.56379(15) 0.87479(13) 0.22902(10) 0.0363(4) Uani 1 1 d . . . . .
H3 H 0.517168 0.913439 0.260173 0.044 Uiso 1 1 calc R U . . .
C4 C 0.57484(17) 0.88108(13) 0.15779(10) 0.0407(4) Uani 1 1 d . . . . .
C5 C 0.64021(16) 0.82108(13) 0.11167(10) 0.0381(4) Uani 1 1 d . . . . .
H5 H 0.647077 0.823642 0.062487 0.046 Uiso 1 1 calc R U . . .
C6 C 0.69610(14) 0.75718(12) 0.13535(10) 0.0319(3) Uani 1 1 d . . . . .
C7 C 0.5166(2) 0.95101(16) 0.13160(12) 0.0574(6) Uani 1 1 d . . . . .
H7A H 0.561765 1.016932 0.150073 0.086 Uiso 1 1 calc R U . . .
H7B H 0.449165 0.958156 0.153067 0.086 Uiso 1 1 calc R U . . .
H7C H 0.500946 0.923302 0.074692 0.086 Uiso 1 1 calc R U . . .
C8 C 0.76233(14) 0.68934(13) 0.08199(10) 0.0346(4) Uani 1 1 d . . . . .
H8A H 0.820706 0.675636 0.114043 0.042 Uiso 1 1 calc R U . . .
H8B H 0.796017 0.725037 0.052288 0.042 Uiso 1 1 calc R U . . .
C10 C 0.66916(14) 0.51069(12) 0.04787(9) 0.0306(3) Uani 1 1 d . . . . .
C11 C 0.69790(14) 0.58976(12) 0.02496(10) 0.0323(3) Uani 1 1 d . . . . .
C12 C 0.66643(15) 0.57330(13) -0.05288(10) 0.0355(4) Uani 1 1 d . . . . .
H12 H 0.684276 0.626511 -0.069410 0.043 Uiso 1 1 calc R U . . .
C13 C 0.61005(16) 0.48241(14) -0.10741(10) 0.0385(4) Uani 1 1 d . . . . .
C14 C 0.58507(15) 0.40455(13) -0.08264(10) 0.0354(4) Uani 1 1 d . . . . .
H14 H 0.547686 0.341519 -0.118935 0.043 Uiso 1 1 calc R U . . .
C15 C 0.61406(14) 0.41791(12) -0.00582(9) 0.0311(3) Uani 1 1 d . . . . .
C17 C 0.5760(2) 0.46776(16) -0.19078(11) 0.0531(5) Uani 1 1 d . . . . .
H17A H 0.500450 0.476021 -0.198277 0.080 Uiso 1 1 calc R U . . .
H17B H 0.584753 0.400114 -0.225256 0.080 Uiso 1 1 calc R U . . .
H17C H 0.620554 0.517630 -0.202985 0.080 Uiso 1 1 calc R U . . .
C18 C 0.58535(13) 0.33533(12) 0.02223(10) 0.0315(3) Uani 1 1 d . . . . .
H18A H 0.547819 0.274649 -0.022274 0.038 Uiso 1 1 calc R U . . .
H18B H 0.535437 0.356588 0.060508 0.038 Uiso 1 1 calc R U . . .
C19 C 0.76381(16) 0.28051(15) 0.00560(11) 0.0414(4) Uani 1 1 d . . . . .
H19A H 0.730800 0.222509 -0.041567 0.062 Uiso 1 1 calc R U . . .
H19B H 0.825189 0.262999 0.031269 0.062 Uiso 1 1 calc R U . . .
H19C H 0.788353 0.336966 -0.008284 0.062 Uiso 1 1 calc R U . . .
C20 C 0.65594(14) 0.22662(12) 0.08839(10) 0.0313(3) Uani 1 1 d . . . . .
H20A H 0.638070 0.161644 0.043115 0.038 Uiso 1 1 calc R U . . .
H20B H 0.720242 0.223338 0.121484 0.038 Uiso 1 1 calc R U . . .
C21 C 0.57165(12) 0.32337(11) 0.20382(9) 0.0258(3) Uani 1 1 d . . . . .
C22 C 0.56416(13) 0.23996(11) 0.13395(9) 0.0281(3) Uani 1 1 d . . . . .
C23 C 0.47295(13) 0.16667(12) 0.10945(10) 0.0314(3) Uani 1 1 d . . . . .
H23 H 0.466926 0.110870 0.061400 0.038 Uiso 1 1 calc R U . . .
C24 C 0.39029(13) 0.17371(12) 0.15417(10) 0.0328(3) Uani 1 1 d . . . . .
C25 C 0.40000(13) 0.25771(12) 0.22277(10) 0.0303(3) Uani 1 1 d . . . . .
H25 H 0.344166 0.263330 0.253594 0.036 Uiso 1 1 calc R U . . .
C26 C 0.48833(12) 0.33434(12) 0.24845(9) 0.0270(3) Uani 1 1 d . . . . .
C27 C 0.29361(15) 0.09234(14) 0.12918(12) 0.0437(4) Uani 1 1 d . . . . .
H27A H 0.289817 0.063285 0.168456 0.066 Uiso 1 1 calc R U . . .
H27B H 0.299929 0.039807 0.079258 0.066 Uiso 1 1 calc R U . . .
H27C H 0.228305 0.121097 0.123585 0.066 Uiso 1 1 calc R U . . .
C28 C 0.49401(12) 0.42562(12) 0.32279(9) 0.0270(3) Uani 1 1 d . . . . .
H28A H 0.420938 0.442698 0.328389 0.032 Uiso 1 1 calc R U . . .
H28B H 0.539131 0.483260 0.319273 0.032 Uiso 1 1 calc R U . . .
C29 C 0.64998(12) 0.43603(11) 0.42330(9) 0.0252(3) Uani 1 1 d . . . . .
C30 C 0.53988(12) 0.40970(11) 0.39430(9) 0.0257(3) Uani 1 1 d . . . . .
C31 C 0.47256(12) 0.36940(11) 0.43289(9) 0.0279(3) Uani 1 1 d . . . . .
H31 H 0.397902 0.351498 0.413421 0.033 Uiso 1 1 calc R U . . .
C32 C 0.51133(13) 0.35446(11) 0.49933(9) 0.0284(3) Uani 1 1 d . . . . .
C33 C 0.62055(13) 0.38299(11) 0.52734(9) 0.0281(3) Uani 1 1 d . . . . .
H33 H 0.648114 0.374186 0.572954 0.034 Uiso 1 1 calc R U . . .
C34 C 0.69112(12) 0.42412(11) 0.49075(9) 0.0267(3) Uani 1 1 d . . . . .
C35 C 0.43769(14) 0.30881(13) 0.53944(10) 0.0349(4) Uani 1 1 d . . . . .
H35A H 0.411502 0.238208 0.505994 0.052 Uiso 1 1 calc R U . . .
H35B H 0.376634 0.345332 0.549847 0.052 Uiso 1 1 calc R U . . .
H35C H 0.476972 0.313144 0.588628 0.052 Uiso 1 1 calc R U . . .
C36 C 0.80875(12) 0.45866(12) 0.52631(9) 0.0291(3) Uani 1 1 d . . . . .
H36A H 0.833188 0.410908 0.548175 0.035 Uiso 1 1 calc R U . . .
H36B H 0.851889 0.458233 0.485111 0.035 Uiso 1 1 calc R U . . .
C37 C 0.83644(12) 0.64902(12) 0.57247(9) 0.0285(3) Uani 1 1 d . . . . .
C38 C 0.82790(12) 0.56320(12) 0.58993(9) 0.0287(3) Uani 1 1 d . . . . .
C39 C 0.83710(12) 0.57776(13) 0.66851(10) 0.0316(3) Uani 1 1 d . . . . .
H39 H 0.829334 0.520404 0.681419 0.038 Uiso 1 1 calc R U . . .
C40 C 0.85707(13) 0.67233(14) 0.72848(10) 0.0338(4) Uani 1 1 d . . . . .
C41 C 0.86921(13) 0.75595(13) 0.70872(10) 0.0330(3) Uani 1 1 d . . . . .
H41 H 0.885450 0.821276 0.748819 0.040 Uiso 1 1 calc R U . . .
C42 C 0.85797(12) 0.74547(13) 0.63132(10) 0.0306(3) Uani 1 1 d . . . . .
C43 C 0.86402(15) 0.68424(16) 0.81255(10) 0.0414(4) Uani 1 1 d . . . . .
H43A H 0.796741 0.702363 0.831305 0.062 Uiso 1 1 calc R U . . .
H43B H 0.923738 0.737260 0.844148 0.062 Uiso 1 1 calc R U . . .
H43C H 0.876087 0.620813 0.816606 0.062 Uiso 1 1 calc R U . . .
C44 C 0.86402(13) 0.83590(13) 0.61002(10) 0.0325(3) Uani 1 1 d . . . . .
H44A H 0.887881 0.897393 0.657708 0.039 Uiso 1 1 calc R U . . .
H44B H 0.791497 0.839919 0.587358 0.039 Uiso 1 1 calc R U . . .
C45 C 1.05265(13) 0.82864(14) 0.58403(11) 0.0370(4) Uani 1 1 d . . . . .
H45A H 1.080191 0.891007 0.629245 0.056 Uiso 1 1 calc R U . . .
H45B H 1.098410 0.821357 0.543792 0.056 Uiso 1 1 calc R U . . .
H45C H 1.052858 0.771416 0.599614 0.056 Uiso 1 1 calc R U . . .
C46 C 0.94199(13) 0.91887(12) 0.52695(10) 0.0301(3) Uani 1 1 d . . . . .
H46A H 0.978226 0.980636 0.571023 0.036 Uiso 1 1 calc R U . . .
H46B H 0.985723 0.906795 0.484453 0.036 Uiso 1 1 calc R U . . .
C47 C 0.77061(12) 0.86533(11) 0.43169(9) 0.0265(3) Uani 1 1 d . . . . .
C48 C 0.83388(13) 0.93702(12) 0.49930(9) 0.0283(3) Uani 1 1 d . . . . .
C49 C 0.79875(13) 1.02777(12) 0.53732(10) 0.0317(3) Uani 1 1 d . . . . .
H49 H 0.841930 1.076617 0.582895 0.038 Uiso 1 1 calc R U . . .
C50 C 0.70140(14) 1.04852(12) 0.50988(10) 0.0332(3) Uani 1 1 d . . . . .
C51 C 0.63918(13) 0.97493(12) 0.44357(10) 0.0308(3) Uani 1 1 d . . . . .
H51 H 0.572025 0.987719 0.425020 0.037 Uiso 1 1 calc R U . . .
C52 C 0.67162(12) 0.88305(12) 0.40324(9) 0.0275(3) Uani 1 1 d . . . . .
C53 C 0.66494(16) 1.14758(14) 0.55148(12) 0.0462(4) Uani 1 1 d . . . . .
H53A H 0.643819 1.149798 0.600828 0.069 Uiso 1 1 calc R U . . .
H53B H 0.603445 1.154822 0.518956 0.069 Uiso 1 1 calc R U . . .
H53C H 0.723837 1.202507 0.561707 0.069 Uiso 1 1 calc R U . . .
C54 C 0.60140(13) 0.80468(12) 0.33181(9) 0.0291(3) Uani 1 1 d . . . . .
H54A H 0.525285 0.809325 0.338074 0.035 Uiso 1 1 calc R U . . .
H54B H 0.614223 0.737406 0.328688 0.035 Uiso 1 1 calc R U . . .
C61 C 0.8046(3) 0.02848(18) 0.13166(15) 0.0714(7) Uani 1 1 d . . . . .
C62 C 0.8437(3) 0.0273(2) 0.20585(15) 0.0762(8) Uani 1 1 d . . . . .
H62A H 0.906825 -0.006811 0.201545 0.114 Uiso 1 1 calc R U . . .
H62B H 0.787422 -0.008504 0.222266 0.114 Uiso 1 1 calc R U . . .
H62C H 0.863611 0.096407 0.244329 0.114 Uiso 1 1 calc R U . . .
C63 C 0.58235(16) 0.15435(14) 0.33651(12) 0.0447(4) Uani 1 1 d . . . . .
H63A H 0.625998 0.100823 0.329643 0.067 Uiso 1 1 calc R U . . .
H63B H 0.611670 0.211719 0.385074 0.067 Uiso 1 1 calc R U . . .
H63C H 0.583490 0.175441 0.292702 0.067 Uiso 1 1 calc R U . . .
C64 C 0.47244(18) 0.11740(14) 0.33962(12) 0.0469(5) Uani 1 1 d . . . . .
N1 N 0.68333(11) 0.30952(10) 0.05944(8) 0.0300(3) Uani 1 1 d . . . . .
H1 H 0.717943 0.371111 0.105441 0.036 Uiso 1 1 calc R U . . .
N2 N 0.94028(10) 0.83189(10) 0.55260(8) 0.0288(3) Uani 1 1 d . . . . .
H2 H 0.915388 0.768662 0.505454 0.035 Uiso 1 1 calc R U . . .
N3 N 0.7733(3) 0.0297(2) 0.07348(15) 0.1117(12) Uani 1 1 d . . . . .
N4 N 0.38661(17) 0.08769(16) 0.34136(14) 0.0683(6) Uani 1 1 d . . . . .
O1 O 0.74049(9) 0.69444(8) 0.23330(6) 0.0289(2) Uani 1 1 d . . . . .
O2 O 0.69453(10) 0.51472(9) 0.12147(6) 0.0356(3) Uani 1 1 d . . . . .
H2A H 0.710966 0.574950 0.152679 0.053 Uiso 1 1 calc R U . . .
O3 O 0.65962(8) 0.39483(8) 0.22606(6) 0.0269(2) Uani 1 1 d . . . . .
O4 O 0.71765(8) 0.47850(8) 0.38777(6) 0.0269(2) Uani 1 1 d . . . . .
O5 O 0.82726(9) 0.64539(8) 0.49812(6) 0.0309(2) Uani 1 1 d . . . . .
H5A H 0.795865 0.588388 0.467063 0.046 Uiso 1 1 calc R U . . .
O6 O 0.80552(9) 0.77697(8) 0.39561(6) 0.0278(2) Uani 1 1 d . . . . .
O7 O 0.80634(8) 0.57617(8) 0.30432(6) 0.0264(2) Uani 1 1 d . . . . .
Cl1 Cl 1.02695(3) 0.70042(3) 0.38631(2) 0.03356(9) Uani 1 1 d . . . . .
Cl2 Cl 0.94271(3) 0.85082(3) 0.29692(2) 0.03783(10) Uani 1 1 d . . . . .
Cl3 Cl 0.80186(3) 0.28508(3) 0.30013(2) 0.03692(10) Uani 1 1 d . . . . .
Cl4 Cl 0.89342(3) 0.40295(3) 0.19110(2) 0.03451(10) Uani 1 1 d . . . . .
Ti1 Ti 0.85639(2) 0.70025(2) 0.30807(2) 0.02653(8) Uani 1 1 d . . . . .
Ti2 Ti 0.78256(2) 0.44696(2) 0.29755(2) 0.02483(7) Uani 1 1 d . . . . .
O9 O 0.93497(9) 0.48828(9) 0.37289(7) 0.0311(2) Uani 1 1 d D . . . .
O8 O 0.93462(10) 0.62292(9) 0.21173(7) 0.0356(3) Uani 1 1 d D . . . .
H8C H 0.9257(18) 0.5568(14) 0.1994(13) 0.053 Uiso 1 1 d D U . . .
H8D H 1.0146(15) 0.6371(16) 0.1998(13) 0.053 Uiso 1 1 d D U . . .
H9A H 0.9692(18) 0.5490(14) 0.3798(13) 0.053 Uiso 1 1 d D U . . .
H9B H 0.9777(17) 0.4437(15) 0.3590(13) 0.053 Uiso 1 1 d D 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
C1 O1 1.3612(19) . ?
C1 C2 1.399(2) . ?
C1 C6 1.405(2) . ?
C2 C3 1.393(2) . ?
C2 C54 1.515(2) . ?
C3 C4 1.394(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(3) . ?
C4 C7 1.511(2) . ?
C5 C6 1.396(2) . ?
C5 H5 0.9500 . ?
C6 C8 1.513(3) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C11 1.522(2) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C10 O2 1.3641(19) . ?
C10 C11 1.397(2) . ?
C10 C15 1.400(2) . ?
C11 C12 1.397(2) . ?
C12 C13 1.393(3) . ?
C12 H12 0.9500 . ?
C13 C14 1.395(2) . ?
C13 C17 1.508(2) . ?
C14 C15 1.385(2) . ?
C14 H14 0.9500 . ?
C15 C18 1.507(2) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 N1 1.514(2) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 N1 1.491(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 C22 1.500(2) . ?
C20 N1 1.5192(19) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 O3 1.3525(18) . ?
C21 C26 1.399(2) . ?
C21 C22 1.400(2) . ?
C22 C23 1.395(2) . ?
C23 C24 1.396(2) . ?
C23 H23 0.9500 . ?
C24 C25 1.387(2) . ?
C24 C27 1.509(2) . ?
C25 C26 1.396(2) . ?
C25 H25 0.9500 . ?
C26 C28 1.512(2) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C30 1.515(2) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 O4 1.3684(18) . ?
C29 C34 1.398(2) . ?
C29 C30 1.402(2) . ?
C30 C31 1.390(2) . ?
C31 C32 1.395(2) . ?
C31 H31 0.9500 . ?
C32 C33 1.389(2) . ?
C32 C35 1.504(2) . ?
C33 C34 1.395(2) . ?
C33 H33 0.9500 . ?
C34 C36 1.519(2) . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C38 1.516(2) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 O5 1.3690(19) . ?
C37 C42 1.400(2) . ?
C37 C38 1.400(2) . ?
C38 C39 1.400(2) . ?
C39 C40 1.390(3) . ?
C39 H39 0.9500 . ?
C40 C41 1.396(2) . ?
C40 C43 1.514(2) . ?
C41 C42 1.393(2) . ?
C41 H41 0.9500 . ?
C42 C44 1.508(2) . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 N2 1.508(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C45 N2 1.498(2) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 C48 1.501(2) . ?
C46 N2 1.5114(19) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 O6 1.3551(19) . ?
C47 C52 1.401(2) . ?
C47 C48 1.401(2) . ?
C48 C49 1.391(2) . ?
C49 C50 1.395(2) . ?
C49 H49 0.9500 . ?
C50 C51 1.392(2) . ?
C50 C53 1.507(2) . ?
C51 C52 1.397(2) . ?
C51 H51 0.9500 . ?
C52 C54 1.512(2) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C61 N3 1.131(3) . ?
C61 C62 1.437(3) . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.453(3) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 N4 1.135(3) . ?
N1 H1 1.0000 . ?
N2 H2 1.0000 . ?
O1 Ti1 1.8975(11) . ?
O2 H2A 0.8400 . ?
O3 Ti2 1.8341(11) . ?
O4 Ti2 1.8809(11) . ?
O5 H5A 0.8400 . ?
O6 Ti1 1.8324(11) . ?
O7 Ti1 1.8202(10) . ?
O7 Ti2 1.8245(10) . ?
Cl1 Ti1 2.4861(5) . ?
Cl2 Ti1 2.4311(5) . ?
Cl3 Ti2 2.4104(4) . ?
Cl4 Ti2 2.4863(5) . ?
Ti1 O8 2.1445(12) . ?
Ti2 O9 2.1570(11) . ?
O9 H9A 0.898(18) . ?
O9 H9B 0.871(18) . ?
O8 H8C 0.892(18) . ?
O8 H8D 1.075(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 119.62(14) . . ?
O1 C1 C6 119.05(15) . . ?
C2 C1 C6 121.23(15) . . ?
C3 C2 C1 118.44(15) . . ?
C3 C2 C54 120.49(16) . . ?
C1 C2 C54 120.99(14) . . ?
C2 C3 C4 121.88(17) . . ?
C2 C3 H3 119.1 . . ?
C4 C3 H3 119.1 . . ?
C5 C4 C3 118.23(16) . . ?
C5 C4 C7 121.20(17) . . ?
C3 C4 C7 120.57(18) . . ?
C4 C5 C6 122.08(16) . . ?
C4 C5 H5 119.0 . . ?
C6 C5 H5 119.0 . . ?
C5 C6 C1 118.04(16) . . ?
C5 C6 C8 120.58(15) . . ?
C1 C6 C8 121.36(14) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C6 C8 C11 113.79(14) . . ?
C6 C8 H8A 108.8 . . ?
C11 C8 H8A 108.8 . . ?
C6 C8 H8B 108.8 . . ?
C11 C8 H8B 108.8 . . ?
H8A C8 H8B 107.7 . . ?
O2 C10 C11 124.29(15) . . ?
O2 C10 C15 114.57(14) . . ?
C11 C10 C15 121.10(15) . . ?
C12 C11 C10 117.24(15) . . ?
C12 C11 C8 121.19(14) . . ?
C10 C11 C8 121.56(14) . . ?
C13 C12 C11 123.00(15) . . ?
C13 C12 H12 118.5 . . ?
C11 C12 H12 118.5 . . ?
C12 C13 C14 118.00(15) . . ?
C12 C13 C17 121.57(16) . . ?
C14 C13 C17 120.43(17) . . ?
C15 C14 C13 120.87(16) . . ?
C15 C14 H14 119.6 . . ?
C13 C14 H14 119.6 . . ?
C14 C15 C10 119.75(15) . . ?
C14 C15 C18 121.50(15) . . ?
C10 C15 C18 118.74(14) . . ?
C13 C17 H17A 109.5 . . ?
C13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C15 C18 N1 112.13(13) . . ?
C15 C18 H18A 109.2 . . ?
N1 C18 H18A 109.2 . . ?
C15 C18 H18B 109.2 . . ?
N1 C18 H18B 109.2 . . ?
H18A C18 H18B 107.9 . . ?
N1 C19 H19A 109.5 . . ?
N1 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N1 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C22 C20 N1 114.16(13) . . ?
C22 C20 H20A 108.7 . . ?
N1 C20 H20A 108.7 . . ?
C22 C20 H20B 108.7 . . ?
N1 C20 H20B 108.7 . . ?
H20A C20 H20B 107.6 . . ?
O3 C21 C26 120.63(14) . . ?
O3 C21 C22 118.58(14) . . ?
C26 C21 C22 120.75(14) . . ?
C23 C22 C21 119.25(15) . . ?
C23 C22 C20 120.35(15) . . ?
C21 C22 C20 120.30(14) . . ?
C22 C23 C24 121.28(15) . . ?
C22 C23 H23 119.4 . . ?
C24 C23 H23 119.4 . . ?
C25 C24 C23 117.90(15) . . ?
C25 C24 C27 120.84(16) . . ?
C23 C24 C27 121.26(16) . . ?
C24 C25 C26 122.79(16) . . ?
C24 C25 H25 118.6 . . ?
C26 C25 H25 118.6 . . ?
C25 C26 C21 117.95(15) . . ?
C25 C26 C28 120.79(14) . . ?
C21 C26 C28 121.25(14) . . ?
C24 C27 H27A 109.5 . . ?
C24 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C24 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 C30 112.81(12) . . ?
C26 C28 H28A 109.0 . . ?
C30 C28 H28A 109.0 . . ?
C26 C28 H28B 109.0 . . ?
C30 C28 H28B 109.0 . . ?
H28A C28 H28B 107.8 . . ?
O4 C29 C34 119.21(13) . . ?
O4 C29 C30 120.01(13) . . ?
C34 C29 C30 120.70(14) . . ?
C31 C30 C29 118.77(14) . . ?
C31 C30 C28 120.15(14) . . ?
C29 C30 C28 121.08(13) . . ?
C30 C31 C32 121.98(14) . . ?
C30 C31 H31 119.0 . . ?
C32 C31 H31 119.0 . . ?
C33 C32 C31 117.79(14) . . ?
C33 C32 C35 120.92(14) . . ?
C31 C32 C35 121.29(15) . . ?
C32 C33 C34 122.26(14) . . ?
C32 C33 H33 118.9 . . ?
C34 C33 H33 118.9 . . ?
C33 C34 C29 118.47(14) . . ?
C33 C34 C36 119.86(14) . . ?
C29 C34 C36 121.62(14) . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C38 C36 C34 112.05(13) . . ?
C38 C36 H36A 109.2 . . ?
C34 C36 H36A 109.2 . . ?
C38 C36 H36B 109.2 . . ?
C34 C36 H36B 109.2 . . ?
H36A C36 H36B 107.9 . . ?
O5 C37 C42 115.41(14) . . ?
O5 C37 C38 123.27(15) . . ?
C42 C37 C38 121.29(14) . . ?
C39 C38 C37 117.32(15) . . ?
C39 C38 C36 121.29(14) . . ?
C37 C38 C36 121.38(14) . . ?
C40 C39 C38 122.96(15) . . ?
C40 C39 H39 118.5 . . ?
C38 C39 H39 118.5 . . ?
C39 C40 C41 117.92(15) . . ?
C39 C40 C43 120.99(16) . . ?
C41 C40 C43 121.08(17) . . ?
C42 C41 C40 121.28(16) . . ?
C42 C41 H41 119.4 . . ?
C40 C41 H41 119.4 . . ?
C41 C42 C37 119.14(15) . . ?
C41 C42 C44 121.21(15) . . ?
C37 C42 C44 119.60(14) . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42 C44 N2 112.27(13) . . ?
C42 C44 H44A 109.2 . . ?
N2 C44 H44A 109.2 . . ?
C42 C44 H44B 109.2 . . ?
N2 C44 H44B 109.2 . . ?
H44A C44 H44B 107.9 . . ?
N2 C45 H45A 109.5 . . ?
N2 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
N2 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C48 C46 N2 115.22(13) . . ?
C48 C46 H46A 108.5 . . ?
N2 C46 H46A 108.5 . . ?
C48 C46 H46B 108.5 . . ?
N2 C46 H46B 108.5 . . ?
H46A C46 H46B 107.5 . . ?
O6 C47 C52 120.50(14) . . ?
O6 C47 C48 118.64(14) . . ?
C52 C47 C48 120.82(14) . . ?
C49 C48 C47 119.32(15) . . ?
C49 C48 C46 120.40(15) . . ?
C47 C48 C46 120.13(14) . . ?
C48 C49 C50 121.34(15) . . ?
C48 C49 H49 119.3 . . ?
C50 C49 H49 119.3 . . ?
C51 C50 C49 118.02(15) . . ?
C51 C50 C53 121.35(16) . . ?
C49 C50 C53 120.63(16) . . ?
C50 C51 C52 122.58(15) . . ?
C50 C51 H51 118.7 . . ?
C52 C51 H51 118.7 . . ?
C51 C52 C47 117.90(15) . . ?
C51 C52 C54 121.02(14) . . ?
C47 C52 C54 121.07(14) . . ?
C50 C53 H53A 109.5 . . ?
C50 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C50 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C52 C54 C2 114.89(13) . . ?
C52 C54 H54A 108.5 . . ?
C2 C54 H54A 108.5 . . ?
C52 C54 H54B 108.5 . . ?
C2 C54 H54B 108.5 . . ?
H54A C54 H54B 107.5 . . ?
N3 C61 C62 179.5(4) . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 H63A 109.5 . . ?
C64 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C64 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
N4 C64 C63 179.3(3) . . ?
C19 N1 C18 111.86(13) . . ?
C19 N1 C20 109.09(13) . . ?
C18 N1 C20 112.90(12) . . ?
C19 N1 H1 107.6 . . ?
C18 N1 H1 107.6 . . ?
C20 N1 H1 107.6 . . ?
C45 N2 C44 112.08(13) . . ?
C45 N2 C46 108.69(12) . . ?
C44 N2 C46 112.83(12) . . ?
C45 N2 H2 107.7 . . ?
C44 N2 H2 107.7 . . ?
C46 N2 H2 107.7 . . ?
C1 O1 Ti1 140.36(10) . . ?
C10 O2 H2A 109.5 . . ?
C21 O3 Ti2 142.30(9) . . ?
C29 O4 Ti2 141.69(10) . . ?
C37 O5 H5A 109.5 . . ?
C47 O6 Ti1 144.37(10) . . ?
Ti1 O7 Ti2 168.84(6) . . ?
O7 Ti1 O6 99.11(5) . . ?
O7 Ti1 O1 92.62(5) . . ?
O6 Ti1 O1 98.13(5) . . ?
O7 Ti1 O8 85.85(5) . . ?
O6 Ti1 O8 172.84(5) . . ?
O1 Ti1 O8 86.74(5) . . ?
O7 Ti1 Cl2 170.03(4) . . ?
O6 Ti1 Cl2 90.54(4) . . ?
O1 Ti1 Cl2 88.45(3) . . ?
O8 Ti1 Cl2 84.32(4) . . ?
O7 Ti1 Cl1 89.48(3) . . ?
O6 Ti1 Cl1 91.46(4) . . ?
O1 Ti1 Cl1 169.72(4) . . ?
O8 Ti1 Cl1 83.38(4) . . ?
Cl2 Ti1 Cl1 87.776(16) . . ?
O7 Ti2 O3 101.81(5) . . ?
O7 Ti2 O4 94.58(5) . . ?
O3 Ti2 O4 97.69(5) . . ?
O7 Ti2 O9 84.30(5) . . ?
O3 Ti2 O9 171.81(5) . . ?
O4 Ti2 O9 87.15(5) . . ?
O7 Ti2 Cl3 164.74(4) . . ?
O3 Ti2 Cl3 92.11(4) . . ?
O4 Ti2 Cl3 89.66(3) . . ?
O9 Ti2 Cl3 81.27(3) . . ?
O7 Ti2 Cl4 87.69(4) . . ?
O3 Ti2 Cl4 90.37(4) . . ?
O4 Ti2 Cl4 170.98(3) . . ?
O9 Ti2 Cl4 84.39(3) . . ?
Cl3 Ti2 Cl4 85.991(16) . . ?
Ti2 O9 H9A 113.0(15) . . ?
Ti2 O9 H9B 113.9(15) . . ?
H9A O9 H9B 110(2) . . ?
Ti1 O8 H8C 112.4(15) . . ?
Ti1 O8 H8D 131.6(12) . . ?
H8C O8 H8D 101.8(17) . . ?

_refine_diff_density_max         0.831
_refine_diff_density_min         -0.376
_refine_diff_density_rms         0.046




####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2057325'
loop_
_audit_author_name
_audit_author_address
'Timothy Prior'
;University of Hull
United Kingdom
;
_audit_update_record             
;
2021-02-24 deposited with the CCDC.	2021-03-05 downloaded from the CCDC.
;

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.148 0.239 0.385 32 -3 ' '
2 0.500 0.500 0.000 660 119 ' '
3 0.852 0.761 0.615 32 -3 ' '
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          ?

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'2(C64 H70 Br12 N8 O6 Ti4), 9(C2 H3 N) [+ 5(C2 H3 N)]'

_chemical_formula_sum            'C146 H171 Br24 N25 O12 Ti8'
_chemical_formula_weight         4769.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 '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                   17.7979(2)
_cell_length_b                   18.13140(10)
_cell_length_c                   18.4582(2)
_cell_angle_alpha                71.1100(10)
_cell_angle_beta                 74.1160(10)
_cell_angle_gamma                66.8570(10)
_cell_volume                     5108.21(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    114275
_cell_measurement_theta_min      2.5530
_cell_measurement_theta_max      70.1830

_exptl_crystal_description       'opaque block'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.550
_exptl_crystal_F_000             2334
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    8.449
_shelx_estimated_absorpt_T_min   0.430
_shelx_estimated_absorpt_T_max   0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.66859
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.79a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RCD3): quarter-chi single'
_diffrn_measurement_method       ω-scans
_diffrn_detector_area_resol_mean 10.000
_diffrn_reflns_number            237393
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         2.567
_diffrn_reflns_theta_max         68.236
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             18616
_reflns_number_gt                16246
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.79a (Rigaku OD, 2020)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Olex2; Mercury'
_computing_publication_material  'CIFTAB, WinGX'
_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)+(0.1249P)²+12.2022P] 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         18616
_refine_ls_number_parameters     986
_refine_ls_number_restraints     137
_refine_ls_R_factor_all          0.0712
_refine_ls_R_factor_gt           0.0660
_refine_ls_wR_factor_ref         0.1896
_refine_ls_wR_factor_gt          0.1848
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_restrained_S_all      1.023
_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 0.12254(7) 0.27922(7) 0.10231(7) 0.0543(3) Uani 1 1 d . . . . .
Ti2 Ti 0.46826(6) -0.05470(6) 0.25367(6) 0.0414(2) Uani 1 1 d . . . . .
Br1 Br 0.08947(5) 0.16083(5) 0.20459(5) 0.0739(2) Uani 1 1 d . . . . .
Br2 Br 0.11407(5) 0.34578(5) 0.20457(4) 0.0653(2) Uani 1 1 d . . . . .
Br3 Br 0.13037(5) 0.40626(5) -0.00236(5) 0.0712(2) Uani 1 1 d . . . . .
Br4 Br 0.08574(5) 0.23086(6) 0.00590(5) 0.0755(2) Uani 1 1 d . . . . .
Br5 Br 0.49418(4) -0.02358(4) 0.10702(3) 0.05338(17) Uani 1 1 d . . . . .
Br6 Br 0.40969(4) -0.09896(4) 0.39367(3) 0.04900(15) Uani 1 1 d . . . . .
O1 O 0.2320(3) 0.2312(3) 0.0835(2) 0.0530(10) Uani 1 1 d . . . . .
O2 O 0.4468(2) 0.0478(2) 0.2554(2) 0.0466(9) Uani 1 1 d . . . . .
O3 O 0.5782(2) -0.0943(2) 0.2590(2) 0.0437(8) Uani 1 1 d . . . . .
C1 C 0.3149(4) 0.2192(3) 0.0572(3) 0.0481(13) Uani 1 1 d . . . . .
C2 C 0.3474(4) 0.2216(4) -0.0219(4) 0.0547(15) Uani 1 1 d . . . . .
C3 C 0.4311(5) 0.2105(4) -0.0463(4) 0.0603(16) Uani 1 1 d . . . . .
H3 H 0.453305 0.213418 -0.099776 0.072 Uiso 1 1 calc R U . . .
C4 C 0.4840(5) 0.1954(5) 0.0036(4) 0.0654(17) Uani 1 1 d . . . . .
C5 C 0.4488(4) 0.1941(4) 0.0810(4) 0.0581(15) Uani 1 1 d . . . . .
H5 H 0.483640 0.185064 0.116092 0.070 Uiso 1 1 calc R U . . .
C6 C 0.3662(4) 0.2054(3) 0.1093(3) 0.0489(13) Uani 1 1 d . . . . .
C7 C 0.5753(6) 0.1806(7) -0.0247(6) 0.096(3) Uani 1 1 d . . . . .
H7A H 0.592587 0.160403 -0.071940 0.143 Uiso 1 1 calc R U . . .
H7B H 0.606588 0.139361 0.015530 0.143 Uiso 1 1 calc R U . . .
H7C H 0.586235 0.232546 -0.036191 0.143 Uiso 1 1 calc R U . . .
C8 C 0.3296(4) 0.2000(4) 0.1945(3) 0.0515(14) Uani 1 1 d . . . . .
H8A H 0.280319 0.249907 0.199260 0.062 Uiso 1 1 calc R U . . .
H8B H 0.310861 0.151305 0.215931 0.062 Uiso 1 1 calc R U . . .
C9 C 0.4483(4) 0.1166(3) 0.2694(3) 0.0447(12) Uani 1 1 d . . . . .
C10 C 0.3895(4) 0.1930(4) 0.2419(4) 0.0507(13) Uani 1 1 d . . . . .
C11 C 0.3921(4) 0.2619(4) 0.2580(5) 0.0639(17) Uani 1 1 d . . . . .
H11 H 0.353919 0.314804 0.239246 0.077 Uiso 1 1 calc R U . . .
C12 C 0.4479(5) 0.2561(5) 0.2999(5) 0.072(2) Uani 1 1 d . . . . .
C13 C 0.5055(4) 0.1784(4) 0.3259(4) 0.0628(17) Uani 1 1 d . . . . .
H13 H 0.544895 0.174082 0.354182 0.075 Uiso 1 1 calc R U . . .
C14 C 0.5065(4) 0.1084(4) 0.3115(4) 0.0510(13) Uani 1 1 d . . . . .
C15 C 0.4474(6) 0.3323(5) 0.3184(7) 0.100(3) Uani 1 1 d . . . . .
H15A H 0.438836 0.323982 0.374862 0.149 Uiso 1 1 calc R U . . .
H15B H 0.402539 0.380796 0.297199 0.149 Uiso 1 1 calc R U . . .
H15C H 0.500640 0.341261 0.295109 0.149 Uiso 1 1 calc R U . . .
C16 C 0.5661(4) 0.0238(4) 0.3426(3) 0.0494(13) Uani 1 1 d . . . . .
H16A H 0.535418 -0.015924 0.363745 0.059 Uiso 1 1 calc R U . . .
H16B H 0.586710 0.026303 0.386153 0.059 Uiso 1 1 calc R U . . .
C17 C 0.6438(3) -0.0689(3) 0.2476(3) 0.0410(11) Uani 1 1 d . . . . .
C18 C 0.6399(3) -0.0089(4) 0.2833(3) 0.0445(12) Uani 1 1 d . . . . .
C19 C 0.7089(4) 0.0151(4) 0.2664(4) 0.0527(14) Uani 1 1 d . . . . .
H19 H 0.706642 0.055479 0.290108 0.063 Uiso 1 1 calc R U . . .
C20 C 0.7818(4) -0.0165(4) 0.2167(4) 0.0546(14) Uani 1 1 d . . . . .
C21 C 0.7841(4) -0.0778(4) 0.1859(4) 0.0511(13) Uani 1 1 d . . . . .
H21 H 0.833468 -0.102258 0.153672 0.061 Uiso 1 1 calc R U . . .
C22 C 0.7179(3) -0.1048(4) 0.2001(3) 0.0450(12) Uani 1 1 d . . . . .
C23 C 0.8546(4) 0.0106(5) 0.2021(5) 0.0687(18) Uani 1 1 d . . . . .
H23A H 0.842594 0.049660 0.233471 0.103 Uiso 1 1 calc R U . . .
H23B H 0.866018 0.037606 0.146966 0.103 Uiso 1 1 calc R U . . .
H23C H 0.903027 -0.037642 0.216393 0.103 Uiso 1 1 calc R U . . .
C24 C 0.7272(4) -0.1772(4) 0.1714(3) 0.0478(13) Uani 1 1 d . . . . .
H24A H 0.705192 -0.216429 0.214732 0.057 Uiso 1 1 calc R U . . .
H24B H 0.787018 -0.206053 0.155940 0.057 Uiso 1 1 calc R U . . .
C25 C 0.7049(4) -0.0887(4) 0.0365(3) 0.0561(15) Uani 1 1 d . . . . .
H25A H 0.690401 -0.038518 0.054170 0.084 Uiso 1 1 calc R U . . .
H25B H 0.673719 -0.076458 -0.004656 0.084 Uiso 1 1 calc R U . . .
H25C H 0.764450 -0.107711 0.016383 0.084 Uiso 1 1 calc R U . . .
C26 C 0.2968(5) 0.2339(4) -0.0792(4) 0.0576(16) Uani 1 1 d . . . . .
H26A H 0.307288 0.277111 -0.125808 0.069 Uiso 1 1 calc R U . . .
H26B H 0.237323 0.253513 -0.056494 0.069 Uiso 1 1 calc R U . . .
C27 C -0.0835(4) 0.3765(4) 0.1277(4) 0.0608(16) Uani 1 1 d . . . . .
C28 C -0.1724(5) 0.4140(6) 0.1415(5) 0.079(2) Uani 1 1 d . . . . .
H28A H -0.197015 0.373499 0.178226 0.119 Uiso 1 1 calc R U . . .
H28B H -0.193187 0.432533 0.092383 0.119 Uiso 1 1 calc R U . . .
H28C H -0.187314 0.461581 0.163204 0.119 Uiso 1 1 calc R U . . .
C29 C 0.4906(3) -0.2495(4) 0.2597(4) 0.0497(13) Uani 1 1 d . . . . .
C30 C 0.4974(5) -0.3345(5) 0.2717(6) 0.083(3) Uani 1 1 d . . . . .
H30A H 0.547527 -0.371296 0.293718 0.125 Uiso 1 1 calc R U . . .
H30B H 0.500654 -0.345095 0.221976 0.125 Uiso 1 1 calc R U . . .
H30C H 0.448658 -0.344824 0.307720 0.125 Uiso 1 1 calc R U . . .
C31 C 0.2955(4) -0.0256(4) 0.1980(4) 0.0619(16) Uani 1 1 d . . . . .
C32 C 0.2370(4) -0.0212(4) 0.1555(4) 0.0602(16) Uani 1 1 d . . . . .
H32A H 0.266325 -0.050391 0.114175 0.090 Uiso 1 1 calc R U . . .
H32B H 0.207714 0.036855 0.132495 0.090 Uiso 1 1 calc R U . . .
H32C H 0.197020 -0.047048 0.190645 0.090 Uiso 1 1 calc R U . . .
N1 N 0.6838(3) -0.1547(3) 0.1032(3) 0.0476(11) Uani 1 1 d . . . . .
H1 H 0.622719 -0.133817 0.122039 0.057 Uiso 1 1 calc R U . . .
N2 N -0.0144(4) 0.3457(4) 0.1189(3) 0.0614(14) Uani 1 1 d . . . . .
N3 N 0.4860(3) -0.1834(3) 0.2508(3) 0.0446(10) Uani 1 1 d . . . . .
N4 N 0.3446(3) -0.0321(3) 0.2327(4) 0.0578(13) Uani 1 1 d . . . . .
Ti3 Ti 0.85081(6) 0.19199(6) 0.60803(6) 0.0444(2) Uani 1 1 d . . . . .
Ti4 Ti 0.81305(6) 0.57124(6) 0.34282(6) 0.0400(2) Uani 1 1 d . . . . .
Br7 Br 0.98505(4) 0.14139(4) 0.51958(4) 0.05925(18) Uani 1 1 d . . . . .
Br8 Br 0.92910(4) 0.10810(4) 0.72059(4) 0.05545(17) Uani 1 1 d . . . . .
Br9 Br 0.71866(4) 0.21921(4) 0.70433(5) 0.0700(2) Uani 1 1 d . . . . .
Br10 Br 0.77637(5) 0.23654(4) 0.49809(5) 0.0688(2) Uani 1 1 d . . . . .
Br11 Br 0.72733(4) 0.58315(4) 0.24859(4) 0.04843(15) Uani 1 1 d . . . . .
Br12 Br 0.92476(4) 0.52094(3) 0.42408(4) 0.04798(15) Uani 1 1 d . . . . .
C41 C 0.8436(3) 0.3638(3) 0.6163(3) 0.0424(11) Uani 1 1 d . . . . .
C42 C 0.8967(3) 0.3715(4) 0.6541(3) 0.0466(12) Uani 1 1 d . . . . .
C43 C 0.8831(4) 0.4473(4) 0.6666(4) 0.0498(13) Uani 1 1 d . . . . .
H43 H 0.918749 0.451483 0.694046 0.060 Uiso 1 1 calc R U . . .
C44 C 0.8190(4) 0.5172(4) 0.6403(3) 0.0492(13) Uani 1 1 d . . . . .
C45 C 0.7652(3) 0.5078(3) 0.6031(3) 0.0465(12) Uani 1 1 d . . . . .
H45 H 0.720037 0.554921 0.585676 0.056 Uiso 1 1 calc R U . . .
C46 C 0.7751(3) 0.4331(3) 0.5907(3) 0.0411(11) Uani 1 1 d . . . . .
C47 C 0.8084(5) 0.6007(4) 0.6487(5) 0.0655(17) Uani 1 1 d . . . . .
H47A H 0.790972 0.601761 0.703662 0.098 Uiso 1 1 calc R U . . .
H47B H 0.766155 0.643444 0.618962 0.098 Uiso 1 1 calc R U . . .
H47C H 0.861167 0.611274 0.629048 0.098 Uiso 1 1 calc R U . . .
C48 C 0.7192(3) 0.4235(3) 0.5482(4) 0.0453(12) Uani 1 1 d . . . . .
H48A H 0.752300 0.407415 0.499628 0.054 Uiso 1 1 calc R U . . .
H48B H 0.698038 0.378129 0.580840 0.054 Uiso 1 1 calc R U . . .
C49 C 0.6584(3) 0.5681(3) 0.4679(3) 0.0395(11) Uani 1 1 d . . . . .
C50 C 0.6467(3) 0.5010(3) 0.5284(3) 0.0424(11) Uani 1 1 d . . . . .
C51 C 0.5671(3) 0.5103(3) 0.5687(3) 0.0452(12) Uani 1 1 d . . . . .
H51 H 0.557631 0.465794 0.610211 0.054 Uiso 1 1 calc R U . . .
C52 C 0.5001(3) 0.5820(3) 0.5513(3) 0.0448(12) Uani 1 1 d . . . . .
C53 C 0.5153(3) 0.6494(3) 0.4931(3) 0.0410(11) Uani 1 1 d . . . . .
H53 H 0.470762 0.699717 0.481814 0.049 Uiso 1 1 calc R U . . .
C54 C 0.5952(3) 0.6437(3) 0.4513(3) 0.0380(10) Uani 1 1 d . . . . .
C55 C 0.4140(4) 0.5880(4) 0.5946(4) 0.0561(15) Uani 1 1 d . . . . .
H55A H 0.403700 0.537135 0.599796 0.084 Uiso 1 1 calc R U . . .
H55B H 0.373743 0.635336 0.565894 0.084 Uiso 1 1 calc R U . . .
H55C H 0.408435 0.595514 0.646271 0.084 Uiso 1 1 calc R U . . .
C56 C 0.6135(3) 0.7161(3) 0.3900(3) 0.0392(11) Uani 1 1 d . . . . .
H56A H 0.560239 0.760737 0.380510 0.047 Uiso 1 1 calc R U . . .
H56B H 0.640828 0.698493 0.341025 0.047 Uiso 1 1 calc R U . . .
C57 C 0.7519(3) 0.7371(3) 0.3755(3) 0.0382(11) Uani 1 1 d . . . . .
C58 C 0.6682(3) 0.7513(3) 0.4100(3) 0.0367(10) Uani 1 1 d . . . . .
C59 C 0.6334(3) 0.8058(3) 0.4583(3) 0.0411(11) Uani 1 1 d . . . . .
H59 H 0.577473 0.814420 0.483433 0.049 Uiso 1 1 calc R U . . .
C60 C 0.6768(3) 0.8480(3) 0.4713(3) 0.0435(12) Uani 1 1 d . . . . .
C61 C 0.6387(4) 0.9058(4) 0.5247(4) 0.0559(15) Uani 1 1 d . . . . .
H61A H 0.648347 0.874792 0.577592 0.084 Uiso 1 1 calc R U . . .
H61B H 0.578913 0.931102 0.524284 0.084 Uiso 1 1 calc R U . . .
H61C H 0.664004 0.949238 0.506811 0.084 Uiso 1 1 calc R U . . .
C62 C 0.7577(3) 0.8369(3) 0.4323(3) 0.0424(11) Uani 1 1 d . . . . .
H62 H 0.787671 0.867115 0.438561 0.051 Uiso 1 1 calc R U . . .
C63 C 0.7961(3) 0.7820(3) 0.3838(3) 0.0395(11) Uani 1 1 d . . . . .
C64 C 0.8812(3) 0.7759(3) 0.3386(3) 0.0438(12) Uani 1 1 d . . . . .
H64A H 0.892365 0.826387 0.335016 0.053 Uiso 1 1 calc R U . . .
H64B H 0.882525 0.774265 0.285145 0.053 Uiso 1 1 calc R U . . .
C65 C 0.9523(4) 0.6980(4) 0.4533(3) 0.0501(13) Uani 1 1 d . . . . .
H65A H 0.997338 0.648548 0.472722 0.075 Uiso 1 1 calc R U . . .
H65B H 0.899424 0.695857 0.486535 0.075 Uiso 1 1 calc R U . . .
H65C H 0.961918 0.747443 0.453774 0.075 Uiso 1 1 calc R U . . .
C66 C 0.9702(3) 0.2984(4) 0.6814(4) 0.0498(13) Uani 1 1 d . . . . .
H66A H 0.974861 0.299019 0.733474 0.060 Uiso 1 1 calc R U . . .
H66B H 0.960512 0.246696 0.686551 0.060 Uiso 1 1 calc R U . . .
C67 C 0.8241(3) 0.0151(4) 0.6182(3) 0.0465(12) Uani 1 1 d . . . . .
C68 C 0.8084(4) -0.0566(4) 0.6166(4) 0.0547(14) Uani 1 1 d . . . . .
H68A H 0.748614 -0.043612 0.621209 0.082 Uiso 1 1 calc R U . . .
H68B H 0.828826 -0.102661 0.660085 0.082 Uiso 1 1 calc R U . . .
H68C H 0.836950 -0.072162 0.567533 0.082 Uiso 1 1 calc R U . . .
C69 C 0.9633(4) 0.5735(4) 0.1866(4) 0.0519(14) Uani 1 1 d . . . . .
C70 C 1.0294(5) 0.5720(5) 0.1187(5) 0.073(2) Uani 1 1 d . . . . .
H70A H 1.015519 0.625791 0.081058 0.110 Uiso 1 1 calc R U . . .
H70B H 1.035339 0.528679 0.094746 0.110 Uiso 1 1 calc R U . . .
H70C H 1.081738 0.560670 0.134981 0.110 Uiso 1 1 calc R U . . .
C71 C 0.8899(4) 0.3722(4) 0.3365(4) 0.0530(14) Uani 1 1 d . . . . .
C72 C 0.9259(6) 0.2877(4) 0.3305(5) 0.078(2) Uani 1 1 d . . . . .
H72A H 0.884415 0.271120 0.320345 0.117 Uiso 1 1 calc R U . . .
H72B H 0.944751 0.251938 0.379338 0.117 Uiso 1 1 calc R U . . .
H72C H 0.973244 0.282595 0.287886 0.117 Uiso 1 1 calc R U . . .
N5 N 0.9494(3) 0.7013(3) 0.3728(3) 0.0424(10) Uani 1 1 d . . . . .
H5A H 0.938585 0.650759 0.374046 0.051 Uiso 1 1 calc R U . . .
N6 N 0.8349(3) 0.0728(3) 0.6197(3) 0.0501(11) Uani 1 1 d . . . . .
N7 N 0.9131(3) 0.5772(3) 0.2395(3) 0.0509(11) Uani 1 1 d . . . . .
N8 N 0.8606(3) 0.4390(3) 0.3414(3) 0.0483(11) Uani 1 1 d . . . . .
N9 N 0.7617(11) 0.2356(7) 0.2693(9) 0.163(5) Uani 1 1 d D U . . .
C73 C 0.7157(10) 0.2168(9) 0.3287(9) 0.132(4) Uani 1 1 d D U . . .
C74 C 0.6650(9) 0.1881(10) 0.4019(9) 0.143(5) Uani 1 1 d D U . . .
H74A H 0.660920 0.135535 0.402389 0.214 Uiso 1 1 calc R U . . .
H74B H 0.609354 0.229390 0.406450 0.214 Uiso 1 1 calc R U . . .
H74C H 0.690792 0.180076 0.445676 0.214 Uiso 1 1 calc R U . . .
N10 N 0.8049(5) 0.0157(5) 0.4162(5) 0.091(2) Uani 1 1 d D U . . .
C75 C 0.8612(5) 0.0399(5) 0.3945(5) 0.0741(19) Uani 1 1 d D U . . .
C76 C 0.9291(5) 0.0725(4) 0.3661(5) 0.074(2) Uani 1 1 d D U . . .
H76A H 0.921672 0.112089 0.315628 0.111 Uiso 1 1 calc R U . . .
H76B H 0.981613 0.027039 0.360299 0.111 Uiso 1 1 calc R U . . .
H76C H 0.930090 0.100429 0.403109 0.111 Uiso 1 1 calc R U . . .
N11 N 0.9809(5) 0.1840(6) 0.8848(5) 0.104(3) Uani 1 1 d D U . . .
C77 C 0.9112(8) 0.2079(11) 0.8783(10) 0.151(6) Uani 1 1 d D U . . .
C78 C 0.8251(9) 0.2598(14) 0.8593(10) 0.200(9) Uani 1 1 d D U . . .
H78A H 0.814423 0.317741 0.856880 0.299 Uiso 1 1 calc R U . . .
H78B H 0.783835 0.239861 0.899695 0.299 Uiso 1 1 calc R U . . .
H78C H 0.821446 0.255198 0.808968 0.299 Uiso 1 1 calc R U . . .
N12 N 0.8006(7) 0.0813(8) -0.0008(7) 0.131(4) Uani 1 1 d D U . . .
C79 C 0.8618(8) 0.0347(8) -0.0262(7) 0.109(3) Uani 1 1 d D U . . .
C80 C 0.9395(8) -0.0185(9) -0.0608(8) 0.127(4) Uani 1 1 d D U . . .
H80A H 0.976857 0.013452 -0.087898 0.191 Uiso 1 1 calc R U . . .
H80B H 0.928607 -0.039845 -0.097940 0.191 Uiso 1 1 calc R U . . .
H80C H 0.965280 -0.064747 -0.020004 0.191 Uiso 1 1 calc R U . . .
C82 C 0.8715(13) 0.2139(11) 0.0803(12) 0.096(6) Uiso 0.5 1 d D . P . .
H82A H 0.875815 0.218771 0.130219 0.144 Uiso 0.5 1 calc R U P . .
H82B H 0.926656 0.185907 0.054285 0.144 Uiso 0.5 1 calc R U P . .
H82C H 0.835240 0.181635 0.089168 0.144 Uiso 0.5 1 calc R U P . .
C81 C 0.8373(14) 0.2949(12) 0.0323(13) 0.104(6) Uiso 0.5 1 d D . P . .
N13 N 0.8024(15) 0.3592(13) -0.0062(14) 0.142(8) Uiso 0.5 1 d D . P . .
O4 O 0.8567(2) 0.2888(2) 0.6036(2) 0.0439(8) Uani 1 1 d . . . . .
O5 O 0.7351(2) 0.5598(2) 0.4236(2) 0.0404(8) Uani 1 1 d . . . . .
O6 O 0.7928(2) 0.6812(2) 0.3303(2) 0.0399(8) 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 O1 1.780(4) . ?
Ti1 N2 2.237(6) . ?
Ti1 Br2 2.4937(13) . ?
Ti1 Br1 2.5059(15) . ?
Ti1 Br3 2.5063(15) . ?
Ti1 Br4 2.5424(13) . ?
Ti2 O2 1.754(4) . ?
Ti2 O3 1.820(4) . ?
Ti2 N4 2.194(5) . ?
Ti2 N3 2.245(5) . ?
Ti2 Br6 2.4997(11) . ?
Ti2 Br5 2.5279(11) . ?
O1 C1 1.372(7) . ?
O2 C9 1.363(7) . ?
O3 C17 1.358(7) . ?
C1 C6 1.401(9) . ?
C1 C2 1.410(8) . ?
C2 C3 1.385(10) . ?
C2 C26 1.480(9) . ?
C3 C4 1.385(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.390(10) . ?
C4 C7 1.507(11) . ?
C5 C6 1.375(9) . ?
C5 H5 0.9500 . ?
C6 C8 1.516(8) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C10 1.501(9) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C14 1.395(8) . ?
C9 C10 1.403(8) . ?
C10 C11 1.394(9) . ?
C11 C12 1.370(10) . ?
C11 H11 0.9500 . ?
C12 C13 1.401(10) . ?
C12 C15 1.525(10) . ?
C13 C14 1.369(9) . ?
C13 H13 0.9500 . ?
C14 C16 1.514(8) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C18 1.516(8) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C17 C22 1.412(8) . ?
C17 C18 1.415(8) . ?
C18 C19 1.384(9) . ?
C19 C20 1.399(9) . ?
C19 H19 0.9500 . ?
C20 C21 1.386(9) . ?
C20 C23 1.489(9) . ?
C21 C22 1.378(8) . ?
C21 H21 0.9500 . ?
C22 C24 1.503(8) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 N1 1.517(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 N1 1.495(8) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 N1 1.521(7) 2_655 ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 N2 1.123(9) . ?
C27 C28 1.440(10) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 N3 1.128(8) . ?
C29 C30 1.444(10) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 N4 1.169(9) . ?
C31 C32 1.431(9) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N1 H1 1.0000 . ?
Ti3 O4 1.774(4) . ?
Ti3 N6 2.224(5) . ?
Ti3 Br10 2.4688(12) . ?
Ti3 Br9 2.5104(12) . ?
Ti3 Br7 2.5154(12) . ?
Ti3 Br8 2.5384(12) . ?
Ti4 O5 1.757(4) . ?
Ti4 O6 1.827(4) . ?
Ti4 N8 2.213(5) . ?
Ti4 N7 2.232(5) . ?
Ti4 Br11 2.5200(11) . ?
Ti4 Br12 2.5210(11) . ?
C41 O4 1.373(7) . ?
C41 C42 1.387(8) . ?
C41 C46 1.420(7) . ?
C42 C43 1.385(8) . ?
C42 C66 1.512(7) . ?
C43 C44 1.382(8) . ?
C43 H43 0.9500 . ?
C44 C45 1.409(8) . ?
C44 C47 1.505(9) . ?
C45 C46 1.382(8) . ?
C45 H45 0.9500 . ?
C46 C48 1.511(7) . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 C50 1.509(7) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 O5 1.364(6) . ?
C49 C54 1.393(7) . ?
C49 C50 1.401(8) . ?
C50 C51 1.380(8) . ?
C51 C52 1.391(8) . ?
C51 H51 0.9500 . ?
C52 C53 1.405(8) . ?
C52 C55 1.501(8) . ?
C53 C54 1.400(8) . ?
C53 H53 0.9500 . ?
C54 C56 1.511(7) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 C58 1.526(7) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 O6 1.375(6) . ?
C57 C63 1.398(7) . ?
C57 C58 1.406(7) . ?
C58 C59 1.393(7) . ?
C59 C60 1.387(8) . ?
C59 H59 0.9500 . ?
C60 C62 1.390(8) . ?
C60 C61 1.508(7) . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.401(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.496(8) . ?
C64 N5 1.509(6) . ?
C64 H64A 0.9900 . ?
C64 H64B 0.9900 . ?
C65 N5 1.482(7) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 N5 1.505(7) 2_766 ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C67 N6 1.145(8) . ?
C67 C68 1.444(8) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 N7 1.127(8) . ?
C69 C70 1.466(9) . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 N8 1.140(7) . ?
C71 C72 1.437(8) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N5 H5A 1.0000 . ?
N9 C73 1.214(13) . ?
C73 C74 1.469(14) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
N10 C75 1.171(9) . ?
C75 C76 1.449(10) . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
N11 C77 1.169(12) . ?
C77 C78 1.517(14) . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
N12 C79 1.173(12) . ?
C79 C80 1.454(13) . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C82 C81 1.436(16) . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C81 N13 1.178(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 N2 176.3(2) . . ?
O1 Ti1 Br2 98.71(14) . . ?
N2 Ti1 Br2 82.17(15) . . ?
O1 Ti1 Br1 97.79(15) . . ?
N2 Ti1 Br1 85.75(17) . . ?
Br2 Ti1 Br1 90.42(5) . . ?
O1 Ti1 Br3 91.34(15) . . ?
N2 Ti1 Br3 85.08(16) . . ?
Br2 Ti1 Br3 91.41(5) . . ?
Br1 Ti1 Br3 170.31(6) . . ?
O1 Ti1 Br4 97.98(14) . . ?
N2 Ti1 Br4 81.19(15) . . ?
Br2 Ti1 Br4 163.32(6) . . ?
Br1 Ti1 Br4 87.19(5) . . ?
Br3 Ti1 Br4 88.33(5) . . ?
O2 Ti2 O3 98.66(18) . . ?
O2 Ti2 N4 94.28(19) . . ?
O3 Ti2 N4 165.60(19) . . ?
O2 Ti2 N3 175.83(18) . . ?
O3 Ti2 N3 85.51(17) . . ?
N4 Ti2 N3 81.57(19) . . ?
O2 Ti2 Br6 95.04(14) . . ?
O3 Ti2 Br6 100.17(12) . . ?
N4 Ti2 Br6 84.87(16) . . ?
N3 Ti2 Br6 84.24(12) . . ?
O2 Ti2 Br5 93.85(13) . . ?
O3 Ti2 Br5 93.18(12) . . ?
N4 Ti2 Br5 79.62(16) . . ?
N3 Ti2 Br5 85.82(12) . . ?
Br6 Ti2 Br5 162.65(5) . . ?
C1 O1 Ti1 162.0(4) . . ?
C9 O2 Ti2 163.2(4) . . ?
C17 O3 Ti2 141.8(3) . . ?
O1 C1 C6 119.6(5) . . ?
O1 C1 C2 119.7(6) . . ?
C6 C1 C2 120.7(6) . . ?
C3 C2 C1 117.9(6) . . ?
C3 C2 C26 119.0(6) . . ?
C1 C2 C26 123.1(6) . . ?
C4 C3 C2 123.1(6) . . ?
C4 C3 H3 118.5 . . ?
C2 C3 H3 118.5 . . ?
C3 C4 C5 116.8(7) . . ?
C3 C4 C7 121.4(7) . . ?
C5 C4 C7 121.8(7) . . ?
C6 C5 C4 123.4(7) . . ?
C6 C5 H5 118.3 . . ?
C4 C5 H5 118.3 . . ?
C5 C6 C1 118.1(6) . . ?
C5 C6 C8 122.7(6) . . ?
C1 C6 C8 119.1(5) . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C10 C8 C6 113.2(5) . . ?
C10 C8 H8A 108.9 . . ?
C6 C8 H8A 108.9 . . ?
C10 C8 H8B 108.9 . . ?
C6 C8 H8B 108.9 . . ?
H8A C8 H8B 107.8 . . ?
O2 C9 C14 119.3(5) . . ?
O2 C9 C10 118.2(5) . . ?
C14 C9 C10 122.5(5) . . ?
C11 C10 C9 116.8(6) . . ?
C11 C10 C8 122.1(6) . . ?
C9 C10 C8 121.1(5) . . ?
C12 C11 C10 122.3(6) . . ?
C12 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C11 C12 C13 118.8(6) . . ?
C11 C12 C15 121.0(7) . . ?
C13 C12 C15 120.3(7) . . ?
C14 C13 C12 121.7(6) . . ?
C14 C13 H13 119.1 . . ?
C12 C13 H13 119.1 . . ?
C13 C14 C9 117.9(6) . . ?
C13 C14 C16 121.9(6) . . ?
C9 C14 C16 120.1(5) . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 C18 114.6(5) . . ?
C14 C16 H16A 108.6 . . ?
C18 C16 H16A 108.6 . . ?
C14 C16 H16B 108.6 . . ?
C18 C16 H16B 108.6 . . ?
H16A C16 H16B 107.6 . . ?
O3 C17 C22 118.7(5) . . ?
O3 C17 C18 121.6(5) . . ?
C22 C17 C18 119.7(5) . . ?
C19 C18 C17 117.6(5) . . ?
C19 C18 C16 120.4(5) . . ?
C17 C18 C16 121.9(5) . . ?
C18 C19 C20 124.0(6) . . ?
C18 C19 H19 118.0 . . ?
C20 C19 H19 118.0 . . ?
C21 C20 C19 116.3(6) . . ?
C21 C20 C23 122.1(6) . . ?
C19 C20 C23 121.5(6) . . ?
C22 C21 C20 122.9(6) . . ?
C22 C21 H21 118.5 . . ?
C20 C21 H21 118.5 . . ?
C21 C22 C17 119.3(5) . . ?
C21 C22 C24 120.1(5) . . ?
C17 C22 C24 120.3(5) . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 N1 114.6(4) . . ?
C22 C24 H24A 108.6 . . ?
N1 C24 H24A 108.6 . . ?
C22 C24 H24B 108.6 . . ?
N1 C24 H24B 108.6 . . ?
H24A C24 H24B 107.6 . . ?
N1 C25 H25A 109.5 . . ?
N1 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
N1 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C2 C26 N1 112.0(5) . 2_655 ?
C2 C26 H26A 109.2 . . ?
N1 C26 H26A 109.2 2_655 . ?
C2 C26 H26B 109.2 . . ?
N1 C26 H26B 109.2 2_655 . ?
H26A C26 H26B 107.9 . . ?
N2 C27 C28 178.1(9) . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N3 C29 C30 179.2(7) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
N4 C31 C32 177.6(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 . . ?
C25 N1 C24 114.0(5) . . ?
C25 N1 C26 112.1(5) . 2_655 ?
C24 N1 C26 107.6(4) . 2_655 ?
C25 N1 H1 107.6 . . ?
C24 N1 H1 107.6 . . ?
C26 N1 H1 107.6 2_655 . ?
C27 N2 Ti1 177.5(6) . . ?
C29 N3 Ti2 170.7(5) . . ?
C31 N4 Ti2 156.7(5) . . ?
O4 Ti3 N6 175.83(19) . . ?
O4 Ti3 Br10 98.37(13) . . ?
N6 Ti3 Br10 81.79(13) . . ?
O4 Ti3 Br9 90.36(13) . . ?
N6 Ti3 Br9 85.48(14) . . ?
Br10 Ti3 Br9 92.72(4) . . ?
O4 Ti3 Br7 97.98(13) . . ?
N6 Ti3 Br7 86.19(13) . . ?
Br10 Ti3 Br7 89.22(4) . . ?
Br9 Ti3 Br7 171.08(5) . . ?
O4 Ti3 Br8 96.99(13) . . ?
N6 Ti3 Br8 83.02(13) . . ?
Br10 Ti3 Br8 164.57(5) . . ?
Br9 Ti3 Br8 88.76(4) . . ?
Br7 Ti3 Br8 87.08(4) . . ?
O5 Ti4 O6 97.10(16) . . ?
O5 Ti4 N8 94.11(18) . . ?
O6 Ti4 N8 168.53(18) . . ?
O5 Ti4 N7 176.04(18) . . ?
O6 Ti4 N7 86.77(18) . . ?
N8 Ti4 N7 82.06(19) . . ?
O5 Ti4 Br11 93.32(12) . . ?
O6 Ti4 Br11 98.92(12) . . ?
N8 Ti4 Br11 82.79(13) . . ?
N7 Ti4 Br11 85.25(14) . . ?
O5 Ti4 Br12 93.83(12) . . ?
O6 Ti4 Br12 95.38(12) . . ?
N8 Ti4 Br12 81.42(13) . . ?
N7 Ti4 Br12 86.58(13) . . ?
Br11 Ti4 Br12 163.08(4) . . ?
O4 C41 C42 120.2(5) . . ?
O4 C41 C46 119.2(5) . . ?
C42 C41 C46 120.5(5) . . ?
C43 C42 C41 119.9(5) . . ?
C43 C42 C66 118.9(5) . . ?
C41 C42 C66 121.2(5) . . ?
C44 C43 C42 121.7(5) . . ?
C44 C43 H43 119.1 . . ?
C42 C43 H43 119.1 . . ?
C43 C44 C45 117.5(5) . . ?
C43 C44 C47 121.5(5) . . ?
C45 C44 C47 121.0(6) . . ?
C46 C45 C44 122.9(5) . . ?
C46 C45 H45 118.5 . . ?
C44 C45 H45 118.5 . . ?
C45 C46 C41 117.5(5) . . ?
C45 C46 C48 123.0(5) . . ?
C41 C46 C48 119.5(5) . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C50 C48 C46 113.4(5) . . ?
C50 C48 H48A 108.9 . . ?
C46 C48 H48A 108.9 . . ?
C50 C48 H48B 108.9 . . ?
C46 C48 H48B 108.9 . . ?
H48A C48 H48B 107.7 . . ?
O5 C49 C54 118.3(5) . . ?
O5 C49 C50 118.9(4) . . ?
C54 C49 C50 122.8(5) . . ?
C51 C50 C49 117.0(5) . . ?
C51 C50 C48 122.6(5) . . ?
C49 C50 C48 120.4(5) . . ?
C50 C51 C52 122.9(5) . . ?
C50 C51 H51 118.6 . . ?
C52 C51 H51 118.6 . . ?
C51 C52 C53 118.3(5) . . ?
C51 C52 C55 121.0(5) . . ?
C53 C52 C55 120.7(5) . . ?
C54 C53 C52 121.0(5) . . ?
C54 C53 H53 119.5 . . ?
C52 C53 H53 119.5 . . ?
C49 C54 C53 117.7(5) . . ?
C49 C54 C56 120.3(5) . . ?
C53 C54 C56 121.9(4) . . ?
C52 C55 H55A 109.5 . . ?
C52 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C52 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 C58 115.1(4) . . ?
C54 C56 H56A 108.5 . . ?
C58 C56 H56A 108.5 . . ?
C54 C56 H56B 108.5 . . ?
C58 C56 H56B 108.5 . . ?
H56A C56 H56B 107.5 . . ?
O6 C57 C63 117.3(5) . . ?
O6 C57 C58 121.9(5) . . ?
C63 C57 C58 120.8(5) . . ?
C59 C58 C57 117.6(5) . . ?
C59 C58 C56 119.8(5) . . ?
C57 C58 C56 122.3(4) . . ?
C60 C59 C58 122.9(5) . . ?
C60 C59 H59 118.5 . . ?
C58 C59 H59 118.5 . . ?
C59 C60 C62 118.0(5) . . ?
C59 C60 C61 122.3(5) . . ?
C62 C60 C61 119.7(5) . . ?
C60 C61 H61A 109.5 . . ?
C60 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C60 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C60 C62 C63 121.3(5) . . ?
C60 C62 H62 119.3 . . ?
C63 C62 H62 119.3 . . ?
C57 C63 C62 119.0(5) . . ?
C57 C63 C64 121.1(5) . . ?
C62 C63 C64 119.8(5) . . ?
C63 C64 N5 114.4(5) . . ?
C63 C64 H64A 108.7 . . ?
N5 C64 H64A 108.7 . . ?
C63 C64 H64B 108.7 . . ?
N5 C64 H64B 108.7 . . ?
H64A C64 H64B 107.6 . . ?
N5 C65 H65A 109.5 . . ?
N5 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
N5 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
N5 C66 C42 112.9(5) 2_766 . ?
N5 C66 H66A 109.0 2_766 . ?
C42 C66 H66A 109.0 . . ?
N5 C66 H66B 109.0 2_766 . ?
C42 C66 H66B 109.0 . . ?
H66A C66 H66B 107.8 . . ?
N6 C67 C68 178.5(6) . . ?
C67 C68 H68A 109.5 . . ?
C67 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C67 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
N7 C69 C70 177.1(8) . . ?
C69 C70 H70A 109.5 . . ?
C69 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
C69 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
N8 C71 C72 179.4(9) . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C65 N5 C66 112.6(4) . 2_766 ?
C65 N5 C64 112.7(4) . . ?
C66 N5 C64 107.8(4) 2_766 . ?
C65 N5 H5A 107.8 . . ?
C66 N5 H5A 107.8 2_766 . ?
C64 N5 H5A 107.8 . . ?
C67 N6 Ti3 172.8(5) . . ?
C69 N7 Ti4 173.5(5) . . ?
C71 N8 Ti4 174.9(5) . . ?
N9 C73 C74 175.6(17) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
N10 C75 C76 178.0(9) . . ?
C75 C76 H76A 109.5 . . ?
C75 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C75 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
N11 C77 C78 165.2(19) . . ?
C77 C78 H78A 109.5 . . ?
C77 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C77 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
N12 C79 C80 176.1(14) . . ?
C79 C80 H80A 109.5 . . ?
C79 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C79 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C81 C82 H82A 109.5 . . ?
C81 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C81 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
N13 C81 C82 173(3) . . ?
C41 O4 Ti3 164.5(4) . . ?
C49 O5 Ti4 160.6(3) . . ?
C57 O6 Ti4 135.9(3) . . ?

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
Br2 Ti1 O1 C1 -75.2(12) . . . . ?
Br1 Ti1 O1 C1 -166.9(12) . . . . ?
Br3 Ti1 O1 C1 16.4(12) . . . . ?
Br4 Ti1 O1 C1 104.9(12) . . . . ?
O3 Ti2 O2 C9 -30.6(14) . . . . ?
N4 Ti2 O2 C9 155.7(13) . . . . ?
Br6 Ti2 O2 C9 70.5(13) . . . . ?
Br5 Ti2 O2 C9 -124.4(13) . . . . ?
O2 Ti2 O3 C17 -18.8(6) . . . . ?
N4 Ti2 O3 C17 135.0(9) . . . . ?
N3 Ti2 O3 C17 161.2(6) . . . . ?
Br6 Ti2 O3 C17 -115.5(5) . . . . ?
Br5 Ti2 O3 C17 75.6(5) . . . . ?
Ti1 O1 C1 C6 104.6(12) . . . . ?
Ti1 O1 C1 C2 -74.9(14) . . . . ?
O1 C1 C2 C3 179.0(5) . . . . ?
C6 C1 C2 C3 -0.5(9) . . . . ?
O1 C1 C2 C26 -2.1(9) . . . . ?
C6 C1 C2 C26 178.5(6) . . . . ?
C1 C2 C3 C4 1.6(10) . . . . ?
C26 C2 C3 C4 -177.4(6) . . . . ?
C2 C3 C4 C5 -2.0(11) . . . . ?
C2 C3 C4 C7 177.8(8) . . . . ?
C3 C4 C5 C6 1.3(11) . . . . ?
C7 C4 C5 C6 -178.4(8) . . . . ?
C4 C5 C6 C1 -0.3(10) . . . . ?
C4 C5 C6 C8 177.2(6) . . . . ?
O1 C1 C6 C5 -179.6(5) . . . . ?
C2 C1 C6 C5 -0.1(9) . . . . ?
O1 C1 C6 C8 2.8(8) . . . . ?
C2 C1 C6 C8 -177.7(5) . . . . ?
C5 C6 C8 C10 7.9(8) . . . . ?
C1 C6 C8 C10 -174.6(5) . . . . ?
Ti2 O2 C9 C14 2.0(17) . . . . ?
Ti2 O2 C9 C10 -176.7(11) . . . . ?
O2 C9 C10 C11 179.3(6) . . . . ?
C14 C9 C10 C11 0.6(9) . . . . ?
O2 C9 C10 C8 -3.4(9) . . . . ?
C14 C9 C10 C8 178.0(6) . . . . ?
C6 C8 C10 C11 95.1(7) . . . . ?
C6 C8 C10 C9 -82.2(7) . . . . ?
C9 C10 C11 C12 -1.3(11) . . . . ?
C8 C10 C11 C12 -178.7(7) . . . . ?
C10 C11 C12 C13 1.6(13) . . . . ?
C10 C11 C12 C15 -178.2(8) . . . . ?
C11 C12 C13 C14 -1.1(13) . . . . ?
C15 C12 C13 C14 178.7(8) . . . . ?
C12 C13 C14 C9 0.4(11) . . . . ?
C12 C13 C14 C16 -177.2(7) . . . . ?
O2 C9 C14 C13 -178.8(6) . . . . ?
C10 C9 C14 C13 -0.2(10) . . . . ?
O2 C9 C14 C16 -1.2(9) . . . . ?
C10 C9 C14 C16 177.4(6) . . . . ?
C13 C14 C16 C18 -102.6(7) . . . . ?
C9 C14 C16 C18 79.9(7) . . . . ?
Ti2 O3 C17 C22 -128.5(5) . . . . ?
Ti2 O3 C17 C18 52.8(8) . . . . ?
O3 C17 C18 C19 -178.0(5) . . . . ?
C22 C17 C18 C19 3.2(8) . . . . ?
O3 C17 C18 C16 6.6(8) . . . . ?
C22 C17 C18 C16 -172.2(5) . . . . ?
C14 C16 C18 C19 82.8(7) . . . . ?
C14 C16 C18 C17 -101.9(7) . . . . ?
C17 C18 C19 C20 -0.2(9) . . . . ?
C16 C18 C19 C20 175.3(6) . . . . ?
C18 C19 C20 C21 -2.7(9) . . . . ?
C18 C19 C20 C23 -178.7(6) . . . . ?
C19 C20 C21 C22 2.6(9) . . . . ?
C23 C20 C21 C22 178.6(6) . . . . ?
C20 C21 C22 C17 0.3(9) . . . . ?
C20 C21 C22 C24 -174.0(5) . . . . ?
O3 C17 C22 C21 177.9(5) . . . . ?
C18 C17 C22 C21 -3.3(8) . . . . ?
O3 C17 C22 C24 -7.8(7) . . . . ?
C18 C17 C22 C24 171.0(5) . . . . ?
C21 C22 C24 N1 -107.4(6) . . . . ?
C17 C22 C24 N1 78.3(7) . . . . ?
C3 C2 C26 N1 71.8(8) . . . 2_655 ?
C1 C2 C26 N1 -107.1(7) . . . 2_655 ?
C22 C24 N1 C25 52.2(7) . . . . ?
C22 C24 N1 C26 177.1(5) . . . 2_655 ?
O4 C41 C42 C43 179.9(5) . . . . ?
C46 C41 C42 C43 -0.3(9) . . . . ?
O4 C41 C42 C66 0.5(8) . . . . ?
C46 C41 C42 C66 -179.7(5) . . . . ?
C41 C42 C43 C44 -2.1(9) . . . . ?
C66 C42 C43 C44 177.4(6) . . . . ?
C42 C43 C44 C45 2.9(9) . . . . ?
C42 C43 C44 C47 -175.3(6) . . . . ?
C43 C44 C45 C46 -1.4(9) . . . . ?
C47 C44 C45 C46 176.7(6) . . . . ?
C44 C45 C46 C41 -0.8(9) . . . . ?
C44 C45 C46 C48 -177.7(6) . . . . ?
O4 C41 C46 C45 -178.6(5) . . . . ?
C42 C41 C46 C45 1.6(8) . . . . ?
O4 C41 C46 C48 -1.5(8) . . . . ?
C42 C41 C46 C48 178.7(5) . . . . ?
C45 C46 C48 C50 -6.1(8) . . . . ?
C41 C46 C48 C50 176.9(5) . . . . ?
O5 C49 C50 C51 -176.3(5) . . . . ?
C54 C49 C50 C51 4.6(8) . . . . ?
O5 C49 C50 C48 4.8(7) . . . . ?
C54 C49 C50 C48 -174.3(5) . . . . ?
C46 C48 C50 C51 -104.2(6) . . . . ?
C46 C48 C50 C49 74.7(7) . . . . ?
C49 C50 C51 C52 0.3(8) . . . . ?
C48 C50 C51 C52 179.2(5) . . . . ?
C50 C51 C52 C53 -3.8(8) . . . . ?
C50 C51 C52 C55 177.4(6) . . . . ?
C51 C52 C53 C54 2.6(8) . . . . ?
C55 C52 C53 C54 -178.6(5) . . . . ?
O5 C49 C54 C53 175.2(4) . . . . ?
C50 C49 C54 C53 -5.7(8) . . . . ?
O5 C49 C54 C56 -4.6(7) . . . . ?
C50 C49 C54 C56 174.5(5) . . . . ?
C52 C53 C54 C49 2.0(7) . . . . ?
C52 C53 C54 C56 -178.2(5) . . . . ?
C49 C54 C56 C58 -67.4(6) . . . . ?
C53 C54 C56 C58 112.8(5) . . . . ?
O6 C57 C58 C59 176.5(4) . . . . ?
C63 C57 C58 C59 -5.9(7) . . . . ?
O6 C57 C58 C56 -9.5(7) . . . . ?
C63 C57 C58 C56 168.1(5) . . . . ?
C54 C56 C58 C59 -80.9(6) . . . . ?
C54 C56 C58 C57 105.3(6) . . . . ?
C57 C58 C59 C60 2.2(8) . . . . ?
C56 C58 C59 C60 -171.9(5) . . . . ?
C58 C59 C60 C62 2.0(8) . . . . ?
C58 C59 C60 C61 -179.1(5) . . . . ?
C59 C60 C62 C63 -2.8(8) . . . . ?
C61 C60 C62 C63 178.3(5) . . . . ?
O6 C57 C63 C62 -177.1(4) . . . . ?
C58 C57 C63 C62 5.1(7) . . . . ?
O6 C57 C63 C64 6.3(7) . . . . ?
C58 C57 C63 C64 -171.4(5) . . . . ?
C60 C62 C63 C57 -0.7(8) . . . . ?
C60 C62 C63 C64 175.9(5) . . . . ?
C57 C63 C64 N5 -81.5(6) . . . . ?
C62 C63 C64 N5 102.0(6) . . . . ?
C43 C42 C66 N5 -79.5(7) . . . 2_766 ?
C41 C42 C66 N5 99.9(6) . . . 2_766 ?
C63 C64 N5 C65 -58.2(6) . . . . ?
C63 C64 N5 C66 176.8(5) . . . 2_766 ?
C42 C41 O4 Ti3 104.3(13) . . . . ?
C46 C41 O4 Ti3 -75.5(15) . . . . ?
Br10 Ti3 O4 C41 100.7(13) . . . . ?
Br9 Ti3 O4 C41 7.9(13) . . . . ?
Br7 Ti3 O4 C41 -169.0(13) . . . . ?
Br8 Ti3 O4 C41 -80.9(13) . . . . ?
C54 C49 O5 Ti4 -34.6(13) . . . . ?
C50 C49 O5 Ti4 146.3(8) . . . . ?
O6 Ti4 O5 C49 66.8(10) . . . . ?
N8 Ti4 O5 C49 -115.6(10) . . . . ?
Br11 Ti4 O5 C49 -32.6(10) . . . . ?
Br12 Ti4 O5 C49 162.7(10) . . . . ?
C63 C57 O6 Ti4 126.4(5) . . . . ?
C58 C57 O6 Ti4 -55.9(7) . . . . ?
O5 Ti4 O6 C57 18.2(5) . . . . ?
N8 Ti4 O6 C57 -149.5(8) . . . . ?
N7 Ti4 O6 C57 -162.6(5) . . . . ?
Br11 Ti4 O6 C57 112.7(4) . . . . ?
Br12 Ti4 O6 C57 -76.3(4) . . . . ?

_refine_diff_density_max         1.543
_refine_diff_density_min         -1.159
_refine_diff_density_rms         0.165


