# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2022

####################################################################### 
# 
# 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_ti14pa6
_database_code_depnum_ccdc_archive 'CCDC 2126646'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2021-12-06 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2021-12-01
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         
'C72 H108 N6 O44 Ti14, 2(C3 H8 O), 2(C2 H3 N), 2(C4 H11 N)'
_chemical_formula_sum            'C90 H152 N10 O46 Ti14'
_chemical_formula_weight         2780.81
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Ti C O N'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   19.4181(2)
_cell_length_b                   16.6427(2)
_cell_length_c                   20.1511(4)
_cell_angle_alpha                90
_cell_angle_beta                 107.688(2)
_cell_angle_gamma                90
_cell_volume                     6204.36(17)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    15892
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.4030
_cell_measurement_theta_min      2.7250
_shelx_estimated_absorpt_T_max   0.992
_shelx_estimated_absorpt_T_min   0.911
_exptl_absorpt_coefficient_mu    7.946
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35631
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.489
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             2876
_exptl_crystal_size_max          0.012
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.001
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0838
_diffrn_reflns_av_unetI/netI     0.0694
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.943
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            44175
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.709
_diffrn_reflns_theta_min         2.768
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.943
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     93.00 177.00   1.00    0.98    --  106.49  57.00 150.00   84
  2  ω     71.00  96.00   1.00    0.17    --   48.45 166.00 153.00   25
  3  ω    101.00 178.00   1.00    0.98    --  106.49 115.00   7.00   77
  4  ω     94.00 178.00   1.00    0.98    --  106.49  38.00-180.00   84
  5  ω    -27.00  27.00   1.00    0.17    --  -48.45  19.00 120.00   54
  6  ω    -27.00  27.00   1.00    0.17    --  -48.45  19.00   0.00   54
  7  ω    -42.00 -14.00   1.00    0.98    --  -86.25  38.00 -60.00   28
  8  ω    -42.00 -13.00   1.00    0.98    --  -86.25  38.00   0.00   29
  9  ω    -72.00 -47.00   1.00    0.98    --  -86.25 115.00   7.00   25
 10  ω    -69.00 -44.00   1.00    0.17    --  -48.45 115.00   7.00   25
 11  ω   -112.00 -86.00   1.00    0.17    --  -48.45 166.00 153.00   26
 12  ω    -98.00 -73.00   1.00    0.98    --  -86.25 166.00 153.00   25
 13  ω     37.00 105.00   1.00    0.98    --  106.49 -99.00 -60.00   68
 14  ω     83.00 108.00   1.00    0.98    --  106.49-115.00 -81.00   25
 15  ω     39.00  66.00   1.00    0.98    --  106.49-115.00 -81.00   27
 16  ω     65.00  91.00   1.00    0.17    --   48.45-115.00 -81.00   26
 17  ω     80.00 105.00   1.00    0.17    --   48.45-166.00 132.00   25
 18  ω     58.00 140.00   1.00    0.98    --  106.49-166.00 132.00   82
 19  ω     34.00  64.00   1.00    0.98    --  106.49 -57.00 120.00   30
 20  ω     35.00  66.00   1.00    0.98    --  106.49 -57.00 -30.00   31
 21  ω     34.00 104.00   1.00    0.98    --  106.49 -77.00 -60.00   70
 22  ω     34.00  66.00   1.00    0.98    --  106.49 -57.00-120.00   32
 23  ω   -115.00 -47.00   1.00    0.17    --  -48.45-166.00 132.00   68
 24  ω   -110.00 -84.00   1.00    0.98    --  -86.25-166.00 132.00   26
 25  ω   -120.00 -73.00   1.00    0.17    --  -48.45-125.00 -60.00   47
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0097305000
_diffrn_orient_matrix_UB_12      0.0730388000
_diffrn_orient_matrix_UB_13      0.0432550000
_diffrn_orient_matrix_UB_21      -0.0335539000
_diffrn_orient_matrix_UB_22      -0.0548646000
_diffrn_orient_matrix_UB_23      0.0435397000
_diffrn_orient_matrix_UB_31      0.0755602000
_diffrn_orient_matrix_UB_32      -0.0149246000
_diffrn_orient_matrix_UB_33      0.0517200000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                9698
_reflns_number_total             12329
_reflns_odcompleteness_completeness 99.16
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.924
_refine_diff_density_min         -0.725
_refine_diff_density_rms         0.111
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     742
_refine_ls_number_reflns         12329
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0899
_refine_ls_R_factor_gt           0.0706
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0626P)²+34.7525P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1852
_refine_ls_wR_factor_ref         0.1953
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 C44-C45 = C44-C43 = O23-C44
 1.45 with sigma of 0.01
 N5-H5
 0.998 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O23 \\sim C43 \\sim C44 \\sim C45: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
4.a Ternary CH refined with riding coordinates:
 C20(H20), C23(H23), C26(H26), C29(H29), C32(H32), C35(H35), C44(H44)
4.b Secondary CH2 refined with riding coordinates:
 C40(H40A,H40B), C41(H41A,H41B)
4.c Me refined with riding coordinates:
 C33(H33A,H33B,H33C)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16)
4.e Idealised Me refined as rotating group:
 C19(H19A,H19B,H19C), C21(H21A,H21B,H21C), C22(H22A,H22B,H22C), C24(H24A,H24B,
 H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,
 H30B,H30C), C31(H31A,H31B,H31C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C),
 C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C43(H43A,H43B,
 H43C), C45(H45A,H45B,H45C)
4.f Idealised tetrahedral OH refined as rotating group:
 O23(H23A)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.63254(4) 0.61996(5) 0.43779(5) 0.0281(2) Uani 1 1 d . . . . .
Ti2 Ti 0.71495(4) 0.42218(5) 0.45737(5) 0.0279(2) Uani 1 1 d . . . . .
Ti3 Ti 0.53281(4) 0.33990(5) 0.38157(5) 0.0273(2) Uani 1 1 d . . . . .
Ti4 Ti 0.43479(4) 0.54510(5) 0.36298(5) 0.0264(2) Uani 1 1 d . . . . .
Ti5 Ti 0.46915(4) 0.41665(5) 0.48243(5) 0.0246(2) Uani 1 1 d . . . . .
Ti6 Ti 0.31239(4) 0.48093(5) 0.42202(5) 0.0266(2) Uani 1 1 d . . . . .
Ti7 Ti 0.37906(4) 0.65801(5) 0.45928(5) 0.0266(2) Uani 1 1 d . . . . .
O1 O 0.72500(18) 0.6876(2) 0.4801(2) 0.0372(9) Uani 1 1 d . . . . .
O2 O 0.7780(2) 0.8039(3) 0.5210(3) 0.0635(15) Uani 1 1 d . . . . .
O3 O 0.6355(2) 0.6277(2) 0.3510(2) 0.0381(9) Uani 1 1 d . . . . .
O4 O 0.68935(17) 0.5275(2) 0.4708(2) 0.0290(8) Uani 1 1 d . . . . .
O5 O 0.9376(2) 0.4103(3) 0.5476(3) 0.0536(13) Uani 1 1 d . . . . .
O6 O 0.82214(18) 0.4493(2) 0.5072(2) 0.0364(9) Uani 1 1 d . . . . .
O7 O 0.72591(19) 0.4260(2) 0.3730(2) 0.0369(9) Uani 1 1 d . . . . .
O8 O 0.62708(17) 0.3648(2) 0.4355(2) 0.0299(8) Uani 1 1 d . . . . .
O9 O 0.5334(3) 0.0950(3) 0.4068(3) 0.0585(13) Uani 1 1 d . . . . .
O10 O 0.56211(18) 0.2212(2) 0.3898(2) 0.0363(9) Uani 1 1 d . . . . .
O11 O 0.5273(2) 0.3475(2) 0.2916(2) 0.0372(9) Uani 1 1 d . . . . .
O12 O 0.47947(16) 0.4327(2) 0.38879(19) 0.0268(7) Uani 1 1 d . . . . .
O13 O 0.43901(18) 0.5566(2) 0.2756(2) 0.0329(8) Uani 1 1 d . . . . .
O14 O 0.53644(17) 0.5878(2) 0.42032(19) 0.0274(7) Uani 1 1 d . . . . .
O15 O 0.39768(17) 0.6469(2) 0.3774(2) 0.0292(8) Uani 1 1 d . . . . .
O16 O 0.34333(17) 0.4966(2) 0.34713(19) 0.0289(8) Uani 1 1 d . . . . .
O17 O 0.34086(18) 0.7568(2) 0.4485(2) 0.0336(8) Uani 1 1 d . . . . .
O18 O 0.29554(17) 0.5898(2) 0.44406(19) 0.0283(8) Uani 1 1 d . . . . .
O19 O 0.22133(18) 0.4468(2) 0.3785(2) 0.0357(9) Uani 1 1 d . . . . .
O20 O 0.37206(17) 0.3856(2) 0.45980(19) 0.0270(7) Uani 1 1 d . . . . .
O21 O 0.52149(17) 0.3229(2) 0.48073(19) 0.0274(7) Uani 1 1 d . . . . .
O22 O 0.43447(16) 0.53132(19) 0.46894(18) 0.0237(7) Uani 1 1 d . . . . .
O23 O 0.6622(4) 0.0418(6) 0.3843(4) 0.114(3) Uani 1 1 d D U . . .
H23A H 0.6230 0.0528 0.3920 0.172 Uiso 1 1 calc R U . . .
N1 N 0.5974(2) 0.7472(3) 0.4386(3) 0.0346(11) Uani 1 1 d . . . . .
N2 N 0.7747(2) 0.3056(3) 0.4741(3) 0.0337(10) Uani 1 1 d . . . . .
N3 N 0.4297(2) 0.2696(3) 0.3538(3) 0.0322(10) Uani 1 1 d . . . . .
N4 N 0.9746(10) 0.890(2) 0.5350(14) 0.316(18) Uani 1 1 d . . . . .
N5 N 0.8564(3) 0.6132(3) 0.5102(3) 0.0443(13) Uani 1 1 d D . . . .
H5 H 0.850(3) 0.5559(16) 0.523(3) 0.020(13) Uiso 1 1 d D . . . .
C1 C 0.5297(3) 0.7746(3) 0.4133(4) 0.0401(14) Uani 1 1 d . . . . .
H1 H 0.4919 0.7376 0.3929 0.048 Uiso 1 1 calc R U . . .
C2 C 0.5132(3) 0.8554(4) 0.4161(4) 0.0531(19) Uani 1 1 d . . . . .
H2 H 0.4647 0.8734 0.3975 0.064 Uiso 1 1 calc R U . . .
C3 C 0.5675(4) 0.9091(4) 0.4461(5) 0.066(2) Uani 1 1 d . . . . .
H3 H 0.5569 0.9644 0.4492 0.079 Uiso 1 1 calc R U . . .
C4 C 0.6384(4) 0.8813(4) 0.4720(5) 0.060(2) Uani 1 1 d . . . . .
H4 H 0.6771 0.9172 0.4923 0.072 Uiso 1 1 calc R U . . .
C5 C 0.6506(3) 0.8000(3) 0.4673(4) 0.0407(14) Uani 1 1 d . . . . .
C6 C 0.7244(3) 0.7634(4) 0.4927(4) 0.0427(15) Uani 1 1 d . . . . .
C7 C 0.7465(3) 0.2329(4) 0.4511(4) 0.0419(14) Uani 1 1 d . . . . .
H7 H 0.6955 0.2273 0.4333 0.050 Uiso 1 1 calc R U . . .
C8 C 0.7898(3) 0.1663(4) 0.4528(4) 0.0533(18) Uani 1 1 d . . . . .
H8 H 0.7688 0.1158 0.4359 0.064 Uiso 1 1 calc R U . . .
C9 C 0.8644(3) 0.1744(4) 0.4796(4) 0.0553(18) Uani 1 1 d . . . . .
H9 H 0.8951 0.1294 0.4814 0.066 Uiso 1 1 calc R U . . .
C10 C 0.8932(3) 0.2480(4) 0.5034(4) 0.0479(16) Uani 1 1 d . . . . .
H10 H 0.9441 0.2549 0.5217 0.058 Uiso 1 1 calc R U . . .
C11 C 0.8470(3) 0.3122(3) 0.5003(3) 0.0355(12) Uani 1 1 d . . . . .
C12 C 0.8736(3) 0.3959(4) 0.5213(3) 0.0368(13) Uani 1 1 d . . . . .
C13 C 0.3630(3) 0.2995(4) 0.3333(3) 0.0376(13) Uani 1 1 d . . . . .
H13 H 0.3558 0.3547 0.3212 0.045 Uiso 1 1 calc R U . . .
C14 C 0.3033(3) 0.2505(4) 0.3295(4) 0.0514(17) Uani 1 1 d . . . . .
H14 H 0.2557 0.2721 0.3147 0.062 Uiso 1 1 calc R U . . .
C15 C 0.3141(4) 0.1710(4) 0.3474(4) 0.059(2) Uani 1 1 d . . . . .
H15 H 0.2742 0.1371 0.3454 0.071 Uiso 1 1 calc R U . . .
C16 C 0.3840(3) 0.1404(4) 0.3686(4) 0.0510(17) Uani 1 1 d . . . . .
H16 H 0.3929 0.0854 0.3809 0.061 Uiso 1 1 calc R U . . .
C17 C 0.4396(3) 0.1917(3) 0.3709(3) 0.0372(13) Uani 1 1 d . . . . .
C18 C 0.5175(3) 0.1651(3) 0.3917(4) 0.0410(14) Uani 1 1 d . . . . .
C19 C 0.6245(10) 0.5814(10) 0.2383(6) 0.175(9) Uani 1 1 d . . . . .
H19A H 0.6768 0.5826 0.2459 0.262 Uiso 1 1 calc R U . . .
H19B H 0.5990 0.5903 0.1889 0.262 Uiso 1 1 calc R U . . .
H19C H 0.6108 0.5289 0.2525 0.262 Uiso 1 1 calc R U . . .
C20 C 0.6055(6) 0.6426(6) 0.2785(5) 0.078(3) Uani 1 1 d . . . . .
H20 H 0.5521 0.6368 0.2691 0.094 Uiso 1 1 calc R U . . .
C21 C 0.6156(9) 0.7247(8) 0.2605(7) 0.140(6) Uani 1 1 d . . . . .
H21A H 0.5913 0.7608 0.2847 0.210 Uiso 1 1 calc R U . . .
H21B H 0.5950 0.7319 0.2101 0.210 Uiso 1 1 calc R U . . .
H21C H 0.6673 0.7371 0.2746 0.210 Uiso 1 1 calc R U . . .
C22 C 0.7045(4) 0.3284(7) 0.2805(6) 0.099(4) Uani 1 1 d . . . . .
H22A H 0.7254 0.2822 0.3099 0.148 Uiso 1 1 calc R U . . .
H22B H 0.7090 0.3204 0.2338 0.148 Uiso 1 1 calc R U . . .
H22C H 0.6533 0.3335 0.2774 0.148 Uiso 1 1 calc R U . . .
C23 C 0.7445(4) 0.4045(5) 0.3124(4) 0.0555(18) Uani 1 1 d . . . . .
H23 H 0.7296 0.4490 0.2776 0.067 Uiso 1 1 calc R U . . .
C24 C 0.8249(4) 0.3938(5) 0.3307(5) 0.063(2) Uani 1 1 d . . . . .
H24A H 0.8491 0.4429 0.3529 0.095 Uiso 1 1 calc R U . . .
H24B H 0.8380 0.3830 0.2883 0.095 Uiso 1 1 calc R U . . .
H24C H 0.8400 0.3486 0.3630 0.095 Uiso 1 1 calc R U . . .
C25 C 0.4818(6) 0.2498(6) 0.2019(5) 0.091(3) Uani 1 1 d . . . . .
H25A H 0.5305 0.2342 0.2021 0.137 Uiso 1 1 calc R U . . .
H25B H 0.4479 0.2419 0.1551 0.137 Uiso 1 1 calc R U . . .
H25C H 0.4669 0.2167 0.2353 0.137 Uiso 1 1 calc R U . . .
C26 C 0.4817(4) 0.3370(5) 0.2219(4) 0.0586(19) Uani 1 1 d . . . . .
H26 H 0.4314 0.3515 0.2206 0.070 Uiso 1 1 calc R U . . .
C27 C 0.5035(5) 0.3915(7) 0.1736(5) 0.086(3) Uani 1 1 d . . . . .
H27A H 0.5101 0.4460 0.1929 0.129 Uiso 1 1 calc R U . . .
H27B H 0.4657 0.3920 0.1284 0.129 Uiso 1 1 calc R U . . .
H27C H 0.5489 0.3725 0.1674 0.129 Uiso 1 1 calc R U . . .
C28 C 0.3436(3) 0.5299(4) 0.1714(4) 0.0551(19) Uani 1 1 d . . . . .
H28A H 0.3614 0.4752 0.1688 0.083 Uiso 1 1 calc R U . . .
H28B H 0.3197 0.5499 0.1243 0.083 Uiso 1 1 calc R U . . .
H28C H 0.3090 0.5295 0.1981 0.083 Uiso 1 1 calc R U . . .
C29 C 0.4066(3) 0.5842(4) 0.2070(3) 0.0445(15) Uani 1 1 d . . . . .
H29 H 0.4431 0.5800 0.1813 0.053 Uiso 1 1 calc R U . . .
C30 C 0.3859(4) 0.6708(4) 0.2080(4) 0.0572(19) Uani 1 1 d . . . . .
H30A H 0.3532 0.6771 0.2363 0.086 Uiso 1 1 calc R U . . .
H30B H 0.3615 0.6889 0.1603 0.086 Uiso 1 1 calc R U . . .
H30C H 0.4294 0.7032 0.2279 0.086 Uiso 1 1 calc R U . . .
C31 C 0.1456(7) 0.4152(7) 0.2648(5) 0.119(5) Uani 1 1 d . . . . .
H31A H 0.1071 0.4374 0.2256 0.179 Uiso 1 1 calc R U . . .
H31B H 0.1271 0.3686 0.2838 0.179 Uiso 1 1 calc R U . . .
H31C H 0.1862 0.3985 0.2487 0.179 Uiso 1 1 calc R U . . .
C32 C 0.1686(5) 0.4730(5) 0.3159(5) 0.088(3) Uani 1 1 d . . . . .
H32 H 0.1274 0.4629 0.3349 0.106 Uiso 1 1 calc R U . . .
C33 C 0.1553(6) 0.5552(6) 0.3096(5) 0.100(4) Uani 1 1 d . . . . .
H33A H 0.1784 0.5813 0.3545 0.149 Uiso 1 1 calc R U . . .
H33B H 0.1751 0.5774 0.2742 0.149 Uiso 1 1 calc R U . . .
H33C H 0.1031 0.5647 0.2959 0.149 Uiso 1 1 calc R U . . .
C34 C 0.2338(4) 0.7957(5) 0.3586(4) 0.059(2) Uani 1 1 d . . . . .
H34A H 0.2295 0.7418 0.3382 0.088 Uiso 1 1 calc R U . . .
H34B H 0.2143 0.8354 0.3217 0.088 Uiso 1 1 calc R U . . .
H34C H 0.2067 0.7981 0.3924 0.088 Uiso 1 1 calc R U . . .
C35 C 0.3132(3) 0.8142(3) 0.3953(3) 0.0413(14) Uani 1 1 d . . . . .
H35 H 0.3406 0.8100 0.3606 0.050 Uiso 1 1 calc R U . . .
C36 C 0.3234(4) 0.8977(4) 0.4263(4) 0.0542(18) Uani 1 1 d . . . . .
H36A H 0.2932 0.9042 0.4571 0.081 Uiso 1 1 calc R U . . .
H36B H 0.3093 0.9376 0.3888 0.081 Uiso 1 1 calc R U . . .
H36C H 0.3743 0.9055 0.4531 0.081 Uiso 1 1 calc R U . . .
C37 C 0.8537(10) 0.9387(9) 0.4489(12) 0.185(9) Uani 1 1 d . . . . .
H37A H 0.8302 0.8942 0.4186 0.277 Uiso 1 1 calc R U . . .
H37B H 0.8644 0.9820 0.4205 0.277 Uiso 1 1 calc R U . . .
H37C H 0.8213 0.9590 0.4741 0.277 Uiso 1 1 calc R U . . .
C38 C 0.9215(11) 0.9101(14) 0.4992(13) 0.174(9) Uani 1 1 d . . . . .
C39 C 0.8749(6) 0.6897(6) 0.4120(6) 0.093(3) Uani 1 1 d . . . . .
H39A H 0.8887 0.6842 0.3693 0.139 Uiso 1 1 calc R U . . .
H39B H 0.9094 0.7250 0.4447 0.139 Uiso 1 1 calc R U . . .
H39C H 0.8263 0.7130 0.4007 0.139 Uiso 1 1 calc R U . . .
C40 C 0.8752(4) 0.6097(5) 0.4441(4) 0.0609(19) Uani 1 1 d . . . . .
H40A H 0.9238 0.5855 0.4534 0.073 Uiso 1 1 calc R U . . .
H40B H 0.8402 0.5744 0.4108 0.073 Uiso 1 1 calc R U . . .
C41 C 0.9084(3) 0.6578(4) 0.5693(4) 0.0527(17) Uani 1 1 d . . . . .
H41A H 0.8889 0.6595 0.6093 0.063 Uiso 1 1 calc R U . . .
H41B H 0.9129 0.7139 0.5546 0.063 Uiso 1 1 calc R U . . .
C42 C 0.9823(4) 0.6194(5) 0.5920(5) 0.070(2) Uani 1 1 d . . . . .
H42A H 1.0055 0.6265 0.5555 0.105 Uiso 1 1 calc R U . . .
H42B H 0.9774 0.5619 0.6002 0.105 Uiso 1 1 calc R U . . .
H42C H 1.0119 0.6449 0.6351 0.105 Uiso 1 1 calc R U . . .
C43 C 0.5724(6) 0.0031(12) 0.2766(8) 0.171(6) Uani 1 1 d D U . . .
H43A H 0.5640 -0.0545 0.2802 0.257 Uiso 1 1 calc R U . . .
H43B H 0.5610 0.0181 0.2273 0.257 Uiso 1 1 calc R U . . .
H43C H 0.5415 0.0335 0.2979 0.257 Uiso 1 1 calc R U . . .
C44 C 0.6481(7) 0.0215(11) 0.3125(6) 0.149(5) Uani 1 1 d D U . . .
H44 H 0.6814 -0.0214 0.3057 0.179 Uiso 1 1 calc R U . . .
C45 C 0.6575(13) 0.0958(11) 0.2800(9) 0.208(8) Uani 1 1 d D U . . .
H45A H 0.6394 0.1403 0.3018 0.311 Uiso 1 1 calc R U . . .
H45B H 0.6305 0.0937 0.2303 0.311 Uiso 1 1 calc R U . . .
H45C H 0.7090 0.1041 0.2857 0.311 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 2.070(4) . ?
Ti1 O3 1.772(4) . ?
Ti1 O4 1.892(3) . ?
Ti1 O14 1.869(3) . ?
Ti1 O20 2.095(4) 3_666 ?
Ti1 N1 2.227(4) . ?
Ti2 O4 1.864(4) . ?
Ti2 O6 2.067(4) . ?
Ti2 O7 1.778(4) . ?
Ti2 O8 1.887(3) . ?
Ti2 O18 2.067(4) 3_666 ?
Ti2 N2 2.233(4) . ?
Ti3 O8 1.870(3) . ?
Ti3 O10 2.049(4) . ?
Ti3 O11 1.787(4) . ?
Ti3 O12 1.890(3) . ?
Ti3 O21 2.095(4) . ?
Ti3 N3 2.238(4) . ?
Ti4 O12 2.061(3) . ?
Ti4 O13 1.798(4) . ?
Ti4 O14 2.086(3) . ?
Ti4 O15 1.898(4) . ?
Ti4 O16 1.888(3) . ?
Ti4 O22 2.149(4) . ?
Ti5 Ti1 2.9636(13) 3_666 ?
Ti5 Ti4 3.1714(13) 3_666 ?
Ti5 Ti7 3.0834(11) 3_666 ?
Ti5 O12 1.975(4) . ?
Ti5 O14 1.997(4) 3_666 ?
Ti5 O20 1.873(3) . ?
Ti5 O21 1.867(3) . ?
Ti5 O22 2.015(3) . ?
Ti5 O22 2.024(3) 3_666 ?
Ti6 Ti1 3.1793(14) 3_666 ?
Ti6 Ti2 3.0942(14) 3_666 ?
Ti6 O4 2.175(4) 3_666 ?
Ti6 O16 1.805(4) . ?
Ti6 O18 1.917(4) . ?
Ti6 O19 1.810(3) . ?
Ti6 O20 1.976(3) . ?
Ti6 O22 2.420(3) . ?
Ti7 Ti2 3.1303(14) 3_666 ?
Ti7 Ti3 3.1432(13) 3_666 ?
Ti7 O8 2.192(4) 3_666 ?
Ti7 O15 1.804(4) . ?
Ti7 O17 1.789(4) . ?
Ti7 O18 1.927(3) . ?
Ti7 O21 1.968(3) 3_666 ?
Ti7 O22 2.348(3) . ?
O1 C6 1.288(7) . ?
O2 C6 1.226(7) . ?
O3 C20 1.420(10) . ?
O4 Ti6 2.176(4) 3_666 ?
O5 C12 1.217(7) . ?
O6 C12 1.303(6) . ?
O7 C23 1.421(8) . ?
O8 Ti7 2.192(4) 3_666 ?
O9 C18 1.222(7) . ?
O10 C18 1.282(7) . ?
O11 C26 1.425(8) . ?
O13 C29 1.410(7) . ?
O14 Ti5 1.997(4) 3_666 ?
O17 C35 1.414(7) . ?
O18 Ti2 2.067(4) 3_666 ?
O19 C32 1.430(8) . ?
O20 Ti1 2.095(4) 3_666 ?
O21 Ti7 1.968(3) 3_666 ?
O22 Ti5 2.024(3) 3_666 ?
O23 H23A 0.8400 . ?
O23 C44 1.429(8) . ?
N1 C1 1.337(7) . ?
N1 C5 1.345(7) . ?
N2 C7 1.350(7) . ?
N2 C11 1.347(7) . ?
N3 C13 1.331(7) . ?
N3 C17 1.340(7) . ?
N4 C38 1.11(3) . ?
N5 H5 1.008(19) . ?
N5 C40 1.485(10) . ?
N5 C41 1.502(8) . ?
C1 H1 0.9500 . ?
C1 C2 1.388(8) . ?
C2 H2 0.9500 . ?
C2 C3 1.375(10) . ?
C3 H3 0.9500 . ?
C3 C4 1.393(10) . ?
C4 H4 0.9500 . ?
C4 C5 1.383(8) . ?
C5 C6 1.496(8) . ?
C7 H7 0.9500 . ?
C7 C8 1.386(8) . ?
C8 H8 0.9500 . ?
C8 C9 1.391(9) . ?
C9 H9 0.9500 . ?
C9 C10 1.372(10) . ?
C10 H10 0.9500 . ?
C10 C11 1.384(8) . ?
C11 C12 1.501(8) . ?
C13 H13 0.9500 . ?
C13 C14 1.401(8) . ?
C14 H14 0.9500 . ?
C14 C15 1.371(10) . ?
C15 H15 0.9500 . ?
C15 C16 1.390(10) . ?
C16 H16 0.9500 . ?
C16 C17 1.365(8) . ?
C17 C18 1.509(8) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C20 1.419(15) . ?
C20 H20 1.0000 . ?
C20 C21 1.442(14) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C22 C23 1.522(12) . ?
C23 H23 1.0000 . ?
C23 C24 1.501(10) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C25 C26 1.506(12) . ?
C26 H26 1.0000 . ?
C26 C27 1.484(12) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C28 C29 1.514(9) . ?
C29 H29 1.0000 . ?
C29 C30 1.498(9) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C31 C32 1.381(12) . ?
C32 H32 1.0000 . ?
C32 C33 1.390(12) . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C34 C35 1.524(9) . ?
C35 H35 1.0000 . ?
C35 C36 1.513(9) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C37 C38 1.48(3) . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C39 C40 1.481(12) . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C41 C42 1.509(10) . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C43 C44 1.460(9) . ?
C44 H44 1.0000 . ?
C44 C45 1.437(9) . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O20 84.81(15) . 3_666 ?
O1 Ti1 N1 73.10(15) . . ?
O3 Ti1 O1 94.78(18) . . ?
O3 Ti1 O4 102.44(18) . . ?
O3 Ti1 O14 99.46(17) . . ?
O3 Ti1 O20 178.28(16) . 3_666 ?
O3 Ti1 N1 92.30(19) . . ?
O4 Ti1 O1 87.56(15) . . ?
O4 Ti1 O20 79.22(15) . 3_666 ?
O4 Ti1 N1 156.66(18) . . ?
O14 Ti1 O1 157.57(17) . . ?
O14 Ti1 O4 106.00(15) . . ?
O14 Ti1 O20 80.44(15) . 3_666 ?
O14 Ti1 N1 89.01(15) . . ?
O20 Ti1 N1 85.98(17) 3_666 . ?
O4 Ti2 O6 89.87(15) . . ?
O4 Ti2 O8 104.31(15) . . ?
O4 Ti2 O18 80.96(16) . 3_666 ?
O4 Ti2 N2 160.83(17) . . ?
O6 Ti2 N2 73.54(16) . . ?
O7 Ti2 O4 102.67(18) . . ?
O7 Ti2 O6 93.51(17) . . ?
O7 Ti2 O8 99.09(18) . . ?
O7 Ti2 O18 176.36(16) . 3_666 ?
O7 Ti2 N2 88.17(18) . . ?
O8 Ti2 O6 158.36(17) . . ?
O8 Ti2 O18 80.16(15) . 3_666 ?
O8 Ti2 N2 89.26(15) . . ?
O18 Ti2 O6 86.16(15) 3_666 . ?
O18 Ti2 N2 88.27(16) 3_666 . ?
O8 Ti3 O10 88.19(15) . . ?
O8 Ti3 O12 103.67(15) . . ?
O8 Ti3 O21 80.96(15) . . ?
O8 Ti3 N3 154.77(18) . . ?
O10 Ti3 O21 84.28(16) . . ?
O10 Ti3 N3 73.82(15) . . ?
O11 Ti3 O8 108.70(18) . . ?
O11 Ti3 O10 94.57(18) . . ?
O11 Ti3 O12 98.90(17) . . ?
O11 Ti3 O21 170.26(16) . . ?
O11 Ti3 N3 90.60(18) . . ?
O12 Ti3 O10 158.02(16) . . ?
O12 Ti3 O21 79.51(15) . . ?
O12 Ti3 N3 88.69(15) . . ?
O21 Ti3 N3 79.78(16) . . ?
O12 Ti4 O14 85.11(13) . . ?
O12 Ti4 O22 77.32(14) . . ?
O13 Ti4 O12 101.69(16) . . ?
O13 Ti4 O14 100.91(16) . . ?
O13 Ti4 O15 100.79(17) . . ?
O13 Ti4 O16 101.55(16) . . ?
O13 Ti4 O22 177.67(14) . . ?
O14 Ti4 O22 76.94(13) . . ?
O15 Ti4 O12 157.23(16) . . ?
O15 Ti4 O14 87.15(14) . . ?
O15 Ti4 O22 80.08(15) . . ?
O16 Ti4 O12 87.51(14) . . ?
O16 Ti4 O14 157.35(16) . . ?
O16 Ti4 O15 91.52(15) . . ?
O16 Ti4 O22 80.56(14) . . ?
Ti1 Ti5 Ti4 78.37(3) 3_666 3_666 ?
Ti1 Ti5 Ti7 115.33(4) 3_666 3_666 ?
Ti7 Ti5 Ti4 59.86(3) 3_666 3_666 ?
O12 Ti5 Ti1 145.46(10) . 3_666 ?
O12 Ti5 Ti4 135.31(10) . 3_666 ?
O12 Ti5 Ti7 93.19(10) . 3_666 ?
O12 Ti5 O14 173.78(14) . 3_666 ?
O12 Ti5 O22 82.50(14) . . ?
O12 Ti5 O22 93.28(14) . 3_666 ?
O14 Ti5 Ti1 38.38(9) 3_666 3_666 ?
O14 Ti5 Ti4 40.06(9) 3_666 3_666 ?
O14 Ti5 Ti7 86.66(10) 3_666 3_666 ?
O14 Ti5 O22 81.88(14) 3_666 3_666 ?
O14 Ti5 O22 93.00(14) 3_666 . ?
O20 Ti5 Ti1 44.60(12) . 3_666 ?
O20 Ti5 Ti4 122.87(12) . 3_666 ?
O20 Ti5 Ti7 139.17(11) . 3_666 ?
O20 Ti5 O12 101.05(15) . . ?
O20 Ti5 O14 82.98(15) . 3_666 ?
O20 Ti5 O22 161.84(16) . 3_666 ?
O20 Ti5 O22 87.60(14) . . ?
O21 Ti5 Ti1 107.12(12) . 3_666 ?
O21 Ti5 Ti4 91.42(11) . 3_666 ?
O21 Ti5 Ti7 37.62(10) . 3_666 ?
O21 Ti5 O12 83.21(15) . . ?
O21 Ti5 O14 100.31(15) . 3_666 ?
O21 Ti5 O20 106.16(15) . . ?
O21 Ti5 O22 86.44(14) . 3_666 ?
O21 Ti5 O22 161.82(16) . . ?
O22 Ti5 Ti1 119.72(11) 3_666 3_666 ?
O22 Ti5 Ti1 91.00(10) . 3_666 ?
O22 Ti5 Ti4 42.04(10) 3_666 3_666 ?
O22 Ti5 Ti4 90.87(10) . 3_666 ?
O22 Ti5 Ti7 132.44(9) . 3_666 ?
O22 Ti5 Ti7 49.60(9) 3_666 3_666 ?
O22 Ti5 O22 83.22(13) . 3_666 ?
Ti2 Ti6 Ti1 70.66(3) 3_666 3_666 ?
O4 Ti6 Ti1 35.51(9) 3_666 3_666 ?
O4 Ti6 Ti2 36.42(9) 3_666 3_666 ?
O4 Ti6 O22 86.75(12) 3_666 . ?
O16 Ti6 Ti1 135.37(11) . 3_666 ?
O16 Ti6 Ti2 139.63(12) . 3_666 ?
O16 Ti6 O4 161.67(14) . 3_666 ?
O16 Ti6 O18 100.44(16) . . ?
O16 Ti6 O19 99.47(18) . . ?
O16 Ti6 O20 97.63(16) . . ?
O16 Ti6 O22 75.00(14) . . ?
O18 Ti6 Ti1 109.16(12) . 3_666 ?
O18 Ti6 Ti2 40.83(12) . 3_666 ?
O18 Ti6 O4 77.03(15) . 3_666 ?
O18 Ti6 O20 142.28(16) . . ?
O18 Ti6 O22 78.34(12) . . ?
O19 Ti6 Ti1 106.26(14) . 3_666 ?
O19 Ti6 Ti2 99.72(14) . 3_666 ?
O19 Ti6 O4 98.82(16) . 3_666 ?
O19 Ti6 O18 101.46(16) . . ?
O19 Ti6 O20 107.85(16) . . ?
O19 Ti6 O22 174.26(17) . . ?
O20 Ti6 Ti1 40.00(11) . 3_666 ?
O20 Ti6 Ti2 109.65(12) . 3_666 ?
O20 Ti6 O4 75.51(14) . 3_666 ?
O20 Ti6 O22 74.79(12) . . ?
O22 Ti6 Ti1 79.09(9) . 3_666 ?
O22 Ti6 Ti2 83.91(9) . 3_666 ?
Ti2 Ti7 Ti3 71.51(3) 3_666 3_666 ?
O8 Ti7 Ti2 36.41(9) 3_666 3_666 ?
O8 Ti7 Ti3 35.72(9) 3_666 3_666 ?
O8 Ti7 O22 85.54(13) 3_666 . ?
O15 Ti7 Ti2 139.39(12) . 3_666 ?
O15 Ti7 Ti3 137.45(11) . 3_666 ?
O15 Ti7 O8 162.21(15) . 3_666 ?
O15 Ti7 O18 100.78(16) . . ?
O15 Ti7 O21 98.43(15) . 3_666 ?
O15 Ti7 O22 76.68(14) . . ?
O17 Ti7 Ti2 99.74(13) . 3_666 ?
O17 Ti7 Ti3 101.02(13) . 3_666 ?
O17 Ti7 O8 97.75(16) . 3_666 ?
O17 Ti7 O15 100.00(18) . . ?
O17 Ti7 O18 102.96(15) . . ?
O17 Ti7 O21 102.71(15) . 3_666 ?
O17 Ti7 O22 176.00(16) . . ?
O18 Ti7 Ti2 40.02(11) . 3_666 ?
O18 Ti7 Ti3 109.88(12) . 3_666 ?
O18 Ti7 O8 76.18(15) . 3_666 ?
O18 Ti7 O21 144.51(16) . 3_666 ?
O18 Ti7 O22 80.00(13) . . ?
O21 Ti7 Ti2 111.25(12) 3_666 3_666 ?
O21 Ti7 Ti3 40.80(11) 3_666 3_666 ?
O21 Ti7 O8 76.44(14) 3_666 3_666 ?
O21 Ti7 O22 75.78(13) 3_666 . ?
O22 Ti7 Ti2 84.26(9) . 3_666 ?
O22 Ti7 Ti3 80.31(9) . 3_666 ?
C6 O1 Ti1 123.7(3) . . ?
C20 O3 Ti1 154.4(5) . . ?
Ti1 O4 Ti6 102.58(16) . 3_666 ?
Ti2 O4 Ti1 150.1(2) . . ?
Ti2 O4 Ti6 99.71(16) . 3_666 ?
C12 O6 Ti2 123.3(4) . . ?
C23 O7 Ti2 161.5(4) . . ?
Ti2 O8 Ti7 99.99(16) . 3_666 ?
Ti3 O8 Ti2 154.7(2) . . ?
Ti3 O8 Ti7 101.11(16) . 3_666 ?
C18 O10 Ti3 122.1(3) . . ?
C26 O11 Ti3 144.9(4) . . ?
Ti3 O12 Ti4 157.1(2) . . ?
Ti3 O12 Ti5 100.36(16) . . ?
Ti5 O12 Ti4 101.94(16) . . ?
C29 O13 Ti4 148.7(4) . . ?
Ti1 O14 Ti4 157.6(2) . . ?
Ti1 O14 Ti5 100.06(16) . 3_666 ?
Ti5 O14 Ti4 101.91(15) 3_666 . ?
Ti7 O15 Ti4 114.98(19) . . ?
Ti6 O16 Ti4 117.08(19) . . ?
C35 O17 Ti7 139.5(4) . . ?
Ti6 O18 Ti2 101.85(16) . 3_666 ?
Ti6 O18 Ti7 113.53(16) . . ?
Ti7 O18 Ti2 103.16(16) . 3_666 ?
C32 O19 Ti6 131.5(5) . . ?
Ti5 O20 Ti1 96.51(15) . 3_666 ?
Ti5 O20 Ti6 107.53(16) . . ?
Ti6 O20 Ti1 102.68(16) . 3_666 ?
Ti5 O21 Ti3 96.92(15) . . ?
Ti5 O21 Ti7 106.98(17) . 3_666 ?
Ti7 O21 Ti3 101.33(15) 3_666 . ?
Ti4 O22 Ti6 86.96(11) . . ?
Ti4 O22 Ti7 87.79(12) . . ?
Ti5 O22 Ti4 97.67(14) . . ?
Ti5 O22 Ti4 98.86(14) 3_666 . ?
Ti5 O22 Ti5 96.78(13) . 3_666 ?
Ti5 O22 Ti6 88.39(12) . . ?
Ti5 O22 Ti6 171.60(18) 3_666 . ?
Ti5 O22 Ti7 171.03(18) . . ?
Ti5 O22 Ti7 89.37(12) 3_666 . ?
Ti7 O22 Ti6 84.78(10) . . ?
C44 O23 H23A 109.5 . . ?
C1 N1 Ti1 126.1(4) . . ?
C1 N1 C5 118.7(5) . . ?
C5 N1 Ti1 115.3(3) . . ?
C7 N2 Ti2 126.1(3) . . ?
C11 N2 Ti2 114.8(4) . . ?
C11 N2 C7 118.3(5) . . ?
C13 N3 Ti3 126.5(4) . . ?
C13 N3 C17 119.4(5) . . ?
C17 N3 Ti3 113.2(3) . . ?
C40 N5 H5 106(3) . . ?
C40 N5 C41 116.2(5) . . ?
C41 N5 H5 112(3) . . ?
N1 C1 H1 119.1 . . ?
N1 C1 C2 121.8(6) . . ?
C2 C1 H1 119.1 . . ?
C1 C2 H2 120.3 . . ?
C3 C2 C1 119.4(6) . . ?
C3 C2 H2 120.3 . . ?
C2 C3 H3 120.4 . . ?
C2 C3 C4 119.2(6) . . ?
C4 C3 H3 120.4 . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 118.0(6) . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.9(5) . . ?
N1 C5 C6 114.3(5) . . ?
C4 C5 C6 122.8(5) . . ?
O1 C6 C5 113.3(5) . . ?
O2 C6 O1 125.0(5) . . ?
O2 C6 C5 121.7(5) . . ?
N2 C7 H7 119.1 . . ?
N2 C7 C8 121.9(5) . . ?
C8 C7 H7 119.1 . . ?
C7 C8 H8 120.5 . . ?
C7 C8 C9 119.0(6) . . ?
C9 C8 H8 120.5 . . ?
C8 C9 H9 120.4 . . ?
C10 C9 C8 119.3(6) . . ?
C10 C9 H9 120.4 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 118.9(6) . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 122.6(6) . . ?
N2 C11 C12 114.5(5) . . ?
C10 C11 C12 122.7(5) . . ?
O5 C12 O6 125.0(6) . . ?
O5 C12 C11 121.6(5) . . ?
O6 C12 C11 113.4(4) . . ?
N3 C13 H13 119.6 . . ?
N3 C13 C14 120.7(6) . . ?
C14 C13 H13 119.6 . . ?
C13 C14 H14 120.4 . . ?
C15 C14 C13 119.3(6) . . ?
C15 C14 H14 120.4 . . ?
C14 C15 H15 120.3 . . ?
C14 C15 C16 119.4(6) . . ?
C16 C15 H15 120.3 . . ?
C15 C16 H16 121.0 . . ?
C17 C16 C15 118.0(6) . . ?
C17 C16 H16 121.0 . . ?
N3 C17 C16 123.1(5) . . ?
N3 C17 C18 114.1(5) . . ?
C16 C17 C18 122.8(6) . . ?
O9 C18 O10 125.6(6) . . ?
O9 C18 C17 120.3(5) . . ?
O10 C18 C17 114.1(5) . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C20 C19 H19A 109.5 . . ?
C20 C19 H19B 109.5 . . ?
C20 C19 H19C 109.5 . . ?
O3 C20 H20 104.8 . . ?
O3 C20 C21 112.4(9) . . ?
C19 C20 O3 111.4(9) . . ?
C19 C20 H20 104.8 . . ?
C19 C20 C21 117.3(12) . . ?
C21 C20 H20 104.8 . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21B 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
H22A C22 H22B 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C23 C22 H22A 109.5 . . ?
C23 C22 H22B 109.5 . . ?
C23 C22 H22C 109.5 . . ?
O7 C23 C22 110.0(7) . . ?
O7 C23 H23 108.6 . . ?
O7 C23 C24 109.5(6) . . ?
C22 C23 H23 108.6 . . ?
C24 C23 C22 111.4(7) . . ?
C24 C23 H23 108.6 . . ?
C23 C24 H24A 109.5 . . ?
C23 C24 H24B 109.5 . . ?
C23 C24 H24C 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H25A C25 H25B 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C26 C25 H25A 109.5 . . ?
C26 C25 H25B 109.5 . . ?
C26 C25 H25C 109.5 . . ?
O11 C26 C25 109.4(7) . . ?
O11 C26 H26 107.8 . . ?
O11 C26 C27 110.9(7) . . ?
C25 C26 H26 107.8 . . ?
C27 C26 C25 112.9(8) . . ?
C27 C26 H26 107.8 . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27B 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C29 C28 H28A 109.5 . . ?
C29 C28 H28B 109.5 . . ?
C29 C28 H28C 109.5 . . ?
O13 C29 C28 109.0(5) . . ?
O13 C29 H29 108.0 . . ?
O13 C29 C30 110.1(6) . . ?
C28 C29 H29 108.0 . . ?
C30 C29 C28 113.5(5) . . ?
C30 C29 H29 108.0 . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30B 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
H31A C31 H31B 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C32 C31 H31A 109.5 . . ?
C32 C31 H31B 109.5 . . ?
C32 C31 H31C 109.5 . . ?
O19 C32 H32 93.0 . . ?
C31 C32 O19 115.3(7) . . ?
C31 C32 H32 93.0 . . ?
C31 C32 C33 127.5(9) . . ?
C33 C32 O19 116.4(7) . . ?
C33 C32 H32 93.0 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33B 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
H34A C34 H34B 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C35 C34 H34A 109.5 . . ?
C35 C34 H34B 109.5 . . ?
C35 C34 H34C 109.5 . . ?
O17 C35 C34 109.1(5) . . ?
O17 C35 H35 108.8 . . ?
O17 C35 C36 109.6(5) . . ?
C34 C35 H35 108.8 . . ?
C36 C35 C34 111.8(5) . . ?
C36 C35 H35 108.8 . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36B 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
H37A C37 H37B 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C38 C37 H37A 109.5 . . ?
C38 C37 H37B 109.5 . . ?
C38 C37 H37C 109.5 . . ?
N4 C38 C37 176(3) . . ?
H39A C39 H39B 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C40 C39 H39A 109.5 . . ?
C40 C39 H39B 109.5 . . ?
C40 C39 H39C 109.5 . . ?
N5 C40 H40A 109.0 . . ?
N5 C40 H40B 109.0 . . ?
C39 C40 N5 112.7(7) . . ?
C39 C40 H40A 109.0 . . ?
C39 C40 H40B 109.0 . . ?
H40A C40 H40B 107.8 . . ?
N5 C41 H41A 109.1 . . ?
N5 C41 H41B 109.1 . . ?
N5 C41 C42 112.3(6) . . ?
H41A C41 H41B 107.9 . . ?
C42 C41 H41A 109.1 . . ?
C42 C41 H41B 109.1 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42B 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
H43A C43 H43B 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C44 C43 H43A 109.5 . . ?
C44 C43 H43B 109.5 . . ?
C44 C43 H43C 109.5 . . ?
O23 C44 C43 113.9(11) . . ?
O23 C44 H44 112.1 . . ?
O23 C44 C45 104.3(13) . . ?
C43 C44 H44 112.1 . . ?
C45 C44 C43 101.6(16) . . ?
C45 C44 H44 112.1 . . ?
C44 C45 H45A 109.5 . . ?
C44 C45 H45B 109.5 . . ?
C44 C45 H45C 109.5 . . ?
H45A C45 H45B 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 Ti5 O20 Ti6 105.5(2) 3_666 . . . ?
Ti1 Ti5 O21 Ti3 146.38(9) 3_666 . . . ?
Ti1 Ti5 O21 Ti7 -109.50(14) 3_666 . . 3_666 ?
Ti1 Ti6 O16 Ti4 -62.0(3) 3_666 . . . ?
Ti1 Ti6 O19 C32 176.2(7) 3_666 . . . ?
Ti1 O1 C6 O2 176.0(6) . . . . ?
Ti1 O1 C6 C5 -5.8(8) . . . . ?
Ti1 O3 C20 C19 -133.1(13) . . . . ?
Ti1 O3 C20 C21 93.1(14) . . . . ?
Ti1 N1 C1 C2 -179.9(5) . . . . ?
Ti1 N1 C5 C4 180.0(6) . . . . ?
Ti1 N1 C5 C6 0.8(7) . . . . ?
Ti2 Ti6 O16 Ti4 55.6(3) 3_666 . . . ?
Ti2 Ti6 O19 C32 103.6(7) 3_666 . . . ?
Ti2 Ti7 O15 Ti4 -58.4(2) 3_666 . . . ?
Ti2 Ti7 O17 C35 -130.6(5) 3_666 . . . ?
Ti2 O6 C12 O5 176.4(5) . . . . ?
Ti2 O6 C12 C11 -2.2(7) . . . . ?
Ti2 O7 C23 C22 60.8(15) . . . . ?
Ti2 O7 C23 C24 -62.0(16) . . . . ?
Ti2 N2 C7 C8 168.1(5) . . . . ?
Ti2 N2 C11 C10 -169.2(5) . . . . ?
Ti2 N2 C11 C12 6.7(7) . . . . ?
Ti3 Ti7 O15 Ti4 64.9(2) 3_666 . . . ?
Ti3 Ti7 O17 C35 156.5(5) 3_666 . . . ?
Ti3 O10 C18 O9 -168.3(6) . . . . ?
Ti3 O10 C18 C17 13.4(8) . . . . ?
Ti3 O11 C26 C25 -82.3(9) . . . . ?
Ti3 O11 C26 C27 152.6(6) . . . . ?
Ti3 N3 C13 C14 -168.4(5) . . . . ?
Ti3 N3 C17 C16 169.8(5) . . . . ?
Ti3 N3 C17 C18 -11.4(7) . . . . ?
Ti4 Ti5 O20 Ti1 -4.38(17) 3_666 . . 3_666 ?
Ti4 Ti5 O20 Ti6 101.15(16) 3_666 . . . ?
Ti4 Ti5 O21 Ti3 -135.36(10) 3_666 . . . ?
Ti4 Ti5 O21 Ti7 -31.23(16) 3_666 . . 3_666 ?
Ti4 O13 C29 C28 -72.5(9) . . . . ?
Ti4 O13 C29 C30 52.6(9) . . . . ?
Ti6 O19 C32 C31 120.6(10) . . . . ?
Ti6 O19 C32 C33 -49.9(14) . . . . ?
Ti7 Ti5 O20 Ti1 76.0(2) 3_666 . . 3_666 ?
Ti7 Ti5 O20 Ti6 -178.44(7) 3_666 . . . ?
Ti7 Ti5 O21 Ti3 -104.1(2) 3_666 . . . ?
Ti7 O17 C35 C34 84.9(7) . . . . ?
Ti7 O17 C35 C36 -152.3(5) . . . . ?
O1 Ti1 O3 C20 -131.6(11) . . . . ?
O1 Ti1 O4 Ti2 -138.2(4) . . . . ?
O1 Ti1 O4 Ti6 84.62(17) . . . 3_666 ?
O1 Ti1 O14 Ti4 142.3(5) . . . . ?
O1 Ti1 O14 Ti5 -49.0(5) . . . 3_666 ?
O3 Ti1 O4 Ti2 -43.8(4) . . . . ?
O3 Ti1 O4 Ti6 178.98(16) . . . 3_666 ?
O3 Ti1 O14 Ti4 13.6(5) . . . . ?
O3 Ti1 O14 Ti5 -177.70(16) . . . 3_666 ?
O4 Ti1 O3 C20 139.9(11) . . . . ?
O4 Ti1 O14 Ti4 -92.3(5) . . . . ?
O4 Ti1 O14 Ti5 76.34(18) . . . 3_666 ?
O4 Ti2 O7 C23 168.4(13) . . . . ?
O4 Ti2 O8 Ti3 63.1(5) . . . . ?
O4 Ti2 O8 Ti7 -83.07(17) . . . 3_666 ?
O4 Ti6 O16 Ti4 -10.8(6) 3_666 . . . ?
O4 Ti6 O19 C32 140.5(7) 3_666 . . . ?
O6 Ti2 O4 Ti1 141.1(4) . . . . ?
O6 Ti2 O4 Ti6 -81.21(16) . . . 3_666 ?
O6 Ti2 O7 C23 77.8(13) . . . . ?
O6 Ti2 O8 Ti3 -167.4(4) . . . . ?
O6 Ti2 O8 Ti7 46.5(5) . . . 3_666 ?
O7 Ti2 O4 Ti1 47.5(4) . . . . ?
O7 Ti2 O4 Ti6 -174.78(15) . . . 3_666 ?
O7 Ti2 O8 Ti3 -42.6(5) . . . . ?
O7 Ti2 O8 Ti7 171.26(16) . . . 3_666 ?
O8 Ti2 O4 Ti1 -55.5(4) . . . . ?
O8 Ti2 O4 Ti6 82.26(17) . . . 3_666 ?
O8 Ti2 O7 C23 -84.5(13) . . . . ?
O8 Ti3 O11 C26 176.6(7) . . . . ?
O8 Ti3 O12 Ti4 88.5(5) . . . . ?
O8 Ti3 O12 Ti5 -77.77(18) . . . . ?
O8 Ti7 O15 Ti4 7.3(6) 3_666 . . . ?
O8 Ti7 O17 C35 -167.4(5) 3_666 . . . ?
O10 Ti3 O8 Ti2 132.4(5) . . . . ?
O10 Ti3 O8 Ti7 -81.57(17) . . . 3_666 ?
O10 Ti3 O11 C26 86.9(8) . . . . ?
O10 Ti3 O12 Ti4 -150.4(4) . . . . ?
O10 Ti3 O12 Ti5 43.3(5) . . . . ?
O11 Ti3 O8 Ti2 38.2(5) . . . . ?
O11 Ti3 O8 Ti7 -175.79(16) . . . 3_666 ?
O11 Ti3 O12 Ti4 -23.3(5) . . . . ?
O11 Ti3 O12 Ti5 170.39(16) . . . . ?
O12 Ti3 O8 Ti2 -66.3(5) . . . . ?
O12 Ti3 O8 Ti7 79.72(17) . . . 3_666 ?
O12 Ti3 O11 C26 -75.6(8) . . . . ?
O12 Ti4 O13 C29 141.6(7) . . . . ?
O12 Ti4 O15 Ti7 -13.4(5) . . . . ?
O12 Ti4 O16 Ti6 83.5(2) . . . . ?
O12 Ti5 O20 Ti1 -175.74(13) . . . 3_666 ?
O12 Ti5 O20 Ti6 -70.21(19) . . . . ?
O12 Ti5 O21 Ti3 0.15(13) . . . . ?
O12 Ti5 O21 Ti7 104.27(18) . . . 3_666 ?
O13 Ti4 O15 Ti7 175.89(18) . . . . ?
O13 Ti4 O16 Ti6 -175.06(19) . . . . ?
O14 Ti1 O3 C20 31.0(11) . . . . ?
O14 Ti1 O4 Ti2 60.0(4) . . . . ?
O14 Ti1 O4 Ti6 -77.23(18) . . . 3_666 ?
O14 Ti4 O13 C29 -131.2(7) . . . . ?
O14 Ti4 O15 Ti7 -83.54(19) . . . . ?
O14 Ti4 O16 Ti6 12.5(5) . . . . ?
O14 Ti5 O20 Ti1 -0.55(13) 3_666 . . 3_666 ?
O14 Ti5 O20 Ti6 104.98(18) 3_666 . . . ?
O14 Ti5 O21 Ti3 -174.67(13) 3_666 . . . ?
O14 Ti5 O21 Ti7 -70.54(19) 3_666 . . 3_666 ?
O15 Ti4 O13 C29 -42.0(7) . . . . ?
O15 Ti4 O16 Ti6 -73.7(2) . . . . ?
O15 Ti7 O17 C35 13.7(6) . . . . ?
O16 Ti4 O13 C29 51.8(7) . . . . ?
O16 Ti4 O15 Ti7 73.8(2) . . . . ?
O16 Ti6 O19 C32 -40.7(7) . . . . ?
O17 Ti7 O15 Ti4 -176.44(18) . . . . ?
O18 Ti2 O4 Ti1 -132.8(4) 3_666 . . . ?
O18 Ti2 O4 Ti6 4.92(13) 3_666 . . 3_666 ?
O18 Ti2 O8 Ti3 141.0(5) 3_666 . . . ?
O18 Ti2 O8 Ti7 -5.13(13) 3_666 . . 3_666 ?
O18 Ti6 O16 Ti4 69.4(2) . . . . ?
O18 Ti6 O19 C32 62.1(7) . . . . ?
O18 Ti7 O15 Ti4 -71.05(19) . . . . ?
O18 Ti7 O17 C35 -89.9(5) . . . . ?
O19 Ti6 O16 Ti4 173.0(2) . . . . ?
O20 Ti1 O4 Ti2 136.7(4) 3_666 . . . ?
O20 Ti1 O4 Ti6 -0.56(13) 3_666 . . 3_666 ?
O20 Ti1 O14 Ti4 -168.1(5) 3_666 . . . ?
O20 Ti1 O14 Ti5 0.56(14) 3_666 . . 3_666 ?
O20 Ti5 O21 Ti3 99.72(16) . . . . ?
O20 Ti5 O21 Ti7 -156.15(17) . . . 3_666 ?
O20 Ti6 O16 Ti4 -77.3(2) . . . . ?
O20 Ti6 O19 C32 -141.9(7) . . . . ?
O21 Ti3 O8 Ti2 -143.1(5) . . . . ?
O21 Ti3 O8 Ti7 2.92(14) . . . 3_666 ?
O21 Ti3 O12 Ti4 166.5(5) . . . . ?
O21 Ti3 O12 Ti5 0.15(13) . . . . ?
O21 Ti5 O20 Ti1 98.21(16) . . . 3_666 ?
O21 Ti5 O20 Ti6 -156.26(17) . . . . ?
O21 Ti7 O15 Ti4 78.96(19) 3_666 . . . ?
O21 Ti7 O17 C35 114.8(5) 3_666 . . . ?
O22 Ti4 O15 Ti7 -6.31(17) . . . . ?
O22 Ti4 O16 Ti6 5.96(18) . . . . ?
O22 Ti5 O20 Ti1 -93.87(15) . . . 3_666 ?
O22 Ti5 O20 Ti1 -34.3(5) 3_666 . . 3_666 ?
O22 Ti5 O20 Ti6 11.67(18) . . . . ?
O22 Ti5 O20 Ti6 71.2(5) 3_666 . . . ?
O22 Ti5 O21 Ti3 -93.59(15) 3_666 . . . ?
O22 Ti5 O21 Ti3 -38.2(5) . . . . ?
O22 Ti5 O21 Ti7 65.9(5) . . . 3_666 ?
O22 Ti5 O21 Ti7 10.54(18) 3_666 . . 3_666 ?
O22 Ti6 O16 Ti4 -5.40(16) . . . . ?
O22 Ti7 O15 Ti4 5.84(15) . . . . ?
N1 Ti1 O3 C20 -58.3(11) . . . . ?
N1 Ti1 O4 Ti2 -171.8(4) . . . . ?
N1 Ti1 O4 Ti6 51.0(5) . . . 3_666 ?
N1 Ti1 O14 Ti4 105.8(5) . . . . ?
N1 Ti1 O14 Ti5 -85.54(18) . . . 3_666 ?
N1 C1 C2 C3 -0.5(12) . . . . ?
N1 C5 C6 O1 2.8(9) . . . . ?
N1 C5 C6 O2 -178.9(7) . . . . ?
N2 Ti2 O4 Ti1 170.6(4) . . . . ?
N2 Ti2 O4 Ti6 -51.6(6) . . . 3_666 ?
N2 Ti2 O7 C23 4.4(13) . . . . ?
N2 Ti2 O8 Ti3 -130.6(5) . . . . ?
N2 Ti2 O8 Ti7 83.24(17) . . . 3_666 ?
N2 C7 C8 C9 0.7(12) . . . . ?
N2 C11 C12 O5 178.0(6) . . . . ?
N2 C11 C12 O6 -3.4(8) . . . . ?
N3 Ti3 O8 Ti2 176.3(4) . . . . ?
N3 Ti3 O8 Ti7 -37.7(4) . . . 3_666 ?
N3 Ti3 O11 C26 13.1(8) . . . . ?
N3 Ti3 O12 Ti4 -113.7(5) . . . . ?
N3 Ti3 O12 Ti5 79.99(17) . . . . ?
N3 C13 C14 C15 0.2(11) . . . . ?
N3 C17 C18 O9 -178.3(6) . . . . ?
N3 C17 C18 O10 0.1(8) . . . . ?
C1 N1 C5 C4 0.2(10) . . . . ?
C1 N1 C5 C6 -178.9(6) . . . . ?
C1 C2 C3 C4 1.2(13) . . . . ?
C2 C3 C4 C5 -1.1(14) . . . . ?
C3 C4 C5 N1 0.4(13) . . . . ?
C3 C4 C5 C6 179.5(8) . . . . ?
C4 C5 C6 O1 -176.3(7) . . . . ?
C4 C5 C6 O2 2.0(12) . . . . ?
C5 N1 C1 C2 -0.1(10) . . . . ?
C7 N2 C11 C10 1.3(9) . . . . ?
C7 N2 C11 C12 177.2(6) . . . . ?
C7 C8 C9 C10 -0.2(12) . . . . ?
C8 C9 C10 C11 0.3(12) . . . . ?
C9 C10 C11 N2 -0.8(11) . . . . ?
C9 C10 C11 C12 -176.4(7) . . . . ?
C10 C11 C12 O5 -6.1(10) . . . . ?
C10 C11 C12 O6 172.6(6) . . . . ?
C11 N2 C7 C8 -1.2(10) . . . . ?
C13 N3 C17 C16 -0.1(10) . . . . ?
C13 N3 C17 C18 178.7(5) . . . . ?
C13 C14 C15 C16 -0.4(12) . . . . ?
C14 C15 C16 C17 0.4(12) . . . . ?
C15 C16 C17 N3 -0.1(11) . . . . ?
C15 C16 C17 C18 -178.8(7) . . . . ?
C16 C17 C18 O9 0.5(11) . . . . ?
C16 C17 C18 O10 178.9(6) . . . . ?
C17 N3 C13 C14 0.0(9) . . . . ?
C40 N5 C41 C42 -62.6(8) . . . . ?
C41 N5 C40 C39 -64.5(9) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.020
_oxdiff_exptl_absorpt_empirical_full_min 0.588
####################################################################### 
# 
# 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_ti6pa8
_database_code_depnum_ccdc_archive 'CCDC 2126645'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2022-01-27 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2022-01-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C60 H60 N12 O28 Ti6'
_chemical_formula_sum            'C60 H60 N12 O28 Ti6'
_chemical_formula_weight         1684.60
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           82
_space_group_name_H-M_alt        'I -4'
_space_group_name_Hall           'I -4'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'y, -x, -z'
'-y, x, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'

_cell_length_a                   15.2721(2)
_cell_length_b                   15.2721(2)
_cell_length_c                   15.8807(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3703.97(12)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3839
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.0110
_cell_measurement_theta_min      3.9850
_shelx_estimated_absorpt_T_max   0.753
_shelx_estimated_absorpt_T_min   0.645
_exptl_absorpt_coefficient_mu    6.016
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.74029
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.928
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            5116
_diffrn_reflns_point_group_measured_fraction_full 0.855
_diffrn_reflns_point_group_measured_fraction_max 0.793
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.164
_diffrn_reflns_theta_min         4.016
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    150.00 178.00   1.00    0.35    --  106.49 125.00 -30.00   28
  2  ω     99.00 146.00   1.00    0.35    --  106.49 125.00 -30.00   47
  3  ω     93.00 178.00   1.00    0.35    --  106.49  25.00  91.00   85
  4  ω     37.00  66.00   1.00    0.35    --  106.49 -57.00 120.00   29
  5  ω     34.00  64.00   1.00    0.35    --  106.49 -57.00-150.00   30
  6  ω   -123.00 -36.00   1.00    0.10    --  -48.45 -25.00 -71.00   87
  7  ω    -41.00 -13.00   1.00    0.35    --  -86.25  38.00  90.00   28
  8  ω    -80.00 -13.00   1.00    0.35    --  -86.25  98.00-115.00   67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0935413000
_diffrn_orient_matrix_UB_12      -0.0182855000
_diffrn_orient_matrix_UB_13      0.0317631000
_diffrn_orient_matrix_UB_21      -0.0172815000
_diffrn_orient_matrix_UB_22      0.0990747000
_diffrn_orient_matrix_UB_23      0.0055542000
_diffrn_orient_matrix_UB_31      -0.0335046000
_diffrn_orient_matrix_UB_32      -0.0001001000
_diffrn_orient_matrix_UB_33      -0.0916438000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.642
_reflns_Friedel_fraction_full    0.718
_reflns_Friedel_fraction_max     0.646
_reflns_number_gt                2921
_reflns_number_total             3062
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details 
;
 Flack x determined using 1081 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.010(6)
_refine_ls_extinction_coef       0.00026(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3062
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0312
_refine_ls_R_factor_gt           0.0301
_refine_ls_restrained_S_all      1.013
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0753
_refine_ls_wR_factor_ref         0.0757
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15)
2.b Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C14(H14A,H14B,H14C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.5000 0.5000 0.72772(5) 0.02097(19) Uani 1 2 d S T P . .
Ti2 Ti 0.64275(4) 0.48005(4) 0.55357(3) 0.01941(15) Uani 1 1 d . . . . .
O1 O 0.58704(18) 0.47569(18) 0.65681(14) 0.0280(6) Uani 1 1 d . . . . .
O2 O 0.58138(15) 0.40217(15) 0.49286(15) 0.0240(5) Uani 1 1 d . . . . .
O3 O 0.53829(17) 0.61993(16) 0.76049(15) 0.0257(5) Uani 1 1 d . . . . .
O4 O 0.5269(2) 0.7389(2) 0.84190(19) 0.0414(7) Uani 1 1 d . . . . .
O5 O 0.73160(17) 0.38627(17) 0.58756(15) 0.0262(5) Uani 1 1 d . . . . .
O6 O 0.8551(2) 0.3126(2) 0.56127(19) 0.0401(7) Uani 1 1 d . . . . .
O7 O 0.74052(17) 0.56210(19) 0.61522(16) 0.0299(6) Uani 1 1 d . . . . .
N1 N 0.4099(2) 0.5406(2) 0.83581(17) 0.0240(6) Uani 1 1 d . . . . .
N2 N 0.74864(19) 0.4857(2) 0.45640(18) 0.0239(6) Uani 1 1 d . . . . .
N3 N 0.7697(2) 0.6705(2) 0.70816(19) 0.0306(7) Uani 1 1 d . . . . .
C1 C 0.3410(3) 0.4981(3) 0.8682(2) 0.0316(8) Uani 1 1 d . . . . .
H1 H 0.3287 0.4405 0.8488 0.038 Uiso 1 1 calc R U . . .
C2 C 0.2870(3) 0.5344(3) 0.9286(3) 0.0383(10) Uani 1 1 d . . . . .
H2 H 0.2382 0.5028 0.9498 0.046 Uiso 1 1 calc R U . . .
C3 C 0.3056(3) 0.6183(3) 0.9577(3) 0.0398(10) Uani 1 1 d . . . . .
H3 H 0.2702 0.6446 0.9998 0.048 Uiso 1 1 calc R U . . .
C4 C 0.3765(3) 0.6628(3) 0.9244(2) 0.0348(9) Uani 1 1 d . . . . .
H4 H 0.3906 0.7201 0.9432 0.042 Uiso 1 1 calc R U . . .
C5 C 0.4264(3) 0.6222(2) 0.8631(2) 0.0265(7) Uani 1 1 d . . . . .
C6 C 0.5030(3) 0.6663(3) 0.8206(2) 0.0285(8) Uani 1 1 d . . . . .
C7 C 0.7534(3) 0.5408(3) 0.3912(2) 0.0323(9) Uani 1 1 d . . . . .
H7 H 0.7099 0.5848 0.3849 0.039 Uiso 1 1 calc R U . . .
C8 C 0.8204(3) 0.5353(3) 0.3328(3) 0.0422(10) Uani 1 1 d . . . . .
H8 H 0.8226 0.5744 0.2862 0.051 Uiso 1 1 calc R U . . .
C9 C 0.8843(3) 0.4715(3) 0.3435(3) 0.0459(11) Uani 1 1 d . . . . .
H9 H 0.9301 0.4658 0.3034 0.055 Uiso 1 1 calc R U . . .
C10 C 0.8812(3) 0.4169(3) 0.4118(3) 0.0382(9) Uani 1 1 d . . . . .
H10 H 0.9254 0.3741 0.4208 0.046 Uiso 1 1 calc R U . . .
C11 C 0.8120(2) 0.4259(2) 0.4675(2) 0.0255(7) Uani 1 1 d . . . . .
C12 C 0.8003(2) 0.3690(2) 0.5448(2) 0.0258(7) Uani 1 1 d . . . . .
C13 C 0.8579(3) 0.6376(4) 0.7262(3) 0.0457(11) Uani 1 1 d . . . . .
H13A H 0.8557 0.5984 0.7750 0.069 Uiso 1 1 calc R U . . .
H13B H 0.8969 0.6869 0.7384 0.069 Uiso 1 1 calc R U . . .
H13C H 0.8800 0.6054 0.6772 0.069 Uiso 1 1 calc R U . . .
C14 C 0.7392(3) 0.7477(3) 0.7538(3) 0.0405(10) Uani 1 1 d . . . . .
H14A H 0.6783 0.7600 0.7382 0.061 Uiso 1 1 calc R U . . .
H14B H 0.7759 0.7981 0.7392 0.061 Uiso 1 1 calc R U . . .
H14C H 0.7427 0.7368 0.8145 0.061 Uiso 1 1 calc R U . . .
C15 C 0.7185(2) 0.6297(2) 0.6548(2) 0.0267(7) Uani 1 1 d . . . . .
H15 H 0.6615 0.6526 0.6456 0.032 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.781(3) 2_665 ?
Ti1 O1 1.781(3) . ?
Ti1 O3 1.992(3) . ?
Ti1 O3 1.992(3) 2_665 ?
Ti1 N1 2.286(3) . ?
Ti1 N1 2.286(3) 2_665 ?
Ti2 O1 1.848(2) . ?
Ti2 O2 1.795(2) . ?
Ti2 O2 1.846(2) 4_656 ?
Ti2 O5 2.045(3) . ?
Ti2 O7 2.181(3) . ?
Ti2 N2 2.237(3) . ?
O2 Ti2 1.846(2) 3_566 ?
O3 C6 1.305(5) . ?
O4 C6 1.215(5) . ?
O5 C12 1.277(5) . ?
O6 C12 1.230(5) . ?
O7 C15 1.254(5) . ?
N1 C1 1.340(5) . ?
N1 C5 1.343(5) . ?
N2 C7 1.337(5) . ?
N2 C11 1.341(5) . ?
N3 C13 1.466(6) . ?
N3 C14 1.460(6) . ?
N3 C15 1.311(5) . ?
C1 H1 0.9500 . ?
C1 C2 1.381(6) . ?
C2 H2 0.9500 . ?
C2 C3 1.391(7) . ?
C3 H3 0.9500 . ?
C3 C4 1.383(6) . ?
C4 H4 0.9500 . ?
C4 C5 1.382(5) . ?
C5 C6 1.509(5) . ?
C7 H7 0.9500 . ?
C7 C8 1.384(6) . ?
C8 H8 0.9500 . ?
C8 C9 1.390(7) . ?
C9 H9 0.9500 . ?
C9 C10 1.369(7) . ?
C10 H10 0.9500 . ?
C10 C11 1.385(5) . ?
C11 C12 1.516(5) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15 0.9500 . ?

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 O1 101.57(16) 2_665 . ?
O1 Ti1 O3 101.11(12) . 2_665 ?
O1 Ti1 O3 97.92(12) . . ?
O1 Ti1 O3 97.92(12) 2_665 2_665 ?
O1 Ti1 O3 101.11(12) 2_665 . ?
O1 Ti1 N1 168.68(12) 2_665 2_665 ?
O1 Ti1 N1 168.68(12) . . ?
O1 Ti1 N1 88.23(11) 2_665 . ?
O1 Ti1 N1 88.23(11) . 2_665 ?
O3 Ti1 O3 149.71(15) 2_665 . ?
O3 Ti1 N1 74.39(11) . . ?
O3 Ti1 N1 82.91(11) . 2_665 ?
O3 Ti1 N1 74.39(11) 2_665 2_665 ?
O3 Ti1 N1 82.91(11) 2_665 . ?
N1 Ti1 N1 82.64(15) 2_665 . ?
O1 Ti2 O5 92.64(11) . . ?
O1 Ti2 O7 86.43(12) . . ?
O1 Ti2 N2 161.10(12) . . ?
O2 Ti2 O1 102.32(12) 4_656 . ?
O2 Ti2 O1 102.25(12) . . ?
O2 Ti2 O2 98.44(13) . 4_656 ?
O2 Ti2 O5 159.84(11) 4_656 . ?
O2 Ti2 O5 91.38(11) . . ?
O2 Ti2 O7 87.25(11) 4_656 . ?
O2 Ti2 O7 168.25(11) . . ?
O2 Ti2 N2 87.77(11) 4_656 . ?
O2 Ti2 N2 91.85(11) . . ?
O5 Ti2 O7 80.20(11) . . ?
O5 Ti2 N2 74.29(11) . . ?
O7 Ti2 N2 78.04(11) . . ?
Ti1 O1 Ti2 153.74(16) . . ?
Ti2 O2 Ti2 153.93(15) . 3_566 ?
C6 O3 Ti1 124.7(2) . . ?
C12 O5 Ti2 123.3(2) . . ?
C15 O7 Ti2 120.9(2) . . ?
C1 N1 Ti1 129.0(2) . . ?
C1 N1 C5 118.2(3) . . ?
C5 N1 Ti1 112.4(2) . . ?
C7 N2 Ti2 126.7(3) . . ?
C7 N2 C11 119.4(3) . . ?
C11 N2 Ti2 113.9(2) . . ?
C14 N3 C13 118.3(3) . . ?
C15 N3 C13 120.8(3) . . ?
C15 N3 C14 120.9(4) . . ?
N1 C1 H1 118.6 . . ?
N1 C1 C2 122.7(4) . . ?
C2 C1 H1 118.6 . . ?
C1 C2 H2 120.7 . . ?
C1 C2 C3 118.6(4) . . ?
C3 C2 H2 120.7 . . ?
C2 C3 H3 120.5 . . ?
C4 C3 C2 119.0(4) . . ?
C4 C3 H3 120.5 . . ?
C3 C4 H4 120.6 . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 H4 120.6 . . ?
N1 C5 C4 122.7(4) . . ?
N1 C5 C6 114.5(3) . . ?
C4 C5 C6 122.9(4) . . ?
O3 C6 C5 113.9(3) . . ?
O4 C6 O3 125.1(4) . . ?
O4 C6 C5 121.0(3) . . ?
N2 C7 H7 119.3 . . ?
N2 C7 C8 121.4(4) . . ?
C8 C7 H7 119.3 . . ?
C7 C8 H8 120.7 . . ?
C7 C8 C9 118.6(4) . . ?
C9 C8 H8 120.7 . . ?
C8 C9 H9 120.0 . . ?
C10 C9 C8 120.0(4) . . ?
C10 C9 H9 120.0 . . ?
C9 C10 H10 120.9 . . ?
C9 C10 C11 118.2(4) . . ?
C11 C10 H10 120.9 . . ?
N2 C11 C10 122.3(4) . . ?
N2 C11 C12 114.3(3) . . ?
C10 C11 C12 123.4(3) . . ?
O5 C12 C11 114.2(3) . . ?
O6 C12 O5 126.3(4) . . ?
O6 C12 C11 119.6(3) . . ?
N3 C13 H13A 109.5 . . ?
N3 C13 H13B 109.5 . . ?
N3 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N3 C14 H14A 109.5 . . ?
N3 C14 H14B 109.5 . . ?
N3 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O7 C15 N3 123.7(4) . . ?
O7 C15 H15 118.1 . . ?
N3 C15 H15 118.1 . . ?

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
Ti1 O3 C6 O4 178.8(3) . . . . ?
Ti1 O3 C6 C5 -2.1(4) . . . . ?
Ti1 N1 C1 C2 -173.6(3) . . . . ?
Ti1 N1 C5 C4 175.8(3) . . . . ?
Ti1 N1 C5 C6 -3.4(4) . . . . ?
Ti2 O5 C12 O6 -178.7(3) . . . . ?
Ti2 O5 C12 C11 1.6(4) . . . . ?
Ti2 O7 C15 N3 164.2(3) . . . . ?
Ti2 N2 C7 C8 -176.9(3) . . . . ?
Ti2 N2 C11 C10 177.4(3) . . . . ?
Ti2 N2 C11 C12 -1.8(4) . . . . ?
O1 Ti1 O1 Ti2 21.0(3) 2_665 . . . ?
O1 Ti2 O2 Ti2 56.7(4) . . . 3_566 ?
O2 Ti2 O1 Ti1 25.3(4) 4_656 . . . ?
O2 Ti2 O1 Ti1 -76.3(4) . . . . ?
O2 Ti2 O2 Ti2 -47.9(3) 4_656 . . 3_566 ?
O3 Ti1 O1 Ti2 -82.1(4) . . . . ?
O3 Ti1 O1 Ti2 121.6(4) 2_665 . . . ?
O5 Ti2 O1 Ti1 -168.3(4) . . . . ?
O5 Ti2 O2 Ti2 149.7(3) . . . 3_566 ?
O7 Ti2 O1 Ti1 111.7(4) . . . . ?
O7 Ti2 O2 Ti2 -166.3(4) . . . 3_566 ?
N1 Ti1 O1 Ti2 -164.7(4) 2_665 . . . ?
N1 Ti1 O1 Ti2 -128.5(5) . . . . ?
N1 C1 C2 C3 -0.8(7) . . . . ?
N1 C5 C6 O3 3.7(5) . . . . ?
N1 C5 C6 O4 -177.1(4) . . . . ?
N2 Ti2 O1 Ti1 146.3(3) . . . . ?
N2 Ti2 O2 Ti2 -135.9(3) . . . 3_566 ?
N2 C7 C8 C9 -0.9(7) . . . . ?
N2 C11 C12 O5 0.3(5) . . . . ?
N2 C11 C12 O6 -179.4(4) . . . . ?
C1 N1 C5 C4 1.6(5) . . . . ?
C1 N1 C5 C6 -177.6(3) . . . . ?
C1 C2 C3 C4 0.9(7) . . . . ?
C2 C3 C4 C5 0.1(6) . . . . ?
C3 C4 C5 N1 -1.4(6) . . . . ?
C3 C4 C5 C6 177.8(4) . . . . ?
C4 C5 C6 O3 -175.5(4) . . . . ?
C4 C5 C6 O4 3.7(6) . . . . ?
C5 N1 C1 C2 -0.5(6) . . . . ?
C7 N2 C11 C10 -2.4(6) . . . . ?
C7 N2 C11 C12 178.4(3) . . . . ?
C7 C8 C9 C10 -1.4(8) . . . . ?
C8 C9 C10 C11 1.8(7) . . . . ?
C9 C10 C11 N2 0.1(7) . . . . ?
C9 C10 C11 C12 179.2(4) . . . . ?
C10 C11 C12 O5 -178.8(4) . . . . ?
C10 C11 C12 O6 1.4(6) . . . . ?
C11 N2 C7 C8 2.8(6) . . . . ?
C13 N3 C15 O7 -1.1(6) . . . . ?
C14 N3 C15 O7 -178.5(4) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.345
_oxdiff_exptl_absorpt_empirical_full_min 0.663
# start Validation Reply Form
_vrf_PLAT601_ti6pa8              
;
PROBLEM: Unit Cell Contains Solvent Accessible VOIDS of . 132 Ang**3
RESPONSE: This is a very small void.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ti17pa4
_database_code_depnum_ccdc_archive 'CCDC 2126648'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2022-01-27 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2022-01-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C56 H96 N4 O48 Ti17'
_chemical_formula_sum            'C56 H96 N4 O48 Ti17'
_chemical_formula_weight         2407.66
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Ti O C N'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_H-M_alt        'P 1 21/m 1'
_space_group_name_Hall           '-P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'

_cell_length_a                   14.1453(18)
_cell_length_b                   25.9558(14)
_cell_length_c                   14.178(2)
_cell_angle_alpha                90
_cell_angle_beta                 112.466(15)
_cell_angle_gamma                90
_cell_volume                     4810.3(11)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3589
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      72.2260
_cell_measurement_theta_min      3.3290
_shelx_estimated_absorpt_T_max   0.889
_shelx_estimated_absorpt_T_min   0.531
_exptl_absorpt_coefficient_mu    12.086
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.60509
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             2436
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0635
_diffrn_reflns_Laue_measured_fraction_full 0.824
_diffrn_reflns_Laue_measured_fraction_max 0.738
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            15616
_diffrn_reflns_point_group_measured_fraction_full 0.824
_diffrn_reflns_point_group_measured_fraction_max 0.738
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.110
_diffrn_reflns_theta_min         3.381
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.824
_diffrn_measured_fraction_theta_max 0.738
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00  66.00   1.00   11.83    --  106.49 -57.00 -90.00   32
  2  ω     35.00  66.00   1.00   11.83    --  106.49 -57.00-120.00   31
  3  ω     37.00 106.00   1.00   11.83    --  106.49-125.00-150.00   69
  4  ω     39.00  85.00   1.00   11.83    --  106.49-134.00  29.00   46
  5  ω     37.00  66.00   1.00   11.83    --  106.49 -57.00  60.00   29
  6  ω    -27.00  27.00   1.00    4.05    --  -48.20  19.00-150.00   54
  7  ω    -78.00 -19.00   1.00   11.83    --  -86.25 103.00-155.00   59
  8  ω   -120.00 -37.00   1.00    4.05    --  -48.20 -21.00-111.00   83
  9  ω   -147.00 -74.00   1.00   11.83    --  -86.25 -21.00-111.00   73
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545305000
_diffrn_orient_matrix_UB_12      0.0148197000
_diffrn_orient_matrix_UB_13      -0.1132351000
_diffrn_orient_matrix_UB_21      0.1010175000
_diffrn_orient_matrix_UB_22      -0.0076137000
_diffrn_orient_matrix_UB_23      -0.0157585000
_diffrn_orient_matrix_UB_31      -0.0278238000
_diffrn_orient_matrix_UB_32      -0.0569380000
_diffrn_orient_matrix_UB_33      -0.0273316000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5265
_reflns_number_total             7758
_reflns_odcompleteness_completeness 83.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.113
_refine_diff_density_rms         0.156
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     641
_refine_ls_number_reflns         7758
_refine_ls_number_restraints     180
_refine_ls_R_factor_all          0.1319
_refine_ls_R_factor_gt           0.1015
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1802P)²+27.5065P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2870
_refine_ls_wR_factor_ref         0.3121
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 O21-C23B = C23B-C24
 1.45 with sigma of 0.02
 C26_$1-C26
 2.35 with sigma of 0.02
 O27-C28
 2.35 with sigma of 0.001
 C26_$1-C25_$1 = O20-C25_$1
 1.45 with sigma of 0.02
 C28-C27
 1.45 with sigma of 0.01
 O20-C26_$1
 2.35 with sigma of 0.02
 O27-C27
 1.45 with sigma of 0.01
 O21-C23A = C23A-C24
 1.45 with sigma of 0.02
 O26-C30A
 2.35 with sigma of 0.02
 C14-O19
 2.35 with sigma of 0.02
 C14-C13
 1.45 with sigma of 0.02
 O23-C19
 1.45 with sigma of 0.02
 C20-C19
 1.45 with sigma of 0.02
 O24-C18
 2.35 with sigma of 0.02
 C17-C18
 1.45 with sigma of 0.02
 O24-C17
 1.45 with sigma of 0.02
 O26-C29
 1.45 with sigma of 0.02
 O26-C30B
 2.35 with sigma of 0.02
 C29-C30B
 1.45 with sigma of 0.02
 O21-C24
 2.35 with sigma of 0.02
 O21-C23A = C23A-C24 = C23B-C24 = O21-C23B
 1.45 with sigma of 0.02
 O22-C22A
 2.35 with sigma of 0.02
 C22A-C21
 1.45 with sigma of 0.02
 O22-C21
 1.45 with sigma of 0.02
 C31-C32
 1.45 with sigma of 0.02
 C18-C17
 1.45 with sigma of 0.02
 C30B-C29
 1.45 with sigma of 0.02
 C30A-C29
 1.45 with sigma of 0.02
 C16-C15 = O25-C15
 1.45 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O20 \\sim C25 \\sim C26: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O27 \\sim C27 \\sim C28: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O21 \\sim C23B \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O21 \\sim C23A \\sim C24: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O19 \\sim C13 \\sim C14: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O26 \\sim C29 \\sim C30A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O28 \\sim C31 \\sim C32: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O22 \\sim C21 \\sim C22B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O23 \\sim C19 \\sim C20: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O24 \\sim C17 \\sim C18: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O26 \\sim C29 \\sim C30B: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O21 \\sim C24: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O25 \\sim C15 \\sim C16: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
O22 \\sim C21 \\sim C22A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02 within 2A
4. Others
 Sof(H29A)=Sof(H29B)=Sof(C30A)=Sof(H30A)=Sof(H30B)=Sof(H30C)=1-FVAR(1)
 Sof(H29C)=Sof(H29D)=Sof(C30B)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(1)
 Fixed Sof: C13(0.5) H13A(0.5) H13B(0.5) C14(0.5) H14A(0.5) H14B(0.5)
 H14C(0.5) H15A(0.5) H15B(0.5) H16A(0.5) H16B(0.5) H16C(0.5) H17A(0.5)
 H17B(0.5) H18B(0.5) H18C(0.5) H21A(0.5) H21B(0.5) H21C(0.5) H21D(0.5)
 C22A(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C22B(0.5) H22D(0.5) H22E(0.5)
 H22F(0.5) C23A(0.5) H23A(0.5) H23B(0.5) C23B(0.5) H23C(0.5) H23D(0.5)
 H24A(0.5) H24B(0.5) H24C(0.5) H24D(0.5) H24E(0.5) H24F(0.5) C26(0.5) H26A(0.5)
 H26B(0.5) H26C(0.5) C25(0.5) H25A(0.5) H25B(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,H19B), C21(H21A,
 H21B), C21(H21C,H21D), C23A(H23A,H23B), C23B(H23C,H23D), C27(H27A,H27B),
 C29(H29A,H29B), C29(H29C,H29D), C31(H31A,H31B), C25(H25A,H25B)
5.b Me refined with riding coordinates:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C26(H26A,H26B,H26C)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10)
5.d Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C22A(H22A,H22B,H22C), C22B(H22D,
 H22E,H22F), C24(H24A,H24B,H24C), C24(H24D,H24E,H24F), C28(H28A,H28B,H28C),
 C30A(H30A,H30B,H30C), C30B(H30D,H30E,H30F), C32(H32A,H32B,H32C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.70047(16) 0.63807(6) 0.53373(15) 0.0469(5) Uani 1 1 d . . . . .
Ti2 Ti 0.55112(16) 0.63923(6) 0.09126(15) 0.0462(5) Uani 1 1 d . . . . .
Ti3 Ti 0.60830(15) 0.61444(6) 0.31125(15) 0.0433(5) Uani 1 1 d . . . . .
Ti4 Ti 0.48664(15) 0.68211(6) 0.42784(16) 0.0449(5) Uani 1 1 d . . . . .
Ti5 Ti 0.40179(15) 0.68216(6) 0.17608(16) 0.0463(5) Uani 1 1 d . . . . .
Ti6 Ti 0.5576(2) 0.7500 0.0468(2) 0.0446(6) Uani 1 2 d S T P . .
Ti7 Ti 0.76611(15) 0.68551(6) 0.19173(16) 0.0453(5) Uani 1 1 d . . . . .
Ti8 Ti 0.85535(15) 0.68600(6) 0.46053(16) 0.0475(5) Uani 1 1 d . . . . .
Ti9 Ti 0.7358(2) 0.7500 0.5798(2) 0.0449(6) Uani 1 2 d S T P . .
Ti10 Ti 0.62708(18) 0.7500 0.31371(19) 0.0357(5) Uani 1 2 d S T P . .
O1 O 0.4535(7) 0.6219(3) -0.0476(7) 0.063(2) Uani 1 1 d . . . . .
O2 O 0.4085(9) 0.5775(4) -0.1929(8) 0.092(3) Uani 1 1 d . . . . .
O3 O 0.7772(7) 0.5746(3) 0.5926(7) 0.063(2) Uani 1 1 d . . . . .
O4 O 0.8630(8) 0.5265(3) 0.7294(8) 0.085(3) Uani 1 1 d . . . . .
O5 O 0.6708(5) 0.6369(2) 0.2155(5) 0.0422(16) Uani 1 1 d . . . . .
O6 O 0.4875(5) 0.6159(2) 0.1816(6) 0.0483(17) Uani 1 1 d . . . . .
O7 O 0.6368(6) 0.6875(2) 0.0553(6) 0.0488(18) Uani 1 1 d . . . . .
O8 O 0.4781(5) 0.7002(2) 0.0907(6) 0.0456(16) Uani 1 1 d . . . . .
O9 O 0.7383(6) 0.6384(2) 0.4191(6) 0.0465(16) Uani 1 1 d . . . . .
O10 O 0.8141(5) 0.6878(2) 0.5825(6) 0.0442(16) Uani 1 1 d . . . . .
O11 O 0.6235(6) 0.6995(2) 0.5299(6) 0.0460(17) Uani 1 1 d . . . . .
O12 O 0.5723(5) 0.6161(2) 0.4339(5) 0.0439(16) Uani 1 1 d . . . . .
O13 O 0.8433(6) 0.6905(2) 0.3269(6) 0.0510(18) Uani 1 1 d . . . . .
O14 O 0.3714(8) 0.7500 0.1847(9) 0.054(3) Uani 1 2 d S T P . .
O15 O 0.4514(8) 0.7500 0.4154(9) 0.047(2) Uani 1 2 d S T P . .
O16 O 0.5484(5) 0.6934(2) 0.3083(5) 0.0404(15) Uani 1 1 d . . . . .
O17 O 0.7449(7) 0.7500 0.4285(7) 0.040(2) Uani 1 2 d S T P . .
O18 O 0.6694(7) 0.7500 0.2087(7) 0.039(2) Uani 1 2 d S T P . .
O19 O 0.9404(7) 0.7500 0.5077(10) 0.058(3) Uani 1 2 d DS TU P . .
O20 O 0.7643(10) 0.7500 0.7139(9) 0.068(3) Uani 1 2 d DS TU P . .
O21 O 0.4286(7) 0.6605(3) 0.5112(7) 0.069(2) Uani 1 1 d D U . . .
O22 O 0.3774(6) 0.6557(2) 0.2979(6) 0.0546(18) Uani 1 1 d D U . . .
O23 O 0.2864(6) 0.6587(3) 0.0792(7) 0.069(2) Uani 1 1 d D U . . .
O24 O 0.4882(10) 0.7500 -0.0854(10) 0.073(3) Uani 1 2 d DS TU P . .
O25 O 0.8166(10) 0.7500 0.1455(10) 0.065(3) Uani 1 2 d DS TU P . .
O26 O 0.8384(6) 0.6406(3) 0.1501(7) 0.059(2) Uani 1 1 d D U . . .
O27 O 0.9554(7) 0.6404(3) 0.5133(8) 0.078(3) Uani 1 1 d D U . . .
O28 O 0.6295(7) 0.5464(2) 0.3167(6) 0.061(2) Uani 1 1 d . U . . .
N1 N 0.6916(8) 0.6288(3) 0.6884(8) 0.060(3) Uani 1 1 d . . . . .
N2 N 0.6068(7) 0.5650(3) 0.0511(8) 0.052(2) Uani 1 1 d . . . . .
C1 C 0.6454(11) 0.6580(4) 0.7346(11) 0.068(3) Uani 1 1 d . . . . .
H1 H 0.5992 0.6833 0.6941 0.081 Uiso 1 1 calc R U . . .
C2 C 0.6577(12) 0.6551(5) 0.8339(12) 0.072(4) Uani 1 1 d . . . . .
H2 H 0.6224 0.6781 0.8613 0.086 Uiso 1 1 calc R U . . .
C3 C 0.7211(12) 0.6190(6) 0.8929(12) 0.079(4) Uani 1 1 d . . . . .
H3 H 0.7321 0.6160 0.9630 0.095 Uiso 1 1 calc R U . . .
C4 C 0.7720(12) 0.5851(6) 0.8471(11) 0.080(4) Uani 1 1 d . . . . .
H4 H 0.8158 0.5584 0.8856 0.096 Uiso 1 1 calc R U . . .
C5 C 0.7553(10) 0.5925(4) 0.7455(10) 0.060(3) Uani 1 1 d . . . . .
C6 C 0.8025(10) 0.5610(4) 0.6897(9) 0.060(3) Uani 1 1 d . . . . .
C7 C 0.6858(10) 0.5368(4) 0.1100(10) 0.059(3) Uani 1 1 d . . . . .
H7 H 0.7235 0.5476 0.1782 0.071 Uiso 1 1 calc R U . . .
C8 C 0.7146(11) 0.4919(4) 0.0740(12) 0.072(4) Uani 1 1 d . . . . .
H8 H 0.7719 0.4725 0.1169 0.086 Uiso 1 1 calc R U . . .
C9 C 0.6585(12) 0.4756(4) -0.0256(13) 0.075(4) Uani 1 1 d . . . . .
H9 H 0.6763 0.4448 -0.0511 0.090 Uiso 1 1 calc R U . . .
C10 C 0.5765(12) 0.5051(4) -0.0866(12) 0.067(4) Uani 1 1 d . . . . .
H10 H 0.5379 0.4953 -0.1552 0.081 Uiso 1 1 calc R U . . .
C11 C 0.5512(10) 0.5499(4) -0.0456(9) 0.055(3) Uani 1 1 d . . . . .
C12 C 0.4631(11) 0.5848(4) -0.1029(11) 0.068(3) Uani 1 1 d . . . . .
C13 C 1.0499(15) 0.754(3) 0.5471(19) 0.084(6) Uani 0.5 1 d D U P A -1
H13A H 1.0808 0.7203 0.5763 0.101 Uiso 0.5 1 calc R U P A -1
H13B H 1.0733 0.7801 0.6019 0.101 Uiso 0.5 1 calc R U P A -1
C14 C 1.082(2) 0.7683(12) 0.464(3) 0.107(9) Uani 0.5 1 d D U P A -1
H14A H 1.0393 0.7503 0.4019 0.160 Uiso 0.5 1 calc R U P A -1
H14B H 1.1537 0.7588 0.4826 0.160 Uiso 0.5 1 calc R U P A -1
H14C H 1.0740 0.8056 0.4534 0.160 Uiso 0.5 1 calc R U P A -1
C15 C 0.8722(17) 0.7500 0.0793(17) 0.085(4) Uani 1 2 d DS TU P . .
H15A H 0.8548 0.7190 0.0352 0.102 Uiso 0.5 1 calc R U P . .
H15B H 0.8548 0.7810 0.0352 0.102 Uiso 0.5 1 calc R U P . .
C16 C 0.9788(19) 0.7500 0.143(2) 0.122(7) Uani 1 2 d DS TU P . .
H16A H 0.9893 0.7314 0.2066 0.183 Uiso 0.5 1 calc R U P B -1
H16B H 1.0027 0.7856 0.1594 0.183 Uiso 0.5 1 calc R U P B -1
H16C H 1.0175 0.7330 0.1075 0.183 Uiso 0.5 1 calc R U P B -1
C17 C 0.4010(17) 0.7500 -0.1760(16) 0.115(6) Uani 1 2 d DS TU P . .
H17A H 0.4017 0.7191 -0.2167 0.138 Uiso 0.5 1 calc R U P . .
H17B H 0.4017 0.7809 -0.2167 0.138 Uiso 0.5 1 calc R U P . .
C18 C 0.3093(15) 0.7500 -0.155(3) 0.181(12) Uani 1 2 d DS TU P . .
H18A H 0.2495 0.7500 -0.2195 0.271 Uiso 0.5 1 calc R U P C -1
H18B H 0.3080 0.7192 -0.1156 0.271 Uiso 0.5 1 calc R U P C -1
H18C H 0.3080 0.7808 -0.1156 0.271 Uiso 0.5 1 calc R U P C -1
C19 C 0.1956(14) 0.6745(7) -0.0023(15) 0.125(5) Uani 1 1 d D U . . .
H19A H 0.1400 0.6777 0.0236 0.150 Uiso 1 1 calc R U . . .
H19B H 0.2069 0.7090 -0.0258 0.150 Uiso 1 1 calc R U . . .
C20 C 0.164(2) 0.6406(10) -0.086(2) 0.207(11) Uani 1 1 d D U . . .
H20A H 0.1012 0.6538 -0.1389 0.311 Uiso 1 1 calc R U . . .
H20B H 0.2178 0.6379 -0.1131 0.311 Uiso 1 1 calc R U . . .
H20C H 0.1508 0.6066 -0.0636 0.311 Uiso 1 1 calc R U . . .
C21 C 0.2936(11) 0.6240(5) 0.2991(13) 0.085(3) Uani 1 1 d D U . . .
H21A H 0.3020 0.6179 0.3708 0.102 Uiso 0.5 1 calc R U P D 1
H21B H 0.2285 0.6428 0.2649 0.102 Uiso 0.5 1 calc R U P D 1
H21C H 0.3125 0.6063 0.3657 0.102 Uiso 0.5 1 calc R U P E 2
H21D H 0.2755 0.5977 0.2445 0.102 Uiso 0.5 1 calc R U P E 2
C22A C 0.288(2) 0.5760(7) 0.250(3) 0.082(6) Uani 0.5 1 d D U P F 1
H22A H 0.2270 0.5573 0.2487 0.122 Uiso 0.5 1 calc R U P F 1
H22B H 0.3491 0.5558 0.2877 0.122 Uiso 0.5 1 calc R U P F 1
H22C H 0.2831 0.5817 0.1802 0.122 Uiso 0.5 1 calc R U P F 1
C22B C 0.206(2) 0.6597(12) 0.282(3) 0.081(7) Uani 0.5 1 d . U P F 2
H22D H 0.2051 0.6859 0.2317 0.121 Uiso 0.5 1 calc R U P F 2
H22E H 0.2139 0.6765 0.3463 0.121 Uiso 0.5 1 calc R U P F 2
H22F H 0.1420 0.6402 0.2561 0.121 Uiso 0.5 1 calc R U P F 2
C23A C 0.4053(18) 0.6334(11) 0.588(2) 0.091(5) Uani 0.5 1 d D U P G 1
H23A H 0.4564 0.6425 0.6562 0.109 Uiso 0.5 1 calc R U P G 1
H23B H 0.4096 0.5959 0.5781 0.109 Uiso 0.5 1 calc R U P G 1
C23B C 0.373(2) 0.6823(8) 0.567(3) 0.089(5) Uani 0.5 1 d D U P G 2
H23C H 0.4215 0.6946 0.6343 0.106 Uiso 0.5 1 calc R U P G 2
H23D H 0.3332 0.7124 0.5295 0.106 Uiso 0.5 1 calc R U P G 2
C24 C 0.3040(14) 0.6462(7) 0.5832(17) 0.108(4) Uani 1 1 d D U . . .
H24A H 0.2667 0.6650 0.5199 0.162 Uiso 0.5 1 calc R U P G 1
H24B H 0.3097 0.6678 0.6419 0.162 Uiso 0.5 1 calc R U P G 1
H24C H 0.2671 0.6145 0.5846 0.162 Uiso 0.5 1 calc R U P G 1
H24D H 0.2616 0.6304 0.5179 0.162 Uiso 0.5 1 calc R U P G 2
H24E H 0.2601 0.6640 0.6119 0.162 Uiso 0.5 1 calc R U P G 2
H24F H 0.3433 0.6194 0.6307 0.162 Uiso 0.5 1 calc R U P G 2
C26 C 0.902(2) 0.7055(4) 0.836(3) 0.138(11) Uani 0.5 1 d D U P H -1
H26A H 0.9629 0.7087 0.8994 0.208 Uiso 0.5 1 calc R U P H -1
H26B H 0.8537 0.6815 0.8468 0.208 Uiso 0.5 1 calc R U P H -1
H26C H 0.9222 0.6925 0.7816 0.208 Uiso 0.5 1 calc R U P H -1
C27 C 1.0171(15) 0.6071(6) 0.5961(12) 0.128(5) Uani 1 1 d D U . . .
H27A H 1.0898 0.6177 0.6206 0.153 Uiso 1 1 calc R U . . .
H27B H 0.9942 0.6097 0.6537 0.153 Uiso 1 1 calc R U . . .
C28 C 1.006(2) 0.5548(4) 0.559(2) 0.210(11) Uani 1 1 d D U . . .
H28A H 0.9339 0.5474 0.5201 0.315 Uiso 1 1 calc R U . . .
H28B H 1.0326 0.5311 0.6174 0.315 Uiso 1 1 calc R U . . .
H28C H 1.0451 0.5503 0.5155 0.315 Uiso 1 1 calc R U . . .
C29 C 0.9226(11) 0.6069(5) 0.1775(12) 0.086(3) Uani 1 1 d D U . . .
H29A H 0.9804 0.6255 0.1698 0.103 Uiso 0.80(3) 1 calc R U P I 5
H29B H 0.9043 0.5779 0.1283 0.103 Uiso 0.80(3) 1 calc R U P I 5
H29C H 0.9043 0.5742 0.2022 0.103 Uiso 0.20(3) 1 calc R U P I 6
H29D H 0.9806 0.6223 0.2345 0.103 Uiso 0.20(3) 1 calc R U P I 6
C30A C 0.9570(15) 0.5861(8) 0.2778(14) 0.097(6) Uani 0.80(3) 1 d D U P I 5
H30A H 0.8987 0.5716 0.2901 0.146 Uiso 0.80(3) 1 calc R U P I 5
H30B H 0.9888 0.6134 0.3276 0.146 Uiso 0.80(3) 1 calc R U P I 5
H30C H 1.0073 0.5588 0.2848 0.146 Uiso 0.80(3) 1 calc R U P I 5
C30B C 0.955(5) 0.596(3) 0.095(3) 0.103(13) Uani 0.20(3) 1 d D U P I 6
H30D H 1.0294 0.5991 0.1190 0.154 Uiso 0.20(3) 1 calc R U P I 6
H30E H 0.9225 0.6201 0.0390 0.154 Uiso 0.20(3) 1 calc R U P I 6
H30F H 0.9348 0.5606 0.0706 0.154 Uiso 0.20(3) 1 calc R U P I 6
C31 C 0.6520(13) 0.5031(4) 0.3816(12) 0.081(3) Uani 1 1 d D U . . .
H31A H 0.7061 0.5121 0.4482 0.098 Uiso 1 1 calc R U . . .
H31B H 0.6780 0.4749 0.3511 0.098 Uiso 1 1 calc R U . . .
C32 C 0.5596(17) 0.4856(8) 0.397(2) 0.147(7) Uani 1 1 d D U . . .
H32A H 0.5142 0.4674 0.3361 0.221 Uiso 1 1 calc R U . . .
H32B H 0.5237 0.5155 0.4098 0.221 Uiso 1 1 calc R U . . .
H32C H 0.5795 0.4624 0.4561 0.221 Uiso 1 1 calc R U . . .
C25 C 0.8525(19) 0.7574(9) 0.8066(18) 0.101(6) Uani 0.5 1 d . U P H -1
H25A H 0.8317 0.7710 0.8610 0.121 Uiso 0.5 1 calc R U P H -1
H25B H 0.9005 0.7821 0.7955 0.121 Uiso 0.5 1 calc R U P H -1


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.973(7) . ?
Ti1 O9 1.896(7) . ?
Ti1 O10 1.970(7) . ?
Ti1 O11 1.920(6) . ?
Ti1 O12 1.912(7) . ?
Ti1 N1 2.256(10) . ?
Ti2 O1 1.977(9) . ?
Ti2 O5 1.921(7) . ?
Ti2 O6 1.923(7) . ?
Ti2 O7 1.943(7) . ?
Ti2 O8 1.889(7) . ?
Ti2 N2 2.235(8) . ?
Ti3 O5 1.970(7) . ?
Ti3 O6 1.975(8) . ?
Ti3 O9 1.989(8) . ?
Ti3 O12 1.991(7) . ?
Ti3 O16 2.212(6) . ?
Ti3 O28 1.788(7) . ?
Ti4 O11 1.976(8) . ?
Ti4 O12 2.082(6) . ?
Ti4 O15 1.821(3) . ?
Ti4 O16 2.203(7) . ?
Ti4 O21 1.769(7) . ?
Ti4 O22 2.019(8) . ?
Ti5 O6 2.089(7) . ?
Ti5 O8 1.962(7) . ?
Ti5 O14 1.828(3) . ?
Ti5 O16 2.220(7) . ?
Ti5 O22 2.008(8) . ?
Ti5 O23 1.791(8) . ?
Ti6 O7 1.949(6) . ?
Ti6 O7 1.948(6) 4_575 ?
Ti6 O8 1.964(7) . ?
Ti6 O8 1.964(7) 4_575 ?
Ti6 O18 2.235(10) . ?
Ti6 O24 1.753(13) . ?
Ti7 O5 1.968(6) . ?
Ti7 O7 2.094(8) . ?
Ti7 O13 1.812(9) . ?
Ti7 O18 2.233(6) . ?
Ti7 O25 2.025(5) . ?
Ti7 O26 1.792(6) . ?
Ti8 Ti9 3.265(3) 4_575 ?
Ti8 O9 1.968(7) . ?
Ti8 O10 2.026(8) . ?
Ti8 O13 1.839(8) . ?
Ti8 O17 2.206(6) . ?
Ti8 O19 2.010(6) . ?
Ti8 O27 1.776(7) . ?
Ti9 Ti1 2.9779(17) 4_575 ?
Ti9 Ti9 0.000(6) 4_575 ?
Ti9 O10 1.949(6) . ?
Ti9 O10 1.949(6) 4_575 ?
Ti9 O11 1.970(7) 4_575 ?
Ti9 O11 1.970(7) . ?
Ti9 O17 2.197(10) . ?
Ti9 O20 1.786(12) . ?
Ti10 O16 1.827(6) . ?
Ti10 O16 1.827(6) 4_575 ?
Ti10 O17 1.831(10) . ?
Ti10 O18 1.804(9) . ?
O1 C12 1.281(14) . ?
O2 C12 1.228(17) . ?
O3 C6 1.332(14) . ?
O4 C6 1.217(14) . ?
O10 Ti9 1.949(6) 4_575 ?
O11 Ti9 1.970(7) 4_575 ?
O14 Ti5 1.828(3) 4_575 ?
O15 Ti4 1.821(3) 4_575 ?
O17 Ti8 2.206(6) 4_575 ?
O17 Ti9 2.197(10) 4_575 ?
O18 Ti7 2.233(6) 4_575 ?
O19 Ti8 2.010(6) 4_575 ?
O19 C13 1.44(2) . ?
O20 Ti9 1.786(12) 4_575 ?
O20 C25 1.438(17) 4_575 ?
O20 C25 1.438(17) . ?
O21 C23A 1.434(13) . ?
O21 C23B 1.436(13) . ?
O22 C21 1.448(12) . ?
O23 C19 1.421(15) . ?
O24 C17 1.400(17) . ?
O25 Ti7 2.025(5) 4_575 ?
O25 C15 1.436(15) . ?
O26 C29 1.409(12) . ?
O27 C27 1.451(10) . ?
O28 C31 1.409(15) . ?
N1 C1 1.325(15) . ?
N1 C5 1.341(16) . ?
N2 C7 1.331(16) . ?
N2 C11 1.351(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.35(2) . ?
C2 H2 0.9500 . ?
C2 C3 1.35(2) . ?
C3 H3 0.9500 . ?
C3 C4 1.44(2) . ?
C4 H4 0.9500 . ?
C4 C5 1.381(19) . ?
C5 C6 1.464(18) . ?
C7 H7 0.9500 . ?
C7 C8 1.395(15) . ?
C8 H8 0.9500 . ?
C8 C9 1.40(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.38(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.406(15) . ?
C11 C12 1.504(19) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.456(19) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.433(18) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.436(14) . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.403(18) . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 H21C 0.9900 . ?
C21 H21D 0.9900 . ?
C21 C22A 1.413(16) . ?
C21 C22B 1.49(3) . ?
C22A H22A 0.9800 . ?
C22A H22B 0.9800 . ?
C22A H22C 0.9800 . ?
C22B H22D 0.9800 . ?
C22B H22E 0.9800 . ?
C22B H22F 0.9800 . ?
C23A H23A 0.9900 . ?
C23A H23B 0.9900 . ?
C23A C24 1.447(14) . ?
C23B H23C 0.9900 . ?
C23B H23D 0.9900 . ?
C23B C24 1.427(13) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C24 H24D 0.9800 . ?
C24 H24E 0.9800 . ?
C24 H24F 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C26 C25 1.501(19) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.440(10) . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 H29C 0.9900 . ?
C29 H29D 0.9900 . ?
C29 C30A 1.422(16) . ?
C29 C30B 1.438(14) . ?
C30A H30A 0.9800 . ?
C30A H30B 0.9800 . ?
C30A H30C 0.9800 . ?
C30B H30D 0.9800 . ?
C30B H30E 0.9800 . ?
C30B H30F 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C31 C32 1.479(17) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 N1 74.1(4) . . ?
O9 Ti1 O3 94.4(3) . . ?
O9 Ti1 O10 80.7(3) . . ?
O9 Ti1 O11 108.4(3) . . ?
O9 Ti1 O12 82.3(3) . . ?
O9 Ti1 N1 166.5(4) . . ?
O10 Ti1 O3 99.0(3) . . ?
O10 Ti1 N1 94.0(3) . . ?
O11 Ti1 O3 156.8(3) . . ?
O11 Ti1 O10 81.0(3) . . ?
O11 Ti1 N1 82.8(3) . . ?
O12 Ti1 O3 106.0(3) . . ?
O12 Ti1 O10 150.6(3) . . ?
O12 Ti1 O11 82.0(3) . . ?
O12 Ti1 N1 107.3(4) . . ?
O1 Ti2 N2 74.3(3) . . ?
O5 Ti2 O1 160.2(3) . . ?
O5 Ti2 O6 81.5(3) . . ?
O5 Ti2 O7 80.9(3) . . ?
O5 Ti2 N2 86.2(3) . . ?
O6 Ti2 O1 105.3(3) . . ?
O6 Ti2 O7 151.2(3) . . ?
O6 Ti2 N2 101.4(3) . . ?
O7 Ti2 O1 98.9(3) . . ?
O7 Ti2 N2 100.0(3) . . ?
O8 Ti2 O1 90.8(3) . . ?
O8 Ti2 O5 108.6(3) . . ?
O8 Ti2 O6 82.7(3) . . ?
O8 Ti2 O7 81.6(3) . . ?
O8 Ti2 N2 165.1(4) . . ?
O5 Ti3 O6 79.0(3) . . ?
O5 Ti3 O9 84.9(3) . . ?
O5 Ti3 O12 158.1(3) . . ?
O5 Ti3 O16 89.0(2) . . ?
O6 Ti3 O9 157.9(3) . . ?
O6 Ti3 O12 113.2(3) . . ?
O6 Ti3 O16 77.0(3) . . ?
O9 Ti3 O12 78.0(3) . . ?
O9 Ti3 O16 87.7(3) . . ?
O12 Ti3 O16 76.9(2) . . ?
O28 Ti3 O5 102.1(3) . . ?
O28 Ti3 O6 97.5(3) . . ?
O28 Ti3 O9 100.6(3) . . ?
O28 Ti3 O12 94.5(3) . . ?
O28 Ti3 O16 166.5(3) . . ?
O11 Ti4 O12 76.5(3) . . ?
O11 Ti4 O16 88.1(3) . . ?
O11 Ti4 O22 160.0(3) . . ?
O12 Ti4 O16 75.3(2) . . ?
O15 Ti4 O11 90.3(4) . . ?
O15 Ti4 O12 159.1(3) . . ?
O15 Ti4 O16 88.4(3) . . ?
O15 Ti4 O22 98.9(4) . . ?
O21 Ti4 O11 99.1(4) . . ?
O21 Ti4 O12 97.0(3) . . ?
O21 Ti4 O15 101.1(4) . . ?
O21 Ti4 O16 168.0(3) . . ?
O21 Ti4 O22 96.5(4) . . ?
O22 Ti4 O12 89.4(3) . . ?
O22 Ti4 O16 74.5(3) . . ?
O6 Ti5 O16 74.6(3) . . ?
O8 Ti5 O6 76.8(3) . . ?
O8 Ti5 O16 86.2(3) . . ?
O8 Ti5 O22 158.3(3) . . ?
O14 Ti5 O6 159.9(4) . . ?
O14 Ti5 O8 90.6(4) . . ?
O14 Ti5 O16 89.1(4) . . ?
O14 Ti5 O22 98.6(4) . . ?
O22 Ti5 O6 88.5(3) . . ?
O22 Ti5 O16 74.4(3) . . ?
O23 Ti5 O6 95.4(3) . . ?
O23 Ti5 O8 99.4(4) . . ?
O23 Ti5 O14 102.1(4) . . ?
O23 Ti5 O16 167.3(3) . . ?
O23 Ti5 O22 97.9(4) . . ?
O7 Ti6 O7 112.7(4) 4_575 . ?
O7 Ti6 O8 156.0(3) 4_575 . ?
O7 Ti6 O8 79.5(3) 4_575 4_575 ?
O7 Ti6 O8 79.5(3) . . ?
O7 Ti6 O8 156.0(3) . 4_575 ?
O7 Ti6 O18 76.8(3) . . ?
O7 Ti6 O18 76.8(3) 4_575 . ?
O8 Ti6 O8 82.2(4) 4_575 . ?
O8 Ti6 O18 86.6(3) . . ?
O8 Ti6 O18 86.6(3) 4_575 . ?
O24 Ti6 O7 98.1(3) . . ?
O24 Ti6 O7 98.1(3) . 4_575 ?
O24 Ti6 O8 100.6(4) . . ?
O24 Ti6 O8 100.6(4) . 4_575 ?
O24 Ti6 O18 170.4(5) . . ?
O5 Ti7 O7 76.1(3) . . ?
O5 Ti7 O18 88.5(2) . . ?
O5 Ti7 O25 159.3(4) . . ?
O7 Ti7 O18 74.1(3) . . ?
O13 Ti7 O5 92.3(3) . . ?
O13 Ti7 O7 159.3(3) . . ?
O13 Ti7 O18 88.8(3) . . ?
O13 Ti7 O25 98.0(5) . . ?
O25 Ti7 O7 88.4(5) . . ?
O25 Ti7 O18 73.8(3) . . ?
O26 Ti7 O5 98.9(3) . . ?
O26 Ti7 O7 96.8(3) . . ?
O26 Ti7 O13 101.9(4) . . ?
O26 Ti7 O18 166.7(4) . . ?
O26 Ti7 O25 96.6(3) . . ?
O9 Ti8 Ti9 86.1(2) . 4_575 ?
O9 Ti8 O10 77.6(3) . . ?
O9 Ti8 O17 87.9(3) . . ?
O9 Ti8 O19 161.3(3) . . ?
O10 Ti8 Ti9 34.00(17) . 4_575 ?
O10 Ti8 O17 75.3(3) . . ?
O13 Ti8 Ti9 129.7(2) . 4_575 ?
O13 Ti8 O9 89.8(3) . . ?
O13 Ti8 O10 159.0(3) . . ?
O13 Ti8 O17 87.7(3) . . ?
O13 Ti8 O19 95.7(4) . . ?
O17 Ti8 Ti9 42.0(3) . 4_575 ?
O19 Ti8 Ti9 76.7(3) . 4_575 ?
O19 Ti8 O10 91.6(4) . . ?
O19 Ti8 O17 74.5(3) . . ?
O27 Ti8 Ti9 127.4(3) . 4_575 ?
O27 Ti8 O9 98.7(4) . . ?
O27 Ti8 O10 95.7(4) . . ?
O27 Ti8 O13 102.8(4) . . ?
O27 Ti8 O17 167.5(4) . . ?
O27 Ti8 O19 97.5(4) . . ?
Ti9 Ti9 Ti1 0(10) 4_575 4_575 ?
Ti9 Ti9 O10 0(10) 4_575 . ?
Ti9 Ti9 O10 0(10) 4_575 4_575 ?
Ti9 Ti9 O11 0(10) 4_575 . ?
Ti9 Ti9 O11 0(10) 4_575 4_575 ?
Ti9 Ti9 O17 0(10) 4_575 . ?
Ti9 Ti9 O20 0(10) 4_575 . ?
O10 Ti9 Ti1 40.8(2) 4_575 4_575 ?
O10 Ti9 Ti1 149.2(2) . 4_575 ?
O10 Ti9 O10 111.8(4) . 4_575 ?
O10 Ti9 O11 80.2(3) . . ?
O10 Ti9 O11 158.7(3) . 4_575 ?
O10 Ti9 O11 80.2(3) 4_575 4_575 ?
O10 Ti9 O11 158.7(3) 4_575 . ?
O10 Ti9 O17 77.0(3) . . ?
O10 Ti9 O17 77.0(3) 4_575 . ?
O11 Ti9 Ti1 39.44(19) 4_575 4_575 ?
O11 Ti9 Ti1 121.7(2) . 4_575 ?
O11 Ti9 O11 83.3(4) . 4_575 ?
O11 Ti9 O17 89.4(3) . . ?
O11 Ti9 O17 89.4(3) 4_575 . ?
O17 Ti9 Ti1 81.57(8) . 4_575 ?
O20 Ti9 Ti1 100.61(8) . 4_575 ?
O20 Ti9 O10 94.8(3) . 4_575 ?
O20 Ti9 O10 94.8(3) . . ?
O20 Ti9 O11 101.9(4) . . ?
O20 Ti9 O11 101.9(4) . 4_575 ?
O20 Ti9 O17 164.9(5) . . ?
O16 Ti10 O16 107.0(4) 4_575 . ?
O16 Ti10 O17 111.7(3) . . ?
O16 Ti10 O17 111.7(3) 4_575 . ?
O18 Ti10 O16 110.7(3) . 4_575 ?
O18 Ti10 O16 110.7(3) . . ?
O18 Ti10 O17 104.9(4) . . ?
C12 O1 Ti2 125.7(9) . . ?
C6 O3 Ti1 123.1(7) . . ?
Ti2 O5 Ti3 99.8(3) . . ?
Ti2 O5 Ti7 104.1(3) . . ?
Ti7 O5 Ti3 145.6(4) . . ?
Ti2 O6 Ti3 99.6(3) . . ?
Ti2 O6 Ti5 97.4(3) . . ?
Ti3 O6 Ti5 109.5(3) . . ?
Ti2 O7 Ti6 98.7(3) . . ?
Ti2 O7 Ti7 98.8(3) . . ?
Ti6 O7 Ti7 110.9(3) . . ?
Ti2 O8 Ti5 103.1(3) . . ?
Ti2 O8 Ti6 100.0(3) . . ?
Ti5 O8 Ti6 150.4(4) . . ?
Ti1 O9 Ti3 100.2(3) . . ?
Ti1 O9 Ti8 103.1(3) . . ?
Ti8 O9 Ti3 148.3(4) . . ?
Ti1 O10 Ti8 98.5(3) . . ?
Ti9 O10 Ti1 98.9(3) 4_575 . ?
Ti9 O10 Ti1 98.9(3) . . ?
Ti9 O10 Ti8 110.5(3) . . ?
Ti9 O10 Ti8 110.5(3) 4_575 . ?
Ti9 O10 Ti9 0.00(17) 4_575 . ?
Ti1 O11 Ti4 102.5(3) . . ?
Ti1 O11 Ti9 99.9(3) . . ?
Ti1 O11 Ti9 99.9(3) . 4_575 ?
Ti9 O11 Ti4 147.7(4) . . ?
Ti9 O11 Ti4 147.7(4) 4_575 . ?
Ti9 O11 Ti9 0.0 4_575 . ?
Ti1 O12 Ti3 99.5(3) . . ?
Ti1 O12 Ti4 99.0(3) . . ?
Ti3 O12 Ti4 108.7(3) . . ?
Ti7 O13 Ti8 150.0(4) . . ?
Ti5 O14 Ti5 148.9(6) . 4_575 ?
Ti4 O15 Ti4 150.7(6) 4_575 . ?
Ti3 O16 Ti5 97.0(2) . . ?
Ti4 O16 Ti3 97.1(2) . . ?
Ti4 O16 Ti5 96.6(3) . . ?
Ti10 O16 Ti3 121.4(3) . . ?
Ti10 O16 Ti4 119.3(3) . . ?
Ti10 O16 Ti5 119.9(3) . . ?
Ti8 O17 Ti8 97.7(4) 4_575 . ?
Ti9 O17 Ti8 95.7(3) 4_575 . ?
Ti9 O17 Ti8 95.7(3) . . ?
Ti9 O17 Ti8 95.7(3) 4_575 4_575 ?
Ti9 O17 Ti8 95.7(3) . 4_575 ?
Ti9 O17 Ti9 0.00(15) 4_575 . ?
Ti10 O17 Ti8 121.0(3) . 4_575 ?
Ti10 O17 Ti8 121.0(3) . . ?
Ti10 O17 Ti9 119.7(4) . . ?
Ti10 O17 Ti9 119.7(4) . 4_575 ?
Ti7 O18 Ti6 96.4(3) 4_575 . ?
Ti7 O18 Ti6 96.4(3) . . ?
Ti7 O18 Ti7 97.1(3) 4_575 . ?
Ti10 O18 Ti6 121.4(5) . . ?
Ti10 O18 Ti7 120.0(3) . 4_575 ?
Ti10 O18 Ti7 120.0(3) . . ?
Ti8 O19 Ti8 111.5(5) . 4_575 ?
C13 O19 Ti8 127(3) . . ?
C13 O19 Ti8 119(3) . 4_575 ?
Ti9 O20 Ti9 0.000(1) 4_575 . ?
C25 O20 Ti9 137.5(17) . 4_575 ?
C25 O20 Ti9 137.5(17) 4_575 . ?
C25 O20 Ti9 137.5(17) 4_575 4_575 ?
C25 O20 Ti9 137.5(17) . . ?
C25 O20 C25 15.3(19) . 4_575 ?
C23A O21 Ti4 164.1(10) . . ?
C23B O21 Ti4 137.7(11) . . ?
Ti5 O22 Ti4 110.2(3) . . ?
C21 O22 Ti4 121.8(8) . . ?
C21 O22 Ti5 128.0(8) . . ?
C19 O23 Ti5 143.2(9) . . ?
C17 O24 Ti6 156.6(14) . . ?
Ti7 O25 Ti7 111.5(4) . 4_575 ?
C15 O25 Ti7 124.1(2) . . ?
C15 O25 Ti7 124.1(2) . 4_575 ?
C29 O26 Ti7 147.4(8) . . ?
C27 O27 Ti8 151.0(12) . . ?
C31 O28 Ti3 143.9(8) . . ?
C1 N1 Ti1 129.9(8) . . ?
C1 N1 C5 116.6(11) . . ?
C5 N1 Ti1 112.8(8) . . ?
C7 N2 Ti2 127.4(8) . . ?
C7 N2 C11 120.0(9) . . ?
C11 N2 Ti2 112.6(7) . . ?
N1 C1 H1 116.9 . . ?
N1 C1 C2 126.3(13) . . ?
C2 C1 H1 116.9 . . ?
C1 C2 H2 120.8 . . ?
C3 C2 C1 118.4(14) . . ?
C3 C2 H2 120.8 . . ?
C2 C3 H3 120.8 . . ?
C2 C3 C4 118.4(13) . . ?
C4 C3 H3 120.8 . . ?
C3 C4 H4 121.0 . . ?
C5 C4 C3 118.0(14) . . ?
C5 C4 H4 121.0 . . ?
N1 C5 C4 122.4(13) . . ?
N1 C5 C6 114.0(11) . . ?
C4 C5 C6 123.6(12) . . ?
O3 C6 C5 114.3(10) . . ?
O4 C6 O3 122.5(12) . . ?
O4 C6 C5 123.1(12) . . ?
N2 C7 H7 119.2 . . ?
N2 C7 C8 121.5(13) . . ?
C8 C7 H7 119.2 . . ?
C7 C8 H8 120.3 . . ?
C9 C8 C7 119.4(14) . . ?
C9 C8 H8 120.3 . . ?
C8 C9 H9 120.6 . . ?
C10 C9 C8 118.9(11) . . ?
C10 C9 H9 120.6 . . ?
C9 C10 H10 120.5 . . ?
C9 C10 C11 118.9(13) . . ?
C11 C10 H10 120.5 . . ?
N2 C11 C10 121.2(12) . . ?
N2 C11 C12 114.4(9) . . ?
C10 C11 C12 124.3(12) . . ?
O1 C12 C11 112.5(12) . . ?
O2 C12 O1 125.5(13) . . ?
O2 C12 C11 122.1(11) . . ?
O19 C13 H13A 109.9 . . ?
O19 C13 H13B 109.9 . . ?
O19 C13 C14 109.0(17) . . ?
H13A C13 H13B 108.3 . . ?
C14 C13 H13A 109.9 . . ?
C14 C13 H13B 109.9 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O25 C15 H15A 110.3 . . ?
O25 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C16 C15 O25 107(2) . . ?
C16 C15 H15A 110.3 . . ?
C16 C15 H15B 110.3 . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O24 C17 H17A 109.4 . . ?
O24 C17 H17B 109.4 . . ?
O24 C17 C18 111.1(17) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O23 C19 H19A 108.8 . . ?
O23 C19 H19B 108.8 . . ?
H19A C19 H19B 107.7 . . ?
C20 C19 O23 113.7(18) . . ?
C20 C19 H19A 108.8 . . ?
C20 C19 H19B 108.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O22 C21 H21A 109.0 . . ?
O22 C21 H21B 109.0 . . ?
O22 C21 H21C 110.5 . . ?
O22 C21 H21D 110.5 . . ?
O22 C21 C22B 106.1(14) . . ?
H21A C21 H21B 107.8 . . ?
H21C C21 H21D 108.7 . . ?
C22A C21 O22 112.9(13) . . ?
C22A C21 H21A 109.0 . . ?
C22A C21 H21B 109.0 . . ?
C22B C21 H21C 110.5 . . ?
C22B C21 H21D 110.5 . . ?
C21 C22A H22A 109.5 . . ?
C21 C22A H22B 109.5 . . ?
C21 C22A H22C 109.5 . . ?
H22A C22A H22B 109.5 . . ?
H22A C22A H22C 109.5 . . ?
H22B C22A H22C 109.5 . . ?
C21 C22B H22D 109.5 . . ?
C21 C22B H22E 109.5 . . ?
C21 C22B H22F 109.5 . . ?
H22D C22B H22E 109.5 . . ?
H22D C22B H22F 109.5 . . ?
H22E C22B H22F 109.5 . . ?
O21 C23A H23A 109.4 . . ?
O21 C23A H23B 109.4 . . ?
O21 C23A C24 111.3(13) . . ?
H23A C23A H23B 108.0 . . ?
C24 C23A H23A 109.4 . . ?
C24 C23A H23B 109.4 . . ?
O21 C23B H23C 109.1 . . ?
O21 C23B H23D 109.1 . . ?
H23C C23B H23D 107.9 . . ?
C24 C23B O21 112.4(13) . . ?
C24 C23B H23C 109.1 . . ?
C24 C23B H23D 109.1 . . ?
C23A C24 H24A 109.5 . . ?
C23A C24 H24B 109.5 . . ?
C23A C24 H24C 109.5 . . ?
C23B C24 H24D 109.5 . . ?
C23B C24 H24E 109.5 . . ?
C23B C24 H24F 109.5 . . ?
H24A C24 H24B 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
H24D C24 H24E 109.5 . . ?
H24D C24 H24F 109.5 . . ?
H24E C24 H24F 109.5 . . ?
H26A C26 H26B 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
O27 C27 H27A 109.9 . . ?
O27 C27 H27B 109.9 . . ?
H27A C27 H27B 108.3 . . ?
C28 C27 O27 108.7(8) . . ?
C28 C27 H27A 109.9 . . ?
C28 C27 H27B 109.9 . . ?
C27 C28 H28A 109.5 . . ?
C27 C28 H28B 109.5 . . ?
C27 C28 H28C 109.5 . . ?
H28A C28 H28B 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
O26 C29 H29A 108.2 . . ?
O26 C29 H29B 108.2 . . ?
O26 C29 H29C 108.9 . . ?
O26 C29 H29D 108.9 . . ?
O26 C29 C30A 116.2(12) . . ?
O26 C29 C30B 113.5(18) . . ?
H29A C29 H29B 107.4 . . ?
H29C C29 H29D 107.7 . . ?
C30A C29 H29A 108.2 . . ?
C30A C29 H29B 108.2 . . ?
C30B C29 H29C 108.9 . . ?
C30B C29 H29D 108.9 . . ?
C29 C30A H30A 109.5 . . ?
C29 C30A H30B 109.5 . . ?
C29 C30A H30C 109.5 . . ?
H30A C30A H30B 109.5 . . ?
H30A C30A H30C 109.5 . . ?
H30B C30A H30C 109.5 . . ?
C29 C30B H30D 109.5 . . ?
C29 C30B H30E 109.5 . . ?
C29 C30B H30F 109.5 . . ?
H30D C30B H30E 109.5 . . ?
H30D C30B H30F 109.5 . . ?
H30E C30B H30F 109.5 . . ?
O28 C31 H31A 109.6 . . ?
O28 C31 H31B 109.6 . . ?
O28 C31 C32 110.5(14) . . ?
H31A C31 H31B 108.1 . . ?
C32 C31 H31A 109.6 . . ?
C32 C31 H31B 109.6 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32B 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O20 C25 C26 106.6(17) . . ?
O20 C25 H25A 110.4 . . ?
O20 C25 H25B 110.4 . . ?
C26 C25 H25A 110.4 . . ?
C26 C25 H25B 110.4 . . ?
H25A C25 H25B 108.6 . . ?

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
Ti1 Ti9 O20 Ti9 0(100) 4_575 . . 4_575 ?
Ti1 Ti9 O20 C25 -108.3(13) 4_575 . . 4_575 ?
Ti1 Ti9 O20 C25 -85.6(13) 4_575 . . . ?
Ti1 O3 C6 O4 -168.1(9) . . . . ?
Ti1 O3 C6 C5 9.1(14) . . . . ?
Ti1 N1 C1 C2 -167.8(11) . . . . ?
Ti1 N1 C5 C4 171.4(10) . . . . ?
Ti1 N1 C5 C6 -10.2(13) . . . . ?
Ti2 O1 C12 O2 -171.6(11) . . . . ?
Ti2 O1 C12 C11 8.1(15) . . . . ?
Ti2 N2 C7 C8 -177.8(8) . . . . ?
Ti2 N2 C11 C10 177.6(9) . . . . ?
Ti2 N2 C11 C12 -2.0(12) . . . . ?
Ti3 O28 C31 C32 78(2) . . . . ?
Ti4 O21 C23A C24 -170(4) . . . . ?
Ti4 O21 C23B C24 152.0(15) . . . . ?
Ti4 O22 C21 C22A -122.7(19) . . . . ?
Ti4 O22 C21 C22B 96.4(17) . . . . ?
Ti5 O22 C21 C22A 60(2) . . . . ?
Ti5 O22 C21 C22B -80.9(18) . . . . ?
Ti5 O23 C19 C20 144(2) . . . . ?
Ti6 O24 C17 C18 0.000(4) . . . . ?
Ti7 O25 C15 C16 93.4(11) 4_575 . . . ?
Ti7 O25 C15 C16 -93.4(11) . . . . ?
Ti7 O26 C29 C30A 26(3) . . . . ?
Ti7 O26 C29 C30B -159(4) . . . . ?
Ti8 O19 C13 C14 96(4) . . . . ?
Ti8 O19 C13 C14 -68(5) 4_575 . . . ?
Ti8 O27 C27 C28 121(2) . . . . ?
Ti9 Ti8 O13 Ti7 -60.3(8) 4_575 . . . ?
Ti9 Ti8 O27 C27 12(2) 4_575 . . . ?
Ti9 Ti9 O20 C25 0.0(6) 4_575 . . 4_575 ?
Ti9 Ti9 O20 C25 0.0(6) 4_575 . . . ?
Ti9 O20 C25 C26 -88(3) 4_575 . . . ?
Ti9 O20 C25 C26 -88(3) . . . . ?
O1 Ti2 O8 Ti5 102.9(4) . . . . ?
O1 Ti2 O8 Ti6 -95.8(4) . . . . ?
O3 Ti1 O9 Ti3 104.7(3) . . . . ?
O3 Ti1 O9 Ti8 -96.9(3) . . . . ?
O5 Ti2 O8 Ti5 -80.9(4) . . . . ?
O5 Ti2 O8 Ti6 80.4(4) . . . . ?
O5 Ti3 O28 C31 144.1(15) . . . . ?
O5 Ti7 O13 Ti8 -25.3(8) . . . . ?
O5 Ti7 O26 C29 -88.6(15) . . . . ?
O6 Ti2 O8 Ti5 -2.5(3) . . . . ?
O6 Ti2 O8 Ti6 158.9(4) . . . . ?
O6 Ti3 O28 C31 -135.6(15) . . . . ?
O6 Ti5 O14 Ti5 28(2) . . . 4_575 ?
O6 Ti5 O23 C19 -152(2) . . . . ?
O7 Ti2 O8 Ti5 -158.3(4) . . . . ?
O7 Ti2 O8 Ti6 3.1(3) . . . . ?
O7 Ti6 O24 C17 122.8(2) . . . . ?
O7 Ti6 O24 C17 -122.8(2) 4_575 . . . ?
O7 Ti7 O13 Ti8 29.6(13) . . . . ?
O7 Ti7 O26 C29 -165.5(15) . . . . ?
O8 Ti5 O14 Ti5 -22.0(14) . . . 4_575 ?
O8 Ti5 O23 C19 -74(2) . . . . ?
O8 Ti6 O24 C17 42.0(2) . . . . ?
O8 Ti6 O24 C17 -42.0(2) 4_575 . . . ?
O9 Ti3 O28 C31 57.1(16) . . . . ?
O9 Ti8 O13 Ti7 24.4(8) . . . . ?
O9 Ti8 O27 C27 -79(2) . . . . ?
O10 Ti1 O9 Ti3 -156.9(3) . . . . ?
O10 Ti1 O9 Ti8 1.5(3) . . . . ?
O10 Ti8 O13 Ti7 -28.0(13) . . . . ?
O10 Ti8 O27 C27 -1(2) . . . . ?
O10 Ti9 O20 Ti9 0(100) 4_575 . . 4_575 ?
O10 Ti9 O20 Ti9 0(100) . . . 4_575 ?
O10 Ti9 O20 C25 67.5(13) . . . . ?
O10 Ti9 O20 C25 44.9(14) . . . 4_575 ?
O10 Ti9 O20 C25 -67.5(13) 4_575 . . 4_575 ?
O10 Ti9 O20 C25 -44.9(14) 4_575 . . . ?
O11 Ti1 O9 Ti3 -79.8(3) . . . . ?
O11 Ti1 O9 Ti8 78.6(4) . . . . ?
O11 Ti4 O15 Ti4 22.7(13) . . . 4_575 ?
O11 Ti4 O21 C23A -56(6) . . . . ?
O11 Ti4 O21 C23B 88(3) . . . . ?
O11 Ti9 O20 Ti9 0(100) 4_575 . . 4_575 ?
O11 Ti9 O20 Ti9 0(100) . . . 4_575 ?
O11 Ti9 O20 C25 148.5(13) . . . . ?
O11 Ti9 O20 C25 125.9(14) . . . 4_575 ?
O11 Ti9 O20 C25 -148.5(13) 4_575 . . 4_575 ?
O11 Ti9 O20 C25 -125.9(14) 4_575 . . . ?
O12 Ti1 O9 Ti3 -1.0(3) . . . . ?
O12 Ti1 O9 Ti8 157.5(3) . . . . ?
O12 Ti3 O28 C31 -21.5(16) . . . . ?
O12 Ti4 O15 Ti4 -27(2) . . . 4_575 ?
O12 Ti4 O21 C23A 21(6) . . . . ?
O12 Ti4 O21 C23B 166(3) . . . . ?
O13 Ti7 O26 C29 5.7(16) . . . . ?
O13 Ti8 O27 C27 -171(2) . . . . ?
O14 Ti5 O23 C19 18(2) . . . . ?
O15 Ti4 O21 C23A -148(6) . . . . ?
O15 Ti4 O21 C23B -4(3) . . . . ?
O16 Ti3 O28 C31 -71(2) . . . . ?
O16 Ti4 O15 Ti4 -65.4(13) . . . 4_575 ?
O16 Ti4 O21 C23A 70(7) . . . . ?
O16 Ti4 O21 C23B -145(3) . . . . ?
O16 Ti5 O14 Ti5 64.2(14) . . . 4_575 ?
O16 Ti5 O23 C19 171(2) . . . . ?
O16 Ti10 O16 Ti3 179.53(10) 4_575 . . . ?
O16 Ti10 O16 Ti4 -59.9(6) 4_575 . . . ?
O16 Ti10 O16 Ti5 58.4(5) 4_575 . . . ?
O16 Ti10 O17 Ti8 -58.5(5) 4_575 . . 4_575 ?
O16 Ti10 O17 Ti8 58.5(5) . . . . ?
O16 Ti10 O17 Ti8 178.5(4) 4_575 . . . ?
O16 Ti10 O17 Ti8 -178.5(4) . . . 4_575 ?
O16 Ti10 O17 Ti9 60.0(3) 4_575 . . . ?
O16 Ti10 O17 Ti9 -60.0(3) . . . . ?
O16 Ti10 O17 Ti9 -60.0(3) . . . 4_575 ?
O16 Ti10 O17 Ti9 60.0(3) 4_575 . . 4_575 ?
O16 Ti10 O18 Ti6 59.3(3) . . . . ?
O16 Ti10 O18 Ti6 -59.3(3) 4_575 . . . ?
O16 Ti10 O18 Ti7 -179.4(4) 4_575 . . . ?
O16 Ti10 O18 Ti7 -60.8(6) . . . . ?
O16 Ti10 O18 Ti7 179.4(4) . . . 4_575 ?
O16 Ti10 O18 Ti7 60.8(6) 4_575 . . 4_575 ?
O17 Ti8 O13 Ti7 -63.5(7) . . . . ?
O17 Ti8 O27 C27 42(3) . . . . ?
O17 Ti9 O20 Ti9 0(100) . . . 4_575 ?
O17 Ti9 O20 C25 -11.3(13) . . . 4_575 ?
O17 Ti9 O20 C25 11.3(13) . . . . ?
O17 Ti10 O16 Ti3 -57.8(5) . . . . ?
O17 Ti10 O16 Ti4 62.7(4) . . . . ?
O17 Ti10 O16 Ti5 -178.9(3) . . . . ?
O17 Ti10 O18 Ti6 180.000(1) . . . . ?
O17 Ti10 O18 Ti7 -59.9(4) . . . 4_575 ?
O17 Ti10 O18 Ti7 59.9(4) . . . . ?
O18 Ti7 O13 Ti8 63.2(7) . . . . ?
O18 Ti7 O26 C29 148.3(17) . . . . ?
O18 Ti10 O16 Ti3 58.7(5) . . . . ?
O18 Ti10 O16 Ti4 179.3(4) . . . . ?
O18 Ti10 O16 Ti5 -62.4(5) . . . . ?
O18 Ti10 O17 Ti8 61.5(4) . . . 4_575 ?
O18 Ti10 O17 Ti8 -61.5(4) . . . . ?
O18 Ti10 O17 Ti9 180.000(1) . . . . ?
O18 Ti10 O17 Ti9 180.000(1) . . . 4_575 ?
O19 Ti8 O13 Ti7 -137.7(7) . . . . ?
O19 Ti8 O27 C27 91(2) . . . . ?
O21 Ti4 O15 Ti4 122.0(13) . . . 4_575 ?
O22 Ti4 O15 Ti4 -139.5(13) . . . 4_575 ?
O22 Ti4 O21 C23A 111(6) . . . . ?
O22 Ti4 O21 C23B -104(3) . . . . ?
O22 Ti5 O14 Ti5 138.2(13) . . . 4_575 ?
O22 Ti5 O23 C19 119(2) . . . . ?
O23 Ti5 O14 Ti5 -121.7(13) . . . 4_575 ?
O25 Ti7 O13 Ti8 136.7(7) . . . . ?
O25 Ti7 O26 C29 105.3(16) . . . . ?
O26 Ti7 O13 Ti8 -124.9(7) . . . . ?
O27 Ti8 O13 Ti7 123.2(8) . . . . ?
N1 Ti1 O9 Ti3 135.4(13) . . . . ?
N1 Ti1 O9 Ti8 -66.2(14) . . . . ?
N1 C1 C2 C3 -1(2) . . . . ?
N1 C5 C6 O3 2.2(15) . . . . ?
N1 C5 C6 O4 179.3(11) . . . . ?
N2 Ti2 O8 Ti5 104.7(12) . . . . ?
N2 Ti2 O8 Ti6 -94.0(12) . . . . ?
N2 C7 C8 C9 -0.9(18) . . . . ?
N2 C11 C12 O1 -3.1(15) . . . . ?
N2 C11 C12 O2 176.6(12) . . . . ?
C1 N1 C5 C4 0.5(18) . . . . ?
C1 N1 C5 C6 178.9(10) . . . . ?
C1 C2 C3 C4 0(2) . . . . ?
C2 C3 C4 C5 2(2) . . . . ?
C3 C4 C5 N1 -2(2) . . . . ?
C3 C4 C5 C6 179.7(12) . . . . ?
C4 C5 C6 O3 -179.5(11) . . . . ?
C4 C5 C6 O4 -2(2) . . . . ?
C5 N1 C1 C2 1(2) . . . . ?
C7 N2 C11 C10 -1.4(16) . . . . ?
C7 N2 C11 C12 179.0(10) . . . . ?
C7 C8 C9 C10 1.0(19) . . . . ?
C8 C9 C10 C11 -1.3(18) . . . . ?
C9 C10 C11 N2 1.5(17) . . . . ?
C9 C10 C11 C12 -179.0(11) . . . . ?
C10 C11 C12 O1 177.3(11) . . . . ?
C10 C11 C12 O2 -3(2) . . . . ?
C11 N2 C7 C8 1.1(17) . . . . ?
C25 O20 C25 C26 10(3) 4_575 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.363
_oxdiff_exptl_absorpt_empirical_full_min 0.667
# start Validation Reply Form
_vrf_PLAT029_ti17pa4             
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.824 Why?
RESPONSE: This is a minor problem caused by imperfect data collection.
;
_vrf_PLAT234_ti17pa4             
;
PROBLEM: Large Hirshfeld Difference C17 --C18 . 0.28 Ang.
RESPONSE: This problem is caused by the disorder of the atoms.
;
_vrf_PLAT341_ti17pa4             
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02347 Ang.
RESPONSE: Bond precision on C-C bonds does not affect the
determination of the binding modes of the ligands.
;
_vrf_PLAT911_ti17pa4             
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L= 0.600 1474 Report
RESPONSE: This problem is caused by the disorder of the atoms.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ti19pa19
_database_code_depnum_ccdc_archive 'CCDC 2126650'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2022-01-27 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2022-01-11
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C120 H90 N19 O70 Ti19, 0.5(C8 H24 N2)'
_chemical_formula_sum            'C124 H102 N20 O70 Ti19'
_chemical_formula_weight         3902.35
_chemical_absolute_configuration ?
_chemical_melting_point          ?
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'

_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.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           31
_space_group_name_H-M_alt        'P m n 21'
_space_group_name_Hall           'P 2ac -2'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y, z+1/2'
'-x, y, z'

_cell_length_a                   22.0234(10)
_cell_length_b                   15.8771(5)
_cell_length_c                   28.8999(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     10105.4(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    7646
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      71.1900
_cell_measurement_theta_min      3.0230
_shelx_estimated_absorpt_T_max   0.878
_shelx_estimated_absorpt_T_min   0.825
_exptl_absorpt_coefficient_mu    6.691
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71104
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3928
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0575
_diffrn_reflns_av_unetI/netI     0.0647
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35091
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.491
_diffrn_reflns_theta_min         2.783
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     38.00  83.00   1.00    9.30    --  106.49 -92.00  96.00   45
  2  ω     36.00 109.00   1.00    9.30    --  106.49-125.00  22.00   73
  3  ω     -3.00  23.00   1.00    0.55    --   48.45 -31.00-118.00   26
  4  ω     35.00  63.00   1.00    9.30    --  106.49 -57.00-120.00   28
  5  ω     98.00 160.00   1.00    9.30    --  106.49  31.00  41.00   62
  6  ω     98.00 176.00   1.00    9.30    --  106.49 125.00-120.00   78
  7  ω    -27.00  24.00   1.00    0.55    --  -48.45  19.00-150.00   51
  8  ω    -61.00 -23.00   1.00    9.30    --  -86.25  92.00-150.00   38
  9  ω    -41.00 -13.00   1.00    9.30    --  -86.25  38.00  30.00   28
 10  ω    -27.00  23.00   1.00    0.55    --  -48.45  19.00 150.00   50
 11  ω   -118.00 -74.00   1.00    0.55    --  -48.45-125.00  60.00   44
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0166552000
_diffrn_orient_matrix_UB_12      -0.0339982000
_diffrn_orient_matrix_UB_13      0.0792882000
_diffrn_orient_matrix_UB_21      0.0131621000
_diffrn_orient_matrix_UB_22      -0.0609224000
_diffrn_orient_matrix_UB_23      -0.0411230000
_diffrn_orient_matrix_UB_31      0.0488877000
_diffrn_orient_matrix_UB_32      0.0049444000
_diffrn_orient_matrix_UB_33      0.0380000000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.960
_reflns_Friedel_fraction_full    0.986
_reflns_Friedel_fraction_max     0.927
_reflns_number_gt                9510
_reflns_number_total             13913
_reflns_odcompleteness_completeness 98.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    ?
_refine_diff_density_max         0.662
_refine_diff_density_min         -0.430
_refine_diff_density_rms         0.078
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.328(14)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1208
_refine_ls_number_reflns         13913
_refine_ls_number_restraints     518
_refine_ls_R_factor_all          0.0965
_refine_ls_R_factor_gt           0.0704
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1320P)²+0.0545P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1918
_refine_ls_wR_factor_ref         0.2147
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.672(14)
 0.328(14)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 C66-C67
 1.45 with sigma of 0.02
 C45-C47
 2.35 with sigma of 0.02
 C47-C43
 2.35 with sigma of 0.02
 C44-C43 = C44-C45 = C46-C45 = C47-C46 = N1-C47 = N1-C43
 1.41 with sigma of 0.01
 O39B-C63A = O40A-C63A
 1.25 with sigma of 0.02
 O36-C54 = O37-C54
 1.25 with sigma of 0.02
 C44-C46
 2.35 with sigma of 0.02
 C47-C48
 1.45 with sigma of 0.02
 O39B-C63B
 1.25 with sigma of 0.02
 C46-N1
 2.35 with sigma of 0.02
 C42-C41
 1.53 with sigma of 0.02
 C43-C45
 2.35 with sigma of 0.02
 C55-C56 = C55-C57 = O38-C55
 1.45 with sigma of 0.01
 O38-C55
 1.45 with sigma of 0.02
 C57-C56
 2.35 with sigma of 0.01
 O38-C57
 2.35 with sigma of 0.01
 O38-C56
 2.35 with sigma of 0.02
 C2-C3 = C2-C1 = N7-C1 = N7-C5 = C5-C4 = C3-C4
 1.41 with sigma of 0.01
 C62B-C63B
 1.45 with sigma of 0.02
 C50-C51 = C50-C49 = N8-C49 = N8-C53 = C53-C52 = C52-C51
 1.41 with sigma of 0.02
 O40B-C63B = O39A-C63B
 1.25 with sigma of 0.02
 C62A-C63A
 1.45 with sigma of 0.02
 N9A-C62A = N9A-C58A = C59A-C58A = C60A-C59A = C61A-C60A = C62A-C61A
 1.41 with sigma of 0.02
 N9B-C62B = C62B-C61B = C61B-C60B = C60B-C59B = C59B-C58B = N9B-C58B
 1.41 with sigma of 0.02
 C65-C64
 1.45 with sigma of 0.02
 N11-C65
 1.45 with sigma of 0.02
 N11-C66
 1.45 with sigma of 0.02
 C67-C66
 1.45 with sigma of 0.02
 C4-C2
 2.35 with sigma of 0.02
 N7-C3
 2.8 with sigma of 0.02
 C5-C2
 2.8 with sigma of 0.02
 C4-C1
 2.8 with sigma of 0.02
4. Restrained planarity
 O24, O25, C43, C44, C45, C46, C47, C48
 with sigma of 0.01
 O39B, O40B, N9B, C58B, C59B, C60B, C61B, C62B, C63B
 with sigma of 0.01
 O36, O37, N8, C49, C50, C51, C52, C53, C54
 with sigma of 0.01
 O3, O4, N7, C1, C2, C3, C4, C5, C6
 with sigma of 0.01
 N9A, C58A, C59A, C60A, C61A, C62A
 with sigma of 0.01
 N2, C37, C38, C39, C40, C41
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
O24 \\sim O25 \\sim N1 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim
C48: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O39B \\sim O40B \\sim N9B \\sim C58B \\sim C59B \\sim C60B \\sim C61B \\sim
C62B \\sim C63B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O36 \\sim O37 \\sim N8 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim
C54: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O38 \\sim C55 \\sim C56 \\sim C57: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 2A
O3 \\sim O4 \\sim N7 \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O39A \\sim O40A \\sim N9A \\sim C58A \\sim C59A \\sim C60A \\sim C61A \\sim
C62A \\sim C63A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02 within 2A
O5 \\sim O6 \\sim N6 \\sim C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
N2 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.02 within 2A
N11 \\sim C64 \\sim C64 \\sim C65 \\sim C66 \\sim C67 \\sim C67: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
C25 \\sim C26 \\sim C27 \\sim C28 \\sim C29: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
6. Others
 Sof(O39B)=Sof(O40B)=Sof(N9B)=Sof(C58B)=Sof(H58B)=Sof(C59B)=Sof(H59B)=
 Sof(C60B)=Sof(H60B)=Sof(C61B)=Sof(H61B)=Sof(C62B)=Sof(C63B)=1-FVAR(1)
 Sof(O39A)=Sof(O40A)=Sof(N9A)=Sof(C58A)=Sof(H58A)=Sof(C59A)=Sof(H59A)=
 Sof(C60A)=Sof(H60A)=Sof(C61A)=Sof(H61A)=Sof(C62A)=Sof(C63A)=FVAR(1)
 Fixed Sof: O36(0.5) O37(0.5) N8(0.5) C49(0.5) H49(0.5) C50(0.5) H50(0.5)
 C51(0.5) H51(0.5) C52(0.5) H52(0.5) C53(0.5) C54(0.5) H11A(0.5) H11B(0.5)
 C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) C65(0.5) H65A(0.5) H65B(0.5) C66(0.5)
 H66A(0.5) H66B(0.5) C67(0.5) H67A(0.5) H67B(0.5) H67C(0.5)
7.a Ternary CH refined with riding coordinates:
 C55(H55)
7.b Secondary CH2 refined with riding coordinates:
 N11(H11A,H11B), C65(H65A,H65B), C66(H66A,H66B)
7.c Me refined with riding coordinates:
 C64(H64A,H64B,H64C), C67(H67A,H67B,H67C)
7.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C13(H13),
 C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25),
  C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34),
 C37(H37), C38(H38), C39(H39), C40(H40), C43(H43), C44(H44), C45(H45), C46(H46),
  C49(H49), C50(H50), C51(H51), C52(H52), C58A(H58A), C58B(H58B), C59A(H59A),
 C59B(H59B), C60A(H60A), C60B(H60B), C61A(H61A), C61B(H61B)
7.e Idealised Me refined as rotating group:
 C56(H56A,H56B,H56C), C57(H57A,H57B,H57C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.41943(14) 0.29450(13) 0.81840(8) 0.0917(7) Uani 1 1 d . . . . .
Ti2 Ti 0.41945(9) 0.18741(12) 0.70784(7) 0.0681(4) Uani 1 1 d . . . . .
Ti3 Ti 0.41942(8) 0.05481(10) 0.59555(7) 0.0606(4) Uani 1 1 d . . . . .
Ti4 Ti 0.41944(9) -0.01157(10) 0.48087(7) 0.0634(4) Uani 1 1 d . . . . .
Ti5 Ti 0.41293(8) 0.24008(10) 0.61156(6) 0.0623(4) Uani 1 1 d . . . . .
Ti6 Ti 0.41023(8) 0.21415(10) 0.49999(7) 0.0608(4) Uani 1 1 d . . . . .
Ti7 Ti 0.41900(8) 0.14938(10) 0.40617(6) 0.0595(4) Uani 1 1 d . . . . .
Ti8 Ti 0.41847(11) 0.21509(17) 0.28719(8) 0.0882(6) Uani 1 1 d . . . . .
Ti9 Ti 0.5000 0.33174(12) 0.54602(8) 0.0606(6) Uani 1 2 d S T P . .
Ti10 Ti 0.32113(11) 0.32789(14) 0.54957(8) 0.0885(6) Uani 1 1 d . . . . .
O1 O 0.5000 0.3184(8) 0.8206(4) 0.131(6) Uani 1 2 d S T P . .
O2 O 0.4113(4) 0.2408(6) 0.7667(3) 0.088(2) Uani 1 1 d . . . . .
O3 O 0.4136(5) 0.1935(8) 0.8558(3) 0.130(4) Uani 1 1 d . U . . .
O4 O 0.4215(6) 0.1288(13) 0.9241(5) 0.185(6) Uani 1 1 d . U . . .
O5 O 0.4029(6) 0.4108(6) 0.8015(5) 0.133(4) Uani 1 1 d . U . . .
O6 O 0.3320(9) 0.5087(9) 0.7855(8) 0.199(6) Uani 1 1 d . U . . .
O7 O 0.5000 0.1652(6) 0.7135(3) 0.072(2) Uani 1 2 d S T P . .
O8 O 0.4104(3) 0.1355(4) 0.6449(2) 0.0695(17) Uani 1 1 d . . . . .
O9 O 0.4164(3) 0.2828(4) 0.6713(2) 0.0689(17) Uani 1 1 d . . . . .
O10 O 0.3973(4) 0.0735(5) 0.7360(3) 0.085(2) Uani 1 1 d . . . . .
O11 O 0.3321(7) -0.0145(6) 0.7717(4) 0.135(4) Uani 1 1 d . . . . .
O12 O 0.5000 0.0380(5) 0.6020(3) 0.063(2) Uani 1 2 d S T P . .
O13 O 0.4039(4) -0.0512(5) 0.6349(2) 0.079(2) Uani 1 1 d . . . . .
O14 O 0.3381(6) -0.1364(7) 0.6680(4) 0.145(4) Uani 1 1 d . . . . .
O15 O 0.4141(3) -0.0169(4) 0.5391(2) 0.0685(16) Uani 1 1 d . . . . .
O16 O 0.5000 -0.0223(5) 0.4667(3) 0.069(2) Uani 1 2 d S T P . .
O17 O 0.3424(7) -0.2385(5) 0.4461(4) 0.143(5) Uani 1 1 d . . . . .
O18 O 0.4043(5) -0.1300(4) 0.4594(3) 0.092(3) Uani 1 1 d . . . . .
O19 O 0.4015(3) 0.0193(4) 0.3939(2) 0.0646(15) Uani 1 1 d . . . . .
O20 O 0.3452(5) -0.0727(5) 0.3546(3) 0.098(3) Uani 1 1 d . . . . .
O21 O 0.5000 0.1318(4) 0.4015(3) 0.059(2) Uani 1 2 d S T P . .
O22 O 0.4076(3) 0.1812(5) 0.3420(3) 0.0768(19) Uani 1 1 d . . . . .
O23 O 0.5000 0.2246(9) 0.2791(4) 0.106(4) Uani 1 2 d S T P . .
O24 O 0.4150(5) 0.0161(13) 0.1934(6) 0.178(6) Uani 1 1 d . U . . .
O25 O 0.4032(5) 0.1090(10) 0.2536(4) 0.139(4) Uani 1 1 d . U . . .
O26 O 0.4093(5) 0.3363(7) 0.2959(5) 0.117(4) Uani 1 1 d . . . . .
O27 O 0.3455(7) 0.4420(6) 0.3078(7) 0.175(7) Uani 1 1 d . . . . .
O28 O 0.4116(4) 0.2454(4) 0.4349(2) 0.0713(18) Uani 1 1 d . . . . .
O29 O 0.4083(3) 0.1046(4) 0.4698(2) 0.0646(16) Uani 1 1 d . . . . .
O30 O 0.5000 0.2422(4) 0.5031(3) 0.0528(17) Uani 1 2 d S T P A .
O31 O 0.3294(3) 0.2428(5) 0.5045(2) 0.0708(17) Uani 1 1 d . . . . .
O32 O 0.4137(2) 0.1518(3) 0.56005(19) 0.0467(11) Uani 1 1 d . . . . .
O33 O 0.4144(3) 0.3182(4) 0.5468(2) 0.0603(14) Uani 1 1 d . . . . .
O34 O 0.5000 0.2693(5) 0.6014(3) 0.0578(19) Uani 1 2 d S T P A .
O35 O 0.3322(4) 0.2708(5) 0.6018(3) 0.085(2) Uani 1 1 d . . . . .
O36 O 0.4985(9) 0.4493(6) 0.5712(4) 0.102(4) Uani 0.5 1 d D U P A -1
O37 O 0.4660(8) 0.5847(7) 0.5661(6) 0.119(6) Uani 0.5 1 d D U P A -1
O38 O 0.2384(5) 0.3357(8) 0.5472(4) 0.132(3) Uani 1 1 d D U . . .
O39A O 0.3263(14) 0.4462(14) 0.5849(12) 0.120(7) Uani 0.539(13) 1 d D U P B 4
O39B O 0.3351(8) 0.4401(13) 0.5808(14) 0.100(7) Uani 0.461(13) 1 d D U P B 3
O40A O 0.3078(12) 0.5704(10) 0.5893(6) 0.117(6) Uani 0.539(13) 1 d D U P B 4
O40B O 0.3593(8) 0.5863(10) 0.5807(6) 0.097(6) Uani 0.461(13) 1 d D U P B 3
N1 N 0.4107(8) 0.2401(10) 0.2089(4) 0.154(5) Uani 1 1 d D U . . .
N2 N 0.3161(5) 0.2358(7) 0.2790(3) 0.099(3) Uani 1 1 d . U . . .
N3 N 0.3160(4) 0.1325(6) 0.3967(3) 0.074(2) Uani 1 1 d . . . . .
N4 N 0.3190(4) 0.0434(7) 0.6025(3) 0.081(3) Uani 1 1 d . . . . .
N5 N 0.3188(5) 0.1794(6) 0.7125(3) 0.080(2) Uani 1 1 d . . . . .
N6 N 0.3169(6) 0.3028(5) 0.8265(4) 0.106(3) Uani 1 1 d . U . . .
N7 N 0.4145(5) 0.3420(11) 0.8900(5) 0.177(5) Uani 1 1 d D U . . .
N8 N 0.4935(8) 0.4194(8) 0.4854(5) 0.108(4) Uani 0.5 1 d D U P A -1
N9A N 0.3198(10) 0.4171(11) 0.4994(7) 0.104(5) Uani 0.539(13) 1 d D U P B 4
N9B N 0.3479(6) 0.4377(12) 0.4916(8) 0.091(5) Uani 0.461(13) 1 d D U P B 3
N10 N 0.3203(6) -0.0245(8) 0.4737(3) 0.093(3) Uani 1 1 d . . . . .
C1 C 0.4152(6) 0.4219(11) 0.9104(6) 0.202(6) Uani 1 1 d D U . . .
H1 H 0.4124 0.4706 0.8914 0.243 Uiso 1 1 calc R U . . .
C2 C 0.4200(7) 0.4309(13) 0.9589(6) 0.223(7) Uani 1 1 d D U . . .
H2 H 0.4204 0.4853 0.9726 0.267 Uiso 1 1 calc R U . . .
C3 C 0.4240(7) 0.3583(15) 0.9867(6) 0.222(7) Uani 1 1 d D U . . .
H3 H 0.4272 0.3649 1.0193 0.266 Uiso 1 1 calc R U . . .
C4 C 0.4235(6) 0.2778(13) 0.9684(6) 0.210(6) Uani 1 1 d D U . . .
H4 H 0.4262 0.2292 0.9874 0.252 Uiso 1 1 calc R U . . .
C5 C 0.4187(3) 0.2721(12) 0.9201(6) 0.184(5) Uani 1 1 d D U . . .
C6 C 0.4184(4) 0.2016(17) 0.9047(8) 0.163(5) Uani 1 1 d . U . . .
C7 C 0.2804(9) 0.2436(7) 0.8376(5) 0.117(4) Uani 1 1 d . U . . .
H7 H 0.2962 0.1901 0.8461 0.141 Uiso 1 1 calc R U . . .
C8 C 0.2205(11) 0.2558(8) 0.8373(6) 0.129(4) Uani 1 1 d . U . . .
H8 H 0.1942 0.2123 0.8477 0.155 Uiso 1 1 calc R U . . .
C9 C 0.1956(11) 0.3336(9) 0.8216(7) 0.137(4) Uani 1 1 d . U . . .
H9 H 0.1531 0.3430 0.8207 0.165 Uiso 1 1 calc R U . . .
C10 C 0.2351(10) 0.3928(8) 0.8080(7) 0.134(4) Uani 1 1 d . U . . .
H10 H 0.2216 0.4457 0.7966 0.161 Uiso 1 1 calc R U . . .
C11 C 0.2941(10) 0.3748(7) 0.8112(6) 0.124(4) Uani 1 1 d . U . . .
C12 C 0.3449(11) 0.4317(10) 0.7933(8) 0.144(4) Uani 1 1 d . U . . .
C13 C 0.2758(6) 0.2380(9) 0.6985(5) 0.097(4) Uani 1 1 d . . . . .
H13 H 0.2903 0.2865 0.6827 0.116 Uiso 1 1 calc R U . . .
C14 C 0.2124(8) 0.2321(14) 0.7054(5) 0.118(5) Uani 1 1 d . . . . .
H14 H 0.1852 0.2745 0.6950 0.141 Uiso 1 1 calc R U . . .
C15 C 0.1939(9) 0.1663(16) 0.7266(9) 0.148(8) Uani 1 1 d . . . . .
H15 H 0.1515 0.1596 0.7311 0.177 Uiso 1 1 calc R U . . .
C16 C 0.2321(9) 0.1039(12) 0.7433(5) 0.116(5) Uani 1 1 d . . . . .
H16 H 0.2165 0.0572 0.7600 0.139 Uiso 1 1 calc R U . . .
C17 C 0.2989(7) 0.1128(8) 0.7341(4) 0.091(3) Uani 1 1 d . . . . .
C18 C 0.3439(7) 0.0523(7) 0.7471(4) 0.094(4) Uani 1 1 d . . . . .
C19 C 0.2747(6) 0.0987(7) 0.5878(4) 0.086(3) Uani 1 1 d . . . . .
H19 H 0.2868 0.1441 0.5685 0.103 Uiso 1 1 calc R U . . .
C20 C 0.2175(6) 0.0929(13) 0.5985(7) 0.121(5) Uani 1 1 d . . . . .
H20 H 0.1889 0.1324 0.5869 0.145 Uiso 1 1 calc R U . . .
C21 C 0.1994(10) 0.028(2) 0.6272(8) 0.158(9) Uani 1 1 d . . . . .
H21 H 0.1581 0.0237 0.6364 0.190 Uiso 1 1 calc R U . . .
C22 C 0.2403(10) -0.0284(12) 0.6421(7) 0.127(6) Uani 1 1 d . . . . .
H22 H 0.2281 -0.0740 0.6613 0.152 Uiso 1 1 calc R U . . .
C23 C 0.3005(6) -0.0196(9) 0.6292(4) 0.090(4) Uani 1 1 d . . . . .
C24 C 0.3507(9) -0.0753(8) 0.6470(5) 0.106(5) Uani 1 1 d . . . . .
C25 C 0.2800(7) 0.0299(13) 0.4821(6) 0.118(4) Uani 1 1 d . U . . .
H25 H 0.2922 0.0865 0.4873 0.142 Uiso 1 1 calc R U . . .
C26 C 0.2140(9) 0.0091(14) 0.4843(7) 0.136(4) Uani 1 1 d . U . . .
H26 H 0.1859 0.0515 0.4933 0.164 Uiso 1 1 calc R U . . .
C27 C 0.1939(10) -0.0669(14) 0.4741(7) 0.143(4) Uani 1 1 d . U . . .
H27 H 0.1520 -0.0814 0.4744 0.172 Uiso 1 1 calc R U . . .
C28 C 0.2379(9) -0.1221(12) 0.4630(6) 0.127(4) Uani 1 1 d . U . . .
H28 H 0.2257 -0.1763 0.4526 0.152 Uiso 1 1 calc R U . . .
C29 C 0.3006(8) -0.1057(8) 0.4657(5) 0.110(4) Uani 1 1 d . U . . .
C30 C 0.3523(9) -0.1664(8) 0.4537(5) 0.108(5) Uani 1 1 d . . . . .
C31 C 0.2737(7) 0.1871(10) 0.4030(4) 0.102(4) Uani 1 1 d . . . . .
H31 H 0.2834 0.2387 0.4179 0.122 Uiso 1 1 calc R U . . .
C32 C 0.2149(9) 0.1735(18) 0.3889(6) 0.147(8) Uani 1 1 d . . . . .
H32 H 0.1854 0.2169 0.3917 0.176 Uiso 1 1 calc R U . . .
C33 C 0.1993(7) 0.0981(18) 0.3711(7) 0.167(10) Uani 1 1 d . . . . .
H33 H 0.1581 0.0870 0.3634 0.200 Uiso 1 1 calc R U . . .
C34 C 0.2418(7) 0.0380(12) 0.3641(5) 0.120(5) Uani 1 1 d . . . . .
H34 H 0.2319 -0.0146 0.3505 0.144 Uiso 1 1 calc R U . . .
C35 C 0.3008(5) 0.0568(8) 0.3780(4) 0.085(3) Uani 1 1 d . . . . .
C36 C 0.3541(7) -0.0064(7) 0.3739(4) 0.089(3) Uani 1 1 d . . . . .
C37 C 0.2760(8) 0.1798(10) 0.2681(4) 0.114(4) Uani 1 1 d . U . . .
H37 H 0.2881 0.1234 0.2622 0.137 Uiso 1 1 calc R U . . .
C38 C 0.2161(9) 0.2016(10) 0.2652(4) 0.126(4) Uani 1 1 d . U . . .
H38 H 0.1869 0.1601 0.2572 0.152 Uiso 1 1 calc R U . . .
C39 C 0.1979(10) 0.2815(11) 0.2735(5) 0.144(4) Uani 1 1 d . U . . .
H39 H 0.1564 0.2971 0.2715 0.172 Uiso 1 1 calc R U . . .
C40 C 0.2415(9) 0.3385(10) 0.2848(6) 0.138(4) Uani 1 1 d . U . . .
H40 H 0.2307 0.3954 0.2909 0.165 Uiso 1 1 calc R U . . .
C41 C 0.3047(7) 0.3121(9) 0.2876(5) 0.118(4) Uani 1 1 d D U . . .
C42 C 0.3575(11) 0.3719(8) 0.2990(8) 0.153(8) Uani 1 1 d D . . . .
C43 C 0.4112(6) 0.3179(11) 0.1874(5) 0.171(5) Uani 1 1 d D U . . .
H43 H 0.4059 0.3673 0.2055 0.205 Uiso 1 1 calc R U . . .
C44 C 0.4192(6) 0.3252(14) 0.1400(5) 0.193(6) Uani 1 1 d D U . . .
H44 H 0.4208 0.3790 0.1256 0.232 Uiso 1 1 calc R U . . .
C45 C 0.4249(6) 0.2515(15) 0.1138(5) 0.194(6) Uani 1 1 d D U . . .
H45 H 0.4304 0.2553 0.0813 0.233 Uiso 1 1 calc R U . . .
C46 C 0.4226(5) 0.1732(14) 0.1347(5) 0.181(6) Uani 1 1 d D U . . .
H46 H 0.4265 0.1236 0.1166 0.217 Uiso 1 1 calc R U . . .
C47 C 0.4145(3) 0.1674(10) 0.1822(4) 0.157(5) Uani 1 1 d D U . . .
C48 C 0.4106(3) 0.0904(14) 0.2124(6) 0.148(4) Uani 1 1 d D U . . .
C49 C 0.4918(10) 0.3986(10) 0.4389(6) 0.113(5) Uani 0.5 1 d D U P A -1
H49 H 0.5034 0.3436 0.4295 0.136 Uiso 0.5 1 calc R U P A -1
C50 C 0.4730(9) 0.4585(11) 0.4046(8) 0.116(6) Uani 0.5 1 d D U P A -1
H50 H 0.4719 0.4446 0.3727 0.139 Uiso 0.5 1 calc R U P A -1
C51 C 0.4565(10) 0.5388(13) 0.4206(8) 0.119(6) Uani 0.5 1 d D U P A -1
H51 H 0.4439 0.5792 0.3984 0.143 Uiso 0.5 1 calc R U P A -1
C52 C 0.4573(8) 0.5628(13) 0.4666(8) 0.114(5) Uani 0.5 1 d D U P A -1
H52 H 0.4459 0.6175 0.4767 0.137 Uiso 0.5 1 calc R U P A -1
C53 C 0.4763(5) 0.4997(9) 0.4969(7) 0.104(5) Uani 0.5 1 d D U P A -1
C54 C 0.4803(6) 0.5142(8) 0.5501(7) 0.103(5) Uani 0.5 1 d D U P A -1
C55 C 0.1737(6) 0.3482(12) 0.5384(6) 0.152(5) Uani 1 1 d D U . . .
H55 H 0.1662 0.3812 0.5095 0.182 Uiso 1 1 calc R U . . .
C56 C 0.1468(11) 0.2642(13) 0.5362(10) 0.220(10) Uani 1 1 d D U . . .
H56A H 0.1367 0.2506 0.5040 0.330 Uiso 1 1 calc R U . . .
H56B H 0.1098 0.2628 0.5550 0.330 Uiso 1 1 calc R U . . .
H56C H 0.1758 0.2227 0.5481 0.330 Uiso 1 1 calc R U . . .
C57 C 0.1483(9) 0.3894(15) 0.5793(9) 0.206(9) Uani 1 1 d D U . . .
H57A H 0.1573 0.3556 0.6068 0.309 Uiso 1 1 calc R U . . .
H57B H 0.1042 0.3947 0.5758 0.309 Uiso 1 1 calc R U . . .
H57C H 0.1663 0.4455 0.5827 0.309 Uiso 1 1 calc R U . . .
C58A C 0.3188(10) 0.4179(13) 0.4503(7) 0.101(5) Uani 0.539(13) 1 d D U P B 4
H58A H 0.3268 0.3651 0.4360 0.121 Uiso 0.539(13) 1 calc R U P B 4
C58B C 0.3527(8) 0.4237(14) 0.4440(8) 0.090(5) Uani 0.461(13) 1 d D U P B 3
H58B H 0.3456 0.3693 0.4314 0.108 Uiso 0.461(13) 1 calc R U P B 3
C59A C 0.3077(11) 0.4853(11) 0.4191(8) 0.108(6) Uani 0.539(13) 1 d D U P B 4
H59A H 0.3084 0.4773 0.3865 0.130 Uiso 0.539(13) 1 calc R U P B 4
C59B C 0.3684(8) 0.4926(12) 0.4146(8) 0.096(6) Uani 0.461(13) 1 d D U P B 3
H59B H 0.3721 0.4860 0.3821 0.116 Uiso 0.461(13) 1 calc R U P B 3
C60A C 0.2956(11) 0.5649(11) 0.4389(7) 0.110(6) Uani 0.539(13) 1 d D U P B 4
H60A H 0.2877 0.6129 0.4202 0.132 Uiso 0.539(13) 1 calc R U P B 4
C60B C 0.3782(9) 0.5714(14) 0.4364(7) 0.102(6) Uani 0.461(13) 1 d D U P B 3
H60B H 0.3887 0.6179 0.4174 0.123 Uiso 0.461(13) 1 calc R U P B 3
C61A C 0.2957(11) 0.5699(12) 0.4883(7) 0.111(6) Uani 0.539(13) 1 d D U P B 4
H61A H 0.2878 0.6224 0.5028 0.133 Uiso 0.539(13) 1 calc R U P B 4
C61B C 0.3734(8) 0.5850(14) 0.4840(7) 0.100(6) Uani 0.461(13) 1 d D U P B 3
H61B H 0.3804 0.6392 0.4969 0.120 Uiso 0.461(13) 1 calc R U P B 3
C62A C 0.3073(11) 0.4990(11) 0.5159(7) 0.112(5) Uani 0.539(13) 1 d D U P B 4
C62B C 0.3577(5) 0.5155(11) 0.5127(7) 0.094(5) Uani 0.461(13) 1 d D U P B 3
C63A C 0.3100(17) 0.5062(12) 0.5662(7) 0.113(5) Uani 0.539(13) 1 d D U P B 4
C63B C 0.3496(6) 0.5132(10) 0.5643(7) 0.099(5) Uani 0.461(13) 1 d D U P B 3
N11 N 0.5000 -0.0875(9) 0.3596(5) 0.099(4) Uani 1 2 d DS TU P . .
H11A H 0.5287 -0.0625 0.3776 0.118 Uiso 0.5 1 calc R U P C .
H11B H 0.4631 -0.0696 0.3697 0.118 Uiso 0.5 1 calc R U P . .
C64 C 0.4563(14) -0.2371(19) 0.3561(11) 0.110(8) Uani 0.5 1 d D U P C -1
H64A H 0.4710 -0.2937 0.3637 0.165 Uiso 0.5 1 calc R U P C -1
H64B H 0.4204 -0.2243 0.3749 0.165 Uiso 0.5 1 calc R U P C -1
H64C H 0.4457 -0.2345 0.3232 0.165 Uiso 0.5 1 calc R U P C -1
C65 C 0.504(2) -0.1759(11) 0.3660(8) 0.105(5) Uani 0.5 1 d D U P C -1
H65A H 0.5144 -0.1843 0.3989 0.126 Uiso 0.5 1 calc R U P C -1
H65B H 0.5394 -0.1944 0.3479 0.126 Uiso 0.5 1 calc R U P C -1
C66 C 0.5084(17) -0.0588(13) 0.3113(6) 0.104(5) Uani 0.5 1 d D U P C -1
H66A H 0.5082 0.0035 0.3115 0.125 Uiso 0.5 1 calc R U P C -1
H66B H 0.5493 -0.0769 0.3012 0.125 Uiso 0.5 1 calc R U P C -1
C67 C 0.4651(13) -0.087(2) 0.2764(8) 0.108(7) Uani 0.5 1 d D U P C -1
H67A H 0.4764 -0.0627 0.2463 0.161 Uiso 0.5 1 calc R U P C -1
H67B H 0.4656 -0.1482 0.2746 0.161 Uiso 0.5 1 calc R U P C -1
H67C H 0.4243 -0.0673 0.2849 0.161 Uiso 0.5 1 calc R U P C -1


_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 1.816(4) . ?
Ti1 O2 1.730(8) . ?
Ti1 O3 1.938(10) . ?
Ti1 O5 1.944(10) . ?
Ti1 N6 2.274(14) . ?
Ti1 N7 2.205(13) . ?
Ti2 O2 1.908(8) . ?
Ti2 O7 1.816(3) . ?
Ti2 O8 2.006(7) . ?
Ti2 O9 1.848(6) . ?
Ti2 O10 2.043(8) . ?
Ti2 N5 2.225(10) . ?
Ti3 O8 1.928(7) . ?
Ti3 O12 1.804(2) . ?
Ti3 O13 2.059(7) . ?
Ti3 O15 1.992(7) . ?
Ti3 O32 1.855(5) . ?
Ti3 N4 2.229(9) . ?
Ti4 O15 1.690(7) . ?
Ti4 O16 1.828(3) . ?
Ti4 O18 2.008(6) . ?
Ti4 O19 2.591(7) . ?
Ti4 O29 1.888(7) . ?
Ti4 N10 2.204(12) . ?
Ti5 Ti9 3.063(2) 4_655 ?
Ti5 O8 1.920(7) . ?
Ti5 O9 1.857(7) . ?
Ti5 O32 2.045(6) . ?
Ti5 O33 2.246(7) . ?
Ti5 O34 1.995(3) . ?
Ti5 O35 1.865(8) . ?
Ti6 O28 1.946(7) . ?
Ti6 O29 1.946(7) . ?
Ti6 O30 2.029(2) . ?
Ti6 O31 1.842(7) . ?
Ti6 O32 2.000(6) . ?
Ti6 O33 2.137(6) . ?
Ti7 O19 2.131(6) . ?
Ti7 O21 1.811(2) . ?
Ti7 O22 1.939(7) . ?
Ti7 O28 1.744(7) . ?
Ti7 O29 1.987(6) . ?
Ti7 N3 2.302(9) . ?
Ti8 O22 1.689(8) . ?
Ti8 O23 1.817(3) . ?
Ti8 O25 1.974(13) . ?
Ti8 O26 1.951(12) . ?
Ti8 N1 2.304(11) . ?
Ti8 N2 2.291(11) . ?
Ti9 Ti6 3.027(2) 4_655 ?
Ti9 Ti9 0.000(5) 4_655 ?
Ti9 O30 1.885(8) . ?
Ti9 O33 1.898(6) . ?
Ti9 O33 1.898(6) 4_655 ?
Ti9 O34 1.882(8) . ?
Ti9 O36 2.004(10) . ?
Ti9 N8 2.242(13) . ?
Ti10 O31 1.886(7) . ?
Ti10 O33 2.061(6) . ?
Ti10 O35 1.778(8) . ?
Ti10 O38 1.827(11) . ?
Ti10 O39A 2.14(3) . ?
Ti10 O39B 2.02(3) . ?
Ti10 N9A 2.03(2) . ?
Ti10 N9B 2.49(2) . ?
O1 Ti1 1.816(4) 4_655 ?
O3 C6 1.42(3) . ?
O4 C6 1.29(3) . ?
O5 C12 1.34(3) . ?
O6 C12 1.28(2) . ?
O7 Ti2 1.816(3) 4_655 ?
O10 C18 1.263(16) . ?
O11 C18 1.305(15) . ?
O12 Ti3 1.804(2) 4_655 ?
O13 C24 1.281(19) . ?
O14 C24 1.178(14) . ?
O16 Ti4 1.828(3) 4_655 ?
O17 C30 1.186(14) . ?
O18 C30 1.293(18) . ?
O19 C36 1.262(15) . ?
O20 C36 1.208(13) . ?
O21 Ti7 1.811(2) 4_655 ?
O23 Ti8 1.817(3) 4_655 ?
O24 C48 1.31(2) . ?
O25 C48 1.236(19) . ?
O26 C42 1.28(2) . ?
O27 C42 1.173(18) . ?
O30 Ti6 2.029(2) 4_655 ?
O30 Ti9 1.885(8) 4_655 ?
O33 Ti9 1.898(6) 4_655 ?
O34 Ti5 1.995(3) 4_655 ?
O34 Ti9 1.882(8) 4_655 ?
O36 C54 1.263(16) . ?
O37 C54 1.252(17) . ?
O38 C55 1.462(10) . ?
O39A C63A 1.15(3) . ?
O39B C63B 1.30(2) . ?
O40A C63A 1.220(18) . ?
O40B C63B 1.273(18) . ?
N1 C43 1.382(11) . ?
N1 C47 1.391(11) . ?
N2 C37 1.292(17) . ?
N2 C41 1.262(18) . ?
N3 C31 1.286(16) . ?
N3 C35 1.359(15) . ?
N4 C19 1.380(15) . ?
N4 C23 1.329(15) . ?
N5 C13 1.388(17) . ?
N5 C17 1.304(16) . ?
N6 C7 1.278(18) . ?
N6 C11 1.324(19) . ?
N7 C1 1.399(11) . ?
N7 C5 1.413(11) . ?
N8 C49 1.385(18) . ?
N8 C53 1.371(17) . ?
N9A C58A 1.420(19) . ?
N9A C62A 1.412(18) . ?
N9B C58B 1.40(2) . ?
N9B C62B 1.394(19) . ?
N10 C25 1.26(2) . ?
N10 C29 1.378(15) . ?
C1 H1 0.9500 . ?
C1 C2 1.414(11) . ?
C2 H2 0.9500 . ?
C2 C3 1.408(11) . ?
C3 H3 0.9500 . ?
C3 C4 1.384(11) . ?
C4 H4 0.9500 . ?
C4 C5 1.402(11) . ?
C5 C6 1.20(3) . ?
C7 H7 0.9500 . ?
C7 C8 1.33(3) . ?
C8 H8 0.9500 . ?
C8 C9 1.43(2) . ?
C9 H9 0.9500 . ?
C9 C10 1.34(2) . ?
C10 H10 0.9500 . ?
C10 C11 1.33(3) . ?
C11 C12 1.53(3) . ?
C13 H13 0.9500 . ?
C13 C14 1.41(2) . ?
C14 H14 0.9500 . ?
C14 C15 1.28(3) . ?
C15 H15 0.9500 . ?
C15 C16 1.38(3) . ?
C16 H16 0.9500 . ?
C16 C17 1.50(2) . ?
C17 C18 1.43(2) . ?
C19 H19 0.9500 . ?
C19 C20 1.300(19) . ?
C20 H20 0.9500 . ?
C20 C21 1.38(3) . ?
C21 H21 0.9500 . ?
C21 C22 1.35(3) . ?
C22 H22 0.9500 . ?
C22 C23 1.38(2) . ?
C23 C24 1.51(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.49(2) . ?
C26 H26 0.9500 . ?
C26 C27 1.32(3) . ?
C27 H27 0.9500 . ?
C27 C28 1.35(3) . ?
C28 H28 0.9500 . ?
C28 C29 1.41(2) . ?
C29 C30 1.53(2) . ?
C31 H31 0.9500 . ?
C31 C32 1.37(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.35(3) . ?
C33 H33 0.9500 . ?
C33 C34 1.35(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.391(18) . ?
C35 C36 1.549(19) . ?
C37 H37 0.9500 . ?
C37 C38 1.37(2) . ?
C38 H38 0.9500 . ?
C38 C39 1.35(2) . ?
C39 H39 0.9500 . ?
C39 C40 1.36(2) . ?
C40 H40 0.9500 . ?
C40 C41 1.46(2) . ?
C41 C42 1.537(18) . ?
C43 H43 0.9500 . ?
C43 C44 1.388(11) . ?
C44 H44 0.9500 . ?
C44 C45 1.399(11) . ?
C45 H45 0.9500 . ?
C45 C46 1.383(11) . ?
C46 H46 0.9500 . ?
C46 C47 1.388(10) . ?
C47 C48 1.504(19) . ?
C49 H49 0.9500 . ?
C49 C50 1.433(18) . ?
C50 H50 0.9500 . ?
C50 C51 1.40(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.38(2) . ?
C52 H52 0.9500 . ?
C52 C53 1.392(19) . ?
C53 C54 1.56(3) . ?
C55 H55 1.0000 . ?
C55 C56 1.460(11) . ?
C55 C57 1.462(11) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58A H58A 0.9500 . ?
C58A C59A 1.420(19) . ?
C58B H58B 0.9500 . ?
C58B C59B 1.43(2) . ?
C59A H59A 0.9500 . ?
C59A C60A 1.413(19) . ?
C59B H59B 0.9500 . ?
C59B C60B 1.42(2) . ?
C60A H60A 0.9500 . ?
C60A C61A 1.43(2) . ?
C60B H60B 0.9500 . ?
C60B C61B 1.40(2) . ?
C61A H61A 0.9500 . ?
C61A C62A 1.403(19) . ?
C61B H61B 0.9500 . ?
C61B C62B 1.42(2) . ?
C62A C63A 1.46(2) . ?
C62B C63B 1.50(2) . ?
N11 H11A 0.9100 . ?
N11 H11B 0.9100 . ?
N11 C65 1.419(18) . ?
N11 C66 1.479(19) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C64 C65 1.45(2) . ?
C65 H65A 0.9900 . ?
C65 H65B 0.9900 . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
C66 C67 1.455(16) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O3 102.6(5) . . ?
O1 Ti1 O5 89.6(6) . . ?
O1 Ti1 N6 162.7(5) . . ?
O1 Ti1 N7 86.7(5) . . ?
O2 Ti1 O1 103.6(5) . . ?
O2 Ti1 O3 93.9(5) . . ?
O2 Ti1 O5 103.4(6) . . ?
O2 Ti1 N6 90.8(4) . . ?
O2 Ti1 N7 167.0(5) . . ?
O3 Ti1 O5 156.0(5) . . ?
O3 Ti1 N6 85.7(4) . . ?
O3 Ti1 N7 75.9(6) . . ?
O5 Ti1 N6 77.6(4) . . ?
O5 Ti1 N7 84.3(6) . . ?
N7 Ti1 N6 80.5(4) . . ?
O2 Ti2 O8 168.7(4) . . ?
O2 Ti2 O10 90.9(4) . . ?
O2 Ti2 N5 83.0(4) . . ?
O7 Ti2 O2 95.6(4) . . ?
O7 Ti2 O8 95.7(4) . . ?
O7 Ti2 O9 104.2(4) . . ?
O7 Ti2 O10 91.5(4) . . ?
O7 Ti2 N5 163.1(4) . . ?
O8 Ti2 O10 88.5(3) . . ?
O8 Ti2 N5 86.1(3) . . ?
O9 Ti2 O2 98.1(4) . . ?
O9 Ti2 O8 79.4(3) . . ?
O9 Ti2 O10 160.9(4) . . ?
O9 Ti2 N5 92.6(4) . . ?
O10 Ti2 N5 71.8(4) . . ?
O8 Ti3 O13 96.8(3) . . ?
O8 Ti3 O15 168.4(3) . . ?
O8 Ti3 N4 83.4(3) . . ?
O12 Ti3 O8 97.1(3) . . ?
O12 Ti3 O13 89.1(4) . . ?
O12 Ti3 O15 93.3(3) . . ?
O12 Ti3 O32 104.3(3) . . ?
O12 Ti3 N4 162.7(4) . . ?
O13 Ti3 N4 73.7(4) . . ?
O15 Ti3 O13 88.6(3) . . ?
O15 Ti3 N4 88.2(3) . . ?
O32 Ti3 O8 81.4(3) . . ?
O32 Ti3 O13 166.6(3) . . ?
O32 Ti3 O15 91.0(3) . . ?
O32 Ti3 N4 92.9(3) . . ?
O15 Ti4 O16 106.5(4) . . ?
O15 Ti4 O18 104.4(3) . . ?
O15 Ti4 O19 164.9(3) . . ?
O15 Ti4 O29 102.0(3) . . ?
O15 Ti4 N10 91.2(3) . . ?
O16 Ti4 O18 90.3(4) . . ?
O16 Ti4 O19 87.1(3) . . ?
O16 Ti4 O29 100.3(3) . . ?
O16 Ti4 N10 158.7(4) . . ?
O18 Ti4 O19 81.5(3) . . ?
O18 Ti4 N10 73.7(5) . . ?
O29 Ti4 O18 147.3(3) . . ?
O29 Ti4 O19 68.4(2) . . ?
O29 Ti4 N10 86.9(4) . . ?
N10 Ti4 O19 77.0(3) . . ?
O8 Ti5 Ti9 137.7(2) . 4_655 ?
O8 Ti5 O32 76.9(3) . . ?
O8 Ti5 O33 153.7(3) . . ?
O8 Ti5 O34 107.7(3) . . ?
O9 Ti5 Ti9 112.1(2) . 4_655 ?
O9 Ti5 O8 81.4(3) . . ?
O9 Ti5 O32 158.0(3) . . ?
O9 Ti5 O33 124.9(3) . . ?
O9 Ti5 O34 90.7(3) . . ?
O9 Ti5 O35 94.9(3) . . ?
O32 Ti5 Ti9 82.53(16) . 4_655 ?
O32 Ti5 O33 76.8(2) . . ?
O33 Ti5 Ti9 38.12(16) . 4_655 ?
O34 Ti5 Ti9 36.5(2) . 4_655 ?
O34 Ti5 O32 92.5(3) . . ?
O34 Ti5 O33 74.6(3) . . ?
O35 Ti5 Ti9 112.3(3) . 4_655 ?
O35 Ti5 O8 105.9(4) . . ?
O35 Ti5 O32 94.4(3) . . ?
O35 Ti5 O33 75.1(3) . . ?
O35 Ti5 O34 146.5(4) . . ?
O28 Ti6 O30 88.4(3) . . ?
O28 Ti6 O32 164.8(3) . . ?
O28 Ti6 O33 114.5(3) . . ?
O29 Ti6 O28 78.2(3) . . ?
O29 Ti6 O30 103.8(3) . . ?
O29 Ti6 O32 87.0(2) . . ?
O29 Ti6 O33 167.2(3) . . ?
O30 Ti6 O33 76.1(3) . . ?
O31 Ti6 O28 91.2(3) . . ?
O31 Ti6 O29 103.4(3) . . ?
O31 Ti6 O30 152.2(3) . . ?
O31 Ti6 O32 95.6(3) . . ?
O31 Ti6 O33 78.8(3) . . ?
O32 Ti6 O30 91.8(3) . . ?
O32 Ti6 O33 80.3(2) . . ?
O19 Ti7 N3 71.9(3) . . ?
O21 Ti7 O19 90.9(3) . . ?
O21 Ti7 O22 95.5(3) . . ?
O21 Ti7 O29 97.5(3) . . ?
O21 Ti7 N3 160.8(4) . . ?
O22 Ti7 O19 94.0(3) . . ?
O22 Ti7 O29 164.6(3) . . ?
O22 Ti7 N3 77.8(3) . . ?
O28 Ti7 O19 155.5(3) . . ?
O28 Ti7 O21 105.2(4) . . ?
O28 Ti7 O22 102.4(3) . . ?
O28 Ti7 O29 82.0(3) . . ?
O28 Ti7 N3 93.8(4) . . ?
O29 Ti7 O19 77.6(3) . . ?
O29 Ti7 N3 87.2(3) . . ?
O22 Ti8 O23 106.7(5) . . ?
O22 Ti8 O25 99.5(5) . . ?
O22 Ti8 O26 100.3(5) . . ?
O22 Ti8 N1 164.8(5) . . ?
O22 Ti8 N2 90.2(4) . . ?
O23 Ti8 O25 100.2(6) . . ?
O23 Ti8 O26 92.1(6) . . ?
O23 Ti8 N1 86.1(6) . . ?
O23 Ti8 N2 161.3(5) . . ?
O25 Ti8 N1 69.6(6) . . ?
O25 Ti8 N2 84.4(4) . . ?
O26 Ti8 O25 152.6(5) . . ?
O26 Ti8 N1 87.0(6) . . ?
O26 Ti8 N2 76.7(4) . . ?
N2 Ti8 N1 78.5(5) . . ?
Ti9 Ti9 Ti6 0(10) 4_655 4_655 ?
Ti9 Ti9 O30 0(10) 4_655 . ?
Ti9 Ti9 O33 0(10) 4_655 . ?
Ti9 Ti9 O33 0(10) 4_655 4_655 ?
Ti9 Ti9 O34 0(10) 4_655 . ?
Ti9 Ti9 O36 0(10) 4_655 . ?
Ti9 Ti9 N8 0(10) 4_655 . ?
O30 Ti9 Ti6 41.09(5) . 4_655 ?
O30 Ti9 O33 85.53(19) . 4_655 ?
O30 Ti9 O33 85.53(19) . . ?
O30 Ti9 O36 160.2(4) . . ?
O30 Ti9 N8 87.4(4) . . ?
O33 Ti9 Ti6 44.47(18) 4_655 4_655 ?
O33 Ti9 Ti6 125.7(2) . 4_655 ?
O33 Ti9 O33 166.9(4) 4_655 . ?
O33 Ti9 O36 96.8(6) 4_655 . ?
O33 Ti9 O36 94.9(6) . . ?
O33 Ti9 N8 98.2(5) 4_655 . ?
O33 Ti9 N8 90.9(5) . . ?
O34 Ti9 Ti6 92.77(19) . 4_655 ?
O34 Ti9 O30 99.3(3) . . ?
O34 Ti9 O33 86.0(2) . 4_655 ?
O34 Ti9 O33 86.0(2) . . ?
O34 Ti9 O36 100.5(4) . . ?
O34 Ti9 N8 172.4(5) . . ?
O36 Ti9 Ti6 138.2(6) . 4_655 ?
O36 Ti9 N8 72.8(5) . . ?
N8 Ti9 Ti6 94.7(4) . 4_655 ?
O31 Ti10 O33 79.8(3) . . ?
O31 Ti10 O39A 162.4(7) . . ?
O31 Ti10 O39B 157.8(8) . . ?
O31 Ti10 N9A 90.5(5) . . ?
O31 Ti10 N9B 90.8(5) . . ?
O33 Ti10 O39A 91.8(9) . . ?
O33 Ti10 N9B 77.9(3) . . ?
O35 Ti10 O31 102.0(3) . . ?
O35 Ti10 O33 81.8(3) . . ?
O35 Ti10 O38 101.7(5) . . ?
O35 Ti10 O39A 92.0(8) . . ?
O35 Ti10 O39B 92.8(9) . . ?
O35 Ti10 N9A 165.0(7) . . ?
O35 Ti10 N9B 153.7(5) . . ?
O38 Ti10 O31 96.9(4) . . ?
O38 Ti10 O33 175.6(4) . . ?
O38 Ti10 O39A 90.6(9) . . ?
O38 Ti10 O39B 96.2(6) . . ?
O38 Ti10 N9A 84.9(8) . . ?
O38 Ti10 N9B 99.4(5) . . ?
O39B Ti10 O33 86.1(5) . . ?
O39B Ti10 N9B 69.4(10) . . ?
N9A Ti10 O33 92.2(7) . . ?
N9A Ti10 O39A 74.3(9) . . ?
Ti1 O1 Ti1 155.5(8) . 4_655 ?
Ti1 O2 Ti2 168.3(6) . . ?
C6 O3 Ti1 118.3(13) . . ?
C12 O5 Ti1 117.2(10) . . ?
Ti2 O7 Ti2 155.3(6) . 4_655 ?
Ti3 O8 Ti2 158.9(4) . . ?
Ti5 O8 Ti2 95.6(3) . . ?
Ti5 O8 Ti3 101.5(3) . . ?
Ti2 O9 Ti5 103.5(3) . . ?
C18 O10 Ti2 123.9(9) . . ?
Ti3 O12 Ti3 159.2(5) . 4_655 ?
C24 O13 Ti3 123.1(9) . . ?
Ti4 O15 Ti3 141.5(4) . . ?
Ti4 O16 Ti4 152.0(6) 4_655 . ?
C30 O18 Ti4 127.2(10) . . ?
Ti7 O19 Ti4 89.7(2) . . ?
C36 O19 Ti4 120.6(7) . . ?
C36 O19 Ti7 122.6(7) . . ?
Ti7 O21 Ti7 160.3(5) . 4_655 ?
Ti8 O22 Ti7 164.0(5) . . ?
Ti8 O23 Ti8 162.4(8) 4_655 . ?
C48 O25 Ti8 130.9(15) . . ?
C42 O26 Ti8 122.5(9) . . ?
Ti7 O28 Ti6 103.8(3) . . ?
Ti4 O29 Ti6 142.6(4) . . ?
Ti4 O29 Ti7 119.4(3) . . ?
Ti6 O29 Ti7 95.3(3) . . ?
Ti6 O30 Ti6 154.1(4) 4_655 . ?
Ti9 O30 Ti6 101.3(2) . 4_655 ?
Ti9 O30 Ti6 101.3(2) . . ?
Ti9 O30 Ti6 101.3(2) 4_655 . ?
Ti9 O30 Ti6 101.3(2) 4_655 4_655 ?
Ti9 O30 Ti9 0.00(11) 4_655 . ?
Ti6 O31 Ti10 108.6(4) . . ?
Ti3 O32 Ti5 99.6(3) . . ?
Ti3 O32 Ti6 153.4(3) . . ?
Ti6 O32 Ti5 107.0(2) . . ?
Ti6 O33 Ti5 95.8(2) . . ?
Ti9 O33 Ti5 95.0(3) 4_655 . ?
Ti9 O33 Ti5 95.0(3) . . ?
Ti9 O33 Ti6 97.1(3) 4_655 . ?
Ti9 O33 Ti6 97.1(3) . . ?
Ti9 O33 Ti9 0.00(14) 4_655 . ?
Ti9 O33 Ti10 169.1(4) 4_655 . ?
Ti9 O33 Ti10 169.1(4) . . ?
Ti10 O33 Ti5 89.7(3) . . ?
Ti10 O33 Ti6 92.3(3) . . ?
Ti5 O34 Ti5 148.0(4) . 4_655 ?
Ti9 O34 Ti5 104.4(2) . 4_655 ?
Ti9 O34 Ti5 104.4(2) . . ?
Ti9 O34 Ti5 104.4(2) 4_655 4_655 ?
Ti9 O34 Ti5 104.4(2) 4_655 . ?
Ti9 O34 Ti9 0.00(8) 4_655 . ?
Ti10 O35 Ti5 113.1(5) . . ?
C54 O36 Ti9 126.1(11) . . ?
C55 O38 Ti10 171.2(11) . . ?
C63A O39A Ti10 119(3) . . ?
C63B O39B Ti10 131(3) . . ?
C43 N1 Ti8 126.4(9) . . ?
C43 N1 C47 119.6(11) . . ?
C47 N1 Ti8 113.3(9) . . ?
C37 N2 Ti8 126.8(10) . . ?
C41 N2 Ti8 108.2(9) . . ?
C41 N2 C37 124.9(13) . . ?
C31 N3 Ti7 128.2(10) . . ?
C31 N3 C35 118.4(11) . . ?
C35 N3 Ti7 113.1(7) . . ?
C19 N4 Ti3 128.5(8) . . ?
C23 N4 Ti3 114.7(9) . . ?
C23 N4 C19 116.2(10) . . ?
C13 N5 Ti2 128.6(8) . . ?
C17 N5 Ti2 114.2(9) . . ?
C17 N5 C13 117.0(11) . . ?
C7 N6 Ti1 127.3(11) . . ?
C7 N6 C11 118.8(16) . . ?
C11 N6 Ti1 113.1(10) . . ?
C1 N7 Ti1 134.8(12) . . ?
C1 N7 C5 117.0(15) . . ?
C5 N7 Ti1 107.8(11) . . ?
C49 N8 Ti9 127.7(10) . . ?
C53 N8 Ti9 114.0(11) . . ?
C53 N8 C49 116.7(15) . . ?
C58A N9A Ti10 136.1(12) . . ?
C62A N9A Ti10 113.8(14) . . ?
C62A N9A C58A 109.1(17) . . ?
C58B N9B Ti10 124.7(13) . . ?
C62B N9B Ti10 111.2(14) . . ?
C62B N9B C58B 124(2) . . ?
C25 N10 Ti4 127.9(10) . . ?
C25 N10 C29 116.9(14) . . ?
C29 N10 Ti4 114.4(11) . . ?
N7 C1 H1 119.7 . . ?
N7 C1 C2 120.7(16) . . ?
C2 C1 H1 119.7 . . ?
C1 C2 H2 120.4 . . ?
C3 C2 C1 119.2(15) . . ?
C3 C2 H2 120.4 . . ?
C2 C3 H3 118.8 . . ?
C4 C3 C2 122.5(15) . . ?
C4 C3 H3 118.8 . . ?
C3 C4 H4 121.9 . . ?
C3 C4 C5 116.3(15) . . ?
C5 C4 H4 121.9 . . ?
C4 C5 N7 124.4(16) . . ?
C6 C5 N7 120.2(18) . . ?
C6 C5 C4 115.3(19) . . ?
O4 C6 O3 111(2) . . ?
C5 C6 O3 117(2) . . ?
C5 C6 O4 132(2) . . ?
N6 C7 H7 119.6 . . ?
N6 C7 C8 120.8(15) . . ?
C8 C7 H7 119.6 . . ?
C7 C8 H8 119.7 . . ?
C7 C8 C9 120.5(16) . . ?
C9 C8 H8 119.7 . . ?
C8 C9 H9 121.6 . . ?
C10 C9 C8 117(2) . . ?
C10 C9 H9 121.6 . . ?
C9 C10 H10 121.2 . . ?
C11 C10 C9 117.5(17) . . ?
C11 C10 H10 121.2 . . ?
N6 C11 C10 125.2(15) . . ?
N6 C11 C12 110.2(17) . . ?
C10 C11 C12 124.3(15) . . ?
O5 C12 C11 119.4(15) . . ?
O6 C12 O5 118.7(19) . . ?
O6 C12 C11 118(2) . . ?
N5 C13 H13 117.0 . . ?
N5 C13 C14 126.0(15) . . ?
C14 C13 H13 117.0 . . ?
C13 C14 H14 122.1 . . ?
C15 C14 C13 115.8(19) . . ?
C15 C14 H14 122.1 . . ?
C14 C15 H15 118.0 . . ?
C14 C15 C16 124.0(19) . . ?
C16 C15 H15 118.0 . . ?
C15 C16 H16 121.1 . . ?
C15 C16 C17 117.7(16) . . ?
C17 C16 H16 121.1 . . ?
N5 C17 C16 119.3(14) . . ?
N5 C17 C18 115.9(11) . . ?
C18 C17 C16 124.8(13) . . ?
O10 C18 O11 122.7(15) . . ?
O10 C18 C17 113.6(10) . . ?
O11 C18 C17 123.4(14) . . ?
N4 C19 H19 117.7 . . ?
C20 C19 N4 124.5(14) . . ?
C20 C19 H19 117.7 . . ?
C19 C20 H20 120.8 . . ?
C19 C20 C21 118.5(18) . . ?
C21 C20 H20 120.8 . . ?
C20 C21 H21 120.1 . . ?
C22 C21 C20 119.8(18) . . ?
C22 C21 H21 120.1 . . ?
C21 C22 H22 120.4 . . ?
C21 C22 C23 119.2(17) . . ?
C23 C22 H22 120.4 . . ?
N4 C23 C22 121.8(16) . . ?
N4 C23 C24 114.5(11) . . ?
C22 C23 C24 123.5(14) . . ?
O13 C24 C23 113.8(9) . . ?
O14 C24 O13 127.1(17) . . ?
O14 C24 C23 119.1(17) . . ?
N10 C25 H25 118.6 . . ?
N10 C25 C26 122.8(18) . . ?
C26 C25 H25 118.6 . . ?
C25 C26 H26 119.3 . . ?
C27 C26 C25 121(2) . . ?
C27 C26 H26 119.3 . . ?
C26 C27 H27 123.0 . . ?
C26 C27 C28 114.0(19) . . ?
C28 C27 H27 123.0 . . ?
C27 C28 H28 117.5 . . ?
C27 C28 C29 125.0(16) . . ?
C29 C28 H28 117.5 . . ?
N10 C29 C28 119.3(17) . . ?
N10 C29 C30 113.2(13) . . ?
C28 C29 C30 126.8(13) . . ?
O17 C30 O18 128.1(18) . . ?
O17 C30 C29 120.9(16) . . ?
O18 C30 C29 110.4(10) . . ?
N3 C31 H31 118.9 . . ?
N3 C31 C32 122.2(16) . . ?
C32 C31 H31 118.9 . . ?
C31 C32 H32 120.2 . . ?
C33 C32 C31 119.5(19) . . ?
C33 C32 H32 120.2 . . ?
C32 C33 H33 119.7 . . ?
C32 C33 C34 120.5(16) . . ?
C34 C33 H33 119.7 . . ?
C33 C34 H34 121.6 . . ?
C33 C34 C35 116.9(16) . . ?
C35 C34 H34 121.6 . . ?
N3 C35 C34 122.3(13) . . ?
N3 C35 C36 114.6(10) . . ?
C34 C35 C36 123.1(12) . . ?
O19 C36 C35 112.5(9) . . ?
O20 C36 O19 128.9(14) . . ?
O20 C36 C35 118.5(13) . . ?
N2 C37 H37 120.0 . . ?
N2 C37 C38 120.0(15) . . ?
C38 C37 H37 120.0 . . ?
C37 C38 H38 119.5 . . ?
C39 C38 C37 120.9(17) . . ?
C39 C38 H38 119.5 . . ?
C38 C39 H39 121.4 . . ?
C38 C39 C40 117.3(19) . . ?
C40 C39 H39 121.4 . . ?
C39 C40 H40 120.1 . . ?
C39 C40 C41 119.7(16) . . ?
C41 C40 H40 120.1 . . ?
N2 C41 C40 117.1(14) . . ?
N2 C41 C42 119.0(13) . . ?
C40 C41 C42 123.9(15) . . ?
O26 C42 C41 112.8(12) . . ?
O27 C42 O26 129.6(19) . . ?
O27 C42 C41 118(2) . . ?
N1 C43 H43 119.4 . . ?
N1 C43 C44 121.3(14) . . ?
C44 C43 H43 119.4 . . ?
C43 C44 H44 120.8 . . ?
C43 C44 C45 118.3(14) . . ?
C45 C44 H44 120.8 . . ?
C44 C45 H45 119.5 . . ?
C46 C45 C44 120.9(13) . . ?
C46 C45 H45 119.5 . . ?
C45 C46 H46 120.1 . . ?
C45 C46 C47 119.7(13) . . ?
C47 C46 H46 120.1 . . ?
N1 C47 C48 110.5(12) . . ?
C46 C47 N1 120.0(12) . . ?
C46 C47 C48 129.5(15) . . ?
O24 C48 C47 119.1(16) . . ?
O25 C48 O24 129(2) . . ?
O25 C48 C47 111.8(18) . . ?
N8 C49 H49 119.4 . . ?
N8 C49 C50 121.3(17) . . ?
C50 C49 H49 119.4 . . ?
C49 C50 H50 121.6 . . ?
C51 C50 C49 117(2) . . ?
C51 C50 H50 121.6 . . ?
C50 C51 H51 117.9 . . ?
C52 C51 C50 124(2) . . ?
C52 C51 H51 117.9 . . ?
C51 C52 H52 122.9 . . ?
C51 C52 C53 114(2) . . ?
C53 C52 H52 122.9 . . ?
N8 C53 C52 127(2) . . ?
N8 C53 C54 111.1(13) . . ?
C52 C53 C54 122.0(17) . . ?
O36 C54 C53 112.0(13) . . ?
O37 C54 O36 129.0(19) . . ?
O37 C54 C53 119.0(15) . . ?
O38 C55 H55 112.1 . . ?
O38 C55 C57 107.1(10) . . ?
C56 C55 O38 106.2(13) . . ?
C56 C55 H55 112.1 . . ?
C56 C55 C57 106.8(11) . . ?
C57 C55 H55 112.1 . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56B 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55 C57 H57A 109.5 . . ?
C55 C57 H57B 109.5 . . ?
C55 C57 H57C 109.5 . . ?
H57A C57 H57B 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
N9A C58A H58A 115.0 . . ?
N9A C58A C59A 130(2) . . ?
C59A C58A H58A 115.0 . . ?
N9B C58B H58B 120.6 . . ?
N9B C58B C59B 119(2) . . ?
C59B C58B H58B 120.6 . . ?
C58A C59A H59A 121.6 . . ?
C60A C59A C58A 117(2) . . ?
C60A C59A H59A 121.6 . . ?
C58B C59B H59B 121.6 . . ?
C60B C59B C58B 117(2) . . ?
C60B C59B H59B 121.6 . . ?
C59A C60A H60A 121.5 . . ?
C59A C60A C61A 117.0(19) . . ?
C61A C60A H60A 121.5 . . ?
C59B C60B H60B 117.9 . . ?
C61B C60B C59B 124(2) . . ?
C61B C60B H60B 117.9 . . ?
C60A C61A H61A 119.2 . . ?
C62A C61A C60A 121.6(19) . . ?
C62A C61A H61A 119.2 . . ?
C60B C61B H61B 120.9 . . ?
C60B C61B C62B 118(2) . . ?
C62B C61B H61B 120.9 . . ?
N9A C62A C63A 113.6(16) . . ?
C61A C62A N9A 125.5(19) . . ?
C61A C62A C63A 120.8(17) . . ?
N9B C62B C61B 118.0(19) . . ?
N9B C62B C63B 113.2(16) . . ?
C61B C62B C63B 128.7(17) . . ?
O39A C63A O40A 116(3) . . ?
O39A C63A C62A 115(2) . . ?
O40A C63A C62A 127.5(19) . . ?
O39B C63B C62B 115(2) . . ?
O40B C63B O39B 136(3) . . ?
O40B C63B C62B 109.2(16) . . ?
H11A N11 H11B 107.5 . . ?
C65 N11 H11A 108.6 . . ?
C65 N11 H11B 108.6 . . ?
C65 N11 C66 114.8(16) . . ?
C66 N11 H11A 108.6 . . ?
C66 N11 H11B 108.6 . . ?
H64A C64 H64B 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C65 C64 H64A 109.5 . . ?
C65 C64 H64B 109.5 . . ?
C65 C64 H64C 109.5 . . ?
N11 C65 C64 127(3) . . ?
N11 C65 H65A 105.7 . . ?
N11 C65 H65B 105.7 . . ?
C64 C65 H65A 105.7 . . ?
C64 C65 H65B 105.7 . . ?
H65A C65 H65B 106.1 . . ?
N11 C66 H66A 107.7 . . ?
N11 C66 H66B 107.7 . . ?
H66A C66 H66B 107.1 . . ?
C67 C66 N11 119(2) . . ?
C67 C66 H66A 107.7 . . ?
C67 C66 H66B 107.7 . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67B 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O3 C6 O4 -171.6(6) . . . . ?
Ti1 O3 C6 C5 8.4(7) . . . . ?
Ti1 O5 C12 O6 174.9(17) . . . . ?
Ti1 O5 C12 C11 19(2) . . . . ?
Ti1 N6 C7 C8 -174.4(12) . . . . ?
Ti1 N6 C11 C10 173.7(15) . . . . ?
Ti1 N6 C11 C12 -1.0(17) . . . . ?
Ti1 N7 C1 C2 -170.8(7) . . . . ?
Ti1 N7 C5 C4 173.2(5) . . . . ?
Ti1 N7 C5 C6 -6.8(5) . . . . ?
Ti2 O10 C18 O11 -168.6(9) . . . . ?
Ti2 O10 C18 C17 5.5(15) . . . . ?
Ti2 N5 C13 C14 -175.0(10) . . . . ?
Ti2 N5 C17 C16 174.5(9) . . . . ?
Ti2 N5 C17 C18 -5.9(13) . . . . ?
Ti3 O13 C24 O14 177.3(13) . . . . ?
Ti3 O13 C24 C23 0.7(15) . . . . ?
Ti3 N4 C19 C20 -170.4(11) . . . . ?
Ti3 N4 C23 C22 171.1(11) . . . . ?
Ti3 N4 C23 C24 -4.4(12) . . . . ?
Ti4 O18 C30 O17 -170.8(12) . . . . ?
Ti4 O18 C30 C29 0.0(15) . . . . ?
Ti4 O19 C36 O20 -89.1(14) . . . . ?
Ti4 O19 C36 C35 87.8(10) . . . . ?
Ti4 N10 C25 C26 -168.4(13) . . . . ?
Ti4 N10 C29 C28 176.7(11) . . . . ?
Ti4 N10 C29 C30 -11.9(14) . . . . ?
Ti6 Ti9 O30 Ti6 167.1(5) 4_655 . . . ?
Ti6 Ti9 O30 Ti9 0(66) 4_655 . . 4_655 ?
Ti6 Ti9 O33 Ti5 88.9(2) 4_655 . . . ?
Ti6 Ti9 O33 Ti6 -7.5(3) 4_655 . . . ?
Ti6 Ti9 O33 Ti9 0(100) 4_655 . . 4_655 ?
Ti6 Ti9 O33 Ti10 -156.1(19) 4_655 . . . ?
Ti6 Ti9 O34 Ti5 -123.8(3) 4_655 . . . ?
Ti6 Ti9 O34 Ti5 42.1(3) 4_655 . . 4_655 ?
Ti6 Ti9 O34 Ti9 0(100) 4_655 . . 4_655 ?
Ti7 O19 C36 O20 159.1(10) . . . . ?
Ti7 O19 C36 C35 -23.9(13) . . . . ?
Ti7 N3 C31 C32 169.1(12) . . . . ?
Ti7 N3 C35 C34 -172.0(12) . . . . ?
Ti7 N3 C35 C36 8.7(13) . . . . ?
Ti8 O25 C48 O24 160.5(8) . . . . ?
Ti8 O25 C48 C47 -19.5(9) . . . . ?
Ti8 O26 C42 O27 173(2) . . . . ?
Ti8 O26 C42 C41 -9(2) . . . . ?
Ti8 N1 C43 C44 166.1(7) . . . . ?
Ti8 N1 C47 C46 -167.3(5) . . . . ?
Ti8 N1 C47 C48 11.0(11) . . . . ?
Ti8 N2 C37 C38 179.0(8) . . . . ?
Ti8 N2 C41 C40 -179.3(8) . . . . ?
Ti8 N2 C41 C42 2.3(13) . . . . ?
Ti9 Ti5 O9 Ti2 -134.6(2) 4_655 . . . ?
Ti9 Ti5 O35 Ti10 12.7(5) 4_655 . . . ?
Ti9 Ti9 O30 Ti6 0.0(2) 4_655 . . 4_655 ?
Ti9 Ti9 O30 Ti6 0.0(2) 4_655 . . . ?
Ti9 Ti9 O33 Ti5 0.00(3) 4_655 . . . ?
Ti9 Ti9 O33 Ti6 0.00(2) 4_655 . . . ?
Ti9 Ti9 O33 Ti10 0.0(4) 4_655 . . . ?
Ti9 Ti9 O34 Ti5 0.0(2) 4_655 . . 4_655 ?
Ti9 Ti9 O34 Ti5 0.00(17) 4_655 . . . ?
Ti9 O36 C54 O37 163.2(12) . . . . ?
Ti9 O36 C54 C53 -16.8(12) . . . . ?
Ti9 N8 C49 C50 164.7(11) . . . . ?
Ti9 N8 C53 C52 -166.8(9) . . . . ?
Ti9 N8 C53 C54 13.2(9) . . . . ?
Ti10 O39A C63A O40A 173(2) . . . . ?
Ti10 O39A C63A C62A -20(5) . . . . ?
Ti10 O39B C63B O40B 180.0(10) . . . . ?
Ti10 O39B C63B C62B -0.1(10) . . . . ?
Ti10 N9A C58A C59A 168.0(19) . . . . ?
Ti10 N9A C62A C61A -171.0(15) . . . . ?
Ti10 N9A C62A C63A 12(2) . . . . ?
Ti10 N9B C58B C59B 179.9(7) . . . . ?
Ti10 N9B C62B C61B -180.0(7) . . . . ?
Ti10 N9B C62B C63B 0.0(7) . . . . ?
O1 Ti1 O2 Ti2 -6(3) . . . . ?
O2 Ti1 O1 Ti1 -52(2) . . . 4_655 ?
O2 Ti2 O7 Ti2 -89.5(13) . . . 4_655 ?
O2 Ti2 O9 Ti5 -172.3(4) . . . . ?
O3 Ti1 O1 Ti1 45(2) . . . 4_655 ?
O3 Ti1 O2 Ti2 -110(3) . . . . ?
O5 Ti1 O1 Ti1 -156(2) . . . 4_655 ?
O5 Ti1 O2 Ti2 87(3) . . . . ?
O7 Ti2 O9 Ti5 89.7(4) . . . . ?
O8 Ti2 O7 Ti2 90.7(13) . . . 4_655 ?
O8 Ti2 O9 Ti5 -3.5(3) . . . . ?
O8 Ti3 O12 Ti3 -84.4(15) . . . 4_655 ?
O8 Ti3 O32 Ti5 5.6(3) . . . . ?
O8 Ti3 O32 Ti6 -177.4(7) . . . . ?
O8 Ti5 O9 Ti2 3.6(3) . . . . ?
O8 Ti5 O35 Ti10 -148.7(4) . . . . ?
O9 Ti2 O7 Ti2 10.3(14) . . . 4_655 ?
O9 Ti5 O35 Ti10 128.9(4) . . . . ?
O10 Ti2 O7 Ti2 179.4(13) . . . 4_655 ?
O10 Ti2 O9 Ti5 -54.9(12) . . . . ?
O12 Ti3 O32 Ti5 -89.6(3) . . . . ?
O12 Ti3 O32 Ti6 87.5(7) . . . . ?
O13 Ti3 O12 Ti3 178.9(15) . . . 4_655 ?
O13 Ti3 O32 Ti5 88.6(12) . . . . ?
O13 Ti3 O32 Ti6 -94.3(14) . . . . ?
O15 Ti3 O12 Ti3 90.4(15) . . . 4_655 ?
O15 Ti3 O32 Ti5 176.7(3) . . . . ?
O15 Ti3 O32 Ti6 -6.2(7) . . . . ?
O15 Ti4 O16 Ti4 -26.7(12) . . . 4_655 ?
O15 Ti4 O29 Ti6 17.7(7) . . . . ?
O15 Ti4 O29 Ti7 173.5(4) . . . . ?
O16 Ti4 O15 Ti3 85.8(7) . . . . ?
O16 Ti4 O29 Ti6 -91.9(7) . . . . ?
O16 Ti4 O29 Ti7 63.9(5) . . . . ?
O18 Ti4 O15 Ti3 -179.5(6) . . . . ?
O18 Ti4 O16 Ti4 -131.8(11) . . . 4_655 ?
O18 Ti4 O29 Ti6 161.1(6) . . . . ?
O18 Ti4 O29 Ti7 -43.1(8) . . . . ?
O19 Ti4 O15 Ti3 -67.9(14) . . . . ?
O19 Ti4 O16 Ti4 146.7(11) . . . 4_655 ?
O19 Ti4 O29 Ti6 -174.5(7) . . . . ?
O19 Ti4 O29 Ti7 -18.7(3) . . . . ?
O19 Ti7 O21 Ti7 -164.3(14) . . . 4_655 ?
O19 Ti7 O28 Ti6 40.5(9) . . . . ?
O21 Ti7 O28 Ti6 -89.1(4) . . . . ?
O22 Ti7 O21 Ti7 101.6(14) . . . 4_655 ?
O22 Ti7 O28 Ti6 171.6(3) . . . . ?
O22 Ti8 O23 Ti8 15(3) . . . 4_655 ?
O23 Ti8 O22 Ti7 11(2) . . . . ?
O25 Ti8 O22 Ti7 114.4(19) . . . . ?
O25 Ti8 O23 Ti8 -89(3) . . . 4_655 ?
O26 Ti8 O22 Ti7 -84.7(19) . . . . ?
O26 Ti8 O23 Ti8 116(3) . . . 4_655 ?
O28 Ti6 O31 Ti10 -120.5(4) . . . . ?
O28 Ti7 O21 Ti7 -3.0(15) . . . 4_655 ?
O29 Ti4 O15 Ti3 -18.9(7) . . . . ?
O29 Ti4 O16 Ti4 79.3(11) . . . 4_655 ?
O29 Ti6 O31 Ti10 161.4(3) . . . . ?
O29 Ti7 O21 Ti7 -86.7(14) . . . 4_655 ?
O29 Ti7 O28 Ti6 6.6(3) . . . . ?
O30 Ti6 O31 Ti10 -31.6(9) . . . . ?
O30 Ti9 O33 Ti5 98.0(3) . . . . ?
O30 Ti9 O33 Ti6 1.6(3) . . . . ?
O30 Ti9 O33 Ti9 0(100) . . . 4_655 ?
O30 Ti9 O33 Ti10 -147(2) . . . . ?
O30 Ti9 O34 Ti5 82.9(3) . . . 4_655 ?
O30 Ti9 O34 Ti5 -82.9(3) . . . . ?
O30 Ti9 O34 Ti9 0(100) . . . 4_655 ?
O31 Ti10 O35 Ti5 73.4(5) . . . . ?
O32 Ti3 O12 Ti3 -1.5(15) . . . 4_655 ?
O32 Ti5 O9 Ti2 -5.7(10) . . . . ?
O32 Ti5 O35 Ti10 -71.1(4) . . . . ?
O32 Ti6 O31 Ti10 73.2(4) . . . . ?
O33 Ti5 O9 Ti2 -175.8(2) . . . . ?
O33 Ti5 O35 Ti10 4.0(4) . . . . ?
O33 Ti6 O31 Ti10 -5.7(3) . . . . ?
O33 Ti9 O30 Ti6 1.7(3) 4_655 . . 4_655 ?
O33 Ti9 O30 Ti6 -168.7(3) . . . 4_655 ?
O33 Ti9 O30 Ti6 -1.7(3) . . . . ?
O33 Ti9 O30 Ti6 168.7(3) 4_655 . . . ?
O33 Ti9 O30 Ti9 0(100) . . . 4_655 ?
O33 Ti9 O30 Ti9 0(64) 4_655 . . 4_655 ?
O33 Ti9 O33 Ti5 50.8(19) 4_655 . . . ?
O33 Ti9 O33 Ti6 -45.6(19) 4_655 . . . ?
O33 Ti9 O33 Ti9 0(100) 4_655 . . 4_655 ?
O33 Ti9 O33 Ti10 165.8(6) 4_655 . . . ?
O33 Ti9 O34 Ti5 -1.9(3) 4_655 . . 4_655 ?
O33 Ti9 O34 Ti5 167.7(4) . . . 4_655 ?
O33 Ti9 O34 Ti5 1.9(3) . . . . ?
O33 Ti9 O34 Ti5 -167.7(4) 4_655 . . . ?
O33 Ti9 O34 Ti9 0(100) . . . 4_655 ?
O33 Ti9 O34 Ti9 0(84) 4_655 . . 4_655 ?
O33 Ti10 O31 Ti6 5.9(3) . . . . ?
O33 Ti10 O35 Ti5 -4.2(4) . . . . ?
O34 Ti5 O9 Ti2 -104.1(4) . . . . ?
O34 Ti5 O35 Ti10 30.2(9) . . . . ?
O34 Ti9 O30 Ti6 83.5(3) . . . . ?
O34 Ti9 O30 Ti6 -83.5(3) . . . 4_655 ?
O34 Ti9 O30 Ti9 0(100) . . . 4_655 ?
O34 Ti9 O33 Ti5 -1.6(3) . . . . ?
O34 Ti9 O33 Ti6 -98.1(3) . . . . ?
O34 Ti9 O33 Ti9 0(100) . . . 4_655 ?
O34 Ti9 O33 Ti10 113(2) . . . . ?
O35 Ti5 O9 Ti2 109.0(4) . . . . ?
O35 Ti10 O31 Ti6 -73.4(4) . . . . ?
O36 Ti9 O30 Ti6 99.3(17) . . . 4_655 ?
O36 Ti9 O30 Ti6 -93.6(18) . . . . ?
O36 Ti9 O30 Ti9 0(100) . . . 4_655 ?
O36 Ti9 O33 Ti5 -101.9(4) . . . . ?
O36 Ti9 O33 Ti6 161.7(4) . . . . ?
O36 Ti9 O33 Ti9 0(47) . . . 4_655 ?
O36 Ti9 O33 Ti10 13(2) . . . . ?
O36 Ti9 O34 Ti5 -98.1(7) . . . 4_655 ?
O36 Ti9 O34 Ti5 96.1(7) . . . . ?
O36 Ti9 O34 Ti9 0(100) . . . 4_655 ?
O38 Ti10 O31 Ti6 -177.0(5) . . . . ?
O38 Ti10 O35 Ti5 173.2(5) . . . . ?
O39A Ti10 O31 Ti6 69(3) . . . . ?
O39A Ti10 O35 Ti5 -95.8(9) . . . . ?
O39B Ti10 O31 Ti6 57.3(19) . . . . ?
O39B Ti10 O35 Ti5 -89.9(6) . . . . ?
N1 Ti8 O22 Ti7 157.2(19) . . . . ?
N1 Ti8 O23 Ti8 -157(3) . . . 4_655 ?
N1 C43 C44 C45 2.1(10) . . . . ?
N1 C47 C48 O24 -178.1(9) . . . . ?
N1 C47 C48 O25 1.9(9) . . . . ?
N2 Ti8 O22 Ti7 -161.2(19) . . . . ?
N2 Ti8 O23 Ti8 168.5(17) . . . 4_655 ?
N2 C37 C38 C39 0.1(4) . . . . ?
N2 C41 C42 O26 4(2) . . . . ?
N2 C41 C42 O27 -178.5(18) . . . . ?
N3 Ti7 O21 Ti7 170.0(9) . . . 4_655 ?
N3 Ti7 O28 Ti6 93.2(4) . . . . ?
N3 C31 C32 C33 5(3) . . . . ?
N3 C35 C36 O19 8.0(15) . . . . ?
N3 C35 C36 O20 -174.7(11) . . . . ?
N4 Ti3 O12 Ti3 -174.9(9) . . . 4_655 ?
N4 Ti3 O32 Ti5 88.5(3) . . . . ?
N4 Ti3 O32 Ti6 -94.5(7) . . . . ?
N4 C19 C20 C21 1(3) . . . . ?
N4 C23 C24 O13 2.6(16) . . . . ?
N4 C23 C24 O14 -174.3(13) . . . . ?
N5 Ti2 O7 Ti2 -173.9(8) . . . 4_655 ?
N5 Ti2 O9 Ti5 -89.0(4) . . . . ?
N5 C13 C14 C15 0(2) . . . . ?
N5 C17 C18 O10 0.9(16) . . . . ?
N5 C17 C18 O11 174.9(12) . . . . ?
N6 Ti1 O1 Ti1 162.2(11) . . . 4_655 ?
N6 Ti1 O2 Ti2 164(3) . . . . ?
N6 C7 C8 C9 4(3) . . . . ?
N6 C11 C12 O5 -11(3) . . . . ?
N6 C11 C12 O6 -167(2) . . . . ?
N7 Ti1 O1 Ti1 120(2) . . . 4_655 ?
N7 Ti1 O2 Ti2 -148(3) . . . . ?
N7 C1 C2 C3 0.0(3) . . . . ?
N7 C5 C6 O3 0.0(3) . . . . ?
N7 C5 C6 O4 179.99(18) . . . . ?
N8 Ti9 O30 Ti6 100.2(5) . . . 4_655 ?
N8 Ti9 O30 Ti6 -92.8(5) . . . . ?
N8 Ti9 O30 Ti9 0(100) . . . 4_655 ?
N8 Ti9 O33 Ti5 -174.7(4) . . . . ?
N8 Ti9 O33 Ti6 88.9(4) . . . . ?
N8 Ti9 O33 Ti9 0(100) . . . 4_655 ?
N8 Ti9 O33 Ti10 -60(2) . . . . ?
N8 C49 C50 C51 0.0(3) . . . . ?
N8 C53 C54 O36 0.0(2) . . . . ?
N8 C53 C54 O37 179.98(15) . . . . ?
N9A Ti10 O31 Ti6 98.1(7) . . . . ?
N9A Ti10 O35 Ti5 -72(3) . . . . ?
N9A C58A C59A C60A 0.0(4) . . . . ?
N9A C62A C63A O39A 6(4) . . . . ?
N9A C62A C63A O40A 171(3) . . . . ?
N9B Ti10 O31 Ti6 83.4(4) . . . . ?
N9B Ti10 O35 Ti5 -44.0(11) . . . . ?
N9B C58B C59B C60B 0.0(3) . . . . ?
N9B C62B C63B O39B 0.0(2) . . . . ?
N9B C62B C63B O40B 180.00(13) . . . . ?
N10 Ti4 O15 Ti3 -106.1(7) . . . . ?
N10 Ti4 O16 Ti4 -172.1(9) . . . 4_655 ?
N10 Ti4 O29 Ti6 108.3(7) . . . . ?
N10 Ti4 O29 Ti7 -95.9(4) . . . . ?
N10 C25 C26 C27 -5(3) . . . . ?
N10 C29 C30 O17 179.8(13) . . . . ?
N10 C29 C30 O18 8.2(16) . . . . ?
C1 N7 C5 C4 0.0(3) . . . . ?
C1 N7 C5 C6 180.0(2) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 0.0(3) . . . . ?
C3 C4 C5 N7 0.0(3) . . . . ?
C3 C4 C5 C6 -180.0(2) . . . . ?
C4 C5 C6 O3 180.00(17) . . . . ?
C4 C5 C6 O4 0.0(4) . . . . ?
C5 N7 C1 C2 0.0(2) . . . . ?
C7 N6 C11 C10 3(3) . . . . ?
C7 N6 C11 C12 -171.7(14) . . . . ?
C7 C8 C9 C10 -1(3) . . . . ?
C8 C9 C10 C11 -1(3) . . . . ?
C9 C10 C11 N6 0(3) . . . . ?
C9 C10 C11 C12 174.3(17) . . . . ?
C10 C11 C12 O5 174.7(19) . . . . ?
C10 C11 C12 O6 18(3) . . . . ?
C11 N6 C7 C8 -5(2) . . . . ?
C13 N5 C17 C16 -1.2(16) . . . . ?
C13 N5 C17 C18 178.4(11) . . . . ?
C13 C14 C15 C16 2(3) . . . . ?
C14 C15 C16 C17 -3(3) . . . . ?
C15 C16 C17 N5 3(2) . . . . ?
C15 C16 C17 C18 -177.0(14) . . . . ?
C16 C17 C18 O10 -179.5(12) . . . . ?
C16 C17 C18 O11 -5(2) . . . . ?
C17 N5 C13 C14 0.1(19) . . . . ?
C19 N4 C23 C22 -0.9(17) . . . . ?
C19 N4 C23 C24 -176.3(10) . . . . ?
C19 C20 C21 C22 -2(3) . . . . ?
C20 C21 C22 C23 1(3) . . . . ?
C21 C22 C23 N4 0(2) . . . . ?
C21 C22 C23 C24 175.0(17) . . . . ?
C22 C23 C24 O13 -172.7(13) . . . . ?
C22 C23 C24 O14 10(2) . . . . ?
C23 N4 C19 C20 0.2(19) . . . . ?
C25 N10 C29 C28 6(2) . . . . ?
C25 N10 C29 C30 177.5(13) . . . . ?
C25 C26 C27 C28 2(3) . . . . ?
C26 C27 C28 C29 6(3) . . . . ?
C27 C28 C29 N10 -10(3) . . . . ?
C27 C28 C29 C30 179.8(18) . . . . ?
C28 C29 C30 O17 -10(2) . . . . ?
C28 C29 C30 O18 178.8(14) . . . . ?
C29 N10 C25 C26 1(2) . . . . ?
C31 N3 C35 C34 2.2(19) . . . . ?
C31 N3 C35 C36 -177.1(10) . . . . ?
C31 C32 C33 C34 -5(3) . . . . ?
C32 C33 C34 C35 3(3) . . . . ?
C33 C34 C35 N3 -1(3) . . . . ?
C33 C34 C35 C36 177.8(16) . . . . ?
C34 C35 C36 O19 -171.3(13) . . . . ?
C34 C35 C36 O20 6(2) . . . . ?
C35 N3 C31 C32 -4(2) . . . . ?
C37 N2 C41 C40 -0.3(8) . . . . ?
C37 N2 C41 C42 -178.7(14) . . . . ?
C37 C38 C39 C40 -0.1(8) . . . . ?
C38 C39 C40 C41 -0.1(11) . . . . ?
C39 C40 C41 N2 0.3(11) . . . . ?
C39 C40 C41 C42 178.6(15) . . . . ?
C40 C41 C42 O26 -174.7(13) . . . . ?
C40 C41 C42 O27 3(3) . . . . ?
C41 N2 C37 C38 0.1(4) . . . . ?
C43 N1 C47 C46 4.1(19) . . . . ?
C43 N1 C47 C48 -177.6(11) . . . . ?
C43 C44 C45 C46 0.0(2) . . . . ?
C44 C45 C46 C47 0.0(2) . . . . ?
C45 C46 C47 N1 -2.0(9) . . . . ?
C45 C46 C47 C48 -179.99(14) . . . . ?
C46 C47 C48 O24 0.0(2) . . . . ?
C46 C47 C48 O25 180.00(13) . . . . ?
C47 N1 C43 C44 -4.1(19) . . . . ?
C49 N8 C53 C52 0.0(3) . . . . ?
C49 N8 C53 C54 179.99(15) . . . . ?
C49 C50 C51 C52 0.1(3) . . . . ?
C50 C51 C52 C53 0.0(3) . . . . ?
C51 C52 C53 N8 0.0(3) . . . . ?
C51 C52 C53 C54 -179.98(19) . . . . ?
C52 C53 C54 O36 -179.98(18) . . . . ?
C52 C53 C54 O37 0.0(3) . . . . ?
C53 N8 C49 C50 0.0(2) . . . . ?
C58A N9A C62A C61A 0.0(8) . . . . ?
C58A N9A C62A C63A -177(2) . . . . ?
C58A C59A C60A C61A 0.1(8) . . . . ?
C58B N9B C62B C61B 0.0(2) . . . . ?
C58B N9B C62B C63B 180.00(14) . . . . ?
C58B C59B C60B C61B 0.0(3) . . . . ?
C59A C60A C61A C62A -0.1(11) . . . . ?
C59B C60B C61B C62B 0.0(3) . . . . ?
C60A C61A C62A N9A 0.1(12) . . . . ?
C60A C61A C62A C63A 177(3) . . . . ?
C60B C61B C62B N9B 0.0(3) . . . . ?
C60B C61B C62B C63B -179.98(19) . . . . ?
C61A C62A C63A O39A -172(3) . . . . ?
C61A C62A C63A O40A -6(5) . . . . ?
C61B C62B C63B O39B 180.00(18) . . . . ?
C61B C62B C63B O40B 0.0(3) . . . . ?
C62A N9A C58A C59A 0.0(3) . . . . ?
C62B N9B C58B C59B 0.0(2) . . . . ?
C65 N11 C66 C67 62(4) . . . . ?
C66 N11 C65 C64 -79(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 566 electrons were 
found in a volume of 3379Å³ in 1 void per unit cell. 
This is consistent with the presence of 
26[CH3CN] per Unit Cell 
which account for 572 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.501 -0.785 0.501 3379.2 565.5 '26 CH3CN'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.407
_oxdiff_exptl_absorpt_empirical_full_min 0.866
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.672(14)
2 0.328(14)
# start Validation Reply Form
_vrf_PLAT733_ti19pa19            
;
PROBLEM: Torsion Calc 0.1(18), Rep 0.0(2) ...... 9.00 s.u.-R
RESPONSE: This alert is caused by the disorder of the reported atoms.
;
_vrf_PLAT213_ti19pa19            
;
PROBLEM: Atom O39B has ADP max/min Ratio ..... 4.5 oblate
RESPONSE: This problem is caused by the disorder of the atoms.
;
_vrf_PLAT234_ti19pa19            
;
PROBLEM: Large Hirshfeld Difference O26 --C42 . 0.26 Ang.
RESPONSE: This problem is caused by the disorder of the atoms.
;
_vrf_PLAT341_ti19pa19            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.02626 Ang.
RESPONSE: Bond precision on C-C bonds does not affect the
determination of the binding modes of the ligands.
;
# end Validation Reply Form
####################################################################### 
# 
# 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_ti18pa8
_database_code_depnum_ccdc_archive 'CCDC 2126649'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2021-12-06 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2021-11-29
_audit_creation_method           
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C66 H86 N8 O56 Ti18'
_chemical_formula_sum            'C66 H86 N8 O56 Ti18'
_chemical_formula_weight         2749.62
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Ti O C'
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'

_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.
;
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_H-M_alt        'I 4 3 2'
_space_group_name_Hall           'I 4 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x, z'
'-x, -y, z'
'y, -x, z'
'x, -z, y'
'x, -y, -z'
'x, z, -y'
'z, y, -x'
'-x, y, -z'
'-z, y, x'
'z, x, y'
'y, z, x'
'-y, -z, x'
'z, -x, -y'
'-y, z, -x'
'-z, -x, y'
'-z, x, -y'
'y, -z, -x'
'y, x, -z'
'-y, -x, -z'
'-x, z, y'
'-x, -z, -y'
'z, -y, x'
'-z, -y, -x'
'x+1/2, y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'x+1/2, -z+1/2, y+1/2'
'x+1/2, -y+1/2, -z+1/2'
'x+1/2, z+1/2, -y+1/2'
'z+1/2, y+1/2, -x+1/2'
'-x+1/2, y+1/2, -z+1/2'
'-z+1/2, y+1/2, x+1/2'
'z+1/2, x+1/2, y+1/2'
'y+1/2, z+1/2, x+1/2'
'-y+1/2, -z+1/2, x+1/2'
'z+1/2, -x+1/2, -y+1/2'
'-y+1/2, z+1/2, -x+1/2'
'-z+1/2, -x+1/2, y+1/2'
'-z+1/2, x+1/2, -y+1/2'
'y+1/2, -z+1/2, -x+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'

_cell_length_a                   32.0910(3)
_cell_length_b                   32.0910(3)
_cell_length_c                   32.0910(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     33048.3(9)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    6261
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      69.0980
_cell_measurement_theta_min      3.8540
_shelx_estimated_absorpt_T_max   0.896
_shelx_estimated_absorpt_T_min   0.728
_exptl_absorpt_coefficient_mu    5.639
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.43449
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'light yellow'
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    0.829
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             8292
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0857
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.955
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            18693
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         76.464
_diffrn_reflns_theta_min         2.754
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.955
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     93.00 165.00   1.00   33.00    --  106.49  38.00-120.00   72
  2  ω    -23.00  25.00   1.00    3.80    --  -48.45  19.00-120.00   48
  3  ω    -65.00 -39.00   1.00   33.00    --  -86.25  78.00 -85.00   26
  4  ω   -105.00 -75.00   1.00   33.00    --  -86.25  78.00 -85.00   30
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0108223000
_diffrn_orient_matrix_UB_12      0.0020988000
_diffrn_orient_matrix_UB_13      -0.0466756000
_diffrn_orient_matrix_UB_21      -0.0468001000
_diffrn_orient_matrix_UB_22      0.0011151000
_diffrn_orient_matrix_UB_23      0.0109069000
_diffrn_orient_matrix_UB_31      0.0015434000
_diffrn_orient_matrix_UB_32      0.0479287000
_diffrn_orient_matrix_UB_33      0.0018551000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.769
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.959
_reflns_number_gt                2831
_reflns_number_total             5244
_reflns_odcompleteness_completeness 99.04
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.84a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.50(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5244
_refine_ls_number_restraints     179
_refine_ls_R_factor_all          0.1433
_refine_ls_R_factor_gt           0.0904
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1830P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2498
_refine_ls_wR_factor_ref         0.3016
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.50(3)
 0.50(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1B-C8B = C7B-C8B = C7B-C6B = C5B-C6B = C4B-C5B = N1B-C4B
 1.33 with sigma of 0.02
 O2-C2
 1.5 with sigma of 0.02
 C7A-N1A
 2.35 with sigma of 0.02
 N1A-C5A
 2.35 with sigma of 0.02
 O4-C3
 1.5 with sigma of 0.02
 N1A-C8A = C8A-C7A = C7A-C6A = C5A-C6A = C5A-C4A = N1A-C4A
 1.33 with sigma of 0.02
 N1A-C6A
 2.75 with sigma of 0.02
 C9B-C8B
 1.5 with sigma of 0.02
 N1B-C7B
 2.35 with sigma of 0.02
 C8A-C9A
 1.5 with sigma of 0.02
 C5B-N1B
 2.35 with sigma of 0.02
 C6B-N1B
 2.75 with sigma of 0.02
 C8B-C4B
 2.35 with sigma of 0.02
 C5A-C7A
 2.35 with sigma of 0.02
 C4A-C7A
 2.75 with sigma of 0.02
 C8B-C6B
 2.35 with sigma of 0.02
 C7B-C5B
 2.35 with sigma of 0.02
 C4A-C6A
 2.35 with sigma of 0.02
 C6B-C4B
 2.35 with sigma of 0.02
 C6A-C8A
 2.35 with sigma of 0.02
 C5A-C8A
 2.75 with sigma of 0.02
 C7B-C4B
 2.75 with sigma of 0.02
 C8B-C5B
 2.75 with sigma of 0.02
4. Rigid bond restraints
 O2, C2
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 O4, C3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
O8A \\sim O9A \\sim N1A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A
O2 \\sim C2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O4 \\sim C3: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
O8B \\sim O9B \\sim N1B \\sim C4B \\sim C5B \\sim C6B \\sim C7B \\sim C8B \\sim
C9B: within 2A with sigma of 0.004 and sigma for terminal atoms of 0.008 within
2A
O1 \\sim C1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 2A
Uanis(N1A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O8B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C7A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
6. Others
 Sof(O8B)=Sof(O9B)=Sof(N1B)=Sof(C4B)=Sof(H4B)=Sof(C5B)=Sof(H5B)=Sof(C6B)=
 Sof(H6B)=Sof(C7B)=Sof(H7B)=Sof(C8B)=Sof(C9B)=1-FVAR(1)
 Sof(O8A)=Sof(O9A)=Sof(N1A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(H7A)=Sof(C8A)=Sof(C9A)=FVAR(1)
 Fixed Sof: H1C(0.25) H1A(0.25) H1B(0.25)
7.a Me refined with riding coordinates:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
7.b Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C4B(H4B), C5A(H5A), C5B(H5B), C6A(H6A), C6B(H6B), C7A(H7A), C7B(H7B)
7.c Idealised Me refined as rotating group:
 C1(H1C,H1A,H1B)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.5000 0.5000 0.20289(13) 0.1129(13) Uani 1 4 d S T P . .
Ti2 Ti 0.45148(7) 0.55025(8) 0.13276(6) 0.0918(7) Uani 1 1 d . . . . .
Ti3 Ti 0.42012(4) 0.50064(8) 0.05594(6) 0.0831(7) Uani 1 1 d . . . . .
O1 O 0.5000 0.5000 0.2584(6) 0.158(6) Uani 1 4 d S TU P . .
O2 O 0.4576(2) 0.5435(3) 0.1925(3) 0.110(2) Uani 1 1 d D U . . .
O3 O 0.5000 0.5000 0.1407(4) 0.082(3) Uani 1 4 d S T P . .
O4 O 0.4123(3) 0.5877(3) 0.1365(3) 0.112(2) Uani 1 1 d D U . . .
O5 O 0.41810(16) 0.5016(3) 0.1222(2) 0.0883(17) Uani 1 1 d . . . . .
O6 O 0.4544(2) 0.45349(18) 0.0689(2) 0.0836(17) Uani 1 1 d . . . . .
O7 O 0.4266(2) 0.5000 0.0000 0.075(2) Uani 1 2 d S T P A .
O8A O 0.3736(4) 0.4612(4) 0.0584(5) 0.067(4) Uani 0.571(11) 1 d . U P A 4
O8B O 0.3663(5) 0.5409(7) 0.0590(8) 0.057(4) Uani 0.429(11) 1 d . U P A 3
O9A O 0.3024(4) 0.4486(5) 0.0617(6) 0.095(5) Uani 0.571(11) 1 d . U P A 4
O9B O 0.3036(5) 0.5437(6) 0.0610(7) 0.068(5) Uani 0.429(11) 1 d . U P A 3
N1A N 0.3671(6) 0.5390(6) 0.0488(8) 0.078(5) Uani 0.571(11) 1 d D U P A 4
N1B N 0.3635(5) 0.4618(6) 0.0471(9) 0.063(4) Uani 0.429(11) 1 d D U P A 3
C1 C 0.5000 0.5000 0.3045(11) 0.184(10) Uani 1 4 d S TU P . .
H1C H 0.4749 0.5141 0.3147 0.275 Uiso 0.25 1 calc R U P B -1
H1A H 0.5247 0.5147 0.3147 0.275 Uiso 0.25 1 calc R U P B -1
H1B H 0.5004 0.4712 0.3147 0.275 Uiso 0.25 1 calc R U P B -1
C2 C 0.4229(7) 0.5557(7) 0.2229(7) 0.223(9) Uani 1 1 d D U . . .
H2A H 0.4319 0.5500 0.2515 0.334 Uiso 1 1 calc R U . . .
H2B H 0.4167 0.5855 0.2199 0.334 Uiso 1 1 calc R U . . .
H2C H 0.3978 0.5395 0.2167 0.334 Uiso 1 1 calc R U . . .
C3 C 0.3705(5) 0.6087(6) 0.1486(7) 0.187(7) Uani 1 1 d D U . . .
H3A H 0.3695 0.6369 0.1369 0.280 Uiso 1 1 calc R U . . .
H3B H 0.3473 0.5923 0.1375 0.280 Uiso 1 1 calc R U . . .
H3C H 0.3683 0.6102 0.1790 0.280 Uiso 1 1 calc R U . . .
C4A C 0.3694(4) 0.5813(5) 0.0481(8) 0.086(4) Uani 0.571(11) 1 d D U P A 4
H4A H 0.3957 0.5945 0.0520 0.103 Uiso 0.571(11) 1 calc R U P A 4
C4B C 0.3632(4) 0.4192(6) 0.0482(9) 0.066(4) Uani 0.429(11) 1 d D U P A 3
H4B H 0.3888 0.4043 0.0491 0.079 Uiso 0.429(11) 1 calc R U P A 3
C5A C 0.3355(5) 0.6046(4) 0.0421(7) 0.089(5) Uani 0.571(11) 1 d D U P A 4
H5A H 0.3381 0.6329 0.0341 0.107 Uiso 0.571(11) 1 calc R U P A 4
C5B C 0.3264(4) 0.3979(5) 0.0481(8) 0.067(4) Uani 0.429(11) 1 d D U P A 3
H5B H 0.3257 0.3685 0.0511 0.080 Uiso 0.429(11) 1 calc R U P A 3
C6A C 0.2973(4) 0.5874(4) 0.0477(7) 0.083(4) Uani 0.571(11) 1 d D U P A 4
H6A H 0.2736 0.6044 0.0528 0.099 Uiso 0.571(11) 1 calc R U P A 4
C6B C 0.2904(4) 0.4205(6) 0.0435(8) 0.065(4) Uani 0.429(11) 1 d D U P A 3
H6B H 0.2660 0.4082 0.0323 0.078 Uiso 0.429(11) 1 calc R U P A 3
C7A C 0.2940(5) 0.5441(5) 0.0457(7) 0.066(5) Uani 0.571(11) 1 d D U P A 4
H7A H 0.2677 0.5313 0.0412 0.080 Uiso 0.571(11) 1 calc R U P A 4
C7B C 0.2909(5) 0.4614(6) 0.0557(10) 0.063(4) Uani 0.429(11) 1 d D U P A 3
H7B H 0.2660 0.4748 0.0644 0.076 Uiso 0.429(11) 1 calc R U P A 3
C8A C 0.3289(6) 0.5205(4) 0.0505(10) 0.068(4) Uani 0.571(11) 1 d D U P A 4
C8B C 0.3283(6) 0.4829(5) 0.0549(13) 0.060(3) Uani 0.429(11) 1 d D U P A 3
C9A C 0.3354(6) 0.4745(5) 0.0597(9) 0.063(4) Uani 0.571(11) 1 d D U P A 4
C9B C 0.3339(7) 0.5306(7) 0.0543(13) 0.059(4) Uani 0.429(11) 1 d D U P A 3


_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 1.78(2) . ?
Ti1 O2 1.978(7) 2_655 ?
Ti1 O2 1.978(7) 4_565 ?
Ti1 O2 1.978(7) . ?
Ti1 O2 1.978(7) 3_665 ?
Ti1 O3 1.996(13) . ?
Ti2 O2 1.940(8) . ?
Ti2 O3 2.256(2) . ?
Ti2 O4 1.744(6) . ?
Ti2 O5 1.924(9) . ?
Ti2 O5 1.932(9) 4_565 ?
Ti2 O6 2.055(7) 4_565 ?
Ti3 Ti2 3.078(3) 2_655 ?
Ti3 O5 2.126(7) . ?
Ti3 O6 1.917(8) . ?
Ti3 O6 1.844(8) 4_565 ?
Ti3 O7 1.807(2) . ?
Ti3 O8A 1.958(14) . ?
Ti3 O8B 2.161(17) . ?
Ti3 N1A 2.114(17) . ?
Ti3 N1B 2.222(16) . ?
O1 C1 1.48(4) . ?
O2 C2 1.531(16) . ?
O3 Ti2 2.256(2) 3_665 ?
O3 Ti2 2.256(2) 2_655 ?
O3 Ti2 2.256(2) 4_565 ?
O4 C3 1.550(15) . ?
O5 Ti2 1.932(9) 2_655 ?
O6 Ti2 2.055(7) 2_655 ?
O6 Ti3 1.844(8) 2_655 ?
O7 Ti3 1.807(2) 6_565 ?
O8A C9A 1.30(2) . ?
O8B C9B 1.10(3) . ?
O9A C9A 1.35(2) . ?
O9B C9B 1.08(3) . ?
N1A C4A 1.36(2) . ?
N1A C8A 1.36(2) . ?
N1B C4B 1.368(19) . ?
N1B C8B 1.338(19) . ?
C1 H1C 1.0442 . ?
C1 H1A 1.0442 . ?
C1 H1B 1.0442 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4A H4A 0.9500 . ?
C4A C5A 1.334(16) . ?
C4B H4B 0.9500 . ?
C4B C5B 1.364(16) . ?
C5A H5A 0.9500 . ?
C5A C6A 1.355(17) . ?
C5B H5B 0.9500 . ?
C5B C6B 1.371(16) . ?
C6A H6A 0.9500 . ?
C6A C7A 1.395(18) . ?
C6B H6B 0.9500 . ?
C6B C7B 1.369(19) . ?
C7A H7A 0.9500 . ?
C7A C8A 1.362(18) . ?
C7B H7B 0.9500 . ?
C7B C8B 1.386(19) . ?
C8A C9A 1.522(17) . ?
C8B C9B 1.54(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O2 99.7(3) . . ?
O1 Ti1 O2 99.7(3) . 4_565 ?
O1 Ti1 O2 99.7(3) . 2_655 ?
O1 Ti1 O2 99.7(3) . 3_665 ?
O1 Ti1 O3 180.0 . . ?
O2 Ti1 O2 88.39(9) . 4_565 ?
O2 Ti1 O2 88.39(9) . 2_655 ?
O2 Ti1 O2 88.39(9) 4_565 3_665 ?
O2 Ti1 O2 160.7(5) 2_655 4_565 ?
O2 Ti1 O2 160.7(5) . 3_665 ?
O2 Ti1 O2 88.39(9) 2_655 3_665 ?
O2 Ti1 O3 80.3(3) 2_655 . ?
O2 Ti1 O3 80.3(3) 3_665 . ?
O2 Ti1 O3 80.3(3) 4_565 . ?
O2 Ti1 O3 80.3(3) . . ?
O2 Ti2 O3 74.9(4) . . ?
O2 Ti2 O6 167.0(3) . 4_565 ?
O4 Ti2 O2 94.7(4) . . ?
O4 Ti2 O3 169.4(4) . . ?
O4 Ti2 O5 99.8(4) . . ?
O4 Ti2 O5 104.5(4) . 4_565 ?
O4 Ti2 O6 98.1(3) . 4_565 ?
O5 Ti2 O2 98.5(4) 4_565 . ?
O5 Ti2 O2 98.1(4) . . ?
O5 Ti2 O3 79.9(2) . . ?
O5 Ti2 O3 79.7(2) 4_565 . ?
O5 Ti2 O5 149.2(3) . 4_565 ?
O5 Ti2 O6 77.4(3) . 4_565 ?
O5 Ti2 O6 80.6(3) 4_565 4_565 ?
O6 Ti2 O3 92.2(3) 4_565 . ?
O5 Ti3 Ti2 38.4(2) . 2_655 ?
O5 Ti3 O8B 85.5(7) . . ?
O5 Ti3 N1B 96.4(8) . . ?
O6 Ti3 Ti2 92.3(2) 4_565 2_655 ?
O6 Ti3 Ti2 40.9(2) . 2_655 ?
O6 Ti3 O5 77.3(3) 4_565 . ?
O6 Ti3 O5 79.1(3) . . ?
O6 Ti3 O6 103.6(3) 4_565 . ?
O6 Ti3 O8A 85.3(4) . . ?
O6 Ti3 O8A 159.9(5) 4_565 . ?
O6 Ti3 O8B 89.2(6) 4_565 . ?
O6 Ti3 O8B 157.2(6) . . ?
O6 Ti3 N1A 92.1(6) 4_565 . ?
O6 Ti3 N1A 161.1(6) . . ?
O6 Ti3 N1B 93.1(6) . . ?
O6 Ti3 N1B 160.5(6) 4_565 . ?
O7 Ti3 Ti2 139.00(16) . 2_655 ?
O7 Ti3 O5 175.2(3) . . ?
O7 Ti3 O6 99.6(3) . 4_565 ?
O7 Ti3 O6 98.1(3) . . ?
O7 Ti3 O8A 96.9(5) . . ?
O7 Ti3 O8B 98.3(7) . . ?
O7 Ti3 N1A 89.5(8) . . ?
O7 Ti3 N1B 87.7(8) . . ?
O8A Ti3 Ti2 82.6(4) . 2_655 ?
O8A Ti3 O5 86.9(5) . . ?
O8A Ti3 N1A 76.6(7) . . ?
O8B Ti3 Ti2 121.1(7) . 2_655 ?
O8B Ti3 N1B 71.8(8) . . ?
N1A Ti3 Ti2 129.4(7) . 2_655 ?
N1A Ti3 O5 94.3(8) . . ?
N1B Ti3 Ti2 93.9(7) . 2_655 ?
C1 O1 Ti1 180.0 . . ?
Ti2 O2 Ti1 108.3(4) . . ?
C2 O2 Ti1 125.0(10) . . ?
C2 O2 Ti2 121.8(10) . . ?
Ti1 O3 Ti2 96.5(3) . 4_565 ?
Ti1 O3 Ti2 96.5(3) . . ?
Ti1 O3 Ti2 96.5(3) . 2_655 ?
Ti1 O3 Ti2 96.5(3) . 3_665 ?
Ti2 O3 Ti2 89.27(7) 2_655 . ?
Ti2 O3 Ti2 167.0(6) 2_655 4_565 ?
Ti2 O3 Ti2 89.27(7) 4_565 3_665 ?
Ti2 O3 Ti2 89.27(7) 4_565 . ?
Ti2 O3 Ti2 89.27(7) 2_655 3_665 ?
Ti2 O3 Ti2 167.0(6) . 3_665 ?
C3 O4 Ti2 160.1(11) . . ?
Ti2 O5 Ti2 110.6(3) . 2_655 ?
Ti2 O5 Ti3 99.9(3) . . ?
Ti2 O5 Ti3 98.5(3) 2_655 . ?
Ti3 O6 Ti2 105.3(4) 2_655 2_655 ?
Ti3 O6 Ti2 101.5(3) . 2_655 ?
Ti3 O6 Ti3 149.1(4) 2_655 . ?
Ti3 O7 Ti3 166.9(4) 6_565 . ?
C9A O8A Ti3 120.6(11) . . ?
C9B O8B Ti3 124.5(19) . . ?
C4A N1A Ti3 122.6(13) . . ?
C4A N1A C8A 119.1(13) . . ?
C8A N1A Ti3 117.7(13) . . ?
C4B N1B Ti3 124.2(12) . . ?
C8B N1B Ti3 112.4(13) . . ?
C8B N1B C4B 119.7(14) . . ?
O1 C1 H1C 116.1 . . ?
O1 C1 H1A 116.1 . . ?
O1 C1 H1B 116.1 . . ?
H1C C1 H1A 102.2 . . ?
H1C C1 H1B 102.2 . . ?
H1A C1 H1B 102.2 . . ?
O2 C2 H2A 109.5 . . ?
O2 C2 H2B 109.5 . . ?
O2 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
O4 C3 H3A 109.5 . . ?
O4 C3 H3B 109.5 . . ?
O4 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1A C4A H4A 119.5 . . ?
C5A C4A N1A 121.1(14) . . ?
C5A C4A H4A 119.5 . . ?
N1B C4B H4B 119.8 . . ?
C5B C4B N1B 120.3(12) . . ?
C5B C4B H4B 119.8 . . ?
C4A C5A H5A 120.3 . . ?
C4A C5A C6A 119.4(13) . . ?
C6A C5A H5A 120.3 . . ?
C4B C5B H5B 121.2 . . ?
C4B C5B C6B 117.7(13) . . ?
C6B C5B H5B 121.2 . . ?
C5A C6A H6A 121.1 . . ?
C5A C6A C7A 117.9(12) . . ?
C7A C6A H6A 121.1 . . ?
C5B C6B H6B 121.0 . . ?
C7B C6B C5B 118.0(13) . . ?
C7B C6B H6B 121.0 . . ?
C6A C7A H7A 120.4 . . ?
C8A C7A C6A 119.1(12) . . ?
C8A C7A H7A 120.4 . . ?
C6B C7B H7B 120.7 . . ?
C6B C7B C8B 118.7(13) . . ?
C8B C7B H7B 120.7 . . ?
N1A C8A C9A 108.0(16) . . ?
C7A C8A N1A 119.5(14) . . ?
C7A C8A C9A 132.5(17) . . ?
N1B C8B C7B 118.9(13) . . ?
N1B C8B C9B 113.7(18) . . ?
C7B C8B C9B 126.5(17) . . ?
O8A C9A O9A 122.9(15) . . ?
O8A C9A C8A 116.1(17) . . ?
O9A C9A C8A 120.0(16) . . ?
O8B C9B C8B 114(2) . . ?
O9B C9B O8B 135(3) . . ?
O9B C9B C8B 106(2) . . ?

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
Ti2 Ti3 O7 Ti3 127.3(2) 2_655 . . 6_565 ?
Ti3 O8A C9A O9A -179.5(19) . . . . ?
Ti3 O8A C9A C8A 12(3) . . . . ?
Ti3 O8B C9B O9B 164(4) . . . . ?
Ti3 O8B C9B C8B 13(4) . . . . ?
Ti3 N1A C4A C5A 177.6(18) . . . . ?
Ti3 N1A C8A C7A -180(2) . . . . ?
Ti3 N1A C8A C9A 3(3) . . . . ?
Ti3 N1B C4B C5B 171(2) . . . . ?
Ti3 N1B C8B C7B -172(3) . . . . ?
Ti3 N1B C8B C9B 18(3) . . . . ?
O2 Ti2 O4 C3 -56(3) . . . . ?
O3 Ti2 O4 C3 -44(4) . . . . ?
O5 Ti2 O4 C3 -156(3) 4_565 . . . ?
O5 Ti2 O4 C3 43(3) . . . . ?
O6 Ti2 O4 C3 122(3) 4_565 . . . ?
O6 Ti3 O7 Ti3 126.88(17) . . . 6_565 ?
O6 Ti3 O7 Ti3 -127.77(16) 4_565 . . 6_565 ?
O8A Ti3 O7 Ti3 40.7(4) . . . 6_565 ?
O8B Ti3 O7 Ti3 -37.2(6) . . . 6_565 ?
N1A Ti3 O7 Ti3 -35.7(6) . . . 6_565 ?
N1A C4A C5A C6A 18(4) . . . . ?
N1A C8A C9A O8A -9(3) . . . . ?
N1A C8A C9A O9A -178(3) . . . . ?
N1B Ti3 O7 Ti3 34.0(5) . . . 6_565 ?
N1B C4B C5B C6B 5(4) . . . . ?
N1B C8B C9B O8B -21(5) . . . . ?
N1B C8B C9B O9B -180(3) . . . . ?
C4A N1A C8A C7A 9(4) . . . . ?
C4A N1A C8A C9A -169(3) . . . . ?
C4A C5A C6A C7A -21(3) . . . . ?
C4B N1B C8B C7B -13(5) . . . . ?
C4B N1B C8B C9B 178(3) . . . . ?
C4B C5B C6B C7B -25(4) . . . . ?
C5A C6A C7A C8A 19(3) . . . . ?
C5B C6B C7B C8B 27(4) . . . . ?
C6A C7A C8A N1A -13(4) . . . . ?
C6A C7A C8A C9A 164(3) . . . . ?
C6B C7B C8B N1B -8(5) . . . . ?
C6B C7B C8B C9B 160(3) . . . . ?
C7A C8A C9A O8A 174(3) . . . . ?
C7A C8A C9A O9A 5(4) . . . . ?
C7B C8B C9B O8B 170(4) . . . . ?
C7B C8B C9B O9B 11(5) . . . . ?
C8A N1A C4A C5A -11(4) . . . . ?
C8B N1B C4B C5B 14(4) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 3030 electrons were 
found in a volume of 19585Å³ in 1 void per unit cell. 
This is consistent with the presence of 
3.5[CH4O] per Asymmetric Unit 
which account for 3024 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.133 -0.872 -0.016 19585.4 3029.5 '168 CH4O'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.013
_oxdiff_exptl_absorpt_empirical_full_min 0.535
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.50(3)
2 0.50(3)

####################################################################### 
# 
# 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_ti15pa15
_database_code_depnum_ccdc_archive 'CCDC 2126647'
loop_
_audit_author_name
_audit_author_address
'Yifeng Wang'
;Shandong University
China
;
_audit_update_record             
;
2021-12-06 deposited with the CCDC.	2022-01-31 downloaded from the CCDC.
;
_audit_creation_date             2021-11-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelxl_version_number           2013-4
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_chemical_formula_moiety         'C95 H65 N15 O61 Ti15, C4 H11 N'
_chemical_formula_sum            'C99 H76 N16 O61 Ti15'
_chemical_formula_weight         3184.25
_chemical_melting_point          ?
_chemical_oxdiff_usercomment     'Ti O C'
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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   15.9539(6)
_cell_length_b                   17.4707(9)
_cell_length_c                   29.0128(9)
_cell_angle_alpha                89.709(3)
_cell_angle_beta                 80.240(3)
_cell_angle_gamma                81.263(4)
_cell_volume                     7875.3(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    12118
_cell_measurement_temperature    172.99(10)
_cell_measurement_theta_max      76.3440
_cell_measurement_theta_min      2.9420
_shelx_estimated_absorpt_T_max   0.821
_shelx_estimated_absorpt_T_min   0.772
_exptl_absorpt_coefficient_mu    6.825
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.343
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3200
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.03
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1059
_diffrn_reflns_av_unetI/netI     0.1111
_diffrn_reflns_Laue_measured_fraction_full 0.957
_diffrn_reflns_Laue_measured_fraction_max 0.901
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            73602
_diffrn_reflns_point_group_measured_fraction_full 0.957
_diffrn_reflns_point_group_measured_fraction_max 0.901
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.593
_diffrn_reflns_theta_min         2.962
_diffrn_ambient_temperature      172.99(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.957
_diffrn_measured_fraction_theta_max 0.901
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -107.00 -72.00   1.00    6.60    --  -86.25  86.00  16.00   35
  2  ω   -158.00-113.00   1.00    6.60    --  -86.25 -86.00-101.00   45
  3  ω   -106.00 -79.00   1.00    6.60    --  -86.25 -86.00-101.00   27
  4  ω    -65.00 -23.00   1.00    6.60    --  -86.25  86.00  16.00   42
  5  ω    135.00 172.00   1.00    6.60    --  106.49  86.00  16.00   37
  6  ω    101.00 131.00   1.00    6.60    --  106.49  86.00  16.00   30
  7  ω    -26.00  27.00   1.00    1.40    --  -48.45  19.00 -90.00   53
  8  ω    -75.00  24.00   1.00    1.40    --  -48.45  86.00  16.00   99
  9  ω   -120.00 -73.00   1.00    1.40    --  -48.45-125.00  60.00   47
 10  ω    -21.00  75.00   1.00    1.40    --   48.45 -86.00-101.00   96
 11  ω   -159.00 -73.00   1.00    6.60    --  -86.25 -38.00 -60.00   86
 12  ω    -66.00 -14.00   1.00    6.60    --  -86.25  57.00  30.00   52
 13  ω     35.00 106.00   1.00    6.60    --  106.49 -99.00 120.00   71
 14  ω     34.00 106.00   1.00    6.60    --  106.49 -99.00 150.00   72
 15  ω     37.00 112.00   1.00    6.60    --  106.49 -86.00-101.00   75
 16  ω     36.00 111.00   1.00    6.60    --  106.49-125.00 120.00   75
 17  ω     94.00 120.00   1.00    6.60    --  106.49  19.00-150.00   26
 18  ω    123.00 177.00   1.00    6.60    --  106.49  19.00-150.00   54
 19  ω     34.00 105.00   1.00    6.60    --  106.49 -99.00  30.00   71
 20  ω     37.00 175.00   1.00    6.60    --  106.49   0.00-180.00  138
 21  ω     34.00 106.00   1.00    6.60    --  106.49 -99.00 -30.00   72
 22  ω     34.00 106.00   1.00    6.60    --  106.49 -99.00-150.00   72
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0604998000
_diffrn_orient_matrix_UB_12      -0.0052046000
_diffrn_orient_matrix_UB_13      -0.0356149000
_diffrn_orient_matrix_UB_21      -0.0479786000
_diffrn_orient_matrix_UB_22      -0.0555062000
_diffrn_orient_matrix_UB_23      0.0322090000
_diffrn_orient_matrix_UB_31      -0.0622017000
_diffrn_orient_matrix_UB_32      0.0696771000
_diffrn_orient_matrix_UB_33      0.0244631000
_diffrn_oxdiff_digest_frames     
;
0127c494afdb3da2e0ebfc1b1324270fff01375d122
;
_diffrn_oxdiff_digest_hkl        
;
01b88409bd41435dd56a9ec9edb127edc0d6a7
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12485
_reflns_number_total             29824
_reflns_odcompleteness_completeness 96.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_collection       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.944
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1725
_refine_ls_number_reflns         29824
_refine_ls_number_restraints     2097
_refine_ls_R_factor_all          0.1590
_refine_ls_R_factor_gt           0.0831
_refine_ls_restrained_S_all      0.989
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1465P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2232
_refine_ls_wR_factor_ref         0.2729
_refine_special_details          
;
 ?
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N13-C81 = N13-C77 = C78-C77 = C78-C79 = C80-C79 = C80-C81
 1.42 with sigma of 0.02
 C80-N13
 2.35 with sigma of 0.02
 C77-C79
 2.35 with sigma of 0.02
 C81-C77
 2.35 with sigma of 0.02
 C78-C80
 2.35 with sigma of 0.02
 C79-C81
 2.35 with sigma of 0.02
 C45-C47
 2.35 with sigma of 0.02
 C48-N8
 2.35 with sigma of 0.02
 C46-C48
 2.35 with sigma of 0.02
 C47-C49
 2.35 with sigma of 0.02
 C45-C46 = C47-C46 = C47-C48 = C48-C49 = N8-C49 = N8-C45
 1.42 with sigma of 0.02
 C49-C45
 2.35 with sigma of 0.02
 N8-C46
 2.35 with sigma of 0.02
 C22-C21
 1.42 with sigma of 0.02
 C24-C23
 1.42 with sigma of 0.02
 C21-C23
 2.35 with sigma of 0.02
 C22-C23
 1.42 with sigma of 0.02
 C20-C22
 2.35 with sigma of 0.02
 N16-H16A
 0.98 with sigma of 0.02
3. Restrained planarity
 O51, O52, N13, C76, C77, C78, C79, C80, C81
 with sigma of 0.01
4. Rigid bond restraints
 C70, C71
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C35, C36
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O37, C44
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 C73, C74
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
5. Uiso/Uaniso restraints and constraints
O51 \\sim O52 \\sim N13 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim
C81: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O41 \\sim O42 \\sim N9 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim
C56: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O39 \\sim O40 \\sim N8 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49 \\sim
C50: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O27 \\sim O28 \\sim N4 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim
C25: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78 \\sim C79 \\sim C80 \\sim C81
\\sim C82 \\sim C83 \\sim C84 \\sim C85 \\sim C86 \\sim C87 \\sim C88 \\sim C89
\\sim C90 \\sim C91 \\sim C92 \\sim C93 \\sim C94 \\sim C95 \\sim C96 \\sim C97
\\sim C98 \\sim C99: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.02
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(N2) \\sim
Ueq, Uanis(C12) \\sim Ueq, Uanis(C11) \\sim Ueq, Uanis(C13) \\sim Ueq,
Uanis(O24) \\sim Ueq, Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N1) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O35)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq,
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O21) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O22) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O52) \\sim Ueq, Uanis(C76) \\sim Ueq, Uanis(O51) \\sim Ueq, Uanis(C77)
\\sim Ueq, Uanis(C78) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C81) \\sim Ueq,
Uanis(C80) \\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C92) \\sim Ueq, Uanis(N15) \\sim Ueq, Uanis(C88) \\sim Ueq, Uanis(C89)
\\sim Ueq, Uanis(C90) \\sim Ueq, Uanis(C91) \\sim Ueq, Uanis(C93) \\sim Ueq,
Uanis(O55) \\sim Ueq, Uanis(O56) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N3) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C15) \\sim Ueq, Uanis(C16)
\\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C19) \\sim Ueq,
Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O54) \\sim Ueq, Uanis(C87) \\sim Ueq, Uanis(O53) \\sim Ueq, Uanis(C86)
\\sim Ueq, Uanis(C85) \\sim Ueq, Uanis(C84) \\sim Ueq, Uanis(C83) \\sim Ueq,
Uanis(C82) \\sim Ueq, Uanis(N14) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C45) \\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C49) \\sim Ueq, Uanis(C50)
\\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(C48) \\sim Ueq,
Uanis(C47) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6.a Secondary CH2 refined with riding coordinates:
 C97(H97A,H97B), C98(H98A,H98B)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11),
 C14(H14), C15(H15), C16(H16), C17(H17), C20(H20), C21(H21), C22(H22), C23(H23),
  C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34),
 C35(H35), C38(H38), C39(H39), C40(H40), C41(H41), C44(H44), C45(H45), C46(H46),
  C47(H47), C48(H48), C51(H51), C52(H52), C53(H53), C54(H54), C57(H57),
 C58(H58), C59(H59), C60(H60), C61(H61), C64(H64), C65(H65), C66(H66), C67(H67),
  C70(H70), C71(H71), C72(H72), C73(H73), C78(H78), C79(H79), C80(H80),
 C81(H81), C82(H82), C83(H83), C84(H84), C85(H85), C88(H88), C89(H89), C90(H90),
  C91(H91), C94(H94), C95(H95)
6.c Idealised Me refined as rotating group:
 C96(H96A,H96B,H96C), C99(H99A,H99B,H99C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
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 0.92625(7) 0.61223(10) 0.70983(5) 0.0975(6) Uani 1 1 d . . . . .
Ti2 Ti 0.88076(9) 0.50754(11) 0.81684(6) 0.1060(7) Uani 1 1 d . . . . .
Ti3 Ti 0.74468(8) 0.64024(9) 0.91014(5) 0.0853(5) Uani 1 1 d . . . . .
Ti4 Ti 0.71394(8) 0.83032(9) 0.85989(5) 0.0784(4) Uani 1 1 d . . . . .
Ti5 Ti 0.82344(8) 0.81568(9) 0.73572(5) 0.0862(5) Uani 1 1 d . . . . .
Ti6 Ti 0.81955(7) 0.68164(9) 0.80646(5) 0.0861(5) Uani 1 1 d . . . . .
Ti7 Ti 0.74287(7) 0.56787(9) 0.66965(5) 0.0838(5) Uani 1 1 d . . . . .
Ti8 Ti 0.69611(9) 0.46410(9) 0.77734(5) 0.0913(5) Uani 1 1 d . . . . .
Ti9 Ti 0.56087(8) 0.59747(8) 0.86594(5) 0.0767(4) Uani 1 1 d . . . . .
Ti10 Ti 0.53172(7) 0.78648(8) 0.81401(4) 0.0703(4) Uani 1 1 d . . . . .
Ti11 Ti 0.64824(7) 0.77169(9) 0.68865(4) 0.0763(4) Uani 1 1 d . . . . .
Ti12 Ti 0.63307(7) 0.64086(8) 0.76270(4) 0.0710(4) Uani 1 1 d . . . . .
Ti13 Ti 0.73241(8) 0.59091(11) 0.54831(5) 0.0948(6) Uani 1 1 d . . . . .
Ti14 Ti 0.69865(8) 0.78700(11) 0.56328(5) 0.0943(5) Uani 1 1 d . . . . .
Ti15 Ti 0.66499(8) 0.80719(9) 0.97771(5) 0.0833(5) Uani 1 1 d . . . . .
O1 O 0.8954(3) 0.5889(4) 0.77209(19) 0.101(2) Uani 1 1 d . . . . .
O2 O 0.8262(3) 0.5931(3) 0.85282(18) 0.098(2) Uani 1 1 d . . . . .
O3 O 0.7604(3) 0.7267(3) 0.86869(16) 0.0813(16) Uani 1 1 d . . . . .
O4 O 0.7803(3) 0.7970(3) 0.79544(17) 0.0868(16) Uani 1 1 d . . . . .
O5 O 0.8685(3) 0.7104(3) 0.72418(17) 0.0898(17) Uani 1 1 d . . . . .
O6 O 0.7931(3) 0.4659(3) 0.8028(2) 0.102(2) Uani 1 1 d . . . . .
O7 O 0.6497(3) 0.6084(3) 0.89573(17) 0.0803(15) Uani 1 1 d . . . . .
O8 O 0.6117(3) 0.8230(3) 0.83965(16) 0.0742(14) Uani 1 1 d . . . . .
O9 O 0.7298(3) 0.8195(3) 0.70734(17) 0.0822(15) Uani 1 1 d . . . . .
O10 O 0.8502(3) 0.5775(3) 0.67753(18) 0.0935(18) Uani 1 1 d . . . . .
O11 O 0.7035(3) 0.5404(3) 0.73445(16) 0.0794(16) Uani 1 1 d . . . . .
O12 O 0.6215(3) 0.5390(3) 0.81517(19) 0.0920(17) Uani 1 1 d . . . . .
O13 O 0.5514(2) 0.6774(3) 0.82181(14) 0.0640(12) Uani 1 1 d . . . . .
O14 O 0.5885(2) 0.7572(3) 0.75372(15) 0.0679(13) Uani 1 1 d . . . . .
O15 O 0.6848(3) 0.6661(3) 0.69592(16) 0.0759(14) Uani 1 1 d . . . . .
O16 O 0.7498(3) 0.5895(3) 0.60665(17) 0.0910(17) Uani 1 1 d . . . . .
O17 O 0.6854(3) 0.6901(4) 0.54272(18) 0.0979(19) Uani 1 1 d . . . . .
O18 O 0.6898(3) 0.7781(3) 0.62401(17) 0.0820(15) Uani 1 1 d . . . . .
O19 O 0.6944(3) 0.7079(3) 0.95960(18) 0.0895(17) Uani 1 1 d . . . . .
O20 O 0.6664(3) 0.8525(3) 0.92267(17) 0.0866(16) Uani 1 1 d . . . . .
O21 O 0.9996(3) 0.4983(4) 0.7019(2) 0.104(2) Uani 1 1 d . U . . .
O22 O 0.9669(4) 0.4337(4) 0.7682(2) 0.116(2) Uani 1 1 d . U . . .
O23 O 0.8962(4) 0.4300(4) 0.8658(2) 0.117(2) Uani 1 1 d . U . . .
O24 O 0.9735(7) 0.3651(7) 0.9158(4) 0.211(5) Uani 1 1 d . U . . .
O25 O 0.8462(5) 0.4940(6) 1.0021(4) 0.175(4) Uani 1 1 d . U . . .
O26 O 0.7713(3) 0.5497(4) 0.9499(2) 0.1008(18) Uani 1 1 d . U . . .
O27 O 0.8852(4) 0.8334(6) 1.0263(3) 0.151(3) Uani 1 1 d . U . . .
O28 O 0.7776(3) 0.8372(4) 0.98622(19) 0.0969(17) Uani 1 1 d . U . . .
O29 O 0.4069(3) 0.8522(3) 1.0262(2) 0.0980(18) Uani 1 1 d . . . . .
O30 O 0.5423(3) 0.8006(3) 0.99611(19) 0.0828(15) Uani 1 1 d . . . . .
O31 O 0.8986(6) 0.9680(5) 0.8719(4) 0.179(4) Uani 1 1 d . . . . .
O32 O 0.8230(3) 0.8696(4) 0.8711(2) 0.102(2) Uani 1 1 d . . . . .
O33 O 0.8557(7) 1.0429(6) 0.7213(4) 0.188(4) Uani 1 1 d . . . . .
O34 O 0.8139(4) 0.9303(4) 0.7445(2) 0.1020(19) Uani 1 1 d . . . . .
O35 O 1.1686(4) 0.6710(7) 0.6967(3) 0.180(4) Uani 1 1 d . U . . .
O36 O 1.0381(3) 0.6439(4) 0.7222(2) 0.106(2) Uani 1 1 d . U . . .
O37 O 0.7739(3) 0.4495(4) 0.6577(2) 0.0965(19) Uani 1 1 d . U . . .
O38 O 0.7624(4) 0.3841(4) 0.7254(2) 0.108(2) Uani 1 1 d . . . . .
O39 O 0.4888(5) 0.3481(5) 0.7811(3) 0.140(3) Uani 1 1 d . U . . .
O40 O 0.5926(4) 0.4204(4) 0.7611(2) 0.1000(18) Uani 1 1 d . U . . .
O41 O 0.3358(5) 0.5053(6) 0.8819(4) 0.170(3) Uani 1 1 d . U . . .
O42 O 0.4473(4) 0.5679(4) 0.8563(2) 0.0972(17) Uani 1 1 d . U . . .
O43 O 0.4831(3) 0.6751(3) 0.91461(18) 0.0847(16) Uani 1 1 d . . . . .
O44 O 0.4538(3) 0.7906(3) 0.8799(2) 0.0809(15) Uani 1 1 d . . . . .
O45 O 0.3670(4) 0.9777(4) 0.7865(3) 0.151(3) Uani 1 1 d . . . . .
O46 O 0.4769(3) 0.8950(3) 0.80246(17) 0.0766(14) Uani 1 1 d . . . . .
O47 O 0.4182(3) 0.8061(4) 0.6391(2) 0.111(2) Uani 1 1 d . . . . .
O48 O 0.5343(3) 0.7567(3) 0.66800(17) 0.0808(15) Uani 1 1 d . . . . .
O49 O 0.4819(4) 0.9388(5) 0.5500(3) 0.139(3) Uani 1 1 d . . . . .
O50 O 0.5792(3) 0.8340(4) 0.55687(19) 0.0987(18) Uani 1 1 d . . . . .
O51 O 0.9482(4) 0.7668(5) 0.4984(3) 0.157(3) Uani 1 1 d . U . . .
O52 O 0.8239(3) 0.7836(3) 0.5481(2) 0.1086(18) Uani 1 1 d . U . . .
O53 O 0.9612(4) 0.5831(5) 0.4578(2) 0.130(3) Uani 1 1 d . U . . .
O54 O 0.8535(3) 0.5894(4) 0.5204(2) 0.106(2) Uani 1 1 d . U . . .
O55 O 0.5378(4) 0.4595(5) 0.5606(3) 0.130(3) Uani 1 1 d . U . . .
O56 O 0.6184(3) 0.5535(4) 0.55315(19) 0.0934(17) Uani 1 1 d . U . . .
O57 O 0.6130(3) 0.5437(3) 0.66652(19) 0.0913(17) Uani 1 1 d . . . . .
O58 O 0.5386(3) 0.6011(3) 0.73404(17) 0.0804(15) Uani 1 1 d . . . . .
O59 O 0.9446(3) 0.8188(4) 0.7597(2) 0.105(2) Uani 1 1 d . . . . .
O60 O 0.9317(3) 0.7216(5) 0.8111(2) 0.102(2) Uani 1 1 d . . . . .
O61 O 0.7255(3) 0.6591(3) 0.78715(16) 0.0749(14) Uani 1 1 d . . . . .
N1 N 1.0056(3) 0.6260(4) 0.6403(2) 0.094(2) Uani 1 1 d . U . . .
N2 N 1.0073(5) 0.5211(5) 0.8405(3) 0.110(3) Uani 1 1 d . U . . .
N3 N 0.8683(4) 0.6557(5) 0.9340(2) 0.094(2) Uani 1 1 d . U . . .
N4 N 0.6872(4) 0.7663(4) 1.0502(3) 0.095(2) Uani 1 1 d . U . . .
N5 N 0.6074(3) 0.9155(3) 1.02192(19) 0.0699(16) Uani 1 1 d . . . . .
N6 N 0.7013(5) 0.9532(4) 0.8383(2) 0.096(2) Uani 1 1 d . . . . .
N7 N 0.8985(4) 0.8553(5) 0.6699(3) 0.103(2) Uani 1 1 d . . . . .
N8 N 0.6739(5) 0.3674(4) 0.8262(2) 0.106(2) Uani 1 1 d D U . . .
N9 N 0.5382(4) 0.5016(4) 0.9145(2) 0.0811(17) Uani 1 1 d . U . . .
N10 N 0.4064(3) 0.7739(4) 0.7901(2) 0.0741(17) Uani 1 1 d . . . . .
N11 N 0.5709(4) 0.8892(4) 0.6882(2) 0.0792(17) Uani 1 1 d . . . . .
N12 N 0.6947(5) 0.9169(5) 0.5707(3) 0.106(2) Uani 1 1 d . . . . .
N13 N 0.7296(5) 0.8021(3) 0.4855(3) 0.135(2) Uani 1 1 d D U . . .
N14 N 0.7396(4) 0.5663(4) 0.4704(2) 0.094(2) Uani 1 1 d . U . . .
N15 N 0.7598(4) 0.4627(5) 0.5509(2) 0.097(2) Uani 1 1 d . U . . .
N16 N 0.4759(4) 0.6808(6) 0.5675(3) 0.117(3) Uani 1 1 d D . . . .
H16A H 0.461(7) 0.732(3) 0.583(4) 0.141 Uiso 1 1 d DR . . . .
C1 C 0.9830(5) 0.6176(6) 0.5974(3) 0.1065(19) Uani 1 1 d . U . . .
H1 H 0.9278 0.6049 0.5958 0.128 Uiso 1 1 calc R . . . .
C2 C 1.0369(5) 0.6269(6) 0.5575(3) 0.110(2) Uani 1 1 d . U . . .
H2 H 1.0207 0.6187 0.5281 0.132 Uiso 1 1 calc R . . . .
C3 C 1.1143(6) 0.6481(7) 0.5595(4) 0.119(2) Uani 1 1 d . U . . .
H3 H 1.1522 0.6574 0.5317 0.143 Uiso 1 1 calc R . . . .
C4 C 1.1373(6) 0.6558(7) 0.6041(3) 0.116(2) Uani 1 1 d . U . . .
H4 H 1.1926 0.6675 0.6067 0.140 Uiso 1 1 calc R . . . .
C5 C 1.0812(5) 0.6468(6) 0.6418(3) 0.1085(19) Uani 1 1 d . U . . .
C6 C 1.1007(6) 0.6518(7) 0.6906(3) 0.111(2) Uani 1 1 d . U . . .
C7 C 1.0049(6) 0.4427(7) 0.7277(4) 0.108(3) Uani 1 1 d . U . . .
H7 H 1.0447 0.3991 0.7147 0.130 Uiso 1 1 calc R . . . .
C8 C 1.0562(7) 0.5723(8) 0.8249(4) 0.125(2) Uani 1 1 d . U . . .
H8 H 1.0433 0.6045 0.7997 0.150 Uiso 1 1 calc R . . . .
C9 C 1.1309(7) 0.5794(8) 0.8465(4) 0.132(2) Uani 1 1 d . U . . .
H9 H 1.1669 0.6175 0.8377 0.158 Uiso 1 1 calc R . . . .
C10 C 1.1443(7) 0.5286(8) 0.8791(5) 0.135(2) Uani 1 1 d . U . . .
H10 H 1.1933 0.5315 0.8932 0.161 Uiso 1 1 calc R . . . .
C11 C 1.0972(7) 0.4729(8) 0.8951(4) 0.135(2) Uani 1 1 d . U . . .
H11 H 1.1127 0.4379 0.9185 0.162 Uiso 1 1 calc R . . . .
C12 C 1.0220(6) 0.4700(7) 0.8743(4) 0.122(2) Uani 1 1 d . U . . .
C13 C 0.9615(7) 0.4150(8) 0.8886(4) 0.125(2) Uani 1 1 d . U . . .
C14 C 0.9150(6) 0.7099(7) 0.9217(4) 0.110(2) Uani 1 1 d . U . . .
H14 H 0.8970 0.7467 0.8998 0.132 Uiso 1 1 calc R . . . .
C15 C 0.9927(6) 0.7168(7) 0.9396(4) 0.119(2) Uani 1 1 d . U . . .
H15 H 1.0264 0.7565 0.9306 0.143 Uiso 1 1 calc R . . . .
C16 C 1.0132(7) 0.6610(7) 0.9705(4) 0.124(2) Uani 1 1 d . U . . .
H16 H 1.0638 0.6616 0.9835 0.149 Uiso 1 1 calc R . . . .
C17 C 0.9650(7) 0.6046(8) 0.9835(4) 0.127(2) Uani 1 1 d . U . . .
H17 H 0.9813 0.5666 1.0052 0.152 Uiso 1 1 calc R . . . .
C18 C 0.8909(6) 0.6041(7) 0.9643(4) 0.111(2) Uani 1 1 d . U . . .
C19 C 0.8359(6) 0.5428(7) 0.9738(4) 0.115(2) Uani 1 1 d . U . . .
C20 C 0.6379(7) 0.7287(6) 1.0822(4) 0.107(2) Uani 1 1 d D U . . .
H20 H 0.5805 0.7269 1.0778 0.128 Uiso 1 1 calc R . . . .
C21 C 0.6644(6) 0.6929(7) 1.1204(4) 0.124(2) Uani 1 1 d D U . . .
H21 H 0.6277 0.6663 1.1418 0.149 Uiso 1 1 calc R . . . .
C22 C 0.7494(7) 0.6979(7) 1.1261(4) 0.130(2) Uani 1 1 d D U . . .
H22 H 0.7717 0.6742 1.1520 0.156 Uiso 1 1 calc R . . . .
C23 C 0.7998(7) 0.7370(7) 1.0941(4) 0.127(2) Uani 1 1 d D U . . .
H23 H 0.8570 0.7410 1.0979 0.152 Uiso 1 1 calc R . . . .
C24 C 0.7669(6) 0.7705(7) 1.0566(4) 0.114(2) Uani 1 1 d D U . . .
C25 C 0.8152(6) 0.8172(7) 1.0210(4) 0.1089(18) Uani 1 1 d . U . . .
C26 C 0.6456(5) 0.9700(5) 1.0359(3) 0.0835(17) Uani 1 1 d . U . . .
H26 H 0.7057 0.9680 1.0256 0.100 Uiso 1 1 calc R . . . .
C27 C 0.6018(5) 1.0306(5) 1.0654(3) 0.0893(19) Uani 1 1 d . U . . .
H27 H 0.6321 1.0681 1.0757 0.107 Uiso 1 1 calc R . . . .
C28 C 0.5153(5) 1.0361(5) 1.0793(3) 0.0849(18) Uani 1 1 d . U . . .
H28 H 0.4841 1.0780 1.0989 0.102 Uiso 1 1 calc R . . . .
C29 C 0.4738(5) 0.9792(5) 1.0642(3) 0.0824(17) Uani 1 1 d . U . . .
H29 H 0.4132 0.9818 1.0729 0.099 Uiso 1 1 calc R . . . .
C30 C 0.5217(4) 0.9190(4) 1.0365(3) 0.0755(17) Uani 1 1 d . U . . .
C31 C 0.4852(5) 0.8557(5) 1.0185(3) 0.0819(17) Uani 1 1 d . U . . .
C32 C 0.6367(6) 0.9904(6) 0.8181(4) 0.112(2) Uani 1 1 d . U . . .
H32 H 0.5920 0.9637 0.8121 0.135 Uiso 1 1 calc R . . . .
C33 C 0.6358(7) 1.0667(7) 0.8063(4) 0.119(2) Uani 1 1 d . U . . .
H33 H 0.5887 1.0938 0.7938 0.143 Uiso 1 1 calc R . . . .
C34 C 0.7043(8) 1.1043(7) 0.8129(4) 0.131(2) Uani 1 1 d . U . . .
H34 H 0.7043 1.1570 0.8047 0.157 Uiso 1 1 calc R . . . .
C35 C 0.7714(7) 1.0647(7) 0.8313(4) 0.126(2) Uani 1 1 d . U . . .
H35 H 0.8194 1.0887 0.8351 0.151 Uiso 1 1 calc R . . . .
C36 C 0.7672(7) 0.9875(7) 0.8442(4) 0.115(2) Uani 1 1 d . U . . .
C37 C 0.8354(7) 0.9377(8) 0.8639(4) 0.116(2) Uani 1 1 d . U . . .
C38 C 0.9334(6) 0.8151(7) 0.6303(4) 0.115(2) Uani 1 1 d . U . . .
H38 H 0.9245 0.7630 0.6270 0.139 Uiso 1 1 calc R . . . .
C39 C 0.9827(6) 0.8493(8) 0.5941(4) 0.123(2) Uani 1 1 d . U . . .
H39 H 1.0087 0.8196 0.5666 0.147 Uiso 1 1 calc R . . . .
C40 C 0.9938(7) 0.9219(8) 0.5972(4) 0.130(3) Uani 1 1 d . U . . .
H40 H 1.0280 0.9449 0.5725 0.156 Uiso 1 1 calc R . . . .
C41 C 0.9551(7) 0.9629(8) 0.6366(4) 0.129(2) Uani 1 1 d . U . . .
H41 H 0.9610 1.0160 0.6389 0.155 Uiso 1 1 calc R . . . .
C42 C 0.9082(6) 0.9305(8) 0.6727(4) 0.116(2) Uani 1 1 d . U . . .
C43 C 0.8553(7) 0.9721(9) 0.7165(4) 0.122(2) Uani 1 1 d . U . . .
C44 C 0.7820(6) 0.3886(7) 0.6825(4) 0.106(2) Uani 1 1 d . U . . .
H44 H 0.8057 0.3414 0.6659 0.128 Uiso 1 1 calc R . . . .
C45 C 0.7254(6) 0.3425(6) 0.8582(3) 0.114(2) Uani 1 1 d D U . . .
H45 H 0.7761 0.3639 0.8598 0.137 Uiso 1 1 calc R . . . .
C46 C 0.7005(7) 0.2842(6) 0.8884(3) 0.119(2) Uani 1 1 d D U . . .
H46 H 0.7338 0.2668 0.9117 0.143 Uiso 1 1 calc R . . . .
C47 C 0.6316(7) 0.2533(6) 0.8848(4) 0.125(2) Uani 1 1 d D U . . .
H47 H 0.6176 0.2126 0.9052 0.150 Uiso 1 1 calc R . . . .
C48 C 0.5788(6) 0.2770(6) 0.8529(4) 0.122(2) Uani 1 1 d D U . . .
H48 H 0.5287 0.2546 0.8513 0.146 Uiso 1 1 calc R . . . .
C49 C 0.6026(6) 0.3357(6) 0.8230(3) 0.111(2) Uani 1 1 d D U . . .
C50 C 0.5575(8) 0.3701(7) 0.7870(4) 0.110(2) Uani 1 1 d . U . . .
C51 C 0.5910(6) 0.4660(5) 0.9428(3) 0.0917(17) Uani 1 1 d . U . . .
H51 H 0.6477 0.4779 0.9403 0.110 Uiso 1 1 calc R . . . .
C52 C 0.5636(6) 0.4121(6) 0.9754(3) 0.0978(19) Uani 1 1 d . U . . .
H52 H 0.6023 0.3864 0.9941 0.117 Uiso 1 1 calc R . . . .
C53 C 0.4804(6) 0.3961(5) 0.9807(3) 0.0954(19) Uani 1 1 d . U . . .
H53 H 0.4610 0.3601 1.0032 0.114 Uiso 1 1 calc R . . . .
C54 C 0.4270(6) 0.4328(6) 0.9531(3) 0.097(2) Uani 1 1 d . U . . .
H54 H 0.3687 0.4245 0.9571 0.117 Uiso 1 1 calc R . . . .
C55 C 0.4574(6) 0.4820(5) 0.9194(3) 0.0915(18) Uani 1 1 d . U . . .
C56 C 0.4102(7) 0.5233(7) 0.8844(4) 0.103(2) Uani 1 1 d . U . . .
C57 C 0.4488(4) 0.7454(6) 0.9134(3) 0.078(2) Uani 1 1 d . U . . .
H57 H 0.4147 0.7666 0.9418 0.094 Uiso 1 1 calc R . . . .
C58 C 0.3770(5) 0.7122(6) 0.7823(3) 0.0930(19) Uani 1 1 d . U . . .
H58 H 0.4073 0.6639 0.7898 0.112 Uiso 1 1 calc R . . . .
C59 C 0.3008(5) 0.7124(6) 0.7631(3) 0.105(2) Uani 1 1 d . U . . .
H59 H 0.2807 0.6655 0.7573 0.126 Uiso 1 1 calc R . . . .
C60 C 0.2585(6) 0.7808(6) 0.7534(4) 0.111(2) Uani 1 1 d . U . . .
H60 H 0.2077 0.7831 0.7401 0.133 Uiso 1 1 calc R . . . .
C61 C 0.2881(5) 0.8479(7) 0.7626(4) 0.112(2) Uani 1 1 d . U . . .
H61 H 0.2579 0.8971 0.7567 0.134 Uiso 1 1 calc R . . . .
C62 C 0.3627(5) 0.8418(6) 0.7808(3) 0.0966(18) Uani 1 1 d . U . . .
C63 C 0.4028(5) 0.9126(6) 0.7897(3) 0.1030(19) Uani 1 1 d . U . . .
C64 C 0.5923(6) 0.9567(6) 0.6992(3) 0.106(2) Uani 1 1 d . U . . .
H64 H 0.6459 0.9569 0.7092 0.127 Uiso 1 1 calc R . . . .
C65 C 0.5412(7) 1.0240(7) 0.6967(4) 0.124(2) Uani 1 1 d . U . . .
H65 H 0.5586 1.0711 0.7048 0.148 Uiso 1 1 calc R . . . .
C66 C 0.4662(7) 1.0248(7) 0.6829(4) 0.119(2) Uani 1 1 d . U . . .
H66 H 0.4281 1.0724 0.6839 0.143 Uiso 1 1 calc R . . . .
C67 C 0.4421(6) 0.9604(6) 0.6675(4) 0.1137(18) Uani 1 1 d . U . . .
H67 H 0.3914 0.9622 0.6542 0.136 Uiso 1 1 calc R . . . .
C68 C 0.4961(5) 0.8902(6) 0.6723(3) 0.1023(17) Uani 1 1 d . U . . .
C69 C 0.4789(5) 0.8124(6) 0.6591(3) 0.0970(18) Uani 1 1 d . U . . .
C70 C 0.7538(8) 0.9516(8) 0.5809(4) 0.129(2) Uani 1 1 d . U . . .
H70 H 0.8081 0.9221 0.5831 0.155 Uiso 1 1 calc R . . . .
C71 C 0.7412(8) 1.0338(8) 0.5892(5) 0.140(3) Uani 1 1 d . U . . .
H71 H 0.7850 1.0590 0.5981 0.168 Uiso 1 1 calc R . . . .
C72 C 0.6620(8) 1.0747(8) 0.5836(4) 0.136(2) Uani 1 1 d . U . . .
H72 H 0.6507 1.1295 0.5876 0.163 Uiso 1 1 calc R . . . .
C73 C 0.6016(8) 1.0355(8) 0.5726(4) 0.131(2) Uani 1 1 d . U . . .
H73 H 0.5468 1.0629 0.5694 0.157 Uiso 1 1 calc R . . . .
C74 C 0.6175(7) 0.9571(7) 0.5659(4) 0.122(2) Uani 1 1 d . U . . .
C75 C 0.5521(7) 0.9098(8) 0.5563(4) 0.119(2) Uani 1 1 d . U . . .
C76 C 0.8677(8) 0.7790(3) 0.5078(4) 0.133(2) Uani 1 1 d . U . . .
C77 C 0.8172(7) 0.7892(3) 0.4694(4) 0.146(2) Uani 1 1 d D U . . .
C78 C 0.8540(8) 0.7861(4) 0.4205(4) 0.161(3) Uani 1 1 d D U . . .
H78 H 0.9145 0.7771 0.4102 0.193 Uiso 1 1 calc R . . . .
C79 C 0.7975(8) 0.7968(5) 0.3896(4) 0.163(3) Uani 1 1 d D U . . .
H79 H 0.8192 0.7952 0.3569 0.195 Uiso 1 1 calc R . . . .
C80 C 0.7101(8) 0.8097(5) 0.4048(4) 0.165(3) Uani 1 1 d D U . . .
H80 H 0.6721 0.8169 0.3827 0.197 Uiso 1 1 calc R . . . .
C81 C 0.6772(7) 0.8123(5) 0.4521(4) 0.147(2) Uani 1 1 d D U . . .
H81 H 0.6165 0.8213 0.4619 0.177 Uiso 1 1 calc R . . . .
C82 C 0.6772(6) 0.5577(6) 0.4464(3) 0.1064(19) Uani 1 1 d . U . . .
H82 H 0.6207 0.5567 0.4631 0.128 Uiso 1 1 calc R . . . .
C83 C 0.6921(6) 0.5501(6) 0.3973(3) 0.112(2) Uani 1 1 d . U . . .
H83 H 0.6457 0.5489 0.3808 0.135 Uiso 1 1 calc R . . . .
C84 C 0.7744(7) 0.5445(7) 0.3738(4) 0.119(2) Uani 1 1 d . U . . .
H84 H 0.7865 0.5332 0.3412 0.143 Uiso 1 1 calc R . . . .
C85 C 0.8428(7) 0.5555(6) 0.3979(3) 0.116(2) Uani 1 1 d . U . . .
H85 H 0.8999 0.5561 0.3820 0.140 Uiso 1 1 calc R . . . .
C86 C 0.8208(6) 0.5652(6) 0.4462(3) 0.108(2) Uani 1 1 d . U . . .
C87 C 0.8857(6) 0.5805(7) 0.4752(3) 0.1117(19) Uani 1 1 d . U . . .
C88 C 0.8363(6) 0.4173(6) 0.5535(3) 0.1000(18) Uani 1 1 d . U . . .
H88 H 0.8863 0.4415 0.5506 0.120 Uiso 1 1 calc R . . . .
C89 C 0.8450(6) 0.3414(6) 0.5599(3) 0.105(2) Uani 1 1 d . U . . .
H89 H 0.9001 0.3124 0.5609 0.126 Uiso 1 1 calc R . . . .
C90 C 0.7712(6) 0.3041(6) 0.5653(3) 0.110(2) Uani 1 1 d . U . . .
H90 H 0.7751 0.2499 0.5699 0.132 Uiso 1 1 calc R . . . .
C91 C 0.6937(6) 0.3495(6) 0.5635(3) 0.107(2) Uani 1 1 d . U . . .
H91 H 0.6426 0.3267 0.5673 0.128 Uiso 1 1 calc R . . . .
C92 C 0.6896(6) 0.4259(6) 0.5564(3) 0.0982(19) Uani 1 1 d . U . . .
C93 C 0.6090(6) 0.4824(7) 0.5565(3) 0.0999(19) Uani 1 1 d . U . . .
C94 C 0.5480(5) 0.5596(5) 0.6967(3) 0.089(3) Uani 1 1 d . U . . .
H94 H 0.4989 0.5384 0.6916 0.106 Uiso 1 1 calc R . . . .
C95 C 0.9680(7) 0.7749(8) 0.7902(4) 0.109(2) Uani 1 1 d . U . . .
H95 H 1.0208 0.7821 0.7994 0.130 Uiso 1 1 calc R . . . .
C96 C 0.3891(9) 0.6223(8) 0.6303(5) 0.159(4) Uani 1 1 d . U . . .
H96A H 0.4430 0.5884 0.6328 0.238 Uiso 1 1 calc GR . . . .
H96B H 0.3409 0.5931 0.6377 0.238 Uiso 1 1 calc GR . . . .
H96C H 0.3807 0.6662 0.6524 0.238 Uiso 1 1 calc GR . . . .
C97 C 0.3933(8) 0.6524(9) 0.5803(5) 0.155(4) Uani 1 1 d . U . . .
H97A H 0.3893 0.6103 0.5585 0.186 Uiso 1 1 calc R . . . .
H97B H 0.3450 0.6948 0.5789 0.186 Uiso 1 1 calc R . . . .
C98 C 0.4826(8) 0.7012(8) 0.5150(4) 0.144(4) Uani 1 1 d . U . . .
H98A H 0.5420 0.7099 0.5027 0.172 Uiso 1 1 calc R . . . .
H98B H 0.4709 0.6566 0.4974 0.172 Uiso 1 1 calc R . . . .
C99 C 0.4237(9) 0.7687(9) 0.5072(5) 0.168(5) Uani 1 1 d . U . . .
H99A H 0.3664 0.7545 0.5077 0.252 Uiso 1 1 calc GR . . . .
H99B H 0.4435 0.7899 0.4766 0.252 Uiso 1 1 calc GR . . . .
H99C H 0.4209 0.8076 0.5318 0.252 Uiso 1 1 calc GR . . . .


_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 1.850(6) . ?
Ti1 O5 1.832(5) . ?
Ti1 O10 1.825(5) . ?
Ti1 O21 2.142(7) . ?
Ti1 O36 2.035(5) . ?
Ti1 N1 2.225(7) . ?
Ti2 O1 1.934(8) . ?
Ti2 O2 1.843(5) . ?
Ti2 O6 1.776(6) . ?
Ti2 O22 2.089(6) . ?
Ti2 O23 1.979(7) . ?
Ti2 N2 2.284(9) . ?
Ti3 O2 2.022(5) . ?
Ti3 O3 1.945(6) . ?
Ti3 O7 1.804(5) . ?
Ti3 O19 1.854(5) . ?
Ti3 O26 1.989(6) . ?
Ti3 N3 2.252(7) . ?
Ti4 O3 1.883(6) . ?
Ti4 O4 2.027(5) . ?
Ti4 O8 1.847(4) . ?
Ti4 O20 1.869(5) . ?
Ti4 O32 2.040(6) . ?
Ti4 N6 2.223(8) . ?
Ti5 O4 1.800(6) . ?
Ti5 O5 1.881(6) . ?
Ti5 O9 1.817(5) . ?
Ti5 O34 2.000(7) . ?
Ti5 O59 2.171(5) . ?
Ti5 N7 2.240(9) . ?
Ti6 O1 2.023(4) . ?
Ti6 O2 2.046(7) . ?
Ti6 O3 1.995(4) . ?
Ti6 O4 2.058(6) . ?
Ti6 O5 2.457(6) . ?
Ti6 O60 2.042(7) . ?
Ti6 O61 1.785(4) . ?
Ti7 O10 1.798(5) . ?
Ti7 O11 1.960(6) . ?
Ti7 O15 1.917(4) . ?
Ti7 O16 1.853(6) . ?
Ti7 O37 2.069(6) . ?
Ti7 O57 2.194(5) . ?
Ti8 O6 1.828(5) . ?
Ti8 O11 1.822(6) . ?
Ti8 O12 1.853(5) . ?
Ti8 O38 2.092(5) . ?
Ti8 O40 2.045(7) . ?
Ti8 N8 2.231(8) . ?
Ti9 O7 1.814(4) . ?
Ti9 O12 1.839(5) . ?
Ti9 O13 1.897(5) . ?
Ti9 O42 2.022(6) . ?
Ti9 O43 2.071(5) . ?
Ti9 N9 2.216(8) . ?
Ti10 O8 1.778(4) . ?
Ti10 O13 1.902(5) . ?
Ti10 O14 1.863(4) . ?
Ti10 O44 2.092(6) . ?
Ti10 O46 2.015(5) . ?
Ti10 N10 2.266(6) . ?
Ti11 O9 1.805(5) . ?
Ti11 O14 1.999(5) . ?
Ti11 O15 1.871(5) . ?
Ti11 O18 1.889(5) . ?
Ti11 O48 2.061(4) . ?
Ti11 N11 2.231(6) . ?
Ti12 O11 2.030(4) . ?
Ti12 O12 2.344(7) . ?
Ti12 O13 2.012(4) . ?
Ti12 O14 2.080(5) . ?
Ti12 O15 2.047(5) . ?
Ti12 O58 2.048(5) . ?
Ti12 O61 1.811(4) . ?
Ti13 O16 1.760(5) . ?
Ti13 O17 1.798(6) . ?
Ti13 O54 1.960(6) . ?
Ti13 O56 2.008(6) . ?
Ti13 N14 2.284(6) . ?
Ti13 N15 2.220(8) . ?
Ti14 O17 1.852(6) . ?
Ti14 O18 1.752(5) . ?
Ti14 O50 1.996(5) . ?
Ti14 O52 1.963(6) . ?
Ti14 N12 2.271(9) . ?
Ti14 N13 2.251(9) . ?
Ti15 O19 1.784(5) . ?
Ti15 O20 1.777(6) . ?
Ti15 O28 2.001(5) . ?
Ti15 O30 1.961(5) . ?
Ti15 N4 2.285(8) . ?
Ti15 N5 2.274(5) . ?
O21 C7 1.224(13) . ?
O22 C7 1.250(13) . ?
O23 C13 1.318(11) . ?
O24 C13 1.190(14) . ?
O25 C19 1.196(13) . ?
O26 C19 1.326(10) . ?
O27 C25 1.228(11) . ?
O28 C25 1.278(10) . ?
O29 C31 1.241(9) . ?
O30 C31 1.310(8) . ?
O31 C37 1.261(13) . ?
O32 C37 1.247(13) . ?
O33 C43 1.246(15) . ?
O34 C43 1.260(15) . ?
O35 C6 1.223(11) . ?
O36 C6 1.259(12) . ?
O37 C44 1.284(12) . ?
O38 C44 1.234(12) . ?
O39 C50 1.253(14) . ?
O40 C50 1.285(13) . ?
O41 C56 1.287(13) . ?
O42 C56 1.262(12) . ?
O43 C57 1.269(10) . ?
O44 C57 1.247(10) . ?
O45 C63 1.202(11) . ?
O46 C63 1.291(9) . ?
O47 C69 1.229(9) . ?
O48 C69 1.268(9) . ?
O49 C75 1.201(11) . ?
O50 C75 1.331(13) . ?
O51 C76 1.252(12) . ?
O52 C76 1.252(13) . ?
O53 C87 1.232(11) . ?
O54 C87 1.328(11) . ?
O55 C93 1.247(12) . ?
O56 C93 1.274(12) . ?
O57 C94 1.234(9) . ?
O58 C94 1.282(8) . ?
O59 C95 1.239(14) . ?
O60 C95 1.269(14) . ?
N1 C1 1.367(10) . ?
N1 C5 1.319(10) . ?
N2 C8 1.304(15) . ?
N2 C12 1.350(13) . ?
N3 C14 1.304(13) . ?
N3 C18 1.308(12) . ?
N4 C20 1.345(13) . ?
N4 C24 1.329(11) . ?
N5 C26 1.307(9) . ?
N5 C30 1.353(9) . ?
N6 C32 1.349(11) . ?
N6 C36 1.322(12) . ?
N7 C38 1.340(11) . ?
N7 C42 1.351(14) . ?
N8 C45 1.368(10) . ?
N8 C49 1.356(11) . ?
N9 C51 1.357(10) . ?
N9 C55 1.368(11) . ?
N10 C58 1.275(11) . ?
N10 C62 1.333(10) . ?
N11 C64 1.331(12) . ?
N11 C68 1.348(10) . ?
N12 C70 1.269(14) . ?
N12 C74 1.351(12) . ?
N13 C77 1.381(11) . ?
N13 C81 1.378(11) . ?
N14 C82 1.332(10) . ?
N14 C86 1.363(12) . ?
N15 C88 1.364(10) . ?
N15 C92 1.359(12) . ?
N16 H16A 0.98(2) . ?
N16 C97 1.468(17) . ?
N16 C98 1.551(14) . ?
C1 H1 0.9500 . ?
C1 C2 1.345(13) . ?
C2 H2 0.9500 . ?
C2 C3 1.352(13) . ?
C3 H3 0.9500 . ?
C3 C4 1.416(13) . ?
C4 H4 0.9500 . ?
C4 C5 1.317(14) . ?
C5 C6 1.506(12) . ?
C7 H7 0.9500 . ?
C8 H8 0.9500 . ?
C8 C9 1.460(14) . ?
C9 H9 0.9500 . ?
C9 C10 1.316(16) . ?
C10 H10 0.9500 . ?
C10 C11 1.351(17) . ?
C11 H11 0.9500 . ?
C11 C12 1.438(14) . ?
C12 C13 1.474(17) . ?
C14 H14 0.9500 . ?
C14 C15 1.443(13) . ?
C15 H15 0.9500 . ?
C15 C16 1.361(15) . ?
C16 H16 0.9500 . ?
C16 C17 1.352(16) . ?
C17 H17 0.9500 . ?
C17 C18 1.393(13) . ?
C18 C19 1.480(16) . ?
C20 H20 0.9500 . ?
C20 C21 1.369(13) . ?
C21 H21 0.9500 . ?
C21 C22 1.409(11) . ?
C22 H22 0.9500 . ?
C22 C23 1.371(12) . ?
C23 H23 0.9500 . ?
C23 C24 1.379(11) . ?
C24 C25 1.497(16) . ?
C26 H26 0.9500 . ?
C26 C27 1.386(10) . ?
C27 H27 0.9500 . ?
C27 C28 1.359(11) . ?
C28 H28 0.9500 . ?
C28 C29 1.387(11) . ?
C29 H29 0.9500 . ?
C29 C30 1.376(10) . ?
C30 C31 1.464(11) . ?
C32 H32 0.9500 . ?
C32 C33 1.374(15) . ?
C33 H33 0.9500 . ?
C33 C34 1.398(15) . ?
C34 H34 0.9500 . ?
C34 C35 1.368(15) . ?
C35 H35 0.9500 . ?
C35 C36 1.407(16) . ?
C36 C37 1.479(15) . ?
C38 H38 0.9500 . ?
C38 C39 1.391(16) . ?
C39 H39 0.9500 . ?
C39 C40 1.312(16) . ?
C40 H40 0.9500 . ?
C40 C41 1.356(14) . ?
C41 H41 0.9500 . ?
C41 C42 1.356(16) . ?
C42 C43 1.520(14) . ?
C44 H44 0.9500 . ?
C45 H45 0.9500 . ?
C45 C46 1.398(11) . ?
C46 H46 0.9500 . ?
C46 C47 1.317(11) . ?
C47 H47 0.9500 . ?
C47 C48 1.375(11) . ?
C48 H48 0.9500 . ?
C48 C49 1.394(11) . ?
C49 C50 1.446(14) . ?
C51 H51 0.9500 . ?
C51 C52 1.396(13) . ?
C52 H52 0.9500 . ?
C52 C53 1.381(13) . ?
C53 H53 0.9500 . ?
C53 C54 1.355(12) . ?
C54 H54 0.9500 . ?
C54 C55 1.374(13) . ?
C55 C56 1.485(13) . ?
C57 H57 0.9500 . ?
C58 H58 0.9500 . ?
C58 C59 1.421(11) . ?
C59 H59 0.9500 . ?
C59 C60 1.333(13) . ?
C60 H60 0.9500 . ?
C60 C61 1.374(14) . ?
C61 H61 0.9500 . ?
C61 C62 1.370(11) . ?
C62 C63 1.518(14) . ?
C64 H64 0.9500 . ?
C64 C65 1.334(13) . ?
C65 H65 0.9500 . ?
C65 C66 1.324(14) . ?
C66 H66 0.9500 . ?
C66 C67 1.344(15) . ?
C67 H67 0.9500 . ?
C67 C68 1.409(13) . ?
C68 C69 1.491(14) . ?
C70 H70 0.9500 . ?
C70 C71 1.436(17) . ?
C71 H71 0.9500 . ?
C71 C72 1.388(15) . ?
C72 H72 0.9500 . ?
C72 C73 1.345(17) . ?
C73 H73 0.9500 . ?
C73 C74 1.363(16) . ?
C74 C75 1.487(16) . ?
C76 C77 1.478(15) . ?
C77 C78 1.437(13) . ?
C78 H78 0.9500 . ?
C78 C79 1.369(12) . ?
C79 H79 0.9500 . ?
C79 C80 1.375(12) . ?
C80 H80 0.9500 . ?
C80 C81 1.381(12) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C82 C83 1.409(12) . ?
C83 H83 0.9500 . ?
C83 C84 1.362(14) . ?
C84 H84 0.9500 . ?
C84 C85 1.429(13) . ?
C85 H85 0.9500 . ?
C85 C86 1.388(13) . ?
C86 C87 1.494(13) . ?
C88 H88 0.9500 . ?
C88 C89 1.328(13) . ?
C89 H89 0.9500 . ?
C89 C90 1.416(14) . ?
C90 H90 0.9500 . ?
C90 C91 1.372(12) . ?
C91 H91 0.9500 . ?
C91 C92 1.343(14) . ?
C92 C93 1.497(12) . ?
C94 H94 0.9500 . ?
C95 H95 0.9500 . ?
C96 H96A 0.9800 . ?
C96 H96B 0.9800 . ?
C96 H96C 0.9800 . ?
C96 C97 1.534(18) . ?
C97 H97A 0.9900 . ?
C97 H97B 0.9900 . ?
C98 H98A 0.9900 . ?
C98 H98B 0.9900 . ?
C98 C99 1.435(15) . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O21 86.3(3) . . ?
O1 Ti1 O36 91.3(2) . . ?
O1 Ti1 N1 161.3(2) . . ?
O5 Ti1 O1 87.7(2) . . ?
O5 Ti1 O21 172.2(2) . . ?
O5 Ti1 O36 91.3(2) . . ?
O5 Ti1 N1 102.9(3) . . ?
O10 Ti1 O1 107.6(3) . . ?
O10 Ti1 O5 98.5(2) . . ?
O10 Ti1 O21 88.0(2) . . ?
O10 Ti1 O36 158.9(2) . . ?
O10 Ti1 N1 86.2(2) . . ?
O21 Ti1 N1 81.6(3) . . ?
O36 Ti1 O21 83.9(2) . . ?
O36 Ti1 N1 73.3(2) . . ?
O1 Ti2 O22 87.1(3) . . ?
O1 Ti2 O23 164.5(3) . . ?
O1 Ti2 N2 90.7(3) . . ?
O2 Ti2 O1 79.3(3) . . ?
O2 Ti2 O22 163.0(4) . . ?
O2 Ti2 O23 100.8(3) . . ?
O2 Ti2 N2 90.0(2) . . ?
O6 Ti2 O1 104.5(3) . . ?
O6 Ti2 O2 102.5(2) . . ?
O6 Ti2 O22 90.6(3) . . ?
O6 Ti2 O23 90.6(3) . . ?
O6 Ti2 N2 161.8(3) . . ?
O22 Ti2 N2 80.1(2) . . ?
O23 Ti2 O22 89.7(3) . . ?
O23 Ti2 N2 73.9(3) . . ?
O2 Ti3 N3 82.6(2) . . ?
O3 Ti3 O2 75.2(2) . . ?
O3 Ti3 O26 160.6(2) . . ?
O3 Ti3 N3 87.9(3) . . ?
O7 Ti3 O2 96.2(2) . . ?
O7 Ti3 O3 103.1(2) . . ?
O7 Ti3 O19 99.7(2) . . ?
O7 Ti3 O26 93.9(3) . . ?
O7 Ti3 N3 168.3(3) . . ?
O19 Ti3 O2 160.8(3) . . ?
O19 Ti3 O3 90.8(2) . . ?
O19 Ti3 O26 95.4(2) . . ?
O19 Ti3 N3 83.9(2) . . ?
O26 Ti3 O2 94.1(2) . . ?
O26 Ti3 N3 74.6(3) . . ?
O3 Ti4 O4 77.4(2) . . ?
O3 Ti4 O32 92.3(2) . . ?
O3 Ti4 N6 161.9(2) . . ?
O4 Ti4 O32 86.0(2) . . ?
O4 Ti4 N6 89.9(2) . . ?
O8 Ti4 O3 103.9(2) . . ?
O8 Ti4 O4 90.23(18) . . ?
O8 Ti4 O20 96.6(2) . . ?
O8 Ti4 O32 162.2(3) . . ?
O8 Ti4 N6 88.8(2) . . ?
O20 Ti4 O3 96.0(2) . . ?
O20 Ti4 O4 171.5(2) . . ?
O20 Ti4 O32 89.0(2) . . ?
O20 Ti4 N6 95.3(2) . . ?
O32 Ti4 N6 73.7(3) . . ?
O4 Ti5 O5 91.4(3) . . ?
O4 Ti5 O9 102.2(2) . . ?
O4 Ti5 O34 95.9(3) . . ?
O4 Ti5 O59 86.5(2) . . ?
O4 Ti5 N7 165.6(2) . . ?
O5 Ti5 O34 162.4(2) . . ?
O5 Ti5 O59 83.1(2) . . ?
O5 Ti5 N7 94.3(3) . . ?
O9 Ti5 O5 98.5(2) . . ?
O9 Ti5 O34 95.6(2) . . ?
O9 Ti5 O59 171.1(3) . . ?
O9 Ti5 N7 90.1(2) . . ?
O34 Ti5 O59 81.4(3) . . ?
O34 Ti5 N7 75.1(3) . . ?
O59 Ti5 N7 81.0(3) . . ?
O1 Ti6 O2 72.6(2) . . ?
O1 Ti6 O4 139.1(3) . . ?
O1 Ti6 O5 68.7(2) . . ?
O1 Ti6 O60 85.7(2) . . ?
O2 Ti6 O4 147.84(19) . . ?
O2 Ti6 O5 141.27(18) . . ?
O3 Ti6 O1 145.6(3) . . ?
O3 Ti6 O2 73.6(2) . . ?
O3 Ti6 O4 74.3(2) . . ?
O3 Ti6 O5 145.0(2) . . ?
O3 Ti6 O60 93.5(2) . . ?
O4 Ti6 O5 70.80(19) . . ?
O60 Ti6 O2 99.7(3) . . ?
O60 Ti6 O4 81.6(2) . . ?
O60 Ti6 O5 79.3(2) . . ?
O61 Ti6 O1 92.80(19) . . ?
O61 Ti6 O2 94.8(2) . . ?
O61 Ti6 O3 96.52(19) . . ?
O61 Ti6 O4 89.4(2) . . ?
O61 Ti6 O5 85.5(2) . . ?
O61 Ti6 O60 164.2(3) . . ?
O10 Ti7 O11 95.6(2) . . ?
O10 Ti7 O15 98.6(2) . . ?
O10 Ti7 O16 100.2(2) . . ?
O10 Ti7 O37 92.9(2) . . ?
O10 Ti7 O57 172.5(3) . . ?
O11 Ti7 O37 84.8(2) . . ?
O11 Ti7 O57 78.3(2) . . ?
O15 Ti7 O11 78.8(2) . . ?
O15 Ti7 O37 160.7(3) . . ?
O15 Ti7 O57 84.70(19) . . ?
O16 Ti7 O11 164.1(2) . . ?
O16 Ti7 O15 99.5(2) . . ?
O16 Ti7 O37 93.7(2) . . ?
O16 Ti7 O57 85.8(2) . . ?
O37 Ti7 O57 82.2(2) . . ?
O6 Ti8 O12 99.3(2) . . ?
O6 Ti8 O38 91.7(2) . . ?
O6 Ti8 O40 157.3(3) . . ?
O6 Ti8 N8 84.8(3) . . ?
O11 Ti8 O6 101.9(3) . . ?
O11 Ti8 O12 85.0(2) . . ?
O11 Ti8 O38 88.9(2) . . ?
O11 Ti8 O40 99.8(3) . . ?
O11 Ti8 N8 173.2(3) . . ?
O12 Ti8 O38 168.4(2) . . ?
O12 Ti8 O40 89.4(2) . . ?
O12 Ti8 N8 94.9(3) . . ?
O38 Ti8 N8 90.0(3) . . ?
O40 Ti8 O38 81.9(2) . . ?
O40 Ti8 N8 73.5(3) . . ?
O7 Ti9 O12 98.8(2) . . ?
O7 Ti9 O13 108.3(2) . . ?
O7 Ti9 O42 158.3(3) . . ?
O7 Ti9 O43 87.82(19) . . ?
O7 Ti9 N9 85.9(2) . . ?
O12 Ti9 O13 84.0(2) . . ?
O12 Ti9 O42 93.1(2) . . ?
O12 Ti9 O43 170.0(2) . . ?
O12 Ti9 N9 98.1(2) . . ?
O13 Ti9 O42 91.0(2) . . ?
O13 Ti9 O43 86.9(2) . . ?
O13 Ti9 N9 165.3(2) . . ?
O42 Ti9 O43 83.2(2) . . ?
O42 Ti9 N9 74.4(3) . . ?
O43 Ti9 N9 89.8(2) . . ?
O8 Ti10 O13 105.5(2) . . ?
O8 Ti10 O14 103.2(2) . . ?
O8 Ti10 O44 89.4(2) . . ?
O8 Ti10 O46 90.8(2) . . ?
O8 Ti10 N10 162.8(2) . . ?
O13 Ti10 O44 85.6(2) . . ?
O13 Ti10 O46 163.0(2) . . ?
O13 Ti10 N10 88.7(2) . . ?
O14 Ti10 O13 81.3(2) . . ?
O14 Ti10 O44 163.8(2) . . ?
O14 Ti10 O46 100.0(2) . . ?
O14 Ti10 N10 88.22(19) . . ?
O44 Ti10 N10 82.0(2) . . ?
O46 Ti10 O44 89.7(2) . . ?
O46 Ti10 N10 74.4(2) . . ?
O9 Ti11 O14 94.2(2) . . ?
O9 Ti11 O15 104.8(2) . . ?
O9 Ti11 O18 95.3(2) . . ?
O9 Ti11 O48 159.9(2) . . ?
O9 Ti11 N11 86.6(2) . . ?
O14 Ti11 O48 85.96(19) . . ?
O14 Ti11 N11 89.9(2) . . ?
O15 Ti11 O14 79.4(2) . . ?
O15 Ti11 O18 98.7(2) . . ?
O15 Ti11 O48 95.0(2) . . ?
O15 Ti11 N11 164.8(2) . . ?
O18 Ti11 O14 170.5(2) . . ?
O18 Ti11 O48 84.9(2) . . ?
O18 Ti11 N11 90.0(2) . . ?
O48 Ti11 N11 73.3(2) . . ?
O11 Ti12 O12 68.8(2) . . ?
O11 Ti12 O14 147.9(2) . . ?
O11 Ti12 O15 74.2(2) . . ?
O11 Ti12 O58 82.39(17) . . ?
O13 Ti12 O11 138.2(2) . . ?
O13 Ti12 O12 69.55(18) . . ?
O13 Ti12 O14 73.69(18) . . ?
O13 Ti12 O15 147.14(19) . . ?
O13 Ti12 O58 92.48(18) . . ?
O14 Ti12 O12 143.23(17) . . ?
O15 Ti12 O12 142.89(17) . . ?
O15 Ti12 O14 73.67(18) . . ?
O15 Ti12 O58 86.5(2) . . ?
O58 Ti12 O12 86.2(2) . . ?
O58 Ti12 O14 94.76(18) . . ?
O61 Ti12 O11 88.44(17) . . ?
O61 Ti12 O12 87.5(2) . . ?
O61 Ti12 O13 92.25(18) . . ?
O61 Ti12 O14 94.7(2) . . ?
O61 Ti12 O15 94.1(2) . . ?
O61 Ti12 O58 170.3(2) . . ?
O16 Ti13 O17 102.0(2) . . ?
O16 Ti13 O54 95.4(2) . . ?
O16 Ti13 O56 103.0(3) . . ?
O16 Ti13 N14 164.8(2) . . ?
O16 Ti13 N15 85.4(3) . . ?
O17 Ti13 O54 103.2(3) . . ?
O17 Ti13 O56 92.6(2) . . ?
O17 Ti13 N14 91.7(3) . . ?
O17 Ti13 N15 165.8(2) . . ?
O54 Ti13 O56 152.7(2) . . ?
O54 Ti13 N14 74.7(2) . . ?
O54 Ti13 N15 88.0(3) . . ?
O56 Ti13 N14 82.8(2) . . ?
O56 Ti13 N15 73.8(3) . . ?
N15 Ti13 N14 82.8(3) . . ?
O17 Ti14 O50 93.3(2) . . ?
O17 Ti14 O52 102.0(2) . . ?
O17 Ti14 N12 163.2(3) . . ?
O17 Ti14 N13 80.2(2) . . ?
O18 Ti14 O17 103.9(3) . . ?
O18 Ti14 O50 101.8(2) . . ?
O18 Ti14 O52 98.2(2) . . ?
O18 Ti14 N12 90.2(3) . . ?
O18 Ti14 N13 171.6(3) . . ?
O50 Ti14 N12 74.6(3) . . ?
O50 Ti14 N13 85.1(3) . . ?
O52 Ti14 O50 151.1(3) . . ?
O52 Ti14 N12 84.8(3) . . ?
O52 Ti14 N13 73.7(3) . . ?
N13 Ti14 N12 87.1(3) . . ?
O19 Ti15 O28 102.6(2) . . ?
O19 Ti15 O30 94.6(2) . . ?
O19 Ti15 N4 86.1(2) . . ?
O19 Ti15 N5 161.4(3) . . ?
O20 Ti15 O19 100.7(2) . . ?
O20 Ti15 O28 93.4(3) . . ?
O20 Ti15 O30 101.4(2) . . ?
O20 Ti15 N4 166.6(3) . . ?
O20 Ti15 N5 96.1(2) . . ?
O28 Ti15 N4 73.8(3) . . ?
O28 Ti15 N5 84.2(2) . . ?
O30 Ti15 O28 154.9(2) . . ?
O30 Ti15 N4 89.4(3) . . ?
O30 Ti15 N5 74.2(2) . . ?
N5 Ti15 N4 79.1(2) . . ?
Ti1 O1 Ti2 145.9(3) . . ?
Ti1 O1 Ti6 109.5(3) . . ?
Ti2 O1 Ti6 102.2(3) . . ?
Ti2 O2 Ti3 150.3(4) . . ?
Ti2 O2 Ti6 104.6(3) . . ?
Ti3 O2 Ti6 102.2(2) . . ?
Ti3 O3 Ti6 106.9(2) . . ?
Ti4 O3 Ti3 141.9(2) . . ?
Ti4 O3 Ti6 107.7(3) . . ?
Ti4 O4 Ti6 100.2(3) . . ?
Ti5 O4 Ti4 152.7(3) . . ?
Ti5 O4 Ti6 107.1(2) . . ?
Ti1 O5 Ti5 172.3(3) . . ?
Ti1 O5 Ti6 94.0(3) . . ?
Ti5 O5 Ti6 90.49(18) . . ?
Ti2 O6 Ti8 155.3(4) . . ?
Ti3 O7 Ti9 161.6(4) . . ?
Ti10 O8 Ti4 161.7(3) . . ?
Ti11 O9 Ti5 149.8(4) . . ?
Ti7 O10 Ti1 152.2(3) . . ?
Ti7 O11 Ti12 102.9(2) . . ?
Ti8 O11 Ti7 147.3(2) . . ?
Ti8 O11 Ti12 109.6(2) . . ?
Ti8 O12 Ti12 96.5(3) . . ?
Ti9 O12 Ti8 163.5(3) . . ?
Ti9 O12 Ti12 97.1(2) . . ?
Ti9 O13 Ti10 144.8(2) . . ?
Ti9 O13 Ti12 107.56(19) . . ?
Ti10 O13 Ti12 102.2(2) . . ?
Ti10 O14 Ti11 157.0(3) . . ?
Ti10 O14 Ti12 101.0(2) . . ?
Ti11 O14 Ti12 100.53(17) . . ?
Ti7 O15 Ti12 103.8(3) . . ?
Ti11 O15 Ti7 149.7(3) . . ?
Ti11 O15 Ti12 106.31(19) . . ?
Ti13 O16 Ti7 162.3(4) . . ?
Ti13 O17 Ti14 137.7(3) . . ?
Ti14 O18 Ti11 164.5(3) . . ?
Ti15 O19 Ti3 145.2(4) . . ?
Ti15 O20 Ti4 138.7(3) . . ?
C7 O21 Ti1 133.4(6) . . ?
C7 O22 Ti2 133.3(7) . . ?
C13 O23 Ti2 127.8(9) . . ?
C19 O26 Ti3 122.5(8) . . ?
C25 O28 Ti15 124.0(7) . . ?
C31 O30 Ti15 124.5(5) . . ?
C37 O32 Ti4 122.9(6) . . ?
C43 O34 Ti5 123.3(6) . . ?
C6 O36 Ti1 124.0(5) . . ?
C44 O37 Ti7 137.0(5) . . ?
C44 O38 Ti8 132.6(7) . . ?
C50 O40 Ti8 121.2(7) . . ?
C56 O42 Ti9 120.3(6) . . ?
C57 O43 Ti9 134.3(6) . . ?
C57 O44 Ti10 133.9(4) . . ?
C63 O46 Ti10 124.7(6) . . ?
C69 O48 Ti11 123.4(6) . . ?
C75 O50 Ti14 124.2(6) . . ?
C76 O52 Ti14 125.8(7) . . ?
C87 O54 Ti13 125.5(5) . . ?
C93 O56 Ti13 123.7(5) . . ?
C94 O57 Ti7 127.1(4) . . ?
C94 O58 Ti12 127.3(4) . . ?
C95 O59 Ti5 121.5(7) . . ?
C95 O60 Ti6 132.4(6) . . ?
Ti6 O61 Ti12 174.8(4) . . ?
C1 N1 Ti1 127.1(6) . . ?
C5 N1 Ti1 114.8(5) . . ?
C5 N1 C1 118.1(8) . . ?
C8 N2 Ti2 125.2(7) . . ?
C8 N2 C12 125.2(10) . . ?
C12 N2 Ti2 109.6(8) . . ?
C14 N3 Ti3 126.9(6) . . ?
C14 N3 C18 120.0(8) . . ?
C18 N3 Ti3 113.0(7) . . ?
C20 N4 Ti15 129.5(6) . . ?
C24 N4 Ti15 111.6(7) . . ?
C24 N4 C20 117.9(8) . . ?
C26 N5 Ti15 129.3(5) . . ?
C26 N5 C30 118.6(6) . . ?
C30 N5 Ti15 112.0(4) . . ?
C32 N6 Ti4 125.3(7) . . ?
C36 N6 Ti4 113.5(7) . . ?
C36 N6 C32 121.1(10) . . ?
C38 N7 Ti5 129.2(8) . . ?
C38 N7 C42 118.5(10) . . ?
C42 N7 Ti5 112.3(6) . . ?
C45 N8 Ti8 124.0(7) . . ?
C49 N8 Ti8 114.6(6) . . ?
C49 N8 C45 121.4(8) . . ?
C51 N9 Ti9 128.0(6) . . ?
C51 N9 C55 116.8(9) . . ?
C55 N9 Ti9 114.8(5) . . ?
C58 N10 Ti10 128.8(5) . . ?
C58 N10 C62 118.6(7) . . ?
C62 N10 Ti10 112.4(6) . . ?
C64 N11 Ti11 127.7(5) . . ?
C64 N11 C68 118.0(7) . . ?
C68 N11 Ti11 114.2(6) . . ?
C70 N12 Ti14 127.0(7) . . ?
C70 N12 C74 120.6(11) . . ?
C74 N12 Ti14 112.3(8) . . ?
C77 N13 Ti14 111.8(7) . . ?
C81 N13 Ti14 131.0(7) . . ?
C81 N13 C77 116.6(9) . . ?
C82 N14 Ti13 130.0(6) . . ?
C82 N14 C86 118.2(7) . . ?
C86 N14 Ti13 111.7(5) . . ?
C88 N15 Ti13 128.0(7) . . ?
C92 N15 Ti13 115.5(5) . . ?
C92 N15 C88 116.0(9) . . ?
C97 N16 H16A 99(7) . . ?
C97 N16 C98 105.6(8) . . ?
C98 N16 H16A 103(7) . . ?
N1 C1 H1 119.1 . . ?
C2 C1 N1 121.8(8) . . ?
C2 C1 H1 119.1 . . ?
C1 C2 H2 120.2 . . ?
C1 C2 C3 119.6(9) . . ?
C3 C2 H2 120.2 . . ?
C2 C3 H3 121.0 . . ?
C2 C3 C4 118.0(10) . . ?
C4 C3 H3 121.0 . . ?
C3 C4 H4 120.4 . . ?
C5 C4 C3 119.3(9) . . ?
C5 C4 H4 120.4 . . ?
N1 C5 C6 113.6(9) . . ?
C4 C5 N1 123.1(8) . . ?
C4 C5 C6 123.1(9) . . ?
O35 C6 O36 125.8(9) . . ?
O35 C6 C5 119.9(10) . . ?
O36 C6 C5 113.8(8) . . ?
O21 C7 O22 130.9(9) . . ?
O21 C7 H7 114.5 . . ?
O22 C7 H7 114.5 . . ?
N2 C8 H8 120.4 . . ?
N2 C8 C9 119.2(12) . . ?
C9 C8 H8 120.4 . . ?
C8 C9 H9 122.8 . . ?
C10 C9 C8 114.4(13) . . ?
C10 C9 H9 122.8 . . ?
C9 C10 H10 115.9 . . ?
C9 C10 C11 128.2(12) . . ?
C11 C10 H10 115.9 . . ?
C10 C11 H11 122.2 . . ?
C10 C11 C12 115.6(12) . . ?
C12 C11 H11 122.2 . . ?
N2 C12 C11 117.3(12) . . ?
N2 C12 C13 119.6(10) . . ?
C11 C12 C13 123.1(11) . . ?
O23 C13 C12 109.0(11) . . ?
O24 C13 O23 127.9(14) . . ?
O24 C13 C12 123.1(11) . . ?
N3 C14 H14 118.3 . . ?
N3 C14 C15 123.5(10) . . ?
C15 C14 H14 118.3 . . ?
C14 C15 H15 123.2 . . ?
C16 C15 C14 113.6(12) . . ?
C16 C15 H15 123.2 . . ?
C15 C16 H16 118.3 . . ?
C17 C16 C15 123.3(10) . . ?
C17 C16 H16 118.3 . . ?
C16 C17 H17 121.0 . . ?
C16 C17 C18 118.0(11) . . ?
C18 C17 H17 121.0 . . ?
N3 C18 C17 121.6(12) . . ?
N3 C18 C19 115.5(9) . . ?
C17 C18 C19 122.8(11) . . ?
O25 C19 O26 123.1(12) . . ?
O25 C19 C18 123.0(10) . . ?
O26 C19 C18 113.9(10) . . ?
N4 C20 H20 117.6 . . ?
N4 C20 C21 124.8(9) . . ?
C21 C20 H20 117.6 . . ?
C20 C21 H21 122.0 . . ?
C20 C21 C22 116.0(11) . . ?
C22 C21 H21 122.0 . . ?
C21 C22 H22 120.2 . . ?
C23 C22 C21 119.6(10) . . ?
C23 C22 H22 120.2 . . ?
C22 C23 H23 120.2 . . ?
C22 C23 C24 119.6(10) . . ?
C24 C23 H23 120.2 . . ?
N4 C24 C23 122.0(11) . . ?
N4 C24 C25 114.3(8) . . ?
C23 C24 C25 123.7(10) . . ?
O27 C25 O28 125.1(11) . . ?
O27 C25 C24 120.3(9) . . ?
O28 C25 C24 114.6(9) . . ?
N5 C26 H26 118.8 . . ?
N5 C26 C27 122.4(7) . . ?
C27 C26 H26 118.8 . . ?
C26 C27 H27 120.1 . . ?
C28 C27 C26 119.8(8) . . ?
C28 C27 H27 120.1 . . ?
C27 C28 H28 120.8 . . ?
C27 C28 C29 118.4(7) . . ?
C29 C28 H28 120.8 . . ?
C28 C29 H29 120.6 . . ?
C30 C29 C28 118.9(7) . . ?
C30 C29 H29 120.6 . . ?
N5 C30 C29 121.9(7) . . ?
N5 C30 C31 114.1(6) . . ?
C29 C30 C31 123.9(7) . . ?
O29 C31 O30 122.7(7) . . ?
O29 C31 C30 122.7(6) . . ?
O30 C31 C30 114.5(6) . . ?
N6 C32 H32 120.0 . . ?
N6 C32 C33 120.0(10) . . ?
C33 C32 H32 120.0 . . ?
C32 C33 H33 120.2 . . ?
C32 C33 C34 119.7(11) . . ?
C34 C33 H33 120.2 . . ?
C33 C34 H34 120.2 . . ?
C35 C34 C33 119.6(13) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 H35 121.0 . . ?
C34 C35 C36 118.1(11) . . ?
C36 C35 H35 121.0 . . ?
N6 C36 C35 121.4(10) . . ?
N6 C36 C37 114.7(11) . . ?
C35 C36 C37 123.8(10) . . ?
O31 C37 C36 117.6(12) . . ?
O32 C37 O31 127.3(11) . . ?
O32 C37 C36 115.1(10) . . ?
N7 C38 H38 119.8 . . ?
N7 C38 C39 120.3(11) . . ?
C39 C38 H38 119.8 . . ?
C38 C39 H39 119.4 . . ?
C40 C39 C38 121.2(10) . . ?
C40 C39 H39 119.4 . . ?
C39 C40 H40 121.0 . . ?
C39 C40 C41 117.9(13) . . ?
C41 C40 H40 121.0 . . ?
C40 C41 H41 119.0 . . ?
C42 C41 C40 122.0(13) . . ?
C42 C41 H41 119.0 . . ?
N7 C42 C41 119.9(10) . . ?
N7 C42 C43 113.2(11) . . ?
C41 C42 C43 126.6(13) . . ?
O33 C43 O34 126.3(10) . . ?
O33 C43 C42 118.5(14) . . ?
O34 C43 C42 115.2(12) . . ?
O37 C44 H44 116.2 . . ?
O38 C44 O37 127.7(8) . . ?
O38 C44 H44 116.2 . . ?
N8 C45 H45 121.3 . . ?
N8 C45 C46 117.5(9) . . ?
C46 C45 H45 121.3 . . ?
C45 C46 H46 119.6 . . ?
C47 C46 C45 120.7(9) . . ?
C47 C46 H46 119.6 . . ?
C46 C47 H47 118.5 . . ?
C46 C47 C48 123.0(10) . . ?
C48 C47 H47 118.5 . . ?
C47 C48 H48 121.7 . . ?
C47 C48 C49 116.6(9) . . ?
C49 C48 H48 121.7 . . ?
N8 C49 C48 120.7(9) . . ?
N8 C49 C50 112.6(10) . . ?
C48 C49 C50 126.6(11) . . ?
O39 C50 O40 123.0(11) . . ?
O39 C50 C49 119.7(13) . . ?
O40 C50 C49 117.2(12) . . ?
N9 C51 H51 119.4 . . ?
N9 C51 C52 121.3(9) . . ?
C52 C51 H51 119.4 . . ?
C51 C52 H52 119.9 . . ?
C53 C52 C51 120.2(9) . . ?
C53 C52 H52 119.9 . . ?
C52 C53 H53 120.7 . . ?
C54 C53 C52 118.6(11) . . ?
C54 C53 H53 120.7 . . ?
C53 C54 H54 120.1 . . ?
C53 C54 C55 119.8(10) . . ?
C55 C54 H54 120.1 . . ?
N9 C55 C54 123.1(8) . . ?
N9 C55 C56 109.6(10) . . ?
C54 C55 C56 127.3(9) . . ?
O41 C56 C55 116.9(11) . . ?
O42 C56 O41 123.5(10) . . ?
O42 C56 C55 119.3(9) . . ?
O43 C57 H57 115.6 . . ?
O44 C57 O43 128.8(7) . . ?
O44 C57 H57 115.6 . . ?
N10 C58 H58 118.5 . . ?
N10 C58 C59 122.9(8) . . ?
C59 C58 H58 118.5 . . ?
C58 C59 H59 121.1 . . ?
C60 C59 C58 117.7(10) . . ?
C60 C59 H59 121.1 . . ?
C59 C60 H60 120.0 . . ?
C59 C60 C61 120.1(8) . . ?
C61 C60 H60 120.0 . . ?
C60 C61 H61 121.0 . . ?
C62 C61 C60 118.0(9) . . ?
C62 C61 H61 121.0 . . ?
N10 C62 C61 122.7(9) . . ?
N10 C62 C63 115.7(7) . . ?
C61 C62 C63 121.6(9) . . ?
O45 C63 O46 124.6(10) . . ?
O45 C63 C62 122.7(7) . . ?
O46 C63 C62 112.7(8) . . ?
N11 C64 H64 118.7 . . ?
N11 C64 C65 122.5(10) . . ?
C65 C64 H64 118.7 . . ?
C64 C65 H65 120.2 . . ?
C66 C65 C64 119.5(12) . . ?
C66 C65 H65 120.2 . . ?
C65 C66 H66 118.9 . . ?
C65 C66 C67 122.2(11) . . ?
C67 C66 H66 118.9 . . ?
C66 C67 H67 121.9 . . ?
C66 C67 C68 116.3(9) . . ?
C68 C67 H67 121.9 . . ?
N11 C68 C67 121.1(10) . . ?
N11 C68 C69 114.3(7) . . ?
C67 C68 C69 124.5(8) . . ?
O47 C69 O48 125.2(9) . . ?
O47 C69 C68 120.7(8) . . ?
O48 C69 C68 114.0(7) . . ?
N12 C70 H70 118.9 . . ?
N12 C70 C71 122.2(11) . . ?
C71 C70 H70 118.9 . . ?
C70 C71 H71 121.6 . . ?
C72 C71 C70 116.7(13) . . ?
C72 C71 H71 121.6 . . ?
C71 C72 H72 120.6 . . ?
C73 C72 C71 118.8(13) . . ?
C73 C72 H72 120.6 . . ?
C72 C73 H73 119.4 . . ?
C72 C73 C74 121.3(12) . . ?
C74 C73 H73 119.4 . . ?
N12 C74 C73 120.3(11) . . ?
N12 C74 C75 115.7(11) . . ?
C73 C74 C75 123.9(11) . . ?
O49 C75 O50 124.9(12) . . ?
O49 C75 C74 122.0(12) . . ?
O50 C75 C74 113.0(9) . . ?
O51 C76 O52 125.6(11) . . ?
O51 C76 C77 119.4(11) . . ?
O52 C76 C77 115.0(10) . . ?
N13 C77 C76 112.4(10) . . ?
N13 C77 C78 123.1(9) . . ?
C78 C77 C76 124.5(10) . . ?
C77 C78 H78 121.6 . . ?
C79 C78 C77 116.7(10) . . ?
C79 C78 H78 121.6 . . ?
C78 C79 H79 119.4 . . ?
C78 C79 C80 121.2(10) . . ?
C80 C79 H79 119.4 . . ?
C79 C80 H80 119.8 . . ?
C79 C80 C81 120.4(10) . . ?
C81 C80 H80 119.8 . . ?
N13 C81 C80 122.0(9) . . ?
N13 C81 H81 119.0 . . ?
C80 C81 H81 119.0 . . ?
N14 C82 H82 118.8 . . ?
N14 C82 C83 122.3(9) . . ?
C83 C82 H82 118.8 . . ?
C82 C83 H83 120.7 . . ?
C84 C83 C82 118.7(8) . . ?
C84 C83 H83 120.7 . . ?
C83 C84 H84 119.7 . . ?
C83 C84 C85 120.6(9) . . ?
C85 C84 H84 119.7 . . ?
C84 C85 H85 122.1 . . ?
C86 C85 C84 115.8(9) . . ?
C86 C85 H85 122.1 . . ?
N14 C86 C85 124.0(8) . . ?
N14 C86 C87 114.8(8) . . ?
C85 C86 C87 121.0(9) . . ?
O53 C87 O54 124.9(8) . . ?
O53 C87 C86 122.0(9) . . ?
O54 C87 C86 113.1(9) . . ?
N15 C88 H88 118.0 . . ?
C89 C88 N15 123.9(10) . . ?
C89 C88 H88 118.0 . . ?
C88 C89 H89 120.4 . . ?
C88 C89 C90 119.2(9) . . ?
C90 C89 H89 120.4 . . ?
C89 C90 H90 121.4 . . ?
C91 C90 C89 117.3(10) . . ?
C91 C90 H90 121.4 . . ?
C90 C91 H91 119.8 . . ?
C92 C91 C90 120.4(10) . . ?
C92 C91 H91 119.8 . . ?
N15 C92 C93 111.0(9) . . ?
C91 C92 N15 123.2(8) . . ?
C91 C92 C93 125.8(10) . . ?
O55 C93 O56 123.6(9) . . ?
O55 C93 C92 120.5(11) . . ?
O56 C93 C92 115.9(9) . . ?
O57 C94 O58 128.2(7) . . ?
O57 C94 H94 115.9 . . ?
O58 C94 H94 115.9 . . ?
O59 C95 O60 129.3(9) . . ?
O59 C95 H95 115.3 . . ?
O60 C95 H95 115.3 . . ?
H96A C96 H96B 109.5 . . ?
H96A C96 H96C 109.5 . . ?
H96B C96 H96C 109.5 . . ?
C97 C96 H96A 109.5 . . ?
C97 C96 H96B 109.5 . . ?
C97 C96 H96C 109.5 . . ?
N16 C97 C96 107.2(10) . . ?
N16 C97 H97A 110.3 . . ?
N16 C97 H97B 110.3 . . ?
C96 C97 H97A 110.3 . . ?
C96 C97 H97B 110.3 . . ?
H97A C97 H97B 108.5 . . ?
N16 C98 H98A 109.0 . . ?
N16 C98 H98B 109.0 . . ?
H98A C98 H98B 107.8 . . ?
C99 C98 N16 112.8(10) . . ?
C99 C98 H98A 109.0 . . ?
C99 C98 H98B 109.0 . . ?
C98 C99 H99A 109.5 . . ?
C98 C99 H99B 109.5 . . ?
C98 C99 H99C 109.5 . . ?
H99A C99 H99B 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ti1 O21 C7 O22 1.3(18) . . . . ?
Ti1 O36 C6 O35 179.7(10) . . . . ?
Ti1 O36 C6 C5 8.2(13) . . . . ?
Ti1 N1 C1 C2 -179.5(7) . . . . ?
Ti1 N1 C5 C4 178.4(9) . . . . ?
Ti1 N1 C5 C6 3.8(11) . . . . ?
Ti2 O22 C7 O21 -5.1(18) . . . . ?
Ti2 O23 C13 O24 -174.6(10) . . . . ?
Ti2 O23 C13 C12 3.9(12) . . . . ?
Ti2 N2 C8 C9 174.0(7) . . . . ?
Ti2 N2 C12 C11 -177.0(8) . . . . ?
Ti2 N2 C12 C13 2.4(11) . . . . ?
Ti3 O26 C19 O25 170.5(9) . . . . ?
Ti3 O26 C19 C18 -5.9(11) . . . . ?
Ti3 N3 C14 C15 178.5(7) . . . . ?
Ti3 N3 C18 C17 -179.3(8) . . . . ?
Ti3 N3 C18 C19 4.8(10) . . . . ?
Ti4 O32 C37 O31 176.5(9) . . . . ?
Ti4 O32 C37 C36 -3.1(12) . . . . ?
Ti4 N6 C32 C33 179.9(7) . . . . ?
Ti4 N6 C36 C35 178.2(7) . . . . ?
Ti4 N6 C36 C37 -0.1(10) . . . . ?
Ti5 O34 C43 O33 -175.9(11) . . . . ?
Ti5 O34 C43 C42 4.9(13) . . . . ?
Ti5 O59 C95 O60 2.6(14) . . . . ?
Ti5 N7 C38 C39 -176.0(7) . . . . ?
Ti5 N7 C42 C41 177.3(8) . . . . ?
Ti5 N7 C42 C43 -8.4(11) . . . . ?
Ti6 O60 C95 O59 -0.6(15) . . . . ?
Ti7 O37 C44 O38 9.0(16) . . . . ?
Ti7 O57 C94 O58 8.7(14) . . . . ?
Ti8 O38 C44 O37 8.4(15) . . . . ?
Ti8 O40 C50 O39 172.2(7) . . . . ?
Ti8 O40 C50 C49 -10.4(10) . . . . ?
Ti8 N8 C45 C46 176.3(6) . . . . ?
Ti8 N8 C49 C48 -177.2(6) . . . . ?
Ti8 N8 C49 C50 2.1(9) . . . . ?
Ti9 O42 C56 O41 176.2(8) . . . . ?
Ti9 O42 C56 C55 -10.6(11) . . . . ?
Ti9 O43 C57 O44 -0.8(12) . . . . ?
Ti9 N9 C51 C52 172.6(5) . . . . ?
Ti9 N9 C55 C54 -169.5(6) . . . . ?
Ti9 N9 C55 C56 9.0(8) . . . . ?
Ti10 O44 C57 O43 -12.0(12) . . . . ?
Ti10 O46 C63 O45 173.7(8) . . . . ?
Ti10 O46 C63 C62 -4.0(11) . . . . ?
Ti10 N10 C58 C59 -173.8(6) . . . . ?
Ti10 N10 C62 C61 175.3(8) . . . . ?
Ti10 N10 C62 C63 -2.4(10) . . . . ?
Ti11 O48 C69 O47 166.5(7) . . . . ?
Ti11 O48 C69 C68 -9.6(11) . . . . ?
Ti11 N11 C64 C65 178.6(8) . . . . ?
Ti11 N11 C68 C67 -176.7(8) . . . . ?
Ti11 N11 C68 C69 1.1(10) . . . . ?
Ti12 O58 C94 O57 -11.2(14) . . . . ?
Ti13 O54 C87 O53 176.6(9) . . . . ?
Ti13 O54 C87 C86 -4.4(13) . . . . ?
Ti13 O56 C93 O55 178.3(7) . . . . ?
Ti13 O56 C93 C92 -0.2(10) . . . . ?
Ti13 N14 C82 C83 173.7(7) . . . . ?
Ti13 N14 C86 C85 -176.6(9) . . . . ?
Ti13 N14 C86 C87 -0.4(11) . . . . ?
Ti13 N15 C88 C89 172.5(6) . . . . ?
Ti13 N15 C92 C91 -172.9(7) . . . . ?
Ti13 N15 C92 C93 3.6(9) . . . . ?
Ti14 O50 C75 O49 175.9(8) . . . . ?
Ti14 O50 C75 C74 -6.1(12) . . . . ?
Ti14 O52 C76 O51 -170.2(4) . . . . ?
Ti14 O52 C76 C77 9.8(4) . . . . ?
Ti14 N12 C70 C71 -173.8(9) . . . . ?
Ti14 N12 C74 C73 175.5(9) . . . . ?
Ti14 N12 C74 C75 -0.8(12) . . . . ?
Ti14 N13 C77 C76 -7.5(3) . . . . ?
Ti14 N13 C77 C78 172.5(3) . . . . ?
Ti14 N13 C81 C80 -170.8(4) . . . . ?
Ti15 O28 C25 O27 178.2(8) . . . . ?
Ti15 O28 C25 C24 -1.7(11) . . . . ?
Ti15 O30 C31 O29 173.9(6) . . . . ?
Ti15 O30 C31 C30 -10.3(10) . . . . ?
Ti15 N4 C20 C21 166.0(7) . . . . ?
Ti15 N4 C24 C23 -168.8(8) . . . . ?
Ti15 N4 C24 C25 13.8(10) . . . . ?
Ti15 N5 C26 C27 -176.0(6) . . . . ?
Ti15 N5 C30 C29 179.3(6) . . . . ?
Ti15 N5 C30 C31 -3.5(8) . . . . ?
O1 Ti1 O5 Ti6 -2.50(19) . . . . ?
O1 Ti1 O10 Ti7 47.3(9) . . . . ?
O1 Ti2 O2 Ti3 162.5(5) . . . . ?
O1 Ti2 O2 Ti6 9.1(2) . . . . ?
O1 Ti2 O6 Ti8 -21.5(9) . . . . ?
O2 Ti2 O6 Ti8 60.5(9) . . . . ?
O2 Ti3 O7 Ti9 -65.1(8) . . . . ?
O2 Ti3 O19 Ti15 40.0(9) . . . . ?
O3 Ti3 O7 Ti9 11.1(8) . . . . ?
O3 Ti3 O19 Ti15 -2.4(5) . . . . ?
O3 Ti4 O8 Ti10 -26.3(11) . . . . ?
O3 Ti4 O20 Ti15 5.9(5) . . . . ?
O4 Ti4 O3 Ti3 -159.5(4) . . . . ?
O4 Ti4 O3 Ti6 -5.1(2) . . . . ?
O4 Ti4 O8 Ti10 50.8(11) . . . . ?
O4 Ti5 O5 Ti6 -3.36(18) . . . . ?
O4 Ti5 O9 Ti11 -66.0(6) . . . . ?
O5 Ti1 O1 Ti2 160.6(5) . . . . ?
O5 Ti1 O1 Ti6 3.2(3) . . . . ?
O5 Ti1 O10 Ti7 -43.0(9) . . . . ?
O5 Ti5 O4 Ti4 -178.5(6) . . . . ?
O5 Ti5 O4 Ti6 4.2(2) . . . . ?
O5 Ti5 O9 Ti11 27.3(6) . . . . ?
O6 Ti2 O2 Ti3 59.8(5) . . . . ?
O6 Ti2 O2 Ti6 -93.6(3) . . . . ?
O6 Ti8 O11 Ti7 92.3(5) . . . . ?
O6 Ti8 O11 Ti12 -95.6(2) . . . . ?
O6 Ti8 O12 Ti9 -46.8(14) . . . . ?
O6 Ti8 O12 Ti12 98.9(3) . . . . ?
O7 Ti3 O19 Ti15 -105.9(5) . . . . ?
O7 Ti9 O12 Ti8 47.7(14) . . . . ?
O7 Ti9 O12 Ti12 -97.9(2) . . . . ?
O7 Ti9 O13 Ti10 -60.9(4) . . . . ?
O7 Ti9 O13 Ti12 85.5(2) . . . . ?
O8 Ti4 O3 Ti3 -72.4(4) . . . . ?
O8 Ti4 O3 Ti6 82.0(2) . . . . ?
O8 Ti4 O20 Ti15 110.7(5) . . . . ?
O8 Ti10 O14 Ti11 -65.2(6) . . . . ?
O8 Ti10 O14 Ti12 93.6(2) . . . . ?
O9 Ti5 O4 Ti4 -79.5(6) . . . . ?
O9 Ti5 O4 Ti6 103.2(2) . . . . ?
O9 Ti5 O5 Ti6 -105.9(2) . . . . ?
O9 Ti11 O15 Ti7 -96.5(5) . . . . ?
O9 Ti11 O15 Ti12 89.3(2) . . . . ?
O9 Ti11 O18 Ti14 -145.7(13) . . . . ?
O10 Ti1 O1 Ti2 62.5(5) . . . . ?
O10 Ti1 O1 Ti6 -95.0(3) . . . . ?
O10 Ti1 O5 Ti6 105.0(2) . . . . ?
O10 Ti7 O16 Ti13 150.8(9) . . . . ?
O11 Ti7 O10 Ti1 -45.6(9) . . . . ?
O11 Ti7 O16 Ti13 -26.5(15) . . . . ?
O11 Ti8 O6 Ti2 20.6(8) . . . . ?
O11 Ti8 O12 Ti9 -148.0(14) . . . . ?
O11 Ti8 O12 Ti12 -2.32(19) . . . . ?
O12 Ti8 O6 Ti2 -66.2(9) . . . . ?
O12 Ti8 O11 Ti7 -169.2(5) . . . . ?
O12 Ti8 O11 Ti12 2.8(2) . . . . ?
O12 Ti9 O7 Ti3 73.6(8) . . . . ?
O12 Ti9 O13 Ti10 -158.1(4) . . . . ?
O12 Ti9 O13 Ti12 -11.8(2) . . . . ?
O13 Ti9 O7 Ti3 -12.9(9) . . . . ?
O13 Ti9 O12 Ti8 155.4(14) . . . . ?
O13 Ti9 O12 Ti12 9.71(18) . . . . ?
O13 Ti10 O8 Ti4 30.8(11) . . . . ?
O13 Ti10 O14 Ti11 -169.2(6) . . . . ?
O13 Ti10 O14 Ti12 -10.41(17) . . . . ?
O14 Ti10 O8 Ti4 -53.7(11) . . . . ?
O14 Ti11 O9 Ti5 68.4(6) . . . . ?
O14 Ti11 O15 Ti7 171.9(5) . . . . ?
O14 Ti11 O15 Ti12 -2.23(18) . . . . ?
O15 Ti7 O10 Ti1 33.8(9) . . . . ?
O15 Ti7 O16 Ti13 -108.7(9) . . . . ?
O15 Ti11 O9 Ti5 -11.7(6) . . . . ?
O15 Ti11 O18 Ti14 108.4(13) . . . . ?
O16 Ti7 O10 Ti1 135.1(8) . . . . ?
O16 Ti13 O17 Ti14 37.6(5) . . . . ?
O17 Ti13 O16 Ti7 114.4(9) . . . . ?
O17 Ti14 O18 Ti11 -78.4(13) . . . . ?
O18 Ti11 O9 Ti5 -112.2(6) . . . . ?
O18 Ti11 O15 Ti7 1.4(5) . . . . ?
O18 Ti11 O15 Ti12 -172.8(2) . . . . ?
O18 Ti14 O17 Ti13 -53.2(5) . . . . ?
O19 Ti3 O7 Ti9 104.2(8) . . . . ?
O19 Ti15 O20 Ti4 -20.5(5) . . . . ?
O20 Ti4 O3 Ti3 25.8(4) . . . . ?
O20 Ti4 O3 Ti6 -179.8(2) . . . . ?
O20 Ti4 O8 Ti10 -124.1(10) . . . . ?
O20 Ti15 O19 Ti3 18.9(5) . . . . ?
O21 Ti1 O1 Ti2 -24.3(5) . . . . ?
O21 Ti1 O1 Ti6 178.3(3) . . . . ?
O21 Ti1 O10 Ti7 132.8(9) . . . . ?
O22 Ti2 O2 Ti3 -160.5(6) . . . . ?
O22 Ti2 O2 Ti6 46.0(8) . . . . ?
O22 Ti2 O6 Ti8 -108.6(8) . . . . ?
O23 Ti2 O2 Ti3 -33.2(5) . . . . ?
O23 Ti2 O2 Ti6 173.3(3) . . . . ?
O23 Ti2 O6 Ti8 161.7(8) . . . . ?
O26 Ti3 O7 Ti9 -159.6(8) . . . . ?
O26 Ti3 O19 Ti15 159.2(5) . . . . ?
O28 Ti15 O19 Ti3 -77.1(5) . . . . ?
O28 Ti15 O20 Ti4 83.0(5) . . . . ?
O30 Ti15 O19 Ti3 121.4(5) . . . . ?
O30 Ti15 O20 Ti4 -117.4(4) . . . . ?
O32 Ti4 O3 Ti3 115.1(4) . . . . ?
O32 Ti4 O3 Ti6 -90.5(2) . . . . ?
O32 Ti4 O8 Ti10 128.3(10) . . . . ?
O32 Ti4 O20 Ti15 -86.3(5) . . . . ?
O34 Ti5 O4 Ti4 17.6(6) . . . . ?
O34 Ti5 O4 Ti6 -159.7(2) . . . . ?
O34 Ti5 O5 Ti6 111.2(8) . . . . ?
O34 Ti5 O9 Ti11 -163.3(6) . . . . ?
O36 Ti1 O1 Ti2 -108.1(5) . . . . ?
O36 Ti1 O1 Ti6 94.5(3) . . . . ?
O36 Ti1 O5 Ti6 -93.8(2) . . . . ?
O36 Ti1 O10 Ti7 -159.7(7) . . . . ?
O37 Ti7 O10 Ti1 -130.7(9) . . . . ?
O37 Ti7 O16 Ti13 57.2(9) . . . . ?
O38 Ti8 O6 Ti2 109.8(8) . . . . ?
O38 Ti8 O11 Ti7 0.8(5) . . . . ?
O38 Ti8 O11 Ti12 172.9(2) . . . . ?
O38 Ti8 O12 Ti9 153.2(13) . . . . ?
O38 Ti8 O12 Ti12 -61.1(16) . . . . ?
O40 Ti8 O6 Ti2 -177.4(6) . . . . ?
O40 Ti8 O11 Ti7 -80.7(5) . . . . ?
O40 Ti8 O11 Ti12 91.3(2) . . . . ?
O40 Ti8 O12 Ti9 112.1(14) . . . . ?
O40 Ti8 O12 Ti12 -102.2(3) . . . . ?
O42 Ti9 O7 Ti3 -164.2(7) . . . . ?
O42 Ti9 O12 Ti8 -114.0(13) . . . . ?
O42 Ti9 O12 Ti12 100.3(3) . . . . ?
O42 Ti9 O13 Ti10 108.9(4) . . . . ?
O42 Ti9 O13 Ti12 -104.8(2) . . . . ?
O43 Ti9 O7 Ti3 -98.9(8) . . . . ?
O43 Ti9 O13 Ti10 25.8(4) . . . . ?
O43 Ti9 O13 Ti12 172.1(2) . . . . ?
O44 Ti10 O8 Ti4 116.1(11) . . . . ?
O44 Ti10 O14 Ti11 154.3(6) . . . . ?
O44 Ti10 O14 Ti12 -46.9(7) . . . . ?
O46 Ti10 O8 Ti4 -154.2(11) . . . . ?
O46 Ti10 O14 Ti11 28.0(6) . . . . ?
O46 Ti10 O14 Ti12 -173.21(19) . . . . ?
O48 Ti11 O9 Ti5 158.1(5) . . . . ?
O48 Ti11 O15 Ti7 87.0(5) . . . . ?
O48 Ti11 O15 Ti12 -87.2(2) . . . . ?
O48 Ti11 O18 Ti14 14.1(13) . . . . ?
O50 Ti14 O17 Ti13 -156.2(5) . . . . ?
O50 Ti14 O18 Ti11 18.1(13) . . . . ?
O51 C76 C77 N13 179.96(13) . . . . ?
O51 C76 C77 C78 0.0(3) . . . . ?
O52 Ti14 O17 Ti13 48.5(5) . . . . ?
O52 Ti14 O18 Ti11 177.0(13) . . . . ?
O52 C76 C77 N13 0.0(2) . . . . ?
O52 C76 C77 C78 -179.93(16) . . . . ?
O54 Ti13 O16 Ti7 -140.8(9) . . . . ?
O54 Ti13 O17 Ti14 -61.0(5) . . . . ?
O56 Ti13 O16 Ti7 18.9(10) . . . . ?
O56 Ti13 O17 Ti14 141.4(5) . . . . ?
O57 Ti7 O16 Ti13 -24.8(9) . . . . ?
O59 Ti5 O4 Ti4 98.6(6) . . . . ?
O59 Ti5 O4 Ti6 -78.8(3) . . . . ?
O59 Ti5 O5 Ti6 82.9(2) . . . . ?
N1 Ti1 O1 Ti2 -74.0(11) . . . . ?
N1 Ti1 O1 Ti6 128.6(8) . . . . ?
N1 Ti1 O5 Ti6 -166.94(18) . . . . ?
N1 Ti1 O10 Ti7 -145.5(9) . . . . ?
N1 C1 C2 C3 -2.6(16) . . . . ?
N1 C5 C6 O35 -179.5(10) . . . . ?
N1 C5 C6 O36 -7.5(14) . . . . ?
N2 Ti2 O2 Ti3 -106.8(5) . . . . ?
N2 Ti2 O2 Ti6 99.7(3) . . . . ?
N2 Ti2 O6 Ti8 -167.2(7) . . . . ?
N2 C8 C9 C10 3.6(15) . . . . ?
N2 C12 C13 O23 -3.9(14) . . . . ?
N2 C12 C13 O24 174.8(11) . . . . ?
N3 Ti3 O7 Ti9 -148.7(10) . . . . ?
N3 Ti3 O19 Ti15 85.3(5) . . . . ?
N3 C14 C15 C16 0.3(14) . . . . ?
N3 C18 C19 O25 -176.4(10) . . . . ?
N3 C18 C19 O26 0.0(13) . . . . ?
N4 Ti15 O19 Ti3 -149.5(5) . . . . ?
N4 Ti15 O20 Ti4 99.4(10) . . . . ?
N4 C20 C21 C22 1.1(15) . . . . ?
N4 C24 C25 O27 170.9(9) . . . . ?
N4 C24 C25 O28 -9.2(12) . . . . ?
N5 Ti15 O19 Ti3 173.2(4) . . . . ?
N5 Ti15 O20 Ti4 167.5(4) . . . . ?
N5 C26 C27 C28 -2.3(14) . . . . ?
N5 C30 C31 O29 -175.9(7) . . . . ?
N5 C30 C31 O30 8.3(11) . . . . ?
N6 Ti4 O3 Ti3 154.0(6) . . . . ?
N6 Ti4 O3 Ti6 -51.6(7) . . . . ?
N6 Ti4 O8 Ti10 140.7(11) . . . . ?
N6 Ti4 O20 Ti15 -159.9(5) . . . . ?
N6 C32 C33 C34 3.6(15) . . . . ?
N6 C36 C37 O31 -177.7(10) . . . . ?
N6 C36 C37 O32 1.9(13) . . . . ?
N7 Ti5 O4 Ti4 68.3(12) . . . . ?
N7 Ti5 O4 Ti6 -109.1(10) . . . . ?
N7 Ti5 O5 Ti6 163.36(19) . . . . ?
N7 Ti5 O9 Ti11 121.7(6) . . . . ?
N7 C38 C39 C40 -2.2(16) . . . . ?
N7 C42 C43 O33 -176.0(11) . . . . ?
N7 C42 C43 O34 3.2(14) . . . . ?
N8 Ti8 O6 Ti2 -160.3(8) . . . . ?
N8 Ti8 O12 Ti9 38.8(14) . . . . ?
N8 Ti8 O12 Ti12 -175.5(3) . . . . ?
N8 C45 C46 C47 2.2(13) . . . . ?
N8 C49 C50 O39 -177.7(8) . . . . ?
N8 C49 C50 O40 4.8(11) . . . . ?
N9 Ti9 O7 Ti3 171.2(8) . . . . ?
N9 Ti9 O12 Ti8 -39.3(14) . . . . ?
N9 Ti9 O12 Ti12 175.03(19) . . . . ?
N9 Ti9 O13 Ti10 102.7(8) . . . . ?
N9 Ti9 O13 Ti12 -110.9(7) . . . . ?
N9 C51 C52 C53 -2.4(11) . . . . ?
N9 C55 C56 O41 173.8(9) . . . . ?
N9 C55 C56 O42 0.2(11) . . . . ?
N10 Ti10 O8 Ti4 175.8(8) . . . . ?
N10 Ti10 O14 Ti11 101.8(6) . . . . ?
N10 Ti10 O14 Ti12 -99.4(2) . . . . ?
N10 C58 C59 C60 -0.8(14) . . . . ?
N10 C62 C63 O45 -173.7(9) . . . . ?
N10 C62 C63 O46 4.1(12) . . . . ?
N11 Ti11 O9 Ti5 158.1(6) . . . . ?
N11 Ti11 O15 Ti7 126.0(8) . . . . ?
N11 Ti11 O15 Ti12 -48.2(9) . . . . ?
N11 Ti11 O18 Ti14 -59.1(13) . . . . ?
N11 C64 C65 C66 0.1(17) . . . . ?
N11 C68 C69 O47 -171.4(8) . . . . ?
N11 C68 C69 O48 4.9(12) . . . . ?
N12 Ti14 O17 Ti13 160.7(7) . . . . ?
N12 Ti14 O18 Ti11 92.3(13) . . . . ?
N12 C70 C71 C72 -2.6(19) . . . . ?
N12 C74 C75 O49 -177.8(10) . . . . ?
N12 C74 C75 O50 4.1(14) . . . . ?
N13 Ti14 O17 Ti13 119.4(5) . . . . ?
N13 C77 C78 C79 0.1(3) . . . . ?
N14 Ti13 O16 Ti7 -92.1(13) . . . . ?
N14 Ti13 O17 Ti14 -135.7(5) . . . . ?
N14 C82 C83 C84 5.9(16) . . . . ?
N14 C86 C87 O53 -178.2(10) . . . . ?
N14 C86 C87 O54 2.7(14) . . . . ?
N15 Ti13 O16 Ti7 -53.3(9) . . . . ?
N15 Ti13 O17 Ti14 157.7(8) . . . . ?
N15 C88 C89 C90 -1.2(13) . . . . ?
N15 C92 C93 O55 179.1(8) . . . . ?
N15 C92 C93 O56 -2.4(11) . . . . ?
C1 N1 C5 C4 -3.6(15) . . . . ?
C1 N1 C5 C6 -178.1(8) . . . . ?
C1 C2 C3 C4 3.1(16) . . . . ?
C2 C3 C4 C5 -3.9(17) . . . . ?
C3 C4 C5 N1 4.2(17) . . . . ?
C3 C4 C5 C6 178.3(10) . . . . ?
C4 C5 C6 O35 5.9(18) . . . . ?
C4 C5 C6 O36 177.9(11) . . . . ?
C5 N1 C1 C2 2.7(14) . . . . ?
C8 N2 C12 C11 0.7(15) . . . . ?
C8 N2 C12 C13 -179.9(10) . . . . ?
C8 C9 C10 C11 -1.2(19) . . . . ?
C9 C10 C11 C12 -1(2) . . . . ?
C10 C11 C12 N2 1.7(16) . . . . ?
C10 C11 C12 C13 -177.7(11) . . . . ?
C11 C12 C13 O23 175.5(9) . . . . ?
C11 C12 C13 O24 -5.9(19) . . . . ?
C12 N2 C8 C9 -3.4(15) . . . . ?
C14 N3 C18 C17 -0.9(14) . . . . ?
C14 N3 C18 C19 -176.8(9) . . . . ?
C14 C15 C16 C17 -0.4(16) . . . . ?
C15 C16 C17 C18 0.0(18) . . . . ?
C16 C17 C18 N3 0.7(16) . . . . ?
C16 C17 C18 C19 176.4(10) . . . . ?
C17 C18 C19 O25 7.7(17) . . . . ?
C17 C18 C19 O26 -175.9(9) . . . . ?
C18 N3 C14 C15 0.3(14) . . . . ?
C20 N4 C24 C23 0.8(13) . . . . ?
C20 N4 C24 C25 -176.6(8) . . . . ?
C20 C21 C22 C23 0.0(16) . . . . ?
C21 C22 C23 C24 -0.5(17) . . . . ?
C22 C23 C24 N4 0.1(16) . . . . ?
C22 C23 C24 C25 177.3(10) . . . . ?
C23 C24 C25 O27 -6.5(16) . . . . ?
C23 C24 C25 O28 173.5(9) . . . . ?
C24 N4 C20 C21 -1.5(13) . . . . ?
C26 N5 C30 C29 2.2(12) . . . . ?
C26 N5 C30 C31 179.4(7) . . . . ?
C26 C27 C28 C29 1.4(13) . . . . ?
C27 C28 C29 C30 1.1(13) . . . . ?
C28 C29 C30 N5 -3.0(12) . . . . ?
C28 C29 C30 C31 -180.0(8) . . . . ?
C29 C30 C31 O29 1.3(14) . . . . ?
C29 C30 C31 O30 -174.5(8) . . . . ?
C30 N5 C26 C27 0.5(12) . . . . ?
C32 N6 C36 C35 2.1(13) . . . . ?
C32 N6 C36 C37 -176.2(8) . . . . ?
C32 C33 C34 C35 -0.4(16) . . . . ?
C33 C34 C35 C36 -1.9(16) . . . . ?
C34 C35 C36 N6 1.1(15) . . . . ?
C34 C35 C36 C37 179.3(10) . . . . ?
C35 C36 C37 O31 4.0(16) . . . . ?
C35 C36 C37 O32 -176.4(9) . . . . ?
C36 N6 C32 C33 -4.5(13) . . . . ?
C38 N7 C42 C41 -2.4(14) . . . . ?
C38 N7 C42 C43 171.9(9) . . . . ?
C38 C39 C40 C41 -0.7(18) . . . . ?
C39 C40 C41 C42 2.0(18) . . . . ?
C40 C41 C42 N7 -0.4(17) . . . . ?
C40 C41 C42 C43 -173.9(11) . . . . ?
C41 C42 C43 O33 -2.2(19) . . . . ?
C41 C42 C43 O34 177.0(10) . . . . ?
C42 N7 C38 C39 3.7(14) . . . . ?
C45 N8 C49 C48 0.9(12) . . . . ?
C45 N8 C49 C50 -179.8(7) . . . . ?
C45 C46 C47 C48 -2.1(15) . . . . ?
C46 C47 C48 C49 1.3(15) . . . . ?
C47 C48 C49 N8 -0.6(13) . . . . ?
C47 C48 C49 C50 -179.9(9) . . . . ?
C48 C49 C50 O39 1.5(14) . . . . ?
C48 C49 C50 O40 -175.9(8) . . . . ?
C49 N8 C45 C46 -1.6(12) . . . . ?
C51 N9 C55 C54 4.2(10) . . . . ?
C51 N9 C55 C56 -177.3(6) . . . . ?
C51 C52 C53 C54 1.0(11) . . . . ?
C52 C53 C54 C55 2.9(11) . . . . ?
C53 C54 C55 N9 -5.7(12) . . . . ?
C53 C54 C55 C56 176.1(8) . . . . ?
C54 C55 C56 O41 -7.8(14) . . . . ?
C54 C55 C56 O42 178.6(8) . . . . ?
C55 N9 C51 C52 -0.1(10) . . . . ?
C58 N10 C62 C61 -0.8(13) . . . . ?
C58 N10 C62 C63 -178.5(8) . . . . ?
C58 C59 C60 C61 -0.9(15) . . . . ?
C59 C60 C61 C62 1.6(16) . . . . ?
C60 C61 C62 N10 -0.8(15) . . . . ?
C60 C61 C62 C63 176.8(10) . . . . ?
C61 C62 C63 O45 8.6(16) . . . . ?
C61 C62 C63 O46 -173.7(8) . . . . ?
C62 N10 C58 C59 1.6(13) . . . . ?
C64 N11 C68 C67 0.0(13) . . . . ?
C64 N11 C68 C69 177.8(9) . . . . ?
C64 C65 C66 C67 -5.5(18) . . . . ?
C65 C66 C67 C68 7.6(18) . . . . ?
C66 C67 C68 N11 -4.9(15) . . . . ?
C66 C67 C68 C69 177.6(11) . . . . ?
C67 C68 C69 O47 6.3(16) . . . . ?
C67 C68 C69 O48 -177.4(9) . . . . ?
C68 N11 C64 C65 2.5(14) . . . . ?
C70 N12 C74 C73 -0.9(17) . . . . ?
C70 N12 C74 C75 -177.2(10) . . . . ?
C70 C71 C72 C73 2.2(19) . . . . ?
C71 C72 C73 C74 -1(2) . . . . ?
C72 C73 C74 N12 0.5(19) . . . . ?
C72 C73 C74 C75 176.5(12) . . . . ?
C73 C74 C75 O49 6.0(19) . . . . ?
C73 C74 C75 O50 -172.1(11) . . . . ?
C74 N12 C70 C71 2.0(18) . . . . ?
C76 C77 C78 C79 -179.98(17) . . . . ?
C77 N13 C81 C80 0.1(2) . . . . ?
C77 C78 C79 C80 -0.1(3) . . . . ?
C78 C79 C80 C81 0.1(3) . . . . ?
C79 C80 C81 N13 -0.1(3) . . . . ?
C81 N13 C77 C76 179.97(13) . . . . ?
C81 N13 C77 C78 -0.1(2) . . . . ?
C82 N14 C86 C85 -0.2(16) . . . . ?
C82 N14 C86 C87 176.1(9) . . . . ?
C82 C83 C84 C85 -7.4(17) . . . . ?
C83 C84 C85 C86 5.3(17) . . . . ?
C84 C85 C86 N14 -1.4(16) . . . . ?
C84 C85 C86 C87 -177.4(10) . . . . ?
C85 C86 C87 O53 -1.9(17) . . . . ?
C85 C86 C87 O54 179.0(10) . . . . ?
C86 N14 C82 C83 -2.0(15) . . . . ?
C88 N15 C92 C91 -0.9(12) . . . . ?
C88 N15 C92 C93 175.6(7) . . . . ?
C88 C89 C90 C91 0.0(13) . . . . ?
C89 C90 C91 C92 0.7(13) . . . . ?
C90 C91 C92 N15 -0.3(14) . . . . ?
C90 C91 C92 C93 -176.3(8) . . . . ?
C91 C92 C93 O55 -4.5(14) . . . . ?
C91 C92 C93 O56 174.0(8) . . . . ?
C92 N15 C88 C89 1.6(12) . . . . ?
C97 N16 C98 C99 70.7(14) . . . . ?
C98 N16 C97 C96 173.2(9) . . . . ?

_smtbx_masks_special_details     
;
A solvent mask was calculated and 483 electrons were 
found in a volume of 2531Å³ in 1 void per unit cell. 
This is consistent with the presence of 
11[CH3CN] per Asymmetric Unit 
which account for 484 electrons 
per unit cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.180 0.000 -0.567 2530.9 483.4 '22 CH3CN'

_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.619
_oxdiff_exptl_absorpt_empirical_full_min 0.498
# start Validation Reply Form
_vrf_PLAT029_ti15pa15            
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.957 Why?
RESPONSE: This is a minor problem caused by imperfect data collection.
;
_vrf_PLAT341_ti15pa15            
;
PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0153 Ang.
RESPONSE: Bond precision on C-C bonds does not affect the
determination of the binding modes of the ligands.
;
# end Validation Reply Form
