# Electronic Supplementary Material (ESI) for RSC Advances.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_Ti3
_database_code_depnum_ccdc_archive 'CCDC 1549583'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C43 H52 Cl3 N O3 Ti2'
_chemical_formula_moiety         'C43 H52 Cl3 N O3 Ti2'
_chemical_formula_weight         833.05
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   16.6846(7)
_cell_length_b                   18.4587(6)
_cell_length_c                   14.6183(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 114.144(5)
_cell_angle_gamma                90.0000
_cell_volume                     4108.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8945
_cell_measurement_theta_min      1.81
_cell_measurement_theta_max      28.89
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1744.00
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.890
_exptl_absorpt_correction_T_max  0.922

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            43125
_diffrn_reflns_av_R_equivalents  0.0777
_diffrn_reflns_theta_max         27.498
_diffrn_reflns_theta_min         2.581
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             9423
_reflns_number_gt                6595
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0898
_refine_ls_R_factor_gt           0.0553
_refine_ls_wR_factor_ref         0.1477
_refine_ls_wR_factor_gt          0.1304
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         9423
_refine_ls_number_parameters     469
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0622P)²+5.1378P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.69
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 -0.11264(4) 0.23007(3) 0.05337(4) 0.01874(14) Uani 1 1 d . . . . .
Ti2 Ti 0.37407(4) 0.34402(3) 0.46534(4) 0.01713(14) Uani 1 1 d . . . . .
Cl1 Cl -0.09709(6) 0.18626(5) 0.20484(6) 0.0306(2) Uani 1 1 d . . . . .
Cl2 Cl -0.21522(6) 0.31738(5) 0.02666(8) 0.0401(3) Uani 1 1 d . . . . .
Cl3 Cl 0.46139(5) 0.40871(5) 0.40655(7) 0.0260(2) Uani 1 1 d . . . . .
O1 O -0.01259(14) 0.27779(12) 0.08654(16) 0.0183(5) Uani 1 1 d . . . . .
O2 O 0.38229(14) 0.25485(11) 0.41971(17) 0.0202(5) Uani 1 1 d . . . . .
O3 O 0.26650(14) 0.37709(12) 0.38763(16) 0.0189(5) Uani 1 1 d . . . . .
N1 N 0.19448(16) 0.23359(14) 0.33259(19) 0.0159(5) Uani 1 1 d . . . . .
C1 C 0.1521(2) 0.21622(17) 0.2250(2) 0.0190(7) Uani 1 1 d . . . . .
H1A H 0.0927 0.1965 0.2092 0.023 Uiso 1 1 calc R U . . .
H1B H 0.1866 0.1783 0.2095 0.023 Uiso 1 1 calc R U . . .
C2 C 0.1444(2) 0.28167(17) 0.1597(2) 0.0180(6) Uani 1 1 d . . . . .
C3 C 0.0635(2) 0.30902(17) 0.0928(2) 0.0166(6) Uani 1 1 d . . . . .
C4 C 0.0573(2) 0.37177(17) 0.0367(2) 0.0187(7) Uani 1 1 d . . . . .
C5 C 0.1345(2) 0.40685(18) 0.0494(2) 0.0219(7) Uani 1 1 d . . . . .
H5 H 0.1313 0.4495 0.0118 0.026 Uiso 1 1 calc R U . . .
C6 C 0.2167(2) 0.38191(19) 0.1153(2) 0.0220(7) Uani 1 1 d . . . . .
C7 C 0.2196(2) 0.31894(18) 0.1687(2) 0.0200(7) Uani 1 1 d . . . . .
H7 H 0.2752 0.3007 0.2130 0.024 Uiso 1 1 calc R U . . .
C8 C 0.2992(2) 0.4224(2) 0.1280(3) 0.0305(8) Uani 1 1 d . . . . .
H8A H 0.2836 0.4651 0.0843 0.037 Uiso 1 1 calc R U . . .
H8B H 0.3299 0.4377 0.1979 0.037 Uiso 1 1 calc R U . . .
H8C H 0.3375 0.3906 0.1099 0.037 Uiso 1 1 calc R U . . .
C9 C -0.0312(2) 0.40098(19) -0.0318(3) 0.0259(8) Uani 1 1 d . . . . .
H9A H -0.0773 0.3686 -0.0306 0.031 Uiso 1 1 calc R U . . .
H9B H -0.0392 0.4493 -0.0092 0.031 Uiso 1 1 calc R U . . .
H9C H -0.0349 0.4040 -0.1003 0.031 Uiso 1 1 calc R U . . .
C10 C -0.1428(2) 0.10913(18) -0.0008(2) 0.0213(7) Uani 1 1 d . . . . .
H10 H -0.1410 0.0670 0.0430 0.026 Uiso 1 1 calc R U . . .
C11 C -0.0715(2) 0.13391(18) -0.0204(2) 0.0194(7) Uani 1 1 d . . . . .
C12 C -0.1041(2) 0.19026(19) -0.0920(2) 0.0226(7) Uani 1 1 d . . . . .
H12 H -0.0705 0.2147 -0.1263 0.027 Uiso 1 1 calc R U . . .
C13 C -0.1954(2) 0.19839(19) -0.1183(3) 0.0246(7) Uani 1 1 d . . . . .
C14 C -0.2192(2) 0.14900(19) -0.0596(2) 0.0228(7) Uani 1 1 d . . . . .
C15 C -0.3094(2) 0.1399(2) -0.0611(3) 0.0291(8) Uani 1 1 d . . . . .
H15A H -0.3078 0.1021 -0.0133 0.035 Uiso 1 1 calc R U . . .
H15B H -0.3282 0.1858 -0.0423 0.035 Uiso 1 1 calc R U . . .
H15C H -0.3509 0.1261 -0.1286 0.035 Uiso 1 1 calc R U . . .
C16 C -0.2558(2) 0.2487(2) -0.1962(3) 0.0354(9) Uani 1 1 d . . . . .
H16A H -0.2222 0.2769 -0.2253 0.043 Uiso 1 1 calc R U . . .
H16B H -0.3011 0.2206 -0.2490 0.043 Uiso 1 1 calc R U . . .
H16C H -0.2836 0.2817 -0.1653 0.043 Uiso 1 1 calc R U . . .
C17 C 0.0206(2) 0.10509(18) 0.0238(2) 0.0227(7) Uani 1 1 d . . . . .
H17A H 0.0566 0.1324 -0.0029 0.027 Uiso 1 1 calc R U . . .
H17B H 0.0452 0.1103 0.0969 0.027 Uiso 1 1 calc R U . . .
H17C H 0.0202 0.0538 0.0065 0.027 Uiso 1 1 calc R U . . .
C18 C 0.2321(2) 0.16934(16) 0.3932(2) 0.0179(6) Uani 1 1 d . . . . .
H18A H 0.1865 0.1311 0.3745 0.021 Uiso 1 1 calc R U . . .
H18B H 0.2485 0.1815 0.4646 0.021 Uiso 1 1 calc R U . . .
C19 C 0.3113(2) 0.13973(17) 0.3820(2) 0.0186(7) Uani 1 1 d . . . . .
C20 C 0.3843(2) 0.18359(17) 0.3980(2) 0.0190(7) Uani 1 1 d . . . . .
C21 C 0.4599(2) 0.15557(19) 0.3924(3) 0.0240(7) Uani 1 1 d . . . . .
C22 C 0.4618(2) 0.0816(2) 0.3724(3) 0.0289(8) Uani 1 1 d . . . . .
H22 H 0.5131 0.0619 0.3688 0.035 Uiso 1 1 calc R U . . .
C23 C 0.3917(2) 0.03623(19) 0.3576(3) 0.0280(8) Uani 1 1 d . . . . .
C24 C 0.3170(2) 0.06654(18) 0.3622(2) 0.0229(7) Uani 1 1 d . . . . .
H24 H 0.2680 0.0361 0.3515 0.027 Uiso 1 1 calc R U . . .
C25 C 0.3960(3) -0.0439(2) 0.3384(3) 0.0415(10) Uani 1 1 d . . . . .
H25A H 0.3404 -0.0669 0.3298 0.050 Uiso 1 1 calc R U . . .
H25B H 0.4061 -0.0507 0.2775 0.050 Uiso 1 1 calc R U . . .
H25C H 0.4443 -0.0659 0.3955 0.050 Uiso 1 1 calc R U . . .
C26 C 0.5379(2) 0.2033(2) 0.4101(3) 0.0348(9) Uani 1 1 d . . . . .
H26A H 0.5845 0.1746 0.4032 0.042 Uiso 1 1 calc R U . . .
H26B H 0.5205 0.2427 0.3608 0.042 Uiso 1 1 calc R U . . .
H26C H 0.5594 0.2237 0.4778 0.042 Uiso 1 1 calc R U . . .
C27 C 0.1358(2) 0.27123(17) 0.3685(2) 0.0183(7) Uani 1 1 d . . . . .
H27A H 0.1634 0.2719 0.4427 0.022 Uiso 1 1 calc R U . . .
H27B H 0.0804 0.2434 0.3476 0.022 Uiso 1 1 calc R U . . .
C28 C 0.1140(2) 0.34778(17) 0.3314(2) 0.0165(6) Uani 1 1 d . . . . .
C29 C 0.1806(2) 0.39804(17) 0.3442(2) 0.0171(6) Uani 1 1 d . . . . .
C30 C 0.1613(2) 0.46905(17) 0.3109(2) 0.0194(7) Uani 1 1 d . . . . .
C31 C 0.0737(2) 0.49055(18) 0.2694(2) 0.0212(7) Uani 1 1 d . . . . .
H31 H 0.0599 0.5394 0.2484 0.025 Uiso 1 1 calc R U . . .
C32 C 0.0059(2) 0.44287(18) 0.2578(2) 0.0200(7) Uani 1 1 d . . . . .
C33 C 0.0276(2) 0.37157(18) 0.2869(2) 0.0185(7) Uani 1 1 d . . . . .
H33 H -0.0183 0.3377 0.2760 0.022 Uiso 1 1 calc R U . . .
C34 C -0.0885(2) 0.4680(2) 0.2155(3) 0.0281(8) Uani 1 1 d . . . . .
H34A H -0.0910 0.5197 0.1993 0.034 Uiso 1 1 calc R U . . .
H34B H -0.1226 0.4405 0.1546 0.034 Uiso 1 1 calc R U . . .
H34C H -0.1131 0.4601 0.2652 0.034 Uiso 1 1 calc R U . . .
C35 C 0.2346(2) 0.51986(18) 0.3191(3) 0.0275(8) Uani 1 1 d . . . . .
H35A H 0.2101 0.5675 0.2925 0.033 Uiso 1 1 calc R U . . .
H35B H 0.2755 0.5247 0.3896 0.033 Uiso 1 1 calc R U . . .
H35C H 0.2660 0.5004 0.2806 0.033 Uiso 1 1 calc R U . . .
C36 C 0.3576(2) 0.31157(19) 0.6098(2) 0.0255(8) Uani 1 1 d . . . . .
H36 H 0.3139 0.2757 0.6130 0.031 Uiso 1 1 calc R U . . .
C37 C 0.3450(2) 0.38742(19) 0.6017(2) 0.0232(7) Uani 1 1 d . . . . .
C38 C 0.4247(2) 0.41784(18) 0.6099(2) 0.0227(7) Uani 1 1 d . . . . .
H38 H 0.4371 0.4709 0.6111 0.027 Uiso 1 1 calc R U . . .
C39 C 0.4879(2) 0.36202(19) 0.6292(2) 0.0252(8) Uani 1 1 d . . . . .
C40 C 0.4465(2) 0.29579(19) 0.6296(2) 0.0267(8) Uani 1 1 d . . . . .
C41 C 0.4875(3) 0.22155(19) 0.6487(3) 0.0376(10) Uani 1 1 d . . . . .
H41A H 0.4431 0.1854 0.6443 0.045 Uiso 1 1 calc R U . . .
H41B H 0.5107 0.2109 0.5985 0.045 Uiso 1 1 calc R U . . .
H41C H 0.5354 0.2201 0.7158 0.045 Uiso 1 1 calc R U . . .
C42 C 0.5821(2) 0.3740(2) 0.6485(3) 0.0340(9) Uani 1 1 d . . . . .
H42A H 0.5924 0.4258 0.6433 0.041 Uiso 1 1 calc R U . . .
H42B H 0.6197 0.3569 0.7160 0.041 Uiso 1 1 calc R U . . .
H42C H 0.5960 0.3472 0.5990 0.041 Uiso 1 1 calc R U . . .
C43 C 0.2626(2) 0.4278(2) 0.5865(3) 0.0314(8) Uani 1 1 d . . . . .
H43A H 0.2169 0.3933 0.5834 0.038 Uiso 1 1 calc R U . . .
H43B H 0.2743 0.4613 0.6425 0.038 Uiso 1 1 calc R U . . .
H43C H 0.2428 0.4552 0.5237 0.038 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.771(2) . ?
Ti1 Cl2 2.2655(11) . ?
Ti1 Cl1 2.2703(10) . ?
Ti1 C12 2.307(3) . ?
Ti1 C11 2.322(3) . ?
Ti1 C10 2.353(3) . ?
Ti1 C13 2.390(3) . ?
Ti1 C14 2.393(3) . ?
Ti2 O3 1.793(2) . ?
Ti2 O2 1.802(2) . ?
Ti2 Cl3 2.3044(10) . ?
Ti2 C36 2.317(3) . ?
Ti2 C38 2.361(3) . ?
Ti2 C37 2.375(3) . ?
Ti2 C40 2.376(3) . ?
Ti2 C39 2.395(3) . ?
O1 C3 1.363(4) . ?
O2 C20 1.357(4) . ?
O3 C29 1.365(4) . ?
N1 C18 1.460(4) . ?
N1 C27 1.463(4) . ?
N1 C1 1.472(4) . ?
C1 C2 1.512(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.390(4) . ?
C2 C3 1.398(4) . ?
C3 C4 1.399(4) . ?
C4 C5 1.384(5) . ?
C4 C9 1.506(4) . ?
C5 C6 1.393(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(5) . ?
C6 C8 1.509(5) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.409(5) . ?
C10 C14 1.418(5) . ?
C10 H10 1.0000 . ?
C11 C12 1.417(5) . ?
C11 C17 1.500(4) . ?
C12 C13 1.418(5) . ?
C12 H12 1.0000 . ?
C13 C14 1.415(5) . ?
C13 C16 1.495(5) . ?
C14 C15 1.506(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.501(4) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C19 C24 1.393(5) . ?
C19 C20 1.399(4) . ?
C20 C21 1.398(5) . ?
C21 C22 1.400(5) . ?
C21 C26 1.503(5) . ?
C22 C23 1.381(5) . ?
C22 H22 0.9500 . ?
C23 C24 1.393(5) . ?
C23 C25 1.512(5) . ?
C24 H24 0.9500 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 C28 1.504(4) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C33 1.388(4) . ?
C28 C29 1.400(4) . ?
C29 C30 1.390(4) . ?
C30 C31 1.391(4) . ?
C30 C35 1.507(5) . ?
C31 C32 1.388(5) . ?
C31 H31 0.9500 . ?
C32 C33 1.385(5) . ?
C32 C34 1.510(4) . ?
C33 H33 0.9500 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 C37 1.413(5) . ?
C36 C40 1.420(5) . ?
C36 H36 1.0000 . ?
C37 C38 1.403(5) . ?
C37 C43 1.498(5) . ?
C38 C39 1.418(5) . ?
C38 H38 1.0000 . ?
C39 C40 1.406(5) . ?
C39 C42 1.494(5) . ?
C40 C41 1.506(5) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 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 Cl2 104.74(8) . . ?
O1 Ti1 Cl1 101.02(8) . . ?
Cl2 Ti1 Cl1 101.44(5) . . ?
O1 Ti1 C12 90.25(11) . . ?
Cl2 Ti1 C12 113.25(9) . . ?
Cl1 Ti1 C12 139.40(9) . . ?
O1 Ti1 C11 94.75(11) . . ?
Cl2 Ti1 C11 144.08(9) . . ?
Cl1 Ti1 C11 104.07(9) . . ?
C12 Ti1 C11 35.65(11) . . ?
O1 Ti1 C10 127.72(11) . . ?
Cl2 Ti1 C10 125.07(9) . . ?
Cl1 Ti1 C10 85.04(9) . . ?
C12 Ti1 C10 58.21(12) . . ?
C11 Ti1 C10 35.07(11) . . ?
O1 Ti1 C13 118.97(11) . . ?
Cl2 Ti1 C13 85.52(9) . . ?
Cl1 Ti1 C13 136.33(9) . . ?
C12 Ti1 C13 35.09(11) . . ?
C11 Ti1 C13 58.59(11) . . ?
C10 Ti1 C13 57.49(12) . . ?
O1 Ti1 C14 148.33(11) . . ?
Cl2 Ti1 C14 91.74(9) . . ?
Cl1 Ti1 C14 101.93(9) . . ?
C12 Ti1 C14 58.22(12) . . ?
C11 Ti1 C14 58.57(11) . . ?
C10 Ti1 C14 34.75(11) . . ?
C13 Ti1 C14 34.42(12) . . ?
O3 Ti2 O2 106.52(10) . . ?
O3 Ti2 Cl3 102.06(8) . . ?
O2 Ti2 Cl3 100.36(8) . . ?
O3 Ti2 C36 101.78(12) . . ?
O2 Ti2 C36 99.01(12) . . ?
Cl3 Ti2 C36 143.38(9) . . ?
O3 Ti2 C38 105.64(11) . . ?
O2 Ti2 C38 143.58(11) . . ?
Cl3 Ti2 C38 89.16(9) . . ?
C36 Ti2 C38 57.72(12) . . ?
O3 Ti2 C37 85.51(11) . . ?
O2 Ti2 C37 133.73(11) . . ?
Cl3 Ti2 C37 121.03(9) . . ?
C36 Ti2 C37 35.04(12) . . ?
C38 Ti2 C37 34.46(11) . . ?
O3 Ti2 C40 136.97(12) . . ?
O2 Ti2 C40 87.00(11) . . ?
Cl3 Ti2 C40 115.69(9) . . ?
C36 Ti2 C40 35.19(12) . . ?
C38 Ti2 C40 57.57(12) . . ?
C37 Ti2 C40 58.13(12) . . ?
O3 Ti2 C39 139.93(12) . . ?
O2 Ti2 C39 110.34(11) . . ?
Cl3 Ti2 C39 86.41(9) . . ?
C36 Ti2 C39 57.69(12) . . ?
C38 Ti2 C39 34.68(12) . . ?
C37 Ti2 C39 57.62(12) . . ?
C40 Ti2 C39 34.28(11) . . ?
C3 O1 Ti1 167.6(2) . . ?
C20 O2 Ti2 170.0(2) . . ?
C29 O3 Ti2 168.4(2) . . ?
C18 N1 C27 110.6(2) . . ?
C18 N1 C1 111.8(2) . . ?
C27 N1 C1 112.8(2) . . ?
N1 C1 C2 112.3(2) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
C7 C2 C3 117.6(3) . . ?
C7 C2 C1 119.8(3) . . ?
C3 C2 C1 122.5(3) . . ?
O1 C3 C2 120.1(3) . . ?
O1 C3 C4 117.9(3) . . ?
C2 C3 C4 121.9(3) . . ?
C5 C4 C3 117.9(3) . . ?
C5 C4 C9 121.9(3) . . ?
C3 C4 C9 120.2(3) . . ?
C4 C5 C6 122.5(3) . . ?
C4 C5 H5 118.8 . . ?
C6 C5 H5 118.8 . . ?
C7 C6 C5 117.6(3) . . ?
C7 C6 C8 121.6(3) . . ?
C5 C6 C8 120.8(3) . . ?
C6 C7 C2 122.6(3) . . ?
C6 C7 H7 118.7 . . ?
C2 C7 H7 118.7 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C14 109.4(3) . . ?
C11 C10 Ti1 71.24(19) . . ?
C14 C10 Ti1 74.16(19) . . ?
C11 C10 H10 125.2 . . ?
C14 C10 H10 125.2 . . ?
Ti1 C10 H10 125.2 . . ?
C10 C11 C12 106.7(3) . . ?
C10 C11 C17 126.8(3) . . ?
C12 C11 C17 126.5(3) . . ?
C10 C11 Ti1 73.69(19) . . ?
C12 C11 Ti1 71.60(19) . . ?
C17 C11 Ti1 121.1(2) . . ?
C11 C12 C13 108.9(3) . . ?
C11 C12 Ti1 72.75(19) . . ?
C13 C12 Ti1 75.7(2) . . ?
C11 C12 H12 125.2 . . ?
C13 C12 H12 125.2 . . ?
Ti1 C12 H12 125.2 . . ?
C14 C13 C12 107.7(3) . . ?
C14 C13 C16 126.4(3) . . ?
C12 C13 C16 125.9(3) . . ?
C14 C13 Ti1 72.91(19) . . ?
C12 C13 Ti1 69.25(18) . . ?
C16 C13 Ti1 124.6(3) . . ?
C13 C14 C10 107.3(3) . . ?
C13 C14 C15 126.1(3) . . ?
C10 C14 C15 126.6(3) . . ?
C13 C14 Ti1 72.67(19) . . ?
C10 C14 Ti1 71.09(18) . . ?
C15 C14 Ti1 122.4(2) . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C11 C17 H17A 109.5 . . ?
C11 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C11 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N1 C18 C19 114.1(3) . . ?
N1 C18 H18A 108.7 . . ?
C19 C18 H18A 108.7 . . ?
N1 C18 H18B 108.7 . . ?
C19 C18 H18B 108.7 . . ?
H18A C18 H18B 107.6 . . ?
C24 C19 C20 117.9(3) . . ?
C24 C19 C18 120.9(3) . . ?
C20 C19 C18 121.1(3) . . ?
O2 C20 C21 118.8(3) . . ?
O2 C20 C19 119.9(3) . . ?
C21 C20 C19 121.4(3) . . ?
C20 C21 C22 118.1(3) . . ?
C20 C21 C26 120.8(3) . . ?
C22 C21 C26 121.1(3) . . ?
C23 C22 C21 122.3(3) . . ?
C23 C22 H22 118.9 . . ?
C21 C22 H22 118.9 . . ?
C22 C23 C24 117.8(3) . . ?
C22 C23 C25 121.4(3) . . ?
C24 C23 C25 120.8(3) . . ?
C19 C24 C23 122.5(3) . . ?
C19 C24 H24 118.8 . . ?
C23 C24 H24 118.8 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C21 C26 H26A 109.5 . . ?
C21 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C21 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
N1 C27 C28 114.5(3) . . ?
N1 C27 H27A 108.6 . . ?
C28 C27 H27A 108.6 . . ?
N1 C27 H27B 108.6 . . ?
C28 C27 H27B 108.6 . . ?
H27A C27 H27B 107.6 . . ?
C33 C28 C29 117.9(3) . . ?
C33 C28 C27 121.2(3) . . ?
C29 C28 C27 120.9(3) . . ?
O3 C29 C30 118.6(3) . . ?
O3 C29 C28 120.0(3) . . ?
C30 C29 C28 121.4(3) . . ?
C29 C30 C31 118.2(3) . . ?
C29 C30 C35 119.7(3) . . ?
C31 C30 C35 122.1(3) . . ?
C32 C31 C30 122.1(3) . . ?
C32 C31 H31 119.0 . . ?
C30 C31 H31 119.0 . . ?
C33 C32 C31 117.8(3) . . ?
C33 C32 C34 121.1(3) . . ?
C31 C32 C34 121.1(3) . . ?
C32 C33 C28 122.4(3) . . ?
C32 C33 H33 118.8 . . ?
C28 C33 H33 118.8 . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C30 C35 H35A 109.5 . . ?
C30 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C30 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C37 C36 C40 109.1(3) . . ?
C37 C36 Ti2 74.71(19) . . ?
C40 C36 Ti2 74.7(2) . . ?
C37 C36 H36 125.1 . . ?
C40 C36 H36 125.1 . . ?
Ti2 C36 H36 125.1 . . ?
C38 C37 C36 106.6(3) . . ?
C38 C37 C43 126.4(3) . . ?
C36 C37 C43 126.9(3) . . ?
C38 C37 Ti2 72.2(2) . . ?
C36 C37 Ti2 70.3(2) . . ?
C43 C37 Ti2 122.2(2) . . ?
C37 C38 C39 109.2(3) . . ?
C37 C38 Ti2 73.30(19) . . ?
C39 C38 Ti2 73.96(19) . . ?
C37 C38 H38 125.2 . . ?
C39 C38 H38 125.2 . . ?
Ti2 C38 H38 125.2 . . ?
C40 C39 C38 107.8(3) . . ?
C40 C39 C42 127.5(3) . . ?
C38 C39 C42 124.7(3) . . ?
C40 C39 Ti2 72.13(19) . . ?
C38 C39 Ti2 71.36(18) . . ?
C42 C39 Ti2 123.5(3) . . ?
C39 C40 C36 107.2(3) . . ?
C39 C40 C41 127.2(3) . . ?
C36 C40 C41 125.6(3) . . ?
C39 C40 Ti2 73.59(19) . . ?
C36 C40 Ti2 70.14(18) . . ?
C41 C40 Ti2 122.2(3) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C37 C43 H43A 109.5 . . ?
C37 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C37 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 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
Cl2 Ti1 O1 C3 -112.6(10) . . . . ?
Cl1 Ti1 O1 C3 142.4(9) . . . . ?
C12 Ti1 O1 C3 1.6(10) . . . . ?
C11 Ti1 O1 C3 37.0(10) . . . . ?
C10 Ti1 O1 C3 50.1(10) . . . . ?
C13 Ti1 O1 C3 -19.5(10) . . . . ?
C14 Ti1 O1 C3 6.6(11) . . . . ?
O2 Ti2 O3 C29 99.7(10) . . . . ?
Cl3 Ti2 O3 C29 -155.5(10) . . . . ?
C36 Ti2 O3 C29 -3.5(10) . . . . ?
C38 Ti2 O3 C29 -63.0(10) . . . . ?
C37 Ti2 O3 C29 -34.7(10) . . . . ?
C40 Ti2 O3 C29 -4.0(11) . . . . ?
C39 Ti2 O3 C29 -56.6(11) . . . . ?
C18 N1 C1 C2 -157.9(3) . . . . ?
C27 N1 C1 C2 76.7(3) . . . . ?
N1 C1 C2 C7 58.6(4) . . . . ?
N1 C1 C2 C3 -118.3(3) . . . . ?
Ti1 O1 C3 C2 -107.3(9) . . . . ?
Ti1 O1 C3 C4 77.6(10) . . . . ?
C7 C2 C3 O1 -175.1(3) . . . . ?
C1 C2 C3 O1 1.8(5) . . . . ?
C7 C2 C3 C4 -0.3(5) . . . . ?
C1 C2 C3 C4 176.7(3) . . . . ?
O1 C3 C4 C5 174.7(3) . . . . ?
C2 C3 C4 C5 -0.2(5) . . . . ?
O1 C3 C4 C9 -2.8(4) . . . . ?
C2 C3 C4 C9 -177.8(3) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C9 C4 C5 C6 177.6(3) . . . . ?
C4 C5 C6 C7 0.7(5) . . . . ?
C4 C5 C6 C8 -179.2(3) . . . . ?
C5 C6 C7 C2 -1.2(5) . . . . ?
C8 C6 C7 C2 178.6(3) . . . . ?
C3 C2 C7 C6 1.0(5) . . . . ?
C1 C2 C7 C6 -176.0(3) . . . . ?
C14 C10 C11 C12 0.4(4) . . . . ?
Ti1 C10 C11 C12 -64.5(2) . . . . ?
C14 C10 C11 C17 -178.2(3) . . . . ?
Ti1 C10 C11 C17 116.9(3) . . . . ?
C14 C10 C11 Ti1 64.8(2) . . . . ?
C10 C11 C12 C13 -1.8(4) . . . . ?
C17 C11 C12 C13 176.8(3) . . . . ?
Ti1 C11 C12 C13 -67.7(2) . . . . ?
C10 C11 C12 Ti1 65.9(2) . . . . ?
C17 C11 C12 Ti1 -115.5(3) . . . . ?
C11 C12 C13 C14 2.5(4) . . . . ?
Ti1 C12 C13 C14 -63.2(2) . . . . ?
C11 C12 C13 C16 -175.9(3) . . . . ?
Ti1 C12 C13 C16 118.4(4) . . . . ?
C11 C12 C13 Ti1 65.7(2) . . . . ?
C12 C13 C14 C10 -2.2(4) . . . . ?
C16 C13 C14 C10 176.2(3) . . . . ?
Ti1 C13 C14 C10 -63.1(2) . . . . ?
C12 C13 C14 C15 178.7(3) . . . . ?
C16 C13 C14 C15 -2.9(6) . . . . ?
Ti1 C13 C14 C15 117.8(3) . . . . ?
C12 C13 C14 Ti1 60.9(2) . . . . ?
C16 C13 C14 Ti1 -120.7(4) . . . . ?
C11 C10 C14 C13 1.2(4) . . . . ?
Ti1 C10 C14 C13 64.1(2) . . . . ?
C11 C10 C14 C15 -179.7(3) . . . . ?
Ti1 C10 C14 C15 -116.8(3) . . . . ?
C11 C10 C14 Ti1 -63.0(2) . . . . ?
C27 N1 C18 C19 -163.2(3) . . . . ?
C1 N1 C18 C19 70.2(3) . . . . ?
N1 C18 C19 C24 -129.8(3) . . . . ?
N1 C18 C19 C20 54.8(4) . . . . ?
C24 C19 C20 O2 -178.5(3) . . . . ?
C18 C19 C20 O2 -3.0(5) . . . . ?
C24 C19 C20 C21 1.3(5) . . . . ?
C18 C19 C20 C21 176.9(3) . . . . ?
O2 C20 C21 C22 178.5(3) . . . . ?
C19 C20 C21 C22 -1.4(5) . . . . ?
O2 C20 C21 C26 0.0(5) . . . . ?
C19 C20 C21 C26 -179.8(3) . . . . ?
C20 C21 C22 C23 0.4(5) . . . . ?
C26 C21 C22 C23 178.8(3) . . . . ?
C21 C22 C23 C24 0.6(5) . . . . ?
C21 C22 C23 C25 -178.6(4) . . . . ?
C20 C19 C24 C23 -0.3(5) . . . . ?
C18 C19 C24 C23 -175.8(3) . . . . ?
C22 C23 C24 C19 -0.7(5) . . . . ?
C25 C23 C24 C19 178.5(3) . . . . ?
C18 N1 C27 C28 163.6(3) . . . . ?
C1 N1 C27 C28 -70.4(3) . . . . ?
N1 C27 C28 C33 128.7(3) . . . . ?
N1 C27 C28 C29 -53.8(4) . . . . ?
Ti2 O3 C29 C30 125.4(10) . . . . ?
Ti2 O3 C29 C28 -56.5(11) . . . . ?
C33 C28 C29 O3 -180.0(3) . . . . ?
C27 C28 C29 O3 2.4(4) . . . . ?
C33 C28 C29 C30 -1.9(5) . . . . ?
C27 C28 C29 C30 -179.6(3) . . . . ?
O3 C29 C30 C31 -178.1(3) . . . . ?
C28 C29 C30 C31 3.8(5) . . . . ?
O3 C29 C30 C35 2.6(5) . . . . ?
C28 C29 C30 C35 -175.4(3) . . . . ?
C29 C30 C31 C32 -2.1(5) . . . . ?
C35 C30 C31 C32 177.1(3) . . . . ?
C30 C31 C32 C33 -1.4(5) . . . . ?
C30 C31 C32 C34 178.1(3) . . . . ?
C31 C32 C33 C28 3.5(5) . . . . ?
C34 C32 C33 C28 -176.1(3) . . . . ?
C29 C28 C33 C32 -1.8(5) . . . . ?
C27 C28 C33 C32 175.8(3) . . . . ?
C40 C36 C37 C38 3.8(4) . . . . ?
Ti2 C36 C37 C38 -63.5(2) . . . . ?
C40 C36 C37 C43 -176.6(3) . . . . ?
Ti2 C36 C37 C43 116.1(3) . . . . ?
C40 C36 C37 Ti2 67.4(2) . . . . ?
C36 C37 C38 C39 -3.6(4) . . . . ?
C43 C37 C38 C39 176.8(3) . . . . ?
Ti2 C37 C38 C39 -65.8(2) . . . . ?
C36 C37 C38 Ti2 62.2(2) . . . . ?
C43 C37 C38 Ti2 -117.4(3) . . . . ?
C37 C38 C39 C40 2.0(4) . . . . ?
Ti2 C38 C39 C40 -63.4(2) . . . . ?
C37 C38 C39 C42 -176.2(3) . . . . ?
Ti2 C38 C39 C42 118.4(4) . . . . ?
C37 C38 C39 Ti2 65.4(2) . . . . ?
C38 C39 C40 C36 0.4(4) . . . . ?
C42 C39 C40 C36 178.6(3) . . . . ?
Ti2 C39 C40 C36 -62.5(2) . . . . ?
C38 C39 C40 C41 -178.8(3) . . . . ?
C42 C39 C40 C41 -0.6(6) . . . . ?
Ti2 C39 C40 C41 118.3(4) . . . . ?
C38 C39 C40 Ti2 62.9(2) . . . . ?
C42 C39 C40 Ti2 -118.9(4) . . . . ?
C37 C36 C40 C39 -2.6(4) . . . . ?
Ti2 C36 C40 C39 64.8(2) . . . . ?
C37 C36 C40 C41 176.6(3) . . . . ?
Ti2 C36 C40 C41 -116.0(4) . . . . ?
C37 C36 C40 Ti2 -67.4(2) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti7
_database_code_depnum_ccdc_archive 'CCDC 1549586'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C69 H99 Cl6 N O3 Ti3'
_chemical_formula_moiety         'C69 H99 Cl6 N O3 Ti3'
_chemical_formula_weight         1346.96
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   13.2258(6)
_cell_length_b                   22.4804(11)
_cell_length_c                   24.4338(12)
_cell_angle_alpha                90.0000
_cell_angle_beta                 99.642(4)
_cell_angle_gamma                90.0000
_cell_volume                     7162.1(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9911
_cell_measurement_theta_min      1.91
_cell_measurement_theta_max      31.28
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       plate
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.330
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.050
_exptl_crystal_density_diffrn    1.249
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848.00
_exptl_absorpt_coefficient_mu    0.593
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.936
_exptl_absorpt_correction_T_max  0.971

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            75160
_diffrn_reflns_av_R_equivalents  0.1157
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.623
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             16446
_reflns_number_gt                10227
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1132
_refine_ls_R_factor_gt           0.0571
_refine_ls_wR_factor_ref         0.1330
_refine_ls_wR_factor_gt          0.1101
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         16446
_refine_ls_number_parameters     739
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0399P)²+5.5057P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.47
_refine_diff_density_min         -0.59
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.87213(4) 0.80126(3) 0.12163(2) 0.01470(13) Uani 1 1 d . . . . .
Ti2 Ti 0.97466(4) 0.61217(3) 0.34628(2) 0.01565(14) Uani 1 1 d . . . . .
Ti3 Ti 0.74388(5) 0.86571(3) 0.41457(3) 0.02058(15) Uani 1 1 d . . . . .
Cl1 Cl 0.99463(7) 0.77997(4) 0.07021(4) 0.0283(2) Uani 1 1 d . . . . .
Cl2 Cl 0.96031(6) 0.79098(4) 0.20809(3) 0.0243(2) Uani 1 1 d . . . . .
Cl3 Cl 1.02344(7) 0.70625(4) 0.33600(4) 0.0256(2) Uani 1 1 d . . . . .
Cl4 Cl 1.08453(6) 0.58496(4) 0.42370(4) 0.0263(2) Uani 1 1 d . . . . .
Cl5 Cl 0.75121(8) 0.95782(4) 0.45159(4) 0.0368(3) Uani 1 1 d . . . . .
Cl6 Cl 0.87265(7) 0.86880(5) 0.36488(4) 0.0351(2) Uani 1 1 d . . . . .
O1 O 0.79022(16) 0.73798(9) 0.11262(9) 0.0161(5) Uani 1 1 d . . . . .
O2 O 0.85303(16) 0.61947(9) 0.36921(9) 0.0147(5) Uani 1 1 d . . . . .
O3 O 0.63185(16) 0.86951(10) 0.36197(9) 0.0182(5) Uani 1 1 d . . . . .
N1 N 0.65644(19) 0.72527(11) 0.25601(10) 0.0137(6) Uani 1 1 d . . . . .
C1 C 0.6853(2) 0.74466(14) 0.20344(13) 0.0153(7) Uani 1 1 d . . . . .
H1A H 0.7599 0.7528 0.2093 0.018 Uiso 1 1 calc R U . . .
H1B H 0.6491 0.7822 0.1915 0.018 Uiso 1 1 calc R U . . .
C2 C 0.6597(2) 0.69900(14) 0.15813(13) 0.0152(7) Uani 1 1 d . . . . .
C3 C 0.7113(2) 0.69792(14) 0.11255(13) 0.0146(7) Uani 1 1 d . . . . .
C4 C 0.6872(2) 0.65629(14) 0.06946(13) 0.0176(7) Uani 1 1 d . . . . .
C5 C 0.6115(3) 0.61473(15) 0.07592(14) 0.0196(7) Uani 1 1 d . . . . .
H5 H 0.5936 0.5860 0.0474 0.024 Uiso 1 1 calc R U . . .
C6 C 0.5609(2) 0.61266(15) 0.12119(13) 0.0187(7) Uani 1 1 d . . . . .
C7 C 0.5853(2) 0.65639(14) 0.16139(13) 0.0160(7) Uani 1 1 d . . . . .
H7 H 0.5498 0.6571 0.1921 0.019 Uiso 1 1 calc R U . . .
C8 C 0.7452(3) 0.65284(15) 0.01998(14) 0.0219(8) Uani 1 1 d . . . . .
C9 C 0.8549(3) 0.63252(17) 0.04285(15) 0.0296(9) Uani 1 1 d . . . . .
H9A H 0.8528 0.5946 0.0623 0.036 Uiso 1 1 calc R U . . .
H9B H 0.8932 0.6275 0.0121 0.036 Uiso 1 1 calc R U . . .
H9C H 0.8889 0.6625 0.0687 0.036 Uiso 1 1 calc R U . . .
C10 C 0.7458(3) 0.71207(15) -0.01075(14) 0.0238(8) Uani 1 1 d . . . . .
H10A H 0.7761 0.7429 0.0153 0.029 Uiso 1 1 calc R U . . .
H10B H 0.7865 0.7080 -0.0406 0.029 Uiso 1 1 calc R U . . .
H10C H 0.6754 0.7232 -0.0266 0.029 Uiso 1 1 calc R U . . .
C11 C 0.6972(3) 0.60673(16) -0.02272(14) 0.0267(8) Uani 1 1 d . . . . .
H11A H 0.6953 0.5679 -0.0046 0.032 Uiso 1 1 calc R U . . .
H11B H 0.6272 0.6190 -0.0384 0.032 Uiso 1 1 calc R U . . .
H11C H 0.7383 0.6038 -0.0524 0.032 Uiso 1 1 calc R U . . .
C12 C 0.4877(3) 0.56259(15) 0.13127(14) 0.0223(8) Uani 1 1 d . . . . .
C13 C 0.4613(3) 0.52132(16) 0.08110(15) 0.0299(9) Uani 1 1 d . . . . .
H13A H 0.5247 0.5050 0.0713 0.036 Uiso 1 1 calc R U . . .
H13B H 0.4179 0.4887 0.0903 0.036 Uiso 1 1 calc R U . . .
H13C H 0.4246 0.5438 0.0496 0.036 Uiso 1 1 calc R U . . .
C14 C 0.5409(3) 0.52469(17) 0.17995(15) 0.0330(10) Uani 1 1 d . . . . .
H14A H 0.6044 0.5081 0.1707 0.040 Uiso 1 1 calc R U . . .
H14B H 0.5569 0.5496 0.2132 0.040 Uiso 1 1 calc R U . . .
H14C H 0.4953 0.4922 0.1870 0.040 Uiso 1 1 calc R U . . .
C15 C 0.3889(3) 0.58808(18) 0.14646(15) 0.0321(9) Uani 1 1 d . . . . .
H15A H 0.4057 0.6145 0.1786 0.039 Uiso 1 1 calc R U . . .
H15B H 0.3522 0.6106 0.1149 0.039 Uiso 1 1 calc R U . . .
H15C H 0.3454 0.5555 0.1556 0.039 Uiso 1 1 calc R U . . .
C16 C 0.7280(2) 0.86019(14) 0.09024(14) 0.0180(7) Uani 1 1 d . . . . .
C17 C 0.8034(2) 0.87368(15) 0.05831(14) 0.0195(7) Uani 1 1 d . . . . .
H17 H 0.7950 0.8697 0.0170 0.023 Uiso 1 1 calc R U . . .
C18 C 0.8881(3) 0.90196(15) 0.09244(14) 0.0195(7) Uani 1 1 d . . . . .
C19 C 0.8655(2) 0.90450(14) 0.14634(14) 0.0188(7) Uani 1 1 d . . . . .
C20 C 0.7678(3) 0.87780(14) 0.14515(14) 0.0192(7) Uani 1 1 d . . . . .
H20 H 0.7291 0.8768 0.1770 0.023 Uiso 1 1 calc R U . . .
C21 C 0.6240(2) 0.83499(16) 0.06916(15) 0.0236(8) Uani 1 1 d . . . . .
H21A H 0.5865 0.8298 0.1002 0.028 Uiso 1 1 calc R U . . .
H21B H 0.5861 0.8623 0.0419 0.028 Uiso 1 1 calc R U . . .
H21C H 0.6313 0.7964 0.0516 0.028 Uiso 1 1 calc R U . . .
C22 C 0.9815(3) 0.92685(17) 0.07406(15) 0.0280(9) Uani 1 1 d . . . . .
H22A H 0.9785 0.9191 0.0344 0.034 Uiso 1 1 calc R U . . .
H22B H 0.9845 0.9699 0.0807 0.034 Uiso 1 1 calc R U . . .
H22C H 1.0427 0.9080 0.0951 0.034 Uiso 1 1 calc R U . . .
C23 C 0.9284(3) 0.93278(16) 0.19607(15) 0.0271(8) Uani 1 1 d . . . . .
H23A H 0.8938 0.9278 0.2283 0.032 Uiso 1 1 calc R U . . .
H23B H 0.9960 0.9138 0.2036 0.032 Uiso 1 1 calc R U . . .
H23C H 0.9365 0.9753 0.1890 0.032 Uiso 1 1 calc R U . . .
C24 C 0.7264(2) 0.67868(15) 0.28134(13) 0.0161(7) Uani 1 1 d . . . . .
H24A H 0.7934 0.6967 0.2968 0.019 Uiso 1 1 calc R U . . .
H24B H 0.7378 0.6497 0.2525 0.019 Uiso 1 1 calc R U . . .
C25 C 0.6846(2) 0.64650(14) 0.32698(13) 0.0148(7) Uani 1 1 d . . . . .
C26 C 0.7498(2) 0.61914(14) 0.37104(13) 0.0144(7) Uani 1 1 d . . . . .
C27 C 0.7117(2) 0.59396(14) 0.41597(13) 0.0146(7) Uani 1 1 d . . . . .
C28 C 0.6049(2) 0.59445(15) 0.41277(14) 0.0192(7) Uani 1 1 d . . . . .
H28 H 0.5772 0.5774 0.4426 0.023 Uiso 1 1 calc R U . . .
C29 C 0.5372(2) 0.61831(15) 0.36860(13) 0.0176(7) Uani 1 1 d . . . . .
C30 C 0.5798(2) 0.64494(14) 0.32638(14) 0.0172(7) Uani 1 1 d . . . . .
H30 H 0.5356 0.6626 0.2961 0.021 Uiso 1 1 calc R U . . .
C31 C 0.7821(2) 0.56736(15) 0.46659(13) 0.0176(7) Uani 1 1 d . . . . .
C32 C 0.8403(3) 0.51408(15) 0.44835(14) 0.0227(8) Uani 1 1 d . . . . .
H32A H 0.8799 0.5268 0.4199 0.027 Uiso 1 1 calc R U . . .
H32B H 0.8870 0.4982 0.4804 0.027 Uiso 1 1 calc R U . . .
H32C H 0.7914 0.4832 0.4331 0.027 Uiso 1 1 calc R U . . .
C33 C 0.7216(3) 0.54585(17) 0.51079(14) 0.0272(9) Uani 1 1 d . . . . .
H33A H 0.6835 0.5793 0.5232 0.033 Uiso 1 1 calc R U . . .
H33B H 0.6734 0.5147 0.4951 0.033 Uiso 1 1 calc R U . . .
H33C H 0.7690 0.5297 0.5424 0.033 Uiso 1 1 calc R U . . .
C34 C 0.8569(3) 0.61518(16) 0.49371(14) 0.0236(8) Uani 1 1 d . . . . .
H34A H 0.8974 0.6302 0.4665 0.028 Uiso 1 1 calc R U . . .
H34B H 0.8183 0.6480 0.5066 0.028 Uiso 1 1 calc R U . . .
H34C H 0.9029 0.5979 0.5253 0.028 Uiso 1 1 calc R U . . .
C35 C 0.4202(2) 0.61496(16) 0.36423(14) 0.0217(8) Uani 1 1 d . . . . .
C36 C 0.3815(3) 0.5688(2) 0.3199(2) 0.0498(13) Uani 1 1 d . . . . .
H36A H 0.4025 0.5802 0.2848 0.060 Uiso 1 1 calc R U . . .
H36B H 0.4106 0.5298 0.3315 0.060 Uiso 1 1 calc R U . . .
H36C H 0.3065 0.5667 0.3149 0.060 Uiso 1 1 calc R U . . .
C37 C 0.3879(3) 0.5975(2) 0.41835(17) 0.0498(13) Uani 1 1 d . . . . .
H37A H 0.4190 0.5592 0.4307 0.060 Uiso 1 1 calc R U . . .
H37B H 0.4108 0.6279 0.4464 0.060 Uiso 1 1 calc R U . . .
H37C H 0.3131 0.5940 0.4131 0.060 Uiso 1 1 calc R U . . .
C38 C 0.3700(3) 0.67446(19) 0.34701(19) 0.0424(11) Uani 1 1 d . . . . .
H38A H 0.3894 0.6872 0.3118 0.051 Uiso 1 1 calc R U . . .
H38B H 0.2953 0.6703 0.3424 0.051 Uiso 1 1 calc R U . . .
H38C H 0.3930 0.7042 0.3757 0.051 Uiso 1 1 calc R U . . .
C39 C 0.8994(2) 0.54080(15) 0.28095(14) 0.0187(7) Uani 1 1 d . . . . .
C40 C 0.9279(2) 0.59113(15) 0.25252(13) 0.0189(7) Uani 1 1 d . . . . .
H40 H 0.8800 0.6156 0.2255 0.023 Uiso 1 1 calc R U . . .
C41 C 1.0362(3) 0.59525(15) 0.26113(14) 0.0193(7) Uani 1 1 d . . . . .
C42 C 1.0732(3) 0.54943(16) 0.29801(14) 0.0231(8) Uani 1 1 d . . . . .
H42 H 1.1473 0.5396 0.3104 0.028 Uiso 1 1 calc R U . . .
C43 C 0.9899(2) 0.51517(15) 0.31012(14) 0.0186(7) Uani 1 1 d . . . . .
C44 C 0.7930(3) 0.51637(16) 0.27834(15) 0.0255(8) Uani 1 1 d . . . . .
H44A H 0.7438 0.5425 0.2554 0.031 Uiso 1 1 calc R U . . .
H44B H 0.7894 0.4765 0.2620 0.031 Uiso 1 1 calc R U . . .
H44C H 0.7764 0.5142 0.3159 0.031 Uiso 1 1 calc R U . . .
C45 C 1.0976(3) 0.63793(16) 0.23330(15) 0.0265(8) Uani 1 1 d . . . . .
H45A H 1.0513 0.6651 0.2098 0.032 Uiso 1 1 calc R U . . .
H45B H 1.1430 0.6608 0.2615 0.032 Uiso 1 1 calc R U . . .
H45C H 1.1389 0.6159 0.2104 0.032 Uiso 1 1 calc R U . . .
C46 C 0.9980(3) 0.45959(15) 0.34411(16) 0.0273(9) Uani 1 1 d . . . . .
H46A H 1.0700 0.4521 0.3597 0.033 Uiso 1 1 calc R U . . .
H46B H 0.9583 0.4642 0.3743 0.033 Uiso 1 1 calc R U . . .
H46C H 0.9708 0.4260 0.3206 0.033 Uiso 1 1 calc R U . . .
C47 C 0.6571(2) 0.77508(14) 0.29402(13) 0.0155(7) Uani 1 1 d . . . . .
H47A H 0.7155 0.8014 0.2902 0.019 Uiso 1 1 calc R U . . .
H47B H 0.6682 0.7597 0.3325 0.019 Uiso 1 1 calc R U . . .
C48 C 0.5601(2) 0.81130(14) 0.28467(13) 0.0170(7) Uani 1 1 d . . . . .
C49 C 0.5500(2) 0.85854(15) 0.32060(13) 0.0163(7) Uani 1 1 d . . . . .
C50 C 0.4601(3) 0.89308(15) 0.31465(14) 0.0203(8) Uani 1 1 d . . . . .
C51 C 0.3826(3) 0.87810(15) 0.27042(14) 0.0213(8) Uani 1 1 d . . . . .
H51 H 0.3220 0.9015 0.2649 0.026 Uiso 1 1 calc R U . . .
C52 C 0.3887(2) 0.83123(15) 0.23414(14) 0.0199(8) Uani 1 1 d . . . . .
C53 C 0.4790(2) 0.79778(15) 0.24256(13) 0.0175(7) Uani 1 1 d . . . . .
H53 H 0.4852 0.7649 0.2189 0.021 Uiso 1 1 calc R U . . .
C54 C 0.4464(3) 0.94505(16) 0.35349(14) 0.0249(8) Uani 1 1 d . . . . .
C55 C 0.5274(3) 0.99252(16) 0.34941(15) 0.0296(9) Uani 1 1 d . . . . .
H55A H 0.5186 1.0257 0.3742 0.036 Uiso 1 1 calc R U . . .
H55B H 0.5959 0.9753 0.3603 0.036 Uiso 1 1 calc R U . . .
H55C H 0.5197 1.0070 0.3111 0.036 Uiso 1 1 calc R U . . .
C56 C 0.3410(3) 0.97493(19) 0.33832(17) 0.0378(10) Uani 1 1 d . . . . .
H56A H 0.2870 0.9456 0.3405 0.045 Uiso 1 1 calc R U . . .
H56B H 0.3355 1.0075 0.3643 0.045 Uiso 1 1 calc R U . . .
H56C H 0.3333 0.9907 0.3005 0.045 Uiso 1 1 calc R U . . .
C57 C 0.4549(3) 0.92216(18) 0.41329(15) 0.0340(10) Uani 1 1 d . . . . .
H57A H 0.4023 0.8918 0.4149 0.041 Uiso 1 1 calc R U . . .
H57B H 0.5230 0.9048 0.4252 0.041 Uiso 1 1 calc R U . . .
H57C H 0.4448 0.9553 0.4379 0.041 Uiso 1 1 calc R U . . .
C58 C 0.3012(3) 0.81415(16) 0.18719(15) 0.0240(8) Uani 1 1 d . . . . .
C59 C 0.2513(3) 0.75716(18) 0.20365(17) 0.0351(10) Uani 1 1 d . . . . .
H59A H 0.3029 0.7255 0.2103 0.042 Uiso 1 1 calc R U . . .
H59B H 0.2227 0.7642 0.2376 0.042 Uiso 1 1 calc R U . . .
H59C H 0.1963 0.7452 0.1737 0.042 Uiso 1 1 calc R U . . .
C60 C 0.3412(3) 0.8034(2) 0.13313(15) 0.0390(11) Uani 1 1 d . . . . .
H60A H 0.3940 0.7723 0.1388 0.047 Uiso 1 1 calc R U . . .
H60B H 0.2846 0.7906 0.1044 0.047 Uiso 1 1 calc R U . . .
H60C H 0.3709 0.8402 0.1214 0.047 Uiso 1 1 calc R U . . .
C61 C 0.2195(3) 0.86243(19) 0.17714(19) 0.0472(12) Uani 1 1 d . . . . .
H61A H 0.1928 0.8700 0.2116 0.057 Uiso 1 1 calc R U . . .
H61B H 0.2497 0.8990 0.1652 0.057 Uiso 1 1 calc R U . . .
H61C H 0.1635 0.8494 0.1482 0.057 Uiso 1 1 calc R U . . .
C62 C 0.6704(3) 0.78726(16) 0.45876(14) 0.0266(9) Uani 1 1 d . . . . .
C63 C 0.7575(3) 0.76564(16) 0.43893(15) 0.0288(9) Uani 1 1 d . . . . .
H63 H 0.7566 0.7322 0.4119 0.035 Uiso 1 1 calc R U . . .
C64 C 0.8473(3) 0.79146(16) 0.46874(15) 0.0277(9) Uani 1 1 d . . . . .
C65 C 0.8142(3) 0.83275(17) 0.50518(14) 0.0270(9) Uani 1 1 d . . . . .
H65 H 0.8603 0.8567 0.5335 0.032 Uiso 1 1 calc R U . . .
C66 C 0.7058(3) 0.82995(17) 0.50002(15) 0.0285(9) Uani 1 1 d . . . . .
C67 C 0.5626(3) 0.76742(18) 0.44038(15) 0.0338(10) Uani 1 1 d . . . . .
H67A H 0.5170 0.7896 0.4608 0.041 Uiso 1 1 calc R U . . .
H67B H 0.5427 0.7748 0.4005 0.041 Uiso 1 1 calc R U . . .
H67C H 0.5571 0.7248 0.4478 0.041 Uiso 1 1 calc R U . . .
C68 C 0.9554(3) 0.77637(19) 0.46501(17) 0.0388(11) Uani 1 1 d . . . . .
H68A H 0.9565 0.7463 0.4361 0.047 Uiso 1 1 calc R U . . .
H68B H 0.9911 0.8122 0.4557 0.047 Uiso 1 1 calc R U . . .
H68C H 0.9896 0.7607 0.5008 0.047 Uiso 1 1 calc R U . . .
C69 C 0.6439(3) 0.86309(19) 0.53630(16) 0.0361(10) Uani 1 1 d . . . . .
H69A H 0.6889 0.8898 0.5610 0.043 Uiso 1 1 calc R U . . .
H69B H 0.5906 0.8864 0.5130 0.043 Uiso 1 1 calc R U . . .
H69C H 0.6117 0.8347 0.5585 0.043 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.779(2) . ?
Ti1 Cl2 2.2474(10) . ?
Ti1 Cl1 2.2615(10) . ?
Ti1 C17 2.324(3) . ?
Ti1 C20 2.337(3) . ?
Ti1 C16 2.343(3) . ?
Ti1 C18 2.394(3) . ?
Ti1 C19 2.404(3) . ?
Ti2 O2 1.798(2) . ?
Ti2 Cl3 2.2377(10) . ?
Ti2 Cl4 2.2680(10) . ?
Ti2 C40 2.319(3) . ?
Ti2 C39 2.362(3) . ?
Ti2 C42 2.365(3) . ?
Ti2 C43 2.374(3) . ?
Ti2 C41 2.388(3) . ?
Ti3 O3 1.793(2) . ?
Ti3 Cl6 2.2521(12) . ?
Ti3 Cl5 2.2551(11) . ?
Ti3 C63 2.326(4) . ?
Ti3 C62 2.361(4) . ?
Ti3 C66 2.369(4) . ?
Ti3 C65 2.372(3) . ?
Ti3 C64 2.409(4) . ?
O1 C3 1.379(4) . ?
O2 C26 1.374(4) . ?
O3 C49 1.374(4) . ?
N1 C47 1.454(4) . ?
N1 C24 1.464(4) . ?
N1 C1 1.466(4) . ?
C1 C2 1.506(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.385(4) . ?
C2 C3 1.400(4) . ?
C3 C4 1.405(4) . ?
C4 C5 1.397(5) . ?
C4 C8 1.538(5) . ?
C5 C6 1.386(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.389(4) . ?
C6 C12 1.532(5) . ?
C7 H7 0.9500 . ?
C8 C10 1.530(5) . ?
C8 C11 1.531(5) . ?
C8 C9 1.535(5) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.529(5) . ?
C12 C13 1.530(5) . ?
C12 C14 1.535(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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.399(5) . ?
C16 C20 1.413(5) . ?
C16 C21 1.497(4) . ?
C17 C18 1.429(5) . ?
C17 H17 1.0000 . ?
C18 C19 1.400(5) . ?
C18 C22 1.491(5) . ?
C19 C20 1.421(5) . ?
C19 C23 1.495(5) . ?
C20 H20 1.0000 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 C25 1.509(4) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C30 1.384(4) . ?
C25 C26 1.403(4) . ?
C26 C27 1.401(4) . ?
C27 C28 1.401(4) . ?
C27 C31 1.539(4) . ?
C28 C29 1.390(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.391(4) . ?
C29 C35 1.535(4) . ?
C30 H30 0.9500 . ?
C31 C33 1.527(5) . ?
C31 C32 1.530(5) . ?
C31 C34 1.534(5) . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 C37 1.508(5) . ?
C35 C38 1.521(5) . ?
C35 C36 1.525(5) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C43 1.409(4) . ?
C39 C40 1.411(5) . ?
C39 C44 1.502(4) . ?
C40 C41 1.416(4) . ?
C40 H40 1.0000 . ?
C41 C42 1.402(5) . ?
C41 C45 1.493(5) . ?
C42 C43 1.416(5) . ?
C42 H42 1.0000 . ?
C43 C46 1.494(5) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 H45A 0.9800 . ?
C45 H45B 0.9800 . ?
C45 H45C 0.9800 . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 C48 1.504(4) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C53 1.390(4) . ?
C48 C49 1.399(5) . ?
C49 C50 1.407(4) . ?
C50 C51 1.400(5) . ?
C50 C54 1.535(5) . ?
C51 C52 1.388(5) . ?
C51 H51 0.9500 . ?
C52 C53 1.398(5) . ?
C52 C58 1.535(5) . ?
C53 H53 0.9500 . ?
C54 C55 1.527(5) . ?
C54 C57 1.535(5) . ?
C54 C56 1.536(5) . ?
C55 H55A 0.9800 . ?
C55 H55B 0.9800 . ?
C55 H55C 0.9800 . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C58 C61 1.522(5) . ?
C58 C60 1.522(5) . ?
C58 C59 1.525(5) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C63 1.409(5) . ?
C62 C66 1.414(5) . ?
C62 C67 1.490(5) . ?
C63 C64 1.410(5) . ?
C63 H63 1.0000 . ?
C64 C65 1.406(5) . ?
C64 C68 1.486(5) . ?
C65 C66 1.419(5) . ?
C65 H65 1.0000 . ?
C66 C69 1.501(5) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 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 Cl2 104.09(8) . . ?
O1 Ti1 Cl1 103.89(8) . . ?
Cl2 Ti1 Cl1 101.14(4) . . ?
O1 Ti1 C17 108.41(11) . . ?
Cl2 Ti1 C17 141.39(9) . . ?
Cl1 Ti1 C17 90.86(9) . . ?
O1 Ti1 C20 104.28(11) . . ?
Cl2 Ti1 C20 94.55(9) . . ?
Cl1 Ti1 C20 143.13(9) . . ?
C17 Ti1 C20 57.77(12) . . ?
O1 Ti1 C16 88.07(11) . . ?
Cl2 Ti1 C16 129.17(9) . . ?
Cl1 Ti1 C16 123.86(9) . . ?
C17 Ti1 C16 34.89(11) . . ?
C20 Ti1 C16 35.15(11) . . ?
O1 Ti1 C18 143.29(11) . . ?
Cl2 Ti1 C18 108.63(9) . . ?
Cl1 Ti1 C18 85.83(9) . . ?
C17 Ti1 C18 35.22(11) . . ?
C20 Ti1 C18 57.47(12) . . ?
C16 Ti1 C18 58.35(11) . . ?
O1 Ti1 C19 139.11(11) . . ?
Cl2 Ti1 C19 84.16(8) . . ?
Cl1 Ti1 C19 113.81(9) . . ?
C17 Ti1 C19 57.58(12) . . ?
C20 Ti1 C19 34.84(11) . . ?
C16 Ti1 C19 58.27(11) . . ?
C18 Ti1 C19 33.93(11) . . ?
O2 Ti2 Cl3 103.80(8) . . ?
O2 Ti2 Cl4 104.27(7) . . ?
Cl3 Ti2 Cl4 101.07(4) . . ?
O2 Ti2 C40 102.81(11) . . ?
Cl3 Ti2 C40 96.67(9) . . ?
Cl4 Ti2 C40 142.81(9) . . ?
O2 Ti2 C39 88.57(11) . . ?
Cl3 Ti2 C39 131.52(9) . . ?
Cl4 Ti2 C39 121.27(9) . . ?
C40 Ti2 C39 35.07(11) . . ?
O2 Ti2 C42 143.78(11) . . ?
Cl3 Ti2 C42 108.32(9) . . ?
Cl4 Ti2 C42 85.73(9) . . ?
C40 Ti2 C42 57.60(12) . . ?
C39 Ti2 C42 57.52(12) . . ?
O2 Ti2 C43 109.64(11) . . ?
Cl3 Ti2 C43 141.49(9) . . ?
Cl4 Ti2 C43 88.87(8) . . ?
C40 Ti2 C43 58.03(12) . . ?
C39 Ti2 C43 34.63(11) . . ?
C42 Ti2 C43 34.76(11) . . ?
O2 Ti2 C41 137.70(11) . . ?
Cl3 Ti2 C41 84.61(9) . . ?
Cl4 Ti2 C41 114.80(9) . . ?
C40 Ti2 C41 34.98(11) . . ?
C39 Ti2 C41 57.97(11) . . ?
C42 Ti2 C41 34.30(11) . . ?
C43 Ti2 C41 57.79(11) . . ?
O3 Ti3 Cl6 102.76(8) . . ?
O3 Ti3 Cl5 102.63(8) . . ?
Cl6 Ti3 Cl5 101.68(5) . . ?
O3 Ti3 C63 104.39(12) . . ?
Cl6 Ti3 C63 97.74(11) . . ?
Cl5 Ti3 C63 142.09(10) . . ?
O3 Ti3 C62 90.53(11) . . ?
Cl6 Ti3 C62 132.54(10) . . ?
Cl5 Ti3 C62 119.72(10) . . ?
C63 Ti3 C62 34.97(13) . . ?
O3 Ti3 C66 112.07(12) . . ?
Cl6 Ti3 C66 141.01(10) . . ?
Cl5 Ti3 C66 87.66(10) . . ?
C63 Ti3 C66 57.66(14) . . ?
C62 Ti3 C66 34.78(12) . . ?
O3 Ti3 C65 146.24(12) . . ?
Cl6 Ti3 C65 107.41(10) . . ?
Cl5 Ti3 C65 85.91(9) . . ?
C63 Ti3 C65 57.15(12) . . ?
C62 Ti3 C65 57.77(12) . . ?
C66 Ti3 C65 34.83(12) . . ?
O3 Ti3 C64 138.73(12) . . ?
Cl6 Ti3 C64 84.63(10) . . ?
Cl5 Ti3 C64 115.69(9) . . ?
C63 Ti3 C64 34.60(12) . . ?
C62 Ti3 C64 58.03(13) . . ?
C66 Ti3 C64 57.70(13) . . ?
C65 Ti3 C64 34.20(12) . . ?
C3 O1 Ti1 165.4(2) . . ?
C26 O2 Ti2 163.0(2) . . ?
C49 O3 Ti3 166.7(2) . . ?
C47 N1 C24 110.2(2) . . ?
C47 N1 C1 110.9(2) . . ?
C24 N1 C1 110.1(2) . . ?
N1 C1 C2 112.5(3) . . ?
N1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
N1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.8 . . ?
C7 C2 C3 118.6(3) . . ?
C7 C2 C1 120.2(3) . . ?
C3 C2 C1 121.1(3) . . ?
O1 C3 C2 117.2(3) . . ?
O1 C3 C4 120.9(3) . . ?
C2 C3 C4 121.9(3) . . ?
C5 C4 C3 116.0(3) . . ?
C5 C4 C8 121.0(3) . . ?
C3 C4 C8 122.8(3) . . ?
C6 C5 C4 124.3(3) . . ?
C6 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C5 C6 C7 117.0(3) . . ?
C5 C6 C12 123.8(3) . . ?
C7 C6 C12 119.0(3) . . ?
C2 C7 C6 122.1(3) . . ?
C2 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C10 C8 C11 106.9(3) . . ?
C10 C8 C9 110.8(3) . . ?
C11 C8 C9 107.8(3) . . ?
C10 C8 C4 112.7(3) . . ?
C11 C8 C4 111.4(3) . . ?
C9 C8 C4 107.1(3) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C12 C13 109.4(3) . . ?
C15 C12 C6 110.7(3) . . ?
C13 C12 C6 112.5(3) . . ?
C15 C12 C14 108.6(3) . . ?
C13 C12 C14 107.3(3) . . ?
C6 C12 C14 108.2(3) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 106.4(3) . . ?
C17 C16 C21 126.2(3) . . ?
C20 C16 C21 127.4(3) . . ?
C17 C16 Ti1 71.81(18) . . ?
C20 C16 Ti1 72.20(18) . . ?
C21 C16 Ti1 123.3(2) . . ?
C16 C17 C18 109.5(3) . . ?
C16 C17 Ti1 73.30(19) . . ?
C18 C17 Ti1 75.06(19) . . ?
C16 C17 H17 125.0 . . ?
C18 C17 H17 125.0 . . ?
Ti1 C17 H17 125.0 . . ?
C19 C18 C17 107.3(3) . . ?
C19 C18 C22 125.9(3) . . ?
C17 C18 C22 126.8(3) . . ?
C19 C18 Ti1 73.43(19) . . ?
C17 C18 Ti1 69.72(18) . . ?
C22 C18 Ti1 124.3(2) . . ?
C18 C19 C20 107.5(3) . . ?
C18 C19 C23 127.2(3) . . ?
C20 C19 C23 125.2(3) . . ?
C18 C19 Ti1 72.64(19) . . ?
C20 C19 Ti1 70.02(18) . . ?
C23 C19 Ti1 125.2(2) . . ?
C16 C20 C19 109.3(3) . . ?
C16 C20 Ti1 72.64(19) . . ?
C19 C20 Ti1 75.14(19) . . ?
C16 C20 H20 125.1 . . ?
C19 C20 H20 125.1 . . ?
Ti1 C20 H20 125.1 . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C22 H22A 109.5 . . ?
C18 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C18 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C19 C23 H23A 109.5 . . ?
C19 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C19 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N1 C24 C25 111.8(2) . . ?
N1 C24 H24A 109.3 . . ?
C25 C24 H24A 109.3 . . ?
N1 C24 H24B 109.3 . . ?
C25 C24 H24B 109.3 . . ?
H24A C24 H24B 107.9 . . ?
C30 C25 C26 118.8(3) . . ?
C30 C25 C24 119.6(3) . . ?
C26 C25 C24 121.6(3) . . ?
O2 C26 C27 121.1(3) . . ?
O2 C26 C25 117.3(3) . . ?
C27 C26 C25 121.5(3) . . ?
C28 C27 C26 116.4(3) . . ?
C28 C27 C31 121.1(3) . . ?
C26 C27 C31 122.5(3) . . ?
C29 C28 C27 124.0(3) . . ?
C29 C28 H28 118.0 . . ?
C27 C28 H28 118.0 . . ?
C28 C29 C30 116.9(3) . . ?
C28 C29 C35 123.1(3) . . ?
C30 C29 C35 119.9(3) . . ?
C25 C30 C29 122.2(3) . . ?
C25 C30 H30 118.9 . . ?
C29 C30 H30 118.9 . . ?
C33 C31 C32 107.9(3) . . ?
C33 C31 C34 107.0(3) . . ?
C32 C31 C34 110.8(3) . . ?
C33 C31 C27 111.9(3) . . ?
C32 C31 C27 109.7(3) . . ?
C34 C31 C27 109.5(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C37 C35 C38 107.3(3) . . ?
C37 C35 C36 109.6(4) . . ?
C38 C35 C36 108.8(3) . . ?
C37 C35 C29 112.4(3) . . ?
C38 C35 C29 111.3(3) . . ?
C36 C35 C29 107.3(3) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C43 C39 C40 107.7(3) . . ?
C43 C39 C44 125.6(3) . . ?
C40 C39 C44 126.7(3) . . ?
C43 C39 Ti2 73.14(19) . . ?
C40 C39 Ti2 70.81(19) . . ?
C44 C39 Ti2 124.2(2) . . ?
C39 C40 C41 109.0(3) . . ?
C39 C40 Ti2 74.12(19) . . ?
C41 C40 Ti2 75.16(19) . . ?
C39 C40 H40 125.1 . . ?
C41 C40 H40 125.1 . . ?
Ti2 C40 H40 125.1 . . ?
C42 C41 C40 106.4(3) . . ?
C42 C41 C45 127.4(3) . . ?
C40 C41 C45 126.1(3) . . ?
C42 C41 Ti2 71.96(19) . . ?
C40 C41 Ti2 69.86(18) . . ?
C45 C41 Ti2 125.8(2) . . ?
C41 C42 C43 109.5(3) . . ?
C41 C42 Ti2 73.7(2) . . ?
C43 C42 Ti2 72.95(19) . . ?
C41 C42 H42 125.1 . . ?
C43 C42 H42 125.1 . . ?
Ti2 C42 H42 125.1 . . ?
C39 C43 C42 107.2(3) . . ?
C39 C43 C46 126.8(3) . . ?
C42 C43 C46 125.8(3) . . ?
C39 C43 Ti2 72.23(19) . . ?
C42 C43 Ti2 72.3(2) . . ?
C46 C43 Ti2 124.3(2) . . ?
C39 C44 H44A 109.5 . . ?
C39 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C39 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C41 C45 H45A 109.5 . . ?
C41 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C41 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C46 H46A 109.5 . . ?
C43 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C43 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
N1 C47 C48 114.0(3) . . ?
N1 C47 H47A 108.8 . . ?
C48 C47 H47A 108.8 . . ?
N1 C47 H47B 108.8 . . ?
C48 C47 H47B 108.8 . . ?
H47A C47 H47B 107.7 . . ?
C53 C48 C49 119.2(3) . . ?
C53 C48 C47 121.8(3) . . ?
C49 C48 C47 119.0(3) . . ?
O3 C49 C48 116.8(3) . . ?
O3 C49 C50 121.7(3) . . ?
C48 C49 C50 121.5(3) . . ?
C51 C50 C49 116.3(3) . . ?
C51 C50 C54 120.9(3) . . ?
C49 C50 C54 122.8(3) . . ?
C52 C51 C50 124.2(3) . . ?
C52 C51 H51 117.9 . . ?
C50 C51 H51 117.9 . . ?
C51 C52 C53 117.0(3) . . ?
C51 C52 C58 123.4(3) . . ?
C53 C52 C58 119.6(3) . . ?
C48 C53 C52 121.7(3) . . ?
C48 C53 H53 119.1 . . ?
C52 C53 H53 119.1 . . ?
C55 C54 C50 109.6(3) . . ?
C55 C54 C57 110.9(3) . . ?
C50 C54 C57 109.6(3) . . ?
C55 C54 C56 107.3(3) . . ?
C50 C54 C56 112.3(3) . . ?
C57 C54 C56 107.2(3) . . ?
C54 C55 H55A 109.5 . . ?
C54 C55 H55B 109.5 . . ?
H55A C55 H55B 109.5 . . ?
C54 C55 H55C 109.5 . . ?
H55A C55 H55C 109.5 . . ?
H55B C55 H55C 109.5 . . ?
C54 C56 H56A 109.5 . . ?
C54 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C54 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C61 C58 C60 108.3(3) . . ?
C61 C58 C59 108.3(3) . . ?
C60 C58 C59 108.9(3) . . ?
C61 C58 C52 111.6(3) . . ?
C60 C58 C52 111.1(3) . . ?
C59 C58 C52 108.5(3) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C63 C62 C66 106.7(3) . . ?
C63 C62 C67 126.1(3) . . ?
C66 C62 C67 127.2(4) . . ?
C63 C62 Ti3 71.2(2) . . ?
C66 C62 Ti3 72.9(2) . . ?
C67 C62 Ti3 122.2(2) . . ?
C62 C63 C64 110.3(3) . . ?
C62 C63 Ti3 73.9(2) . . ?
C64 C63 Ti3 75.9(2) . . ?
C62 C63 H63 124.5 . . ?
C64 C63 H63 124.5 . . ?
Ti3 C63 H63 124.5 . . ?
C65 C64 C63 105.9(3) . . ?
C65 C64 C68 126.5(3) . . ?
C63 C64 C68 127.6(3) . . ?
C65 C64 Ti3 71.5(2) . . ?
C63 C64 Ti3 69.5(2) . . ?
C68 C64 Ti3 126.0(3) . . ?
C64 C65 C66 109.4(3) . . ?
C64 C65 Ti3 74.3(2) . . ?
C66 C65 Ti3 72.5(2) . . ?
C64 C65 H65 125.1 . . ?
C66 C65 H65 125.1 . . ?
Ti3 C65 H65 125.1 . . ?
C62 C66 C65 107.6(3) . . ?
C62 C66 C69 127.6(4) . . ?
C65 C66 C69 124.6(3) . . ?
C62 C66 Ti3 72.3(2) . . ?
C65 C66 Ti3 72.7(2) . . ?
C69 C66 Ti3 124.7(3) . . ?
C62 C67 H67A 109.5 . . ?
C62 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C62 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 C68 H68A 109.5 . . ?
C64 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C64 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C66 C69 H69A 109.5 . . ?
C66 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C66 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 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
Cl2 Ti1 O1 C3 83.5(8) . . . . ?
Cl1 Ti1 O1 C3 -171.0(8) . . . . ?
C17 Ti1 O1 C3 -75.4(8) . . . . ?
C20 Ti1 O1 C3 -15.1(8) . . . . ?
C16 Ti1 O1 C3 -46.6(8) . . . . ?
C18 Ti1 O1 C3 -69.1(9) . . . . ?
C19 Ti1 O1 C3 -14.0(9) . . . . ?
Cl3 Ti2 O2 C26 107.9(7) . . . . ?
Cl4 Ti2 O2 C26 -146.6(7) . . . . ?
C40 Ti2 O2 C26 7.6(7) . . . . ?
C39 Ti2 O2 C26 -24.7(7) . . . . ?
C42 Ti2 O2 C26 -44.1(8) . . . . ?
C43 Ti2 O2 C26 -52.7(7) . . . . ?
C41 Ti2 O2 C26 10.7(8) . . . . ?
Cl6 Ti3 O3 C49 81.8(9) . . . . ?
Cl5 Ti3 O3 C49 -172.9(9) . . . . ?
C63 Ti3 O3 C49 -19.8(9) . . . . ?
C62 Ti3 O3 C49 -52.3(9) . . . . ?
C66 Ti3 O3 C49 -80.3(9) . . . . ?
C65 Ti3 O3 C49 -71.2(10) . . . . ?
C64 Ti3 O3 C49 -14.7(10) . . . . ?
C47 N1 C1 C2 -165.2(3) . . . . ?
C24 N1 C1 C2 72.6(3) . . . . ?
N1 C1 C2 C7 22.1(4) . . . . ?
N1 C1 C2 C3 -156.8(3) . . . . ?
Ti1 O1 C3 C2 -33.3(10) . . . . ?
Ti1 O1 C3 C4 149.3(7) . . . . ?
C7 C2 C3 O1 -175.1(3) . . . . ?
C1 C2 C3 O1 3.8(4) . . . . ?
C7 C2 C3 C4 2.2(5) . . . . ?
C1 C2 C3 C4 -178.9(3) . . . . ?
O1 C3 C4 C5 174.9(3) . . . . ?
C2 C3 C4 C5 -2.4(5) . . . . ?
O1 C3 C4 C8 -0.6(5) . . . . ?
C2 C3 C4 C8 -177.9(3) . . . . ?
C3 C4 C5 C6 0.0(5) . . . . ?
C8 C4 C5 C6 175.6(3) . . . . ?
C4 C5 C6 C7 2.4(5) . . . . ?
C4 C5 C6 C12 -172.4(3) . . . . ?
C3 C2 C7 C6 0.4(5) . . . . ?
C1 C2 C7 C6 -178.5(3) . . . . ?
C5 C6 C7 C2 -2.6(5) . . . . ?
C12 C6 C7 C2 172.4(3) . . . . ?
C5 C4 C8 C10 129.4(3) . . . . ?
C3 C4 C8 C10 -55.3(4) . . . . ?
C5 C4 C8 C11 9.2(4) . . . . ?
C3 C4 C8 C11 -175.5(3) . . . . ?
C5 C4 C8 C9 -108.5(4) . . . . ?
C3 C4 C8 C9 66.8(4) . . . . ?
C5 C6 C12 C15 -133.1(3) . . . . ?
C7 C6 C12 C15 52.2(4) . . . . ?
C5 C6 C12 C13 -10.4(5) . . . . ?
C7 C6 C12 C13 174.9(3) . . . . ?
C5 C6 C12 C14 107.9(4) . . . . ?
C7 C6 C12 C14 -66.7(4) . . . . ?
C20 C16 C17 C18 -2.5(4) . . . . ?
C21 C16 C17 C18 174.7(3) . . . . ?
Ti1 C16 C17 C18 -66.9(2) . . . . ?
C20 C16 C17 Ti1 64.4(2) . . . . ?
C21 C16 C17 Ti1 -118.4(3) . . . . ?
C16 C17 C18 C19 1.5(4) . . . . ?
Ti1 C17 C18 C19 -64.3(2) . . . . ?
C16 C17 C18 C22 -175.9(3) . . . . ?
Ti1 C17 C18 C22 118.3(3) . . . . ?
C16 C17 C18 Ti1 65.8(2) . . . . ?
C17 C18 C19 C20 0.2(4) . . . . ?
C22 C18 C19 C20 177.6(3) . . . . ?
Ti1 C18 C19 C20 -61.7(2) . . . . ?
C17 C18 C19 C23 -176.8(3) . . . . ?
C22 C18 C19 C23 0.7(6) . . . . ?
Ti1 C18 C19 C23 121.4(3) . . . . ?
C17 C18 C19 Ti1 61.9(2) . . . . ?
C22 C18 C19 Ti1 -120.7(3) . . . . ?
C17 C16 C20 C19 2.6(4) . . . . ?
C21 C16 C20 C19 -174.5(3) . . . . ?
Ti1 C16 C20 C19 66.8(2) . . . . ?
C17 C16 C20 Ti1 -64.2(2) . . . . ?
C21 C16 C20 Ti1 118.7(3) . . . . ?
C18 C19 C20 C16 -1.8(4) . . . . ?
C23 C19 C20 C16 175.2(3) . . . . ?
Ti1 C19 C20 C16 -65.2(2) . . . . ?
C18 C19 C20 Ti1 63.4(2) . . . . ?
C23 C19 C20 Ti1 -119.6(3) . . . . ?
C47 N1 C24 C25 72.1(3) . . . . ?
C1 N1 C24 C25 -165.3(3) . . . . ?
N1 C24 C25 C30 25.2(4) . . . . ?
N1 C24 C25 C26 -153.3(3) . . . . ?
Ti2 O2 C26 C27 132.8(6) . . . . ?
Ti2 O2 C26 C25 -49.0(8) . . . . ?
C30 C25 C26 O2 177.5(3) . . . . ?
C24 C25 C26 O2 -4.1(5) . . . . ?
C30 C25 C26 C27 -4.3(5) . . . . ?
C24 C25 C26 C27 174.1(3) . . . . ?
O2 C26 C27 C28 -178.1(3) . . . . ?
C25 C26 C27 C28 3.7(5) . . . . ?
O2 C26 C27 C31 2.2(5) . . . . ?
C25 C26 C27 C31 -175.9(3) . . . . ?
C26 C27 C28 C29 -0.4(5) . . . . ?
C31 C27 C28 C29 179.3(3) . . . . ?
C27 C28 C29 C30 -2.3(5) . . . . ?
C27 C28 C29 C35 176.1(3) . . . . ?
C26 C25 C30 C29 1.5(5) . . . . ?
C24 C25 C30 C29 -177.0(3) . . . . ?
C28 C29 C30 C25 1.7(5) . . . . ?
C35 C29 C30 C25 -176.7(3) . . . . ?
C28 C27 C31 C33 -2.6(4) . . . . ?
C26 C27 C31 C33 177.1(3) . . . . ?
C28 C27 C31 C32 117.1(3) . . . . ?
C26 C27 C31 C32 -63.3(4) . . . . ?
C28 C27 C31 C34 -121.1(3) . . . . ?
C26 C27 C31 C34 58.5(4) . . . . ?
C28 C29 C35 C37 14.4(5) . . . . ?
C30 C29 C35 C37 -167.2(4) . . . . ?
C28 C29 C35 C38 134.8(4) . . . . ?
C30 C29 C35 C38 -46.8(4) . . . . ?
C28 C29 C35 C36 -106.2(4) . . . . ?
C30 C29 C35 C36 72.2(4) . . . . ?
C43 C39 C40 C41 3.3(4) . . . . ?
C44 C39 C40 C41 -173.4(3) . . . . ?
Ti2 C39 C40 C41 67.7(2) . . . . ?
C43 C39 C40 Ti2 -64.3(2) . . . . ?
C44 C39 C40 Ti2 118.9(3) . . . . ?
C39 C40 C41 C42 -3.9(4) . . . . ?
Ti2 C40 C41 C42 63.1(2) . . . . ?
C39 C40 C41 C45 172.7(3) . . . . ?
Ti2 C40 C41 C45 -120.3(3) . . . . ?
C39 C40 C41 Ti2 -67.0(2) . . . . ?
C40 C41 C42 C43 3.0(4) . . . . ?
C45 C41 C42 C43 -173.6(3) . . . . ?
Ti2 C41 C42 C43 64.7(2) . . . . ?
C40 C41 C42 Ti2 -61.7(2) . . . . ?
C45 C41 C42 Ti2 121.7(4) . . . . ?
C40 C39 C43 C42 -1.5(4) . . . . ?
C44 C39 C43 C42 175.3(3) . . . . ?
Ti2 C39 C43 C42 -64.3(2) . . . . ?
C40 C39 C43 C46 -177.2(3) . . . . ?
C44 C39 C43 C46 -0.4(6) . . . . ?
Ti2 C39 C43 C46 120.0(3) . . . . ?
C40 C39 C43 Ti2 62.8(2) . . . . ?
C44 C39 C43 Ti2 -120.4(3) . . . . ?
C41 C42 C43 C39 -1.0(4) . . . . ?
Ti2 C42 C43 C39 64.2(2) . . . . ?
C41 C42 C43 C46 174.8(3) . . . . ?
Ti2 C42 C43 C46 -120.0(3) . . . . ?
C41 C42 C43 Ti2 -65.2(2) . . . . ?
C24 N1 C47 C48 -154.4(3) . . . . ?
C1 N1 C47 C48 83.4(3) . . . . ?
N1 C47 C48 C53 -0.9(4) . . . . ?
N1 C47 C48 C49 176.8(3) . . . . ?
Ti3 O3 C49 C48 -28.6(11) . . . . ?
Ti3 O3 C49 C50 151.3(8) . . . . ?
C53 C48 C49 O3 179.1(3) . . . . ?
C47 C48 C49 O3 1.4(4) . . . . ?
C53 C48 C49 C50 -0.8(5) . . . . ?
C47 C48 C49 C50 -178.5(3) . . . . ?
O3 C49 C50 C51 179.1(3) . . . . ?
C48 C49 C50 C51 -1.0(5) . . . . ?
O3 C49 C50 C54 -0.1(5) . . . . ?
C48 C49 C50 C54 179.8(3) . . . . ?
C49 C50 C51 C52 1.8(5) . . . . ?
C54 C50 C51 C52 -178.9(3) . . . . ?
C50 C51 C52 C53 -0.8(5) . . . . ?
C50 C51 C52 C58 177.7(3) . . . . ?
C49 C48 C53 C52 1.9(5) . . . . ?
C47 C48 C53 C52 179.5(3) . . . . ?
C51 C52 C53 C48 -1.1(5) . . . . ?
C58 C52 C53 C48 -179.7(3) . . . . ?
C51 C50 C54 C55 -117.7(4) . . . . ?
C49 C50 C54 C55 61.4(4) . . . . ?
C51 C50 C54 C57 120.4(4) . . . . ?
C49 C50 C54 C57 -60.4(4) . . . . ?
C51 C50 C54 C56 1.4(5) . . . . ?
C49 C50 C54 C56 -179.4(3) . . . . ?
C51 C52 C58 C61 13.2(5) . . . . ?
C53 C52 C58 C61 -168.4(3) . . . . ?
C51 C52 C58 C60 134.1(4) . . . . ?
C53 C52 C58 C60 -47.4(4) . . . . ?
C51 C52 C58 C59 -106.2(4) . . . . ?
C53 C52 C58 C59 72.3(4) . . . . ?
C66 C62 C63 C64 3.0(4) . . . . ?
C67 C62 C63 C64 -175.6(3) . . . . ?
Ti3 C62 C63 C64 67.8(3) . . . . ?
C66 C62 C63 Ti3 -64.8(2) . . . . ?
C67 C62 C63 Ti3 116.6(4) . . . . ?
C62 C63 C64 C65 -3.9(4) . . . . ?
Ti3 C63 C64 C65 62.6(3) . . . . ?
C62 C63 C64 C68 173.2(4) . . . . ?
Ti3 C63 C64 C68 -120.3(4) . . . . ?
C62 C63 C64 Ti3 -66.5(3) . . . . ?
C63 C64 C65 C66 3.2(4) . . . . ?
C68 C64 C65 C66 -173.9(4) . . . . ?
Ti3 C64 C65 C66 64.5(3) . . . . ?
C63 C64 C65 Ti3 -61.3(2) . . . . ?
C68 C64 C65 Ti3 121.5(4) . . . . ?
C63 C62 C66 C65 -1.0(4) . . . . ?
C67 C62 C66 C65 177.6(3) . . . . ?
Ti3 C62 C66 C65 -64.6(3) . . . . ?
C63 C62 C66 C69 -175.8(4) . . . . ?
C67 C62 C66 C69 2.8(6) . . . . ?
Ti3 C62 C66 C69 120.6(4) . . . . ?
C63 C62 C66 Ti3 63.6(2) . . . . ?
C67 C62 C66 Ti3 -117.8(4) . . . . ?
C64 C65 C66 C62 -1.4(4) . . . . ?
Ti3 C65 C66 C62 64.3(3) . . . . ?
C64 C65 C66 C69 173.6(4) . . . . ?
Ti3 C65 C66 C69 -120.6(4) . . . . ?
C64 C65 C66 Ti3 -65.7(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti1
_database_code_depnum_ccdc_archive 'CCDC 1549581'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C42 H45 Cl6 N O3 Ti3'
_chemical_formula_moiety         'C42 H45 Cl6 N O3 Ti3'
_chemical_formula_weight         968.24
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'R -3 c:H'
_space_group_name_Hall           '-R 3 2"c'
_space_group_IT_number           167
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, z+1/2'
'x, x-y, z+1/2'
'-x+y, y, z+1/2'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'-y+2/3, -x+1/3, z+5/6'
'x+2/3, x-y+1/3, z+5/6'
'-x+y+2/3, y+1/3, z+5/6'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-y+1/3, -x+2/3, z+7/6'
'x+1/3, x-y+2/3, z+7/6'
'-x+y+1/3, y+2/3, z+7/6'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, -z-1/2'
'-x, -x+y, -z-1/2'
'x-y, -y, -z-1/2'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'y+2/3, x+1/3, -z-1/6'
'-x+2/3, -x+y+1/3, -z-1/6'
'x-y+2/3, -y+1/3, -z-1/6'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
'y+1/3, x+2/3, -z+1/6'
'-x+1/3, -x+y+2/3, -z+1/6'
'x-y+1/3, -y+2/3, -z+1/6'
#------------------------------------------------------------------------------
_cell_length_a                   16.059(2)
_cell_length_b                   16.059(2)
_cell_length_c                   63.922(6)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_volume                     14276(3)
_cell_formula_units_Z            12
_cell_measurement_reflns_used    3693
_cell_measurement_theta_min      1.94
_cell_measurement_theta_max      29.87
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.160
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             5952.00
_exptl_absorpt_coefficient_mu    0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.471
_exptl_absorpt_correction_T_max  0.871

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            47281
_diffrn_reflns_av_R_equivalents  0.1014
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         2.537
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -82
_diffrn_reflns_limit_l_max       82
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             3657
_reflns_number_gt                2694
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt)., SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0982
_refine_ls_wR_factor_ref         0.2220
_refine_ls_wR_factor_gt          0.2086
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         3657
_refine_ls_number_parameters     166
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0449P)²+338.0268P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.61
_refine_diff_density_min         -1.14
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.10567(9) 0.39766(9) 0.46057(2) 0.0400(3) Uani 1 1 d . . . . .
Cl1 Cl 0.05200(17) 0.24779(17) 0.44836(3) 0.0657(6) Uani 1 1 d . . . . .
Cl2 Cl 0.24579(14) 0.48561(18) 0.44358(2) 0.0634(6) Uani 1 1 d . . . . .
O1 O 0.1440(3) 0.3950(3) 0.48670(5) 0.0387(10) Uani 1 1 d . . . . .
N1 N 0.3333 0.6667 0.51144(11) 0.0303(18) Uani 1 3 d S T P . .
C1 C 0.2969(5) 0.5680(4) 0.50426(8) 0.0355(14) Uani 1 1 d . . . . .
H1A H 0.3489 0.5520 0.5054 0.043 Uiso 1 1 calc R U . . .
H1B H 0.2788 0.5634 0.4893 0.043 Uiso 1 1 calc R U . . .
C2 C 0.2109(5) 0.4955(4) 0.51663(8) 0.0345(13) Uani 1 1 d . . . . .
C3 C 0.1397(5) 0.4092(5) 0.50783(8) 0.0366(14) Uani 1 1 d . . . . .
C4 C 0.0659(5) 0.3379(5) 0.51960(9) 0.0412(15) Uani 1 1 d . . . . .
C5 C 0.0618(5) 0.3545(5) 0.54089(9) 0.0409(15) Uani 1 1 d . . . . .
H5 H 0.0118 0.3064 0.5492 0.049 Uiso 1 1 calc R U . . .
C6 C 0.1293(5) 0.4399(4) 0.55009(8) 0.0355(13) Uani 1 1 d . . . . .
C7 C 0.2032(5) 0.5098(4) 0.53813(8) 0.0340(13) Uani 1 1 d . . . . .
H7 H 0.2494 0.5683 0.5445 0.041 Uiso 1 1 calc R U . . .
C8 C 0.1255(6) 0.4572(5) 0.57326(8) 0.0477(17) Uani 1 1 d . . . . .
H8A H 0.1786 0.5210 0.5770 0.057 Uiso 1 1 calc R U . . .
H8B H 0.0641 0.4535 0.5766 0.057 Uiso 1 1 calc R U . . .
H8C H 0.1312 0.4082 0.5812 0.057 Uiso 1 1 calc R U . . .
C9 C -0.0074(6) 0.2437(6) 0.50973(11) 0.0570(19) Uani 1 1 d . . . . .
H9A H -0.0536 0.2025 0.5204 0.068 Uiso 1 1 calc R U . . .
H9B H -0.0414 0.2562 0.4985 0.068 Uiso 1 1 calc R U . . .
H9C H 0.0254 0.2113 0.5039 0.068 Uiso 1 1 calc R U . . .
C10 C -0.0035(5) 0.4343(5) 0.47604(9) 0.0436(16) Uani 1 1 d . . . . .
H10 H -0.0194 0.4287 0.4913 0.052 Uiso 1 1 calc R U . . .
C11 C -0.0537(5) 0.3632(6) 0.46098(10) 0.0513(18) Uani 1 1 d . . . . .
H11 H -0.1119 0.2988 0.4634 0.062 Uiso 1 1 calc R U . . .
C12 C -0.0150(5) 0.4056(6) 0.44122(9) 0.054(2) Uani 1 1 d . . . . .
H12 H -0.0403 0.3748 0.4273 0.064 Uiso 1 1 calc R U . . .
C13 C 0.0583(5) 0.4992(6) 0.44436(10) 0.0480(17) Uani 1 1 d . . . . .
H13 H 0.0945 0.5470 0.4331 0.058 Uiso 1 1 calc R U . . .
C14 C 0.0674(5) 0.5182(5) 0.46590(9) 0.0439(16) Uani 1 1 d . . . . .
H14 H 0.1096 0.5820 0.4726 0.053 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.788(4) . ?
Ti1 Cl2 2.249(2) . ?
Ti1 Cl1 2.252(2) . ?
Ti1 C10 2.330(6) . ?
Ti1 C14 2.330(7) . ?
Ti1 C11 2.333(7) . ?
Ti1 C12 2.356(7) . ?
Ti1 C13 2.356(7) . ?
O1 C3 1.377(6) . ?
N1 C1 1.462(6) 3_565 ?
N1 C1 1.462(6) . ?
N1 C1 1.462(6) 2_665 ?
C1 C2 1.510(8) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.400(9) . ?
C2 C7 1.409(7) . ?
C3 C4 1.387(9) . ?
C4 C5 1.395(8) . ?
C4 C9 1.514(10) . ?
C5 C6 1.384(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.385(8) . ?
C6 C8 1.514(7) . ?
C7 H7 0.9500 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 C11 1.400(9) . ?
C10 C14 1.414(10) . ?
C10 H10 1.0000 . ?
C11 C12 1.422(10) . ?
C11 H11 1.0000 . ?
C12 C13 1.384(11) . ?
C12 H12 1.0000 . ?
C13 C14 1.402(8) . ?
C13 H13 1.0000 . ?
C14 H14 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 Cl2 102.58(16) . . ?
O1 Ti1 Cl1 104.50(16) . . ?
Cl2 Ti1 Cl1 103.41(9) . . ?
O1 Ti1 C10 85.5(2) . . ?
Cl2 Ti1 C10 133.6(2) . . ?
Cl1 Ti1 C10 118.9(2) . . ?
O1 Ti1 C14 96.9(2) . . ?
Cl2 Ti1 C14 98.4(2) . . ?
Cl1 Ti1 C14 145.0(2) . . ?
C10 Ti1 C14 35.3(2) . . ?
O1 Ti1 C11 109.5(2) . . ?
Cl2 Ti1 C11 142.1(2) . . ?
Cl1 Ti1 C11 87.8(2) . . ?
C10 Ti1 C11 34.9(2) . . ?
C14 Ti1 C11 58.8(3) . . ?
O1 Ti1 C12 142.6(2) . . ?
Cl2 Ti1 C12 107.7(2) . . ?
Cl1 Ti1 C12 89.5(2) . . ?
C10 Ti1 C12 57.7(2) . . ?
C14 Ti1 C12 57.7(2) . . ?
C11 Ti1 C12 35.3(2) . . ?
O1 Ti1 C13 131.4(2) . . ?
Cl2 Ti1 C13 85.5(2) . . ?
Cl1 Ti1 C13 120.24(19) . . ?
C10 Ti1 C13 57.8(2) . . ?
C14 Ti1 C13 34.8(2) . . ?
C11 Ti1 C13 58.2(3) . . ?
C12 Ti1 C13 34.1(3) . . ?
C3 O1 Ti1 149.9(4) . . ?
C1 N1 C1 110.6(3) 3_565 . ?
C1 N1 C1 110.6(3) 3_565 2_665 ?
C1 N1 C1 110.6(3) . 2_665 ?
N1 C1 C2 112.8(5) . . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1A 109.0 . . ?
N1 C1 H1B 109.0 . . ?
C2 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C3 C2 C7 117.3(5) . . ?
C3 C2 C1 122.2(5) . . ?
C7 C2 C1 120.4(5) . . ?
O1 C3 C4 119.2(6) . . ?
O1 C3 C2 118.3(5) . . ?
C4 C3 C2 122.5(5) . . ?
C3 C4 C5 118.3(6) . . ?
C3 C4 C9 121.0(5) . . ?
C5 C4 C9 120.6(6) . . ?
C6 C5 C4 121.0(6) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C5 C6 C7 119.8(5) . . ?
C5 C6 C8 120.9(6) . . ?
C7 C6 C8 119.2(6) . . ?
C6 C7 C2 121.0(6) . . ?
C6 C7 H7 119.5 . . ?
C2 C7 H7 119.5 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C14 108.8(5) . . ?
C11 C10 Ti1 72.6(4) . . ?
C14 C10 Ti1 72.3(4) . . ?
C11 C10 H10 125.5 . . ?
C14 C10 H10 125.5 . . ?
Ti1 C10 H10 125.5 . . ?
C10 C11 C12 106.5(7) . . ?
C10 C11 Ti1 72.4(4) . . ?
C12 C11 Ti1 73.2(4) . . ?
C10 C11 H11 126.4 . . ?
C12 C11 H11 126.4 . . ?
Ti1 C11 H11 126.4 . . ?
C13 C12 C11 108.8(6) . . ?
C13 C12 Ti1 72.9(4) . . ?
C11 C12 Ti1 71.5(4) . . ?
C13 C12 H12 125.5 . . ?
C11 C12 H12 125.5 . . ?
Ti1 C12 H12 125.5 . . ?
C12 C13 C14 108.6(6) . . ?
C12 C13 Ti1 72.9(4) . . ?
C14 C13 Ti1 71.6(4) . . ?
C12 C13 H13 125.6 . . ?
C14 C13 H13 125.6 . . ?
Ti1 C13 H13 125.6 . . ?
C13 C14 C10 107.2(6) . . ?
C13 C14 Ti1 73.6(4) . . ?
C10 C14 Ti1 72.3(4) . . ?
C13 C14 H14 126.1 . . ?
C10 C14 H14 126.1 . . ?
Ti1 C14 H14 126.1 . . ?

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
Cl2 Ti1 O1 C3 127.6(8) . . . . ?
Cl1 Ti1 O1 C3 -124.7(8) . . . . ?
C10 Ti1 O1 C3 -6.1(9) . . . . ?
C14 Ti1 O1 C3 27.4(9) . . . . ?
C11 Ti1 O1 C3 -31.8(9) . . . . ?
C12 Ti1 O1 C3 -15.9(11) . . . . ?
C13 Ti1 O1 C3 32.5(10) . . . . ?
C1 N1 C1 C2 -76.0(8) 3_565 . . . ?
C1 N1 C1 C2 161.1(5) 2_665 . . . ?
N1 C1 C2 C3 150.4(6) . . . . ?
N1 C1 C2 C7 -34.0(8) . . . . ?
Ti1 O1 C3 C4 82.4(10) . . . . ?
Ti1 O1 C3 C2 -98.1(9) . . . . ?
C7 C2 C3 O1 177.9(5) . . . . ?
C1 C2 C3 O1 -6.3(9) . . . . ?
C7 C2 C3 C4 -2.6(10) . . . . ?
C1 C2 C3 C4 173.2(6) . . . . ?
O1 C3 C4 C5 -178.8(6) . . . . ?
C2 C3 C4 C5 1.7(10) . . . . ?
O1 C3 C4 C9 2.3(10) . . . . ?
C2 C3 C4 C9 -177.2(7) . . . . ?
C3 C4 C5 C6 0.1(10) . . . . ?
C9 C4 C5 C6 179.0(7) . . . . ?
C4 C5 C6 C7 -1.0(10) . . . . ?
C4 C5 C6 C8 -179.1(6) . . . . ?
C5 C6 C7 C2 0.1(10) . . . . ?
C8 C6 C7 C2 178.2(6) . . . . ?
C3 C2 C7 C6 1.7(9) . . . . ?
C1 C2 C7 C6 -174.2(6) . . . . ?
C14 C10 C11 C12 -2.1(8) . . . . ?
Ti1 C10 C11 C12 -65.8(5) . . . . ?
C14 C10 C11 Ti1 63.7(5) . . . . ?
C10 C11 C12 C13 1.4(8) . . . . ?
Ti1 C11 C12 C13 -63.8(5) . . . . ?
C10 C11 C12 Ti1 65.3(5) . . . . ?
C11 C12 C13 C14 -0.2(8) . . . . ?
Ti1 C12 C13 C14 -63.1(5) . . . . ?
C11 C12 C13 Ti1 62.9(5) . . . . ?
C12 C13 C14 C10 -1.0(8) . . . . ?
Ti1 C13 C14 C10 -65.0(5) . . . . ?
C12 C13 C14 Ti1 64.0(5) . . . . ?
C11 C10 C14 C13 1.9(8) . . . . ?
Ti1 C10 C14 C13 65.9(5) . . . . ?
C11 C10 C14 Ti1 -63.9(5) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 219.0 37.5
2 0.000 0.000 0.250 6.9 2.1
3 0.000 0.000 0.500 219.0 38.2
4 0.000 0.000 0.750 6.9 1.5
5 0.333 0.667 0.167 221.1 38.0
6 0.333 0.667 0.667 221.1 37.4
7 0.333 0.667 0.417 7.1 1.6
8 0.333 0.667 0.917 7.1 2.2
9 0.667 0.333 0.333 221.2 37.4
10 0.667 0.333 0.833 221.1 38.1
11 0.667 0.333 0.083 7.1 1.6
12 0.667 0.333 0.583 7.1 2.2
_platon_squeeze_details          
; ?
;


#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti4
_database_code_depnum_ccdc_archive 'CCDC 1549584'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C60 H81 Cl6 N O3 Ti3'
_chemical_formula_moiety         'C60 H81 Cl6 N O3 Ti3'
_chemical_formula_weight         1220.72
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      trigonal
_space_group_name_H-M_alt        'R -3:H'
_space_group_name_Hall           '-R 3'
_space_group_IT_number           148
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
#------------------------------------------------------------------------------
_cell_length_a                   24.4075(13)
_cell_length_b                   24.4075(13)
_cell_length_c                   23.4369(16)
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                120.0000
_cell_volume                     12091.4(12)
_cell_formula_units_Z            6
_cell_measurement_reflns_used    3919
_cell_measurement_theta_min      1.98
_cell_measurement_theta_max      31.78
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.070
_exptl_crystal_density_diffrn    1.006
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3840.00
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.952
_exptl_absorpt_correction_T_max  0.964

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            43023
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.595
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             6172
_reflns_number_gt                3304
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt)., SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1434
_refine_ls_R_factor_gt           0.0750
_refine_ls_wR_factor_ref         0.2317
_refine_ls_wR_factor_gt          0.1975
_refine_ls_number_restraints     25
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         6172
_refine_ls_number_parameters     220
_refine_ls_goodness_of_fit_ref   0.984
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1174P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.87
_refine_diff_density_min         -0.35
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.54550(4) 0.44272(4) 0.76933(3) 0.0382(3) Uani 1 1 d . . . . .
Cl1 Cl 0.45778(6) 0.43734(6) 0.80772(6) 0.0556(4) Uani 1 1 d . . . . .
Cl2 Cl 0.59093(5) 0.42821(5) 0.84628(5) 0.0477(3) Uani 1 1 d . . . . .
O1 O 0.51675(12) 0.37056(13) 0.73144(12) 0.0358(7) Uani 1 1 d . . . . .
N1 N 0.6667 0.3333 0.6982(2) 0.0306(12) Uani 1 3 d S T P . .
C1 C 0.61930(18) 0.35015(18) 0.71563(17) 0.0315(9) Uani 1 1 d . . . . .
H1A H 0.6391 0.3968 0.7164 0.038 Uiso 1 1 calc R U . . .
H1B H 0.6047 0.3343 0.7548 0.038 Uiso 1 1 calc R U . . .
C2 C 0.56262(18) 0.32284(19) 0.67578(17) 0.0343(9) Uani 1 1 d . . . . .
C3 C 0.51099(19) 0.33084(19) 0.68685(17) 0.0354(9) Uani 1 1 d . . . . .
C4 C 0.4547(2) 0.2989(2) 0.65483(18) 0.0433(11) Uani 1 1 d . . . . .
C5 C 0.4556(2) 0.2650(2) 0.6076(2) 0.0472(11) Uani 1 1 d . . . . .
H5 H 0.4189 0.2445 0.5843 0.057 Uiso 1 1 calc R U . . .
C6 C 0.5086(2) 0.2600(2) 0.59288(18) 0.0420(11) Uani 1 1 d . . . . .
C7 C 0.56014(19) 0.28755(19) 0.62785(17) 0.0345(9) Uani 1 1 d . . . . .
H7 H 0.5955 0.2826 0.6194 0.041 Uiso 1 1 calc R U . . .
C8 C 0.5069(2) 0.2235(2) 0.5385(2) 0.0506(12) Uani 1 1 d . . . . .
C9 C 0.5673(3) 0.2238(4) 0.5285(3) 0.100(3) Uani 1 1 d . . . . .
H9A H 0.6026 0.2675 0.5287 0.119 Uiso 1 1 calc R U . . .
H9B H 0.5736 0.1997 0.5587 0.119 Uiso 1 1 calc R U . . .
H9C H 0.5656 0.2044 0.4914 0.119 Uiso 1 1 calc R U . . .
C10 C 0.4506(3) 0.1587(3) 0.5388(3) 0.102(3) Uani 1 1 d . . . . .
H10A H 0.4124 0.1614 0.5455 0.122 Uiso 1 1 calc R U . . .
H10B H 0.4472 0.1383 0.5019 0.122 Uiso 1 1 calc R U . . .
H10C H 0.4552 0.1337 0.5692 0.122 Uiso 1 1 calc R U . . .
C11 C 0.4980(4) 0.2586(4) 0.4867(3) 0.094(2) Uani 1 1 d . . . . .
H11A H 0.5340 0.3018 0.4846 0.113 Uiso 1 1 calc R U . . .
H11B H 0.4954 0.2360 0.4514 0.113 Uiso 1 1 calc R U . . .
H11C H 0.4589 0.2601 0.4917 0.113 Uiso 1 1 calc R U . . .
C12 C 0.3948(2) 0.3014(3) 0.6710(2) 0.0582(14) Uani 1 1 d . . . . .
C13 C 0.3777(2) 0.2821(3) 0.7337(2) 0.0569(13) Uani 1 1 d . . . . .
H13A H 0.4128 0.3111 0.7582 0.068 Uiso 1 1 calc R U . . .
H13B H 0.3397 0.2840 0.7438 0.068 Uiso 1 1 calc R U . . .
H13C H 0.3696 0.2388 0.7392 0.068 Uiso 1 1 calc R U . . .
C14 C 0.4040(3) 0.3681(3) 0.6603(3) 0.0745(18) Uani 1 1 d . . . . .
H14A H 0.4399 0.3994 0.6829 0.089 Uiso 1 1 calc R U . . .
H14B H 0.4123 0.3786 0.6197 0.089 Uiso 1 1 calc R U . . .
H14C H 0.3656 0.3687 0.6715 0.089 Uiso 1 1 calc R U . . .
C15 C 0.3382(3) 0.2545(4) 0.6349(3) 0.093(2) Uani 1 1 d . . . . .
H15A H 0.3475 0.2654 0.5944 0.112 Uiso 1 1 calc R U . . .
H15B H 0.3305 0.2116 0.6412 0.112 Uiso 1 1 calc R U . . .
H15C H 0.3006 0.2567 0.6458 0.112 Uiso 1 1 calc R U . . .
C16 C 0.6027(5) 0.4954(3) 0.6877(4) 0.099(2) Uani 1 1 d . U . . .
H16 H 0.6056 0.4732 0.6530 0.119 Uiso 1 1 calc R U . . .
C17 C 0.6412(3) 0.5132(3) 0.7267(4) 0.082(2) Uani 1 1 d . . . . .
H17 H 0.6798 0.5088 0.7272 0.098 Uiso 1 1 calc R U . . .
C18 C 0.6279(4) 0.5476(3) 0.7669(3) 0.094(2) Uani 1 1 d . U . . .
H18 H 0.6550 0.5741 0.7991 0.113 Uiso 1 1 calc R U . . .
C19 C 0.5717(4) 0.5451(3) 0.7436(4) 0.098(3) Uani 1 1 d . U . . .
H19 H 0.5510 0.5695 0.7562 0.118 Uiso 1 1 calc R U . . .
C20 C 0.5617(4) 0.5115(4) 0.6941(4) 0.096(3) Uani 1 1 d . U . . .
H20 H 0.5290 0.5048 0.6650 0.115 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.774(3) . ?
Ti1 Cl2 2.2362(14) . ?
Ti1 Cl1 2.2647(14) . ?
Ti1 C17 2.323(6) . ?
Ti1 C20 2.328(6) . ?
Ti1 C19 2.328(6) . ?
Ti1 C18 2.336(5) . ?
Ti1 C16 2.339(7) . ?
O1 C3 1.384(5) . ?
N1 C1 1.465(4) 2_655 ?
N1 C1 1.465(4) 3_665 ?
N1 C1 1.465(4) . ?
C1 C2 1.519(5) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.393(6) . ?
C2 C7 1.398(6) . ?
C3 C4 1.410(6) . ?
C4 C5 1.388(6) . ?
C4 C12 1.542(6) . ?
C5 C6 1.402(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.364(6) . ?
C6 C8 1.545(6) . ?
C7 H7 0.9500 . ?
C8 C10 1.488(8) . ?
C8 C9 1.489(7) . ?
C8 C11 1.563(8) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.534(7) . ?
C12 C13 1.536(7) . ?
C12 C14 1.551(8) . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C17 1.223(10) . ?
C16 C20 1.254(11) . ?
C16 H16 1.0000 . ?
C17 C18 1.403(10) . ?
C17 H17 1.0000 . ?
C18 C19 1.449(10) . ?
C18 H18 1.0000 . ?
C19 C20 1.370(11) . ?
C19 H19 1.0000 . ?
C20 H20 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 Cl2 103.16(10) . . ?
O1 Ti1 Cl1 104.37(10) . . ?
Cl2 Ti1 Cl1 101.52(6) . . ?
O1 Ti1 C17 105.8(2) . . ?
Cl2 Ti1 C17 94.0(2) . . ?
Cl1 Ti1 C17 141.72(17) . . ?
O1 Ti1 C20 100.2(3) . . ?
Cl2 Ti1 C20 143.72(18) . . ?
Cl1 Ti1 C20 99.1(3) . . ?
C17 Ti1 C20 52.7(2) . . ?
O1 Ti1 C19 134.1(3) . . ?
Cl2 Ti1 C19 119.1(3) . . ?
Cl1 Ti1 C19 84.83(16) . . ?
C17 Ti1 C19 57.2(2) . . ?
C20 Ti1 C19 34.2(3) . . ?
O1 Ti1 C18 140.6(2) . . ?
Cl2 Ti1 C18 88.27(18) . . ?
Cl1 Ti1 C18 110.2(3) . . ?
C17 Ti1 C18 35.0(3) . . ?
C20 Ti1 C18 56.5(2) . . ?
C19 Ti1 C18 36.2(3) . . ?
O1 Ti1 C16 88.1(2) . . ?
Cl2 Ti1 C16 122.7(3) . . ?
Cl1 Ti1 C16 130.1(3) . . ?
C17 Ti1 C16 30.4(2) . . ?
C20 Ti1 C16 31.2(3) . . ?
C19 Ti1 C16 55.2(3) . . ?
C18 Ti1 C16 55.0(3) . . ?
C3 O1 Ti1 157.6(3) . . ?
C1 N1 C1 112.6(2) 2_655 3_665 ?
C1 N1 C1 112.6(2) 2_655 . ?
C1 N1 C1 112.6(2) 3_665 . ?
N1 C1 C2 112.3(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C7 118.2(4) . . ?
C3 C2 C1 120.9(4) . . ?
C7 C2 C1 120.9(3) . . ?
O1 C3 C2 117.2(4) . . ?
O1 C3 C4 121.3(4) . . ?
C2 C3 C4 121.5(4) . . ?
C5 C4 C3 116.9(4) . . ?
C5 C4 C12 121.2(4) . . ?
C3 C4 C12 121.9(4) . . ?
C4 C5 C6 122.6(4) . . ?
C4 C5 H5 118.7 . . ?
C6 C5 H5 118.7 . . ?
C7 C6 C5 118.2(4) . . ?
C7 C6 C8 122.1(4) . . ?
C5 C6 C8 119.6(4) . . ?
C6 C7 C2 122.1(4) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
C10 C8 C9 113.1(5) . . ?
C10 C8 C6 110.7(4) . . ?
C9 C8 C6 112.8(4) . . ?
C10 C8 C11 106.2(5) . . ?
C9 C8 C11 106.5(5) . . ?
C6 C8 C11 107.1(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C12 C13 107.2(5) . . ?
C15 C12 C4 110.6(4) . . ?
C13 C12 C4 110.0(4) . . ?
C15 C12 C14 107.3(5) . . ?
C13 C12 C14 110.6(4) . . ?
C4 C12 C14 111.0(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17 C16 C20 113.0(8) . . ?
C17 C16 Ti1 74.1(4) . . ?
C20 C16 Ti1 73.9(5) . . ?
C17 C16 H16 123.4 . . ?
C20 C16 H16 123.4 . . ?
Ti1 C16 H16 123.4 . . ?
C16 C17 C18 110.4(7) . . ?
C16 C17 Ti1 75.5(4) . . ?
C18 C17 Ti1 73.0(3) . . ?
C16 C17 H17 124.6 . . ?
C18 C17 H17 124.6 . . ?
Ti1 C17 H17 124.6 . . ?
C17 C18 C19 102.6(6) . . ?
C17 C18 Ti1 72.0(3) . . ?
C19 C18 Ti1 71.6(3) . . ?
C17 C18 H18 128.2 . . ?
C19 C18 H18 128.2 . . ?
Ti1 C18 H18 128.2 . . ?
C20 C19 C18 103.1(6) . . ?
C20 C19 Ti1 72.9(4) . . ?
C18 C19 Ti1 72.2(3) . . ?
C20 C19 H19 127.9 . . ?
C18 C19 H19 127.9 . . ?
Ti1 C19 H19 127.9 . . ?
C16 C20 C19 110.9(7) . . ?
C16 C20 Ti1 74.9(4) . . ?
C19 C20 Ti1 72.9(4) . . ?
C16 C20 H20 124.4 . . ?
C19 C20 H20 124.4 . . ?
Ti1 C20 H20 124.4 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl2 Ti1 O1 C3 -117.6(6) . . . . ?
Cl1 Ti1 O1 C3 136.6(6) . . . . ?
C17 Ti1 O1 C3 -19.5(7) . . . . ?
C20 Ti1 O1 C3 34.4(7) . . . . ?
C19 Ti1 O1 C3 39.8(7) . . . . ?
C18 Ti1 O1 C3 -14.0(8) . . . . ?
C16 Ti1 O1 C3 5.5(7) . . . . ?
C1 N1 C1 C2 -79.9(6) 2_655 . . . ?
C1 N1 C1 C2 151.6(4) 3_665 . . . ?
N1 C1 C2 C3 176.6(4) . . . . ?
N1 C1 C2 C7 -1.6(5) . . . . ?
Ti1 O1 C3 C2 68.1(8) . . . . ?
Ti1 O1 C3 C4 -113.2(6) . . . . ?
C7 C2 C3 O1 -174.3(3) . . . . ?
C1 C2 C3 O1 7.4(6) . . . . ?
C7 C2 C3 C4 6.9(6) . . . . ?
C1 C2 C3 C4 -171.4(4) . . . . ?
O1 C3 C4 C5 173.9(4) . . . . ?
C2 C3 C4 C5 -7.4(7) . . . . ?
O1 C3 C4 C12 -5.9(7) . . . . ?
C2 C3 C4 C12 172.8(4) . . . . ?
C3 C4 C5 C6 2.5(7) . . . . ?
C12 C4 C5 C6 -177.6(5) . . . . ?
C4 C5 C6 C7 2.6(7) . . . . ?
C4 C5 C6 C8 -177.8(5) . . . . ?
C5 C6 C7 C2 -3.2(6) . . . . ?
C8 C6 C7 C2 177.3(4) . . . . ?
C3 C2 C7 C6 -1.5(6) . . . . ?
C1 C2 C7 C6 176.8(4) . . . . ?
C7 C6 C8 C10 126.1(6) . . . . ?
C5 C6 C8 C10 -53.4(7) . . . . ?
C7 C6 C8 C9 -1.6(7) . . . . ?
C5 C6 C8 C9 178.8(5) . . . . ?
C7 C6 C8 C11 -118.5(5) . . . . ?
C5 C6 C8 C11 61.9(6) . . . . ?
C5 C4 C12 C15 9.0(7) . . . . ?
C3 C4 C12 C15 -171.2(5) . . . . ?
C5 C4 C12 C13 127.2(5) . . . . ?
C3 C4 C12 C13 -53.0(6) . . . . ?
C5 C4 C12 C14 -110.0(5) . . . . ?
C3 C4 C12 C14 69.8(6) . . . . ?
C20 C16 C17 C18 -1.0(9) . . . . ?
Ti1 C16 C17 C18 -65.3(4) . . . . ?
C20 C16 C17 Ti1 64.3(6) . . . . ?
C16 C17 C18 C19 1.2(7) . . . . ?
Ti1 C17 C18 C19 -65.6(4) . . . . ?
C16 C17 C18 Ti1 66.9(5) . . . . ?
C17 C18 C19 C20 -1.0(6) . . . . ?
Ti1 C18 C19 C20 -66.9(4) . . . . ?
C17 C18 C19 Ti1 65.9(4) . . . . ?
C17 C16 C20 C19 0.2(10) . . . . ?
Ti1 C16 C20 C19 64.6(5) . . . . ?
C17 C16 C20 Ti1 -64.4(6) . . . . ?
C18 C19 C20 C16 0.6(8) . . . . ?
Ti1 C19 C20 C16 -65.8(6) . . . . ?
C18 C19 C20 Ti1 66.4(4) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.005 -0.003 -0.008 4032.3 376.1
_platon_squeeze_details          
; ?
;

#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti9
_database_code_depnum_ccdc_archive 'CCDC 1549587'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C81 H129 N O3 Ti3'
_chemical_formula_moiety         'C81 H129 N O3 Ti3'
_chemical_formula_weight         1308.62
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   19.9129(4)
_cell_length_b                   19.9654(3)
_cell_length_c                   20.1690(4)
_cell_angle_alpha                90.0000
_cell_angle_beta                 98.7979(19)
_cell_angle_gamma                90.0000
_cell_volume                     7924.2(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    27521
_cell_measurement_theta_min      2.31
_cell_measurement_theta_max      30.33
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.108
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.046
_exptl_crystal_density_diffrn    1.097
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2848.00
_exptl_absorpt_coefficient_mu    0.339
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.892
_exptl_absorpt_correction_T_max  0.985

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB P200'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 5.811
_diffrn_reflns_number            65232
_diffrn_reflns_av_R_equivalents  0.0458
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measured_fraction_theta_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             17594
_reflns_number_gt                13851
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;
    Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt).
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0738
_refine_ls_R_factor_gt           0.0579
_refine_ls_wR_factor_ref         0.1774
_refine_ls_wR_factor_gt          0.1664
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    mixed
_refine_ls_number_reflns         17594
_refine_ls_number_parameters     805
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.0987P)²+9.4361P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         0.70
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.51189(2) 0.53696(2) 0.80883(2) 0.01835(10) Uani 1 1 d . . . . .
Ti2 Ti 0.38246(2) 0.74257(2) 0.52058(2) 0.02402(11) Uani 1 1 d . . . . .
Ti3 Ti 0.23200(2) 0.78453(2) 0.84358(2) 0.02708(12) Uani 1 1 d . . . . .
O1 O 0.56716(8) 0.59880(7) 0.77837(8) 0.0181(3) Uani 1 1 d . . . . .
O2 O 0.38485(8) 0.82087(8) 0.56738(8) 0.0215(3) Uani 1 1 d . . . . .
O3 O 0.31436(9) 0.79177(9) 0.89587(8) 0.0240(4) Uani 1 1 d . . . . .
N1 N 0.46332(10) 0.78258(9) 0.76986(9) 0.0176(4) Uani 1 1 d . . . . .
C1 C 0.49686(11) 0.71843(11) 0.78711(12) 0.0185(4) Uani 1 1 d . . . . .
H1A H 0.4697 0.6821 0.7627 0.022 Uiso 1 1 calc R U . . .
H1B H 0.4989 0.7102 0.8358 0.022 Uiso 1 1 calc R U . . .
C2 C 0.56817(11) 0.71698(11) 0.76961(11) 0.0166(4) Uani 1 1 d . . . . .
C3 C 0.60027(12) 0.77616(11) 0.75657(11) 0.0183(4) Uani 1 1 d . . . . .
H3 H 0.5773 0.8175 0.7596 0.022 Uiso 1 1 calc R U . . .
C4 C 0.66531(12) 0.77651(11) 0.73918(11) 0.0188(4) Uani 1 1 d . . . . .
C5 C 0.69755(12) 0.71491(11) 0.73597(11) 0.0193(4) Uani 1 1 d . . . . .
H5 H 0.7420 0.7144 0.7243 0.023 Uiso 1 1 calc R U . . .
C6 C 0.66790(11) 0.65357(11) 0.74903(11) 0.0175(4) Uani 1 1 d . . . . .
C7 C 0.60183(11) 0.65562(10) 0.76621(11) 0.0163(4) Uani 1 1 d . . . . .
C8 C 0.70527(12) 0.58741(11) 0.74233(12) 0.0200(5) Uani 1 1 d . . . . .
C9 C 0.66657(14) 0.54737(12) 0.68303(13) 0.0270(5) Uani 1 1 d . . . . .
H9A H 0.6901 0.5049 0.6783 0.032 Uiso 1 1 calc R U . . .
H9B H 0.6203 0.5383 0.6915 0.032 Uiso 1 1 calc R U . . .
H9C H 0.6648 0.5735 0.6417 0.032 Uiso 1 1 calc R U . . .
C10 C 0.71094(13) 0.54745(12) 0.80823(13) 0.0258(5) Uani 1 1 d . . . . .
H10A H 0.7349 0.5053 0.8035 0.031 Uiso 1 1 calc R U . . .
H10B H 0.7362 0.5738 0.8448 0.031 Uiso 1 1 calc R U . . .
H10C H 0.6653 0.5379 0.8184 0.031 Uiso 1 1 calc R U . . .
C11 C 0.77812(13) 0.59833(12) 0.72830(15) 0.0289(6) Uani 1 1 d . . . . .
H11A H 0.8000 0.5548 0.7244 0.035 Uiso 1 1 calc R U . . .
H11B H 0.7770 0.6233 0.6863 0.035 Uiso 1 1 calc R U . . .
H11C H 0.8039 0.6238 0.7652 0.035 Uiso 1 1 calc R U . . .
C12 C 0.69744(12) 0.84386(11) 0.72412(12) 0.0225(5) Uani 1 1 d . . . . .
C13 C 0.65517(16) 0.87582(14) 0.66235(15) 0.0378(7) Uani 1 1 d . . . . .
H13A H 0.6081 0.8810 0.6702 0.045 Uiso 1 1 calc R U . . .
H13B H 0.6740 0.9199 0.6542 0.045 Uiso 1 1 calc R U . . .
H13C H 0.6564 0.8471 0.6232 0.045 Uiso 1 1 calc R U . . .
C14 C 0.69725(15) 0.89052(13) 0.78468(14) 0.0316(6) Uani 1 1 d . . . . .
H14A H 0.6506 0.8961 0.7937 0.038 Uiso 1 1 calc R U . . .
H14B H 0.7253 0.8710 0.8241 0.038 Uiso 1 1 calc R U . . .
H14C H 0.7158 0.9343 0.7749 0.038 Uiso 1 1 calc R U . . .
C15 C 0.77069(14) 0.83611(13) 0.71128(15) 0.0317(6) Uani 1 1 d . . . . .
H15A H 0.7981 0.8157 0.7506 0.038 Uiso 1 1 calc R U . . .
H15B H 0.7716 0.8074 0.6720 0.038 Uiso 1 1 calc R U . . .
H15C H 0.7893 0.8802 0.7030 0.038 Uiso 1 1 calc R U . . .
C16 C 0.41694(13) 0.54836(13) 0.74587(13) 0.0282(5) Uani 1 1 d . . . . .
H16A H 0.3842 0.5164 0.7594 0.034 Uiso 1 1 calc R U . . .
H16B H 0.4002 0.5941 0.7500 0.034 Uiso 1 1 calc R U . . .
H16C H 0.4226 0.5399 0.6992 0.034 Uiso 1 1 calc R U . . .
C17 C 0.53980(14) 0.44702(12) 0.76293(13) 0.0288(5) Uani 1 1 d . . . . .
H17A H 0.5127 0.4097 0.7761 0.035 Uiso 1 1 calc R U . . .
H17B H 0.5313 0.4521 0.7140 0.035 Uiso 1 1 calc R U . . .
H17C H 0.5882 0.4380 0.7776 0.035 Uiso 1 1 calc R U . . .
C18 C 0.54111(13) 0.56763(12) 0.92306(12) 0.0242(5) Uani 1 1 d . . . . .
C19 C 0.46942(13) 0.57327(12) 0.90735(12) 0.0250(5) Uani 1 1 d . . . . .
C20 C 0.44202(13) 0.50791(12) 0.89187(12) 0.0249(5) Uani 1 1 d . . . . .
C21 C 0.49687(13) 0.46216(11) 0.89926(12) 0.0233(5) Uani 1 1 d . . . . .
C22 C 0.55811(13) 0.49878(12) 0.91783(12) 0.0232(5) Uani 1 1 d . . . . .
C23 C 0.62740(13) 0.46798(13) 0.93317(14) 0.0297(6) Uani 1 1 d . . . . .
H23A H 0.6614 0.5033 0.9446 0.036 Uiso 1 1 calc R U . . .
H23B H 0.6287 0.4371 0.9711 0.036 Uiso 1 1 calc R U . . .
H23C H 0.6374 0.4434 0.8938 0.036 Uiso 1 1 calc R U . . .
C24 C 0.49088(14) 0.38733(12) 0.89464(14) 0.0298(6) Uani 1 1 d . . . . .
H24A H 0.5364 0.3673 0.9016 0.036 Uiso 1 1 calc R U . . .
H24B H 0.4652 0.3709 0.9291 0.036 Uiso 1 1 calc R U . . .
H24C H 0.4672 0.3748 0.8502 0.036 Uiso 1 1 calc R U . . .
C25 C 0.36819(14) 0.49069(15) 0.87749(15) 0.0353(6) Uani 1 1 d . . . . .
H25A H 0.3412 0.5319 0.8749 0.042 Uiso 1 1 calc R U . . .
H25B H 0.3588 0.4667 0.8347 0.042 Uiso 1 1 calc R U . . .
H25C H 0.3562 0.4622 0.9135 0.042 Uiso 1 1 calc R U . . .
C26 C 0.42673(17) 0.63484(14) 0.91146(16) 0.0340(6) Uani 1 1 d . . . . .
C27 C 0.59092(15) 0.62362(13) 0.94310(13) 0.0308(6) Uani 1 1 d . . . . .
H27A H 0.6372 0.6055 0.9510 0.037 Uiso 1 1 calc R U . . .
H27B H 0.5873 0.6570 0.9071 0.037 Uiso 1 1 calc R U . . .
H27C H 0.5807 0.6448 0.9842 0.037 Uiso 1 1 calc R U . . .
C28 C 0.44177(12) 0.78790(11) 0.69720(11) 0.0193(4) Uani 1 1 d . . . . .
H28A H 0.3976 0.7649 0.6850 0.023 Uiso 1 1 calc R U . . .
H28B H 0.4754 0.7650 0.6737 0.023 Uiso 1 1 calc R U . . .
C29 C 0.43477(11) 0.86012(11) 0.67391(11) 0.0179(4) Uani 1 1 d . . . . .
C30 C 0.45830(12) 0.91215(11) 0.71731(11) 0.0200(4) Uani 1 1 d . . . . .
H30 H 0.4807 0.9019 0.7612 0.024 Uiso 1 1 calc R U . . .
C31 C 0.44960(13) 0.97879(12) 0.69776(12) 0.0233(5) Uani 1 1 d . . . . .
C32 C 0.41449(13) 0.99153(12) 0.63391(12) 0.0251(5) Uani 1 1 d . . . . .
H32 H 0.4073 1.0369 0.6205 0.030 Uiso 1 1 calc R U . . .
C33 C 0.38917(12) 0.94131(12) 0.58818(12) 0.0232(5) Uani 1 1 d . . . . .
C34 C 0.40318(12) 0.87426(11) 0.60867(11) 0.0197(4) Uani 1 1 d . . . . .
C35 C 0.34551(14) 0.95877(13) 0.52056(13) 0.0290(5) Uani 1 1 d . . . . .
C36 C 0.27657(14) 0.92353(15) 0.51770(14) 0.0349(6) Uani 1 1 d . . . . .
H36A H 0.2837 0.8751 0.5223 0.042 Uiso 1 1 calc R U . . .
H36B H 0.2538 0.9399 0.5543 0.042 Uiso 1 1 calc R U . . .
H36C H 0.2482 0.9331 0.4746 0.042 Uiso 1 1 calc R U . . .
C37 C 0.33206(17) 1.03405(15) 0.51315(16) 0.0411(7) Uani 1 1 d . . . . .
H37A H 0.3753 1.0579 0.5148 0.049 Uiso 1 1 calc R U . . .
H37B H 0.3034 1.0429 0.4701 0.049 Uiso 1 1 calc R U . . .
H37C H 0.3089 1.0496 0.5498 0.049 Uiso 1 1 calc R U . . .
C38 C 0.38088(15) 0.93641(16) 0.46149(13) 0.0344(6) Uani 1 1 d . . . . .
H38A H 0.3901 0.8882 0.4649 0.041 Uiso 1 1 calc R U . . .
H38B H 0.3513 0.9459 0.4191 0.041 Uiso 1 1 calc R U . . .
H38C H 0.4237 0.9609 0.4628 0.041 Uiso 1 1 calc R U . . .
C39 C 0.47549(14) 1.03649(12) 0.74549(13) 0.0287(5) Uani 1 1 d . . . . .
C40 C 0.51479(18) 1.01166(15) 0.81225(15) 0.0423(7) Uani 1 1 d . . . . .
H40A H 0.4856 0.9822 0.8343 0.051 Uiso 1 1 calc R U . . .
H40B H 0.5551 0.9868 0.8038 0.051 Uiso 1 1 calc R U . . .
H40C H 0.5289 1.0501 0.8413 0.051 Uiso 1 1 calc R U . . .
C41 C 0.4148(2) 1.07719(17) 0.76212(19) 0.0529(9) Uani 1 1 d . . . . .
H41A H 0.3849 1.0480 0.7835 0.063 Uiso 1 1 calc R U . . .
H41B H 0.4313 1.1138 0.7927 0.063 Uiso 1 1 calc R U . . .
H41C H 0.3896 1.0958 0.7207 0.063 Uiso 1 1 calc R U . . .
C42 C 0.5216(2) 1.0818(2) 0.71242(17) 0.0584(10) Uani 1 1 d . . . . .
H42A H 0.5604 1.0560 0.7017 0.070 Uiso 1 1 calc R U . . .
H42B H 0.4963 1.1004 0.6710 0.070 Uiso 1 1 calc R U . . .
H42C H 0.5381 1.1184 0.7431 0.070 Uiso 1 1 calc R U . . .
C43 C 0.29267(15) 0.75619(16) 0.45033(15) 0.0388(7) Uani 1 1 d . . . . .
H43A H 0.2851 0.7167 0.4212 0.047 Uiso 1 1 calc R U . . .
H43B H 0.2539 0.7622 0.4743 0.047 Uiso 1 1 calc R U . . .
H43C H 0.2976 0.7959 0.4230 0.047 Uiso 1 1 calc R U . . .
C44 C 0.34185(16) 0.67051(14) 0.58196(14) 0.0363(6) Uani 1 1 d . . . . .
H44A H 0.3391 0.6268 0.5596 0.044 Uiso 1 1 calc R U . . .
H44B H 0.3715 0.6672 0.6253 0.044 Uiso 1 1 calc R U . . .
H44C H 0.2963 0.6845 0.5891 0.044 Uiso 1 1 calc R U . . .
C45 C 0.49896(15) 0.71030(16) 0.52701(14) 0.0359(6) Uani 1 1 d . . . . .
C46 C 0.46034(17) 0.65233(15) 0.50658(16) 0.0414(7) Uani 1 1 d . . . . .
C47 C 0.42250(16) 0.66656(16) 0.44239(15) 0.0390(7) Uani 1 1 d . . . . .
C48 C 0.43813(15) 0.73242(16) 0.42500(14) 0.0356(6) Uani 1 1 d . . . . .
C49 C 0.48554(14) 0.75904(15) 0.47756(14) 0.0343(6) Uani 1 1 d . . . . .
C50 C 0.52086(16) 0.82657(17) 0.47982(17) 0.0425(7) Uani 1 1 d . . . . .
H50A H 0.5030 0.8523 0.4396 0.051 Uiso 1 1 calc R U . . .
H50B H 0.5125 0.8511 0.5198 0.051 Uiso 1 1 calc R U . . .
H50C H 0.5698 0.8198 0.4815 0.051 Uiso 1 1 calc R U . . .
C51 C 0.41261(18) 0.7656(2) 0.35875(15) 0.0486(8) Uani 1 1 d . . . . .
H51A H 0.3800 0.7360 0.3317 0.058 Uiso 1 1 calc R U . . .
H51B H 0.3903 0.8080 0.3667 0.058 Uiso 1 1 calc R U . . .
H51C H 0.4510 0.7745 0.3348 0.058 Uiso 1 1 calc R U . . .
C52 C 0.3775(2) 0.61706(19) 0.40028(19) 0.0557(9) Uani 1 1 d . . . . .
H52A H 0.3760 0.5751 0.4253 0.067 Uiso 1 1 calc R U . . .
H52B H 0.3316 0.6355 0.3895 0.067 Uiso 1 1 calc R U . . .
H52C H 0.3958 0.6083 0.3587 0.067 Uiso 1 1 calc R U . . .
C53 C 0.4655(2) 0.58547(18) 0.5415(2) 0.0606(10) Uani 1 1 d . . . . .
H53A H 0.4329 0.5542 0.5167 0.073 Uiso 1 1 calc R U . . .
H53B H 0.5116 0.5678 0.5434 0.073 Uiso 1 1 calc R U . . .
H53C H 0.4552 0.5909 0.5872 0.073 Uiso 1 1 calc R U . . .
C54 C 0.55353(17) 0.7158(2) 0.58807(16) 0.0510(9) Uani 1 1 d . . . . .
H54A H 0.5532 0.6753 0.6155 0.061 Uiso 1 1 calc R U . . .
H54B H 0.5981 0.7206 0.5736 0.061 Uiso 1 1 calc R U . . .
H54C H 0.5446 0.7550 0.6146 0.061 Uiso 1 1 calc R U . . .
C55 C 0.40611(12) 0.79304(12) 0.80584(11) 0.0201(5) Uani 1 1 d . . . . .
H55A H 0.3787 0.7515 0.8036 0.024 Uiso 1 1 calc R U . . .
H55B H 0.3769 0.8290 0.7834 0.024 Uiso 1 1 calc R U . . .
C56 C 0.42788(12) 0.81186(11) 0.87888(11) 0.0199(5) Uani 1 1 d . . . . .
C57 C 0.49376(12) 0.83109(12) 0.90294(12) 0.0229(5) Uani 1 1 d . . . . .
H57 H 0.5256 0.8351 0.8726 0.027 Uiso 1 1 calc R U . . .
C58 C 0.51467(13) 0.84485(13) 0.97088(12) 0.0267(5) Uani 1 1 d . . . . .
C59 C 0.46681(14) 0.83537(14) 1.01400(12) 0.0288(5) Uani 1 1 d . . . . .
H59 H 0.4808 0.8429 1.0606 0.035 Uiso 1 1 calc R U . . .
C60 C 0.39976(13) 0.81557(12) 0.99282(12) 0.0253(5) Uani 1 1 d . . . . .
C61 C 0.37991(12) 0.80703(12) 0.92288(12) 0.0210(5) Uani 1 1 d . . . . .
C62 C 0.35178(14) 0.79933(14) 1.04370(13) 0.0302(6) Uani 1 1 d . . . . .
C63 C 0.32815(16) 0.72599(14) 1.03385(14) 0.0344(6) Uani 1 1 d . . . . .
H63A H 0.3052 0.7197 0.9877 0.041 Uiso 1 1 calc R U . . .
H63B H 0.3676 0.6962 1.0423 0.041 Uiso 1 1 calc R U . . .
H63C H 0.2966 0.7155 1.0652 0.041 Uiso 1 1 calc R U . . .
C64 C 0.38725(16) 0.80582(17) 1.11674(13) 0.0383(7) Uani 1 1 d . . . . .
H64A H 0.3549 0.7951 1.1472 0.046 Uiso 1 1 calc R U . . .
H64B H 0.4257 0.7747 1.1245 0.046 Uiso 1 1 calc R U . . .
H64C H 0.4037 0.8518 1.1250 0.046 Uiso 1 1 calc R U . . .
C65 C 0.29004(15) 0.84710(16) 1.03409(14) 0.0364(6) Uani 1 1 d . . . . .
H65A H 0.2666 0.8438 0.9878 0.044 Uiso 1 1 calc R U . . .
H65B H 0.2588 0.8345 1.0651 0.044 Uiso 1 1 calc R U . . .
H65C H 0.3056 0.8932 1.0433 0.044 Uiso 1 1 calc R U . . .
C66 C 0.58737(14) 0.86765(16) 0.99854(14) 0.0348(6) Uani 1 1 d . . . . .
C67 C 0.58397(19) 0.9376(2) 1.0299(2) 0.0591(10) Uani 1 1 d . . . . .
H67A H 0.5546 0.9360 1.0647 0.071 Uiso 1 1 calc R U . . .
H67B H 0.6297 0.9516 1.0499 0.071 Uiso 1 1 calc R U . . .
H67C H 0.5654 0.9696 0.9951 0.071 Uiso 1 1 calc R U . . .
C68 C 0.61926(18) 0.8185(2) 1.05315(18) 0.0575(10) Uani 1 1 d . . . . .
H68A H 0.5904 0.8155 1.0883 0.069 Uiso 1 1 calc R U . . .
H68B H 0.6232 0.7741 1.0332 0.069 Uiso 1 1 calc R U . . .
H68C H 0.6645 0.8345 1.0727 0.069 Uiso 1 1 calc R U . . .
C69 C 0.63299(17) 0.8712(2) 0.94495(16) 0.0495(8) Uani 1 1 d . . . . .
H69A H 0.6135 0.9024 0.9097 0.059 Uiso 1 1 calc R U . . .
H69B H 0.6782 0.8870 0.9650 0.059 Uiso 1 1 calc R U . . .
H69C H 0.6368 0.8267 0.9256 0.059 Uiso 1 1 calc R U . . .
C70 C 0.17516(15) 0.73121(18) 0.90764(17) 0.0436(8) Uani 1 1 d . . . . .
H70A H 0.1288 0.7241 0.8845 0.052 Uiso 1 1 calc R U . . .
H70B H 0.1968 0.6878 0.9193 0.052 Uiso 1 1 calc R U . . .
H70C H 0.1738 0.7572 0.9486 0.052 Uiso 1 1 calc R U . . .
C71 C 0.24490(15) 0.70104(15) 0.78119(17) 0.0398(7) Uani 1 1 d . . . . .
H71A H 0.2025 0.6928 0.7506 0.048 Uiso 1 1 calc R U . . .
H71B H 0.2815 0.7105 0.7551 0.048 Uiso 1 1 calc R U . . .
H71C H 0.2566 0.6613 0.8091 0.048 Uiso 1 1 calc R U . . .
C72 C 0.22593(14) 0.88665(14) 0.78173(16) 0.0338(6) Uani 1 1 d . . . . .
C73 C 0.19311(15) 0.89818(14) 0.83786(15) 0.0356(6) Uani 1 1 d . . . . .
C74 C 0.13470(14) 0.85720(14) 0.83080(14) 0.0337(6) Uani 1 1 d . . . . .
C75 C 0.13138(14) 0.82031(14) 0.77091(15) 0.0333(6) Uani 1 1 d . . . . .
C76 C 0.18878(15) 0.83851(13) 0.73977(14) 0.0339(6) Uani 1 1 d . . . . .
C77 C 0.20328(19) 0.81483(17) 0.67241(16) 0.0472(8) Uani 1 1 d . . . . .
H77A H 0.1695 0.7812 0.6544 0.057 Uiso 1 1 calc R U . . .
H77B H 0.2010 0.8529 0.6415 0.057 Uiso 1 1 calc R U . . .
H77C H 0.2488 0.7949 0.6775 0.057 Uiso 1 1 calc R U . . .
C78 C 0.28578(16) 0.92730(16) 0.7658(2) 0.0494(9) Uani 1 1 d . . . . .
H78A H 0.3000 0.9103 0.7245 0.059 Uiso 1 1 calc R U . . .
H78B H 0.2724 0.9744 0.7596 0.059 Uiso 1 1 calc R U . . .
H78C H 0.3236 0.9235 0.8029 0.059 Uiso 1 1 calc R U . . .
C79 C 0.07628(16) 0.77140(16) 0.74448(18) 0.0431(7) Uani 1 1 d . . . . .
H79A H 0.0857 0.7524 0.7020 0.052 Uiso 1 1 calc R U . . .
H79B H 0.0748 0.7353 0.7772 0.052 Uiso 1 1 calc R U . . .
H79C H 0.0324 0.7946 0.7370 0.052 Uiso 1 1 calc R U . . .
C80 C 0.08106(17) 0.85898(19) 0.87654(17) 0.0474(8) Uani 1 1 d . . . . .
H80A H 0.0961 0.8886 0.9147 0.057 Uiso 1 1 calc R U . . .
H80B H 0.0383 0.8759 0.8516 0.057 Uiso 1 1 calc R U . . .
H80C H 0.0741 0.8137 0.8929 0.057 Uiso 1 1 calc R U . . .
C81 C 0.2141(2) 0.94940(17) 0.89150(19) 0.0522(9) Uani 1 1 d . . . . .
H81A H 0.1832 0.9475 0.9249 0.063 Uiso 1 1 calc R U . . .
H81B H 0.2606 0.9400 0.9133 0.063 Uiso 1 1 calc R U . . .
H81C H 0.2123 0.9941 0.8713 0.063 Uiso 1 1 calc R U . . .
H26A H 0.4544(16) 0.6742(17) 0.9256(15) 0.033(8) Uiso 1 1 d . . . . .
H26B H 0.4001(16) 0.6436(15) 0.8678(17) 0.032(8) Uiso 1 1 d . . . . .
H26C H 0.396(2) 0.629(2) 0.940(2) 0.071(13) Uiso 1 1 d . . . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT Version 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.8221(15) . ?
Ti1 C16 2.122(3) . ?
Ti1 C17 2.133(3) . ?
Ti1 C18 2.369(2) . ?
Ti1 C22 2.375(2) . ?
Ti1 C19 2.388(2) . ?
Ti1 C20 2.406(2) . ?
Ti1 C21 2.411(2) . ?
Ti2 O2 1.8231(17) . ?
Ti2 C43 2.122(3) . ?
Ti2 C44 2.136(3) . ?
Ti2 C49 2.371(3) . ?
Ti2 C48 2.375(3) . ?
Ti2 C45 2.392(3) . ?
Ti2 C47 2.410(3) . ?
Ti2 C46 2.422(3) . ?
Ti3 O3 1.8150(18) . ?
Ti3 C71 2.128(3) . ?
Ti3 C70 2.129(3) . ?
Ti3 C72 2.384(3) . ?
Ti3 C73 2.395(3) . ?
Ti3 C76 2.395(3) . ?
Ti3 C74 2.403(3) . ?
Ti3 C75 2.403(3) . ?
O1 C7 1.369(3) . ?
O2 C34 1.367(3) . ?
O3 C61 1.370(3) . ?
N1 C55 1.456(3) . ?
N1 C1 1.462(3) . ?
N1 C28 1.467(3) . ?
C1 C2 1.515(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C3 1.387(3) . ?
C2 C7 1.403(3) . ?
C3 C4 1.393(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.393(3) . ?
C4 C12 1.539(3) . ?
C5 C6 1.402(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.411(3) . ?
C6 C8 1.532(3) . ?
C8 C11 1.535(3) . ?
C8 C10 1.540(3) . ?
C8 C9 1.543(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.528(4) . ?
C12 C13 1.532(4) . ?
C12 C14 1.537(3) . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.419(4) . ?
C18 C22 1.424(3) . ?
C18 C27 1.508(3) . ?
C19 C20 1.430(3) . ?
C19 C26 1.504(4) . ?
C20 C21 1.414(4) . ?
C20 C25 1.495(4) . ?
C21 C22 1.422(3) . ?
C21 C24 1.501(3) . ?
C22 C23 1.499(4) . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 H26A 0.98(3) . ?
C26 H26B 0.97(3) . ?
C26 H26C 0.92(5) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 C29 1.516(3) . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.393(3) . ?
C29 C34 1.398(3) . ?
C30 C31 1.391(3) . ?
C30 H30 0.9500 . ?
C31 C32 1.392(4) . ?
C31 C39 1.539(3) . ?
C32 C33 1.403(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.416(3) . ?
C33 C35 1.541(3) . ?
C35 C37 1.530(4) . ?
C35 C36 1.536(4) . ?
C35 C38 1.540(4) . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 H37A 0.9800 . ?
C37 H37B 0.9800 . ?
C37 H37C 0.9800 . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 C42 1.515(4) . ?
C39 C41 1.535(4) . ?
C39 C40 1.532(4) . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
C45 C49 1.390(4) . ?
C45 C46 1.415(4) . ?
C45 C54 1.517(4) . ?
C46 C47 1.423(5) . ?
C46 C53 1.506(5) . ?
C47 C48 1.408(4) . ?
C47 C52 1.506(4) . ?
C48 C49 1.411(4) . ?
C48 C51 1.509(4) . ?
C49 C50 1.518(4) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
C55 C56 1.518(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C56 C57 1.382(3) . ?
C56 C61 1.403(3) . ?
C57 C58 1.397(3) . ?
C57 H57 0.9500 . ?
C58 C59 1.398(4) . ?
C58 C66 1.539(4) . ?
C59 C60 1.395(4) . ?
C59 H59 0.9500 . ?
C60 C61 1.416(3) . ?
C60 C62 1.540(3) . ?
C62 C64 1.538(4) . ?
C62 C63 1.542(4) . ?
C62 C65 1.545(4) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C69 1.516(4) . ?
C66 C68 1.538(5) . ?
C66 C67 1.538(5) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 H69A 0.9800 . ?
C69 H69B 0.9800 . ?
C69 H69C 0.9800 . ?
C70 H70A 0.9800 . ?
C70 H70B 0.9800 . ?
C70 H70C 0.9800 . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 C73 1.410(4) . ?
C72 C76 1.413(4) . ?
C72 C78 1.517(4) . ?
C73 C74 1.411(4) . ?
C73 C81 1.501(4) . ?
C74 C75 1.408(4) . ?
C74 C80 1.515(4) . ?
C75 C76 1.433(4) . ?
C75 C79 1.504(4) . ?
C76 C77 1.507(4) . ?
C77 H77A 0.9800 . ?
C77 H77B 0.9800 . ?
C77 H77C 0.9800 . ?
C78 H78A 0.9800 . ?
C78 H78B 0.9800 . ?
C78 H78C 0.9800 . ?
C79 H79A 0.9800 . ?
C79 H79B 0.9800 . ?
C79 H79C 0.9800 . ?
C80 H80A 0.9800 . ?
C80 H80B 0.9800 . ?
C80 H80C 0.9800 . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 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 C16 104.74(9) . . ?
O1 Ti1 C17 102.31(8) . . ?
C16 Ti1 C17 95.63(11) . . ?
O1 Ti1 C18 94.68(8) . . ?
C16 Ti1 C18 128.17(10) . . ?
C17 Ti1 C18 126.75(10) . . ?
O1 Ti1 C22 111.16(8) . . ?
C16 Ti1 C22 140.51(9) . . ?
C17 Ti1 C22 92.39(10) . . ?
C18 Ti1 C22 34.92(8) . . ?
O1 Ti1 C19 112.58(8) . . ?
C16 Ti1 C19 93.95(10) . . ?
C17 Ti1 C19 139.97(9) . . ?
C18 Ti1 C19 34.70(9) . . ?
C22 Ti1 C19 57.57(9) . . ?
O1 Ti1 C20 147.29(8) . . ?
C16 Ti1 C20 83.41(10) . . ?
C17 Ti1 C20 108.42(9) . . ?
C18 Ti1 C20 57.82(9) . . ?
C22 Ti1 C20 57.44(9) . . ?
C19 Ti1 C20 34.71(8) . . ?
O1 Ti1 C21 145.69(8) . . ?
C16 Ti1 C21 108.47(9) . . ?
C17 Ti1 C21 82.96(9) . . ?
C18 Ti1 C21 57.64(8) . . ?
C22 Ti1 C21 34.56(8) . . ?
C19 Ti1 C21 57.17(8) . . ?
C20 Ti1 C21 34.14(8) . . ?
O2 Ti2 C43 100.86(10) . . ?
O2 Ti2 C44 105.05(9) . . ?
C43 Ti2 C44 96.80(13) . . ?
O2 Ti2 C49 96.60(9) . . ?
C43 Ti2 C49 115.22(12) . . ?
C44 Ti2 C49 137.00(12) . . ?
O2 Ti2 C48 120.99(10) . . ?
C43 Ti2 C48 85.36(11) . . ?
C44 Ti2 C48 132.70(11) . . ?
C49 Ti2 C48 34.60(10) . . ?
O2 Ti2 C45 104.75(9) . . ?
C43 Ti2 C45 141.43(11) . . ?
C44 Ti2 C45 103.72(12) . . ?
C49 Ti2 C45 33.93(11) . . ?
C48 Ti2 C45 56.75(10) . . ?
O2 Ti2 C47 153.32(10) . . ?
C43 Ti2 C47 88.46(11) . . ?
C44 Ti2 C47 98.49(11) . . ?
C49 Ti2 C47 57.07(10) . . ?
C48 Ti2 C47 34.21(11) . . ?
C45 Ti2 C47 56.69(10) . . ?
O2 Ti2 C46 137.04(10) . . ?
C43 Ti2 C46 120.44(12) . . ?
C44 Ti2 C46 82.67(12) . . ?
C49 Ti2 C46 56.96(11) . . ?
C48 Ti2 C46 56.98(11) . . ?
C45 Ti2 C46 34.20(11) . . ?
C47 Ti2 C46 34.26(11) . . ?
O3 Ti3 C71 103.06(10) . . ?
O3 Ti3 C70 101.79(10) . . ?
C71 Ti3 C70 95.20(14) . . ?
O3 Ti3 C72 101.83(9) . . ?
C71 Ti3 C72 111.21(12) . . ?
C70 Ti3 C72 139.14(11) . . ?
O3 Ti3 C73 102.08(9) . . ?
C71 Ti3 C73 141.38(12) . . ?
C70 Ti3 C73 107.76(12) . . ?
C72 Ti3 C73 34.32(10) . . ?
O3 Ti3 C76 130.10(9) . . ?
C71 Ti3 C76 83.99(11) . . ?
C70 Ti3 C76 127.05(12) . . ?
C72 Ti3 C76 34.39(10) . . ?
C73 Ti3 C76 57.39(10) . . ?
O3 Ti3 C74 131.03(9) . . ?
C71 Ti3 C74 125.31(11) . . ?
C70 Ti3 C74 82.66(11) . . ?
C72 Ti3 C74 56.76(10) . . ?
C73 Ti3 C74 34.22(10) . . ?
C76 Ti3 C74 57.21(9) . . ?
O3 Ti3 C75 157.79(9) . . ?
C71 Ti3 C75 92.12(11) . . ?
C70 Ti3 C75 92.74(11) . . ?
C72 Ti3 C75 57.02(10) . . ?
C73 Ti3 C75 57.02(10) . . ?
C76 Ti3 C75 34.75(10) . . ?
C74 Ti3 C75 34.07(10) . . ?
C7 O1 Ti1 165.62(14) . . ?
C34 O2 Ti2 165.28(15) . . ?
C61 O3 Ti3 166.03(15) . . ?
C55 N1 C1 111.76(17) . . ?
C55 N1 C28 110.84(18) . . ?
C1 N1 C28 110.77(17) . . ?
N1 C1 C2 111.82(17) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C3 C2 C7 119.8(2) . . ?
C3 C2 C1 120.22(19) . . ?
C7 C2 C1 119.99(19) . . ?
C2 C3 C4 121.7(2) . . ?
C2 C3 H3 119.2 . . ?
C4 C3 H3 119.2 . . ?
C3 C4 C5 117.4(2) . . ?
C3 C4 C12 119.0(2) . . ?
C5 C4 C12 123.6(2) . . ?
C4 C5 C6 123.5(2) . . ?
C4 C5 H5 118.2 . . ?
C6 C5 H5 118.2 . . ?
C5 C6 C7 117.1(2) . . ?
C5 C6 C8 120.8(2) . . ?
C7 C6 C8 122.02(19) . . ?
O1 C7 C2 117.19(19) . . ?
O1 C7 C6 122.30(19) . . ?
C2 C7 C6 120.49(19) . . ?
C6 C8 C11 112.28(19) . . ?
C6 C8 C10 110.06(18) . . ?
C11 C8 C10 106.6(2) . . ?
C6 C8 C9 108.86(19) . . ?
C11 C8 C9 107.7(2) . . ?
C10 C8 C9 111.26(19) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C12 C13 108.9(2) . . ?
C15 C12 C14 108.3(2) . . ?
C13 C12 C14 109.0(2) . . ?
C15 C12 C4 112.42(19) . . ?
C13 C12 C4 109.3(2) . . ?
C14 C12 C4 108.73(19) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
Ti1 C16 H16A 109.5 . . ?
Ti1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
Ti1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
Ti1 C17 H17A 109.5 . . ?
Ti1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
Ti1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C19 C18 C22 107.6(2) . . ?
C19 C18 C27 126.8(2) . . ?
C22 C18 C27 125.6(2) . . ?
C19 C18 Ti1 73.39(14) . . ?
C22 C18 Ti1 72.79(14) . . ?
C27 C18 Ti1 120.40(16) . . ?
C18 C19 C20 108.3(2) . . ?
C18 C19 C26 127.6(2) . . ?
C20 C19 C26 123.9(2) . . ?
C18 C19 Ti1 71.91(13) . . ?
C20 C19 Ti1 73.34(13) . . ?
C26 C19 Ti1 124.68(17) . . ?
C21 C20 C19 107.7(2) . . ?
C21 C20 C25 126.4(2) . . ?
C19 C20 C25 125.7(2) . . ?
C21 C20 Ti1 73.11(13) . . ?
C19 C20 Ti1 71.95(13) . . ?
C25 C20 Ti1 125.22(18) . . ?
C20 C21 C22 108.2(2) . . ?
C20 C21 C24 125.7(2) . . ?
C22 C21 C24 125.8(2) . . ?
C20 C21 Ti1 72.75(13) . . ?
C22 C21 Ti1 71.35(13) . . ?
C24 C21 Ti1 125.99(17) . . ?
C21 C22 C18 108.2(2) . . ?
C21 C22 C23 124.7(2) . . ?
C18 C22 C23 127.1(2) . . ?
C21 C22 Ti1 74.09(14) . . ?
C18 C22 Ti1 72.29(13) . . ?
C23 C22 Ti1 122.47(17) . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C21 C24 H24A 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C21 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C19 C26 H26A 112.1(19) . . ?
C19 C26 H26B 109.4(18) . . ?
H26A C26 H26B 109(3) . . ?
C19 C26 H26C 112(3) . . ?
H26A C26 H26C 108(3) . . ?
H26B C26 H26C 106(3) . . ?
C18 C27 H27A 109.5 . . ?
C18 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C18 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N1 C28 C29 112.18(18) . . ?
N1 C28 H28A 109.2 . . ?
C29 C28 H28A 109.2 . . ?
N1 C28 H28B 109.2 . . ?
C29 C28 H28B 109.2 . . ?
H28A C28 H28B 107.9 . . ?
C30 C29 C34 120.0(2) . . ?
C30 C29 C28 120.6(2) . . ?
C34 C29 C28 119.4(2) . . ?
C31 C30 C29 121.3(2) . . ?
C31 C30 H30 119.3 . . ?
C29 C30 H30 119.3 . . ?
C30 C31 C32 117.4(2) . . ?
C30 C31 C39 121.6(2) . . ?
C32 C31 C39 121.0(2) . . ?
C31 C32 C33 123.8(2) . . ?
C31 C32 H32 118.1 . . ?
C33 C32 H32 118.1 . . ?
C32 C33 C34 116.7(2) . . ?
C32 C33 C35 121.2(2) . . ?
C34 C33 C35 122.1(2) . . ?
O2 C34 C29 117.1(2) . . ?
O2 C34 C33 122.5(2) . . ?
C29 C34 C33 120.4(2) . . ?
C37 C35 C36 107.7(2) . . ?
C37 C35 C38 107.6(2) . . ?
C36 C35 C38 110.5(2) . . ?
C37 C35 C33 112.0(2) . . ?
C36 C35 C33 108.0(2) . . ?
C38 C35 C33 110.9(2) . . ?
C35 C36 H36A 109.5 . . ?
C35 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C35 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 H37A 109.5 . . ?
C35 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C35 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C35 C38 H38A 109.5 . . ?
C35 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C35 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C42 C39 C41 109.3(3) . . ?
C42 C39 C40 108.5(3) . . ?
C41 C39 C40 107.0(3) . . ?
C42 C39 C31 109.8(2) . . ?
C41 C39 C31 109.5(2) . . ?
C40 C39 C31 112.6(2) . . ?
C39 C40 H40A 109.5 . . ?
C39 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C39 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C39 C41 H41A 109.5 . . ?
C39 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C39 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C39 C42 H42A 109.5 . . ?
C39 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C39 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
Ti2 C43 H43A 109.5 . . ?
Ti2 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
Ti2 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
Ti2 C44 H44A 109.5 . . ?
Ti2 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Ti2 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C49 C45 C46 109.1(3) . . ?
C49 C45 C54 124.6(3) . . ?
C46 C45 C54 125.8(3) . . ?
C49 C45 Ti2 72.19(16) . . ?
C46 C45 Ti2 74.05(17) . . ?
C54 C45 Ti2 126.38(18) . . ?
C45 C46 C47 106.9(3) . . ?
C45 C46 C53 126.4(3) . . ?
C47 C46 C53 126.2(3) . . ?
C45 C46 Ti2 71.76(16) . . ?
C47 C46 Ti2 72.44(17) . . ?
C53 C46 Ti2 127.2(2) . . ?
C48 C47 C46 107.8(3) . . ?
C48 C47 C52 127.4(3) . . ?
C46 C47 C52 124.7(3) . . ?
C48 C47 Ti2 71.51(15) . . ?
C46 C47 Ti2 73.30(16) . . ?
C52 C47 Ti2 123.7(2) . . ?
C49 C48 C47 108.2(3) . . ?
C49 C48 C51 126.6(3) . . ?
C47 C48 C51 125.0(3) . . ?
C49 C48 Ti2 72.53(15) . . ?
C47 C48 Ti2 74.28(16) . . ?
C51 C48 Ti2 123.1(2) . . ?
C45 C49 C48 108.0(3) . . ?
C45 C49 C50 124.3(3) . . ?
C48 C49 C50 127.6(3) . . ?
C45 C49 Ti2 73.88(17) . . ?
C48 C49 Ti2 72.86(16) . . ?
C50 C49 Ti2 122.37(19) . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C48 C51 H51A 109.5 . . ?
C48 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C48 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C47 C52 H52A 109.5 . . ?
C47 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C47 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C46 C53 H53A 109.5 . . ?
C46 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C46 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C45 C54 H54A 109.5 . . ?
C45 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C45 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1 C55 C56 112.95(19) . . ?
N1 C55 H55A 109.0 . . ?
C56 C55 H55A 109.0 . . ?
N1 C55 H55B 109.0 . . ?
C56 C55 H55B 109.0 . . ?
H55A C55 H55B 107.8 . . ?
C57 C56 C61 119.9(2) . . ?
C57 C56 C55 121.6(2) . . ?
C61 C56 C55 118.4(2) . . ?
C56 C57 C58 121.6(2) . . ?
C56 C57 H57 119.2 . . ?
C58 C57 H57 119.2 . . ?
C57 C58 C59 117.0(2) . . ?
C57 C58 C66 122.4(2) . . ?
C59 C58 C66 120.5(2) . . ?
C60 C59 C58 124.0(2) . . ?
C60 C59 H59 118.0 . . ?
C58 C59 H59 118.0 . . ?
C59 C60 C61 116.6(2) . . ?
C59 C60 C62 121.2(2) . . ?
C61 C60 C62 122.1(2) . . ?
O3 C61 C56 117.6(2) . . ?
O3 C61 C60 121.8(2) . . ?
C56 C61 C60 120.6(2) . . ?
C64 C62 C60 112.3(2) . . ?
C64 C62 C63 106.8(2) . . ?
C60 C62 C63 108.8(2) . . ?
C64 C62 C65 108.0(2) . . ?
C60 C62 C65 110.5(2) . . ?
C63 C62 C65 110.4(2) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C69 C66 C68 108.3(3) . . ?
C69 C66 C58 112.9(2) . . ?
C68 C66 C58 109.5(3) . . ?
C69 C66 C67 108.6(3) . . ?
C68 C66 C67 108.9(3) . . ?
C58 C66 C67 108.6(2) . . ?
C66 C67 H67A 109.5 . . ?
C66 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C66 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C66 C68 H68A 109.5 . . ?
C66 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
C66 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
C66 C69 H69A 109.5 . . ?
C66 C69 H69B 109.5 . . ?
H69A C69 H69B 109.5 . . ?
C66 C69 H69C 109.5 . . ?
H69A C69 H69C 109.5 . . ?
H69B C69 H69C 109.5 . . ?
Ti3 C70 H70A 109.5 . . ?
Ti3 C70 H70B 109.5 . . ?
H70A C70 H70B 109.5 . . ?
Ti3 C70 H70C 109.5 . . ?
H70A C70 H70C 109.5 . . ?
H70B C70 H70C 109.5 . . ?
Ti3 C71 H71A 109.5 . . ?
Ti3 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
Ti3 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C73 C72 C76 109.1(2) . . ?
C73 C72 C78 124.0(3) . . ?
C76 C72 C78 126.4(3) . . ?
C73 C72 Ti3 73.27(16) . . ?
C76 C72 Ti3 73.24(15) . . ?
C78 C72 Ti3 126.18(19) . . ?
C72 C73 C74 107.5(3) . . ?
C72 C73 C81 125.3(3) . . ?
C74 C73 C81 127.0(3) . . ?
C72 C73 Ti3 72.41(16) . . ?
C74 C73 Ti3 73.20(16) . . ?
C81 C73 Ti3 123.9(2) . . ?
C75 C74 C73 108.6(2) . . ?
C75 C74 C80 126.2(3) . . ?
C73 C74 C80 124.9(3) . . ?
C75 C74 Ti3 72.98(16) . . ?
C73 C74 Ti3 72.58(16) . . ?
C80 C74 Ti3 125.5(2) . . ?
C74 C75 C76 107.9(3) . . ?
C74 C75 C79 125.4(3) . . ?
C76 C75 C79 126.6(3) . . ?
C74 C75 Ti3 72.95(16) . . ?
C76 C75 Ti3 72.31(16) . . ?
C79 C75 Ti3 121.20(19) . . ?
C72 C76 C75 106.8(2) . . ?
C72 C76 C77 126.8(3) . . ?
C75 C76 C77 126.2(3) . . ?
C72 C76 Ti3 72.37(16) . . ?
C75 C76 Ti3 72.94(16) . . ?
C77 C76 Ti3 123.65(19) . . ?
C76 C77 H77A 109.5 . . ?
C76 C77 H77B 109.5 . . ?
H77A C77 H77B 109.5 . . ?
C76 C77 H77C 109.5 . . ?
H77A C77 H77C 109.5 . . ?
H77B C77 H77C 109.5 . . ?
C72 C78 H78A 109.5 . . ?
C72 C78 H78B 109.5 . . ?
H78A C78 H78B 109.5 . . ?
C72 C78 H78C 109.5 . . ?
H78A C78 H78C 109.5 . . ?
H78B C78 H78C 109.5 . . ?
C75 C79 H79A 109.5 . . ?
C75 C79 H79B 109.5 . . ?
H79A C79 H79B 109.5 . . ?
C75 C79 H79C 109.5 . . ?
H79A C79 H79C 109.5 . . ?
H79B C79 H79C 109.5 . . ?
C74 C80 H80A 109.5 . . ?
C74 C80 H80B 109.5 . . ?
H80A C80 H80B 109.5 . . ?
C74 C80 H80C 109.5 . . ?
H80A C80 H80C 109.5 . . ?
H80B C80 H80C 109.5 . . ?
C73 C81 H81A 109.5 . . ?
C73 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C73 C81 H81C 109.5 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 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
C16 Ti1 O1 C7 86.4(6) . . . . ?
C17 Ti1 O1 C7 -174.3(6) . . . . ?
C18 Ti1 O1 C7 -45.1(6) . . . . ?
C22 Ti1 O1 C7 -76.8(6) . . . . ?
C19 Ti1 O1 C7 -14.4(6) . . . . ?
C20 Ti1 O1 C7 -14.6(7) . . . . ?
C21 Ti1 O1 C7 -78.7(6) . . . . ?
C43 Ti2 O2 C34 -167.4(6) . . . . ?
C44 Ti2 O2 C34 92.4(6) . . . . ?
C49 Ti2 O2 C34 -50.1(6) . . . . ?
C48 Ti2 O2 C34 -76.3(6) . . . . ?
C45 Ti2 O2 C34 -16.5(6) . . . . ?
C47 Ti2 O2 C34 -58.7(7) . . . . ?
C46 Ti2 O2 C34 -3.1(6) . . . . ?
C71 Ti3 O3 C61 89.1(7) . . . . ?
C70 Ti3 O3 C61 -172.7(6) . . . . ?
C72 Ti3 O3 C61 -26.2(7) . . . . ?
C73 Ti3 O3 C61 -61.3(7) . . . . ?
C76 Ti3 O3 C61 -4.0(7) . . . . ?
C74 Ti3 O3 C61 -82.2(7) . . . . ?
C75 Ti3 O3 C61 -42.9(8) . . . . ?
C55 N1 C1 C2 -160.67(19) . . . . ?
C28 N1 C1 C2 75.2(2) . . . . ?
N1 C1 C2 C3 15.9(3) . . . . ?
N1 C1 C2 C7 -163.75(19) . . . . ?
C7 C2 C3 C4 0.8(3) . . . . ?
C1 C2 C3 C4 -178.8(2) . . . . ?
C2 C3 C4 C5 -0.6(3) . . . . ?
C2 C3 C4 C12 178.9(2) . . . . ?
C3 C4 C5 C6 0.2(3) . . . . ?
C12 C4 C5 C6 -179.3(2) . . . . ?
C4 C5 C6 C7 0.0(3) . . . . ?
C4 C5 C6 C8 178.0(2) . . . . ?
Ti1 O1 C7 C2 -33.0(7) . . . . ?
Ti1 O1 C7 C6 148.8(5) . . . . ?
C3 C2 C7 O1 -178.8(2) . . . . ?
C1 C2 C7 O1 0.8(3) . . . . ?
C3 C2 C7 C6 -0.6(3) . . . . ?
C1 C2 C7 C6 179.1(2) . . . . ?
C5 C6 C7 O1 178.3(2) . . . . ?
C8 C6 C7 O1 0.4(3) . . . . ?
C5 C6 C7 C2 0.2(3) . . . . ?
C8 C6 C7 C2 -177.7(2) . . . . ?
C5 C6 C8 C11 6.3(3) . . . . ?
C7 C6 C8 C11 -175.9(2) . . . . ?
C5 C6 C8 C10 124.9(2) . . . . ?
C7 C6 C8 C10 -57.2(3) . . . . ?
C5 C6 C8 C9 -112.9(2) . . . . ?
C7 C6 C8 C9 64.9(3) . . . . ?
C3 C4 C12 C15 175.5(2) . . . . ?
C5 C4 C12 C15 -5.0(3) . . . . ?
C3 C4 C12 C13 -63.4(3) . . . . ?
C5 C4 C12 C13 116.2(3) . . . . ?
C3 C4 C12 C14 55.6(3) . . . . ?
C5 C4 C12 C14 -124.9(2) . . . . ?
C22 C18 C19 C20 -0.4(3) . . . . ?
C27 C18 C19 C20 -179.3(2) . . . . ?
Ti1 C18 C19 C20 64.82(16) . . . . ?
C22 C18 C19 C26 174.5(2) . . . . ?
C27 C18 C19 C26 -4.4(4) . . . . ?
Ti1 C18 C19 C26 -120.3(2) . . . . ?
C22 C18 C19 Ti1 -65.25(16) . . . . ?
C27 C18 C19 Ti1 115.9(2) . . . . ?
C18 C19 C20 C21 1.0(3) . . . . ?
C26 C19 C20 C21 -174.2(2) . . . . ?
Ti1 C19 C20 C21 64.88(16) . . . . ?
C18 C19 C20 C25 175.3(2) . . . . ?
C26 C19 C20 C25 0.1(4) . . . . ?
Ti1 C19 C20 C25 -120.8(2) . . . . ?
C18 C19 C20 Ti1 -63.89(16) . . . . ?
C26 C19 C20 Ti1 121.0(2) . . . . ?
C19 C20 C21 C22 -1.2(3) . . . . ?
C25 C20 C21 C22 -175.4(2) . . . . ?
Ti1 C20 C21 C22 62.94(16) . . . . ?
C19 C20 C21 C24 173.6(2) . . . . ?
C25 C20 C21 C24 -0.7(4) . . . . ?
Ti1 C20 C21 C24 -122.3(2) . . . . ?
C19 C20 C21 Ti1 -64.11(16) . . . . ?
C25 C20 C21 Ti1 121.7(3) . . . . ?
C20 C21 C22 C18 0.9(3) . . . . ?
C24 C21 C22 C18 -173.8(2) . . . . ?
Ti1 C21 C22 C18 64.76(16) . . . . ?
C20 C21 C22 C23 177.4(2) . . . . ?
C24 C21 C22 C23 2.6(4) . . . . ?
Ti1 C21 C22 C23 -118.8(2) . . . . ?
C20 C21 C22 Ti1 -63.84(16) . . . . ?
C24 C21 C22 Ti1 121.4(2) . . . . ?
C19 C18 C22 C21 -0.3(3) . . . . ?
C27 C18 C22 C21 178.6(2) . . . . ?
Ti1 C18 C22 C21 -65.94(16) . . . . ?
C19 C18 C22 C23 -176.6(2) . . . . ?
C27 C18 C22 C23 2.3(4) . . . . ?
Ti1 C18 C22 C23 117.7(2) . . . . ?
C19 C18 C22 Ti1 65.65(16) . . . . ?
C27 C18 C22 Ti1 -115.4(2) . . . . ?
C55 N1 C28 C29 79.5(2) . . . . ?
C1 N1 C28 C29 -155.87(19) . . . . ?
N1 C28 C29 C30 10.2(3) . . . . ?
N1 C28 C29 C34 -168.6(2) . . . . ?
C34 C29 C30 C31 1.6(3) . . . . ?
C28 C29 C30 C31 -177.1(2) . . . . ?
C29 C30 C31 C32 2.1(3) . . . . ?
C29 C30 C31 C39 -180.0(2) . . . . ?
C30 C31 C32 C33 -1.6(4) . . . . ?
C39 C31 C32 C33 -179.5(2) . . . . ?
C31 C32 C33 C34 -2.5(4) . . . . ?
C31 C32 C33 C35 174.8(2) . . . . ?
Ti2 O2 C34 C29 -47.1(7) . . . . ?
Ti2 O2 C34 C33 135.1(5) . . . . ?
C30 C29 C34 O2 176.3(2) . . . . ?
C28 C29 C34 O2 -5.0(3) . . . . ?
C30 C29 C34 C33 -5.9(3) . . . . ?
C28 C29 C34 C33 172.9(2) . . . . ?
C32 C33 C34 O2 -176.1(2) . . . . ?
C35 C33 C34 O2 6.7(4) . . . . ?
C32 C33 C34 C29 6.2(3) . . . . ?
C35 C33 C34 C29 -171.0(2) . . . . ?
C32 C33 C35 C37 -2.7(4) . . . . ?
C34 C33 C35 C37 174.4(2) . . . . ?
C32 C33 C35 C36 -121.2(3) . . . . ?
C34 C33 C35 C36 55.9(3) . . . . ?
C32 C33 C35 C38 117.6(3) . . . . ?
C34 C33 C35 C38 -65.3(3) . . . . ?
C30 C31 C39 C42 125.1(3) . . . . ?
C32 C31 C39 C42 -57.0(4) . . . . ?
C30 C31 C39 C41 -114.9(3) . . . . ?
C32 C31 C39 C41 63.0(3) . . . . ?
C30 C31 C39 C40 4.0(4) . . . . ?
C32 C31 C39 C40 -178.1(3) . . . . ?
C49 C45 C46 C47 0.2(3) . . . . ?
C54 C45 C46 C47 -171.9(3) . . . . ?
Ti2 C45 C46 C47 64.4(2) . . . . ?
C49 C45 C46 C53 172.7(3) . . . . ?
C54 C45 C46 C53 0.5(5) . . . . ?
Ti2 C45 C46 C53 -123.2(3) . . . . ?
C49 C45 C46 Ti2 -64.17(19) . . . . ?
C54 C45 C46 Ti2 123.7(3) . . . . ?
C45 C46 C47 C48 -0.3(3) . . . . ?
C53 C46 C47 C48 -172.8(3) . . . . ?
Ti2 C46 C47 C48 63.6(2) . . . . ?
C45 C46 C47 C52 176.3(3) . . . . ?
C53 C46 C47 C52 3.8(5) . . . . ?
Ti2 C46 C47 C52 -119.8(3) . . . . ?
C45 C46 C47 Ti2 -64.0(2) . . . . ?
C53 C46 C47 Ti2 123.6(3) . . . . ?
C46 C47 C48 C49 0.3(3) . . . . ?
C52 C47 C48 C49 -176.2(3) . . . . ?
Ti2 C47 C48 C49 65.11(19) . . . . ?
C46 C47 C48 C51 175.5(3) . . . . ?
C52 C47 C48 C51 -1.0(5) . . . . ?
Ti2 C47 C48 C51 -119.7(3) . . . . ?
C46 C47 C48 Ti2 -64.8(2) . . . . ?
C52 C47 C48 Ti2 118.7(3) . . . . ?
C46 C45 C49 C48 0.0(3) . . . . ?
C54 C45 C49 C48 172.2(3) . . . . ?
Ti2 C45 C49 C48 -65.41(19) . . . . ?
C46 C45 C49 C50 -176.1(3) . . . . ?
C54 C45 C49 C50 -3.8(4) . . . . ?
Ti2 C45 C49 C50 118.5(3) . . . . ?
C46 C45 C49 Ti2 65.4(2) . . . . ?
C54 C45 C49 Ti2 -122.4(3) . . . . ?
C47 C48 C49 C45 -0.2(3) . . . . ?
C51 C48 C49 C45 -175.3(3) . . . . ?
Ti2 C48 C49 C45 66.08(19) . . . . ?
C47 C48 C49 C50 175.7(3) . . . . ?
C51 C48 C49 C50 0.6(5) . . . . ?
Ti2 C48 C49 C50 -118.0(3) . . . . ?
C47 C48 C49 Ti2 -66.3(2) . . . . ?
C51 C48 C49 Ti2 118.6(3) . . . . ?
C1 N1 C55 C56 75.7(2) . . . . ?
C28 N1 C55 C56 -160.20(18) . . . . ?
N1 C55 C56 C57 13.4(3) . . . . ?
N1 C55 C56 C61 -164.4(2) . . . . ?
C61 C56 C57 C58 1.2(4) . . . . ?
C55 C56 C57 C58 -176.4(2) . . . . ?
C56 C57 C58 C59 2.8(4) . . . . ?
C56 C57 C58 C66 -178.8(2) . . . . ?
C57 C58 C59 C60 -2.4(4) . . . . ?
C66 C58 C59 C60 179.2(3) . . . . ?
C58 C59 C60 C61 -2.1(4) . . . . ?
C58 C59 C60 C62 173.9(2) . . . . ?
Ti3 O3 C61 C56 -37.6(8) . . . . ?
Ti3 O3 C61 C60 144.4(6) . . . . ?
C57 C56 C61 O3 176.1(2) . . . . ?
C55 C56 C61 O3 -6.2(3) . . . . ?
C57 C56 C61 C60 -6.0(3) . . . . ?
C55 C56 C61 C60 171.8(2) . . . . ?
C59 C60 C61 O3 -175.9(2) . . . . ?
C62 C60 C61 O3 8.2(4) . . . . ?
C59 C60 C61 C56 6.2(3) . . . . ?
C62 C60 C61 C56 -169.7(2) . . . . ?
C59 C60 C62 C64 -1.6(4) . . . . ?
C61 C60 C62 C64 174.2(2) . . . . ?
C59 C60 C62 C63 -119.7(3) . . . . ?
C61 C60 C62 C63 56.1(3) . . . . ?
C59 C60 C62 C65 119.0(3) . . . . ?
C61 C60 C62 C65 -65.3(3) . . . . ?
C57 C58 C66 C69 -1.7(4) . . . . ?
C59 C58 C66 C69 176.6(3) . . . . ?
C57 C58 C66 C68 -122.4(3) . . . . ?
C59 C58 C66 C68 55.9(4) . . . . ?
C57 C58 C66 C67 118.8(3) . . . . ?
C59 C58 C66 C67 -62.9(4) . . . . ?
C76 C72 C73 C74 -0.3(3) . . . . ?
C78 C72 C73 C74 172.0(3) . . . . ?
Ti3 C72 C73 C74 -65.31(19) . . . . ?
C76 C72 C73 C81 -175.5(3) . . . . ?
C78 C72 C73 C81 -3.2(4) . . . . ?
Ti3 C72 C73 C81 119.6(3) . . . . ?
C76 C72 C73 Ti3 64.98(19) . . . . ?
C78 C72 C73 Ti3 -122.7(3) . . . . ?
C72 C73 C74 C75 0.2(3) . . . . ?
C81 C73 C74 C75 175.2(3) . . . . ?
Ti3 C73 C74 C75 -64.56(19) . . . . ?
C72 C73 C74 C80 -173.6(3) . . . . ?
C81 C73 C74 C80 1.4(5) . . . . ?
Ti3 C73 C74 C80 121.6(3) . . . . ?
C72 C73 C74 Ti3 64.78(19) . . . . ?
C81 C73 C74 Ti3 -120.2(3) . . . . ?
C73 C74 C75 C76 0.0(3) . . . . ?
C80 C74 C75 C76 173.7(3) . . . . ?
Ti3 C74 C75 C76 -64.33(19) . . . . ?
C73 C74 C75 C79 -179.2(3) . . . . ?
C80 C74 C75 C79 -5.4(5) . . . . ?
Ti3 C74 C75 C79 116.5(3) . . . . ?
C73 C74 C75 Ti3 64.30(19) . . . . ?
C80 C74 C75 Ti3 -121.9(3) . . . . ?
C73 C72 C76 C75 0.3(3) . . . . ?
C78 C72 C76 C75 -171.7(3) . . . . ?
Ti3 C72 C76 C75 65.31(18) . . . . ?
C73 C72 C76 C77 175.8(3) . . . . ?
C78 C72 C76 C77 3.7(5) . . . . ?
Ti3 C72 C76 C77 -119.2(3) . . . . ?
C73 C72 C76 Ti3 -65.00(19) . . . . ?
C78 C72 C76 Ti3 122.9(3) . . . . ?
C74 C75 C76 C72 -0.2(3) . . . . ?
C79 C75 C76 C72 178.9(3) . . . . ?
Ti3 C75 C76 C72 -64.92(19) . . . . ?
C74 C75 C76 C77 -175.7(3) . . . . ?
C79 C75 C76 C77 3.4(5) . . . . ?
Ti3 C75 C76 C77 119.6(3) . . . . ?
C74 C75 C76 Ti3 64.75(19) . . . . ?
C79 C75 C76 Ti3 -116.1(3) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti2
_database_code_depnum_ccdc_archive 'CCDC 1549582'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C47 H60 Cl3 N O3 Ti2'
_chemical_formula_moiety         'C47 H60 Cl3 N O3 Ti2'
_chemical_formula_weight         889.15
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 -X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 +X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   14.275(7)
_cell_length_b                   22.520(10)
_cell_length_c                   14.984(7)
_cell_angle_alpha                90.0000
_cell_angle_beta                 100.408(6)
_cell_angle_gamma                90.0000
_cell_volume                     4738(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    10576
_cell_measurement_theta_min      3.02
_cell_measurement_theta_max      27.49
_cell_measurement_temperature    273
#------------------------------------------------------------------------------
_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.060
_exptl_crystal_density_diffrn    1.246
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1872.00
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_T_max  0.968

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            49820
_diffrn_reflns_av_R_equivalents  0.0801
_diffrn_reflns_theta_max         27.490
_diffrn_reflns_theta_min         3.019
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       19
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             10837
_reflns_number_gt                8074
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt)., SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.0999
_refine_ls_R_factor_gt           0.0721
_refine_ls_wR_factor_ref         0.2152
_refine_ls_wR_factor_gt          0.1857
_refine_ls_number_restraints     0
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         10837
_refine_ls_number_parameters     505
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1005P)²+9.5208P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.000
_refine_diff_density_max         0.59
_refine_diff_density_min         -0.75
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.19676(5) 0.41835(3) 0.27932(5) 0.01946(17) Uani 1 1 d . . . . .
Ti2 Ti 0.67383(5) 0.19234(3) 0.47634(5) 0.01733(17) Uani 1 1 d . . . . .
Cl1 Cl 0.24355(8) 0.42275(5) 0.43314(7) 0.0320(3) Uani 1 1 d . . . . .
Cl2 Cl 0.03828(7) 0.39755(5) 0.26192(8) 0.0320(3) Uani 1 1 d . . . . .
Cl3 Cl 0.71146(8) 0.13254(4) 0.36228(7) 0.0266(2) Uani 1 1 d . . . . .
O1 O 0.24535(19) 0.34962(12) 0.25154(19) 0.0216(6) Uani 1 1 d . . . . .
O2 O 0.54687(19) 0.18091(12) 0.46136(19) 0.0207(6) Uani 1 1 d . . . . .
O3 O 0.69464(19) 0.26492(12) 0.43244(19) 0.0211(6) Uani 1 1 d . . . . .
N1 N 0.4955(2) 0.30782(14) 0.4182(2) 0.0169(6) Uani 1 1 d . . . . .
C1 C 0.4414(3) 0.33554(17) 0.3368(3) 0.0194(8) Uani 1 1 d . . . . .
H1A H 0.4848 0.3580 0.3069 0.023 Uiso 1 1 calc R U . . .
H1B H 0.3961 0.3632 0.3546 0.023 Uiso 1 1 calc R U . . .
C2 C 0.3885(3) 0.29182(17) 0.2705(3) 0.0192(8) Uani 1 1 d . . . . .
C3 C 0.2934(3) 0.30091(17) 0.2295(3) 0.0208(8) Uani 1 1 d . . . . .
C4 C 0.2436(3) 0.25963(18) 0.1680(3) 0.0243(8) Uani 1 1 d . . . . .
C5 C 0.2905(3) 0.20765(18) 0.1514(3) 0.0239(8) Uani 1 1 d . . . . .
H5 H 0.2580 0.1796 0.1119 0.029 Uiso 1 1 calc R U . . .
C6 C 0.3837(3) 0.19640(18) 0.1919(3) 0.0232(8) Uani 1 1 d . . . . .
C7 C 0.4321(3) 0.23899(17) 0.2498(3) 0.0197(8) Uani 1 1 d . . . . .
H7 H 0.4955 0.2322 0.2756 0.024 Uiso 1 1 calc R U . . .
C8 C 0.4320(3) 0.13797(18) 0.1778(3) 0.0261(9) Uani 1 1 d . . . . .
H8A H 0.4962 0.1384 0.2111 0.031 Uiso 1 1 calc R U . . .
H8B H 0.3976 0.1059 0.1991 0.031 Uiso 1 1 calc R U . . .
H8C H 0.4329 0.1326 0.1144 0.031 Uiso 1 1 calc R U . . .
C9 C 0.1421(3) 0.2722(2) 0.1226(4) 0.0382(11) Uani 1 1 d . . . . .
H9A H 0.1226 0.3100 0.1426 0.046 Uiso 1 1 calc R U . . .
H9B H 0.1381 0.2730 0.0579 0.046 Uiso 1 1 calc R U . . .
H9C H 0.1010 0.2417 0.1383 0.046 Uiso 1 1 calc R U . . .
C10 C 0.2818(3) 0.46502(19) 0.1793(3) 0.0265(9) Uani 1 1 d . . . . .
C11 C 0.3036(3) 0.49610(19) 0.2617(3) 0.0277(9) Uani 1 1 d . . . . .
C12 C 0.2186(3) 0.52408(19) 0.2779(3) 0.0306(10) Uani 1 1 d . . . . .
C13 C 0.1448(3) 0.5100(2) 0.2052(3) 0.0299(10) Uani 1 1 d . . . . .
C14 C 0.1834(3) 0.47247(19) 0.1446(3) 0.0268(9) Uani 1 1 d . . . . .
C15 C 0.3514(3) 0.4313(2) 0.1342(3) 0.0352(11) Uani 1 1 d . . . . .
H15A H 0.3185 0.4141 0.0787 0.042 Uiso 1 1 calc R U . . .
H15B H 0.3997 0.4579 0.1212 0.042 Uiso 1 1 calc R U . . .
H15C H 0.3804 0.4004 0.1740 0.042 Uiso 1 1 calc R U . . .
C16 C 0.4004(4) 0.5036(2) 0.3202(4) 0.0422(13) Uani 1 1 d . . . . .
H16A H 0.3947 0.5269 0.3726 0.051 Uiso 1 1 calc R U . . .
H16B H 0.4261 0.4653 0.3391 0.051 Uiso 1 1 calc R U . . .
H16C H 0.4420 0.5234 0.2861 0.051 Uiso 1 1 calc R U . . .
C17 C 0.2111(5) 0.5650(2) 0.3546(4) 0.0485(14) Uani 1 1 d . . . . .
H17A H 0.2714 0.5669 0.3950 0.058 Uiso 1 1 calc R U . . .
H17B H 0.1936 0.6039 0.3312 0.058 Uiso 1 1 calc R U . . .
H17C H 0.1635 0.5505 0.3869 0.058 Uiso 1 1 calc R U . . .
C18 C 0.0456(4) 0.5336(3) 0.1902(4) 0.0497(15) Uani 1 1 d . . . . .
H18A H 0.0098 0.5169 0.1356 0.060 Uiso 1 1 calc R U . . .
H18B H 0.0161 0.5232 0.2407 0.060 Uiso 1 1 calc R U . . .
H18C H 0.0471 0.5761 0.1846 0.060 Uiso 1 1 calc R U . . .
C19 C 0.1307(4) 0.4476(2) 0.0567(3) 0.0382(12) Uani 1 1 d . . . . .
H19A H 0.0649 0.4589 0.0488 0.046 Uiso 1 1 calc R U . . .
H19B H 0.1580 0.4628 0.0074 0.046 Uiso 1 1 calc R U . . .
H19C H 0.1355 0.4051 0.0579 0.046 Uiso 1 1 calc R U . . .
C20 C 0.4332(3) 0.28297(17) 0.4770(3) 0.0210(8) Uani 1 1 d . . . . .
H20A H 0.3817 0.3106 0.4794 0.025 Uiso 1 1 calc R U . . .
H20B H 0.4695 0.2790 0.5380 0.025 Uiso 1 1 calc R U . . .
C21 C 0.3910(3) 0.22278(18) 0.4458(3) 0.0200(8) Uani 1 1 d . . . . .
C22 C 0.4502(3) 0.17394(18) 0.4406(3) 0.0196(8) Uani 1 1 d . . . . .
C23 C 0.4126(3) 0.11809(18) 0.4124(3) 0.0226(8) Uani 1 1 d . . . . .
C24 C 0.3141(3) 0.1134(2) 0.3862(3) 0.0263(9) Uani 1 1 d . . . . .
H24 H 0.2881 0.0769 0.3660 0.032 Uiso 1 1 calc R U . . .
C25 C 0.2537(3) 0.1613(2) 0.3893(3) 0.0264(9) Uani 1 1 d . . . . .
C26 C 0.2929(3) 0.2152(2) 0.4204(3) 0.0257(9) Uani 1 1 d . . . . .
H26 H 0.2528 0.2472 0.4245 0.031 Uiso 1 1 calc R U . . .
C27 C 0.1467(3) 0.1555(2) 0.3552(4) 0.0346(11) Uani 1 1 d . . . . .
H27A H 0.1318 0.1154 0.3363 0.042 Uiso 1 1 calc R U . . .
H27B H 0.1132 0.1658 0.4032 0.042 Uiso 1 1 calc R U . . .
H27C H 0.1278 0.1819 0.3048 0.042 Uiso 1 1 calc R U . . .
C28 C 0.4776(3) 0.06593(19) 0.4077(3) 0.0302(10) Uani 1 1 d . . . . .
H28A H 0.5424 0.0778 0.4284 0.036 Uiso 1 1 calc R U . . .
H28B H 0.4615 0.0345 0.4455 0.036 Uiso 1 1 calc R U . . .
H28C H 0.4701 0.0522 0.3461 0.036 Uiso 1 1 calc R U . . .
C29 C 0.5621(3) 0.35097(18) 0.4693(3) 0.0204(8) Uani 1 1 d . . . . .
H29A H 0.5869 0.3348 0.5289 0.025 Uiso 1 1 calc R U . . .
H29B H 0.5277 0.3871 0.4776 0.025 Uiso 1 1 calc R U . . .
C30 C 0.6448(3) 0.36604(17) 0.4223(3) 0.0180(7) Uani 1 1 d . . . . .
C31 C 0.7090(3) 0.32158(17) 0.4080(3) 0.0181(7) Uani 1 1 d . . . . .
C32 C 0.7876(3) 0.33477(18) 0.3669(3) 0.0216(8) Uani 1 1 d . . . . .
C33 C 0.7987(3) 0.39379(19) 0.3406(3) 0.0249(9) Uani 1 1 d . . . . .
H33 H 0.8496 0.4030 0.3121 0.030 Uiso 1 1 calc R U . . .
C34 C 0.7374(3) 0.43878(18) 0.3551(3) 0.0217(8) Uani 1 1 d . . . . .
C35 C 0.6605(3) 0.42415(17) 0.3969(3) 0.0197(8) Uani 1 1 d . . . . .
H35 H 0.6189 0.4539 0.4080 0.024 Uiso 1 1 calc R U . . .
C36 C 0.7527(3) 0.5018(2) 0.3262(3) 0.0309(10) Uani 1 1 d . . . . .
H36A H 0.7036 0.5269 0.3415 0.037 Uiso 1 1 calc R U . . .
H36B H 0.8138 0.5156 0.3568 0.037 Uiso 1 1 calc R U . . .
H36C H 0.7506 0.5029 0.2618 0.037 Uiso 1 1 calc R U . . .
C37 C 0.8590(3) 0.28784(19) 0.3531(3) 0.0273(9) Uani 1 1 d . . . . .
H37A H 0.8402 0.2504 0.3749 0.033 Uiso 1 1 calc R U . . .
H37B H 0.8614 0.2847 0.2897 0.033 Uiso 1 1 calc R U . . .
H37C H 0.9207 0.2986 0.3861 0.033 Uiso 1 1 calc R U . . .
C38 C 0.7991(3) 0.21574(19) 0.6006(3) 0.0213(8) Uani 1 1 d . . . . .
C39 C 0.8201(3) 0.15916(18) 0.5670(3) 0.0216(8) Uani 1 1 d . . . . .
C40 C 0.7457(3) 0.11879(19) 0.5816(3) 0.0241(8) Uani 1 1 d . . . . .
C41 C 0.6803(3) 0.15070(18) 0.6227(3) 0.0211(8) Uani 1 1 d . . . . .
C42 C 0.7108(3) 0.21030(18) 0.6320(3) 0.0229(8) Uani 1 1 d . . . . .
C43 C 0.6628(3) 0.2585(2) 0.6775(3) 0.0278(9) Uani 1 1 d . . . . .
H43A H 0.6965 0.2952 0.6754 0.033 Uiso 1 1 calc R U . . .
H43B H 0.5982 0.2632 0.6463 0.033 Uiso 1 1 calc R U . . .
H43C H 0.6630 0.2478 0.7395 0.033 Uiso 1 1 calc R U . . .
C44 C 0.8584(3) 0.2708(2) 0.6039(3) 0.0310(10) Uani 1 1 d . . . . .
H44A H 0.8275 0.3026 0.6299 0.037 Uiso 1 1 calc R U . . .
H44B H 0.9198 0.2637 0.6404 0.037 Uiso 1 1 calc R U . . .
H44C H 0.8658 0.2814 0.5435 0.037 Uiso 1 1 calc R U . . .
C45 C 0.9061(3) 0.1434(2) 0.5283(3) 0.0348(11) Uani 1 1 d . . . . .
H45A H 0.9028 0.1024 0.5107 0.042 Uiso 1 1 calc R U . . .
H45B H 0.9085 0.1678 0.4762 0.042 Uiso 1 1 calc R U . . .
H45C H 0.9622 0.1500 0.5731 0.042 Uiso 1 1 calc R U . . .
C46 C 0.7442(4) 0.05342(19) 0.5614(3) 0.0343(10) Uani 1 1 d . . . . .
H46A H 0.7974 0.0435 0.5331 0.041 Uiso 1 1 calc R U . . .
H46B H 0.7483 0.0315 0.6169 0.041 Uiso 1 1 calc R U . . .
H46C H 0.6860 0.0435 0.5212 0.041 Uiso 1 1 calc R U . . .
C47 C 0.5929(3) 0.1268(2) 0.6521(3) 0.0295(9) Uani 1 1 d . . . . .
H47A H 0.5612 0.1583 0.6781 0.035 Uiso 1 1 calc R U . . .
H47B H 0.5508 0.1107 0.6006 0.035 Uiso 1 1 calc R U . . .
H47C H 0.6106 0.0962 0.6965 0.035 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrystalClear-SM Expert 2.0 r15 (Rigaku, 2011)'
_computing_cell_refinement       'CrystalClear-SM Expert 2.0 r15'
_computing_data_reduction        'CrystalClear-SM Expert 2.0 r15'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.776(3) . ?
Ti1 Cl2 2.2787(16) . ?
Ti1 Cl1 2.2830(16) . ?
Ti1 C14 2.336(4) . ?
Ti1 C10 2.341(4) . ?
Ti1 C11 2.368(4) . ?
Ti1 C13 2.396(4) . ?
Ti1 C12 2.402(5) . ?
Ti2 O2 1.804(3) . ?
Ti2 O3 1.807(3) . ?
Ti2 Cl3 2.3139(14) . ?
Ti2 C42 2.332(4) . ?
Ti2 C41 2.371(4) . ?
Ti2 C40 2.387(4) . ?
Ti2 C39 2.396(4) . ?
Ti2 C38 2.396(4) . ?
O1 C3 1.365(5) . ?
O2 C22 1.368(5) . ?
O3 C31 1.353(5) . ?
N1 C1 1.461(5) . ?
N1 C20 1.471(5) . ?
N1 C29 1.474(5) . ?
C1 C2 1.502(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C3 1.401(6) . ?
C2 C7 1.403(5) . ?
C3 C4 1.408(6) . ?
C4 C5 1.393(6) . ?
C4 C9 1.513(6) . ?
C5 C6 1.383(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.390(6) . ?
C6 C8 1.518(6) . ?
C7 H7 0.9300 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C10 C11 1.405(6) . ?
C10 C14 1.417(6) . ?
C10 C15 1.504(6) . ?
C11 C12 1.427(6) . ?
C11 C16 1.505(6) . ?
C12 C13 1.408(7) . ?
C12 C17 1.491(7) . ?
C13 C14 1.422(6) . ?
C13 C18 1.491(6) . ?
C14 C19 1.502(6) . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.522(5) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C26 1.394(6) . ?
C21 C22 1.398(6) . ?
C22 C23 1.402(6) . ?
C23 C24 1.393(6) . ?
C23 C28 1.506(6) . ?
C24 C25 1.387(6) . ?
C24 H24 0.9300 . ?
C25 C26 1.382(6) . ?
C25 C27 1.525(6) . ?
C26 H26 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 C30 1.519(5) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C35 1.392(5) . ?
C30 C31 1.399(5) . ?
C31 C32 1.406(5) . ?
C32 C33 1.403(6) . ?
C32 C37 1.508(6) . ?
C33 C34 1.381(6) . ?
C33 H33 0.9300 . ?
C34 C35 1.398(5) . ?
C34 C36 1.511(6) . ?
C35 H35 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 C39 1.422(6) . ?
C38 C42 1.429(6) . ?
C38 C44 1.496(6) . ?
C39 C40 1.445(6) . ?
C39 C45 1.491(6) . ?
C40 C41 1.405(6) . ?
C40 C46 1.502(6) . ?
C41 C42 1.410(6) . ?
C41 C47 1.496(6) . ?
C42 C43 1.511(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 Cl2 102.46(10) . . ?
O1 Ti1 Cl1 102.66(10) . . ?
Cl2 Ti1 Cl1 103.16(5) . . ?
O1 Ti1 C14 103.10(15) . . ?
Cl2 Ti1 C14 94.81(11) . . ?
Cl1 Ti1 C14 144.39(12) . . ?
O1 Ti1 C10 88.38(14) . . ?
Cl2 Ti1 C10 129.64(12) . . ?
Cl1 Ti1 C10 122.39(12) . . ?
C14 Ti1 C10 35.28(15) . . ?
O1 Ti1 C11 109.37(15) . . ?
Cl2 Ti1 C11 141.76(11) . . ?
Cl1 Ti1 C11 90.19(12) . . ?
C14 Ti1 C11 58.11(16) . . ?
C10 Ti1 C11 34.70(16) . . ?
O1 Ti1 C13 137.98(15) . . ?
Cl2 Ti1 C13 84.62(12) . . ?
Cl1 Ti1 C13 116.11(13) . . ?
C14 Ti1 C13 34.93(15) . . ?
C10 Ti1 C13 57.97(15) . . ?
C11 Ti1 C13 57.55(15) . . ?
O1 Ti1 C12 143.63(15) . . ?
Cl2 Ti1 C12 109.28(12) . . ?
Cl1 Ti1 C12 87.18(12) . . ?
C14 Ti1 C12 57.71(16) . . ?
C10 Ti1 C12 57.75(16) . . ?
C11 Ti1 C12 34.81(15) . . ?
C13 Ti1 C12 34.13(16) . . ?
O2 Ti2 O3 108.14(12) . . ?
O2 Ti2 Cl3 100.79(10) . . ?
O3 Ti2 Cl3 100.50(10) . . ?
O2 Ti2 C42 100.93(14) . . ?
O3 Ti2 C42 100.66(14) . . ?
Cl3 Ti2 C42 143.03(11) . . ?
O2 Ti2 C41 85.92(13) . . ?
O3 Ti2 C41 135.48(14) . . ?
Cl3 Ti2 C41 118.52(11) . . ?
C42 Ti2 C41 34.88(14) . . ?
O2 Ti2 C40 106.57(14) . . ?
O3 Ti2 C40 142.11(14) . . ?
Cl3 Ti2 C40 87.42(11) . . ?
C42 Ti2 C40 57.78(14) . . ?
C41 Ti2 C40 34.35(14) . . ?
O2 Ti2 C39 141.20(14) . . ?
O3 Ti2 C39 107.75(14) . . ?
Cl3 Ti2 C39 86.69(11) . . ?
C42 Ti2 C39 58.04(14) . . ?
C41 Ti2 C39 57.88(14) . . ?
C40 Ti2 C39 35.18(14) . . ?
O2 Ti2 C38 136.07(13) . . ?
O3 Ti2 C38 86.28(14) . . ?
Cl3 Ti2 C38 117.49(11) . . ?
C42 Ti2 C38 35.16(14) . . ?
C41 Ti2 C38 57.97(14) . . ?
C40 Ti2 C38 57.85(14) . . ?
C39 Ti2 C38 34.52(14) . . ?
C3 O1 Ti1 172.4(3) . . ?
C22 O2 Ti2 173.9(3) . . ?
C31 O3 Ti2 174.0(3) . . ?
C1 N1 C20 112.2(3) . . ?
C1 N1 C29 110.3(3) . . ?
C20 N1 C29 110.0(3) . . ?
N1 C1 C2 113.5(3) . . ?
N1 C1 H1A 108.9 . . ?
C2 C1 H1A 108.9 . . ?
N1 C1 H1B 108.9 . . ?
C2 C1 H1B 108.9 . . ?
H1A C1 H1B 107.7 . . ?
C3 C2 C7 117.4(4) . . ?
C3 C2 C1 121.7(3) . . ?
C7 C2 C1 120.8(3) . . ?
O1 C3 C2 120.1(4) . . ?
O1 C3 C4 118.2(4) . . ?
C2 C3 C4 121.7(4) . . ?
C5 C4 C3 118.0(4) . . ?
C5 C4 C9 122.0(4) . . ?
C3 C4 C9 120.0(4) . . ?
C6 C5 C4 122.1(4) . . ?
C6 C5 H5 119.0 . . ?
C4 C5 H5 119.0 . . ?
C5 C6 C7 118.5(4) . . ?
C5 C6 C8 121.6(4) . . ?
C7 C6 C8 119.8(4) . . ?
C6 C7 C2 122.2(4) . . ?
C6 C7 H7 118.9 . . ?
C2 C7 H7 118.9 . . ?
C6 C8 H8A 109.5 . . ?
C6 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C6 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C11 C10 C14 108.1(4) . . ?
C11 C10 C15 125.9(4) . . ?
C14 C10 C15 125.9(4) . . ?
C11 C10 Ti1 73.7(3) . . ?
C14 C10 Ti1 72.2(2) . . ?
C15 C10 Ti1 121.5(3) . . ?
C10 C11 C12 108.0(4) . . ?
C10 C11 C16 127.0(4) . . ?
C12 C11 C16 124.8(4) . . ?
C10 C11 Ti1 71.6(2) . . ?
C12 C11 Ti1 73.9(3) . . ?
C16 C11 Ti1 124.0(3) . . ?
C13 C12 C11 108.0(4) . . ?
C13 C12 C17 126.0(5) . . ?
C11 C12 C17 125.8(5) . . ?
C13 C12 Ti1 72.7(3) . . ?
C11 C12 Ti1 71.3(2) . . ?
C17 C12 Ti1 125.3(3) . . ?
C12 C13 C14 107.9(4) . . ?
C12 C13 C18 126.4(5) . . ?
C14 C13 C18 125.6(5) . . ?
C12 C13 Ti1 73.1(3) . . ?
C14 C13 Ti1 70.2(2) . . ?
C18 C13 Ti1 125.7(3) . . ?
C10 C14 C13 108.0(4) . . ?
C10 C14 C19 125.7(4) . . ?
C13 C14 C19 126.2(4) . . ?
C10 C14 Ti1 72.6(2) . . ?
C13 C14 Ti1 74.9(3) . . ?
C19 C14 Ti1 120.8(3) . . ?
C10 C15 H15A 109.5 . . ?
C10 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C10 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C11 C16 H16A 109.5 . . ?
C11 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C11 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C12 C17 H17A 109.5 . . ?
C12 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C12 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C13 C18 H18A 109.5 . . ?
C13 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C13 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C14 C19 H19A 109.5 . . ?
C14 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C14 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N1 C20 C21 113.8(3) . . ?
N1 C20 H20A 108.8 . . ?
C21 C20 H20A 108.8 . . ?
N1 C20 H20B 108.8 . . ?
C21 C20 H20B 108.8 . . ?
H20A C20 H20B 107.7 . . ?
C26 C21 C22 118.4(4) . . ?
C26 C21 C20 121.1(4) . . ?
C22 C21 C20 120.5(3) . . ?
O2 C22 C21 119.5(3) . . ?
O2 C22 C23 119.1(4) . . ?
C21 C22 C23 121.4(4) . . ?
C24 C23 C22 117.7(4) . . ?
C24 C23 C28 121.7(4) . . ?
C22 C23 C28 120.5(4) . . ?
C25 C24 C23 122.2(4) . . ?
C25 C24 H24 118.9 . . ?
C23 C24 H24 118.9 . . ?
C26 C25 C24 118.5(4) . . ?
C26 C25 C27 120.5(4) . . ?
C24 C25 C27 120.9(4) . . ?
C25 C26 C21 121.8(4) . . ?
C25 C26 H26 119.1 . . ?
C21 C26 H26 119.1 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C23 C28 H28A 109.5 . . ?
C23 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C23 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
N1 C29 C30 112.9(3) . . ?
N1 C29 H29A 109.0 . . ?
C30 C29 H29A 109.0 . . ?
N1 C29 H29B 109.0 . . ?
C30 C29 H29B 109.0 . . ?
H29A C29 H29B 107.8 . . ?
C35 C30 C31 119.3(4) . . ?
C35 C30 C29 120.9(3) . . ?
C31 C30 C29 119.7(3) . . ?
O3 C31 C30 119.9(3) . . ?
O3 C31 C32 119.3(3) . . ?
C30 C31 C32 120.8(4) . . ?
C33 C32 C31 117.5(4) . . ?
C33 C32 C37 120.8(4) . . ?
C31 C32 C37 121.6(4) . . ?
C34 C33 C32 123.0(4) . . ?
C34 C33 H33 118.5 . . ?
C32 C33 H33 118.5 . . ?
C33 C34 C35 117.9(4) . . ?
C33 C34 C36 121.0(4) . . ?
C35 C34 C36 121.1(4) . . ?
C30 C35 C34 121.5(4) . . ?
C30 C35 H35 119.3 . . ?
C34 C35 H35 119.3 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C32 C37 H37A 109.5 . . ?
C32 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
C32 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
C39 C38 C42 107.2(4) . . ?
C39 C38 C44 126.9(4) . . ?
C42 C38 C44 126.0(4) . . ?
C39 C38 Ti2 72.7(2) . . ?
C42 C38 Ti2 70.0(2) . . ?
C44 C38 Ti2 123.1(3) . . ?
C38 C39 C40 107.6(3) . . ?
C38 C39 C45 126.3(4) . . ?
C40 C39 C45 126.1(4) . . ?
C38 C39 Ti2 72.7(2) . . ?
C40 C39 Ti2 72.1(2) . . ?
C45 C39 Ti2 123.2(3) . . ?
C41 C40 C39 108.0(4) . . ?
C41 C40 C46 127.1(4) . . ?
C39 C40 C46 124.7(4) . . ?
C41 C40 Ti2 72.2(2) . . ?
C39 C40 Ti2 72.7(2) . . ?
C46 C40 Ti2 123.9(3) . . ?
C40 C41 C42 108.2(4) . . ?
C40 C41 C47 126.9(4) . . ?
C42 C41 C47 124.9(4) . . ?
C40 C41 Ti2 73.4(2) . . ?
C42 C41 Ti2 71.1(2) . . ?
C47 C41 Ti2 121.3(3) . . ?
C41 C42 C38 108.9(4) . . ?
C41 C42 C43 124.9(4) . . ?
C38 C42 C43 125.9(4) . . ?
C41 C42 Ti2 74.1(2) . . ?
C38 C42 Ti2 74.9(2) . . ?
C43 C42 Ti2 122.4(3) . . ?
C42 C43 H43A 109.5 . . ?
C42 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C42 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C38 C44 H44A 109.5 . . ?
C38 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C38 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C39 C45 H45A 109.5 . . ?
C39 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C39 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C40 C46 H46A 109.5 . . ?
C40 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C40 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C41 C47 H47A 109.5 . . ?
C41 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C41 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 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
C20 N1 C1 C2 -70.1(4) . . . . ?
C29 N1 C1 C2 166.9(3) . . . . ?
N1 C1 C2 C3 134.1(4) . . . . ?
N1 C1 C2 C7 -43.6(5) . . . . ?
C7 C2 C3 O1 175.8(3) . . . . ?
C1 C2 C3 O1 -2.0(6) . . . . ?
C7 C2 C3 C4 -1.6(6) . . . . ?
C1 C2 C3 C4 -179.4(4) . . . . ?
O1 C3 C4 C5 -174.8(4) . . . . ?
C2 C3 C4 C5 2.7(6) . . . . ?
O1 C3 C4 C9 4.8(6) . . . . ?
C2 C3 C4 C9 -177.7(4) . . . . ?
C3 C4 C5 C6 -1.3(6) . . . . ?
C9 C4 C5 C6 179.1(4) . . . . ?
C4 C5 C6 C7 -1.0(6) . . . . ?
C4 C5 C6 C8 176.2(4) . . . . ?
C5 C6 C7 C2 2.1(6) . . . . ?
C8 C6 C7 C2 -175.1(4) . . . . ?
C3 C2 C7 C6 -0.8(6) . . . . ?
C1 C2 C7 C6 177.0(4) . . . . ?
C14 C10 C11 C12 -1.0(5) . . . . ?
C15 C10 C11 C12 177.2(4) . . . . ?
Ti1 C10 C11 C12 -65.4(3) . . . . ?
C14 C10 C11 C16 -176.4(4) . . . . ?
C15 C10 C11 C16 1.8(7) . . . . ?
Ti1 C10 C11 C16 119.2(4) . . . . ?
C14 C10 C11 Ti1 64.4(3) . . . . ?
C15 C10 C11 Ti1 -117.4(4) . . . . ?
C10 C11 C12 C13 0.0(5) . . . . ?
C16 C11 C12 C13 175.5(4) . . . . ?
Ti1 C11 C12 C13 -63.9(3) . . . . ?
C10 C11 C12 C17 -175.5(4) . . . . ?
C16 C11 C12 C17 0.0(7) . . . . ?
Ti1 C11 C12 C17 120.6(5) . . . . ?
C10 C11 C12 Ti1 63.9(3) . . . . ?
C16 C11 C12 Ti1 -120.6(4) . . . . ?
C11 C12 C13 C14 1.0(5) . . . . ?
C17 C12 C13 C14 176.5(5) . . . . ?
Ti1 C12 C13 C14 -62.0(3) . . . . ?
C11 C12 C13 C18 -174.7(5) . . . . ?
C17 C12 C13 C18 0.7(8) . . . . ?
Ti1 C12 C13 C18 122.3(5) . . . . ?
C11 C12 C13 Ti1 63.0(3) . . . . ?
C17 C12 C13 Ti1 -121.5(5) . . . . ?
C11 C10 C14 C13 1.6(5) . . . . ?
C15 C10 C14 C13 -176.6(4) . . . . ?
Ti1 C10 C14 C13 67.1(3) . . . . ?
C11 C10 C14 C19 178.7(4) . . . . ?
C15 C10 C14 C19 0.5(7) . . . . ?
Ti1 C10 C14 C19 -115.8(4) . . . . ?
C11 C10 C14 Ti1 -65.4(3) . . . . ?
C15 C10 C14 Ti1 116.4(4) . . . . ?
C12 C13 C14 C10 -1.6(5) . . . . ?
C18 C13 C14 C10 174.2(4) . . . . ?
Ti1 C13 C14 C10 -65.5(3) . . . . ?
C12 C13 C14 C19 -178.7(4) . . . . ?
C18 C13 C14 C19 -2.9(7) . . . . ?
Ti1 C13 C14 C19 117.4(4) . . . . ?
C12 C13 C14 Ti1 63.9(3) . . . . ?
C18 C13 C14 Ti1 -120.3(5) . . . . ?
C1 N1 C20 C21 79.9(4) . . . . ?
C29 N1 C20 C21 -156.9(3) . . . . ?
N1 C20 C21 C26 -117.4(4) . . . . ?
N1 C20 C21 C22 61.5(5) . . . . ?
C26 C21 C22 O2 177.2(3) . . . . ?
C20 C21 C22 O2 -1.7(5) . . . . ?
C26 C21 C22 C23 -1.4(6) . . . . ?
C20 C21 C22 C23 179.7(3) . . . . ?
O2 C22 C23 C24 -176.0(3) . . . . ?
C21 C22 C23 C24 2.5(6) . . . . ?
O2 C22 C23 C28 1.8(6) . . . . ?
C21 C22 C23 C28 -179.7(4) . . . . ?
C22 C23 C24 C25 -1.5(6) . . . . ?
C28 C23 C24 C25 -179.3(4) . . . . ?
C23 C24 C25 C26 -0.7(6) . . . . ?
C23 C24 C25 C27 176.6(4) . . . . ?
C24 C25 C26 C21 2.0(6) . . . . ?
C27 C25 C26 C21 -175.3(4) . . . . ?
C22 C21 C26 C25 -1.0(6) . . . . ?
C20 C21 C26 C25 177.9(4) . . . . ?
C1 N1 C29 C30 -71.1(4) . . . . ?
C20 N1 C29 C30 164.6(3) . . . . ?
N1 C29 C30 C35 120.3(4) . . . . ?
N1 C29 C30 C31 -62.8(5) . . . . ?
C35 C30 C31 O3 179.9(3) . . . . ?
C29 C30 C31 O3 2.9(5) . . . . ?
C35 C30 C31 C32 -1.2(6) . . . . ?
C29 C30 C31 C32 -178.2(3) . . . . ?
O3 C31 C32 C33 178.5(3) . . . . ?
C30 C31 C32 C33 -0.3(6) . . . . ?
O3 C31 C32 C37 -2.8(6) . . . . ?
C30 C31 C32 C37 178.3(4) . . . . ?
C31 C32 C33 C34 1.4(6) . . . . ?
C37 C32 C33 C34 -177.3(4) . . . . ?
C32 C33 C34 C35 -0.8(6) . . . . ?
C32 C33 C34 C36 179.6(4) . . . . ?
C31 C30 C35 C34 1.8(6) . . . . ?
C29 C30 C35 C34 178.8(3) . . . . ?
C33 C34 C35 C30 -0.8(6) . . . . ?
C36 C34 C35 C30 178.8(4) . . . . ?
C42 C38 C39 C40 -2.2(4) . . . . ?
C44 C38 C39 C40 177.1(4) . . . . ?
Ti2 C38 C39 C40 -64.1(3) . . . . ?
C42 C38 C39 C45 -179.2(4) . . . . ?
C44 C38 C39 C45 0.1(7) . . . . ?
Ti2 C38 C39 C45 118.9(4) . . . . ?
C42 C38 C39 Ti2 61.9(3) . . . . ?
C44 C38 C39 Ti2 -118.8(4) . . . . ?
C38 C39 C40 C41 0.5(4) . . . . ?
C45 C39 C40 C41 177.5(4) . . . . ?
Ti2 C39 C40 C41 -64.0(3) . . . . ?
C38 C39 C40 C46 -175.7(4) . . . . ?
C45 C39 C40 C46 1.3(7) . . . . ?
Ti2 C39 C40 C46 119.7(4) . . . . ?
C38 C39 C40 Ti2 64.6(3) . . . . ?
C45 C39 C40 Ti2 -118.5(4) . . . . ?
C39 C40 C41 C42 1.4(4) . . . . ?
C46 C40 C41 C42 177.6(4) . . . . ?
Ti2 C40 C41 C42 -63.0(3) . . . . ?
C39 C40 C41 C47 -178.6(4) . . . . ?
C46 C40 C41 C47 -2.4(7) . . . . ?
Ti2 C40 C41 C47 117.1(4) . . . . ?
C39 C40 C41 Ti2 64.4(3) . . . . ?
C46 C40 C41 Ti2 -119.5(4) . . . . ?
C40 C41 C42 C38 -2.8(4) . . . . ?
C47 C41 C42 C38 177.1(4) . . . . ?
Ti2 C41 C42 C38 -67.4(3) . . . . ?
C40 C41 C42 C43 -176.7(4) . . . . ?
C47 C41 C42 C43 3.3(6) . . . . ?
Ti2 C41 C42 C43 118.8(4) . . . . ?
C40 C41 C42 Ti2 64.5(3) . . . . ?
C47 C41 C42 Ti2 -115.5(4) . . . . ?
C39 C38 C42 C41 3.1(4) . . . . ?
C44 C38 C42 C41 -176.2(4) . . . . ?
Ti2 C38 C42 C41 66.8(3) . . . . ?
C39 C38 C42 C43 177.0(4) . . . . ?
C44 C38 C42 C43 -2.4(7) . . . . ?
Ti2 C38 C42 C43 -119.3(4) . . . . ?
C39 C38 C42 Ti2 -63.7(3) . . . . ?
C44 C38 C42 Ti2 117.0(4) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 0.000 0.000 0.000 257.7 -1.0
2 0.000 0.500 0.500 257.7 -0.6
3 0.088 0.667 0.201 15.0 -0.3
4 0.088 0.833 0.701 15.1 -0.3
5 0.444 0.035 0.024 13.6 -0.1
6 0.444 0.465 0.524 13.3 -0.3
7 0.561 0.538 0.474 13.1 -0.3
8 0.561 0.962 0.974 12.7 -0.5
9 0.912 0.167 0.298 14.9 -0.5
10 0.912 0.333 0.798 15.1 -0.7
_platon_squeeze_details          
; ?
;

#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
####################################################################### 
# 
# 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_Ti5
_database_code_depnum_ccdc_archive 'CCDC 1549585'
_audit_update_record             
;
2017-05-12 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;

#==============================================================================
# CHEMICAL DATA

_chemical_formula_sum            'C75 H111 Cl6 N O3 Ti3'
_chemical_formula_moiety         'C75 H111 Cl6 N O3 Ti3'
_chemical_formula_weight         1431.12
_chemical_melting_point          ?

#==============================================================================
# CRYSTAL DATA
_space_group_crystal_system      monoclinic
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
_space_group_IT_number           14
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2-Z
3 -X,-Y,-Z
4 -1/2+X,-1/2-Y,-1/2+Z
#------------------------------------------------------------------------------
_cell_length_a                   17.5836(9)
_cell_length_b                   22.4075(10)
_cell_length_c                   21.6663(10)
_cell_angle_alpha                90.0000
_cell_angle_beta                 94.814(4)
_cell_angle_gamma                90.0000
_cell_volume                     8506.5(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8223
_cell_measurement_theta_min      1.84
_cell_measurement_theta_max      30.92
_cell_measurement_temperature    93
#------------------------------------------------------------------------------
_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.190
_exptl_crystal_size_min          0.100
_exptl_crystal_density_diffrn    1.117
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3040.00
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.929
_exptl_absorpt_correction_T_max  0.951

#==============================================================================
# EXPERIMENTAL DATA

_diffrn_ambient_temperature      93
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_device_type  'Rigaku XtaLAB mini'
_diffrn_measurement_method       ω
_diffrn_detector_area_resol_mean 13.653
_diffrn_reflns_number            89388
_diffrn_reflns_av_R_equivalents  0.1354
_diffrn_reflns_theta_max         27.499
_diffrn_reflns_theta_min         2.599
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_standards_number         0
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_reflns_number_total             19531
_reflns_number_gt                10706
_reflns_threshold_expression     F²>2.0σ(F²)
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

#==============================================================================
# REFINEMENT DATA

_refine_special_details          
;Refinement was performed using all reflections. The weighted 
    R-factor (wR) and goodness of fit (S) are based on F².
    R-factor (gt) are based on F. The threshold expression of
    F² > 2.0 sigma(F²) is used only for calculating R-factor (gt)., SQUEEZE
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_R_factor_all          0.1382
_refine_ls_R_factor_gt           0.0757
_refine_ls_wR_factor_ref         0.2209
_refine_ls_wR_factor_gt          0.1910
_refine_ls_number_restraints     48
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_reflns         19531
_refine_ls_number_parameters     793
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w = 1/[σ²(Fo²)+(0.1099P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_refine_ls_shift/su_max          0.001
_refine_diff_density_max         1.23
_refine_diff_density_min         -0.55
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(Vol. C, Table 6.1.1.4)
;
Cl Cl 0.1484 0.1585
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Ti Ti 0.2776 0.4457
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;

#==============================================================================
# ATOMIC COORDINATES AND THERMAL PARAMETERS

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 0.48107(4) 0.07514(3) 0.25411(4) 0.01671(18) Uani 1 1 d . . . . .
Ti2 Ti 0.65054(5) 0.29990(4) 0.47561(4) 0.01875(19) Uani 1 1 d . . . . .
Ti3 Ti 0.81685(4) 0.25585(3) 0.19045(4) 0.01815(19) Uani 1 1 d . . . . .
Cl1 Cl 0.58178(7) 0.09334(5) 0.32349(5) 0.0284(3) Uani 1 1 d . . . . .
Cl2 Cl 0.42210(7) 0.00010(5) 0.30188(6) 0.0286(3) Uani 1 1 d . . . . .
Cl3 Cl 0.70457(7) 0.23047(5) 0.41751(5) 0.0266(3) Uani 1 1 d . . . . .
Cl4 Cl 0.75169(7) 0.33116(6) 0.53902(6) 0.0312(3) Uani 1 1 d . . . . .
Cl5 Cl 0.88700(7) 0.19674(5) 0.13181(6) 0.0296(3) Uani 1 1 d . . . . .
Cl6 Cl 0.78373(7) 0.19132(5) 0.26341(6) 0.0263(3) Uani 1 1 d . . . . .
O1 O 0.42014(16) 0.13792(12) 0.26351(13) 0.0175(6) Uani 1 1 d . . . . .
O2 O 0.63557(17) 0.36217(13) 0.42411(13) 0.0200(7) Uani 1 1 d . . . . .
O3 O 0.73059(16) 0.26516(13) 0.14145(13) 0.0182(7) Uani 1 1 d . . . . .
N1 N 0.54732(19) 0.29758(15) 0.25114(16) 0.0161(8) Uani 1 1 d . . . . .
C1 C 0.5093(2) 0.23923(18) 0.2472(2) 0.0167(9) Uani 1 1 d . . . . .
H1A H 0.5346 0.2122 0.2787 0.020 Uiso 1 1 calc R U . . .
H1B H 0.5146 0.2216 0.2059 0.020 Uiso 1 1 calc R U . . .
C2 C 0.4263(2) 0.24401(18) 0.25743(19) 0.0161(9) Uani 1 1 d . . . . .
C3 C 0.3826(3) 0.19179(19) 0.26434(19) 0.0190(9) Uani 1 1 d . . . . .
C4 C 0.3034(2) 0.19508(18) 0.27205(19) 0.0156(9) Uani 1 1 d . . . . .
C5 C 0.2728(3) 0.2523(2) 0.2748(2) 0.0209(10) Uani 1 1 d . . . . .
H5 H 0.2200 0.2558 0.2804 0.025 Uiso 1 1 calc R U . . .
C6 C 0.3141(3) 0.3043(2) 0.2698(2) 0.0223(10) Uani 1 1 d . . . . .
C7 C 0.3912(3) 0.2986(2) 0.2599(2) 0.0223(10) Uani 1 1 d . . . . .
H7 H 0.4203 0.3336 0.2547 0.027 Uiso 1 1 calc R U . . .
C8 C 0.2797(3) 0.3672(2) 0.2740(2) 0.0259(11) Uani 1 1 d . . . . .
C9 C 0.2893(3) 0.4024(2) 0.2144(3) 0.0409(14) Uani 1 1 d . . . . .
H9A H 0.3435 0.4043 0.2072 0.049 Uiso 1 1 calc R U . . .
H9B H 0.2611 0.3824 0.1793 0.049 Uiso 1 1 calc R U . . .
H9C H 0.2694 0.4429 0.2185 0.049 Uiso 1 1 calc R U . . .
C10 C 0.3219(3) 0.4003(2) 0.3291(3) 0.0449(16) Uani 1 1 d . . . . .
H10A H 0.3766 0.4018 0.3235 0.054 Uiso 1 1 calc R U . . .
H10B H 0.3020 0.4410 0.3313 0.054 Uiso 1 1 calc R U . . .
H10C H 0.3140 0.3791 0.3676 0.054 Uiso 1 1 calc R U . . .
C11 C 0.1958(3) 0.3653(2) 0.2833(3) 0.0361(13) Uani 1 1 d . . . . .
H11A H 0.1881 0.3431 0.3212 0.043 Uiso 1 1 calc R U . . .
H11B H 0.1766 0.4061 0.2870 0.043 Uiso 1 1 calc R U . . .
H11C H 0.1682 0.3456 0.2478 0.043 Uiso 1 1 calc R U . . .
C12 C 0.2541(2) 0.1399(2) 0.2804(2) 0.0212(10) Uani 1 1 d . . . . .
C13 C 0.2594(3) 0.0969(2) 0.2252(2) 0.0246(10) Uani 1 1 d . . . . .
H13A H 0.2277 0.0617 0.2308 0.030 Uiso 1 1 calc R U . . .
H13B H 0.2414 0.1172 0.1866 0.030 Uiso 1 1 calc R U . . .
H13C H 0.3126 0.0845 0.2230 0.030 Uiso 1 1 calc R U . . .
C14 C 0.2807(3) 0.1084(2) 0.3415(2) 0.0314(12) Uani 1 1 d . . . . .
H14A H 0.2490 0.0731 0.3467 0.038 Uiso 1 1 calc R U . . .
H14B H 0.3341 0.0962 0.3406 0.038 Uiso 1 1 calc R U . . .
H14C H 0.2760 0.1358 0.3762 0.038 Uiso 1 1 calc R U . . .
C15 C 0.1693(3) 0.1558(2) 0.2819(2) 0.0288(11) Uani 1 1 d . . . . .
H15A H 0.1398 0.1194 0.2872 0.035 Uiso 1 1 calc R U . . .
H15B H 0.1630 0.1831 0.3165 0.035 Uiso 1 1 calc R U . . .
H15C H 0.1510 0.1752 0.2429 0.035 Uiso 1 1 calc R U . . .
C16 C 0.4784(2) 0.09386(18) 0.1473(2) 0.0175(9) Uani 1 1 d . . . . .
C17 C 0.5569(3) 0.09116(19) 0.1696(2) 0.0194(10) Uani 1 1 d . . . . .
C18 C 0.5738(3) 0.03206(19) 0.1910(2) 0.0200(10) Uani 1 1 d . . . . .
C19 C 0.5068(3) -0.00175(19) 0.1811(2) 0.0219(10) Uani 1 1 d . . . . .
C20 C 0.4473(3) 0.03569(19) 0.1549(2) 0.0190(9) Uani 1 1 d . . . . .
C21 C 0.4371(3) 0.1461(2) 0.1173(2) 0.0245(10) Uani 1 1 d . . . . .
H21A H 0.4714 0.1806 0.1181 0.029 Uiso 1 1 calc R U . . .
H21B H 0.4201 0.1362 0.0743 0.029 Uiso 1 1 calc R U . . .
H21C H 0.3926 0.1557 0.1399 0.029 Uiso 1 1 calc R U . . .
C22 C 0.6163(3) 0.1392(2) 0.1662(2) 0.0270(11) Uani 1 1 d . . . . .
H22A H 0.5918 0.1760 0.1501 0.032 Uiso 1 1 calc R U . . .
H22B H 0.6412 0.1466 0.2077 0.032 Uiso 1 1 calc R U . . .
H22C H 0.6545 0.1264 0.1385 0.032 Uiso 1 1 calc R U . . .
C23 C 0.6503(3) 0.0107(2) 0.2144(2) 0.0299(12) Uani 1 1 d . . . . .
H23A H 0.6862 0.0443 0.2166 0.036 Uiso 1 1 calc R U . . .
H23B H 0.6479 -0.0065 0.2558 0.036 Uiso 1 1 calc R U . . .
H23C H 0.6675 -0.0198 0.1863 0.036 Uiso 1 1 calc R U . . .
C24 C 0.4998(3) -0.0676(2) 0.1921(2) 0.0314(12) Uani 1 1 d . . . . .
H24A H 0.4470 -0.0802 0.1815 0.038 Uiso 1 1 calc R U . . .
H24B H 0.5336 -0.0892 0.1661 0.038 Uiso 1 1 calc R U . . .
H24C H 0.5144 -0.0765 0.2358 0.038 Uiso 1 1 calc R U . . .
C25 C 0.3692(3) 0.0163(2) 0.1314(2) 0.0316(12) Uani 1 1 d . . . . .
H25A H 0.3396 0.0510 0.1158 0.038 Uiso 1 1 calc R U . . .
H25B H 0.3727 -0.0126 0.0978 0.038 Uiso 1 1 calc R U . . .
H25C H 0.3439 -0.0024 0.1651 0.038 Uiso 1 1 calc R U . . .
C26 C 0.5634(2) 0.31545(18) 0.31551(19) 0.0160(9) Uani 1 1 d . . . . .
H26A H 0.6081 0.2928 0.3338 0.019 Uiso 1 1 calc R U . . .
H26B H 0.5191 0.3050 0.3388 0.019 Uiso 1 1 calc R U . . .
C27 C 0.5791(2) 0.38069(19) 0.32259(19) 0.0177(9) Uani 1 1 d . . . . .
C28 C 0.6162(2) 0.40291(19) 0.3783(2) 0.0176(9) Uani 1 1 d . . . . .
C29 C 0.6340(3) 0.4643(2) 0.3850(2) 0.0241(10) Uani 1 1 d . . . . .
C30 C 0.6126(3) 0.5009(2) 0.3342(2) 0.0269(11) Uani 1 1 d . . . . .
H30 H 0.6239 0.5423 0.3378 0.032 Uiso 1 1 calc R U . . .
C31 C 0.5759(3) 0.4806(2) 0.2789(2) 0.0232(10) Uani 1 1 d . . . . .
C32 C 0.5598(3) 0.4203(2) 0.2749(2) 0.0227(10) Uani 1 1 d . . . . .
H32 H 0.5342 0.4053 0.2377 0.027 Uiso 1 1 calc R U . . .
C33 C 0.5580(3) 0.5239(2) 0.2246(2) 0.0347(11) Uani 1 1 d . U . . .
C34 C 0.5066(5) 0.4986(3) 0.1751(4) 0.089(2) Uani 1 1 d . U . . .
H34A H 0.5258 0.4595 0.1634 0.106 Uiso 1 1 calc R U . . .
H34B H 0.4556 0.4940 0.1896 0.106 Uiso 1 1 calc R U . . .
H34C H 0.5039 0.5253 0.1392 0.106 Uiso 1 1 calc R U . . .
C35 C 0.6333(4) 0.5387(4) 0.1950(4) 0.077(2) Uani 1 1 d . U . . .
H35A H 0.6701 0.5559 0.2265 0.092 Uiso 1 1 calc R U . . .
H35B H 0.6545 0.5020 0.1787 0.092 Uiso 1 1 calc R U . . .
H35C H 0.6228 0.5673 0.1612 0.092 Uiso 1 1 calc R U . . .
C36 C 0.5328(4) 0.5832(3) 0.2450(3) 0.0555(16) Uani 1 1 d . U . . .
H36A H 0.5692 0.5981 0.2782 0.067 Uiso 1 1 calc R U . . .
H36B H 0.5304 0.6110 0.2100 0.067 Uiso 1 1 calc R U . . .
H36C H 0.4822 0.5797 0.2604 0.067 Uiso 1 1 calc R U . . .
C37 C 0.6765(3) 0.4900(2) 0.4438(2) 0.0294(12) Uani 1 1 d . . . . .
C38 C 0.7578(3) 0.4630(2) 0.4510(2) 0.0365(13) Uani 1 1 d . . . . .
H38A H 0.7542 0.4194 0.4534 0.044 Uiso 1 1 calc R U . . .
H38B H 0.7852 0.4741 0.4152 0.044 Uiso 1 1 calc R U . . .
H38C H 0.7853 0.4783 0.4889 0.044 Uiso 1 1 calc R U . . .
C39 C 0.6872(4) 0.5576(2) 0.4404(3) 0.0502(17) Uani 1 1 d . . . . .
H39A H 0.7145 0.5675 0.4042 0.060 Uiso 1 1 calc R U . . .
H39B H 0.6372 0.5771 0.4369 0.060 Uiso 1 1 calc R U . . .
H39C H 0.7168 0.5715 0.4780 0.060 Uiso 1 1 calc R U . . .
C40 C 0.6338(3) 0.4761(2) 0.5008(2) 0.0363(13) Uani 1 1 d . . . . .
H40A H 0.6264 0.4329 0.5039 0.044 Uiso 1 1 calc R U . . .
H40B H 0.6637 0.4904 0.5381 0.044 Uiso 1 1 calc R U . . .
H40C H 0.5841 0.4961 0.4970 0.044 Uiso 1 1 calc R U . . .
C41 C 0.5240(2) 0.3028(2) 0.5018(2) 0.0186(9) Uani 1 1 d . . . . .
C42 C 0.5354(3) 0.2454(2) 0.4776(2) 0.0229(10) Uani 1 1 d . . . . .
C43 C 0.5896(3) 0.2152(2) 0.5178(2) 0.0270(11) Uani 1 1 d . . . . .
C44 C 0.6129(3) 0.2536(2) 0.5677(2) 0.0256(11) Uani 1 1 d . . . . .
C45 C 0.5724(3) 0.3082(2) 0.5572(2) 0.0216(10) Uani 1 1 d . . . . .
C46 C 0.4679(3) 0.3486(2) 0.4756(2) 0.0274(11) Uani 1 1 d . . . . .
H46A H 0.4717 0.3845 0.5014 0.033 Uiso 1 1 calc R U . . .
H46B H 0.4793 0.3587 0.4333 0.033 Uiso 1 1 calc R U . . .
H46C H 0.4161 0.3323 0.4748 0.033 Uiso 1 1 calc R U . . .
C47 C 0.4906(3) 0.2166(2) 0.4230(2) 0.0303(12) Uani 1 1 d . . . . .
H47A H 0.4565 0.2463 0.4020 0.036 Uiso 1 1 calc R U . . .
H47B H 0.5258 0.2014 0.3940 0.036 Uiso 1 1 calc R U . . .
H47C H 0.4602 0.1836 0.4375 0.036 Uiso 1 1 calc R U . . .
C48 C 0.6144(3) 0.1513(2) 0.5117(3) 0.0387(14) Uani 1 1 d . . . . .
H48A H 0.6526 0.1414 0.5457 0.046 Uiso 1 1 calc R U . . .
H48B H 0.5701 0.1249 0.5134 0.046 Uiso 1 1 calc R U . . .
H48C H 0.6365 0.1459 0.4720 0.046 Uiso 1 1 calc R U . . .
C49 C 0.6678(3) 0.2377(2) 0.6211(2) 0.0375(13) Uani 1 1 d . . . . .
H49A H 0.6744 0.2719 0.6493 0.045 Uiso 1 1 calc R U . . .
H49B H 0.6481 0.2036 0.6432 0.045 Uiso 1 1 calc R U . . .
H49C H 0.7171 0.2272 0.6060 0.045 Uiso 1 1 calc R U . . .
C50 C 0.5755(3) 0.3598(2) 0.6017(2) 0.0280(11) Uani 1 1 d . . . . .
H50A H 0.6141 0.3518 0.6360 0.034 Uiso 1 1 calc R U . . .
H50B H 0.5889 0.3963 0.5802 0.034 Uiso 1 1 calc R U . . .
H50C H 0.5256 0.3648 0.6180 0.034 Uiso 1 1 calc R U . . .
C51 C 0.6181(2) 0.2962(2) 0.21945(19) 0.0172(9) Uani 1 1 d . . . . .
H51A H 0.6468 0.2594 0.2315 0.021 Uiso 1 1 calc R U . . .
H51B H 0.6502 0.3308 0.2333 0.021 Uiso 1 1 calc R U . . .
C52 C 0.6034(2) 0.29802(18) 0.1498(2) 0.0176(9) Uani 1 1 d . . . . .
C53 C 0.6614(2) 0.28179(18) 0.11246(19) 0.0150(9) Uani 1 1 d . . . . .
C54 C 0.6479(3) 0.28041(19) 0.0472(2) 0.0199(10) Uani 1 1 d . . . . .
C55 C 0.5756(3) 0.2987(2) 0.0226(2) 0.0239(10) Uani 1 1 d . . . . .
H55 H 0.5655 0.2990 -0.0212 0.029 Uiso 1 1 calc R U . . .
C56 C 0.5174(3) 0.3165(2) 0.0587(2) 0.0215(10) Uani 1 1 d . . . . .
C57 C 0.5326(2) 0.31592(19) 0.1229(2) 0.0184(9) Uani 1 1 d . . . . .
H57 H 0.4941 0.3279 0.1485 0.022 Uiso 1 1 calc R U . . .
C58 C 0.4393(3) 0.3345(3) 0.0277(2) 0.0359(11) Uani 1 1 d . U . . .
C59 C 0.3857(4) 0.3551(4) 0.0717(3) 0.0699(19) Uani 1 1 d . U . . .
H59A H 0.3797 0.3241 0.1028 0.084 Uiso 1 1 calc R U . . .
H59B H 0.4055 0.3915 0.0923 0.084 Uiso 1 1 calc R U . . .
H59C H 0.3360 0.3635 0.0494 0.084 Uiso 1 1 calc R U . . .
C60 C 0.4068(4) 0.2787(3) -0.0072(4) 0.0734(19) Uani 1 1 d . U . . .
H60A H 0.4427 0.2652 -0.0364 0.088 Uiso 1 1 calc R U . . .
H60B H 0.3990 0.2468 0.0226 0.088 Uiso 1 1 calc R U . . .
H60C H 0.3579 0.2887 -0.0299 0.088 Uiso 1 1 calc R U . . .
C61 C 0.4479(4) 0.3833(4) -0.0203(4) 0.081(2) Uani 1 1 d . U . . .
H61A H 0.4836 0.3700 -0.0499 0.097 Uiso 1 1 calc R U . . .
H61B H 0.3981 0.3916 -0.0423 0.097 Uiso 1 1 calc R U . . .
H61C H 0.4676 0.4197 0.0006 0.097 Uiso 1 1 calc R U . . .
C62 C 0.7066(3) 0.2574(2) 0.0040(2) 0.0238(10) Uani 1 1 d . . . . .
C63 C 0.7233(3) 0.1920(2) 0.0188(2) 0.0290(11) Uani 1 1 d . . . . .
H63A H 0.7426 0.1881 0.0624 0.035 Uiso 1 1 calc R U . . .
H63B H 0.6764 0.1686 0.0112 0.035 Uiso 1 1 calc R U . . .
H63C H 0.7618 0.1772 -0.0076 0.035 Uiso 1 1 calc R U . . .
C64 C 0.6769(3) 0.2616(2) -0.0640(2) 0.0354(13) Uani 1 1 d . . . . .
H64A H 0.6657 0.3033 -0.0747 0.042 Uiso 1 1 calc R U . . .
H64B H 0.7157 0.2463 -0.0898 0.042 Uiso 1 1 calc R U . . .
H64C H 0.6302 0.2377 -0.0711 0.042 Uiso 1 1 calc R U . . .
C65 C 0.7804(3) 0.2951(2) 0.0120(2) 0.0312(12) Uani 1 1 d . . . . .
H65A H 0.8013 0.2936 0.0553 0.037 Uiso 1 1 calc R U . . .
H65B H 0.8178 0.2790 -0.0146 0.037 Uiso 1 1 calc R U . . .
H65C H 0.7687 0.3366 0.0004 0.037 Uiso 1 1 calc R U . . .
C66 C 0.8344(3) 0.35913(19) 0.1985(2) 0.0249(11) Uani 1 1 d . . . . .
C67 C 0.9019(3) 0.3349(2) 0.1767(2) 0.0299(12) Uani 1 1 d . . . . .
C68 C 0.9374(3) 0.2989(2) 0.2250(3) 0.0316(12) Uani 1 1 d . . . . .
C69 C 0.8933(3) 0.3000(2) 0.2751(2) 0.0244(10) Uani 1 1 d . . . . .
C70 C 0.8291(2) 0.33754(19) 0.2603(2) 0.0194(10) Uani 1 1 d . . . . .
C71 C 0.7811(3) 0.4016(2) 0.1638(3) 0.0394(14) Uani 1 1 d . . . . .
H71A H 0.7391 0.4114 0.1890 0.047 Uiso 1 1 calc R U . . .
H71B H 0.8087 0.4381 0.1547 0.047 Uiso 1 1 calc R U . . .
H71C H 0.7606 0.3831 0.1250 0.047 Uiso 1 1 calc R U . . .
C72 C 0.9343(4) 0.3493(3) 0.1179(3) 0.0572(19) Uani 1 1 d . . . . .
H72A H 0.9811 0.3262 0.1146 0.069 Uiso 1 1 calc R U . . .
H72B H 0.8972 0.3394 0.0831 0.069 Uiso 1 1 calc R U . . .
H72C H 0.9462 0.3920 0.1168 0.069 Uiso 1 1 calc R U . . .
C73 C 1.0117(3) 0.2651(3) 0.2249(3) 0.061(2) Uani 1 1 d . . . . .
H73A H 1.0330 0.2705 0.1849 0.073 Uiso 1 1 calc R U . . .
H73B H 1.0479 0.2802 0.2581 0.073 Uiso 1 1 calc R U . . .
H73C H 1.0025 0.2225 0.2316 0.073 Uiso 1 1 calc R U . . .
C74 C 0.9115(4) 0.2723(2) 0.3372(3) 0.0443(15) Uani 1 1 d . . . . .
H74A H 0.8699 0.2803 0.3635 0.053 Uiso 1 1 calc R U . . .
H74B H 0.9175 0.2291 0.3325 0.053 Uiso 1 1 calc R U . . .
H74C H 0.9591 0.2894 0.3565 0.053 Uiso 1 1 calc R U . . .
C75 C 0.7737(3) 0.3559(2) 0.3049(2) 0.0316(12) Uani 1 1 d . . . . .
H75A H 0.7346 0.3817 0.2839 0.038 Uiso 1 1 calc R U . . .
H75B H 0.7494 0.3204 0.3209 0.038 Uiso 1 1 calc R U . . .
H75C H 0.8006 0.3778 0.3393 0.038 Uiso 1 1 calc R U . . .


#==============================================================================
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL Version 2014/7 (Sheldrick, 2008)'
_computing_publication_material  'CrystalStructure 4.2 (Rigaku, 2015)'
_computing_molecular_graphics    'CrystalStructure 4.2'

#==============================================================================
# MOLECULAR GEOMETRY

_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 1.790(3) . ?
Ti1 Cl1 2.2616(14) . ?
Ti1 Cl2 2.2701(14) . ?
Ti1 C16 2.348(4) . ?
Ti1 C20 2.353(4) . ?
Ti1 C17 2.381(4) . ?
Ti1 C19 2.407(4) . ?
Ti1 C18 2.414(4) . ?
Ti2 O2 1.792(3) . ?
Ti2 Cl3 2.2602(14) . ?
Ti2 Cl4 2.2652(14) . ?
Ti2 C45 2.335(4) . ?
Ti2 C41 2.343(4) . ?
Ti2 C42 2.368(5) . ?
Ti2 C44 2.391(4) . ?
Ti2 C43 2.398(5) . ?
Ti3 O3 1.789(3) . ?
Ti3 Cl6 2.2546(14) . ?
Ti3 Cl5 2.2700(14) . ?
Ti3 C66 2.339(4) . ?
Ti3 C67 2.353(5) . ?
Ti3 C70 2.373(4) . ?
Ti3 C68 2.391(5) . ?
Ti3 C69 2.395(5) . ?
O1 C3 1.377(5) . ?
O2 C28 1.371(5) . ?
O3 C53 1.373(5) . ?
N1 C26 1.456(5) . ?
N1 C1 1.468(5) . ?
N1 C51 1.471(5) . ?
C1 C2 1.498(6) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 C7 1.373(6) . ?
C2 C3 1.415(6) . ?
C3 C4 1.417(6) . ?
C4 C5 1.394(6) . ?
C4 C12 1.530(6) . ?
C5 C6 1.382(6) . ?
C5 H5 0.9500 . ?
C6 C7 1.395(6) . ?
C6 C8 1.541(6) . ?
C7 H7 0.9500 . ?
C8 C11 1.506(7) . ?
C8 C9 1.533(7) . ?
C8 C10 1.542(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 C15 1.536(6) . ?
C12 C14 1.540(7) . ?
C12 C13 1.545(6) . ?
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 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 C20 1.428(6) . ?
C16 C17 1.425(6) . ?
C16 C21 1.497(6) . ?
C17 C18 1.426(6) . ?
C17 C22 1.506(6) . ?
C18 C19 1.401(6) . ?
C18 C23 1.477(6) . ?
C19 C20 1.422(6) . ?
C19 C24 1.502(6) . ?
C20 C25 1.489(6) . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C27 1.493(6) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 C32 1.382(6) . ?
C27 C28 1.412(6) . ?
C28 C29 1.417(6) . ?
C29 C30 1.398(7) . ?
C29 C37 1.534(6) . ?
C30 C31 1.390(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.383(6) . ?
C31 C33 1.537(6) . ?
C32 H32 0.9500 . ?
C33 C34 1.456(8) . ?
C33 C36 1.479(7) . ?
C33 C35 1.554(9) . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C35 H35A 0.9800 . ?
C35 H35B 0.9800 . ?
C35 H35C 0.9800 . ?
C36 H36A 0.9800 . ?
C36 H36B 0.9800 . ?
C36 H36C 0.9800 . ?
C37 C39 1.528(7) . ?
C37 C40 1.530(7) . ?
C37 C38 1.547(8) . ?
C38 H38A 0.9800 . ?
C38 H38B 0.9800 . ?
C38 H38C 0.9800 . ?
C39 H39A 0.9800 . ?
C39 H39B 0.9800 . ?
C39 H39C 0.9800 . ?
C40 H40A 0.9800 . ?
C40 H40B 0.9800 . ?
C40 H40C 0.9800 . ?
C41 C42 1.410(6) . ?
C41 C45 1.416(6) . ?
C41 C46 1.501(6) . ?
C42 C43 1.410(7) . ?
C42 C47 1.510(6) . ?
C43 C44 1.416(7) . ?
C43 C48 1.505(7) . ?
C44 C45 1.425(6) . ?
C44 C49 1.486(7) . ?
C45 C50 1.503(6) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 C52 1.509(6) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C57 1.389(6) . ?
C52 C53 1.402(6) . ?
C53 C54 1.414(6) . ?
C54 C55 1.398(6) . ?
C54 C62 1.539(6) . ?
C55 C56 1.397(6) . ?
C55 H55 0.9500 . ?
C56 C57 1.395(6) . ?
C56 C58 1.531(6) . ?
C57 H57 0.9500 . ?
C58 C59 1.471(8) . ?
C58 C61 1.526(8) . ?
C58 C60 1.546(9) . ?
C59 H59A 0.9800 . ?
C59 H59B 0.9800 . ?
C59 H59C 0.9800 . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 C64 1.523(6) . ?
C62 C63 1.524(6) . ?
C62 C65 1.545(7) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 C67 1.421(7) . ?
C66 C70 1.434(6) . ?
C66 C71 1.493(7) . ?
C67 C68 1.424(8) . ?
C67 C72 1.475(7) . ?
C68 C69 1.386(7) . ?
C68 C73 1.511(7) . ?
C69 C70 1.423(6) . ?
C69 C74 1.492(7) . ?
C70 C75 1.487(6) . ?
C71 H71A 0.9800 . ?
C71 H71B 0.9800 . ?
C71 H71C 0.9800 . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C73 H73A 0.9800 . ?
C73 H73B 0.9800 . ?
C73 H73C 0.9800 . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 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 Cl1 103.02(10) . . ?
O1 Ti1 Cl2 103.27(10) . . ?
Cl1 Ti1 Cl2 101.11(5) . . ?
O1 Ti1 C16 90.52(14) . . ?
Cl1 Ti1 C16 124.93(12) . . ?
Cl2 Ti1 C16 127.55(11) . . ?
O1 Ti1 C20 106.95(14) . . ?
Cl1 Ti1 C20 142.96(12) . . ?
Cl2 Ti1 C20 92.77(11) . . ?
C16 Ti1 C20 35.37(15) . . ?
O1 Ti1 C17 110.38(14) . . ?
Cl1 Ti1 C17 91.49(12) . . ?
Cl2 Ti1 C17 140.26(11) . . ?
C16 Ti1 C17 35.07(15) . . ?
C20 Ti1 C17 57.93(15) . . ?
O1 Ti1 C19 141.68(15) . . ?
Cl1 Ti1 C19 112.69(12) . . ?
Cl2 Ti1 C19 83.56(11) . . ?
C16 Ti1 C19 57.98(15) . . ?
C20 Ti1 C19 34.73(15) . . ?
C17 Ti1 C19 56.93(15) . . ?
O1 Ti1 C18 144.82(14) . . ?
Cl1 Ti1 C18 85.43(11) . . ?
Cl2 Ti1 C18 108.53(11) . . ?
C16 Ti1 C18 58.15(15) . . ?
C20 Ti1 C18 57.55(15) . . ?
C17 Ti1 C18 34.59(14) . . ?
C19 Ti1 C18 33.78(15) . . ?
O2 Ti2 Cl3 103.63(10) . . ?
O2 Ti2 Cl4 101.75(11) . . ?
Cl3 Ti2 Cl4 101.85(5) . . ?
O2 Ti2 C45 110.11(15) . . ?
Cl3 Ti2 C45 141.08(12) . . ?
Cl4 Ti2 C45 89.91(12) . . ?
O2 Ti2 C41 92.09(15) . . ?
Cl3 Ti2 C41 127.33(12) . . ?
Cl4 Ti2 C41 123.88(12) . . ?
C45 Ti2 C41 35.23(15) . . ?
O2 Ti2 C42 109.36(15) . . ?
Cl3 Ti2 C42 93.16(12) . . ?
Cl4 Ti2 C42 141.04(12) . . ?
C45 Ti2 C42 57.94(16) . . ?
C41 Ti2 C42 34.83(15) . . ?
O2 Ti2 C44 145.17(15) . . ?
Cl3 Ti2 C44 108.96(12) . . ?
Cl4 Ti2 C44 83.48(13) . . ?
C45 Ti2 C44 35.07(15) . . ?
C41 Ti2 C44 58.31(15) . . ?
C42 Ti2 C44 57.60(16) . . ?
O2 Ti2 C43 143.76(16) . . ?
Cl3 Ti2 C43 83.66(12) . . ?
Cl4 Ti2 C43 111.53(13) . . ?
C45 Ti2 C43 57.64(16) . . ?
C41 Ti2 C43 57.72(16) . . ?
C42 Ti2 C43 34.40(16) . . ?
C44 Ti2 C43 34.39(16) . . ?
O3 Ti3 Cl6 103.58(10) . . ?
O3 Ti3 Cl5 102.09(10) . . ?
Cl6 Ti3 Cl5 101.70(5) . . ?
O3 Ti3 C66 91.65(15) . . ?
Cl6 Ti3 C66 128.51(13) . . ?
Cl5 Ti3 C66 122.96(13) . . ?
O3 Ti3 C67 110.68(17) . . ?
Cl6 Ti3 C67 140.88(14) . . ?
Cl5 Ti3 C67 89.26(13) . . ?
C66 Ti3 C67 35.26(17) . . ?
O3 Ti3 C70 108.39(14) . . ?
Cl6 Ti3 C70 93.60(12) . . ?
Cl5 Ti3 C70 141.46(11) . . ?
C66 Ti3 C70 35.43(16) . . ?
C67 Ti3 C70 58.36(16) . . ?
O3 Ti3 C68 145.49(17) . . ?
Cl6 Ti3 C68 108.26(15) . . ?
Cl5 Ti3 C68 84.35(12) . . ?
C66 Ti3 C68 57.98(17) . . ?
C67 Ti3 C68 34.92(18) . . ?
C70 Ti3 C68 57.21(16) . . ?
O3 Ti3 C69 143.10(15) . . ?
Cl6 Ti3 C69 83.65(12) . . ?
Cl5 Ti3 C69 111.91(12) . . ?
C66 Ti3 C69 58.15(16) . . ?
C67 Ti3 C69 57.60(17) . . ?
C70 Ti3 C69 34.71(15) . . ?
C68 Ti3 C69 33.65(17) . . ?
C3 O1 Ti1 169.3(3) . . ?
C28 O2 Ti2 169.8(3) . . ?
C53 O3 Ti3 167.9(3) . . ?
C26 N1 C1 110.6(3) . . ?
C26 N1 C51 110.5(3) . . ?
C1 N1 C51 110.7(3) . . ?
N1 C1 C2 111.9(3) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C7 C2 C3 118.8(4) . . ?
C7 C2 C1 121.1(4) . . ?
C3 C2 C1 120.1(4) . . ?
O1 C3 C2 117.3(4) . . ?
O1 C3 C4 121.6(4) . . ?
C2 C3 C4 121.1(4) . . ?
C5 C4 C3 116.1(4) . . ?
C5 C4 C12 120.8(4) . . ?
C3 C4 C12 123.0(4) . . ?
C6 C5 C4 124.3(4) . . ?
C6 C5 H5 117.9 . . ?
C4 C5 H5 117.9 . . ?
C5 C6 C7 117.3(4) . . ?
C5 C6 C8 123.7(4) . . ?
C7 C6 C8 119.0(4) . . ?
C2 C7 C6 122.3(4) . . ?
C2 C7 H7 118.9 . . ?
C6 C7 H7 118.9 . . ?
C11 C8 C9 107.8(4) . . ?
C11 C8 C10 108.8(4) . . ?
C9 C8 C10 109.0(4) . . ?
C11 C8 C6 112.1(4) . . ?
C9 C8 C6 110.4(4) . . ?
C10 C8 C6 108.6(4) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C4 C12 C15 112.1(4) . . ?
C4 C12 C14 109.7(4) . . ?
C15 C12 C14 108.3(4) . . ?
C4 C12 C13 109.9(4) . . ?
C15 C12 C13 106.5(4) . . ?
C14 C12 C13 110.2(4) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C20 C16 C17 106.9(4) . . ?
C20 C16 C21 125.9(4) . . ?
C17 C16 C21 127.0(4) . . ?
C20 C16 Ti1 72.5(2) . . ?
C17 C16 Ti1 73.7(2) . . ?
C21 C16 Ti1 122.4(3) . . ?
C18 C17 C16 108.6(4) . . ?
C18 C17 C22 123.7(4) . . ?
C16 C17 C22 127.5(4) . . ?
C18 C17 Ti1 74.0(3) . . ?
C16 C17 Ti1 71.2(2) . . ?
C22 C17 Ti1 125.5(3) . . ?
C19 C18 C17 107.7(4) . . ?
C19 C18 C23 127.4(4) . . ?
C17 C18 C23 124.8(4) . . ?
C19 C18 Ti1 72.8(3) . . ?
C17 C18 Ti1 71.4(2) . . ?
C23 C18 Ti1 125.1(3) . . ?
C18 C19 C20 108.8(4) . . ?
C18 C19 C24 125.9(4) . . ?
C20 C19 C24 125.2(4) . . ?
C18 C19 Ti1 73.4(2) . . ?
C20 C19 Ti1 70.6(2) . . ?
C24 C19 Ti1 125.2(3) . . ?
C19 C20 C16 108.0(4) . . ?
C19 C20 C25 126.2(4) . . ?
C16 C20 C25 125.3(4) . . ?
C19 C20 Ti1 74.7(3) . . ?
C16 C20 Ti1 72.1(2) . . ?
C25 C20 Ti1 125.2(3) . . ?
C16 C21 H21A 109.5 . . ?
C16 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C16 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C17 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C18 C23 H23A 109.5 . . ?
C18 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C18 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C19 C24 H24A 109.5 . . ?
C19 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C19 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C20 C25 H25A 109.5 . . ?
C20 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C20 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
N1 C26 C27 112.8(3) . . ?
N1 C26 H26A 109.0 . . ?
C27 C26 H26A 109.0 . . ?
N1 C26 H26B 109.0 . . ?
C27 C26 H26B 109.0 . . ?
H26A C26 H26B 107.8 . . ?
C32 C27 C28 118.6(4) . . ?
C32 C27 C26 121.3(4) . . ?
C28 C27 C26 120.1(4) . . ?
O2 C28 C27 116.9(4) . . ?
O2 C28 C29 122.2(4) . . ?
C27 C28 C29 120.9(4) . . ?
C30 C29 C28 116.5(4) . . ?
C30 C29 C37 120.9(4) . . ?
C28 C29 C37 122.6(4) . . ?
C31 C30 C29 124.2(4) . . ?
C31 C30 H30 117.9 . . ?
C29 C30 H30 117.9 . . ?
C32 C31 C30 116.9(4) . . ?
C32 C31 C33 122.8(4) . . ?
C30 C31 C33 120.3(4) . . ?
C31 C32 C27 123.0(4) . . ?
C31 C32 H32 118.5 . . ?
C27 C32 H32 118.5 . . ?
C34 C33 C36 112.8(5) . . ?
C34 C33 C31 113.1(5) . . ?
C36 C33 C31 112.6(5) . . ?
C34 C33 C35 106.1(6) . . ?
C36 C33 C35 102.6(5) . . ?
C31 C33 C35 108.8(5) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C33 C35 H35A 109.5 . . ?
C33 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C33 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C33 C36 H36A 109.5 . . ?
C33 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C33 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C39 C37 C40 108.2(4) . . ?
C39 C37 C29 112.6(4) . . ?
C40 C37 C29 110.8(4) . . ?
C39 C37 C38 106.1(5) . . ?
C40 C37 C38 110.5(4) . . ?
C29 C37 C38 108.6(4) . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C37 C40 H40A 109.5 . . ?
C37 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C37 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C42 C41 C45 107.4(4) . . ?
C42 C41 C46 126.2(4) . . ?
C45 C41 C46 126.3(4) . . ?
C42 C41 Ti2 73.5(3) . . ?
C45 C41 Ti2 72.1(2) . . ?
C46 C41 Ti2 122.3(3) . . ?
C43 C42 C41 108.5(4) . . ?
C43 C42 C47 124.1(4) . . ?
C41 C42 C47 126.9(4) . . ?
C43 C42 Ti2 74.0(3) . . ?
C41 C42 Ti2 71.6(3) . . ?
C47 C42 Ti2 126.7(3) . . ?
C42 C43 C44 108.5(4) . . ?
C42 C43 C48 126.0(5) . . ?
C44 C43 C48 125.3(5) . . ?
C42 C43 Ti2 71.6(3) . . ?
C44 C43 Ti2 72.5(3) . . ?
C48 C43 Ti2 125.3(3) . . ?
C43 C44 C45 106.9(4) . . ?
C43 C44 C49 125.2(5) . . ?
C45 C44 C49 127.8(5) . . ?
C43 C44 Ti2 73.1(3) . . ?
C45 C44 Ti2 70.3(2) . . ?
C49 C44 Ti2 123.1(3) . . ?
C41 C45 C44 108.6(4) . . ?
C41 C45 C50 126.6(4) . . ?
C44 C45 C50 124.5(4) . . ?
C41 C45 Ti2 72.7(2) . . ?
C44 C45 Ti2 74.6(3) . . ?
C50 C45 Ti2 123.7(3) . . ?
C41 C46 H46A 109.5 . . ?
C41 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C41 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C42 C47 H47A 109.5 . . ?
C42 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C42 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C43 C48 H48A 109.5 . . ?
C43 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C43 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C44 C49 H49A 109.5 . . ?
C44 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C44 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C45 C50 H50A 109.5 . . ?
C45 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C45 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
N1 C51 C52 112.7(3) . . ?
N1 C51 H51A 109.1 . . ?
C52 C51 H51A 109.1 . . ?
N1 C51 H51B 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.8 . . ?
C57 C52 C53 120.1(4) . . ?
C57 C52 C51 120.0(4) . . ?
C53 C52 C51 119.9(4) . . ?
O3 C53 C52 117.7(4) . . ?
O3 C53 C54 121.3(4) . . ?
C52 C53 C54 120.9(4) . . ?
C55 C54 C53 116.5(4) . . ?
C55 C54 C62 120.0(4) . . ?
C53 C54 C62 123.4(4) . . ?
C54 C55 C56 123.8(4) . . ?
C54 C55 H55 118.1 . . ?
C56 C55 H55 118.1 . . ?
C57 C56 C55 117.8(4) . . ?
C57 C56 C58 122.0(4) . . ?
C55 C56 C58 120.2(4) . . ?
C52 C57 C56 120.8(4) . . ?
C52 C57 H57 119.6 . . ?
C56 C57 H57 119.6 . . ?
C59 C58 C61 108.8(6) . . ?
C59 C58 C56 113.5(5) . . ?
C61 C58 C56 110.6(5) . . ?
C59 C58 C60 109.9(6) . . ?
C61 C58 C60 107.5(6) . . ?
C56 C58 C60 106.4(5) . . ?
C58 C59 H59A 109.5 . . ?
C58 C59 H59B 109.5 . . ?
H59A C59 H59B 109.5 . . ?
C58 C59 H59C 109.5 . . ?
H59A C59 H59C 109.5 . . ?
H59B C59 H59C 109.5 . . ?
C58 C60 H60A 109.5 . . ?
C58 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C58 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C58 C61 H61A 109.5 . . ?
C58 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C58 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C64 C62 C63 107.8(4) . . ?
C64 C62 C54 112.0(4) . . ?
C63 C62 C54 108.7(4) . . ?
C64 C62 C65 107.0(4) . . ?
C63 C62 C65 110.9(4) . . ?
C54 C62 C65 110.4(4) . . ?
C62 C63 H63A 109.5 . . ?
C62 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C62 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C62 C64 H64A 109.5 . . ?
C62 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C62 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C62 C65 H65A 109.5 . . ?
C62 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C62 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C67 C66 C70 107.6(4) . . ?
C67 C66 C71 125.7(5) . . ?
C70 C66 C71 126.7(5) . . ?
C67 C66 Ti3 72.9(3) . . ?
C70 C66 Ti3 73.6(2) . . ?
C71 C66 Ti3 121.3(3) . . ?
C66 C67 C68 107.4(4) . . ?
C66 C67 C72 126.7(5) . . ?
C68 C67 C72 125.6(5) . . ?
C66 C67 Ti3 71.8(3) . . ?
C68 C67 Ti3 74.0(3) . . ?
C72 C67 Ti3 124.8(4) . . ?
C69 C68 C67 109.0(4) . . ?
C69 C68 C73 123.5(5) . . ?
C67 C68 C73 127.5(5) . . ?
C69 C68 Ti3 73.3(3) . . ?
C67 C68 Ti3 71.1(3) . . ?
C73 C68 Ti3 122.8(3) . . ?
C68 C69 C70 108.6(4) . . ?
C68 C69 C74 127.4(5) . . ?
C70 C69 C74 123.7(5) . . ?
C68 C69 Ti3 73.0(3) . . ?
C70 C69 Ti3 71.8(2) . . ?
C74 C69 Ti3 125.7(3) . . ?
C69 C70 C66 107.3(4) . . ?
C69 C70 C75 124.6(4) . . ?
C66 C70 C75 127.7(4) . . ?
C69 C70 Ti3 73.5(3) . . ?
C66 C70 Ti3 71.0(2) . . ?
C75 C70 Ti3 126.8(3) . . ?
C66 C71 H71A 109.5 . . ?
C66 C71 H71B 109.5 . . ?
H71A C71 H71B 109.5 . . ?
C66 C71 H71C 109.5 . . ?
H71A C71 H71C 109.5 . . ?
H71B C71 H71C 109.5 . . ?
C67 C72 H72A 109.5 . . ?
C67 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C67 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C68 C73 H73A 109.5 . . ?
C68 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C68 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C69 C74 H74A 109.5 . . ?
C69 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C69 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C70 C75 H75A 109.5 . . ?
C70 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C70 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 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
Cl1 Ti1 O1 C3 77.7(15) . . . . ?
Cl2 Ti1 O1 C3 -177.4(15) . . . . ?
C16 Ti1 O1 C3 -48.5(15) . . . . ?
C20 Ti1 O1 C3 -80.3(15) . . . . ?
C17 Ti1 O1 C3 -18.9(16) . . . . ?
C19 Ti1 O1 C3 -80.9(16) . . . . ?
C18 Ti1 O1 C3 -23.1(16) . . . . ?
Cl3 Ti2 O2 C28 59.9(16) . . . . ?
Cl4 Ti2 O2 C28 165.4(16) . . . . ?
C45 Ti2 O2 C28 -100.4(16) . . . . ?
C41 Ti2 O2 C28 -69.4(16) . . . . ?
C42 Ti2 O2 C28 -38.4(17) . . . . ?
C44 Ti2 O2 C28 -99.1(16) . . . . ?
C43 Ti2 O2 C28 -38.0(17) . . . . ?
Cl6 Ti3 O3 C53 88.4(13) . . . . ?
Cl5 Ti3 O3 C53 -166.2(13) . . . . ?
C66 Ti3 O3 C53 -42.0(13) . . . . ?
C67 Ti3 O3 C53 -72.4(13) . . . . ?
C70 Ti3 O3 C53 -10.1(13) . . . . ?
C68 Ti3 O3 C53 -68.6(14) . . . . ?
C69 Ti3 O3 C53 -9.2(14) . . . . ?
C26 N1 C1 C2 78.1(4) . . . . ?
C51 N1 C1 C2 -159.2(3) . . . . ?
N1 C1 C2 C7 9.5(6) . . . . ?
N1 C1 C2 C3 -170.8(4) . . . . ?
Ti1 O1 C3 C2 -25.8(17) . . . . ?
Ti1 O1 C3 C4 154.5(13) . . . . ?
C7 C2 C3 O1 -178.1(4) . . . . ?
C1 C2 C3 O1 2.3(6) . . . . ?
C7 C2 C3 C4 1.7(6) . . . . ?
C1 C2 C3 C4 -178.0(4) . . . . ?
O1 C3 C4 C5 177.3(4) . . . . ?
C2 C3 C4 C5 -2.4(6) . . . . ?
O1 C3 C4 C12 0.4(6) . . . . ?
C2 C3 C4 C12 -179.4(4) . . . . ?
C3 C4 C5 C6 0.7(6) . . . . ?
C12 C4 C5 C6 177.8(4) . . . . ?
C4 C5 C6 C7 1.6(7) . . . . ?
C4 C5 C6 C8 -179.0(4) . . . . ?
C3 C2 C7 C6 0.9(7) . . . . ?
C1 C2 C7 C6 -179.5(4) . . . . ?
C5 C6 C7 C2 -2.5(7) . . . . ?
C8 C6 C7 C2 178.1(4) . . . . ?
C5 C6 C8 C11 -0.7(7) . . . . ?
C7 C6 C8 C11 178.8(4) . . . . ?
C5 C6 C8 C9 -120.9(5) . . . . ?
C7 C6 C8 C9 58.5(6) . . . . ?
C5 C6 C8 C10 119.6(5) . . . . ?
C7 C6 C8 C10 -61.0(6) . . . . ?
C5 C4 C12 C15 8.3(6) . . . . ?
C3 C4 C12 C15 -174.9(4) . . . . ?
C5 C4 C12 C14 -112.1(5) . . . . ?
C3 C4 C12 C14 64.7(5) . . . . ?
C5 C4 C12 C13 126.5(4) . . . . ?
C3 C4 C12 C13 -56.7(5) . . . . ?
C20 C16 C17 C18 -0.4(5) . . . . ?
C21 C16 C17 C18 -176.3(4) . . . . ?
Ti1 C16 C17 C18 65.0(3) . . . . ?
C20 C16 C17 C22 173.8(4) . . . . ?
C21 C16 C17 C22 -2.1(7) . . . . ?
Ti1 C16 C17 C22 -120.8(5) . . . . ?
C20 C16 C17 Ti1 -65.4(3) . . . . ?
C21 C16 C17 Ti1 118.7(4) . . . . ?
C16 C17 C18 C19 1.1(5) . . . . ?
C22 C17 C18 C19 -173.4(4) . . . . ?
Ti1 C17 C18 C19 64.3(3) . . . . ?
C16 C17 C18 C23 176.5(4) . . . . ?
C22 C17 C18 C23 2.0(7) . . . . ?
Ti1 C17 C18 C23 -120.3(5) . . . . ?
C16 C17 C18 Ti1 -63.2(3) . . . . ?
C22 C17 C18 Ti1 122.3(4) . . . . ?
C17 C18 C19 C20 -1.3(5) . . . . ?
C23 C18 C19 C20 -176.6(4) . . . . ?
Ti1 C18 C19 C20 62.1(3) . . . . ?
C17 C18 C19 C24 174.8(4) . . . . ?
C23 C18 C19 C24 -0.5(8) . . . . ?
Ti1 C18 C19 C24 -121.8(5) . . . . ?
C17 C18 C19 Ti1 -63.4(3) . . . . ?
C23 C18 C19 Ti1 121.4(5) . . . . ?
C18 C19 C20 C16 1.1(5) . . . . ?
C24 C19 C20 C16 -175.1(4) . . . . ?
Ti1 C19 C20 C16 64.9(3) . . . . ?
C18 C19 C20 C25 173.4(4) . . . . ?
C24 C19 C20 C25 -2.8(7) . . . . ?
Ti1 C19 C20 C25 -122.8(5) . . . . ?
C18 C19 C20 Ti1 -63.9(3) . . . . ?
C24 C19 C20 Ti1 120.0(4) . . . . ?
C17 C16 C20 C19 -0.4(5) . . . . ?
C21 C16 C20 C19 175.5(4) . . . . ?
Ti1 C16 C20 C19 -66.7(3) . . . . ?
C17 C16 C20 C25 -172.8(4) . . . . ?
C21 C16 C20 C25 3.2(7) . . . . ?
Ti1 C16 C20 C25 121.0(4) . . . . ?
C17 C16 C20 Ti1 66.2(3) . . . . ?
C21 C16 C20 Ti1 -117.8(4) . . . . ?
C1 N1 C26 C27 -162.1(3) . . . . ?
C51 N1 C26 C27 75.0(4) . . . . ?
N1 C26 C27 C32 16.2(6) . . . . ?
N1 C26 C27 C28 -162.1(4) . . . . ?
Ti2 O2 C28 C27 -11.0(19) . . . . ?
Ti2 O2 C28 C29 170.8(14) . . . . ?
C32 C27 C28 O2 -178.9(4) . . . . ?
C26 C27 C28 O2 -0.5(6) . . . . ?
C32 C27 C28 C29 -0.6(7) . . . . ?
C26 C27 C28 C29 177.7(4) . . . . ?
O2 C28 C29 C30 178.5(4) . . . . ?
C27 C28 C29 C30 0.3(7) . . . . ?
O2 C28 C29 C37 0.2(7) . . . . ?
C27 C28 C29 C37 -177.9(4) . . . . ?
C28 C29 C30 C31 -0.1(7) . . . . ?
C37 C29 C30 C31 178.1(5) . . . . ?
C29 C30 C31 C32 0.3(8) . . . . ?
C29 C30 C31 C33 -177.2(5) . . . . ?
C30 C31 C32 C27 -0.6(7) . . . . ?
C33 C31 C32 C27 176.8(5) . . . . ?
C28 C27 C32 C31 0.8(7) . . . . ?
C26 C27 C32 C31 -177.5(4) . . . . ?
C32 C31 C33 C34 14.1(8) . . . . ?
C30 C31 C33 C34 -168.5(6) . . . . ?
C32 C31 C33 C36 143.4(5) . . . . ?
C30 C31 C33 C36 -39.2(7) . . . . ?
C32 C31 C33 C35 -103.5(6) . . . . ?
C30 C31 C33 C35 73.9(6) . . . . ?
C30 C29 C37 C39 3.2(7) . . . . ?
C28 C29 C37 C39 -178.6(5) . . . . ?
C30 C29 C37 C40 124.5(5) . . . . ?
C28 C29 C37 C40 -57.3(6) . . . . ?
C30 C29 C37 C38 -113.9(5) . . . . ?
C28 C29 C37 C38 64.2(6) . . . . ?
C45 C41 C42 C43 0.7(5) . . . . ?
C46 C41 C42 C43 -176.4(4) . . . . ?
Ti2 C41 C42 C43 65.3(3) . . . . ?
C45 C41 C42 C47 172.9(4) . . . . ?
C46 C41 C42 C47 -4.2(7) . . . . ?
Ti2 C41 C42 C47 -122.5(5) . . . . ?
C45 C41 C42 Ti2 -64.6(3) . . . . ?
C46 C41 C42 Ti2 118.3(4) . . . . ?
C41 C42 C43 C44 -0.2(5) . . . . ?
C47 C42 C43 C44 -172.6(4) . . . . ?
Ti2 C42 C43 C44 63.6(3) . . . . ?
C41 C42 C43 C48 175.5(5) . . . . ?
C47 C42 C43 C48 3.0(8) . . . . ?
Ti2 C42 C43 C48 -120.7(5) . . . . ?
C41 C42 C43 Ti2 -63.8(3) . . . . ?
C47 C42 C43 Ti2 123.8(4) . . . . ?
C42 C43 C44 C45 -0.4(5) . . . . ?
C48 C43 C44 C45 -176.2(5) . . . . ?
Ti2 C43 C44 C45 62.6(3) . . . . ?
C42 C43 C44 C49 178.0(4) . . . . ?
C48 C43 C44 C49 2.3(8) . . . . ?
Ti2 C43 C44 C49 -118.9(5) . . . . ?
C42 C43 C44 Ti2 -63.0(3) . . . . ?
C48 C43 C44 Ti2 121.3(5) . . . . ?
C42 C41 C45 C44 -1.0(5) . . . . ?
C46 C41 C45 C44 176.2(4) . . . . ?
Ti2 C41 C45 C44 -66.5(3) . . . . ?
C42 C41 C45 C50 -174.9(4) . . . . ?
C46 C41 C45 C50 2.2(7) . . . . ?
Ti2 C41 C45 C50 119.5(5) . . . . ?
C42 C41 C45 Ti2 65.6(3) . . . . ?
C46 C41 C45 Ti2 -117.3(4) . . . . ?
C43 C44 C45 C41 0.9(5) . . . . ?
C49 C44 C45 C41 -177.6(5) . . . . ?
Ti2 C44 C45 C41 65.3(3) . . . . ?
C43 C44 C45 C50 175.0(4) . . . . ?
C49 C44 C45 C50 -3.5(8) . . . . ?
Ti2 C44 C45 C50 -120.6(4) . . . . ?
C43 C44 C45 Ti2 -64.4(3) . . . . ?
C49 C44 C45 Ti2 117.2(5) . . . . ?
C26 N1 C51 C52 -161.2(3) . . . . ?
C1 N1 C51 C52 76.0(4) . . . . ?
N1 C51 C52 C57 16.6(6) . . . . ?
N1 C51 C52 C53 -163.6(4) . . . . ?
Ti3 O3 C53 C52 -38.3(15) . . . . ?
Ti3 O3 C53 C54 144.1(11) . . . . ?
C57 C52 C53 O3 179.2(4) . . . . ?
C51 C52 C53 O3 -0.6(6) . . . . ?
C57 C52 C53 C54 -3.2(6) . . . . ?
C51 C52 C53 C54 177.0(4) . . . . ?
O3 C53 C54 C55 -179.6(4) . . . . ?
C52 C53 C54 C55 2.9(6) . . . . ?
O3 C53 C54 C62 3.4(6) . . . . ?
C52 C53 C54 C62 -174.1(4) . . . . ?
C53 C54 C55 C56 -1.4(7) . . . . ?
C62 C54 C55 C56 175.7(4) . . . . ?
C54 C55 C56 C57 0.0(7) . . . . ?
C54 C55 C56 C58 -178.7(4) . . . . ?
C53 C52 C57 C56 1.8(6) . . . . ?
C51 C52 C57 C56 -178.4(4) . . . . ?
C55 C56 C57 C52 -0.2(7) . . . . ?
C58 C56 C57 C52 178.5(4) . . . . ?
C57 C56 C58 C59 4.5(8) . . . . ?
C55 C56 C58 C59 -176.9(5) . . . . ?
C57 C56 C58 C61 127.0(6) . . . . ?
C55 C56 C58 C61 -54.3(7) . . . . ?
C57 C56 C58 C60 -116.5(6) . . . . ?
C55 C56 C58 C60 62.1(6) . . . . ?
C55 C54 C62 C64 3.5(6) . . . . ?
C53 C54 C62 C64 -179.6(4) . . . . ?
C55 C54 C62 C63 -115.6(5) . . . . ?
C53 C54 C62 C63 61.3(6) . . . . ?
C55 C54 C62 C65 122.6(5) . . . . ?
C53 C54 C62 C65 -60.5(6) . . . . ?
C70 C66 C67 C68 -0.1(5) . . . . ?
C71 C66 C67 C68 177.4(4) . . . . ?
Ti3 C66 C67 C68 -66.0(3) . . . . ?
C70 C66 C67 C72 -173.8(5) . . . . ?
C71 C66 C67 C72 3.6(8) . . . . ?
Ti3 C66 C67 C72 120.3(5) . . . . ?
C70 C66 C67 Ti3 65.9(3) . . . . ?
C71 C66 C67 Ti3 -116.6(5) . . . . ?
C66 C67 C68 C69 0.6(5) . . . . ?
C72 C67 C68 C69 174.4(5) . . . . ?
Ti3 C67 C68 C69 -64.0(3) . . . . ?
C66 C67 C68 C73 -178.2(5) . . . . ?
C72 C67 C68 C73 -4.4(8) . . . . ?
Ti3 C67 C68 C73 117.3(5) . . . . ?
C66 C67 C68 Ti3 64.5(3) . . . . ?
C72 C67 C68 Ti3 -121.6(5) . . . . ?
C67 C68 C69 C70 -0.9(5) . . . . ?
C73 C68 C69 C70 178.0(5) . . . . ?
Ti3 C68 C69 C70 -63.4(3) . . . . ?
C67 C68 C69 C74 -175.2(5) . . . . ?
C73 C68 C69 C74 3.6(8) . . . . ?
Ti3 C68 C69 C74 122.3(5) . . . . ?
C67 C68 C69 Ti3 62.5(3) . . . . ?
C73 C68 C69 Ti3 -118.7(5) . . . . ?
C68 C69 C70 C66 0.8(5) . . . . ?
C74 C69 C70 C66 175.4(4) . . . . ?
Ti3 C69 C70 C66 -63.4(3) . . . . ?
C68 C69 C70 C75 -172.2(4) . . . . ?
C74 C69 C70 C75 2.4(7) . . . . ?
Ti3 C69 C70 C75 123.7(4) . . . . ?
C68 C69 C70 Ti3 64.2(3) . . . . ?
C74 C69 C70 Ti3 -121.2(5) . . . . ?
C67 C66 C70 C69 -0.4(5) . . . . ?
C71 C66 C70 C69 -177.8(4) . . . . ?
Ti3 C66 C70 C69 65.0(3) . . . . ?
C67 C66 C70 C75 172.2(4) . . . . ?
C71 C66 C70 C75 -5.2(7) . . . . ?
Ti3 C66 C70 C75 -122.3(5) . . . . ?
C67 C66 C70 Ti3 -65.5(3) . . . . ?
C71 C66 C70 Ti3 117.1(5) . . . . ?

#==============================================================================

#==============================================================================
# Additional structures and associated data_? identifiers
# should be added at this point if there is more than one 
# structure analysis in the CIF.



loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
1 -0.002 0.500 0.000 662.0 18.8
2 0.000 0.500 0.500 271.6 0.0
3 0.156 0.000 0.500 661.9 18.2
4 0.110 0.375 0.155 10.5 -0.2
5 0.167 0.783 0.088 11.2 0.8
6 0.167 0.750 0.361 7.0 -0.9
7 0.500 1.000 0.000 271.6 0.1
8 0.333 0.283 0.412 11.2 0.6
9 0.333 0.250 0.139 7.0 -1.0
10 0.389 0.875 0.345 10.4 -0.1
11 0.610 0.125 0.655 11.0 0.2
12 0.667 0.717 0.588 11.2 0.8
13 0.667 0.750 0.861 7.0 -0.8
14 0.833 0.217 0.912 11.2 0.6
15 0.833 0.250 0.639 7.0 -1.0
16 0.889 0.625 0.845 11.0 0.3
_platon_squeeze_details          
; ?
;
#==============================================================================
#     End of CIF
#==============================================================================
_chemical_properties_physical    ', Air-sensitive,Moisture-sensitive'
