# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

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

data_1_2MeCN
_database_code_depnum_ccdc_archive 'CCDC 1554491'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_1_2MeCN             
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weak data set. This is the best that could be achieved with the crystals available.
;
_vrf_PLAT129_1_2MeCN             
;
PROBLEM: Unusual Space group Specified ..................       A121 Check
RESPONSE: Space group selected to allow comparison with similar structures.
;
# Added during the CSD deposition process: Tuesday 06 June 2017 11:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C54 H74 Cl2 O4 Ti, 2(C2 H3 N)'
_chemical_formula_sum            'C58 H80 Cl2 N2 O4 Ti'
_chemical_formula_weight         988.04

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_H-M_alt        'A 1 2 1'
_symmetry_space_group_name_Hall  'A 2y'
_shelx_space_group_comment       
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;

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

_cell_length_a                   17.2312(16)
_cell_length_b                   12.1620(8)
_cell_length_c                   27.103(2)
_cell_angle_alpha                90
_cell_angle_beta                 101.229(9)
_cell_angle_gamma                90
_cell_volume                     5571.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    140(2)
_cell_measurement_reflns_used    4274
_cell_measurement_theta_min      3.4299
_cell_measurement_theta_max      22.4990

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.178
_exptl_crystal_F_000             2120
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    0.295
_shelx_estimated_absorpt_T_min   0.914
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.914
_exptl_absorpt_correction_T_max  0.974
_exptl_absorpt_process_details   
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
 Empirical absorption correction using spherical harmonics,
  implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      140(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Oxford Diffraction Xcalibur 3/Sapphire3 CCD'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_method       'Thin slice φ and ω scans'
_diffrn_detector_area_resol_mean 16.0050
_diffrn_reflns_number            30661
_diffrn_reflns_av_unetI/netI     0.2212
_diffrn_reflns_av_R_equivalents  0.1442
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.506
_diffrn_reflns_theta_max         22.499
_diffrn_reflns_theta_full        22.499
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             7245
_reflns_number_gt                3472
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.893
_reflns_Friedel_fraction_max     0.997
_reflns_Friedel_fraction_full    0.997

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

_computing_data_collection       
;
 CrysAlisPro CCD, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_cell_refinement       
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55 
;
_computing_data_reduction        
;
 CrysAlisPro RED, Oxford Diffraction Ltd., Version 1.171.33.55
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  
'SHELXL-2016/6 (Sheldrick, 2016) and WINGX (Farrugia, 2012)'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0612P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
; 
 Flack x determined using 1036 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.03(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         7245
_refine_ls_number_parameters     592
_refine_ls_number_restraints     295
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0667
_refine_ls_wR_factor_ref         0.1441
_refine_ls_wR_factor_gt          0.1271
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_restrained_S_all      0.804
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.69469(14) 0.38051(18) 0.58161(9) 0.0416(7) Uani 1 1 d . . . . .
Cl1 Cl 0.5574(2) 0.3543(3) 0.56577(14) 0.0585(11) Uani 1 1 d . . . . .
Cl2 Cl 0.6999(2) 0.2146(3) 0.53911(14) 0.0649(12) Uani 1 1 d . . . . .
O1 O 0.7101(4) 0.3033(6) 0.6529(3) 0.041(2) Uani 1 1 d . . . . .
O2 O 0.8002(5) 0.3888(7) 0.5926(3) 0.044(2) Uani 1 1 d . . . . .
O3 O 0.6931(4) 0.4732(6) 0.5160(3) 0.039(2) Uani 1 1 d . . . . .
O4 O 0.6739(4) 0.5062(6) 0.6120(3) 0.038(2) Uani 1 1 d . . . . .
C1 C 0.7457(7) 0.3676(9) 0.6957(4) 0.032(3) Uani 1 1 d . U . . .
C2 C 0.6986(7) 0.4371(9) 0.7183(5) 0.034(3) Uani 1 1 d . U . . .
C3 C 0.7346(7) 0.4952(9) 0.7597(4) 0.032(3) Uani 1 1 d . U . . .
H3 H 0.702868 0.541460 0.775942 0.039 Uiso 1 1 calc R U . . .
C4 C 0.8148(7) 0.4900(9) 0.7789(4) 0.034(3) Uani 1 1 d . U . . .
C5 C 0.8591(7) 0.4236(8) 0.7530(4) 0.030(3) Uani 1 1 d . U . . .
H5 H 0.914745 0.420951 0.764940 0.036 Uiso 1 1 calc R U . . .
C6 C 0.8282(7) 0.3615(10) 0.7116(4) 0.032(3) Uani 1 1 d . U . . .
C7 C 0.8559(8) 0.5527(10) 0.8270(5) 0.041(3) Uani 1 1 d . . . . .
C8 C 0.7960(9) 0.6125(11) 0.8509(5) 0.075(5) Uani 1 1 d . . . . .
H8A H 0.822956 0.648147 0.881966 0.113 Uiso 1 1 calc R U . . .
H8B H 0.757022 0.559920 0.858685 0.113 Uiso 1 1 calc R U . . .
H8C H 0.769182 0.668268 0.827554 0.113 Uiso 1 1 calc R U . . .
C9 C 0.8934(8) 0.4673(10) 0.8668(5) 0.064(4) Uani 1 1 d . . . . .
H9A H 0.941304 0.436974 0.857553 0.096 Uiso 1 1 calc R U . . .
H9B H 0.855513 0.407782 0.868209 0.096 Uiso 1 1 calc R U . . .
H9C H 0.907070 0.502833 0.899762 0.096 Uiso 1 1 calc R U . . .
C10 C 0.9169(10) 0.6278(12) 0.8142(5) 0.087(6) Uani 1 1 d . . . . .
H10A H 0.938581 0.673302 0.843479 0.131 Uiso 1 1 calc R U . . .
H10B H 0.892960 0.675196 0.786098 0.131 Uiso 1 1 calc R U . . .
H10C H 0.959551 0.584450 0.804533 0.131 Uiso 1 1 calc R U . . .
C11 C 0.8838(7) 0.3035(9) 0.6836(5) 0.035(3) Uani 1 1 d . . . . .
H11A H 0.926051 0.267428 0.708308 0.042 Uiso 1 1 calc R U . . .
H11B H 0.854321 0.245287 0.662281 0.042 Uiso 1 1 calc R U . . .
C12 C 0.8768(8) 0.4147(9) 0.6044(4) 0.036(3) Uani 1 1 d . . . . .
C13 C 0.9215(6) 0.3786(9) 0.6510(4) 0.029(3) Uani 1 1 d . . . . .
C14 C 0.9983(7) 0.4226(8) 0.6657(4) 0.034(3) Uani 1 1 d . . . . .
H14 H 1.029499 0.401629 0.697125 0.041 Uiso 1 1 calc R U . . .
C15 C 1.0295(6) 0.4954(9) 0.6355(4) 0.026(3) Uani 1 1 d . . . . .
C16 C 0.9867(7) 0.5148(8) 0.5881(4) 0.028(3) Uani 1 1 d . . . . .
H16 H 1.010369 0.557685 0.565640 0.033 Uiso 1 1 calc R U . . .
C17 C 0.9117(7) 0.4755(8) 0.5714(4) 0.024(3) Uani 1 1 d . . . . .
C18 C 1.1116(7) 0.5476(10) 0.6563(4) 0.036(3) Uani 1 1 d . U . . .
C19 C 1.1084(8) 0.6047(11) 0.7051(5) 0.060(4) Uani 1 1 d . U . . .
H19A H 1.162056 0.625813 0.721710 0.091 Uiso 1 1 calc R U . . .
H19B H 1.085891 0.554819 0.726967 0.091 Uiso 1 1 calc R U . . .
H19C H 1.075342 0.670591 0.698378 0.091 Uiso 1 1 calc R U . . .
C20 C 1.1752(7) 0.4552(9) 0.6656(5) 0.047(3) Uani 1 1 d . U . . .
H20A H 1.172785 0.412304 0.634726 0.071 Uiso 1 1 calc R U . . .
H20B H 1.165114 0.406767 0.692576 0.071 Uiso 1 1 calc R U . . .
H20C H 1.227852 0.488186 0.675423 0.071 Uiso 1 1 calc R U . . .
C21 C 1.1352(8) 0.6252(10) 0.6200(5) 0.053(3) Uani 1 1 d . U . . .
H21A H 1.099249 0.688454 0.615517 0.079 Uiso 1 1 calc R U . . .
H21B H 1.132637 0.588228 0.587553 0.079 Uiso 1 1 calc R U . . .
H21C H 1.189402 0.650520 0.632687 0.079 Uiso 1 1 calc R U . . .
C22 C 0.8654(7) 0.4984(9) 0.5191(4) 0.030(3) Uani 1 1 d . . . . .
H22A H 0.836470 0.431255 0.505524 0.035 Uiso 1 1 calc R U . . .
H22B H 0.902377 0.518150 0.496780 0.035 Uiso 1 1 calc R U . . .
C23 C 0.7292(7) 0.5816(9) 0.5215(4) 0.026(3) Uani 1 1 d . . . . .
C24 C 0.8060(7) 0.5932(9) 0.5198(4) 0.031(3) Uani 1 1 d . . . . .
C25 C 0.8362(7) 0.6983(9) 0.5225(4) 0.035(3) Uani 1 1 d . . . . .
H25 H 0.890248 0.707015 0.520402 0.042 Uiso 1 1 calc R U . . .
C26 C 0.7928(7) 0.7933(10) 0.5280(4) 0.029(3) Uani 1 1 d . . . . .
C27 C 0.7153(7) 0.7711(10) 0.5341(4) 0.039(3) Uani 1 1 d . . . . .
H27 H 0.683873 0.830910 0.541392 0.047 Uiso 1 1 calc R U . . .
C28 C 0.6814(7) 0.6659(9) 0.5302(4) 0.030(3) Uani 1 1 d . . . . .
C29 C 0.8242(7) 0.9066(9) 0.5278(5) 0.036(3) Uani 1 1 d . . . . .
C30 C 0.8177(8) 0.9645(10) 0.5773(5) 0.062(4) Uani 1 1 d . . . . .
H30A H 0.764960 0.951728 0.584691 0.093 Uiso 1 1 calc R U . . .
H30B H 0.826113 1.043631 0.574055 0.093 Uiso 1 1 calc R U . . .
H30C H 0.857867 0.934953 0.604747 0.093 Uiso 1 1 calc R U . . .
C31 C 0.9087(8) 0.9080(10) 0.5213(6) 0.077(5) Uani 1 1 d . . . . .
H31A H 0.942984 0.881786 0.552284 0.116 Uiso 1 1 calc R U . . .
H31B H 0.923780 0.983278 0.514285 0.116 Uiso 1 1 calc R U . . .
H31C H 0.914679 0.860016 0.493287 0.116 Uiso 1 1 calc R U . . .
C32 C 0.7749(8) 0.9716(10) 0.4845(5) 0.063(4) Uani 1 1 d . . . . .
H32A H 0.775576 0.933916 0.452617 0.094 Uiso 1 1 calc R U . . .
H32B H 0.797136 1.045562 0.483497 0.094 Uiso 1 1 calc R U . . .
H32C H 0.720218 0.977139 0.489565 0.094 Uiso 1 1 calc R U . . .
C33 C 0.5959(7) 0.6535(9) 0.5363(4) 0.033(3) Uani 1 1 d . . . . .
H33A H 0.574718 0.586280 0.517935 0.040 Uiso 1 1 calc R U . . .
H33B H 0.565949 0.716377 0.518847 0.040 Uiso 1 1 calc R U . . .
C34 C 0.6123(7) 0.5707(10) 0.6227(5) 0.036(3) Uani 1 1 d . . . . .
C35 C 0.5757(7) 0.6467(8) 0.5889(5) 0.027(3) Uani 1 1 d . . . . .
C36 C 0.5163(6) 0.7057(9) 0.5993(4) 0.027(3) Uani 1 1 d . . . . .
H36 H 0.493475 0.761181 0.576277 0.032 Uiso 1 1 calc R U . . .
C37 C 0.4860(7) 0.6888(9) 0.6434(4) 0.028(3) Uani 1 1 d . . . . .
C38 C 0.5219(7) 0.6113(9) 0.6752(4) 0.028(3) Uani 1 1 d . . . . .
H38 H 0.503158 0.600136 0.705526 0.034 Uiso 1 1 calc R U . . .
C39 C 0.5845(7) 0.5462(9) 0.6669(4) 0.030(3) Uani 1 1 d . . . . .
C40 C 0.4149(8) 0.7588(9) 0.6539(5) 0.041(3) Uani 1 1 d . . . . .
C41 C 0.4428(8) 0.8802(10) 0.6612(5) 0.073(4) Uani 1 1 d . . . . .
H41A H 0.398128 0.926657 0.665515 0.109 Uiso 1 1 calc R U . . .
H41B H 0.462809 0.904617 0.631549 0.109 Uiso 1 1 calc R U . . .
H41C H 0.484947 0.885812 0.691076 0.109 Uiso 1 1 calc R U . . .
C42 C 0.3470(7) 0.7552(10) 0.6093(4) 0.059(4) Uani 1 1 d . . . . .
H42A H 0.332124 0.678539 0.601269 0.089 Uiso 1 1 calc R U . . .
H42B H 0.363251 0.789719 0.580209 0.089 Uiso 1 1 calc R U . . .
H42C H 0.301679 0.794993 0.617381 0.089 Uiso 1 1 calc R U . . .
C43 C 0.3856(7) 0.7242(10) 0.7006(4) 0.053(4) Uani 1 1 d . . . . .
H43A H 0.341762 0.771933 0.705198 0.080 Uiso 1 1 calc R U . . .
H43B H 0.428815 0.730531 0.729917 0.080 Uiso 1 1 calc R U . . .
H43C H 0.367368 0.647806 0.697008 0.080 Uiso 1 1 calc R U . . .
C44 C 0.6114(7) 0.4470(9) 0.6982(4) 0.035(3) Uani 1 1 d . . . . .
H44A H 0.594030 0.380819 0.677699 0.041 Uiso 1 1 calc R U . . .
H44B H 0.583894 0.446310 0.727028 0.041 Uiso 1 1 calc R U . . .
C45 C 0.6682(8) 0.2026(10) 0.6646(5) 0.062(4) Uani 1 1 d . . . . .
H45A H 0.645562 0.215977 0.694957 0.075 Uiso 1 1 calc R U . . .
H45B H 0.624007 0.186565 0.636315 0.075 Uiso 1 1 calc R U . . .
C46 C 0.7208(8) 0.1070(9) 0.6734(5) 0.054(4) Uani 1 1 d . . . . .
H46A H 0.766289 0.122768 0.700933 0.065 Uiso 1 1 calc R U . . .
H46B H 0.741442 0.089940 0.642604 0.065 Uiso 1 1 calc R U . . .
C47 C 0.6721(8) 0.0059(9) 0.6880(6) 0.059(4) Uani 1 1 d . . . . .
H47A H 0.652665 0.023381 0.719123 0.071 Uiso 1 1 calc R U . . .
H47B H 0.625471 -0.006937 0.660827 0.071 Uiso 1 1 calc R U . . .
C48 C 0.7197(8) -0.0938(10) 0.6958(6) 0.073(5) Uani 1 1 d . . . . .
H48A H 0.770513 -0.076673 0.718538 0.088 Uiso 1 1 calc R U . . .
H48B H 0.731868 -0.117150 0.663114 0.088 Uiso 1 1 calc R U . . .
C49 C 0.6816(8) -0.1874(10) 0.7174(5) 0.065(5) Uani 1 1 d . . . . .
H49A H 0.669919 -0.165690 0.750030 0.097 Uiso 1 1 calc R U . . .
H49B H 0.717502 -0.250655 0.721974 0.097 Uiso 1 1 calc R U . . .
H49C H 0.632318 -0.207313 0.694504 0.097 Uiso 1 1 calc R U . . .
C50 C 0.6456(7) 0.4444(9) 0.4661(4) 0.039(3) Uani 1 1 d . . . . .
H50A H 0.607815 0.385385 0.470227 0.046 Uiso 1 1 calc R U . . .
H50B H 0.614571 0.509455 0.451869 0.046 Uiso 1 1 calc R U . . .
C51 C 0.6950(7) 0.4072(10) 0.4305(4) 0.047(4) Uani 1 1 d . . . . .
H51A H 0.730420 0.347574 0.446341 0.056 Uiso 1 1 calc R U . . .
H51B H 0.728545 0.469007 0.423412 0.056 Uiso 1 1 calc R U . . .
C52 C 0.6451(7) 0.3649(11) 0.3804(4) 0.055(4) Uani 1 1 d . . . . .
H52A H 0.601064 0.416653 0.368642 0.066 Uiso 1 1 calc R U . . .
H52B H 0.678595 0.362383 0.354562 0.066 Uiso 1 1 calc R U . . .
C53 C 0.6112(8) 0.2493(10) 0.3863(5) 0.067(4) Uani 1 1 d . . . . .
H53A H 0.655006 0.198051 0.399448 0.081 Uiso 1 1 calc R U . . .
H53B H 0.575631 0.252320 0.410904 0.081 Uiso 1 1 calc R U . . .
C54 C 0.5650(8) 0.2066(13) 0.3356(6) 0.088(6) Uani 1 1 d . . . . .
H54A H 0.531112 0.265329 0.318492 0.132 Uiso 1 1 calc R U . . .
H54B H 0.532261 0.143887 0.341356 0.132 Uiso 1 1 calc R U . . .
H54C H 0.602359 0.183471 0.314536 0.132 Uiso 1 1 calc R U . . .
N1 N 0.9324(8) 0.8190(10) 0.7024(5) 0.076(4) Uani 1 1 d . . . . .
C55 C 0.8923(9) 0.7518(12) 0.6841(5) 0.045(4) Uani 1 1 d . . . . .
C56 C 0.8413(9) 0.6657(10) 0.6608(5) 0.060(4) Uani 1 1 d . . . . .
H56A H 0.825870 0.619224 0.686811 0.090 Uiso 1 1 calc R U . . .
H56B H 0.869169 0.621076 0.639667 0.090 Uiso 1 1 calc R U . . .
H56C H 0.793877 0.697944 0.639947 0.090 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.786(8) . ?
Ti1 O4 1.805(8) . ?
Ti1 O3 2.101(8) . ?
Ti1 O1 2.118(8) . ?
Ti1 Cl2 2.334(4) . ?
Ti1 Cl1 2.342(4) . ?
O1 C1 1.435(12) . ?
O1 C45 1.487(14) . ?
O2 C12 1.335(13) . ?
O3 C23 1.453(13) . ?
O3 C50 1.480(12) . ?
O4 C34 1.395(13) . ?
C1 C2 1.393(15) . ?
C1 C6 1.405(14) . ?
C2 C3 1.367(14) . ?
C2 C44 1.500(15) . ?
C3 C4 1.380(14) . ?
C3 H3 0.9500 . ?
C4 C5 1.392(15) . ?
C4 C7 1.557(16) . ?
C5 C6 1.373(14) . ?
C5 H5 0.9500 . ?
C6 C11 1.508(14) . ?
C7 C10 1.484(17) . ?
C7 C8 1.508(16) . ?
C7 C9 1.545(15) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.503(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.386(14) . ?
C12 C13 1.414(14) . ?
C13 C14 1.412(14) . ?
C14 C15 1.382(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.373(14) . ?
C15 C18 1.552(14) . ?
C16 C17 1.370(14) . ?
C16 H16 0.9500 . ?
C17 C22 1.510(13) . ?
C18 C21 1.477(15) . ?
C18 C19 1.504(15) . ?
C18 C20 1.557(15) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.544(15) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C24 1.341(15) . ?
C23 C28 1.365(14) . ?
C24 C25 1.377(14) . ?
C25 C26 1.400(15) . ?
C25 H25 0.9500 . ?
C26 C27 1.405(15) . ?
C26 C29 1.480(15) . ?
C27 C28 1.401(15) . ?
C27 H27 0.9500 . ?
C28 C33 1.523(15) . ?
C29 C31 1.500(16) . ?
C29 C32 1.529(15) . ?
C29 C30 1.540(16) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.532(15) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.365(14) . ?
C34 C39 1.407(16) . ?
C35 C36 1.324(13) . ?
C36 C37 1.410(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.344(14) . ?
C37 C40 1.562(16) . ?
C38 C39 1.391(15) . ?
C38 H38 0.9500 . ?
C39 C44 1.496(14) . ?
C40 C42 1.510(15) . ?
C40 C43 1.512(14) . ?
C40 C41 1.553(16) . ?
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 0.9900 . ?
C44 H44B 0.9900 . ?
C45 C46 1.464(15) . ?
C45 H45A 0.9900 . ?
C45 H45B 0.9900 . ?
C46 C47 1.583(16) . ?
C46 H46A 0.9900 . ?
C46 H46B 0.9900 . ?
C47 C48 1.457(16) . ?
C47 H47A 0.9900 . ?
C47 H47B 0.9900 . ?
C48 C49 1.490(16) . ?
C48 H48A 0.9900 . ?
C48 H48B 0.9900 . ?
C49 H49A 0.9800 . ?
C49 H49B 0.9800 . ?
C49 H49C 0.9800 . ?
C50 C51 1.476(15) . ?
C50 H50A 0.9900 . ?
C50 H50B 0.9900 . ?
C51 C52 1.548(14) . ?
C51 H51A 0.9900 . ?
C51 H51B 0.9900 . ?
C52 C53 1.543(17) . ?
C52 H52A 0.9900 . ?
C52 H52B 0.9900 . ?
C53 C54 1.539(16) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N1 C55 1.121(15) . ?
C55 C56 1.432(17) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 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
O2 Ti1 O4 99.3(4) . . ?
O2 Ti1 O3 87.5(3) . . ?
O4 Ti1 O3 87.7(3) . . ?
O2 Ti1 O1 86.0(3) . . ?
O4 Ti1 O1 87.7(3) . . ?
O3 Ti1 O1 171.4(3) . . ?
O2 Ti1 Cl2 89.7(3) . . ?
O4 Ti1 Cl2 170.9(3) . . ?
O3 Ti1 Cl2 92.4(3) . . ?
O1 Ti1 Cl2 93.2(2) . . ?
O2 Ti1 Cl1 175.3(3) . . ?
O4 Ti1 Cl1 85.2(3) . . ?
O3 Ti1 Cl1 94.1(2) . . ?
O1 Ti1 Cl1 92.8(2) . . ?
Cl2 Ti1 Cl1 85.78(15) . . ?
C1 O1 C45 115.1(9) . . ?
C1 O1 Ti1 117.0(6) . . ?
C45 O1 Ti1 125.5(7) . . ?
C12 O2 Ti1 168.6(8) . . ?
C23 O3 C50 117.3(8) . . ?
C23 O3 Ti1 117.7(6) . . ?
C50 O3 Ti1 124.1(6) . . ?
C34 O4 Ti1 142.9(7) . . ?
C2 C1 C6 122.7(11) . . ?
C2 C1 O1 119.5(10) . . ?
C6 C1 O1 117.7(11) . . ?
C3 C2 C1 117.6(12) . . ?
C3 C2 C44 121.3(12) . . ?
C1 C2 C44 121.1(11) . . ?
C2 C3 C4 123.1(12) . . ?
C2 C3 H3 118.4 . . ?
C4 C3 H3 118.4 . . ?
C3 C4 C5 116.4(12) . . ?
C3 C4 C7 123.5(11) . . ?
C5 C4 C7 120.1(11) . . ?
C6 C5 C4 124.6(12) . . ?
C6 C5 H5 117.7 . . ?
C4 C5 H5 117.7 . . ?
C5 C6 C1 115.4(11) . . ?
C5 C6 C11 119.0(11) . . ?
C1 C6 C11 125.2(11) . . ?
C10 C7 C8 112.3(12) . . ?
C10 C7 C9 111.0(12) . . ?
C8 C7 C9 104.6(11) . . ?
C10 C7 C4 109.4(11) . . ?
C8 C7 C4 111.0(11) . . ?
C9 C7 C4 108.4(9) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C6 113.7(9) . . ?
C13 C11 H11A 108.8 . . ?
C6 C11 H11A 108.8 . . ?
C13 C11 H11B 108.8 . . ?
C6 C11 H11B 108.8 . . ?
H11A C11 H11B 107.7 . . ?
O2 C12 C17 120.3(11) . . ?
O2 C12 C13 118.8(11) . . ?
C17 C12 C13 120.9(11) . . ?
C14 C13 C12 116.8(11) . . ?
C14 C13 C11 123.6(10) . . ?
C12 C13 C11 119.4(10) . . ?
C15 C14 C13 121.9(10) . . ?
C15 C14 H14 119.1 . . ?
C13 C14 H14 119.1 . . ?
C16 C15 C14 117.7(11) . . ?
C16 C15 C18 123.6(11) . . ?
C14 C15 C18 118.6(10) . . ?
C17 C16 C15 123.3(11) . . ?
C17 C16 H16 118.4 . . ?
C15 C16 H16 118.4 . . ?
C16 C17 C12 118.3(10) . . ?
C16 C17 C22 122.5(11) . . ?
C12 C17 C22 119.2(11) . . ?
C21 C18 C19 110.7(11) . . ?
C21 C18 C15 111.7(10) . . ?
C19 C18 C15 108.7(10) . . ?
C21 C18 C20 107.1(10) . . ?
C19 C18 C20 109.6(10) . . ?
C15 C18 C20 109.1(9) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C17 C22 C24 110.9(9) . . ?
C17 C22 H22A 109.5 . . ?
C24 C22 H22A 109.5 . . ?
C17 C22 H22B 109.5 . . ?
C24 C22 H22B 109.5 . . ?
H22A C22 H22B 108.1 . . ?
C24 C23 C28 124.1(11) . . ?
C24 C23 O3 119.9(10) . . ?
C28 C23 O3 116.0(11) . . ?
C23 C24 C25 117.4(11) . . ?
C23 C24 C22 125.7(10) . . ?
C25 C24 C22 116.7(11) . . ?
C24 C25 C26 124.6(12) . . ?
C24 C25 H25 117.7 . . ?
C26 C25 H25 117.7 . . ?
C25 C26 C27 113.2(11) . . ?
C25 C26 C29 124.4(11) . . ?
C27 C26 C29 122.5(11) . . ?
C28 C27 C26 123.9(12) . . ?
C28 C27 H27 118.0 . . ?
C26 C27 H27 118.0 . . ?
C23 C28 C27 116.3(11) . . ?
C23 C28 C33 125.0(11) . . ?
C27 C28 C33 118.7(10) . . ?
C26 C29 C31 112.0(10) . . ?
C26 C29 C32 109.6(10) . . ?
C31 C29 C32 108.2(11) . . ?
C26 C29 C30 109.5(10) . . ?
C31 C29 C30 109.4(11) . . ?
C32 C29 C30 108.0(10) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C28 C33 C35 120.4(10) . . ?
C28 C33 H33A 107.2 . . ?
C35 C33 H33A 107.2 . . ?
C28 C33 H33B 107.2 . . ?
C35 C33 H33B 107.2 . . ?
H33A C33 H33B 106.8 . . ?
C35 C34 O4 120.8(12) . . ?
C35 C34 C39 121.7(11) . . ?
O4 C34 C39 117.2(11) . . ?
C36 C35 C34 120.0(12) . . ?
C36 C35 C33 119.5(11) . . ?
C34 C35 C33 120.1(10) . . ?
C35 C36 C37 122.0(11) . . ?
C35 C36 H36 119.0 . . ?
C37 C36 H36 119.0 . . ?
C38 C37 C36 116.5(11) . . ?
C38 C37 C40 123.0(11) . . ?
C36 C37 C40 120.5(10) . . ?
C37 C38 C39 124.7(12) . . ?
C37 C38 H38 117.6 . . ?
C39 C38 H38 117.6 . . ?
C38 C39 C34 114.9(11) . . ?
C38 C39 C44 122.1(12) . . ?
C34 C39 C44 122.3(12) . . ?
C42 C40 C43 109.3(10) . . ?
C42 C40 C41 107.6(11) . . ?
C43 C40 C41 107.6(10) . . ?
C42 C40 C37 110.6(10) . . ?
C43 C40 C37 113.7(10) . . ?
C41 C40 C37 107.9(10) . . ?
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 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 C2 116.7(10) . . ?
C39 C44 H44A 108.1 . . ?
C2 C44 H44A 108.1 . . ?
C39 C44 H44B 108.1 . . ?
C2 C44 H44B 108.1 . . ?
H44A C44 H44B 107.3 . . ?
C46 C45 O1 112.2(11) . . ?
C46 C45 H45A 109.2 . . ?
O1 C45 H45A 109.2 . . ?
C46 C45 H45B 109.2 . . ?
O1 C45 H45B 109.2 . . ?
H45A C45 H45B 107.9 . . ?
C45 C46 C47 108.4(11) . . ?
C45 C46 H46A 110.0 . . ?
C47 C46 H46A 110.0 . . ?
C45 C46 H46B 110.0 . . ?
C47 C46 H46B 110.0 . . ?
H46A C46 H46B 108.4 . . ?
C48 C47 C46 111.8(11) . . ?
C48 C47 H47A 109.3 . . ?
C46 C47 H47A 109.3 . . ?
C48 C47 H47B 109.3 . . ?
C46 C47 H47B 109.3 . . ?
H47A C47 H47B 107.9 . . ?
C47 C48 C49 114.4(12) . . ?
C47 C48 H48A 108.7 . . ?
C49 C48 H48A 108.7 . . ?
C47 C48 H48B 108.7 . . ?
C49 C48 H48B 108.7 . . ?
H48A C48 H48B 107.6 . . ?
C48 C49 H49A 109.5 . . ?
C48 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C48 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C51 C50 O3 112.5(10) . . ?
C51 C50 H50A 109.1 . . ?
O3 C50 H50A 109.1 . . ?
C51 C50 H50B 109.1 . . ?
O3 C50 H50B 109.1 . . ?
H50A C50 H50B 107.8 . . ?
C50 C51 C52 112.5(10) . . ?
C50 C51 H51A 109.1 . . ?
C52 C51 H51A 109.1 . . ?
C50 C51 H51B 109.1 . . ?
C52 C51 H51B 109.1 . . ?
H51A C51 H51B 107.8 . . ?
C53 C52 C51 111.6(11) . . ?
C53 C52 H52A 109.3 . . ?
C51 C52 H52A 109.3 . . ?
C53 C52 H52B 109.3 . . ?
C51 C52 H52B 109.3 . . ?
H52A C52 H52B 108.0 . . ?
C54 C53 C52 110.8(12) . . ?
C54 C53 H53A 109.5 . . ?
C52 C53 H53A 109.5 . . ?
C54 C53 H53B 109.5 . . ?
C52 C53 H53B 109.5 . . ?
H53A C53 H53B 108.1 . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N1 C55 C56 180(2) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 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
O4 Ti1 O2 C12 -6(4) . . . . ?
O3 Ti1 O2 C12 81(4) . . . . ?
O1 Ti1 O2 C12 -93(4) . . . . ?
Cl2 Ti1 O2 C12 173(4) . . . . ?
O2 Ti1 O4 C34 178.9(13) . . . . ?
O3 Ti1 O4 C34 91.8(13) . . . . ?
O1 Ti1 O4 C34 -95.5(13) . . . . ?
Cl1 Ti1 O4 C34 -2.4(13) . . . . ?
C45 O1 C1 C2 -78.8(13) . . . . ?
Ti1 O1 C1 C2 84.7(11) . . . . ?
C45 O1 C1 C6 104.2(12) . . . . ?
Ti1 O1 C1 C6 -92.2(10) . . . . ?
C6 C1 C2 C3 -4.5(17) . . . . ?
O1 C1 C2 C3 178.7(9) . . . . ?
C6 C1 C2 C44 175.9(10) . . . . ?
O1 C1 C2 C44 -0.9(16) . . . . ?
C1 C2 C3 C4 1.6(17) . . . . ?
C44 C2 C3 C4 -178.8(10) . . . . ?
C2 C3 C4 C5 1.7(17) . . . . ?
C2 C3 C4 C7 -177.8(10) . . . . ?
C3 C4 C5 C6 -2.3(17) . . . . ?
C7 C4 C5 C6 177.2(10) . . . . ?
C4 C5 C6 C1 -0.4(16) . . . . ?
C4 C5 C6 C11 172.9(10) . . . . ?
C2 C1 C6 C5 3.9(16) . . . . ?
O1 C1 C6 C5 -179.2(9) . . . . ?
C2 C1 C6 C11 -169.0(11) . . . . ?
O1 C1 C6 C11 7.9(16) . . . . ?
C3 C4 C7 C10 -120.8(13) . . . . ?
C5 C4 C7 C10 59.8(15) . . . . ?
C3 C4 C7 C8 3.6(17) . . . . ?
C5 C4 C7 C8 -175.8(10) . . . . ?
C3 C4 C7 C9 118.0(13) . . . . ?
C5 C4 C7 C9 -61.4(14) . . . . ?
C5 C6 C11 C13 -76.3(13) . . . . ?
C1 C6 C11 C13 96.4(13) . . . . ?
Ti1 O2 C12 C17 -84(4) . . . . ?
Ti1 O2 C12 C13 96(4) . . . . ?
O2 C12 C13 C14 -169.8(10) . . . . ?
C17 C12 C13 C14 10.4(16) . . . . ?
O2 C12 C13 C11 5.7(16) . . . . ?
C17 C12 C13 C11 -174.0(10) . . . . ?
C6 C11 C13 C14 98.5(13) . . . . ?
C6 C11 C13 C12 -76.8(14) . . . . ?
C12 C13 C14 C15 -1.6(16) . . . . ?
C11 C13 C14 C15 -177.0(10) . . . . ?
C13 C14 C15 C16 -7.0(16) . . . . ?
C13 C14 C15 C18 174.9(10) . . . . ?
C14 C15 C16 C17 7.4(16) . . . . ?
C18 C15 C16 C17 -174.6(10) . . . . ?
C15 C16 C17 C12 1.1(16) . . . . ?
C15 C16 C17 C22 179.6(10) . . . . ?
O2 C12 C17 C16 170.0(10) . . . . ?
C13 C12 C17 C16 -10.3(16) . . . . ?
O2 C12 C17 C22 -8.6(15) . . . . ?
C13 C12 C17 C22 171.2(10) . . . . ?
C16 C15 C18 C21 3.5(15) . . . . ?
C14 C15 C18 C21 -178.6(10) . . . . ?
C16 C15 C18 C19 125.9(12) . . . . ?
C14 C15 C18 C19 -56.1(13) . . . . ?
C16 C15 C18 C20 -114.7(12) . . . . ?
C14 C15 C18 C20 63.3(13) . . . . ?
C16 C17 C22 C24 -99.4(12) . . . . ?
C12 C17 C22 C24 79.0(13) . . . . ?
C50 O3 C23 C24 -100.3(13) . . . . ?
Ti1 O3 C23 C24 90.3(12) . . . . ?
C50 O3 C23 C28 82.0(13) . . . . ?
Ti1 O3 C23 C28 -87.4(11) . . . . ?
C28 C23 C24 C25 -6.1(18) . . . . ?
O3 C23 C24 C25 176.5(10) . . . . ?
C28 C23 C24 C22 169.0(11) . . . . ?
O3 C23 C24 C22 -8.4(18) . . . . ?
C17 C22 C24 C23 -96.4(14) . . . . ?
C17 C22 C24 C25 78.7(13) . . . . ?
C23 C24 C25 C26 1.6(18) . . . . ?
C22 C24 C25 C26 -174.0(10) . . . . ?
C24 C25 C26 C27 4.1(17) . . . . ?
C24 C25 C26 C29 -176.2(11) . . . . ?
C25 C26 C27 C28 -6.0(17) . . . . ?
C29 C26 C27 C28 174.2(12) . . . . ?
C24 C23 C28 C27 4.2(18) . . . . ?
O3 C23 C28 C27 -178.3(10) . . . . ?
C24 C23 C28 C33 -175.0(11) . . . . ?
O3 C23 C28 C33 2.6(17) . . . . ?
C26 C27 C28 C23 2.3(18) . . . . ?
C26 C27 C28 C33 -178.5(11) . . . . ?
C25 C26 C29 C31 -0.5(18) . . . . ?
C27 C26 C29 C31 179.2(12) . . . . ?
C25 C26 C29 C32 119.6(12) . . . . ?
C27 C26 C29 C32 -60.7(16) . . . . ?
C25 C26 C29 C30 -122.1(12) . . . . ?
C27 C26 C29 C30 57.6(15) . . . . ?
C23 C28 C33 C35 96.7(14) . . . . ?
C27 C28 C33 C35 -82.5(14) . . . . ?
Ti1 O4 C34 C35 -86.1(15) . . . . ?
Ti1 O4 C34 C39 87.4(15) . . . . ?
O4 C34 C35 C36 178.7(10) . . . . ?
C39 C34 C35 C36 5.4(17) . . . . ?
O4 C34 C35 C33 6.6(16) . . . . ?
C39 C34 C35 C33 -166.6(10) . . . . ?
C28 C33 C35 C36 134.4(11) . . . . ?
C28 C33 C35 C34 -53.5(15) . . . . ?
C34 C35 C36 C37 -3.6(17) . . . . ?
C33 C35 C36 C37 168.6(10) . . . . ?
C35 C36 C37 C38 1.7(16) . . . . ?
C35 C36 C37 C40 -178.9(10) . . . . ?
C36 C37 C38 C39 -1.7(16) . . . . ?
C40 C37 C38 C39 179.0(10) . . . . ?
C37 C38 C39 C34 3.3(16) . . . . ?
C37 C38 C39 C44 -167.6(10) . . . . ?
C35 C34 C39 C38 -5.1(16) . . . . ?
O4 C34 C39 C38 -178.6(9) . . . . ?
C35 C34 C39 C44 165.8(11) . . . . ?
O4 C34 C39 C44 -7.7(16) . . . . ?
C38 C37 C40 C42 -128.6(12) . . . . ?
C36 C37 C40 C42 52.1(14) . . . . ?
C38 C37 C40 C43 -5.2(15) . . . . ?
C36 C37 C40 C43 175.5(10) . . . . ?
C38 C37 C40 C41 114.1(12) . . . . ?
C36 C37 C40 C41 -65.3(14) . . . . ?
C38 C39 C44 C2 -131.4(12) . . . . ?
C34 C39 C44 C2 58.3(15) . . . . ?
C3 C2 C44 C39 79.0(14) . . . . ?
C1 C2 C44 C39 -101.3(13) . . . . ?
C1 O1 C45 C46 -89.2(13) . . . . ?
Ti1 O1 C45 C46 108.9(11) . . . . ?
O1 C45 C46 C47 177.4(11) . . . . ?
C45 C46 C47 C48 178.2(13) . . . . ?
C46 C47 C48 C49 170.8(12) . . . . ?
C23 O3 C50 C51 81.5(12) . . . . ?
Ti1 O3 C50 C51 -109.8(10) . . . . ?
O3 C50 C51 C52 173.7(10) . . . . ?
C50 C51 C52 C53 -76.0(13) . . . . ?
C51 C52 C53 C54 -177.4(11) . . . . ?

_refine_diff_density_max         0.421
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.056


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
####################################################################### 
# 
# 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_cr543
_database_code_depnum_ccdc_archive 'CCDC 1554493'
_audit_update_record             
;
2018-06-08 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         
'C94.62 H116.35 Cl2.69 N2 O11.96 Si1.31 Ti4, 10(C2 H3 N)'
_chemical_formula_sum            'C114.62 H146.35 Cl2.69 N12 O11.96 Si1.31 Ti4'
_chemical_formula_weight         2207.32

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

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

_cell_length_a                   31.7283(3)
_cell_length_b                   14.26944(14)
_cell_length_c                   28.7967(3)
_cell_angle_alpha                90
_cell_angle_beta                 111.2143(12)
_cell_angle_gamma                90
_cell_volume                     12154.1(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    59808
_cell_measurement_theta_min      1.5920
_cell_measurement_theta_max      27.5610

_exptl_crystal_description       'Cut Needle'
_exptl_crystal_colour            Red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.206
_exptl_crystal_F_000             4663
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.385
_shelx_estimated_absorpt_T_min   0.877
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_T_max  1.000
_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_special_details   ?
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Rotating Anode'
_diffrn_measurement_device_type  
; 
Rigaku FRE+ equipped with HF Varimax confocal mirrors 
and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_detector                 'CCD area detector'
_diffrn_detector_type            'Rigaku HG Saturn724+ (2x2 bin mode)'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_radiation_collimation    0.2
_diffrn_radiation_monochromator  'Confocal mirrors, HF Varimax'
_diffrn_detector_area_resol_mean 28.5714
_diffrn_reflns_number            97082
_diffrn_reflns_av_unetI/netI     0.0124
_diffrn_reflns_av_R_equivalents  0.0259
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_theta_min         2.360
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             13919
_reflns_number_gt                13137
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       '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, 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0478P)²+36.0626P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13919
_refine_ls_number_parameters     804
_refine_ls_number_restraints     411
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0572
_refine_ls_wR_factor_ref         0.1470
_refine_ls_wR_factor_gt          0.1455
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_restrained_S_all      1.211
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.46551(2) 0.45508(3) 0.27466(2) 0.02076(10) Uani 1 1 d D . . . .
Ti2 Ti 0.41708(2) 0.37472(3) 0.16393(2) 0.02270(10) Uani 1 1 d D . . . .
Cl1 Cl 0.44142(3) 0.22446(5) 0.18775(2) 0.04000(17) Uani 1 1 d D . . . .
Cl2X Cl 0.44938(13) 0.6095(2) 0.27729(14) 0.0577(9) Uani 0.346(3) 1 d D U P A 2
O1 O 0.42202(5) 0.36969(12) 0.10323(6) 0.0254(3) Uani 1 1 d . . . . .
O2 O 0.35605(5) 0.36134(12) 0.14295(6) 0.0237(3) Uani 1 1 d . . . . .
O3 O 0.40787(5) 0.39900(12) 0.23409(6) 0.0226(3) Uani 1 1 d . . . . .
O4 O 0.46425(5) 0.41145(12) 0.33216(6) 0.0231(3) Uani 1 1 d . . . . .
O5 O 0.47131(5) 0.43655(14) 0.20851(6) 0.0291(4) Uani 1 1 d . . . . .
C1 C 0.40517(8) 0.39628(17) 0.05433(8) 0.0235(4) Uani 1 1 d . . . . .
C2 C 0.43375(7) 0.44732(17) 0.03609(8) 0.0235(4) Uani 1 1 d . . . . .
C3 C 0.41723(8) 0.47773(17) -0.01304(8) 0.0250(5) Uani 1 1 d . . . . .
H3 H 0.436510 0.512816 -0.025205 0.030 Uiso 1 1 calc R U . . .
C4 C 0.37281(8) 0.45819(18) -0.04540(8) 0.0262(5) Uani 1 1 d . . . . .
C5 C 0.34571(8) 0.40694(18) -0.02625(8) 0.0264(5) Uani 1 1 d . . . . .
H5 H 0.315652 0.392829 -0.047521 0.032 Uiso 1 1 calc R U . . .
C6 C 0.36074(8) 0.37493(17) 0.02323(8) 0.0245(5) Uani 1 1 d . . . . .
C7 C 0.35650(8) 0.4958(2) -0.09883(9) 0.0318(5) Uani 1 1 d . . . . .
C8 C 0.30670(9) 0.4715(2) -0.12794(10) 0.0404(7) Uani 1 1 d . . . . .
H8A H 0.287885 0.496992 -0.110436 0.061 Uiso 1 1 calc R U . . .
H8B H 0.303129 0.403266 -0.130555 0.061 Uiso 1 1 calc R U . . .
H8C H 0.297317 0.498767 -0.161391 0.061 Uiso 1 1 calc R U . . .
C9 C 0.36170(9) 0.6023(2) -0.09765(10) 0.0400(6) Uani 1 1 d . . . . .
H9A H 0.343734 0.629921 -0.079723 0.060 Uiso 1 1 calc R U . . .
H9B H 0.351118 0.626486 -0.131806 0.060 Uiso 1 1 calc R U . . .
H9C H 0.393603 0.618730 -0.080671 0.060 Uiso 1 1 calc R U . . .
C10 C 0.38526(10) 0.4523(3) -0.12648(10) 0.0430(7) Uani 1 1 d . . . . .
H10A H 0.374841 0.476005 -0.160730 0.065 Uiso 1 1 calc R U . . .
H10B H 0.382170 0.383925 -0.126989 0.065 Uiso 1 1 calc R U . . .
H10C H 0.417065 0.469296 -0.109306 0.065 Uiso 1 1 calc R U . . .
C11 C 0.32734(8) 0.32275(18) 0.04068(8) 0.0263(5) Uani 1 1 d . . . . .
H11A H 0.305304 0.288627 0.012304 0.032 Uiso 1 1 calc R U . . .
H11B H 0.343693 0.276317 0.066447 0.032 Uiso 1 1 calc R U . . .
C12 C 0.31925(7) 0.40928(17) 0.11335(8) 0.0237(4) Uani 1 1 d . . . . .
C13 C 0.30256(8) 0.39121(18) 0.06197(8) 0.0256(5) Uani 1 1 d . . . . .
C14 C 0.26626(8) 0.4450(2) 0.03179(9) 0.0306(5) Uani 1 1 d . . . . .
H14 H 0.253977 0.432352 -0.002938 0.037 Uiso 1 1 calc R U . . .
C15 C 0.24732(8) 0.5170(2) 0.05089(10) 0.0322(5) Uani 1 1 d . . . . .
C16 C 0.26528(8) 0.53295(18) 0.10245(9) 0.0294(5) Uani 1 1 d . . . . .
H16 H 0.252728 0.581176 0.116182 0.035 Uiso 1 1 calc R U . . .
C17 C 0.30123(8) 0.47961(18) 0.13419(9) 0.0255(5) Uani 1 1 d . . . . .
C18 C 0.20832(9) 0.5754(2) 0.01522(11) 0.0406(6) Uani 1 1 d . . . . .
C19 C 0.19507(10) 0.6561(2) 0.04160(12) 0.0482(8) Uani 1 1 d . . . . .
H19A H 0.184419 0.631313 0.067132 0.072 Uiso 1 1 calc R U . . .
H19B H 0.170886 0.692652 0.017337 0.072 Uiso 1 1 calc R U . . .
H19C H 0.221385 0.696531 0.057327 0.072 Uiso 1 1 calc R U . . .
C20 C 0.16726(10) 0.5112(3) -0.00845(13) 0.0512(8) Uani 1 1 d . . . . .
H20A H 0.175243 0.460942 -0.026940 0.077 Uiso 1 1 calc R U . . .
H20B H 0.142150 0.547843 -0.031262 0.077 Uiso 1 1 calc R U . . .
H20C H 0.158183 0.483988 0.017746 0.077 Uiso 1 1 calc R U . . .
C21 C 0.22311(12) 0.6160(3) -0.02651(12) 0.0521(8) Uani 1 1 d . . . . .
H21A H 0.250037 0.655093 -0.011601 0.078 Uiso 1 1 calc R U . . .
H21B H 0.198557 0.654014 -0.049218 0.078 Uiso 1 1 calc R U . . .
H21C H 0.230074 0.564453 -0.045068 0.078 Uiso 1 1 calc R U . . .
C22 C 0.32370(8) 0.50279(17) 0.18917(9) 0.0257(5) Uani 1 1 d . . . . .
H22A H 0.353776 0.530391 0.194822 0.031 Uiso 1 1 calc R U . . .
H22B H 0.305371 0.551011 0.197894 0.031 Uiso 1 1 calc R U . . .
C23 C 0.37074(8) 0.37243(17) 0.24592(8) 0.0238(4) Uani 1 1 d . . . . .
C24 C 0.32968(8) 0.42006(17) 0.22394(8) 0.0248(5) Uani 1 1 d . . . . .
C25 C 0.29191(8) 0.3897(2) 0.23387(9) 0.0294(5) Uani 1 1 d . . . . .
H25 H 0.264205 0.422570 0.219206 0.035 Uiso 1 1 calc R U . . .
C26 C 0.29327(8) 0.3135(2) 0.26430(9) 0.0325(6) Uani 1 1 d . . . . .
C27 C 0.33490(9) 0.26865(19) 0.28614(9) 0.0310(5) Uani 1 1 d . . . . .
H27 H 0.336864 0.216852 0.307543 0.037 Uiso 1 1 calc R U . . .
C28 C 0.37390(8) 0.29667(18) 0.27789(8) 0.0263(5) Uani 1 1 d . . . . .
C29 C 0.25064(9) 0.2763(3) 0.27208(10) 0.0456(8) Uani 1 1 d . . . . .
C30 C 0.21126(11) 0.3439(4) 0.25252(18) 0.0835(16) Uani 1 1 d . . . . .
H30A H 0.185149 0.318454 0.258834 0.125 Uiso 1 1 calc R U . . .
H30B H 0.203396 0.352613 0.216605 0.125 Uiso 1 1 calc R U . . .
H30C H 0.219773 0.404396 0.269470 0.125 Uiso 1 1 calc R U . . .
C31 C 0.23777(16) 0.1828(4) 0.24351(14) 0.0808(16) Uani 1 1 d . . . . .
H31A H 0.263136 0.138885 0.256031 0.121 Uiso 1 1 calc R U . . .
H31B H 0.230794 0.193949 0.207918 0.121 Uiso 1 1 calc R U . . .
H31C H 0.211222 0.156194 0.248429 0.121 Uiso 1 1 calc R U . . .
C32 C 0.26002(10) 0.2559(3) 0.32675(11) 0.0476(8) Uani 1 1 d . . . . .
H32A H 0.269411 0.313745 0.346127 0.071 Uiso 1 1 calc R U . . .
H32B H 0.284162 0.209160 0.338851 0.071 Uiso 1 1 calc R U . . .
H32C H 0.232523 0.231721 0.330516 0.071 Uiso 1 1 calc R U . . .
C33 C 0.41746(8) 0.24159(18) 0.30343(8) 0.0275(5) Uani 1 1 d . . . . .
H33A H 0.410263 0.173864 0.301482 0.033 Uiso 1 1 calc R U . . .
H33B H 0.438217 0.252330 0.285262 0.033 Uiso 1 1 calc R U . . .
C34 C 0.46500(7) 0.35310(17) 0.36955(8) 0.0226(4) Uani 1 1 d . . . . .
C35 C 0.44133(8) 0.26861(17) 0.35768(8) 0.0250(5) Uani 1 1 d . . . . .
C36 C 0.44032(8) 0.21173(18) 0.39665(9) 0.0266(5) Uani 1 1 d . . . . .
H36 H 0.423968 0.154468 0.389098 0.032 Uiso 1 1 calc R U . . .
C37 C 0.46275(8) 0.23670(18) 0.44662(8) 0.0255(5) Uani 1 1 d . . . . .
C38 C 0.48773(7) 0.31997(18) 0.45646(8) 0.0246(5) Uani 1 1 d . . . . .
H38 H 0.503983 0.336989 0.490111 0.029 Uiso 1 1 calc R U . . .
C39 C 0.48961(7) 0.37862(17) 0.41877(8) 0.0226(4) Uani 1 1 d . . . . .
C40 C 0.45994(8) 0.17818(19) 0.49000(9) 0.0299(5) Uani 1 1 d . . . . .
C41 C 0.43437(11) 0.0865(2) 0.47234(11) 0.0421(7) Uani 1 1 d . . . . .
H41A H 0.403474 0.100180 0.449768 0.063 Uiso 1 1 calc R U . . .
H41B H 0.433387 0.051262 0.501150 0.063 Uiso 1 1 calc R U . . .
H41C H 0.449823 0.049119 0.454767 0.063 Uiso 1 1 calc R U . . .
C42 C 0.43495(10) 0.2355(2) 0.51728(10) 0.0368(6) Uani 1 1 d . . . . .
H42A H 0.451613 0.293592 0.530032 0.055 Uiso 1 1 calc R U . . .
H42B H 0.432831 0.198776 0.545099 0.055 Uiso 1 1 calc R U . . .
H42C H 0.404486 0.250749 0.494080 0.055 Uiso 1 1 calc R U . . .
C43 C 0.50771(10) 0.1549(3) 0.52698(11) 0.0459(7) Uani 1 1 d . . . . .
H43A H 0.523971 0.118411 0.509974 0.069 Uiso 1 1 calc R U . . .
H43B H 0.505396 0.118360 0.554763 0.069 Uiso 1 1 calc R U . . .
H43C H 0.524154 0.213232 0.539723 0.069 Uiso 1 1 calc R U . . .
C44 C 0.51792(7) 0.46734(17) 0.43051(8) 0.0240(4) Uani 1 1 d . . . . .
H44A H 0.517631 0.495930 0.399069 0.029 Uiso 1 1 calc R U . . .
H44B H 0.504486 0.512845 0.447127 0.029 Uiso 1 1 calc R U . . .
N1 N 0.39964(7) 0.52572(15) 0.13884(8) 0.0284(4) Uani 1 1 d . . . . .
C45 C 0.38236(10) 0.5739(2) 0.10530(12) 0.0436(7) Uani 1 1 d . . . . .
C46 C 0.35778(13) 0.6291(3) 0.06067(15) 0.0621(10) Uani 1 1 d . . . . .
H46A H 0.325190 0.619950 0.051765 0.093 Uiso 1 1 calc R U . . .
H46B H 0.366639 0.608588 0.033017 0.093 Uiso 1 1 calc R U . . .
H46C H 0.365122 0.695623 0.067426 0.093 Uiso 1 1 calc R U . . .
O6 O 0.45920(12) 0.5750(3) 0.27618(13) 0.0290(7) Uani 0.654(3) 1 d . U P A 1
Si1 Si 0.46602(4) 0.69048(8) 0.27867(4) 0.0339(4) Uani 0.654(3) 1 d . U P A 1
O7 O 0.500000 0.7174(3) 0.250000 0.0638(16) Uani 0.654(3) 2 d S TU P A 1
C60 C 0.4091(2) 0.7419(4) 0.2453(3) 0.083(2) Uani 0.654(3) 1 d . U P A 1
H60A H 0.388362 0.722544 0.261800 0.124 Uiso 0.654(3) 1 calc R U P A 1
H60B H 0.397536 0.719865 0.210705 0.124 Uiso 0.654(3) 1 calc R U P A 1
H60C H 0.411322 0.810444 0.245753 0.124 Uiso 0.654(3) 1 calc R U P A 1
C61 C 0.4947(3) 0.7221(5) 0.3454(2) 0.088(2) Uani 0.654(3) 1 d . U P A 1
H61A H 0.525667 0.697537 0.357532 0.132 Uiso 0.654(3) 1 calc R U P A 1
H61B H 0.478077 0.695060 0.364968 0.132 Uiso 0.654(3) 1 calc R U P A 1
H61C H 0.495580 0.790493 0.348948 0.132 Uiso 0.654(3) 1 calc R U P A 1
N2 N 0.52161(18) 0.0056(3) 0.38357(16) 0.1001(15) Uani 1 1 d D . . B 1
C47 C 0.54128(14) 0.0691(3) 0.40375(14) 0.0593(9) Uani 1 1 d D . . B 1
C48 C 0.56584(12) 0.1486(2) 0.42965(12) 0.0489(7) Uani 1 1 d D . . B 1
H48A H 0.546443 0.204166 0.420603 0.073 Uiso 1 1 calc R U . B 1
H48B H 0.592439 0.158260 0.420531 0.073 Uiso 1 1 calc R U . B 1
H48C H 0.575556 0.137924 0.465628 0.073 Uiso 1 1 calc R U . B 1
N3 N 0.21960(13) 0.6393(3) 0.41126(13) 0.0823(12) Uani 1 1 d D U . C 1
C49 C 0.19859(12) 0.6406(3) 0.37165(13) 0.0573(9) Uani 1 1 d D U . C 1
C50 C 0.1717(2) 0.6422(6) 0.31987(17) 0.148(4) Uani 1 1 d D U . C 1
H50A H 0.140522 0.658882 0.315480 0.222 Uiso 1 1 calc R U . C 1
H50B H 0.172154 0.580211 0.305439 0.222 Uiso 1 1 calc R U . C 1
H50C H 0.183923 0.688749 0.303083 0.222 Uiso 1 1 calc R U . C 1
N4 N 0.4176(6) -0.0156(14) 0.2396(8) 0.204(8) Uani 0.5 1 d D U P D -1
C51 C 0.4543(6) -0.0022(10) 0.2451(6) 0.133(5) Uani 0.5 1 d D U P D -1
C52 C 0.5000(8) 0.0129(7) 0.2491(16) 0.125(5) Uani 0.5 1 d D U P D -1
H52A H 0.501165 0.019548 0.215694 0.187 Uiso 0.5 1 calc R U P D -1
H52B H 0.518610 -0.040637 0.265984 0.187 Uiso 0.5 1 calc R U P D -1
H52C H 0.511615 0.070096 0.268294 0.187 Uiso 0.5 1 calc R U P D -1
N5 N 0.33133(18) 0.0340(4) 0.3456(2) 0.0851(16) Uani 0.788(5) 1 d D U P E 1
C53 C 0.36188(18) -0.0053(4) 0.3441(2) 0.0661(13) Uani 0.788(5) 1 d D U P E 1
C54 C 0.4013(2) -0.0577(6) 0.3439(3) 0.088(2) Uani 0.788(5) 1 d D U P E 1
H54A H 0.404098 -0.115551 0.363164 0.131 Uiso 0.788(5) 1 calc R U P E 1
H54B H 0.428507 -0.019477 0.358988 0.131 Uiso 0.788(5) 1 calc R U P E 1
H54C H 0.397712 -0.073214 0.309576 0.131 Uiso 0.788(5) 1 calc R U P E 1
N5X N 0.3769(7) 1.0044(12) 0.2672(6) 0.083(6) Uani 0.212(5) 1 d D U P E 2
C53X C 0.3943(6) 0.9686(12) 0.3041(6) 0.058(4) Uani 0.212(5) 1 d D U P E 2
C54X C 0.4198(9) 0.917(3) 0.3478(9) 0.108(10) Uani 0.212(5) 1 d D U P E 2
H54D H 0.423378 0.852071 0.338587 0.162 Uiso 0.212(5) 1 calc R U P E 2
H54E H 0.403897 0.917530 0.371267 0.162 Uiso 0.212(5) 1 calc R U P E 2
H54F H 0.449673 0.945727 0.363393 0.162 Uiso 0.212(5) 1 calc R U P E 2
N6 N 0.37721(18) 0.8100(6) 0.4271(4) 0.165(4) Uani 0.788(5) 1 d D U P E 1
C55 C 0.33992(16) 0.8119(4) 0.4151(2) 0.0717(15) Uani 0.788(5) 1 d D U P E 1
C56 C 0.29334(12) 0.8172(3) 0.40001(14) 0.0586(9) Uani 1 1 d D U . . .
H56A H 0.281481 0.856197 0.370040 0.088 Uiso 0.788(5) 1 calc R U P E 1
H56B H 0.285132 0.845148 0.426671 0.088 Uiso 0.788(5) 1 calc R U P E 1
H56C H 0.280409 0.754167 0.392657 0.088 Uiso 0.788(5) 1 calc R U P E 1
H56D H 0.261082 0.830417 0.391373 0.088 Uiso 0.212(5) 1 calc R U P E 2
H56E H 0.307008 0.802393 0.435575 0.088 Uiso 0.212(5) 1 calc R U P E 2
H56F H 0.296992 0.763799 0.380427 0.088 Uiso 0.212(5) 1 calc R U P E 2
N6X N 0.3313(7) 0.9678(12) 0.3784(7) 0.084(5) Uani 0.212(5) 1 d D U P E 2
C55X C 0.3162(7) 0.9017(12) 0.3888(8) 0.074(4) Uani 0.212(5) 1 d D U P E 2
N7 N 0.3960(6) 0.8142(10) 0.1264(5) 0.103(5) Uani 0.303(6) 1 d D U P F 1
C57 C 0.3900(7) 0.8850(10) 0.1393(5) 0.088(5) Uani 0.303(6) 1 d D U P F 1
C58 C 0.3798(7) 0.9758(11) 0.1519(6) 0.095(5) Uani 0.303(6) 1 d D U P F 1
N7X N 0.3526(9) 0.769(2) 0.1477(8) 0.116(7) Uani 0.197(6) 1 d D U P F 2
C57X C 0.3898(10) 0.790(3) 0.1641(12) 0.122(8) Uani 0.197(6) 1 d D U P F 2
C58X C 0.4378(10) 0.796(2) 0.1716(11) 0.117(8) Uani 0.197(6) 1 d D U P F 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O6 1.725(4) . ?
Ti1 O4 1.7828(16) . ?
Ti1 O5 1.9026(16) 2_655 ?
Ti1 O3 1.9502(16) . ?
Ti1 O5 1.9967(16) . ?
Ti1 Cl2X 2.269(3) . ?
Ti1 Ti1 3.0096(7) 2_655 ?
Ti1 Ti2 3.2091(5) . ?
Ti2 O1 1.8118(16) . ?
Ti2 O2 1.8180(16) . ?
Ti2 O5 1.9464(17) . ?
Ti2 O3 2.1713(15) . ?
Ti2 N1 2.276(2) . ?
Ti2 Cl1 2.2981(8) . ?
O1 C1 1.367(3) . ?
O2 C12 1.356(3) . ?
O3 C23 1.392(3) . ?
O4 C34 1.354(3) . ?
C1 C6 1.403(3) . ?
C1 C2 1.405(3) . ?
C2 C3 1.389(3) . ?
C2 C44 1.514(3) 2_655 ?
C3 C4 1.408(3) . ?
C3 H3 0.9500 . ?
C4 C5 1.386(3) . ?
C4 C7 1.532(3) . ?
C5 C6 1.405(3) . ?
C5 H5 0.9500 . ?
C6 C11 1.522(3) . ?
C7 C9 1.528(4) . ?
C7 C8 1.536(3) . ?
C7 C10 1.542(4) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.515(3) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 C17 1.394(3) . ?
C12 C13 1.403(3) . ?
C13 C14 1.395(3) . ?
C14 C15 1.399(4) . ?
C14 H14 0.9500 . ?
C15 C16 1.403(4) . ?
C15 C18 1.536(4) . ?
C16 C17 1.400(3) . ?
C16 H16 0.9500 . ?
C17 C22 1.519(3) . ?
C18 C19 1.521(5) . ?
C18 C20 1.535(4) . ?
C18 C21 1.552(4) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C24 1.515(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C23 C28 1.400(3) . ?
C23 C24 1.401(3) . ?
C24 C25 1.398(3) . ?
C25 C26 1.388(4) . ?
C25 H25 0.9500 . ?
C26 C27 1.396(4) . ?
C26 C29 1.543(3) . ?
C27 C28 1.400(3) . ?
C27 H27 0.9500 . ?
C28 C33 1.527(3) . ?
C29 C30 1.516(5) . ?
C29 C32 1.521(4) . ?
C29 C31 1.543(6) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.519(3) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 C35 1.396(3) . ?
C34 C39 1.397(3) . ?
C35 C36 1.395(3) . ?
C36 C37 1.401(3) . ?
C36 H36 0.9500 . ?
C37 C38 1.399(3) . ?
C37 C40 1.532(3) . ?
C38 C39 1.389(3) . ?
C38 H38 0.9500 . ?
C39 C44 1.518(3) . ?
C40 C41 1.527(4) . ?
C40 C42 1.538(4) . ?
C40 C43 1.541(4) . ?
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 0.9900 . ?
C44 H44B 0.9900 . ?
N1 C45 1.150(4) . ?
C45 C46 1.468(4) . ?
C46 H46A 0.9800 . ?
C46 H46B 0.9800 . ?
C46 H46C 0.9800 . ?
O6 Si1 1.661(4) . ?
Si1 O7 1.6235(16) . ?
Si1 C61 1.861(6) . ?
Si1 C60 1.864(6) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
N2 C47 1.134(5) . ?
C47 C48 1.424(5) . ?
C48 H48A 0.9800 . ?
C48 H48B 0.9800 . ?
C48 H48C 0.9800 . ?
N3 C49 1.094(5) . ?
C49 C50 1.425(5) . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
N4 C51 1.131(13) . ?
C51 C52 1.430(15) . ?
C52 H52A 0.9800 . ?
C52 H52B 0.9800 . ?
C52 H52C 0.9800 . ?
N5 C53 1.134(6) . ?
C53 C54 1.458(8) . ?
C54 H54A 0.9800 . ?
C54 H54B 0.9800 . ?
C54 H54C 0.9800 . ?
N5X C53X 1.127(13) . ?
C53X C54X 1.429(14) . ?
C54X H54D 0.9800 . ?
C54X H54E 0.9800 . ?
C54X H54F 0.9800 . ?
N6 C55 1.107(6) . ?
C55 C56 1.383(6) . ?
C56 C55X 1.501(12) . ?
C56 H56A 0.9800 . ?
C56 H56B 0.9800 . ?
C56 H56C 0.9800 . ?
C56 H56D 0.9800 . ?
C56 H56E 0.9800 . ?
C56 H56F 0.9800 . ?
N6X C55X 1.144(13) . ?
N7 C57 1.116(12) . ?
C57 C58 1.415(13) . ?
N7X C57X 1.139(14) . ?
C57X C58X 1.462(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O6 Ti1 O4 106.32(14) . . ?
O6 Ti1 O5 104.64(13) . 2_655 ?
O4 Ti1 O5 95.19(7) . 2_655 ?
O6 Ti1 O3 109.26(12) . . ?
O4 Ti1 O3 94.70(7) . . ?
O5 Ti1 O3 140.24(8) 2_655 . ?
O6 Ti1 O5 101.96(14) . . ?
O4 Ti1 O5 151.71(8) . . ?
O5 Ti1 O5 76.83(7) 2_655 . ?
O3 Ti1 O5 76.37(7) . . ?
O4 Ti1 Cl2X 103.12(10) . . ?
O5 Ti1 Cl2X 110.86(12) 2_655 . ?
O3 Ti1 Cl2X 104.15(12) . . ?
O5 Ti1 Cl2X 105.08(10) . . ?
O6 Ti1 Ti1 97.06(13) . 2_655 ?
O4 Ti1 Ti1 134.65(6) . 2_655 ?
O5 Ti1 Ti1 40.63(5) 2_655 2_655 ?
O3 Ti1 Ti1 113.68(5) . 2_655 ?
O5 Ti1 Ti1 38.36(5) . 2_655 ?
O6 Ti1 Ti2 111.19(12) . . ?
O4 Ti1 Ti2 129.38(6) . . ?
O5 Ti1 Ti2 106.55(5) 2_655 . ?
O3 Ti1 Ti2 41.42(4) . . ?
O5 Ti1 Ti2 35.01(5) . . ?
Cl2X Ti1 Ti2 110.33(10) . . ?
Ti1 Ti1 Ti2 72.515(15) 2_655 . ?
O1 Ti2 O2 97.40(7) . . ?
O1 Ti2 O5 106.85(7) . . ?
O2 Ti2 O5 147.99(8) . . ?
O1 Ti2 O3 172.59(7) . . ?
O2 Ti2 O3 80.80(6) . . ?
O5 Ti2 O3 72.45(6) . . ?
O1 Ti2 N1 80.06(8) . . ?
O2 Ti2 N1 83.49(7) . . ?
O5 Ti2 N1 80.54(8) . . ?
O3 Ti2 N1 92.59(7) . . ?
O1 Ti2 Cl1 96.54(6) . . ?
O2 Ti2 Cl1 101.75(6) . . ?
O5 Ti2 Cl1 96.01(6) . . ?
O3 Ti2 Cl1 90.86(5) . . ?
N1 Ti2 Cl1 174.14(6) . . ?
O1 Ti2 Ti1 142.68(6) . . ?
O2 Ti2 Ti1 115.92(5) . . ?
O5 Ti2 Ti1 36.05(5) . . ?
O3 Ti2 Ti1 36.45(4) . . ?
N1 Ti2 Ti1 87.20(6) . . ?
Cl1 Ti2 Ti1 92.78(2) . . ?
C1 O1 Ti2 147.66(15) . . ?
C12 O2 Ti2 136.67(15) . . ?
C23 O3 Ti1 131.16(13) . . ?
C23 O3 Ti2 126.52(13) . . ?
Ti1 O3 Ti2 102.13(7) . . ?
C34 O4 Ti1 162.38(16) . . ?
Ti1 O5 Ti2 146.04(10) 2_655 . ?
Ti1 O5 Ti1 101.01(7) 2_655 . ?
Ti2 O5 Ti1 108.94(8) . . ?
O1 C1 C6 121.7(2) . . ?
O1 C1 C2 117.7(2) . . ?
C6 C1 C2 120.6(2) . . ?
C3 C2 C1 119.1(2) . . ?
C3 C2 C44 120.7(2) . 2_655 ?
C1 C2 C44 120.2(2) . 2_655 ?
C2 C3 C4 122.1(2) . . ?
C2 C3 H3 119.0 . . ?
C4 C3 H3 119.0 . . ?
C5 C4 C3 117.3(2) . . ?
C5 C4 C7 123.5(2) . . ?
C3 C4 C7 119.3(2) . . ?
C4 C5 C6 122.9(2) . . ?
C4 C5 H5 118.6 . . ?
C6 C5 H5 118.6 . . ?
C1 C6 C5 118.1(2) . . ?
C1 C6 C11 123.7(2) . . ?
C5 C6 C11 118.2(2) . . ?
C9 C7 C4 109.4(2) . . ?
C9 C7 C8 108.5(2) . . ?
C4 C7 C8 112.1(2) . . ?
C9 C7 C10 109.4(2) . . ?
C4 C7 C10 109.3(2) . . ?
C8 C7 C10 108.2(2) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C6 110.1(2) . . ?
C13 C11 H11A 109.6 . . ?
C6 C11 H11A 109.6 . . ?
C13 C11 H11B 109.6 . . ?
C6 C11 H11B 109.6 . . ?
H11A C11 H11B 108.2 . . ?
O2 C12 C17 119.1(2) . . ?
O2 C12 C13 118.7(2) . . ?
C17 C12 C13 122.0(2) . . ?
C14 C13 C12 117.8(2) . . ?
C14 C13 C11 122.3(2) . . ?
C12 C13 C11 119.5(2) . . ?
C13 C14 C15 122.3(2) . . ?
C13 C14 H14 118.9 . . ?
C15 C14 H14 118.9 . . ?
C14 C15 C16 117.9(2) . . ?
C14 C15 C18 119.5(2) . . ?
C16 C15 C18 122.7(3) . . ?
C17 C16 C15 121.7(2) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C12 C17 C16 118.3(2) . . ?
C12 C17 C22 119.7(2) . . ?
C16 C17 C22 121.7(2) . . ?
C19 C18 C20 109.3(3) . . ?
C19 C18 C15 112.2(2) . . ?
C20 C18 C15 108.8(3) . . ?
C19 C18 C21 108.6(3) . . ?
C20 C18 C21 108.9(3) . . ?
C15 C18 C21 108.9(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C24 C22 C17 114.7(2) . . ?
C24 C22 H22A 108.6 . . ?
C17 C22 H22A 108.6 . . ?
C24 C22 H22B 108.6 . . ?
C17 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
O3 C23 C28 120.4(2) . . ?
O3 C23 C24 119.2(2) . . ?
C28 C23 C24 120.3(2) . . ?
C25 C24 C23 118.9(2) . . ?
C25 C24 C22 117.7(2) . . ?
C23 C24 C22 123.4(2) . . ?
C26 C25 C24 122.6(2) . . ?
C26 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
C25 C26 C27 116.9(2) . . ?
C25 C26 C29 122.2(2) . . ?
C27 C26 C29 120.9(3) . . ?
C26 C27 C28 122.9(2) . . ?
C26 C27 H27 118.5 . . ?
C28 C27 H27 118.5 . . ?
C23 C28 C27 118.3(2) . . ?
C23 C28 C33 123.4(2) . . ?
C27 C28 C33 118.2(2) . . ?
C30 C29 C32 109.4(3) . . ?
C30 C29 C26 112.1(3) . . ?
C32 C29 C26 111.3(2) . . ?
C30 C29 C31 109.2(3) . . ?
C32 C29 C31 107.5(3) . . ?
C26 C29 C31 107.2(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C28 113.1(2) . . ?
C35 C33 H33A 109.0 . . ?
C28 C33 H33A 109.0 . . ?
C35 C33 H33B 109.0 . . ?
C28 C33 H33B 109.0 . . ?
H33A C33 H33B 107.8 . . ?
O4 C34 C35 118.90(19) . . ?
O4 C34 C39 119.3(2) . . ?
C35 C34 C39 121.8(2) . . ?
C36 C35 C34 118.2(2) . . ?
C36 C35 C33 122.1(2) . . ?
C34 C35 C33 119.7(2) . . ?
C35 C36 C37 121.8(2) . . ?
C35 C36 H36 119.1 . . ?
C37 C36 H36 119.1 . . ?
C38 C37 C36 117.6(2) . . ?
C38 C37 C40 119.6(2) . . ?
C36 C37 C40 122.8(2) . . ?
C39 C38 C37 122.3(2) . . ?
C39 C38 H38 118.8 . . ?
C37 C38 H38 118.8 . . ?
C38 C39 C34 118.0(2) . . ?
C38 C39 C44 121.2(2) . . ?
C34 C39 C44 120.8(2) . . ?
C41 C40 C37 112.1(2) . . ?
C41 C40 C42 108.4(2) . . ?
C37 C40 C42 108.6(2) . . ?
C41 C40 C43 108.5(2) . . ?
C37 C40 C43 110.4(2) . . ?
C42 C40 C43 108.8(2) . . ?
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 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C2 C44 C39 111.5(2) 2_655 . ?
C2 C44 H44A 109.3 2_655 . ?
C39 C44 H44A 109.3 . . ?
C2 C44 H44B 109.3 2_655 . ?
C39 C44 H44B 109.3 . . ?
H44A C44 H44B 108.0 . . ?
C45 N1 Ti2 145.0(2) . . ?
N1 C45 C46 175.4(4) . . ?
C45 C46 H46A 109.5 . . ?
C45 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C45 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
Si1 O6 Ti1 166.2(2) . . ?
O7 Si1 O6 108.3(2) . . ?
O7 Si1 C61 107.5(3) . . ?
O6 Si1 C61 107.0(3) . . ?
O7 Si1 C60 110.0(3) . . ?
O6 Si1 C60 106.4(3) . . ?
C61 Si1 C60 117.3(4) . . ?
Si1 O7 Si1 152.6(3) 2_655 . ?
Si1 C60 H60A 109.5 . . ?
Si1 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
Si1 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
Si1 C61 H61A 109.5 . . ?
Si1 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
Si1 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
N2 C47 C48 179.3(4) . . ?
C47 C48 H48A 109.5 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C47 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
N3 C49 C50 179.3(5) . . ?
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 . . ?
N4 C51 C52 177(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
N5 C53 C54 177.8(7) . . ?
C53 C54 H54A 109.5 . . ?
C53 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C53 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
N5X C53X C54X 173(3) . . ?
C53X C54X H54D 109.5 . . ?
C53X C54X H54E 109.5 . . ?
H54D C54X H54E 109.5 . . ?
C53X C54X H54F 109.5 . . ?
H54D C54X H54F 109.5 . . ?
H54E C54X H54F 109.5 . . ?
N6 C55 C56 178.2(7) . . ?
C55 C56 H56A 109.5 . . ?
C55 C56 H56B 109.5 . . ?
H56A C56 H56B 109.5 . . ?
C55 C56 H56C 109.5 . . ?
H56A C56 H56C 109.5 . . ?
H56B C56 H56C 109.5 . . ?
C55X C56 H56D 109.5 . . ?
C55X C56 H56E 109.5 . . ?
H56D C56 H56E 109.5 . . ?
C55X C56 H56F 109.5 . . ?
H56D C56 H56F 109.5 . . ?
H56E C56 H56F 109.5 . . ?
N6X C55X C56 176(2) . . ?
N7 C57 C58 175.4(18) . . ?
N7X C57X C58X 161(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
O2 Ti2 O1 C1 42.0(3) . . . . ?
O5 Ti2 O1 C1 -116.9(3) . . . . ?
N1 Ti2 O1 C1 -40.0(3) . . . . ?
Cl1 Ti2 O1 C1 144.8(3) . . . . ?
Ti1 Ti2 O1 C1 -111.9(3) . . . . ?
O1 Ti2 O2 C12 -61.5(2) . . . . ?
O5 Ti2 O2 C12 77.9(3) . . . . ?
O3 Ti2 O2 C12 111.3(2) . . . . ?
N1 Ti2 O2 C12 17.6(2) . . . . ?
Cl1 Ti2 O2 C12 -159.8(2) . . . . ?
Ti1 Ti2 O2 C12 101.2(2) . . . . ?
O6 Ti1 O4 C34 -180(77) . . . . ?
O5 Ti1 O4 C34 -73.1(5) 2_655 . . . ?
O3 Ti1 O4 C34 68.4(5) . . . . ?
O5 Ti1 O4 C34 -1.3(6) . . . . ?
Cl2X Ti1 O4 C34 174.1(5) . . . . ?
Ti1 Ti1 O4 C34 -62.0(5) 2_655 . . . ?
Ti2 Ti1 O4 C34 43.3(5) . . . . ?
Ti2 O1 C1 C6 -58.6(4) . . . . ?
Ti2 O1 C1 C2 120.5(3) . . . . ?
O1 C1 C2 C3 -178.2(2) . . . . ?
C6 C1 C2 C3 1.0(4) . . . . ?
O1 C1 C2 C44 2.8(3) . . . 2_655 ?
C6 C1 C2 C44 -178.1(2) . . . 2_655 ?
C1 C2 C3 C4 -0.7(4) . . . . ?
C44 C2 C3 C4 178.4(2) 2_655 . . . ?
C2 C3 C4 C5 0.1(4) . . . . ?
C2 C3 C4 C7 178.7(2) . . . . ?
C3 C4 C5 C6 0.2(4) . . . . ?
C7 C4 C5 C6 -178.3(2) . . . . ?
O1 C1 C6 C5 178.4(2) . . . . ?
C2 C1 C6 C5 -0.7(4) . . . . ?
O1 C1 C6 C11 1.1(4) . . . . ?
C2 C1 C6 C11 -178.0(2) . . . . ?
C4 C5 C6 C1 0.1(4) . . . . ?
C4 C5 C6 C11 177.5(2) . . . . ?
C5 C4 C7 C9 121.5(3) . . . . ?
C3 C4 C7 C9 -57.0(3) . . . . ?
C5 C4 C7 C8 1.1(4) . . . . ?
C3 C4 C7 C8 -177.4(2) . . . . ?
C5 C4 C7 C10 -118.8(3) . . . . ?
C3 C4 C7 C10 62.7(3) . . . . ?
C1 C6 C11 C13 87.1(3) . . . . ?
C5 C6 C11 C13 -90.2(3) . . . . ?
Ti2 O2 C12 C17 -88.2(3) . . . . ?
Ti2 O2 C12 C13 87.1(3) . . . . ?
O2 C12 C13 C14 -176.4(2) . . . . ?
C17 C12 C13 C14 -1.3(3) . . . . ?
O2 C12 C13 C11 -3.1(3) . . . . ?
C17 C12 C13 C11 172.0(2) . . . . ?
C6 C11 C13 C14 79.7(3) . . . . ?
C6 C11 C13 C12 -93.3(2) . . . . ?
C12 C13 C14 C15 1.9(4) . . . . ?
C11 C13 C14 C15 -171.2(2) . . . . ?
C13 C14 C15 C16 -1.5(4) . . . . ?
C13 C14 C15 C18 178.1(2) . . . . ?
C14 C15 C16 C17 0.5(4) . . . . ?
C18 C15 C16 C17 -179.2(2) . . . . ?
O2 C12 C17 C16 175.4(2) . . . . ?
C13 C12 C17 C16 0.3(3) . . . . ?
O2 C12 C17 C22 1.4(3) . . . . ?
C13 C12 C17 C22 -173.7(2) . . . . ?
C15 C16 C17 C12 0.1(4) . . . . ?
C15 C16 C17 C22 174.0(2) . . . . ?
C14 C15 C18 C19 -174.4(3) . . . . ?
C16 C15 C18 C19 5.2(4) . . . . ?
C14 C15 C18 C20 64.5(3) . . . . ?
C16 C15 C18 C20 -115.8(3) . . . . ?
C14 C15 C18 C21 -54.1(4) . . . . ?
C16 C15 C18 C21 125.6(3) . . . . ?
C12 C17 C22 C24 -54.7(3) . . . . ?
C16 C17 C22 C24 131.6(2) . . . . ?
Ti1 O3 C23 C28 -68.5(3) . . . . ?
Ti2 O3 C23 C28 105.6(2) . . . . ?
Ti1 O3 C23 C24 114.0(2) . . . . ?
Ti2 O3 C23 C24 -72.0(3) . . . . ?
O3 C23 C24 C25 176.5(2) . . . . ?
C28 C23 C24 C25 -1.0(3) . . . . ?
O3 C23 C24 C22 -2.7(3) . . . . ?
C28 C23 C24 C22 179.7(2) . . . . ?
C17 C22 C24 C25 -78.3(3) . . . . ?
C17 C22 C24 C23 100.9(3) . . . . ?
C23 C24 C25 C26 -0.7(4) . . . . ?
C22 C24 C25 C26 178.6(2) . . . . ?
C24 C25 C26 C27 1.6(4) . . . . ?
C24 C25 C26 C29 -175.6(2) . . . . ?
C25 C26 C27 C28 -0.9(4) . . . . ?
C29 C26 C27 C28 176.4(2) . . . . ?
O3 C23 C28 C27 -175.9(2) . . . . ?
C24 C23 C28 C27 1.6(3) . . . . ?
O3 C23 C28 C33 2.8(3) . . . . ?
C24 C23 C28 C33 -179.7(2) . . . . ?
C26 C27 C28 C23 -0.6(4) . . . . ?
C26 C27 C28 C33 -179.4(2) . . . . ?
C25 C26 C29 C30 -12.4(4) . . . . ?
C27 C26 C29 C30 170.5(3) . . . . ?
C25 C26 C29 C32 -135.3(3) . . . . ?
C27 C26 C29 C32 47.6(4) . . . . ?
C25 C26 C29 C31 107.4(3) . . . . ?
C27 C26 C29 C31 -69.8(3) . . . . ?
C23 C28 C33 C35 101.6(3) . . . . ?
C27 C28 C33 C35 -79.7(3) . . . . ?
Ti1 O4 C34 C35 -42.5(6) . . . . ?
Ti1 O4 C34 C39 137.0(4) . . . . ?
O4 C34 C35 C36 -176.5(2) . . . . ?
C39 C34 C35 C36 4.0(3) . . . . ?
O4 C34 C35 C33 3.2(3) . . . . ?
C39 C34 C35 C33 -176.3(2) . . . . ?
C28 C33 C35 C36 104.7(3) . . . . ?
C28 C33 C35 C34 -75.0(3) . . . . ?
C34 C35 C36 C37 -0.9(3) . . . . ?
C33 C35 C36 C37 179.4(2) . . . . ?
C35 C36 C37 C38 -2.0(3) . . . . ?
C35 C36 C37 C40 176.5(2) . . . . ?
C36 C37 C38 C39 2.1(3) . . . . ?
C40 C37 C38 C39 -176.5(2) . . . . ?
C37 C38 C39 C34 0.9(3) . . . . ?
C37 C38 C39 C44 -178.5(2) . . . . ?
O4 C34 C39 C38 176.48(19) . . . . ?
C35 C34 C39 C38 -4.0(3) . . . . ?
O4 C34 C39 C44 -4.2(3) . . . . ?
C35 C34 C39 C44 175.4(2) . . . . ?
C38 C37 C40 C41 -175.6(2) . . . . ?
C36 C37 C40 C41 5.9(3) . . . . ?
C38 C37 C40 C42 64.6(3) . . . . ?
C36 C37 C40 C42 -113.9(3) . . . . ?
C38 C37 C40 C43 -54.6(3) . . . . ?
C36 C37 C40 C43 126.9(3) . . . . ?
C38 C39 C44 C2 52.9(3) . . . 2_655 ?
C34 C39 C44 C2 -126.4(2) . . . 2_655 ?
O4 Ti1 O6 Si1 110.4(10) . . . . ?
O5 Ti1 O6 Si1 10.4(11) 2_655 . . . ?
O3 Ti1 O6 Si1 -148.5(10) . . . . ?
O5 Ti1 O6 Si1 -68.9(11) . . . . ?
Ti1 Ti1 O6 Si1 -30.3(11) 2_655 . . . ?
Ti2 Ti1 O6 Si1 -104.2(10) . . . . ?
Ti1 O6 Si1 O7 34.6(11) . . . . ?
Ti1 O6 Si1 C61 -81.1(11) . . . . ?
Ti1 O6 Si1 C60 152.8(10) . . . . ?
O6 Si1 O7 Si1 -5.51(13) . . . 2_655 ?
C61 Si1 O7 Si1 109.8(3) . . . 2_655 ?
C60 Si1 O7 Si1 -121.4(3) . . . 2_655 ?

_refine_diff_density_max         1.006
_refine_diff_density_min         -0.646
_refine_diff_density_rms         0.067


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

data_2_7_25MeCN
_database_code_depnum_ccdc_archive 'CCDC 1554492'
_audit_update_record             
;
2017-06-06 deposited with the CCDC.
2018-06-11 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_THETM01_2_7_25MeCN          
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: Weakly diffracting, best that could be obtained even with a rotating anode source.
;
_vrf_PLAT029_2_7_25MeCN          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.823 Note
RESPONSE: Problematic data set with several reflections rejected during data reduction.
;
_vrf_PLAT213_2_7_25MeCN          
;
PROBLEM: Atom C54             has ADP max/min Ratio .....        5.6 oblate
RESPONSE: Part of disordered tBu group, already split & restraints applied.
;
_vrf_PLAT413_2_7_25MeCN          
;
PROBLEM: Short Inter XH3 .. XHn     H91C   ..  H93C    ..       1.63 Ang.
RESPONSE: Part of MeCN of crystallisation.
;
# Added during the CSD deposition process: Tuesday 06 June 2017 11:36 AM
# end Validation Reply Form


_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C98 H127 Cl O9 Ti2, 7.25(C2 H3 N)'
_chemical_formula_sum            'C112.50 H148.75 Cl N7.25 O9 Ti2'
_chemical_formula_weight         1877.88

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   26.816(2)
_cell_length_b                   13.2305(9)
_cell_length_c                   32.648(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.480(3)
_cell_angle_gamma                90
_cell_volume                     11215.2(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    55457
_cell_measurement_theta_min      2.91
_cell_measurement_theta_max      27.48

_exptl_crystal_description       lath
_exptl_crystal_colour            red
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_F_000             4030
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.280
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.222
_shelx_estimated_absorpt_T_min   0.940
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.940
_exptl_absorpt_correction_T_max  0.993
_exptl_absorpt_process_details   'SADABS v2007/2, Sheldrick, G.M., (2007)'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker-Nonius FR591 rotating anode'
_diffrn_measurement_device_type  
'Bruker-Nonius APEX II CCD camera on κ-goniostat'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_measurement_method       'φ & ω scans'
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_reflns_number            35666
_diffrn_reflns_av_unetI/netI     0.1220
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         2.936
_diffrn_reflns_theta_max         22.500
_diffrn_reflns_theta_full        22.500
_diffrn_measured_fraction_theta_max 0.823
_diffrn_measured_fraction_theta_full 0.823
_diffrn_reflns_Laue_measured_fraction_max 0.823
_diffrn_reflns_Laue_measured_fraction_full 0.823
_diffrn_reflns_point_group_measured_fraction_max 0.823
_diffrn_reflns_point_group_measured_fraction_full 0.823
_reflns_number_total             12068
_reflns_number_gt                7470
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997) & COLLECT'
_computing_data_reduction        'DENZO & COLLECT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_refine_special_details          ', SQUEEZE'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0391P)²+114.3493P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         12068
_refine_ls_number_parameters     1299
_refine_ls_number_restraints     725
_refine_ls_R_factor_all          0.1868
_refine_ls_R_factor_gt           0.1222
_refine_ls_wR_factor_ref         0.2753
_refine_ls_wR_factor_gt          0.2325
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_restrained_S_all      1.045
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.45517(8) 0.52887(13) 0.22183(6) 0.0371(5) Uani 1 1 d . . . . .
Ti2 Ti 0.37535(7) 0.46264(13) 0.12143(5) 0.0350(5) Uani 1 1 d . . . . .
Cl1 Cl 0.43600(11) 0.60561(18) 0.14911(8) 0.0418(7) Uani 1 1 d . . . . .
O9 O 0.4045(3) 0.4286(6) 0.1847(2) 0.048(2) Uani 1 1 d D . . . .
H9 H 0.397(5) 0.376(5) 0.196(4) 0.073 Uiso 1 1 d D U . . .
O1 O 0.3854(3) 0.6172(4) 0.23718(19) 0.0336(17) Uani 1 1 d . . . . .
C1 C 0.3995(4) 0.6740(7) 0.2755(3) 0.034(3) Uani 1 1 d . . . . .
C2 C 0.3971(4) 0.6305(7) 0.3134(3) 0.033(3) Uani 1 1 d . . . . .
C3 C 0.4097(4) 0.6916(8) 0.3494(3) 0.040(3) Uani 1 1 d . . . . .
H3 H 0.408261 0.662818 0.375763 0.048 Uiso 1 1 calc R U . . .
C4 C 0.4242(4) 0.7918(7) 0.3487(3) 0.032(3) Uani 1 1 d . . . . .
C5 C 0.4282(4) 0.8292(7) 0.3101(3) 0.038(3) Uani 1 1 d . . . . .
H5 H 0.439253 0.897089 0.308819 0.046 Uiso 1 1 calc R U . . .
C6 C 0.4168(4) 0.7729(7) 0.2731(3) 0.037(3) Uani 1 1 d . . . . .
C7 C 0.4374(4) 0.8603(7) 0.3880(3) 0.048(3) Uani 1 1 d D . . . .
C8 C 0.4928(4) 0.8989(9) 0.3951(4) 0.073(4) Uani 1 1 d D . . . .
H8A H 0.500693 0.945015 0.419333 0.109 Uiso 1 1 calc R U . . .
H8B H 0.496500 0.934778 0.369744 0.109 Uiso 1 1 calc R U . . .
H8C H 0.516670 0.841511 0.400661 0.109 Uiso 1 1 calc R U . . .
C9 C 0.4005(4) 0.9522(7) 0.3805(3) 0.047(3) Uani 1 1 d D . . . .
H9A H 0.409520 0.997553 0.404981 0.071 Uiso 1 1 calc R U . . .
H9B H 0.364957 0.928737 0.376619 0.071 Uiso 1 1 calc R U . . .
H9C H 0.403655 0.988588 0.355117 0.071 Uiso 1 1 calc R U . . .
C10 C 0.4322(5) 0.8039(8) 0.4278(3) 0.057(3) Uani 1 1 d D . . . .
H10A H 0.455756 0.746071 0.432955 0.085 Uiso 1 1 calc R U . . .
H10B H 0.396681 0.779829 0.423713 0.085 Uiso 1 1 calc R U . . .
H10C H 0.440698 0.849660 0.452158 0.085 Uiso 1 1 calc R U . . .
C11 C 0.4228(4) 0.8219(7) 0.2328(3) 0.040(3) Uani 1 1 d . . . . .
H11A H 0.402210 0.783307 0.208360 0.048 Uiso 1 1 calc R U . . .
H11B H 0.408500 0.891189 0.231083 0.048 Uiso 1 1 calc R U . . .
O2 O 0.4857(3) 0.6498(5) 0.23805(19) 0.0365(18) Uani 1 1 d . . . . .
C12 C 0.5055(4) 0.7378(7) 0.2291(3) 0.036(3) Uani 1 1 d . . . . .
C13 C 0.4774(4) 0.8277(7) 0.2291(3) 0.037(3) Uani 1 1 d . . . . .
C14 C 0.5015(5) 0.9177(7) 0.2225(3) 0.040(3) Uani 1 1 d . . . . .
H14 H 0.483613 0.979152 0.223650 0.048 Uiso 1 1 calc R U . . .
C15 C 0.5488(5) 0.9235(8) 0.2145(3) 0.043(3) Uani 1 1 d . . . . .
C16 C 0.5738(4) 0.8322(8) 0.2112(3) 0.043(3) Uani 1 1 d . . . . .
H16 H 0.606014 0.833412 0.204005 0.051 Uiso 1 1 calc R U . . .
C17 C 0.5524(5) 0.7386(7) 0.2182(3) 0.037(3) Uani 1 1 d . . . . .
C18 C 0.5736(5) 1.0237(8) 0.2073(4) 0.068(3) Uani 1 1 d D U . . .
C19 C 0.5443(9) 1.1150(12) 0.2176(8) 0.077(6) Uani 0.676(18) 1 d D U P A 1
H19A H 0.561678 1.177150 0.212555 0.115 Uiso 0.676(18) 1 calc R U P A 1
H19B H 0.509071 1.114347 0.199597 0.115 Uiso 0.676(18) 1 calc R U P A 1
H19C H 0.543219 1.112148 0.247407 0.115 Uiso 0.676(18) 1 calc R U P A 1
C20 C 0.5755(10) 1.0317(13) 0.1600(5) 0.078(6) Uani 0.676(18) 1 d D U P A 1
H20A H 0.594236 0.973648 0.152727 0.118 Uiso 0.676(18) 1 calc R U P A 1
H20B H 0.540317 1.032249 0.141930 0.118 Uiso 0.676(18) 1 calc R U P A 1
H20C H 0.593086 1.094312 0.155783 0.118 Uiso 0.676(18) 1 calc R U P A 1
C21 C 0.6287(7) 1.0287(15) 0.2352(8) 0.091(6) Uani 0.676(18) 1 d D U P A 1
H21A H 0.648377 0.970607 0.229149 0.136 Uiso 0.676(18) 1 calc R U P A 1
H21B H 0.645136 1.091377 0.229372 0.136 Uiso 0.676(18) 1 calc R U P A 1
H21C H 0.627934 1.027270 0.265090 0.136 Uiso 0.676(18) 1 calc R U P A 1
C19X C 0.5735(19) 1.099(3) 0.2421(11) 0.080(9) Uani 0.324(18) 1 d D U P A 2
H19D H 0.538452 1.104930 0.245816 0.120 Uiso 0.324(18) 1 calc R U P A 2
H19E H 0.596630 1.075049 0.268507 0.120 Uiso 0.324(18) 1 calc R U P A 2
H19F H 0.585169 1.164558 0.234469 0.120 Uiso 0.324(18) 1 calc R U P A 2
C20X C 0.5385(15) 1.065(3) 0.1644(9) 0.077(9) Uani 0.324(18) 1 d D U P A 2
H20D H 0.538523 1.016265 0.141734 0.115 Uiso 0.324(18) 1 calc R U P A 2
H20E H 0.503262 1.073726 0.167267 0.115 Uiso 0.324(18) 1 calc R U P A 2
H20F H 0.551936 1.129821 0.157577 0.115 Uiso 0.324(18) 1 calc R U P A 2
C21X C 0.6275(11) 1.012(3) 0.2007(17) 0.084(8) Uani 0.324(18) 1 d D U P A 2
H21D H 0.626728 0.963294 0.178039 0.127 Uiso 0.324(18) 1 calc R U P A 2
H21E H 0.639449 1.077717 0.192909 0.127 Uiso 0.324(18) 1 calc R U P A 2
H21F H 0.650911 0.988208 0.226948 0.127 Uiso 0.324(18) 1 calc R U P A 2
C22 C 0.5784(4) 0.6407(7) 0.2094(3) 0.042(3) Uani 1 1 d . . . . .
H22A H 0.554843 0.605106 0.185554 0.051 Uiso 1 1 calc R U . . .
H22B H 0.609917 0.658239 0.200364 0.051 Uiso 1 1 calc R U . . .
O3 O 0.5168(3) 0.4670(5) 0.2193(2) 0.0397(18) Uani 1 1 d . . . . .
C23 C 0.5608(4) 0.4855(7) 0.2503(3) 0.032(3) Uani 1 1 d . . . . .
C24 C 0.5929(4) 0.5688(7) 0.2468(3) 0.038(3) Uani 1 1 d . . . . .
C25 C 0.6376(4) 0.5845(8) 0.2770(3) 0.041(3) Uani 1 1 d . . . . .
H25 H 0.658805 0.639597 0.273399 0.050 Uiso 1 1 calc R U . . .
C26 C 0.6540(5) 0.5232(8) 0.3135(4) 0.051(3) Uani 1 1 d . . . . .
C27 C 0.6205(4) 0.4419(8) 0.3172(3) 0.046(3) Uani 1 1 d . . . . .
H27 H 0.629464 0.399327 0.341384 0.055 Uiso 1 1 calc R U . . .
C28 C 0.5749(4) 0.4230(7) 0.2866(3) 0.042(3) Uani 1 1 d . . . . .
C29 C 0.7047(5) 0.5423(9) 0.3455(4) 0.060(4) Uani 1 1 d . . . . .
C30 C 0.7022(6) 0.6479(10) 0.3653(4) 0.095(5) Uani 1 1 d . . . . .
H30A H 0.693919 0.698875 0.342790 0.143 Uiso 1 1 calc R U . . .
H30B H 0.735583 0.663776 0.384552 0.143 Uiso 1 1 calc R U . . .
H30C H 0.675478 0.648040 0.380994 0.143 Uiso 1 1 calc R U . . .
C31 C 0.7492(5) 0.5364(12) 0.3241(4) 0.086(5) Uani 1 1 d . . . . .
H31A H 0.749446 0.469686 0.311179 0.129 Uiso 1 1 calc R U . . .
H31B H 0.781796 0.547219 0.345276 0.129 Uiso 1 1 calc R U . . .
H31C H 0.744832 0.588682 0.302240 0.129 Uiso 1 1 calc R U . . .
C32 C 0.7150(6) 0.4658(11) 0.3825(4) 0.092(5) Uani 1 1 d . . . . .
H32A H 0.687661 0.470945 0.397440 0.138 Uiso 1 1 calc R U . . .
H32B H 0.748301 0.480981 0.402118 0.138 Uiso 1 1 calc R U . . .
H32C H 0.715711 0.397148 0.371408 0.138 Uiso 1 1 calc R U . . .
C33 C 0.5392(4) 0.3386(7) 0.2935(4) 0.051(3) Uani 1 1 d . . . . .
H33A H 0.515755 0.320407 0.265951 0.061 Uiso 1 1 calc R U . . .
H33B H 0.560177 0.278261 0.304337 0.061 Uiso 1 1 calc R U . . .
O4 O 0.4518(3) 0.4681(5) 0.2703(2) 0.0434(19) Uani 1 1 d . . . . .
C34 C 0.4636(5) 0.4293(7) 0.3099(4) 0.046(3) Uani 1 1 d . . . . .
C35 C 0.5069(4) 0.3655(7) 0.3242(4) 0.043(3) Uani 1 1 d . . . . .
C36 C 0.5156(5) 0.3310(7) 0.3649(4) 0.049(3) Uani 1 1 d . . . . .
H36 H 0.544351 0.287621 0.374910 0.059 Uiso 1 1 calc R U . . .
C37 C 0.4860(5) 0.3543(7) 0.3925(4) 0.042(3) Uani 1 1 d . . . . .
C38 C 0.4441(5) 0.4177(7) 0.3770(3) 0.043(3) Uani 1 1 d . . . . .
H38 H 0.423036 0.436718 0.395256 0.052 Uiso 1 1 calc R U . . .
C39 C 0.4319(4) 0.4543(7) 0.3356(3) 0.039(3) Uani 1 1 d . . . . .
C40 C 0.4991(5) 0.3114(8) 0.4370(3) 0.049(3) Uani 1 1 d . . . . .
C41 C 0.5553(5) 0.3307(11) 0.4582(4) 0.081(5) Uani 1 1 d . . . . .
H41A H 0.576874 0.295719 0.442529 0.121 Uiso 1 1 calc R U . . .
H41B H 0.563126 0.305454 0.487325 0.121 Uiso 1 1 calc R U . . .
H41C H 0.562133 0.403490 0.458420 0.121 Uiso 1 1 calc R U . . .
C42 C 0.4903(5) 0.1958(8) 0.4340(4) 0.065(4) Uani 1 1 d . . . . .
H42A H 0.454174 0.181772 0.420038 0.098 Uiso 1 1 calc R U . . .
H42B H 0.498824 0.166521 0.462430 0.098 Uiso 1 1 calc R U . . .
H42C H 0.512456 0.165822 0.417426 0.098 Uiso 1 1 calc R U . . .
C43 C 0.4651(5) 0.3565(9) 0.4645(4) 0.071(4) Uani 1 1 d . . . . .
H43A H 0.467714 0.430359 0.464586 0.106 Uiso 1 1 calc R U . . .
H43B H 0.476929 0.331144 0.493543 0.106 Uiso 1 1 calc R U . . .
H43C H 0.429168 0.336450 0.452824 0.106 Uiso 1 1 calc R U . . .
C44 C 0.3839(4) 0.5191(7) 0.3182(3) 0.044(3) Uani 1 1 d . . . . .
H44A H 0.360819 0.514042 0.337486 0.053 Uiso 1 1 calc R U . . .
H44B H 0.365188 0.492210 0.290299 0.053 Uiso 1 1 calc R U . . .
O5 O 0.3452(3) 0.3409(5) 0.1091(2) 0.0396(18) Uani 1 1 d . . . . .
C45 C 0.3134(4) 0.2650(7) 0.0921(3) 0.038(3) Uani 1 1 d . . . . .
C46 C 0.2605(4) 0.2743(7) 0.0912(3) 0.039(3) Uani 1 1 d . . . . .
C47 C 0.2279(4) 0.1955(7) 0.0716(3) 0.045(3) Uani 1 1 d . . . . .
H47 H 0.191957 0.200956 0.069106 0.054 Uiso 1 1 calc R U . . .
C48 C 0.2466(5) 0.1099(7) 0.0556(4) 0.049(3) Uani 1 1 d . . . . .
C49 C 0.2983(5) 0.1040(7) 0.0580(3) 0.042(3) Uani 1 1 d . . . . .
H49 H 0.311040 0.046391 0.046496 0.050 Uiso 1 1 calc R U . . .
C50 C 0.3334(4) 0.1805(7) 0.0770(3) 0.037(3) Uani 1 1 d . . . . .
C51 C 0.2096(5) 0.0277(9) 0.0334(4) 0.076(3) Uani 1 1 d D U . . .
C52 C 0.2365(10) -0.0684(16) 0.0247(10) 0.117(8) Uani 0.585(14) 1 d D U P B 1
H52A H 0.264812 -0.050669 0.012000 0.175 Uiso 0.585(14) 1 calc R U P B 1
H52B H 0.250208 -0.104648 0.051301 0.175 Uiso 0.585(14) 1 calc R U P B 1
H52C H 0.211801 -0.111560 0.005178 0.175 Uiso 0.585(14) 1 calc R U P B 1
C53 C 0.1845(9) 0.0733(16) -0.0119(6) 0.084(6) Uani 0.585(14) 1 d D U P B 1
H53A H 0.211429 0.085021 -0.026899 0.127 Uiso 0.585(14) 1 calc R U P B 1
H53B H 0.159084 0.025694 -0.028068 0.127 Uiso 0.585(14) 1 calc R U P B 1
H53C H 0.167541 0.137464 -0.008841 0.127 Uiso 0.585(14) 1 calc R U P B 1
C54 C 0.1645(8) 0.0132(19) 0.0532(7) 0.090(6) Uani 0.585(14) 1 d D U P B 1
H54A H 0.150057 0.079196 0.057480 0.135 Uiso 0.585(14) 1 calc R U P B 1
H54B H 0.138041 -0.027994 0.034408 0.135 Uiso 0.585(14) 1 calc R U P B 1
H54C H 0.176448 -0.021081 0.080531 0.135 Uiso 0.585(14) 1 calc R U P B 1
C52X C 0.2158(12) -0.0580(17) 0.0676(8) 0.081(8) Uani 0.415(14) 1 d D U P B 2
H52D H 0.252130 -0.077886 0.076850 0.122 Uiso 0.415(14) 1 calc R U P B 2
H52E H 0.204275 -0.032966 0.091981 0.122 Uiso 0.415(14) 1 calc R U P B 2
H52F H 0.195019 -0.116606 0.055443 0.122 Uiso 0.415(14) 1 calc R U P B 2
C53X C 0.2270(14) -0.027(3) -0.0030(9) 0.098(8) Uani 0.415(14) 1 d D U P B 2
H53D H 0.263779 -0.042280 0.006259 0.147 Uiso 0.415(14) 1 calc R U P B 2
H53E H 0.207333 -0.089228 -0.010402 0.147 Uiso 0.415(14) 1 calc R U P B 2
H53F H 0.220721 0.017852 -0.027811 0.147 Uiso 0.415(14) 1 calc R U P B 2
C54X C 0.1526(8) 0.054(3) 0.0209(13) 0.110(9) Uani 0.415(14) 1 d D U P B 2
H54D H 0.132888 -0.004153 0.006993 0.165 Uiso 0.415(14) 1 calc R U P B 2
H54E H 0.141178 0.072044 0.046190 0.165 Uiso 0.415(14) 1 calc R U P B 2
H54F H 0.147051 0.111646 0.001316 0.165 Uiso 0.415(14) 1 calc R U P B 2
C55 C 0.3903(4) 0.1757(7) 0.0803(3) 0.035(3) Uani 1 1 d . . . . .
H55A H 0.399831 0.105672 0.074607 0.042 Uiso 1 1 calc R U . . .
H55B H 0.409455 0.193622 0.109402 0.042 Uiso 1 1 calc R U . . .
O6 O 0.4433(3) 0.3708(4) 0.10364(19) 0.0351(17) Uani 1 1 d . . . . .
C56 C 0.4309(4) 0.3400(7) 0.0610(3) 0.033(3) Uani 1 1 d . . . . .
C57 C 0.4058(4) 0.2470(7) 0.0492(3) 0.033(3) Uani 1 1 d . . . . .
C58 C 0.3922(4) 0.2234(7) 0.0060(3) 0.035(3) Uani 1 1 d . . . . .
H58 H 0.376235 0.160028 -0.002339 0.042 Uiso 1 1 calc R U . . .
C59 C 0.4005(4) 0.2865(7) -0.0248(3) 0.034(3) Uani 1 1 d . . . . .
C60 C 0.4237(4) 0.3804(7) -0.0108(3) 0.036(3) Uani 1 1 d . . . . .
H60 H 0.428995 0.427133 -0.031418 0.043 Uiso 1 1 calc R U . . .
C61 C 0.4390(4) 0.4075(7) 0.0313(3) 0.034(3) Uani 1 1 d . . . . .
C62 C 0.3868(4) 0.2587(7) -0.0718(3) 0.041(3) Uani 1 1 d . . . . .
C63 C 0.3440(5) 0.1782(8) -0.0825(3) 0.059(4) Uani 1 1 d . . . . .
H63A H 0.356247 0.115539 -0.067314 0.089 Uiso 1 1 calc R U . . .
H63B H 0.334893 0.165287 -0.113026 0.089 Uiso 1 1 calc R U . . .
H63C H 0.313587 0.202690 -0.073975 0.089 Uiso 1 1 calc R U . . .
C64 C 0.4357(5) 0.2166(10) -0.0816(4) 0.069(4) Uani 1 1 d . . . . .
H64A H 0.463379 0.266655 -0.073763 0.104 Uiso 1 1 calc R U . . .
H64B H 0.428972 0.201766 -0.111854 0.104 Uiso 1 1 calc R U . . .
H64C H 0.445974 0.154473 -0.065320 0.104 Uiso 1 1 calc R U . . .
C65 C 0.3693(6) 0.3507(8) -0.1002(4) 0.075(4) Uani 1 1 d . . . . .
H65A H 0.339488 0.381856 -0.092963 0.112 Uiso 1 1 calc R U . . .
H65B H 0.359807 0.329281 -0.129871 0.112 Uiso 1 1 calc R U . . .
H65C H 0.397486 0.399901 -0.095945 0.112 Uiso 1 1 calc R U . . .
C66 C 0.4625(4) 0.5113(6) 0.0418(3) 0.036(3) Uani 1 1 d . . . . .
H66A H 0.479023 0.514078 0.072526 0.043 Uiso 1 1 calc R U . . .
H66B H 0.489902 0.520563 0.026680 0.043 Uiso 1 1 calc R U . . .
O7 O 0.3727(2) 0.5187(4) 0.07047(19) 0.0322(16) Uani 1 1 d . . . . .
C67 C 0.3827(4) 0.6001(7) 0.0481(3) 0.035(3) Uani 1 1 d . . . . .
C68 C 0.4250(4) 0.5980(7) 0.0307(3) 0.027(2) Uani 1 1 d . . . . .
C69 C 0.4331(4) 0.6779(7) 0.0059(3) 0.030(2) Uani 1 1 d . . . . .
H69 H 0.461527 0.675672 -0.006545 0.037 Uiso 1 1 calc R U . . .
C70 C 0.4003(4) 0.7624(6) -0.0014(3) 0.036(3) Uani 1 1 d . . . . .
C71 C 0.3610(4) 0.7661(7) 0.0183(3) 0.038(3) Uani 1 1 d . . . . .
H71 H 0.339582 0.824348 0.014526 0.046 Uiso 1 1 calc R U . . .
C72 C 0.3508(4) 0.6868(6) 0.0442(3) 0.030(2) Uani 1 1 d . . . . .
C73 C 0.4098(4) 0.8521(7) -0.0295(3) 0.037(3) Uani 1 1 d . . . . .
C74 C 0.4564(4) 0.8363(7) -0.0475(3) 0.046(3) Uani 1 1 d . . . . .
H74A H 0.450223 0.778389 -0.066827 0.069 Uiso 1 1 calc R U . . .
H74B H 0.486896 0.823368 -0.024368 0.069 Uiso 1 1 calc R U . . .
H74C H 0.462030 0.897052 -0.062942 0.069 Uiso 1 1 calc R U . . .
C75 C 0.3624(5) 0.8672(8) -0.0654(4) 0.065(4) Uani 1 1 d . . . . .
H75A H 0.368007 0.923894 -0.083046 0.098 Uiso 1 1 calc R U . . .
H75B H 0.332774 0.881982 -0.053824 0.098 Uiso 1 1 calc R U . . .
H75C H 0.355571 0.805659 -0.082570 0.098 Uiso 1 1 calc R U . . .
C76 C 0.4216(5) 0.9468(7) -0.0015(4) 0.062(4) Uani 1 1 d . . . . .
H76A H 0.427720 1.004274 -0.018492 0.092 Uiso 1 1 calc R U . . .
H76B H 0.452315 0.934799 0.021595 0.092 Uiso 1 1 calc R U . . .
H76C H 0.392235 0.961661 0.010389 0.092 Uiso 1 1 calc R U . . .
C77 C 0.3123(4) 0.6967(7) 0.0698(3) 0.039(3) Uani 1 1 d . . . . .
H77A H 0.295599 0.763578 0.063717 0.046 Uiso 1 1 calc R U . . .
H77B H 0.331059 0.696129 0.100038 0.046 Uiso 1 1 calc R U . . .
O8 O 0.3152(3) 0.5268(5) 0.1255(2) 0.0382(18) Uani 1 1 d . . . . .
C78 C 0.2746(4) 0.5361(7) 0.0905(3) 0.037(3) Uani 1 1 d . . . . .
C79 C 0.2708(4) 0.6175(7) 0.0632(3) 0.037(3) Uani 1 1 d . . . . .
C80 C 0.2270(4) 0.6241(7) 0.0288(3) 0.037(3) Uani 1 1 d . . . . .
H80 H 0.223549 0.681190 0.010686 0.045 Uiso 1 1 calc R U . . .
C81 C 0.1885(4) 0.5510(7) 0.0202(3) 0.039(3) Uani 1 1 d . . . . .
C82 C 0.1941(4) 0.4703(8) 0.0480(3) 0.040(3) Uani 1 1 d . . . . .
H82 H 0.168286 0.419446 0.043117 0.048 Uiso 1 1 calc R U . . .
C83 C 0.2359(4) 0.4608(7) 0.0826(3) 0.036(3) Uani 1 1 d . . . . .
C84 C 0.1406(4) 0.5652(8) -0.0167(3) 0.053(3) Uani 1 1 d D U . . .
C85 C 0.1561(11) 0.601(3) -0.0571(7) 0.070(7) Uani 0.62(4) 1 d D U P C 1
H85A H 0.176574 0.663302 -0.050729 0.104 Uiso 0.62(4) 1 calc R U P C 1
H85B H 0.176506 0.548652 -0.066365 0.104 Uiso 0.62(4) 1 calc R U P C 1
H85C H 0.124987 0.614738 -0.079552 0.104 Uiso 0.62(4) 1 calc R U P C 1
C86 C 0.1087(13) 0.4685(17) -0.0278(11) 0.080(8) Uani 0.62(4) 1 d D U P C 1
H86A H 0.078805 0.481957 -0.051441 0.120 Uiso 0.62(4) 1 calc R U P C 1
H86B H 0.129979 0.415637 -0.036020 0.120 Uiso 0.62(4) 1 calc R U P C 1
H86C H 0.097036 0.445888 -0.003212 0.120 Uiso 0.62(4) 1 calc R U P C 1
C87 C 0.1055(11) 0.647(3) -0.0037(9) 0.078(8) Uani 0.62(4) 1 d D U P C 1
H87A H 0.125037 0.710074 0.003593 0.117 Uiso 0.62(4) 1 calc R U P C 1
H87B H 0.075514 0.659671 -0.027421 0.117 Uiso 0.62(4) 1 calc R U P C 1
H87C H 0.093877 0.623450 0.020781 0.117 Uiso 0.62(4) 1 calc R U P C 1
C85X C 0.1443(19) 0.650(3) -0.0491(12) 0.068(9) Uani 0.38(4) 1 d D U P C 2
H85D H 0.154873 0.713116 -0.033966 0.102 Uiso 0.38(4) 1 calc R U P C 2
H85E H 0.169796 0.630117 -0.064525 0.102 Uiso 0.38(4) 1 calc R U P C 2
H85F H 0.110651 0.658476 -0.069041 0.102 Uiso 0.38(4) 1 calc R U P C 2
C86X C 0.1240(19) 0.468(2) -0.0419(16) 0.067(10) Uani 0.38(4) 1 d D U P C 2
H86D H 0.093382 0.480928 -0.064888 0.101 Uiso 0.38(4) 1 calc R U P C 2
H86E H 0.152024 0.443754 -0.053748 0.101 Uiso 0.38(4) 1 calc R U P C 2
H86F H 0.115934 0.415647 -0.023092 0.101 Uiso 0.38(4) 1 calc R U P C 2
C87X C 0.0968(13) 0.593(4) 0.0049(12) 0.065(9) Uani 0.38(4) 1 d D U P C 2
H87D H 0.105894 0.654909 0.021374 0.097 Uiso 0.38(4) 1 calc R U P C 2
H87E H 0.064619 0.603065 -0.016832 0.097 Uiso 0.38(4) 1 calc R U P C 2
H87F H 0.092341 0.537583 0.023682 0.097 Uiso 0.38(4) 1 calc R U P C 2
C88 C 0.2411(4) 0.3648(7) 0.1102(3) 0.042(3) Uani 1 1 d . . . . .
H88A H 0.264915 0.379159 0.138032 0.050 Uiso 1 1 calc R U . . .
H88B H 0.207017 0.348452 0.115091 0.050 Uiso 1 1 calc R U . . .
C102 C 0.3298(5) 0.6033(8) 0.2207(3) 0.048(3) Uani 1 1 d . . . . .
H98A H 0.313908 0.593200 0.244687 0.058 Uiso 1 1 calc R U . . .
H98B H 0.323529 0.541601 0.203009 0.058 Uiso 1 1 calc R U . . .
C103 C 0.3044(4) 0.6915(7) 0.1948(3) 0.046(3) Uani 1 1 d . . . . .
H99A H 0.321030 0.703722 0.171397 0.055 Uiso 1 1 calc R U . . .
H99B H 0.308988 0.752864 0.212738 0.055 Uiso 1 1 calc R U . . .
C104 C 0.2472(5) 0.6722(8) 0.1767(4) 0.054(3) Uani 1 1 d . . . . .
H10D H 0.230487 0.665562 0.200360 0.064 Uiso 1 1 calc R U . . .
H10E H 0.242966 0.607163 0.161236 0.064 Uiso 1 1 calc R U . . .
C105 C 0.2197(5) 0.7549(9) 0.1468(4) 0.071(4) Uani 1 1 d . . . . .
H10F H 0.240080 0.770191 0.126125 0.085 Uiso 1 1 calc R U . . .
H10G H 0.218507 0.817022 0.163434 0.085 Uiso 1 1 calc R U . . .
C106 C 0.1648(6) 0.7272(11) 0.1227(5) 0.104(5) Uani 1 1 d . . . . .
H10H H 0.165525 0.665290 0.106363 0.157 Uiso 1 1 calc R U . . .
H10I H 0.150080 0.782387 0.103464 0.157 Uiso 1 1 calc R U . . .
H10J H 0.143717 0.716103 0.142847 0.157 Uiso 1 1 calc R U . . .
C107 C 0.4902(4) 0.3275(7) 0.1314(3) 0.040(3) Uani 1 1 d . . . . .
H10K H 0.494369 0.257096 0.122495 0.048 Uiso 1 1 calc R U . . .
H10L H 0.486482 0.325731 0.160769 0.048 Uiso 1 1 calc R U . . .
C108 C 0.5383(4) 0.3884(7) 0.1300(3) 0.039(3) Uani 1 1 d . . . . .
H10M H 0.542874 0.387817 0.100890 0.047 Uiso 1 1 calc R U . . .
H10N H 0.533639 0.459418 0.137872 0.047 Uiso 1 1 calc R U . . .
C109 C 0.5855(4) 0.3454(7) 0.1598(3) 0.045(3) Uani 1 1 d . . . . .
H10O H 0.590112 0.274965 0.151230 0.054 Uiso 1 1 calc R U . . .
H10P H 0.579640 0.343118 0.188584 0.054 Uiso 1 1 calc R U . . .
C110 C 0.6349(4) 0.4034(9) 0.1618(4) 0.063(4) Uani 1 1 d . . . . .
H10Q H 0.642245 0.401505 0.133601 0.075 Uiso 1 1 calc R U . . .
H10R H 0.629654 0.474948 0.168570 0.075 Uiso 1 1 calc R U . . .
C111 C 0.6813(5) 0.3629(10) 0.1942(5) 0.098(5) Uani 1 1 d . . . . .
H10S H 0.674918 0.366298 0.222457 0.148 Uiso 1 1 calc R U . . .
H10T H 0.711662 0.403666 0.193678 0.148 Uiso 1 1 calc R U . . .
H10U H 0.687419 0.292498 0.187481 0.148 Uiso 1 1 calc R U . . .
N1 N 0.4035(13) 0.233(2) 0.2162(7) 0.325(14) Uani 1 1 d D U . . .
C90 C 0.4173(12) 0.196(2) 0.2511(7) 0.259(12) Uani 1 1 d D U . . .
C91 C 0.4169(10) 0.1603(18) 0.2915(6) 0.225(12) Uani 1 1 d D U . . .
H91A H 0.401069 0.211016 0.306239 0.337 Uiso 1 1 calc R U . . .
H91B H 0.452253 0.147343 0.307807 0.337 Uiso 1 1 calc R U . . .
H91C H 0.396926 0.097528 0.288752 0.337 Uiso 1 1 calc R U . . .
N2 N 0.3035(10) 0.0696(15) 0.1696(6) 0.146(8) Uani 0.75 1 d D U P D 1
C92 C 0.2972(12) 0.0509(18) 0.2039(6) 0.148(9) Uani 0.75 1 d D U P D 1
C93 C 0.3129(12) 0.0122(18) 0.2452(6) 0.165(10) Uani 0.75 1 d D U P D 1
H93A H 0.285179 0.021700 0.259582 0.247 Uiso 0.75 1 calc R U P D 1
H93B H 0.320472 -0.060045 0.244081 0.247 Uiso 0.75 1 calc R U P D 1
H93C H 0.343790 0.047971 0.260818 0.247 Uiso 0.75 1 calc R U P D 1
N3 N 0.5727(8) 0.6203(11) 0.4227(4) 0.154(7) Uani 1 1 d D U . . .
C94 C 0.5582(7) 0.6329(11) 0.3864(4) 0.097(5) Uani 1 1 d D U . . .
C95 C 0.5426(5) 0.6508(9) 0.3424(3) 0.062(3) Uani 1 1 d D U . . .
H95A H 0.548060 0.722150 0.336704 0.093 Uiso 1 1 calc R U . . .
H95B H 0.506006 0.634223 0.331885 0.093 Uiso 1 1 calc R U . . .
H95C H 0.562937 0.608429 0.327972 0.093 Uiso 1 1 calc R U . . .
N4 N 0.3703(5) 0.9125(8) 0.1260(4) 0.079(3) Uani 1 1 d D U . . .
C96 C 0.4086(5) 0.8833(10) 0.1199(4) 0.062(3) Uani 1 1 d D U . . .
C97 C 0.4556(5) 0.8461(9) 0.1128(4) 0.062(3) Uani 1 1 d D U . . .
H97A H 0.477326 0.819667 0.139336 0.093 Uiso 1 1 calc R U . . .
H97B H 0.473668 0.901131 0.102468 0.093 Uiso 1 1 calc R U . . .
H97C H 0.448098 0.791928 0.091667 0.093 Uiso 1 1 calc R U . . .
N5 N 0.2236(9) 0.320(2) -0.0747(8) 0.153(10) Uani 0.658(19) 1 d D U P E 1
C98 C 0.2502(10) 0.349(2) -0.0418(8) 0.121(7) Uani 0.658(19) 1 d D U P E 1
C99 C 0.2858(6) 0.4010(12) -0.0095(5) 0.103(5) Uani 1 1 d D U . . .
H99C H 0.320597 0.375439 -0.007648 0.155 Uiso 0.658(19) 1 calc R U P E 1
H99D H 0.277034 0.390209 0.017562 0.155 Uiso 0.658(19) 1 calc R U P E 1
H99E H 0.284457 0.473395 -0.016006 0.155 Uiso 0.658(19) 1 calc R U P E 1
H99F H 0.275527 0.455414 0.007032 0.155 Uiso 0.342(19) 1 calc R U P E 2
H99G H 0.323359 0.400822 -0.004739 0.155 Uiso 0.342(19) 1 calc R U P E 2
H99H H 0.274465 0.335899 -0.000689 0.155 Uiso 0.342(19) 1 calc R U P E 2
N5X N 0.2418(17) 0.429(4) -0.0892(8) 0.142(11) Uani 0.342(19) 1 d D U P E 2
C98X C 0.263(2) 0.417(5) -0.0530(8) 0.117(8) Uani 0.342(19) 1 d D U P E 2
N6 N 0.2735(16) 0.839(3) 0.2817(12) 0.177(12) Uani 0.5 1 d D U P . .
C100 C 0.2277(17) 0.828(5) 0.2713(17) 0.166(13) Uani 0.346(17) 1 d D U P F 1
C101 C 0.1795(16) 0.825(2) 0.2813(13) 0.101(12) Uani 0.346(17) 1 d D U P F 1
C10X C 0.272(5) 0.755(5) 0.293(4) 0.172(14) Uani 0.154(17) 1 d D U P F 2
C11X C 0.256(6) 0.659(6) 0.305(6) 0.22(2) Uani 0.154(17) 1 d D U P F 2


_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 O4 1.796(7) . ?
Ti1 O2 1.814(6) . ?
Ti1 O3 1.864(7) . ?
Ti1 O9 2.061(7) . ?
Ti1 O1 2.363(7) . ?
Ti1 Cl1 2.514(3) . ?
Ti2 O5 1.802(6) . ?
Ti2 O7 1.807(6) . ?
Ti2 O8 1.856(7) . ?
Ti2 O9 2.067(7) . ?
Ti2 O6 2.380(7) . ?
Ti2 Cl1 2.511(3) . ?
O9 H9 0.83(2) . ?
O1 C1 1.427(11) . ?
O1 C102 1.465(12) . ?
C1 C2 1.380(13) . ?
C1 C6 1.397(13) . ?
C2 C3 1.399(13) . ?
C2 C44 1.533(13) . ?
C3 C4 1.383(13) . ?
C3 H3 0.9500 . ?
C4 C5 1.384(13) . ?
C4 C7 1.539(13) . ?
C5 C6 1.385(13) . ?
C5 H5 0.9500 . ?
C6 C11 1.513(13) . ?
C7 C8 1.534(12) . ?
C7 C10 1.534(11) . ?
C7 C9 1.548(13) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 C13 1.501(14) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
O2 C12 1.343(11) . ?
C12 C17 1.391(14) . ?
C12 C13 1.407(14) . ?
C13 C14 1.397(13) . ?
C14 C15 1.359(14) . ?
C14 H14 0.9500 . ?
C15 C16 1.399(14) . ?
C15 C18 1.528(15) . ?
C16 C17 1.406(13) . ?
C16 H16 0.9500 . ?
C17 C22 1.532(13) . ?
C18 C19X 1.507(18) . ?
C18 C21X 1.520(18) . ?
C18 C19 1.524(15) . ?
C18 C21 1.531(16) . ?
C18 C20 1.561(18) . ?
C18 C20X 1.58(2) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C19X H19D 0.9800 . ?
C19X H19E 0.9800 . ?
C19X H19F 0.9800 . ?
C20X H20D 0.9800 . ?
C20X H20E 0.9800 . ?
C20X H20F 0.9800 . ?
C21X H21D 0.9800 . ?
C21X H21E 0.9800 . ?
C21X H21F 0.9800 . ?
C22 C24 1.520(13) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
O3 C23 1.370(11) . ?
C23 C28 1.415(13) . ?
C23 C24 1.422(13) . ?
C24 C25 1.363(13) . ?
C25 C26 1.417(14) . ?
C25 H25 0.9500 . ?
C26 C27 1.427(15) . ?
C26 C29 1.514(15) . ?
C27 C28 1.396(14) . ?
C27 H27 0.9500 . ?
C28 C33 1.525(14) . ?
C29 C31 1.526(16) . ?
C29 C32 1.547(16) . ?
C29 C30 1.549(16) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 C35 1.519(14) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
O4 C34 1.355(12) . ?
C34 C39 1.377(14) . ?
C34 C35 1.417(15) . ?
C35 C36 1.369(14) . ?
C36 C37 1.377(14) . ?
C36 H36 0.9500 . ?
C37 C38 1.394(14) . ?
C37 C40 1.517(14) . ?
C38 C39 1.395(13) . ?
C38 H38 0.9500 . ?
C39 C44 1.531(13) . ?
C40 C41 1.514(15) . ?
C40 C42 1.547(14) . ?
C40 C43 1.549(16) . ?
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 0.9900 . ?
C44 H44B 0.9900 . ?
O5 C45 1.344(11) . ?
C45 C50 1.383(13) . ?
C45 C46 1.417(14) . ?
C46 C47 1.407(14) . ?
C46 C88 1.500(13) . ?
C47 C48 1.391(14) . ?
C47 H47 0.9500 . ?
C48 C49 1.371(14) . ?
C48 C51 1.528(15) . ?
C49 C50 1.416(14) . ?
C49 H49 0.9500 . ?
C50 C55 1.504(13) . ?
C51 C54 1.517(14) . ?
C51 C54X 1.520(16) . ?
C51 C52 1.524(14) . ?
C51 C53X 1.557(19) . ?
C51 C52X 1.571(15) . ?
C51 C53 1.584(17) . ?
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 . ?
C52X H52D 0.9800 . ?
C52X H52E 0.9800 . ?
C52X H52F 0.9800 . ?
C53X H53D 0.9800 . ?
C53X H53E 0.9800 . ?
C53X H53F 0.9800 . ?
C54X H54D 0.9800 . ?
C54X H54E 0.9800 . ?
C54X H54F 0.9800 . ?
C55 C57 1.519(12) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
O6 C56 1.408(11) . ?
O6 C107 1.469(11) . ?
C56 C61 1.376(13) . ?
C56 C57 1.408(13) . ?
C57 C58 1.399(13) . ?
C58 C59 1.369(12) . ?
C58 H58 0.9500 . ?
C59 C60 1.412(13) . ?
C59 C62 1.529(14) . ?
C60 C61 1.382(13) . ?
C60 H60 0.9500 . ?
C61 C66 1.513(12) . ?
C62 C64 1.528(15) . ?
C62 C65 1.531(14) . ?
C62 C63 1.541(14) . ?
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 C68 1.510(13) . ?
C66 H66A 0.9900 . ?
C66 H66B 0.9900 . ?
O7 C67 1.363(11) . ?
C67 C68 1.391(13) . ?
C67 C72 1.418(13) . ?
C68 C69 1.381(12) . ?
C69 C70 1.405(13) . ?
C69 H69 0.9500 . ?
C70 C71 1.369(14) . ?
C70 C73 1.559(13) . ?
C71 C72 1.416(13) . ?
C71 H71 0.9500 . ?
C72 C77 1.485(13) . ?
C73 C75 1.513(14) . ?
C73 C74 1.522(14) . ?
C73 C76 1.537(13) . ?
C74 H74A 0.9800 . ?
C74 H74B 0.9800 . ?
C74 H74C 0.9800 . ?
C75 H75A 0.9800 . ?
C75 H75B 0.9800 . ?
C75 H75C 0.9800 . ?
C76 H76A 0.9800 . ?
C76 H76B 0.9800 . ?
C76 H76C 0.9800 . ?
C77 C79 1.505(13) . ?
C77 H77A 0.9900 . ?
C77 H77B 0.9900 . ?
O8 C78 1.374(11) . ?
C78 C79 1.387(13) . ?
C78 C83 1.415(14) . ?
C79 C80 1.409(13) . ?
C80 C81 1.390(13) . ?
C80 H80 0.9500 . ?
C81 C82 1.385(13) . ?
C81 C84 1.537(14) . ?
C82 C83 1.382(13) . ?
C82 H82 0.9500 . ?
C83 C88 1.544(13) . ?
C84 C86 1.531(18) . ?
C84 C86X 1.54(2) . ?
C84 C85 1.554(15) . ?
C84 C87X 1.555(17) . ?
C84 C85X 1.558(17) . ?
C84 C87 1.563(15) . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?
C86 H86A 0.9800 . ?
C86 H86B 0.9800 . ?
C86 H86C 0.9800 . ?
C87 H87A 0.9800 . ?
C87 H87B 0.9800 . ?
C87 H87C 0.9800 . ?
C85X H85D 0.9800 . ?
C85X H85E 0.9800 . ?
C85X H85F 0.9800 . ?
C86X H86D 0.9800 . ?
C86X H86E 0.9800 . ?
C86X H86F 0.9800 . ?
C87X H87D 0.9800 . ?
C87X H87E 0.9800 . ?
C87X H87F 0.9800 . ?
C88 H88A 0.9900 . ?
C88 H88B 0.9900 . ?
C102 C103 1.501(13) . ?
C102 H98A 0.9900 . ?
C102 H98B 0.9900 . ?
C103 C104 1.520(15) . ?
C103 H99A 0.9900 . ?
C103 H99B 0.9900 . ?
C104 C105 1.527(15) . ?
C104 H10D 0.9900 . ?
C104 H10E 0.9900 . ?
C105 C106 1.530(17) . ?
C105 H10F 0.9900 . ?
C105 H10G 0.9900 . ?
C106 H10H 0.9800 . ?
C106 H10I 0.9800 . ?
C106 H10J 0.9800 . ?
C107 C108 1.530(13) . ?
C107 H10K 0.9900 . ?
C107 H10L 0.9900 . ?
C108 C109 1.502(13) . ?
C108 H10M 0.9900 . ?
C108 H10N 0.9900 . ?
C109 C110 1.519(15) . ?
C109 H10O 0.9900 . ?
C109 H10P 0.9900 . ?
C110 C111 1.515(15) . ?
C110 H10Q 0.9900 . ?
C110 H10R 0.9900 . ?
C111 H10S 0.9800 . ?
C111 H10T 0.9800 . ?
C111 H10U 0.9800 . ?
N1 C90 1.208(16) . ?
C90 C91 1.407(16) . ?
C91 H91A 0.9800 . ?
C91 H91B 0.9800 . ?
C91 H91C 0.9800 . ?
N2 C92 1.197(15) . ?
C92 C93 1.406(16) . ?
C93 H93A 0.9800 . ?
C93 H93B 0.9800 . ?
C93 H93C 0.9800 . ?
N3 C94 1.163(12) . ?
C94 C95 1.414(13) . ?
C95 H95A 0.9800 . ?
C95 H95B 0.9800 . ?
C95 H95C 0.9800 . ?
N4 C96 1.160(12) . ?
C96 C97 1.425(13) . ?
C97 H97A 0.9800 . ?
C97 H97B 0.9800 . ?
C97 H97C 0.9800 . ?
N5 C98 1.190(16) . ?
C98 C99 1.413(16) . ?
C99 C98X 1.416(17) . ?
C99 H99C 0.9800 . ?
C99 H99D 0.9800 . ?
C99 H99E 0.9800 . ?
C99 H99F 0.9800 . ?
C99 H99G 0.9800 . ?
C99 H99H 0.9800 . ?
N5X C98X 1.186(17) . ?
N6 C10X 1.186(18) . ?
N6 C100 1.198(18) . ?
C100 C101 1.413(18) . ?
C10X C11X 1.413(19) . ?

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
O4 Ti1 O2 104.8(3) . . ?
O4 Ti1 O3 94.7(3) . . ?
O2 Ti1 O3 93.4(3) . . ?
O4 Ti1 O9 93.4(3) . . ?
O2 Ti1 O9 157.1(3) . . ?
O3 Ti1 O9 98.8(3) . . ?
O4 Ti1 O1 79.5(3) . . ?
O2 Ti1 O1 79.9(3) . . ?
O3 Ti1 O1 169.7(3) . . ?
O9 Ti1 O1 90.2(3) . . ?
O4 Ti1 Cl1 165.7(3) . . ?
O2 Ti1 Cl1 83.7(2) . . ?
O3 Ti1 Cl1 96.3(2) . . ?
O9 Ti1 Cl1 75.8(2) . . ?
O1 Ti1 Cl1 90.85(17) . . ?
O5 Ti2 O7 104.5(3) . . ?
O5 Ti2 O8 94.4(3) . . ?
O7 Ti2 O8 92.5(3) . . ?
O5 Ti2 O9 93.7(3) . . ?
O7 Ti2 O9 158.0(3) . . ?
O8 Ti2 O9 98.4(3) . . ?
O5 Ti2 O6 79.5(3) . . ?
O7 Ti2 O6 80.8(3) . . ?
O8 Ti2 O6 169.4(3) . . ?
O9 Ti2 O6 90.6(3) . . ?
O5 Ti2 Cl1 165.4(2) . . ?
O7 Ti2 Cl1 83.9(2) . . ?
O8 Ti2 Cl1 97.2(2) . . ?
O9 Ti2 Cl1 75.8(2) . . ?
O6 Ti2 Cl1 90.33(17) . . ?
Ti2 Cl1 Ti1 89.81(10) . . ?
Ti1 O9 Ti2 118.5(4) . . ?
Ti1 O9 H9 119(9) . . ?
Ti2 O9 H9 123(9) . . ?
C1 O1 C102 114.2(7) . . ?
C1 O1 Ti1 113.4(6) . . ?
C102 O1 Ti1 130.3(5) . . ?
C2 C1 C6 122.1(9) . . ?
C2 C1 O1 120.3(8) . . ?
C6 C1 O1 117.6(9) . . ?
C1 C2 C3 117.2(9) . . ?
C1 C2 C44 123.9(9) . . ?
C3 C2 C44 118.8(9) . . ?
C4 C3 C2 123.4(9) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 116.3(9) . . ?
C3 C4 C7 123.9(9) . . ?
C5 C4 C7 119.7(8) . . ?
C4 C5 C6 123.4(9) . . ?
C4 C5 H5 118.3 . . ?
C6 C5 H5 118.3 . . ?
C5 C6 C1 117.3(9) . . ?
C5 C6 C11 118.7(9) . . ?
C1 C6 C11 124.0(9) . . ?
C8 C7 C10 109.0(9) . . ?
C8 C7 C4 109.4(8) . . ?
C10 C7 C4 111.6(8) . . ?
C8 C7 C9 108.6(9) . . ?
C10 C7 C9 109.1(8) . . ?
C4 C7 C9 109.0(8) . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C11 C6 114.2(8) . . ?
C13 C11 H11A 108.7 . . ?
C6 C11 H11A 108.7 . . ?
C13 C11 H11B 108.7 . . ?
C6 C11 H11B 108.7 . . ?
H11A C11 H11B 107.6 . . ?
C12 O2 Ti1 151.1(6) . . ?
O2 C12 C17 119.7(9) . . ?
O2 C12 C13 119.4(10) . . ?
C17 C12 C13 120.8(9) . . ?
C14 C13 C12 116.9(10) . . ?
C14 C13 C11 123.6(10) . . ?
C12 C13 C11 119.3(9) . . ?
C15 C14 C13 124.6(10) . . ?
C15 C14 H14 117.7 . . ?
C13 C14 H14 117.7 . . ?
C14 C15 C16 117.0(10) . . ?
C14 C15 C18 122.8(10) . . ?
C16 C15 C18 120.2(11) . . ?
C15 C16 C17 121.7(11) . . ?
C15 C16 H16 119.2 . . ?
C17 C16 H16 119.2 . . ?
C12 C17 C16 118.7(9) . . ?
C12 C17 C22 121.6(9) . . ?
C16 C17 C22 119.5(10) . . ?
C19X C18 C21X 111(2) . . ?
C19X C18 C15 111.9(19) . . ?
C21X C18 C15 113.6(17) . . ?
C19 C18 C15 112.7(11) . . ?
C19 C18 C21 108.0(14) . . ?
C15 C18 C21 109.8(12) . . ?
C19 C18 C20 108.1(12) . . ?
C15 C18 C20 109.4(11) . . ?
C21 C18 C20 108.7(12) . . ?
C19X C18 C20X 109.2(18) . . ?
C21X C18 C20X 106.6(18) . . ?
C15 C18 C20X 104.4(16) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C18 C21 H21A 109.5 . . ?
C18 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C18 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C18 C19X H19D 109.5 . . ?
C18 C19X H19E 109.5 . . ?
H19D C19X H19E 109.5 . . ?
C18 C19X H19F 109.5 . . ?
H19D C19X H19F 109.5 . . ?
H19E C19X H19F 109.5 . . ?
C18 C20X H20D 109.5 . . ?
C18 C20X H20E 109.5 . . ?
H20D C20X H20E 109.5 . . ?
C18 C20X H20F 109.5 . . ?
H20D C20X H20F 109.5 . . ?
H20E C20X H20F 109.5 . . ?
C18 C21X H21D 109.5 . . ?
C18 C21X H21E 109.5 . . ?
H21D C21X H21E 109.5 . . ?
C18 C21X H21F 109.5 . . ?
H21D C21X H21F 109.5 . . ?
H21E C21X H21F 109.5 . . ?
C24 C22 C17 114.6(8) . . ?
C24 C22 H22A 108.6 . . ?
C17 C22 H22A 108.6 . . ?
C24 C22 H22B 108.6 . . ?
C17 C22 H22B 108.6 . . ?
H22A C22 H22B 107.6 . . ?
C23 O3 Ti1 119.9(6) . . ?
O3 C23 C28 120.9(9) . . ?
O3 C23 C24 120.4(8) . . ?
C28 C23 C24 118.7(10) . . ?
C25 C24 C23 120.1(9) . . ?
C25 C24 C22 119.2(10) . . ?
C23 C24 C22 120.7(9) . . ?
C24 C25 C26 123.6(10) . . ?
C24 C25 H25 118.2 . . ?
C26 C25 H25 118.2 . . ?
C25 C26 C27 115.7(10) . . ?
C25 C26 C29 121.4(11) . . ?
C27 C26 C29 122.8(10) . . ?
C28 C27 C26 122.1(10) . . ?
C28 C27 H27 119.0 . . ?
C26 C27 H27 119.0 . . ?
C27 C28 C23 119.9(10) . . ?
C27 C28 C33 119.6(9) . . ?
C23 C28 C33 120.4(10) . . ?
C26 C29 C31 110.3(10) . . ?
C26 C29 C32 112.7(11) . . ?
C31 C29 C32 108.4(11) . . ?
C26 C29 C30 108.2(9) . . ?
C31 C29 C30 110.9(12) . . ?
C32 C29 C30 106.4(11) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C29 C32 H32A 109.5 . . ?
C29 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C29 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C35 C33 C28 114.1(9) . . ?
C35 C33 H33A 108.7 . . ?
C28 C33 H33A 108.7 . . ?
C35 C33 H33B 108.7 . . ?
C28 C33 H33B 108.7 . . ?
H33A C33 H33B 107.6 . . ?
C34 O4 Ti1 163.8(8) . . ?
O4 C34 C39 117.3(10) . . ?
O4 C34 C35 121.1(10) . . ?
C39 C34 C35 121.6(10) . . ?
C36 C35 C34 116.4(11) . . ?
C36 C35 C33 125.1(11) . . ?
C34 C35 C33 118.5(10) . . ?
C35 C36 C37 125.1(11) . . ?
C35 C36 H36 117.5 . . ?
C37 C36 H36 117.5 . . ?
C36 C37 C38 116.3(10) . . ?
C36 C37 C40 120.7(11) . . ?
C38 C37 C40 123.0(11) . . ?
C37 C38 C39 122.2(11) . . ?
C37 C38 H38 118.9 . . ?
C39 C38 H38 118.9 . . ?
C34 C39 C38 118.4(10) . . ?
C34 C39 C44 119.9(9) . . ?
C38 C39 C44 121.7(11) . . ?
C41 C40 C37 109.8(9) . . ?
C41 C40 C42 108.3(10) . . ?
C37 C40 C42 108.2(9) . . ?
C41 C40 C43 109.4(10) . . ?
C37 C40 C43 112.5(10) . . ?
C42 C40 C43 108.5(9) . . ?
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 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C43 H43A 109.5 . . ?
C40 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C40 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C39 C44 C2 112.5(8) . . ?
C39 C44 H44A 109.1 . . ?
C2 C44 H44A 109.1 . . ?
C39 C44 H44B 109.1 . . ?
C2 C44 H44B 109.1 . . ?
H44A C44 H44B 107.8 . . ?
C45 O5 Ti2 164.3(7) . . ?
O5 C45 C50 119.2(10) . . ?
O5 C45 C46 118.2(9) . . ?
C50 C45 C46 122.5(10) . . ?
C47 C46 C45 116.7(10) . . ?
C47 C46 C88 122.6(10) . . ?
C45 C46 C88 120.6(9) . . ?
C48 C47 C46 122.1(11) . . ?
C48 C47 H47 118.9 . . ?
C46 C47 H47 118.9 . . ?
C49 C48 C47 118.7(10) . . ?
C49 C48 C51 121.0(10) . . ?
C47 C48 C51 120.3(11) . . ?
C48 C49 C50 122.4(10) . . ?
C48 C49 H49 118.8 . . ?
C50 C49 H49 118.8 . . ?
C45 C50 C49 117.4(10) . . ?
C45 C50 C55 119.1(9) . . ?
C49 C50 C55 123.5(9) . . ?
C54 C51 C52 116.0(16) . . ?
C54 C51 C48 112.4(12) . . ?
C54X C51 C48 117.0(16) . . ?
C52 C51 C48 113.6(13) . . ?
C54X C51 C53X 111.9(17) . . ?
C48 C51 C53X 114.0(16) . . ?
C54X C51 C52X 106.2(18) . . ?
C48 C51 C52X 103.6(13) . . ?
C53X C51 C52X 102.2(14) . . ?
C54 C51 C53 104.4(13) . . ?
C52 C51 C53 104.7(14) . . ?
C48 C51 C53 104.2(11) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C51 C52X H52D 109.5 . . ?
C51 C52X H52E 109.5 . . ?
H52D C52X H52E 109.5 . . ?
C51 C52X H52F 109.5 . . ?
H52D C52X H52F 109.5 . . ?
H52E C52X H52F 109.5 . . ?
C51 C53X H53D 109.5 . . ?
C51 C53X H53E 109.5 . . ?
H53D C53X H53E 109.5 . . ?
C51 C53X H53F 109.5 . . ?
H53D C53X H53F 109.5 . . ?
H53E C53X H53F 109.5 . . ?
C51 C54X H54D 109.5 . . ?
C51 C54X H54E 109.5 . . ?
H54D C54X H54E 109.5 . . ?
C51 C54X H54F 109.5 . . ?
H54D C54X H54F 109.5 . . ?
H54E C54X H54F 109.5 . . ?
C50 C55 C57 111.6(8) . . ?
C50 C55 H55A 109.3 . . ?
C57 C55 H55A 109.3 . . ?
C50 C55 H55B 109.3 . . ?
C57 C55 H55B 109.3 . . ?
H55A C55 H55B 108.0 . . ?
C56 O6 C107 116.8(7) . . ?
C56 O6 Ti2 112.5(5) . . ?
C107 O6 Ti2 129.7(6) . . ?
C61 C56 C57 121.5(9) . . ?
C61 C56 O6 117.9(8) . . ?
C57 C56 O6 120.3(9) . . ?
C58 C57 C56 117.3(8) . . ?
C58 C57 C55 119.2(8) . . ?
C56 C57 C55 123.4(9) . . ?
C59 C58 C57 123.7(9) . . ?
C59 C58 H58 118.1 . . ?
C57 C58 H58 118.1 . . ?
C58 C59 C60 115.9(9) . . ?
C58 C59 C62 123.3(9) . . ?
C60 C59 C62 120.8(9) . . ?
C61 C60 C59 123.3(9) . . ?
C61 C60 H60 118.4 . . ?
C59 C60 H60 118.4 . . ?
C56 C61 C60 118.2(9) . . ?
C56 C61 C66 124.1(9) . . ?
C60 C61 C66 117.7(8) . . ?
C64 C62 C59 107.1(9) . . ?
C64 C62 C65 108.2(10) . . ?
C59 C62 C65 112.1(8) . . ?
C64 C62 C63 109.3(9) . . ?
C59 C62 C63 111.9(9) . . ?
C65 C62 C63 108.3(9) . . ?
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 . . ?
C68 C66 C61 114.8(8) . . ?
C68 C66 H66A 108.6 . . ?
C61 C66 H66A 108.6 . . ?
C68 C66 H66B 108.6 . . ?
C61 C66 H66B 108.6 . . ?
H66A C66 H66B 107.5 . . ?
C67 O7 Ti2 148.1(6) . . ?
O7 C67 C68 119.5(8) . . ?
O7 C67 C72 119.5(9) . . ?
C68 C67 C72 121.0(9) . . ?
C69 C68 C67 119.2(9) . . ?
C69 C68 C66 122.0(9) . . ?
C67 C68 C66 118.6(8) . . ?
C68 C69 C70 121.7(9) . . ?
C68 C69 H69 119.1 . . ?
C70 C69 H69 119.1 . . ?
C71 C70 C69 118.1(9) . . ?
C71 C70 C73 120.6(9) . . ?
C69 C70 C73 121.2(10) . . ?
C70 C71 C72 122.8(9) . . ?
C70 C71 H71 118.6 . . ?
C72 C71 H71 118.6 . . ?
C71 C72 C67 116.8(9) . . ?
C71 C72 C77 122.3(9) . . ?
C67 C72 C77 120.6(9) . . ?
C75 C73 C74 109.4(9) . . ?
C75 C73 C76 111.2(9) . . ?
C74 C73 C76 106.0(9) . . ?
C75 C73 C70 109.0(9) . . ?
C74 C73 C70 113.2(8) . . ?
C76 C73 C70 108.1(8) . . ?
C73 C74 H74A 109.5 . . ?
C73 C74 H74B 109.5 . . ?
H74A C74 H74B 109.5 . . ?
C73 C74 H74C 109.5 . . ?
H74A C74 H74C 109.5 . . ?
H74B C74 H74C 109.5 . . ?
C73 C75 H75A 109.5 . . ?
C73 C75 H75B 109.5 . . ?
H75A C75 H75B 109.5 . . ?
C73 C75 H75C 109.5 . . ?
H75A C75 H75C 109.5 . . ?
H75B C75 H75C 109.5 . . ?
C73 C76 H76A 109.5 . . ?
C73 C76 H76B 109.5 . . ?
H76A C76 H76B 109.5 . . ?
C73 C76 H76C 109.5 . . ?
H76A C76 H76C 109.5 . . ?
H76B C76 H76C 109.5 . . ?
C72 C77 C79 116.8(8) . . ?
C72 C77 H77A 108.1 . . ?
C79 C77 H77A 108.1 . . ?
C72 C77 H77B 108.1 . . ?
C79 C77 H77B 108.1 . . ?
H77A C77 H77B 107.3 . . ?
C78 O8 Ti2 120.3(6) . . ?
O8 C78 C79 121.4(9) . . ?
O8 C78 C83 118.9(9) . . ?
C79 C78 C83 119.7(10) . . ?
C78 C79 C80 118.2(9) . . ?
C78 C79 C77 121.0(10) . . ?
C80 C79 C77 120.8(9) . . ?
C81 C80 C79 123.1(9) . . ?
C81 C80 H80 118.4 . . ?
C79 C80 H80 118.4 . . ?
C82 C81 C80 116.8(10) . . ?
C82 C81 C84 122.7(9) . . ?
C80 C81 C84 120.4(9) . . ?
C83 C82 C81 122.5(10) . . ?
C83 C82 H82 118.7 . . ?
C81 C82 H82 118.7 . . ?
C82 C83 C78 119.6(9) . . ?
C82 C83 C88 119.2(9) . . ?
C78 C83 C88 121.1(9) . . ?
C86 C84 C81 113.1(15) . . ?
C86X C84 C81 113(2) . . ?
C86 C84 C85 107.9(13) . . ?
C81 C84 C85 110.7(13) . . ?
C86X C84 C87X 106.8(17) . . ?
C81 C84 C87X 104.6(17) . . ?
C86X C84 C85X 107.3(17) . . ?
C81 C84 C85X 115.8(18) . . ?
C87X C84 C85X 108.9(19) . . ?
C86 C84 C87 107.9(14) . . ?
C81 C84 C87 108.4(12) . . ?
C85 C84 C87 108.9(14) . . ?
C84 C85 H85A 109.5 . . ?
C84 C85 H85B 109.5 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.5 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?
C84 C86 H86A 109.5 . . ?
C84 C86 H86B 109.5 . . ?
H86A C86 H86B 109.5 . . ?
C84 C86 H86C 109.5 . . ?
H86A C86 H86C 109.5 . . ?
H86B C86 H86C 109.5 . . ?
C84 C87 H87A 109.5 . . ?
C84 C87 H87B 109.5 . . ?
H87A C87 H87B 109.5 . . ?
C84 C87 H87C 109.5 . . ?
H87A C87 H87C 109.5 . . ?
H87B C87 H87C 109.5 . . ?
C84 C85X H85D 109.5 . . ?
C84 C85X H85E 109.5 . . ?
H85D C85X H85E 109.5 . . ?
C84 C85X H85F 109.5 . . ?
H85D C85X H85F 109.5 . . ?
H85E C85X H85F 109.5 . . ?
C84 C86X H86D 109.5 . . ?
C84 C86X H86E 109.5 . . ?
H86D C86X H86E 109.5 . . ?
C84 C86X H86F 109.5 . . ?
H86D C86X H86F 109.5 . . ?
H86E C86X H86F 109.5 . . ?
C84 C87X H87D 109.5 . . ?
C84 C87X H87E 109.5 . . ?
H87D C87X H87E 109.5 . . ?
C84 C87X H87F 109.5 . . ?
H87D C87X H87F 109.5 . . ?
H87E C87X H87F 109.5 . . ?
C46 C88 C83 113.9(8) . . ?
C46 C88 H88A 108.8 . . ?
C83 C88 H88A 108.8 . . ?
C46 C88 H88B 108.8 . . ?
C83 C88 H88B 108.8 . . ?
H88A C88 H88B 107.7 . . ?
O1 C102 C103 112.8(9) . . ?
O1 C102 H98A 109.0 . . ?
C103 C102 H98A 109.0 . . ?
O1 C102 H98B 109.0 . . ?
C103 C102 H98B 109.0 . . ?
H98A C102 H98B 107.8 . . ?
C102 C103 C104 111.1(9) . . ?
C102 C103 H99A 109.4 . . ?
C104 C103 H99A 109.4 . . ?
C102 C103 H99B 109.4 . . ?
C104 C103 H99B 109.4 . . ?
H99A C103 H99B 108.0 . . ?
C103 C104 C105 114.0(10) . . ?
C103 C104 H10D 108.7 . . ?
C105 C104 H10D 108.7 . . ?
C103 C104 H10E 108.7 . . ?
C105 C104 H10E 108.7 . . ?
H10D C104 H10E 107.6 . . ?
C104 C105 C106 114.0(12) . . ?
C104 C105 H10F 108.8 . . ?
C106 C105 H10F 108.8 . . ?
C104 C105 H10G 108.8 . . ?
C106 C105 H10G 108.8 . . ?
H10F C105 H10G 107.7 . . ?
C105 C106 H10H 109.5 . . ?
C105 C106 H10I 109.5 . . ?
H10H C106 H10I 109.5 . . ?
C105 C106 H10J 109.5 . . ?
H10H C106 H10J 109.5 . . ?
H10I C106 H10J 109.5 . . ?
O6 C107 C108 112.0(7) . . ?
O6 C107 H10K 109.2 . . ?
C108 C107 H10K 109.2 . . ?
O6 C107 H10L 109.2 . . ?
C108 C107 H10L 109.2 . . ?
H10K C107 H10L 107.9 . . ?
C109 C108 C107 111.3(8) . . ?
C109 C108 H10M 109.4 . . ?
C107 C108 H10M 109.4 . . ?
C109 C108 H10N 109.4 . . ?
C107 C108 H10N 109.4 . . ?
H10M C108 H10N 108.0 . . ?
C108 C109 C110 115.0(9) . . ?
C108 C109 H10O 108.5 . . ?
C110 C109 H10O 108.5 . . ?
C108 C109 H10P 108.5 . . ?
C110 C109 H10P 108.5 . . ?
H10O C109 H10P 107.5 . . ?
C111 C110 C109 114.0(10) . . ?
C111 C110 H10Q 108.7 . . ?
C109 C110 H10Q 108.7 . . ?
C111 C110 H10R 108.7 . . ?
C109 C110 H10R 108.7 . . ?
H10Q C110 H10R 107.6 . . ?
C110 C111 H10S 109.5 . . ?
C110 C111 H10T 109.5 . . ?
H10S C111 H10T 109.5 . . ?
C110 C111 H10U 109.5 . . ?
H10S C111 H10U 109.5 . . ?
H10T C111 H10U 109.5 . . ?
N1 C90 C91 162(4) . . ?
C90 C91 H91A 109.5 . . ?
C90 C91 H91B 109.5 . . ?
H91A C91 H91B 109.5 . . ?
C90 C91 H91C 109.5 . . ?
H91A C91 H91C 109.5 . . ?
H91B C91 H91C 109.5 . . ?
N2 C92 C93 153(3) . . ?
C92 C93 H93A 109.5 . . ?
C92 C93 H93B 109.5 . . ?
H93A C93 H93B 109.5 . . ?
C92 C93 H93C 109.5 . . ?
H93A C93 H93C 109.5 . . ?
H93B C93 H93C 109.5 . . ?
N3 C94 C95 177(2) . . ?
C94 C95 H95A 109.5 . . ?
C94 C95 H95B 109.5 . . ?
H95A C95 H95B 109.5 . . ?
C94 C95 H95C 109.5 . . ?
H95A C95 H95C 109.5 . . ?
H95B C95 H95C 109.5 . . ?
N4 C96 C97 179.2(15) . . ?
C96 C97 H97A 109.5 . . ?
C96 C97 H97B 109.5 . . ?
H97A C97 H97B 109.5 . . ?
C96 C97 H97C 109.5 . . ?
H97A C97 H97C 109.5 . . ?
H97B C97 H97C 109.5 . . ?
N5 C98 C99 165(4) . . ?
C98 C99 H99C 109.5 . . ?
C98 C99 H99D 109.5 . . ?
H99C C99 H99D 109.5 . . ?
C98 C99 H99E 109.5 . . ?
H99C C99 H99E 109.5 . . ?
H99D C99 H99E 109.5 . . ?
C98X C99 H99F 109.5 . . ?
C98X C99 H99G 109.5 . . ?
H99F C99 H99G 109.5 . . ?
C98X C99 H99H 109.5 . . ?
H99F C99 H99H 109.5 . . ?
H99G C99 H99H 109.5 . . ?
N5X C98X C99 178(7) . . ?
N6 C100 C101 150(5) . . ?
N6 C10X C11X 165(10) . . ?

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
C102 O1 C1 C2 75.3(11) . . . . ?
Ti1 O1 C1 C2 -90.0(10) . . . . ?
C102 O1 C1 C6 -106.5(10) . . . . ?
Ti1 O1 C1 C6 88.3(9) . . . . ?
C6 C1 C2 C3 4.0(16) . . . . ?
O1 C1 C2 C3 -177.9(9) . . . . ?
C6 C1 C2 C44 -173.2(9) . . . . ?
O1 C1 C2 C44 5.0(15) . . . . ?
C1 C2 C3 C4 0.0(16) . . . . ?
C44 C2 C3 C4 177.2(9) . . . . ?
C2 C3 C4 C5 -3.0(16) . . . . ?
C2 C3 C4 C7 179.0(10) . . . . ?
C3 C4 C5 C6 2.2(16) . . . . ?
C7 C4 C5 C6 -179.6(10) . . . . ?
C4 C5 C6 C1 1.4(16) . . . . ?
C4 C5 C6 C11 -179.7(9) . . . . ?
C2 C1 C6 C5 -4.6(15) . . . . ?
O1 C1 C6 C5 177.2(9) . . . . ?
C2 C1 C6 C11 176.5(10) . . . . ?
O1 C1 C6 C11 -1.7(15) . . . . ?
C3 C4 C7 C8 120.5(11) . . . . ?
C5 C4 C7 C8 -57.5(13) . . . . ?
C3 C4 C7 C10 -0.3(15) . . . . ?
C5 C4 C7 C10 -178.3(9) . . . . ?
C3 C4 C7 C9 -120.9(10) . . . . ?
C5 C4 C7 C9 61.1(12) . . . . ?
C5 C6 C11 C13 78.4(12) . . . . ?
C1 C6 C11 C13 -102.8(12) . . . . ?
O4 Ti1 O2 C12 175.6(14) . . . . ?
O3 Ti1 O2 C12 79.8(14) . . . . ?
O9 Ti1 O2 C12 -42.5(18) . . . . ?
O1 Ti1 O2 C12 -108.2(14) . . . . ?
Cl1 Ti1 O2 C12 -16.2(14) . . . . ?
Ti1 O2 C12 C17 -71.8(17) . . . . ?
Ti1 O2 C12 C13 105.5(14) . . . . ?
O2 C12 C13 C14 175.6(8) . . . . ?
C17 C12 C13 C14 -7.2(14) . . . . ?
O2 C12 C13 C11 -8.9(14) . . . . ?
C17 C12 C13 C11 168.3(9) . . . . ?
C6 C11 C13 C14 -124.1(10) . . . . ?
C6 C11 C13 C12 60.7(12) . . . . ?
C12 C13 C14 C15 2.8(15) . . . . ?
C11 C13 C14 C15 -172.5(10) . . . . ?
C13 C14 C15 C16 2.5(16) . . . . ?
C13 C14 C15 C18 179.8(10) . . . . ?
C14 C15 C16 C17 -3.6(15) . . . . ?
C18 C15 C16 C17 179.0(10) . . . . ?
O2 C12 C17 C16 -176.6(8) . . . . ?
C13 C12 C17 C16 6.2(15) . . . . ?
O2 C12 C17 C22 9.6(15) . . . . ?
C13 C12 C17 C22 -167.6(9) . . . . ?
C15 C16 C17 C12 -0.7(15) . . . . ?
C15 C16 C17 C22 173.3(9) . . . . ?
C14 C15 C18 C19X 51(3) . . . . ?
C16 C15 C18 C19X -131(2) . . . . ?
C14 C15 C18 C21X 178(2) . . . . ?
C16 C15 C18 C21X -5(3) . . . . ?
C14 C15 C18 C19 10.0(18) . . . . ?
C16 C15 C18 C19 -172.8(14) . . . . ?
C14 C15 C18 C21 130.4(14) . . . . ?
C16 C15 C18 C21 -52.4(16) . . . . ?
C14 C15 C18 C20 -110.3(14) . . . . ?
C16 C15 C18 C20 66.9(16) . . . . ?
C14 C15 C18 C20X -67(2) . . . . ?
C16 C15 C18 C20X 111(2) . . . . ?
C12 C17 C22 C24 -62.1(13) . . . . ?
C16 C17 C22 C24 124.1(10) . . . . ?
O4 Ti1 O3 C23 -63.3(7) . . . . ?
O2 Ti1 O3 C23 41.9(7) . . . . ?
O9 Ti1 O3 C23 -157.5(6) . . . . ?
O1 Ti1 O3 C23 -7.8(18) . . . . ?
Cl1 Ti1 O3 C23 125.9(6) . . . . ?
Ti1 O3 C23 C28 91.4(9) . . . . ?
Ti1 O3 C23 C24 -88.0(10) . . . . ?
O3 C23 C24 C25 -177.6(9) . . . . ?
C28 C23 C24 C25 3.0(14) . . . . ?
O3 C23 C24 C22 1.9(14) . . . . ?
C28 C23 C24 C22 -177.5(9) . . . . ?
C17 C22 C24 C25 -82.0(13) . . . . ?
C17 C22 C24 C23 98.5(11) . . . . ?
C23 C24 C25 C26 -1.9(16) . . . . ?
C22 C24 C25 C26 178.6(9) . . . . ?
C24 C25 C26 C27 -0.2(16) . . . . ?
C24 C25 C26 C29 178.2(10) . . . . ?
C25 C26 C27 C28 1.1(15) . . . . ?
C29 C26 C27 C28 -177.3(10) . . . . ?
C26 C27 C28 C23 0.1(16) . . . . ?
C26 C27 C28 C33 -176.6(10) . . . . ?
O3 C23 C28 C27 178.5(9) . . . . ?
C24 C23 C28 C27 -2.1(14) . . . . ?
O3 C23 C28 C33 -4.8(14) . . . . ?
C24 C23 C28 C33 174.6(9) . . . . ?
C25 C26 C29 C31 -58.3(14) . . . . ?
C27 C26 C29 C31 120.0(13) . . . . ?
C25 C26 C29 C32 -179.5(11) . . . . ?
C27 C26 C29 C32 -1.2(16) . . . . ?
C25 C26 C29 C30 63.2(15) . . . . ?
C27 C26 C29 C30 -118.5(12) . . . . ?
C27 C28 C33 C35 77.1(12) . . . . ?
C23 C28 C33 C35 -99.5(12) . . . . ?
O2 Ti1 O4 C34 -51(2) . . . . ?
O3 Ti1 O4 C34 44(2) . . . . ?
O9 Ti1 O4 C34 143(2) . . . . ?
O1 Ti1 O4 C34 -128(2) . . . . ?
Cl1 Ti1 O4 C34 -176.1(19) . . . . ?
Ti1 O4 C34 C39 131(2) . . . . ?
Ti1 O4 C34 C35 -49(3) . . . . ?
O4 C34 C35 C36 179.5(9) . . . . ?
C39 C34 C35 C36 -0.5(16) . . . . ?
O4 C34 C35 C33 -1.9(15) . . . . ?
C39 C34 C35 C33 178.1(9) . . . . ?
C28 C33 C35 C36 -105.0(12) . . . . ?
C28 C33 C35 C34 76.5(13) . . . . ?
C34 C35 C36 C37 -0.6(16) . . . . ?
C33 C35 C36 C37 -179.1(10) . . . . ?
C35 C36 C37 C38 0.2(16) . . . . ?
C35 C36 C37 C40 179.8(10) . . . . ?
C36 C37 C38 C39 1.2(15) . . . . ?
C40 C37 C38 C39 -178.3(9) . . . . ?
O4 C34 C39 C38 -178.1(9) . . . . ?
C35 C34 C39 C38 1.9(15) . . . . ?
O4 C34 C39 C44 3.1(14) . . . . ?
C35 C34 C39 C44 -176.9(9) . . . . ?
C37 C38 C39 C34 -2.3(15) . . . . ?
C37 C38 C39 C44 176.5(9) . . . . ?
C36 C37 C40 C41 51.1(14) . . . . ?
C38 C37 C40 C41 -129.4(12) . . . . ?
C36 C37 C40 C42 -66.9(13) . . . . ?
C38 C37 C40 C42 112.6(12) . . . . ?
C36 C37 C40 C43 173.3(10) . . . . ?
C38 C37 C40 C43 -7.2(15) . . . . ?
C34 C39 C44 C2 -74.4(12) . . . . ?
C38 C39 C44 C2 106.9(11) . . . . ?
C1 C2 C44 C39 99.8(12) . . . . ?
C3 C2 C44 C39 -77.3(12) . . . . ?
O7 Ti2 O5 C45 -44(3) . . . . ?
O8 Ti2 O5 C45 50(3) . . . . ?
O9 Ti2 O5 C45 148(3) . . . . ?
O6 Ti2 O5 C45 -122(3) . . . . ?
Cl1 Ti2 O5 C45 -168(2) . . . . ?
Ti2 O5 C45 C50 126(2) . . . . ?
Ti2 O5 C45 C46 -55(3) . . . . ?
O5 C45 C46 C47 177.4(8) . . . . ?
C50 C45 C46 C47 -3.8(14) . . . . ?
O5 C45 C46 C88 -2.3(14) . . . . ?
C50 C45 C46 C88 176.5(9) . . . . ?
C45 C46 C47 C48 3.1(15) . . . . ?
C88 C46 C47 C48 -177.2(9) . . . . ?
C46 C47 C48 C49 -2.1(16) . . . . ?
C46 C47 C48 C51 -178.2(10) . . . . ?
C47 C48 C49 C50 1.6(16) . . . . ?
C51 C48 C49 C50 177.7(10) . . . . ?
O5 C45 C50 C49 -177.8(8) . . . . ?
C46 C45 C50 C49 3.4(14) . . . . ?
O5 C45 C50 C55 0.4(13) . . . . ?
C46 C45 C50 C55 -178.4(9) . . . . ?
C48 C49 C50 C45 -2.2(15) . . . . ?
C48 C49 C50 C55 179.6(9) . . . . ?
C49 C48 C51 C54 148.1(15) . . . . ?
C47 C48 C51 C54 -35.8(18) . . . . ?
C49 C48 C51 C54X -162(2) . . . . ?
C47 C48 C51 C54X 14(2) . . . . ?
C49 C48 C51 C52 14(2) . . . . ?
C47 C48 C51 C52 -170.0(16) . . . . ?
C49 C48 C51 C53X -29(2) . . . . ?
C47 C48 C51 C53X 146.9(17) . . . . ?
C49 C48 C51 C52X 81.0(17) . . . . ?
C47 C48 C51 C52X -102.9(16) . . . . ?
C49 C48 C51 C53 -99.4(14) . . . . ?
C47 C48 C51 C53 76.7(15) . . . . ?
C45 C50 C55 C57 -72.2(11) . . . . ?
C49 C50 C55 C57 105.8(10) . . . . ?
C107 O6 C56 C61 -105.7(10) . . . . ?
Ti2 O6 C56 C61 85.0(9) . . . . ?
C107 O6 C56 C57 80.8(11) . . . . ?
Ti2 O6 C56 C57 -88.5(9) . . . . ?
C61 C56 C57 C58 3.6(15) . . . . ?
O6 C56 C57 C58 176.8(9) . . . . ?
C61 C56 C57 C55 -172.5(9) . . . . ?
O6 C56 C57 C55 0.7(15) . . . . ?
C50 C55 C57 C58 -72.3(11) . . . . ?
C50 C55 C57 C56 103.8(11) . . . . ?
C56 C57 C58 C59 -1.9(16) . . . . ?
C55 C57 C58 C59 174.4(9) . . . . ?
C57 C58 C59 C60 -0.8(15) . . . . ?
C57 C58 C59 C62 178.2(10) . . . . ?
C58 C59 C60 C61 2.1(15) . . . . ?
C62 C59 C60 C61 -176.9(10) . . . . ?
C57 C56 C61 C60 -2.4(15) . . . . ?
O6 C56 C61 C60 -175.8(9) . . . . ?
C57 C56 C61 C66 175.9(9) . . . . ?
O6 C56 C61 C66 2.5(15) . . . . ?
C59 C60 C61 C56 -0.6(16) . . . . ?
C59 C60 C61 C66 -179.0(9) . . . . ?
C58 C59 C62 C64 -95.5(12) . . . . ?
C60 C59 C62 C64 83.5(12) . . . . ?
C58 C59 C62 C65 146.0(11) . . . . ?
C60 C59 C62 C65 -35.0(14) . . . . ?
C58 C59 C62 C63 24.2(14) . . . . ?
C60 C59 C62 C63 -156.8(10) . . . . ?
C56 C61 C66 C68 -106.6(11) . . . . ?
C60 C61 C66 C68 71.7(12) . . . . ?
O5 Ti2 O7 C67 177.5(12) . . . . ?
O8 Ti2 O7 C67 82.3(12) . . . . ?
O9 Ti2 O7 C67 -37.7(16) . . . . ?
O6 Ti2 O7 C67 -106.0(12) . . . . ?
Cl1 Ti2 O7 C67 -14.7(12) . . . . ?
Ti2 O7 C67 C68 103.0(12) . . . . ?
Ti2 O7 C67 C72 -74.9(15) . . . . ?
O7 C67 C68 C69 176.1(8) . . . . ?
C72 C67 C68 C69 -6.1(14) . . . . ?
O7 C67 C68 C66 -7.9(13) . . . . ?
C72 C67 C68 C66 170.0(8) . . . . ?
C61 C66 C68 C69 -126.4(10) . . . . ?
C61 C66 C68 C67 57.7(12) . . . . ?
C67 C68 C69 C70 1.4(14) . . . . ?
C66 C68 C69 C70 -174.5(9) . . . . ?
C68 C69 C70 C71 3.0(14) . . . . ?
C68 C69 C70 C73 -180.0(8) . . . . ?
C69 C70 C71 C72 -2.7(15) . . . . ?
C73 C70 C71 C72 -179.8(8) . . . . ?
C70 C71 C72 C67 -1.7(14) . . . . ?
C70 C71 C72 C77 172.2(10) . . . . ?
O7 C67 C72 C71 -176.0(8) . . . . ?
C68 C67 C72 C71 6.2(14) . . . . ?
O7 C67 C72 C77 10.0(14) . . . . ?
C68 C67 C72 C77 -167.8(9) . . . . ?
C71 C70 C73 C75 -60.2(12) . . . . ?
C69 C70 C73 C75 122.7(11) . . . . ?
C71 C70 C73 C74 177.8(9) . . . . ?
C69 C70 C73 C74 0.8(13) . . . . ?
C71 C70 C73 C76 60.7(13) . . . . ?
C69 C70 C73 C76 -116.3(11) . . . . ?
C71 C72 C77 C79 125.2(10) . . . . ?
C67 C72 C77 C79 -61.1(13) . . . . ?
O5 Ti2 O8 C78 -65.2(7) . . . . ?
O7 Ti2 O8 C78 39.6(7) . . . . ?
O9 Ti2 O8 C78 -159.6(7) . . . . ?
O6 Ti2 O8 C78 -11.4(18) . . . . ?
Cl1 Ti2 O8 C78 123.8(6) . . . . ?
Ti2 O8 C78 C79 -87.8(10) . . . . ?
Ti2 O8 C78 C83 92.4(9) . . . . ?
O8 C78 C79 C80 -177.6(8) . . . . ?
C83 C78 C79 C80 2.2(14) . . . . ?
O8 C78 C79 C77 2.7(15) . . . . ?
C83 C78 C79 C77 -177.5(9) . . . . ?
C72 C77 C79 C78 98.4(12) . . . . ?
C72 C77 C79 C80 -81.4(12) . . . . ?
C78 C79 C80 C81 -2.5(15) . . . . ?
C77 C79 C80 C81 177.2(9) . . . . ?
C79 C80 C81 C82 1.7(15) . . . . ?
C79 C80 C81 C84 177.3(9) . . . . ?
C80 C81 C82 C83 -0.7(15) . . . . ?
C84 C81 C82 C83 -176.1(9) . . . . ?
C81 C82 C83 C78 0.5(15) . . . . ?
C81 C82 C83 C88 -175.8(9) . . . . ?
O8 C78 C83 C82 178.5(8) . . . . ?
C79 C78 C83 C82 -1.3(14) . . . . ?
O8 C78 C83 C88 -5.3(14) . . . . ?
C79 C78 C83 C88 174.9(9) . . . . ?
C82 C81 C84 C86 -18(2) . . . . ?
C80 C81 C84 C86 166.9(18) . . . . ?
C82 C81 C84 C86X -46(2) . . . . ?
C80 C81 C84 C86X 139(2) . . . . ?
C82 C81 C84 C85 -139.0(17) . . . . ?
C80 C81 C84 C85 45.7(19) . . . . ?
C82 C81 C84 C87X 70(2) . . . . ?
C80 C81 C84 C87X -105(2) . . . . ?
C82 C81 C84 C85X -170(3) . . . . ?
C80 C81 C84 C85X 14(3) . . . . ?
C82 C81 C84 C87 102(2) . . . . ?
C80 C81 C84 C87 -74(2) . . . . ?
C47 C46 C88 C83 -102.8(11) . . . . ?
C45 C46 C88 C83 76.9(12) . . . . ?
C82 C83 C88 C46 77.8(12) . . . . ?
C78 C83 C88 C46 -98.4(11) . . . . ?
C1 O1 C102 C103 83.8(10) . . . . ?
Ti1 O1 C102 C103 -114.1(8) . . . . ?
O1 C102 C103 C104 177.5(8) . . . . ?
C102 C103 C104 C105 -174.9(9) . . . . ?
C103 C104 C105 C106 169.9(11) . . . . ?
C56 O6 C107 C108 86.5(10) . . . . ?
Ti2 O6 C107 C108 -106.4(8) . . . . ?
O6 C107 C108 C109 177.8(8) . . . . ?
C107 C108 C109 C110 -177.9(9) . . . . ?
C108 C109 C110 C111 176.1(11) . . . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O9 H9 N1 0.83(2) 2.00(6) 2.79(3) 159(12) .

_refine_diff_density_max         0.504
_refine_diff_density_min         -0.382
_refine_diff_density_rms         0.079


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: acetonitrile'
