# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2014

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#
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#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
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#  fide research purposes only. It may contain copyright material
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data_cd211563

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C48 H65 Cl3 N2 O2 Ti'
_chemical_formula_weight         856.27

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'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pca2(1)

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

_cell_length_a                   17.9918(16)
_cell_length_b                   12.0283(11)
_cell_length_c                   22.162(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     4796.0(7)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1246
_cell_measurement_theta_min      4.998
_cell_measurement_theta_max      28.269

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.341
_exptl_crystal_size_mid          0.215
_exptl_crystal_size_min          0.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1824
_exptl_absorpt_coefficient_mu    0.383
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.41848
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            27081
_diffrn_reflns_av_R_equivalents  0.1323
_diffrn_reflns_av_sigmaI/netI    0.1547
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         1.69
_diffrn_reflns_theta_max         25.50
_reflns_number_total             8516
_reflns_number_gt                3601
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0953P)²+0.0000P] 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 H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.04(6)
_chemical_absolute_configuration ad
_refine_ls_number_reflns         8516
_refine_ls_number_parameters     501
_refine_ls_number_restraints     159
_refine_ls_R_factor_all          0.1970
_refine_ls_R_factor_gt           0.0782
_refine_ls_wR_factor_ref         0.2198
_refine_ls_wR_factor_gt          0.1640
_refine_ls_goodness_of_fit_ref   0.960
_refine_ls_restrained_S_all      0.972
_refine_ls_shift/su_max          0.039
_refine_ls_shift/su_mean         0.004

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.18395(8) 0.65682(12) 0.77411(6) 0.0566(4) Uani 1 1 d . . .
Cl1 Cl 0.17956(14) 0.6135(2) 0.67121(10) 0.0799(7) Uani 1 1 d . . .
Cl2 Cl 0.15727(14) 0.8383(2) 0.75030(12) 0.0845(8) Uani 1 1 d . . .
Cl3 Cl 0.06965(13) 0.5827(2) 0.79199(11) 0.0830(7) Uani 1 1 d . . .
N1 N 0.3114(3) 0.6948(5) 0.7672(3) 0.0514(16) Uani 1 1 d . . .
N2 N 0.2356(4) 0.4836(5) 0.7871(3) 0.0627(18) Uani 1 1 d . . .
O1 O 0.2012(3) 0.6931(4) 0.8512(2) 0.0569(14) Uani 1 1 d . . .
O2 O 0.4313(3) 0.5532(6) 0.6649(3) 0.0767(17) Uani 1 1 d . . .
C1 C 0.2458(5) 0.7465(7) 0.8920(3) 0.054(2) Uani 1 1 d . . .
C2 C 0.2220(5) 0.7600(7) 0.9524(4) 0.059(2) Uani 1 1 d . . .
C3 C 0.2724(5) 0.8099(7) 0.9900(4) 0.064(2) Uani 1 1 d . . .
H3 H 0.2591 0.8182 1.0303 0.076 Uiso 1 1 calc R . .
C4 C 0.3414(5) 0.8487(7) 0.9726(3) 0.056(2) Uani 1 1 d . A .
C5 C 0.3598(5) 0.8394(7) 0.9130(4) 0.057(2) Uani 1 1 d . . .
H5 H 0.4050 0.8675 0.8995 0.068 Uiso 1 1 calc R . .
C6 C 0.3121(4) 0.7888(6) 0.8722(3) 0.0483(19) Uani 1 1 d . . .
C7 C 0.3323(4) 0.7927(7) 0.8051(3) 0.053(2) Uani 1 1 d . . .
H7A H 0.3090 0.8581 0.7877 0.063 Uiso 1 1 calc R . .
H7B H 0.3856 0.8029 0.8019 0.063 Uiso 1 1 calc R . .
C8 C 0.3505(5) 0.5947(6) 0.7896(4) 0.059(2) Uani 1 1 d . . .
H8A H 0.3495 0.5943 0.8334 0.071 Uiso 1 1 calc R . .
H8B H 0.4021 0.5972 0.7769 0.071 Uiso 1 1 calc R . .
C9 C 0.3152(5) 0.4895(6) 0.7664(4) 0.065(2) Uani 1 1 d . . .
H9A H 0.3170 0.4886 0.7226 0.078 Uiso 1 1 calc R . .
H9B H 0.3423 0.4255 0.7812 0.078 Uiso 1 1 calc R . .
C10 C 0.2002(5) 0.3917(7) 0.7516(5) 0.089(3) Uani 1 1 d . . .
H10A H 0.2292 0.3252 0.7557 0.133 Uiso 1 1 calc R . .
H10B H 0.1978 0.4126 0.7098 0.133 Uiso 1 1 calc R . .
H10C H 0.1509 0.3785 0.7665 0.133 Uiso 1 1 calc R . .
C11 C 0.2344(6) 0.4499(8) 0.8517(4) 0.087(3) Uani 1 1 d . . .
H11A H 0.2585 0.3792 0.8562 0.130 Uiso 1 1 calc R . .
H11B H 0.1838 0.4441 0.8652 0.130 Uiso 1 1 calc R . .
H11C H 0.2600 0.5046 0.8754 0.130 Uiso 1 1 calc R . .
C12 C 0.1418(5) 0.7280(9) 0.9735(4) 0.071(3) Uani 1 1 d . . .
C13 C 0.1282(6) 0.6018(9) 0.9648(5) 0.097(3) Uani 1 1 d . . .
H13A H 0.1624 0.5606 0.9893 0.145 Uiso 1 1 calc R . .
H13B H 0.1355 0.5827 0.9231 0.145 Uiso 1 1 calc R . .
H13C H 0.0782 0.5840 0.9764 0.145 Uiso 1 1 calc R . .
C14 C 0.1327(7) 0.7557(10) 1.0398(5) 0.118(4) Uani 1 1 d U . .
H14A H 0.1694 0.7163 1.0629 0.177 Uiso 1 1 calc R . .
H14B H 0.0839 0.7340 1.0530 0.177 Uiso 1 1 calc R . .
H14C H 0.1389 0.8342 1.0456 0.177 Uiso 1 1 calc R . .
C15 C 0.0864(6) 0.7919(10) 0.9368(5) 0.099(4) Uani 1 1 d . . .
H15A H 0.0370 0.7722 0.9492 0.149 Uiso 1 1 calc R . .
H15B H 0.0927 0.7743 0.8948 0.149 Uiso 1 1 calc R . .
H15C H 0.0939 0.8701 0.9428 0.149 Uiso 1 1 calc R . .
C16 C 0.3937(5) 0.9029(8) 1.0193(4) 0.077(3) Uani 1 1 d DU . .
C17 C 0.4487(19) 0.812(3) 1.0414(16) 0.151(13) Uani 0.50 1 d PDU A 1
H17A H 0.4858 0.7992 1.0111 0.226 Uiso 0.50 1 calc PR A 1
H17B H 0.4220 0.7442 1.0489 0.226 Uiso 0.50 1 calc PR A 1
H17C H 0.4723 0.8363 1.0780 0.226 Uiso 0.50 1 calc PR A 1
C18 C 0.3502(14) 0.955(2) 1.0720(11) 0.123(11) Uani 0.60 1 d PDU A 1
H18A H 0.3841 0.9753 1.1035 0.185 Uiso 0.60 1 calc PR A 1
H18B H 0.3149 0.9019 1.0872 0.185 Uiso 0.60 1 calc PR A 1
H18C H 0.3244 1.0199 1.0581 0.185 Uiso 0.60 1 calc PR A 1
C19 C 0.4361(16) 0.999(2) 0.9912(12) 0.116(11) Uani 0.50 1 d PDU A 1
H19A H 0.4677 1.0328 1.0210 0.174 Uiso 0.50 1 calc PR A 1
H19B H 0.4015 1.0538 0.9764 0.174 Uiso 0.50 1 calc PR A 1
H19C H 0.4659 0.9725 0.9583 0.174 Uiso 0.50 1 calc PR A 1
C17' C 0.4185(17) 0.816(2) 1.0643(12) 0.115(10) Uani 0.50 1 d PDU A 2
H17D H 0.4315 0.7487 1.0434 0.172 Uiso 0.50 1 calc PR A 2
H17E H 0.3789 0.8008 1.0922 0.172 Uiso 0.50 1 calc PR A 2
H17F H 0.4611 0.8427 1.0861 0.172 Uiso 0.50 1 calc PR A 2
C18' C 0.362(3) 1.017(2) 1.040(2) 0.151(14) Uani 0.40 1 d PDU A 2
H18D H 0.3961 1.0520 1.0669 0.227 Uiso 0.40 1 calc PR A 2
H18E H 0.3151 1.0062 1.0594 0.227 Uiso 0.40 1 calc PR A 2
H18F H 0.3550 1.0638 1.0048 0.227 Uiso 0.40 1 calc PR A 2
C19' C 0.4648(10) 0.9485(19) 0.9918(9) 0.078(7) Uani 0.50 1 d PDU A 2
H19D H 0.4936 0.8884 0.9756 0.117 Uiso 0.50 1 calc PR A 2
H19E H 0.4930 0.9861 1.0224 0.117 Uiso 0.50 1 calc PR A 2
H19F H 0.4527 0.9998 0.9602 0.117 Uiso 0.50 1 calc PR A 2
C20 C 0.3341(4) 0.7212(8) 0.7034(3) 0.055(2) Uani 1 1 d . . .
H20A H 0.3178 0.6604 0.6779 0.065 Uiso 1 1 calc R . .
H20B H 0.3072 0.7870 0.6908 0.065 Uiso 1 1 calc R . .
C21 C 0.4151(5) 0.7406(8) 0.6915(3) 0.059(2) Uani 1 1 d . . .
C22 C 0.4461(6) 0.8476(8) 0.6946(4) 0.073(3) Uani 1 1 d . . .
H22 H 0.4157 0.9060 0.7067 0.088 Uiso 1 1 calc R . .
C23 C 0.5187(7) 0.8704(11) 0.6809(5) 0.108(4) Uani 1 1 d . . .
H23 H 0.5383 0.9417 0.6841 0.130 Uiso 1 1 calc R . .
C24 C 0.5614(7) 0.7800(12) 0.6618(5) 0.097(3) Uani 1 1 d . . .
H24 H 0.6111 0.7922 0.6523 0.116 Uiso 1 1 calc R . .
C25 C 0.5350(6) 0.6788(10) 0.6565(4) 0.081(3) Uani 1 1 d . . .
H25 H 0.5657 0.6224 0.6423 0.097 Uiso 1 1 calc R . .
C26 C 0.4623(5) 0.6549(9) 0.6716(4) 0.067(3) Uani 1 1 d . . .
C27 C 0.4747(6) 0.4679(8) 0.6388(5) 0.099(4) Uani 1 1 d . . .
H27A H 0.4959 0.4939 0.6016 0.148 Uiso 1 1 calc R . .
H27B H 0.4439 0.4043 0.6310 0.148 Uiso 1 1 calc R . .
H27C H 0.5138 0.4475 0.6661 0.148 Uiso 1 1 calc R . .
C33 C 0.6540(8) 0.8837(13) 0.9098(8) 0.225(10) Uiso 1 1 d GD . .
C28 C 0.6183(9) 0.8929(12) 0.8544(7) 0.237(9) Uani 1 1 d GDU . .
H28 H 0.6281 0.9534 0.8295 0.284 Uiso 1 1 calc R . .
C29 C 0.5680(8) 0.8119(17) 0.8362(5) 0.235(8) Uani 1 1 d GU . .
H29 H 0.5442 0.8181 0.7992 0.282 Uiso 1 1 calc R . .
C30 C 0.5534(7) 0.7215(13) 0.8735(9) 0.243(8) Uani 1 1 d GU . .
H30 H 0.5197 0.6673 0.8613 0.291 Uiso 1 1 calc R . .
C31 C 0.5890(9) 0.7122(11) 0.9289(8) 0.259(8) Uani 1 1 d GU . .
H31 H 0.5792 0.6518 0.9538 0.311 Uiso 1 1 calc R . .
C32 C 0.6393(8) 0.7933(16) 0.9471(5) 0.257(9) Uani 1 1 d GDU . .
H32 H 0.6632 0.7871 0.9842 0.308 Uiso 1 1 calc R . .
C35 C 0.6685(6) 0.4851(8) 0.5147(5) 0.142(4) Uani 1 1 d GU . .
H35 H 0.6884 0.4241 0.5348 0.170 Uiso 1 1 calc R . .
C36 C 0.6143(6) 0.4698(7) 0.4708(5) 0.148(4) Uani 1 1 d GU . .
H36 H 0.5979 0.3985 0.4615 0.178 Uiso 1 1 calc R . .
C37 C 0.5847(5) 0.5611(10) 0.4407(4) 0.159(4) Uani 1 1 d GU . .
H37 H 0.5485 0.5508 0.4113 0.190 Uiso 1 1 calc R . .
C38 C 0.6093(6) 0.6676(8) 0.4546(5) 0.169(4) Uani 1 1 d GU . .
H38 H 0.5894 0.7286 0.4345 0.203 Uiso 1 1 calc R . .
C39 C 0.6634(7) 0.6829(7) 0.4986(5) 0.165(4) Uani 1 1 d GU . .
H39 H 0.6799 0.7542 0.5078 0.198 Uiso 1 1 calc R . .
C40 C 0.6931(5) 0.5917(10) 0.5286(4) 0.153(4) Uani 1 1 d GDU . .
C41 C 0.7586(10) 0.6103(14) 0.5718(8) 0.209(7) Uani 1 1 d DU . .
H41A H 0.8013 0.6340 0.5493 0.313 Uiso 1 1 calc R . .
H41B H 0.7698 0.5421 0.5924 0.313 Uiso 1 1 calc R . .
H41C H 0.7457 0.6664 0.6008 0.313 Uiso 1 1 calc R . .
C42 C 0.4284(7) 0.1699(8) 0.7144(10) 0.294(10) Uani 1 1 d GDU . .
H42 H 0.4766 0.1978 0.7125 0.353 Uiso 1 1 calc R . .
C43 C 0.3888(10) 0.1508(10) 0.6616(8) 0.296(10) Uani 1 1 d GU . .
H43 H 0.4104 0.1658 0.6243 0.355 Uiso 1 1 calc R . .
C44 C 0.3168(10) 0.1091(11) 0.6644(8) 0.294(9) Uani 1 1 d GU . .
H44 H 0.2903 0.0962 0.6291 0.352 Uiso 1 1 calc R . .
C45 C 0.2845(6) 0.0866(8) 0.7200(10) 0.287(9) Uani 1 1 d GU . .
H45 H 0.2364 0.0587 0.7219 0.344 Uiso 1 1 calc R . .
C46 C 0.3242(9) 0.1057(9) 0.7729(8) 0.280(9) Uani 1 1 d GDU . .
H46 H 0.3026 0.0907 0.8101 0.336 Uiso 1 1 calc R . .
C47 C 0.3961(9) 0.1474(11) 0.7700(8) 0.298(9) Uani 1 1 d GDU . .
C48 C 0.4493(13) 0.126(2) 0.8230(11) 0.363(12) Uani 1 1 d DU . .
H48A H 0.4212 0.1172 0.8595 0.545 Uiso 1 1 calc R . .
H48B H 0.4830 0.1870 0.8271 0.545 Uiso 1 1 calc R . .
H48C H 0.4770 0.0588 0.8154 0.545 Uiso 1 1 calc R . .
C34 C 0.726(2) 0.948(4) 0.923(2) 0.32(4) Uiso 1 1 d D . .
H34A H 0.7478 0.9196 0.9600 0.527 Uiso 1 1 calc R . .
H34B H 0.7151 1.0252 0.9282 0.527 Uiso 1 1 calc R . .
H34C H 0.7604 0.9379 0.8907 0.527 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.791(5) . ?
Ti1 Cl3 2.276(3) . ?
Ti1 Cl2 2.296(3) . ?
Ti1 N2 2.300(7) . ?
Ti1 Cl1 2.340(2) . ?
Ti1 N1 2.343(6) . ?
N1 C8 1.482(9) . ?
N1 C7 1.494(9) . ?
N1 C20 1.504(9) . ?
N2 C11 1.488(10) . ?
N2 C10 1.499(10) . ?
N2 C9 1.505(10) . ?
O1 C1 1.369(9) . ?
O2 C26 1.353(11) . ?
O2 C27 1.413(10) . ?
C1 C6 1.368(10) . ?
C1 C2 1.414(10) . ?
C2 C3 1.369(11) . ?
C2 C12 1.565(12) . ?
C3 C4 1.383(11) . ?
C3 H3 0.9300 . ?
C4 C5 1.367(10) . ?
C4 C16 1.542(11) . ?
C5 C6 1.387(11) . ?
C5 H5 0.9300 . ?
C6 C7 1.533(10) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.507(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 C15 1.499(13) . ?
C12 C14 1.516(12) . ?
C12 C13 1.549(14) . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 0.9600 . ?
C14 H14A 0.9604 . ?
C14 H14B 0.9604 . ?
C14 H14C 0.9604 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C16 C17' 1.515(16) . ?
C16 C19' 1.520(15) . ?
C16 C19 1.523(17) . ?
C16 C18 1.539(15) . ?
C16 C18' 1.555(19) . ?
C16 C17 1.555(18) . ?
C17 H17A 0.9614 . ?
C17 H17B 0.9614 . ?
C17 H17C 0.9614 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9601 . ?
C19 H19B 0.9601 . ?
C19 H19C 0.9601 . ?
C17' H17D 0.9600 . ?
C17' H17E 0.9600 . ?
C17' H17F 0.9600 . ?
C18' H18D 0.9601 . ?
C18' H18E 0.9601 . ?
C18' H18F 0.9601 . ?
C19' H19D 0.9601 . ?
C19' H19E 0.9601 . ?
C19' H19F 0.9601 . ?
C20 C21 1.500(11) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.404(11) . ?
C21 C26 1.407(11) . ?
C22 C23 1.369(13) . ?
C22 H22 0.9300 . ?
C23 C24 1.397(14) . ?
C23 H23 0.9300 . ?
C24 C25 1.312(13) . ?
C24 H24 0.9300 . ?
C25 C26 1.380(12) . ?
C25 H25 0.9300 . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C33 C28 1.3900 . ?
C33 C32 1.3900 . ?
C33 C34 1.539(14) . ?
C28 C29 1.3900 . ?
C28 H28 0.9300 . ?
C29 C30 1.3900 . ?
C29 H29 0.9300 . ?
C30 C31 1.3900 . ?
C30 H30 0.9300 . ?
C31 C32 1.3900 . ?
C31 H31 0.9300 . ?
C32 H32 0.9300 . ?
C35 C36 1.3900 . ?
C35 C40 1.3900 . ?
C35 H35 0.9300 . ?
C36 C37 1.3900 . ?
C36 H36 0.9300 . ?
C37 C38 1.3900 . ?
C37 H37 0.9300 . ?
C38 C39 1.3900 . ?
C38 H38 0.9300 . ?
C39 C40 1.3900 . ?
C39 H39 0.9300 . ?
C40 C41 1.536(15) . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 C43 1.3900 . ?
C42 C47 1.3900 . ?
C42 H42 0.9300 . ?
C43 C44 1.3900 . ?
C43 H43 0.9300 . ?
C44 C45 1.3900 . ?
C44 H44 0.9300 . ?
C45 C46 1.3900 . ?
C45 H45 0.9300 . ?
C46 C47 1.3900 . ?
C46 H46 0.9300 . ?
C47 C48 1.537(13) . ?
C48 H48A 0.9609 . ?
C48 H48B 0.9609 . ?
C48 H48C 0.9609 . ?
C34 H34A 0.9754 . ?
C34 H34B 0.9748 . ?
C34 H34C 0.9746 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 Cl3 94.94(18) . . ?
O1 Ti1 Cl2 91.36(19) . . ?
Cl3 Ti1 Cl2 102.90(11) . . ?
O1 Ti1 N2 91.8(2) . . ?
Cl3 Ti1 N2 89.34(19) . . ?
Cl2 Ti1 N2 167.05(19) . . ?
O1 Ti1 Cl1 171.81(19) . . ?
Cl3 Ti1 Cl1 92.98(10) . . ?
Cl2 Ti1 Cl1 88.88(10) . . ?
N2 Ti1 Cl1 86.23(18) . . ?
O1 Ti1 N1 81.1(2) . . ?
Cl3 Ti1 N1 166.41(17) . . ?
Cl2 Ti1 N1 90.23(17) . . ?
N2 Ti1 N1 77.9(2) . . ?
Cl1 Ti1 N1 90.71(16) . . ?
C8 N1 C7 109.4(6) . . ?
C8 N1 C20 111.0(6) . . ?
C7 N1 C20 107.1(6) . . ?
C8 N1 Ti1 106.5(4) . . ?
C7 N1 Ti1 111.3(4) . . ?
C20 N1 Ti1 111.6(4) . . ?
C11 N2 C10 107.4(7) . . ?
C11 N2 C9 108.7(7) . . ?
C10 N2 C9 106.2(7) . . ?
C11 N2 Ti1 111.2(5) . . ?
C10 N2 Ti1 115.5(5) . . ?
C9 N2 Ti1 107.6(4) . . ?
C1 O1 Ti1 147.8(5) . . ?
C26 O2 C27 118.3(7) . . ?
O1 C1 C6 118.2(7) . . ?
O1 C1 C2 120.0(7) . . ?
C6 C1 C2 121.7(8) . . ?
C3 C2 C1 115.1(8) . . ?
C3 C2 C12 122.4(7) . . ?
C1 C2 C12 122.3(8) . . ?
C2 C3 C4 125.0(8) . . ?
C2 C3 H3 117.5 . . ?
C4 C3 H3 117.5 . . ?
C5 C4 C3 117.3(8) . . ?
C5 C4 C16 122.4(8) . . ?
C3 C4 C16 120.2(7) . . ?
C4 C5 C6 121.0(8) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C1 C6 C5 119.6(7) . . ?
C1 C6 C7 122.0(7) . . ?
C5 C6 C7 118.1(7) . . ?
N1 C7 C6 117.5(6) . . ?
N1 C7 H7A 107.9 . . ?
C6 C7 H7A 107.9 . . ?
N1 C7 H7B 107.9 . . ?
C6 C7 H7B 107.9 . . ?
H7A C7 H7B 107.2 . . ?
N1 C8 C9 111.5(7) . . ?
N1 C8 H8A 109.3 . . ?
C9 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C9 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
N2 C9 C8 109.7(7) . . ?
N2 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
N2 C9 H9B 109.8 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 H10A 109.4 . . ?
N2 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
N2 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
N2 C11 H11A 109.4 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C15 C12 C14 110.0(9) . . ?
C15 C12 C13 109.2(9) . . ?
C14 C12 C13 108.6(8) . . ?
C15 C12 C2 108.9(8) . . ?
C14 C12 C2 109.6(8) . . ?
C13 C12 C2 110.5(8) . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.4 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.4 . . ?
H14B C14 H14C 109.4 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C17' C16 C19' 105.3(16) . . ?
C17' C16 C19 130.4(18) . . ?
C19' C16 C19 30.5(13) . . ?
C17' C16 C4 109.3(13) . . ?
C19' C16 C4 113.4(10) . . ?
C19 C16 C4 110.7(13) . . ?
C17' C16 C18 86.0(18) . . ?
C19' C16 C18 125.8(14) . . ?
C19 C16 C18 104.8(15) . . ?
C4 C16 C18 111.8(12) . . ?
C17' C16 C18' 122(2) . . ?
C19' C16 C18' 96(2) . . ?
C19 C16 C18' 68(2) . . ?
C4 C16 C18' 110(2) . . ?
C18 C16 C18' 40.1(18) . . ?
C17' C16 C17 28.0(17) . . ?
C19' C16 C17 81.0(18) . . ?
C19 C16 C17 110(2) . . ?
C4 C16 C17 107.6(15) . . ?
C18 C16 C17 112(2) . . ?
C18' C16 C17 140(3) . . ?
C16 C17 H17A 109.7 . . ?
C16 C17 H17B 109.3 . . ?
C16 C17 H17C 109.8 . . ?
C16 C18 H18A 109.6 . . ?
C16 C18 H18B 109.5 . . ?
C16 C18 H18C 109.3 . . ?
C16 C19 H19A 109.5 . . ?
C16 C19 H19B 109.3 . . ?
C16 C19 H19C 109.6 . . ?
C16 C17' H17D 109.5 . . ?
C16 C17' H17E 109.6 . . ?
H17D C17' H17E 109.5 . . ?
C16 C17' H17F 109.3 . . ?
H17D C17' H17F 109.5 . . ?
H17E C17' H17F 109.5 . . ?
C16 C18' H18D 109.5 . . ?
C16 C18' H18E 109.6 . . ?
H18D C18' H18E 109.5 . . ?
C16 C18' H18F 109.4 . . ?
H18D C18' H18F 109.5 . . ?
H18E C18' H18F 109.5 . . ?
C16 C19' H19D 109.6 . . ?
C16 C19' H19E 109.4 . . ?
H19D C19' H19E 109.5 . . ?
C16 C19' H19F 109.4 . . ?
H19D C19' H19F 109.5 . . ?
H19E C19' H19F 109.5 . . ?
C21 C20 N1 117.5(6) . . ?
C21 C20 H20A 107.9 . . ?
N1 C20 H20A 107.9 . . ?
C21 C20 H20B 107.9 . . ?
N1 C20 H20B 107.9 . . ?
H20A C20 H20B 107.2 . . ?
C22 C21 C26 116.6(9) . . ?
C22 C21 C20 121.3(8) . . ?
C26 C21 C20 121.9(8) . . ?
C23 C22 C21 123.5(10) . . ?
C23 C22 H22 118.3 . . ?
C21 C22 H22 118.2 . . ?
C22 C23 C24 115.8(11) . . ?
C22 C23 H23 122.1 . . ?
C24 C23 H23 122.1 . . ?
C25 C24 C23 123.4(11) . . ?
C25 C24 H24 118.3 . . ?
C23 C24 H24 118.3 . . ?
C24 C25 C26 121.0(11) . . ?
C24 C25 H25 119.5 . . ?
C26 C25 H25 119.5 . . ?
O2 C26 C25 123.6(9) . . ?
O2 C26 C21 116.6(8) . . ?
C25 C26 C21 119.7(10) . . ?
O2 C27 H27A 109.4 . . ?
O2 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
O2 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C28 C33 C32 120.0 . . ?
C28 C33 C34 121.5(11) . . ?
C32 C33 C34 115.7(11) . . ?
C33 C28 C29 120.0 . . ?
C33 C28 H28 120.0 . . ?
C29 C28 H28 120.0 . . ?
C30 C29 C28 120.0 . . ?
C30 C29 H29 120.0 . . ?
C28 C29 H29 120.0 . . ?
C29 C30 C31 120.0 . . ?
C29 C30 H30 120.0 . . ?
C31 C30 H30 120.0 . . ?
C32 C31 C30 120.0 . . ?
C32 C31 H31 120.0 . . ?
C30 C31 H31 120.0 . . ?
C31 C32 C33 120.0 . . ?
C31 C32 H32 120.0 . . ?
C33 C32 H32 120.0 . . ?
C36 C35 C40 120.0 . . ?
C36 C35 H35 120.0 . . ?
C40 C35 H35 120.0 . . ?
C37 C36 C35 120.0 . . ?
C37 C36 H36 120.0 . . ?
C35 C36 H36 120.0 . . ?
C36 C37 C38 120.0 . . ?
C36 C37 H37 120.0 . . ?
C38 C37 H37 120.0 . . ?
C37 C38 C39 120.0 . . ?
C37 C38 H38 120.0 . . ?
C39 C38 H38 120.0 . . ?
C38 C39 C40 120.0 . . ?
C38 C39 H39 120.0 . . ?
C40 C39 H39 120.0 . . ?
C39 C40 C35 120.0 . . ?
C39 C40 C41 118.6(11) . . ?
C35 C40 C41 121.1(11) . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.4 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C43 C42 C47 120.0 . . ?
C43 C42 H42 120.1 . . ?
C47 C42 H42 119.9 . . ?
C44 C43 C42 120.0 . . ?
C44 C43 H43 120.0 . . ?
C42 C43 H43 120.0 . . ?
C43 C44 C45 120.0 . . ?
C43 C44 H44 120.0 . . ?
C45 C44 H44 120.0 . . ?
C46 C45 C44 120.0 . . ?
C46 C45 H45 120.0 . . ?
C44 C45 H45 120.0 . . ?
C45 C46 C47 120.0 . . ?
C45 C46 H46 120.0 . . ?
C47 C46 H46 120.0 . . ?
C46 C47 C42 120.0 . . ?
C46 C47 C48 118.9(10) . . ?
C42 C47 C48 116.8(11) . . ?
C47 C48 H48A 109.4 . . ?
C47 C48 H48B 109.5 . . ?
H48A C48 H48B 109.4 . . ?
C47 C48 H48C 109.7 . . ?
H48A C48 H48C 109.4 . . ?
H48B C48 H48C 109.4 . . ?
C33 C34 H34A 111.3 . . ?
C33 C34 H34B 110.8 . . ?
H34A C34 H34B 108.0 . . ?
C33 C34 H34C 110.7 . . ?
H34A C34 H34C 107.9 . . ?
H34B C34 H34C 108.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ti1 N1 C8 80.2(4) . . . . ?
Cl3 Ti1 N1 C8 6.3(10) . . . . ?
Cl2 Ti1 N1 C8 171.5(4) . . . . ?
N2 Ti1 N1 C8 -13.6(4) . . . . ?
Cl1 Ti1 N1 C8 -99.6(4) . . . . ?
O1 Ti1 N1 C7 -38.9(5) . . . . ?
Cl3 Ti1 N1 C7 -112.9(8) . . . . ?
Cl2 Ti1 N1 C7 52.4(5) . . . . ?
N2 Ti1 N1 C7 -132.7(5) . . . . ?
Cl1 Ti1 N1 C7 141.3(5) . . . . ?
O1 Ti1 N1 C20 -158.5(5) . . . . ?
Cl3 Ti1 N1 C20 127.6(7) . . . . ?
Cl2 Ti1 N1 C20 -67.2(5) . . . . ?
N2 Ti1 N1 C20 107.7(5) . . . . ?
Cl1 Ti1 N1 C20 21.7(5) . . . . ?
O1 Ti1 N2 C11 22.6(6) . . . . ?
Cl3 Ti1 N2 C11 -72.3(5) . . . . ?
Cl2 Ti1 N2 C11 126.6(8) . . . . ?
Cl1 Ti1 N2 C11 -165.3(5) . . . . ?
N1 Ti1 N2 C11 103.1(6) . . . . ?
O1 Ti1 N2 C10 145.3(6) . . . . ?
Cl3 Ti1 N2 C10 50.3(6) . . . . ?
Cl2 Ti1 N2 C10 -110.8(9) . . . . ?
Cl1 Ti1 N2 C10 -42.7(6) . . . . ?
N1 Ti1 N2 C10 -134.2(6) . . . . ?
O1 Ti1 N2 C9 -96.4(5) . . . . ?
Cl3 Ti1 N2 C9 168.7(5) . . . . ?
Cl2 Ti1 N2 C9 7.6(12) . . . . ?
Cl1 Ti1 N2 C9 75.7(5) . . . . ?
N1 Ti1 N2 C9 -15.9(5) . . . . ?
Cl3 Ti1 O1 C1 -172.0(9) . . . . ?
Cl2 Ti1 O1 C1 -68.9(9) . . . . ?
N2 Ti1 O1 C1 98.5(10) . . . . ?
Cl1 Ti1 O1 C1 23(2) . . . . ?
N1 Ti1 O1 C1 21.1(9) . . . . ?
Ti1 O1 C1 C6 -7.9(14) . . . . ?
Ti1 O1 C1 C2 170.0(7) . . . . ?
O1 C1 C2 C3 177.0(7) . . . . ?
C6 C1 C2 C3 -5.1(12) . . . . ?
O1 C1 C2 C12 -7.0(12) . . . . ?
C6 C1 C2 C12 170.8(8) . . . . ?
C1 C2 C3 C4 1.8(13) . . . . ?
C12 C2 C3 C4 -174.1(9) . . . . ?
C2 C3 C4 C5 2.0(13) . . . . ?
C2 C3 C4 C16 -179.6(8) . . . . ?
C3 C4 C5 C6 -2.6(12) . . . . ?
C16 C4 C5 C6 179.1(8) . . . . ?
O1 C1 C6 C5 -177.5(7) . . . . ?
C2 C1 C6 C5 4.7(12) . . . . ?
O1 C1 C6 C7 8.9(11) . . . . ?
C2 C1 C6 C7 -169.0(8) . . . . ?
C4 C5 C6 C1 -0.6(12) . . . . ?
C4 C5 C6 C7 173.3(7) . . . . ?
C8 N1 C7 C6 -62.0(8) . . . . ?
C20 N1 C7 C6 177.6(6) . . . . ?
Ti1 N1 C7 C6 55.4(8) . . . . ?
C1 C6 C7 N1 -40.1(11) . . . . ?
C5 C6 C7 N1 146.2(7) . . . . ?
C7 N1 C8 C9 162.8(7) . . . . ?
C20 N1 C8 C9 -79.3(8) . . . . ?
Ti1 N1 C8 C9 42.4(7) . . . . ?
C11 N2 C9 C8 -76.9(8) . . . . ?
C10 N2 C9 C8 167.9(7) . . . . ?
Ti1 N2 C9 C8 43.7(8) . . . . ?
N1 C8 C9 N2 -60.3(9) . . . . ?
C3 C2 C12 C15 117.8(9) . . . . ?
C1 C2 C12 C15 -57.8(12) . . . . ?
C3 C2 C12 C14 -2.6(13) . . . . ?
C1 C2 C12 C14 -178.2(9) . . . . ?
C3 C2 C12 C13 -122.2(9) . . . . ?
C1 C2 C12 C13 62.1(11) . . . . ?
C5 C4 C16 C17' -114.6(16) . . . . ?
C3 C4 C16 C17' 67.1(17) . . . . ?
C5 C4 C16 C19' 2.5(16) . . . . ?
C3 C4 C16 C19' -175.8(13) . . . . ?
C5 C4 C16 C19 35.4(17) . . . . ?
C3 C4 C16 C19 -142.9(15) . . . . ?
C5 C4 C16 C18 151.9(14) . . . . ?
C3 C4 C16 C18 -26.4(16) . . . . ?
C5 C4 C16 C18' 109(2) . . . . ?
C3 C4 C16 C18' -69(2) . . . . ?
C5 C4 C16 C17 -85.1(18) . . . . ?
C3 C4 C16 C17 96.6(18) . . . . ?
C8 N1 C20 C21 -57.8(9) . . . . ?
C7 N1 C20 C21 61.6(9) . . . . ?
Ti1 N1 C20 C21 -176.4(6) . . . . ?
N1 C20 C21 C22 -91.1(10) . . . . ?
N1 C20 C21 C26 94.6(9) . . . . ?
C26 C21 C22 C23 -1.6(13) . . . . ?
C20 C21 C22 C23 -176.2(9) . . . . ?
C21 C22 C23 C24 1.4(15) . . . . ?
C22 C23 C24 C25 0.5(17) . . . . ?
C23 C24 C25 C26 -2.0(17) . . . . ?
C27 O2 C26 C25 -2.4(13) . . . . ?
C27 O2 C26 C21 173.3(7) . . . . ?
C24 C25 C26 O2 177.3(9) . . . . ?
C24 C25 C26 C21 1.7(14) . . . . ?
C22 C21 C26 O2 -175.8(7) . . . . ?
C20 C21 C26 O2 -1.3(11) . . . . ?
C22 C21 C26 C25 0.1(11) . . . . ?
C20 C21 C26 C25 174.6(8) . . . . ?
C32 C33 C28 C29 0.0 . . . . ?
C34 C33 C28 C29 160(3) . . . . ?
C33 C28 C29 C30 0.0 . . . . ?
C28 C29 C30 C31 0.0 . . . . ?
C29 C30 C31 C32 0.0 . . . . ?
C30 C31 C32 C33 0.0 . . . . ?
C28 C33 C32 C31 0.0 . . . . ?
C34 C33 C32 C31 -161(3) . . . . ?
C40 C35 C36 C37 0.0 . . . . ?
C35 C36 C37 C38 0.0 . . . . ?
C36 C37 C38 C39 0.0 . . . . ?
C37 C38 C39 C40 0.0 . . . . ?
C38 C39 C40 C35 0.0 . . . . ?
C38 C39 C40 C41 173.5(12) . . . . ?
C36 C35 C40 C39 0.0 . . . . ?
C36 C35 C40 C41 -173.3(12) . . . . ?
C47 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C45 0.0 . . . . ?
C43 C44 C45 C46 0.0 . . . . ?
C44 C45 C46 C47 0.0 . . . . ?
C45 C46 C47 C42 0.0 . . . . ?
C45 C46 C47 C48 -156.0(16) . . . . ?
C43 C42 C47 C46 0.0 . . . . ?
C43 C42 C47 C48 156.5(16) . . . . ?

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.057
_database_code_depnum_ccdc_archive 'CCDC 968903'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
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# 
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#  data retrieval see:
#                         www.ccdc.cam.ac.uk
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#
data_a01015a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C29 H43 Cl3 N2 O2 Ti'
_chemical_formula_weight         605.90

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

loop_
_symmetry_equiv_pos_as_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                   31.567(14)
_cell_length_b                   12.607(5)
_cell_length_c                   24.650(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 127.231(8)
_cell_angle_gamma                90.00
_cell_volume                     7810(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    942
_cell_measurement_theta_min      2.922
_cell_measurement_theta_max      24.232

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.031
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2560
_exptl_absorpt_coefficient_mu    0.446
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8244
_exptl_absorpt_correction_T_max  0.9361
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            8551
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0889
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         1.62
_diffrn_reflns_theta_max         27.50
_reflns_number_total             8551
_reflns_number_gt                4143
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1495P)²+0.0000P] 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_number_reflns         8551
_refine_ls_number_parameters     334
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1486
_refine_ls_R_factor_gt           0.0840
_refine_ls_wR_factor_ref         0.2684
_refine_ls_wR_factor_gt          0.2359
_refine_ls_goodness_of_fit_ref   0.996
_refine_ls_restrained_S_all      1.003
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.14670(3) 0.92362(7) 0.62956(4) 0.0405(3) Uani 1 1 d . . .
C1 C 0.2756(5) 0.9083(8) 1.0746(5) 0.136(4) Uani 1 1 d . . .
H1A H 0.3138 0.9096 1.1055 0.205 Uiso 1 1 calc R . .
H1B H 0.2637 0.8368 1.0596 0.205 Uiso 1 1 calc R . .
H1C H 0.2615 0.9342 1.0974 0.205 Uiso 1 1 calc R . .
C2 C 0.2720(5) 1.0913(8) 1.0320(6) 0.141(4) Uani 1 1 d U . .
H2A H 0.2582 1.1330 0.9919 0.211 Uiso 1 1 calc R . .
H2B H 0.3101 1.0962 1.0620 0.211 Uiso 1 1 calc R . .
H2C H 0.2580 1.1175 1.0549 0.211 Uiso 1 1 calc R . .
C3 C 0.1960(5) 0.9685(11) 0.9723(6) 0.160(5) Uani 1 1 d . . .
H3A H 0.1785 1.0099 0.9314 0.241 Uiso 1 1 calc R . .
H3B H 0.1857 0.9933 0.9995 0.241 Uiso 1 1 calc R . .
H3C H 0.1861 0.8953 0.9607 0.241 Uiso 1 1 calc R . .
C4 C 0.2560(3) 0.9795(6) 1.0124(3) 0.0738(19) Uani 1 1 d . . .
C5 C 0.2738(2) 0.9356(5) 0.9716(3) 0.0541(14) Uani 1 1 d . . .
C6 C 0.2493(2) 0.9620(4) 0.9032(2) 0.0434(12) Uani 1 1 d . . .
C7 C 0.26264(19) 0.9114(4) 0.8658(2) 0.0399(11) Uani 1 1 d . . .
C8 C 0.3055(2) 0.8409(4) 0.8988(2) 0.0428(12) Uani 1 1 d . . .
H8A H 0.3155 0.8084 0.8742 0.051 Uiso 1 1 calc R . .
C9 C 0.3332(2) 0.8187(4) 0.9666(3) 0.0521(14) Uani 1 1 d . . .
C10 C 0.3158(2) 0.8650(5) 1.0008(3) 0.0575(15) Uani 1 1 d . . .
H10A H 0.3335 0.8476 1.0464 0.069 Uiso 1 1 calc R . .
C11 C 0.2269(3) 1.1415(5) 0.8663(3) 0.0745(19) Uani 1 1 d . . .
H11A H 0.1975 1.1901 0.8436 0.112 Uiso 1 1 calc R . .
H11B H 0.2409 1.1356 0.8410 0.112 Uiso 1 1 calc R . .
H11C H 0.2542 1.1671 0.9114 0.112 Uiso 1 1 calc R . .
C12 C 0.3802(2) 0.7441(5) 1.0023(3) 0.0705(18) Uani 1 1 d . . .
H12A H 0.3864 0.7201 0.9707 0.106 Uiso 1 1 calc R . .
H12B H 0.3729 0.6843 1.0196 0.106 Uiso 1 1 calc R . .
H12C H 0.4112 0.7805 1.0394 0.106 Uiso 1 1 calc R . .
C13 C 0.23301(18) 0.9358(4) 0.7909(2) 0.0393(11) Uani 1 1 d . . .
H13A H 0.2431 0.9920 0.7765 0.047 Uiso 1 1 calc R . .
C14 C 0.1447(2) 0.8682(4) 0.7513(3) 0.0450(12) Uani 1 1 d . . .
H14A H 0.1230 0.8048 0.7323 0.054 Uiso 1 1 calc R . .
H14B H 0.1618 0.8695 0.7998 0.054 Uiso 1 1 calc R . .
C15 C 0.1103(2) 0.9634(5) 0.7186(3) 0.0516(14) Uani 1 1 d . . .
H15A H 0.0840 0.9642 0.7272 0.062 Uiso 1 1 calc R . .
H15B H 0.1318 1.0269 0.7387 0.062 Uiso 1 1 calc R . .
C16 C 0.0564(3) 1.0690(5) 0.6175(4) 0.078(2) Uani 1 1 d . . .
H16A H 0.0307 1.0784 0.6260 0.117 Uiso 1 1 calc R . .
H16B H 0.0388 1.0719 0.5693 0.117 Uiso 1 1 calc R . .
H16C H 0.0825 1.1243 0.6397 0.117 Uiso 1 1 calc R . .
C17 C 0.0400(2) 0.8823(5) 0.6110(3) 0.0671(18) Uani 1 1 d . . .
H17A H 0.0138 0.9000 0.6176 0.101 Uiso 1 1 calc R . .
H17B H 0.0549 0.8140 0.6307 0.101 Uiso 1 1 calc R . .
H17C H 0.0235 0.8803 0.5631 0.101 Uiso 1 1 calc R . .
C18 C 0.20557(19) 0.7533(4) 0.7500(2) 0.0406(11) Uani 1 1 d . . .
H18A H 0.2409 0.7360 0.7845 0.049 Uiso 1 1 calc R . .
C19 C 0.16606(18) 0.6699(4) 0.7023(2) 0.0361(11) Uani 1 1 d . . .
C20 C 0.13110(18) 0.6872(4) 0.6323(2) 0.0378(11) Uani 1 1 d . . .
C21 C 0.10240(18) 0.6052(4) 0.5855(2) 0.0411(12) Uani 1 1 d . . .
C22 C 0.10502(19) 0.5066(4) 0.6128(3) 0.0501(13) Uani 1 1 d . . .
H22A H 0.0856 0.4506 0.5832 0.060 Uiso 1 1 calc R . .
C23 C 0.1356(2) 0.4887(4) 0.6825(3) 0.0485(13) Uani 1 1 d . . .
C24 C 0.16694(19) 0.5703(4) 0.7263(3) 0.0433(12) Uani 1 1 d . . .
H24A H 0.1892 0.5578 0.7730 0.052 Uiso 1 1 calc R . .
C25 C 0.1350(3) 0.3798(5) 0.7094(4) 0.0724(19) Uani 1 1 d . . .
H25A H 0.1583 0.3806 0.7583 0.109 Uiso 1 1 calc R . .
H25B H 0.1469 0.3270 0.6933 0.109 Uiso 1 1 calc R . .
H25C H 0.0995 0.3633 0.6935 0.109 Uiso 1 1 calc R . .
C26 C 0.0715(2) 0.6223(5) 0.5082(3) 0.0546(14) Uani 1 1 d . . .
C27 C 0.0267(2) 0.7025(5) 0.4808(3) 0.0674(18) Uani 1 1 d . . .
H27A H 0.0025 0.6774 0.4893 0.101 Uiso 1 1 calc R . .
H27B H 0.0080 0.7112 0.4327 0.101 Uiso 1 1 calc R . .
H27C H 0.0413 0.7694 0.5033 0.101 Uiso 1 1 calc R . .
C28 C 0.1102(3) 0.6605(6) 0.4947(3) 0.076(2) Uani 1 1 d . . .
H28A H 0.1265 0.7256 0.5188 0.114 Uiso 1 1 calc R . .
H28B H 0.0913 0.6722 0.4467 0.114 Uiso 1 1 calc R . .
H28C H 0.1372 0.6078 0.5100 0.114 Uiso 1 1 calc R . .
C29 C 0.0474(3) 0.5184(5) 0.4684(3) 0.0723(19) Uani 1 1 d . . .
H29A H 0.0224 0.4916 0.4750 0.108 Uiso 1 1 calc R . .
H29B H 0.0752 0.4673 0.4846 0.108 Uiso 1 1 calc R . .
H29C H 0.0296 0.5314 0.4208 0.108 Uiso 1 1 calc R . .
Cl1 Cl 0.17760(6) 1.09701(11) 0.66860(7) 0.0597(4) Uani 1 1 d . . .
Cl2 Cl 0.09028(6) 0.97575(12) 0.51894(7) 0.0653(5) Uani 1 1 d . . .
Cl3 Cl 0.22316(5) 0.88544(13) 0.64286(7) 0.0572(4) Uani 1 1 d . . .
N1 N 0.08295(16) 0.9638(4) 0.6445(2) 0.0516(11) Uani 1 1 d . . .
N2 N 0.18610(15) 0.8651(3) 0.74007(19) 0.0356(9) Uani 1 1 d . . .
O2 O 0.12587(12) 0.7885(3) 0.61044(15) 0.0412(8) Uani 1 1 d . . .
O3 O 0.20898(15) 1.0383(3) 0.87074(19) 0.0544(10) Uani 1 1 d . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.783(3) . ?
Ti1 Cl2 2.2721(18) . ?
Ti1 Cl3 2.282(2) . ?
Ti1 N1 2.310(4) . ?
Ti1 N2 2.326(4) . ?
Ti1 Cl1 2.3493(19) . ?
C1 C4 1.547(10) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C4 1.477(11) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 C4 1.522(13) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 C5 1.523(8) . ?
C5 C10 1.383(8) . ?
C5 C6 1.404(7) . ?
C6 C7 1.381(7) . ?
C6 O3 1.397(6) . ?
C7 C8 1.397(7) . ?
C7 C13 1.511(6) . ?
C8 C9 1.366(7) . ?
C8 H8A 0.9300 . ?
C9 C10 1.381(8) . ?
C9 C12 1.511(8) . ?
C10 H10A 0.9300 . ?
C11 O3 1.448(7) . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 N2 1.521(6) . ?
C13 H13A 0.9300 . ?
C14 C15 1.487(7) . ?
C14 N2 1.491(6) . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C15 N1 1.476(7) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 N1 1.493(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C17 N1 1.491(7) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 N2 1.497(6) . ?
C18 C19 1.507(6) . ?
C18 H18A 0.9300 . ?
C19 C24 1.381(7) . ?
C19 C20 1.393(6) . ?
C20 O2 1.357(6) . ?
C20 C21 1.398(7) . ?
C21 C22 1.392(7) . ?
C21 C26 1.543(7) . ?
C22 C23 1.389(7) . ?
C22 H22A 0.9300 . ?
C23 C24 1.382(7) . ?
C23 C25 1.530(7) . ?
C24 H24A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C26 C27 1.524(8) . ?
C26 C28 1.526(9) . ?
C26 C29 1.534(8) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 H28A 0.9600 . ?
C28 H28B 0.9600 . ?
C28 H28C 0.9600 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 Cl2 93.61(11) . . ?
O2 Ti1 Cl3 91.45(12) . . ?
Cl2 Ti1 Cl3 103.08(7) . . ?
O2 Ti1 N1 91.95(16) . . ?
Cl2 Ti1 N1 90.10(13) . . ?
Cl3 Ti1 N1 166.15(12) . . ?
O2 Ti1 N2 81.77(14) . . ?
Cl2 Ti1 N2 166.54(11) . . ?
Cl3 Ti1 N2 89.72(10) . . ?
N1 Ti1 N2 77.49(15) . . ?
O2 Ti1 Cl1 172.81(11) . . ?
Cl2 Ti1 Cl1 92.99(6) . . ?
Cl3 Ti1 Cl1 89.80(7) . . ?
N1 Ti1 Cl1 85.22(13) . . ?
N2 Ti1 Cl1 91.16(11) . . ?
C4 C1 H1A 109.5 . . ?
C4 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
C4 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C4 C2 H2A 109.5 . . ?
C4 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C4 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C4 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C2 C4 C3 110.1(8) . . ?
C2 C4 C5 111.9(6) . . ?
C3 C4 C5 110.5(6) . . ?
C2 C4 C1 112.1(8) . . ?
C3 C4 C1 100.7(7) . . ?
C5 C4 C1 111.0(6) . . ?
C10 C5 C6 115.8(5) . . ?
C10 C5 C4 120.7(5) . . ?
C6 C5 C4 123.4(6) . . ?
C7 C6 O3 118.4(4) . . ?
C7 C6 C5 121.5(5) . . ?
O3 C6 C5 120.0(5) . . ?
C6 C7 C8 118.9(4) . . ?
C6 C7 C13 120.5(5) . . ?
C8 C7 C13 120.5(4) . . ?
C9 C8 C7 121.3(5) . . ?
C9 C8 H8A 119.3 . . ?
C7 C8 H8A 119.3 . . ?
C8 C9 C10 117.6(5) . . ?
C8 C9 C12 121.0(5) . . ?
C10 C9 C12 121.3(5) . . ?
C9 C10 C5 124.3(5) . . ?
C9 C10 H10A 117.8 . . ?
C5 C10 H10A 117.8 . . ?
O3 C11 H11A 109.5 . . ?
O3 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
O3 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C7 C13 N2 117.5(4) . . ?
C7 C13 H13A 121.3 . . ?
N2 C13 H13A 121.3 . . ?
C15 C14 N2 111.0(4) . . ?
C15 C14 H14A 109.4 . . ?
N2 C14 H14A 109.4 . . ?
C15 C14 H14B 109.4 . . ?
N2 C14 H14B 109.4 . . ?
H14A C14 H14B 108.0 . . ?
N1 C15 C14 111.1(4) . . ?
N1 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
N1 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N1 C16 H16A 109.5 . . ?
N1 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
N1 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
N1 C17 H17A 109.5 . . ?
N1 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N1 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 C19 117.7(4) . . ?
N2 C18 H18A 121.1 . . ?
C19 C18 H18A 121.1 . . ?
C24 C19 C20 118.0(4) . . ?
C24 C19 C18 120.5(4) . . ?
C20 C19 C18 121.2(4) . . ?
O2 C20 C19 117.1(4) . . ?
O2 C20 C21 120.4(4) . . ?
C19 C20 C21 122.5(5) . . ?
C22 C21 C20 116.3(5) . . ?
C22 C21 C26 122.0(5) . . ?
C20 C21 C26 121.7(5) . . ?
C23 C22 C21 122.5(5) . . ?
C23 C22 H22A 118.8 . . ?
C21 C22 H22A 118.8 . . ?
C24 C23 C22 118.6(5) . . ?
C24 C23 C25 121.3(5) . . ?
C22 C23 C25 120.0(5) . . ?
C19 C24 C23 121.5(5) . . ?
C19 C24 H24A 119.2 . . ?
C23 C24 H24A 119.2 . . ?
C23 C25 H25A 109.5 . . ?
C23 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C23 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C27 C26 C28 110.2(5) . . ?
C27 C26 C29 108.4(5) . . ?
C28 C26 C29 106.4(5) . . ?
C27 C26 C21 111.3(5) . . ?
C28 C26 C21 108.8(5) . . ?
C29 C26 C21 111.6(5) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C15 N1 C17 109.7(5) . . ?
C15 N1 C16 107.7(5) . . ?
C17 N1 C16 106.7(4) . . ?
C15 N1 Ti1 106.5(3) . . ?
C17 N1 Ti1 110.4(4) . . ?
C16 N1 Ti1 115.6(4) . . ?
C14 N2 C18 108.3(4) . . ?
C14 N2 C13 110.9(4) . . ?
C18 N2 C13 108.6(3) . . ?
C14 N2 Ti1 107.5(3) . . ?
C18 N2 Ti1 111.5(3) . . ?
C13 N2 Ti1 110.1(3) . . ?
C20 O2 Ti1 149.0(3) . . ?
C6 O3 C11 113.5(4) . . ?

_diffrn_measured_fraction_theta_max 0.954
_diffrn_reflns_theta_full        27.50
_diffrn_measured_fraction_theta_full 0.954
_refine_diff_density_max         1.547
_refine_diff_density_min         -0.632
_refine_diff_density_rms         0.201

_database_code_depnum_ccdc_archive 'CCDC 968904'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_cd211547

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C66 H78 Br4 Cl4 N4 O5 Ti2'
_chemical_formula_weight         1564.56

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   12.5385(17)
_cell_length_b                   16.754(2)
_cell_length_c                   18.355(2)
_cell_angle_alpha                99.214(3)
_cell_angle_beta                 93.923(3)
_cell_angle_gamma                103.434(3)
_cell_volume                     3679.6(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    1793
_cell_measurement_theta_min      5.176
_cell_measurement_theta_max      41.118

_exptl_crystal_description       prismatic
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.311
_exptl_crystal_size_mid          0.145
_exptl_crystal_size_min          0.056
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1588
_exptl_absorpt_coefficient_mu    2.581
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.0832
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21588
_diffrn_reflns_av_R_equivalents  0.0601
_diffrn_reflns_av_sigmaI/netI    0.1394
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.68
_diffrn_reflns_theta_max         25.50
_reflns_number_total             13665
_reflns_number_gt                6314
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1236P)²+0.0000P] 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_number_reflns         13665
_refine_ls_number_parameters     578
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1737
_refine_ls_R_factor_gt           0.0802
_refine_ls_wR_factor_ref         0.2592
_refine_ls_wR_factor_gt          0.2050
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_restrained_S_all      0.996
_refine_ls_shift/su_max          0.020
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.96687(10) 0.33494(9) 0.31361(8) 0.0380(4) Uani 1 1 d . . .
Ti2 Ti 0.86077(10) 0.34580(8) 0.12730(8) 0.0354(4) Uani 1 1 d . . .
Br1 Br 1.01539(10) 0.06233(8) 0.27021(7) 0.0882(4) Uani 1 1 d . . .
Br2 Br 0.55625(15) -0.08682(9) 0.22629(13) 0.1617(9) Uani 1 1 d . . .
Br3 Br 0.56195(8) 0.10932(7) 0.08014(7) 0.0756(4) Uani 1 1 d . . .
Br4 Br 0.83565(11) -0.11692(6) 0.05136(8) 0.0978(5) Uani 1 1 d . . .
Cl1 Cl 1.15130(16) 0.34384(15) 0.30310(12) 0.0566(6) Uani 1 1 d . . .
Cl2 Cl 0.99701(17) 0.47897(13) 0.35458(13) 0.0526(6) Uani 1 1 d . . .
Cl3 Cl 0.70188(16) 0.38839(14) 0.14696(12) 0.0516(6) Uani 1 1 d . . .
Cl4 Cl 0.96731(16) 0.48088(12) 0.13150(13) 0.0496(6) Uani 1 1 d . . .
N1 N 0.7921(5) 0.3104(4) 0.3506(3) 0.0382(16) Uani 1 1 d . . .
N2 N 1.0029(5) 0.3270(4) 0.4397(4) 0.0489(18) Uani 1 1 d . . .
N3 N 1.0005(5) 0.2895(4) 0.0778(3) 0.0351(15) Uani 1 1 d . . .
N4 N 0.8240(5) 0.3433(4) -0.0007(4) 0.0460(17) Uani 1 1 d . . .
O1 O 0.9155(4) 0.3427(3) 0.2198(3) 0.0402(13) Uani 1 1 d . . .
O2 O 0.9314(4) 0.2190(3) 0.2958(3) 0.0490(15) Uani 1 1 d . . .
O3 O 0.7844(4) 0.2342(3) 0.1065(3) 0.0417(13) Uani 1 1 d . . .
O4 O 0.7030(5) 0.4218(4) 0.5044(3) 0.0672(19) Uani 1 1 d . . .
O5 O 1.1995(5) 0.3755(4) -0.0348(4) 0.0649(18) Uani 1 1 d . . .
C1 C 0.8495(7) 0.1524(5) 0.2813(5) 0.049(2) Uani 1 1 d . . .
C2 C 0.8676(8) 0.0723(6) 0.2674(6) 0.066(3) Uani 1 1 d . . .
C3 C 0.7812(10) 0.0003(6) 0.2502(6) 0.083(3) Uani 1 1 d . . .
H3 H 0.7951 -0.0523 0.2395 0.099 Uiso 1 1 calc R . .
C4 C 0.6738(10) 0.0096(6) 0.2497(6) 0.080(3) Uani 1 1 d . . .
C5 C 0.6534(8) 0.0870(7) 0.2670(6) 0.071(3) Uani 1 1 d . . .
H5 H 0.5810 0.0915 0.2684 0.085 Uiso 1 1 calc R . .
C6 C 0.7395(7) 0.1589(5) 0.2823(5) 0.051(2) Uani 1 1 d . . .
C7 C 0.7126(6) 0.2441(5) 0.2944(5) 0.048(2) Uani 1 1 d . . .
H7A H 0.7109 0.2633 0.2473 0.058 Uiso 1 1 calc R . .
H7B H 0.6394 0.2375 0.3103 0.058 Uiso 1 1 calc R . .
C8 C 0.7993(6) 0.2822(5) 0.4248(4) 0.043(2) Uani 1 1 d . . .
H8A H 0.7335 0.2862 0.4486 0.052 Uiso 1 1 calc R . .
H8B H 0.8031 0.2244 0.4171 0.052 Uiso 1 1 calc R . .
C9 C 0.8992(6) 0.3351(6) 0.4740(5) 0.050(2) Uani 1 1 d . . .
H9A H 0.9008 0.3180 0.5220 0.061 Uiso 1 1 calc R . .
H9B H 0.8954 0.3930 0.4816 0.061 Uiso 1 1 calc R . .
C10 C 0.7483(6) 0.3879(5) 0.3573(5) 0.044(2) Uani 1 1 d . . .
H10A H 0.7521 0.4071 0.3102 0.053 Uiso 1 1 calc R . .
H10B H 0.7975 0.4310 0.3942 0.053 Uiso 1 1 calc R . .
C11 C 0.6315(6) 0.3802(5) 0.3780(5) 0.049(2) Uani 1 1 d . . .
C12 C 0.5421(7) 0.3615(7) 0.3230(5) 0.067(3) Uani 1 1 d . . .
H12 H 0.5548 0.3536 0.2734 0.080 Uiso 1 1 calc R . .
C13 C 0.4367(8) 0.3546(8) 0.3404(7) 0.089(4) Uani 1 1 d . . .
H13 H 0.3779 0.3403 0.3031 0.106 Uiso 1 1 calc R . .
C14 C 0.4184(8) 0.3693(8) 0.4155(7) 0.093(4) Uani 1 1 d . . .
H14 H 0.3468 0.3648 0.4277 0.112 Uiso 1 1 calc R . .
C15 C 0.5041(7) 0.3903(7) 0.4711(6) 0.072(3) Uani 1 1 d . . .
H15 H 0.4908 0.4004 0.5206 0.086 Uiso 1 1 calc R . .
C16 C 0.6117(6) 0.3965(6) 0.4526(5) 0.055(2) Uani 1 1 d . . .
C17 C 0.6862(9) 0.4327(8) 0.5824(6) 0.087(4) Uani 1 1 d . . .
H17A H 0.6482 0.4759 0.5938 0.130 Uiso 1 1 calc R . .
H17B H 0.7564 0.4479 0.6121 0.130 Uiso 1 1 calc R . .
H17C H 0.6430 0.3814 0.5930 0.130 Uiso 1 1 calc R . .
C18 C 1.0963(7) 0.3949(6) 0.4827(5) 0.068(3) Uani 1 1 d . . .
H18A H 1.1045 0.3871 0.5333 0.102 Uiso 1 1 calc R . .
H18B H 1.0810 0.4481 0.4813 0.102 Uiso 1 1 calc R . .
H18C H 1.1634 0.3927 0.4610 0.102 Uiso 1 1 calc R . .
C19 C 1.0290(8) 0.2462(6) 0.4478(5) 0.067(3) Uani 1 1 d . . .
H19A H 1.0843 0.2364 0.4162 0.101 Uiso 1 1 calc R . .
H19B H 0.9635 0.2017 0.4340 0.101 Uiso 1 1 calc R . .
H19C H 1.0561 0.2485 0.4985 0.101 Uiso 1 1 calc R . .
C20 C 0.7973(6) 0.1562(5) 0.0926(4) 0.0403(19) Uani 1 1 d . . .
C21 C 0.7039(7) 0.0888(5) 0.0784(5) 0.053(2) Uani 1 1 d . . .
C22 C 0.7150(8) 0.0064(5) 0.0659(5) 0.059(3) Uani 1 1 d . . .
H22 H 0.6536 -0.0388 0.0576 0.071 Uiso 1 1 calc R . .
C23 C 0.8191(8) -0.0049(5) 0.0663(6) 0.060(3) Uani 1 1 d . . .
C24 C 0.9130(7) 0.0601(5) 0.0770(5) 0.051(2) Uani 1 1 d . . .
H24 H 0.9822 0.0491 0.0746 0.061 Uiso 1 1 calc R . .
C25 C 0.9032(6) 0.1410(5) 0.0911(4) 0.0394(19) Uani 1 1 d . . .
C26 C 1.0054(6) 0.2126(5) 0.1086(4) 0.0399(19) Uani 1 1 d . . .
H26A H 1.0213 0.2282 0.1621 0.048 Uiso 1 1 calc R . .
H26B H 1.0669 0.1927 0.0900 0.048 Uiso 1 1 calc R . .
C27 C 0.9716(7) 0.2671(5) -0.0051(4) 0.045(2) Uani 1 1 d . . .
H27A H 0.9168 0.2142 -0.0177 0.054 Uiso 1 1 calc R . .
H27B H 1.0368 0.2612 -0.0289 0.054 Uiso 1 1 calc R . .
C28 C 0.9265(7) 0.3346(5) -0.0332(5) 0.048(2) Uani 1 1 d . . .
H28A H 0.9815 0.3874 -0.0204 0.058 Uiso 1 1 calc R . .
H28B H 0.9116 0.3210 -0.0869 0.058 Uiso 1 1 calc R . .
C29 C 1.1114(6) 0.3508(5) 0.0990(4) 0.0403(19) Uani 1 1 d . . .
H29A H 1.1208 0.3679 0.1525 0.048 Uiso 1 1 calc R . .
H29B H 1.1089 0.3999 0.0779 0.048 Uiso 1 1 calc R . .
C30 C 1.2135(6) 0.3239(5) 0.0769(5) 0.043(2) Uani 1 1 d . . .
C31 C 1.2745(6) 0.2917(5) 0.1250(5) 0.048(2) Uani 1 1 d . . .
H31 H 1.2474 0.2818 0.1695 0.057 Uiso 1 1 calc R . .
C32 C 1.3750(7) 0.2732(6) 0.1104(6) 0.065(3) Uani 1 1 d . . .
H32 H 1.4130 0.2501 0.1433 0.078 Uiso 1 1 calc R . .
C33 C 1.4159(8) 0.2908(7) 0.0447(7) 0.077(3) Uani 1 1 d . . .
H33 H 1.4830 0.2799 0.0338 0.093 Uiso 1 1 calc R . .
C34 C 1.3589(7) 0.3243(6) -0.0050(6) 0.063(3) Uani 1 1 d . . .
H34 H 1.3876 0.3360 -0.0486 0.076 Uiso 1 1 calc R . .
C35 C 1.2589(6) 0.3401(5) 0.0109(5) 0.048(2) Uani 1 1 d . . .
C36 C 1.2416(9) 0.3941(8) -0.1023(6) 0.087(4) Uani 1 1 d . . .
H36A H 1.3198 0.4175 -0.0931 0.131 Uiso 1 1 calc R . .
H36B H 1.2067 0.4335 -0.1203 0.131 Uiso 1 1 calc R . .
H36C H 1.2265 0.3438 -0.1387 0.131 Uiso 1 1 calc R . .
C37 C 0.7281(7) 0.2726(6) -0.0359(5) 0.061(3) Uani 1 1 d . . .
H37A H 0.7179 0.2721 -0.0883 0.092 Uiso 1 1 calc R . .
H37B H 0.6627 0.2798 -0.0142 0.092 Uiso 1 1 calc R . .
H37C H 0.7425 0.2208 -0.0276 0.092 Uiso 1 1 calc R . .
C38 C 0.7962(8) 0.4203(6) -0.0205(5) 0.067(3) Uani 1 1 d . . .
H38A H 0.8562 0.4679 -0.0015 0.100 Uiso 1 1 calc R . .
H38B H 0.7306 0.4279 0.0008 0.100 Uiso 1 1 calc R . .
H38C H 0.7840 0.4142 -0.0736 0.100 Uiso 1 1 calc R . .
C39 C 0.8116(8) 0.1299(5) 0.5629(5) 0.193(8) Uiso 1 1 d G . .
C40 C 0.7204(7) 0.1635(4) 0.5690(4) 0.174(7) Uiso 1 1 d G . .
C41 C 0.6264(8) 0.1300(5) 0.5188(4) 0.222(10) Uiso 1 1 d GD . .
C42 C 0.6235(9) 0.0630(5) 0.4625(4) 0.176(8) Uiso 1 1 d G . .
C43 C 0.7147(10) 0.0295(5) 0.4565(5) 0.183(8) Uiso 1 1 d G . .
C44 C 0.8088(9) 0.0629(6) 0.5067(5) 0.214(10) Uiso 1 1 d G . .
C46 C 0.5616(6) 0.3293(5) 0.7785(4) 0.128(5) Uiso 1 1 d G . .
C47 C 0.6414(7) 0.2872(4) 0.7582(3) 0.159(7) Uiso 1 1 d G . .
C48 C 0.7461(6) 0.3317(4) 0.7484(3) 0.155(6) Uiso 1 1 d G . .
C49 C 0.7711(6) 0.4184(4) 0.7591(4) 0.150(6) Uiso 1 1 d G . .
C50 C 0.6913(8) 0.4604(4) 0.7794(4) 0.104(4) Uiso 1 1 d G . .
C51 C 0.5866(7) 0.4159(5) 0.7891(4) 0.181(8) Uiso 1 1 d GD . .
C52 C 0.514(2) 0.4687(16) 0.8094(16) 0.275(13) Uiso 1 1 d D . .
C53 C 0.2722(14) -0.0261(12) 0.2757(9) 0.178(8) Uiso 1 1 d G . .
C54 C 0.2350(13) -0.0725(7) 0.2050(13) 0.322(17) Uiso 1 1 d G . .
C55 C 0.2322(13) -0.0324(12) 0.1444(8) 0.222(10) Uiso 1 1 d G . .
C56 C 0.2667(12) 0.0540(13) 0.1546(8) 0.209(9) Uiso 1 1 d G . .
C57 C 0.3039(11) 0.1004(7) 0.2253(11) 0.156(6) Uiso 1 1 d G . .
C58 C 0.3066(13) 0.0603(12) 0.2858(7) 0.311(16) Uiso 1 1 d GD . .
C59 C 0.338(2) 0.1088(16) 0.3562(12) 0.266(13) Uiso 1 1 d D . .
C60 C 0.1741(17) 0.3697(8) 0.6907(9) 0.159(7) Uiso 1 1 d G . .
C61 C 0.2596(13) 0.3509(13) 0.6524(9) 0.242(11) Uiso 1 1 d G . .
C62 C 0.2682(15) 0.2689(17) 0.6362(9) 0.264(13) Uiso 1 1 d G . .
C63 C 0.191(2) 0.2056(9) 0.6583(11) 0.258(12) Uiso 1 1 d G . .
C64 C 0.1058(16) 0.2245(11) 0.6966(11) 0.275(14) Uiso 1 1 d GD . .
C65 C 0.0972(12) 0.3065(15) 0.7128(9) 0.234(11) Uiso 1 1 d GD . .
C66 C 0.002(5) 0.317(4) 0.753(5) 0.38(9) Uiso 1 1 d D . .
C45 C 0.524(3) 0.158(3) 0.525(3) 0.37(3) Uiso 1 1 d D . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.831(5) . ?
Ti1 O2 1.858(6) . ?
Ti1 N1 2.303(6) . ?
Ti1 Cl1 2.306(2) . ?
Ti1 Cl2 2.343(3) . ?
Ti1 N2 2.359(7) . ?
Ti2 O1 1.801(5) . ?
Ti2 O3 1.857(5) . ?
Ti2 Cl3 2.299(2) . ?
Ti2 Cl4 2.332(2) . ?
Ti2 N3 2.343(6) . ?
Ti2 N4 2.355(7) . ?
Br1 C2 1.897(10) . ?
Br2 C4 1.885(10) . ?
Br3 C21 1.892(8) . ?
Br4 C23 1.914(9) . ?
N1 C7 1.506(9) . ?
N1 C10 1.514(9) . ?
N1 C8 1.515(10) . ?
N2 C19 1.492(11) . ?
N2 C18 1.502(10) . ?
N2 C9 1.508(10) . ?
N3 C26 1.500(9) . ?
N3 C27 1.506(9) . ?
N3 C29 1.508(9) . ?
N4 C28 1.480(10) . ?
N4 C37 1.500(10) . ?
N4 C38 1.504(10) . ?
O2 C1 1.306(9) . ?
O3 C20 1.339(9) . ?
O4 C16 1.376(9) . ?
O4 C17 1.450(11) . ?
O5 C35 1.376(10) . ?
O5 C36 1.429(11) . ?
C1 C2 1.399(12) . ?
C1 C6 1.409(11) . ?
C2 C3 1.398(13) . ?
C3 C4 1.391(15) . ?
C3 H3 0.9300 . ?
C4 C5 1.371(14) . ?
C5 C6 1.393(12) . ?
C5 H5 0.9300 . ?
C6 C7 1.528(12) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.498(11) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 C11 1.519(10) . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 C12 1.397(11) . ?
C11 C16 1.403(12) . ?
C12 C13 1.364(13) . ?
C12 H12 0.9300 . ?
C13 C14 1.406(15) . ?
C13 H13 0.9300 . ?
C14 C15 1.371(13) . ?
C14 H14 0.9300 . ?
C15 C16 1.399(11) . ?
C15 H15 0.9300 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C20 C21 1.402(11) . ?
C20 C25 1.410(10) . ?
C21 C22 1.403(12) . ?
C22 C23 1.361(12) . ?
C22 H22 0.9300 . ?
C23 C24 1.384(12) . ?
C24 C25 1.375(11) . ?
C24 H24 0.9300 . ?
C25 C26 1.514(10) . ?
C26 H26A 0.9700 . ?
C26 H26B 0.9700 . ?
C27 C28 1.520(11) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C28 H28A 0.9700 . ?
C28 H28B 0.9700 . ?
C29 C30 1.512(10) . ?
C29 H29A 0.9700 . ?
C29 H29B 0.9700 . ?
C30 C31 1.381(11) . ?
C30 C35 1.411(12) . ?
C31 C32 1.398(11) . ?
C31 H31 0.9300 . ?
C32 C33 1.390(14) . ?
C32 H32 0.9300 . ?
C33 C34 1.384(13) . ?
C33 H33 0.9300 . ?
C34 C35 1.382(11) . ?
C34 H34 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9600 . ?
C37 H37B 0.9600 . ?
C37 H37C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 C40 1.3900 . ?
C39 C44 1.3900 . ?
C40 C41 1.3900 . ?
C41 C42 1.3900 . ?
C41 C45 1.474(19) . ?
C42 C43 1.3900 . ?
C43 C44 1.3900 . ?
C46 C47 1.3900 . ?
C46 C51 1.3900 . ?
C47 C48 1.3900 . ?
C48 C49 1.3900 . ?
C49 C50 1.3900 . ?
C50 C51 1.3900 . ?
C51 C52 1.437(17) . ?
C53 C54 1.3900 . ?
C53 C58 1.3900 . ?
C54 C55 1.3900 . ?
C55 C56 1.3900 . ?
C56 C57 1.3900 . ?
C57 C58 1.3900 . ?
C58 C59 1.388(17) . ?
C60 C61 1.3900 . ?
C60 C65 1.3900 . ?
C61 C62 1.3900 . ?
C62 C63 1.3900 . ?
C63 C64 1.3900 . ?
C64 C65 1.3900 . ?
C65 C66 1.48(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O2 94.7(2) . . ?
O1 Ti1 N1 92.2(2) . . ?
O2 Ti1 N1 80.8(2) . . ?
O1 Ti1 Cl1 101.97(17) . . ?
O2 Ti1 Cl1 92.72(18) . . ?
N1 Ti1 Cl1 164.89(18) . . ?
O1 Ti1 Cl2 91.95(18) . . ?
O2 Ti1 Cl2 170.2(2) . . ?
N1 Ti1 Cl2 91.73(17) . . ?
Cl1 Ti1 Cl2 92.95(9) . . ?
O1 Ti1 N2 170.2(2) . . ?
O2 Ti1 N2 86.3(3) . . ?
N1 Ti1 N2 78.3(2) . . ?
Cl1 Ti1 N2 87.74(17) . . ?
Cl2 Ti1 N2 85.98(19) . . ?
O1 Ti2 O3 95.0(2) . . ?
O1 Ti2 Cl3 102.64(17) . . ?
O3 Ti2 Cl3 91.99(17) . . ?
O1 Ti2 Cl4 92.54(18) . . ?
O3 Ti2 Cl4 169.31(19) . . ?
Cl3 Ti2 Cl4 93.79(9) . . ?
O1 Ti2 N3 90.4(2) . . ?
O3 Ti2 N3 81.5(2) . . ?
Cl3 Ti2 N3 165.91(16) . . ?
Cl4 Ti2 N3 90.80(16) . . ?
O1 Ti2 N4 167.9(2) . . ?
O3 Ti2 N4 85.6(2) . . ?
Cl3 Ti2 N4 89.37(17) . . ?
Cl4 Ti2 N4 85.49(18) . . ?
N3 Ti2 N4 77.7(2) . . ?
C7 N1 C10 106.7(5) . . ?
C7 N1 C8 110.3(6) . . ?
C10 N1 C8 110.5(6) . . ?
C7 N1 Ti1 110.7(5) . . ?
C10 N1 Ti1 111.4(4) . . ?
C8 N1 Ti1 107.2(4) . . ?
C19 N2 C18 106.7(7) . . ?
C19 N2 C9 111.0(7) . . ?
C18 N2 C9 107.4(7) . . ?
C19 N2 Ti1 111.2(5) . . ?
C18 N2 Ti1 115.2(5) . . ?
C9 N2 Ti1 105.4(5) . . ?
C26 N3 C27 109.7(6) . . ?
C26 N3 C29 107.6(5) . . ?
C27 N3 C29 111.8(6) . . ?
C26 N3 Ti2 109.7(4) . . ?
C27 N3 Ti2 107.4(4) . . ?
C29 N3 Ti2 110.7(4) . . ?
C28 N4 C37 111.0(7) . . ?
C28 N4 C38 107.9(7) . . ?
C37 N4 C38 105.2(7) . . ?
C28 N4 Ti2 105.6(5) . . ?
C37 N4 Ti2 111.9(5) . . ?
C38 N4 Ti2 115.2(5) . . ?
Ti2 O1 Ti1 177.4(3) . . ?
C1 O2 Ti1 143.9(5) . . ?
C20 O3 Ti2 143.4(5) . . ?
C16 O4 C17 118.4(7) . . ?
C35 O5 C36 118.6(7) . . ?
O2 C1 C2 121.5(8) . . ?
O2 C1 C6 120.8(7) . . ?
C2 C1 C6 117.6(8) . . ?
C3 C2 C1 122.5(9) . . ?
C3 C2 Br1 119.3(8) . . ?
C1 C2 Br1 118.2(7) . . ?
C4 C3 C2 117.9(10) . . ?
C4 C3 H3 121.0 . . ?
C2 C3 H3 121.0 . . ?
C5 C4 C3 121.1(10) . . ?
C5 C4 Br2 120.4(9) . . ?
C3 C4 Br2 118.5(8) . . ?
C4 C5 C6 120.9(10) . . ?
C4 C5 H5 119.5 . . ?
C6 C5 H5 119.5 . . ?
C5 C6 C1 119.9(8) . . ?
C5 C6 C7 119.2(8) . . ?
C1 C6 C7 120.8(7) . . ?
N1 C7 C6 114.9(6) . . ?
N1 C7 H7A 108.5 . . ?
C6 C7 H7A 108.5 . . ?
N1 C7 H7B 108.5 . . ?
C6 C7 H7B 108.5 . . ?
H7A C7 H7B 107.5 . . ?
C9 C8 N1 110.5(6) . . ?
C9 C8 H8A 109.5 . . ?
N1 C8 H8A 109.5 . . ?
C9 C8 H8B 109.5 . . ?
N1 C8 H8B 109.5 . . ?
H8A C8 H8B 108.1 . . ?
C8 C9 N2 110.6(7) . . ?
C8 C9 H9A 109.5 . . ?
N2 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
N2 C9 H9B 109.5 . . ?
H9A C9 H9B 108.1 . . ?
N1 C10 C11 117.5(6) . . ?
N1 C10 H10A 107.9 . . ?
C11 C10 H10A 107.9 . . ?
N1 C10 H10B 107.9 . . ?
C11 C10 H10B 107.9 . . ?
H10A C10 H10B 107.2 . . ?
C12 C11 C16 118.4(8) . . ?
C12 C11 C10 120.8(8) . . ?
C16 C11 C10 120.7(7) . . ?
C13 C12 C11 121.7(9) . . ?
C13 C12 H12 119.1 . . ?
C11 C12 H12 119.1 . . ?
C12 C13 C14 118.8(9) . . ?
C12 C13 H13 120.6 . . ?
C14 C13 H13 120.6 . . ?
C15 C14 C13 121.4(9) . . ?
C15 C14 H14 119.3 . . ?
C13 C14 H14 119.3 . . ?
C14 C15 C16 119.2(9) . . ?
C14 C15 H15 120.4 . . ?
C16 C15 H15 120.4 . . ?
O4 C16 C15 123.0(8) . . ?
O4 C16 C11 116.5(7) . . ?
C15 C16 C11 120.4(8) . . ?
O4 C17 H17A 109.5 . . ?
O4 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
O4 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N2 C18 H18A 109.5 . . ?
N2 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N2 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
N2 C19 H19A 109.5 . . ?
N2 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
N2 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O3 C20 C21 119.4(7) . . ?
O3 C20 C25 121.0(7) . . ?
C21 C20 C25 119.5(7) . . ?
C20 C21 C22 120.7(8) . . ?
C20 C21 Br3 119.4(6) . . ?
C22 C21 Br3 119.8(6) . . ?
C23 C22 C21 117.5(8) . . ?
C23 C22 H22 121.3 . . ?
C21 C22 H22 121.3 . . ?
C22 C23 C24 123.5(8) . . ?
C22 C23 Br4 117.9(7) . . ?
C24 C23 Br4 118.6(7) . . ?
C25 C24 C23 119.4(8) . . ?
C25 C24 H24 120.3 . . ?
C23 C24 H24 120.3 . . ?
C24 C25 C20 119.3(7) . . ?
C24 C25 C26 120.0(7) . . ?
C20 C25 C26 120.6(7) . . ?
N3 C26 C25 116.5(6) . . ?
N3 C26 H26A 108.2 . . ?
C25 C26 H26A 108.2 . . ?
N3 C26 H26B 108.2 . . ?
C25 C26 H26B 108.2 . . ?
H26A C26 H26B 107.3 . . ?
N3 C27 C28 110.0(6) . . ?
N3 C27 H27A 109.7 . . ?
C28 C27 H27A 109.7 . . ?
N3 C27 H27B 109.7 . . ?
C28 C27 H27B 109.7 . . ?
H27A C27 H27B 108.2 . . ?
N4 C28 C27 111.4(7) . . ?
N4 C28 H28A 109.3 . . ?
C27 C28 H28A 109.3 . . ?
N4 C28 H28B 109.3 . . ?
C27 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
N3 C29 C30 118.9(6) . . ?
N3 C29 H29A 107.6 . . ?
C30 C29 H29A 107.6 . . ?
N3 C29 H29B 107.6 . . ?
C30 C29 H29B 107.6 . . ?
H29A C29 H29B 107.0 . . ?
C31 C30 C35 116.6(7) . . ?
C31 C30 C29 121.1(8) . . ?
C35 C30 C29 121.9(7) . . ?
C30 C31 C32 123.4(9) . . ?
C30 C31 H31 118.3 . . ?
C32 C31 H31 118.3 . . ?
C33 C32 C31 117.4(9) . . ?
C33 C32 H32 121.3 . . ?
C31 C32 H32 121.3 . . ?
C34 C33 C32 121.5(9) . . ?
C34 C33 H33 119.3 . . ?
C32 C33 H33 119.3 . . ?
C35 C34 C33 119.2(10) . . ?
C35 C34 H34 120.4 . . ?
C33 C34 H34 120.4 . . ?
O5 C35 C34 122.3(9) . . ?
O5 C35 C30 115.9(7) . . ?
C34 C35 C30 121.8(9) . . ?
O5 C36 H36A 109.5 . . ?
O5 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
O5 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
N4 C37 H37A 109.5 . . ?
N4 C37 H37B 109.5 . . ?
H37A C37 H37B 109.5 . . ?
N4 C37 H37C 109.5 . . ?
H37A C37 H37C 109.5 . . ?
H37B C37 H37C 109.5 . . ?
N4 C38 H38A 109.5 . . ?
N4 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
N4 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C40 C39 C44 120.0 . . ?
C41 C40 C39 120.0 . . ?
C42 C41 C40 120.0 . . ?
C42 C41 C45 116.7(19) . . ?
C40 C41 C45 123.2(19) . . ?
C41 C42 C43 120.0 . . ?
C42 C43 C44 120.0 . . ?
C43 C44 C39 120.0 . . ?
C47 C46 C51 120.0 . . ?
C48 C47 C46 120.0 . . ?
C47 C48 C49 120.0 . . ?
C50 C49 C48 120.0 . . ?
C49 C50 C51 120.0 . . ?
C50 C51 C46 120.0 . . ?
C50 C51 C52 112.9(14) . . ?
C46 C51 C52 127.1(14) . . ?
C54 C53 C58 120.0 . . ?
C55 C54 C53 120.0 . . ?
C56 C55 C54 120.0 . . ?
C55 C56 C57 120.0 . . ?
C58 C57 C56 120.0 . . ?
C59 C58 C57 118(2) . . ?
C59 C58 C53 121(2) . . ?
C57 C58 C53 120.0 . . ?
C61 C60 C65 120.0 . . ?
C60 C61 C62 120.0 . . ?
C63 C62 C61 120.0 . . ?
C64 C63 C62 120.0 . . ?
C63 C64 C65 120.0 . . ?
C64 C65 C60 120.0 . . ?
C64 C65 C66 114.2(18) . . ?
C60 C65 C66 125.8(18) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O1 Ti1 N1 C7 48.0(5) . . . . ?
O2 Ti1 N1 C7 -46.4(5) . . . . ?
Cl1 Ti1 N1 C7 -111.9(7) . . . . ?
Cl2 Ti1 N1 C7 140.0(5) . . . . ?
N2 Ti1 N1 C7 -134.4(5) . . . . ?
O1 Ti1 N1 C10 -70.6(5) . . . . ?
O2 Ti1 N1 C10 -165.0(5) . . . . ?
Cl1 Ti1 N1 C10 129.5(7) . . . . ?
Cl2 Ti1 N1 C10 21.4(5) . . . . ?
N2 Ti1 N1 C10 107.0(5) . . . . ?
O1 Ti1 N1 C8 168.3(5) . . . . ?
O2 Ti1 N1 C8 74.0(5) . . . . ?
Cl1 Ti1 N1 C8 8.4(10) . . . . ?
Cl2 Ti1 N1 C8 -99.6(4) . . . . ?
N2 Ti1 N1 C8 -14.1(5) . . . . ?
O1 Ti1 N2 C19 119.4(14) . . . . ?
O2 Ti1 N2 C19 23.5(6) . . . . ?
N1 Ti1 N2 C19 104.9(6) . . . . ?
Cl1 Ti1 N2 C19 -69.4(5) . . . . ?
Cl2 Ti1 N2 C19 -162.5(5) . . . . ?
O1 Ti1 N2 C18 -119.2(14) . . . . ?
O2 Ti1 N2 C18 145.0(6) . . . . ?
N1 Ti1 N2 C18 -133.6(6) . . . . ?
Cl1 Ti1 N2 C18 52.1(6) . . . . ?
Cl2 Ti1 N2 C18 -41.0(6) . . . . ?
O1 Ti1 N2 C9 -1.0(17) . . . . ?
O2 Ti1 N2 C9 -96.8(5) . . . . ?
N1 Ti1 N2 C9 -15.4(5) . . . . ?
Cl1 Ti1 N2 C9 170.3(5) . . . . ?
Cl2 Ti1 N2 C9 77.2(5) . . . . ?
O1 Ti2 N3 C26 50.9(5) . . . . ?
O3 Ti2 N3 C26 -44.0(4) . . . . ?
Cl3 Ti2 N3 C26 -107.4(8) . . . . ?
Cl4 Ti2 N3 C26 143.5(4) . . . . ?
N4 Ti2 N3 C26 -131.3(5) . . . . ?
O1 Ti2 N3 C27 170.0(5) . . . . ?
O3 Ti2 N3 C27 75.1(5) . . . . ?
Cl3 Ti2 N3 C27 11.7(10) . . . . ?
Cl4 Ti2 N3 C27 -97.4(4) . . . . ?
N4 Ti2 N3 C27 -12.2(5) . . . . ?
O1 Ti2 N3 C29 -67.6(5) . . . . ?
O3 Ti2 N3 C29 -162.6(5) . . . . ?
Cl3 Ti2 N3 C29 134.1(6) . . . . ?
Cl4 Ti2 N3 C29 24.9(5) . . . . ?
N4 Ti2 N3 C29 110.1(5) . . . . ?
O1 Ti2 N4 C28 -6.9(15) . . . . ?
O3 Ti2 N4 C28 -100.0(5) . . . . ?
Cl3 Ti2 N4 C28 168.0(5) . . . . ?
Cl4 Ti2 N4 C28 74.1(5) . . . . ?
N3 Ti2 N4 C28 -17.7(5) . . . . ?
O1 Ti2 N4 C37 114.1(12) . . . . ?
O3 Ti2 N4 C37 21.0(5) . . . . ?
Cl3 Ti2 N4 C37 -71.1(5) . . . . ?
Cl4 Ti2 N4 C37 -164.9(5) . . . . ?
N3 Ti2 N4 C37 103.3(5) . . . . ?
O1 Ti2 N4 C38 -125.8(12) . . . . ?
O3 Ti2 N4 C38 141.1(6) . . . . ?
Cl3 Ti2 N4 C38 49.0(6) . . . . ?
Cl4 Ti2 N4 C38 -44.8(6) . . . . ?
N3 Ti2 N4 C38 -136.6(6) . . . . ?
O3 Ti2 O1 Ti1 -12(7) . . . . ?
Cl3 Ti2 O1 Ti1 81(7) . . . . ?
Cl4 Ti2 O1 Ti1 176(7) . . . . ?
N3 Ti2 O1 Ti1 -93(7) . . . . ?
N4 Ti2 O1 Ti1 -104(7) . . . . ?
O2 Ti1 O1 Ti2 27(7) . . . . ?
N1 Ti1 O1 Ti2 -54(7) . . . . ?
Cl1 Ti1 O1 Ti2 120(7) . . . . ?
Cl2 Ti1 O1 Ti2 -146(7) . . . . ?
N2 Ti1 O1 Ti2 -68(8) . . . . ?
O1 Ti1 O2 C1 -66.6(10) . . . . ?
N1 Ti1 O2 C1 24.9(10) . . . . ?
Cl1 Ti1 O2 C1 -168.8(10) . . . . ?
Cl2 Ti1 O2 C1 65.8(16) . . . . ?
N2 Ti1 O2 C1 103.6(10) . . . . ?
O1 Ti2 O3 C20 -70.9(8) . . . . ?
Cl3 Ti2 O3 C20 -173.8(8) . . . . ?
Cl4 Ti2 O3 C20 63.4(14) . . . . ?
N3 Ti2 O3 C20 18.8(8) . . . . ?
N4 Ti2 O3 C20 97.0(8) . . . . ?
Ti1 O2 C1 C2 176.0(7) . . . . ?
Ti1 O2 C1 C6 -6.6(15) . . . . ?
O2 C1 C2 C3 -178.6(9) . . . . ?
C6 C1 C2 C3 4.0(15) . . . . ?
O2 C1 C2 Br1 0.2(13) . . . . ?
C6 C1 C2 Br1 -177.3(7) . . . . ?
C1 C2 C3 C4 -2.2(17) . . . . ?
Br1 C2 C3 C4 179.0(9) . . . . ?
C2 C3 C4 C5 -1.2(18) . . . . ?
C2 C3 C4 Br2 179.7(8) . . . . ?
C3 C4 C5 C6 2.9(17) . . . . ?
Br2 C4 C5 C6 -178.1(8) . . . . ?
C4 C5 C6 C1 -1.0(15) . . . . ?
C4 C5 C6 C7 174.6(9) . . . . ?
O2 C1 C6 C5 -179.8(8) . . . . ?
C2 C1 C6 C5 -2.3(13) . . . . ?
O2 C1 C6 C7 4.7(13) . . . . ?
C2 C1 C6 C7 -177.9(8) . . . . ?
C10 N1 C7 C6 -177.2(7) . . . . ?
C8 N1 C7 C6 -57.0(9) . . . . ?
Ti1 N1 C7 C6 61.4(8) . . . . ?
C5 C6 C7 N1 145.6(8) . . . . ?
C1 C6 C7 N1 -38.8(11) . . . . ?
C7 N1 C8 C9 164.0(6) . . . . ?
C10 N1 C8 C9 -78.2(7) . . . . ?
Ti1 N1 C8 C9 43.4(7) . . . . ?
N1 C8 C9 N2 -61.8(9) . . . . ?
C19 N2 C9 C8 -76.1(9) . . . . ?
C18 N2 C9 C8 167.7(7) . . . . ?
Ti1 N2 C9 C8 44.4(8) . . . . ?
C7 N1 C10 C11 56.4(9) . . . . ?
C8 N1 C10 C11 -63.6(8) . . . . ?
Ti1 N1 C10 C11 177.3(6) . . . . ?
N1 C10 C11 C12 -92.5(10) . . . . ?
N1 C10 C11 C16 91.1(10) . . . . ?
C16 C11 C12 C13 -3.4(16) . . . . ?
C10 C11 C12 C13 -179.8(10) . . . . ?
C11 C12 C13 C14 2.0(18) . . . . ?
C12 C13 C14 C15 0(2) . . . . ?
C13 C14 C15 C16 -0.5(19) . . . . ?
C17 O4 C16 C15 7.8(14) . . . . ?
C17 O4 C16 C11 -175.0(9) . . . . ?
C14 C15 C16 O4 176.2(11) . . . . ?
C14 C15 C16 C11 -0.9(16) . . . . ?
C12 C11 C16 O4 -174.5(9) . . . . ?
C10 C11 C16 O4 2.0(13) . . . . ?
C12 C11 C16 C15 2.8(14) . . . . ?
C10 C11 C16 C15 179.2(9) . . . . ?
Ti2 O3 C20 C21 -179.0(6) . . . . ?
Ti2 O3 C20 C25 0.1(13) . . . . ?
O3 C20 C21 C22 -178.1(8) . . . . ?
C25 C20 C21 C22 2.8(13) . . . . ?
O3 C20 C21 Br3 -0.7(11) . . . . ?
C25 C20 C21 Br3 -179.8(6) . . . . ?
C20 C21 C22 C23 -1.6(14) . . . . ?
Br3 C21 C22 C23 -179.0(7) . . . . ?
C21 C22 C23 C24 -1.2(15) . . . . ?
C21 C22 C23 Br4 178.7(7) . . . . ?
C22 C23 C24 C25 2.9(15) . . . . ?
Br4 C23 C24 C25 -177.1(6) . . . . ?
C23 C24 C25 C20 -1.6(13) . . . . ?
C23 C24 C25 C26 175.4(8) . . . . ?
O3 C20 C25 C24 179.7(7) . . . . ?
C21 C20 C25 C24 -1.2(12) . . . . ?
O3 C20 C25 C26 2.8(12) . . . . ?
C21 C20 C25 C26 -178.1(8) . . . . ?
C27 N3 C26 C25 -55.8(8) . . . . ?
C29 N3 C26 C25 -177.6(6) . . . . ?
Ti2 N3 C26 C25 61.8(7) . . . . ?
C24 C25 C26 N3 142.7(7) . . . . ?
C20 C25 C26 N3 -40.4(10) . . . . ?
C26 N3 C27 C28 159.7(6) . . . . ?
C29 N3 C27 C28 -81.0(8) . . . . ?
Ti2 N3 C27 C28 40.7(7) . . . . ?
C37 N4 C28 C27 -75.0(9) . . . . ?
C38 N4 C28 C27 170.3(7) . . . . ?
Ti2 N4 C28 C27 46.6(7) . . . . ?
N3 C27 C28 N4 -61.8(9) . . . . ?
C26 N3 C29 C30 55.9(9) . . . . ?
C27 N3 C29 C30 -64.6(9) . . . . ?
Ti2 N3 C29 C30 175.7(6) . . . . ?
N3 C29 C30 C31 -94.1(9) . . . . ?
N3 C29 C30 C35 94.2(9) . . . . ?
C35 C30 C31 C32 -1.6(12) . . . . ?
C29 C30 C31 C32 -173.8(8) . . . . ?
C30 C31 C32 C33 1.9(14) . . . . ?
C31 C32 C33 C34 -0.9(15) . . . . ?
C32 C33 C34 C35 -0.4(15) . . . . ?
C36 O5 C35 C34 2.0(13) . . . . ?
C36 O5 C35 C30 179.5(8) . . . . ?
C33 C34 C35 O5 178.0(8) . . . . ?
C33 C34 C35 C30 0.7(14) . . . . ?
C31 C30 C35 O5 -177.3(7) . . . . ?
C29 C30 C35 O5 -5.1(11) . . . . ?
C31 C30 C35 C34 0.3(12) . . . . ?
C29 C30 C35 C34 172.4(8) . . . . ?
C44 C39 C40 C41 0.0 . . . . ?
C39 C40 C41 C42 0.0 . . . . ?
C39 C40 C41 C45 175(3) . . . . ?
C40 C41 C42 C43 0.0 . . . . ?
C45 C41 C42 C43 -176(2) . . . . ?
C41 C42 C43 C44 0.0 . . . . ?
C42 C43 C44 C39 0.0 . . . . ?
C40 C39 C44 C43 0.0 . . . . ?
C51 C46 C47 C48 0.0 . . . . ?
C46 C47 C48 C49 0.0 . . . . ?
C47 C48 C49 C50 0.0 . . . . ?
C48 C49 C50 C51 0.0 . . . . ?
C49 C50 C51 C46 0.0 . . . . ?
C49 C50 C51 C52 -179.4(14) . . . . ?
C47 C46 C51 C50 0.0 . . . . ?
C47 C46 C51 C52 179.3(16) . . . . ?
C58 C53 C54 C55 0.0 . . . . ?
C53 C54 C55 C56 0.0 . . . . ?
C54 C55 C56 C57 0.0 . . . . ?
C55 C56 C57 C58 0.0 . . . . ?
C56 C57 C58 C59 -176(2) . . . . ?
C56 C57 C58 C53 0.0 . . . . ?
C54 C53 C58 C59 176(2) . . . . ?
C54 C53 C58 C57 0.0 . . . . ?
C65 C60 C61 C62 0.0 . . . . ?
C60 C61 C62 C63 0.0 . . . . ?
C61 C62 C63 C64 0.0 . . . . ?
C62 C63 C64 C65 0.0 . . . . ?
C63 C64 C65 C60 0.0 . . . . ?
C63 C64 C65 C66 179(5) . . . . ?
C61 C60 C65 C64 0.0 . . . . ?
C61 C60 C65 C66 -179(6) . . . . ?

_diffrn_measured_fraction_theta_max 0.997
_diffrn_reflns_theta_full        25.50
_diffrn_measured_fraction_theta_full 0.997
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.110
_database_code_depnum_ccdc_archive 'CCDC 968905'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_a10620a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C32 H53 Cl N2 O5 Ti'
_chemical_formula_weight         629.11

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   12.595(4)
_cell_length_b                   13.269(4)
_cell_length_c                   21.982(7)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.538(4)
_cell_angle_gamma                90.00
_cell_volume                     3556(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    783
_cell_measurement_theta_min      2.268
_cell_measurement_theta_max      20.021

_exptl_crystal_description       rod
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1352
_exptl_absorpt_coefficient_mu    0.353
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9588
_exptl_absorpt_correction_T_max  0.9791
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            14395
_diffrn_reflns_av_R_equivalents  0.0542
_diffrn_reflns_av_sigmaI/netI    0.0757
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.70
_diffrn_reflns_theta_max         25.01
_reflns_number_total             6253
_reflns_number_gt                3366
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART'
_computing_cell_refinement       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.1153P)²+0.0000P] 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_number_reflns         6253
_refine_ls_number_parameters     379
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1138
_refine_ls_R_factor_gt           0.0671
_refine_ls_wR_factor_ref         0.2081
_refine_ls_wR_factor_gt          0.1849
_refine_ls_goodness_of_fit_ref   0.954
_refine_ls_restrained_S_all      0.966
_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.50724(6) 1.06144(6) 0.19727(3) 0.0532(3) Uani 1 1 d . . .
Cl1 Cl 0.67614(9) 0.79240(10) 0.11681(6) 0.0731(4) Uani 1 1 d . . .
N1 N 0.3302(2) 1.0407(2) 0.12684(15) 0.0476(8) Uani 1 1 d . . .
N2 N 0.5213(3) 1.1482(3) 0.10447(16) 0.0588(9) Uani 1 1 d . . .
O1 O 0.5329(2) 0.9451(2) 0.14876(13) 0.0589(8) Uani 1 1 d . . .
O2 O 0.1619(3) 1.2290(2) 0.04119(16) 0.0743(10) Uani 1 1 d . . .
O3 O 0.4562(2) 1.1841(2) 0.21617(13) 0.0606(8) Uani 1 1 d . . .
O4 O 0.6506(2) 1.0791(2) 0.23082(14) 0.0708(9) Uani 1 1 d . . .
O5 O 0.4611(3) 0.9877(2) 0.25484(14) 0.0738(9) Uani 1 1 d . . .
C1 C 0.0893(3) 1.1643(3) 0.0568(2) 0.0598(12) Uani 1 1 d . . .
C2 C -0.0215(4) 1.1602(4) 0.0250(2) 0.0746(14) Uani 1 1 d . . .
H2 H -0.0477 1.2010 -0.0100 0.090 Uiso 1 1 calc R . .
C3 C -0.0920(4) 1.0968(4) 0.0447(3) 0.0785(15) Uani 1 1 d . . .
H3 H -0.1657 1.0951 0.0234 0.094 Uiso 1 1 calc R . .
C4 C -0.0542(4) 1.0363(4) 0.0955(3) 0.0765(14) Uani 1 1 d . . .
H4 H -0.1017 0.9928 0.1088 0.092 Uiso 1 1 calc R . .
C5 C 0.0571(4) 1.0402(4) 0.1277(2) 0.0678(13) Uani 1 1 d . . .
H5 H 0.0822 0.9995 0.1628 0.081 Uiso 1 1 calc R . .
C6 C 0.1298(3) 1.1022(3) 0.1089(2) 0.0522(10) Uani 1 1 d . . .
C7 C 0.2486(3) 1.1078(3) 0.14604(19) 0.0545(11) Uani 1 1 d . . .
H7A H 0.2730 1.1768 0.1444 0.065 Uiso 1 1 calc R . .
H7B H 0.2511 1.0931 0.1896 0.065 Uiso 1 1 calc R . .
C8 C 0.1288(5) 1.2853(4) -0.0147(3) 0.0991(19) Uani 1 1 d . . .
H8A H 0.1015 1.2405 -0.0494 0.149 Uiso 1 1 calc R . .
H8B H 0.1904 1.3221 -0.0215 0.149 Uiso 1 1 calc R . .
H8C H 0.0721 1.3316 -0.0112 0.149 Uiso 1 1 calc R . .
C9 C 0.3424(3) 1.0651(3) 0.06322(18) 0.0534(11) Uani 1 1 d . . .
H9A H 0.2704 1.0740 0.0349 0.064 Uiso 1 1 calc R . .
H9B H 0.3782 1.0095 0.0478 0.064 Uiso 1 1 calc R . .
C10 C 0.4088(3) 1.1598(3) 0.0640(2) 0.0600(11) Uani 1 1 d . . .
H10A H 0.4124 1.1758 0.0215 0.072 Uiso 1 1 calc R . .
H10B H 0.3727 1.2154 0.0794 0.072 Uiso 1 1 calc R . .
C11 C 0.5683(4) 1.2497(4) 0.1203(3) 0.0811(15) Uani 1 1 d . . .
H11A H 0.6421 1.2437 0.1456 0.122 Uiso 1 1 calc R . .
H11B H 0.5249 1.2859 0.1432 0.122 Uiso 1 1 calc R . .
H11C H 0.5683 1.2854 0.0823 0.122 Uiso 1 1 calc R . .
C12 C 0.5909(4) 1.0956(4) 0.0695(2) 0.0766(14) Uani 1 1 d . . .
H12A H 0.5573 1.0327 0.0537 0.115 Uiso 1 1 calc R . .
H12B H 0.6619 1.0831 0.0970 0.115 Uiso 1 1 calc R . .
H12C H 0.5986 1.1368 0.0349 0.115 Uiso 1 1 calc R . .
C13 C 0.4789(3) 0.8634(3) 0.12406(19) 0.0513(10) Uani 1 1 d . . .
C14 C 0.5341(3) 0.7816(3) 0.10648(19) 0.0537(11) Uani 1 1 d . . .
C15 C 0.4834(4) 0.6934(3) 0.0840(2) 0.0615(12) Uani 1 1 d . . .
H15 H 0.5249 0.6409 0.0740 0.074 Uiso 1 1 calc R . .
C16 C 0.3714(4) 0.6805(3) 0.0758(2) 0.0604(12) Uani 1 1 d . . .
C17 C 0.3153(4) 0.7635(3) 0.0888(2) 0.0595(12) Uani 1 1 d . . .
H17 H 0.2394 0.7588 0.0810 0.071 Uiso 1 1 calc R . .
C18 C 0.3645(3) 0.8546(3) 0.11309(19) 0.0505(10) Uani 1 1 d . . .
C19 C 0.2941(3) 0.9355(3) 0.1296(2) 0.0551(11) Uani 1 1 d . . .
H19A H 0.2213 0.9292 0.1017 0.066 Uiso 1 1 calc R . .
H19B H 0.2873 0.9228 0.1719 0.066 Uiso 1 1 calc R . .
C20 C 0.3152(4) 0.5806(4) 0.0552(3) 0.0858(17) Uani 1 1 d . . .
C21 C 0.3564(10) 0.5029(6) 0.0988(6) 0.286(9) Uani 1 1 d . . .
H21A H 0.3297 0.5120 0.1357 0.429 Uiso 1 1 calc R . .
H21B H 0.4351 0.5051 0.1102 0.429 Uiso 1 1 calc R . .
H21C H 0.3324 0.4388 0.0801 0.429 Uiso 1 1 calc R . .
C22 C 0.3409(8) 0.5419(7) -0.0063(5) 0.181(4) Uani 1 1 d U . .
H22A H 0.3045 0.4787 -0.0180 0.271 Uiso 1 1 calc R . .
H22B H 0.4187 0.5329 0.0005 0.271 Uiso 1 1 calc R . .
H22C H 0.3156 0.5901 -0.0392 0.271 Uiso 1 1 calc R . .
C23 C 0.1943(6) 0.5851(5) 0.0408(5) 0.184(5) Uani 1 1 d . . .
H23A H 0.1649 0.5182 0.0339 0.276 Uiso 1 1 calc R . .
H23B H 0.1672 0.6249 0.0037 0.276 Uiso 1 1 calc R . .
H23C H 0.1724 0.6152 0.0754 0.276 Uiso 1 1 calc R . .
C24 C 0.5462(8) 1.3083(9) 0.2863(5) 0.237(6) Uani 1 1 d . . .
H24A H 0.5160 1.3674 0.2630 0.356 Uiso 1 1 calc R . .
H24B H 0.6105 1.2874 0.2737 0.356 Uiso 1 1 calc R . .
H24C H 0.5655 1.3234 0.3304 0.356 Uiso 1 1 calc R . .
C25 C 0.4703(8) 1.2326(5) 0.2744(4) 0.128(3) Uani 1 1 d . . .
H25 H 0.5062 1.1803 0.3040 0.154 Uiso 1 1 calc R . .
C26 C 0.3804(9) 1.2503(10) 0.2930(6) 0.287(9) Uani 1 1 d . . .
H26A H 0.3991 1.2842 0.3329 0.431 Uiso 1 1 calc R . .
H26B H 0.3447 1.1877 0.2971 0.431 Uiso 1 1 calc R . .
H26C H 0.3319 1.2920 0.2626 0.431 Uiso 1 1 calc R . .
C27 C 0.7865(6) 0.9928(7) 0.3065(4) 0.169(4) Uani 1 1 d . . .
H27A H 0.7653 1.0369 0.3360 0.254 Uiso 1 1 calc R . .
H27B H 0.8643 0.9820 0.3191 0.254 Uiso 1 1 calc R . .
H27C H 0.7492 0.9295 0.3054 0.254 Uiso 1 1 calc R . .
C28 C 0.7568(5) 1.0390(5) 0.2434(3) 0.108(2) Uani 1 1 d . . .
H28 H 0.7577 0.9862 0.2124 0.129 Uiso 1 1 calc R . .
C29 C 0.8352(5) 1.1202(6) 0.2357(4) 0.132(3) Uani 1 1 d . . .
H29A H 0.8235 1.1365 0.1920 0.198 Uiso 1 1 calc R . .
H29B H 0.9092 1.0970 0.2518 0.198 Uiso 1 1 calc R . .
H29C H 0.8233 1.1792 0.2584 0.198 Uiso 1 1 calc R . .
C30 C 0.5053(14) 0.9450(8) 0.3615(4) 0.291(9) Uani 1 1 d . . .
H30A H 0.5242 0.8891 0.3899 0.436 Uiso 1 1 calc R . .
H30B H 0.4391 0.9758 0.3667 0.436 Uiso 1 1 calc R . .
H30C H 0.5637 0.9936 0.3705 0.436 Uiso 1 1 calc R . .
C31 C 0.4885(8) 0.9098(8) 0.2974(4) 0.151(3) Uani 1 1 d . . .
H31 H 0.5641 0.8958 0.2956 0.182 Uiso 1 1 calc R . .
C32 C 0.4436(13) 0.8197(8) 0.2859(5) 0.262(8) Uani 1 1 d . . .
H32A H 0.3781 0.8170 0.3006 0.393 Uiso 1 1 calc R . .
H32B H 0.4944 0.7695 0.3072 0.393 Uiso 1 1 calc R . .
H32C H 0.4257 0.8070 0.2415 0.393 Uiso 1 1 calc R . .


_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 1.787(3) . ?
Ti1 O5 1.808(3) . ?
Ti1 O3 1.836(3) . ?
Ti1 O1 1.949(3) . ?
Ti1 N2 2.387(4) . ?
Ti1 N1 2.390(3) . ?
Cl1 C14 1.752(4) . ?
N1 C19 1.474(5) . ?
N1 C9 1.480(5) . ?
N1 C7 1.498(5) . ?
N2 C11 1.477(6) . ?
N2 C12 1.478(6) . ?
N2 C10 1.480(5) . ?
O1 C13 1.322(5) . ?
O2 C1 1.361(5) . ?
O2 C8 1.408(6) . ?
O3 C25 1.404(7) . ?
O4 C28 1.401(6) . ?
O5 C31 1.379(8) . ?
C1 C2 1.396(6) . ?
C1 C6 1.399(6) . ?
C2 C3 1.371(7) . ?
C2 H2 0.9300 . ?
C3 C4 1.360(7) . ?
C3 H3 0.9300 . ?
C4 C5 1.404(6) . ?
C4 H4 0.9300 . ?
C5 C6 1.370(6) . ?
C5 H5 0.9300 . ?
C6 C7 1.516(5) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 H8A 0.9600 . ?
C8 H8B 0.9600 . ?
C8 H8C 0.9600 . ?
C9 C10 1.507(6) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 0.9700 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C12 H12A 0.9600 . ?
C12 H12B 0.9600 . ?
C12 H12C 0.9600 . ?
C13 C14 1.395(6) . ?
C13 C18 1.405(5) . ?
C14 C15 1.365(6) . ?
C15 C16 1.388(6) . ?
C15 H15 0.9300 . ?
C16 C17 1.377(6) . ?
C16 C20 1.516(6) . ?
C17 C18 1.401(6) . ?
C17 H17 0.9300 . ?
C18 C19 1.495(5) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.415(9) . ?
C20 C23 1.477(8) . ?
C20 C22 1.554(10) . ?
C21 H21A 0.9600 . ?
C21 H21B 0.9600 . ?
C21 H21C 0.9600 . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C24 C25 1.366(11) . ?
C24 H24A 0.9600 . ?
C24 H24B 0.9600 . ?
C24 H24C 0.9600 . ?
C25 C26 1.317(11) . ?
C25 H25 0.9800 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C27 C28 1.476(9) . ?
C27 H27A 0.9600 . ?
C27 H27B 0.9600 . ?
C27 H27C 0.9600 . ?
C28 C29 1.500(9) . ?
C28 H28 0.9800 . ?
C29 H29A 0.9600 . ?
C29 H29B 0.9600 . ?
C29 H29C 0.9600 . ?
C30 C31 1.449(12) . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 C32 1.320(10) . ?
C31 H31 0.9800 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O4 Ti1 O5 104.58(15) . . ?
O4 Ti1 O3 99.53(13) . . ?
O5 Ti1 O3 97.43(15) . . ?
O4 Ti1 O1 92.31(13) . . ?
O5 Ti1 O1 94.64(14) . . ?
O3 Ti1 O1 160.37(13) . . ?
O4 Ti1 N2 90.30(14) . . ?
O5 Ti1 N2 164.86(13) . . ?
O3 Ti1 N2 82.60(13) . . ?
O1 Ti1 N2 81.73(13) . . ?
O4 Ti1 N1 164.71(14) . . ?
O5 Ti1 N1 88.82(13) . . ?
O3 Ti1 N1 85.75(12) . . ?
O1 Ti1 N1 79.06(11) . . ?
N2 Ti1 N1 76.07(12) . . ?
C19 N1 C9 110.6(3) . . ?
C19 N1 C7 108.0(3) . . ?
C9 N1 C7 112.2(3) . . ?
C19 N1 Ti1 109.3(2) . . ?
C9 N1 Ti1 106.6(2) . . ?
C7 N1 Ti1 110.1(2) . . ?
C11 N2 C12 107.4(4) . . ?
C11 N2 C10 108.2(4) . . ?
C12 N2 C10 109.9(3) . . ?
C11 N2 Ti1 110.5(3) . . ?
C12 N2 Ti1 113.5(3) . . ?
C10 N2 Ti1 107.3(2) . . ?
C13 O1 Ti1 137.3(3) . . ?
C1 O2 C8 119.0(4) . . ?
C25 O3 Ti1 129.9(4) . . ?
C28 O4 Ti1 148.0(4) . . ?
C31 O5 Ti1 144.2(5) . . ?
O2 C1 C2 123.3(4) . . ?
O2 C1 C6 116.6(4) . . ?
C2 C1 C6 120.1(5) . . ?
C3 C2 C1 120.6(5) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.1(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C3 C4 C5 119.4(5) . . ?
C3 C4 H4 120.3 . . ?
C5 C4 H4 120.3 . . ?
C6 C5 C4 121.9(5) . . ?
C6 C5 H5 119.1 . . ?
C4 C5 H5 119.1 . . ?
C5 C6 C1 117.8(4) . . ?
C5 C6 C7 120.7(4) . . ?
C1 C6 C7 121.3(4) . . ?
N1 C7 C6 118.3(3) . . ?
N1 C7 H7A 107.7 . . ?
C6 C7 H7A 107.7 . . ?
N1 C7 H7B 107.7 . . ?
C6 C7 H7B 107.7 . . ?
H7A C7 H7B 107.1 . . ?
O2 C8 H8A 109.5 . . ?
O2 C8 H8B 109.5 . . ?
H8A C8 H8B 109.5 . . ?
O2 C8 H8C 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
N1 C9 C10 111.1(3) . . ?
N1 C9 H9A 109.4 . . ?
C10 C9 H9A 109.4 . . ?
N1 C9 H9B 109.4 . . ?
C10 C9 H9B 109.4 . . ?
H9A C9 H9B 108.0 . . ?
N2 C10 C9 111.4(3) . . ?
N2 C10 H10A 109.3 . . ?
C9 C10 H10A 109.3 . . ?
N2 C10 H10B 109.3 . . ?
C9 C10 H10B 109.3 . . ?
H10A C10 H10B 108.0 . . ?
N2 C11 H11A 109.5 . . ?
N2 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
N2 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N2 C12 H12A 109.5 . . ?
N2 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N2 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
O1 C13 C14 120.7(4) . . ?
O1 C13 C18 122.6(4) . . ?
C14 C13 C18 116.7(4) . . ?
C15 C14 C13 123.2(4) . . ?
C15 C14 Cl1 119.1(3) . . ?
C13 C14 Cl1 117.7(3) . . ?
C14 C15 C16 121.4(4) . . ?
C14 C15 H15 119.3 . . ?
C16 C15 H15 119.3 . . ?
C17 C16 C15 115.6(4) . . ?
C17 C16 C20 122.4(4) . . ?
C15 C16 C20 122.0(4) . . ?
C16 C17 C18 124.7(4) . . ?
C16 C17 H17 117.7 . . ?
C18 C17 H17 117.7 . . ?
C17 C18 C13 118.3(4) . . ?
C17 C18 C19 118.6(4) . . ?
C13 C18 C19 123.0(4) . . ?
N1 C19 C18 117.5(3) . . ?
N1 C19 H19A 107.9 . . ?
C18 C19 H19A 107.9 . . ?
N1 C19 H19B 107.9 . . ?
C18 C19 H19B 107.9 . . ?
H19A C19 H19B 107.2 . . ?
C21 C20 C23 111.0(8) . . ?
C21 C20 C16 111.8(6) . . ?
C23 C20 C16 114.0(4) . . ?
C21 C20 C22 103.1(8) . . ?
C23 C20 C22 104.8(7) . . ?
C16 C20 C22 111.4(5) . . ?
C20 C21 H21A 109.5 . . ?
C20 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C20 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
C20 C22 H22A 109.5 . . ?
C20 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C20 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C20 C23 H23A 109.5 . . ?
C20 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C20 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C25 C24 H24A 109.5 . . ?
C25 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C25 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
C26 C25 C24 115.1(8) . . ?
C26 C25 O3 116.3(8) . . ?
C24 C25 O3 115.6(8) . . ?
C26 C25 H25 102.2 . . ?
C24 C25 H25 102.2 . . ?
O3 C25 H25 102.2 . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C28 C27 H27A 109.5 . . ?
C28 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C28 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
O4 C28 C27 110.3(6) . . ?
O4 C28 C29 109.2(6) . . ?
C27 C28 C29 112.7(6) . . ?
O4 C28 H28 108.2 . . ?
C27 C28 H28 108.2 . . ?
C29 C28 H28 108.2 . . ?
C28 C29 H29A 109.5 . . ?
C28 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C28 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C31 C30 H30A 109.5 . . ?
C31 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C31 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C32 C31 O5 121.7(7) . . ?
C32 C31 C30 115.4(9) . . ?
O5 C31 C30 111.6(9) . . ?
C32 C31 H31 101.2 . . ?
O5 C31 H31 101.2 . . ?
C30 C31 H31 101.2 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.614
_refine_diff_density_min         -0.380
_refine_diff_density_rms         0.059

_database_code_depnum_ccdc_archive 'CCDC 991086'
