# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
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data_e3559a_a
_database_code_depnum_ccdc_archive 'CCDC 1880954'
_audit_update_record             
;
2018-11-27 deposited with the CCDC.
2019-01-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C68 H51 N7 O7 Ti, C H Cl3  solvent'
_chemical_formula_sum            'C69 H52 Cl3 N7 O7 Ti  solvent '
_chemical_formula_weight         1245.42

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'
Ti Ti 0.2776 0.4457 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

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

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

_cell_length_a                   23.6828(12)
_cell_length_b                   31.4643(16)
_cell_length_c                   18.0577(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13455.9(11)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    18000
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             5152
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.302
_shelx_estimated_absorpt_T_min   0.982
_shelx_estimated_absorpt_T_max   0.985
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18797
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_v_R_equivalents   0.0871
_diffrn_reflns_av_R_equivalents  0.0215
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_k_max       44
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.559
_diffrn_reflns_theta_max         30.126
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measured_fraction_theta_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.946
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_point_group_measured_fraction_full 0.984
_reflns_number_total             18797
_reflns_number_gt                10327
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²+0.5130P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         18797
_refine_ls_number_parameters     823
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1576
_refine_ls_R_factor_gt           0.1013
_refine_ls_wR_factor_ref         0.3424
_refine_ls_wR_factor_gt          0.3011
_refine_ls_goodness_of_fit_ref   1.132
_refine_ls_restrained_S_all      1.132
_refine_ls_shift/su_max          0.069
_refine_ls_shift/su_mean         0.006

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.46415(3) 0.67060(2) 0.36563(3) 0.02469(18) Uani 1 1 d . . . . .
C1 C 0.47071(19) 0.70258(12) 0.1300(2) 0.0417(10) Uani 1 1 d . . . . .
C2 C 0.51299(18) 0.71894(12) 0.1753(2) 0.0409(9) Uani 1 1 d . . . . .
H2 H 0.5040 0.7268 0.2247 0.049 Uiso 1 1 calc R U . . .
C3 C 0.5671(2) 0.72393(15) 0.1505(3) 0.0574(13) Uani 1 1 d . . . . .
H3 H 0.5954 0.7347 0.1826 0.069 Uiso 1 1 calc R U . . .
C4 C 0.5803(2) 0.71313(16) 0.0779(3) 0.0622(13) Uani 1 1 d . . . . .
H4 H 0.6178 0.7169 0.0602 0.075 Uiso 1 1 calc R U . . .
C5 C 0.5395(2) 0.69703(16) 0.0316(3) 0.0598(13) Uani 1 1 d . . . . .
H5 H 0.5487 0.6895 -0.0179 0.072 Uiso 1 1 calc R U . . .
C6 C 0.4855(2) 0.69192(13) 0.0572(2) 0.0463(10) Uani 1 1 d . . . . .
H6 H 0.4574 0.6809 0.0249 0.056 Uiso 1 1 calc R U . . .
C7 C 0.41242(18) 0.69553(11) 0.1556(2) 0.0388(9) Uani 1 1 d . . . . .
C8 C 0.39997(16) 0.67445(10) 0.22361(19) 0.0329(8) Uani 1 1 d . . . . .
O1 O 0.44410(10) 0.66371(7) 0.26733(12) 0.0290(5) Uani 1 1 d . . . . .
C9 C 0.34525(17) 0.66394(11) 0.2427(2) 0.0379(9) Uani 1 1 d . . . . .
C10 C 0.3007(2) 0.67756(15) 0.1971(3) 0.0512(11) Uani 1 1 d . . . . .
H10 H 0.2628 0.6718 0.2110 0.061 Uiso 1 1 calc R U . . .
C11 C 0.3120(2) 0.69941(15) 0.1316(3) 0.0591(13) Uani 1 1 d . . . . .
H11 H 0.2818 0.7086 0.1009 0.071 Uiso 1 1 calc R U . . .
C12 C 0.3664(2) 0.70761(14) 0.1118(2) 0.0494(11) Uani 1 1 d . . . . .
H12 H 0.3734 0.7221 0.0665 0.059 Uiso 1 1 calc R U . . .
C13 C 0.32902(16) 0.63547(12) 0.3071(2) 0.0393(9) Uani 1 1 d . . . . .
C14 C 0.34701(15) 0.64205(11) 0.3801(2) 0.0338(8) Uani 1 1 d . . . . .
O2 O 0.38776(10) 0.67102(7) 0.39470(14) 0.0306(5) Uani 1 1 d . . . . .
C15 C 0.32390(16) 0.61777(12) 0.4390(2) 0.0381(8) Uani 1 1 d . . . . .
C16 C 0.28560(19) 0.58556(14) 0.4211(3) 0.0514(11) Uani 1 1 d . . . . .
H16 H 0.2696 0.5690 0.4598 0.062 Uiso 1 1 calc R U . . .
C17 C 0.2705(2) 0.57725(17) 0.3493(3) 0.0617(13) Uani 1 1 d . . . . .
H17 H 0.2460 0.5542 0.3383 0.074 Uiso 1 1 calc R U . . .
C18 C 0.29103(18) 0.60257(15) 0.2929(3) 0.0506(11) Uani 1 1 d . . . . .
H18 H 0.2790 0.5975 0.2434 0.061 Uiso 1 1 calc R U . . .
C19 C 0.33729(16) 0.62703(12) 0.5185(2) 0.0381(8) Uani 1 1 d . . . . .
C20 C 0.3435(2) 0.66834(13) 0.5447(3) 0.0480(10) Uani 1 1 d . . . . .
H20 H 0.3422 0.6916 0.5112 0.058 Uiso 1 1 calc R U . . .
C21 C 0.3517(2) 0.67574(15) 0.6201(3) 0.0540(12) Uani 1 1 d . . . . .
H21 H 0.3551 0.7041 0.6377 0.065 Uiso 1 1 calc R U . . .
C22 C 0.3550(2) 0.64202(17) 0.6699(3) 0.0572(12) Uani 1 1 d . . . . .
H22 H 0.3612 0.6472 0.7211 0.069 Uiso 1 1 calc R U . . .
C23 C 0.3489(2) 0.60107(17) 0.6439(3) 0.0624(13) Uani 1 1 d . . . . .
H23 H 0.3513 0.5779 0.6774 0.075 Uiso 1 1 calc R U . . .
C24 C 0.33917(19) 0.59334(14) 0.5686(2) 0.0488(10) Uani 1 1 d . . . . .
H24 H 0.3338 0.5650 0.5516 0.059 Uiso 1 1 calc R U . . .
C25 C 0.4181(2) 0.80246(12) 0.3501(2) 0.0455(10) Uani 1 1 d . . . . .
C26 C 0.3958(3) 0.83830(18) 0.3856(3) 0.081(2) Uani 1 1 d . . . . .
H26 H 0.4204 0.8591 0.4059 0.098 Uiso 1 1 calc R U . . .
C27 C 0.3385(4) 0.8433(3) 0.3910(3) 0.120(4) Uani 1 1 d . . . . .
H27 H 0.3235 0.8678 0.4146 0.144 Uiso 1 1 calc R U . . .
C28 C 0.3033(3) 0.8138(3) 0.3629(3) 0.096(3) Uani 1 1 d . . . . .
H28 H 0.2637 0.8179 0.3673 0.116 Uiso 1 1 calc R U . . .
C29 C 0.3231(2) 0.7775(2) 0.3275(3) 0.0729(16) Uani 1 1 d . . . . .
H29 H 0.2979 0.7565 0.3091 0.087 Uiso 1 1 calc R U . . .
C30 C 0.38080(19) 0.77306(13) 0.3202(3) 0.0508(11) Uani 1 1 d . . . . .
H30 H 0.3954 0.7493 0.2940 0.061 Uiso 1 1 calc R U . . .
C31 C 0.48022(19) 0.79755(11) 0.3412(2) 0.0396(9) Uani 1 1 d . . . . .
C32 C 0.50777(16) 0.75941(10) 0.36132(18) 0.0309(7) Uani 1 1 d . . . . .
O3 O 0.47552(11) 0.72710(7) 0.38647(14) 0.0330(6) Uani 1 1 d . . . . .
C33 C 0.56669(17) 0.75579(11) 0.35719(19) 0.0335(8) Uani 1 1 d . . . . .
C34 C 0.5967(2) 0.79044(13) 0.3272(2) 0.0472(10) Uani 1 1 d . . . . .
H34 H 0.6364 0.7881 0.3210 0.057 Uiso 1 1 calc R U . . .
C35 C 0.5699(3) 0.82778(13) 0.3064(2) 0.0578(14) Uani 1 1 d . . . . .
H35 H 0.5909 0.8506 0.2858 0.069 Uiso 1 1 calc R U . . .
C36 C 0.5126(2) 0.83124(12) 0.3162(2) 0.0507(12) Uani 1 1 d . . . . .
H36 H 0.4946 0.8575 0.3056 0.061 Uiso 1 1 calc R U . . .
C37 C 0.60155(16) 0.72017(11) 0.3883(2) 0.0351(8) Uani 1 1 d . . . . .
C38 C 0.58858(16) 0.67634(11) 0.38037(19) 0.0306(7) Uani 1 1 d . . . . .
O4 O 0.54214(10) 0.66336(7) 0.34475(14) 0.0294(5) Uani 1 1 d . . . . .
C39 C 0.62608(16) 0.64602(12) 0.4101(2) 0.0375(8) Uani 1 1 d . . . . .
C40 C 0.6745(2) 0.65896(16) 0.4473(3) 0.0599(13) Uani 1 1 d . . . . .
H40 H 0.6995 0.6384 0.4674 0.072 Uiso 1 1 calc R U . . .
C41 C 0.6863(2) 0.70178(16) 0.4552(3) 0.0597(13) Uani 1 1 d . . . . .
H41 H 0.7196 0.7105 0.4803 0.072 Uiso 1 1 calc R U . . .
C42 C 0.65022(18) 0.73160(14) 0.4270(2) 0.0462(10) Uani 1 1 d . . . . .
H42 H 0.6585 0.7609 0.4340 0.055 Uiso 1 1 calc R U . . .
C43 C 0.61629(16) 0.59936(12) 0.4005(2) 0.0386(9) Uani 1 1 d . . . . .
C44 C 0.62483(18) 0.57178(14) 0.4589(3) 0.0488(10) Uani 1 1 d . . . . .
H44 H 0.6371 0.5829 0.5051 0.059 Uiso 1 1 calc R U . . .
C45 C 0.6160(2) 0.52851(15) 0.4523(3) 0.0597(13) Uani 1 1 d . . . . .
H45 H 0.6210 0.5104 0.4939 0.072 Uiso 1 1 calc R U . . .
C46 C 0.5999(2) 0.51183(15) 0.3844(3) 0.0643(14) Uani 1 1 d . . . . .
H46 H 0.5948 0.4821 0.3784 0.077 Uiso 1 1 calc R U . . .
C47 C 0.59175(19) 0.53847(14) 0.3272(3) 0.0558(12) Uani 1 1 d . . . . .
H47 H 0.5801 0.5273 0.2807 0.067 Uiso 1 1 calc R U . . .
C48 C 0.60000(18) 0.58185(13) 0.3345(2) 0.0450(9) Uani 1 1 d . . . . .
H48 H 0.5942 0.5998 0.2929 0.054 Uiso 1 1 calc R U . . .
N1 N 0.48635(12) 0.65457(8) 0.48236(15) 0.0276(6) Uani 1 1 d . . . . .
C49 C 0.49901(17) 0.68341(11) 0.5346(2) 0.0381(9) Uani 1 1 d . . . . .
H49 H 0.4987 0.7128 0.5222 0.046 Uiso 1 1 calc R U . . .
C50 C 0.5125(2) 0.67123(12) 0.6058(2) 0.0499(11) Uani 1 1 d . . . . .
H50 H 0.5221 0.6915 0.6427 0.060 Uiso 1 1 calc R U . . .
C51 C 0.5113(2) 0.62807(13) 0.6211(2) 0.0498(11) Uani 1 1 d . . . . .
H51 H 0.5195 0.6190 0.6701 0.060 Uiso 1 1 calc R U . . .
N2 N 0.49931(16) 0.59877(10) 0.57007(17) 0.0418(8) Uani 1 1 d . . . . .
C52 C 0.48670(15) 0.61356(10) 0.50346(19) 0.0294(7) Uani 1 1 d . . . . .
C53 C 0.47202(14) 0.58236(10) 0.44559(18) 0.0260(7) Uani 1 1 d . . . . .
N3 N 0.45920(12) 0.59896(8) 0.37862(15) 0.0253(6) Uani 1 1 d . . . . .
N4 N 0.47368(13) 0.54151(9) 0.46223(17) 0.0350(7) Uani 1 1 d . . . . .
C54 C 0.46249(16) 0.51449(11) 0.4070(2) 0.0354(8) Uani 1 1 d . . . . .
H54 H 0.4650 0.4848 0.4164 0.042 Uiso 1 1 calc R U . . .
C55 C 0.44727(14) 0.52790(10) 0.33623(19) 0.0283(7) Uani 1 1 d . . . . .
C56 C 0.44585(14) 0.57163(10) 0.32439(18) 0.0261(7) Uani 1 1 d . . . . .
H56 H 0.4353 0.5823 0.2771 0.031 Uiso 1 1 calc R U . . .
C57 C 0.43821(15) 0.49722(10) 0.27676(19) 0.0302(7) Uani 1 1 d . . . . .
N5 N 0.4420(2) 0.45499(10) 0.2898(2) 0.0606(12) Uani 1 1 d . . . . .
N6 N 0.4346(2) 0.43446(10) 0.2279(2) 0.0613(12) Uani 1 1 d . . . . .
N7 N 0.42489(13) 0.46320(9) 0.17439(16) 0.0327(7) Uani 1 1 d . . . . .
C58 C 0.42698(14) 0.50285(10) 0.20287(19) 0.0298(7) Uani 1 1 d . . . . .
H58 H 0.4218 0.5290 0.1773 0.036 Uiso 1 1 calc R U . . .
C59 C 0.41882(16) 0.44946(13) 0.0982(2) 0.0380(8) Uani 1 1 d . . . . .
H59A H 0.3944 0.4699 0.0717 0.046 Uiso 1 1 calc R U . . .
H59B H 0.3997 0.4215 0.0975 0.046 Uiso 1 1 calc R U . . .
C60 C 0.47474(15) 0.44582(11) 0.0575(2) 0.0337(8) Uani 1 1 d . . . . .
C61 C 0.52448(16) 0.46017(12) 0.0862(2) 0.0393(9) Uani 1 1 d . . . . .
H61 H 0.5256 0.4719 0.1347 0.047 Uiso 1 1 calc R U . . .
C62 C 0.57424(17) 0.45761(12) 0.0437(2) 0.0412(9) Uani 1 1 d . . . . .
C63 C 0.57215(15) 0.44109(11) -0.0272(2) 0.0355(8) Uani 1 1 d . . . . .
C64 C 0.52125(16) 0.42586(11) -0.0559(2) 0.0335(8) Uani 1 1 d . . . . .
C65 C 0.47308(16) 0.42806(12) -0.0138(2) 0.0367(8) Uani 1 1 d . . . . .
H65 H 0.4385 0.4175 -0.0330 0.044 Uiso 1 1 calc R U . . .
O5 O 0.62593(12) 0.47156(11) 0.06599(19) 0.0577(9) Uani 1 1 d . . . . .
C66 C 0.6294(2) 0.4890(2) 0.1388(3) 0.0702(16) Uani 1 1 d . . . . .
H66A H 0.6029 0.5127 0.1434 0.105 Uiso 1 1 calc R U . . .
H66B H 0.6679 0.4992 0.1479 0.105 Uiso 1 1 calc R U . . .
H66C H 0.6199 0.4670 0.1752 0.105 Uiso 1 1 calc R U . . .
O6 O 0.61954(11) 0.44253(9) -0.07124(16) 0.0464(7) Uani 1 1 d . . . . .
C67 C 0.6536(2) 0.40528(15) -0.0721(3) 0.0536(11) Uani 1 1 d . . . . .
H67A H 0.6679 0.3997 -0.0221 0.080 Uiso 1 1 calc R U . . .
H67B H 0.6855 0.4095 -0.1059 0.080 Uiso 1 1 calc R U . . .
H67C H 0.6310 0.3811 -0.0889 0.080 Uiso 1 1 calc R U . . .
O7 O 0.52402(12) 0.40972(9) -0.12579(14) 0.0414(6) Uani 1 1 d . . . . .
C68 C 0.47286(18) 0.39547(13) -0.1580(2) 0.0426(9) Uani 1 1 d . . . . .
H68A H 0.4549 0.3747 -0.1251 0.064 Uiso 1 1 calc R U . . .
H68B H 0.4808 0.3822 -0.2059 0.064 Uiso 1 1 calc R U . . .
H68C H 0.4474 0.4197 -0.1651 0.064 Uiso 1 1 calc R U . . .
C69 C 0.6923(8) 0.6129(6) 1.0652(14) 0.187(13) Uani 0.5 1 d . . P . .
H69 H 0.7278 0.6293 1.0742 0.224 Uiso 0.5 1 calc R U P . .
Cl1 Cl 0.7251(4) 0.5687(3) 1.0382(6) 0.244(5) Uani 0.5 1 d . . P . .
Cl2 Cl 0.6709(2) 0.6426(2) 1.0014(4) 0.158(2) Uani 0.5 1 d . . P . .
Cl3 Cl 0.6669(2) 0.6204(3) 1.1496(4) 0.212(4) Uani 0.5 1 d . . P . .
C70 C 0.7480(6) 0.5300(4) 0.8639(10) 0.105(5) Uani 0.5 1 d . . P . .
H70 H 0.7900 0.5330 0.8657 0.126 Uiso 0.5 1 calc R U P . .
Cl4 Cl 0.72889(16) 0.51074(17) 0.9505(3) 0.141(2) Uani 0.5 1 d . . P . .
Cl5 Cl 0.72148(13) 0.58356(11) 0.8501(2) 0.0879(10) Uani 0.5 1 d . . P . .
Cl6 Cl 0.7365(3) 0.49673(18) 0.8030(4) 0.158(2) Uani 0.5 1 d . . P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.837(2) . ?
Ti1 O1 1.850(2) . ?
Ti1 O2 1.884(2) . ?
Ti1 O4 1.899(2) . ?
Ti1 N1 2.230(3) . ?
Ti1 N3 2.269(3) . ?
C1 C2 1.392(6) . ?
C1 C6 1.401(6) . ?
C1 C7 1.473(6) . ?
C2 C3 1.365(7) . ?
C2 H2 0.9500 . ?
C3 C4 1.390(7) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(7) . ?
C4 H4 0.9500 . ?
C5 C6 1.370(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.400(6) . ?
C7 C8 1.426(5) . ?
C8 O1 1.353(4) . ?
C8 C9 1.381(6) . ?
C9 C10 1.405(6) . ?
C9 C13 1.517(6) . ?
C10 C11 1.394(7) . ?
C10 H10 0.9500 . ?
C11 C12 1.363(7) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.395(6) . ?
C13 C14 1.401(5) . ?
C14 O2 1.354(4) . ?
C14 C15 1.420(5) . ?
C15 C16 1.398(6) . ?
C15 C19 1.499(6) . ?
C16 C17 1.371(7) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(7) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.391(5) . ?
C19 C24 1.394(5) . ?
C20 C21 1.395(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.393(6) . ?
C21 H21 0.9500 . ?
C22 C23 1.379(7) . ?
C22 H22 0.9500 . ?
C23 C24 1.400(7) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.389(6) . ?
C25 C26 1.400(6) . ?
C25 C31 1.488(6) . ?
C26 C27 1.370(11) . ?
C26 H26 0.9500 . ?
C27 C28 1.348(12) . ?
C27 H27 0.9500 . ?
C28 C29 1.389(9) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(7) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.384(6) . ?
C31 C32 1.413(5) . ?
C32 O3 1.350(4) . ?
C32 C33 1.402(6) . ?
C33 C34 1.410(5) . ?
C33 C37 1.502(5) . ?
C34 C35 1.386(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.374(8) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.395(5) . ?
C37 C38 1.420(5) . ?
C38 O4 1.338(4) . ?
C38 C39 1.409(5) . ?
C39 C40 1.391(6) . ?
C39 C43 1.496(5) . ?
C40 C41 1.383(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.368(6) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.368(6) . ?
C43 C44 1.381(6) . ?
C44 C45 1.382(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(8) . ?
C45 H45 0.9500 . ?
C46 C47 1.344(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(6) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 C49 1.342(4) . ?
N1 C52 1.345(4) . ?
C49 C50 1.380(6) . ?
C49 H49 0.9500 . ?
C50 C51 1.386(5) . ?
C50 H50 0.9500 . ?
C51 N2 1.334(5) . ?
C51 H51 0.9500 . ?
N2 C52 1.324(4) . ?
C52 C53 1.475(4) . ?
C53 N4 1.321(4) . ?
C53 N3 1.352(4) . ?
N3 C56 1.341(4) . ?
N4 C54 1.337(5) . ?
C54 C55 1.393(5) . ?
C54 H54 0.9500 . ?
C55 C56 1.393(4) . ?
C55 C57 1.460(4) . ?
C56 H56 0.9500 . ?
C57 N5 1.353(4) . ?
C57 C58 1.372(5) . ?
N5 N6 1.302(5) . ?
N6 N7 1.344(4) . ?
N7 C58 1.350(4) . ?
N7 C59 1.449(4) . ?
C58 H58 0.9500 . ?
C59 C60 1.520(5) . ?
C59 H59A 0.9900 . ?
C59 H59B 0.9900 . ?
C60 C61 1.364(5) . ?
C60 C65 1.404(5) . ?
C61 C62 1.408(6) . ?
C61 H61 0.9500 . ?
C62 O5 1.361(5) . ?
C62 C63 1.384(5) . ?
C63 O6 1.376(5) . ?
C63 C64 1.397(5) . ?
C64 O7 1.362(4) . ?
C64 C65 1.373(5) . ?
C65 H65 0.9500 . ?
O5 C66 1.427(5) . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
O6 C67 1.424(5) . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
O7 C68 1.417(5) . ?
C68 H68A 0.9800 . ?
C68 H68B 0.9800 . ?
C68 H68C 0.9800 . ?
C69 Cl2 1.57(2) . ?
C69 Cl3 1.65(2) . ?
C69 Cl1 1.667(18) . ?
C69 H69 1.0000 . ?
Cl1 Cl4 2.416(11) . ?
C70 Cl6 1.544(16) . ?
C70 Cl4 1.738(18) . ?
C70 Cl5 1.814(12) . ?
C70 H70 1.0000 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O1 110.33(11) . . ?
O3 Ti1 O2 94.41(11) . . ?
O1 Ti1 O2 91.24(11) . . ?
O3 Ti1 O4 90.82(11) . . ?
O1 Ti1 O4 92.59(11) . . ?
O2 Ti1 O4 172.03(11) . . ?
O3 Ti1 N1 89.47(10) . . ?
O1 Ti1 N1 160.18(10) . . ?
O2 Ti1 N1 87.97(11) . . ?
O4 Ti1 N1 86.06(11) . . ?
O3 Ti1 N3 161.38(11) . . ?
O1 Ti1 N3 88.26(10) . . ?
O2 Ti1 N3 85.90(10) . . ?
O4 Ti1 N3 87.23(10) . . ?
N1 Ti1 N3 71.93(10) . . ?
C2 C1 C6 117.5(4) . . ?
C2 C1 C7 123.0(4) . . ?
C6 C1 C7 119.5(4) . . ?
C3 C2 C1 121.6(4) . . ?
C3 C2 H2 119.2 . . ?
C1 C2 H2 119.2 . . ?
C2 C3 C4 119.5(4) . . ?
C2 C3 H3 120.2 . . ?
C4 C3 H3 120.2 . . ?
C5 C4 C3 120.3(5) . . ?
C5 C4 H4 119.9 . . ?
C3 C4 H4 119.9 . . ?
C6 C5 C4 119.7(4) . . ?
C6 C5 H5 120.2 . . ?
C4 C5 H5 120.2 . . ?
C5 C6 C1 121.4(4) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C12 C7 C8 116.9(4) . . ?
C12 C7 C1 120.7(4) . . ?
C8 C7 C1 122.3(3) . . ?
O1 C8 C9 121.3(3) . . ?
O1 C8 C7 117.3(3) . . ?
C9 C8 C7 121.4(3) . . ?
C8 O1 Ti1 136.8(2) . . ?
C8 C9 C10 119.0(4) . . ?
C8 C9 C13 124.8(3) . . ?
C10 C9 C13 116.0(4) . . ?
C11 C10 C9 120.3(4) . . ?
C11 C10 H10 119.9 . . ?
C9 C10 H10 119.9 . . ?
C12 C11 C10 119.8(4) . . ?
C12 C11 H11 120.1 . . ?
C10 C11 H11 120.1 . . ?
C11 C12 C7 122.5(4) . . ?
C11 C12 H12 118.8 . . ?
C7 C12 H12 118.8 . . ?
C18 C13 C14 118.6(4) . . ?
C18 C13 C9 117.4(4) . . ?
C14 C13 C9 123.8(3) . . ?
O2 C14 C13 120.0(3) . . ?
O2 C14 C15 119.4(3) . . ?
C13 C14 C15 120.6(4) . . ?
C14 O2 Ti1 128.7(2) . . ?
C16 C15 C14 117.9(4) . . ?
C16 C15 C19 119.9(4) . . ?
C14 C15 C19 122.1(3) . . ?
C17 C16 C15 121.7(4) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C16 C17 C18 119.7(4) . . ?
C16 C17 H17 120.1 . . ?
C18 C17 H17 120.1 . . ?
C17 C18 C13 121.3(4) . . ?
C17 C18 H18 119.4 . . ?
C13 C18 H18 119.4 . . ?
C20 C19 C24 119.1(4) . . ?
C20 C19 C15 122.0(4) . . ?
C24 C19 C15 118.7(4) . . ?
C19 C20 C21 120.2(4) . . ?
C19 C20 H20 119.9 . . ?
C21 C20 H20 119.9 . . ?
C22 C21 C20 120.7(4) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.6 . . ?
C23 C22 C21 119.1(5) . . ?
C23 C22 H22 120.4 . . ?
C21 C22 H22 120.4 . . ?
C22 C23 C24 120.7(4) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C19 C24 C23 120.2(4) . . ?
C19 C24 H24 119.9 . . ?
C23 C24 H24 119.9 . . ?
C30 C25 C26 118.3(5) . . ?
C30 C25 C31 121.2(3) . . ?
C26 C25 C31 120.4(5) . . ?
C27 C26 C25 119.9(6) . . ?
C27 C26 H26 120.0 . . ?
C25 C26 H26 120.0 . . ?
C28 C27 C26 120.5(6) . . ?
C28 C27 H27 119.8 . . ?
C26 C27 H27 119.8 . . ?
C27 C28 C29 122.0(6) . . ?
C27 C28 H28 119.0 . . ?
C29 C28 H28 119.0 . . ?
C30 C29 C28 117.6(6) . . ?
C30 C29 H29 121.2 . . ?
C28 C29 H29 121.2 . . ?
C29 C30 C25 121.7(5) . . ?
C29 C30 H30 119.2 . . ?
C25 C30 H30 119.2 . . ?
C36 C31 C32 118.6(4) . . ?
C36 C31 C25 120.2(4) . . ?
C32 C31 C25 121.1(4) . . ?
O3 C32 C33 121.3(3) . . ?
O3 C32 C31 117.7(4) . . ?
C33 C32 C31 121.0(3) . . ?
C32 O3 Ti1 138.0(2) . . ?
C32 C33 C34 117.3(4) . . ?
C32 C33 C37 126.0(3) . . ?
C34 C33 C37 116.4(4) . . ?
C35 C34 C33 122.0(5) . . ?
C35 C34 H34 119.0 . . ?
C33 C34 H34 119.0 . . ?
C36 C35 C34 118.9(4) . . ?
C36 C35 H35 120.5 . . ?
C34 C35 H35 120.5 . . ?
C35 C36 C31 121.9(4) . . ?
C35 C36 H36 119.0 . . ?
C31 C36 H36 119.0 . . ?
C42 C37 C38 118.7(4) . . ?
C42 C37 C33 116.7(3) . . ?
C38 C37 C33 124.6(3) . . ?
O4 C38 C39 119.6(3) . . ?
O4 C38 C37 121.5(3) . . ?
C39 C38 C37 118.8(3) . . ?
C38 O4 Ti1 131.9(2) . . ?
C40 C39 C38 120.4(4) . . ?
C40 C39 C43 118.1(4) . . ?
C38 C39 C43 121.5(3) . . ?
C41 C40 C39 120.1(4) . . ?
C41 C40 H40 119.9 . . ?
C39 C40 H40 119.9 . . ?
C42 C41 C40 120.2(4) . . ?
C42 C41 H41 119.9 . . ?
C40 C41 H41 119.9 . . ?
C41 C42 C37 121.7(4) . . ?
C41 C42 H42 119.1 . . ?
C37 C42 H42 119.1 . . ?
C48 C43 C44 117.0(4) . . ?
C48 C43 C39 122.7(4) . . ?
C44 C43 C39 120.3(4) . . ?
C43 C44 C45 122.1(5) . . ?
C43 C44 H44 119.0 . . ?
C45 C44 H44 119.0 . . ?
C44 C45 C46 119.3(5) . . ?
C44 C45 H45 120.3 . . ?
C46 C45 H45 120.3 . . ?
C47 C46 C45 118.9(4) . . ?
C47 C46 H46 120.6 . . ?
C45 C46 H46 120.6 . . ?
C46 C47 C48 121.4(5) . . ?
C46 C47 H47 119.3 . . ?
C48 C47 H47 119.3 . . ?
C43 C48 C47 121.3(4) . . ?
C43 C48 H48 119.3 . . ?
C47 C48 H48 119.3 . . ?
C49 N1 C52 116.6(3) . . ?
C49 N1 Ti1 124.3(2) . . ?
C52 N1 Ti1 119.1(2) . . ?
N1 C49 C50 121.2(3) . . ?
N1 C49 H49 119.4 . . ?
C50 C49 H49 119.4 . . ?
C49 C50 C51 117.0(4) . . ?
C49 C50 H50 121.5 . . ?
C51 C50 H50 121.5 . . ?
N2 C51 C50 122.9(4) . . ?
N2 C51 H51 118.5 . . ?
C50 C51 H51 118.5 . . ?
C52 N2 C51 115.6(3) . . ?
N2 C52 N1 126.6(3) . . ?
N2 C52 C53 117.6(3) . . ?
N1 C52 C53 115.9(3) . . ?
N4 C53 N3 125.9(3) . . ?
N4 C53 C52 118.6(3) . . ?
N3 C53 C52 115.4(3) . . ?
C56 N3 C53 117.3(3) . . ?
C56 N3 Ti1 125.0(2) . . ?
C53 N3 Ti1 117.7(2) . . ?
C53 N4 C54 116.3(3) . . ?
N4 C54 C55 122.9(3) . . ?
N4 C54 H54 118.6 . . ?
C55 C54 H54 118.6 . . ?
C54 C55 C56 116.5(3) . . ?
C54 C55 C57 120.8(3) . . ?
C56 C55 C57 122.5(3) . . ?
N3 C56 C55 121.0(3) . . ?
N3 C56 H56 119.5 . . ?
C55 C56 H56 119.5 . . ?
N5 C57 C58 108.0(3) . . ?
N5 C57 C55 120.8(3) . . ?
C58 C57 C55 131.2(3) . . ?
N6 N5 C57 109.2(3) . . ?
N5 N6 N7 107.9(3) . . ?
N6 N7 C58 110.0(3) . . ?
N6 N7 C59 119.9(3) . . ?
C58 N7 C59 129.9(3) . . ?
N7 C58 C57 105.0(3) . . ?
N7 C58 H58 127.5 . . ?
C57 C58 H58 127.5 . . ?
N7 C59 C60 113.3(3) . . ?
N7 C59 H59A 108.9 . . ?
C60 C59 H59A 108.9 . . ?
N7 C59 H59B 108.9 . . ?
C60 C59 H59B 108.9 . . ?
H59A C59 H59B 107.7 . . ?
C61 C60 C65 120.3(3) . . ?
C61 C60 C59 123.0(3) . . ?
C65 C60 C59 116.7(3) . . ?
C60 C61 C62 119.8(4) . . ?
C60 C61 H61 120.1 . . ?
C62 C61 H61 120.1 . . ?
O5 C62 C63 115.3(4) . . ?
O5 C62 C61 125.0(4) . . ?
C63 C62 C61 119.7(4) . . ?
O6 C63 C62 119.6(3) . . ?
O6 C63 C64 120.1(3) . . ?
C62 C63 C64 120.2(3) . . ?
O7 C64 C65 124.9(3) . . ?
O7 C64 C63 115.5(3) . . ?
C65 C64 C63 119.6(3) . . ?
C64 C65 C60 120.3(3) . . ?
C64 C65 H65 119.8 . . ?
C60 C65 H65 119.8 . . ?
C62 O5 C66 116.6(4) . . ?
O5 C66 H66A 109.5 . . ?
O5 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
O5 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C63 O6 C67 116.2(3) . . ?
O6 C67 H67A 109.5 . . ?
O6 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
O6 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
C64 O7 C68 117.2(3) . . ?
O7 C68 H68A 109.5 . . ?
O7 C68 H68B 109.5 . . ?
H68A C68 H68B 109.5 . . ?
O7 C68 H68C 109.5 . . ?
H68A C68 H68C 109.5 . . ?
H68B C68 H68C 109.5 . . ?
Cl2 C69 Cl3 118.4(9) . . ?
Cl2 C69 Cl1 115.7(16) . . ?
Cl3 C69 Cl1 123.9(11) . . ?
Cl2 C69 H69 94.8 . . ?
Cl3 C69 H69 94.8 . . ?
Cl1 C69 H69 94.8 . . ?
C69 Cl1 Cl4 147.0(12) . . ?
Cl6 C70 Cl4 111.0(9) . . ?
Cl6 C70 Cl5 118.1(9) . . ?
Cl4 C70 Cl5 111.0(9) . . ?
Cl6 C70 H70 105.2 . . ?
Cl4 C70 H70 105.2 . . ?
Cl5 C70 H70 105.2 . . ?
C70 Cl4 Cl1 109.6(6) . . ?

_refine_diff_density_max         1.831
_refine_diff_density_min         -0.994
_refine_diff_density_rms         0.109

_shelxl_version_number           2014/6



