# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

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

data_e3568a_a
_database_code_depnum_ccdc_archive 'CCDC 2109006'
loop_
_audit_author_name
_audit_author_address
'Nathalie Kyritsakas'
;University of Strasbourg 
France
;
_audit_update_record             
;
2021-09-10 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C118 H88 N8 O14 Ti2), 3(C7 H8)'
_chemical_formula_sum            'C257 H200 N16 O28 Ti4'
_chemical_formula_weight         4151.92

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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.2859(6)
_cell_length_b                   22.1422(16)
_cell_length_c                   24.4996(17)
_cell_angle_alpha                93.9150(10)
_cell_angle_beta                 95.999(2)
_cell_angle_gamma                97.1670(10)
_cell_volume                     5487.2(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    39000
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             2166
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.214
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.975
_exptl_absorpt_correction_T_max  0.991
_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            23568
_diffrn_reflns_av_unetI/netI     0.1055
_diffrn_reflns_v_R_equivalents   0.060
_diffrn_reflns_av_R_equivalents  0.058
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_theta_min         1.303
_diffrn_reflns_theta_max         27.511
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measured_fraction_theta_full 0.955
_diffrn_reflns_Laue_measured_fraction_max 0.932
_diffrn_reflns_Laue_measured_fraction_full 0.955
_diffrn_reflns_point_group_measured_fraction_max 0.932
_diffrn_reflns_point_group_measured_fraction_full 0.955
_reflns_number_total             23568
_reflns_number_gt                14495
_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, 2014)'
_computing_structure_refinement  'SHELXL-2014/6 (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)+(0.1378P)²+1.1917P] 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         23568
_refine_ls_number_parameters     1401
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1326
_refine_ls_R_factor_gt           0.0829
_refine_ls_wR_factor_ref         0.2382
_refine_ls_wR_factor_gt          0.2142
_refine_ls_goodness_of_fit_ref   1.097
_refine_ls_restrained_S_all      1.097
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.045

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 0.69466(6) 0.54550(3) 0.75523(2) 0.01969(15) Uani 1 1 d . . . . .
Ti2 Ti 0.81864(6) 0.94189(3) 0.74878(2) 0.01959(15) Uani 1 1 d . . . . .
C1 C 0.6922(4) 0.36212(16) 0.70121(17) 0.0325(9) Uani 1 1 d . . . . .
C2 C 0.7146(5) 0.3451(2) 0.75491(19) 0.0451(11) Uani 1 1 d . . . . .
H2 H 0.6473 0.3456 0.7786 0.054 Uiso 1 1 calc R U . . .
C3 C 0.8352(5) 0.3273(2) 0.7737(2) 0.0505(13) Uani 1 1 d . . . . .
H3 H 0.8505 0.3163 0.8103 0.061 Uiso 1 1 calc R U . . .
C4 C 0.9325(5) 0.3256(2) 0.7392(2) 0.0537(13) Uani 1 1 d . . . . .
H4 H 1.0140 0.3124 0.7518 0.064 Uiso 1 1 calc R U . . .
C5 C 0.9110(5) 0.3432(3) 0.6864(3) 0.0667(16) Uani 1 1 d . . . . .
H5 H 0.9788 0.3433 0.6629 0.080 Uiso 1 1 calc R U . . .
C6 C 0.7901(5) 0.3607(2) 0.6677(2) 0.0533(13) Uani 1 1 d . . . . .
H6 H 0.7754 0.3718 0.6310 0.064 Uiso 1 1 calc R U . . .
C7 C 0.5621(4) 0.38079(16) 0.68144(16) 0.0327(9) Uani 1 1 d . . . . .
C8 C 0.5489(4) 0.44331(16) 0.68169(14) 0.0266(8) Uani 1 1 d . . . . .
O1 O 0.6577(2) 0.48317(11) 0.69719(10) 0.0260(6) Uani 1 1 d . . . . .
C9 C 0.4261(4) 0.46244(16) 0.66294(14) 0.0259(8) Uani 1 1 d . . . . .
C10 C 0.3208(4) 0.41700(18) 0.64644(17) 0.0356(9) Uani 1 1 d . . . . .
H10 H 0.2368 0.4285 0.6354 0.043 Uiso 1 1 calc R U . . .
C11 C 0.3341(5) 0.35513(19) 0.6455(2) 0.0460(12) Uani 1 1 d . . . . .
H11 H 0.2607 0.3252 0.6329 0.055 Uiso 1 1 calc R U . . .
C12 C 0.4538(5) 0.33761(18) 0.66303(19) 0.0428(11) Uani 1 1 d . . . . .
H12 H 0.4628 0.2954 0.6625 0.051 Uiso 1 1 calc R U . . .
C13 C 0.4076(4) 0.52724(16) 0.65495(14) 0.0249(8) Uani 1 1 d . . . . .
C14 C 0.4533(3) 0.57814(16) 0.69250(14) 0.0214(7) Uani 1 1 d . . . . .
O2 O 0.5317(2) 0.57155(10) 0.73940(9) 0.0220(5) Uani 1 1 d . . . . .
C15 C 0.4188(3) 0.63673(15) 0.68272(14) 0.0225(7) Uani 1 1 d . . . . .
C16 C 0.3366(4) 0.64245(17) 0.63435(15) 0.0279(8) Uani 1 1 d . . . . .
H16 H 0.3101 0.6811 0.6277 0.033 Uiso 1 1 calc R U . . .
C17 C 0.2938(4) 0.59361(18) 0.59648(15) 0.0311(9) Uani 1 1 d . . . . .
H17 H 0.2402 0.5988 0.5636 0.037 Uiso 1 1 calc R U . . .
C18 C 0.3290(4) 0.53674(17) 0.60644(15) 0.0299(8) Uani 1 1 d . . . . .
H18 H 0.2994 0.5032 0.5799 0.036 Uiso 1 1 calc R U . . .
C19 C 0.4624(3) 0.69304(16) 0.72068(14) 0.0234(7) Uani 1 1 d . . . . .
C20 C 0.4850(4) 0.69300(17) 0.77776(16) 0.0315(9) Uani 1 1 d . . . . .
H20 H 0.4816 0.6552 0.7940 0.038 Uiso 1 1 calc R U . . .
C21 C 0.5125(4) 0.74717(17) 0.81139(16) 0.0309(9) Uani 1 1 d . . . . .
H21 H 0.5273 0.7453 0.8501 0.037 Uiso 1 1 calc R U . . .
C22 C 0.5189(3) 0.80434(16) 0.79012(15) 0.0242(7) Uani 1 1 d . . . . .
C23 C 0.5024(4) 0.80419(17) 0.73262(15) 0.0305(8) Uani 1 1 d . . . . .
H23 H 0.5100 0.8419 0.7161 0.037 Uiso 1 1 calc R U . . .
C24 C 0.4753(4) 0.75004(17) 0.69955(15) 0.0302(8) Uani 1 1 d . . . . .
H24 H 0.4649 0.7517 0.6607 0.036 Uiso 1 1 calc R U . . .
C25 C 0.5340(4) 0.86068(16) 0.82772(14) 0.0244(8) Uani 1 1 d . . . . .
C26 C 0.5986(3) 0.91811(16) 0.81639(14) 0.0240(8) Uani 1 1 d . . . . .
O3 O 0.6496(2) 0.92248(11) 0.76750(9) 0.0229(5) Uani 1 1 d . . . . .
C27 C 0.6084(4) 0.96996(16) 0.85368(15) 0.0265(8) Uani 1 1 d . . . . .
C28 C 0.5540(4) 0.96302(18) 0.90373(16) 0.0334(9) Uani 1 1 d . . . . .
H28 H 0.5616 0.9973 0.9299 0.040 Uiso 1 1 calc R U . . .
C29 C 0.4896(4) 0.90753(19) 0.91567(16) 0.0356(9) Uani 1 1 d . . . . .
H29 H 0.4523 0.9040 0.9494 0.043 Uiso 1 1 calc R U . . .
C30 C 0.4801(4) 0.85706(18) 0.87783(16) 0.0319(9) Uani 1 1 d . . . . .
H30 H 0.4360 0.8191 0.8861 0.038 Uiso 1 1 calc R U . . .
C31 C 0.6660(4) 1.03321(17) 0.84443(14) 0.0280(8) Uani 1 1 d . . . . .
C32 C 0.7860(4) 1.04742(16) 0.82284(14) 0.0268(8) Uani 1 1 d . . . . .
O4 O 0.8582(2) 1.00385(10) 0.80721(10) 0.0252(5) Uani 1 1 d . . . . .
C33 C 0.8403(4) 1.10901(17) 0.81970(16) 0.0317(9) Uani 1 1 d . . . . .
C34 C 0.7718(4) 1.15549(18) 0.83836(18) 0.0393(10) Uani 1 1 d . . . . .
H34 H 0.8064 1.1969 0.8358 0.047 Uiso 1 1 calc R U . . .
C35 C 0.6544(5) 1.14208(18) 0.86042(18) 0.0422(11) Uani 1 1 d . . . . .
H35 H 0.6097 1.1741 0.8737 0.051 Uiso 1 1 calc R U . . .
C36 C 0.6022(4) 1.08191(18) 0.86314(17) 0.0348(9) Uani 1 1 d . . . . .
H36 H 0.5209 1.0732 0.8781 0.042 Uiso 1 1 calc R U . . .
C37 C 0.9670(4) 1.12393(16) 0.79608(17) 0.0353(9) Uani 1 1 d . . . . .
C38 C 1.0829(5) 1.1049(2) 0.8198(2) 0.0483(12) Uani 1 1 d . . . . .
H38 H 1.0812 1.0808 0.8505 0.058 Uiso 1 1 calc R U . . .
C39 C 1.2008(5) 1.1215(2) 0.7983(2) 0.0560(14) Uani 1 1 d . . . . .
H39 H 1.2797 1.1091 0.8150 0.067 Uiso 1 1 calc R U . . .
C40 C 1.2058(5) 1.1551(2) 0.7538(2) 0.0550(14) Uani 1 1 d . . . . .
H40 H 1.2872 1.1659 0.7395 0.066 Uiso 1 1 calc R U . . .
C41 C 1.0923(5) 1.1732(2) 0.7299(2) 0.0554(13) Uani 1 1 d . . . . .
H41 H 1.0947 1.1963 0.6986 0.066 Uiso 1 1 calc R U . . .
C42 C 0.9728(5) 1.15782(19) 0.75122(19) 0.0442(11) Uani 1 1 d . . . . .
H42 H 0.8947 1.1709 0.7345 0.053 Uiso 1 1 calc R U . . .
C43 C 0.5040(4) 0.40946(17) 0.85811(16) 0.0289(8) Uani 1 1 d . . . . .
C44 C 0.4192(4) 0.42187(18) 0.81337(16) 0.0311(9) Uani 1 1 d . . . . .
H44 H 0.4198 0.4626 0.8035 0.037 Uiso 1 1 calc R U . . .
C45 C 0.3342(4) 0.37530(19) 0.78328(19) 0.0402(10) Uani 1 1 d . . . . .
H45 H 0.2748 0.3844 0.7535 0.048 Uiso 1 1 calc R U . . .
C46 C 0.3349(5) 0.3158(2) 0.7962(2) 0.0513(12) Uani 1 1 d . . . . .
H46 H 0.2780 0.2838 0.7747 0.062 Uiso 1 1 calc R U . . .
C47 C 0.4170(5) 0.3026(2) 0.8399(2) 0.0522(13) Uani 1 1 d . . . . .
H47 H 0.4172 0.2616 0.8487 0.063 Uiso 1 1 calc R U . . .
C48 C 0.4998(4) 0.34881(19) 0.8712(2) 0.0405(10) Uani 1 1 d . . . . .
H48 H 0.5548 0.3393 0.9021 0.049 Uiso 1 1 calc R U . . .
C49 C 0.5957(4) 0.45869(17) 0.89266(15) 0.0284(8) Uani 1 1 d . . . . .
C50 C 0.6845(4) 0.50001(16) 0.86866(14) 0.0238(8) Uani 1 1 d . . . . .
O5 O 0.6802(2) 0.49583(10) 0.81305(9) 0.0228(5) Uani 1 1 d . . . . .
C51 C 0.7795(4) 0.54147(17) 0.90341(14) 0.0269(8) Uani 1 1 d . . . . .
C52 C 0.7714(4) 0.5433(2) 0.96018(16) 0.0375(10) Uani 1 1 d . . . . .
H52 H 0.8297 0.5729 0.9839 0.045 Uiso 1 1 calc R U . . .
C53 C 0.6816(5) 0.5035(2) 0.98290(17) 0.0446(11) Uani 1 1 d . . . . .
H53 H 0.6785 0.5057 1.0216 0.054 Uiso 1 1 calc R U . . .
C54 C 0.5975(4) 0.4609(2) 0.94925(17) 0.0396(10) Uani 1 1 d . . . . .
H54 H 0.5390 0.4322 0.9650 0.047 Uiso 1 1 calc R U . . .
C55 C 0.8946(4) 0.58025(16) 0.88634(14) 0.0270(8) Uani 1 1 d . . . . .
C56 C 0.8894(4) 0.61551(15) 0.84074(14) 0.0233(7) Uani 1 1 d . . . . .
O6 O 0.7773(2) 0.61132(10) 0.80615(10) 0.0236(5) Uani 1 1 d . . . . .
C57 C 1.0022(4) 0.65619(16) 0.83081(15) 0.0266(8) Uani 1 1 d . . . . .
C58 C 1.1186(4) 0.65798(19) 0.86686(18) 0.0373(10) Uani 1 1 d . . . . .
H58 H 1.1948 0.6846 0.8610 0.045 Uiso 1 1 calc R U . . .
C59 C 1.1249(4) 0.6220(2) 0.91054(17) 0.0388(10) Uani 1 1 d . . . . .
H59 H 1.2047 0.6237 0.9342 0.047 Uiso 1 1 calc R U . . .
C60 C 1.0141(4) 0.58320(19) 0.91972(16) 0.0344(9) Uani 1 1 d . . . . .
H60 H 1.0197 0.5580 0.9495 0.041 Uiso 1 1 calc R U . . .
C61 C 0.9999(4) 0.69813(16) 0.78647(16) 0.0291(8) Uani 1 1 d . . . . .
C62 C 1.1155(4) 0.71889(16) 0.76454(16) 0.0302(8) Uani 1 1 d . . . . .
H62 H 1.1947 0.7034 0.7766 0.036 Uiso 1 1 calc R U . . .
C63 C 1.1181(4) 0.76152(17) 0.72570(18) 0.0356(9) Uani 1 1 d . . . . .
H63 H 1.1990 0.7749 0.7120 0.043 Uiso 1 1 calc R U . . .
C64 C 1.0032(4) 0.78537(16) 0.70613(16) 0.0293(8) Uani 1 1 d . . . . .
C65 C 0.8862(4) 0.76335(16) 0.72733(16) 0.0280(8) Uani 1 1 d . . . . .
H65 H 0.8062 0.7777 0.7144 0.034 Uiso 1 1 calc R U . . .
C66 C 0.8845(4) 0.72145(16) 0.76648(16) 0.0281(8) Uani 1 1 d . . . . .
H66 H 0.8037 0.7081 0.7803 0.034 Uiso 1 1 calc R U . . .
C67 C 1.0089(4) 0.82950(16) 0.66341(16) 0.0292(8) Uani 1 1 d . . . . .
C68 C 0.9168(4) 0.87283(15) 0.65753(15) 0.0257(8) Uani 1 1 d . . . . .
O7 O 0.8275(2) 0.87745(10) 0.69404(10) 0.0236(5) Uani 1 1 d . . . . .
C69 C 0.9200(4) 0.91111(16) 0.61411(14) 0.0272(8) Uani 1 1 d . . . . .
C70 C 1.0185(4) 0.90824(18) 0.57902(16) 0.0351(9) Uani 1 1 d . . . . .
H70 H 1.0229 0.9349 0.5503 0.042 Uiso 1 1 calc R U . . .
C71 C 1.1104(4) 0.8672(2) 0.58517(18) 0.0427(10) Uani 1 1 d . . . . .
H71 H 1.1772 0.8661 0.5612 0.051 Uiso 1 1 calc R U . . .
C72 C 1.1025(4) 0.82821(19) 0.62668(18) 0.0389(10) Uani 1 1 d . . . . .
H72 H 1.1634 0.7994 0.6302 0.047 Uiso 1 1 calc R U . . .
C73 C 0.8197(4) 0.95268(17) 0.60054(15) 0.0295(8) Uani 1 1 d . . . . .
C74 C 0.7718(4) 0.99268(16) 0.63886(14) 0.0258(8) Uani 1 1 d . . . . .
O8 O 0.8054(2) 0.99466(10) 0.69367(9) 0.0244(5) Uani 1 1 d . . . . .
C75 C 0.6919(4) 1.03618(18) 0.61946(16) 0.0333(9) Uani 1 1 d . . . . .
C76 C 0.6555(5) 1.0367(2) 0.56276(18) 0.0471(12) Uani 1 1 d . . . . .
H76 H 0.6015 1.0658 0.5499 0.057 Uiso 1 1 calc R U . . .
C77 C 0.6963(5) 0.9960(2) 0.52563(17) 0.0507(12) Uani 1 1 d . . . . .
H77 H 0.6697 0.9963 0.4873 0.061 Uiso 1 1 calc R U . . .
C78 C 0.7773(5) 0.9544(2) 0.54480(16) 0.0413(10) Uani 1 1 d . . . . .
H78 H 0.8048 0.9261 0.5189 0.050 Uiso 1 1 calc R U . . .
C79 C 0.6512(4) 1.08326(17) 0.65745(16) 0.0313(9) Uani 1 1 d . . . . .
C80 C 0.5753(4) 1.06854(18) 0.69937(16) 0.0341(9) Uani 1 1 d . . . . .
H80 H 0.5541 1.0270 0.7063 0.041 Uiso 1 1 calc R U . . .
C81 C 0.5300(4) 1.1140(2) 0.73130(18) 0.0407(10) Uani 1 1 d . . . . .
H81 H 0.4753 1.1033 0.7590 0.049 Uiso 1 1 calc R U . . .
C82 C 0.5642(5) 1.1751(2) 0.7228(2) 0.0464(12) Uani 1 1 d . . . . .
H82 H 0.5346 1.2064 0.7450 0.056 Uiso 1 1 calc R U . . .
C83 C 0.6415(5) 1.1898(2) 0.6820(2) 0.0539(13) Uani 1 1 d . . . . .
H83 H 0.6657 1.2314 0.6760 0.065 Uiso 1 1 calc R U . . .
C84 C 0.6839(5) 1.14484(19) 0.6498(2) 0.0454(11) Uani 1 1 d . . . . .
H84 H 0.7369 1.1559 0.6215 0.054 Uiso 1 1 calc R U . . .
N1 N 0.9010(3) 0.52674(13) 0.74858(11) 0.0236(6) Uani 1 1 d . . . . .
C85 C 0.9577(4) 0.48853(16) 0.78037(15) 0.0279(8) Uani 1 1 d . . . . .
H85 H 0.9067 0.4659 0.8041 0.033 Uiso 1 1 calc R U . . .
C86 C 1.0899(4) 0.48102(19) 0.77958(17) 0.0388(10) Uani 1 1 d . . . . .
H86 H 1.1286 0.4539 0.8028 0.047 Uiso 1 1 calc R U . . .
C87 C 1.1639(4) 0.5130(2) 0.74514(19) 0.0433(11) Uani 1 1 d . . . . .
H87 H 1.2546 0.5087 0.7447 0.052 Uiso 1 1 calc R U . . .
C88 C 1.1047(4) 0.55171(19) 0.71078(17) 0.0373(10) Uani 1 1 d . . . . .
H88 H 1.1535 0.5738 0.6860 0.045 Uiso 1 1 calc R U . . .
C89 C 0.9736(4) 0.55735(16) 0.71357(14) 0.0264(8) Uani 1 1 d . . . . .
C90 C 0.9016(4) 0.59712(16) 0.68055(14) 0.0260(8) Uani 1 1 d . . . . .
N2 N 0.7733(3) 0.60149(13) 0.68915(12) 0.0256(7) Uani 1 1 d . . . . .
N3 N 0.7229(3) 0.63889(14) 0.65614(13) 0.0313(7) Uani 1 1 d . . . . .
N4 N 0.8204(3) 0.65781(15) 0.62541(13) 0.0315(7) Uani 1 1 d . . . . .
C91 C 0.9321(4) 0.63379(18) 0.63949(15) 0.0313(9) Uani 1 1 d . . . . .
H91 H 1.0135 0.6407 0.6244 0.038 Uiso 1 1 calc R U . . .
C92 C 0.8062(5) 0.7054(2) 0.5864(2) 0.0488(12) Uani 1 1 d . . . . .
H92A H 0.8587 0.6976 0.5557 0.059 Uiso 1 1 calc R U . . .
H92B H 0.8432 0.7456 0.6056 0.059 Uiso 1 1 calc R U . . .
C93 C 0.6649(4) 0.7080(2) 0.56303(16) 0.0375(10) Uani 1 1 d . . . . .
C94 C 0.5940(4) 0.6601(2) 0.52975(17) 0.0392(10) Uani 1 1 d . . . . .
H94 H 0.6318 0.6238 0.5228 0.047 Uiso 1 1 calc R U . . .
C95 C 0.4673(4) 0.6647(2) 0.50634(16) 0.0382(10) Uani 1 1 d . . . . .
C96 C 0.4117(5) 0.7176(2) 0.5184(2) 0.0465(11) Uani 1 1 d . . . . .
C97 C 0.4839(5) 0.7656(2) 0.55146(19) 0.0468(11) Uani 1 1 d . . . . .
C98 C 0.6116(5) 0.7615(2) 0.57396(17) 0.0424(11) Uani 1 1 d . . . . .
H98 H 0.6618 0.7947 0.5965 0.051 Uiso 1 1 calc R U . . .
O9 O 0.3885(3) 0.62087(14) 0.47205(13) 0.0478(8) Uani 1 1 d . . . . .
C99 C 0.4387(6) 0.5647(2) 0.4611(2) 0.0570(13) Uani 1 1 d . . . . .
H99A H 0.5220 0.5727 0.4451 0.086 Uiso 1 1 calc R U . . .
H99B H 0.3747 0.5376 0.4352 0.086 Uiso 1 1 calc R U . . .
H99C H 0.4540 0.5453 0.4956 0.086 Uiso 1 1 calc R U . . .
O10 O 0.2813(4) 0.71956(17) 0.49864(17) 0.0687(11) Uani 1 1 d . . . . .
C100 C 0.2724(8) 0.7529(3) 0.4526(3) 0.099(3) Uani 1 1 d . . . . .
H10A H 0.2981 0.7964 0.4640 0.149 Uiso 1 1 calc R U . . .
H10B H 0.1815 0.7464 0.4347 0.149 Uiso 1 1 calc R U . . .
H10C H 0.3315 0.7394 0.4267 0.149 Uiso 1 1 calc R U . . .
O11 O 0.4178(4) 0.81438(16) 0.56211(18) 0.0687(11) Uani 1 1 d . . . . .
C101 C 0.4913(6) 0.8693(2) 0.5897(3) 0.0704(17) Uani 1 1 d . . . . .
H10D H 0.5296 0.8609 0.6263 0.106 Uiso 1 1 calc R U . . .
H10E H 0.4325 0.9005 0.5935 0.106 Uiso 1 1 calc R U . . .
H10F H 0.5621 0.8841 0.5681 0.106 Uiso 1 1 calc R U . . .
N5 N 1.0378(3) 0.95110(13) 0.75376(12) 0.0237(6) Uani 1 1 d . . . . .
C102 C 1.1051(4) 0.98856(17) 0.72289(16) 0.0323(9) Uani 1 1 d . . . . .
H102 H 1.0588 1.0150 0.7015 0.039 Uiso 1 1 calc R U . . .
C103 C 1.2394(4) 0.9903(2) 0.72090(18) 0.0389(10) Uani 1 1 d . . . . .
H103 H 1.2841 1.0168 0.6979 0.047 Uiso 1 1 calc R U . . .
C104 C 1.3072(4) 0.9530(2) 0.75289(19) 0.0451(12) Uani 1 1 d . . . . .
H104 H 1.3994 0.9533 0.7521 0.054 Uiso 1 1 calc R U . . .
C105 C 1.2402(4) 0.9152(2) 0.78594(18) 0.0415(11) Uani 1 1 d . . . . .
H105 H 1.2855 0.8898 0.8088 0.050 Uiso 1 1 calc R U . . .
C106 C 1.1056(4) 0.91515(17) 0.78525(14) 0.0263(8) Uani 1 1 d . . . . .
C107 C 1.0232(4) 0.87714(16) 0.81837(14) 0.0252(8) Uani 1 1 d . . . . .
N6 N 0.8904(3) 0.87911(13) 0.81288(12) 0.0237(6) Uani 1 1 d . . . . .
N7 N 0.8336(3) 0.84364(14) 0.84676(12) 0.0268(7) Uani 1 1 d . . . . .
N8 N 0.9305(3) 0.81887(14) 0.87457(12) 0.0256(7) Uani 1 1 d . . . . .
C108 C 1.0485(4) 0.83750(17) 0.85785(15) 0.0283(8) Uani 1 1 d . . . . .
H108 H 1.1314 0.8258 0.8706 0.034 Uiso 1 1 calc R U . . .
C109 C 0.9054(4) 0.77217(19) 0.91359(17) 0.0379(10) Uani 1 1 d . . . . .
H10G H 0.9806 0.7774 0.9430 0.045 Uiso 1 1 calc R U . . .
H10H H 0.9035 0.7315 0.8938 0.045 Uiso 1 1 calc R U . . .
C110 C 0.7797(4) 0.77246(18) 0.94055(15) 0.0324(9) Uani 1 1 d . . . . .
C111 C 0.6904(4) 0.71933(19) 0.93478(17) 0.0350(9) Uani 1 1 d . . . . .
H111 H 0.7056 0.6849 0.9122 0.042 Uiso 1 1 calc R U . . .
C112 C 0.5780(4) 0.71678(19) 0.96241(16) 0.0362(9) Uani 1 1 d . . . . .
C113 C 0.5582(4) 0.76663(19) 0.99668(17) 0.0366(9) Uani 1 1 d . . . . .
C114 C 0.6475(4) 0.81963(19) 1.00239(16) 0.0348(9) Uani 1 1 d . . . . .
C115 C 0.7593(4) 0.82343(19) 0.97384(16) 0.0343(9) Uani 1 1 d . . . . .
H115 H 0.8199 0.8599 0.9771 0.041 Uiso 1 1 calc R U . . .
O12 O 0.4812(3) 0.66747(14) 0.95826(15) 0.0529(8) Uani 1 1 d . . . . .
C116 C 0.4899(5) 0.6175(2) 0.9201(2) 0.0483(11) Uani 1 1 d . . . . .
H11A H 0.5044 0.6325 0.8842 0.072 Uiso 1 1 calc R U . . .
H11B H 0.4077 0.5892 0.9164 0.072 Uiso 1 1 calc R U . . .
H11C H 0.5638 0.5963 0.9332 0.072 Uiso 1 1 calc R U . . .
O13 O 0.4515(3) 0.76275(15) 1.02693(13) 0.0473(8) Uani 1 1 d . . . . .
C117 C 0.3382(5) 0.7812(3) 1.0002(2) 0.0604(14) Uani 1 1 d . . . . .
H11D H 0.3580 0.8233 0.9907 0.091 Uiso 1 1 calc R U . . .
H11E H 0.2684 0.7787 1.0246 0.091 Uiso 1 1 calc R U . . .
H11F H 0.3087 0.7544 0.9665 0.091 Uiso 1 1 calc R U . . .
O14 O 0.6181(3) 0.86608(14) 1.03680(12) 0.0447(7) Uani 1 1 d . . . . .
C118 C 0.7103(5) 0.9212(2) 1.0439(2) 0.0532(12) Uani 1 1 d . . . . .
H11G H 0.7958 0.9125 1.0609 0.080 Uiso 1 1 calc R U . . .
H11H H 0.6772 0.9518 1.0678 0.080 Uiso 1 1 calc R U . . .
H11I H 0.7206 0.9369 1.0080 0.080 Uiso 1 1 calc R U . . .
C119 C 0.0632(5) 0.3036(2) 0.91192(19) 0.0443(11) Uani 1 1 d . . . . .
C120 C -0.0585(6) 0.2953(2) 0.9303(2) 0.0566(13) Uani 1 1 d . . . . .
H120 H -0.0950 0.2556 0.9376 0.068 Uiso 1 1 calc R U . . .
C121 C -0.1301(6) 0.3439(3) 0.9384(2) 0.0642(15) Uani 1 1 d . . . . .
H121 H -0.2134 0.3375 0.9521 0.077 Uiso 1 1 calc R U . . .
C122 C -0.0796(6) 0.4010(3) 0.9265(2) 0.0625(15) Uani 1 1 d . . . . .
H122 H -0.1298 0.4339 0.9305 0.075 Uiso 1 1 calc R U . . .
C123 C 0.0444(6) 0.4113(2) 0.90848(19) 0.0557(14) Uani 1 1 d . . . . .
H123 H 0.0798 0.4513 0.9013 0.067 Uiso 1 1 calc R U . . .
C124 C 0.1155(5) 0.3634(2) 0.90112(18) 0.0475(11) Uani 1 1 d . . . . .
H124 H 0.2002 0.3704 0.8887 0.057 Uiso 1 1 calc R U . . .
C125 C 0.1359(6) 0.2502(2) 0.9025(2) 0.0646(15) Uani 1 1 d . . . . .
H12A H 0.0933 0.2149 0.9190 0.097 Uiso 1 1 calc R U . . .
H12B H 0.2273 0.2603 0.9195 0.097 Uiso 1 1 calc R U . . .
H12C H 0.1350 0.2403 0.8628 0.097 Uiso 1 1 calc R U . . .
C126 C 0.8539(10) 0.8123(3) 0.4390(3) 0.0653(15) Uani 0.5 1 d G . P . .
C127 C 0.7237(9) 0.8214(3) 0.4250(3) 0.0653(15) Uani 0.5 1 d G . P . .
H127 H 0.6540 0.7903 0.4292 0.078 Uiso 0.5 1 calc R U P . .
C128 C 0.6955(7) 0.8761(4) 0.4048(3) 0.0653(15) Uani 0.5 1 d G . P . .
H128 H 0.6066 0.8823 0.3952 0.078 Uiso 0.5 1 calc R U P . .
C129 C 0.7976(10) 0.9216(3) 0.3987(3) 0.0653(15) Uani 0.5 1 d G . P . .
H129 H 0.7783 0.9590 0.3849 0.078 Uiso 0.5 1 calc R U P . .
C130 C 0.9277(8) 0.9126(3) 0.4127(3) 0.0653(15) Uani 0.5 1 d G . P . .
H130 H 0.9975 0.9437 0.4085 0.078 Uiso 0.5 1 calc R U P . .
C131 C 0.9559(8) 0.8579(4) 0.4329(3) 0.0653(15) Uani 0.5 1 d G . P . .
H131 H 1.0449 0.8517 0.4425 0.078 Uiso 0.5 1 calc R U P . .
C132 C 0.8932(16) 0.7587(6) 0.4584(4) 0.0653(15) Uani 0.5 1 d . . P . .
H13A H 0.8151 0.7298 0.4624 0.098 Uiso 0.5 1 calc R U P . .
H13B H 0.9465 0.7682 0.4942 0.098 Uiso 0.5 1 calc R U P . .
H13C H 0.9457 0.7404 0.4322 0.098 Uiso 0.5 1 calc R U 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 O2 1.851(2) . ?
Ti1 O5 1.859(2) . ?
Ti1 O1 1.886(2) . ?
Ti1 O6 1.904(2) . ?
Ti1 N1 2.233(3) . ?
Ti1 N2 2.261(3) . ?
Ti2 O3 1.851(3) . ?
Ti2 O8 1.850(2) . ?
Ti2 O4 1.889(2) . ?
Ti2 O7 1.908(2) . ?
Ti2 N5 2.227(3) . ?
Ti2 N6 2.292(3) . ?
C1 C6 1.367(6) . ?
C1 C2 1.397(6) . ?
C1 C7 1.492(5) . ?
C2 C3 1.390(6) . ?
C2 H2 0.9500 . ?
C3 C4 1.377(8) . ?
C3 H3 0.9500 . ?
C4 C5 1.380(8) . ?
C4 H4 0.9500 . ?
C5 C6 1.391(7) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.389(6) . ?
C7 C8 1.407(5) . ?
C8 O1 1.340(4) . ?
C8 C9 1.423(5) . ?
C9 C10 1.389(5) . ?
C9 C13 1.494(5) . ?
C10 C11 1.393(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.372(6) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C14 1.405(5) . ?
C13 C18 1.409(5) . ?
C14 O2 1.361(4) . ?
C14 C15 1.416(5) . ?
C15 C16 1.404(5) . ?
C15 C19 1.495(5) . ?
C16 C17 1.372(5) . ?
C16 H16 0.9500 . ?
C17 C18 1.383(5) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.393(5) . ?
C19 C20 1.393(5) . ?
C20 C21 1.389(5) . ?
C20 H20 0.9500 . ?
C21 C22 1.398(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.401(5) . ?
C22 C25 1.481(5) . ?
C23 C24 1.382(5) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.402(5) . ?
C25 C26 1.418(5) . ?
C26 O3 1.361(4) . ?
C26 C27 1.404(5) . ?
C27 C28 1.410(5) . ?
C27 C31 1.493(5) . ?
C28 C29 1.386(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.390(6) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C32 1.402(6) . ?
C31 C36 1.406(5) . ?
C32 O4 1.347(4) . ?
C32 C33 1.418(5) . ?
C33 C34 1.396(5) . ?
C33 C37 1.490(6) . ?
C34 C35 1.381(7) . ?
C34 H34 0.9500 . ?
C35 C36 1.382(6) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.375(6) . ?
C37 C38 1.397(6) . ?
C38 C39 1.390(7) . ?
C38 H38 0.9500 . ?
C39 C40 1.363(8) . ?
C39 H39 0.9500 . ?
C40 C41 1.368(7) . ?
C40 H40 0.9500 . ?
C41 C42 1.398(7) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C44 1.393(5) . ?
C43 C48 1.398(5) . ?
C43 C49 1.498(5) . ?
C44 C45 1.381(6) . ?
C44 H44 0.9500 . ?
C45 C46 1.377(6) . ?
C45 H45 0.9500 . ?
C46 C47 1.363(7) . ?
C46 H46 0.9500 . ?
C47 C48 1.377(7) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C54 1.382(5) . ?
C49 C50 1.412(5) . ?
C50 O5 1.355(4) . ?
C50 C51 1.421(5) . ?
C51 C52 1.400(5) . ?
C51 C55 1.488(5) . ?
C52 C53 1.383(6) . ?
C52 H52 0.9500 . ?
C53 C54 1.362(6) . ?
C53 H53 0.9500 . ?
C54 H54 0.9500 . ?
C55 C60 1.395(5) . ?
C55 C56 1.406(5) . ?
C56 O6 1.348(4) . ?
C56 C57 1.430(5) . ?
C57 C58 1.407(5) . ?
C57 C61 1.477(5) . ?
C58 C59 1.379(6) . ?
C58 H58 0.9500 . ?
C59 C60 1.386(6) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 C62 1.395(6) . ?
C61 C66 1.408(5) . ?
C62 C63 1.385(6) . ?
C62 H62 0.9500 . ?
C63 C64 1.406(5) . ?
C63 H63 0.9500 . ?
C64 C65 1.406(5) . ?
C64 C67 1.480(5) . ?
C65 C66 1.379(5) . ?
C65 H65 0.9500 . ?
C66 H66 0.9500 . ?
C67 C72 1.387(6) . ?
C67 C68 1.433(5) . ?
C68 O7 1.356(4) . ?
C68 C69 1.405(5) . ?
C69 C70 1.401(5) . ?
C69 C73 1.493(5) . ?
C70 C71 1.394(6) . ?
C70 H70 0.9500 . ?
C71 C72 1.381(6) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?
C73 C78 1.394(5) . ?
C73 C74 1.415(5) . ?
C74 O8 1.347(4) . ?
C74 C75 1.416(5) . ?
C75 C76 1.402(6) . ?
C75 C79 1.479(5) . ?
C76 C77 1.370(7) . ?
C76 H76 0.9500 . ?
C77 C78 1.391(6) . ?
C77 H77 0.9500 . ?
C78 H78 0.9500 . ?
C79 C80 1.386(6) . ?
C79 C84 1.394(5) . ?
C80 C81 1.388(6) . ?
C80 H80 0.9500 . ?
C81 C82 1.392(6) . ?
C81 H81 0.9500 . ?
C82 C83 1.373(7) . ?
C82 H82 0.9500 . ?
C83 C84 1.370(7) . ?
C83 H83 0.9500 . ?
C84 H84 0.9500 . ?
N1 C85 1.335(4) . ?
N1 C89 1.356(5) . ?
C85 C86 1.393(6) . ?
C85 H85 0.9500 . ?
C86 C87 1.368(6) . ?
C86 H86 0.9500 . ?
C87 C88 1.392(5) . ?
C87 H87 0.9500 . ?
C88 C89 1.378(6) . ?
C88 H88 0.9500 . ?
C89 C90 1.454(5) . ?
C90 N2 1.372(5) . ?
C90 C91 1.372(5) . ?
N2 N3 1.311(4) . ?
N3 N4 1.358(5) . ?
N4 C91 1.348(5) . ?
N4 C92 1.479(5) . ?
C91 H91 0.9500 . ?
C92 C93 1.516(6) . ?
C92 H92A 0.9900 . ?
C92 H92B 0.9900 . ?
C93 C94 1.374(6) . ?
C93 C98 1.386(6) . ?
C94 C95 1.386(6) . ?
C94 H94 0.9500 . ?
C95 O9 1.361(5) . ?
C95 C96 1.393(6) . ?
C96 C97 1.378(7) . ?
C96 O10 1.385(6) . ?
C97 O11 1.370(6) . ?
C97 C98 1.387(6) . ?
C98 H98 0.9500 . ?
O9 C99 1.423(6) . ?
C99 H99A 0.9800 . ?
C99 H99B 0.9800 . ?
C99 H99C 0.9800 . ?
O10 C100 1.390(7) . ?
C100 H10A 0.9800 . ?
C100 H10B 0.9800 . ?
C100 H10C 0.9800 . ?
O11 C101 1.435(6) . ?
C101 H10D 0.9800 . ?
C101 H10E 0.9800 . ?
C101 H10F 0.9800 . ?
N5 C102 1.338(5) . ?
N5 C106 1.351(4) . ?
C102 C103 1.383(6) . ?
C102 H102 0.9500 . ?
C103 C104 1.380(6) . ?
C103 H103 0.9500 . ?
C104 C105 1.376(6) . ?
C104 H104 0.9500 . ?
C105 C106 1.382(6) . ?
C105 H105 0.9500 . ?
C106 C107 1.464(5) . ?
C107 N6 1.365(5) . ?
C107 C108 1.376(5) . ?
N6 N7 1.313(4) . ?
N7 N8 1.343(4) . ?
N8 C108 1.347(5) . ?
N8 C109 1.473(5) . ?
C108 H108 0.9500 . ?
C109 C110 1.513(6) . ?
C109 H10G 0.9900 . ?
C109 H10H 0.9900 . ?
C110 C111 1.389(6) . ?
C110 C115 1.397(6) . ?
C111 C112 1.397(6) . ?
C111 H111 0.9500 . ?
C112 O12 1.373(5) . ?
C112 C113 1.389(6) . ?
C113 C114 1.387(6) . ?
C113 O13 1.385(5) . ?
C114 O14 1.369(5) . ?
C114 C115 1.403(6) . ?
C115 H115 0.9500 . ?
O12 C116 1.417(6) . ?
C116 H11A 0.9800 . ?
C116 H11B 0.9800 . ?
C116 H11C 0.9800 . ?
O13 C117 1.396(6) . ?
C117 H11D 0.9800 . ?
C117 H11E 0.9800 . ?
C117 H11F 0.9800 . ?
O14 C118 1.438(6) . ?
C118 H11G 0.9800 . ?
C118 H11H 0.9800 . ?
C118 H11I 0.9800 . ?
C119 C120 1.369(7) . ?
C119 C124 1.420(7) . ?
C119 C125 1.492(7) . ?
C120 C121 1.392(7) . ?
C120 H120 0.9500 . ?
C121 C122 1.368(8) . ?
C121 H121 0.9500 . ?
C122 C123 1.390(8) . ?
C122 H122 0.9500 . ?
C123 C124 1.374(7) . ?
C123 H123 0.9500 . ?
C124 H124 0.9500 . ?
C125 H12A 0.9800 . ?
C125 H12B 0.9800 . ?
C125 H12C 0.9800 . ?


loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O5 106.84(11) . . ?
O2 Ti1 O1 91.87(11) . . ?
O5 Ti1 O1 97.49(11) . . ?
O2 Ti1 O6 99.49(10) . . ?
O5 Ti1 O6 89.54(10) . . ?
O1 Ti1 O6 164.34(12) . . ?
O2 Ti1 N1 161.47(11) . . ?
O5 Ti1 N1 91.30(11) . . ?
O1 Ti1 N1 81.84(11) . . ?
O6 Ti1 N1 84.03(11) . . ?
O2 Ti1 N2 89.53(11) . . ?
O5 Ti1 N2 163.55(11) . . ?
O1 Ti1 N2 83.19(11) . . ?
O6 Ti1 N2 86.14(11) . . ?
N1 Ti1 N2 72.48(11) . . ?
O3 Ti2 O8 106.15(11) . . ?
O3 Ti2 O4 91.32(11) . . ?
O8 Ti2 O4 95.43(10) . . ?
O3 Ti2 O7 101.55(11) . . ?
O8 Ti2 O7 88.97(10) . . ?
O4 Ti2 O7 164.68(11) . . ?
O3 Ti2 N5 160.03(10) . . ?
O8 Ti2 N5 93.20(11) . . ?
O4 Ti2 N5 81.79(11) . . ?
O7 Ti2 N5 83.32(11) . . ?
O3 Ti2 N6 88.50(10) . . ?
O8 Ti2 N6 165.33(12) . . ?
O4 Ti2 N6 84.75(10) . . ?
O7 Ti2 N6 87.31(10) . . ?
N5 Ti2 N6 72.28(11) . . ?
C6 C1 C2 119.0(4) . . ?
C6 C1 C7 121.4(4) . . ?
C2 C1 C7 119.6(4) . . ?
C3 C2 C1 120.1(5) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 119.9 . . ?
C4 C3 C2 120.2(5) . . ?
C4 C3 H3 119.9 . . ?
C2 C3 H3 119.9 . . ?
C5 C4 C3 119.7(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 120.0(5) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C1 C6 C5 121.0(5) . . ?
C1 C6 H6 119.5 . . ?
C5 C6 H6 119.5 . . ?
C12 C7 C8 119.5(4) . . ?
C12 C7 C1 121.2(3) . . ?
C8 C7 C1 119.3(3) . . ?
O1 C8 C7 117.2(3) . . ?
O1 C8 C9 122.1(3) . . ?
C7 C8 C9 120.6(3) . . ?
C8 O1 Ti1 130.6(2) . . ?
C10 C9 C8 117.1(3) . . ?
C10 C9 C13 118.6(3) . . ?
C8 C9 C13 124.0(3) . . ?
C9 C10 C11 122.4(4) . . ?
C9 C10 H10 118.8 . . ?
C11 C10 H10 118.8 . . ?
C12 C11 C10 119.6(4) . . ?
C12 C11 H11 120.2 . . ?
C10 C11 H11 120.2 . . ?
C11 C12 C7 120.9(4) . . ?
C11 C12 H12 119.6 . . ?
C7 C12 H12 119.6 . . ?
C14 C13 C18 117.7(3) . . ?
C14 C13 C9 126.3(3) . . ?
C18 C13 C9 115.8(3) . . ?
O2 C14 C13 119.9(3) . . ?
O2 C14 C15 118.8(3) . . ?
C13 C14 C15 121.2(3) . . ?
C14 O2 Ti1 135.2(2) . . ?
C16 C15 C14 118.0(3) . . ?
C16 C15 C19 117.5(3) . . ?
C14 C15 C19 124.6(3) . . ?
C17 C16 C15 121.7(3) . . ?
C17 C16 H16 119.2 . . ?
C15 C16 H16 119.2 . . ?
C16 C17 C18 119.7(3) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C13 121.7(3) . . ?
C17 C18 H18 119.2 . . ?
C13 C18 H18 119.2 . . ?
C24 C19 C20 116.2(3) . . ?
C24 C19 C15 119.8(3) . . ?
C20 C19 C15 123.8(3) . . ?
C21 C20 C19 121.3(3) . . ?
C21 C20 H20 119.3 . . ?
C19 C20 H20 119.3 . . ?
C20 C21 C22 122.2(3) . . ?
C20 C21 H21 118.9 . . ?
C22 C21 H21 118.9 . . ?
C21 C22 C23 116.3(3) . . ?
C21 C22 C25 120.2(3) . . ?
C23 C22 C25 123.4(3) . . ?
C24 C23 C22 121.0(3) . . ?
C24 C23 H23 119.5 . . ?
C22 C23 H23 119.5 . . ?
C23 C24 C19 122.8(3) . . ?
C23 C24 H24 118.6 . . ?
C19 C24 H24 118.6 . . ?
C30 C25 C26 117.8(3) . . ?
C30 C25 C22 117.8(3) . . ?
C26 C25 C22 124.5(3) . . ?
O3 C26 C27 120.0(3) . . ?
O3 C26 C25 118.3(3) . . ?
C27 C26 C25 121.6(3) . . ?
C26 O3 Ti2 133.5(2) . . ?
C26 C27 C28 117.8(3) . . ?
C26 C27 C31 126.1(3) . . ?
C28 C27 C31 116.0(3) . . ?
C29 C28 C27 121.7(4) . . ?
C29 C28 H28 119.1 . . ?
C27 C28 H28 119.1 . . ?
C28 C29 C30 119.3(4) . . ?
C28 C29 H29 120.4 . . ?
C30 C29 H29 120.4 . . ?
C29 C30 C25 121.8(4) . . ?
C29 C30 H30 119.1 . . ?
C25 C30 H30 119.1 . . ?
C32 C31 C36 117.8(3) . . ?
C32 C31 C27 124.0(3) . . ?
C36 C31 C27 117.9(4) . . ?
O4 C32 C31 121.9(3) . . ?
O4 C32 C33 117.2(4) . . ?
C31 C32 C33 120.8(3) . . ?
C32 O4 Ti2 129.3(2) . . ?
C34 C33 C32 118.8(4) . . ?
C34 C33 C37 120.5(4) . . ?
C32 C33 C37 120.7(3) . . ?
C35 C34 C33 120.9(4) . . ?
C35 C34 H34 119.6 . . ?
C33 C34 H34 119.5 . . ?
C34 C35 C36 119.8(4) . . ?
C34 C35 H35 120.1 . . ?
C36 C35 H35 120.1 . . ?
C35 C36 C31 121.8(4) . . ?
C35 C36 H36 119.1 . . ?
C31 C36 H36 119.1 . . ?
C42 C37 C38 118.7(4) . . ?
C42 C37 C33 120.7(4) . . ?
C38 C37 C33 120.6(4) . . ?
C39 C38 C37 119.4(5) . . ?
C39 C38 H38 120.3 . . ?
C37 C38 H38 120.3 . . ?
C40 C39 C38 121.6(5) . . ?
C40 C39 H39 119.2 . . ?
C38 C39 H39 119.2 . . ?
C39 C40 C41 119.2(5) . . ?
C39 C40 H40 120.4 . . ?
C41 C40 H40 120.4 . . ?
C40 C41 C42 120.3(5) . . ?
C40 C41 H41 119.8 . . ?
C42 C41 H41 119.8 . . ?
C37 C42 C41 120.7(5) . . ?
C37 C42 H42 119.6 . . ?
C41 C42 H42 119.6 . . ?
C44 C43 C48 117.8(4) . . ?
C44 C43 C49 122.3(3) . . ?
C48 C43 C49 119.9(3) . . ?
C45 C44 C43 120.4(4) . . ?
C45 C44 H44 119.8 . . ?
C43 C44 H44 119.8 . . ?
C44 C45 C46 120.4(4) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C47 C46 C45 120.1(4) . . ?
C47 C46 H46 120.0 . . ?
C45 C46 H46 119.9 . . ?
C46 C47 C48 120.2(4) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C47 C48 C43 121.1(4) . . ?
C47 C48 H48 119.5 . . ?
C43 C48 H48 119.5 . . ?
C54 C49 C50 120.0(4) . . ?
C54 C49 C43 118.6(4) . . ?
C50 C49 C43 121.2(3) . . ?
O5 C50 C49 118.1(3) . . ?
O5 C50 C51 122.6(3) . . ?
C49 C50 C51 119.2(3) . . ?
C50 O5 Ti1 140.3(2) . . ?
C52 C51 C50 117.6(4) . . ?
C52 C51 C55 115.6(3) . . ?
C50 C51 C55 126.7(3) . . ?
C53 C52 C51 122.2(4) . . ?
C53 C52 H52 118.9 . . ?
C51 C52 H52 118.9 . . ?
C54 C53 C52 119.4(4) . . ?
C54 C53 H53 120.3 . . ?
C52 C53 H53 120.3 . . ?
C53 C54 C49 121.3(4) . . ?
C53 C54 H54 119.3 . . ?
C49 C54 H54 119.3 . . ?
C60 C55 C56 118.6(4) . . ?
C60 C55 C51 116.8(3) . . ?
C56 C55 C51 124.6(3) . . ?
O6 C56 C55 120.0(3) . . ?
O6 C56 C57 119.5(3) . . ?
C55 C56 C57 120.6(3) . . ?
C56 O6 Ti1 129.6(2) . . ?
C58 C57 C56 117.9(3) . . ?
C58 C57 C61 118.9(4) . . ?
C56 C57 C61 123.2(3) . . ?
C59 C58 C57 121.5(4) . . ?
C59 C58 H58 119.2 . . ?
C57 C58 H58 119.2 . . ?
C58 C59 C60 119.7(4) . . ?
C58 C59 H59 120.2 . . ?
C60 C59 H59 120.2 . . ?
C59 C60 C55 121.7(4) . . ?
C59 C60 H60 119.1 . . ?
C55 C60 H60 119.1 . . ?
C62 C61 C66 117.0(3) . . ?
C62 C61 C57 120.6(3) . . ?
C66 C61 C57 122.3(4) . . ?
C63 C62 C61 121.8(3) . . ?
C63 C62 H62 119.1 . . ?
C61 C62 H62 119.1 . . ?
C62 C63 C64 121.2(4) . . ?
C62 C63 H63 119.4 . . ?
C64 C63 H63 119.4 . . ?
C63 C64 C65 116.9(4) . . ?
C63 C64 C67 119.7(4) . . ?
C65 C64 C67 123.4(3) . . ?
C66 C65 C64 121.7(3) . . ?
C66 C65 H65 119.2 . . ?
C64 C65 H65 119.2 . . ?
C65 C66 C61 121.4(4) . . ?
C65 C66 H66 119.3 . . ?
C61 C66 H66 119.3 . . ?
C72 C67 C68 118.4(4) . . ?
C72 C67 C64 119.8(3) . . ?
C68 C67 C64 121.8(3) . . ?
O7 C68 C69 119.8(3) . . ?
O7 C68 C67 120.2(3) . . ?
C69 C68 C67 120.0(3) . . ?
C68 O7 Ti2 129.2(2) . . ?
C70 C69 C68 118.8(3) . . ?
C70 C69 C73 117.0(3) . . ?
C68 C69 C73 124.2(3) . . ?
C71 C70 C69 121.7(4) . . ?
C71 C70 H70 119.2 . . ?
C69 C70 H70 119.2 . . ?
C72 C71 C70 118.8(4) . . ?
C72 C71 H71 120.6 . . ?
C70 C71 H71 120.6 . . ?
C71 C72 C67 122.4(4) . . ?
C71 C72 H72 118.8 . . ?
C67 C72 H72 118.8 . . ?
C78 C73 C74 118.2(3) . . ?
C78 C73 C69 116.2(3) . . ?
C74 C73 C69 125.5(3) . . ?
O8 C74 C73 123.3(3) . . ?
O8 C74 C75 117.2(3) . . ?
C73 C74 C75 119.4(3) . . ?
C74 O8 Ti2 139.4(2) . . ?
C76 C75 C74 119.6(4) . . ?
C76 C75 C79 118.8(3) . . ?
C74 C75 C79 121.5(3) . . ?
C77 C76 C75 121.1(4) . . ?
C77 C76 H76 119.4 . . ?
C75 C76 H76 119.4 . . ?
C76 C77 C78 119.1(4) . . ?
C76 C77 H77 120.5 . . ?
C78 C77 H77 120.5 . . ?
C77 C78 C73 122.5(4) . . ?
C77 C78 H78 118.8 . . ?
C73 C78 H78 118.8 . . ?
C80 C79 C84 118.0(4) . . ?
C80 C79 C75 122.3(4) . . ?
C84 C79 C75 119.6(4) . . ?
C79 C80 C81 120.6(4) . . ?
C79 C80 H80 119.7 . . ?
C81 C80 H80 119.7 . . ?
C80 C81 C82 120.3(4) . . ?
C80 C81 H81 119.9 . . ?
C82 C81 H81 119.9 . . ?
C83 C82 C81 119.1(4) . . ?
C83 C82 H82 120.4 . . ?
C81 C82 H82 120.4 . . ?
C84 C83 C82 120.5(4) . . ?
C84 C83 H83 119.7 . . ?
C82 C83 H83 119.7 . . ?
C83 C84 C79 121.5(5) . . ?
C83 C84 H84 119.3 . . ?
C79 C84 H84 119.3 . . ?
C85 N1 C89 118.7(3) . . ?
C85 N1 Ti1 121.7(3) . . ?
C89 N1 Ti1 119.4(2) . . ?
N1 C85 C86 121.6(4) . . ?
N1 C85 H85 119.2 . . ?
C86 C85 H85 119.2 . . ?
C87 C86 C85 119.6(4) . . ?
C87 C86 H86 120.2 . . ?
C85 C86 H86 120.2 . . ?
C86 C87 C88 119.2(4) . . ?
C86 C87 H87 120.4 . . ?
C88 C87 H87 120.4 . . ?
C89 C88 C87 118.4(4) . . ?
C89 C88 H88 120.8 . . ?
C87 C88 H88 120.8 . . ?
N1 C89 C88 122.4(3) . . ?
N1 C89 C90 114.1(3) . . ?
C88 C89 C90 123.5(4) . . ?
N2 C90 C91 107.6(3) . . ?
N2 C90 C89 118.2(3) . . ?
C91 C90 C89 134.2(4) . . ?
N3 N2 C90 110.5(3) . . ?
N3 N2 Ti1 133.9(3) . . ?
C90 N2 Ti1 115.6(2) . . ?
N2 N3 N4 105.3(3) . . ?
C91 N4 N3 112.3(3) . . ?
C91 N4 C92 125.5(3) . . ?
N3 N4 C92 121.8(3) . . ?
N4 C91 C90 104.4(3) . . ?
N4 C91 H91 127.8 . . ?
C90 C91 H91 127.8 . . ?
N4 C92 C93 113.8(4) . . ?
N4 C92 H92A 108.8 . . ?
C93 C92 H92A 108.8 . . ?
N4 C92 H92B 108.8 . . ?
C93 C92 H92B 108.8 . . ?
H92A C92 H92B 107.7 . . ?
C94 C93 C98 121.0(4) . . ?
C94 C93 C92 121.0(4) . . ?
C98 C93 C92 118.0(4) . . ?
C93 C94 C95 120.2(4) . . ?
C93 C94 H94 119.9 . . ?
C95 C94 H94 119.9 . . ?
O9 C95 C94 125.6(4) . . ?
O9 C95 C96 115.3(4) . . ?
C94 C95 C96 119.2(4) . . ?
C97 C96 O10 121.0(4) . . ?
C97 C96 C95 120.2(4) . . ?
O10 C96 C95 118.7(4) . . ?
O11 C97 C96 115.2(4) . . ?
O11 C97 C98 124.2(4) . . ?
C96 C97 C98 120.5(4) . . ?
C93 C98 C97 118.9(4) . . ?
C93 C98 H98 120.5 . . ?
C97 C98 H98 120.6 . . ?
C95 O9 C99 117.1(4) . . ?
O9 C99 H99A 109.5 . . ?
O9 C99 H99B 109.5 . . ?
H99A C99 H99B 109.5 . . ?
O9 C99 H99C 109.5 . . ?
H99A C99 H99C 109.5 . . ?
H99B C99 H99C 109.5 . . ?
C96 O10 C100 110.9(5) . . ?
O10 C100 H10A 109.5 . . ?
O10 C100 H10B 109.5 . . ?
H10A C100 H10B 109.5 . . ?
O10 C100 H10C 109.5 . . ?
H10A C100 H10C 109.5 . . ?
H10B C100 H10C 109.5 . . ?
C97 O11 C101 118.3(4) . . ?
O11 C101 H10D 109.4 . . ?
O11 C101 H10E 109.5 . . ?
H10D C101 H10E 109.5 . . ?
O11 C101 H10F 109.5 . . ?
H10D C101 H10F 109.5 . . ?
H10E C101 H10F 109.5 . . ?
C102 N5 C106 118.0(3) . . ?
C102 N5 Ti2 121.6(2) . . ?
C106 N5 Ti2 120.2(2) . . ?
N5 C102 C103 122.6(3) . . ?
N5 C102 H102 118.7 . . ?
C103 C102 H102 118.7 . . ?
C104 C103 C102 118.7(4) . . ?
C104 C103 H103 120.6 . . ?
C102 C103 H103 120.6 . . ?
C105 C104 C103 119.5(4) . . ?
C105 C104 H104 120.3 . . ?
C103 C104 H104 120.3 . . ?
C104 C105 C106 118.7(4) . . ?
C104 C105 H105 120.7 . . ?
C106 C105 H105 120.7 . . ?
N5 C106 C105 122.5(4) . . ?
N5 C106 C107 113.6(3) . . ?
C105 C106 C107 123.9(3) . . ?
N6 C107 C108 106.8(3) . . ?
N6 C107 C106 118.9(3) . . ?
C108 C107 C106 134.2(3) . . ?
N7 N6 C107 110.3(3) . . ?
N7 N6 Ti2 135.0(2) . . ?
C107 N6 Ti2 114.6(2) . . ?
N6 N7 N8 106.3(3) . . ?
N7 N8 C108 111.3(3) . . ?
N7 N8 C109 122.9(3) . . ?
C108 N8 C109 125.4(3) . . ?
N8 C108 C107 105.2(3) . . ?
N8 C108 H108 127.4 . . ?
C107 C108 H108 127.4 . . ?
N8 C109 C110 116.2(3) . . ?
N8 C109 H10G 108.2 . . ?
C110 C109 H10G 108.2 . . ?
N8 C109 H10H 108.2 . . ?
C110 C109 H10H 108.2 . . ?
H10G C109 H10H 107.4 . . ?
C111 C110 C115 121.0(4) . . ?
C111 C110 C109 118.3(4) . . ?
C115 C110 C109 120.5(4) . . ?
C110 C111 C112 119.6(4) . . ?
C110 C111 H111 120.2 . . ?
C112 C111 H111 120.2 . . ?
O12 C112 C113 115.6(4) . . ?
O12 C112 C111 124.5(4) . . ?
C113 C112 C111 119.9(4) . . ?
C114 C113 O13 119.6(4) . . ?
C114 C113 C112 120.4(4) . . ?
O13 C113 C112 120.0(4) . . ?
O14 C114 C113 115.6(4) . . ?
O14 C114 C115 124.0(4) . . ?
C113 C114 C115 120.4(4) . . ?
C110 C115 C114 118.7(4) . . ?
C110 C115 H115 120.7 . . ?
C114 C115 H115 120.7 . . ?
C112 O12 C116 118.0(3) . . ?
O12 C116 H11A 109.5 . . ?
O12 C116 H11B 109.5 . . ?
H11A C116 H11B 109.5 . . ?
O12 C116 H11C 109.5 . . ?
H11A C116 H11C 109.5 . . ?
H11B C116 H11C 109.5 . . ?
C113 O13 C117 114.2(3) . . ?
O13 C117 H11D 109.5 . . ?
O13 C117 H11E 109.5 . . ?
H11D C117 H11E 109.5 . . ?
O13 C117 H11F 109.5 . . ?
H11D C117 H11F 109.5 . . ?
H11E C117 H11F 109.5 . . ?
C114 O14 C118 116.5(3) . . ?
O14 C118 H11G 109.5 . . ?
O14 C118 H11H 109.5 . . ?
H11G C118 H11H 109.5 . . ?
O14 C118 H11I 109.5 . . ?
H11G C118 H11I 109.5 . . ?
H11H C118 H11I 109.5 . . ?
C120 C119 C124 118.2(5) . . ?
C120 C119 C125 120.1(5) . . ?
C124 C119 C125 121.7(5) . . ?
C119 C120 C121 121.6(5) . . ?
C119 C120 H120 119.2 . . ?
C121 C120 H120 119.2 . . ?
C122 C121 C120 119.4(6) . . ?
C122 C121 H121 120.3 . . ?
C120 C121 H121 120.3 . . ?
C121 C122 C123 120.7(5) . . ?
C121 C122 H122 119.7 . . ?
C123 C122 H122 119.7 . . ?
C124 C123 C122 119.7(5) . . ?
C124 C123 H123 120.1 . . ?
C122 C123 H123 120.1 . . ?
C123 C124 C119 120.4(5) . . ?
C123 C124 H124 119.8 . . ?
C119 C124 H124 119.8 . . ?
C119 C125 H12A 109.5 . . ?
C119 C125 H12B 109.5 . . ?
H12A C125 H12B 109.5 . . ?
C119 C125 H12C 109.5 . . ?
H12A C125 H12C 109.5 . . ?
H12B C125 H12C 109.5 . . ?


_refine_diff_density_max         1.252
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.085

_shelxl_version_number           2014/6



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

data_e3656a_a
_database_code_depnum_ccdc_archive 'CCDC 2109008'
loop_
_audit_author_name
_audit_author_address
'Nathalie Kyritsakas'
;University of Strasbourg 
France
;
_audit_update_record             
;
2021-09-10 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C80 H64 N10 O10 Ti, 4(C H2 Cl2)'
_chemical_formula_sum            'C84 H72 Cl8 N10 O10 Ti'
_chemical_formula_weight         1713.01

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

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

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

_cell_length_a                   18.6632(4)
_cell_length_b                   18.1926(3)
_cell_length_c                   23.9583(5)
_cell_angle_alpha                90
_cell_angle_beta                 97.2220(10)
_cell_angle_gamma                90
_cell_volume                     8070.1(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    94000
_cell_measurement_theta_min      2.5
_cell_measurement_theta_max      25.

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_F_000             3536
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.070
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.060
_exptl_absorpt_coefficient_mu    0.437
_shelx_estimated_absorpt_T_min   0.970
_shelx_estimated_absorpt_T_max   0.974
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.968
_exptl_absorpt_correction_T_max  0.971
_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            94763
_diffrn_reflns_av_unetI/netI     0.0198
_diffrn_reflns_av_R_equivalents  0.0317
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.569
_diffrn_reflns_theta_max         30.153
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             11891
_reflns_number_gt                9386
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       '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)+(0.1141P)²+18.6663P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         11891
_refine_ls_number_parameters     533
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0703
_refine_ls_wR_factor_ref         0.2151
_refine_ls_wR_factor_gt          0.1967
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_restrained_S_all      1.042
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.5000 0.33292(2) 0.2500 0.01736(12) Uani 1 2 d S T P A 6
N1 N 0.45230(9) 0.43258(9) 0.28685(7) 0.0219(3) Uani 1 1 d . . . A 6
C1 C 0.47209(11) 0.49854(10) 0.26944(8) 0.0218(4) Uani 1 1 d . . . A 6
N2 N 0.44601(10) 0.56272(10) 0.28358(8) 0.0274(4) Uani 1 1 d . . . A 6
C2 C 0.39848(12) 0.56053(11) 0.32045(9) 0.0275(4) Uani 1 1 d . . . A 6
H2 H 0.3783 0.6055 0.3313 0.033 Uiso 1 1 calc R U . A 6
C3 C 0.37689(11) 0.49551(11) 0.34392(8) 0.0235(4) Uani 1 1 d . . . A 6
C4 C 0.40474(11) 0.43106(11) 0.32432(9) 0.0238(4) Uani 1 1 d . . . A 6
H4 H 0.3898 0.3851 0.3377 0.029 Uiso 1 1 calc R U . A 6
C5 C 0.32951(11) 0.49823(11) 0.38805(9) 0.0238(4) Uani 1 1 d . . . A 6
N3 N 0.28963(12) 0.55978(11) 0.39440(9) 0.0339(4) Uani 1 1 d . . . A 6
N4 N 0.25646(11) 0.55162(11) 0.43866(9) 0.0342(4) Uani 1 1 d . . . A 6
N5 N 0.27499(10) 0.48533(10) 0.46090(8) 0.0270(4) Uani 1 1 d . . . A 6
C6 C 0.32046(13) 0.45030(12) 0.43074(9) 0.0292(4) Uani 1 1 d . . . A 6
H6 H 0.3415 0.4031 0.4375 0.035 Uiso 1 1 calc R U . A 6
C7 C 0.25091(14) 0.46403(14) 0.51424(9) 0.0328(5) Uani 1 1 d . . . A 6
H7A H 0.2212 0.5042 0.5270 0.039 Uiso 1 1 calc R U . A 6
H7B H 0.2938 0.4581 0.5427 0.039 Uiso 1 1 calc R U . A 6
C8 C 0.20764(12) 0.39394(13) 0.51126(9) 0.0292(4) Uani 1 1 d . . . A 6
C9 C 0.14758(14) 0.38526(15) 0.47171(10) 0.0349(5) Uani 1 1 d . . . A 6
H9 H 0.1345 0.4224 0.4444 0.042 Uiso 1 1 calc R U . A 6
C10 C 0.10642(14) 0.32137(16) 0.47239(11) 0.0386(5) Uani 1 1 d . . . A 6
C11 C 0.12512(14) 0.26732(13) 0.51279(11) 0.0353(5) Uani 1 1 d . . . A 6
C12 C 0.18572(13) 0.27682(13) 0.55213(10) 0.0321(5) Uani 1 1 d . . . A 6
C13 C 0.22759(12) 0.34004(13) 0.55136(10) 0.0301(4) Uani 1 1 d . . . A 6
H13 H 0.2694 0.3463 0.5780 0.036 Uiso 1 1 calc R U . A 6
O1 O 0.04625(13) 0.30653(15) 0.43571(10) 0.0600(6) Uani 1 1 d . . . A 6
C14 C 0.0218(2) 0.3623(3) 0.39678(18) 0.0814(13) Uani 1 1 d . . . A 6
H14A H 0.0106 0.4067 0.4172 0.122 Uiso 1 1 calc R U . A 6
H14B H -0.0217 0.3454 0.3730 0.122 Uiso 1 1 calc R U . A 6
H14C H 0.0596 0.3734 0.3732 0.122 Uiso 1 1 calc R U . A 6
O2 O 0.08503(12) 0.20417(11) 0.51318(9) 0.0486(5) Uani 1 1 d . . . A 6
C15 C 0.0259(2) 0.21087(19) 0.54509(17) 0.0605(9) Uani 1 1 d . . . A 6
H15A H 0.0442 0.2198 0.5847 0.091 Uiso 1 1 calc R U . A 6
H15B H -0.0024 0.1653 0.5420 0.091 Uiso 1 1 calc R U . A 6
H15C H -0.0049 0.2520 0.5306 0.091 Uiso 1 1 calc R U . A 6
O3 O 0.19908(12) 0.22131(10) 0.59009(9) 0.0461(5) Uani 1 1 d . . . A 6
C16 C 0.2605(2) 0.22862(18) 0.63069(13) 0.0523(7) Uani 1 1 d . . . A 6
H16A H 0.3037 0.2341 0.6117 0.078 Uiso 1 1 calc R U . A 6
H16B H 0.2653 0.1848 0.6546 0.078 Uiso 1 1 calc R U . A 6
H16C H 0.2550 0.2721 0.6539 0.078 Uiso 1 1 calc R U . A 6
C17 C 0.37356(13) 0.47589(13) 0.13738(10) 0.0320(5) Uani 1 1 d . . . A 6
C18 C 0.41304(17) 0.44736(17) 0.09714(13) 0.0479(7) Uani 1 1 d . . . A 6
H18 H 0.4134 0.3958 0.0908 0.057 Uiso 1 1 calc R U . A 6
C19 C 0.4519(2) 0.4932(2) 0.06607(16) 0.0661(11) Uani 1 1 d . . . A 6
H19 H 0.4788 0.4727 0.0387 0.079 Uiso 1 1 calc R U . A 6
C20 C 0.45225(19) 0.5678(2) 0.07432(17) 0.0648(11) Uani 1 1 d . . . A 6
H20 H 0.4787 0.5988 0.0524 0.078 Uiso 1 1 calc R U . A 6
C21 C 0.41441(17) 0.59738(18) 0.11419(15) 0.0530(8) Uani 1 1 d . . . A 6
H21 H 0.4150 0.6490 0.1203 0.064 Uiso 1 1 calc R U . A 6
C22 C 0.37467(15) 0.55157(15) 0.14604(12) 0.0394(6) Uani 1 1 d . . . A 6
H22 H 0.3484 0.5723 0.1737 0.047 Uiso 1 1 calc R U . A 6
C23 C 0.32825(12) 0.42760(12) 0.16819(9) 0.0278(4) Uani 1 1 d . . . A 6
C24 C 0.35462(10) 0.36084(11) 0.19276(8) 0.0226(4) Uani 1 1 d . . . A 6
O4 O 0.42389(7) 0.34244(8) 0.19081(6) 0.0221(3) Uani 1 1 d . . . A 6
C25 C 0.30905(11) 0.31456(12) 0.21928(9) 0.0256(4) Uani 1 1 d . . . A 6
C26 C 0.23786(12) 0.33776(15) 0.22174(11) 0.0365(5) Uani 1 1 d . . . A 6
H26 H 0.2066 0.3074 0.2400 0.044 Uiso 1 1 calc R U . A 6
C27 C 0.21179(14) 0.40345(16) 0.19834(13) 0.0431(6) Uani 1 1 d . . . A 6
H27 H 0.1634 0.4179 0.2007 0.052 Uiso 1 1 calc R U . A 6
C28 C 0.25670(14) 0.44764(15) 0.17161(12) 0.0383(5) Uani 1 1 d . . . A 6
H28 H 0.2387 0.4926 0.1552 0.046 Uiso 1 1 calc R U . A 6
C29 C 0.32957(11) 0.24033(11) 0.24200(9) 0.0241(4) Uani 1 1 d . . . A 6
C30 C 0.39237(10) 0.22463(10) 0.27903(8) 0.0197(3) Uani 1 1 d . . . A 6
O5 O 0.44440(7) 0.27580(8) 0.29140(6) 0.0222(3) Uani 1 1 d . . . A 6
C31 C 0.40186(11) 0.15548(11) 0.30548(9) 0.0234(4) Uani 1 1 d . . . A 6
C32 C 0.35039(14) 0.10122(12) 0.29044(11) 0.0346(5) Uani 1 1 d . . . A 6
H32 H 0.3565 0.0541 0.3075 0.041 Uiso 1 1 calc R U . A 6
C33 C 0.29082(15) 0.11380(15) 0.25148(12) 0.0429(6) Uani 1 1 d . . . A 6
H33 H 0.2575 0.0754 0.2406 0.052 Uiso 1 1 calc R U . A 6
C34 C 0.28026(13) 0.18328(14) 0.22841(11) 0.0356(5) Uani 1 1 d . . . A 6
H34 H 0.2383 0.1925 0.2026 0.043 Uiso 1 1 calc R U . A 6
C35 C 0.46275(11) 0.13841(11) 0.34946(9) 0.0253(4) Uani 1 1 d . . . A 6
C36 C 0.44851(13) 0.10176(13) 0.39800(10) 0.0323(5) Uani 1 1 d . . . A 6
H36 H 0.4000 0.0901 0.4028 0.039 Uiso 1 1 calc R U . A 6
C37 C 0.50383(17) 0.08205(16) 0.43926(12) 0.0444(6) Uani 1 1 d . . . A 6
H37 H 0.4930 0.0571 0.4720 0.053 Uiso 1 1 calc R U . A 6
C38 C 0.57432(18) 0.0983(2) 0.43325(14) 0.0546(8) Uani 1 1 d . . . A 6
H38 H 0.6123 0.0840 0.4613 0.066 Uiso 1 1 calc R U . A 6
C39 C 0.58922(16) 0.1356(2) 0.38583(16) 0.0626(10) Uani 1 1 d . . . A 6
H39 H 0.6378 0.1474 0.3814 0.075 Uiso 1 1 calc R U . A 6
C40 C 0.53399(14) 0.15579(18) 0.34469(13) 0.0465(7) Uani 1 1 d . . . A 6
H40 H 0.5451 0.1821 0.3126 0.056 Uiso 1 1 calc R U . A 6
C41 C 0.2117(3) 0.7475(3) 0.5806(2) 0.0980(17) Uani 1 1 d . . . B 6
H41A H 0.2307 0.7919 0.5636 0.118 Uiso 1 1 calc R U . B 6
H41B H 0.2385 0.7420 0.6188 0.118 Uiso 1 1 calc R U . B 6
Cl1 Cl 0.23029(15) 0.67381(8) 0.54185(8) 0.1395(8) Uani 1 1 d . . . B 6
Cl2 Cl 0.12197(11) 0.76263(12) 0.58759(12) 0.1520(8) Uani 1 1 d . . . B 6
C42 C 0.0599(5) 0.4985(4) 0.2989(4) 0.072(2) Uani 0.5 1 d . . P C 6
H42A H 0.0680 0.5463 0.2809 0.086 Uiso 0.5 1 calc R U P C 6
H42B H 0.0357 0.5086 0.3326 0.086 Uiso 0.5 1 calc R U P C 6
Cl3 Cl 0.0000 0.44320(14) 0.2500 0.1193(8) Uani 1 2 d S T P C 6
Cl4 Cl 0.14454(12) 0.45731(13) 0.32064(8) 0.0709(5) Uani 0.5 1 d . . P C 6
C43 C -0.0008(4) 0.2232(3) 0.2703(4) 0.060(2) Uani 0.5 1 d D . P D 6
H43A H -0.028(2) 0.246(2) 0.297(3) 0.063 Uiso 0.5 1 d D U P E 6
H43B H -0.010(2) 0.1727(13) 0.268(3) 0.063 Uiso 0.5 1 d D U P F 6
Cl5 Cl 0.07754(7) 0.25293(10) 0.26145(14) 0.1625(11) Uani 1 1 d D . . D 6


_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 O5 1.8437(14) . ?
Ti1 O5 1.8437(14) 2_655 ?
Ti1 O4 1.8847(14) 2_655 ?
Ti1 O4 1.8848(14) . ?
Ti1 N1 2.2486(17) 2_655 ?
Ti1 N1 2.2487(16) . ?
N1 C1 1.337(2) . ?
N1 C4 1.340(2) . ?
C1 N2 1.325(2) . ?
C1 C1 1.482(4) 2_655 ?
N2 C2 1.329(3) . ?
C2 C3 1.391(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(3) . ?
C3 C5 1.462(3) . ?
C4 H4 0.9500 . ?
C5 N3 1.364(3) . ?
C5 C6 1.371(3) . ?
N3 N4 1.302(3) . ?
N4 N5 1.346(3) . ?
N5 C6 1.343(3) . ?
N5 C7 1.459(3) . ?
C6 H6 0.9500 . ?
C7 C8 1.506(3) . ?
C7 H7A 0.9900 . ?
C7 H7B 0.9900 . ?
C8 C9 1.383(3) . ?
C8 C13 1.390(3) . ?
C9 C10 1.394(4) . ?
C9 H9 0.9500 . ?
C10 O1 1.363(3) . ?
C10 C11 1.393(4) . ?
C11 O2 1.372(3) . ?
C11 C12 1.389(4) . ?
C12 O3 1.361(3) . ?
C12 C13 1.392(3) . ?
C13 H13 0.9500 . ?
O1 C14 1.414(5) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
O2 C15 1.425(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
O3 C16 1.413(4) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C18 1.386(4) . ?
C17 C22 1.392(4) . ?
C17 C23 1.480(3) . ?
C18 C19 1.383(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.372(6) . ?
C19 H19 0.9500 . ?
C20 C21 1.368(6) . ?
C20 H20 0.9500 . ?
C21 C22 1.403(4) . ?
C21 H21 0.9500 . ?
C22 H22 0.9500 . ?
C23 C28 1.397(3) . ?
C23 C24 1.411(3) . ?
C24 O4 1.342(2) . ?
C24 C25 1.404(3) . ?
C25 C26 1.402(3) . ?
C25 C29 1.488(3) . ?
C26 C27 1.382(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.376(4) . ?
C27 H27 0.9500 . ?
C28 H28 0.9500 . ?
C29 C34 1.398(3) . ?
C29 C30 1.407(3) . ?
C30 O5 1.351(2) . ?
C30 C31 1.410(3) . ?
C31 C32 1.393(3) . ?
C31 C35 1.482(3) . ?
C32 C33 1.378(4) . ?
C32 H32 0.9500 . ?
C33 C34 1.384(4) . ?
C33 H33 0.9500 . ?
C34 H34 0.9500 . ?
C35 C40 1.385(3) . ?
C35 C36 1.395(3) . ?
C36 C37 1.384(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.373(5) . ?
C37 H37 0.9500 . ?
C38 C39 1.381(4) . ?
C38 H38 0.9500 . ?
C39 C40 1.383(4) . ?
C39 H39 0.9500 . ?
C40 H40 0.9500 . ?
C41 Cl1 1.692(6) . ?
C41 Cl2 1.726(7) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C42 Cl4 1.767(9) . ?
C42 Cl3 1.818(10) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
Cl3 C42 1.818(10) 2 ?
C43 C43 0.976(16) 2 ?
C43 Cl5 1.599(6) . ?
C43 Cl5 1.627(9) 2 ?
C43 H43A 0.956(17) . ?
C43 H43B 0.934(17) . ?
Cl5 C43 1.627(9) 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
O5 Ti1 O5 111.38(9) . 2_655 ?
O5 Ti1 O4 93.95(6) . 2_655 ?
O5 Ti1 O4 91.98(6) 2_655 2_655 ?
O5 Ti1 O4 91.98(6) . . ?
O5 Ti1 O4 93.95(6) 2_655 . ?
O4 Ti1 O4 169.46(9) 2_655 . ?
O5 Ti1 N1 160.57(7) . 2_655 ?
O5 Ti1 N1 88.05(6) 2_655 2_655 ?
O4 Ti1 N1 85.60(6) 2_655 2_655 ?
O4 Ti1 N1 85.91(6) . 2_655 ?
O5 Ti1 N1 88.05(6) . . ?
O5 Ti1 N1 160.57(7) 2_655 . ?
O4 Ti1 N1 85.91(6) 2_655 . ?
O4 Ti1 N1 85.60(6) . . ?
N1 Ti1 N1 72.54(9) 2_655 . ?
C1 N1 C4 117.37(17) . . ?
C1 N1 Ti1 117.54(12) . . ?
C4 N1 Ti1 125.08(13) . . ?
N2 C1 N1 125.87(18) . . ?
N2 C1 C1 118.05(11) . 2_655 ?
N1 C1 C1 116.07(11) . 2_655 ?
C1 N2 C2 116.15(18) . . ?
N2 C2 C3 123.08(19) . . ?
N2 C2 H2 118.5 . . ?
C3 C2 H2 118.5 . . ?
C4 C3 C2 116.21(18) . . ?
C4 C3 C5 124.02(18) . . ?
C2 C3 C5 119.73(18) . . ?
N1 C4 C3 121.13(18) . . ?
N1 C4 H4 119.4 . . ?
C3 C4 H4 119.4 . . ?
N3 C5 C6 108.60(18) . . ?
N3 C5 C3 119.78(18) . . ?
C6 C5 C3 131.36(19) . . ?
N4 N3 C5 108.62(19) . . ?
N3 N4 N5 107.45(18) . . ?
C6 N5 N4 111.14(18) . . ?
C6 N5 C7 129.1(2) . . ?
N4 N5 C7 119.51(18) . . ?
N5 C6 C5 104.19(19) . . ?
N5 C6 H6 127.9 . . ?
C5 C6 H6 127.9 . . ?
N5 C7 C8 113.93(18) . . ?
N5 C7 H7A 108.8 . . ?
C8 C7 H7A 108.8 . . ?
N5 C7 H7B 108.8 . . ?
C8 C7 H7B 108.8 . . ?
H7A C7 H7B 107.7 . . ?
C9 C8 C13 121.1(2) . . ?
C9 C8 C7 120.8(2) . . ?
C13 C8 C7 118.0(2) . . ?
C8 C9 C10 119.2(2) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
O1 C10 C11 115.0(2) . . ?
O1 C10 C9 124.6(3) . . ?
C11 C10 C9 120.4(2) . . ?
O2 C11 C12 119.9(2) . . ?
O2 C11 C10 120.5(2) . . ?
C12 C11 C10 119.7(2) . . ?
O3 C12 C11 115.2(2) . . ?
O3 C12 C13 124.5(2) . . ?
C11 C12 C13 120.3(2) . . ?
C8 C13 C12 119.3(2) . . ?
C8 C13 H13 120.3 . . ?
C12 C13 H13 120.3 . . ?
C10 O1 C14 117.0(3) . . ?
O1 C14 H14A 109.5 . . ?
O1 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
O1 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C11 O2 C15 113.1(2) . . ?
O2 C15 H15A 109.5 . . ?
O2 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
O2 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C12 O3 C16 117.0(2) . . ?
O3 C16 H16A 109.5 . . ?
O3 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
O3 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C18 C17 C22 118.4(2) . . ?
C18 C17 C23 120.8(2) . . ?
C22 C17 C23 120.8(2) . . ?
C19 C18 C17 120.7(3) . . ?
C19 C18 H18 119.7 . . ?
C17 C18 H18 119.7 . . ?
C20 C19 C18 120.8(3) . . ?
C20 C19 H19 119.6 . . ?
C18 C19 H19 119.6 . . ?
C21 C20 C19 119.8(3) . . ?
C21 C20 H20 120.1 . . ?
C19 C20 H20 120.1 . . ?
C20 C21 C22 120.0(3) . . ?
C20 C21 H21 120.0 . . ?
C22 C21 H21 120.0 . . ?
C17 C22 C21 120.3(3) . . ?
C17 C22 H22 119.8 . . ?
C21 C22 H22 119.8 . . ?
C28 C23 C24 119.1(2) . . ?
C28 C23 C17 119.0(2) . . ?
C24 C23 C17 121.87(18) . . ?
O4 C24 C25 120.47(18) . . ?
O4 C24 C23 119.16(18) . . ?
C25 C24 C23 120.37(18) . . ?
C24 O4 Ti1 129.42(13) . . ?
C26 C25 C24 118.0(2) . . ?
C26 C25 C29 117.35(19) . . ?
C24 C25 C29 124.54(18) . . ?
C27 C26 C25 122.0(2) . . ?
C27 C26 H26 119.0 . . ?
C25 C26 H26 119.0 . . ?
C28 C27 C26 119.3(2) . . ?
C28 C27 H27 120.3 . . ?
C26 C27 H27 120.3 . . ?
C27 C28 C23 121.2(2) . . ?
C27 C28 H28 119.4 . . ?
C23 C28 H28 119.4 . . ?
C34 C29 C30 117.89(19) . . ?
C34 C29 C25 117.18(19) . . ?
C30 C29 C25 124.77(18) . . ?
O5 C30 C29 121.14(17) . . ?
O5 C30 C31 118.03(17) . . ?
C29 C30 C31 120.80(17) . . ?
C30 O5 Ti1 135.08(13) . . ?
C32 C31 C30 118.2(2) . . ?
C32 C31 C35 118.52(19) . . ?
C30 C31 C35 123.26(18) . . ?
C33 C32 C31 121.9(2) . . ?
C33 C32 H32 119.0 . . ?
C31 C32 H32 119.0 . . ?
C32 C33 C34 119.0(2) . . ?
C32 C33 H33 120.5 . . ?
C34 C33 H33 120.5 . . ?
C33 C34 C29 121.9(2) . . ?
C33 C34 H34 119.0 . . ?
C29 C34 H34 119.0 . . ?
C40 C35 C36 117.6(2) . . ?
C40 C35 C31 123.5(2) . . ?
C36 C35 C31 118.92(19) . . ?
C37 C36 C35 121.1(2) . . ?
C37 C36 H36 119.5 . . ?
C35 C36 H36 119.5 . . ?
C38 C37 C36 120.5(2) . . ?
C38 C37 H37 119.7 . . ?
C36 C37 H37 119.7 . . ?
C37 C38 C39 119.1(3) . . ?
C37 C38 H38 120.4 . . ?
C39 C38 H38 120.4 . . ?
C38 C39 C40 120.5(3) . . ?
C38 C39 H39 119.7 . . ?
C40 C39 H39 119.7 . . ?
C39 C40 C35 121.1(2) . . ?
C39 C40 H40 119.4 . . ?
C35 C40 H40 119.4 . . ?
Cl1 C41 Cl2 116.6(3) . . ?
Cl1 C41 H41A 108.1 . . ?
Cl2 C41 H41A 108.1 . . ?
Cl1 C41 H41B 108.1 . . ?
Cl2 C41 H41B 108.1 . . ?
H41A C41 H41B 107.3 . . ?
Cl4 C42 Cl3 114.2(4) . . ?
Cl4 C42 H42A 108.7 . . ?
Cl3 C42 H42A 108.7 . . ?
Cl4 C42 H42B 108.7 . . ?
Cl3 C42 H42B 108.7 . . ?
H42A C42 H42B 107.6 . . ?
C42 Cl3 C42 112.7(5) . 2 ?
C43 C43 Cl5 74.0(7) 2 . ?
C43 C43 Cl5 70.8(9) 2 2 ?
Cl5 C43 Cl5 126.3(4) . 2 ?
C43 C43 H43A 138(5) 2 . ?
Cl5 C43 H43A 121(2) . . ?
Cl5 C43 H43A 69(4) 2 . ?
C43 C43 H43B 89(4) 2 . ?
Cl5 C43 H43B 119(2) . . ?
Cl5 C43 H43B 99(4) 2 . ?
H43A C43 H43B 111(2) . . ?
C43 Cl5 C43 35.2(5) . 2 ?

_refine_diff_density_max         1.231
_refine_diff_density_min         -1.495
_refine_diff_density_rms         0.088

_shelxl_version_number           2014/6

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

data_e3254a_a
_database_code_depnum_ccdc_archive 'CCDC 2109007'
loop_
_audit_author_name
_audit_author_address
'Nathalie Kyritsakas'
;University of Strasbourg 
France
;
_audit_update_record             
;
2021-09-10 deposited with the CCDC.	2021-10-18 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C65 H50 N4 O7 Ti'
_chemical_formula_sum            'C65 H50 N4 O7 Ti'
_chemical_formula_weight         1046.99

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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   19.0876(5)
_cell_length_b                   19.9757(5)
_cell_length_c                   13.5022(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.8410(13)
_cell_angle_gamma                90
_cell_volume                     5111.6(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    130000
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      27.54

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.360
_exptl_crystal_F_000             2184
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.060
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.230
_shelx_estimated_absorpt_T_min   0.986
_shelx_estimated_absorpt_T_max   0.989
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      173(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  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            130801
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_av_R_equivalents  0.0494
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         1.829
_diffrn_reflns_theta_max         30.109
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.913
_diffrn_measured_fraction_theta_full 0.959
_diffrn_reflns_Laue_measured_fraction_max 0.913
_diffrn_reflns_Laue_measured_fraction_full 0.959
_diffrn_reflns_point_group_measured_fraction_max 0.913
_diffrn_reflns_point_group_measured_fraction_full 0.959
_reflns_number_total             13727
_reflns_number_gt                10274
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-97 (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)+(0.0610P)²+3.4625P] 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         13727
_refine_ls_number_parameters     697
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0479
_refine_ls_wR_factor_ref         0.1380
_refine_ls_wR_factor_gt          0.1233
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.21111(2) 0.51027(2) 0.65516(2) 0.01946(8) Uani 1 1 d . . . . .
C1 C 0.07617(10) 0.42560(10) 0.42860(15) 0.0286(4) Uani 1 1 d . . . . .
C2 C 0.09219(11) 0.39085(12) 0.34425(16) 0.0385(5) Uani 1 1 d . . . . .
H2 H 0.0995 0.3438 0.3481 0.046 Uiso 1 1 calc R U . . .
C3 C 0.09752(12) 0.42369(15) 0.25529(17) 0.0479(6) Uani 1 1 d . . . . .
H3 H 0.1090 0.3992 0.1990 0.057 Uiso 1 1 calc R U . . .
C4 C 0.08627(12) 0.49207(14) 0.24788(18) 0.0468(6) Uani 1 1 d . . . . .
H4 H 0.0896 0.5147 0.1867 0.056 Uiso 1 1 calc R U . . .
C5 C 0.07026(11) 0.52690(12) 0.33009(17) 0.0388(5) Uani 1 1 d . . . . .
H5 H 0.0622 0.5738 0.3253 0.047 Uiso 1 1 calc R U . . .
C6 C 0.06576(10) 0.49460(10) 0.41941(15) 0.0303(4) Uani 1 1 d . . . . .
H6 H 0.0554 0.5197 0.4756 0.036 Uiso 1 1 calc R U . . .
C7 C 0.07078(9) 0.38876(9) 0.52322(15) 0.0274(4) Uani 1 1 d . . . . .
C8 C 0.09470(9) 0.41667(8) 0.61702(14) 0.0230(3) Uani 1 1 d . . . . .
O1 O 0.12108(7) 0.47955(6) 0.62045(9) 0.0241(3) Uani 1 1 d . . . . .
C9 C 0.09076(9) 0.38125(9) 0.70626(15) 0.0273(4) Uani 1 1 d . . . . .
C10 C 0.06279(11) 0.31656(10) 0.69937(18) 0.0381(5) Uani 1 1 d . . . . .
H10 H 0.0598 0.2915 0.7585 0.046 Uiso 1 1 calc R U . . .
C11 C 0.03936(13) 0.28841(11) 0.6077(2) 0.0475(6) Uani 1 1 d . . . . .
H11 H 0.0208 0.2442 0.6044 0.057 Uiso 1 1 calc R U . . .
C12 C 0.04295(12) 0.32430(11) 0.52160(18) 0.0408(5) Uani 1 1 d . . . . .
H12 H 0.0260 0.3046 0.4593 0.049 Uiso 1 1 calc R U . . .
C13 C 0.11150(10) 0.41078(9) 0.80669(15) 0.0272(4) Uani 1 1 d . . . . .
C14 C 0.17765(9) 0.44116(8) 0.83481(14) 0.0238(4) Uani 1 1 d . . . . .
O2 O 0.22269(6) 0.45059(6) 0.76687(9) 0.0222(2) Uani 1 1 d . . . . .
C15 C 0.19611(10) 0.46239(9) 0.93455(14) 0.0274(4) Uani 1 1 d . . . . .
C16 C 0.14630(12) 0.45628(11) 1.00139(16) 0.0366(5) Uani 1 1 d . . . . .
H16 H 0.1580 0.4710 1.0682 0.044 Uiso 1 1 calc R U . . .
C17 C 0.08048(12) 0.42946(13) 0.97321(18) 0.0419(5) Uani 1 1 d . . . . .
H17 H 0.0469 0.4270 1.0196 0.050 Uiso 1 1 calc R U . . .
C18 C 0.06376(11) 0.40621(11) 0.87744(17) 0.0365(5) Uani 1 1 d . . . . .
H18 H 0.0188 0.3866 0.8589 0.044 Uiso 1 1 calc R U . . .
C19 C 0.26678(11) 0.49054(9) 0.97018(14) 0.0281(4) Uani 1 1 d . . . . .
C20 C 0.27347(12) 0.54306(10) 1.03889(15) 0.0351(4) Uani 1 1 d . . . . .
H20 H 0.2324 0.5615 1.0616 0.042 Uiso 1 1 calc R U . . .
C21 C 0.33918(13) 0.56874(11) 1.07447(17) 0.0426(5) Uani 1 1 d . . . . .
H21 H 0.3426 0.6047 1.1209 0.051 Uiso 1 1 calc R U . . .
C22 C 0.39957(13) 0.54243(13) 1.04280(19) 0.0472(6) Uani 1 1 d . . . . .
H22 H 0.4445 0.5599 1.0677 0.057 Uiso 1 1 calc R U . . .
C23 C 0.39423(12) 0.49069(12) 0.97489(18) 0.0440(5) Uani 1 1 d . . . . .
H23 H 0.4357 0.4726 0.9527 0.053 Uiso 1 1 calc R U . . .
C24 C 0.32839(11) 0.46464(10) 0.93843(16) 0.0333(4) Uani 1 1 d . . . . .
H24 H 0.3254 0.4290 0.8916 0.040 Uiso 1 1 calc R U . . .
C25 C 0.25574(10) 0.33070(9) 0.50285(15) 0.0284(4) Uani 1 1 d . . . . .
C26 C 0.27307(13) 0.32597(10) 0.60590(16) 0.0365(5) Uani 1 1 d . . . . .
H26 H 0.2967 0.3621 0.6413 0.044 Uiso 1 1 calc R U . . .
C27 C 0.25630(15) 0.26933(11) 0.6573(2) 0.0479(6) Uani 1 1 d . . . . .
H27 H 0.2683 0.2671 0.7276 0.058 Uiso 1 1 calc R U . . .
C28 C 0.22207(14) 0.21562(11) 0.6069(2) 0.0507(6) Uani 1 1 d . . . . .
H28 H 0.2107 0.1768 0.6424 0.061 Uiso 1 1 calc R U . . .
C29 C 0.20484(13) 0.21921(11) 0.5055(2) 0.0468(6) Uani 1 1 d . . . . .
H29 H 0.1817 0.1826 0.4706 0.056 Uiso 1 1 calc R U . . .
C30 C 0.22098(11) 0.27582(10) 0.45372(17) 0.0354(5) Uani 1 1 d . . . . .
H30 H 0.2083 0.2777 0.3836 0.043 Uiso 1 1 calc R U . . .
C31 C 0.27266(10) 0.38990(9) 0.44291(14) 0.0261(4) Uani 1 1 d . . . . .
C32 C 0.27455(9) 0.45583(8) 0.48168(14) 0.0233(4) Uani 1 1 d . . . . .
O3 O 0.26639(7) 0.46372(6) 0.57852(10) 0.0265(3) Uani 1 1 d . . . . .
C33 C 0.28736(10) 0.51138(9) 0.42193(14) 0.0254(4) Uani 1 1 d . . . . .
C34 C 0.29588(11) 0.49936(10) 0.32265(16) 0.0335(4) Uani 1 1 d . . . . .
H34 H 0.3016 0.5364 0.2802 0.040 Uiso 1 1 calc R U . . .
C35 C 0.29627(12) 0.43547(11) 0.28353(16) 0.0376(5) Uani 1 1 d . . . . .
H35 H 0.3037 0.4287 0.2159 0.045 Uiso 1 1 calc R U . . .
C36 C 0.28565(11) 0.38147(10) 0.34409(15) 0.0339(4) Uani 1 1 d . . . . .
H36 H 0.2872 0.3375 0.3177 0.041 Uiso 1 1 calc R U . . .
C37 C 0.29918(10) 0.58129(9) 0.46030(14) 0.0263(4) Uani 1 1 d . . . . .
C38 C 0.25753(9) 0.61461(8) 0.52442(14) 0.0231(4) Uani 1 1 d . . . . .
O4 O 0.20536(6) 0.58278(6) 0.56310(9) 0.0223(3) Uani 1 1 d . . . . .
C39 C 0.27132(10) 0.68274(9) 0.55033(15) 0.0263(4) Uani 1 1 d . . . . .
C40 C 0.32819(10) 0.71476(9) 0.51435(16) 0.0329(4) Uani 1 1 d . . . . .
H40 H 0.3382 0.7600 0.5324 0.039 Uiso 1 1 calc R U . . .
C41 C 0.37023(10) 0.68229(10) 0.45333(17) 0.0359(5) Uani 1 1 d . . . . .
H41 H 0.4088 0.7048 0.4298 0.043 Uiso 1 1 calc R U . . .
C42 C 0.35547(10) 0.61657(10) 0.42687(17) 0.0328(4) Uani 1 1 d . . . . .
H42 H 0.3844 0.5944 0.3846 0.039 Uiso 1 1 calc R U . . .
C43 C 0.22693(10) 0.72119(8) 0.61370(15) 0.0273(4) Uani 1 1 d . . . . .
C44 C 0.15355(10) 0.71509(9) 0.60379(15) 0.0307(4) Uani 1 1 d . . . . .
H44 H 0.1310 0.6835 0.5581 0.037 Uiso 1 1 calc R U . . .
C45 C 0.11314(12) 0.75449(10) 0.65972(18) 0.0389(5) Uani 1 1 d . . . . .
H45 H 0.0633 0.7498 0.6519 0.047 Uiso 1 1 calc R U . . .
C46 C 0.14536(14) 0.80074(11) 0.7271(2) 0.0482(6) Uani 1 1 d . . . . .
H46 H 0.1176 0.8280 0.7651 0.058 Uiso 1 1 calc R U . . .
C47 C 0.21758(14) 0.80694(11) 0.73874(19) 0.0469(6) Uani 1 1 d . . . . .
H47 H 0.2398 0.8384 0.7850 0.056 Uiso 1 1 calc R U . . .
C48 C 0.25820(12) 0.76751(9) 0.68335(17) 0.0359(5) Uani 1 1 d . . . . .
H48 H 0.3081 0.7719 0.6927 0.043 Uiso 1 1 calc R U . . .
N1 N 0.16775(8) 0.58262(7) 0.76130(11) 0.0220(3) Uani 1 1 d . . . . .
C49 C 0.09925(10) 0.58573(9) 0.77410(15) 0.0276(4) Uani 1 1 d . . . . .
H49 H 0.0666 0.5583 0.7340 0.033 Uiso 1 1 calc R U . . .
C50 C 0.07456(11) 0.62773(11) 0.84400(17) 0.0364(5) Uani 1 1 d . . . . .
H50 H 0.0258 0.6288 0.8522 0.044 Uiso 1 1 calc R U . . .
C51 C 0.12209(12) 0.66797(12) 0.90133(18) 0.0415(5) Uani 1 1 d . . . . .
H51 H 0.1063 0.6972 0.9496 0.050 Uiso 1 1 calc R U . . .
C52 C 0.19258(11) 0.66572(10) 0.88849(16) 0.0338(4) Uani 1 1 d . . . . .
H52 H 0.2259 0.6933 0.9272 0.041 Uiso 1 1 calc R U . . .
C53 C 0.21365(9) 0.62235(8) 0.81785(14) 0.0238(4) Uani 1 1 d . . . . .
C54 C 0.28712(9) 0.61301(8) 0.80076(14) 0.0241(4) Uani 1 1 d . . . . .
N2 N 0.30229(8) 0.56556(7) 0.73473(12) 0.0236(3) Uani 1 1 d . . . . .
N3 N 0.37063(8) 0.56195(8) 0.73094(13) 0.0289(3) Uani 1 1 d . . . . .
N4 N 0.39909(8) 0.60821(8) 0.79549(13) 0.0311(4) Uani 1 1 d . . . . .
C55 C 0.35016(10) 0.64068(9) 0.84003(15) 0.0293(4) Uani 1 1 d . . . . .
H55 H 0.3575 0.6753 0.8883 0.035 Uiso 1 1 calc R U . . .
C56 C 0.47610(10) 0.61887(12) 0.80813(18) 0.0393(5) Uani 1 1 d . . . . .
H56A H 0.5004 0.5750 0.8106 0.047 Uiso 1 1 calc R U . . .
H56B H 0.4902 0.6422 0.8721 0.047 Uiso 1 1 calc R U . . .
C57 C 0.49870(10) 0.65997(11) 0.72347(17) 0.0368(5) Uani 1 1 d . . . . .
C58 C 0.49909(12) 0.72935(12) 0.73046(18) 0.0411(5) Uani 1 1 d . . . . .
H58 H 0.4888 0.7509 0.7898 0.049 Uiso 1 1 calc R U . . .
C59 C 0.51482(12) 0.76700(11) 0.64858(18) 0.0420(5) Uani 1 1 d . . . . .
C60 C 0.52933(11) 0.73552(11) 0.56261(17) 0.0381(5) Uani 1 1 d . . . . .
C61 C 0.53164(11) 0.66580(12) 0.55794(18) 0.0385(5) Uani 1 1 d . . . . .
C62 C 0.51513(11) 0.62817(12) 0.63899(18) 0.0393(5) Uani 1 1 d . . . . .
H62 H 0.5152 0.5807 0.6358 0.047 Uiso 1 1 calc R U . . .
O5 O 0.51638(11) 0.83567(9) 0.64650(14) 0.0575(5) Uani 1 1 d . . . . .
C63 C 0.5190(2) 0.86873(15) 0.7383(2) 0.0797(11) Uani 1 1 d . . . . .
H63A H 0.4727 0.8662 0.7626 0.120 Uiso 1 1 calc R U . . .
H63B H 0.5317 0.9158 0.7300 0.120 Uiso 1 1 calc R U . . .
H63C H 0.5544 0.8474 0.7866 0.120 Uiso 1 1 calc R U . . .
O6 O 0.53786(8) 0.77300(9) 0.47942(13) 0.0460(4) Uani 1 1 d . . . . .
C64 C 0.60793(12) 0.79679(12) 0.4768(2) 0.0500(6) Uani 1 1 d . . . . .
H64A H 0.6212 0.8259 0.5344 0.075 Uiso 1 1 calc R U . . .
H64B H 0.6103 0.8222 0.4152 0.075 Uiso 1 1 calc R U . . .
H64C H 0.6404 0.7587 0.4789 0.075 Uiso 1 1 calc R U . . .
O7 O 0.54912(9) 0.63992(9) 0.47132(13) 0.0488(4) Uani 1 1 d . . . . .
C65 C 0.55244(14) 0.56883(13) 0.4657(2) 0.0528(6) Uani 1 1 d . . . . .
H65A H 0.5826 0.5516 0.5239 0.079 Uiso 1 1 calc R U . . .
H65B H 0.5721 0.5558 0.4047 0.079 Uiso 1 1 calc R U . . .
H65C H 0.5049 0.5502 0.4646 0.079 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.8191(13) . ?
Ti1 O1 1.8322(13) . ?
Ti1 O4 1.9033(12) . ?
Ti1 O2 1.9147(12) . ?
Ti1 N2 2.2266(15) . ?
Ti1 N1 2.2604(15) . ?
C1 C6 1.396(3) . ?
C1 C2 1.398(3) . ?
C1 C7 1.488(3) . ?
C2 C3 1.383(3) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.375(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(3) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.392(3) . ?
C7 C8 1.409(3) . ?
C8 O1 1.3521(19) . ?
C8 C9 1.407(3) . ?
C9 C10 1.397(3) . ?
C9 C13 1.488(3) . ?
C10 C11 1.384(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.375(3) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.400(3) . ?
C13 C14 1.412(3) . ?
C14 O2 1.343(2) . ?
C14 C15 1.416(3) . ?
C15 C16 1.392(3) . ?
C15 C19 1.488(3) . ?
C16 C17 1.377(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.375(3) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C20 1.396(3) . ?
C19 C24 1.398(3) . ?
C20 C21 1.387(3) . ?
C20 H20 0.9500 . ?
C21 C22 1.380(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.377(3) . ?
C22 H22 0.9500 . ?
C23 C24 1.395(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.394(3) . ?
C25 C30 1.406(3) . ?
C25 C31 1.490(3) . ?
C26 C27 1.385(3) . ?
C26 H26 0.9500 . ?
C27 C28 1.391(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.372(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.383(3) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.396(3) . ?
C31 C32 1.416(2) . ?
C32 O3 1.344(2) . ?
C32 C33 1.410(2) . ?
C33 C34 1.390(3) . ?
C33 C37 1.497(3) . ?
C34 C35 1.381(3) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(3) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.404(3) . ?
C37 C38 1.410(3) . ?
C38 O4 1.339(2) . ?
C38 C39 1.422(2) . ?
C39 C40 1.396(3) . ?
C39 C43 1.487(3) . ?
C40 C41 1.379(3) . ?
C40 H40 0.9500 . ?
C41 C42 1.381(3) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.401(3) . ?
C43 C44 1.396(3) . ?
C44 C45 1.387(3) . ?
C44 H44 0.9500 . ?
C45 C46 1.388(3) . ?
C45 H45 0.9500 . ?
C46 C47 1.374(4) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(3) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 C49 1.341(2) . ?
N1 C53 1.350(2) . ?
C49 C50 1.387(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.379(3) . ?
C50 H50 0.9500 . ?
C51 C52 1.378(3) . ?
C51 H51 0.9500 . ?
C52 C53 1.383(3) . ?
C52 H52 0.9500 . ?
C53 C54 1.460(3) . ?
C54 N2 1.356(2) . ?
C54 C55 1.372(2) . ?
N2 N3 1.313(2) . ?
N3 N4 1.340(2) . ?
N4 C55 1.337(3) . ?
N4 C56 1.475(2) . ?
C55 H55 0.9500 . ?
C56 C57 1.511(3) . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C57 C62 1.374(3) . ?
C57 C58 1.389(3) . ?
C58 C59 1.399(3) . ?
C58 H58 0.9500 . ?
C59 O5 1.372(3) . ?
C59 C60 1.377(3) . ?
C60 O6 1.376(3) . ?
C60 C61 1.395(3) . ?
C61 O7 1.356(3) . ?
C61 C62 1.394(3) . ?
C62 H62 0.9500 . ?
O5 C63 1.400(4) . ?
C63 H63A 0.9800 . ?
C63 H63B 0.9800 . ?
C63 H63C 0.9800 . ?
O6 C64 1.424(3) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
O7 C65 1.424(3) . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O1 105.85(6) . . ?
O3 Ti1 O4 90.55(5) . . ?
O1 Ti1 O4 96.22(5) . . ?
O3 Ti1 O2 96.28(5) . . ?
O1 Ti1 O2 90.56(5) . . ?
O4 Ti1 O2 168.71(5) . . ?
O3 Ti1 N2 93.15(6) . . ?
O1 Ti1 N2 160.90(6) . . ?
O4 Ti1 N2 85.33(5) . . ?
O2 Ti1 N2 85.32(5) . . ?
O3 Ti1 N1 165.57(6) . . ?
O1 Ti1 N1 88.47(5) . . ?
O4 Ti1 N1 86.02(5) . . ?
O2 Ti1 N1 85.15(5) . . ?
N2 Ti1 N1 72.61(5) . . ?
C6 C1 C2 117.4(2) . . ?
C6 C1 C7 122.73(18) . . ?
C2 C1 C7 119.86(18) . . ?
C3 C2 C1 121.2(2) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 120.3(2) . . ?
C2 C3 H3 119.9 . . ?
C4 C3 H3 119.9 . . ?
C5 C4 C3 119.2(2) . . ?
C5 C4 H4 120.4 . . ?
C3 C4 H4 120.4 . . ?
C6 C5 C4 120.8(2) . . ?
C6 C5 H5 119.6 . . ?
C4 C5 H5 119.6 . . ?
C5 C6 C1 121.1(2) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C12 C7 C8 117.54(18) . . ?
C12 C7 C1 120.59(18) . . ?
C8 C7 C1 121.86(16) . . ?
O1 C8 C7 118.54(16) . . ?
O1 C8 C9 119.70(16) . . ?
C7 C8 C9 121.74(16) . . ?
C8 O1 Ti1 130.84(11) . . ?
C10 C9 C8 117.85(18) . . ?
C10 C9 C13 119.04(18) . . ?
C8 C9 C13 123.04(16) . . ?
C9 C10 C11 121.0(2) . . ?
C9 C10 H10 119.5 . . ?
C11 C10 H10 119.5 . . ?
C12 C11 C10 120.07(19) . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C7 121.8(2) . . ?
C11 C12 H12 119.1 . . ?
C7 C12 H12 119.1 . . ?
C18 C13 C14 118.60(19) . . ?
C18 C13 C9 118.15(17) . . ?
C14 C13 C9 123.22(17) . . ?
O2 C14 C13 120.09(17) . . ?
O2 C14 C15 120.04(16) . . ?
C13 C14 C15 119.87(17) . . ?
C14 O2 Ti1 127.01(11) . . ?
C16 C15 C14 118.60(18) . . ?
C16 C15 C19 119.11(18) . . ?
C14 C15 C19 122.29(17) . . ?
C17 C16 C15 121.7(2) . . ?
C17 C16 H16 119.1 . . ?
C15 C16 H16 119.1 . . ?
C18 C17 C16 119.5(2) . . ?
C18 C17 H17 120.2 . . ?
C16 C17 H17 120.2 . . ?
C17 C18 C13 121.5(2) . . ?
C17 C18 H18 119.2 . . ?
C13 C18 H18 119.2 . . ?
C20 C19 C24 117.92(19) . . ?
C20 C19 C15 120.44(18) . . ?
C24 C19 C15 121.63(17) . . ?
C21 C20 C19 121.0(2) . . ?
C21 C20 H20 119.5 . . ?
C19 C20 H20 119.5 . . ?
C22 C21 C20 120.4(2) . . ?
C22 C21 H21 119.8 . . ?
C20 C21 H21 119.8 . . ?
C23 C22 C21 119.6(2) . . ?
C23 C22 H22 120.2 . . ?
C21 C22 H22 120.2 . . ?
C22 C23 C24 120.5(2) . . ?
C22 C23 H23 119.8 . . ?
C24 C23 H23 119.8 . . ?
C23 C24 C19 120.6(2) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
C26 C25 C30 117.42(18) . . ?
C26 C25 C31 123.69(17) . . ?
C30 C25 C31 118.89(18) . . ?
C27 C26 C25 120.9(2) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C28 120.5(2) . . ?
C26 C27 H27 119.8 . . ?
C28 C27 H27 119.8 . . ?
C29 C28 C27 119.4(2) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 120.4(2) . . ?
C28 C29 H29 119.8 . . ?
C30 C29 H29 119.8 . . ?
C29 C30 C25 121.3(2) . . ?
C29 C30 H30 119.3 . . ?
C25 C30 H30 119.3 . . ?
C36 C31 C32 117.77(17) . . ?
C36 C31 C25 119.87(17) . . ?
C32 C31 C25 122.34(17) . . ?
O3 C32 C33 120.81(16) . . ?
O3 C32 C31 117.89(16) . . ?
C33 C32 C31 121.25(17) . . ?
C32 O3 Ti1 139.07(11) . . ?
C34 C33 C32 117.63(17) . . ?
C34 C33 C37 117.69(17) . . ?
C32 C33 C37 124.42(17) . . ?
C35 C34 C33 122.33(19) . . ?
C35 C34 H34 118.8 . . ?
C33 C34 H34 118.8 . . ?
C34 C35 C36 119.1(2) . . ?
C34 C35 H35 120.4 . . ?
C36 C35 H35 120.4 . . ?
C35 C36 C31 121.74(19) . . ?
C35 C36 H36 119.1 . . ?
C31 C36 H36 119.1 . . ?
C42 C37 C38 118.01(17) . . ?
C42 C37 C33 116.52(17) . . ?
C38 C37 C33 125.45(16) . . ?
O4 C38 C37 121.02(15) . . ?
O4 C38 C39 118.88(16) . . ?
C37 C38 C39 120.09(16) . . ?
C38 O4 Ti1 128.93(11) . . ?
C40 C39 C38 118.80(18) . . ?
C40 C39 C43 118.91(16) . . ?
C38 C39 C43 122.29(16) . . ?
C41 C40 C39 121.63(18) . . ?
C41 C40 H40 119.2 . . ?
C39 C40 H40 119.2 . . ?
C40 C41 C42 119.11(18) . . ?
C40 C41 H41 120.4 . . ?
C42 C41 H41 120.4 . . ?
C41 C42 C37 122.3(2) . . ?
C41 C42 H42 118.8 . . ?
C37 C42 H42 118.8 . . ?
C48 C43 C44 117.66(19) . . ?
C48 C43 C39 120.04(18) . . ?
C44 C43 C39 122.24(17) . . ?
C45 C44 C43 121.00(19) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C44 C45 C46 120.2(2) . . ?
C44 C45 H45 119.9 . . ?
C46 C45 H45 119.9 . . ?
C47 C46 C45 119.6(2) . . ?
C47 C46 H46 120.2 . . ?
C45 C46 H46 120.2 . . ?
C46 C47 C48 120.4(2) . . ?
C46 C47 H47 119.8 . . ?
C48 C47 H47 119.8 . . ?
C47 C48 C43 121.1(2) . . ?
C47 C48 H48 119.4 . . ?
C43 C48 H48 119.4 . . ?
C49 N1 C53 118.51(16) . . ?
C49 N1 Ti1 123.21(12) . . ?
C53 N1 Ti1 118.21(12) . . ?
N1 C49 C50 122.11(17) . . ?
N1 C49 H49 118.9 . . ?
C50 C49 H49 118.9 . . ?
C51 C50 C49 118.73(19) . . ?
C51 C50 H50 120.6 . . ?
C49 C50 H50 120.6 . . ?
C50 C51 C52 119.84(19) . . ?
C50 C51 H51 120.1 . . ?
C52 C51 H51 120.1 . . ?
C53 C52 C51 118.40(18) . . ?
C53 C52 H52 120.8 . . ?
C51 C52 H52 120.8 . . ?
N1 C53 C52 122.42(17) . . ?
N1 C53 C54 113.98(15) . . ?
C52 C53 C54 123.55(16) . . ?
N2 C54 C55 106.83(16) . . ?
N2 C54 C53 118.53(15) . . ?
C55 C54 C53 134.59(17) . . ?
N3 N2 C54 110.79(15) . . ?
N3 N2 Ti1 132.59(12) . . ?
C54 N2 Ti1 116.62(11) . . ?
N2 N3 N4 105.32(15) . . ?
C55 N4 N3 112.10(15) . . ?
C55 N4 C56 128.15(18) . . ?
N3 N4 C56 119.74(18) . . ?
N4 C55 C54 104.96(17) . . ?
N4 C55 H55 127.5 . . ?
C54 C55 H55 127.5 . . ?
N4 C56 C57 111.17(17) . . ?
N4 C56 H56A 109.4 . . ?
C57 C56 H56A 109.4 . . ?
N4 C56 H56B 109.4 . . ?
C57 C56 H56B 109.4 . . ?
H56A C56 H56B 108.0 . . ?
C62 C57 C58 121.2(2) . . ?
C62 C57 C56 119.4(2) . . ?
C58 C57 C56 119.4(2) . . ?
C57 C58 C59 118.9(2) . . ?
C57 C58 H58 120.6 . . ?
C59 C58 H58 120.6 . . ?
O5 C59 C60 115.6(2) . . ?
O5 C59 C58 124.1(2) . . ?
C60 C59 C58 120.3(2) . . ?
O6 C60 C59 119.7(2) . . ?
O6 C60 C61 119.9(2) . . ?
C59 C60 C61 120.3(2) . . ?
O7 C61 C60 115.6(2) . . ?
O7 C61 C62 125.0(2) . . ?
C60 C61 C62 119.4(2) . . ?
C57 C62 C61 119.8(2) . . ?
C57 C62 H62 120.1 . . ?
C61 C62 H62 120.1 . . ?
C59 O5 C63 116.9(2) . . ?
O5 C63 H63A 109.5 . . ?
O5 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
O5 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C60 O6 C64 113.89(18) . . ?
O6 C64 H64A 109.5 . . ?
O6 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
O6 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C61 O7 C65 116.3(2) . . ?
O7 C65 H65A 109.5 . . ?
O7 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
O7 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?

_refine_diff_density_max         0.511
_refine_diff_density_min         -0.510
_refine_diff_density_rms         0.054

_shelxl_version_number           2014-3

