# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_e3003a
_audit_block_doi                 10.5517/ccdc.csd.cc1l8r7v
_database_code_depnum_ccdc_archive 'CCDC 1468167'
_audit_update_record             
;
2016-06-28 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C58 H42 N4 O4 Ti'
_chemical_formula_sum            'C58 H42 N4 O4 Ti'
_chemical_formula_weight         906.85

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

_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'

_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'

_cell_length_a                   11.8033(3)
_cell_length_b                   16.0200(4)
_cell_length_c                   23.9080(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4520.7(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    90000
_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    1.332
_exptl_crystal_F_000             1888
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.244
_shelx_estimated_absorpt_T_min   0.988
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9879
_exptl_absorpt_correction_T_max  0.9903
_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            90802
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_av_R_equivalents  0.0572
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_theta_min         1.530
_diffrn_reflns_theta_max         30.107
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13305
_reflns_number_gt                10641
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    1.000

_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)+(0.0372P)²+0.8683P] 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_abs_structure_details 
;
 Flack x determined using 4114 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.023(8)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         13305
_refine_ls_number_parameters     606
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0618
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.0917
_refine_ls_wR_factor_gt          0.0820
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.002
_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 0.35519(4) 0.50901(2) 0.97106(2) 0.02065(9) Uani 1 1 d . . . . .
C1 C 0.1309(2) 0.48242(17) 0.83372(11) 0.0327(6) Uani 1 1 d . . . . .
C2 C 0.0674(2) 0.5115(2) 0.87873(12) 0.0393(6) Uani 1 1 d . . . . .
H2 H 0.0710 0.4829 0.9135 0.047 Uiso 1 1 calc R U . . .
C3 C -0.0007(3) 0.5811(2) 0.87377(15) 0.0489(8) Uani 1 1 d . . . . .
H3 H -0.0427 0.6000 0.9052 0.059 Uiso 1 1 calc R U . . .
C4 C -0.0086(3) 0.6238(2) 0.82337(16) 0.0525(9) Uani 1 1 d . . . . .
H4 H -0.0555 0.6718 0.8201 0.063 Uiso 1 1 calc R U . . .
C5 C 0.0521(3) 0.5955(2) 0.77854(15) 0.0535(9) Uani 1 1 d . . . . .
H5 H 0.0465 0.6238 0.7437 0.064 Uiso 1 1 calc R U . . .
C6 C 0.1216(3) 0.5263(2) 0.78320(12) 0.0432(7) Uani 1 1 d . . . . .
H6 H 0.1638 0.5082 0.7516 0.052 Uiso 1 1 calc R U . . .
C7 C 0.2046(2) 0.40724(17) 0.83754(11) 0.0308(6) Uani 1 1 d . . . . .
C8 C 0.2678(2) 0.38916(15) 0.88617(10) 0.0259(5) Uani 1 1 d . . . . .
O1 O 0.25955(15) 0.44287(10) 0.92921(7) 0.0281(4) Uani 1 1 d . . . . .
C9 C 0.3376(2) 0.31781(15) 0.88990(11) 0.0288(5) Uani 1 1 d . . . . .
C10 C 0.3452(2) 0.26700(17) 0.84277(12) 0.0381(6) Uani 1 1 d . . . . .
H10 H 0.3925 0.2190 0.8439 0.046 Uiso 1 1 calc R U . . .
C11 C 0.2854(3) 0.28488(19) 0.79426(12) 0.0441(7) Uani 1 1 d . . . . .
H11 H 0.2924 0.2495 0.7626 0.053 Uiso 1 1 calc R U . . .
C12 C 0.2158(3) 0.35370(19) 0.79194(12) 0.0397(7) Uani 1 1 d . . . . .
H12 H 0.1747 0.3649 0.7586 0.048 Uiso 1 1 calc R U . . .
C13 C 0.3967(2) 0.29094(15) 0.94208(11) 0.0288(5) Uani 1 1 d . . . . .
C14 C 0.4620(2) 0.34361(14) 0.97669(11) 0.0256(5) Uani 1 1 d . . . . .
O2 O 0.46864(13) 0.42559(9) 0.96624(7) 0.0243(3) Uani 1 1 d . . . . .
C15 C 0.5191(2) 0.31117(14) 1.02414(12) 0.0289(5) Uani 1 1 d . . . . .
C16 C 0.5062(2) 0.22602(16) 1.03668(13) 0.0363(6) Uani 1 1 d . . . . .
H16 H 0.5439 0.2033 1.0683 0.044 Uiso 1 1 calc R U . . .
C17 C 0.4399(2) 0.17486(16) 1.00387(13) 0.0398(7) Uani 1 1 d . . . . .
H17 H 0.4308 0.1177 1.0135 0.048 Uiso 1 1 calc R U . . .
C18 C 0.3868(2) 0.20645(16) 0.95722(13) 0.0359(6) Uani 1 1 d . . . . .
H18 H 0.3423 0.1703 0.9347 0.043 Uiso 1 1 calc R U . . .
C19 C 0.5879(2) 0.36521(15) 1.06139(12) 0.0299(6) Uani 1 1 d . . . . .
C20 C 0.6536(2) 0.43122(15) 1.04086(12) 0.0340(6) Uani 1 1 d . . . . .
H20 H 0.6540 0.4428 1.0019 0.041 Uiso 1 1 calc R U . . .
C21 C 0.7179(2) 0.47978(17) 1.07658(14) 0.0419(7) Uani 1 1 d . . . . .
H21 H 0.7623 0.5241 1.0618 0.050 Uiso 1 1 calc R U . . .
C22 C 0.7187(3) 0.46483(18) 1.13351(15) 0.0456(8) Uani 1 1 d . . . . .
H22 H 0.7630 0.4985 1.1578 0.055 Uiso 1 1 calc R U . . .
C23 C 0.6543(3) 0.40050(19) 1.15442(14) 0.0456(7) Uani 1 1 d . . . . .
H23 H 0.6542 0.3897 1.1935 0.055 Uiso 1 1 calc R U . . .
C24 C 0.5894(2) 0.35121(18) 1.11900(13) 0.0382(7) Uani 1 1 d . . . . .
H24 H 0.5453 0.3072 1.1342 0.046 Uiso 1 1 calc R U . . .
C25 C 0.5461(2) 0.57281(17) 0.82572(10) 0.0289(5) Uani 1 1 d . . . . .
C26 C 0.5039(2) 0.49216(18) 0.82585(11) 0.0382(6) Uani 1 1 d . . . . .
H26 H 0.4270 0.4829 0.8358 0.046 Uiso 1 1 calc R U . . .
C27 C 0.5712(3) 0.4252(2) 0.81183(14) 0.0484(8) Uani 1 1 d . . . . .
H27 H 0.5405 0.3703 0.8122 0.058 Uiso 1 1 calc R U . . .
C28 C 0.6836(3) 0.4375(2) 0.79710(14) 0.0468(8) Uani 1 1 d . . . . .
H28 H 0.7303 0.3912 0.7877 0.056 Uiso 1 1 calc R U . . .
C29 C 0.7269(2) 0.5171(2) 0.79623(13) 0.0449(7) Uani 1 1 d . . . . .
H29 H 0.8038 0.5260 0.7861 0.054 Uiso 1 1 calc R U . . .
C30 C 0.6589(2) 0.58406(17) 0.80998(11) 0.0359(6) Uani 1 1 d . . . . .
H30 H 0.6895 0.6389 0.8087 0.043 Uiso 1 1 calc R U . . .
C31 C 0.4737(2) 0.64522(16) 0.84143(10) 0.0274(5) Uani 1 1 d . . . . .
C32 C 0.4186(2) 0.64754(15) 0.89387(10) 0.0246(5) Uani 1 1 d . . . . .
O3 O 0.43730(14) 0.58211(10) 0.92839(7) 0.0255(4) Uani 1 1 d . . . . .
C33 C 0.3538(2) 0.71694(14) 0.91038(10) 0.0267(5) Uani 1 1 d . . . . .
C34 C 0.3434(2) 0.78223(16) 0.87151(12) 0.0355(6) Uani 1 1 d . . . . .
H34 H 0.2982 0.8292 0.8809 0.043 Uiso 1 1 calc R U . . .
C35 C 0.3966(2) 0.78056(18) 0.82013(12) 0.0397(7) Uani 1 1 d . . . . .
H35 H 0.3876 0.8258 0.7948 0.048 Uiso 1 1 calc R U . . .
C36 C 0.4624(2) 0.71341(18) 0.80560(11) 0.0360(6) Uani 1 1 d . . . . .
H36 H 0.5009 0.7134 0.7707 0.043 Uiso 1 1 calc R U . . .
C37 C 0.3024(2) 0.73011(14) 0.96694(11) 0.0267(5) Uani 1 1 d . . . . .
C38 C 0.2454(2) 0.66891(15) 0.99843(10) 0.0249(5) Uani 1 1 d . . . . .
O4 O 0.24012(13) 0.58942(10) 0.98096(7) 0.0243(4) Uani 1 1 d . . . . .
C39 C 0.1936(2) 0.68929(16) 1.05006(11) 0.0288(5) Uani 1 1 d . . . . .
C40 C 0.1988(2) 0.77185(16) 1.06862(12) 0.0347(6) Uani 1 1 d . . . . .
H40 H 0.1619 0.7868 1.1025 0.042 Uiso 1 1 calc R U . . .
C41 C 0.2562(2) 0.83213(16) 1.03884(13) 0.0388(7) Uani 1 1 d . . . . .
H41 H 0.2593 0.8879 1.0523 0.047 Uiso 1 1 calc R U . . .
C42 C 0.3090(2) 0.81101(16) 0.98947(12) 0.0334(6) Uani 1 1 d . . . . .
H42 H 0.3512 0.8524 0.9700 0.040 Uiso 1 1 calc R U . . .
C43 C 0.1390(2) 0.62551(16) 1.08577(11) 0.0304(5) Uani 1 1 d . . . . .
C44 C 0.0665(2) 0.56402(18) 1.06452(12) 0.0359(6) Uani 1 1 d . . . . .
H44 H 0.0522 0.5618 1.0255 0.043 Uiso 1 1 calc R U . . .
C45 C 0.0155(2) 0.5064(2) 1.09960(13) 0.0436(7) Uani 1 1 d . . . . .
H45 H -0.0336 0.4652 1.0844 0.052 Uiso 1 1 calc R U . . .
C46 C 0.0356(3) 0.5085(2) 1.15689(13) 0.0462(7) Uani 1 1 d . . . . .
H46 H -0.0001 0.4692 1.1809 0.055 Uiso 1 1 calc R U . . .
C47 C 0.1076(3) 0.5678(2) 1.17843(13) 0.0450(7) Uani 1 1 d . . . . .
H47 H 0.1222 0.5693 1.2175 0.054 Uiso 1 1 calc R U . . .
C48 C 0.1588(2) 0.62521(18) 1.14333(12) 0.0380(6) Uani 1 1 d . . . . .
H48 H 0.2088 0.6655 1.1588 0.046 Uiso 1 1 calc R U . . .
N1 N 0.29490(16) 0.43780(12) 1.04579(8) 0.0227(4) Uani 1 1 d . . . . .
C49 C 0.2274(2) 0.37062(15) 1.04242(11) 0.0297(6) Uani 1 1 d . . . . .
H49 H 0.1978 0.3545 1.0071 0.036 Uiso 1 1 calc R U . . .
C50 C 0.2001(2) 0.32474(17) 1.08903(12) 0.0354(6) Uani 1 1 d . . . . .
H50 H 0.1526 0.2770 1.0864 0.042 Uiso 1 1 calc R U . . .
C51 C 0.2440(3) 0.35011(18) 1.13993(12) 0.0388(7) Uani 1 1 d . . . . .
N2 N 0.31230(19) 0.41730(14) 1.14383(9) 0.0331(5) Uani 1 1 d . . . . .
C52 C 0.3346(2) 0.45732(14) 1.09672(10) 0.0241(5) Uani 1 1 d . . . . .
C53 C 0.2175(4) 0.3065(3) 1.19341(15) 0.0754(13) Uani 1 1 d . . . . .
H53A H 0.2859 0.2790 1.2075 0.113 Uiso 1 1 calc R U . . .
H53B H 0.1583 0.2647 1.1869 0.113 Uiso 1 1 calc R U . . .
H53C H 0.1908 0.3473 1.2210 0.113 Uiso 1 1 calc R U . . .
C54 C 0.4109(2) 0.53159(14) 1.09828(10) 0.0228(5) Uani 1 1 d . . . . .
N3 N 0.43389(16) 0.56472(12) 1.04770(8) 0.0210(4) Uani 1 1 d . . . . .
C55 C 0.4994(2) 0.63317(14) 1.04757(11) 0.0254(5) Uani 1 1 d . . . . .
H55 H 0.5172 0.6593 1.0130 0.030 Uiso 1 1 calc R U . . .
C56 C 0.5413(2) 0.66637(16) 1.09636(11) 0.0288(5) Uani 1 1 d . . . . .
H56 H 0.5857 0.7158 1.0960 0.035 Uiso 1 1 calc R U . . .
C57 C 0.5170(2) 0.62587(16) 1.14604(11) 0.0283(5) Uani 1 1 d . . . . .
N4 N 0.44888(17) 0.55828(13) 1.14709(8) 0.0275(4) Uani 1 1 d . . . . .
C58 C 0.5663(3) 0.6525(2) 1.20125(12) 0.0437(7) Uani 1 1 d . . . . .
H58A H 0.5081 0.6813 1.2232 0.066 Uiso 1 1 calc R U . . .
H58B H 0.6302 0.6903 1.1947 0.066 Uiso 1 1 calc R U . . .
H58C H 0.5926 0.6032 1.2218 0.066 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 1.8307(16) . ?
Ti1 O1 1.8434(17) . ?
Ti1 O4 1.8868(16) . ?
Ti1 O2 1.8954(16) . ?
Ti1 N1 2.2360(19) . ?
Ti1 N3 2.2397(19) . ?
C1 C2 1.392(4) . ?
C1 C6 1.402(4) . ?
C1 C7 1.489(4) . ?
C2 C3 1.380(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.388(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.366(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.384(5) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.394(4) . ?
C7 C8 1.412(4) . ?
C8 O1 1.345(3) . ?
C8 C9 1.411(3) . ?
C9 C10 1.393(3) . ?
C9 C13 1.493(4) . ?
C10 C11 1.388(4) . ?
C10 H10 0.9500 . ?
C11 C12 1.376(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.406(4) . ?
C13 C14 1.411(4) . ?
C14 O2 1.339(3) . ?
C14 C15 1.418(4) . ?
C15 C16 1.405(3) . ?
C15 C19 1.484(4) . ?
C16 C17 1.379(4) . ?
C16 H16 0.9500 . ?
C17 C18 1.376(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.396(4) . ?
C19 C20 1.400(4) . ?
C20 C21 1.382(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(5) . ?
C21 H21 0.9500 . ?
C22 C23 1.375(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.388(4) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C26 1.385(4) . ?
C25 C30 1.395(4) . ?
C25 C31 1.489(4) . ?
C26 C27 1.376(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.387(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.374(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.379(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.395(4) . ?
C31 C32 1.413(3) . ?
C32 O3 1.352(3) . ?
C32 C33 1.406(3) . ?
C33 C34 1.404(3) . ?
C33 C37 1.497(4) . ?
C34 C35 1.380(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.372(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C42 1.406(3) . ?
C37 C38 1.407(3) . ?
C38 O4 1.342(3) . ?
C38 C39 1.415(3) . ?
C39 C40 1.396(4) . ?
C39 C43 1.480(4) . ?
C40 C41 1.378(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.377(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.396(4) . ?
C43 C44 1.400(4) . ?
C44 C45 1.385(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.391(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.374(5) . ?
C46 H46 0.9500 . ?
C47 C48 1.385(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 C52 1.342(3) . ?
N1 C49 1.342(3) . ?
C49 C50 1.373(4) . ?
C49 H49 0.9500 . ?
C50 C51 1.384(4) . ?
C50 H50 0.9500 . ?
C51 N2 1.348(3) . ?
C51 C53 1.490(4) . ?
N2 C52 1.323(3) . ?
C52 C54 1.493(3) . ?
C53 H53A 0.9800 . ?
C53 H53B 0.9800 . ?
C53 H53C 0.9800 . ?
C54 N4 1.321(3) . ?
C54 N3 1.348(3) . ?
N3 C55 1.342(3) . ?
C55 C56 1.374(4) . ?
C55 H55 0.9500 . ?
C56 C57 1.383(4) . ?
C56 H56 0.9500 . ?
C57 N4 1.349(3) . ?
C57 C58 1.504(4) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 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 112.92(8) . . ?
O3 Ti1 O4 90.82(7) . . ?
O1 Ti1 O4 91.13(7) . . ?
O3 Ti1 O2 92.47(7) . . ?
O1 Ti1 O2 89.68(7) . . ?
O4 Ti1 O2 176.00(8) . . ?
O3 Ti1 N1 160.07(8) . . ?
O1 Ti1 N1 86.87(8) . . ?
O4 Ti1 N1 91.09(7) . . ?
O2 Ti1 N1 85.05(7) . . ?
O3 Ti1 N3 88.93(7) . . ?
O1 Ti1 N3 157.98(8) . . ?
O4 Ti1 N3 85.64(7) . . ?
O2 Ti1 N3 92.16(7) . . ?
N1 Ti1 N3 71.44(7) . . ?
C2 C1 C6 117.2(3) . . ?
C2 C1 C7 122.5(2) . . ?
C6 C1 C7 120.3(3) . . ?
C3 C2 C1 121.2(3) . . ?
C3 C2 H2 119.4 . . ?
C1 C2 H2 119.4 . . ?
C2 C3 C4 120.8(3) . . ?
C2 C3 H3 119.6 . . ?
C4 C3 H3 119.6 . . ?
C5 C4 C3 118.8(3) . . ?
C5 C4 H4 120.6 . . ?
C3 C4 H4 120.6 . . ?
C4 C5 C6 120.9(3) . . ?
C4 C5 H5 119.6 . . ?
C6 C5 H5 119.6 . . ?
C5 C6 C1 121.1(3) . . ?
C5 C6 H6 119.4 . . ?
C1 C6 H6 119.4 . . ?
C12 C7 C8 117.9(3) . . ?
C12 C7 C1 120.4(2) . . ?
C8 C7 C1 121.7(2) . . ?
O1 C8 C9 120.8(2) . . ?
O1 C8 C7 117.4(2) . . ?
C9 C8 C7 121.8(2) . . ?
C8 O1 Ti1 137.60(16) . . ?
C10 C9 C8 117.4(2) . . ?
C10 C9 C13 118.5(2) . . ?
C8 C9 C13 124.0(2) . . ?
C11 C10 C9 121.5(3) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C7 121.2(3) . . ?
C11 C12 H12 119.4 . . ?
C7 C12 H12 119.4 . . ?
C18 C13 C14 118.1(3) . . ?
C18 C13 C9 117.0(2) . . ?
C14 C13 C9 125.0(2) . . ?
O2 C14 C13 120.6(2) . . ?
O2 C14 C15 118.7(2) . . ?
C13 C14 C15 120.6(2) . . ?
C14 O2 Ti1 129.70(15) . . ?
C16 C15 C14 118.4(2) . . ?
C16 C15 C19 119.8(2) . . ?
C14 C15 C19 121.8(2) . . ?
C17 C16 C15 121.1(3) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C18 C17 C16 120.1(2) . . ?
C18 C17 H17 120.0 . . ?
C16 C17 H17 120.0 . . ?
C17 C18 C13 121.7(3) . . ?
C17 C18 H18 119.2 . . ?
C13 C18 H18 119.2 . . ?
C24 C19 C20 117.4(3) . . ?
C24 C19 C15 120.4(2) . . ?
C20 C19 C15 122.2(3) . . ?
C21 C20 C19 120.8(3) . . ?
C21 C20 H20 119.6 . . ?
C19 C20 H20 119.6 . . ?
C22 C21 C20 121.0(3) . . ?
C22 C21 H21 119.5 . . ?
C20 C21 H21 119.5 . . ?
C23 C22 C21 119.0(3) . . ?
C23 C22 H22 120.5 . . ?
C21 C22 H22 120.5 . . ?
C22 C23 C24 120.6(3) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 121.2(3) . . ?
C23 C24 H24 119.4 . . ?
C19 C24 H24 119.4 . . ?
C26 C25 C30 117.7(3) . . ?
C26 C25 C31 121.3(2) . . ?
C30 C25 C31 121.0(2) . . ?
C27 C26 C25 121.3(3) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C26 C27 C28 120.2(3) . . ?
C26 C27 H27 119.9 . . ?
C28 C27 H27 119.9 . . ?
C29 C28 C27 119.4(3) . . ?
C29 C28 H28 120.3 . . ?
C27 C28 H28 120.3 . . ?
C28 C29 C30 120.2(3) . . ?
C28 C29 H29 119.9 . . ?
C30 C29 H29 119.9 . . ?
C29 C30 C25 121.2(3) . . ?
C29 C30 H30 119.4 . . ?
C25 C30 H30 119.4 . . ?
C36 C31 C32 118.7(2) . . ?
C36 C31 C25 120.7(2) . . ?
C32 C31 C25 120.6(2) . . ?
O3 C32 C33 122.0(2) . . ?
O3 C32 C31 116.5(2) . . ?
C33 C32 C31 121.4(2) . . ?
C32 O3 Ti1 138.56(16) . . ?
C34 C33 C32 116.8(2) . . ?
C34 C33 C37 117.2(2) . . ?
C32 C33 C37 125.8(2) . . ?
C35 C34 C33 122.3(3) . . ?
C35 C34 H34 118.8 . . ?
C33 C34 H34 118.8 . . ?
C36 C35 C34 119.9(3) . . ?
C36 C35 H35 120.1 . . ?
C34 C35 H35 120.1 . . ?
C35 C36 C31 120.9(3) . . ?
C35 C36 H36 119.6 . . ?
C31 C36 H36 119.6 . . ?
C42 C37 C38 117.6(2) . . ?
C42 C37 C33 117.0(2) . . ?
C38 C37 C33 125.4(2) . . ?
O4 C38 C37 121.1(2) . . ?
O4 C38 C39 118.1(2) . . ?
C37 C38 C39 120.8(2) . . ?
C38 O4 Ti1 130.83(15) . . ?
C40 C39 C38 118.5(3) . . ?
C40 C39 C43 119.3(2) . . ?
C38 C39 C43 122.1(2) . . ?
C41 C40 C39 121.4(3) . . ?
C41 C40 H40 119.3 . . ?
C39 C40 H40 119.3 . . ?
C42 C41 C40 119.6(2) . . ?
C42 C41 H41 120.2 . . ?
C40 C41 H41 120.2 . . ?
C41 C42 C37 122.0(3) . . ?
C41 C42 H42 119.0 . . ?
C37 C42 H42 119.0 . . ?
C48 C43 C44 117.2(3) . . ?
C48 C43 C39 119.9(2) . . ?
C44 C43 C39 122.9(2) . . ?
C45 C44 C43 121.0(3) . . ?
C45 C44 H44 119.5 . . ?
C43 C44 H44 119.5 . . ?
C44 C45 C46 120.4(3) . . ?
C44 C45 H45 119.8 . . ?
C46 C45 H45 119.8 . . ?
C47 C46 C45 119.4(3) . . ?
C47 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
C46 C47 C48 120.2(3) . . ?
C46 C47 H47 119.9 . . ?
C48 C47 H47 119.9 . . ?
C47 C48 C43 121.8(3) . . ?
C47 C48 H48 119.1 . . ?
C43 C48 H48 119.1 . . ?
C52 N1 C49 116.7(2) . . ?
C52 N1 Ti1 119.68(15) . . ?
C49 N1 Ti1 123.39(16) . . ?
N1 C49 C50 121.3(2) . . ?
N1 C49 H49 119.3 . . ?
C50 C49 H49 119.3 . . ?
C49 C50 C51 118.0(2) . . ?
C49 C50 H50 121.0 . . ?
C51 C50 H50 121.0 . . ?
N2 C51 C50 121.3(2) . . ?
N2 C51 C53 116.1(3) . . ?
C50 C51 C53 122.6(3) . . ?
C52 N2 C51 116.6(2) . . ?
N2 C52 N1 126.2(2) . . ?
N2 C52 C54 119.0(2) . . ?
N1 C52 C54 114.8(2) . . ?
C51 C53 H53A 109.5 . . ?
C51 C53 H53B 109.5 . . ?
H53A C53 H53B 109.5 . . ?
C51 C53 H53C 109.5 . . ?
H53A C53 H53C 109.5 . . ?
H53B C53 H53C 109.5 . . ?
N4 C54 N3 126.6(2) . . ?
N4 C54 C52 119.0(2) . . ?
N3 C54 C52 114.4(2) . . ?
C55 N3 C54 116.1(2) . . ?
C55 N3 Ti1 124.25(16) . . ?
C54 N3 Ti1 119.56(15) . . ?
N3 C55 C56 121.4(2) . . ?
N3 C55 H55 119.3 . . ?
C56 C55 H55 119.3 . . ?
C55 C56 C57 118.2(2) . . ?
C55 C56 H56 120.9 . . ?
C57 C56 H56 120.9 . . ?
N4 C57 C56 121.0(2) . . ?
N4 C57 C58 116.2(2) . . ?
C56 C57 C58 122.7(2) . . ?
C54 N4 C57 116.5(2) . . ?
C57 C58 H58A 109.5 . . ?
C57 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C57 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?

_refine_diff_density_max         0.216
_refine_diff_density_min         -0.342
_refine_diff_density_rms         0.046

_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_e3303a_a
_audit_block_doi                 10.5517/ccdc.csd.cc1l8r8w
_database_code_depnum_ccdc_archive 'CCDC 1468168'
_audit_update_record             
;
2016-06-28 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C80 H54 N4 O4 Ti), C5 H12'
_chemical_formula_sum            'C165 H120 N8 O8 Ti2'
_chemical_formula_weight         2438.48

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                   20.622(2)
_cell_length_b                   13.9118(16)
_cell_length_c                   23.906(3)
_cell_angle_alpha                90
_cell_angle_beta                 96.372(4)
_cell_angle_gamma                90
_cell_volume                     6816.0(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    26000
_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    1.188
_exptl_crystal_F_000             2548
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.179
_shelx_estimated_absorpt_T_min   0.991
_shelx_estimated_absorpt_T_max   0.993
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.992
_exptl_absorpt_correction_T_max  0.995
_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            13151
_diffrn_reflns_av_unetI/netI     0.1817
_diffrn_reflns_av_R_equivalents  0.1213
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.769
_diffrn_reflns_theta_max         27.333
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.846
_diffrn_measured_fraction_theta_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.846
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_point_group_measured_fraction_full 0.968
_reflns_number_total             13151
_reflns_number_gt                4890
_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.
Because we didn't identify the solvents we use the squeeze
command. The cristal didn't diffract too much that is why the
ratio observed/ unique reflection is low
;

_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)+(0.1314P)²+0.7164P] 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         13151
_refine_ls_number_parameters     717
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.2594
_refine_ls_R_factor_gt           0.1288
_refine_ls_wR_factor_ref         0.3330
_refine_ls_wR_factor_gt          0.2970
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_restrained_S_all      1.165
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.029

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 0.71639(6) 0.40758(8) 0.14235(4) 0.0424(4) Uani 1 1 d . . . . .
N1 N 0.6423(2) 0.3772(3) 0.20194(17) 0.0625(17) Uani 1 1 d G . . . .
C1 C 0.5801(3) 0.3452(3) 0.18211(15) 0.075(2) Uani 1 1 d G . . . .
H1 H 0.5693 0.3327 0.1431 0.090 Uiso 1 1 calc R U . . .
C2 C 0.5337(2) 0.3316(4) 0.2193(2) 0.0874(12) Uani 1 1 d G . . . .
H2 H 0.4912 0.3097 0.2058 0.105 Uiso 1 1 calc R U . . .
C3 C 0.5495(3) 0.3499(3) 0.2764(2) 0.0874(12) Uani 1 1 d DG . . . .
N2 N 0.6117(3) 0.3819(3) 0.29620(14) 0.0874(12) Uani 1 1 d G . . . .
C4 C 0.6581(2) 0.3955(3) 0.25899(19) 0.066(2) Uani 1 1 d G . . . .
C5 C 0.4971(5) 0.3345(5) 0.3131(3) 0.0874(12) Uani 1 1 d D . . . .
H5 H 0.4557 0.3111 0.2976 0.105 Uiso 1 1 calc R U . . .
C6 C 0.5078(5) 0.3526(5) 0.3657(3) 0.0874(12) Uani 1 1 d D . . . .
H6 H 0.5508 0.3729 0.3787 0.105 Uiso 1 1 calc R U . . .
C7 C 0.4609(5) 0.3461(6) 0.4098(4) 0.0874(12) Uani 1 1 d D . . . .
C8 C 0.3959(5) 0.3208(6) 0.3957(4) 0.097(3) Uani 1 1 d D . . . .
H8 H 0.3824 0.3026 0.3579 0.116 Uiso 1 1 calc R U . . .
C9 C 0.3506(7) 0.3205(7) 0.4326(4) 0.131(4) Uani 1 1 d D . . . .
H9 H 0.3068 0.3031 0.4202 0.157 Uiso 1 1 calc R U . . .
C10 C 0.3671(4) 0.3445(5) 0.4864(2) 0.1218(19) Uani 1 1 d DG . . . .
C11 C 0.3216(3) 0.3508(5) 0.5251(3) 0.1218(19) Uani 1 1 d G . . . .
H11 H 0.2776 0.3325 0.5144 0.146 Uiso 1 1 calc R U . . .
C12 C 0.3406(3) 0.3838(5) 0.5793(3) 0.1218(19) Uani 1 1 d G . . . .
H12 H 0.3095 0.3881 0.6057 0.146 Uiso 1 1 calc R U . . .
C13 C 0.4050(4) 0.4106(4) 0.5949(2) 0.1218(19) Uani 1 1 d G . . . .
H13 H 0.4180 0.4331 0.6319 0.146 Uiso 1 1 calc R U . . .
C14 C 0.4505(3) 0.4042(5) 0.5563(3) 0.1218(19) Uani 1 1 d G . . . .
H14 H 0.4945 0.4225 0.5669 0.146 Uiso 1 1 calc R U . . .
C15 C 0.4315(4) 0.3712(5) 0.5020(3) 0.118(4) Uani 1 1 d DG . . . .
C16 C 0.4820(5) 0.3700(8) 0.4632(4) 0.122(4) Uani 1 1 d D . . . .
H16 H 0.5263 0.3850 0.4750 0.146 Uiso 1 1 calc R U . . .
N3 N 0.7581(3) 0.4459(3) 0.22996(13) 0.0644(17) Uani 1 1 d G . . . .
C17 C 0.7175(2) 0.4306(3) 0.27183(18) 0.067(2) Uani 1 1 d G . . . .
N4 N 0.7395(3) 0.4514(3) 0.32758(16) 0.1150(16) Uani 1 1 d DG . . . .
C20 C 0.8021(3) 0.4875(4) 0.34147(15) 0.1150(16) Uani 1 1 d DG . . . .
C19 C 0.8426(2) 0.5028(4) 0.2996(2) 0.1150(16) Uani 1 1 d DG . . . .
H19 H 0.8854 0.5274 0.3091 0.138 Uiso 1 1 calc R U . . .
C18 C 0.8206(3) 0.4820(4) 0.2438(2) 0.091(3) Uani 1 1 d G . . . .
H18 H 0.8483 0.4924 0.2152 0.110 Uiso 1 1 calc R U . . .
C21 C 0.8091(5) 0.4935(6) 0.4020(3) 0.1150(16) Uani 1 1 d D . . . .
H21 H 0.7741 0.4679 0.4199 0.138 Uiso 1 1 calc R U . . .
C22 C 0.8549(5) 0.5277(6) 0.4335(3) 0.1150(16) Uani 1 1 d D . . . .
H22 H 0.8877 0.5525 0.4125 0.138 Uiso 1 1 calc R U . . .
C23 C 0.8720(7) 0.5400(7) 0.4906(3) 0.1150(16) Uani 1 1 d D . . . .
C24 C 0.9354(6) 0.5793(7) 0.5059(4) 0.111(3) Uani 1 1 d . . . . .
H24 H 0.9615 0.5946 0.4768 0.133 Uiso 1 1 calc R U . . .
C25 C 0.9595(6) 0.5952(7) 0.5579(4) 0.110(4) Uani 1 1 d . . . . .
H25 H 1.0013 0.6239 0.5660 0.132 Uiso 1 1 calc R U . . .
C26 C 0.9234(5) 0.5697(5) 0.6012(3) 0.072(2) Uani 1 1 d . . . . .
C27 C 0.9499(5) 0.5846(7) 0.6610(3) 0.100(3) Uani 1 1 d . . . . .
H27 H 0.9919 0.6123 0.6698 0.120 Uiso 1 1 calc R U . . .
C28 C 0.9153(6) 0.5597(7) 0.7017(4) 0.100(3) Uani 1 1 d . . . . .
H28 H 0.9328 0.5669 0.7399 0.120 Uiso 1 1 calc R U . . .
C29 C 0.8517(6) 0.5219(7) 0.6880(4) 0.105(3) Uani 1 1 d . . . . .
H29 H 0.8265 0.5055 0.7175 0.126 Uiso 1 1 calc R U . . .
C30 C 0.8257(5) 0.5085(6) 0.6333(4) 0.088(3) Uani 1 1 d . . . . .
H30 H 0.7829 0.4833 0.6252 0.106 Uiso 1 1 calc R U . . .
C31 C 0.8616(5) 0.5313(5) 0.5906(3) 0.072(2) Uani 1 1 d . . . . .
C32 C 0.8363(6) 0.5174(6) 0.5324(4) 0.1150(16) Uani 1 1 d . . . . .
H32 H 0.7936 0.4918 0.5235 0.138 Uiso 1 1 calc R U . . .
C33 C 0.8693(4) 0.4097(6) 0.0317(3) 0.0578(19) Uani 1 1 d . . . . .
C34 C 0.8250(4) 0.3351(6) 0.0261(3) 0.0561(19) Uani 1 1 d . . . . .
H34 H 0.7806 0.3474 0.0305 0.067 Uiso 1 1 calc R U . . .
C35 C 0.8437(4) 0.2446(6) 0.0144(3) 0.066(2) Uani 1 1 d . . . . .
H35 H 0.8117 0.1952 0.0114 0.079 Uiso 1 1 calc R U . . .
C36 C 0.9071(5) 0.2210(6) 0.0069(3) 0.077(2) Uani 1 1 d . . . . .
H36 H 0.9196 0.1567 0.0000 0.092 Uiso 1 1 calc R U . . .
C37 C 0.9520(4) 0.2969(6) 0.0098(3) 0.071(2) Uani 1 1 d . . . . .
H37 H 0.9956 0.2844 0.0024 0.085 Uiso 1 1 calc R U . . .
C38 C 0.9345(4) 0.3900(6) 0.0231(3) 0.072(2) Uani 1 1 d . . . . .
H38 H 0.9662 0.4398 0.0264 0.086 Uiso 1 1 calc R U . . .
C39 C 0.8522(4) 0.5096(5) 0.0458(3) 0.064(2) Uani 1 1 d . . . . .
C40 C 0.8130(4) 0.5281(5) 0.0880(3) 0.060(2) Uani 1 1 d . . . . .
O1 O 0.7925(2) 0.4513(3) 0.11693(17) 0.0523(12) Uani 1 1 d . . . . .
C41 C 0.7996(4) 0.6227(5) 0.1064(4) 0.071(2) Uani 1 1 d . . . . .
C42 C 0.8245(5) 0.6974(6) 0.0745(5) 0.103(4) Uani 1 1 d . . . . .
H42 H 0.8141 0.7622 0.0824 0.124 Uiso 1 1 calc R U . . .
C43 C 0.8605(5) 0.6801(7) 0.0352(6) 0.126(4) Uani 1 1 d . . . . .
H43 H 0.8787 0.7331 0.0174 0.151 Uiso 1 1 calc R U . . .
C44 C 0.8748(4) 0.5863(6) 0.0170(4) 0.094(3) Uani 1 1 d . . . . .
H44 H 0.8991 0.5765 -0.0141 0.113 Uiso 1 1 calc R U . . .
C45 C 0.7637(4) 0.6522(5) 0.1531(3) 0.066(2) Uani 1 1 d . . . . .
C46 C 0.7022(4) 0.6116(5) 0.1633(3) 0.0580(19) Uani 1 1 d . . . . .
O2 O 0.6809(2) 0.5322(3) 0.13546(16) 0.0493(11) Uani 1 1 d . . . . .
C47 C 0.6639(5) 0.6514(5) 0.2026(3) 0.072(2) Uani 1 1 d . . . . .
C48 C 0.6903(6) 0.7302(7) 0.2343(4) 0.097(3) Uani 1 1 d . . . . .
H48 H 0.6650 0.7598 0.2604 0.117 Uiso 1 1 calc R U . . .
C49 C 0.7509(6) 0.7654(7) 0.2288(5) 0.112(4) Uani 1 1 d . . . . .
H49 H 0.7693 0.8141 0.2536 0.134 Uiso 1 1 calc R U . . .
C50 C 0.7850(5) 0.7303(6) 0.1874(5) 0.109(3) Uani 1 1 d . . . . .
H50 H 0.8251 0.7602 0.1816 0.130 Uiso 1 1 calc R U . . .
C51 C 0.5938(4) 0.6192(5) 0.2032(3) 0.061(2) Uani 1 1 d . . . . .
C52 C 0.5548(4) 0.5969(5) 0.1537(3) 0.066(2) Uani 1 1 d . . . . .
H52 H 0.5725 0.5976 0.1187 0.079 Uiso 1 1 calc R U . . .
C53 C 0.4902(5) 0.5737(6) 0.1560(4) 0.079(2) Uani 1 1 d . . . . .
H53 H 0.4632 0.5590 0.1223 0.095 Uiso 1 1 calc R U . . .
C54 C 0.4643(5) 0.5718(6) 0.2069(4) 0.086(3) Uani 1 1 d . . . . .
H54 H 0.4195 0.5558 0.2072 0.103 Uiso 1 1 calc R U . . .
C55 C 0.5003(5) 0.5918(6) 0.2564(4) 0.089(2) Uani 1 1 d . . . . .
H55 H 0.4818 0.5889 0.2911 0.107 Uiso 1 1 calc R U . . .
C56 C 0.5656(5) 0.6167(6) 0.2547(4) 0.089(2) Uani 1 1 d . . . . .
H56 H 0.5917 0.6324 0.2888 0.107 Uiso 1 1 calc R U . . .
C57 C 0.6388(4) 0.4287(5) -0.0269(3) 0.058(2) Uani 1 1 d . . . . .
C58 C 0.5951(4) 0.4853(6) -0.0029(3) 0.073(2) Uani 1 1 d . . . . .
H58 H 0.5722 0.4596 0.0260 0.087 Uiso 1 1 calc R U . . .
C59 C 0.5839(5) 0.5785(6) -0.0201(4) 0.084(3) Uani 1 1 d . . . . .
H59 H 0.5534 0.6163 -0.0028 0.101 Uiso 1 1 calc R U . . .
C60 C 0.6148(6) 0.6169(7) -0.0605(4) 0.102(3) Uani 1 1 d . . . . .
H60 H 0.6046 0.6807 -0.0727 0.122 Uiso 1 1 calc R U . . .
C61 C 0.6614(5) 0.5658(7) -0.0850(4) 0.097(3) Uani 1 1 d . . . . .
H61 H 0.6844 0.5948 -0.1130 0.117 Uiso 1 1 calc R U . . .
C62 C 0.6746(4) 0.4701(6) -0.0682(3) 0.077(2) Uani 1 1 d . . . . .
H62 H 0.7070 0.4339 -0.0842 0.092 Uiso 1 1 calc R U . . .
C63 C 0.6505(3) 0.3251(5) -0.0115(3) 0.0523(18) Uani 1 1 d . . . . .
C64 C 0.6587(3) 0.2940(5) 0.0445(2) 0.0406(16) Uani 1 1 d . . . . .
O3 O 0.6568(2) 0.3630(3) 0.08446(16) 0.0482(11) Uani 1 1 d . . . . .
C65 C 0.6683(3) 0.1982(5) 0.0584(2) 0.0433(16) Uani 1 1 d . . . . .
C66 C 0.6714(3) 0.1321(5) 0.0135(3) 0.0589(19) Uani 1 1 d . . . . .
H66 H 0.6784 0.0659 0.0218 0.071 Uiso 1 1 calc R U . . .
C67 C 0.6646(4) 0.1618(6) -0.0413(3) 0.069(2) Uani 1 1 d . . . . .
H67 H 0.6677 0.1164 -0.0706 0.082 Uiso 1 1 calc R U . . .
C68 C 0.6532(4) 0.2569(5) -0.0544(3) 0.065(2) Uani 1 1 d . . . . .
H68 H 0.6470 0.2766 -0.0927 0.078 Uiso 1 1 calc R U . . .
C69 C 0.6737(3) 0.1590(4) 0.1166(2) 0.0418(16) Uani 1 1 d . . . . .
C70 C 0.7148(3) 0.1987(4) 0.1621(2) 0.0420(16) Uani 1 1 d . . . . .
O4 O 0.7475(2) 0.2804(3) 0.15548(15) 0.0432(11) Uani 1 1 d . . . . .
C71 C 0.7228(3) 0.1514(4) 0.2151(2) 0.0436(16) Uani 1 1 d . . . . .
C72 C 0.6891(3) 0.0667(5) 0.2225(3) 0.0568(19) Uani 1 1 d . . . . .
H72 H 0.6954 0.0338 0.2575 0.068 Uiso 1 1 calc R U . . .
C73 C 0.6462(4) 0.0299(5) 0.1786(3) 0.066(2) Uani 1 1 d . . . . .
H73 H 0.6207 -0.0253 0.1845 0.079 Uiso 1 1 calc R U . . .
C74 C 0.6408(3) 0.0736(5) 0.1269(3) 0.0578(19) Uani 1 1 d . . . . .
H74 H 0.6136 0.0449 0.0967 0.069 Uiso 1 1 calc R U . . .
C75 C 0.7694(4) 0.1890(4) 0.2620(2) 0.0468(17) Uani 1 1 d . . . . .
C76 C 0.7505(4) 0.1936(5) 0.3175(3) 0.067(2) Uani 1 1 d . . . . .
H76 H 0.7077 0.1746 0.3237 0.080 Uiso 1 1 calc R U . . .
C77 C 0.7922(5) 0.2242(6) 0.3614(3) 0.079(2) Uani 1 1 d . . . . .
H77 H 0.7781 0.2270 0.3979 0.095 Uiso 1 1 calc R U . . .
C78 C 0.8553(6) 0.2518(7) 0.3537(3) 0.092(3) Uani 1 1 d . . . . .
H78 H 0.8846 0.2726 0.3848 0.111 Uiso 1 1 calc R U . . .
C79 C 0.8753(4) 0.2486(6) 0.3000(3) 0.079(2) Uani 1 1 d . . . . .
H79 H 0.9184 0.2672 0.2943 0.095 Uiso 1 1 calc R U . . .
C80 C 0.8322(4) 0.2184(5) 0.2548(3) 0.0573(19) Uani 1 1 d . . . . .
H80 H 0.8459 0.2177 0.2182 0.069 Uiso 1 1 calc R U . . .
C81 C 0.1688(14) 0.2141(15) 0.6242(9) 0.158(11) Uani 0.5 1 d D . P . .
H81A H 0.1783 0.2276 0.5858 0.237 Uiso 0.5 1 calc R U P . .
H81B H 0.2040 0.2396 0.6510 0.237 Uiso 0.5 1 calc R U P . .
H81C H 0.1275 0.2446 0.6308 0.237 Uiso 0.5 1 calc R U P . .
C82 C 0.1634(10) 0.1028(17) 0.6325(8) 0.178(15) Uani 0.5 1 d D . P . .
H82A H 0.1810 0.0685 0.6012 0.214 Uiso 0.5 1 calc R U P . .
H82B H 0.1888 0.0832 0.6683 0.214 Uiso 0.5 1 calc R U P . .
C83 C 0.0946(9) 0.0793(9) 0.6337(6) 0.080(6) Uani 0.5 1 d D . P . .
H83A H 0.0705 0.1044 0.5986 0.096 Uiso 0.5 1 calc R U P . .
H83B H 0.0789 0.1153 0.6653 0.096 Uiso 0.5 1 calc R U P . .
C84 C 0.0750(14) -0.0251(11) 0.6394(8) 0.22(2) Uani 0.5 1 d D . P . .
H84A H 0.1036 -0.0519 0.6717 0.261 Uiso 0.5 1 calc R U P . .
H84B H 0.0863 -0.0589 0.6054 0.261 Uiso 0.5 1 calc R U P . .
C85 C 0.0050(11) -0.0541(19) 0.6475(9) 0.138(10) Uani 0.5 1 d D . P . .
H85A H -0.0142 -0.0053 0.6703 0.208 Uiso 0.5 1 calc R U P . .
H85B H 0.0054 -0.1163 0.6668 0.208 Uiso 0.5 1 calc R U P . .
H85C H -0.0209 -0.0592 0.6107 0.208 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 O1 1.848(4) . ?
Ti1 O3 1.853(4) . ?
Ti1 O2 1.881(4) . ?
Ti1 O4 1.896(4) . ?
Ti1 N3 2.238(3) . ?
Ti1 N1 2.242(4) . ?
N1 C1 1.3900 . ?
N1 C4 1.3900 . ?
C1 C2 1.3900 . ?
C1 H1 0.9500 . ?
C2 C3 1.3900 . ?
C2 H2 0.9500 . ?
C3 N2 1.3900 . ?
C3 C5 1.482(8) . ?
N2 C4 1.3900 . ?
C4 C17 1.323(6) . ?
C5 C6 1.277(9) . ?
C5 H5 0.9500 . ?
C6 C7 1.511(10) . ?
C6 H6 0.9500 . ?
C7 C16 1.343(10) . ?
C7 C8 1.391(11) . ?
C8 C9 1.354(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.335(10) . ?
C9 H9 0.9500 . ?
C10 C11 1.3900 . ?
C10 C15 1.3900 . ?
C11 C12 1.3900 . ?
C11 H11 0.9500 . ?
C12 C13 1.3900 . ?
C12 H12 0.9500 . ?
C13 C14 1.3900 . ?
C13 H13 0.9500 . ?
C14 C15 1.3900 . ?
C14 H14 0.9500 . ?
C15 C16 1.469(9) . ?
C16 H16 0.9500 . ?
N3 C17 1.3900 . ?
N3 C18 1.3900 . ?
C17 N4 1.3900 . ?
N4 C20 1.3900 . ?
C20 C19 1.3900 . ?
C20 C21 1.439(6) . ?
C19 C18 1.3900 . ?
C19 H19 0.9500 . ?
C18 H18 0.9500 . ?
C21 C22 1.237(8) . ?
C21 H21 0.9500 . ?
C22 C23 1.381(7) . ?
C22 H22 0.9500 . ?
C23 C32 1.343(14) . ?
C23 C24 1.428(15) . ?
C24 C25 1.305(12) . ?
C24 H24 0.9500 . ?
C25 C26 1.386(11) . ?
C25 H25 0.9500 . ?
C26 C31 1.380(11) . ?
C26 C27 1.488(11) . ?
C27 C28 1.315(11) . ?
C27 H27 0.9500 . ?
C28 C29 1.417(13) . ?
C28 H28 0.9500 . ?
C29 C30 1.370(11) . ?
C29 H29 0.9500 . ?
C30 C31 1.362(11) . ?
C30 H30 0.9500 . ?
C31 C32 1.445(11) . ?
C32 H32 0.9500 . ?
C33 C34 1.380(9) . ?
C33 C38 1.408(10) . ?
C33 C39 1.482(10) . ?
C34 C35 1.354(10) . ?
C34 H34 0.9500 . ?
C35 C36 1.380(10) . ?
C35 H35 0.9500 . ?
C36 C37 1.402(10) . ?
C36 H36 0.9500 . ?
C37 C38 1.392(10) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C44 1.379(10) . ?
C39 C40 1.385(9) . ?
C40 O1 1.364(7) . ?
C40 C41 1.425(10) . ?
C41 C42 1.418(11) . ?
C41 C45 1.466(10) . ?
C42 C43 1.283(12) . ?
C42 H42 0.9500 . ?
C43 C44 1.418(13) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
C45 C50 1.403(11) . ?
C45 C46 1.432(10) . ?
C46 O2 1.338(7) . ?
C46 C47 1.408(10) . ?
C47 C48 1.408(11) . ?
C47 C51 1.513(11) . ?
C48 C49 1.362(13) . ?
C48 H48 0.9500 . ?
C49 C50 1.367(13) . ?
C49 H49 0.9500 . ?
C50 H50 0.9500 . ?
C51 C52 1.389(10) . ?
C51 C56 1.421(10) . ?
C52 C53 1.377(10) . ?
C52 H52 0.9500 . ?
C53 C54 1.383(11) . ?
C53 H53 0.9500 . ?
C54 C55 1.355(12) . ?
C54 H54 0.9500 . ?
C55 C56 1.395(12) . ?
C55 H55 0.9500 . ?
C56 H56 0.9500 . ?
C57 C58 1.369(10) . ?
C57 C62 1.420(10) . ?
C57 C63 1.500(9) . ?
C58 C59 1.373(11) . ?
C58 H58 0.9500 . ?
C59 C60 1.327(12) . ?
C59 H59 0.9500 . ?
C60 C61 1.378(13) . ?
C60 H60 0.9500 . ?
C61 C62 1.408(11) . ?
C61 H61 0.9500 . ?
C62 H62 0.9500 . ?
C63 C68 1.403(9) . ?
C63 C64 1.399(8) . ?
C64 O3 1.358(7) . ?
C64 C65 1.382(8) . ?
C65 C66 1.419(8) . ?
C65 C69 1.489(8) . ?
C66 C67 1.367(9) . ?
C66 H66 0.9500 . ?
C67 C68 1.374(9) . ?
C67 H67 0.9500 . ?
C68 H68 0.9500 . ?
C69 C74 1.403(9) . ?
C69 C70 1.415(8) . ?
C70 O4 1.340(7) . ?
C70 C71 1.422(8) . ?
C71 C72 1.389(9) . ?
C71 C75 1.487(9) . ?
C72 C73 1.393(9) . ?
C72 H72 0.9500 . ?
C73 C74 1.371(9) . ?
C73 H73 0.9500 . ?
C74 H74 0.9500 . ?
C75 C80 1.387(9) . ?
C75 C76 1.424(9) . ?
C76 C77 1.350(10) . ?
C76 H76 0.9500 . ?
C77 C78 1.390(11) . ?
C77 H77 0.9500 . ?
C78 C79 1.392(11) . ?
C78 H78 0.9500 . ?
C79 C80 1.387(9) . ?
C79 H79 0.9500 . ?
C80 H80 0.9500 . ?
C81 C82 1.565(18) . ?
C81 H81A 0.9800 . ?
C81 H81B 0.9800 . ?
C81 H81C 0.9800 . ?
C82 C83 1.461(16) . ?
C82 H82A 0.9900 . ?
C82 H82B 0.9900 . ?
C83 C84 1.517(16) . ?
C83 H83A 0.9900 . ?
C83 H83B 0.9900 . ?
C84 C85 1.531(18) . ?
C84 H84A 0.9900 . ?
C84 H84B 0.9900 . ?
C85 H85A 0.9800 . ?
C85 H85B 0.9800 . ?
C85 H85C 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O3 112.43(19) . . ?
O1 Ti1 O2 90.20(19) . . ?
O3 Ti1 O2 91.37(18) . . ?
O1 Ti1 O4 94.47(18) . . ?
O3 Ti1 O4 89.74(17) . . ?
O2 Ti1 O4 174.38(18) . . ?
O1 Ti1 N3 88.7(2) . . ?
O3 Ti1 N3 158.9(2) . . ?
O2 Ti1 N3 88.15(17) . . ?
O4 Ti1 N3 88.83(16) . . ?
O1 Ti1 N1 159.2(2) . . ?
O3 Ti1 N1 88.2(2) . . ?
O2 Ti1 N1 86.77(17) . . ?
O4 Ti1 N1 87.75(16) . . ?
N3 Ti1 N1 70.62(19) . . ?
C1 N1 C4 120.0 . . ?
C1 N1 Ti1 120.8(3) . . ?
C4 N1 Ti1 119.1(3) . . ?
N1 C1 C2 120.0 . . ?
N1 C1 H1 120.0 . . ?
C2 C1 H1 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
N2 C3 C2 120.0 . . ?
N2 C3 C5 123.4(5) . . ?
C2 C3 C5 116.6(5) . . ?
C3 N2 C4 120.0 . . ?
C17 C4 N2 126.0(4) . . ?
C17 C4 N1 113.9(4) . . ?
N2 C4 N1 120.0 . . ?
C6 C5 C3 119.8(9) . . ?
C6 C5 H5 120.1 . . ?
C3 C5 H5 120.1 . . ?
C5 C6 C7 128.4(10) . . ?
C5 C6 H6 115.8 . . ?
C7 C6 H6 115.8 . . ?
C16 C7 C8 119.6(9) . . ?
C16 C7 C6 119.0(10) . . ?
C8 C7 C6 121.4(9) . . ?
C9 C8 C7 124.0(10) . . ?
C9 C8 H8 118.0 . . ?
C7 C8 H8 118.0 . . ?
C10 C9 C8 120.4(12) . . ?
C10 C9 H9 119.7 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 122.4(8) . . ?
C9 C10 C15 117.3(8) . . ?
C11 C10 C15 120.0 . . ?
C12 C11 C10 120.0 . . ?
C12 C11 H11 120.0 . . ?
C10 C11 H11 120.0 . . ?
C11 C12 C13 120.0 . . ?
C11 C12 H12 120.0 . . ?
C13 C12 H12 120.0 . . ?
C14 C13 C12 120.0 . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 120.0 . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 120.0 . . ?
C14 C15 C16 116.6(7) . . ?
C10 C15 C16 123.4(7) . . ?
C7 C16 C15 115.2(9) . . ?
C7 C16 H16 122.3 . . ?
C15 C16 H16 122.5 . . ?
C17 N3 C18 120.0 . . ?
C17 N3 Ti1 116.0(3) . . ?
C18 N3 Ti1 124.0(3) . . ?
C4 C17 N3 120.3(4) . . ?
C4 C17 N4 119.7(4) . . ?
N3 C17 N4 120.0 . . ?
C20 N4 C17 120.0 . . ?
C19 C20 N4 120.0 . . ?
C19 C20 C21 135.5(5) . . ?
N4 C20 C21 104.4(5) . . ?
C20 C19 C18 120.0 . . ?
C20 C19 H19 120.0 . . ?
C18 C19 H19 120.0 . . ?
C19 C18 N3 120.0 . . ?
C19 C18 H18 120.0 . . ?
N3 C18 H18 120.0 . . ?
C22 C21 C20 128.3(9) . . ?
C22 C21 H21 115.9 . . ?
C20 C21 H21 115.8 . . ?
C21 C22 C23 138.1(11) . . ?
C21 C22 H22 111.0 . . ?
C23 C22 H22 111.0 . . ?
C32 C23 C22 127.2(12) . . ?
C32 C23 C24 117.5(8) . . ?
C22 C23 C24 115.3(11) . . ?
C25 C24 C23 123.4(10) . . ?
C25 C24 H24 118.3 . . ?
C23 C24 H24 118.3 . . ?
C24 C25 C26 119.3(10) . . ?
C24 C25 H25 120.4 . . ?
C26 C25 H25 120.4 . . ?
C31 C26 C25 121.7(8) . . ?
C31 C26 C27 117.5(8) . . ?
C25 C26 C27 120.8(9) . . ?
C28 C27 C26 120.2(9) . . ?
C28 C27 H27 119.9 . . ?
C26 C27 H27 119.9 . . ?
C27 C28 C29 119.3(9) . . ?
C27 C28 H28 120.3 . . ?
C29 C28 H28 120.3 . . ?
C30 C29 C28 121.7(9) . . ?
C30 C29 H29 119.1 . . ?
C28 C29 H29 119.1 . . ?
C29 C30 C31 119.7(9) . . ?
C29 C30 H30 120.1 . . ?
C31 C30 H30 120.2 . . ?
C30 C31 C26 121.4(8) . . ?
C30 C31 C32 121.5(9) . . ?
C26 C31 C32 117.1(9) . . ?
C23 C32 C31 121.1(11) . . ?
C23 C32 H32 119.4 . . ?
C31 C32 H32 119.5 . . ?
C34 C33 C38 118.1(7) . . ?
C34 C33 C39 123.7(7) . . ?
C38 C33 C39 118.1(7) . . ?
C35 C34 C33 121.2(7) . . ?
C35 C34 H34 119.4 . . ?
C33 C34 H34 119.4 . . ?
C34 C35 C36 123.0(8) . . ?
C34 C35 H35 118.5 . . ?
C36 C35 H35 118.5 . . ?
C35 C36 C37 116.4(8) . . ?
C35 C36 H36 121.8 . . ?
C37 C36 H36 121.8 . . ?
C38 C37 C36 121.7(8) . . ?
C38 C37 H37 119.2 . . ?
C36 C37 H37 119.2 . . ?
C37 C38 C33 119.5(7) . . ?
C37 C38 H38 120.3 . . ?
C33 C38 H38 120.3 . . ?
C44 C39 C40 118.6(7) . . ?
C44 C39 C33 120.6(7) . . ?
C40 C39 C33 120.9(6) . . ?
O1 C40 C39 117.6(6) . . ?
O1 C40 C41 119.1(7) . . ?
C39 C40 C41 123.0(7) . . ?
C40 O1 Ti1 138.3(4) . . ?
C42 C41 C40 114.7(8) . . ?
C42 C41 C45 116.7(7) . . ?
C40 C41 C45 128.6(7) . . ?
C43 C42 C41 121.9(8) . . ?
C43 C42 H42 119.0 . . ?
C41 C42 H42 119.0 . . ?
C42 C43 C44 123.7(8) . . ?
C42 C43 H43 118.2 . . ?
C44 C43 H43 118.1 . . ?
C39 C44 C43 117.7(9) . . ?
C39 C44 H44 121.2 . . ?
C43 C44 H44 121.2 . . ?
C50 C45 C46 115.6(8) . . ?
C50 C45 C41 120.6(8) . . ?
C46 C45 C41 123.5(7) . . ?
O2 C46 C47 118.6(7) . . ?
O2 C46 C45 119.2(6) . . ?
C47 C46 C45 122.2(7) . . ?
C46 O2 Ti1 127.9(4) . . ?
C48 C47 C46 116.9(8) . . ?
C48 C47 C51 122.6(8) . . ?
C46 C47 C51 119.8(7) . . ?
C49 C48 C47 122.3(9) . . ?
C49 C48 H48 118.8 . . ?
C47 C48 H48 118.9 . . ?
C48 C49 C50 119.5(9) . . ?
C48 C49 H49 120.3 . . ?
C50 C49 H49 120.3 . . ?
C49 C50 C45 123.2(10) . . ?
C49 C50 H50 118.4 . . ?
C45 C50 H50 118.4 . . ?
C52 C51 C56 118.6(8) . . ?
C52 C51 C47 121.5(7) . . ?
C56 C51 C47 119.8(8) . . ?
C53 C52 C51 119.4(8) . . ?
C53 C52 H52 120.3 . . ?
C51 C52 H52 120.3 . . ?
C52 C53 C54 120.6(8) . . ?
C52 C53 H53 119.7 . . ?
C54 C53 H53 119.7 . . ?
C55 C54 C53 122.5(9) . . ?
C55 C54 H54 118.7 . . ?
C53 C54 H54 118.7 . . ?
C54 C55 C56 117.6(9) . . ?
C54 C55 H55 121.2 . . ?
C56 C55 H55 121.2 . . ?
C55 C56 C51 121.4(9) . . ?
C55 C56 H56 119.3 . . ?
C51 C56 H56 119.3 . . ?
C58 C57 C62 118.4(7) . . ?
C58 C57 C63 123.0(7) . . ?
C62 C57 C63 118.6(7) . . ?
C59 C58 C57 121.0(8) . . ?
C59 C58 H58 119.5 . . ?
C57 C58 H58 119.5 . . ?
C60 C59 C58 121.3(9) . . ?
C60 C59 H59 119.3 . . ?
C58 C59 H59 119.3 . . ?
C59 C60 C61 121.1(9) . . ?
C59 C60 H60 119.5 . . ?
C61 C60 H60 119.4 . . ?
C60 C61 C62 119.2(9) . . ?
C60 C61 H61 120.4 . . ?
C62 C61 H61 120.4 . . ?
C61 C62 C57 118.9(8) . . ?
C61 C62 H62 120.5 . . ?
C57 C62 H62 120.5 . . ?
C68 C63 C64 118.7(6) . . ?
C68 C63 C57 119.3(6) . . ?
C64 C63 C57 122.1(6) . . ?
O3 C64 C65 121.8(5) . . ?
O3 C64 C63 116.4(6) . . ?
C65 C64 C63 121.8(6) . . ?
C64 O3 Ti1 133.9(4) . . ?
C64 C65 C66 117.4(6) . . ?
C64 C65 C69 124.9(5) . . ?
C66 C65 C69 117.7(6) . . ?
C67 C66 C65 121.4(7) . . ?
C67 C66 H66 119.3 . . ?
C65 C66 H66 119.3 . . ?
C66 C67 C68 120.4(7) . . ?
C66 C67 H67 119.8 . . ?
C68 C67 H67 119.8 . . ?
C67 C68 C63 120.3(7) . . ?
C67 C68 H68 119.8 . . ?
C63 C68 H68 119.8 . . ?
C74 C69 C70 117.2(6) . . ?
C74 C69 C65 119.1(5) . . ?
C70 C69 C65 123.5(5) . . ?
O4 C70 C69 120.5(5) . . ?
O4 C70 C71 119.2(5) . . ?
C69 C70 C71 120.3(5) . . ?
C70 O4 Ti1 130.2(4) . . ?
C72 C71 C70 119.7(6) . . ?
C72 C71 C75 119.6(6) . . ?
C70 C71 C75 120.6(5) . . ?
C71 C72 C73 120.1(6) . . ?
C71 C72 H72 119.9 . . ?
C73 C72 H72 119.9 . . ?
C74 C73 C72 119.8(6) . . ?
C74 C73 H73 120.1 . . ?
C72 C73 H73 120.1 . . ?
C73 C74 C69 122.7(6) . . ?
C73 C74 H74 118.7 . . ?
C69 C74 H74 118.7 . . ?
C80 C75 C76 117.2(6) . . ?
C80 C75 C71 123.0(6) . . ?
C76 C75 C71 119.8(6) . . ?
C77 C76 C75 121.6(8) . . ?
C77 C76 H76 119.2 . . ?
C75 C76 H76 119.2 . . ?
C76 C77 C78 120.6(8) . . ?
C76 C77 H77 119.7 . . ?
C78 C77 H77 119.7 . . ?
C77 C78 C79 119.4(8) . . ?
C77 C78 H78 120.3 . . ?
C79 C78 H78 120.3 . . ?
C80 C79 C78 119.9(8) . . ?
C80 C79 H79 120.0 . . ?
C78 C79 H79 120.0 . . ?
C75 C80 C79 121.3(7) . . ?
C75 C80 H80 119.3 . . ?
C79 C80 H80 119.4 . . ?
C82 C81 H81A 109.5 . . ?
C82 C81 H81B 109.5 . . ?
H81A C81 H81B 109.5 . . ?
C82 C81 H81C 109.4 . . ?
H81A C81 H81C 109.5 . . ?
H81B C81 H81C 109.5 . . ?
C83 C82 C81 107.9(19) . . ?
C83 C82 H82A 110.1 . . ?
C81 C82 H82A 110.1 . . ?
C83 C82 H82B 110.2 . . ?
C81 C82 H82B 110.1 . . ?
H82A C82 H82B 108.5 . . ?
C82 C83 C84 119.0(17) . . ?
C82 C83 H83A 107.6 . . ?
C84 C83 H83A 107.6 . . ?
C82 C83 H83B 107.5 . . ?
C84 C83 H83B 107.6 . . ?
H83A C83 H83B 107.0 . . ?
C83 C84 C85 122(2) . . ?
C83 C84 H84A 106.8 . . ?
C85 C84 H84A 106.8 . . ?
C83 C84 H84B 106.8 . . ?
C85 C84 H84B 106.9 . . ?
H84A C84 H84B 106.7 . . ?
C84 C85 H85A 109.6 . . ?
C84 C85 H85B 109.4 . . ?
H85A C85 H85B 109.5 . . ?
C84 C85 H85C 109.4 . . ?
H85A C85 H85C 109.5 . . ?
H85B C85 H85C 109.5 . . ?

_refine_diff_density_max         1.024
_refine_diff_density_min         -0.696
_refine_diff_density_rms         0.094

_shelxl_version_number           2014/6

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.010 0.217 0.186 108 7 ' '
2 0.990 0.283 0.686 108 7 ' '
3 1.010 0.717 0.314 108 7 ' '
4 0.010 0.783 0.814 108 7 ' '
_platon_squeeze_details          
;
;


####################################################################### 
# 
# 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_e3348a_a
_audit_block_doi                 10.5517/ccdc.csd.cc1l8r9x
_database_code_depnum_ccdc_archive 'CCDC 1468169'
_audit_update_record             
;
2016-06-28 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '4(C88 H58 N4 O4 Ti), C H Cl3, 4(H2 O)'
_chemical_formula_sum            'C353 H241 Cl3 N16 O20 Ti4'
_chemical_formula_weight         5360.00

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           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   21.6458(9)
_cell_length_b                   18.2186(10)
_cell_length_c                   19.9733(11)
_cell_angle_alpha                90
_cell_angle_beta                 112.479(2)
_cell_angle_gamma                90
_cell_volume                     7278.1(6)
_cell_formula_units_Z            1
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    19000
_cell_measurement_theta_min      2.54
_cell_measurement_theta_max      25.50

_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_density_meas      none
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_F_000             2787
_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    0.211
_shelx_estimated_absorpt_T_min   0.987
_shelx_estimated_absorpt_T_max   0.990
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.986
_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_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            19714
_diffrn_reflns_av_unetI/netI     0.0636
_diffrn_reflns_av_R_equivalents  0.0869
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         1.512
_diffrn_reflns_theta_max         30.155
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measured_fraction_theta_full 0.964
_diffrn_reflns_Laue_measured_fraction_max 0.915
_diffrn_reflns_Laue_measured_fraction_full 0.964
_diffrn_reflns_point_group_measured_fraction_max 0.915
_diffrn_reflns_point_group_measured_fraction_full 0.964
_reflns_number_total             19714
_reflns_number_gt                11199
_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.
Because we didn't identify the solvents we used the squezze
command. We didn't put the hydrogen on the solvent because
of the disorder
;

_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-2014/6 (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)+(0.1988P)²+0.0062P] 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         19714
_refine_ls_number_parameters     915
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.1491
_refine_ls_R_factor_gt           0.0912
_refine_ls_wR_factor_ref         0.3117
_refine_ls_wR_factor_gt          0.2751
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_restrained_S_all      1.078
_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 0.0000 0.76807(4) 0.2500 0.02736(19) Uani 1 2 d S T P . .
N1 N 0.00802(12) 0.66907(12) 0.31916(13) 0.0271(5) Uani 1 1 d . . . . .
C1 C 0.00610(14) 0.60254(14) 0.28924(15) 0.0262(6) Uani 1 1 d . . . . .
N2 N 0.01435(13) 0.53922(12) 0.32281(13) 0.0293(5) Uani 1 1 d . . . . .
C2 C 0.02811(16) 0.54085(15) 0.39408(17) 0.0325(6) Uani 1 1 d . . . . .
C3 C 0.03342(16) 0.60683(16) 0.43043(17) 0.0348(7) Uani 1 1 d . . . . .
H3 H 0.0446 0.6082 0.4813 0.042 Uiso 1 1 calc R U . . .
C4 C 0.02184(16) 0.67061(16) 0.38997(17) 0.0324(6) Uani 1 1 d . . . . .
H4 H 0.0238 0.7165 0.4133 0.039 Uiso 1 1 calc R U . . .
C5 C 0.03595(18) 0.46987(17) 0.43109(18) 0.0392(7) Uani 1 1 d . . . . .
H5 H 0.0550 0.4686 0.4825 0.047 Uiso 1 1 calc R U . . .
C6 C 0.01719(19) 0.40741(17) 0.39485(18) 0.0424(8) Uani 1 1 d . . . . .
H6 H -0.0002 0.4101 0.3435 0.051 Uiso 1 1 calc R U . . .
C7 C 0.0210(2) 0.33388(18) 0.42755(19) 0.0459(8) Uani 1 1 d . . . . .
C8 C -0.0364(2) 0.29138(19) 0.4082(2) 0.0511(9) Uani 1 1 d . . . . .
C9 C -0.0982(3) 0.3129(3) 0.3546(3) 0.0705(13) Uani 1 1 d . . . . .
H9 H -0.1017 0.3594 0.3320 0.085 Uiso 1 1 calc R U . . .
C10 C -0.1533(3) 0.2681(3) 0.3342(4) 0.0949(18) Uani 1 1 d . . . . .
H10 H -0.1938 0.2827 0.2964 0.114 Uiso 1 1 calc R U . . .
C11 C -0.1494(3) 0.2003(3) 0.3695(4) 0.096(2) Uani 1 1 d . . . . .
H11 H -0.1876 0.1694 0.3556 0.115 Uiso 1 1 calc R U . . .
C12 C -0.0932(3) 0.1793(3) 0.4219(3) 0.0772(15) Uani 1 1 d . . . . .
H12 H -0.0921 0.1340 0.4457 0.093 Uiso 1 1 calc R U . . .
C13 C -0.0358(2) 0.2221(2) 0.4428(2) 0.0575(11) Uani 1 1 d . . . . .
C14 C 0.0233(3) 0.2004(2) 0.4974(3) 0.0665(13) Uani 1 1 d . . . . .
H14 H 0.0237 0.1565 0.5232 0.080 Uiso 1 1 calc R U . . .
C15 C 0.0818(3) 0.2404(2) 0.5157(2) 0.0610(12) Uani 1 1 d . . . . .
C16 C 0.1430(3) 0.2163(3) 0.5706(3) 0.0833(16) Uani 1 1 d . . . . .
H16 H 0.1432 0.1734 0.5976 0.100 Uiso 1 1 calc R U . . .
C17 C 0.2002(4) 0.2534(4) 0.5846(4) 0.102(2) Uani 1 1 d . . . . .
H17 H 0.2400 0.2370 0.6223 0.122 Uiso 1 1 calc R U . . .
C18 C 0.2022(3) 0.3171(3) 0.5439(3) 0.0791(15) Uani 1 1 d . . . . .
H18 H 0.2435 0.3407 0.5517 0.095 Uiso 1 1 calc R U . . .
C19 C 0.1442(2) 0.3437(2) 0.4938(2) 0.0591(10) Uani 1 1 d . . . . .
H19 H 0.1453 0.3872 0.4681 0.071 Uiso 1 1 calc R U . . .
C20 C 0.0823(2) 0.30807(19) 0.4793(2) 0.0490(9) Uani 1 1 d . . . . .
C21 C -0.04526(18) 0.96269(17) 0.3472(2) 0.0419(8) Uani 1 1 d . . . . .
C22 C -0.0821(2) 0.9592(3) 0.2731(2) 0.0655(12) Uani 1 1 d . . . . .
H22 H -0.0616 0.9404 0.2422 0.079 Uiso 1 1 calc R U . . .
C23 C -0.1481(2) 0.9826(3) 0.2431(3) 0.0761(14) Uani 1 1 d . . . . .
H23 H -0.1718 0.9814 0.1921 0.091 Uiso 1 1 calc R U . . .
C24 C -0.1790(2) 1.0071(2) 0.2865(3) 0.0589(11) Uani 1 1 d . . . . .
H24 H -0.2235 1.0250 0.2660 0.071 Uiso 1 1 calc R U . . .
C25 C -0.1455(2) 1.0058(2) 0.3600(3) 0.0589(11) Uani 1 1 d . . . . .
H25 H -0.1679 1.0200 0.3906 0.071 Uiso 1 1 calc R U . . .
C26 C -0.0794(2) 0.98419(19) 0.3902(2) 0.0504(9) Uani 1 1 d . . . . .
H26 H -0.0569 0.9840 0.4414 0.060 Uiso 1 1 calc R U . . .
C27 C 0.02694(18) 0.94468(17) 0.37986(18) 0.0393(7) Uani 1 1 d . . . . .
O1 O 0.00677(11) 0.82626(11) 0.32813(12) 0.0334(5) Uani 1 1 d . . . . .
C28 C 0.05160(16) 0.87583(16) 0.37041(17) 0.0342(7) Uani 1 1 d . . . . .
C29 C 0.12017(17) 0.85885(18) 0.40581(18) 0.0390(7) Uani 1 1 d . . . . .
C30 C 0.16268(19) 0.9140(2) 0.4448(2) 0.0509(9) Uani 1 1 d . . . . .
H30 H 0.2092 0.9041 0.4673 0.061 Uiso 1 1 calc R U . . .
C31 C 0.1394(2) 0.9835(2) 0.4522(2) 0.0574(10) Uani 1 1 d . . . . .
H31 H 0.1696 1.0209 0.4781 0.069 Uiso 1 1 calc R U . . .
C32 C 0.0720(2) 0.99703(19) 0.4214(2) 0.0518(10) Uani 1 1 d . . . . .
H32 H 0.0556 1.0435 0.4286 0.062 Uiso 1 1 calc R U . . .
C33 C 0.14927(16) 0.78338(19) 0.40987(19) 0.0404(7) Uani 1 1 d . . . . .
C34 C 0.13729(15) 0.73735(17) 0.34949(17) 0.0337(6) Uani 1 1 d . . . . .
O2 O 0.09426(11) 0.75821(11) 0.28394(11) 0.0317(5) Uani 1 1 d . . . . .
C35 C 0.16984(16) 0.66873(18) 0.35880(19) 0.0388(7) Uani 1 1 d . . . . .
C36 C 0.21218(18) 0.6476(2) 0.4288(2) 0.0506(9) Uani 1 1 d . . . . .
H36 H 0.2346 0.6017 0.4355 0.061 Uiso 1 1 calc R U . . .
C37 C 0.2222(2) 0.6916(2) 0.4881(2) 0.0577(11) Uani 1 1 d . . . . .
H37 H 0.2501 0.6757 0.5353 0.069 Uiso 1 1 calc R U . . .
C38 C 0.19149(19) 0.7583(2) 0.4781(2) 0.0518(9) Uani 1 1 d . . . . .
H38 H 0.1991 0.7889 0.5190 0.062 Uiso 1 1 calc R U . . .
C39 C 0.16186(15) 0.61782(18) 0.2978(2) 0.0384(7) Uani 1 1 d . . . . .
C40 C 0.16409(17) 0.54179(19) 0.3095(2) 0.0484(9) Uani 1 1 d . . . . .
H40 H 0.1673 0.5235 0.3553 0.058 Uiso 1 1 calc R U . . .
C41 C 0.1616(2) 0.4930(2) 0.2554(3) 0.0624(12) Uani 1 1 d . . . . .
H41 H 0.1647 0.4417 0.2648 0.075 Uiso 1 1 calc R U . . .
C42 C 0.1549(2) 0.5178(2) 0.1894(3) 0.0636(12) Uani 1 1 d . . . . .
H42 H 0.1522 0.4841 0.1521 0.076 Uiso 1 1 calc R U . . .
C43 C 0.15183(19) 0.5931(2) 0.1758(2) 0.0544(10) Uani 1 1 d . . . . .
H43 H 0.1475 0.6108 0.1295 0.065 Uiso 1 1 calc R U . . .
C44 C 0.15513(17) 0.64186(19) 0.2300(2) 0.0421(8) Uani 1 1 d . . . . .
H44 H 0.1527 0.6931 0.2203 0.051 Uiso 1 1 calc R U . . .
Ti2 Ti 0.5000 0.26360(3) 0.7500 0.02541(18) Uani 1 2 d S T P . .
N3 N 0.50741(12) 0.16453(12) 0.68796(13) 0.0275(5) Uani 1 1 d . . . . .
C45 C 0.50705(14) 0.09760(14) 0.71630(15) 0.0257(6) Uani 1 1 d . . . . .
N4 N 0.51979(13) 0.03488(12) 0.69115(13) 0.0311(5) Uani 1 1 d . . . . .
C46 C 0.53525(17) 0.03871(16) 0.63206(17) 0.0353(7) Uani 1 1 d . . . . .
C47 C 0.53543(19) 0.10468(17) 0.59875(18) 0.0402(8) Uani 1 1 d . . . . .
H47 H 0.5453 0.1068 0.5563 0.048 Uiso 1 1 calc R U . . .
C48 C 0.52103(17) 0.16765(16) 0.62821(17) 0.0350(7) Uani 1 1 d . . . . .
H48 H 0.5208 0.2137 0.6058 0.042 Uiso 1 1 calc R U . . .
C49 C 0.55225(19) -0.02988(17) 0.60533(18) 0.0415(8) Uani 1 1 d . . . . .
H49 H 0.5664 -0.0272 0.5659 0.050 Uiso 1 1 calc R U . . .
C50 C 0.54928(19) -0.09525(17) 0.63221(19) 0.0443(8) Uani 1 1 d . . . . .
H50 H 0.5378 -0.0976 0.6735 0.053 Uiso 1 1 calc R U . . .
C51 C 0.5626(2) -0.16527(17) 0.60261(19) 0.0453(8) Uani 1 1 d . . . . .
C52 C 0.5073(2) -0.21181(17) 0.56889(18) 0.0448(8) Uani 1 1 d . . . . .
C53 C 0.4419(2) -0.1937(2) 0.5615(2) 0.0580(11) Uani 1 1 d . . . . .
H53 H 0.4343 -0.1485 0.5808 0.070 Uiso 1 1 calc R U . . .
C54 C 0.3885(3) -0.2396(3) 0.5269(3) 0.0723(13) Uani 1 1 d . . . . .
H54 H 0.3447 -0.2254 0.5218 0.087 Uiso 1 1 calc R U . . .
C55 C 0.3992(3) -0.3081(3) 0.4991(3) 0.0802(16) Uani 1 1 d . . . . .
H55 H 0.3628 -0.3407 0.4770 0.096 Uiso 1 1 calc R U . . .
C56 C 0.4618(3) -0.3268(2) 0.5041(2) 0.0701(14) Uani 1 1 d . . . . .
H56 H 0.4682 -0.3722 0.4844 0.084 Uiso 1 1 calc R U . . .
C57 C 0.5180(2) -0.27997(19) 0.5382(2) 0.0548(10) Uani 1 1 d . . . . .
C58 C 0.5807(3) -0.2973(2) 0.5408(3) 0.0703(13) Uani 1 1 d . . . . .
H58 H 0.5866 -0.3413 0.5184 0.084 Uiso 1 1 calc R U . . .
C59 C 0.6351(3) -0.2530(3) 0.5747(3) 0.0712(14) Uani 1 1 d . . . . .
C60 C 0.6980(4) -0.2714(3) 0.5771(4) 0.111(2) Uani 1 1 d . . . . .
H60 H 0.7029 -0.3145 0.5528 0.133 Uiso 1 1 calc R U . . .
C61 C 0.7545(4) -0.2289(4) 0.6139(5) 0.130(3) Uani 1 1 d . . . . .
H61 H 0.7971 -0.2429 0.6149 0.156 Uiso 1 1 calc R U . . .
C62 C 0.7468(3) -0.1629(3) 0.6505(4) 0.0924(18) Uani 1 1 d . . . . .
H62 H 0.7849 -0.1344 0.6779 0.111 Uiso 1 1 calc R U . . .
C63 C 0.6858(2) -0.1423(3) 0.6455(3) 0.0712(13) Uani 1 1 d . . . . .
H63 H 0.6816 -0.0978 0.6682 0.085 Uiso 1 1 calc R U . . .
C64 C 0.6254(2) -0.1849(2) 0.6069(2) 0.0609(11) Uani 1 1 d . . . . .
C65 C 0.55177(16) 0.45551(15) 0.88790(17) 0.0320(6) Uani 1 1 d . . . . .
C66 C 0.59178(19) 0.4433(2) 0.8482(2) 0.0472(9) Uani 1 1 d . . . . .
H66 H 0.5719 0.4251 0.8000 0.057 Uiso 1 1 calc R U . . .
C67 C 0.6592(2) 0.4572(2) 0.8775(2) 0.0608(11) Uani 1 1 d . . . . .
H67 H 0.6858 0.4479 0.8499 0.073 Uiso 1 1 calc R U . . .
C68 C 0.6889(2) 0.4848(2) 0.9478(2) 0.0578(11) Uani 1 1 d . . . . .
H68 H 0.7355 0.4950 0.9679 0.069 Uiso 1 1 calc R U . . .
C69 C 0.6509(2) 0.4972(2) 0.9878(2) 0.0512(9) Uani 1 1 d . . . . .
H69 H 0.6710 0.5156 1.0358 0.061 Uiso 1 1 calc R U . . .
C70 C 0.58270(18) 0.48284(17) 0.95787(19) 0.0418(8) Uani 1 1 d . . . . .
H70 H 0.5566 0.4919 0.9859 0.050 Uiso 1 1 calc R U . . .
C71 C 0.47846(16) 0.44128(15) 0.85790(16) 0.0323(7) Uani 1 1 d . . . . .
C72 C 0.45162(15) 0.37267(14) 0.82843(15) 0.0271(6) Uani 1 1 d . . . . .
O3 O 0.49483(10) 0.32087(10) 0.82407(11) 0.0304(4) Uani 1 1 d . . . . .
C73 C 0.38316(16) 0.35786(16) 0.80690(16) 0.0323(6) Uani 1 1 d . . . . .
C74 C 0.34142(18) 0.41534(17) 0.81009(19) 0.0383(7) Uani 1 1 d . . . . .
H74 H 0.2947 0.4071 0.7945 0.046 Uiso 1 1 calc R U . . .
C75 C 0.36743(18) 0.48436(18) 0.8358(2) 0.0437(8) Uani 1 1 d . . . . .
H75 H 0.3382 0.5232 0.8359 0.052 Uiso 1 1 calc R U . . .
C76 C 0.43491(18) 0.49654(17) 0.86085(18) 0.0392(8) Uani 1 1 d . . . . .
H76 H 0.4523 0.5431 0.8805 0.047 Uiso 1 1 calc R U . . .
C77 C 0.35180(16) 0.28374(17) 0.78667(17) 0.0343(7) Uani 1 1 d . . . . .
C78 C 0.36293(15) 0.23622(16) 0.73656(17) 0.0321(6) Uani 1 1 d . . . . .
O4 O 0.40631(11) 0.25521(11) 0.70589(11) 0.0305(4) Uani 1 1 d . . . . .
C79 C 0.32956(16) 0.16732(17) 0.71842(19) 0.0383(7) Uani 1 1 d . . . . .
C80 C 0.28608(18) 0.14853(19) 0.7525(2) 0.0486(9) Uani 1 1 d . . . . .
H80 H 0.2632 0.1029 0.7411 0.058 Uiso 1 1 calc R U . . .
C81 C 0.2753(2) 0.1940(2) 0.8019(2) 0.0520(9) Uani 1 1 d . . . . .
H81 H 0.2460 0.1795 0.8247 0.062 Uiso 1 1 calc R U . . .
C82 C 0.30763(18) 0.26085(19) 0.8180(2) 0.0440(8) Uani 1 1 d . . . . .
H82 H 0.2994 0.2923 0.8517 0.053 Uiso 1 1 calc R U . . .
C83 C 0.33748(16) 0.11623(18) 0.6644(2) 0.0409(8) Uani 1 1 d . . . . .
C84 C 0.34349(19) 0.1408(2) 0.6009(2) 0.0520(9) Uani 1 1 d . . . . .
H84 H 0.3455 0.1920 0.5928 0.062 Uiso 1 1 calc R U . . .
C85 C 0.3466(2) 0.0913(3) 0.5495(3) 0.0648(12) Uani 1 1 d . . . . .
H85 H 0.3498 0.1087 0.5062 0.078 Uiso 1 1 calc R U . . .
C86 C 0.3449(3) 0.0164(3) 0.5614(3) 0.0786(15) Uani 1 1 d . . . . .
H86 H 0.3467 -0.0176 0.5261 0.094 Uiso 1 1 calc R U . . .
C87 C 0.3406(2) -0.0081(2) 0.6241(3) 0.0708(14) Uani 1 1 d . . . . .
H87 H 0.3403 -0.0594 0.6328 0.085 Uiso 1 1 calc R U . . .
C88 C 0.33668(19) 0.04103(19) 0.6751(3) 0.0538(10) Uani 1 1 d . . . . .
H88 H 0.3334 0.0230 0.7182 0.065 Uiso 1 1 calc R U . . .
C90 C 1.0000 0.1925(5) 0.2500 0.100 Uani 0.5 2 d DS T P . .
Cl1 Cl 1.0513(4) 0.1358(5) 0.2422(8) 0.219(7) Uani 0.25 1 d D . P . .
Cl2 Cl 0.9315(3) 0.1863(4) 0.1741(3) 0.118(3) Uani 0.25 1 d D . P . .
Cl3 Cl 1.0256(2) 0.2770(3) 0.2638(3) 0.118(3) Uani 0.25 1 d D . P . .
O5 O 0.3394(3) 0.7777(3) 0.6913(3) 0.0698(17) Uani 0.5 1 d . . P . .
O6 O 0.4076(4) 0.6394(3) 0.6700(5) 0.105(3) 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 O1 1.845(2) 2 ?
Ti1 O1 1.845(2) . ?
Ti1 O2 1.897(2) 2 ?
Ti1 O2 1.897(2) . ?
Ti1 N1 2.238(2) . ?
Ti1 N1 2.238(2) 2 ?
N1 C4 1.329(4) . ?
N1 C1 1.345(3) . ?
C1 N2 1.312(3) . ?
C1 C1 1.487(6) 2 ?
N2 C2 1.339(4) . ?
C2 C3 1.386(4) . ?
C2 C5 1.467(4) . ?
C3 C4 1.382(4) . ?
C3 H3 0.9500 . ?
C4 H4 0.9500 . ?
C5 C6 1.326(5) . ?
C5 H5 0.9500 . ?
C6 C7 1.479(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.389(5) . ?
C7 C20 1.415(5) . ?
C8 C9 1.412(6) . ?
C8 C13 1.435(5) . ?
C9 C10 1.371(7) . ?
C9 H9 0.9500 . ?
C10 C11 1.409(9) . ?
C10 H10 0.9500 . ?
C11 C12 1.321(8) . ?
C11 H11 0.9500 . ?
C12 C13 1.389(7) . ?
C12 H12 0.9500 . ?
C13 C14 1.384(7) . ?
C14 C15 1.384(7) . ?
C14 H14 0.9500 . ?
C15 C16 1.427(7) . ?
C15 C20 1.435(5) . ?
C16 C17 1.342(9) . ?
C16 H16 0.9500 . ?
C17 C18 1.428(8) . ?
C17 H17 0.9500 . ?
C18 C19 1.360(6) . ?
C18 H18 0.9500 . ?
C19 C20 1.415(6) . ?
C19 H19 0.9500 . ?
C21 C26 1.387(5) . ?
C21 C22 1.389(6) . ?
C21 C27 1.482(5) . ?
C22 C23 1.389(6) . ?
C22 H22 0.9500 . ?
C23 C24 1.357(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.365(6) . ?
C24 H24 0.9500 . ?
C25 C26 1.380(6) . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C27 C32 1.389(5) . ?
C27 C28 1.404(4) . ?
O1 C28 1.358(4) . ?
C28 C29 1.413(5) . ?
C29 C30 1.384(5) . ?
C29 C33 1.502(5) . ?
C30 C31 1.392(6) . ?
C30 H30 0.9500 . ?
C31 C32 1.371(6) . ?
C31 H31 0.9500 . ?
C32 H32 0.9500 . ?
C33 C38 1.396(5) . ?
C33 C34 1.409(5) . ?
C34 O2 1.339(4) . ?
C34 C35 1.412(4) . ?
C35 C36 1.401(5) . ?
C35 C39 1.487(5) . ?
C36 C37 1.378(6) . ?
C36 H36 0.9500 . ?
C37 C38 1.363(6) . ?
C37 H37 0.9500 . ?
C38 H38 0.9500 . ?
C39 C44 1.377(5) . ?
C39 C40 1.403(5) . ?
C40 C41 1.385(6) . ?
C40 H40 0.9500 . ?
C41 C42 1.347(7) . ?
C41 H41 0.9500 . ?
C42 C43 1.395(6) . ?
C42 H42 0.9500 . ?
C43 C44 1.380(5) . ?
C43 H43 0.9500 . ?
C44 H44 0.9500 . ?
Ti2 O3 1.848(2) 2_656 ?
Ti2 O3 1.8484(19) . ?
Ti2 O4 1.883(2) . ?
Ti2 O4 1.883(2) 2_656 ?
Ti2 N3 2.230(2) . ?
Ti2 N3 2.230(2) 2_656 ?
N3 C48 1.335(4) . ?
N3 C45 1.346(3) . ?
C45 N4 1.319(3) . ?
C45 C45 1.490(5) 2_656 ?
N4 C46 1.346(4) . ?
C46 C47 1.375(4) . ?
C46 C49 1.460(4) . ?
C47 C48 1.378(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C50 1.318(5) . ?
C49 H49 0.9500 . ?
C50 C51 1.480(4) . ?
C50 H50 0.9500 . ?
C51 C64 1.377(6) . ?
C51 C52 1.410(5) . ?
C52 C53 1.405(6) . ?
C52 C57 1.442(5) . ?
C53 C54 1.379(6) . ?
C53 H53 0.9500 . ?
C54 C55 1.421(7) . ?
C54 H54 0.9500 . ?
C55 C56 1.363(7) . ?
C55 H55 0.9500 . ?
C56 C57 1.427(6) . ?
C56 H56 0.9500 . ?
C57 C58 1.375(7) . ?
C58 C59 1.373(7) . ?
C58 H58 0.9500 . ?
C59 C60 1.387(8) . ?
C59 C64 1.447(5) . ?
C60 C61 1.395(10) . ?
C60 H60 0.9500 . ?
C61 C62 1.449(8) . ?
C61 H61 0.9500 . ?
C62 C63 1.340(7) . ?
C62 H62 0.9500 . ?
C63 C64 1.461(6) . ?
C63 H63 0.9500 . ?
C65 C70 1.391(4) . ?
C65 C66 1.398(5) . ?
C65 C71 1.489(5) . ?
C66 C67 1.373(6) . ?
C66 H66 0.9500 . ?
C67 C68 1.397(6) . ?
C67 H67 0.9500 . ?
C68 C69 1.366(6) . ?
C68 H68 0.9500 . ?
C69 C70 1.389(5) . ?
C69 H69 0.9500 . ?
C70 H70 0.9500 . ?
C71 C76 1.396(4) . ?
C71 C72 1.409(4) . ?
C72 O3 1.355(3) . ?
C72 C73 1.402(4) . ?
C73 C74 1.400(4) . ?
C73 C77 1.496(4) . ?
C74 C75 1.393(5) . ?
C74 H74 0.9500 . ?
C75 C76 1.369(5) . ?
C75 H75 0.9500 . ?
C76 H76 0.9500 . ?
C77 C82 1.392(5) . ?
C77 C78 1.412(4) . ?
C78 O4 1.348(4) . ?
C78 C79 1.424(4) . ?
C79 C80 1.398(5) . ?
C79 C83 1.484(5) . ?
C80 C81 1.375(5) . ?
C80 H80 0.9500 . ?
C81 C82 1.380(5) . ?
C81 H81 0.9500 . ?
C82 H82 0.9500 . ?
C83 C88 1.388(5) . ?
C83 C84 1.397(5) . ?
C84 C85 1.387(5) . ?
C84 H84 0.9500 . ?
C85 C86 1.389(7) . ?
C85 H85 0.9500 . ?
C86 C87 1.367(8) . ?
C86 H86 0.9500 . ?
C87 C88 1.382(6) . ?
C87 H87 0.9500 . ?
C88 H88 0.9500 . ?
C90 Cl1 1.566(7) . ?
C90 Cl1 1.566(7) 2_755 ?
C90 Cl3 1.624(8) 2_755 ?
C90 Cl3 1.625(8) . ?
C90 Cl2 1.670(5) . ?
C90 Cl2 1.670(5) 2_755 ?
Cl1 Cl2 1.816(14) 2_755 ?
Cl1 Cl1 2.36(2) 2_755 ?
Cl2 Cl1 1.816(14) 2_755 ?
Cl2 Cl3 2.061(9) 2_755 ?
Cl3 Cl3 1.032(10) 2_755 ?
Cl3 Cl2 2.061(9) 2_755 ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ti1 O1 109.88(13) 2 . ?
O1 Ti1 O2 91.46(9) 2 2 ?
O1 Ti1 O2 94.79(9) . 2 ?
O1 Ti1 O2 94.78(9) 2 . ?
O1 Ti1 O2 91.46(9) . . ?
O2 Ti1 O2 169.13(12) 2 . ?
O1 Ti1 N1 161.32(9) 2 . ?
O1 Ti1 N1 88.77(9) . . ?
O2 Ti1 N1 87.89(9) 2 . ?
O2 Ti1 N1 83.34(9) . . ?
O1 Ti1 N1 88.77(9) 2 2 ?
O1 Ti1 N1 161.32(9) . 2 ?
O2 Ti1 N1 83.34(9) 2 2 ?
O2 Ti1 N1 87.89(9) . 2 ?
N1 Ti1 N1 72.60(12) . 2 ?
C4 N1 C1 116.6(2) . . ?
C4 N1 Ti1 124.94(18) . . ?
C1 N1 Ti1 118.04(18) . . ?
N2 C1 N1 126.2(3) . . ?
N2 C1 C1 118.26(16) . 2 ?
N1 C1 C1 115.55(16) . 2 ?
C1 N2 C2 117.1(2) . . ?
N2 C2 C3 121.1(3) . . ?
N2 C2 C5 116.9(3) . . ?
C3 C2 C5 122.0(3) . . ?
C4 C3 C2 117.5(3) . . ?
C4 C3 H3 121.2 . . ?
C2 C3 H3 121.2 . . ?
N1 C4 C3 121.4(3) . . ?
N1 C4 H4 119.3 . . ?
C3 C4 H4 119.3 . . ?
C6 C5 C2 121.9(3) . . ?
C6 C5 H5 119.0 . . ?
C2 C5 H5 119.0 . . ?
C5 C6 C7 125.6(3) . . ?
C5 C6 H6 117.2 . . ?
C7 C6 H6 117.2 . . ?
C8 C7 C20 120.5(3) . . ?
C8 C7 C6 119.3(3) . . ?
C20 C7 C6 120.1(3) . . ?
C7 C8 C9 122.9(4) . . ?
C7 C8 C13 120.9(4) . . ?
C9 C8 C13 116.1(4) . . ?
C10 C9 C8 121.6(5) . . ?
C10 C9 H9 119.2 . . ?
C8 C9 H9 119.2 . . ?
C9 C10 C11 119.6(6) . . ?
C9 C10 H10 120.2 . . ?
C11 C10 H10 120.2 . . ?
C12 C11 C10 120.7(5) . . ?
C12 C11 H11 119.6 . . ?
C10 C11 H11 119.6 . . ?
C11 C12 C13 121.5(5) . . ?
C11 C12 H12 119.3 . . ?
C13 C12 H12 119.3 . . ?
C14 C13 C12 121.8(4) . . ?
C14 C13 C8 117.8(4) . . ?
C12 C13 C8 120.4(5) . . ?
C13 C14 C15 122.3(4) . . ?
C13 C14 H14 118.8 . . ?
C15 C14 H14 118.8 . . ?
C14 C15 C16 121.9(4) . . ?
C14 C15 C20 120.1(4) . . ?
C16 C15 C20 118.0(5) . . ?
C17 C16 C15 121.1(5) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 121.1(5) . . ?
C16 C17 H17 119.4 . . ?
C18 C17 H17 119.4 . . ?
C19 C18 C17 119.2(5) . . ?
C19 C18 H18 120.4 . . ?
C17 C18 H18 120.4 . . ?
C18 C19 C20 121.5(5) . . ?
C18 C19 H19 119.2 . . ?
C20 C19 H19 119.2 . . ?
C7 C20 C19 123.2(3) . . ?
C7 C20 C15 118.0(4) . . ?
C19 C20 C15 118.7(4) . . ?
C26 C21 C22 116.7(4) . . ?
C26 C21 C27 120.8(3) . . ?
C22 C21 C27 122.6(3) . . ?
C21 C22 C23 121.5(4) . . ?
C21 C22 H22 119.3 . . ?
C23 C22 H22 119.3 . . ?
C24 C23 C22 120.1(5) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 119.5(4) . . ?
C23 C24 H24 120.3 . . ?
C25 C24 H24 120.3 . . ?
C24 C25 C26 120.8(4) . . ?
C24 C25 H25 119.6 . . ?
C26 C25 H25 119.6 . . ?
C25 C26 C21 121.2(4) . . ?
C25 C26 H26 119.4 . . ?
C21 C26 H26 119.4 . . ?
C32 C27 C28 118.5(3) . . ?
C32 C27 C21 119.5(3) . . ?
C28 C27 C21 122.0(3) . . ?
C28 O1 Ti1 135.6(2) . . ?
O1 C28 C27 117.4(3) . . ?
O1 C28 C29 122.0(3) . . ?
C27 C28 C29 120.6(3) . . ?
C30 C29 C28 117.9(3) . . ?
C30 C29 C33 117.3(3) . . ?
C28 C29 C33 124.5(3) . . ?
C29 C30 C31 122.0(4) . . ?
C29 C30 H30 119.0 . . ?
C31 C30 H30 119.0 . . ?
C32 C31 C30 118.9(3) . . ?
C32 C31 H31 120.6 . . ?
C30 C31 H31 120.6 . . ?
C31 C32 C27 121.9(3) . . ?
C31 C32 H32 119.1 . . ?
C27 C32 H32 119.1 . . ?
C38 C33 C34 118.6(3) . . ?
C38 C33 C29 117.2(3) . . ?
C34 C33 C29 124.2(3) . . ?
O2 C34 C33 120.0(3) . . ?
O2 C34 C35 120.4(3) . . ?
C33 C34 C35 119.7(3) . . ?
C34 O2 Ti1 128.9(2) . . ?
C36 C35 C34 118.5(3) . . ?
C36 C35 C39 118.2(3) . . ?
C34 C35 C39 123.3(3) . . ?
C37 C36 C35 121.8(3) . . ?
C37 C36 H36 119.1 . . ?
C35 C36 H36 119.1 . . ?
C38 C37 C36 119.0(4) . . ?
C38 C37 H37 120.5 . . ?
C36 C37 H37 120.5 . . ?
C37 C38 C33 122.4(4) . . ?
C37 C38 H38 118.8 . . ?
C33 C38 H38 118.8 . . ?
C44 C39 C40 117.5(3) . . ?
C44 C39 C35 122.9(3) . . ?
C40 C39 C35 119.6(3) . . ?
C41 C40 C39 121.0(4) . . ?
C41 C40 H40 119.5 . . ?
C39 C40 H40 119.5 . . ?
C42 C41 C40 120.3(4) . . ?
C42 C41 H41 119.8 . . ?
C40 C41 H41 119.8 . . ?
C41 C42 C43 120.0(4) . . ?
C41 C42 H42 120.0 . . ?
C43 C42 H42 120.0 . . ?
C44 C43 C42 119.7(4) . . ?
C44 C43 H43 120.1 . . ?
C42 C43 H43 120.1 . . ?
C39 C44 C43 121.4(3) . . ?
C39 C44 H44 119.3 . . ?
C43 C44 H44 119.3 . . ?
O3 Ti2 O3 111.27(13) 2_656 . ?
O3 Ti2 O4 93.17(9) 2_656 . ?
O3 Ti2 O4 92.08(9) . . ?
O3 Ti2 O4 92.08(9) 2_656 2_656 ?
O3 Ti2 O4 93.17(9) . 2_656 ?
O4 Ti2 O4 170.69(12) . 2_656 ?
O3 Ti2 N3 88.45(8) 2_656 . ?
O3 Ti2 N3 160.23(9) . . ?
O4 Ti2 N3 88.15(9) . . ?
O4 Ti2 N3 84.31(9) 2_656 . ?
O3 Ti2 N3 160.23(9) 2_656 2_656 ?
O3 Ti2 N3 88.44(8) . 2_656 ?
O4 Ti2 N3 84.31(9) . 2_656 ?
O4 Ti2 N3 88.15(9) 2_656 2_656 ?
N3 Ti2 N3 71.90(12) . 2_656 ?
C48 N3 C45 116.9(2) . . ?
C48 N3 Ti2 123.34(18) . . ?
C45 N3 Ti2 119.12(18) . . ?
N4 C45 N3 126.1(2) . . ?
N4 C45 C45 119.27(16) . 2_656 ?
N3 C45 C45 114.59(15) . 2_656 ?
C45 N4 C46 116.6(2) . . ?
N4 C46 C47 121.2(3) . . ?
N4 C46 C49 117.3(3) . . ?
C47 C46 C49 121.6(3) . . ?
C46 C47 C48 118.6(3) . . ?
C46 C47 H47 120.7 . . ?
C48 C47 H47 120.7 . . ?
N3 C48 C47 120.6(3) . . ?
N3 C48 H48 119.7 . . ?
C47 C48 H48 119.7 . . ?
C50 C49 C46 124.5(3) . . ?
C50 C49 H49 117.8 . . ?
C46 C49 H49 117.8 . . ?
C49 C50 C51 124.7(3) . . ?
C49 C50 H50 117.7 . . ?
C51 C50 H50 117.7 . . ?
C64 C51 C52 120.7(3) . . ?
C64 C51 C50 122.6(4) . . ?
C52 C51 C50 116.7(3) . . ?
C53 C52 C51 123.1(3) . . ?
C53 C52 C57 118.4(4) . . ?
C51 C52 C57 118.5(4) . . ?
C54 C53 C52 122.0(4) . . ?
C54 C53 H53 119.0 . . ?
C52 C53 H53 119.0 . . ?
C53 C54 C55 119.8(5) . . ?
C53 C54 H54 120.1 . . ?
C55 C54 H54 120.1 . . ?
C56 C55 C54 119.8(5) . . ?
C56 C55 H55 120.1 . . ?
C54 C55 H55 120.1 . . ?
C55 C56 C57 121.9(4) . . ?
C55 C56 H56 119.1 . . ?
C57 C56 H56 119.1 . . ?
C58 C57 C56 122.0(4) . . ?
C58 C57 C52 119.9(4) . . ?
C56 C57 C52 118.1(4) . . ?
C59 C58 C57 122.1(4) . . ?
C59 C58 H58 119.0 . . ?
C57 C58 H58 119.0 . . ?
C58 C59 C60 121.3(4) . . ?
C58 C59 C64 118.7(4) . . ?
C60 C59 C64 119.9(5) . . ?
C59 C60 C61 122.3(5) . . ?
C59 C60 H60 118.9 . . ?
C61 C60 H60 118.9 . . ?
C60 C61 C62 118.8(6) . . ?
C60 C61 H61 120.6 . . ?
C62 C61 H61 120.6 . . ?
C63 C62 C61 119.6(6) . . ?
C63 C62 H62 120.2 . . ?
C61 C62 H62 120.2 . . ?
C62 C63 C64 123.2(4) . . ?
C62 C63 H63 118.4 . . ?
C64 C63 H63 118.4 . . ?
C51 C64 C59 120.1(4) . . ?
C51 C64 C63 123.8(3) . . ?
C59 C64 C63 116.0(4) . . ?
C70 C65 C66 117.6(3) . . ?
C70 C65 C71 119.8(3) . . ?
C66 C65 C71 122.7(3) . . ?
C67 C66 C65 121.1(3) . . ?
C67 C66 H66 119.4 . . ?
C65 C66 H66 119.4 . . ?
C66 C67 C68 120.0(4) . . ?
C66 C67 H67 120.0 . . ?
C68 C67 H67 120.0 . . ?
C69 C68 C67 119.9(4) . . ?
C69 C68 H68 120.0 . . ?
C67 C68 H68 120.0 . . ?
C68 C69 C70 119.8(3) . . ?
C68 C69 H69 120.1 . . ?
C70 C69 H69 120.1 . . ?
C69 C70 C65 121.6(3) . . ?
C69 C70 H70 119.2 . . ?
C65 C70 H70 119.2 . . ?
C76 C71 C72 118.7(3) . . ?
C76 C71 C65 119.4(3) . . ?
C72 C71 C65 121.9(3) . . ?
O3 C72 C73 121.4(2) . . ?
O3 C72 C71 117.4(3) . . ?
C73 C72 C71 121.2(3) . . ?
C72 O3 Ti2 134.37(19) . . ?
C74 C73 C72 117.8(3) . . ?
C74 C73 C77 117.0(3) . . ?
C72 C73 C77 125.0(3) . . ?
C75 C74 C73 121.0(3) . . ?
C75 C74 H74 119.5 . . ?
C73 C74 H74 119.5 . . ?
C76 C75 C74 120.4(3) . . ?
C76 C75 H75 119.8 . . ?
C74 C75 H75 119.8 . . ?
C75 C76 C71 120.7(3) . . ?
C75 C76 H76 119.6 . . ?
C71 C76 H76 119.6 . . ?
C82 C77 C78 117.9(3) . . ?
C82 C77 C73 117.9(3) . . ?
C78 C77 C73 124.2(3) . . ?
O4 C78 C77 120.1(3) . . ?
O4 C78 C79 119.0(3) . . ?
C77 C78 C79 120.9(3) . . ?
C78 O4 Ti2 128.39(19) . . ?
C80 C79 C78 117.5(3) . . ?
C80 C79 C83 119.1(3) . . ?
C78 C79 C83 123.3(3) . . ?
C81 C80 C79 122.1(3) . . ?
C81 C80 H80 118.9 . . ?
C79 C80 H80 118.9 . . ?
C80 C81 C82 119.3(3) . . ?
C80 C81 H81 120.4 . . ?
C82 C81 H81 120.4 . . ?
C81 C82 C77 122.2(3) . . ?
C81 C82 H82 118.9 . . ?
C77 C82 H82 118.9 . . ?
C88 C83 C84 117.9(4) . . ?
C88 C83 C79 119.7(3) . . ?
C84 C83 C79 122.4(3) . . ?
C85 C84 C83 120.7(4) . . ?
C85 C84 H84 119.6 . . ?
C83 C84 H84 119.6 . . ?
C84 C85 C86 120.1(5) . . ?
C84 C85 H85 120.0 . . ?
C86 C85 H85 120.0 . . ?
C87 C86 C85 119.6(4) . . ?
C87 C86 H86 120.2 . . ?
C85 C86 H86 120.2 . . ?
C86 C87 C88 120.5(4) . . ?
C86 C87 H87 119.7 . . ?
C88 C87 H87 119.7 . . ?
C87 C88 C83 121.2(4) . . ?
C87 C88 H88 119.4 . . ?
C83 C88 H88 119.4 . . ?
Cl1 C90 Cl1 97.6(11) . 2_755 ?
Cl1 C90 Cl3 144.8(7) . 2_755 ?
Cl1 C90 Cl3 115.7(4) 2_755 2_755 ?
Cl1 C90 Cl3 115.7(4) . . ?
Cl1 C90 Cl3 144.8(7) 2_755 . ?
Cl3 C90 Cl3 37.0(4) 2_755 . ?
Cl1 C90 Cl2 106.4(5) . . ?
Cl1 C90 Cl2 68.2(5) 2_755 . ?
Cl3 C90 Cl2 77.4(4) 2_755 . ?
Cl3 C90 Cl2 110.2(5) . . ?
Cl1 C90 Cl2 68.2(5) . 2_755 ?
Cl1 C90 Cl2 106.4(5) 2_755 2_755 ?
Cl3 C90 Cl2 110.2(5) 2_755 2_755 ?
Cl3 C90 Cl2 77.4(4) . 2_755 ?
Cl2 C90 Cl2 172.3(8) . 2_755 ?
C90 Cl1 Cl2 58.6(4) . 2_755 ?
C90 Cl1 Cl1 41.2(5) . 2_755 ?
Cl2 Cl1 Cl1 75.6(8) 2_755 2_755 ?
C90 Cl2 Cl1 53.2(3) . 2_755 ?
C90 Cl2 Cl3 50.3(4) . 2_755 ?
Cl1 Cl2 Cl3 88.1(5) 2_755 2_755 ?
Cl3 Cl3 C90 71.5(2) 2_755 . ?
Cl3 Cl3 Cl2 117.8(4) 2_755 2_755 ?
C90 Cl3 Cl2 52.3(2) . 2_755 ?

_refine_diff_density_max         2.194
_refine_diff_density_min         -0.571
_refine_diff_density_rms         0.112

_shelxl_version_number           2014/6


loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.694 0.059 0.600 25 1 ' '
2 0.306 0.059 0.900 25 1 ' '
3 0.500 0.339 0.250 148 41 ' '
4 0.159 0.449 0.029 8 0 ' '
5 0.841 0.449 0.471 9 0 ' '
6 0.163 0.553 0.535 9 0 ' '
7 0.837 0.553 0.965 10 0 ' '
8 0.500 0.663 0.750 146 41 ' '
9 0.694 0.941 0.100 25 1 ' '
10 0.306 0.941 0.400 25 1 ' '
_platon_squeeze_details          
;
;




####################################################################### 
# 
# 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_e3144n
_audit_block_doi                 10.5517/ccdc.csd.cc1l9dpz
_database_code_depnum_ccdc_archive 'CCDC 1468801'
_audit_update_record             
;
2016-06-28 deposited with the CCDC.
2016-10-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H50 N4 O4 Ti'
_chemical_formula_sum            'C72 H50 N4 O4 Ti'
_chemical_formula_weight         1083.06

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/n'
_space_group_name_Hall           '-P 2yn'

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

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

_cell_length_a                   13.5432(3)
_cell_length_b                   14.0231(4)
_cell_length_c                   29.0361(8)
_cell_angle_alpha                90
_cell_angle_beta                 93.2494(14)
_cell_angle_gamma                90
_cell_volume                     5505.6(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    65000
_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    1.307
_exptl_crystal_F_000             2256
_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    0.213
_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  0.987
_exptl_absorpt_correction_T_max  0.987
_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            65399
_diffrn_reflns_av_unetI/netI     0.0853
_diffrn_reflns_av_R_equivalents  0.0763
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_theta_min         1.405
_diffrn_reflns_theta_max         30.105
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             16143
_reflns_number_gt                9291
_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-97 (Sheldrick, 2008)'
_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)+(0.1000P)²] 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         16143
_refine_ls_number_parameters     730
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1257
_refine_ls_R_factor_gt           0.0606
_refine_ls_wR_factor_ref         0.1947
_refine_ls_wR_factor_gt          0.1519
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.036
_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 0.10504(3) 0.35702(3) 0.13456(2) 0.02281(11) Uani 1 1 d . . . . .
C1 C -0.18968(17) 0.2702(2) 0.16202(9) 0.0374(6) Uani 1 1 d . . . . .
C2 C -0.1412(2) 0.1970(3) 0.18617(10) 0.0530(8) Uani 1 1 d . . . . .
H2 H -0.0940 0.1593 0.1714 0.064 Uiso 1 1 calc R U . . .
C3 C -0.1610(3) 0.1785(3) 0.23153(11) 0.0737(11) Uani 1 1 d . . . . .
H3 H -0.1273 0.1281 0.2476 0.088 Uiso 1 1 calc R U . . .
C4 C -0.2292(2) 0.2327(4) 0.25365(11) 0.0771(12) Uani 1 1 d . . . . .
H4 H -0.2437 0.2186 0.2846 0.092 Uiso 1 1 calc R U . . .
C5 C -0.2761(2) 0.3072(3) 0.23072(11) 0.0607(9) Uani 1 1 d . . . . .
H5 H -0.3214 0.3460 0.2461 0.073 Uiso 1 1 calc R U . . .
C6 C -0.25711(18) 0.3256(2) 0.18513(10) 0.0472(7) Uani 1 1 d . . . . .
H6 H -0.2904 0.3766 0.1693 0.057 Uiso 1 1 calc R U . . .
C7 C -0.17497(16) 0.28664(18) 0.11227(8) 0.0330(6) Uani 1 1 d . . . . .
C8 C -0.08100(15) 0.27791(16) 0.09383(8) 0.0278(5) Uani 1 1 d . . . . .
O1 O -0.00001(10) 0.26715(11) 0.12235(5) 0.0266(3) Uani 1 1 d . . . . .
C9 C -0.07157(15) 0.28253(17) 0.04576(8) 0.0278(5) Uani 1 1 d . . . . .
C10 C -0.15586(17) 0.30427(19) 0.01731(8) 0.0353(6) Uani 1 1 d . . . . .
H10 H -0.1504 0.3086 -0.0151 0.042 Uiso 1 1 calc R U . . .
C11 C -0.24656(17) 0.3195(2) 0.03548(9) 0.0420(7) Uani 1 1 d . . . . .
H11 H -0.3021 0.3374 0.0159 0.050 Uiso 1 1 calc R U . . .
C12 C -0.25591(17) 0.3084(2) 0.08240(9) 0.0400(6) Uani 1 1 d . . . . .
H12 H -0.3191 0.3159 0.0945 0.048 Uiso 1 1 calc R U . . .
C13 C 0.02200(16) 0.25968(17) 0.02374(7) 0.0274(5) Uani 1 1 d . . . . .
C14 C 0.11392(15) 0.30109(16) 0.03695(7) 0.0242(5) Uani 1 1 d . . . . .
O2 O 0.12394(11) 0.36401(11) 0.07204(5) 0.0274(3) Uani 1 1 d . . . . .
C15 C 0.19964(16) 0.27769(16) 0.01435(7) 0.0263(5) Uani 1 1 d . . . . .
C16 C 0.19188(18) 0.21009(18) -0.02103(8) 0.0344(6) Uani 1 1 d . . . . .
H16 H 0.2493 0.1925 -0.0363 0.041 Uiso 1 1 calc R U . . .
C17 C 0.10284(19) 0.16863(19) -0.03416(9) 0.0381(6) Uani 1 1 d . . . . .
H17 H 0.0989 0.1229 -0.0583 0.046 Uiso 1 1 calc R U . . .
C18 C 0.01895(18) 0.19372(18) -0.01202(8) 0.0339(6) Uani 1 1 d . . . . .
H18 H -0.0424 0.1651 -0.0215 0.041 Uiso 1 1 calc R U . . .
C19 C 0.29648(16) 0.32212(18) 0.02847(7) 0.0286(5) Uani 1 1 d . . . . .
C20 C 0.38007(17) 0.2641(2) 0.03572(8) 0.0365(6) Uani 1 1 d . . . . .
H20 H 0.3740 0.1969 0.0327 0.044 Uiso 1 1 calc R U . . .
C21 C 0.47196(18) 0.3044(3) 0.04732(9) 0.0483(7) Uani 1 1 d . . . . .
H21 H 0.5283 0.2646 0.0523 0.058 Uiso 1 1 calc R U . . .
C22 C 0.48153(19) 0.4021(3) 0.05169(10) 0.0506(8) Uani 1 1 d . . . . .
H22 H 0.5446 0.4296 0.0589 0.061 Uiso 1 1 calc R U . . .
C23 C 0.3997(2) 0.4593(2) 0.04553(10) 0.0482(7) Uani 1 1 d . . . . .
H23 H 0.4061 0.5263 0.0491 0.058 Uiso 1 1 calc R U . . .
C24 C 0.30755(18) 0.42000(19) 0.03411(9) 0.0374(6) Uani 1 1 d . . . . .
H24 H 0.2514 0.4604 0.0301 0.045 Uiso 1 1 calc R U . . .
C25 C 0.25406(18) 0.08783(17) 0.13311(8) 0.0318(5) Uani 1 1 d . . . . .
C26 C 0.1730(2) 0.09857(19) 0.10183(9) 0.0416(6) Uani 1 1 d . . . . .
H26 H 0.1607 0.1588 0.0877 0.050 Uiso 1 1 calc R U . . .
C27 C 0.1104(2) 0.0234(2) 0.09108(10) 0.0544(8) Uani 1 1 d . . . . .
H27 H 0.0560 0.0322 0.0694 0.065 Uiso 1 1 calc R U . . .
C28 C 0.1260(3) -0.0644(2) 0.11140(10) 0.0560(8) Uani 1 1 d . . . . .
H28 H 0.0820 -0.1158 0.1043 0.067 Uiso 1 1 calc R U . . .
C29 C 0.2067(2) -0.0768(2) 0.14227(10) 0.0524(8) Uani 1 1 d . . . . .
H29 H 0.2188 -0.1373 0.1562 0.063 Uiso 1 1 calc R U . . .
C30 C 0.2694(2) -0.00157(18) 0.15288(9) 0.0434(7) Uani 1 1 d . . . . .
H30 H 0.3244 -0.0111 0.1742 0.052 Uiso 1 1 calc R U . . .
C31 C 0.32332(17) 0.16775(17) 0.14529(8) 0.0298(5) Uani 1 1 d . . . . .
C32 C 0.29080(15) 0.25668(17) 0.16055(7) 0.0268(5) Uani 1 1 d . . . . .
O3 O 0.19117(10) 0.27017(11) 0.16248(5) 0.0291(4) Uani 1 1 d . . . . .
C33 C 0.35873(16) 0.32808(17) 0.17561(8) 0.0283(5) Uani 1 1 d . . . . .
C34 C 0.45940(17) 0.3083(2) 0.17180(9) 0.0360(6) Uani 1 1 d . . . . .
H34 H 0.5064 0.3565 0.1801 0.043 Uiso 1 1 calc R U . . .
C35 C 0.49260(18) 0.2222(2) 0.15662(9) 0.0426(7) Uani 1 1 d . . . . .
H35 H 0.5614 0.2107 0.1549 0.051 Uiso 1 1 calc R U . . .
C36 C 0.42452(18) 0.1521(2) 0.14386(9) 0.0393(6) Uani 1 1 d . . . . .
H36 H 0.4474 0.0919 0.1339 0.047 Uiso 1 1 calc R U . . .
C37 C 0.33202(15) 0.41873(17) 0.19883(8) 0.0278(5) Uani 1 1 d . . . . .
C38 C 0.25320(16) 0.47859(17) 0.18414(7) 0.0268(5) Uani 1 1 d . . . . .
O4 O 0.19443(11) 0.45584(11) 0.14697(5) 0.0263(3) Uani 1 1 d . . . . .
C39 C 0.23342(17) 0.56383(17) 0.20789(8) 0.0296(5) Uani 1 1 d . . . . .
C40 C 0.29586(19) 0.58940(19) 0.24593(8) 0.0381(6) Uani 1 1 d . . . . .
H40 H 0.2839 0.6468 0.2621 0.046 Uiso 1 1 calc R U . . .
C41 C 0.3747(2) 0.5321(2) 0.26033(9) 0.0433(7) Uani 1 1 d . . . . .
H41 H 0.4172 0.5507 0.2859 0.052 Uiso 1 1 calc R U . . .
C42 C 0.39175(17) 0.44796(19) 0.23755(8) 0.0359(6) Uani 1 1 d . . . . .
H42 H 0.4453 0.4086 0.2483 0.043 Uiso 1 1 calc R U . . .
C43 C 0.14690(18) 0.62367(17) 0.19348(8) 0.0327(5) Uani 1 1 d . . . . .
C44 C 0.12414(19) 0.64816(17) 0.14740(9) 0.0353(6) Uani 1 1 d . . . . .
H44 H 0.1660 0.6271 0.1243 0.042 Uiso 1 1 calc R U . . .
C45 C 0.0418(2) 0.70247(19) 0.13489(10) 0.0457(7) Uani 1 1 d . . . . .
H45 H 0.0281 0.7188 0.1034 0.055 Uiso 1 1 calc R U . . .
C46 C -0.0205(2) 0.7331(2) 0.16776(12) 0.0540(8) Uani 1 1 d . . . . .
H46 H -0.0777 0.7696 0.1591 0.065 Uiso 1 1 calc R U . . .
C47 C 0.0008(2) 0.7104(2) 0.21318(11) 0.0516(8) Uani 1 1 d . . . . .
H47 H -0.0419 0.7314 0.2360 0.062 Uiso 1 1 calc R U . . .
C48 C 0.0838(2) 0.65722(19) 0.22620(10) 0.0417(6) Uani 1 1 d . . . . .
H48 H 0.0981 0.6434 0.2579 0.050 Uiso 1 1 calc R U . . .
N1 N -0.01435(13) 0.46582(14) 0.12217(6) 0.0263(4) Uani 1 1 d . . . . .
C49 C -0.03896(17) 0.50097(17) 0.08005(8) 0.0320(5) Uani 1 1 d . . . . .
H49 H 0.0040 0.4910 0.0558 0.038 Uiso 1 1 calc R U . . .
C50 C -0.12487(18) 0.55094(19) 0.07152(9) 0.0379(6) Uani 1 1 d . . . . .
H50 H -0.1412 0.5773 0.0419 0.046 Uiso 1 1 calc R U . . .
C51 C -0.18679(17) 0.56193(18) 0.10700(8) 0.0339(6) Uani 1 1 d . . . . .
N2 N -0.16154(14) 0.53102(15) 0.14997(7) 0.0328(5) Uani 1 1 d . . . . .
C52 C -0.07555(16) 0.48554(16) 0.15532(8) 0.0277(5) Uani 1 1 d . . . . .
C53 C -0.28450(18) 0.6062(2) 0.09778(9) 0.0392(6) Uani 1 1 d . . . . .
H53 H -0.2983 0.6317 0.0678 0.047 Uiso 1 1 calc R U . . .
C54 C -0.35435(18) 0.61390(19) 0.12708(9) 0.0374(6) Uani 1 1 d . . . . .
H54 H -0.3411 0.5895 0.1573 0.045 Uiso 1 1 calc R U . . .
C55 C -0.45160(17) 0.65760(18) 0.11640(8) 0.0342(6) Uani 1 1 d . . . . .
C56 C -0.47450(18) 0.7044(2) 0.07501(9) 0.0396(6) Uani 1 1 d . . . . .
H56 H -0.4260 0.7082 0.0527 0.048 Uiso 1 1 calc R U . . .
C57 C -0.56637(19) 0.7456(2) 0.06543(9) 0.0434(7) Uani 1 1 d . . . . .
H57 H -0.5802 0.7778 0.0370 0.052 Uiso 1 1 calc R U . . .
C58 C -0.63714(18) 0.7397(2) 0.09718(10) 0.0462(7) Uani 1 1 d . . . . .
H58 H -0.7003 0.7678 0.0908 0.055 Uiso 1 1 calc R U . . .
C59 C -0.6166(2) 0.6930(2) 0.13841(10) 0.0505(8) Uani 1 1 d . . . . .
H59 H -0.6657 0.6890 0.1604 0.061 Uiso 1 1 calc R U . . .
C60 C -0.52465(19) 0.6520(2) 0.14781(9) 0.0440(7) Uani 1 1 d . . . . .
H60 H -0.5115 0.6195 0.1762 0.053 Uiso 1 1 calc R U . . .
C61 C -0.04177(16) 0.44796(17) 0.20138(8) 0.0287(5) Uani 1 1 d . . . . .
N3 N 0.03793(13) 0.39050(14) 0.20126(6) 0.0279(4) Uani 1 1 d . . . . .
C62 C 0.06980(18) 0.35481(18) 0.24252(8) 0.0351(6) Uani 1 1 d . . . . .
H62 H 0.1257 0.3138 0.2445 0.042 Uiso 1 1 calc R U . . .
C63 C 0.02246(19) 0.37688(19) 0.28209(8) 0.0384(6) Uani 1 1 d . . . . .
H63 H 0.0448 0.3510 0.3111 0.046 Uiso 1 1 calc R U . . .
C64 C -0.05872(17) 0.43785(19) 0.27858(8) 0.0339(5) Uani 1 1 d . . . . .
N4 N -0.09063(14) 0.47326(15) 0.23752(7) 0.0325(5) Uani 1 1 d . . . . .
C65 C -0.1147(2) 0.4696(2) 0.31811(9) 0.0410(6) Uani 1 1 d . . . . .
H65 H -0.1698 0.5105 0.3119 0.049 Uiso 1 1 calc R U . . .
C66 C -0.0934(2) 0.4452(2) 0.36136(9) 0.0428(6) Uani 1 1 d . . . . .
H66 H -0.0408 0.4012 0.3670 0.051 Uiso 1 1 calc R U . . .
C67 C -0.1437(2) 0.4800(2) 0.40193(9) 0.0444(7) Uani 1 1 d . . . . .
C68 C -0.2333(3) 0.5284(2) 0.39832(11) 0.0605(9) Uani 1 1 d . . . . .
H68 H -0.2650 0.5397 0.3688 0.073 Uiso 1 1 calc R U . . .
C69 C -0.2764(3) 0.5603(3) 0.43754(13) 0.0713(11) Uani 1 1 d . . . . .
H69 H -0.3385 0.5919 0.4349 0.086 Uiso 1 1 calc R U . . .
C70 C -0.2300(3) 0.5466(2) 0.48035(13) 0.0689(10) Uani 1 1 d . . . . .
H70 H -0.2587 0.5708 0.5070 0.083 Uiso 1 1 calc R U . . .
C71 C -0.1427(3) 0.4981(2) 0.48450(11) 0.0621(9) Uani 1 1 d . . . . .
H71 H -0.1114 0.4873 0.5141 0.075 Uiso 1 1 calc R U . . .
C72 C -0.0997(2) 0.4647(2) 0.44538(10) 0.0520(7) Uani 1 1 d . . . . .
H72 H -0.0390 0.4307 0.4485 0.062 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 1.8423(15) . ?
Ti1 O2 1.8504(16) . ?
Ti1 O4 1.8618(15) . ?
Ti1 O1 1.9185(15) . ?
Ti1 N3 2.2351(19) . ?
Ti1 N1 2.2373(18) . ?
C1 C2 1.387(4) . ?
C1 C6 1.399(4) . ?
C1 C7 1.487(3) . ?
C2 C3 1.384(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.383(5) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.387(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
C7 C12 1.393(3) . ?
C7 C8 1.414(3) . ?
C8 O1 1.345(2) . ?
C8 C9 1.410(3) . ?
C9 C10 1.404(3) . ?
C9 C13 1.486(3) . ?
C10 C11 1.381(3) . ?
C10 H10 0.9500 . ?
C11 C12 1.384(4) . ?
C11 H11 0.9500 . ?
C12 H12 0.9500 . ?
C13 C18 1.389(3) . ?
C13 C14 1.407(3) . ?
C14 O2 1.349(3) . ?
C14 C15 1.405(3) . ?
C15 C16 1.397(3) . ?
C15 C19 1.488(3) . ?
C16 C17 1.373(3) . ?
C16 H16 0.9500 . ?
C17 C18 1.382(4) . ?
C17 H17 0.9500 . ?
C18 H18 0.9500 . ?
C19 C24 1.390(4) . ?
C19 C20 1.400(3) . ?
C20 C21 1.390(4) . ?
C20 H20 0.9500 . ?
C21 C22 1.382(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.371(4) . ?
C22 H22 0.9500 . ?
C23 C24 1.387(3) . ?
C23 H23 0.9500 . ?
C24 H24 0.9500 . ?
C25 C30 1.390(3) . ?
C25 C26 1.392(3) . ?
C25 C31 1.491(3) . ?
C26 C27 1.378(4) . ?
C26 H26 0.9500 . ?
C27 C28 1.375(4) . ?
C27 H27 0.9500 . ?
C28 C29 1.384(4) . ?
C28 H28 0.9500 . ?
C29 C30 1.378(4) . ?
C29 H29 0.9500 . ?
C30 H30 0.9500 . ?
C31 C36 1.391(3) . ?
C31 C32 1.403(3) . ?
C32 O3 1.367(3) . ?
C32 C33 1.412(3) . ?
C33 C34 1.402(3) . ?
C33 C37 1.493(3) . ?
C34 C35 1.370(4) . ?
C34 H34 0.9500 . ?
C35 C36 1.383(4) . ?
C35 H35 0.9500 . ?
C36 H36 0.9500 . ?
C37 C38 1.405(3) . ?
C37 C42 1.408(3) . ?
C38 O4 1.343(2) . ?
C38 C39 1.413(3) . ?
C39 C40 1.399(3) . ?
C39 C43 1.482(3) . ?
C40 C41 1.382(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.378(4) . ?
C41 H41 0.9500 . ?
C42 H42 0.9500 . ?
C43 C48 1.395(4) . ?
C43 C44 1.399(3) . ?
C44 C45 1.382(4) . ?
C44 H44 0.9500 . ?
C45 C46 1.379(4) . ?
C45 H45 0.9500 . ?
C46 C47 1.372(4) . ?
C46 H46 0.9500 . ?
C47 C48 1.384(4) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
N1 C52 1.334(3) . ?
N1 C49 1.343(3) . ?
C49 C50 1.369(3) . ?
C49 H49 0.9500 . ?
C50 C51 1.373(4) . ?
C50 H50 0.9500 . ?
C51 N2 1.347(3) . ?
C51 C53 1.473(3) . ?
N2 C52 1.329(3) . ?
C52 C61 1.485(3) . ?
C53 C54 1.312(4) . ?
C53 H53 0.9500 . ?
C54 C55 1.470(3) . ?
C54 H54 0.9500 . ?
C55 C60 1.385(4) . ?
C55 C56 1.389(3) . ?
C56 C57 1.386(3) . ?
C56 H56 0.9500 . ?
C57 C58 1.369(4) . ?
C57 H57 0.9500 . ?
C58 C59 1.379(4) . ?
C58 H58 0.9500 . ?
C59 C60 1.385(4) . ?
C59 H59 0.9500 . ?
C60 H60 0.9500 . ?
C61 N4 1.320(3) . ?
C61 N3 1.347(3) . ?
N3 C62 1.347(3) . ?
C62 C63 1.382(4) . ?
C62 H62 0.9500 . ?
C63 C64 1.392(4) . ?
C63 H63 0.9500 . ?
C64 N4 1.340(3) . ?
C64 C65 1.479(4) . ?
C65 C66 1.317(4) . ?
C65 H65 0.9500 . ?
C66 C67 1.477(4) . ?
C66 H66 0.9500 . ?
C67 C72 1.381(4) . ?
C67 C68 1.389(4) . ?
C68 C69 1.383(5) . ?
C68 H68 0.9500 . ?
C69 C70 1.375(5) . ?
C69 H69 0.9500 . ?
C70 C71 1.362(5) . ?
C70 H70 0.9500 . ?
C71 C72 1.388(4) . ?
C71 H71 0.9500 . ?
C72 H72 0.9500 . ?

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 O2 110.32(7) . . ?
O3 Ti1 O4 91.05(7) . . ?
O2 Ti1 O4 91.48(7) . . ?
O3 Ti1 O1 95.25(7) . . ?
O2 Ti1 O1 89.76(6) . . ?
O4 Ti1 O1 172.72(7) . . ?
O3 Ti1 N3 92.07(7) . . ?
O2 Ti1 N3 157.61(7) . . ?
O4 Ti1 N3 88.16(7) . . ?
O1 Ti1 N3 87.97(7) . . ?
O3 Ti1 N1 162.83(7) . . ?
O2 Ti1 N1 86.85(7) . . ?
O4 Ti1 N1 88.83(7) . . ?
O1 Ti1 N1 84.07(7) . . ?
N3 Ti1 N1 70.76(7) . . ?
C2 C1 C6 118.2(3) . . ?
C2 C1 C7 121.3(3) . . ?
C6 C1 C7 120.4(2) . . ?
C3 C2 C1 120.5(3) . . ?
C3 C2 H2 119.7 . . ?
C1 C2 H2 119.7 . . ?
C4 C3 C2 120.7(4) . . ?
C4 C3 H3 119.7 . . ?
C2 C3 H3 119.7 . . ?
C5 C4 C3 119.7(3) . . ?
C5 C4 H4 120.2 . . ?
C3 C4 H4 120.2 . . ?
C4 C5 C6 119.9(3) . . ?
C4 C5 H5 120.0 . . ?
C6 C5 H5 120.0 . . ?
C5 C6 C1 121.0(3) . . ?
C5 C6 H6 119.5 . . ?
C1 C6 H6 119.5 . . ?
C12 C7 C8 118.5(2) . . ?
C12 C7 C1 119.7(2) . . ?
C8 C7 C1 121.8(2) . . ?
O1 C8 C9 119.88(19) . . ?
O1 C8 C7 119.8(2) . . ?
C9 C8 C7 120.32(19) . . ?
C8 O1 Ti1 127.63(14) . . ?
C10 C9 C8 118.4(2) . . ?
C10 C9 C13 118.6(2) . . ?
C8 C9 C13 122.90(18) . . ?
C11 C10 C9 121.3(2) . . ?
C11 C10 H10 119.3 . . ?
C9 C10 H10 119.3 . . ?
C10 C11 C12 119.5(2) . . ?
C10 C11 H11 120.3 . . ?
C12 C11 H11 120.3 . . ?
C11 C12 C7 121.7(2) . . ?
C11 C12 H12 119.2 . . ?
C7 C12 H12 119.2 . . ?
C18 C13 C14 117.8(2) . . ?
C18 C13 C9 118.4(2) . . ?
C14 C13 C9 123.8(2) . . ?
O2 C14 C15 117.08(18) . . ?
O2 C14 C13 121.7(2) . . ?
C15 C14 C13 121.2(2) . . ?
C14 O2 Ti1 133.86(14) . . ?
C16 C15 C14 118.2(2) . . ?
C16 C15 C19 121.0(2) . . ?
C14 C15 C19 120.8(2) . . ?
C17 C16 C15 121.3(2) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 119.7(2) . . ?
C16 C17 H17 120.2 . . ?
C18 C17 H17 120.2 . . ?
C17 C18 C13 121.8(2) . . ?
C17 C18 H18 119.1 . . ?
C13 C18 H18 119.1 . . ?
C24 C19 C20 118.4(2) . . ?
C24 C19 C15 122.2(2) . . ?
C20 C19 C15 119.4(2) . . ?
C21 C20 C19 120.4(3) . . ?
C21 C20 H20 119.8 . . ?
C19 C20 H20 119.8 . . ?
C22 C21 C20 120.2(3) . . ?
C22 C21 H21 119.9 . . ?
C20 C21 H21 119.9 . . ?
C23 C22 C21 119.8(2) . . ?
C23 C22 H22 120.1 . . ?
C21 C22 H22 120.1 . . ?
C22 C23 C24 120.6(3) . . ?
C22 C23 H23 119.7 . . ?
C24 C23 H23 119.7 . . ?
C23 C24 C19 120.7(2) . . ?
C23 C24 H24 119.7 . . ?
C19 C24 H24 119.7 . . ?
C30 C25 C26 117.4(2) . . ?
C30 C25 C31 120.2(2) . . ?
C26 C25 C31 122.4(2) . . ?
C27 C26 C25 121.1(2) . . ?
C27 C26 H26 119.4 . . ?
C25 C26 H26 119.4 . . ?
C28 C27 C26 120.7(3) . . ?
C28 C27 H27 119.7 . . ?
C26 C27 H27 119.7 . . ?
C27 C28 C29 119.1(3) . . ?
C27 C28 H28 120.4 . . ?
C29 C28 H28 120.4 . . ?
C30 C29 C28 120.1(3) . . ?
C30 C29 H29 119.9 . . ?
C28 C29 H29 119.9 . . ?
C29 C30 C25 121.5(3) . . ?
C29 C30 H30 119.3 . . ?
C25 C30 H30 119.3 . . ?
C36 C31 C32 118.5(2) . . ?
C36 C31 C25 118.8(2) . . ?
C32 C31 C25 122.6(2) . . ?
O3 C32 C31 117.7(2) . . ?
O3 C32 C33 121.1(2) . . ?
C31 C32 C33 121.2(2) . . ?
C32 O3 Ti1 132.49(14) . . ?
C34 C33 C32 117.1(2) . . ?
C34 C33 C37 117.7(2) . . ?
C32 C33 C37 125.0(2) . . ?
C35 C34 C33 122.5(2) . . ?
C35 C34 H34 118.7 . . ?
C33 C34 H34 118.7 . . ?
C34 C35 C36 119.1(2) . . ?
C34 C35 H35 120.5 . . ?
C36 C35 H35 120.5 . . ?
C35 C36 C31 121.5(2) . . ?
C35 C36 H36 119.2 . . ?
C31 C36 H36 119.2 . . ?
C38 C37 C42 117.4(2) . . ?
C38 C37 C33 124.82(19) . . ?
C42 C37 C33 117.7(2) . . ?
O4 C38 C37 120.5(2) . . ?
O4 C38 C39 118.24(19) . . ?
C37 C38 C39 121.26(19) . . ?
C38 O4 Ti1 132.98(14) . . ?
C40 C39 C38 118.6(2) . . ?
C40 C39 C43 120.7(2) . . ?
C38 C39 C43 120.65(19) . . ?
C41 C40 C39 120.8(2) . . ?
C41 C40 H40 119.6 . . ?
C39 C40 H40 119.6 . . ?
C42 C41 C40 120.0(2) . . ?
C42 C41 H41 120.0 . . ?
C40 C41 H41 120.0 . . ?
C41 C42 C37 121.9(2) . . ?
C41 C42 H42 119.1 . . ?
C37 C42 H42 119.1 . . ?
C48 C43 C44 117.3(2) . . ?
C48 C43 C39 120.2(2) . . ?
C44 C43 C39 122.5(2) . . ?
C45 C44 C43 121.2(3) . . ?
C45 C44 H44 119.4 . . ?
C43 C44 H44 119.4 . . ?
C46 C45 C44 120.4(3) . . ?
C46 C45 H45 119.8 . . ?
C44 C45 H45 119.8 . . ?
C47 C46 C45 119.3(3) . . ?
C47 C46 H46 120.4 . . ?
C45 C46 H46 120.4 . . ?
C46 C47 C48 120.8(3) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C47 C48 C43 121.0(3) . . ?
C47 C48 H48 119.5 . . ?
C43 C48 H48 119.5 . . ?
C52 N1 C49 116.65(19) . . ?
C52 N1 Ti1 119.88(14) . . ?
C49 N1 Ti1 122.45(16) . . ?
N1 C49 C50 121.2(2) . . ?
N1 C49 H49 119.4 . . ?
C50 C49 H49 119.4 . . ?
C49 C50 C51 118.1(2) . . ?
C49 C50 H50 121.0 . . ?
C51 C50 H50 121.0 . . ?
N2 C51 C50 121.7(2) . . ?
N2 C51 C53 118.8(2) . . ?
C50 C51 C53 119.4(2) . . ?
C52 N2 C51 115.9(2) . . ?
N2 C52 N1 126.2(2) . . ?
N2 C52 C61 119.9(2) . . ?
N1 C52 C61 113.81(19) . . ?
C54 C53 C51 126.2(2) . . ?
C54 C53 H53 116.9 . . ?
C51 C53 H53 116.9 . . ?
C53 C54 C55 124.6(2) . . ?
C53 C54 H54 117.7 . . ?
C55 C54 H54 117.7 . . ?
C60 C55 C56 117.6(2) . . ?
C60 C55 C54 120.2(2) . . ?
C56 C55 C54 122.2(2) . . ?
C57 C56 C55 121.6(2) . . ?
C57 C56 H56 119.2 . . ?
C55 C56 H56 119.2 . . ?
C58 C57 C56 119.6(3) . . ?
C58 C57 H57 120.2 . . ?
C56 C57 H57 120.2 . . ?
C57 C58 C59 119.9(2) . . ?
C57 C58 H58 120.0 . . ?
C59 C58 H58 120.0 . . ?
C58 C59 C60 120.2(3) . . ?
C58 C59 H59 119.9 . . ?
C60 C59 H59 119.9 . . ?
C55 C60 C59 121.0(3) . . ?
C55 C60 H60 119.5 . . ?
C59 C60 H60 119.5 . . ?
N4 C61 N3 126.9(2) . . ?
N4 C61 C52 118.5(2) . . ?
N3 C61 C52 114.6(2) . . ?
C62 N3 C61 115.9(2) . . ?
C62 N3 Ti1 124.56(16) . . ?
C61 N3 Ti1 119.54(14) . . ?
N3 C62 C63 121.1(2) . . ?
N3 C62 H62 119.5 . . ?
C63 C62 H62 119.5 . . ?
C62 C63 C64 118.6(2) . . ?
C62 C63 H63 120.7 . . ?
C64 C63 H63 120.7 . . ?
N4 C64 C63 120.4(2) . . ?
N4 C64 C65 115.2(2) . . ?
C63 C64 C65 124.4(2) . . ?
C61 N4 C64 117.2(2) . . ?
C66 C65 C64 124.6(3) . . ?
C66 C65 H65 117.7 . . ?
C64 C65 H65 117.7 . . ?
C65 C66 C67 126.1(3) . . ?
C65 C66 H66 117.0 . . ?
C67 C66 H66 117.0 . . ?
C72 C67 C68 118.3(3) . . ?
C72 C67 C66 118.8(3) . . ?
C68 C67 C66 122.8(3) . . ?
C69 C68 C67 120.3(3) . . ?
C69 C68 H68 119.9 . . ?
C67 C68 H68 119.9 . . ?
C70 C69 C68 120.4(3) . . ?
C70 C69 H69 119.8 . . ?
C68 C69 H69 119.8 . . ?
C71 C70 C69 120.0(3) . . ?
C71 C70 H70 120.0 . . ?
C69 C70 H70 120.0 . . ?
C70 C71 C72 119.9(3) . . ?
C70 C71 H71 120.0 . . ?
C72 C71 H71 120.0 . . ?
C67 C72 C71 121.0(3) . . ?
C67 C72 H72 119.5 . . ?
C71 C72 H72 119.5 . . ?

_refine_diff_density_max         0.411
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.106

_shelxl_version_number           2013-4

