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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_e2513a

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C88 H72 N8 O28 Ti10, 6(C5 H5 N)'
_chemical_formula_sum            'C118 H102 N14 O28 Ti10'
_chemical_formula_weight         2643.14

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'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   I-4
_symmetry_space_group_name_Hall  I-4

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

_cell_length_a                   18.8962(3)
_cell_length_b                   18.8962(3)
_cell_length_c                   16.0089(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     5716.2(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    9799
_cell_measurement_theta_min      2.72
_cell_measurement_theta_max      26.51

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_exptl_crystal_density_meas      none
_exptl_crystal_density_diffrn    1.536
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2704
_exptl_absorpt_coefficient_mu    0.742
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9362
_exptl_absorpt_correction_T_max  0.9499
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            39869
_diffrn_reflns_av_R_equivalents  0.0417
_diffrn_reflns_av_sigmaI/netI    0.1056
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.16
_diffrn_reflns_theta_max         29.08
_reflns_number_total             7313
_reflns_number_gt                5008
_reflns_threshold_expression     >2sigma(I)

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

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

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0182P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.007(16)
_refine_ls_number_reflns         7313
_refine_ls_number_parameters     385
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0638
_refine_ls_R_factor_gt           0.0388
_refine_ls_wR_factor_ref         0.0670
_refine_ls_wR_factor_gt          0.0646
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.96299(2) 0.61735(2) 0.77194(3) 0.02132(11) Uani 1 1 d . . .
Ti2 Ti 1.10026(3) 0.65538(3) 0.88065(3) 0.02542(12) Uani 1 1 d . . .
Ti3 Ti 1.0000 0.5000 0.90202(4) 0.02331(16) Uani 1 2 d S . .
O1 O 1.03253(9) 0.69738(9) 0.78779(10) 0.0253(4) Uani 1 1 d . . .
C1 C 1.06403(14) 0.74915(14) 0.74279(16) 0.0283(6) Uani 1 1 d . . .
C2 C 1.12858(15) 0.77192(14) 0.77694(17) 0.0305(6) Uani 1 1 d . . .
O2 O 1.14920(10) 0.73960(10) 0.84754(11) 0.0296(4) Uani 1 1 d . . .
C3 C 1.16608(17) 0.82564(16) 0.7379(2) 0.0460(8) Uani 1 1 d . . .
H3 H 1.2093 0.8427 0.7606 0.055 Uiso 1 1 calc R . .
C4 C 1.1379(2) 0.85433(19) 0.6633(2) 0.0597(10) Uani 1 1 d . . .
H4 H 1.1631 0.8908 0.6352 0.072 Uiso 1 1 calc R . .
C5 C 1.07605(18) 0.83120(18) 0.6309(2) 0.0537(9) Uani 1 1 d . . .
H5 H 1.0583 0.8516 0.5809 0.064 Uiso 1 1 calc R . .
C6 C 1.03843(18) 0.77811(16) 0.66997(19) 0.0422(8) Uani 1 1 d . . .
H6 H 0.9952 0.7617 0.6467 0.051 Uiso 1 1 calc R . .
N1 N 1.03884(12) 0.72676(12) 0.97047(14) 0.0315(6) Uani 1 1 d . . .
C7 C 1.04621(19) 0.79735(17) 0.9724(2) 0.0462(8) Uani 1 1 d . . .
H7 H 1.0774 0.8184 0.9331 0.055 Uiso 1 1 calc R . .
C8 C 1.0122(2) 0.8407(2) 1.0267(2) 0.0624(11) Uani 1 1 d . . .
H8 H 1.0183 0.8906 1.0238 0.075 Uiso 1 1 calc R . .
C9 C 0.9685(2) 0.8109(2) 1.0863(2) 0.0627(11) Uani 1 1 d . . .
H9 H 0.9456 0.8392 1.1273 0.075 Uiso 1 1 calc R . .
C10 C 0.9593(2) 0.7389(2) 1.0841(2) 0.0630(11) Uani 1 1 d . . .
H10 H 0.9280 0.7169 1.1227 0.076 Uiso 1 1 calc R . .
C11 C 0.99473(19) 0.69844(18) 1.02717(18) 0.0459(8) Uani 1 1 d . . .
H11 H 0.9880 0.6486 1.0276 0.055 Uiso 1 1 calc R . .
N2 N 0.89018(12) 0.67668(12) 0.85955(13) 0.0267(5) Uani 1 1 d . . .
C12 C 0.84832(17) 0.64368(17) 0.91485(17) 0.0380(7) Uani 1 1 d . . .
H12 H 0.8502 0.5935 0.9187 0.046 Uiso 1 1 calc R . .
C13 C 0.80232(17) 0.68051(19) 0.96660(19) 0.0500(9) Uani 1 1 d . . .
H13 H 0.7741 0.6556 1.0060 0.060 Uiso 1 1 calc R . .
C14 C 0.79758(17) 0.75200(19) 0.96103(19) 0.0460(8) Uani 1 1 d . . .
H14 H 0.7664 0.7780 0.9961 0.055 Uiso 1 1 calc R . .
C15 C 0.83878(19) 0.78513(17) 0.9037(2) 0.0497(9) Uani 1 1 d . . .
H15 H 0.8362 0.8351 0.8978 0.060 Uiso 1 1 calc R . .
C16 C 0.88394(16) 0.74733(16) 0.85431(17) 0.0380(8) Uani 1 1 d . . .
H16 H 0.9121 0.7720 0.8147 0.046 Uiso 1 1 calc R . .
O3 O 1.14524(10) 0.62397(10) 0.97521(11) 0.0322(5) Uani 1 1 d . . .
C17 C 1.13689(15) 0.58796(16) 1.04766(17) 0.0310(7) Uani 1 1 d . . .
C18 C 1.16368(17) 0.61667(18) 1.12061(18) 0.0427(8) Uani 1 1 d . . .
H18 H 1.1883 0.6604 1.1185 0.051 Uiso 1 1 calc R . .
C19 C 1.15524(18) 0.58299(18) 1.19602(18) 0.0479(9) Uani 1 1 d . . .
H19 H 1.1726 0.6038 1.2460 0.057 Uiso 1 1 calc R . .
C20 C 0.8794(2) 0.48248(18) 1.19816(17) 0.0481(9) Uani 1 1 d . . .
H20 H 0.8838 0.5074 1.2495 0.058 Uiso 1 1 calc R . .
C21 C 0.90744(15) 0.51113(15) 1.12527(16) 0.0350(7) Uani 1 1 d . . .
H21 H 0.9322 0.5549 1.1274 0.042 Uiso 1 1 calc R . .
C22 C 0.89967(15) 0.47657(15) 1.04973(15) 0.0290(7) Uani 1 1 d . . .
O4 O 0.92831(11) 0.50485(10) 0.98049(10) 0.0334(5) Uani 1 1 d . . .
O5 O 1.01794(9) 0.59822(9) 0.88095(10) 0.0235(4) Uani 1 1 d . . .
O6 O 0.92752(9) 0.52841(9) 0.80552(9) 0.0213(4) Uani 1 1 d . . .
O7 O 0.90241(9) 0.64802(9) 0.69490(10) 0.0246(4) Uani 1 1 d . . .
N3 N 0.8483(3) 0.9402(2) 0.5913(3) 0.1232(17) Uani 1 1 d . . .
C23 C 0.8749(3) 0.8755(4) 0.5781(3) 0.1014(17) Uani 1 1 d . . .
H23 H 0.9134 0.8703 0.5404 0.122 Uiso 1 1 calc R . .
C24 C 0.8494(3) 0.8179(3) 0.6159(4) 0.0971(19) Uani 1 1 d . . .
H24 H 0.8686 0.7729 0.6025 0.117 Uiso 1 1 calc R . .
C25 C 0.7953(4) 0.8227(3) 0.6745(4) 0.0986(17) Uani 1 1 d . . .
H25 H 0.7777 0.7821 0.7025 0.118 Uiso 1 1 calc R . .
C26 C 0.7689(4) 0.8878(3) 0.6897(4) 0.123(2) Uani 1 1 d . . .
H26 H 0.7308 0.8942 0.7277 0.147 Uiso 1 1 calc R . .
C27 C 0.7986(4) 0.9445(3) 0.6489(4) 0.142(3) Uani 1 1 d . . .
H27 H 0.7821 0.9903 0.6634 0.170 Uiso 1 1 calc R . .
N4 N 1.0000 0.0000 0.1206(3) 0.160(4) Uani 1 2 d S . .
C28 C 0.9452(4) 0.0195(3) 0.1638(3) 0.113(2) Uani 1 1 d . . .
H28 H 0.9042 0.0344 0.1343 0.135 Uiso 1 1 calc R . .
C29 C 0.9434(3) 0.0199(5) 0.2405(4) 0.161(3) Uani 1 1 d . . .
H29 H 0.9019 0.0343 0.2692 0.193 Uiso 1 1 calc R . .
C30 C 1.0000 0.0000 0.2819(6) 0.309(13) Uani 1 2 d S . .
H30 H 1.0000 0.0000 0.3412 0.371 Uiso 1 2 calc SR . .

loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti1 0.0199(3) 0.0190(3) 0.0251(2) -0.00092(19) 0.0004(2) -0.0001(2)
Ti2 0.0248(3) 0.0232(3) 0.0283(3) -0.0005(2) -0.0017(2) -0.0042(2)
Ti3 0.0264(4) 0.0203(4) 0.0232(4) 0.000 0.000 -0.0033(3)
O1 0.0221(10) 0.0220(10) 0.0318(10) -0.0017(8) 0.0023(8) -0.0036(8)
C1 0.0260(15) 0.0217(14) 0.0372(17) 0.0046(12) 0.0085(13) 0.0000(11)
C2 0.0288(16) 0.0237(15) 0.0389(17) -0.0011(13) 0.0016(13) -0.0027(12)
O2 0.0296(11) 0.0261(11) 0.0333(11) -0.0010(8) -0.0015(8) -0.0050(9)
C3 0.0377(18) 0.0362(18) 0.064(2) 0.0055(16) 0.0005(16) -0.0130(15)
C4 0.055(3) 0.042(2) 0.082(3) 0.0290(19) -0.002(2) -0.0125(19)
C5 0.051(2) 0.053(2) 0.057(2) 0.0280(18) 0.0032(19) -0.0047(18)
C6 0.042(2) 0.0363(19) 0.049(2) 0.0135(15) -0.0050(15) -0.0016(15)
N1 0.0287(14) 0.0314(15) 0.0344(13) -0.0048(11) -0.0018(11) -0.0051(11)
C7 0.052(2) 0.036(2) 0.0503(19) -0.0141(16) 0.0083(16) -0.0035(16)
C8 0.058(3) 0.043(2) 0.086(3) -0.019(2) 0.012(2) 0.0020(19)
C9 0.067(3) 0.057(3) 0.063(2) -0.0113(19) 0.023(2) 0.015(2)
C10 0.074(3) 0.065(3) 0.050(2) 0.0067(19) 0.0306(19) 0.014(2)
C11 0.053(2) 0.043(2) 0.0414(18) 0.0049(16) 0.0069(16) 0.0011(17)
N2 0.0232(12) 0.0276(14) 0.0294(13) -0.0025(10) 0.0003(10) 0.0000(10)
C12 0.0378(18) 0.0290(17) 0.0472(18) 0.0019(14) 0.0052(15) 0.0063(14)
C13 0.042(2) 0.053(2) 0.055(2) -0.0008(17) 0.0266(16) 0.0012(17)
C14 0.037(2) 0.048(2) 0.053(2) -0.0132(17) 0.0140(16) 0.0084(16)
C15 0.058(2) 0.0288(19) 0.063(2) -0.0125(16) 0.0002(18) 0.0094(16)
C16 0.044(2) 0.0291(18) 0.0411(18) -0.0017(13) 0.0086(14) 0.0069(15)
O3 0.0350(12) 0.0322(12) 0.0294(11) 0.0009(9) -0.0036(8) -0.0038(9)
C17 0.0252(16) 0.0387(18) 0.0290(16) -0.0007(14) -0.0042(12) 0.0013(14)
C18 0.046(2) 0.0421(18) 0.0402(19) -0.0043(16) -0.0084(15) -0.0156(15)
C19 0.059(2) 0.055(2) 0.0295(18) 0.0002(16) -0.0150(15) -0.0164(18)
C20 0.066(2) 0.054(2) 0.0242(16) -0.0047(14) 0.0042(16) -0.0142(19)
C21 0.0367(18) 0.0335(17) 0.0348(17) -0.0067(14) 0.0049(14) -0.0030(14)
C22 0.0301(17) 0.0314(17) 0.0256(15) 0.0017(13) 0.0012(12) 0.0040(13)
O4 0.0494(13) 0.0244(11) 0.0265(10) 0.0023(8) 0.0143(9) -0.0010(9)
O5 0.0260(10) 0.0210(10) 0.0235(9) -0.0045(8) 0.0000(8) -0.0051(8)
O6 0.0201(9) 0.0209(10) 0.0228(9) 0.0009(7) 0.0005(8) 0.0005(7)
O7 0.0228(10) 0.0231(10) 0.0278(9) -0.0011(8) 0.0001(8) 0.0023(8)
N3 0.172(5) 0.061(3) 0.136(4) 0.000(3) 0.030(4) 0.012(3)
C23 0.102(4) 0.101(5) 0.100(4) -0.013(3) -0.032(3) 0.037(4)
C24 0.112(5) 0.047(3) 0.132(5) -0.012(3) -0.081(4) 0.029(3)
C25 0.122(5) 0.058(3) 0.116(4) 0.016(3) -0.050(4) -0.020(3)
C26 0.159(6) 0.074(4) 0.135(5) 0.003(4) 0.033(4) -0.007(4)
C27 0.200(7) 0.051(3) 0.175(6) 0.000(4) 0.076(5) 0.018(4)
N4 0.306(11) 0.124(6) 0.050(4) 0.000 0.000 0.143(7)
C28 0.168(6) 0.103(4) 0.067(3) -0.017(3) -0.038(3) 0.051(4)
C29 0.050(3) 0.316(11) 0.117(5) 0.067(6) 0.006(3) -0.007(5)
C30 0.089(8) 0.73(4) 0.107(8) 0.000 0.000 0.120(15)

_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 O7 1.7798(17) . ?
Ti1 O6 1.8874(17) . ?
Ti1 O6 1.9454(17) 7_566 ?
Ti1 O1 2.0196(17) . ?
Ti1 O5 2.0626(16) . ?
Ti1 N2 2.262(2) . ?
Ti1 Ti3 3.1213(6) . ?
Ti1 Ti2 3.2053(6) . ?
Ti1 Ti2 3.3278(6) 8_646 ?
Ti1 Ti1 3.3623(7) 8_646 ?
Ti1 Ti1 3.3624(7) 7_566 ?
Ti2 O3 1.8348(19) . ?
Ti2 O7 1.8627(17) 7_566 ?
Ti2 O5 1.8939(17) . ?
Ti2 O2 1.9154(18) . ?
Ti2 O1 2.1160(18) . ?
Ti2 N1 2.288(2) . ?
Ti2 Ti1 3.3278(6) 7_566 ?
Ti3 O4 1.8498(18) . ?
Ti3 O4 1.8498(18) 2_765 ?
Ti3 O5 1.9166(16) . ?
Ti3 O5 1.9166(16) 2_765 ?
Ti3 O6 2.1332(16) 2_765 ?
Ti3 O6 2.1332(16) . ?
Ti3 Ti1 3.1213(6) 2_765 ?
O1 C1 1.353(3) . ?
C1 C6 1.376(4) . ?
C1 C2 1.404(4) . ?
C2 O2 1.342(3) . ?
C2 C3 1.386(4) . ?
C3 C4 1.417(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.350(5) . ?
C4 H4 0.9500 . ?
C5 C6 1.379(4) . ?
C5 H5 0.9500 . ?
C6 H6 0.9500 . ?
N1 C7 1.342(4) . ?
N1 C11 1.344(4) . ?
C7 C8 1.357(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.383(5) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(5) . ?
C9 H9 0.9500 . ?
C10 C11 1.365(5) . ?
C10 H10 0.9500 . ?
C11 H11 0.9500 . ?
N2 C12 1.341(4) . ?
N2 C16 1.343(4) . ?
C12 C13 1.388(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.357(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.357(5) . ?
C14 H14 0.9500 . ?
C15 C16 1.365(4) . ?
C15 H15 0.9500 . ?
C16 H16 0.9500 . ?
O3 C17 1.354(3) . ?
C17 C18 1.384(4) . ?
C17 C22 1.402(4) 2_765 ?
C18 C19 1.374(4) . ?
C18 H18 0.9500 . ?
C19 C20 1.400(4) 2_765 ?
C19 H19 0.9500 . ?
C20 C21 1.391(4) . ?
C20 C19 1.400(4) 2_765 ?
C20 H20 0.9500 . ?
C21 C22 1.382(4) . ?
C21 H21 0.9500 . ?
C22 O4 1.344(3) . ?
C22 C17 1.402(4) 2_765 ?
O6 Ti1 1.9455(17) 8_646 ?
O7 Ti2 1.8626(17) 8_646 ?
N3 C27 1.319(7) . ?
N3 C23 1.338(6) . ?
C23 C24 1.333(7) . ?
C23 H23 0.9500 . ?
C24 C25 1.391(7) . ?
C24 H24 0.9500 . ?
C25 C26 1.348(7) . ?
C25 H25 0.9500 . ?
C26 C27 1.375(8) . ?
C26 H26 0.9500 . ?
C27 H27 0.9500 . ?
N4 C28 1.298(6) . ?
N4 C28 1.298(6) 2_755 ?
C28 C29 1.228(6) . ?
C28 H28 0.9500 . ?
C29 C30 1.314(7) . ?
C29 H29 0.9500 . ?
C30 C29 1.314(7) 2_755 ?
C30 H30 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
O7 Ti1 O6 105.01(8) . . ?
O7 Ti1 O6 96.25(7) . 7_566 ?
O6 Ti1 O6 91.10(10) . 7_566 ?
O7 Ti1 O1 105.17(8) . . ?
O6 Ti1 O1 149.55(7) . . ?
O6 Ti1 O1 89.60(7) 7_566 . ?
O7 Ti1 O5 165.28(7) . . ?
O6 Ti1 O5 77.39(7) . . ?
O6 Ti1 O5 98.22(7) 7_566 . ?
O1 Ti1 O5 72.38(7) . . ?
O7 Ti1 N2 82.94(8) . . ?
O6 Ti1 N2 92.80(8) . . ?
O6 Ti1 N2 176.10(8) 7_566 . ?
O1 Ti1 N2 86.94(8) . . ?
O5 Ti1 N2 82.44(7) . . ?
O7 Ti1 Ti3 146.91(6) . . ?
O6 Ti1 Ti3 42.01(5) . . ?
O6 Ti1 Ti3 88.47(5) 7_566 . ?
O1 Ti1 Ti3 107.60(5) . . ?
O5 Ti1 Ti3 36.70(5) . . ?
N2 Ti1 Ti3 94.29(6) . . ?
O7 Ti1 Ti2 145.46(6) . . ?
O6 Ti1 Ti2 109.42(5) . . ?
O6 Ti1 Ti2 85.96(5) 7_566 . ?
O1 Ti1 Ti2 40.29(5) . . ?
O5 Ti1 Ti2 34.16(5) . . ?
N2 Ti1 Ti2 92.55(6) . . ?
Ti3 Ti1 Ti2 67.403(12) . . ?
O7 Ti1 Ti2 24.58(6) . 8_646 ?
O6 Ti1 Ti2 83.34(5) . 8_646 ?
O6 Ti1 Ti2 85.24(5) 7_566 8_646 ?
O1 Ti1 Ti2 127.03(5) . 8_646 ?
O5 Ti1 Ti2 160.46(5) . 8_646 ?
N2 Ti1 Ti2 95.42(6) . 8_646 ?
Ti3 Ti1 Ti2 124.850(17) . 8_646 ?
Ti2 Ti1 Ti2 164.630(17) . 8_646 ?
O7 Ti1 Ti1 81.22(6) . 8_646 ?
O6 Ti1 Ti1 29.17(5) . 8_646 ?
O6 Ti1 Ti1 77.04(5) 7_566 8_646 ?
O1 Ti1 Ti1 165.85(5) . 8_646 ?
O5 Ti1 Ti1 104.60(5) . 8_646 ?
N2 Ti1 Ti1 106.55(6) . 8_646 ?
Ti3 Ti1 Ti1 67.932(11) . 8_646 ?
Ti2 Ti1 Ti1 132.326(16) . 8_646 ?
Ti2 Ti1 Ti1 57.251(16) 8_646 8_646 ?
O7 Ti1 Ti1 124.07(6) . 7_566 ?
O6 Ti1 Ti1 88.02(5) . 7_566 ?
O6 Ti1 Ti1 28.22(5) 7_566 7_566 ?
O1 Ti1 Ti1 78.46(5) . 7_566 ?
O5 Ti1 Ti1 70.18(5) . 7_566 ?
N2 Ti1 Ti1 151.75(6) . 7_566 ?
Ti3 Ti1 Ti1 67.932(11) . 7_566 ?
Ti2 Ti1 Ti1 60.833(16) . 7_566 ?
Ti2 Ti1 Ti1 112.701(19) 8_646 7_566 ?
Ti1 Ti1 Ti1 87.499(6) 8_646 7_566 ?
O3 Ti2 O7 96.98(8) . 7_566 ?
O3 Ti2 O5 101.18(8) . . ?
O7 Ti2 O5 93.74(7) 7_566 . ?
O3 Ti2 O2 105.87(8) . . ?
O7 Ti2 O2 94.22(8) 7_566 . ?
O5 Ti2 O2 150.60(8) . . ?
O3 Ti2 O1 168.85(8) . . ?
O7 Ti2 O1 93.26(7) 7_566 . ?
O5 Ti2 O1 73.67(7) . . ?
O2 Ti2 O1 77.64(7) . . ?
O3 Ti2 N1 84.67(8) . . ?
O7 Ti2 N1 178.23(8) 7_566 . ?
O5 Ti2 N1 85.29(8) . . ?
O2 Ti2 N1 85.93(8) . . ?
O1 Ti2 N1 85.04(7) . . ?
O3 Ti2 Ti1 138.62(6) . . ?
O7 Ti2 Ti1 84.73(5) 7_566 . ?
O5 Ti2 Ti1 37.70(5) . . ?
O2 Ti2 Ti1 115.27(6) . . ?
O1 Ti2 Ti1 38.11(5) . . ?
N1 Ti2 Ti1 93.61(6) . . ?
O3 Ti2 Ti1 110.07(6) . 7_566 ?
O7 Ti2 Ti1 23.42(5) 7_566 7_566 ?
O5 Ti2 Ti1 72.44(5) . 7_566 ?
O2 Ti2 Ti1 107.97(6) . 7_566 ?
O1 Ti2 Ti1 78.18(5) . 7_566 ?
N1 Ti2 Ti1 155.07(6) . 7_566 ?
Ti1 Ti2 Ti1 61.917(16) . 7_566 ?
O4 Ti3 O4 94.45(12) . 2_765 ?
O4 Ti3 O5 101.60(8) . . ?
O4 Ti3 O5 92.17(8) 2_765 . ?
O4 Ti3 O5 92.17(8) . 2_765 ?
O4 Ti3 O5 101.60(8) 2_765 2_765 ?
O5 Ti3 O5 159.73(10) . 2_765 ?
O4 Ti3 O6 167.02(7) . 2_765 ?
O4 Ti3 O6 90.53(7) 2_765 2_765 ?
O5 Ti3 O6 90.16(7) . 2_765 ?
O5 Ti3 O6 75.07(7) 2_765 2_765 ?
O4 Ti3 O6 90.53(7) . . ?
O4 Ti3 O6 167.02(7) 2_765 . ?
O5 Ti3 O6 75.07(7) . . ?
O5 Ti3 O6 90.16(7) 2_765 . ?
O6 Ti3 O6 87.19(9) 2_765 . ?
O4 Ti3 Ti1 130.72(6) . 2_765 ?
O4 Ti3 Ti1 104.71(6) 2_765 2_765 ?
O5 Ti3 Ti1 122.07(5) . 2_765 ?
O5 Ti3 Ti1 40.03(5) 2_765 2_765 ?
O6 Ti3 Ti1 36.31(5) 2_765 2_765 ?
O6 Ti3 Ti1 80.76(5) . 2_765 ?
O4 Ti3 Ti1 104.70(6) . . ?
O4 Ti3 Ti1 130.72(6) 2_765 . ?
O5 Ti3 Ti1 40.03(5) . . ?
O5 Ti3 Ti1 122.07(5) 2_765 . ?
O6 Ti3 Ti1 80.76(5) 2_765 . ?
O6 Ti3 Ti1 36.31(5) . . ?
Ti1 Ti3 Ti1 96.30(2) 2_765 . ?
C1 O1 Ti1 139.54(16) . . ?
C1 O1 Ti2 112.28(16) . . ?
Ti1 O1 Ti2 101.59(7) . . ?
O1 C1 C6 125.7(3) . . ?
O1 C1 C2 113.4(2) . . ?
C6 C1 C2 120.9(3) . . ?
O2 C2 C3 124.3(3) . . ?
O2 C2 C1 116.1(2) . . ?
C3 C2 C1 119.5(3) . . ?
C2 O2 Ti2 118.08(16) . . ?
C2 C3 C4 117.9(3) . . ?
C2 C3 H3 121.1 . . ?
C4 C3 H3 121.1 . . ?
C5 C4 C3 121.7(3) . . ?
C5 C4 H4 119.2 . . ?
C3 C4 H4 119.2 . . ?
C4 C5 C6 120.5(3) . . ?
C4 C5 H5 119.7 . . ?
C6 C5 H5 119.7 . . ?
C1 C6 C5 119.5(3) . . ?
C1 C6 H6 120.3 . . ?
C5 C6 H6 120.3 . . ?
C7 N1 C11 116.4(3) . . ?
C7 N1 Ti2 123.2(2) . . ?
C11 N1 Ti2 120.3(2) . . ?
N1 C7 C8 124.5(3) . . ?
N1 C7 H7 117.7 . . ?
C8 C7 H7 117.7 . . ?
C7 C8 C9 118.6(4) . . ?
C7 C8 H8 120.7 . . ?
C9 C8 H8 120.7 . . ?
C10 C9 C8 117.5(3) . . ?
C10 C9 H9 121.2 . . ?
C8 C9 H9 121.2 . . ?
C11 C10 C9 120.7(3) . . ?
C11 C10 H10 119.7 . . ?
C9 C10 H10 119.7 . . ?
N1 C11 C10 122.2(3) . . ?
N1 C11 H11 118.9 . . ?
C10 C11 H11 118.9 . . ?
C12 N2 C16 116.9(2) . . ?
C12 N2 Ti1 122.52(18) . . ?
C16 N2 Ti1 120.49(18) . . ?
N2 C12 C13 122.0(3) . . ?
N2 C12 H12 119.0 . . ?
C13 C12 H12 119.0 . . ?
C14 C13 C12 120.1(3) . . ?
C14 C13 H13 120.0 . . ?
C12 C13 H13 120.0 . . ?
C13 C14 C15 117.8(3) . . ?
C13 C14 H14 121.1 . . ?
C15 C14 H14 121.1 . . ?
C14 C15 C16 120.6(3) . . ?
C14 C15 H15 119.7 . . ?
C16 C15 H15 119.7 . . ?
N2 C16 C15 122.6(3) . . ?
N2 C16 H16 118.7 . . ?
C15 C16 H16 118.7 . . ?
C17 O3 Ti2 144.63(18) . . ?
O3 C17 C18 118.9(3) . . ?
O3 C17 C22 121.0(2) . 2_765 ?
C18 C17 C22 120.1(3) . 2_765 ?
C19 C18 C17 121.2(3) . . ?
C19 C18 H18 119.4 . . ?
C17 C18 H18 119.4 . . ?
C18 C19 C20 119.0(3) . 2_765 ?
C18 C19 H19 120.5 . . ?
C20 C19 H19 120.5 2_765 . ?
C21 C20 C19 120.1(3) . 2_765 ?
C21 C20 H20 119.9 . . ?
C19 C20 H20 120.0 2_765 . ?
C22 C21 C20 120.6(3) . . ?
C22 C21 H21 119.7 . . ?
C20 C21 H21 119.7 . . ?
O4 C22 C21 119.4(3) . . ?
O4 C22 C17 121.6(2) . 2_765 ?
C21 C22 C17 118.9(2) . 2_765 ?
C22 O4 Ti3 146.63(18) . . ?
Ti2 O5 Ti3 134.27(9) . . ?
Ti2 O5 Ti1 108.14(8) . . ?
Ti3 O5 Ti1 103.27(7) . . ?
Ti1 O6 Ti1 122.62(8) . 8_646 ?
Ti1 O6 Ti3 101.68(7) . . ?
Ti1 O6 Ti3 125.56(8) 8_646 . ?
Ti1 O7 Ti2 132.01(10) . 8_646 ?
C27 N3 C23 115.7(5) . . ?
C24 C23 N3 122.5(6) . . ?
C24 C23 H23 118.7 . . ?
N3 C23 H23 118.7 . . ?
C23 C24 C25 121.2(5) . . ?
C23 C24 H24 119.4 . . ?
C25 C24 H24 119.4 . . ?
C26 C25 C24 117.0(6) . . ?
C26 C25 H25 121.5 . . ?
C24 C25 H25 121.5 . . ?
C25 C26 C27 118.2(6) . . ?
C25 C26 H26 120.9 . . ?
C27 C26 H26 120.9 . . ?
N3 C27 C26 125.1(5) . . ?
N3 C27 H27 117.4 . . ?
C26 C27 H27 117.4 . . ?
C28 N4 C28 115.7(6) . 2_755 ?
C29 C28 N4 123.8(6) . . ?
C29 C28 H28 118.1 . . ?
N4 C28 H28 118.1 . . ?
C28 C29 C30 118.7(7) . . ?
C28 C29 H29 120.7 . . ?
C30 C29 H29 120.7 . . ?
C29 C30 C29 119.3(9) 2_755 . ?
C29 C30 H30 120.3 2_755 . ?
C29 C30 H30 120.3 . . ?

_diffrn_measured_fraction_theta_max 0.987
_diffrn_reflns_theta_full        29.08
_diffrn_measured_fraction_theta_full 0.987
_refine_diff_density_max         0.358
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.053
_database_code_depnum_ccdc_archive 'CCDC 953666'