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

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#                                CCDC 
# 
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#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
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#  fide research purposes only. It may contain copyright material
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data_2

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C74 H122 N4 O7 Ti2'
_chemical_formula_sum            'C74 H122 N4 O7 Ti2'
_chemical_melting_point          ?

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1275.56

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_int_tables_number      15
_chemical_absolute_configuration ?

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

_cell_length_a                   21.183(3)
_cell_length_b                   10.8850(13)
_cell_length_c                   32.283(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.157(8)
_cell_angle_gamma                90.00
_cell_volume                     7276.8(17)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    9312
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      24.76
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2776
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8989
_exptl_absorpt_correction_T_max  0.9476
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            40097
_diffrn_reflns_av_R_equivalents  0.0522
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_theta_min         2.57
_diffrn_reflns_theta_max         25.12
_reflns_number_total             6454
_reflns_number_gt                4848
_reflns_threshold_expression     >2σ(I)

_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          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
One of the tBu fragments presents disorder. C61 and the methyl groups attached to it were modelled and gave 62/38% occupancies.
SADI restraints and EADP constraints were applied to obtain suitable C61-C(Me) distances.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0708P)²+30.2415P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6454
_refine_ls_number_parameters     407
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.0911
_refine_ls_R_factor_gt           0.0642
_refine_ls_wR_factor_ref         0.1681
_refine_ls_wR_factor_gt          0.1572
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.049
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.08706(3) 0.02718(5) 0.011298(17) 0.01565(17) Uani 1 1 d . . .
O1 O 0.09545(11) 0.00934(19) -0.04616(7) 0.0194(5) Uani 1 1 d . . .
O2 O 0.09893(11) 0.0151(2) 0.07161(7) 0.0228(5) Uani 1 1 d . . .
O3 O 0.0000 0.0000 0.0000 0.0180(7) Uani 1 2 d S . .
O4 O 0.09561(11) 0.1947(2) 0.01129(7) 0.0233(5) Uani 1 1 d . . .
N1 N 0.10254(12) -0.1801(2) 0.01420(8) 0.0170(6) Uani 1 1 d . . .
N2 N 0.20430(14) -0.0035(3) 0.02770(9) 0.0259(7) Uani 1 1 d . . .
C31 C 0.11472(18) 0.0902(3) -0.12952(10) 0.0264(8) Uani 1 1 d . . .
C11 C 0.10017(15) -0.0764(3) -0.07508(9) 0.0171(7) Uani 1 1 d . . .
C12 C 0.11335(16) -0.0445(3) -0.11509(10) 0.0214(7) Uani 1 1 d . . .
C15 C 0.09893(16) -0.2922(3) -0.09453(10) 0.0217(7) Uani 1 1 d . . .
H15 H 0.0940 -0.3740 -0.0875 0.026 Uiso 1 1 calc R . .
C51 C 0.11936(18) 0.1016(3) 0.16112(10) 0.0280(8) Uani 1 1 d . . .
C16 C 0.09172(15) -0.2001(3) -0.06564(9) 0.0181(7) Uani 1 1 d . . .
C26 C 0.09600(16) -0.1925(3) 0.09206(10) 0.0216(7) Uani 1 1 d . . .
C27 C 0.06918(16) -0.2296(3) 0.04709(9) 0.0190(7) Uani 1 1 d . . .
H27A H 0.0699 -0.3186 0.0456 0.023 Uiso 1 1 calc R . .
H27B H 0.0243 -0.2043 0.0398 0.023 Uiso 1 1 calc R . .
C22 C 0.11803(16) -0.0328(3) 0.14634(10) 0.0246(8) Uani 1 1 d . . .
C17 C 0.06692(16) -0.2348(3) -0.02679(9) 0.0184(7) Uani 1 1 d . . .
H17A H 0.0220 -0.2103 -0.0311 0.022 Uiso 1 1 calc R . .
H17B H 0.0684 -0.3235 -0.0241 0.022 Uiso 1 1 calc R . .
C21 C 0.10417(16) -0.0676(3) 0.10287(9) 0.0190(7) Uani 1 1 d . . .
C13 C 0.12016(16) -0.1399(3) -0.14235(10) 0.0234(7) Uani 1 1 d . . .
H13 H 0.1300 -0.1200 -0.1683 0.028 Uiso 1 1 calc R . .
C14 C 0.11321(16) -0.2645(3) -0.13322(10) 0.0225(7) Uani 1 1 d . . .
C25 C 0.10675(18) -0.2827(3) 0.12311(10) 0.0269(8) Uani 1 1 d . A .
H25 H 0.1023 -0.3649 0.1152 0.032 Uiso 1 1 calc R . .
C1 C 0.17079(16) -0.2190(3) 0.02286(10) 0.0215(7) Uani 1 1 d . . .
H1A H 0.1841 -0.2324 -0.0038 0.026 Uiso 1 1 calc R . .
H1B H 0.1752 -0.2963 0.0382 0.026 Uiso 1 1 calc R . .
C41 C 0.11843(19) -0.3618(3) -0.16687(10) 0.0292(8) Uani 1 1 d . . .
C23 C 0.12802(18) -0.1286(4) 0.17608(11) 0.0319(9) Uani 1 1 d . A .
H23 H 0.1381 -0.1076 0.2046 0.038 Uiso 1 1 calc R . .
C53 C 0.0603(2) 0.1710(4) 0.13772(13) 0.0426(10) Uani 1 1 d . . .
H53A H 0.0219 0.1314 0.1424 0.064 Uiso 1 1 calc R . .
H53B H 0.0599 0.1717 0.1079 0.064 Uiso 1 1 calc R . .
H53C H 0.0617 0.2539 0.1480 0.064 Uiso 1 1 calc R . .
C2 C 0.21428(17) -0.1248(3) 0.04842(11) 0.0275(8) Uani 1 1 d . . .
H2A H 0.2052 -0.1195 0.0766 0.033 Uiso 1 1 calc R . .
H2B H 0.2590 -0.1495 0.0512 0.033 Uiso 1 1 calc R . .
C32 C 0.1692(2) 0.1621(4) -0.10093(13) 0.0398(10) Uani 1 1 d . . .
H32A H 0.1642 0.1573 -0.0721 0.060 Uiso 1 1 calc R . .
H32B H 0.1674 0.2465 -0.1097 0.060 Uiso 1 1 calc R . .
H32C H 0.2101 0.1275 -0.1030 0.060 Uiso 1 1 calc R . .
C44 C 0.0637(2) -0.3394(4) -0.20547(11) 0.0387(10) Uani 1 1 d . . .
H44A H 0.0675 -0.2580 -0.2161 0.058 Uiso 1 1 calc R . .
H44B H 0.0229 -0.3477 -0.1973 0.058 Uiso 1 1 calc R . .
H44C H 0.0665 -0.3984 -0.2271 0.058 Uiso 1 1 calc R . .
C24 C 0.1239(2) -0.2527(4) 0.16576(11) 0.0351(9) Uani 1 1 d . . .
C33 C 0.0502(2) 0.1514(4) -0.12876(13) 0.0398(10) Uani 1 1 d . . .
H33A H 0.0160 0.1064 -0.1466 0.060 Uiso 1 1 calc R . .
H33B H 0.0506 0.2342 -0.1390 0.060 Uiso 1 1 calc R . .
H33C H 0.0435 0.1523 -0.1003 0.060 Uiso 1 1 calc R . .
C34 C 0.1259(3) 0.1011(4) -0.17485(12) 0.0517(13) Uani 1 1 d . . .
H34A H 0.0928 0.0566 -0.1939 0.077 Uiso 1 1 calc R . .
H34B H 0.1674 0.0673 -0.1760 0.077 Uiso 1 1 calc R . .
H34C H 0.1245 0.1860 -0.1830 0.077 Uiso 1 1 calc R . .
C3 C 0.23490(18) -0.0014(4) -0.00927(13) 0.0354(9) Uani 1 1 d . . .
H3A H 0.2146 -0.0614 -0.0296 0.053 Uiso 1 1 calc R . .
H3B H 0.2800 -0.0204 -0.0003 0.053 Uiso 1 1 calc R . .
H3C H 0.2300 0.0787 -0.0220 0.053 Uiso 1 1 calc R . .
C73 C 0.0820(2) 0.3829(4) -0.02934(16) 0.0548(12) Uani 1 1 d . . .
H73A H 0.0832 0.3387 -0.0549 0.082 Uiso 1 1 calc R . .
H73B H 0.1012 0.4624 -0.0304 0.082 Uiso 1 1 calc R . .
H73C H 0.0380 0.3923 -0.0266 0.082 Uiso 1 1 calc R . .
C43 C 0.1105(3) -0.4915(3) -0.15107(12) 0.0474(12) Uani 1 1 d . . .
H43A H 0.1134 -0.5494 -0.1730 0.071 Uiso 1 1 calc R . .
H43B H 0.0692 -0.4989 -0.1435 0.071 Uiso 1 1 calc R . .
H43C H 0.1441 -0.5079 -0.1267 0.071 Uiso 1 1 calc R . .
C52 C 0.1793(2) 0.1674(4) 0.15250(17) 0.0549(13) Uani 1 1 d . . .
H52A H 0.2175 0.1258 0.1672 0.082 Uiso 1 1 calc R . .
H52B H 0.1798 0.2507 0.1623 0.082 Uiso 1 1 calc R . .
H52C H 0.1782 0.1670 0.1226 0.082 Uiso 1 1 calc R . .
C71 C 0.1200(2) 0.3109(4) 0.00904(14) 0.0424(10) Uani 1 1 d . . .
H71 H 0.1646 0.3026 0.0054 0.051 Uiso 1 1 calc R . .
C54 C 0.1213(3) 0.1129(4) 0.20844(13) 0.0637(15) Uani 1 1 d . . .
H54A H 0.1585 0.0703 0.2240 0.096 Uiso 1 1 calc R . .
H54B H 0.0829 0.0775 0.2147 0.096 Uiso 1 1 calc R . .
H54C H 0.1238 0.1981 0.2164 0.096 Uiso 1 1 calc R . .
C42 C 0.1830(2) -0.3511(4) -0.17975(14) 0.0524(12) Uani 1 1 d . . .
H42A H 0.1878 -0.2696 -0.1900 0.079 Uiso 1 1 calc R . .
H42B H 0.1849 -0.4095 -0.2017 0.079 Uiso 1 1 calc R . .
H42C H 0.2171 -0.3675 -0.1557 0.079 Uiso 1 1 calc R . .
C72 C 0.1218(3) 0.3802(4) 0.05045(15) 0.0652(15) Uani 1 1 d . . .
H72A H 0.1460 0.3334 0.0737 0.098 Uiso 1 1 calc R . .
H72B H 0.0786 0.3920 0.0544 0.098 Uiso 1 1 calc R . .
H72C H 0.1421 0.4586 0.0493 0.098 Uiso 1 1 calc R . .
C4 C 0.2373(2) 0.0893(4) 0.05775(14) 0.0448(11) Uani 1 1 d . . .
H4A H 0.2314 0.1690 0.0448 0.067 Uiso 1 1 calc R . .
H4B H 0.2826 0.0707 0.0653 0.067 Uiso 1 1 calc R . .
H4C H 0.2195 0.0887 0.0827 0.067 Uiso 1 1 calc R . .
C61A C 0.1269(5) -0.3454(9) 0.2028(3) 0.036(2) Uani 0.617(5) 1 d PD A 1
C62A C 0.1230(6) -0.4773(7) 0.1852(2) 0.070(3) Uani 0.617(5) 1 d PD A 1
H62A H 0.0832 -0.4876 0.1648 0.104 Uiso 0.617(5) 1 calc PR A 1
H62B H 0.1246 -0.5348 0.2079 0.104 Uiso 0.617(5) 1 calc PR A 1
H62C H 0.1586 -0.4919 0.1717 0.104 Uiso 0.617(5) 1 calc PR A 1
C63A C 0.1891(5) -0.321(2) 0.2362(4) 0.058(3) Uani 0.617(5) 1 d PD A 1
H63A H 0.1883 -0.2390 0.2468 0.086 Uiso 0.617(5) 1 calc PR A 1
H63B H 0.2259 -0.3311 0.2235 0.086 Uiso 0.617(5) 1 calc PR A 1
H63C H 0.1918 -0.3785 0.2591 0.086 Uiso 0.617(5) 1 calc PR A 1
C64A C 0.0684(4) -0.3315(6) 0.2238(2) 0.0464(15) Uani 0.617(5) 1 d PD A 1
H64A H 0.0681 -0.2504 0.2354 0.070 Uiso 0.617(5) 1 calc PR A 1
H64B H 0.0712 -0.3911 0.2460 0.070 Uiso 0.617(5) 1 calc PR A 1
H64C H 0.0293 -0.3444 0.2029 0.070 Uiso 0.617(5) 1 calc PR A 1
C61B C 0.1451(8) -0.3616(16) 0.1956(6) 0.036(2) Uani 0.383(5) 1 d PD A 2
C62B C 0.0843(8) -0.4352(12) 0.1960(4) 0.070(3) Uani 0.383(5) 1 d PD A 2
H62D H 0.0516 -0.3817 0.2023 0.104 Uiso 0.383(5) 1 calc PR A 2
H62E H 0.0937 -0.4984 0.2171 0.104 Uiso 0.383(5) 1 calc PR A 2
H62F H 0.0691 -0.4720 0.1687 0.104 Uiso 0.383(5) 1 calc PR A 2
C63B C 0.1679(11) -0.316(4) 0.2408(7) 0.058(3) Uani 0.383(5) 1 d PD A 2
H63D H 0.1363 -0.2605 0.2477 0.086 Uiso 0.383(5) 1 calc PR A 2
H63E H 0.2083 -0.2733 0.2433 0.086 Uiso 0.383(5) 1 calc PR A 2
H63F H 0.1734 -0.3842 0.2599 0.086 Uiso 0.383(5) 1 calc PR A 2
C64B C 0.1970(6) -0.4465(10) 0.1866(3) 0.0464(15) Uani 0.383(5) 1 d PD A 2
H64D H 0.2359 -0.4006 0.1872 0.070 Uiso 0.383(5) 1 calc PR A 2
H64E H 0.1830 -0.4828 0.1591 0.070 Uiso 0.383(5) 1 calc PR A 2
H64F H 0.2052 -0.5100 0.2077 0.070 Uiso 0.383(5) 1 calc PR A 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.8271(6) . ?
Ti1 O4 1.833(2) . ?
Ti1 O1 1.910(2) . ?
Ti1 O2 1.915(2) . ?
Ti1 N1 2.279(3) . ?
Ti1 N2 2.451(3) . ?
O1 C11 1.339(4) . ?
O2 C21 1.339(4) . ?
O3 Ti1 1.8271(6) 5 ?
O4 C71 1.374(5) . ?
N1 C1 1.476(4) . ?
N1 C27 1.495(4) . ?
N1 C17 1.501(4) . ?
N2 C4 1.471(5) . ?
N2 C3 1.473(5) . ?
N2 C2 1.475(4) . ?
C31 C33 1.525(5) . ?
C31 C32 1.532(5) . ?
C31 C34 1.535(5) . ?
C31 C12 1.540(5) . ?
C11 C16 1.400(5) . ?
C11 C12 1.421(4) . ?
C12 C13 1.389(5) . ?
C15 C14 1.379(5) . ?
C15 C16 1.399(4) . ?
C15 H15 0.9300 . ?
C51 C53 1.519(5) . ?
C51 C54 1.524(5) . ?
C51 C52 1.534(6) . ?
C51 C22 1.538(5) . ?
C16 C17 1.506(4) . ?
C26 C25 1.388(4) . ?
C26 C21 1.405(5) . ?
C26 C27 1.499(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C22 C23 1.402(5) . ?
C22 C21 1.423(4) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C13 C14 1.402(5) . ?
C13 H13 0.9300 . ?
C14 C41 1.538(4) . ?
C25 C24 1.387(5) . ?
C25 H25 0.9300 . ?
C1 C2 1.504(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C41 C42 1.515(6) . ?
C41 C43 1.522(5) . ?
C41 C44 1.532(5) . ?
C23 C24 1.390(5) . ?
C23 H23 0.9300 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C24 C61B 1.53(2) . ?
C24 C61A 1.556(12) . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C73 C71 1.542(6) . ?
C73 H73A 0.9600 . ?
C73 H73B 0.9600 . ?
C73 H73C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C71 C72 1.528(6) . ?
C71 H71 0.9800 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C72 H72A 0.9600 . ?
C72 H72B 0.9600 . ?
C72 H72C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C61A C63A 1.538(10) . ?
C61A C64A 1.540(9) . ?
C61A C62A 1.541(10) . ?
C62A H62A 0.9600 . ?
C62A H62B 0.9600 . ?
C62A H62C 0.9600 . ?
C63A H63A 0.9600 . ?
C63A H63B 0.9600 . ?
C63A H63C 0.9600 . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
C61B C64B 1.510(13) . ?
C61B C62B 1.521(14) . ?
C61B C63B 1.522(14) . ?
C62B H62D 0.9600 . ?
C62B H62E 0.9600 . ?
C62B H62F 0.9600 . ?
C63B H63D 0.9600 . ?
C63B H63E 0.9600 . ?
C63B H63F 0.9600 . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O4 104.88(8) . . ?
O3 Ti1 O1 94.94(7) . . ?
O4 Ti1 O1 94.11(10) . . ?
O3 Ti1 O2 95.90(8) . . ?
O4 Ti1 O2 94.39(10) . . ?
O1 Ti1 O2 164.04(10) . . ?
O3 Ti1 N1 88.76(7) . . ?
O4 Ti1 N1 166.35(10) . . ?
O1 Ti1 N1 84.10(9) . . ?
O2 Ti1 N1 84.46(9) . . ?
O3 Ti1 N2 162.83(7) . . ?
O4 Ti1 N2 92.28(10) . . ?
O1 Ti1 N2 84.18(10) . . ?
O2 Ti1 N2 82.00(10) . . ?
N1 Ti1 N2 74.08(9) . . ?
C11 O1 Ti1 141.6(2) . . ?
C21 O2 Ti1 141.7(2) . . ?
Ti1 O3 Ti1 180.000(9) . 5 ?
C71 O4 Ti1 162.6(3) . . ?
C1 N1 C27 110.6(2) . . ?
C1 N1 C17 110.1(2) . . ?
C27 N1 C17 104.9(2) . . ?
C1 N1 Ti1 114.78(19) . . ?
C27 N1 Ti1 107.52(18) . . ?
C17 N1 Ti1 108.38(18) . . ?
C4 N2 C3 107.1(3) . . ?
C4 N2 C2 108.2(3) . . ?
C3 N2 C2 109.6(3) . . ?
C4 N2 Ti1 111.6(2) . . ?
C3 N2 Ti1 114.9(2) . . ?
C2 N2 Ti1 105.2(2) . . ?
C33 C31 C32 109.3(3) . . ?
C33 C31 C34 107.5(3) . . ?
C32 C31 C34 106.7(3) . . ?
C33 C31 C12 109.7(3) . . ?
C32 C31 C12 111.3(3) . . ?
C34 C31 C12 112.2(3) . . ?
O1 C11 C16 119.1(3) . . ?
O1 C11 C12 121.4(3) . . ?
C16 C11 C12 119.5(3) . . ?
C13 C12 C11 117.3(3) . . ?
C13 C12 C31 120.6(3) . . ?
C11 C12 C31 121.8(3) . . ?
C14 C15 C16 121.5(3) . . ?
C14 C15 H15 119.2 . . ?
C16 C15 H15 119.2 . . ?
C53 C51 C54 107.7(3) . . ?
C53 C51 C52 107.7(3) . . ?
C54 C51 C52 107.2(4) . . ?
C53 C51 C22 111.1(3) . . ?
C54 C51 C22 112.5(3) . . ?
C52 C51 C22 110.5(3) . . ?
C15 C16 C11 120.4(3) . . ?
C15 C16 C17 118.8(3) . . ?
C11 C16 C17 120.3(3) . . ?
C25 C26 C21 120.9(3) . . ?
C25 C26 C27 118.7(3) . . ?
C21 C26 C27 120.2(3) . . ?
N1 C27 C26 116.8(3) . . ?
N1 C27 H27A 108.1 . . ?
C26 C27 H27A 108.1 . . ?
N1 C27 H27B 108.1 . . ?
C26 C27 H27B 108.1 . . ?
H27A C27 H27B 107.3 . . ?
C23 C22 C21 116.6(3) . . ?
C23 C22 C51 120.3(3) . . ?
C21 C22 C51 123.0(3) . . ?
N1 C17 C16 115.8(3) . . ?
N1 C17 H17A 108.3 . . ?
C16 C17 H17A 108.3 . . ?
N1 C17 H17B 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
O2 C21 C26 118.5(3) . . ?
O2 C21 C22 122.1(3) . . ?
C26 C21 C22 119.4(3) . . ?
C12 C13 C14 124.1(3) . . ?
C12 C13 H13 117.9 . . ?
C14 C13 H13 117.9 . . ?
C15 C14 C13 117.0(3) . . ?
C15 C14 C41 123.5(3) . . ?
C13 C14 C41 119.4(3) . . ?
C24 C25 C26 121.3(3) . . ?
C24 C25 H25 119.4 . . ?
C26 C25 H25 119.4 . . ?
N1 C1 C2 111.7(3) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 107.9 . . ?
C42 C41 C43 109.4(4) . . ?
C42 C41 C44 109.6(3) . . ?
C43 C41 C44 107.7(3) . . ?
C42 C41 C14 110.1(3) . . ?
C43 C41 C14 111.9(3) . . ?
C44 C41 C14 108.1(3) . . ?
C24 C23 C22 124.4(3) . . ?
C24 C23 H23 117.8 . . ?
C22 C23 H23 117.8 . . ?
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 . . ?
N2 C2 C1 110.4(3) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C25 C24 C23 117.2(3) . . ?
C25 C24 C61B 115.0(7) . . ?
C23 C24 C61B 127.3(7) . . ?
C25 C24 C61A 124.7(5) . . ?
C23 C24 C61A 117.1(4) . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C71 C73 H73A 109.5 . . ?
C71 C73 H73B 109.5 . . ?
H73A C73 H73B 109.5 . . ?
C71 C73 H73C 109.5 . . ?
H73A C73 H73C 109.5 . . ?
H73B C73 H73C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
O4 C71 C72 110.4(3) . . ?
O4 C71 C73 111.8(4) . . ?
C72 C71 C73 111.4(4) . . ?
O4 C71 H71 107.7 . . ?
C72 C71 H71 107.7 . . ?
C73 C71 H71 107.7 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C71 C72 H72A 109.5 . . ?
C71 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C71 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C63A C61A C64A 109.0(7) . . ?
C63A C61A C62A 113.0(13) . . ?
C64A C61A C62A 105.5(7) . . ?
C63A C61A C24 108.5(10) . . ?
C64A C61A C24 111.6(7) . . ?
C62A C61A C24 109.3(6) . . ?
C61A C62A H62A 109.5 . . ?
C61A C62A H62B 109.5 . . ?
H62A C62A H62B 109.5 . . ?
C61A C62A H62C 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
C61A C63A H63A 109.5 . . ?
C61A C63A H63B 109.5 . . ?
H63A C63A H63B 109.5 . . ?
C61A C63A H63C 109.5 . . ?
H63A C63A H63C 109.5 . . ?
H63B C63A H63C 109.5 . . ?
C61A C64A H64A 109.5 . . ?
C61A C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C61A C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
C64B C61B C62B 109.4(13) . . ?
C64B C61B C63B 106.8(18) . . ?
C62B C61B C63B 105.2(16) . . ?
C64B C61B C24 118.7(11) . . ?
C62B C61B C24 106.0(12) . . ?
C63B C61B C24 109.9(19) . . ?
C61B C62B H62D 109.5 . . ?
C61B C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
C61B C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
C61B C63B H63D 109.5 . . ?
C61B C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C61B C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
C61B C64B H64D 109.5 . . ?
C61B C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C61B C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Ti1 O1 C11 -80.8(3) . . . . ?
O4 Ti1 O1 C11 173.9(3) . . . . ?
O2 Ti1 O1 C11 51.9(5) . . . . ?
N1 Ti1 O1 C11 7.5(3) . . . . ?
N2 Ti1 O1 C11 82.0(3) . . . . ?
O3 Ti1 O2 C21 78.9(3) . . . . ?
O4 Ti1 O2 C21 -175.7(3) . . . . ?
O1 Ti1 O2 C21 -53.7(6) . . . . ?
N1 Ti1 O2 C21 -9.3(3) . . . . ?
N2 Ti1 O2 C21 -84.0(3) . . . . ?
O3 Ti1 O4 C71 -158.4(8) . . . . ?
O1 Ti1 O4 C71 -62.2(8) . . . . ?
O2 Ti1 O4 C71 104.3(8) . . . . ?
N1 Ti1 O4 C71 19.7(11) . . . . ?
N2 Ti1 O4 C71 22.1(8) . . . . ?
O3 Ti1 N1 C1 179.38(19) . . . . ?
O4 Ti1 N1 C1 1.2(5) . . . . ?
O1 Ti1 N1 C1 84.3(2) . . . . ?
O2 Ti1 N1 C1 -84.6(2) . . . . ?
N2 Ti1 N1 C1 -1.33(19) . . . . ?
O3 Ti1 N1 C27 -57.06(18) . . . . ?
O4 Ti1 N1 C27 124.8(4) . . . . ?
O1 Ti1 N1 C27 -152.2(2) . . . . ?
O2 Ti1 N1 C27 38.99(19) . . . . ?
N2 Ti1 N1 C27 122.2(2) . . . . ?
O3 Ti1 N1 C17 55.88(18) . . . . ?
O4 Ti1 N1 C17 -122.3(4) . . . . ?
O1 Ti1 N1 C17 -39.21(19) . . . . ?
O2 Ti1 N1 C17 151.9(2) . . . . ?
N2 Ti1 N1 C17 -124.8(2) . . . . ?
O3 Ti1 N2 C4 -140.1(3) . . . . ?
O4 Ti1 N2 C4 38.1(3) . . . . ?
O1 Ti1 N2 C4 132.0(3) . . . . ?
O2 Ti1 N2 C4 -56.0(3) . . . . ?
N1 Ti1 N2 C4 -142.5(3) . . . . ?
O3 Ti1 N2 C3 97.6(3) . . . . ?
O4 Ti1 N2 C3 -84.2(2) . . . . ?
O1 Ti1 N2 C3 9.7(2) . . . . ?
O2 Ti1 N2 C3 -178.3(2) . . . . ?
N1 Ti1 N2 C3 95.2(2) . . . . ?
O3 Ti1 N2 C2 -23.0(4) . . . . ?
O4 Ti1 N2 C2 155.2(2) . . . . ?
O1 Ti1 N2 C2 -110.9(2) . . . . ?
O2 Ti1 N2 C2 61.1(2) . . . . ?
N1 Ti1 N2 C2 -25.38(19) . . . . ?
Ti1 O1 C11 C16 7.5(5) . . . . ?
Ti1 O1 C11 C12 -172.7(2) . . . . ?
O1 C11 C12 C13 177.3(3) . . . . ?
C16 C11 C12 C13 -2.9(5) . . . . ?
O1 C11 C12 C31 -7.6(5) . . . . ?
C16 C11 C12 C31 172.2(3) . . . . ?
C33 C31 C12 C13 117.9(4) . . . . ?
C32 C31 C12 C13 -121.0(4) . . . . ?
C34 C31 C12 C13 -1.5(5) . . . . ?
C33 C31 C12 C11 -57.2(4) . . . . ?
C32 C31 C12 C11 63.9(4) . . . . ?
C34 C31 C12 C11 -176.6(3) . . . . ?
C14 C15 C16 C11 -1.3(5) . . . . ?
C14 C15 C16 C17 171.4(3) . . . . ?
O1 C11 C16 C15 -177.4(3) . . . . ?
C12 C11 C16 C15 2.8(5) . . . . ?
O1 C11 C16 C17 10.0(5) . . . . ?
C12 C11 C16 C17 -169.8(3) . . . . ?
C1 N1 C27 C26 59.7(3) . . . . ?
C17 N1 C27 C26 178.4(3) . . . . ?
Ti1 N1 C27 C26 -66.4(3) . . . . ?
C25 C26 C27 N1 -131.8(3) . . . . ?
C21 C26 C27 N1 54.1(4) . . . . ?
C53 C51 C22 C23 -130.0(4) . . . . ?
C54 C51 C22 C23 -9.2(5) . . . . ?
C52 C51 C22 C23 110.5(4) . . . . ?
C53 C51 C22 C21 47.2(5) . . . . ?
C54 C51 C22 C21 168.0(4) . . . . ?
C52 C51 C22 C21 -72.3(4) . . . . ?
C1 N1 C17 C16 -60.3(3) . . . . ?
C27 N1 C17 C16 -179.3(3) . . . . ?
Ti1 N1 C17 C16 66.0(3) . . . . ?
C15 C16 C17 N1 134.9(3) . . . . ?
C11 C16 C17 N1 -52.5(4) . . . . ?
Ti1 O2 C21 C26 -4.4(5) . . . . ?
Ti1 O2 C21 C22 175.2(2) . . . . ?
C25 C26 C21 O2 174.0(3) . . . . ?
C27 C26 C21 O2 -12.0(5) . . . . ?
C25 C26 C21 C22 -5.6(5) . . . . ?
C27 C26 C21 C22 168.3(3) . . . . ?
C23 C22 C21 O2 -174.4(3) . . . . ?
C51 C22 C21 O2 8.3(5) . . . . ?
C23 C22 C21 C26 5.2(5) . . . . ?
C51 C22 C21 C26 -172.1(3) . . . . ?
C11 C12 C13 C14 1.7(5) . . . . ?
C31 C12 C13 C14 -173.5(3) . . . . ?
C16 C15 C14 C13 0.0(5) . . . . ?
C16 C15 C14 C41 -177.0(3) . . . . ?
C12 C13 C14 C15 -0.2(5) . . . . ?
C12 C13 C14 C41 176.9(3) . . . . ?
C21 C26 C25 C24 2.0(6) . . . . ?
C27 C26 C25 C24 -172.1(3) . . . . ?
C27 N1 C1 C2 -93.5(3) . . . . ?
C17 N1 C1 C2 151.0(3) . . . . ?
Ti1 N1 C1 C2 28.4(3) . . . . ?
C15 C14 C41 C42 -125.8(4) . . . . ?
C13 C14 C41 C42 57.3(4) . . . . ?
C15 C14 C41 C43 -3.9(5) . . . . ?
C13 C14 C41 C43 179.2(3) . . . . ?
C15 C14 C41 C44 114.4(4) . . . . ?
C13 C14 C41 C44 -62.5(4) . . . . ?
C21 C22 C23 C24 -1.4(6) . . . . ?
C51 C22 C23 C24 176.0(4) . . . . ?
C4 N2 C2 C1 168.4(3) . . . . ?
C3 N2 C2 C1 -75.0(4) . . . . ?
Ti1 N2 C2 C1 49.1(3) . . . . ?
N1 C1 C2 N2 -53.8(4) . . . . ?
C26 C25 C24 C23 1.9(6) . . . . ?
C26 C25 C24 C61B -170.2(7) . . . . ?
C26 C25 C24 C61A 170.4(5) . . . . ?
C22 C23 C24 C25 -2.2(6) . . . . ?
C22 C23 C24 C61B 168.8(7) . . . . ?
C22 C23 C24 C61A -171.6(5) . . . . ?
Ti1 O4 C71 C72 -120.6(8) . . . . ?
Ti1 O4 C71 C73 114.7(8) . . . . ?
C25 C24 C61A C63A 136.1(8) . . . . ?
C23 C24 C61A C63A -55.3(10) . . . . ?
C61B C24 C61A C63A 71(3) . . . . ?
C25 C24 C61A C64A -103.8(7) . . . . ?
C23 C24 C61A C64A 64.7(8) . . . . ?
C61B C24 C61A C64A -169(3) . . . . ?
C25 C24 C61A C62A 12.5(10) . . . . ?
C23 C24 C61A C62A -179.0(6) . . . . ?
C61B C24 C61A C62A -53(3) . . . . ?
C25 C24 C61B C64B 52.1(15) . . . . ?
C23 C24 C61B C64B -119.0(12) . . . . ?
C61A C24 C61B C64B 177(4) . . . . ?
C25 C24 C61B C62B -71.4(10) . . . . ?
C23 C24 C61B C62B 117.5(11) . . . . ?
C61A C24 C61B C62B 53(2) . . . . ?
C25 C24 C61B C63B 175.4(10) . . . . ?
C23 C24 C61B C63B 4.3(15) . . . . ?
C61A C24 C61B C63B -60(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        25.12
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         1.120
_refine_diff_density_min         -0.429
_refine_diff_density_rms         0.075

_database_code_depnum_ccdc_archive 'CCDC 994885'
#######################################################################
#
#                 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_4

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C34 H54 Cl2 N2 O2 Ti'
_chemical_formula_sum            'C34 H54 Cl2 N2 O2 Ti'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            orange

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         641.59

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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

_cell_length_a                   16.7000(11)
_cell_length_b                   15.6390(10)
_cell_length_c                   15.1740(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.821(2)
_cell_angle_gamma                90.00
_cell_volume                     3567.3(4)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1290
_cell_measurement_theta_min      2.60
_cell_measurement_theta_max      20.42
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.195
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1376
_exptl_absorpt_coefficient_mu    0.420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9282
_exptl_absorpt_correction_T_max  0.9834
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15392
_diffrn_reflns_av_R_equivalents  0.0811
_diffrn_reflns_av_sigmaI/netI    0.1376
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         1.98
_diffrn_reflns_theta_max         25.03
_reflns_number_total             6294
_reflns_number_gt                3432
_reflns_threshold_expression     >2σ(I)

_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          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
One of the tBu fragments presents disordered methyl groups. The methyl groups attached to C61 were modelled and gave 24/76% occupancies.
SADI restraints and EADP constraints were applied on the disordered atoms in order to obtain suitable C61-C(Me) distances.
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0499P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         6294
_refine_ls_number_parameters     380
_refine_ls_number_restraints     15
_refine_ls_R_factor_all          0.1358
_refine_ls_R_factor_gt           0.0590
_refine_ls_wR_factor_ref         0.1272
_refine_ls_wR_factor_gt          0.1093
_refine_ls_goodness_of_fit_ref   0.906
_refine_ls_restrained_S_all      0.907
_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 0.48147(4) 0.25712(4) 0.47157(5) 0.0217(2) Uani 1 1 d . . .
Cl1 Cl 0.52339(6) 0.14452(6) 0.40308(7) 0.0296(3) Uani 1 1 d . . .
Cl2 Cl 0.43430(7) 0.35541(7) 0.34568(7) 0.0355(3) Uani 1 1 d . . .
O1 O 0.36592(15) 0.22136(15) 0.43121(16) 0.0255(7) Uani 1 1 d . . .
N1 N 0.44397(19) 0.34275(19) 0.5687(2) 0.0216(8) Uani 1 1 d . . .
O2 O 0.58967(15) 0.31032(16) 0.52896(17) 0.0245(6) Uani 1 1 d . . .
N2 N 0.5277(2) 0.1771(2) 0.6130(2) 0.0268(8) Uani 1 1 d . . .
C11 C 0.2841(2) 0.2464(2) 0.4180(2) 0.0221(9) Uani 1 1 d . . .
C15 C 0.1937(2) 0.3462(2) 0.4553(2) 0.0234(9) Uani 1 1 d . . .
H15 H 0.1894 0.3956 0.4871 0.028 Uiso 1 1 calc R . .
C2 C 0.5241(2) 0.2335(2) 0.6904(2) 0.0272(10) Uani 1 1 d . . .
H2A H 0.5768 0.2691 0.7177 0.033 Uiso 1 1 calc R . .
H2B H 0.5230 0.1986 0.7428 0.033 Uiso 1 1 calc R . .
C27 C 0.5042(2) 0.4184(2) 0.6101(3) 0.0251(10) Uani 1 1 d . . .
H27A H 0.4909 0.4424 0.6612 0.030 Uiso 1 1 calc R . .
H27B H 0.4869 0.4610 0.5585 0.030 Uiso 1 1 calc R . .
C16 C 0.2772(2) 0.3211(2) 0.4642(3) 0.0237(9) Uani 1 1 d . . .
C21 C 0.6421(2) 0.3644(2) 0.5999(3) 0.0235(9) Uani 1 1 d . . .
C31 C 0.2131(2) 0.1233(2) 0.2964(3) 0.0278(10) Uani 1 1 d . . .
C14 C 0.1173(2) 0.3003(2) 0.4007(3) 0.0224(9) Uani 1 1 d . . .
C1 C 0.4430(2) 0.2888(2) 0.6489(3) 0.0257(10) Uani 1 1 d . . .
H1A H 0.3901 0.2532 0.6238 0.031 Uiso 1 1 calc R . .
H1B H 0.4414 0.3250 0.7000 0.031 Uiso 1 1 calc R . .
C22 C 0.7332(2) 0.3739(2) 0.6232(3) 0.0261(10) Uani 1 1 d . . .
C23 C 0.7826(2) 0.4244(3) 0.7043(3) 0.0292(10) Uani 1 1 d . . .
H23 H 0.8428 0.4317 0.7211 0.035 Uiso 1 1 calc R . .
C26 C 0.6037(2) 0.4091(2) 0.6521(3) 0.0213(9) Uani 1 1 d . A .
C24 C 0.7482(3) 0.4648(2) 0.7618(3) 0.0261(10) Uani 1 1 d . A .
C13 C 0.1271(2) 0.2280(2) 0.3525(3) 0.0252(10) Uani 1 1 d . . .
H13 H 0.0762 0.1971 0.3141 0.030 Uiso 1 1 calc R . .
C61 C 0.8082(3) 0.5185(3) 0.8510(3) 0.0317(11) Uani 1 1 d D . .
C32 C 0.2744(3) 0.0532(3) 0.3603(3) 0.0460(13) Uani 1 1 d . . .
H32A H 0.2760 0.0069 0.3197 0.069 Uiso 1 1 calc R . .
H32B H 0.2525 0.0328 0.4054 0.069 Uiso 1 1 calc R . .
H32C H 0.3333 0.0758 0.3962 0.069 Uiso 1 1 calc R . .
C41 C 0.0250(2) 0.3262(3) 0.3889(3) 0.0310(10) Uani 1 1 d . . .
C12 C 0.2077(2) 0.1990(2) 0.3579(3) 0.0230(9) Uani 1 1 d . . .
C25 C 0.6578(3) 0.4564(2) 0.7327(3) 0.0277(10) Uani 1 1 d . . .
H25 H 0.6325 0.4838 0.7689 0.033 Uiso 1 1 calc R A .
C17 C 0.3534(2) 0.3816(2) 0.5135(3) 0.0256(10) Uani 1 1 d . . .
H17A H 0.3407 0.4166 0.5587 0.031 Uiso 1 1 calc R . .
H17B H 0.3556 0.4194 0.4639 0.031 Uiso 1 1 calc R . .
C51 C 0.7724(2) 0.3354(3) 0.5575(3) 0.0312(10) Uani 1 1 d . . .
C52 C 0.7654(2) 0.2387(3) 0.5525(3) 0.0387(11) Uani 1 1 d . . .
H52A H 0.7905 0.2173 0.5108 0.058 Uiso 1 1 calc R . .
H52B H 0.7039 0.2223 0.5266 0.058 Uiso 1 1 calc R . .
H52C H 0.7972 0.2153 0.6171 0.058 Uiso 1 1 calc R . .
C53 C 0.7233(3) 0.3723(3) 0.4538(3) 0.0442(12) Uani 1 1 d . . .
H53A H 0.7276 0.4336 0.4566 0.066 Uiso 1 1 calc R . .
H53B H 0.6618 0.3558 0.4266 0.066 Uiso 1 1 calc R . .
H53C H 0.7497 0.3507 0.4133 0.066 Uiso 1 1 calc R . .
C34 C 0.1213(3) 0.0827(3) 0.2372(3) 0.0386(11) Uani 1 1 d . . .
H34A H 0.0810 0.1252 0.1959 0.058 Uiso 1 1 calc R . .
H34B H 0.0992 0.0603 0.2812 0.058 Uiso 1 1 calc R . .
H34C H 0.1266 0.0372 0.1976 0.058 Uiso 1 1 calc R . .
C44 C 0.0266(2) 0.4021(3) 0.4522(3) 0.0359(11) Uani 1 1 d . . .
H44A H -0.0330 0.4158 0.4413 0.054 Uiso 1 1 calc R . .
H44B H 0.0526 0.4504 0.4354 0.054 Uiso 1 1 calc R . .
H44C H 0.0613 0.3880 0.5199 0.054 Uiso 1 1 calc R . .
C54 C 0.8711(3) 0.3585(3) 0.5948(3) 0.0438(12) Uani 1 1 d . . .
H54A H 0.8778 0.4195 0.5991 0.066 Uiso 1 1 calc R . .
H54B H 0.8930 0.3367 0.5502 0.066 Uiso 1 1 calc R . .
H54C H 0.9043 0.3337 0.6583 0.066 Uiso 1 1 calc R . .
C33 C 0.2478(3) 0.1548(3) 0.2240(3) 0.0429(12) Uani 1 1 d . . .
H33A H 0.2097 0.1993 0.1841 0.064 Uiso 1 1 calc R . .
H33B H 0.2484 0.1081 0.1832 0.064 Uiso 1 1 calc R . .
H33C H 0.3071 0.1766 0.2594 0.064 Uiso 1 1 calc R . .
C42 C -0.0190(3) 0.2508(3) 0.4152(4) 0.0692(17) Uani 1 1 d . . .
H42A H -0.0206 0.2023 0.3758 0.104 Uiso 1 1 calc R . .
H42B H -0.0785 0.2661 0.4031 0.104 Uiso 1 1 calc R . .
H42C H 0.0146 0.2369 0.4831 0.104 Uiso 1 1 calc R . .
C4 C 0.6197(3) 0.1456(3) 0.6478(3) 0.0396(12) Uani 1 1 d . . .
H4A H 0.6591 0.1930 0.6578 0.059 Uiso 1 1 calc R . .
H4B H 0.6232 0.1076 0.5999 0.059 Uiso 1 1 calc R . .
H4C H 0.6366 0.1154 0.7085 0.059 Uiso 1 1 calc R . .
C43 C -0.0319(3) 0.3522(3) 0.2813(3) 0.0570(15) Uani 1 1 d . . .
H43A H -0.0347 0.3054 0.2391 0.086 Uiso 1 1 calc R . .
H43B H -0.0055 0.4009 0.2657 0.086 Uiso 1 1 calc R . .
H43C H -0.0909 0.3665 0.2722 0.086 Uiso 1 1 calc R . .
C3 C 0.4692(3) 0.1019(3) 0.5989(3) 0.0388(12) Uani 1 1 d . . .
H3A H 0.4086 0.1206 0.5757 0.058 Uiso 1 1 calc R . .
H3B H 0.4870 0.0725 0.6601 0.058 Uiso 1 1 calc R . .
H3C H 0.4741 0.0639 0.5518 0.058 Uiso 1 1 calc R . .
C62A C 0.7663(17) 0.5994(13) 0.864(2) 0.056(3) Uani 0.237(9) 1 d PD A 1
H62A H 0.8081 0.6298 0.9199 0.084 Uiso 0.237(9) 1 calc PR A 1
H62B H 0.7144 0.5858 0.8730 0.084 Uiso 0.237(9) 1 calc PR A 1
H62C H 0.7495 0.6345 0.8065 0.084 Uiso 0.237(9) 1 calc PR A 1
C63A C 0.8991(13) 0.5371(19) 0.8500(19) 0.069(3) Uani 0.237(9) 1 d PD A 1
H63A H 0.9355 0.5701 0.9068 0.103 Uiso 0.237(9) 1 calc PR A 1
H63B H 0.8896 0.5686 0.7920 0.103 Uiso 0.237(9) 1 calc PR A 1
H63C H 0.9284 0.4841 0.8507 0.103 Uiso 0.237(9) 1 calc PR A 1
C64A C 0.832(2) 0.458(2) 0.9383(19) 0.086(4) Uani 0.237(9) 1 d PD A 1
H64A H 0.8706 0.4876 0.9974 0.129 Uiso 0.237(9) 1 calc PR A 1
H64B H 0.8628 0.4091 0.9298 0.129 Uiso 0.237(9) 1 calc PR A 1
H64C H 0.7793 0.4404 0.9425 0.129 Uiso 0.237(9) 1 calc PR A 1
C62B C 0.7557(5) 0.5650(6) 0.8980(5) 0.056(3) Uani 0.763(9) 1 d PD A 2
H62D H 0.7106 0.6001 0.8498 0.084 Uiso 0.763(9) 1 calc PR A 2
H62E H 0.7953 0.6003 0.9507 0.084 Uiso 0.763(9) 1 calc PR A 2
H62F H 0.7281 0.5238 0.9229 0.084 Uiso 0.763(9) 1 calc PR A 2
C63B C 0.8519(6) 0.5896(5) 0.8165(5) 0.069(3) Uani 0.763(9) 1 d PD A 2
H63D H 0.8066 0.6262 0.7710 0.103 Uiso 0.763(9) 1 calc PR A 2
H63E H 0.8852 0.5643 0.7852 0.103 Uiso 0.763(9) 1 calc PR A 2
H63F H 0.8911 0.6225 0.8719 0.103 Uiso 0.763(9) 1 calc PR A 2
C64B C 0.8762(6) 0.4616(6) 0.9284(6) 0.086(4) Uani 0.763(9) 1 d PD A 2
H64D H 0.9133 0.4957 0.9838 0.129 Uiso 0.763(9) 1 calc PR A 2
H64E H 0.9123 0.4341 0.9018 0.129 Uiso 0.763(9) 1 calc PR A 2
H64F H 0.8461 0.4191 0.9484 0.129 Uiso 0.763(9) 1 calc PR A 2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O2 1.829(2) . ?
Ti1 O1 1.839(2) . ?
Ti1 N1 2.272(3) . ?
Ti1 Cl1 2.3033(12) . ?
Ti1 Cl2 2.3068(12) . ?
Ti1 N2 2.307(3) . ?
O1 C11 1.350(4) . ?
N1 C1 1.487(4) . ?
N1 C27 1.502(4) . ?
N1 C17 1.502(4) . ?
O2 C21 1.349(4) . ?
N2 C4 1.475(4) . ?
N2 C3 1.484(5) . ?
N2 C2 1.491(4) . ?
C11 C16 1.393(5) . ?
C11 C12 1.411(5) . ?
C15 C14 1.381(5) . ?
C15 C16 1.397(5) . ?
C15 H15 0.9300 . ?
C2 C1 1.495(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C27 C26 1.505(4) . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C16 C17 1.498(5) . ?
C21 C26 1.403(5) . ?
C21 C22 1.412(5) . ?
C31 C32 1.525(5) . ?
C31 C33 1.529(5) . ?
C31 C12 1.534(5) . ?
C31 C34 1.536(5) . ?
C14 C13 1.395(5) . ?
C14 C41 1.527(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C22 C23 1.390(5) . ?
C22 C51 1.535(5) . ?
C23 C24 1.389(5) . ?
C23 H23 0.9300 . ?
C26 C25 1.377(5) . ?
C24 C25 1.383(5) . ?
C24 C61 1.535(5) . ?
C13 C12 1.389(5) . ?
C13 H13 0.9300 . ?
C61 C62A 1.499(14) . ?
C61 C64B 1.516(7) . ?
C61 C64A 1.529(15) . ?
C61 C62B 1.534(7) . ?
C61 C63B 1.541(7) . ?
C61 C63A 1.552(14) . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C41 C44 1.520(5) . ?
C41 C42 1.530(6) . ?
C41 C43 1.543(5) . ?
C25 H25 0.9300 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C51 C52 1.516(5) . ?
C51 C54 1.534(5) . ?
C51 C53 1.536(5) . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
C53 H53A 0.9600 . ?
C53 H53B 0.9600 . ?
C53 H53C 0.9600 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C54 H54A 0.9600 . ?
C54 H54B 0.9600 . ?
C54 H54C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C62A H62A 0.9600 . ?
C62A H62B 0.9600 . ?
C62A H62C 0.9600 . ?
C63A H63A 0.9600 . ?
C63A H63B 0.9600 . ?
C63A H63C 0.9600 . ?
C64A H64A 0.9600 . ?
C64A H64B 0.9600 . ?
C64A H64C 0.9600 . ?
C62B H62D 0.9600 . ?
C62B H62E 0.9600 . ?
C62B H62F 0.9600 . ?
C63B H63D 0.9600 . ?
C63B H63E 0.9600 . ?
C63B H63F 0.9600 . ?
C64B H64D 0.9600 . ?
C64B H64E 0.9600 . ?
C64B H64F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O1 166.58(11) . . ?
O2 Ti1 N1 85.25(11) . . ?
O1 Ti1 N1 81.35(10) . . ?
O2 Ti1 Cl1 97.54(8) . . ?
O1 Ti1 Cl1 95.64(8) . . ?
N1 Ti1 Cl1 165.28(9) . . ?
O2 Ti1 Cl2 90.08(9) . . ?
O1 Ti1 Cl2 89.80(8) . . ?
N1 Ti1 Cl2 93.06(8) . . ?
Cl1 Ti1 Cl2 101.36(4) . . ?
O2 Ti1 N2 86.73(11) . . ?
O1 Ti1 N2 91.27(11) . . ?
N1 Ti1 N2 77.94(11) . . ?
Cl1 Ti1 N2 87.76(8) . . ?
Cl2 Ti1 N2 170.66(9) . . ?
C11 O1 Ti1 144.0(2) . . ?
C1 N1 C27 110.5(3) . . ?
C1 N1 C17 108.6(3) . . ?
C27 N1 C17 104.1(3) . . ?
C1 N1 Ti1 107.5(2) . . ?
C27 N1 Ti1 114.3(2) . . ?
C17 N1 Ti1 111.8(2) . . ?
C21 O2 Ti1 145.9(2) . . ?
C4 N2 C3 107.7(3) . . ?
C4 N2 C2 108.0(3) . . ?
C3 N2 C2 109.4(3) . . ?
C4 N2 Ti1 112.9(2) . . ?
C3 N2 Ti1 111.3(2) . . ?
C2 N2 Ti1 107.5(2) . . ?
O1 C11 C16 117.9(3) . . ?
O1 C11 C12 121.0(3) . . ?
C16 C11 C12 121.1(3) . . ?
C14 C15 C16 122.3(4) . . ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
N2 C2 C1 110.5(3) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
N1 C27 C26 121.0(3) . . ?
N1 C27 H27A 107.1 . . ?
C26 C27 H27A 107.1 . . ?
N1 C27 H27B 107.1 . . ?
C26 C27 H27B 107.1 . . ?
H27A C27 H27B 106.8 . . ?
C11 C16 C15 119.0(3) . . ?
C11 C16 C17 122.9(3) . . ?
C15 C16 C17 117.8(3) . . ?
O2 C21 C26 117.7(3) . . ?
O2 C21 C22 121.3(3) . . ?
C26 C21 C22 120.9(3) . . ?
C32 C31 C33 109.2(3) . . ?
C32 C31 C12 111.6(3) . . ?
C33 C31 C12 109.3(3) . . ?
C32 C31 C34 107.3(3) . . ?
C33 C31 C34 107.9(3) . . ?
C12 C31 C34 111.6(3) . . ?
C15 C14 C13 116.6(3) . . ?
C15 C14 C41 123.7(3) . . ?
C13 C14 C41 119.7(3) . . ?
N1 C1 C2 110.1(3) . . ?
N1 C1 H1A 109.6 . . ?
C2 C1 H1A 109.6 . . ?
N1 C1 H1B 109.6 . . ?
C2 C1 H1B 109.6 . . ?
H1A C1 H1B 108.2 . . ?
C23 C22 C21 116.2(4) . . ?
C23 C22 C51 122.7(3) . . ?
C21 C22 C51 120.9(3) . . ?
C24 C23 C22 124.5(4) . . ?
C24 C23 H23 117.8 . . ?
C22 C23 H23 117.8 . . ?
C25 C26 C21 119.0(3) . . ?
C25 C26 C27 120.0(3) . . ?
C21 C26 C27 120.1(3) . . ?
C25 C24 C23 116.7(3) . . ?
C25 C24 C61 122.5(4) . . ?
C23 C24 C61 120.9(4) . . ?
C12 C13 C14 124.5(3) . . ?
C12 C13 H13 117.8 . . ?
C14 C13 H13 117.8 . . ?
C62A C61 C64B 129.0(11) . . ?
C62A C61 C64A 111.8(17) . . ?
C64B C61 C62B 107.8(5) . . ?
C64A C61 C62B 83.0(14) . . ?
C62A C61 C24 114.4(11) . . ?
C64B C61 C24 110.0(5) . . ?
C64A C61 C24 104.6(14) . . ?
C62B C61 C24 112.5(4) . . ?
C62A C61 C63B 75.6(11) . . ?
C64B C61 C63B 112.3(5) . . ?
C64A C61 C63B 138.8(12) . . ?
C62B C61 C63B 105.5(5) . . ?
C24 C61 C63B 108.6(4) . . ?
C62A C61 C63A 110.9(14) . . ?
C64B C61 C63A 73.2(11) . . ?
C64A C61 C63A 103.4(14) . . ?
C62B C61 C63A 132.5(9) . . ?
C24 C61 C63A 111.1(9) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C44 C41 C14 113.1(3) . . ?
C44 C41 C42 108.4(4) . . ?
C14 C41 C42 109.8(3) . . ?
C44 C41 C43 107.2(3) . . ?
C14 C41 C43 108.6(3) . . ?
C42 C41 C43 109.6(4) . . ?
C13 C12 C11 116.5(3) . . ?
C13 C12 C31 121.9(3) . . ?
C11 C12 C31 121.5(3) . . ?
C26 C25 C24 122.5(4) . . ?
C26 C25 H25 118.7 . . ?
C24 C25 H25 118.7 . . ?
C16 C17 N1 117.0(3) . . ?
C16 C17 H17A 108.1 . . ?
N1 C17 H17A 108.1 . . ?
C16 C17 H17B 108.1 . . ?
N1 C17 H17B 108.1 . . ?
H17A C17 H17B 107.3 . . ?
C52 C51 C54 107.5(3) . . ?
C52 C51 C22 112.2(3) . . ?
C54 C51 C22 111.2(3) . . ?
C52 C51 C53 109.2(3) . . ?
C54 C51 C53 107.4(3) . . ?
C22 C51 C53 109.2(3) . . ?
C51 C52 H52A 109.5 . . ?
C51 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C51 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
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 . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C51 C54 H54A 109.5 . . ?
C51 C54 H54B 109.5 . . ?
H54A C54 H54B 109.5 . . ?
C51 C54 H54C 109.5 . . ?
H54A C54 H54C 109.5 . . ?
H54B C54 H54C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C61 C62A H62A 109.5 . . ?
C61 C62A H62B 109.5 . . ?
H62A C62A H62B 109.5 . . ?
C61 C62A H62C 109.5 . . ?
H62A C62A H62C 109.5 . . ?
H62B C62A H62C 109.5 . . ?
C61 C63A H63A 109.5 . . ?
C61 C63A H63B 109.5 . . ?
H63A C63A H63B 109.5 . . ?
C61 C63A H63C 109.5 . . ?
H63A C63A H63C 109.5 . . ?
H63B C63A H63C 109.5 . . ?
C61 C64A H64A 109.5 . . ?
C61 C64A H64B 109.5 . . ?
H64A C64A H64B 109.5 . . ?
C61 C64A H64C 109.5 . . ?
H64A C64A H64C 109.5 . . ?
H64B C64A H64C 109.5 . . ?
C61 C62B H62D 109.5 . . ?
C61 C62B H62E 109.5 . . ?
H62D C62B H62E 109.5 . . ?
C61 C62B H62F 109.5 . . ?
H62D C62B H62F 109.5 . . ?
H62E C62B H62F 109.5 . . ?
C61 C63B H63D 109.5 . . ?
C61 C63B H63E 109.5 . . ?
H63D C63B H63E 109.5 . . ?
C61 C63B H63F 109.5 . . ?
H63D C63B H63F 109.5 . . ?
H63E C63B H63F 109.5 . . ?
C61 C64B H64D 109.5 . . ?
C61 C64B H64E 109.5 . . ?
H64D C64B H64E 109.5 . . ?
C61 C64B H64F 109.5 . . ?
H64D C64B H64F 109.5 . . ?
H64E C64B H64F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ti1 O1 C11 27.0(7) . . . . ?
N1 Ti1 O1 C11 30.6(4) . . . . ?
Cl1 Ti1 O1 C11 -163.9(4) . . . . ?
Cl2 Ti1 O1 C11 -62.5(4) . . . . ?
N2 Ti1 O1 C11 108.2(4) . . . . ?
O2 Ti1 N1 C1 -105.5(2) . . . . ?
O1 Ti1 N1 C1 75.3(2) . . . . ?
Cl1 Ti1 N1 C1 -3.8(5) . . . . ?
Cl2 Ti1 N1 C1 164.7(2) . . . . ?
N2 Ti1 N1 C1 -17.8(2) . . . . ?
O2 Ti1 N1 C27 17.5(2) . . . . ?
O1 Ti1 N1 C27 -161.7(2) . . . . ?
Cl1 Ti1 N1 C27 119.2(3) . . . . ?
Cl2 Ti1 N1 C27 -72.3(2) . . . . ?
N2 Ti1 N1 C27 105.2(2) . . . . ?
O2 Ti1 N1 C17 135.4(2) . . . . ?
O1 Ti1 N1 C17 -43.8(2) . . . . ?
Cl1 Ti1 N1 C17 -122.9(3) . . . . ?
Cl2 Ti1 N1 C17 45.6(2) . . . . ?
N2 Ti1 N1 C17 -136.9(2) . . . . ?
O1 Ti1 O2 C21 11.9(8) . . . . ?
N1 Ti1 O2 C21 8.3(4) . . . . ?
Cl1 Ti1 O2 C21 -157.1(4) . . . . ?
Cl2 Ti1 O2 C21 101.4(4) . . . . ?
N2 Ti1 O2 C21 -69.8(4) . . . . ?
O2 Ti1 N2 C4 -44.6(3) . . . . ?
O1 Ti1 N2 C4 148.7(3) . . . . ?
N1 Ti1 N2 C4 -130.4(3) . . . . ?
Cl1 Ti1 N2 C4 53.1(3) . . . . ?
O2 Ti1 N2 C3 -165.8(3) . . . . ?
O1 Ti1 N2 C3 27.5(3) . . . . ?
N1 Ti1 N2 C3 108.3(3) . . . . ?
Cl1 Ti1 N2 C3 -68.1(2) . . . . ?
O2 Ti1 N2 C2 74.4(2) . . . . ?
O1 Ti1 N2 C2 -92.3(2) . . . . ?
N1 Ti1 N2 C2 -11.5(2) . . . . ?
Cl1 Ti1 N2 C2 172.1(2) . . . . ?
Ti1 O1 C11 C16 -16.8(6) . . . . ?
Ti1 O1 C11 C12 162.1(3) . . . . ?
C4 N2 C2 C1 162.0(3) . . . . ?
C3 N2 C2 C1 -81.1(4) . . . . ?
Ti1 N2 C2 C1 39.9(3) . . . . ?
C1 N1 C27 C26 77.2(4) . . . . ?
C17 N1 C27 C26 -166.4(3) . . . . ?
Ti1 N1 C27 C26 -44.2(4) . . . . ?
O1 C11 C16 C15 -177.2(3) . . . . ?
C12 C11 C16 C15 3.9(5) . . . . ?
O1 C11 C16 C17 10.3(5) . . . . ?
C12 C11 C16 C17 -168.7(3) . . . . ?
C14 C15 C16 C11 -1.1(6) . . . . ?
C14 C15 C16 C17 171.8(3) . . . . ?
Ti1 O2 C21 C26 -8.9(6) . . . . ?
Ti1 O2 C21 C22 169.1(3) . . . . ?
C16 C15 C14 C13 -1.5(6) . . . . ?
C16 C15 C14 C41 -179.6(3) . . . . ?
C27 N1 C1 C2 -79.6(4) . . . . ?
C17 N1 C1 C2 166.8(3) . . . . ?
Ti1 N1 C1 C2 45.7(3) . . . . ?
N2 C2 C1 N1 -59.4(4) . . . . ?
O2 C21 C22 C23 -173.4(3) . . . . ?
C26 C21 C22 C23 4.5(6) . . . . ?
O2 C21 C22 C51 10.8(6) . . . . ?
C26 C21 C22 C51 -171.3(4) . . . . ?
C21 C22 C23 C24 0.0(6) . . . . ?
C51 C22 C23 C24 175.7(4) . . . . ?
O2 C21 C26 C25 172.0(3) . . . . ?
C22 C21 C26 C25 -6.1(6) . . . . ?
O2 C21 C26 C27 -19.3(5) . . . . ?
C22 C21 C26 C27 162.7(3) . . . . ?
N1 C27 C26 C25 -143.6(4) . . . . ?
N1 C27 C26 C21 47.7(5) . . . . ?
C22 C23 C24 C25 -3.0(6) . . . . ?
C22 C23 C24 C61 179.2(4) . . . . ?
C15 C14 C13 C12 1.6(6) . . . . ?
C41 C14 C13 C12 179.8(4) . . . . ?
C25 C24 C61 C62A -37.9(14) . . . . ?
C23 C24 C61 C62A 139.9(13) . . . . ?
C25 C24 C61 C64B 116.5(6) . . . . ?
C23 C24 C61 C64B -65.8(7) . . . . ?
C25 C24 C61 C64A 84.7(14) . . . . ?
C23 C24 C61 C64A -97.6(14) . . . . ?
C25 C24 C61 C62B -3.7(6) . . . . ?
C23 C24 C61 C62B 174.0(5) . . . . ?
C25 C24 C61 C63B -120.1(5) . . . . ?
C23 C24 C61 C63B 57.6(6) . . . . ?
C25 C24 C61 C63A -164.4(13) . . . . ?
C23 C24 C61 C63A 13.4(14) . . . . ?
C15 C14 C41 C44 -6.4(6) . . . . ?
C13 C14 C41 C44 175.5(4) . . . . ?
C15 C14 C41 C42 -127.7(4) . . . . ?
C13 C14 C41 C42 54.3(5) . . . . ?
C15 C14 C41 C43 112.5(4) . . . . ?
C13 C14 C41 C43 -65.5(5) . . . . ?
C14 C13 C12 C11 1.0(6) . . . . ?
C14 C13 C12 C31 -174.8(4) . . . . ?
O1 C11 C12 C13 177.3(3) . . . . ?
C16 C11 C12 C13 -3.8(5) . . . . ?
O1 C11 C12 C31 -6.8(6) . . . . ?
C16 C11 C12 C31 172.1(3) . . . . ?
C32 C31 C12 C13 -124.1(4) . . . . ?
C33 C31 C12 C13 115.0(4) . . . . ?
C34 C31 C12 C13 -4.1(5) . . . . ?
C32 C31 C12 C11 60.3(5) . . . . ?
C33 C31 C12 C11 -60.6(5) . . . . ?
C34 C31 C12 C11 -179.8(3) . . . . ?
C21 C26 C25 C24 3.0(6) . . . . ?
C27 C26 C25 C24 -165.8(3) . . . . ?
C23 C24 C25 C26 1.4(6) . . . . ?
C61 C24 C25 C26 179.3(4) . . . . ?
C11 C16 C17 N1 -38.3(5) . . . . ?
C15 C16 C17 N1 149.1(3) . . . . ?
C1 N1 C17 C16 -61.4(4) . . . . ?
C27 N1 C17 C16 -179.1(3) . . . . ?
Ti1 N1 C17 C16 57.1(4) . . . . ?
C23 C22 C51 C52 121.7(4) . . . . ?
C21 C22 C51 C52 -62.7(5) . . . . ?
C23 C22 C51 C54 1.3(5) . . . . ?
C21 C22 C51 C54 176.8(4) . . . . ?
C23 C22 C51 C53 -117.0(4) . . . . ?
C21 C22 C51 C53 58.5(5) . . . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        25.03
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.073

_database_code_depnum_ccdc_archive 'CCDC 994886'
#######################################################################
#
#                 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_5

_audit_creation_method           SHELXL-97
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         'C68 H110 N4 O7 Ti2, 4(C4 H8 O)'
_chemical_formula_sum            'C84 H142 N4 O11 Ti2'
_chemical_melting_point          ?

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow

_diffrn_ambient_temperature      150(2)
_chemical_formula_weight         1479.82

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/c'
_symmetry_int_tables_number      14
_chemical_absolute_configuration ?

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

_cell_length_a                   13.080(2)
_cell_length_b                   13.894(3)
_cell_length_c                   23.193(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 95.620(9)
_cell_angle_gamma                90.00
_cell_volume                     4194.7(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1353
_cell_measurement_theta_min      2.68
_cell_measurement_theta_max      18.47
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.04
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.172
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1612
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9292
_exptl_absorpt_correction_T_max  0.9901
_exptl_absorpt_process_details   'SADABS,  G. M. Sheldrick, 1996'

_exptl_special_details           
;
 ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_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_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            31375
_diffrn_reflns_av_R_equivalents  0.1430
_diffrn_reflns_av_sigmaI/netI    0.1760
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         25.14
_reflns_number_total             7447
_reflns_number_gt                3737
_reflns_threshold_expression     >2σ(I)

_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          
;
 Refinement of F² against ALL reflections.  The weighted R-factor wR and
 goodness of fit S are based on F², conventional R-factors R are based
 on F, with F set to zero for negative F². The threshold expression of
 F² > 2σ(F²) is used only for calculating R-factors(gt) etc. and is
 not relevant to the choice of reflections for refinement.  R-factors based
 on F² are statistically about twice as large as those based on F, and R-
 factors based on ALL data will be even larger.
One of the tBu fragments presents disordered methyl groups. The methyl groups attached to C51 were modelled and gave 77/23% occupancies.
EADP constraints were apllied on disordered atoms.   
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0609P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7447
_refine_ls_number_parameters     468
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1721
_refine_ls_R_factor_gt           0.0693
_refine_ls_wR_factor_ref         0.1525
_refine_ls_wR_factor_gt          0.1282
_refine_ls_goodness_of_fit_ref   0.926
_refine_ls_restrained_S_all      0.926
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.04761(5) 0.42653(5) 0.44391(3) 0.0174(2) Uani 1 1 d . . .
O3 O 0.0000 0.5000 0.5000 0.0210(9) Uani 1 2 d S . .
O2 O 0.15459(17) 0.37237(19) 0.49439(11) 0.0227(7) Uani 1 1 d . A .
O1 O -0.06690(17) 0.44536(19) 0.38777(10) 0.0185(6) Uani 1 1 d . . .
N1 N -0.0452(2) 0.2981(2) 0.47195(12) 0.0163(8) Uani 1 1 d . A .
O4 O 0.13273(18) 0.5054(2) 0.40816(11) 0.0256(7) Uani 1 1 d . . .
H4 H 0.1087 0.5148 0.3746 0.038 Uiso 1 1 calc R . .
N2 N 0.0925(2) 0.2930(2) 0.38365(13) 0.0234(8) Uani 1 1 d . . .
C26 C 0.0943(3) 0.2493(3) 0.55202(16) 0.0164(9) Uani 1 1 d . A .
C61 C 0.2315(3) 0.0669(3) 0.65558(16) 0.0255(10) Uani 1 1 d . . .
C23 C 0.2913(3) 0.2075(3) 0.59576(16) 0.0220(10) Uani 1 1 d . . .
H23 H 0.3581 0.1934 0.6109 0.026 Uiso 1 1 calc R . .
C16 C -0.2058(3) 0.3473(3) 0.40819(16) 0.0187(9) Uani 1 1 d . . .
C31 C -0.1790(3) 0.5235(3) 0.28210(16) 0.0215(10) Uani 1 1 d . . .
C11 C -0.1617(3) 0.4125(3) 0.37260(16) 0.0181(9) Uani 1 1 d . . .
C1 C -0.0337(3) 0.2101(3) 0.43717(16) 0.0204(10) Uani 1 1 d . . .
H1A H -0.0859 0.2097 0.4044 0.024 Uiso 1 1 calc R . .
H1B H -0.0443 0.1539 0.4607 0.024 Uiso 1 1 calc R . .
C51 C 0.3706(3) 0.3489(3) 0.54880(16) 0.0234(10) Uani 1 1 d . . .
C22 C 0.2769(3) 0.2865(3) 0.55857(16) 0.0199(10) Uani 1 1 d . A .
C21 C 0.1762(3) 0.3046(3) 0.53469(16) 0.0198(10) Uani 1 1 d . . .
C15 C -0.3017(3) 0.3071(3) 0.39087(16) 0.0203(10) Uani 1 1 d . . .
H15 H -0.3287 0.2621 0.4148 0.024 Uiso 1 1 calc R . .
C41 C -0.4652(3) 0.2925(3) 0.32074(17) 0.0249(10) Uani 1 1 d . . .
C2 C 0.0713(3) 0.2045(3) 0.41542(17) 0.0242(10) Uani 1 1 d . . .
H2A H 0.1231 0.1962 0.4479 0.029 Uiso 1 1 calc R . .
H2B H 0.0743 0.1493 0.3900 0.029 Uiso 1 1 calc R . .
C13 C -0.3142(3) 0.4006(3) 0.30586(16) 0.0224(10) Uani 1 1 d . . .
H13 H -0.3517 0.4195 0.2716 0.027 Uiso 1 1 calc R . .
C12 C -0.2186(3) 0.4434(3) 0.31969(16) 0.0212(10) Uani 1 1 d . . .
C32 C -0.0804(3) 0.4940(3) 0.25703(17) 0.0296(11) Uani 1 1 d . . .
H32A H -0.0926 0.4369 0.2341 0.044 Uiso 1 1 calc R . .
H32B H -0.0279 0.4815 0.2880 0.044 Uiso 1 1 calc R . .
H32C H -0.0585 0.5450 0.2332 0.044 Uiso 1 1 calc R . .
C14 C -0.3579(3) 0.3317(3) 0.33940(16) 0.0207(10) Uani 1 1 d . . .
C17 C -0.1558(2) 0.3267(3) 0.46819(15) 0.0179(9) Uani 1 1 d . . .
H17A H -0.1617 0.3836 0.4918 0.021 Uiso 1 1 calc R . .
H17B H -0.1939 0.2756 0.4849 0.021 Uiso 1 1 calc R . .
C3 C 0.0372(3) 0.2911(3) 0.32570(17) 0.0347(11) Uani 1 1 d . . .
H3A H 0.0503 0.3496 0.3057 0.052 Uiso 1 1 calc R . .
H3B H -0.0351 0.2852 0.3289 0.052 Uiso 1 1 calc R . .
H3C H 0.0603 0.2372 0.3045 0.052 Uiso 1 1 calc R . .
C42 C -0.4721(3) 0.2564(3) 0.25845(18) 0.0384(13) Uani 1 1 d . . .
H42A H -0.4540 0.3075 0.2335 0.058 Uiso 1 1 calc R . .
H42B H -0.5410 0.2355 0.2468 0.058 Uiso 1 1 calc R . .
H42C H -0.4256 0.2035 0.2558 0.058 Uiso 1 1 calc R . .
C33 C -0.1571(3) 0.6153(3) 0.31819(18) 0.0358(12) Uani 1 1 d . . .
H33A H -0.1330 0.6649 0.2941 0.054 Uiso 1 1 calc R . .
H33B H -0.1055 0.6020 0.3496 0.054 Uiso 1 1 calc R . .
H33C H -0.2190 0.6362 0.3335 0.054 Uiso 1 1 calc R . .
C25 C 0.1140(3) 0.1730(3) 0.58928(16) 0.0207(10) Uani 1 1 d . . .
H25 H 0.0592 0.1364 0.5998 0.025 Uiso 1 1 calc R A .
O6 O 0.7637(3) 0.0990(3) 0.51722(18) 0.0699(12) Uani 1 1 d . . .
C44 C -0.4944(3) 0.2097(3) 0.35862(18) 0.0335(12) Uani 1 1 d . . .
H44A H -0.5624 0.1878 0.3455 0.050 Uiso 1 1 calc R . .
H44B H -0.4929 0.2312 0.3981 0.050 Uiso 1 1 calc R . .
H44C H -0.4465 0.1579 0.3563 0.050 Uiso 1 1 calc R . .
C4 C 0.2032(3) 0.2974(3) 0.3769(2) 0.0396(12) Uani 1 1 d . . .
H4A H 0.2180 0.3553 0.3567 0.059 Uiso 1 1 calc R . .
H4B H 0.2224 0.2426 0.3552 0.059 Uiso 1 1 calc R . .
H4C H 0.2415 0.2972 0.4144 0.059 Uiso 1 1 calc R . .
C24 C 0.2134(3) 0.1488(3) 0.61165(16) 0.0230(10) Uani 1 1 d . A .
O5 O 0.1777(3) 0.6035(3) 0.31071(15) 0.0717(12) Uani 1 1 d . . .
C34 C -0.2577(3) 0.5495(3) 0.23118(18) 0.0400(13) Uani 1 1 d . . .
H34A H -0.2729 0.4934 0.2077 0.060 Uiso 1 1 calc R . .
H34B H -0.2299 0.5988 0.2083 0.060 Uiso 1 1 calc R . .
H34C H -0.3194 0.5724 0.2457 0.060 Uiso 1 1 calc R . .
C27 C -0.0145(3) 0.2799(3) 0.53481(16) 0.0215(10) Uani 1 1 d . . .
H27A H -0.0596 0.2306 0.5477 0.026 Uiso 1 1 calc R A .
H27B H -0.0272 0.3383 0.5559 0.026 Uiso 1 1 calc R . .
C64 C 0.3447(3) 0.0414(3) 0.6682(2) 0.0453(13) Uani 1 1 d . . .
H64A H 0.3718 0.0222 0.6330 0.068 Uiso 1 1 calc R . .
H64B H 0.3520 -0.0105 0.6956 0.068 Uiso 1 1 calc R . .
H64C H 0.3817 0.0966 0.6841 0.068 Uiso 1 1 calc R . .
C43 C -0.5436(3) 0.3746(3) 0.32497(19) 0.0368(12) Uani 1 1 d . . .
H43A H -0.5264 0.4274 0.3010 0.055 Uiso 1 1 calc R . .
H43B H -0.5419 0.3957 0.3645 0.055 Uiso 1 1 calc R . .
H43C H -0.6112 0.3518 0.3120 0.055 Uiso 1 1 calc R . .
C63 C 0.1752(4) -0.0248(3) 0.6338(2) 0.0512(14) Uani 1 1 d . . .
H63A H 0.1997 -0.0446 0.5980 0.077 Uiso 1 1 calc R . .
H63B H 0.1028 -0.0123 0.6278 0.077 Uiso 1 1 calc R . .
H63C H 0.1879 -0.0750 0.6621 0.077 Uiso 1 1 calc R . .
C62 C 0.1913(4) 0.0984(3) 0.71231(18) 0.0458(13) Uani 1 1 d . . .
H62A H 0.2027 0.0480 0.7405 0.069 Uiso 1 1 calc R . .
H62B H 0.1190 0.1116 0.7057 0.069 Uiso 1 1 calc R . .
H62C H 0.2268 0.1555 0.7264 0.069 Uiso 1 1 calc R . .
C71 C 0.2812(4) 0.6112(4) 0.3343(3) 0.0727(19) Uani 1 1 d . . .
H71A H 0.3271 0.6131 0.3040 0.087 Uiso 1 1 calc R . .
H71B H 0.3003 0.5576 0.3599 0.087 Uiso 1 1 calc R . .
C72 C 0.2845(4) 0.7041(5) 0.3672(3) 0.0717(18) Uani 1 1 d . . .
H72A H 0.2673 0.6938 0.4065 0.086 Uiso 1 1 calc R . .
H72B H 0.3522 0.7330 0.3686 0.086 Uiso 1 1 calc R . .
C73 C 0.2070(5) 0.7659(4) 0.3347(3) 0.0780(19) Uani 1 1 d . . .
H73A H 0.1703 0.8044 0.3609 0.094 Uiso 1 1 calc R . .
H73B H 0.2389 0.8085 0.3086 0.094 Uiso 1 1 calc R . .
C83 C 0.7002(5) -0.0432(4) 0.5532(3) 0.0777(19) Uani 1 1 d . . .
H83A H 0.7115 -0.0788 0.5892 0.093 Uiso 1 1 calc R . .
H83B H 0.6777 -0.0875 0.5222 0.093 Uiso 1 1 calc R . .
C81 C 0.6562(4) 0.1066(4) 0.5138(3) 0.0694(18) Uani 1 1 d . . .
H81A H 0.6257 0.0906 0.4752 0.083 Uiso 1 1 calc R . .
H81B H 0.6358 0.1715 0.5231 0.083 Uiso 1 1 calc R . .
C82 C 0.6231(4) 0.0358(4) 0.5577(2) 0.0665(18) Uani 1 1 d . . .
H82A H 0.6281 0.0633 0.5963 0.080 Uiso 1 1 calc R . .
H82B H 0.5535 0.0133 0.5474 0.080 Uiso 1 1 calc R . .
C74 C 0.1375(6) 0.6969(6) 0.3023(4) 0.125(3) Uani 1 1 d . . .
H74A H 0.0698 0.7002 0.3159 0.150 Uiso 1 1 calc R . .
H74B H 0.1312 0.7127 0.2614 0.150 Uiso 1 1 calc R . .
C84 C 0.7945(5) 0.0085(4) 0.5405(3) 0.0763(19) Uani 1 1 d . . .
H84A H 0.8403 0.0166 0.5757 0.092 Uiso 1 1 calc R . .
H84B H 0.8304 -0.0276 0.5129 0.092 Uiso 1 1 calc R . .
C52A C 0.3468(4) 0.4451(5) 0.5171(4) 0.049(2) Uani 0.766(6) 1 d P A 1
H52A H 0.4097 0.4789 0.5132 0.073 Uiso 0.766(6) 1 calc PR A 1
H52B H 0.3036 0.4837 0.5391 0.073 Uiso 0.766(6) 1 calc PR A 1
H52C H 0.3121 0.4327 0.4794 0.073 Uiso 0.766(6) 1 calc PR A 1
C53A C 0.4433(4) 0.2914(5) 0.5145(3) 0.0429(19) Uani 0.766(6) 1 d P A 1
H53A H 0.5019 0.3302 0.5082 0.064 Uiso 0.766(6) 1 calc PR A 1
H53B H 0.4082 0.2731 0.4779 0.064 Uiso 0.766(6) 1 calc PR A 1
H53C H 0.4655 0.2347 0.5359 0.064 Uiso 0.766(6) 1 calc PR A 1
C54A C 0.4278(4) 0.3767(5) 0.6077(3) 0.0413(18) Uani 0.766(6) 1 d P A 1
H54A H 0.4862 0.4158 0.6015 0.062 Uiso 0.766(6) 1 calc PR A 1
H54B H 0.4504 0.3195 0.6284 0.062 Uiso 0.766(6) 1 calc PR A 1
H54C H 0.3824 0.4122 0.6299 0.062 Uiso 0.766(6) 1 calc PR A 1
C52B C 0.3425(16) 0.4519(17) 0.5590(12) 0.049(2) Uani 0.234(6) 1 d P A 2
H52D H 0.3997 0.4927 0.5530 0.073 Uiso 0.234(6) 1 calc PR A 2
H52E H 0.3251 0.4592 0.5980 0.073 Uiso 0.234(6) 1 calc PR A 2
H52F H 0.2846 0.4696 0.5324 0.073 Uiso 0.234(6) 1 calc PR A 2
C53B C 0.3972(15) 0.3377(17) 0.4854(9) 0.0429(19) Uani 0.234(6) 1 d P A 2
H53D H 0.4556 0.3770 0.4794 0.064 Uiso 0.234(6) 1 calc PR A 2
H53E H 0.3395 0.3576 0.4593 0.064 Uiso 0.234(6) 1 calc PR A 2
H53F H 0.4129 0.2715 0.4781 0.064 Uiso 0.234(6) 1 calc PR A 2
C54B C 0.4673(15) 0.3223(17) 0.5868(9) 0.0413(18) Uani 0.234(6) 1 d P A 2
H54D H 0.5225 0.3637 0.5781 0.062 Uiso 0.234(6) 1 calc PR A 2
H54E H 0.4851 0.2567 0.5797 0.062 Uiso 0.234(6) 1 calc PR A 2
H54F H 0.4556 0.3298 0.6268 0.062 Uiso 0.234(6) 1 calc PR A 2


_geom_special_details            
;
 All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell s.u.'s are taken
 into account individually in the estimation of s.u.'s in distances, angles
 and torsion angles; correlations between s.u.'s in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell s.u.'s is used for estimating s.u.'s 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 1.8112(7) . ?
Ti1 O4 1.819(3) . ?
Ti1 O2 1.890(2) . ?
Ti1 O1 1.904(2) . ?
Ti1 N1 2.288(3) . ?
Ti1 N2 2.429(3) . ?
O3 Ti1 1.8112(7) 3_566 ?
O2 C21 1.338(4) . ?
O1 C11 1.336(4) . ?
N1 C1 1.480(5) . ?
N1 C17 1.494(4) . ?
N1 C27 1.495(4) . ?
O4 H4 0.8200 . ?
N2 C3 1.462(5) . ?
N2 C4 1.474(5) . ?
N2 C2 1.474(5) . ?
C26 C25 1.376(5) . ?
C26 C21 1.408(5) . ?
C26 C27 1.501(5) . ?
C61 C64 1.522(5) . ?
C61 C62 1.529(6) . ?
C61 C24 1.531(6) . ?
C61 C63 1.532(6) . ?
C23 C24 1.384(5) . ?
C23 C22 1.397(5) . ?
C23 H23 0.9300 . ?
C16 C11 1.388(5) . ?
C16 C15 1.396(5) . ?
C16 C17 1.506(5) . ?
C31 C32 1.522(5) . ?
C31 C34 1.532(5) . ?
C31 C12 1.535(5) . ?
C31 C33 1.536(5) . ?
C11 C12 1.437(5) . ?
C1 C2 1.511(5) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C51 C52B 1.50(3) . ?
C51 C54B 1.515(19) . ?
C51 C53A 1.523(7) . ?
C51 C22 1.536(5) . ?
C51 C54A 1.541(6) . ?
C51 C52A 1.543(7) . ?
C51 C53B 1.55(2) . ?
C22 C21 1.402(5) . ?
C15 C14 1.382(5) . ?
C15 H15 0.9300 . ?
C41 C44 1.519(6) . ?
C41 C42 1.523(5) . ?
C41 C14 1.528(5) . ?
C41 C43 1.543(5) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C13 C14 1.391(5) . ?
C13 C12 1.393(5) . ?
C13 H13 0.9300 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C25 C24 1.393(5) . ?
C25 H25 0.9300 . ?
O6 C81 1.406(6) . ?
O6 C84 1.412(6) . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
O5 C74 1.406(7) . ?
O5 C71 1.414(6) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C27 H27A 0.9700 . ?
C27 H27B 0.9700 . ?
C64 H64A 0.9600 . ?
C64 H64B 0.9600 . ?
C64 H64C 0.9600 . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C63 H63A 0.9600 . ?
C63 H63B 0.9600 . ?
C63 H63C 0.9600 . ?
C62 H62A 0.9600 . ?
C62 H62B 0.9600 . ?
C62 H62C 0.9600 . ?
C71 C72 1.497(7) . ?
C71 H71A 0.9700 . ?
C71 H71B 0.9700 . ?
C72 C73 1.477(7) . ?
C72 H72A 0.9700 . ?
C72 H72B 0.9700 . ?
C73 C74 1.476(8) . ?
C73 H73A 0.9700 . ?
C73 H73B 0.9700 . ?
C83 C84 1.481(7) . ?
C83 C82 1.502(7) . ?
C83 H83A 0.9700 . ?
C83 H83B 0.9700 . ?
C81 C82 1.509(7) . ?
C81 H81A 0.9700 . ?
C81 H81B 0.9700 . ?
C82 H82A 0.9700 . ?
C82 H82B 0.9700 . ?
C74 H74A 0.9700 . ?
C74 H74B 0.9700 . ?
C84 H84A 0.9700 . ?
C84 H84B 0.9700 . ?
C52A H52A 0.9600 . ?
C52A H52B 0.9600 . ?
C52A H52C 0.9600 . ?
C53A H53A 0.9600 . ?
C53A H53B 0.9600 . ?
C53A H53C 0.9600 . ?
C54A H54A 0.9600 . ?
C54A H54B 0.9600 . ?
C54A H54C 0.9600 . ?
C52B H52D 0.9600 . ?
C52B H52E 0.9600 . ?
C52B H52F 0.9600 . ?
C53B H53D 0.9600 . ?
C53B H53E 0.9600 . ?
C53B H53F 0.9600 . ?
C54B H54D 0.9600 . ?
C54B H54E 0.9600 . ?
C54B H54F 0.9600 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O4 104.88(10) . . ?
O3 Ti1 O2 93.74(8) . . ?
O4 Ti1 O2 94.18(11) . . ?
O3 Ti1 O1 96.37(8) . . ?
O4 Ti1 O1 94.65(11) . . ?
O2 Ti1 O1 164.40(12) . . ?
O3 Ti1 N1 90.36(8) . . ?
O4 Ti1 N1 164.74(12) . . ?
O2 Ti1 N1 83.95(10) . . ?
O1 Ti1 N1 84.14(10) . . ?
O3 Ti1 N2 164.39(9) . . ?
O4 Ti1 N2 90.26(12) . . ?
O2 Ti1 N2 81.17(11) . . ?
O1 Ti1 N2 85.96(11) . . ?
N1 Ti1 N2 74.49(11) . . ?
Ti1 O3 Ti1 180.00(3) 3_566 . ?
C21 O2 Ti1 143.7(2) . . ?
C11 O1 Ti1 141.3(2) . . ?
C1 N1 C17 109.7(3) . . ?
C1 N1 C27 111.1(3) . . ?
C17 N1 C27 105.5(3) . . ?
C1 N1 Ti1 113.9(2) . . ?
C17 N1 Ti1 108.3(2) . . ?
C27 N1 Ti1 108.0(2) . . ?
Ti1 O4 H4 109.5 . . ?
C3 N2 C4 107.7(3) . . ?
C3 N2 C2 110.1(3) . . ?
C4 N2 C2 108.8(3) . . ?
C3 N2 Ti1 114.7(2) . . ?
C4 N2 Ti1 109.0(2) . . ?
C2 N2 Ti1 106.4(2) . . ?
C25 C26 C21 119.9(3) . . ?
C25 C26 C27 120.0(3) . . ?
C21 C26 C27 119.8(3) . . ?
C64 C61 C62 108.1(3) . . ?
C64 C61 C24 112.7(3) . . ?
C62 C61 C24 108.4(3) . . ?
C64 C61 C63 107.3(4) . . ?
C62 C61 C63 109.1(4) . . ?
C24 C61 C63 111.2(3) . . ?
C24 C23 C22 124.7(3) . . ?
C24 C23 H23 117.7 . . ?
C22 C23 H23 117.7 . . ?
C11 C16 C15 120.2(3) . . ?
C11 C16 C17 120.4(3) . . ?
C15 C16 C17 119.1(3) . . ?
C32 C31 C34 107.4(3) . . ?
C32 C31 C12 111.6(3) . . ?
C34 C31 C12 111.7(3) . . ?
C32 C31 C33 108.2(3) . . ?
C34 C31 C33 107.5(3) . . ?
C12 C31 C33 110.4(3) . . ?
O1 C11 C16 119.7(3) . . ?
O1 C11 C12 120.8(3) . . ?
C16 C11 C12 119.5(3) . . ?
N1 C1 C2 111.6(3) . . ?
N1 C1 H1A 109.3 . . ?
C2 C1 H1A 109.3 . . ?
N1 C1 H1B 109.3 . . ?
C2 C1 H1B 109.3 . . ?
H1A C1 H1B 108.0 . . ?
C52B C51 C54B 110.1(12) . . ?
C52B C51 C53A 139.2(10) . . ?
C54B C51 C53A 69.4(9) . . ?
C52B C51 C22 107.7(8) . . ?
C54B C51 C22 114.2(9) . . ?
C53A C51 C22 109.2(4) . . ?
C52B C51 C54A 74.1(9) . . ?
C53A C51 C54A 108.7(4) . . ?
C22 C51 C54A 109.6(4) . . ?
C54B C51 C52A 127.3(9) . . ?
C53A C51 C52A 108.3(5) . . ?
C22 C51 C52A 115.6(3) . . ?
C54A C51 C52A 105.2(4) . . ?
C52B C51 C53B 109.0(13) . . ?
C54B C51 C53B 106.0(11) . . ?
C22 C51 C53B 109.8(8) . . ?
C54A C51 C53B 137.0(8) . . ?
C52A C51 C53B 71.9(9) . . ?
C23 C22 C21 116.7(3) . . ?
C23 C22 C51 118.2(3) . . ?
C21 C22 C51 125.0(4) . . ?
O2 C21 C22 121.9(3) . . ?
O2 C21 C26 118.0(3) . . ?
C22 C21 C26 120.1(4) . . ?
C14 C15 C16 122.5(4) . . ?
C14 C15 H15 118.8 . . ?
C16 C15 H15 118.8 . . ?
C44 C41 C42 107.7(4) . . ?
C44 C41 C14 112.5(3) . . ?
C42 C41 C14 110.7(3) . . ?
C44 C41 C43 108.5(3) . . ?
C42 C41 C43 109.0(3) . . ?
C14 C41 C43 108.4(3) . . ?
N2 C2 C1 110.2(3) . . ?
N2 C2 H2A 109.6 . . ?
C1 C2 H2A 109.6 . . ?
N2 C2 H2B 109.6 . . ?
C1 C2 H2B 109.6 . . ?
H2A C2 H2B 108.1 . . ?
C14 C13 C12 125.0(3) . . ?
C14 C13 H13 117.5 . . ?
C12 C13 H13 117.5 . . ?
C13 C12 C11 116.6(4) . . ?
C13 C12 C31 121.6(3) . . ?
C11 C12 C31 121.7(3) . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C15 C14 C13 116.1(3) . . ?
C15 C14 C41 123.6(4) . . ?
C13 C14 C41 120.2(3) . . ?
N1 C17 C16 115.8(3) . . ?
N1 C17 H17A 108.3 . . ?
C16 C17 H17A 108.3 . . ?
N1 C17 H17B 108.3 . . ?
C16 C17 H17B 108.3 . . ?
H17A C17 H17B 107.4 . . ?
N2 C3 H3A 109.5 . . ?
N2 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N2 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C31 C33 H33A 109.5 . . ?
C31 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C31 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
C26 C25 C24 122.0(4) . . ?
C26 C25 H25 119.0 . . ?
C24 C25 H25 119.0 . . ?
C81 O6 C84 109.6(4) . . ?
C41 C44 H44A 109.5 . . ?
C41 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C41 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
N2 C4 H4A 109.5 . . ?
N2 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N2 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C23 C24 C25 116.4(4) . . ?
C23 C24 C61 123.0(3) . . ?
C25 C24 C61 120.4(4) . . ?
C74 O5 C71 108.4(4) . . ?
C31 C34 H34A 109.5 . . ?
C31 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C31 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
N1 C27 C26 117.7(3) . . ?
N1 C27 H27A 107.9 . . ?
C26 C27 H27A 107.9 . . ?
N1 C27 H27B 107.9 . . ?
C26 C27 H27B 107.9 . . ?
H27A C27 H27B 107.2 . . ?
C61 C64 H64A 109.5 . . ?
C61 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C61 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C61 C63 H63A 109.5 . . ?
C61 C63 H63B 109.5 . . ?
H63A C63 H63B 109.5 . . ?
C61 C63 H63C 109.5 . . ?
H63A C63 H63C 109.5 . . ?
H63B C63 H63C 109.5 . . ?
C61 C62 H62A 109.5 . . ?
C61 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C61 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
O5 C71 C72 103.9(4) . . ?
O5 C71 H71A 111.0 . . ?
C72 C71 H71A 111.0 . . ?
O5 C71 H71B 111.0 . . ?
C72 C71 H71B 111.0 . . ?
H71A C71 H71B 109.0 . . ?
C73 C72 C71 105.0(5) . . ?
C73 C72 H72A 110.8 . . ?
C71 C72 H72A 110.8 . . ?
C73 C72 H72B 110.8 . . ?
C71 C72 H72B 110.8 . . ?
H72A C72 H72B 108.8 . . ?
C74 C73 C72 103.8(5) . . ?
C74 C73 H73A 111.0 . . ?
C72 C73 H73A 111.0 . . ?
C74 C73 H73B 111.0 . . ?
C72 C73 H73B 111.0 . . ?
H73A C73 H73B 109.0 . . ?
C84 C83 C82 103.8(5) . . ?
C84 C83 H83A 111.0 . . ?
C82 C83 H83A 111.0 . . ?
C84 C83 H83B 111.0 . . ?
C82 C83 H83B 111.0 . . ?
H83A C83 H83B 109.0 . . ?
O6 C81 C82 105.4(4) . . ?
O6 C81 H81A 110.7 . . ?
C82 C81 H81A 110.7 . . ?
O6 C81 H81B 110.7 . . ?
C82 C81 H81B 110.7 . . ?
H81A C81 H81B 108.8 . . ?
C83 C82 C81 101.0(4) . . ?
C83 C82 H82A 111.6 . . ?
C81 C82 H82A 111.6 . . ?
C83 C82 H82B 111.6 . . ?
C81 C82 H82B 111.6 . . ?
H82A C82 H82B 109.4 . . ?
O5 C74 C73 109.0(5) . . ?
O5 C74 H74A 109.9 . . ?
C73 C74 H74A 109.9 . . ?
O5 C74 H74B 109.9 . . ?
C73 C74 H74B 109.9 . . ?
H74A C74 H74B 108.3 . . ?
O6 C84 C83 107.2(5) . . ?
O6 C84 H84A 110.3 . . ?
C83 C84 H84A 110.3 . . ?
O6 C84 H84B 110.3 . . ?
C83 C84 H84B 110.3 . . ?
H84A C84 H84B 108.5 . . ?
C51 C52A H52A 109.5 . . ?
C51 C52A H52B 109.5 . . ?
H52A C52A H52B 109.5 . . ?
C51 C52A H52C 109.5 . . ?
H52A C52A H52C 109.5 . . ?
H52B C52A H52C 109.5 . . ?
C51 C53A H53A 109.5 . . ?
C51 C53A H53B 109.5 . . ?
H53A C53A H53B 109.5 . . ?
C51 C53A H53C 109.5 . . ?
H53A C53A H53C 109.5 . . ?
H53B C53A H53C 109.5 . . ?
C51 C54A H54A 109.5 . . ?
C51 C54A H54B 109.5 . . ?
H54A C54A H54B 109.5 . . ?
C51 C54A H54C 109.5 . . ?
H54A C54A H54C 109.5 . . ?
H54B C54A H54C 109.5 . . ?
C51 C52B H52D 109.5 . . ?
C51 C52B H52E 109.5 . . ?
H52D C52B H52E 109.5 . . ?
C51 C52B H52F 109.5 . . ?
H52D C52B H52F 109.5 . . ?
H52E C52B H52F 109.5 . . ?
C51 C53B H53D 109.5 . . ?
C51 C53B H53E 109.5 . . ?
H53D C53B H53E 109.5 . . ?
C51 C53B H53F 109.5 . . ?
H53D C53B H53F 109.5 . . ?
H53E C53B H53F 109.5 . . ?
C51 C54B H54D 109.5 . . ?
C51 C54B H54E 109.5 . . ?
H54D C54B H54E 109.5 . . ?
C51 C54B H54F 109.5 . . ?
H54D C54B H54F 109.5 . . ?
H54E C54B H54F 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O3 Ti1 O2 C21 80.9(4) . . . . ?
O4 Ti1 O2 C21 -173.9(4) . . . . ?
O1 Ti1 O2 C21 -49.5(7) . . . . ?
N1 Ti1 O2 C21 -9.1(4) . . . . ?
N2 Ti1 O2 C21 -84.3(4) . . . . ?
O3 Ti1 O1 C11 -82.6(4) . . . . ?
O4 Ti1 O1 C11 171.9(4) . . . . ?
O2 Ti1 O1 C11 47.5(6) . . . . ?
N1 Ti1 O1 C11 7.1(4) . . . . ?
N2 Ti1 O1 C11 81.9(4) . . . . ?
O3 Ti1 N1 C1 179.9(2) . . . . ?
O4 Ti1 N1 C1 -2.7(5) . . . . ?
O2 Ti1 N1 C1 -86.4(2) . . . . ?
O1 Ti1 N1 C1 83.5(2) . . . . ?
N2 Ti1 N1 C1 -3.9(2) . . . . ?
O3 Ti1 N1 C17 57.6(2) . . . . ?
O4 Ti1 N1 C17 -125.0(4) . . . . ?
O2 Ti1 N1 C17 151.3(2) . . . . ?
O1 Ti1 N1 C17 -38.8(2) . . . . ?
N2 Ti1 N1 C17 -126.2(2) . . . . ?
O3 Ti1 N1 C27 -56.2(2) . . . . ?
O4 Ti1 N1 C27 121.2(4) . . . . ?
O2 Ti1 N1 C27 37.5(2) . . . . ?
O1 Ti1 N1 C27 -152.6(2) . . . . ?
N2 Ti1 N1 C27 120.0(2) . . . . ?
O3 Ti1 N2 C3 112.8(3) . . . . ?
O4 Ti1 N2 C3 -81.1(3) . . . . ?
O2 Ti1 N2 C3 -175.3(3) . . . . ?
O1 Ti1 N2 C3 13.6(3) . . . . ?
N1 Ti1 N2 C3 98.6(3) . . . . ?
O3 Ti1 N2 C4 -126.3(3) . . . . ?
O4 Ti1 N2 C4 39.8(3) . . . . ?
O2 Ti1 N2 C4 -54.4(3) . . . . ?
O1 Ti1 N2 C4 134.4(3) . . . . ?
N1 Ti1 N2 C4 -140.6(3) . . . . ?
O3 Ti1 N2 C2 -9.2(4) . . . . ?
O4 Ti1 N2 C2 156.9(2) . . . . ?
O2 Ti1 N2 C2 62.7(2) . . . . ?
O1 Ti1 N2 C2 -108.4(2) . . . . ?
N1 Ti1 N2 C2 -23.4(2) . . . . ?
Ti1 O1 C11 C16 7.3(6) . . . . ?
Ti1 O1 C11 C12 -172.4(3) . . . . ?
C15 C16 C11 O1 -175.3(3) . . . . ?
C17 C16 C11 O1 10.6(6) . . . . ?
C15 C16 C11 C12 4.4(6) . . . . ?
C17 C16 C11 C12 -169.7(3) . . . . ?
C17 N1 C1 C2 152.5(3) . . . . ?
C27 N1 C1 C2 -91.2(4) . . . . ?
Ti1 N1 C1 C2 31.0(4) . . . . ?
C24 C23 C22 C21 -2.1(6) . . . . ?
C24 C23 C22 C51 175.5(4) . . . . ?
C52B C51 C22 C23 -129.0(11) . . . . ?
C54B C51 C22 C23 -6.4(11) . . . . ?
C53A C51 C22 C23 69.0(5) . . . . ?
C54A C51 C22 C23 -50.0(5) . . . . ?
C52A C51 C22 C23 -168.7(5) . . . . ?
C53B C51 C22 C23 112.5(10) . . . . ?
C52B C51 C22 C21 48.4(11) . . . . ?
C54B C51 C22 C21 171.0(11) . . . . ?
C53A C51 C22 C21 -113.6(5) . . . . ?
C54A C51 C22 C21 127.4(5) . . . . ?
C52A C51 C22 C21 8.7(6) . . . . ?
C53B C51 C22 C21 -70.1(11) . . . . ?
Ti1 O2 C21 C22 174.9(3) . . . . ?
Ti1 O2 C21 C26 -3.7(6) . . . . ?
C23 C22 C21 O2 -173.5(3) . . . . ?
C51 C22 C21 O2 9.0(6) . . . . ?
C23 C22 C21 C26 5.0(6) . . . . ?
C51 C22 C21 C26 -172.4(4) . . . . ?
C25 C26 C21 O2 174.0(3) . . . . ?
C27 C26 C21 O2 -12.4(5) . . . . ?
C25 C26 C21 C22 -4.7(6) . . . . ?
C27 C26 C21 C22 169.0(3) . . . . ?
C11 C16 C15 C14 -2.0(6) . . . . ?
C17 C16 C15 C14 172.1(4) . . . . ?
C3 N2 C2 C1 -77.3(4) . . . . ?
C4 N2 C2 C1 164.8(3) . . . . ?
Ti1 N2 C2 C1 47.6(3) . . . . ?
N1 C1 C2 N2 -54.2(4) . . . . ?
C14 C13 C12 C11 0.5(6) . . . . ?
C14 C13 C12 C31 -176.1(4) . . . . ?
O1 C11 C12 C13 176.1(3) . . . . ?
C16 C11 C12 C13 -3.6(5) . . . . ?
O1 C11 C12 C31 -7.3(6) . . . . ?
C16 C11 C12 C31 173.0(4) . . . . ?
C32 C31 C12 C13 -118.6(4) . . . . ?
C34 C31 C12 C13 1.6(5) . . . . ?
C33 C31 C12 C13 121.1(4) . . . . ?
C32 C31 C12 C11 65.0(5) . . . . ?
C34 C31 C12 C11 -174.8(4) . . . . ?
C33 C31 C12 C11 -55.3(5) . . . . ?
C16 C15 C14 C13 -1.0(6) . . . . ?
C16 C15 C14 C41 -176.9(4) . . . . ?
C12 C13 C14 C15 1.8(6) . . . . ?
C12 C13 C14 C41 177.8(4) . . . . ?
C44 C41 C14 C15 -11.2(5) . . . . ?
C42 C41 C14 C15 -131.8(4) . . . . ?
C43 C41 C14 C15 108.7(4) . . . . ?
C44 C41 C14 C13 173.0(4) . . . . ?
C42 C41 C14 C13 52.5(5) . . . . ?
C43 C41 C14 C13 -67.0(5) . . . . ?
C1 N1 C17 C16 -59.2(4) . . . . ?
C27 N1 C17 C16 -178.9(3) . . . . ?
Ti1 N1 C17 C16 65.6(3) . . . . ?
C11 C16 C17 N1 -52.9(5) . . . . ?
C15 C16 C17 N1 133.0(4) . . . . ?
C21 C26 C25 C24 1.1(6) . . . . ?
C27 C26 C25 C24 -172.6(4) . . . . ?
C22 C23 C24 C25 -1.4(6) . . . . ?
C22 C23 C24 C61 -176.0(4) . . . . ?
C26 C25 C24 C23 1.9(6) . . . . ?
C26 C25 C24 C61 176.6(4) . . . . ?
C64 C61 C24 C23 -14.1(5) . . . . ?
C62 C61 C24 C23 105.6(4) . . . . ?
C63 C61 C24 C23 -134.6(4) . . . . ?
C64 C61 C24 C25 171.6(4) . . . . ?
C62 C61 C24 C25 -68.8(5) . . . . ?
C63 C61 C24 C25 51.0(5) . . . . ?
C1 N1 C27 C26 61.1(4) . . . . ?
C17 N1 C27 C26 179.9(3) . . . . ?
Ti1 N1 C27 C26 -64.5(4) . . . . ?
C25 C26 C27 N1 -133.3(4) . . . . ?
C21 C26 C27 N1 53.0(5) . . . . ?
C74 O5 C71 C72 28.6(7) . . . . ?
O5 C71 C72 C73 -31.6(6) . . . . ?
C71 C72 C73 C74 22.5(7) . . . . ?
C84 O6 C81 C82 22.8(6) . . . . ?
C84 C83 C82 C81 33.5(6) . . . . ?
O6 C81 C82 C83 -34.8(6) . . . . ?
C71 O5 C74 C73 -14.7(8) . . . . ?
C72 C73 C74 O5 -5.7(8) . . . . ?
C81 O6 C84 C83 -0.8(7) . . . . ?
C82 C83 C84 O6 -21.5(7) . . . . ?

_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.14
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.440
_refine_diff_density_rms         0.072

_database_code_depnum_ccdc_archive 'CCDC 994887'
