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

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

data_a
_database_code_depnum_ccdc_archive 'CCDC 990411'
_audit_update_record             
;
2014-11-12 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C28 H30 N6 O2 Ti'
_chemical_formula_sum            'C28 H30 N6 O2 Ti'
_chemical_formula_weight         530.45

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_space_group_name_Hall  '-C 2yc'
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                   8.7336(17)
_cell_length_b                   16.212(6)
_cell_length_c                   18.952(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.30(3)
_cell_angle_gamma                90.00
_cell_volume                     2681.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.314
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1112
_exptl_absorpt_coefficient_mu    0.356
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.843
_exptl_absorpt_correction_T_max  0.867
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12023
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_sigmaI/netI    0.0454
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.31
_diffrn_reflns_theta_max         27.49
_reflns_number_total             3070
_reflns_number_gt                2422
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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 > 2sigma(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. 
;

_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)+(0.0840P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3070
_refine_ls_number_parameters     170
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0578
_refine_ls_R_factor_gt           0.0456
_refine_ls_wR_factor_ref         0.1365
_refine_ls_wR_factor_gt          0.1289
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_restrained_S_all      1.076
_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 0.5000 -0.04320(2) 0.2500 0.04402(17) Uani 1 2 d S . .
O1 O 0.36926(15) 0.02707(8) 0.20780(7) 0.0538(3) Uani 1 1 d . . .
N3 N 0.37974(17) -0.24120(9) 0.11006(8) 0.0487(4) Uani 1 1 d . . .
N2 N 0.64383(17) -0.07665(10) 0.16854(8) 0.0502(4) Uani 1 1 d . . .
N1 N 0.38353(17) -0.14760(9) 0.19417(8) 0.0481(4) Uani 1 1 d . . .
C7 C 0.4602(2) -0.17767(10) 0.14052(9) 0.0461(4) Uani 1 1 d . . .
C2 C 0.2458(2) -0.25147(11) 0.14766(10) 0.0559(5) Uani 1 1 d . . .
C8 C 0.6063(2) -0.14304(11) 0.12597(9) 0.0502(4) Uani 1 1 d . . .
C4 C 0.1817(3) -0.36706(15) 0.07328(14) 0.0819(7) Uani 1 1 d . . .
H4 H 0.1171 -0.4106 0.0604 0.098 Uiso 1 1 calc R . .
C12 C 0.2296(2) 0.03900(12) 0.16840(12) 0.0620(5) Uani 1 1 d . . .
H12 H 0.1589 -0.0053 0.1804 0.074 Uiso 1 1 calc R . .
C1 C 0.2517(2) -0.19209(12) 0.19923(11) 0.0561(5) Uani 1 1 d . . .
H1 H 0.1776 -0.1835 0.2324 0.067 Uiso 1 1 calc R . .
C6 C 0.4131(2) -0.29203(13) 0.05320(11) 0.0609(5) Uani 1 1 d . . .
H6 H 0.5011 -0.2836 0.0281 0.073 Uiso 1 1 calc R . .
C14 C 0.2583(4) 0.03359(18) 0.09119(14) 0.1019(10) Uani 1 1 d . . .
H14A H 0.3120 0.0820 0.0768 0.153 Uiso 1 1 calc R . .
H14B H 0.1622 0.0297 0.0649 0.153 Uiso 1 1 calc R . .
H14C H 0.3189 -0.0144 0.0823 0.153 Uiso 1 1 calc R . .
C11 C 0.7900(3) -0.05476(14) 0.15278(12) 0.0653(6) Uani 1 1 d . . .
H11 H 0.8450 -0.0114 0.1736 0.078 Uiso 1 1 calc R . .
C3 C 0.1467(3) -0.31754(14) 0.12774(13) 0.0757(6) Uani 1 1 d . . .
H3 H 0.0579 -0.3268 0.1521 0.091 Uiso 1 1 calc R . .
C5 C 0.3164(3) -0.35296(14) 0.03556(13) 0.0762(6) Uani 1 1 d . . .
H5 H 0.3377 -0.3870 -0.0023 0.091 Uiso 1 1 calc R . .
C10 C 0.8432(3) -0.10588(19) 0.10207(14) 0.0903(9) Uani 1 1 d . . .
H10 H 0.9391 -0.1034 0.0826 0.108 Uiso 1 1 calc R . .
C9 C 0.7276(3) -0.16245(17) 0.08471(13) 0.0835(8) Uani 1 1 d . . .
H9 H 0.7315 -0.2049 0.0518 0.100 Uiso 1 1 calc R . .
C13 C 0.1609(4) 0.11897(18) 0.18876(16) 0.1045(10) Uani 1 1 d . . .
H13A H 0.1548 0.1214 0.2392 0.157 Uiso 1 1 calc R . .
H13B H 0.0599 0.1237 0.1672 0.157 Uiso 1 1 calc R . .
H13C H 0.2237 0.1634 0.1730 0.157 Uiso 1 1 calc R . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O1 1.7798(13) 2_655 ?
Ti1 O1 1.7799(13) . ?
Ti1 N2 2.1003(16) . ?
Ti1 N2 2.1004(16) 2_655 ?
Ti1 N1 2.2209(15) 2_655 ?
Ti1 N1 2.2209(16) . ?
O1 C12 1.418(2) . ?
N3 C7 1.362(2) . ?
N3 C6 1.397(2) . ?
N3 C2 1.404(3) . ?
N2 C11 1.369(3) . ?
N2 C8 1.377(2) . ?
N1 C7 1.332(2) . ?
N1 C1 1.365(2) . ?
C7 C8 1.432(2) . ?
C2 C1 1.371(3) . ?
C2 C3 1.419(3) . ?
C8 C9 1.378(3) . ?
C4 C3 1.352(3) . ?
C4 C5 1.420(4) . ?
C4 H4 0.9300 . ?
C12 C13 1.486(3) . ?
C12 C14 1.497(4) . ?
C12 H12 0.9800 . ?
C1 H1 0.9300 . ?
C6 C5 1.334(3) . ?
C6 H6 0.9300 . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C11 C10 1.364(3) . ?
C11 H11 0.9300 . ?
C3 H3 0.9300 . ?
C5 H5 0.9300 . ?
C10 C9 1.393(4) . ?
C10 H10 0.9300 . ?
C9 H9 0.9300 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 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
O1 Ti1 O1 100.41(9) 2_655 . ?
O1 Ti1 N2 95.96(6) 2_655 . ?
O1 Ti1 N2 103.11(6) . . ?
O1 Ti1 N2 103.11(6) 2_655 2_655 ?
O1 Ti1 N2 95.96(6) . 2_655 ?
N2 Ti1 N2 150.07(9) . 2_655 ?
O1 Ti1 N1 90.02(6) 2_655 2_655 ?
O1 Ti1 N1 167.20(6) . 2_655 ?
N2 Ti1 N1 82.96(6) . 2_655 ?
N2 Ti1 N1 74.28(6) 2_655 2_655 ?
O1 Ti1 N1 167.20(6) 2_655 . ?
O1 Ti1 N1 90.02(6) . . ?
N2 Ti1 N1 74.28(6) . . ?
N2 Ti1 N1 82.96(6) 2_655 . ?
N1 Ti1 N1 80.70(8) 2_655 . ?
C12 O1 Ti1 147.87(12) . . ?
C7 N3 C6 130.78(18) . . ?
C7 N3 C2 107.49(15) . . ?
C6 N3 C2 121.72(17) . . ?
C11 N2 C8 106.06(16) . . ?
C11 N2 Ti1 133.12(14) . . ?
C8 N2 Ti1 119.83(12) . . ?
C7 N1 C1 108.13(15) . . ?
C7 N1 Ti1 114.08(11) . . ?
C1 N1 Ti1 137.78(12) . . ?
N1 C7 N3 109.51(15) . . ?
N1 C7 C8 118.87(15) . . ?
N3 C7 C8 131.58(16) . . ?
C1 C2 N3 105.68(16) . . ?
C1 C2 C3 136.4(2) . . ?
N3 C2 C3 117.79(19) . . ?
N2 C8 C9 109.94(17) . . ?
N2 C8 C7 112.75(15) . . ?
C9 C8 C7 137.00(18) . . ?
C3 C4 C5 120.4(2) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
O1 C12 C13 109.26(19) . . ?
O1 C12 C14 109.4(2) . . ?
C13 C12 C14 113.0(2) . . ?
O1 C12 H12 108.4 . . ?
C13 C12 H12 108.4 . . ?
C14 C12 H12 108.4 . . ?
N1 C1 C2 109.18(17) . . ?
N1 C1 H1 125.4 . . ?
C2 C1 H1 125.4 . . ?
C5 C6 N3 118.7(2) . . ?
C5 C6 H6 120.6 . . ?
N3 C6 H6 120.6 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C10 C11 N2 110.0(2) . . ?
C10 C11 H11 125.0 . . ?
N2 C11 H11 125.0 . . ?
C4 C3 C2 119.8(2) . . ?
C4 C3 H3 120.1 . . ?
C2 C3 H3 120.1 . . ?
C6 C5 C4 121.5(2) . . ?
C6 C5 H5 119.2 . . ?
C4 C5 H5 119.2 . . ?
C11 C10 C9 107.6(2) . . ?
C11 C10 H10 126.2 . . ?
C9 C10 H10 126.2 . . ?
C8 C9 C10 106.3(2) . . ?
C8 C9 H9 126.8 . . ?
C10 C9 H9 126.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 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
O1 Ti1 O1 C12 -173.2(3) 2_655 . . . ?
N2 Ti1 O1 C12 88.2(2) . . . . ?
N2 Ti1 O1 C12 -68.6(2) 2_655 . . . ?
N1 Ti1 O1 C12 -29.0(4) 2_655 . . . ?
N1 Ti1 O1 C12 14.3(2) . . . . ?
O1 Ti1 N2 C11 1.50(19) 2_655 . . . ?
O1 Ti1 N2 C11 103.66(19) . . . . ?
N2 Ti1 N2 C11 -128.16(19) 2_655 . . . ?
N1 Ti1 N2 C11 -87.79(19) 2_655 . . . ?
N1 Ti1 N2 C11 -170.07(19) . . . . ?
O1 Ti1 N2 C8 168.44(13) 2_655 . . . ?
O1 Ti1 N2 C8 -89.39(14) . . . . ?
N2 Ti1 N2 C8 38.78(12) 2_655 . . . ?
N1 Ti1 N2 C8 79.15(13) 2_655 . . . ?
N1 Ti1 N2 C8 -3.12(13) . . . . ?
O1 Ti1 N1 C7 -40.6(3) 2_655 . . . ?
O1 Ti1 N1 C7 104.20(12) . . . . ?
N2 Ti1 N1 C7 0.58(12) . . . . ?
N2 Ti1 N1 C7 -159.80(13) 2_655 . . . ?
N1 Ti1 N1 C7 -84.66(12) 2_655 . . . ?
O1 Ti1 N1 C1 138.8(3) 2_655 . . . ?
O1 Ti1 N1 C1 -76.37(19) . . . . ?
N2 Ti1 N1 C1 -180.0(2) . . . . ?
N2 Ti1 N1 C1 19.63(19) 2_655 . . . ?
N1 Ti1 N1 C1 94.77(19) 2_655 . . . ?
C1 N1 C7 N3 0.28(19) . . . . ?
Ti1 N1 C7 N3 179.87(10) . . . . ?
C1 N1 C7 C8 -177.71(16) . . . . ?
Ti1 N1 C7 C8 1.9(2) . . . . ?
C6 N3 C7 N1 -179.41(17) . . . . ?
C2 N3 C7 N1 -0.56(19) . . . . ?
C6 N3 C7 C8 -1.8(3) . . . . ?
C2 N3 C7 C8 177.08(18) . . . . ?
C7 N3 C2 C1 0.6(2) . . . . ?
C6 N3 C2 C1 179.59(17) . . . . ?
C7 N3 C2 C3 -176.73(18) . . . . ?
C6 N3 C2 C3 2.2(3) . . . . ?
C11 N2 C8 C9 0.4(2) . . . . ?
Ti1 N2 C8 C9 -169.76(16) . . . . ?
C11 N2 C8 C7 175.11(16) . . . . ?
Ti1 N2 C8 C7 5.0(2) . . . . ?
N1 C7 C8 N2 -4.4(2) . . . . ?
N3 C7 C8 N2 178.15(17) . . . . ?
N1 C7 C8 C9 168.4(2) . . . . ?
N3 C7 C8 C9 -9.1(4) . . . . ?
Ti1 O1 C12 C13 146.9(2) . . . . ?
Ti1 O1 C12 C14 -88.9(3) . . . . ?
C7 N1 C1 C2 0.1(2) . . . . ?
Ti1 N1 C1 C2 -179.32(13) . . . . ?
N3 C2 C1 N1 -0.5(2) . . . . ?
C3 C2 C1 N1 176.1(2) . . . . ?
C7 N3 C6 C5 177.13(18) . . . . ?
C2 N3 C6 C5 -1.6(3) . . . . ?
C8 N2 C11 C10 -0.2(3) . . . . ?
Ti1 N2 C11 C10 168.04(18) . . . . ?
C5 C4 C3 C2 -0.5(4) . . . . ?
C1 C2 C3 C4 -177.5(2) . . . . ?
N3 C2 C3 C4 -1.2(3) . . . . ?
N3 C6 C5 C4 -0.2(4) . . . . ?
C3 C4 C5 C6 1.2(4) . . . . ?
N2 C11 C10 C9 0.0(3) . . . . ?
N2 C8 C9 C10 -0.4(3) . . . . ?
C7 C8 C9 C10 -173.3(2) . . . . ?
C11 C10 C9 C8 0.3(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_theta_full        27.49
_diffrn_measured_fraction_theta_full 0.993
_refine_diff_density_max         0.369
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.043
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_t
_database_code_depnum_ccdc_archive 'CCDC 1030010'
_audit_update_record             
;
2014-10-27 deposited with the CCDC.
2014-12-22 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 N8 Ti'
_chemical_formula_sum            'C30 H36 N8 Ti'
_chemical_formula_weight         556.54

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'
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_space_hall_name_H-M    '-P 2ybc'

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                   23.010(9)
_cell_length_b                   13.712(5)
_cell_length_c                   21.228(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 115.456(7)
_cell_angle_gamma                90.00
_cell_volume                     6048(4)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    3277
_cell_measurement_theta_min      2.28
_cell_measurement_theta_max      21.02

_exptl_crystal_description       block
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2352
_exptl_absorpt_coefficient_mu    0.315
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.860
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_process_details   'SADABS (Bruker, 2005)'

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEXII 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            35810
_diffrn_reflns_av_R_equivalents  0.0663
_diffrn_reflns_av_sigmaI/netI    0.0793
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.78
_diffrn_reflns_theta_max         26.22
_reflns_number_total             12166
_reflns_number_gt                6042
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX-II (Bruker, 2005)'
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'

_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 > 2sigma(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. 
;

_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)+(0.0626P)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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         12094
_refine_ls_number_parameters     711
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1290
_refine_ls_R_factor_gt           0.0507
_refine_ls_wR_factor_ref         0.1438
_refine_ls_wR_factor_gt          0.1111
_refine_ls_goodness_of_fit_ref   0.950
_refine_ls_restrained_S_all      0.950
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.002

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 0.07865(3) 0.73124(4) 0.18170(3) 0.04752(16) Uani 1 1 d . . .
N1 N 0.11883(11) 0.62064(18) 0.26712(13) 0.0499(6) Uani 1 1 d . . .
N3 N 0.01225(11) 0.74147(18) 0.23585(12) 0.0485(6) Uani 1 1 d . . .
N2 N 0.15018(11) 0.80587(18) 0.26991(13) 0.0510(6) Uani 1 1 d . . .
C8 C 0.18386(13) 0.7546(2) 0.33145(15) 0.0471(7) Uani 1 1 d . . .
N8 N -0.08035(12) 0.69745(18) 0.23668(13) 0.0515(6) Uani 1 1 d . . .
N7 N 0.18439(11) 0.58055(19) 0.37552(13) 0.0499(6) Uani 1 1 d . . .
N6 N 0.03704(12) 0.84389(19) 0.12851(13) 0.0564(7) Uani 1 1 d . . .
N4 N 0.00585(11) 0.62555(18) 0.13151(12) 0.0511(6) Uani 1 1 d . . .
C18 C -0.03816(14) 0.6808(2) 0.20778(15) 0.0464(7) Uani 1 1 d . . .
C19 C -0.04149(14) 0.6119(2) 0.15503(15) 0.0475(8) Uani 1 1 d . . .
C2 C 0.14869(15) 0.4960(2) 0.34324(17) 0.0548(8) Uani 1 1 d . . .
C11 C 0.17725(15) 0.8964(2) 0.28064(18) 0.0590(9) Uani 1 1 d . . .
H11 H 0.1645 0.9464 0.2479 0.071 Uiso 1 1 calc R . .
C12 C 0.00364(16) 0.7966(2) 0.28539(16) 0.0563(8) Uani 1 1 d . . .
H12 H 0.0322 0.8439 0.3131 0.068 Uiso 1 1 calc R . .
N5 N 0.13337(12) 0.6920(2) 0.13935(14) 0.0592(7) Uani 1 1 d . . .
C1 C 0.10822(15) 0.5243(2) 0.27637(16) 0.0555(8) Uani 1 1 d . . .
H1 H 0.0783 0.4842 0.2426 0.067 Uiso 1 1 calc R . .
C7 C 0.16462(13) 0.6541(2) 0.32764(15) 0.0463(7) Uani 1 1 d . . .
C22 C -0.00470(16) 0.5553(2) 0.08239(16) 0.0610(9) Uani 1 1 d . . .
H22 H 0.0195 0.5476 0.0572 0.073 Uiso 1 1 calc R . .
C3 C 0.16205(17) 0.4087(3) 0.38305(19) 0.0687(10) Uani 1 1 d . . .
H3 H 0.1397 0.3518 0.3632 0.082 Uiso 1 1 calc R . .
C17 C -0.14072(16) 0.6579(3) 0.22170(18) 0.0640(9) Uani 1 1 d . . .
H17 H -0.1580 0.6100 0.1877 0.077 Uiso 1 1 calc R . .
C6 C 0.23136(15) 0.5786(3) 0.44478(17) 0.0649(9) Uani 1 1 d . . .
H6 H 0.2549 0.6343 0.4655 0.078 Uiso 1 1 calc R . .
C21 C -0.05620(17) 0.4974(3) 0.07515(18) 0.0705(10) Uani 1 1 d . . .
H21 H -0.0722 0.4445 0.0452 0.085 Uiso 1 1 calc R . .
C10 C 0.22646(16) 0.9032(3) 0.3472(2) 0.0678(10) Uani 1 1 d . . .
H10 H 0.2519 0.9578 0.3668 0.081 Uiso 1 1 calc R . .
C9 C 0.23098(15) 0.8131(2) 0.37964(17) 0.0609(9) Uani 1 1 d . . .
H9 H 0.2599 0.7959 0.4246 0.073 Uiso 1 1 calc R . .
C14 C -0.08906(19) 0.8027(3) 0.32506(19) 0.0704(10) Uani 1 1 d . . .
H14 H -0.0724 0.8499 0.3597 0.084 Uiso 1 1 calc R . .
C5 C 0.24177(17) 0.4945(3) 0.48082(19) 0.0760(11) Uani 1 1 d . . .
H5 H 0.2723 0.4930 0.5271 0.091 Uiso 1 1 calc R . .
C20 C -0.08011(16) 0.5331(2) 0.12156(17) 0.0623(9) Uani 1 1 d . . .
H20 H -0.1147 0.5089 0.1284 0.075 Uiso 1 1 calc R . .
C27 C 0.00766(17) 0.8331(3) 0.05145(17) 0.0729(10) Uani 1 1 d . . .
H27A H 0.0253 0.7754 0.0397 0.088 Uiso 1 1 calc R . .
H27B H 0.0197 0.8890 0.0316 0.088 Uiso 1 1 calc R . .
C4 C 0.20745(18) 0.4084(3) 0.4501(2) 0.0803(12) Uani 1 1 d . . .
H4 H 0.2161 0.3512 0.4760 0.096 Uiso 1 1 calc R . .
C23 C 0.15963(18) 0.5929(3) 0.14393(19) 0.0764(11) Uani 1 1 d . . .
H23A H 0.1575 0.5753 0.0987 0.092 Uiso 1 1 calc R . .
H23B H 0.1325 0.5477 0.1543 0.092 Uiso 1 1 calc R . .
C15 C -0.1476(2) 0.7630(3) 0.3094(2) 0.0820(12) Uani 1 1 d . . .
H15 H -0.1711 0.7839 0.3332 0.098 Uiso 1 1 calc R . .
C16 C -0.17370(18) 0.6896(3) 0.2569(2) 0.0801(11) Uani 1 1 d . . .
H16 H -0.2140 0.6634 0.2469 0.096 Uiso 1 1 calc R . .
C28 C -0.06564(17) 0.8249(3) 0.01795(19) 0.0948(14) Uani 1 1 d . . .
H28A H -0.0782 0.7708 0.0381 0.142 Uiso 1 1 calc R . .
H28B H -0.0810 0.8147 -0.0313 0.142 Uiso 1 1 calc R . .
H28C H -0.0838 0.8839 0.0260 0.142 Uiso 1 1 calc R . .
Ti2 Ti 0.43490(2) 0.22835(4) 0.32908(3) 0.04748(16) Uani 1 1 d . . .
N16 N 0.57098(12) 0.25204(18) 0.23910(14) 0.0544(7) Uani 1 1 d . . .
N12 N 0.50987(12) 0.33329(18) 0.36589(13) 0.0529(7) Uani 1 1 d . . .
N11 N 0.48712(12) 0.21299(18) 0.25954(13) 0.0512(6) Uani 1 1 d . . .
N9 N 0.37951(12) 0.32661(19) 0.23783(13) 0.0560(7) Uani 1 1 d . . .
N10 N 0.35801(12) 0.14134(19) 0.25727(13) 0.0548(7) Uani 1 1 d . . .
C37 C 0.32968(15) 0.2818(3) 0.18677(16) 0.0549(8) Uani 1 1 d . . .
C48 C 0.53926(14) 0.2703(2) 0.27969(16) 0.0504(8) Uani 1 1 d . . .
N14 N 0.48368(12) 0.11926(18) 0.38123(12) 0.0520(7) Uani 1 1 d . . .
N13 N 0.39276(12) 0.27721(19) 0.38326(13) 0.0568(7) Uani 1 1 d . . .
N15 N 0.30024(13) 0.3449(2) 0.13223(14) 0.0638(8) Uani 1 1 d . . .
C55 C 0.52100(16) 0.1306(2) 0.45748(16) 0.0624(9) Uani 1 1 d . . .
H55A H 0.5143 0.0732 0.4803 0.075 Uiso 1 1 calc R . .
H55B H 0.5042 0.1862 0.4726 0.075 Uiso 1 1 calc R . .
C49 C 0.55365(15) 0.3378(2) 0.33668(17) 0.0550(8) Uani 1 1 d . . .
C42 C 0.48458(16) 0.1574(2) 0.20427(16) 0.0588(9) Uani 1 1 d . . .
H42 H 0.4528 0.1119 0.1802 0.071 Uiso 1 1 calc R . .
C52 C 0.53256(16) 0.3969(2) 0.42091(17) 0.0641(9) Uani 1 1 d . . .
H52 H 0.5131 0.4084 0.4506 0.077 Uiso 1 1 calc R . .
C38 C 0.31546(14) 0.1814(3) 0.19424(16) 0.0538(8) Uani 1 1 d . . .
C43 C 0.53566(17) 0.1792(2) 0.19000(17) 0.0583(9) Uani 1 1 d . . .
C53 C 0.50278(16) 0.0351(2) 0.35149(17) 0.0596(9) Uani 1 1 d . . .
H53A H 0.5449 0.0482 0.3533 0.071 Uiso 1 1 calc R . .
H53B H 0.4727 0.0292 0.3027 0.071 Uiso 1 1 calc R . .
C31 C 0.38290(17) 0.4198(3) 0.21567(19) 0.0659(10) Uani 1 1 d . . .
H31 H 0.4133 0.4663 0.2412 0.079 Uiso 1 1 calc R . .
C40 C 0.28042(17) 0.0303(3) 0.1985(2) 0.0743(11) Uani 1 1 d . . .
H40 H 0.2567 -0.0272 0.1877 0.089 Uiso 1 1 calc R . .
C32 C 0.33412(17) 0.4337(3) 0.14958(19) 0.0669(10) Uani 1 1 d . . .
C44 C 0.5594(2) 0.1483(3) 0.1412(2) 0.0769(11) Uani 1 1 d . . .
H44 H 0.5374 0.1009 0.1082 0.092 Uiso 1 1 calc R . .
C41 C 0.33531(16) 0.0496(2) 0.25833(19) 0.0651(9) Uani 1 1 d . . .
H41 H 0.3545 0.0057 0.2949 0.078 Uiso 1 1 calc R . .
C57 C 0.37247(17) 0.3801(3) 0.38062(19) 0.0748(11) Uani 1 1 d . . .
H57A H 0.3947 0.4190 0.3596 0.090 Uiso 1 1 calc R . .
H57B H 0.3856 0.4034 0.4279 0.090 Uiso 1 1 calc R . .
C39 C 0.26748(16) 0.1143(3) 0.15720(19) 0.0677(10) Uani 1 1 d . . .
H39 H 0.2334 0.1234 0.1135 0.081 Uiso 1 1 calc R . .
C47 C 0.62722(16) 0.2925(3) 0.2404(2) 0.0682(10) Uani 1 1 d . . .
H47 H 0.6496 0.3403 0.2729 0.082 Uiso 1 1 calc R . .
C50 C 0.60185(17) 0.4039(3) 0.3726(2) 0.0759(11) Uani 1 1 d . . .
H50 H 0.6365 0.4202 0.3631 0.091 Uiso 1 1 calc R . .
C51 C 0.58820(17) 0.4416(3) 0.4263(2) 0.0805(12) Uani 1 1 d . . .
H51 H 0.6122 0.4879 0.4593 0.097 Uiso 1 1 calc R . .
C46 C 0.6485(2) 0.2612(3) 0.1940(2) 0.0837(12) Uani 1 1 d . . .
H46 H 0.6862 0.2872 0.1950 0.100 Uiso 1 1 calc R . .
C33 C 0.3116(2) 0.5115(3) 0.1000(2) 0.0973(15) Uani 1 1 d . . .
H33 H 0.3327 0.5713 0.1096 0.117 Uiso 1 1 calc R . .
C59 C 0.36678(18) 0.2126(3) 0.4204(2) 0.0785(11) Uani 1 1 d . . .
H59A H 0.3856 0.1484 0.4237 0.094 Uiso 1 1 calc R . .
H59B H 0.3208 0.2063 0.3924 0.094 Uiso 1 1 calc R . .
C54 C 0.50553(19) -0.0628(2) 0.38733(19) 0.0827(12) Uani 1 1 d . . .
H54A H 0.5392 -0.0610 0.4340 0.124 Uiso 1 1 calc R . .
H54B H 0.5141 -0.1140 0.3616 0.124 Uiso 1 1 calc R . .
H54C H 0.4651 -0.0747 0.3889 0.124 Uiso 1 1 calc R . .
C56 C 0.59377(16) 0.1449(3) 0.48179(18) 0.0854(12) Uani 1 1 d . . .
H56A H 0.6120 0.0866 0.4726 0.128 Uiso 1 1 calc R . .
H56B H 0.6138 0.1583 0.5309 0.128 Uiso 1 1 calc R . .
H56C H 0.6010 0.1986 0.4570 0.128 Uiso 1 1 calc R . .
C45 C 0.6142(2) 0.1884(3) 0.1432(2) 0.0888(13) Uani 1 1 d . . .
H45 H 0.6295 0.1684 0.1112 0.107 Uiso 1 1 calc R . .
C36 C 0.24513(18) 0.3320(3) 0.06911(18) 0.0864(13) Uani 1 1 d . . .
H36 H 0.2226 0.2734 0.0589 0.104 Uiso 1 1 calc R . .
C29 C 0.01650(17) 0.9324(2) 0.15311(18) 0.0717(10) Uani 1 1 d . . .
H29A H 0.0398 0.9356 0.2035 0.086 Uiso 1 1 calc R . .
H29B H -0.0289 0.9265 0.1418 0.086 Uiso 1 1 calc R . .
C60 C 0.3778(2) 0.2441(3) 0.4925(2) 0.1105(16) Uani 1 1 d . . .
H60A H 0.4231 0.2534 0.5206 0.166 Uiso 1 1 calc R . .
H60B H 0.3620 0.1948 0.5133 0.166 Uiso 1 1 calc R . .
H60C H 0.3555 0.3043 0.4898 0.166 Uiso 1 1 calc R . .
C25 C 0.16492(19) 0.7651(3) 0.1133(2) 0.0920(13) Uani 1 1 d . . .
H25A H 0.2102 0.7677 0.1453 0.110 Uiso 1 1 calc R . .
H25B H 0.1466 0.8286 0.1140 0.110 Uiso 1 1 calc R . .
C58 C 0.30051(19) 0.3960(3) 0.3399(2) 0.1083(16) Uani 1 1 d . . .
H58A H 0.2867 0.3713 0.2933 0.162 Uiso 1 1 calc R . .
H58B H 0.2912 0.4645 0.3380 0.162 Uiso 1 1 calc R . .
H58C H 0.2782 0.3622 0.3625 0.162 Uiso 1 1 calc R . .
C24 C 0.22812(19) 0.5805(3) 0.1981(2) 0.1108(16) Uani 1 1 d . . .
H24A H 0.2558 0.6227 0.1872 0.166 Uiso 1 1 calc R . .
H24B H 0.2412 0.5140 0.1983 0.166 Uiso 1 1 calc R . .
H24C H 0.2309 0.5970 0.2432 0.166 Uiso 1 1 calc R . .
C30 C 0.0270(3) 1.0272(3) 0.1226(2) 0.128(2) Uani 1 1 d . . .
H30A H 0.0714 1.0324 0.1311 0.192 Uiso 1 1 calc R . .
H30B H 0.0158 1.0812 0.1440 0.192 Uiso 1 1 calc R . .
H30C H 0.0004 1.0281 0.0732 0.192 Uiso 1 1 calc R . .
C26 C 0.1593(3) 0.7473(4) 0.0402(3) 0.156(3) Uani 1 1 d . . .
H26A H 0.1822 0.6889 0.0400 0.233 Uiso 1 1 calc R . .
H26B H 0.1774 0.8015 0.0262 0.233 Uiso 1 1 calc R . .
H26C H 0.1148 0.7401 0.0083 0.233 Uiso 1 1 calc R . .
C13 C -0.05320(16) 0.7717(2) 0.28814(16) 0.0540(8) Uani 1 1 d . . .
C34 C 0.2586(3) 0.4967(4) 0.0383(3) 0.1111(19) Uani 1 1 d . . .
H34 H 0.2440 0.5466 0.0055 0.133 Uiso 1 1 calc R . .
C35 C 0.2259(2) 0.4067(5) 0.0240(2) 0.1144(18) Uani 1 1 d . . .
H35 H 0.1898 0.3988 -0.0182 0.137 Uiso 1 1 calc R . .


_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 N6 1.910(3) . ?
Ti1 N5 1.912(3) . ?
Ti1 N4 2.123(3) . ?
Ti1 N2 2.148(3) . ?
Ti1 N1 2.236(3) . ?
Ti1 N3 2.277(2) . ?
N1 C7 1.344(3) . ?
N1 C1 1.373(4) . ?
N3 C18 1.341(3) . ?
N3 C12 1.377(4) . ?
N2 C11 1.363(4) . ?
N2 C8 1.390(4) . ?
C8 C9 1.383(4) . ?
C8 C7 1.439(4) . ?
N8 C18 1.372(4) . ?
N8 C17 1.395(4) . ?
N8 C13 1.426(4) . ?
N7 C7 1.363(4) . ?
N7 C6 1.402(4) . ?
N7 C2 1.416(4) . ?
N6 C29 1.477(4) . ?
N6 C27 1.485(4) . ?
N4 C22 1.362(4) . ?
N4 C19 1.392(4) . ?
C18 C19 1.442(4) . ?
C19 C20 1.384(4) . ?
C2 C1 1.377(4) . ?
C2 C3 1.420(4) . ?
C11 C10 1.383(4) . ?
C12 C13 1.377(4) . ?
N5 C23 1.474(4) . ?
N5 C25 1.478(4) . ?
C22 C21 1.380(4) . ?
C3 C4 1.356(5) . ?
C17 C16 1.345(5) . ?
C6 C5 1.347(5) . ?
C21 C20 1.407(4) . ?
C10 C9 1.396(5) . ?
C14 C15 1.354(5) . ?
C14 C13 1.425(4) . ?
C5 C4 1.414(5) . ?
C27 C28 1.527(4) . ?
C23 C24 1.509(5) . ?
C15 C16 1.430(5) . ?
Ti2 N14 1.912(3) . ?
Ti2 N13 1.916(3) . ?
Ti2 N12 2.121(3) . ?
Ti2 N10 2.135(3) . ?
Ti2 N9 2.252(3) . ?
Ti2 N11 2.279(3) . ?
N16 C48 1.371(4) . ?
N16 C47 1.397(4) . ?
N16 C43 1.420(4) . ?
N12 C52 1.369(4) . ?
N12 C49 1.393(4) . ?
N11 C48 1.342(4) . ?
N11 C42 1.379(4) . ?
N9 C37 1.341(4) . ?
N9 C31 1.376(4) . ?
N10 C41 1.365(4) . ?
N10 C38 1.388(4) . ?
C37 N15 1.369(4) . ?
C37 C38 1.439(5) . ?
C48 C49 1.444(4) . ?
N14 C53 1.470(4) . ?
N14 C55 1.479(4) . ?
N13 C59 1.473(4) . ?
N13 C57 1.480(4) . ?
N15 C36 1.405(4) . ?
N15 C32 1.406(4) . ?
C55 C56 1.538(4) . ?
C49 C50 1.380(4) . ?
C42 C43 1.367(4) . ?
C52 C51 1.379(5) . ?
C38 C39 1.393(4) . ?
C43 C44 1.426(5) . ?
C53 C54 1.530(4) . ?
C31 C32 1.382(4) . ?
C40 C41 1.379(5) . ?
C40 C39 1.399(5) . ?
C32 C33 1.430(5) . ?
C44 C45 1.360(5) . ?
C57 C58 1.519(5) . ?
C47 C46 1.345(5) . ?
C50 C51 1.406(5) . ?
C46 C45 1.432(5) . ?
C33 C34 1.367(6) . ?
C59 C60 1.503(5) . ?
C36 C35 1.341(6) . ?
C29 C30 1.518(5) . ?
C25 C26 1.519(6) . ?
C34 C35 1.409(7) . ?

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
N6 Ti1 N5 102.32(12) . . ?
N6 Ti1 N4 99.70(11) . . ?
N5 Ti1 N4 96.26(11) . . ?
N6 Ti1 N2 97.57(11) . . ?
N5 Ti1 N2 97.53(11) . . ?
N4 Ti1 N2 155.02(10) . . ?
N6 Ti1 N1 162.79(10) . . ?
N5 Ti1 N1 93.69(11) . . ?
N4 Ti1 N1 84.61(9) . . ?
N2 Ti1 N1 73.82(10) . . ?
N6 Ti1 N3 88.51(10) . . ?
N5 Ti1 N3 167.17(11) . . ?
N4 Ti1 N3 74.90(10) . . ?
N2 Ti1 N3 87.69(10) . . ?
N1 Ti1 N3 76.45(9) . . ?
C7 N1 C1 107.8(3) . . ?
C7 N1 Ti1 115.1(2) . . ?
C1 N1 Ti1 137.0(2) . . ?
C18 N3 C12 107.4(3) . . ?
C18 N3 Ti1 112.18(19) . . ?
C12 N3 Ti1 140.1(2) . . ?
C11 N2 C8 105.9(3) . . ?
C11 N2 Ti1 134.7(2) . . ?
C8 N2 Ti1 119.14(19) . . ?
C9 C8 N2 110.2(3) . . ?
C9 C8 C7 136.2(3) . . ?
N2 C8 C7 113.5(3) . . ?
C18 N8 C17 131.3(3) . . ?
C18 N8 C13 107.5(2) . . ?
C17 N8 C13 121.2(3) . . ?
C7 N7 C6 131.0(3) . . ?
C7 N7 C2 107.8(2) . . ?
C6 N7 C2 121.1(3) . . ?
C29 N6 C27 114.1(3) . . ?
C29 N6 Ti1 127.6(2) . . ?
C27 N6 Ti1 116.5(2) . . ?
C22 N4 C19 105.6(3) . . ?
C22 N4 Ti1 135.2(2) . . ?
C19 N4 Ti1 118.82(19) . . ?
N3 C18 N8 110.0(3) . . ?
N3 C18 C19 119.9(3) . . ?
N8 C18 C19 130.1(3) . . ?
C20 C19 N4 110.5(3) . . ?
C20 C19 C18 135.9(3) . . ?
N4 C19 C18 113.7(3) . . ?
C1 C2 N7 105.2(3) . . ?
C1 C2 C3 136.8(3) . . ?
N7 C2 C3 118.0(3) . . ?
N2 C11 C10 110.3(3) . . ?
N3 C12 C13 110.4(3) . . ?
C23 N5 C25 113.4(3) . . ?
C23 N5 Ti1 124.2(2) . . ?
C25 N5 Ti1 121.0(2) . . ?
N1 C1 C2 109.6(3) . . ?
N1 C7 N7 109.5(3) . . ?
N1 C7 C8 118.4(3) . . ?
N7 C7 C8 132.1(3) . . ?
N4 C22 C21 110.8(3) . . ?
C4 C3 C2 119.9(4) . . ?
C16 C17 N8 119.5(4) . . ?
C5 C6 N7 118.8(3) . . ?
C22 C21 C20 107.3(3) . . ?
C11 C10 C9 107.4(3) . . ?
C8 C9 C10 106.3(3) . . ?
C15 C14 C13 119.7(4) . . ?
C6 C5 C4 121.6(3) . . ?
C19 C20 C21 105.9(3) . . ?
N6 C27 C28 114.2(3) . . ?
C3 C4 C5 120.5(4) . . ?
N5 C23 C24 114.7(3) . . ?
C14 C15 C16 121.0(4) . . ?
C17 C16 C15 120.8(4) . . ?
N14 Ti2 N13 104.39(11) . . ?
N14 Ti2 N12 97.78(10) . . ?
N13 Ti2 N12 94.76(11) . . ?
N14 Ti2 N10 94.38(11) . . ?
N13 Ti2 N10 98.40(11) . . ?
N12 Ti2 N10 159.28(10) . . ?
N14 Ti2 N9 160.18(10) . . ?
N13 Ti2 N9 93.54(11) . . ?
N12 Ti2 N9 88.91(10) . . ?
N10 Ti2 N9 74.41(10) . . ?
N14 Ti2 N11 87.77(10) . . ?
N13 Ti2 N11 164.82(10) . . ?
N12 Ti2 N11 74.31(10) . . ?
N10 Ti2 N11 89.53(10) . . ?
N9 Ti2 N11 76.06(9) . . ?
C48 N16 C47 130.8(3) . . ?
C48 N16 C43 107.4(3) . . ?
C47 N16 C43 121.8(3) . . ?
C52 N12 C49 105.5(3) . . ?
C52 N12 Ti2 134.3(2) . . ?
C49 N12 Ti2 119.7(2) . . ?
C48 N11 C42 107.5(3) . . ?
C48 N11 Ti2 112.8(2) . . ?
C42 N11 Ti2 139.6(2) . . ?
C37 N9 C31 107.7(3) . . ?
C37 N9 Ti2 113.1(2) . . ?
C31 N9 Ti2 139.1(2) . . ?
C41 N10 C38 105.3(3) . . ?
C41 N10 Ti2 135.1(2) . . ?
C38 N10 Ti2 119.5(2) . . ?
N9 C37 N15 109.5(3) . . ?
N9 C37 C38 120.3(3) . . ?
N15 C37 C38 130.1(3) . . ?
N11 C48 N16 109.7(3) . . ?
N11 C48 C49 119.6(3) . . ?
N16 C48 C49 130.7(3) . . ?
C53 N14 C55 114.3(2) . . ?
C53 N14 Ti2 125.1(2) . . ?
C55 N14 Ti2 118.2(2) . . ?
C59 N13 C57 113.6(3) . . ?
C59 N13 Ti2 122.5(2) . . ?
C57 N13 Ti2 122.9(2) . . ?
C37 N15 C36 130.0(4) . . ?
C37 N15 C32 108.0(3) . . ?
C36 N15 C32 122.0(3) . . ?
N14 C55 C56 114.6(3) . . ?
C50 C49 N12 110.3(3) . . ?
C50 C49 C48 136.3(3) . . ?
N12 C49 C48 113.3(3) . . ?
C43 C42 N11 110.0(3) . . ?
N12 C52 C51 110.8(3) . . ?
N10 C38 C39 110.0(3) . . ?
N10 C38 C37 112.7(3) . . ?
C39 C38 C37 137.1(3) . . ?
C42 C43 N16 105.4(3) . . ?
C42 C43 C44 136.9(4) . . ?
N16 C43 C44 117.7(3) . . ?
N14 C53 C54 115.5(3) . . ?
N9 C31 C32 109.5(3) . . ?
C41 C40 C39 106.4(3) . . ?
C31 C32 N15 105.3(3) . . ?
C31 C32 C33 136.8(4) . . ?
N15 C32 C33 117.9(4) . . ?
C45 C44 C43 119.8(4) . . ?
N10 C41 C40 111.6(3) . . ?
N13 C57 C58 114.0(3) . . ?
C38 C39 C40 106.7(3) . . ?
C46 C47 N16 119.0(4) . . ?
C49 C50 C51 106.4(3) . . ?
C52 C51 C50 107.0(3) . . ?
C47 C46 C45 121.2(4) . . ?
C34 C33 C32 119.1(5) . . ?
N13 C59 C60 116.3(3) . . ?
C44 C45 C46 120.6(4) . . ?
C35 C36 N15 118.1(5) . . ?
N6 C29 C30 114.8(3) . . ?
N5 C25 C26 115.7(4) . . ?
C12 C13 N8 104.8(3) . . ?
C12 C13 C14 137.3(3) . . ?
N8 C13 C14 117.9(3) . . ?
C33 C34 C35 120.7(5) . . ?
C36 C35 C34 122.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        26.22
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.249
_refine_diff_density_rms         0.043
