# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_clampti
_database_code_depnum_ccdc_archive 'CCDC 1845533'
_audit_update_record             
;
2018-05-27 deposited with the CCDC.
2018-12-26 downloaded from the CCDC.
;

# Collected as sb1304

# start Validation Reply Form
_vrf_PLAT413_clampti             
;
PROBLEM: Short Inter XH3 .. XHn     H43A     ..H82E             1.82 Ang.  
RESPONSE: H82E is on the methyl group of a disordered lattice CH3CN
and so its location is not well fixed.
;
# end Validation Reply Form

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
'κ6-[Tris(2-(3,5-di-tert-butyl-2-oxyphenyl)amido-4-methylphenyl)amino]titanium(IV) diacetonitrile solvate'
_chemical_name_common            '(MeClamp)Ti . 2 CH3CN'
_chemical_melting_point          ?
_chemical_formula_moiety         'C63 H78 N4 O3 Ti, 2 (C2 H3 N)'
_chemical_formula_sum            'C67 H84 N6 O3 Ti'
_chemical_formula_weight         1069.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Pbca

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

_cell_length_a                   22.8836(6)
_cell_length_b                   12.2462(3)
_cell_length_c                   45.2221(12)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     12672.9(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    120(2)
_cell_measurement_reflns_used    9395
_cell_measurement_theta_min      3.86
_cell_measurement_theta_max      71.43

_exptl_crystal_description       tablet
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      .
_exptl_crystal_density_diffrn    1.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4592
_exptl_absorpt_coefficient_mu    1.511
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7095
_exptl_absorpt_correction_T_max  0.8926
_exptl_absorpt_process_details   
;
Blessing, R. H. (1995) Acta Cryst. A51, 33-38.

Sheldrick, G.M. (2008) SADABS v2008/1. Bruker AXS Inc. 
Madison, WI USA.
;

_exptl_crystal_recrystallization_method 
'Crystals were grown by dissolving the compound as a crude oil in CH3CNand allowing the CH3CN solution to stand at room temperature.'

_exptl_special_details           
;
 Crystals were mounted in a mixture of DuPont Krytox GPL 105 PFPE lubricant and 
DuPont Krytox GPL205 grease.
;

_diffrn_ambient_temperature      120(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean 8.33
_diffrn_reflns_number            180382
_diffrn_reflns_av_R_equivalents  0.0439
_diffrn_reflns_av_sigmaI/netI    0.0169
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_limit_l_max       55
_diffrn_reflns_theta_min         1.95
_diffrn_reflns_theta_max         71.53
_reflns_number_total             12331
_reflns_number_gt                11853
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_cell_refinement       'APEX2/SAINT (Bruker, 2004; Sheldrick, 2003)'
_computing_data_reduction        SAINT/XPREP
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    'XP (Sheldrick, 1998)'
_computing_publication_material  'XCIF (Sheldrick, 2001)'

_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.

 Amidophenoxide ring 1 was disordered in two different orientations (probably
 driven by the disorder of the tert-butyl group centered at C18, which is
 in two different orientations in the two ring orientations).  All thermal
 parameters of the corresponding atoms in the two orientations were fixed as
 equal, and their occupancies were allowed to refine, giving 57.8(2)% 
 occupancy for the main orientation.  No disorder was apparent for C11, and 
 the two sites for C173 were so close that the refinement was only stable if
 their coordinates were fixed as equal.

 One of the acetonitriles of solvation was discerned in three different 
 orientations.  Thermal parameters of the corresponding atoms were fixed as
 equal and the sum of the occupancy factors constrained to 1.00; occupancies
 refined to 67.1(3), 23.7(5), and 9.2(5)%. 
;

_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)+(0.0596P)²+6.3429P] 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         12331
_refine_ls_number_parameters     750
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0406
_refine_ls_wR_factor_ref         0.1118
_refine_ls_wR_factor_gt          0.1106
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.039
_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
Ti Ti 0.452740(10) 0.636921(19) 0.114138(5) 0.01779(7) Uani 1 1 d . A .
O1 O 0.52482(4) 0.64100(8) 0.13939(2) 0.0250(2) Uani 1 1 d . A .
O2 O 0.42116(4) 0.74300(7) 0.14270(2) 0.0225(2) Uani 1 1 d . A .
O3 O 0.47387(4) 0.75502(8) 0.08922(2) 0.02087(19) Uani 1 1 d . A .
N N 0.40413(5) 0.43340(9) 0.09782(2) 0.0204(2) Uani 1 1 d . A .
N1 N 0.50860(5) 0.51525(10) 0.09627(2) 0.0209(2) Uani 1 1 d . . .
N2 N 0.41587(5) 0.53957(9) 0.14818(2) 0.0187(2) Uani 1 1 d . . .
N3 N 0.38259(5) 0.64365(9) 0.08528(2) 0.0179(2) Uani 1 1 d . . .
C11 C 0.56227(6) 0.56195(15) 0.13765(3) 0.0304(3) Uani 1 1 d . . .
C12 C 0.5566(6) 0.5006(6) 0.1120(3) 0.0191(12) Uani 0.578(2) 1 d P A 1
C13 C 0.5985(3) 0.4149(3) 0.10824(14) 0.0279(9) Uani 0.578(2) 1 d P A 1
H13A H 0.5947 0.3658 0.0921 0.033 Uiso 0.578(2) 1 calc PR A 1
C14 C 0.64436(15) 0.4031(3) 0.12782(8) 0.0333(7) Uani 0.578(2) 1 d P A 1
C15 C 0.64808(16) 0.4745(3) 0.15262(8) 0.0335(7) Uani 0.578(2) 1 d P A 1
H15A H 0.6796 0.4647 0.1661 0.040 Uiso 0.578(2) 1 calc PR A 1
C16 C 0.6086(3) 0.5569(4) 0.15821(17) 0.0269(10) Uani 0.578(2) 1 d P A 1
C17 C 0.6125(6) 0.6289(7) 0.1869(3) 0.0337(17) Uani 0.578(2) 1 d P A 1
C171 C 0.6633(6) 0.5969(6) 0.2060(3) 0.052(2) Uani 0.578(2) 1 d P A 1
H17A H 0.6998 0.6122 0.1955 0.078 Uiso 0.578(2) 1 calc PR A 1
H17B H 0.6610 0.5188 0.2105 0.078 Uiso 0.578(2) 1 calc PR A 1
H17C H 0.6622 0.6389 0.2244 0.078 Uiso 0.578(2) 1 calc PR A 1
C172 C 0.6183(3) 0.7489(5) 0.17748(17) 0.0422(12) Uani 0.578(2) 1 d P A 1
H17D H 0.6559 0.7599 0.1676 0.063 Uiso 0.578(2) 1 calc PR A 1
H17E H 0.6161 0.7960 0.1950 0.063 Uiso 0.578(2) 1 calc PR A 1
H17F H 0.5865 0.7676 0.1639 0.063 Uiso 0.578(2) 1 calc PR A 1
C173 C 0.55511(8) 0.60941(17) 0.20460(4) 0.0397(4) Uani 0.578(2) 1 d P A 1
H17G H 0.5215 0.6300 0.1924 0.060 Uiso 0.578(2) 1 calc PR A 1
H17H H 0.5555 0.6539 0.2226 0.060 Uiso 0.578(2) 1 calc PR A 1
H17I H 0.5521 0.5321 0.2100 0.060 Uiso 0.578(2) 1 calc PR A 1
C18 C 0.69145(15) 0.3144(3) 0.12409(7) 0.0461(7) Uani 0.578(2) 1 d P A 1
C181 C 0.6813(7) 0.2423(10) 0.0976(3) 0.070(3) Uani 0.578(2) 1 d P A 1
H18A H 0.7125 0.1877 0.0963 0.105 Uiso 0.578(2) 1 calc PR A 1
H18B H 0.6813 0.2870 0.0796 0.105 Uiso 0.578(2) 1 calc PR A 1
H18C H 0.6435 0.2055 0.0995 0.105 Uiso 0.578(2) 1 calc PR A 1
C182 C 0.75096(17) 0.3697(4) 0.12112(10) 0.0683(10) Uani 0.578(2) 1 d P A 1
H18D H 0.7813 0.3139 0.1188 0.102 Uiso 0.578(2) 1 calc PR A 1
H18E H 0.7589 0.4129 0.1389 0.102 Uiso 0.578(2) 1 calc PR A 1
H18F H 0.7508 0.4176 0.1038 0.102 Uiso 0.578(2) 1 calc PR A 1
C183 C 0.6914(2) 0.2400(4) 0.15150(9) 0.0640(9) Uani 0.578(2) 1 d P A 1
H18G H 0.7214 0.1836 0.1493 0.096 Uiso 0.578(2) 1 calc PR A 1
H18H H 0.6530 0.2054 0.1535 0.096 Uiso 0.578(2) 1 calc PR A 1
H18I H 0.6997 0.2837 0.1692 0.096 Uiso 0.578(2) 1 calc PR A 1
C12A C 0.5545(8) 0.4736(9) 0.1139(4) 0.0191(12) Uani 0.422(2) 1 d P A 2
C13A C 0.5880(4) 0.3801(5) 0.1098(2) 0.0279(9) Uani 0.422(2) 1 d P A 2
H13B H 0.5824 0.3345 0.0931 0.033 Uiso 0.422(2) 1 calc PR A 2
C14A C 0.6289(2) 0.3564(4) 0.13067(11) 0.0333(7) Uani 0.422(2) 1 d P A 2
C15A C 0.6356(2) 0.4277(5) 0.15533(12) 0.0335(7) Uani 0.422(2) 1 d P A 2
H15B H 0.6643 0.4087 0.1696 0.040 Uiso 0.422(2) 1 calc PR A 2
C16A C 0.6042(5) 0.5217(6) 0.1604(2) 0.0269(10) Uani 0.422(2) 1 d P A 2
C17A C 0.6106(9) 0.5983(12) 0.1855(5) 0.0337(17) Uani 0.422(2) 1 d P A 2
C174 C 0.6605(8) 0.5568(9) 0.2074(4) 0.052(2) Uani 0.422(2) 1 d P A 2
H17J H 0.6507 0.4834 0.2144 0.078 Uiso 0.422(2) 1 calc PR A 2
H17K H 0.6634 0.6067 0.2242 0.078 Uiso 0.422(2) 1 calc PR A 2
H17L H 0.6979 0.5547 0.1968 0.078 Uiso 0.422(2) 1 calc PR A 2
C175 C 0.6285(5) 0.7134(7) 0.1761(3) 0.0422(12) Uani 0.422(2) 1 d P A 2
H17M H 0.5984 0.7441 0.1631 0.063 Uiso 0.422(2) 1 calc PR A 2
H17N H 0.6658 0.7103 0.1655 0.063 Uiso 0.422(2) 1 calc PR A 2
H17O H 0.6327 0.7596 0.1937 0.063 Uiso 0.422(2) 1 calc PR A 2
C176 C 0.55511(8) 0.60941(17) 0.20460(4) 0.0397(4) Uani 0.422(2) 1 d P A 2
H17P H 0.5626 0.6604 0.2209 0.060 Uiso 0.422(2) 1 calc PR A 2
H17Q H 0.5445 0.5378 0.2127 0.060 Uiso 0.422(2) 1 calc PR A 2
H17R H 0.5230 0.6371 0.1924 0.060 Uiso 0.422(2) 1 calc PR A 2
C18A C 0.6646(2) 0.2500(4) 0.12903(10) 0.0461(7) Uani 0.422(2) 1 d P A 2
C184 C 0.6672(9) 0.2081(15) 0.0966(5) 0.070(3) Uani 0.422(2) 1 d P A 2
H18J H 0.6877 0.2617 0.0843 0.105 Uiso 0.422(2) 1 calc PR A 2
H18K H 0.6274 0.1979 0.0891 0.105 Uiso 0.422(2) 1 calc PR A 2
H18L H 0.6882 0.1383 0.0960 0.105 Uiso 0.422(2) 1 calc PR A 2
C185 C 0.7244(2) 0.2624(6) 0.14258(14) 0.0683(10) Uani 0.422(2) 1 d P A 2
H18M H 0.7465 0.3177 0.1316 0.102 Uiso 0.422(2) 1 calc PR A 2
H18N H 0.7451 0.1924 0.1416 0.102 Uiso 0.422(2) 1 calc PR A 2
H18O H 0.7205 0.2850 0.1633 0.102 Uiso 0.422(2) 1 calc PR A 2
C186 C 0.6320(3) 0.1598(5) 0.14717(12) 0.0640(9) Uani 0.422(2) 1 d P A 2
H18P H 0.6300 0.1816 0.1680 0.096 Uiso 0.422(2) 1 calc PR A 2
H18Q H 0.6531 0.0905 0.1455 0.096 Uiso 0.422(2) 1 calc PR A 2
H18R H 0.5923 0.1509 0.1394 0.096 Uiso 0.422(2) 1 calc PR A 2
C21 C 0.40251(6) 0.71057(11) 0.16874(3) 0.0208(3) Uani 1 1 d . . .
C22 C 0.39629(6) 0.59519(11) 0.17235(3) 0.0200(3) Uani 1 1 d . A .
C23 C 0.37204(6) 0.55143(12) 0.19837(3) 0.0235(3) Uani 1 1 d . . .
H23A H 0.3653 0.4751 0.2000 0.028 Uiso 1 1 calc R A .
C24 C 0.35805(6) 0.62024(13) 0.22154(3) 0.0263(3) Uani 1 1 d . A .
C25 C 0.36908(6) 0.73305(12) 0.21831(3) 0.0272(3) Uani 1 1 d . . .
H25A H 0.3610 0.7791 0.2347 0.033 Uiso 1 1 calc R A .
C26 C 0.39093(6) 0.78113(11) 0.19289(3) 0.0243(3) Uani 1 1 d . A .
C27 C 0.40555(7) 0.90291(12) 0.19071(3) 0.0310(3) Uani 1 1 d . . .
C271 C 0.47119(8) 0.91476(13) 0.18427(4) 0.0385(4) Uani 1 1 d . A .
H27A H 0.4937 0.8804 0.2002 0.058 Uiso 1 1 calc R . .
H27B H 0.4813 0.9924 0.1831 0.058 Uiso 1 1 calc R . .
H27C H 0.4804 0.8791 0.1654 0.058 Uiso 1 1 calc R . .
C272 C 0.39195(9) 0.96326(14) 0.21969(4) 0.0430(4) Uani 1 1 d . A .
H27D H 0.4142 0.9302 0.2359 0.064 Uiso 1 1 calc R . .
H27E H 0.3501 0.9578 0.2240 0.064 Uiso 1 1 calc R . .
H27F H 0.4029 1.0403 0.2177 0.064 Uiso 1 1 calc R . .
C273 C 0.37003(9) 0.95652(13) 0.16584(4) 0.0432(4) Uani 1 1 d . A .
H27G H 0.3782 0.9193 0.1471 0.065 Uiso 1 1 calc R . .
H27H H 0.3809 1.0337 0.1642 0.065 Uiso 1 1 calc R . .
H27I H 0.3283 0.9508 0.1704 0.065 Uiso 1 1 calc R . .
C28 C 0.33376(7) 0.57133(15) 0.25022(3) 0.0353(4) Uani 1 1 d . . .
C281 C 0.38025(10) 0.4957(2) 0.26360(4) 0.0565(6) Uani 1 1 d . A .
H28A H 0.4156 0.5379 0.2680 0.085 Uiso 1 1 calc R . .
H28B H 0.3896 0.4376 0.2495 0.085 Uiso 1 1 calc R . .
H28C H 0.3652 0.4634 0.2819 0.085 Uiso 1 1 calc R . .
C282 C 0.27820(8) 0.50553(17) 0.24341(4) 0.0459(4) Uani 1 1 d . A .
H28D H 0.2486 0.5540 0.2349 0.069 Uiso 1 1 calc R . .
H28E H 0.2631 0.4733 0.2617 0.069 Uiso 1 1 calc R . .
H28F H 0.2875 0.4473 0.2293 0.069 Uiso 1 1 calc R . .
C283 C 0.31835(10) 0.65899(19) 0.27302(4) 0.0537(5) Uani 1 1 d . A .
H28G H 0.2886 0.7079 0.2648 0.081 Uiso 1 1 calc R . .
H28H H 0.3534 0.7011 0.2779 0.081 Uiso 1 1 calc R . .
H28I H 0.3031 0.6241 0.2909 0.081 Uiso 1 1 calc R . .
C31 C 0.43474(6) 0.79759(11) 0.07055(3) 0.0188(2) Uani 1 1 d . . .
C32 C 0.38286(6) 0.73559(10) 0.06711(3) 0.0185(2) Uani 1 1 d . A .
C33 C 0.34122(6) 0.76867(11) 0.04617(3) 0.0215(3) Uani 1 1 d . . .
H33A H 0.3076 0.7249 0.0427 0.026 Uiso 1 1 calc R A .
C34 C 0.34891(6) 0.86497(11) 0.03048(3) 0.0234(3) Uani 1 1 d . A .
C35 C 0.39990(6) 0.92646(11) 0.03524(3) 0.0235(3) Uani 1 1 d . . .
H35A H 0.4047 0.9925 0.0245 0.028 Uiso 1 1 calc R A .
C36 C 0.44367(6) 0.89554(11) 0.05491(3) 0.0210(3) Uani 1 1 d . A .
C37 C 0.49908(6) 0.96352(11) 0.06014(3) 0.0255(3) Uani 1 1 d . . .
C371 C 0.50550(7) 0.98924(12) 0.09326(3) 0.0306(3) Uani 1 1 d . A .
H37A H 0.4713 1.0305 0.1000 0.046 Uiso 1 1 calc R . .
H37B H 0.5409 1.0327 0.0964 0.046 Uiso 1 1 calc R . .
H37C H 0.5084 0.9209 0.1044 0.046 Uiso 1 1 calc R . .
C372 C 0.49737(8) 1.07293(13) 0.04359(4) 0.0358(4) Uani 1 1 d . A .
H37D H 0.4636 1.1154 0.0503 0.054 Uiso 1 1 calc R . .
H37E H 0.4942 1.0594 0.0223 0.054 Uiso 1 1 calc R . .
H37F H 0.5333 1.1138 0.0477 0.054 Uiso 1 1 calc R . .
C373 C 0.55257(7) 0.89851(14) 0.04940(4) 0.0351(4) Uani 1 1 d . A .
H37G H 0.5483 0.8822 0.0283 0.053 Uiso 1 1 calc R . .
H37H H 0.5554 0.8301 0.0605 0.053 Uiso 1 1 calc R . .
H37I H 0.5880 0.9418 0.0525 0.053 Uiso 1 1 calc R . .
C38 C 0.30316(7) 0.90147(13) 0.00759(3) 0.0293(3) Uani 1 1 d . . .
C381 C 0.31830(11) 0.8516(2) -0.02183(4) 0.0662(7) Uani 1 1 d . A .
H38A H 0.3185 0.7719 -0.0201 0.099 Uiso 1 1 calc R . .
H38B H 0.3571 0.8768 -0.0280 0.099 Uiso 1 1 calc R . .
H38C H 0.2892 0.8737 -0.0366 0.099 Uiso 1 1 calc R . .
C382 C 0.30322(10) 1.02720(18) 0.00390(5) 0.0567(5) Uani 1 1 d . A .
H38D H 0.2738 1.0482 -0.0108 0.085 Uiso 1 1 calc R . .
H38E H 0.3419 1.0513 -0.0028 0.085 Uiso 1 1 calc R . .
H38F H 0.2940 1.0617 0.0229 0.085 Uiso 1 1 calc R . .
C383 C 0.24177(8) 0.87183(18) 0.01756(4) 0.0497(5) Uani 1 1 d . A .
H38G H 0.2390 0.7926 0.0202 0.074 Uiso 1 1 calc R . .
H38H H 0.2136 0.8953 0.0025 0.074 Uiso 1 1 calc R . .
H38I H 0.2332 0.9085 0.0363 0.074 Uiso 1 1 calc R . .
C41 C 0.43496(6) 0.41770(11) 0.07074(3) 0.0203(3) Uani 1 1 d . . .
C42 C 0.49299(6) 0.45318(11) 0.07115(3) 0.0213(3) Uani 1 1 d . A .
C43 C 0.52915(6) 0.43126(12) 0.04696(3) 0.0248(3) Uani 1 1 d . . .
H43A H 0.5691 0.4524 0.0475 0.030 Uiso 1 1 calc R A .
C44 C 0.50684(7) 0.37848(12) 0.02206(3) 0.0254(3) Uani 1 1 d . A .
C45 C 0.44777(7) 0.34950(12) 0.02160(3) 0.0263(3) Uani 1 1 d . . .
H45A H 0.4320 0.3163 0.0044 0.032 Uiso 1 1 calc R A .
C46 C 0.41168(6) 0.36816(11) 0.04573(3) 0.0239(3) Uani 1 1 d . A .
H46A H 0.3717 0.3474 0.0452 0.029 Uiso 1 1 calc R . .
C47 C 0.54600(7) 0.35325(14) -0.00395(3) 0.0326(3) Uani 1 1 d . . .
H47A H 0.5815 0.3977 -0.0027 0.049 Uiso 1 1 calc R A .
H47B H 0.5254 0.3700 -0.0224 0.049 Uiso 1 1 calc R . .
H47C H 0.5565 0.2757 -0.0037 0.049 Uiso 1 1 calc R . .
C51 C 0.42471(6) 0.37177(11) 0.12254(3) 0.0194(3) Uani 1 1 d . . .
C52 C 0.42884(6) 0.42889(11) 0.14949(3) 0.0193(3) Uani 1 1 d . A .
C53 C 0.45431(6) 0.37757(11) 0.17394(3) 0.0226(3) Uani 1 1 d . . .
H53A H 0.4566 0.4155 0.1922 0.027 Uiso 1 1 calc R A .
C54 C 0.47627(7) 0.27243(12) 0.17199(3) 0.0273(3) Uani 1 1 d . A .
C55 C 0.47162(7) 0.21714(12) 0.14500(3) 0.0285(3) Uani 1 1 d . . .
H55A H 0.4858 0.1445 0.1435 0.034 Uiso 1 1 calc R A .
C56 C 0.44664(6) 0.26647(12) 0.12037(3) 0.0239(3) Uani 1 1 d . A .
H56A H 0.4446 0.2282 0.1021 0.029 Uiso 1 1 calc R . .
C57 C 0.50592(9) 0.22222(13) 0.19852(4) 0.0414(4) Uani 1 1 d . . .
H57A H 0.5291 0.2780 0.2087 0.062 Uiso 1 1 calc R A .
H57B H 0.5316 0.1628 0.1920 0.062 Uiso 1 1 calc R . .
H57C H 0.4763 0.1933 0.2121 0.062 Uiso 1 1 calc R . .
C61 C 0.34449(6) 0.46730(11) 0.09686(3) 0.0180(2) Uani 1 1 d . . .
C62 C 0.33357(6) 0.57676(11) 0.08875(3) 0.0177(2) Uani 1 1 d . A .
C63 C 0.27502(6) 0.61121(11) 0.08780(3) 0.0195(3) Uani 1 1 d . . .
H63A H 0.2665 0.6845 0.0824 0.023 Uiso 1 1 calc R A .
C64 C 0.22916(6) 0.54050(11) 0.09457(3) 0.0214(3) Uani 1 1 d . A .
C65 C 0.24160(6) 0.43324(11) 0.10289(3) 0.0238(3) Uani 1 1 d . . .
H65A H 0.2106 0.3846 0.1076 0.029 Uiso 1 1 calc R A .
C66 C 0.29909(6) 0.39737(11) 0.10425(3) 0.0221(3) Uani 1 1 d . A .
H66A H 0.3074 0.3247 0.1103 0.027 Uiso 1 1 calc R . .
C67 C 0.16683(6) 0.58055(13) 0.09338(3) 0.0274(3) Uani 1 1 d . . .
H67A H 0.1635 0.6386 0.0786 0.041 Uiso 1 1 calc R A .
H67B H 0.1555 0.6092 0.1128 0.041 Uiso 1 1 calc R . .
H67C H 0.1410 0.5199 0.0880 0.041 Uiso 1 1 calc R . .
N7 N 0.33304(11) 0.24987(18) 0.20813(7) 0.0861(8) Uani 1 1 d . . .
C71 C 0.29982(10) 0.22675(16) 0.19011(6) 0.0567(6) Uani 1 1 d . . .
C72 C 0.25833(10) 0.1959(2) 0.16775(5) 0.0579(5) Uani 1 1 d . . .
H72A H 0.2783 0.1549 0.1521 0.087 Uiso 1 1 calc R . .
H72B H 0.2405 0.2617 0.1593 0.087 Uiso 1 1 calc R . .
H72C H 0.2278 0.1502 0.1766 0.087 Uiso 1 1 calc R . .
N8A N 0.6968(4) 0.4886(6) 0.0582(2) 0.196(4) Uani 0.671(3) 1 d P B 1
C81A C 0.6746(2) 0.5669(5) 0.06463(16) 0.112(2) Uani 0.671(3) 1 d P B 1
C82A C 0.6488(2) 0.6622(4) 0.07465(14) 0.117(2) Uani 0.671(3) 1 d P B 1
H82A H 0.6075 0.6630 0.0689 0.176 Uiso 0.671(3) 1 calc PR B 1
H82B H 0.6687 0.7253 0.0659 0.176 Uiso 0.671(3) 1 calc PR B 1
H82C H 0.6518 0.6658 0.0962 0.176 Uiso 0.671(3) 1 calc PR B 1
N8B N 0.6439(9) 0.7435(17) 0.0944(6) 0.196(4) Uani 0.237(5) 1 d P C 2
C81B C 0.6488(2) 0.6622(4) 0.07465(14) 0.112(2) Uani 0.237(5) 1 d P C 2
C82B C 0.6498(6) 0.6236(13) 0.0486(4) 0.117(2) Uani 0.237(5) 1 d P C 2
H82D H 0.6375 0.6800 0.0346 0.176 Uiso 0.237(5) 1 calc PR C 2
H82E H 0.6230 0.5612 0.0474 0.176 Uiso 0.237(5) 1 calc PR C 2
H82F H 0.6895 0.5996 0.0438 0.176 Uiso 0.237(5) 1 calc PR C 2
N8C N 0.6498(6) 0.6236(13) 0.0486(4) 0.196(4) Uani 0.092(5) 1 d P D 3
C81C C 0.6746(2) 0.5669(5) 0.06463(16) 0.112(2) Uani 0.092(5) 1 d P D 3
C82C C 0.726(2) 0.497(4) 0.0824(13) 0.117(2) Uani 0.092(5) 1 d P D 3
H82G H 0.7616 0.4965 0.0707 0.176 Uiso 0.092(5) 1 calc PR D 3
H82H H 0.7122 0.4215 0.0853 0.176 Uiso 0.092(5) 1 calc PR D 3
H82I H 0.7331 0.5306 0.1016 0.176 Uiso 0.092(5) 1 calc PR D 3


_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
Ti O3 1.8961(9) . ?
Ti O2 1.9693(10) . ?
Ti O1 2.0069(10) . ?
Ti N3 2.0704(11) . ?
Ti N2 2.1219(11) . ?
Ti N1 2.1231(12) . ?
Ti N 2.8274(12) . ?
O1 C11 1.2952(19) . ?
O2 C21 1.3141(16) . ?
O3 C31 1.3367(16) . ?
N C41 1.4263(16) . ?
N C61 1.4273(17) . ?
N C51 1.4286(17) . ?
N1 C12 1.321(13) . ?
N1 C42 1.4127(17) . ?
N1 C12A 1.415(18) . ?
N2 C22 1.3637(17) . ?
N2 C52 1.3889(17) . ?
N3 C32 1.3938(17) . ?
N3 C62 1.3980(17) . ?
C11 C12 1.388(13) . ?
C11 C16 1.412(8) . ?
C11 C16A 1.491(11) . ?
C11 C12A 1.533(18) . ?
C12 C13 1.431(13) . ?
C13 C14 1.381(7) . ?
C13 H13A 0.9500 . ?
C14 C15 1.425(5) . ?
C14 C18 1.539(4) . ?
C15 C16 1.378(8) . ?
C15 H15A 0.9500 . ?
C16 C17 1.572(12) . ?
C17 C171 1.499(19) . ?
C17 C172 1.537(12) . ?
C17 C173 1.556(16) . ?
C171 H17A 0.9800 . ?
C171 H17B 0.9800 . ?
C171 H17C 0.9800 . ?
C172 H17D 0.9800 . ?
C172 H17E 0.9800 . ?
C172 H17F 0.9800 . ?
C173 H17G 0.9800 . ?
C173 H17H 0.9800 . ?
C173 H17I 0.9800 . ?
C18 C181 1.507(11) . ?
C18 C182 1.527(6) . ?
C18 C183 1.538(5) . ?
C181 H18A 0.9800 . ?
C181 H18B 0.9800 . ?
C181 H18C 0.9800 . ?
C182 H18D 0.9800 . ?
C182 H18E 0.9800 . ?
C182 H18F 0.9800 . ?
C183 H18G 0.9800 . ?
C183 H18H 0.9800 . ?
C183 H18I 0.9800 . ?
C12A C13A 1.390(18) . ?
C13A C14A 1.361(11) . ?
C13A H13B 0.9500 . ?
C14A C15A 1.425(8) . ?
C14A C18A 1.541(6) . ?
C15A C16A 1.376(12) . ?
C15A H15B 0.9500 . ?
C16A C17A 1.479(18) . ?
C17A C175 1.527(18) . ?
C17A C174 1.59(3) . ?
C174 H17J 0.9800 . ?
C174 H17K 0.9800 . ?
C174 H17L 0.9800 . ?
C175 H17M 0.9800 . ?
C175 H17N 0.9800 . ?
C175 H17O 0.9800 . ?
C18A C185 1.507(7) . ?
C18A C184 1.55(2) . ?
C18A C186 1.566(8) . ?
C184 H18J 0.9800 . ?
C184 H18K 0.9800 . ?
C184 H18L 0.9800 . ?
C185 H18M 0.9800 . ?
C185 H18N 0.9800 . ?
C185 H18O 0.9800 . ?
C186 H18P 0.9800 . ?
C186 H18Q 0.9800 . ?
C186 H18R 0.9800 . ?
C21 C26 1.4177(18) . ?
C21 C22 1.4295(19) . ?
C22 C23 1.4072(19) . ?
C23 C24 1.382(2) . ?
C23 H23A 0.9500 . ?
C24 C25 1.412(2) . ?
C24 C28 1.533(2) . ?
C25 C26 1.385(2) . ?
C25 H25A 0.9500 . ?
C26 C27 1.532(2) . ?
C27 C273 1.535(2) . ?
C27 C272 1.536(2) . ?
C27 C271 1.537(2) . ?
C271 H27A 0.9800 . ?
C271 H27B 0.9800 . ?
C271 H27C 0.9800 . ?
C272 H27D 0.9800 . ?
C272 H27E 0.9800 . ?
C272 H27F 0.9800 . ?
C273 H27G 0.9800 . ?
C273 H27H 0.9800 . ?
C273 H27I 0.9800 . ?
C28 C283 1.530(2) . ?
C28 C281 1.535(3) . ?
C28 C282 1.536(2) . ?
C281 H28A 0.9800 . ?
C281 H28B 0.9800 . ?
C281 H28C 0.9800 . ?
C282 H28D 0.9800 . ?
C282 H28E 0.9800 . ?
C282 H28F 0.9800 . ?
C283 H28G 0.9800 . ?
C283 H28H 0.9800 . ?
C283 H28I 0.9800 . ?
C31 C36 1.4075(19) . ?
C31 C32 1.4178(18) . ?
C32 C33 1.4031(18) . ?
C33 C34 1.3874(19) . ?
C33 H33A 0.9500 . ?
C34 C35 1.405(2) . ?
C34 C38 1.5388(19) . ?
C35 C36 1.392(2) . ?
C35 H35A 0.9500 . ?
C36 C37 1.5353(19) . ?
C37 C372 1.535(2) . ?
C37 C371 1.538(2) . ?
C37 C373 1.539(2) . ?
C371 H37A 0.9800 . ?
C371 H37B 0.9800 . ?
C371 H37C 0.9800 . ?
C372 H37D 0.9800 . ?
C372 H37E 0.9800 . ?
C372 H37F 0.9800 . ?
C373 H37G 0.9800 . ?
C373 H37H 0.9800 . ?
C373 H37I 0.9800 . ?
C38 C381 1.504(2) . ?
C38 C383 1.519(2) . ?
C38 C382 1.549(3) . ?
C381 H38A 0.9800 . ?
C381 H38B 0.9800 . ?
C381 H38C 0.9800 . ?
C382 H38D 0.9800 . ?
C382 H38E 0.9800 . ?
C382 H38F 0.9800 . ?
C383 H38G 0.9800 . ?
C383 H38H 0.9800 . ?
C383 H38I 0.9800 . ?
C41 C46 1.3897(19) . ?
C41 C42 1.3974(19) . ?
C42 C43 1.3977(19) . ?
C43 C44 1.395(2) . ?
C43 H43A 0.9500 . ?
C44 C45 1.398(2) . ?
C44 C47 1.5105(19) . ?
C45 C46 1.387(2) . ?
C45 H45A 0.9500 . ?
C46 H46A 0.9500 . ?
C47 H47A 0.9800 . ?
C47 H47B 0.9800 . ?
C47 H47C 0.9800 . ?
C51 C56 1.3872(19) . ?
C51 C52 1.4084(18) . ?
C52 C53 1.3991(19) . ?
C53 C54 1.385(2) . ?
C53 H53A 0.9500 . ?
C54 C55 1.400(2) . ?
C54 C57 1.509(2) . ?
C55 C56 1.390(2) . ?
C55 H55A 0.9500 . ?
C56 H56A 0.9500 . ?
C57 H57A 0.9800 . ?
C57 H57B 0.9800 . ?
C57 H57C 0.9800 . ?
C61 C66 1.3872(19) . ?
C61 C62 1.4119(18) . ?
C62 C63 1.4054(18) . ?
C63 C64 1.3945(19) . ?
C63 H63A 0.9500 . ?
C64 C65 1.396(2) . ?
C64 C67 1.5093(19) . ?
C65 C66 1.388(2) . ?
C65 H65A 0.9500 . ?
C66 H66A 0.9500 . ?
C67 H67A 0.9800 . ?
C67 H67B 0.9800 . ?
C67 H67C 0.9800 . ?
N7 C71 1.150(4) . ?
C71 C72 1.438(4) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
N8A C81A 1.124(8) . ?
C81A C82A 1.384(8) . ?
C82A H82A 0.9800 . ?
C82A H82B 0.9800 . ?
C82A H82C 0.9800 . ?
C82B H82D 0.9800 . ?
C82B H82E 0.9800 . ?
C82B H82F 0.9800 . ?
C82C H82G 0.9800 . ?
C82C H82H 0.9800 . ?
C82C H82I 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti O2 88.86(4) . . ?
O3 Ti O1 96.29(4) . . ?
O2 Ti O1 84.95(4) . . ?
O3 Ti N3 78.04(4) . . ?
O2 Ti N3 95.89(4) . . ?
O1 Ti N3 174.24(4) . . ?
O3 Ti N2 163.96(4) . . ?
O2 Ti N2 75.46(4) . . ?
O1 Ti N2 85.87(4) . . ?
N3 Ti N2 99.87(4) . . ?
O3 Ti N1 98.95(4) . . ?
O2 Ti N1 159.01(4) . . ?
O1 Ti N1 74.88(4) . . ?
N3 Ti N1 104.76(4) . . ?
N2 Ti N1 96.96(4) . . ?
C11 O1 Ti 119.38(9) . . ?
C21 O2 Ti 120.50(8) . . ?
C31 O3 Ti 120.13(8) . . ?
C41 N C61 119.09(10) . . ?
C41 N C51 115.95(11) . . ?
C61 N C51 119.52(11) . . ?
C12 N1 C42 124.8(5) . . ?
C42 N1 C12A 116.6(7) . . ?
C12 N1 Ti 113.0(5) . . ?
C42 N1 Ti 122.10(9) . . ?
C12A N1 Ti 119.0(8) . . ?
C22 N2 C52 121.57(11) . . ?
C22 N2 Ti 115.57(9) . . ?
C52 N2 Ti 119.63(8) . . ?
C32 N3 C62 122.89(11) . . ?
C32 N3 Ti 113.60(8) . . ?
C62 N3 Ti 121.88(8) . . ?
O1 C11 C12 113.2(5) . . ?
O1 C11 C16 119.3(3) . . ?
C12 C11 C16 126.6(6) . . ?
O1 C11 C16A 129.1(4) . . ?
C12 C11 C16A 117.3(6) . . ?
O1 C11 C12A 119.5(7) . . ?
C16 C11 C12A 121.1(7) . . ?
C16A C11 C12A 108.9(7) . . ?
N1 C12 C11 117.0(9) . . ?
N1 C12 C13 126.3(9) . . ?
C11 C12 C13 115.7(9) . . ?
C14 C13 C12 120.7(7) . . ?
C14 C13 H13A 119.7 . . ?
C12 C13 H13A 119.7 . . ?
C13 C14 C15 119.0(4) . . ?
C13 C14 C18 122.4(4) . . ?
C15 C14 C18 118.5(3) . . ?
C16 C15 C14 123.7(4) . . ?
C16 C15 H15A 118.1 . . ?
C14 C15 H15A 118.1 . . ?
C15 C16 C11 113.8(5) . . ?
C15 C16 C17 121.7(8) . . ?
C11 C16 C17 124.2(7) . . ?
C171 C17 C172 110.0(8) . . ?
C171 C17 C173 108.6(11) . . ?
C172 C17 C173 111.2(8) . . ?
C171 C17 C16 111.9(9) . . ?
C172 C17 C16 108.2(10) . . ?
C173 C17 C16 106.9(7) . . ?
C17 C171 H17A 109.5 . . ?
C17 C171 H17B 109.5 . . ?
H17A C171 H17B 109.5 . . ?
C17 C171 H17C 109.5 . . ?
H17A C171 H17C 109.5 . . ?
H17B C171 H17C 109.5 . . ?
C17 C172 H17D 109.5 . . ?
C17 C172 H17E 109.5 . . ?
H17D C172 H17E 109.5 . . ?
C17 C172 H17F 109.5 . . ?
H17D C172 H17F 109.5 . . ?
H17E C172 H17F 109.5 . . ?
C17 C173 H17G 109.5 . . ?
C17 C173 H17H 109.5 . . ?
H17G C173 H17H 109.5 . . ?
C17 C173 H17I 109.5 . . ?
H17G C173 H17I 109.5 . . ?
H17H C173 H17I 109.5 . . ?
C181 C18 C182 109.1(7) . . ?
C181 C18 C183 107.1(7) . . ?
C182 C18 C183 109.6(3) . . ?
C181 C18 C14 113.1(6) . . ?
C182 C18 C14 108.7(3) . . ?
C183 C18 C14 109.2(3) . . ?
C18 C181 H18A 109.5 . . ?
C18 C181 H18B 109.5 . . ?
H18A C181 H18B 109.5 . . ?
C18 C181 H18C 109.5 . . ?
H18A C181 H18C 109.5 . . ?
H18B C181 H18C 109.5 . . ?
C18 C182 H18D 109.5 . . ?
C18 C182 H18E 109.5 . . ?
H18D C182 H18E 109.5 . . ?
C18 C182 H18F 109.5 . . ?
H18D C182 H18F 109.5 . . ?
H18E C182 H18F 109.5 . . ?
C18 C183 H18G 109.5 . . ?
C18 C183 H18H 109.5 . . ?
H18G C183 H18H 109.5 . . ?
C18 C183 H18I 109.5 . . ?
H18G C183 H18I 109.5 . . ?
H18H C183 H18I 109.5 . . ?
C13A C12A N1 129.0(14) . . ?
C13A C12A C11 127.7(14) . . ?
N1 C12A C11 103.1(9) . . ?
C14A C13A C12A 117.5(11) . . ?
C14A C13A H13B 121.2 . . ?
C12A C13A H13B 121.2 . . ?
C13A C14A C15A 119.0(6) . . ?
C13A C14A C18A 120.9(5) . . ?
C15A C14A C18A 120.0(4) . . ?
C16A C15A C14A 126.0(7) . . ?
C16A C15A H15B 117.0 . . ?
C14A C15A H15B 117.0 . . ?
C15A C16A C17A 127.3(12) . . ?
C15A C16A C11 119.8(8) . . ?
C17A C16A C11 112.5(11) . . ?
C16A C17A C175 113.5(16) . . ?
C16A C17A C174 110.1(13) . . ?
C175 C17A C174 106.0(12) . . ?
C17A C174 H17J 109.5 . . ?
C17A C174 H17K 109.5 . . ?
H17J C174 H17K 109.5 . . ?
C17A C174 H17L 109.5 . . ?
H17J C174 H17L 109.5 . . ?
H17K C174 H17L 109.5 . . ?
C17A C175 H17M 109.5 . . ?
C17A C175 H17N 109.5 . . ?
H17M C175 H17N 109.5 . . ?
C17A C175 H17O 109.5 . . ?
H17M C175 H17O 109.5 . . ?
H17N C175 H17O 109.5 . . ?
C185 C18A C14A 112.1(5) . . ?
C185 C18A C184 112.5(9) . . ?
C14A C18A C184 110.2(9) . . ?
C185 C18A C186 107.0(4) . . ?
C14A C18A C186 108.6(4) . . ?
C184 C18A C186 106.3(9) . . ?
C18A C184 H18J 109.5 . . ?
C18A C184 H18K 109.5 . . ?
H18J C184 H18K 109.5 . . ?
C18A C184 H18L 109.5 . . ?
H18J C184 H18L 109.5 . . ?
H18K C184 H18L 109.5 . . ?
C18A C185 H18M 109.5 . . ?
C18A C185 H18N 109.5 . . ?
H18M C185 H18N 109.5 . . ?
C18A C185 H18O 109.5 . . ?
H18M C185 H18O 109.5 . . ?
H18N C185 H18O 109.5 . . ?
C18A C186 H18P 109.5 . . ?
C18A C186 H18Q 109.5 . . ?
H18P C186 H18Q 109.5 . . ?
C18A C186 H18R 109.5 . . ?
H18P C186 H18R 109.5 . . ?
H18Q C186 H18R 109.5 . . ?
O2 C21 C26 124.54(12) . . ?
O2 C21 C22 115.68(11) . . ?
C26 C21 C22 119.73(12) . . ?
N2 C22 C23 127.57(12) . . ?
N2 C22 C21 111.68(11) . . ?
C23 C22 C21 120.74(12) . . ?
C24 C23 C22 119.54(13) . . ?
C24 C23 H23A 120.2 . . ?
C22 C23 H23A 120.2 . . ?
C23 C24 C25 118.49(13) . . ?
C23 C24 C28 119.15(14) . . ?
C25 C24 C28 122.31(13) . . ?
C26 C25 C24 124.49(13) . . ?
C26 C25 H25A 117.8 . . ?
C24 C25 H25A 117.8 . . ?
C25 C26 C21 116.60(13) . . ?
C25 C26 C27 123.11(13) . . ?
C21 C26 C27 120.20(13) . . ?
C26 C27 C273 110.36(13) . . ?
C26 C27 C272 111.67(14) . . ?
C273 C27 C272 108.17(14) . . ?
C26 C27 C271 108.52(12) . . ?
C273 C27 C271 109.76(15) . . ?
C272 C27 C271 108.32(14) . . ?
C27 C271 H27A 109.5 . . ?
C27 C271 H27B 109.5 . . ?
H27A C271 H27B 109.5 . . ?
C27 C271 H27C 109.5 . . ?
H27A C271 H27C 109.5 . . ?
H27B C271 H27C 109.5 . . ?
C27 C272 H27D 109.5 . . ?
C27 C272 H27E 109.5 . . ?
H27D C272 H27E 109.5 . . ?
C27 C272 H27F 109.5 . . ?
H27D C272 H27F 109.5 . . ?
H27E C272 H27F 109.5 . . ?
C27 C273 H27G 109.5 . . ?
C27 C273 H27H 109.5 . . ?
H27G C273 H27H 109.5 . . ?
C27 C273 H27I 109.5 . . ?
H27G C273 H27I 109.5 . . ?
H27H C273 H27I 109.5 . . ?
C283 C28 C24 112.31(15) . . ?
C283 C28 C281 108.50(16) . . ?
C24 C28 C281 108.54(13) . . ?
C283 C28 C282 108.21(14) . . ?
C24 C28 C282 109.59(13) . . ?
C281 C28 C282 109.65(17) . . ?
C28 C281 H28A 109.5 . . ?
C28 C281 H28B 109.5 . . ?
H28A C281 H28B 109.5 . . ?
C28 C281 H28C 109.5 . . ?
H28A C281 H28C 109.5 . . ?
H28B C281 H28C 109.5 . . ?
C28 C282 H28D 109.5 . . ?
C28 C282 H28E 109.5 . . ?
H28D C282 H28E 109.5 . . ?
C28 C282 H28F 109.5 . . ?
H28D C282 H28F 109.5 . . ?
H28E C282 H28F 109.5 . . ?
C28 C283 H28G 109.5 . . ?
C28 C283 H28H 109.5 . . ?
H28G C283 H28H 109.5 . . ?
C28 C283 H28I 109.5 . . ?
H28G C283 H28I 109.5 . . ?
H28H C283 H28I 109.5 . . ?
O3 C31 C36 123.54(12) . . ?
O3 C31 C32 114.92(11) . . ?
C36 C31 C32 121.53(12) . . ?
N3 C32 C33 128.91(12) . . ?
N3 C32 C31 111.82(11) . . ?
C33 C32 C31 119.20(12) . . ?
C34 C33 C32 120.29(13) . . ?
C34 C33 H33A 119.9 . . ?
C32 C33 H33A 119.9 . . ?
C33 C34 C35 118.85(13) . . ?
C33 C34 C38 120.30(13) . . ?
C35 C34 C38 120.81(12) . . ?
C36 C35 C34 123.33(13) . . ?
C36 C35 H35A 118.3 . . ?
C34 C35 H35A 118.3 . . ?
C35 C36 C31 116.65(13) . . ?
C35 C36 C37 123.04(12) . . ?
C31 C36 C37 120.31(12) . . ?
C372 C37 C36 112.15(12) . . ?
C372 C37 C371 107.37(12) . . ?
C36 C37 C371 109.88(11) . . ?
C372 C37 C373 108.55(12) . . ?
C36 C37 C373 109.14(12) . . ?
C371 C37 C373 109.72(13) . . ?
C37 C371 H37A 109.5 . . ?
C37 C371 H37B 109.5 . . ?
H37A C371 H37B 109.5 . . ?
C37 C371 H37C 109.5 . . ?
H37A C371 H37C 109.5 . . ?
H37B C371 H37C 109.5 . . ?
C37 C372 H37D 109.5 . . ?
C37 C372 H37E 109.5 . . ?
H37D C372 H37E 109.5 . . ?
C37 C372 H37F 109.5 . . ?
H37D C372 H37F 109.5 . . ?
H37E C372 H37F 109.5 . . ?
C37 C373 H37G 109.5 . . ?
C37 C373 H37H 109.5 . . ?
H37G C373 H37H 109.5 . . ?
C37 C373 H37I 109.5 . . ?
H37G C373 H37I 109.5 . . ?
H37H C373 H37I 109.5 . . ?
C381 C38 C383 112.24(17) . . ?
C381 C38 C34 108.68(13) . . ?
C383 C38 C34 111.12(12) . . ?
C381 C38 C382 107.93(17) . . ?
C383 C38 C382 105.68(15) . . ?
C34 C38 C382 111.15(14) . . ?
C38 C381 H38A 109.5 . . ?
C38 C381 H38B 109.5 . . ?
H38A C381 H38B 109.5 . . ?
C38 C381 H38C 109.5 . . ?
H38A C381 H38C 109.5 . . ?
H38B C381 H38C 109.5 . . ?
C38 C382 H38D 109.5 . . ?
C38 C382 H38E 109.5 . . ?
H38D C382 H38E 109.5 . . ?
C38 C382 H38F 109.5 . . ?
H38D C382 H38F 109.5 . . ?
H38E C382 H38F 109.5 . . ?
C38 C383 H38G 109.5 . . ?
C38 C383 H38H 109.5 . . ?
H38G C383 H38H 109.5 . . ?
C38 C383 H38I 109.5 . . ?
H38G C383 H38I 109.5 . . ?
H38H C383 H38I 109.5 . . ?
C46 C41 C42 120.73(12) . . ?
C46 C41 N 124.61(13) . . ?
C42 C41 N 114.63(12) . . ?
C41 C42 C43 119.51(13) . . ?
C41 C42 N1 114.73(11) . . ?
C43 C42 N1 125.66(13) . . ?
C44 C43 C42 120.27(13) . . ?
C44 C43 H43A 119.9 . . ?
C42 C43 H43A 119.9 . . ?
C43 C44 C45 118.91(13) . . ?
C43 C44 C47 120.40(14) . . ?
C45 C44 C47 120.69(13) . . ?
C46 C45 C44 121.49(13) . . ?
C46 C45 H45A 119.3 . . ?
C44 C45 H45A 119.3 . . ?
C45 C46 C41 118.93(13) . . ?
C45 C46 H46A 120.5 . . ?
C41 C46 H46A 120.5 . . ?
C44 C47 H47A 109.5 . . ?
C44 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C44 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C56 C51 C52 119.89(12) . . ?
C56 C51 N 123.72(12) . . ?
C52 C51 N 115.91(11) . . ?
N2 C52 C53 124.13(12) . . ?
N2 C52 C51 115.68(11) . . ?
C53 C52 C51 119.27(12) . . ?
C54 C53 C52 121.21(13) . . ?
C54 C53 H53A 119.4 . . ?
C52 C53 H53A 119.4 . . ?
C53 C54 C55 118.54(13) . . ?
C53 C54 C57 119.41(13) . . ?
C55 C54 C57 122.02(13) . . ?
C56 C55 C54 121.31(13) . . ?
C56 C55 H55A 119.3 . . ?
C54 C55 H55A 119.3 . . ?
C51 C56 C55 119.76(13) . . ?
C51 C56 H56A 120.1 . . ?
C55 C56 H56A 120.1 . . ?
C54 C57 H57A 109.5 . . ?
C54 C57 H57B 109.5 . . ?
H57A C57 H57B 109.5 . . ?
C54 C57 H57C 109.5 . . ?
H57A C57 H57C 109.5 . . ?
H57B C57 H57C 109.5 . . ?
C66 C61 C62 121.07(12) . . ?
C66 C61 N 121.96(12) . . ?
C62 C61 N 116.95(12) . . ?
N3 C62 C63 125.86(12) . . ?
N3 C62 C61 116.32(11) . . ?
C63 C62 C61 117.49(12) . . ?
C64 C63 C62 121.62(12) . . ?
C64 C63 H63A 119.2 . . ?
C62 C63 H63A 119.2 . . ?
C63 C64 C65 119.34(12) . . ?
C63 C64 C67 120.10(13) . . ?
C65 C64 C67 120.55(13) . . ?
C66 C65 C64 120.21(12) . . ?
C66 C65 H65A 119.9 . . ?
C64 C65 H65A 119.9 . . ?
C61 C66 C65 120.24(12) . . ?
C61 C66 H66A 119.9 . . ?
C65 C66 H66A 119.9 . . ?
C64 C67 H67A 109.5 . . ?
C64 C67 H67B 109.5 . . ?
H67A C67 H67B 109.5 . . ?
C64 C67 H67C 109.5 . . ?
H67A C67 H67C 109.5 . . ?
H67B C67 H67C 109.5 . . ?
N7 C71 C72 179.0(3) . . ?
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 . . ?
N8A C81A C82A 175.7(10) . . ?
H82D C82B H82E 109.5 . . ?
H82D C82B H82F 109.5 . . ?
H82E C82B H82F 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
Ti N C41 C42 37.49(12) . . . . ?
Ti N C51 C52 33.02(12) . . . . ?
Ti N C61 C62 31.05(11) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        71.53
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.719
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.055

_shelxl_version_number           2013-4

