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

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

data_Compound1
_database_code_depnum_ccdc_archive 'CCDC 1476528'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C20 H22 Cl N3 O3 Ti, C6 H5 F'
_chemical_formula_sum            'C26 H27 Cl F N3 O3 Ti'
_chemical_formula_weight         531.85

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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'
F F 0.0171 0.0103 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   17.700(10)
_cell_length_b                   7.391(4)
_cell_length_c                   19.676(12)
_cell_angle_alpha                90
_cell_angle_beta                 111.032(8)
_cell_angle_gamma                90
_cell_volume                     2403(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    2149
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      18.84

_exptl_crystal_description       lath
_exptl_crystal_colour            brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_F_000             1104
_exptl_transmission_factor_min   0.4643
_exptl_transmission_factor_max   1.0000
_exptl_crystal_size_max          0.408
_exptl_crystal_size_mid          0.083
_exptl_crystal_size_min          0.016
_exptl_absorpt_coefficient_mu    0.510
_shelx_estimated_absorpt_T_min   0.819
_shelx_estimated_absorpt_T_max   0.992
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS Rotating anode'
_diffrn_measurement_device_type  'Bruker APEX-II Pt135 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            13120
_diffrn_reflns_av_unetI/netI     0.0831
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.116
_diffrn_reflns_theta_max         18.932
_diffrn_reflns_theta_full        18.932
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1905
_reflns_number_gt                1394
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0400
0.00 0.00 -1.00 0.0070
-2.00 0.00 1.00 0.0080
2.00 0.00 -1.00 0.0080
-2.00 -2.00 1.00 0.1850
-1.00 -2.00 1.00 0.2000
1.00 2.00 -1.00 0.0870

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

# start Validation Reply Form
_vrf_REFNR01_Compound1           
;
PROBLEM: Ratio of reflections to parameters is < 6 for a
RESPONSE: THE CRYSTALS DIFFRACTS POORLY DESPITE GOOD SIZE.
AN INTEGRATION WAS MADE TO A COMBINED LEVEL OF DATA COMPLETENESS (99.5%)
AND A MEAN I/sigmA(I) OF 4.0, RESULTING IN A RESOLUTION OF INTEGRATION OF 
1.10 ANGSTROEMS. UNFORTUNATELY SOME EXTRA REFINEMENT PARAMETERS MUST BE 
USED TO REFINE AN INVERSION DISORDER OF AN i-PROPYL GROUP AND A ROTATIONALLY 
DISORDERED 1-FLUORO-BENZENE. 
;
_vrf_THETM01_Compound1           
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: THE CRYSTALS DIFFRACTS POORLY DESPITE GOOD SIZE.
AN INTEGRATION WAS MADE TO A COMBINED LEVEL OF DATA COMPLETENESS (99.5%)
AND A MEAN I/sigmA(I) OF 4.0, RESULTING IN A RESOLUTION OF INTEGRATION OF 
1.10 ANGSTROEMS. UNFORTUNATELY SOME EXTRA REFINEMENT PARAMETERS MUST BE 
USED TO REFINE AN INVERSION DISORDER OF AN i-PROPYL GROUP AND A ROTATIONALLY 
DISORDERED 1-FLUORO-BENZENE. 
;
_vrf_PLAT088_Compound1           
;
PROBLEM: Poor Data / Parameter Ratio ....................       5.81 Note  
RESPONSE: THE CRYSTALS DIFFRACTS POORLY DESPITE GOOD SIZE.
AN INTEGRATION WAS MADE TO A COMBINED LEVEL OF DATA COMPLETENESS (99.5%)
AND A MEAN I/sigmA(I) OF 4.0, RESULTING IN A RESOLUTION OF INTEGRATION OF 
1.10 ANGSTROEMS. UNFORTUNATELY SOME EXTRA REFINEMENT PARAMETERS MUST BE 
USED TO REFINE AN INVERSION DISORDER OF AN i-PROPYL GROUP AND A ROTATIONALLY 
DISORDERED 1-FLUORO-BENZENE. 
;
# end Validation Reply Form

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
'Poorly diffracting crystals. Integrated to 1.10 Ångström'
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1131P)²+1.2328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         1905
_refine_ls_number_parameters     328
_refine_ls_number_restraints     448
_refine_ls_R_factor_all          0.0879
_refine_ls_R_factor_gt           0.0645
_refine_ls_wR_factor_ref         0.1785
_refine_ls_wR_factor_gt          0.1593
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_restrained_S_all      0.962
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.33251(9) 0.23423(18) 0.28668(7) 0.0329(6) Uani 1 1 d . U . . .
Cl1 Cl 0.34502(12) 0.2177(3) 0.17170(10) 0.0389(7) Uani 1 1 d . U . . .
O1 O 0.2347(3) 0.3520(7) 0.2567(3) 0.0412(15) Uani 1 1 d . U . . .
N1 N 0.2696(4) 0.3801(8) 0.4054(3) 0.0320(16) Uani 1 1 d . U . . .
C1 C 0.3336(5) 0.3163(9) 0.3932(4) 0.0304(18) Uani 1 1 d . U . . .
O2 O 0.4382(3) 0.1705(6) 0.3405(3) 0.0305(13) Uani 1 1 d . U . . .
N2 N 0.3959(4) 0.3082(8) 0.4541(3) 0.0308(16) Uani 1 1 d . U . . .
C2 C 0.3761(5) 0.3674(10) 0.5171(4) 0.035(2) Uani 1 1 d . U . . .
H2A H 0.4064 0.4783 0.5393 0.042 Uiso 1 1 calc R U . . .
H2B H 0.3881 0.2714 0.5546 0.042 Uiso 1 1 calc R U . . .
O3 O 0.2912(3) 0.0175(6) 0.2871(3) 0.0386(14) Uani 1 1 d D U . . .
N3 N 0.3866(4) 0.5133(9) 0.2858(3) 0.0365(18) Uani 1 1 d . U . . .
C3 C 0.2868(5) 0.4037(10) 0.4842(4) 0.035(2) Uani 1 1 d . U . . .
H3A H 0.2558 0.3162 0.5020 0.042 Uiso 1 1 calc R U . . .
H3B H 0.2739 0.5281 0.4952 0.042 Uiso 1 1 calc R U . . .
C4 C 0.1926(5) 0.4149(9) 0.3564(4) 0.0307(18) Uani 1 1 d . U . . .
C5 C 0.1775(5) 0.4062(10) 0.2809(4) 0.036(2) Uani 1 1 d . U . . .
C6 C 0.1021(5) 0.4462(10) 0.2343(4) 0.036(2) Uani 1 1 d . U . . .
H6 H 0.0909 0.4371 0.1835 0.044 Uiso 1 1 calc R U . . .
C7 C 0.0420(5) 0.4988(10) 0.2572(5) 0.042(2) Uani 1 1 d . U . . .
H7 H -0.0096 0.5296 0.2227 0.051 Uiso 1 1 calc R U . . .
C8 C 0.0561(5) 0.5077(10) 0.3317(4) 0.040(2) Uani 1 1 d . U . . .
H8 H 0.0143 0.5414 0.3489 0.048 Uiso 1 1 calc R U . . .
C9 C 0.1316(5) 0.4664(10) 0.3787(4) 0.035(2) Uani 1 1 d . U . . .
H9 H 0.1422 0.4739 0.4295 0.042 Uiso 1 1 calc R U . . .
C10 C 0.4739(5) 0.2498(9) 0.4645(4) 0.0272(18) Uani 1 1 d . U . . .
C11 C 0.4936(5) 0.1807(9) 0.4071(4) 0.0288(18) Uani 1 1 d . U . . .
C12 C 0.5713(5) 0.1228(9) 0.4209(4) 0.0297(19) Uani 1 1 d . U . . .
H12 H 0.5853 0.0792 0.3815 0.036 Uiso 1 1 calc R U . . .
C13 C 0.6288(5) 0.1255(10) 0.4885(4) 0.037(2) Uani 1 1 d . U . . .
H13 H 0.6818 0.0813 0.4968 0.044 Uiso 1 1 calc R U . . .
C14 C 0.6087(5) 0.1944(10) 0.5454(4) 0.036(2) Uani 1 1 d . U . . .
H14 H 0.6483 0.1999 0.5932 0.043 Uiso 1 1 calc R U . . .
C15 C 0.5330(5) 0.2531(10) 0.5327(4) 0.036(2) Uani 1 1 d . U . . .
H15 H 0.5199 0.2985 0.5723 0.044 Uiso 1 1 calc R U . . .
C16 C 0.4121(5) 0.6454(11) 0.2724(4) 0.032(2) Uani 1 1 d . U . . .
C17 C 0.4427(5) 0.8077(10) 0.2540(4) 0.041(2) Uani 1 1 d . U . . .
H17A H 0.4529 0.8953 0.2937 0.049 Uiso 1 1 calc R U . . .
H17B H 0.4030 0.8578 0.2093 0.049 Uiso 1 1 calc R U . . .
H17C H 0.4933 0.7824 0.2462 0.049 Uiso 1 1 calc R U . . .
C18 C 0.2277(7) -0.1166(17) 0.2724(6) 0.037(3) Uani 0.474(11) 1 d D U P A 1
H18 H 0.2522 -0.2403 0.2810 0.045 Uiso 0.474(11) 1 calc R U P A 1
C19 C 0.1742(10) -0.098(3) 0.1940(7) 0.043(4) Uani 0.474(11) 1 d D U P A 1
H19A H 0.1347 -0.1967 0.1807 0.065 Uiso 0.474(11) 1 calc R U P A 1
H19B H 0.2072 -0.1028 0.1634 0.065 Uiso 0.474(11) 1 calc R U P A 1
H19C H 0.1457 0.0183 0.1868 0.065 Uiso 0.474(11) 1 calc R U P A 1
C20 C 0.1844(12) -0.082(5) 0.3240(9) 0.041(3) Uani 0.474(11) 1 d D U P A 1
H20A H 0.1421 -0.1736 0.3166 0.062 Uiso 0.474(11) 1 calc R U P A 1
H20B H 0.1597 0.0384 0.3149 0.062 Uiso 0.474(11) 1 calc R U P A 1
H20C H 0.2230 -0.0889 0.3742 0.062 Uiso 0.474(11) 1 calc R U P A 1
C18A C 0.2071(6) -0.0334(17) 0.2523(6) 0.037(3) Uani 0.526(11) 1 d D U P A 2
H18A H 0.1743 0.0758 0.2299 0.045 Uiso 0.526(11) 1 calc R U P A 2
C19A C 0.2037(11) -0.167(2) 0.1939(7) 0.043(4) Uani 0.526(11) 1 d D U P A 2
H19D H 0.1471 -0.1948 0.1652 0.065 Uiso 0.526(11) 1 calc R U P A 2
H19E H 0.2320 -0.2777 0.2162 0.065 Uiso 0.526(11) 1 calc R U P A 2
H19F H 0.2297 -0.1145 0.1621 0.065 Uiso 0.526(11) 1 calc R U P A 2
C20A C 0.1790(12) -0.108(4) 0.3100(9) 0.041(3) Uani 0.526(11) 1 d D U P A 2
H20D H 0.1238 -0.1549 0.2874 0.062 Uiso 0.526(11) 1 calc R U P A 2
H20E H 0.1798 -0.0120 0.3446 0.062 Uiso 0.526(11) 1 calc R U P A 2
H20F H 0.2152 -0.2063 0.3359 0.062 Uiso 0.526(11) 1 calc R U P A 2
C21 C 0.1466(4) -0.0990(6) 0.5083(3) 0.061(3) Uani 0.5 1 d DG U P B 3
C22 C 0.0801(4) -0.0480(7) 0.4479(3) 0.054(2) Uani 0.5 1 d DG U P B 3
H22 H 0.0595 -0.1276 0.4075 0.065 Uiso 0.5 1 calc R U P B 3
C23 C 0.0438(3) 0.1193(8) 0.4467(3) 0.053(2) Uani 0.5 1 d DG U P B 3
H23 H -0.0016 0.1541 0.4055 0.064 Uiso 0.5 1 calc R U P B 3
C24 C 0.0740(3) 0.2357(6) 0.5058(3) 0.056(2) Uani 0.5 1 d DG U P B 3
H24 H 0.0492 0.3501 0.5050 0.067 Uiso 0.5 1 calc R U P B 3
C25 C 0.1404(4) 0.1848(7) 0.5661(3) 0.056(2) Uani 0.5 1 d DG U P B 3
H25 H 0.1610 0.2643 0.6065 0.067 Uiso 0.5 1 calc R U P B 3
C26 C 0.1767(3) 0.0174(8) 0.5674(3) 0.058(2) Uani 0.5 1 d DG U P B 3
H26 H 0.2221 -0.0174 0.6086 0.070 Uiso 0.5 1 calc R U P B 3
F1 F 0.1785(7) -0.2444(13) 0.5159(6) 0.069(3) Uani 0.5 1 d . U P B 3
C21A C 0.1466(4) -0.0990(6) 0.5083(3) 0.061(3) Uani 0.5 1 d D U P C 4
H21A H 0.1714 -0.2133 0.5091 0.074 Uiso 0.5 1 calc R U P C 4
C22A C 0.0801(4) -0.0480(7) 0.4479(3) 0.054(2) Uani 0.5 1 d D U P C 4
H22A H 0.0595 -0.1276 0.4075 0.065 Uiso 0.5 1 calc R U P C 4
C23A C 0.0438(3) 0.1193(8) 0.4467(3) 0.053(2) Uani 0.5 1 d D U P C 4
H23A H -0.0016 0.1541 0.4055 0.064 Uiso 0.5 1 calc R U P C 4
C24A C 0.0740(3) 0.2357(6) 0.5058(3) 0.056(2) Uani 0.5 1 d D U P C 4
F1A F 0.0433(7) 0.3796(13) 0.5069(6) 0.079(3) Uani 0.5 1 d . U P C 4
C25A C 0.1404(4) 0.1848(7) 0.5661(3) 0.056(2) Uani 0.5 1 d D U P C 4
H25A H 0.1610 0.2643 0.6065 0.067 Uiso 0.5 1 calc R U P C 4
C26A C 0.1767(3) 0.0174(8) 0.5674(3) 0.058(2) Uani 0.5 1 d D U P C 4
H26A H 0.2221 -0.0174 0.6086 0.070 Uiso 0.5 1 calc R U P C 4


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.762(5) . ?
Ti1 O1 1.835(6) . ?
Ti1 O2 1.850(5) . ?
Ti1 C1 2.175(8) . ?
Ti1 N3 2.276(7) . ?
Ti1 Cl1 2.354(3) . ?
O1 C5 1.327(9) . ?
N1 C1 1.327(9) . ?
N1 C4 1.382(9) . ?
N1 C3 1.477(9) . ?
C1 N2 1.307(9) . ?
O2 C11 1.328(9) . ?
N2 C10 1.388(9) . ?
N2 C2 1.472(9) . ?
C2 C3 1.501(10) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
O3 C18A 1.447(9) . ?
O3 C18 1.447(9) . ?
N3 C16 1.145(9) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C9 1.359(10) . ?
C4 C5 1.412(11) . ?
C5 C6 1.354(10) . ?
C6 C7 1.352(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.397(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.360(10) . ?
C8 H8 0.9500 . ?
C9 H9 0.9500 . ?
C10 C15 1.374(10) . ?
C10 C11 1.394(10) . ?
C11 C12 1.371(10) . ?
C12 C13 1.354(10) . ?
C12 H12 0.9500 . ?
C13 C14 1.388(11) . ?
C13 H13 0.9500 . ?
C14 C15 1.344(11) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.416(11) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 C19 1.498(8) . ?
C18 C20 1.498(8) . ?
C18 H18 1.0000 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C18A C20A 1.498(8) . ?
C18A C19A 1.498(8) . ?
C18A H18A 1.0000 . ?
C19A H19D 0.9800 . ?
C19A H19E 0.9800 . ?
C19A H19F 0.9800 . ?
C20A H20D 0.9800 . ?
C20A H20E 0.9800 . ?
C20A H20F 0.9800 . ?
C21 F1 1.198(10) . ?
C21 C22 1.3900 . ?
C21 C26 1.3900 . ?
C22 C23 1.3900 . ?
C22 H22 0.9500 . ?
C23 C24 1.3900 . ?
C23 H23 0.9500 . ?
C24 C25 1.3900 . ?
C24 H24 0.9500 . ?
C25 C26 1.3900 . ?
C25 H25 0.9500 . ?
C26 H26 0.9500 . ?
C21A C22A 1.3900 . ?
C21A C26A 1.3900 . ?
C21A H21A 0.9500 . ?
C22A C23A 1.3900 . ?
C22A H22A 0.9500 . ?
C23A C24A 1.3900 . ?
C23A H23A 0.9500 . ?
C24A F1A 1.198(10) . ?
C24A C25A 1.3900 . ?
C25A C26A 1.3900 . ?
C25A H25A 0.9500 . ?
C26A H26A 0.9500 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O1 95.0(2) . . ?
O3 Ti1 O2 95.9(2) . . ?
O1 Ti1 O2 161.5(2) . . ?
O3 Ti1 C1 96.3(3) . . ?
O1 Ti1 C1 81.9(3) . . ?
O2 Ti1 C1 82.1(3) . . ?
O3 Ti1 N3 179.5(2) . . ?
O1 Ti1 N3 85.3(2) . . ?
O2 Ti1 N3 83.9(2) . . ?
C1 Ti1 N3 84.0(2) . . ?
O3 Ti1 Cl1 98.00(17) . . ?
O1 Ti1 Cl1 96.82(17) . . ?
O2 Ti1 Cl1 96.46(17) . . ?
C1 Ti1 Cl1 165.7(2) . . ?
N3 Ti1 Cl1 81.66(16) . . ?
C5 O1 Ti1 141.4(5) . . ?
C1 N1 C4 129.1(7) . . ?
C1 N1 C3 111.3(6) . . ?
C4 N1 C3 119.5(6) . . ?
N2 C1 N1 110.2(7) . . ?
N2 C1 Ti1 125.7(6) . . ?
N1 C1 Ti1 124.1(6) . . ?
C11 O2 Ti1 142.0(5) . . ?
C1 N2 C10 128.1(7) . . ?
C1 N2 C2 112.4(6) . . ?
C10 N2 C2 119.5(6) . . ?
N2 C2 C3 102.8(6) . . ?
N2 C2 H2A 111.2 . . ?
C3 C2 H2A 111.2 . . ?
N2 C2 H2B 111.2 . . ?
C3 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
C18A O3 Ti1 126.3(6) . . ?
C18 O3 Ti1 156.2(7) . . ?
C16 N3 Ti1 167.3(6) . . ?
N1 C3 C2 102.8(6) . . ?
N1 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N1 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C9 C4 N1 121.6(7) . . ?
C9 C4 C5 118.7(8) . . ?
N1 C4 C5 119.5(7) . . ?
O1 C5 C6 121.1(7) . . ?
O1 C5 C4 120.7(7) . . ?
C6 C5 C4 118.1(8) . . ?
C7 C6 C5 122.6(8) . . ?
C7 C6 H6 118.7 . . ?
C5 C6 H6 118.7 . . ?
C6 C7 C8 119.9(8) . . ?
C6 C7 H7 120.1 . . ?
C8 C7 H7 120.1 . . ?
C9 C8 C7 117.7(8) . . ?
C9 C8 H8 121.1 . . ?
C7 C8 H8 121.1 . . ?
C4 C9 C8 122.9(8) . . ?
C4 C9 H9 118.5 . . ?
C8 C9 H9 118.5 . . ?
C15 C10 N2 120.4(7) . . ?
C15 C10 C11 118.2(7) . . ?
N2 C10 C11 121.3(7) . . ?
O2 C11 C12 120.7(7) . . ?
O2 C11 C10 120.6(7) . . ?
C12 C11 C10 118.7(7) . . ?
C13 C12 C11 122.4(7) . . ?
C13 C12 H12 118.8 . . ?
C11 C12 H12 118.8 . . ?
C12 C13 C14 118.6(7) . . ?
C12 C13 H13 120.7 . . ?
C14 C13 H13 120.7 . . ?
C15 C14 C13 119.8(7) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C10 122.3(8) . . ?
C14 C15 H15 118.9 . . ?
C10 C15 H15 118.9 . . ?
N3 C16 C17 178.5(9) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
O3 C18 C19 107.5(9) . . ?
O3 C18 C20 107.4(11) . . ?
C19 C18 C20 113.2(13) . . ?
O3 C18 H18 109.6 . . ?
C19 C18 H18 109.6 . . ?
C20 C18 H18 109.6 . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C18A C20A 107.6(9) . . ?
O3 C18A C19A 106.5(9) . . ?
C20A C18A C19A 114.0(13) . . ?
O3 C18A H18A 109.5 . . ?
C20A C18A H18A 109.5 . . ?
C19A C18A H18A 109.5 . . ?
C18A C19A H19D 109.5 . . ?
C18A C19A H19E 109.5 . . ?
H19D C19A H19E 109.5 . . ?
C18A C19A H19F 109.5 . . ?
H19D C19A H19F 109.5 . . ?
H19E C19A H19F 109.5 . . ?
C18A C20A H20D 109.5 . . ?
C18A C20A H20E 109.5 . . ?
H20D C20A H20E 109.5 . . ?
C18A C20A H20F 109.5 . . ?
H20D C20A H20F 109.5 . . ?
H20E C20A H20F 109.5 . . ?
F1 C21 C22 124.5(7) . . ?
F1 C21 C26 115.3(7) . . ?
C22 C21 C26 120.0 . . ?
C21 C22 C23 120.0 . . ?
C21 C22 H22 120.0 . . ?
C23 C22 H22 120.0 . . ?
C24 C23 C22 120.0 . . ?
C24 C23 H23 120.0 . . ?
C22 C23 H23 120.0 . . ?
C25 C24 C23 120.0 . . ?
C25 C24 H24 120.0 . . ?
C23 C24 H24 120.0 . . ?
C24 C25 C26 120.0 . . ?
C24 C25 H25 120.0 . . ?
C26 C25 H25 120.0 . . ?
C25 C26 C21 120.0 . . ?
C25 C26 H26 120.0 . . ?
C21 C26 H26 120.0 . . ?
C22A C21A C26A 120.0 . . ?
C22A C21A H21A 120.0 . . ?
C26A C21A H21A 120.0 . . ?
C23A C22A C21A 120.0 . . ?
C23A C22A H22A 120.0 . . ?
C21A C22A H22A 120.0 . . ?
C22A C23A C24A 120.0 . . ?
C22A C23A H23A 120.0 . . ?
C24A C23A H23A 120.0 . . ?
F1A C24A C23A 121.6(7) . . ?
F1A C24A C25A 118.4(7) . . ?
C23A C24A C25A 120.0 . . ?
C26A C25A C24A 120.0 . . ?
C26A C25A H25A 120.0 . . ?
C24A C25A H25A 120.0 . . ?
C25A C26A C21A 120.0 . . ?
C25A C26A H26A 120.0 . . ?
C21A C26A H26A 120.0 . . ?

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 C5 74.4(8) . . . . ?
O2 Ti1 O1 C5 -51.4(12) . . . . ?
C1 Ti1 O1 C5 -21.2(8) . . . . ?
N3 Ti1 O1 C5 -105.9(8) . . . . ?
Cl1 Ti1 O1 C5 173.1(8) . . . . ?
C4 N1 C1 N2 178.0(6) . . . . ?
C3 N1 C1 N2 -5.7(8) . . . . ?
C4 N1 C1 Ti1 -2.9(10) . . . . ?
C3 N1 C1 Ti1 173.4(5) . . . . ?
O3 Ti1 O2 C11 -102.0(7) . . . . ?
O1 Ti1 O2 C11 23.7(12) . . . . ?
C1 Ti1 O2 C11 -6.4(7) . . . . ?
N3 Ti1 O2 C11 78.4(7) . . . . ?
Cl1 Ti1 O2 C11 159.2(7) . . . . ?
N1 C1 N2 C10 -179.8(6) . . . . ?
Ti1 C1 N2 C10 1.1(11) . . . . ?
N1 C1 N2 C2 1.3(8) . . . . ?
Ti1 C1 N2 C2 -177.8(5) . . . . ?
C1 N2 C2 C3 3.5(8) . . . . ?
C10 N2 C2 C3 -175.6(6) . . . . ?
O1 Ti1 O3 C18A 15.9(6) . . . . ?
O2 Ti1 O3 C18A -179.2(6) . . . . ?
C1 Ti1 O3 C18A 98.2(6) . . . . ?
Cl1 Ti1 O3 C18A -81.8(6) . . . . ?
O1 Ti1 O3 C18 10.6(14) . . . . ?
O2 Ti1 O3 C18 175.6(13) . . . . ?
C1 Ti1 O3 C18 93.0(14) . . . . ?
Cl1 Ti1 O3 C18 -87.0(13) . . . . ?
C1 N1 C3 C2 7.5(8) . . . . ?
C4 N1 C3 C2 -175.8(6) . . . . ?
N2 C2 C3 N1 -6.2(7) . . . . ?
C1 N1 C4 C9 174.4(7) . . . . ?
C3 N1 C4 C9 -1.5(10) . . . . ?
C1 N1 C4 C5 -9.0(11) . . . . ?
C3 N1 C4 C5 175.1(6) . . . . ?
Ti1 O1 C5 C6 -160.8(6) . . . . ?
Ti1 O1 C5 C4 16.0(12) . . . . ?
C9 C4 C5 O1 -178.2(7) . . . . ?
N1 C4 C5 O1 5.1(10) . . . . ?
C9 C4 C5 C6 -1.3(11) . . . . ?
N1 C4 C5 C6 -178.1(6) . . . . ?
O1 C5 C6 C7 178.8(7) . . . . ?
C4 C5 C6 C7 2.0(11) . . . . ?
C5 C6 C7 C8 -2.1(12) . . . . ?
C6 C7 C8 C9 1.6(11) . . . . ?
N1 C4 C9 C8 177.6(7) . . . . ?
C5 C4 C9 C8 1.0(11) . . . . ?
C7 C8 C9 C4 -1.1(11) . . . . ?
C1 N2 C10 C15 178.9(7) . . . . ?
C2 N2 C10 C15 -2.3(10) . . . . ?
C1 N2 C10 C11 -3.4(11) . . . . ?
C2 N2 C10 C11 175.4(6) . . . . ?
Ti1 O2 C11 C12 -174.3(5) . . . . ?
Ti1 O2 C11 C10 6.0(11) . . . . ?
C15 C10 C11 O2 178.4(6) . . . . ?
N2 C10 C11 O2 0.6(10) . . . . ?
C15 C10 C11 C12 -1.4(10) . . . . ?
N2 C10 C11 C12 -179.1(6) . . . . ?
O2 C11 C12 C13 -177.8(6) . . . . ?
C10 C11 C12 C13 2.0(11) . . . . ?
C11 C12 C13 C14 -1.9(11) . . . . ?
C12 C13 C14 C15 1.2(11) . . . . ?
C13 C14 C15 C10 -0.7(11) . . . . ?
N2 C10 C15 C14 178.6(7) . . . . ?
C11 C10 C15 C14 0.8(11) . . . . ?
Ti1 O3 C18 C19 49(2) . . . . ?
Ti1 O3 C18 C20 -73(2) . . . . ?
Ti1 O3 C18A C20A -122.3(14) . . . . ?
Ti1 O3 C18A C19A 115.1(10) . . . . ?
F1 C21 C22 C23 175.2(9) . . . . ?
C26 C21 C22 C23 0.0 . . . . ?
C21 C22 C23 C24 0.0 . . . . ?
C22 C23 C24 C25 0.0 . . . . ?
C23 C24 C25 C26 0.0 . . . . ?
C24 C25 C26 C21 0.0 . . . . ?
F1 C21 C26 C25 -175.6(8) . . . . ?
C22 C21 C26 C25 0.0 . . . . ?
C26A C21A C22A C23A 0.0 . . . . ?
C21A C22A C23A C24A 0.0 . . . . ?
C22A C23A C24A F1A -178.9(9) . . . . ?
C22A C23A C24A C25A 0.0 . . . . ?
F1A C24A C25A C26A 178.9(8) . . . . ?
C23A C24A C25A C26A 0.0 . . . . ?
C24A C25A C26A C21A 0.0 . . . . ?
C22A C21A C26A C25A 0.0 . . . . ?

_refine_diff_density_max         0.747
_refine_diff_density_min         -0.287
_refine_diff_density_rms         0.093


_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_Compound4
_database_code_depnum_ccdc_archive 'CCDC 1476529'
_audit_update_record             
;
2016-05-30 deposited with the CCDC.
2016-06-14 downloaded from the CCDC.
;
#data_JH25_a - Copy

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H52 N4 O8 Ti2, C4 H8 O'
_chemical_formula_sum            'C46 H60 N4 O9 Ti2'
_chemical_formula_weight         908.78

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

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+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                   29.100(4)
_cell_length_b                   19.218(3)
_cell_length_c                   20.797(3)
_cell_angle_alpha                90
_cell_angle_beta                 130.641(2)
_cell_angle_gamma                90
_cell_volume                     8825(2)
_cell_formula_units_Z            8
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9879
_cell_measurement_theta_min      2.35
_cell_measurement_theta_max      30.49

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.368
_exptl_crystal_F_000             3840
_exptl_transmission_factor_min   0.5002
_exptl_transmission_factor_max   0.7461
_exptl_crystal_size_max          0.480
_exptl_crystal_size_mid          0.340
_exptl_crystal_size_min          0.320
_exptl_absorpt_coefficient_mu    0.422
_shelx_estimated_absorpt_T_min   0.823
_shelx_estimated_absorpt_T_max   0.877
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS Rotating anode'
_diffrn_measurement_device_type  'Bruker APEX-II Pt135 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            55583
_diffrn_reflns_av_unetI/netI     0.0412
_diffrn_reflns_av_R_equivalents  0.0630
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         1.845
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             9018
_reflns_number_gt                7400
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0509P)²+21.0862P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9018
_refine_ls_number_parameters     615
_refine_ls_number_restraints     36
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0458
_refine_ls_wR_factor_ref         0.1269
_refine_ls_wR_factor_gt          0.1176
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_restrained_S_all      1.058
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.29759(2) 0.51373(2) 0.65030(3) 0.02057(11) Uani 1 1 d . . . . .
Ti2 Ti 0.26390(2) 0.42961(2) 0.75512(3) 0.01989(11) Uani 1 1 d . . . . .
O1 O 0.23708(7) 0.52967(8) 0.53321(10) 0.0235(3) Uani 1 1 d . . . . .
O2 O 0.32907(7) 0.50381(8) 0.76932(10) 0.0212(3) Uani 1 1 d . . . . .
O3 O 0.35042(8) 0.58341(9) 0.67508(11) 0.0280(4) Uani 1 1 d . . . . .
O4 O 0.23886(7) 0.44238(8) 0.64242(10) 0.0219(3) Uani 1 1 d . . . . .
O5 O 0.34170(8) 0.44176(9) 0.65490(11) 0.0266(4) Uani 1 1 d D . . . .
O6 O 0.22082(7) 0.50547(8) 0.74965(10) 0.0237(3) Uani 1 1 d . . . . .
O7 O 0.32367(7) 0.36165(8) 0.79415(10) 0.0238(3) Uani 1 1 d . . . . .
O8 O 0.21285(7) 0.36760(8) 0.74589(10) 0.0240(3) Uani 1 1 d . . . . .
N1 N 0.19848(9) 0.63095(10) 0.59025(12) 0.0224(4) Uani 1 1 d . . . . .
N2 N 0.27033(9) 0.63524(10) 0.72653(12) 0.0218(4) Uani 1 1 d . . . . .
N3 N 0.31094(9) 0.49909(11) 0.92822(13) 0.0260(4) Uani 1 1 d . . . . .
N4 N 0.37062(9) 0.41400(11) 0.95492(12) 0.0254(4) Uani 1 1 d . . . . .
C1 C 0.24920(10) 0.59985(12) 0.65650(14) 0.0215(5) Uani 1 1 d . . . . .
C2 C 0.18052(11) 0.69019(13) 0.61499(16) 0.0287(5) Uani 1 1 d . . . . .
H2A H 0.1427 0.6799 0.6042 0.034 Uiso 1 1 calc R U . . .
H2B H 0.1747 0.7330 0.5839 0.034 Uiso 1 1 calc R U . . .
C3 C 0.23364(11) 0.69770(12) 0.70899(15) 0.0255(5) Uani 1 1 d . . . . .
H3A H 0.2564 0.7411 0.7215 0.031 Uiso 1 1 calc R U . . .
H3B H 0.2202 0.6970 0.7422 0.031 Uiso 1 1 calc R U . . .
C4 C 0.32503(10) 0.62048(12) 0.80840(14) 0.0231(5) Uani 1 1 d . . . . .
C5 C 0.34993(11) 0.66918(13) 0.87329(16) 0.0277(5) Uani 1 1 d . . . . .
H5 H 0.3291 0.7115 0.8622 0.033 Uiso 1 1 calc R U . . .
C6 C 0.40448(12) 0.65664(14) 0.95337(16) 0.0325(6) Uani 1 1 d . . . . .
H6 H 0.4204 0.6898 0.9972 0.039 Uiso 1 1 calc R U . . .
C7 C 0.43595(12) 0.59600(14) 0.96989(16) 0.0318(6) Uani 1 1 d . . . . .
H7 H 0.4744 0.5883 1.0242 0.038 Uiso 1 1 calc R U . . .
C8 C 0.41093(11) 0.54614(13) 0.90640(15) 0.0272(5) Uani 1 1 d . . . . .
H8 H 0.4325 0.5043 0.9179 0.033 Uiso 1 1 calc R U . . .
C9 C 0.35485(10) 0.55656(12) 0.82654(15) 0.0227(5) Uani 1 1 d . . . . .
C10 C 0.16162(10) 0.60886(12) 0.50520(15) 0.0230(5) Uani 1 1 d . . . . .
C11 C 0.18165(11) 0.55729(12) 0.47980(15) 0.0231(5) Uani 1 1 d . . . . .
C12 C 0.14210(11) 0.53590(13) 0.39517(16) 0.0279(5) Uani 1 1 d . . . . .
H12 H 0.1544 0.5003 0.3775 0.033 Uiso 1 1 calc R U . . .
C13 C 0.08543(12) 0.56542(14) 0.33669(16) 0.0323(6) Uani 1 1 d . . . . .
H13 H 0.0592 0.5502 0.2794 0.039 Uiso 1 1 calc R U . . .
C14 C 0.06690(12) 0.61715(14) 0.36159(17) 0.0346(6) Uani 1 1 d . . . . .
H14 H 0.0282 0.6380 0.3212 0.041 Uiso 1 1 calc R U . . .
C15 C 0.10465(11) 0.63851(13) 0.44506(16) 0.0300(5) Uani 1 1 d . . . . .
H15 H 0.0915 0.6740 0.4617 0.036 Uiso 1 1 calc R U . . .
C16 C 0.35704(12) 0.65575(13) 0.67181(17) 0.0307(5) Uani 1 1 d . . . . .
H16 H 0.3409 0.6802 0.6960 0.037 Uiso 1 1 calc R U . . .
C17 C 0.32112(13) 0.67949(14) 0.58096(18) 0.0356(6) Uani 1 1 d . . . . .
H17A H 0.3276 0.7294 0.5801 0.053 Uiso 1 1 calc R U . . .
H17B H 0.2779 0.6707 0.5489 0.053 Uiso 1 1 calc R U . . .
H17C H 0.3346 0.6537 0.5551 0.053 Uiso 1 1 calc R U . . .
C18 C 0.42382(14) 0.67171(17) 0.7268(2) 0.0465(7) Uani 1 1 d . . . . .
H18A H 0.4295 0.7220 0.7276 0.070 Uiso 1 1 calc R U . . .
H18B H 0.4403 0.6481 0.7040 0.070 Uiso 1 1 calc R U . . .
H18C H 0.4449 0.6553 0.7847 0.070 Uiso 1 1 calc R U . . .
C19 C 0.19974(12) 0.39812(14) 0.56920(16) 0.0312(6) Uani 1 1 d . . . . .
H19 H 0.2022 0.4137 0.5257 0.037 Uiso 1 1 calc R U . . .
C20 C 0.22131(17) 0.32334(14) 0.59188(19) 0.0466(8) Uani 1 1 d . . . . .
H20A H 0.1957 0.2944 0.5409 0.070 Uiso 1 1 calc R U . . .
H20B H 0.2188 0.3066 0.6340 0.070 Uiso 1 1 calc R U . . .
H20C H 0.2634 0.3207 0.6154 0.070 Uiso 1 1 calc R U . . .
C21 C 0.13505(14) 0.4077(2) 0.53241(19) 0.0521(8) Uani 1 1 d . . . . .
H21A H 0.1081 0.3791 0.4813 0.078 Uiso 1 1 calc R U . . .
H21B H 0.1236 0.4568 0.5178 0.078 Uiso 1 1 calc R U . . .
H21C H 0.1315 0.3934 0.5742 0.078 Uiso 1 1 calc R U . . .
C22 C 0.39479(19) 0.4061(2) 0.7204(3) 0.0453(11) Uani 0.605(4) 1 d D U P A 1
H22 H 0.3911 0.3893 0.7623 0.054 Uiso 0.605(4) 1 calc R U P A 1
C23 C 0.4028(6) 0.3438(5) 0.6832(6) 0.063(2) Uani 0.605(4) 1 d D U P A 1
H23A H 0.4325 0.3117 0.7288 0.095 Uiso 0.605(4) 1 calc R U P A 1
H23B H 0.4170 0.3597 0.6540 0.095 Uiso 0.605(4) 1 calc R U P A 1
H23C H 0.3639 0.3197 0.6427 0.095 Uiso 0.605(4) 1 calc R U P A 1
C24 C 0.4487(2) 0.4553(3) 0.7646(4) 0.0560(13) Uani 0.605(4) 1 d D U P A 1
H24A H 0.4858 0.4304 0.8101 0.084 Uiso 0.605(4) 1 calc R U P A 1
H24B H 0.4429 0.4946 0.7886 0.084 Uiso 0.605(4) 1 calc R U P A 1
H24C H 0.4521 0.4725 0.7235 0.084 Uiso 0.605(4) 1 calc R U P A 1
C22A C 0.4013(2) 0.4223(4) 0.6941(4) 0.0453(11) Uani 0.395(4) 1 d D U P A 2
H22A H 0.4169 0.4538 0.6739 0.054 Uiso 0.395(4) 1 calc R U P A 2
C23A C 0.3990(9) 0.3482(7) 0.6661(9) 0.063(2) Uani 0.395(4) 1 d D U P A 2
H23D H 0.4403 0.3299 0.6999 0.095 Uiso 0.395(4) 1 calc R U P A 2
H23E H 0.3796 0.3482 0.6060 0.095 Uiso 0.395(4) 1 calc R U P A 2
H23F H 0.3757 0.3188 0.6743 0.095 Uiso 0.395(4) 1 calc R U P A 2
C24A C 0.4432(4) 0.4271(6) 0.7903(4) 0.0560(13) Uani 0.395(4) 1 d D U P A 2
H24D H 0.4849 0.4172 0.8149 0.084 Uiso 0.395(4) 1 calc R U P A 2
H24E H 0.4306 0.3930 0.8113 0.084 Uiso 0.395(4) 1 calc R U P A 2
H24F H 0.4411 0.4740 0.8067 0.084 Uiso 0.395(4) 1 calc R U P A 2
C25 C 0.31960(10) 0.44839(12) 0.89247(15) 0.0229(5) Uani 1 1 d . . . . .
C26 C 0.35864(13) 0.50131(15) 1.02125(16) 0.0343(6) Uani 1 1 d . . . . .
H26A H 0.3420 0.4907 1.0491 0.041 Uiso 1 1 calc R U . . .
H26B H 0.3786 0.5474 1.0406 0.041 Uiso 1 1 calc R U . . .
C27 C 0.40221(12) 0.44543(15) 1.03928(16) 0.0333(6) Uani 1 1 d . . . . .
H27A H 0.4416 0.4657 1.0622 0.040 Uiso 1 1 calc R U . . .
H27B H 0.4091 0.4107 1.0799 0.040 Uiso 1 1 calc R U . . .
C28 C 0.39721(11) 0.35795(13) 0.94553(15) 0.0260(5) Uani 1 1 d . . . . .
C29 C 0.44809(11) 0.32444(14) 1.01721(17) 0.0335(6) Uani 1 1 d . . . . .
H29 H 0.4642 0.3394 1.0719 0.040 Uiso 1 1 calc R U . . .
C30 C 0.47543(12) 0.26998(15) 1.00999(19) 0.0378(6) Uani 1 1 d . . . . .
H30 H 0.5095 0.2473 1.0595 0.045 Uiso 1 1 calc R U . . .
C31 C 0.45337(12) 0.24833(13) 0.93104(19) 0.0346(6) Uani 1 1 d . . . . .
H31 H 0.4728 0.2116 0.9261 0.042 Uiso 1 1 calc R U . . .
C32 C 0.40297(11) 0.28041(12) 0.85942(17) 0.0287(5) Uani 1 1 d . . . . .
H32 H 0.3880 0.2654 0.8052 0.034 Uiso 1 1 calc R U . . .
C33 C 0.37352(10) 0.33447(12) 0.86491(15) 0.0241(5) Uani 1 1 d . . . . .
C34 C 0.26139(12) 0.54561(12) 0.88657(16) 0.0276(5) Uani 1 1 d . . . . .
C35 C 0.21695(11) 0.54595(12) 0.79790(16) 0.0261(5) Uani 1 1 d . . . . .
C36 C 0.16678(13) 0.59001(13) 0.75879(18) 0.0320(6) Uani 1 1 d . . . . .
H36 H 0.1355 0.5892 0.6989 0.038 Uiso 1 1 calc R U . . .
C37 C 0.16267(14) 0.63494(13) 0.8074(2) 0.0379(7) Uani 1 1 d . . . . .
H37 H 0.1286 0.6649 0.7804 0.045 Uiso 1 1 calc R U . . .
C38 C 0.20742(15) 0.63632(14) 0.8939(2) 0.0392(7) Uani 1 1 d . . . . .
H38 H 0.2048 0.6680 0.9265 0.047 Uiso 1 1 calc R U . . .
C39 C 0.25648(14) 0.59144(13) 0.93392(19) 0.0342(6) Uani 1 1 d . . . . .
H39 H 0.2869 0.5919 0.9939 0.041 Uiso 1 1 calc R U . . .
C40 C 0.17071(11) 0.37022(13) 0.75969(16) 0.0279(5) Uani 1 1 d . . . . .
H40 H 0.1585 0.4197 0.7558 0.033 Uiso 1 1 calc R U . . .
C41 C 0.11496(12) 0.32798(14) 0.69218(18) 0.0344(6) Uani 1 1 d . . . . .
H41A H 0.0851 0.3322 0.6996 0.052 Uiso 1 1 calc R U . . .
H41B H 0.1263 0.2790 0.6972 0.052 Uiso 1 1 calc R U . . .
H41C H 0.0974 0.3454 0.6360 0.052 Uiso 1 1 calc R U . . .
C42 C 0.20183(13) 0.34324(14) 0.84790(17) 0.0335(6) Uani 1 1 d . . . . .
H42A H 0.1728 0.3419 0.8570 0.050 Uiso 1 1 calc R U . . .
H42B H 0.2355 0.3741 0.8898 0.050 Uiso 1 1 calc R U . . .
H42C H 0.2173 0.2963 0.8539 0.050 Uiso 1 1 calc R U . . .
O1S O -0.0025(2) 0.3490(2) 0.3360(3) 0.0552(12) Uani 0.5 1 d D . P B -2
C1S C 0.0202(5) 0.2992(4) 0.3142(5) 0.056(2) Uani 0.5 1 d D . P B -2
H1S1 H 0.0086 0.2517 0.3175 0.068 Uiso 0.5 1 calc R U P B -2
H1S2 H 0.0650 0.3019 0.3526 0.068 Uiso 0.5 1 calc R U P B -2
C2S C -0.0082(4) 0.3167(4) 0.2231(4) 0.057(2) Uani 0.5 1 d D . P B -2
H2S1 H 0.0163 0.2985 0.2094 0.068 Uiso 0.5 1 calc R U P B -2
H2S2 H -0.0500 0.2985 0.1816 0.068 Uiso 0.5 1 calc R U P B -2
C3S C -0.0074(5) 0.3960(3) 0.2259(5) 0.065(2) Uani 0.5 1 d D . P B -2
H3S1 H -0.0437 0.4156 0.1716 0.078 Uiso 0.5 1 calc R U P B -2
H3S2 H 0.0293 0.4146 0.2379 0.078 Uiso 0.5 1 calc R U P B -2
C4S C -0.0070(4) 0.4130(3) 0.2979(4) 0.0527(17) Uani 0.5 1 d D . P B -2
H4S1 H 0.0278 0.4434 0.3401 0.063 Uiso 0.5 1 calc R U P B -2
H4S2 H -0.0447 0.4376 0.2755 0.063 Uiso 0.5 1 calc R U P B -2
O2S O 0.0168(2) 0.5675(2) 0.5669(3) 0.0495(11) Uani 0.5 1 d D . P C -2
C5S C 0.0110(4) 0.4983(4) 0.5840(5) 0.060(2) Uani 0.5 1 d D . P C -2
H5S1 H -0.0122 0.4972 0.6037 0.073 Uiso 0.5 1 calc R U P C -2
H5S2 H 0.0513 0.4775 0.6284 0.073 Uiso 0.5 1 calc R U P C -2
C6S C -0.0227(10) 0.4585(7) 0.5009(7) 0.065(4) Uani 0.5 1 d D . P C -2
H6S1 H -0.0036 0.4127 0.5103 0.078 Uiso 0.5 1 calc R U P C -2
H6S2 H -0.0656 0.4513 0.4736 0.078 Uiso 0.5 1 calc R U P C -2
C7S C -0.0174(4) 0.5054(4) 0.4467(5) 0.059(2) Uani 0.5 1 d D . P C -2
H7S1 H -0.0006 0.4797 0.4248 0.071 Uiso 0.5 1 calc R U P C -2
H7S2 H -0.0571 0.5253 0.3985 0.071 Uiso 0.5 1 calc R U P C -2
C8S C 0.0261(8) 0.5618(7) 0.5091(7) 0.057(3) Uani 0.5 1 d D . P C -2
H8S1 H 0.0685 0.5486 0.5385 0.069 Uiso 0.5 1 calc R U P C -2
H8S2 H 0.0173 0.6066 0.4794 0.069 Uiso 0.5 1 calc R U P C -2


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.8413(17) . ?
Ti1 O5 1.8465(17) . ?
Ti1 O1 1.8811(16) . ?
Ti1 O2 2.0122(16) . ?
Ti1 O4 2.1126(16) . ?
Ti1 C1 2.231(2) . ?
Ti1 Ti2 3.3332(6) . ?
Ti2 O8 1.8145(16) . ?
Ti2 O6 1.8772(16) . ?
Ti2 O7 1.8844(16) . ?
Ti2 O4 1.9646(16) . ?
Ti2 C25 2.210(2) . ?
Ti2 O2 2.2332(16) . ?
O1 C11 1.336(3) . ?
O2 C9 1.358(3) . ?
O3 C16 1.411(3) . ?
O4 C19 1.442(3) . ?
O5 C22 1.404(4) . ?
O5 C22A 1.404(4) . ?
O6 C35 1.331(3) . ?
O7 C33 1.327(3) . ?
O8 C40 1.431(3) . ?
N1 C1 1.336(3) . ?
N1 C10 1.410(3) . ?
N1 C2 1.478(3) . ?
N2 C1 1.340(3) . ?
N2 C4 1.408(3) . ?
N2 C3 1.485(3) . ?
N3 C25 1.345(3) . ?
N3 C34 1.415(3) . ?
N3 C26 1.474(3) . ?
N4 C25 1.348(3) . ?
N4 C28 1.412(3) . ?
N4 C27 1.479(3) . ?
C2 C3 1.515(3) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 C5 1.396(3) . ?
C4 C9 1.406(3) . ?
C5 C6 1.381(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.380(4) . ?
C6 H6 0.9500 . ?
C7 C8 1.392(4) . ?
C7 H7 0.9500 . ?
C8 C9 1.390(3) . ?
C8 H8 0.9500 . ?
C10 C15 1.391(3) . ?
C10 C11 1.415(3) . ?
C11 C12 1.397(3) . ?
C12 C13 1.381(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(4) . ?
C13 H13 0.9500 . ?
C14 C15 1.380(4) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C18 1.511(4) . ?
C16 C17 1.516(4) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C21 1.512(4) . ?
C19 C20 1.515(4) . ?
C19 H19 1.0000 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C21 H21A 0.9800 . ?
C21 H21B 0.9800 . ?
C21 H21C 0.9800 . ?
C22 C23 1.524(4) . ?
C22 C24 1.524(4) . ?
C22 H22 1.0000 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C22A C24A 1.524(4) . ?
C22A C23A 1.524(4) . ?
C22A H22A 1.0000 . ?
C23A H23D 0.9800 . ?
C23A H23E 0.9800 . ?
C23A H23F 0.9800 . ?
C24A H24D 0.9800 . ?
C24A H24E 0.9800 . ?
C24A H24F 0.9800 . ?
C26 C27 1.511(4) . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C28 C29 1.398(3) . ?
C28 C33 1.409(3) . ?
C29 C30 1.381(4) . ?
C29 H29 0.9500 . ?
C30 C31 1.381(4) . ?
C30 H30 0.9500 . ?
C31 C32 1.380(4) . ?
C31 H31 0.9500 . ?
C32 C33 1.398(3) . ?
C32 H32 0.9500 . ?
C34 C39 1.396(3) . ?
C34 C35 1.402(4) . ?
C35 C36 1.401(4) . ?
C36 C37 1.392(4) . ?
C36 H36 0.9500 . ?
C37 C38 1.372(4) . ?
C37 H37 0.9500 . ?
C38 C39 1.388(4) . ?
C38 H38 0.9500 . ?
C39 H39 0.9500 . ?
C40 C42 1.513(4) . ?
C40 C41 1.515(4) . ?
C40 H40 1.0000 . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
O1S C1S 1.397(10) . ?
O1S C4S 1.424(7) . ?
C1S C2S 1.533(5) . ?
C1S H1S1 0.9900 . ?
C1S H1S2 0.9900 . ?
C2S C3S 1.524(5) . ?
C2S H2S1 0.9900 . ?
C2S H2S2 0.9900 . ?
C3S C4S 1.525(5) . ?
C3S H3S1 0.9900 . ?
C3S H3S2 0.9900 . ?
C4S H4S1 0.9900 . ?
C4S H4S2 0.9900 . ?
O2S C8S 1.397(11) . ?
O2S C5S 1.415(8) . ?
C5S C6S 1.526(5) . ?
C5S H5S1 0.9900 . ?
C5S H5S2 0.9900 . ?
C6S C7S 1.526(5) . ?
C6S H6S1 0.9900 . ?
C6S H6S2 0.9900 . ?
C7S C8S 1.524(5) . ?
C7S H7S1 0.9900 . ?
C7S H7S2 0.9900 . ?
C8S H8S1 0.9900 . ?
C8S H8S2 0.9900 . ?

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 O5 96.01(8) . . ?
O3 Ti1 O1 98.67(7) . . ?
O5 Ti1 O1 102.83(7) . . ?
O3 Ti1 O2 95.53(7) . . ?
O5 Ti1 O2 96.96(7) . . ?
O1 Ti1 O2 154.18(7) . . ?
O3 Ti1 O4 168.39(7) . . ?
O5 Ti1 O4 91.03(7) . . ?
O1 Ti1 O4 88.71(7) . . ?
O2 Ti1 O4 74.40(6) . . ?
O3 Ti1 C1 83.55(8) . . ?
O5 Ti1 C1 175.19(8) . . ?
O1 Ti1 C1 81.96(8) . . ?
O2 Ti1 C1 78.34(7) . . ?
O4 Ti1 C1 88.67(7) . . ?
O3 Ti1 Ti2 135.83(5) . . ?
O5 Ti1 Ti2 95.37(5) . . ?
O1 Ti1 Ti2 119.97(5) . . ?
O2 Ti1 Ti2 40.68(5) . . ?
O4 Ti1 Ti2 33.72(4) . . ?
C1 Ti1 Ti2 81.74(6) . . ?
O8 Ti2 O6 92.02(7) . . ?
O8 Ti2 O7 93.02(7) . . ?
O6 Ti2 O7 163.13(7) . . ?
O8 Ti2 O4 108.29(7) . . ?
O6 Ti2 O4 96.69(7) . . ?
O7 Ti2 O4 96.99(7) . . ?
O8 Ti2 C25 96.01(8) . . ?
O6 Ti2 C25 81.38(8) . . ?
O7 Ti2 C25 82.08(8) . . ?
O4 Ti2 C25 155.69(8) . . ?
O8 Ti2 O2 178.27(7) . . ?
O6 Ti2 O2 89.32(7) . . ?
O7 Ti2 O2 85.39(7) . . ?
O4 Ti2 O2 72.62(6) . . ?
C25 Ti2 O2 83.11(7) . . ?
O8 Ti2 Ti1 144.95(5) . . ?
O6 Ti2 Ti1 93.04(5) . . ?
O7 Ti2 Ti1 92.05(5) . . ?
O4 Ti2 Ti1 36.66(5) . . ?
C25 Ti2 Ti1 119.05(6) . . ?
O2 Ti2 Ti1 35.97(4) . . ?
C11 O1 Ti1 138.29(15) . . ?
C9 O2 Ti1 123.81(14) . . ?
C9 O2 Ti2 121.97(13) . . ?
Ti1 O2 Ti2 103.34(7) . . ?
C16 O3 Ti1 144.91(16) . . ?
C19 O4 Ti2 127.61(14) . . ?
C19 O4 Ti1 120.47(13) . . ?
Ti2 O4 Ti1 109.62(7) . . ?
C22 O5 Ti1 134.8(2) . . ?
C22A O5 Ti1 141.6(3) . . ?
C35 O6 Ti2 142.11(16) . . ?
C33 O7 Ti2 141.81(15) . . ?
C40 O8 Ti2 134.86(14) . . ?
C1 N1 C10 125.86(19) . . ?
C1 N1 C2 112.90(19) . . ?
C10 N1 C2 121.07(19) . . ?
C1 N2 C4 124.7(2) . . ?
C1 N2 C3 113.30(19) . . ?
C4 N2 C3 121.70(19) . . ?
C25 N3 C34 127.0(2) . . ?
C25 N3 C26 113.0(2) . . ?
C34 N3 C26 119.9(2) . . ?
C25 N4 C28 126.8(2) . . ?
C25 N4 C27 112.7(2) . . ?
C28 N4 C27 120.2(2) . . ?
N1 C1 N2 108.1(2) . . ?
N1 C1 Ti1 125.96(16) . . ?
N2 C1 Ti1 125.41(17) . . ?
N1 C2 C3 103.16(19) . . ?
N1 C2 H2A 111.1 . . ?
C3 C2 H2A 111.1 . . ?
N1 C2 H2B 111.1 . . ?
C3 C2 H2B 111.1 . . ?
H2A C2 H2B 109.1 . . ?
N2 C3 C2 101.89(18) . . ?
N2 C3 H3A 111.4 . . ?
C2 C3 H3A 111.4 . . ?
N2 C3 H3B 111.4 . . ?
C2 C3 H3B 111.4 . . ?
H3A C3 H3B 109.3 . . ?
C5 C4 C9 119.0(2) . . ?
C5 C4 N2 120.0(2) . . ?
C9 C4 N2 121.0(2) . . ?
C6 C5 C4 120.9(2) . . ?
C6 C5 H5 119.5 . . ?
C4 C5 H5 119.5 . . ?
C7 C6 C5 120.2(2) . . ?
C7 C6 H6 119.9 . . ?
C5 C6 H6 119.9 . . ?
C6 C7 C8 119.5(2) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C9 C8 C7 121.1(2) . . ?
C9 C8 H8 119.5 . . ?
C7 C8 H8 119.5 . . ?
O2 C9 C8 119.2(2) . . ?
O2 C9 C4 121.7(2) . . ?
C8 C9 C4 119.0(2) . . ?
C15 C10 N1 119.5(2) . . ?
C15 C10 C11 119.4(2) . . ?
N1 C10 C11 121.2(2) . . ?
O1 C11 C12 119.2(2) . . ?
O1 C11 C10 122.4(2) . . ?
C12 C11 C10 118.3(2) . . ?
C13 C12 C11 121.3(2) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C12 C13 C14 119.9(2) . . ?
C12 C13 H13 120.0 . . ?
C14 C13 H13 120.0 . . ?
C15 C14 C13 120.0(2) . . ?
C15 C14 H14 120.0 . . ?
C13 C14 H14 120.0 . . ?
C14 C15 C10 121.0(2) . . ?
C14 C15 H15 119.5 . . ?
C10 C15 H15 119.5 . . ?
O3 C16 C18 108.2(2) . . ?
O3 C16 C17 110.6(2) . . ?
C18 C16 C17 112.7(2) . . ?
O3 C16 H16 108.4 . . ?
C18 C16 H16 108.4 . . ?
C17 C16 H16 108.4 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O4 C19 C21 109.2(2) . . ?
O4 C19 C20 110.4(2) . . ?
C21 C19 C20 113.6(3) . . ?
O4 C19 H19 107.8 . . ?
C21 C19 H19 107.8 . . ?
C20 C19 H19 107.8 . . ?
C19 C20 H20A 109.5 . . ?
C19 C20 H20B 109.5 . . ?
H20A C20 H20B 109.5 . . ?
C19 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C19 C21 H21A 109.5 . . ?
C19 C21 H21B 109.5 . . ?
H21A C21 H21B 109.5 . . ?
C19 C21 H21C 109.5 . . ?
H21A C21 H21C 109.5 . . ?
H21B C21 H21C 109.5 . . ?
O5 C22 C23 109.0(5) . . ?
O5 C22 C24 109.4(3) . . ?
C23 C22 C24 110.9(6) . . ?
O5 C22 H22 109.2 . . ?
C23 C22 H22 109.2 . . ?
C24 C22 H22 109.2 . . ?
C22 C23 H23A 109.5 . . ?
C22 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C22 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
C22 C24 H24A 109.5 . . ?
C22 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
C22 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
O5 C22A C24A 112.1(5) . . ?
O5 C22A C23A 107.3(10) . . ?
C24A C22A C23A 110.9(6) . . ?
O5 C22A H22A 108.8 . . ?
C24A C22A H22A 108.8 . . ?
C23A C22A H22A 108.8 . . ?
C22A C23A H23D 109.5 . . ?
C22A C23A H23E 109.5 . . ?
H23D C23A H23E 109.5 . . ?
C22A C23A H23F 109.5 . . ?
H23D C23A H23F 109.5 . . ?
H23E C23A H23F 109.5 . . ?
C22A C24A H24D 109.5 . . ?
C22A C24A H24E 109.5 . . ?
H24D C24A H24E 109.5 . . ?
C22A C24A H24F 109.5 . . ?
H24D C24A H24F 109.5 . . ?
H24E C24A H24F 109.5 . . ?
N3 C25 N4 107.9(2) . . ?
N3 C25 Ti2 126.07(17) . . ?
N4 C25 Ti2 125.86(17) . . ?
N3 C26 C27 103.1(2) . . ?
N3 C26 H26A 111.2 . . ?
C27 C26 H26A 111.2 . . ?
N3 C26 H26B 111.2 . . ?
C27 C26 H26B 111.2 . . ?
H26A C26 H26B 109.1 . . ?
N4 C27 C26 102.9(2) . . ?
N4 C27 H27A 111.2 . . ?
C26 C27 H27A 111.2 . . ?
N4 C27 H27B 111.2 . . ?
C26 C27 H27B 111.2 . . ?
H27A C27 H27B 109.1 . . ?
C29 C28 C33 118.6(2) . . ?
C29 C28 N4 119.9(2) . . ?
C33 C28 N4 121.4(2) . . ?
C30 C29 C28 121.2(3) . . ?
C30 C29 H29 119.4 . . ?
C28 C29 H29 119.4 . . ?
C29 C30 C31 120.2(2) . . ?
C29 C30 H30 119.9 . . ?
C31 C30 H30 119.9 . . ?
C32 C31 C30 119.5(3) . . ?
C32 C31 H31 120.2 . . ?
C30 C31 H31 120.2 . . ?
C31 C32 C33 121.4(3) . . ?
C31 C32 H32 119.3 . . ?
C33 C32 H32 119.3 . . ?
O7 C33 C32 119.2(2) . . ?
O7 C33 C28 121.8(2) . . ?
C32 C33 C28 119.0(2) . . ?
C39 C34 C35 119.6(2) . . ?
C39 C34 N3 119.9(2) . . ?
C35 C34 N3 120.5(2) . . ?
O6 C35 C36 118.9(2) . . ?
O6 C35 C34 122.0(2) . . ?
C36 C35 C34 119.1(2) . . ?
C37 C36 C35 120.2(3) . . ?
C37 C36 H36 119.9 . . ?
C35 C36 H36 119.9 . . ?
C38 C37 C36 120.5(3) . . ?
C38 C37 H37 119.8 . . ?
C36 C37 H37 119.8 . . ?
C37 C38 C39 120.1(2) . . ?
C37 C38 H38 119.9 . . ?
C39 C38 H38 119.9 . . ?
C38 C39 C34 120.4(3) . . ?
C38 C39 H39 119.8 . . ?
C34 C39 H39 119.8 . . ?
O8 C40 C42 108.5(2) . . ?
O8 C40 C41 109.6(2) . . ?
C42 C40 C41 112.0(2) . . ?
O8 C40 H40 108.9 . . ?
C42 C40 H40 108.9 . . ?
C41 C40 H40 108.9 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C1S O1S C4S 107.6(5) . . ?
O1S C1S C2S 105.2(5) . . ?
O1S C1S H1S1 110.7 . . ?
C2S C1S H1S1 110.7 . . ?
O1S C1S H1S2 110.7 . . ?
C2S C1S H1S2 110.7 . . ?
H1S1 C1S H1S2 108.8 . . ?
C3S C2S C1S 100.9(5) . . ?
C3S C2S H2S1 111.6 . . ?
C1S C2S H2S1 111.6 . . ?
C3S C2S H2S2 111.6 . . ?
C1S C2S H2S2 111.6 . . ?
H2S1 C2S H2S2 109.4 . . ?
C2S C3S C4S 104.0(5) . . ?
C2S C3S H3S1 111.0 . . ?
C4S C3S H3S1 111.0 . . ?
C2S C3S H3S2 111.0 . . ?
C4S C3S H3S2 111.0 . . ?
H3S1 C3S H3S2 109.0 . . ?
O1S C4S C3S 107.5(5) . . ?
O1S C4S H4S1 110.2 . . ?
C3S C4S H4S1 110.2 . . ?
O1S C4S H4S2 110.2 . . ?
C3S C4S H4S2 110.2 . . ?
H4S1 C4S H4S2 108.5 . . ?
C8S O2S C5S 105.4(7) . . ?
O2S C5S C6S 106.2(7) . . ?
O2S C5S H5S1 110.5 . . ?
C6S C5S H5S1 110.5 . . ?
O2S C5S H5S2 110.5 . . ?
C6S C5S H5S2 110.5 . . ?
H5S1 C5S H5S2 108.7 . . ?
C7S C6S C5S 104.0(8) . . ?
C7S C6S H6S1 111.0 . . ?
C5S C6S H6S1 111.0 . . ?
C7S C6S H6S2 111.0 . . ?
C5S C6S H6S2 111.0 . . ?
H6S1 C6S H6S2 109.0 . . ?
C8S C7S C6S 102.6(7) . . ?
C8S C7S H7S1 111.2 . . ?
C6S C7S H7S1 111.2 . . ?
C8S C7S H7S2 111.2 . . ?
C6S C7S H7S2 111.2 . . ?
H7S1 C7S H7S2 109.2 . . ?
O2S C8S C7S 105.6(8) . . ?
O2S C8S H8S1 110.6 . . ?
C7S C8S H8S1 110.6 . . ?
O2S C8S H8S2 110.6 . . ?
C7S C8S H8S2 110.6 . . ?
H8S1 C8S H8S2 108.7 . . ?

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 -104.7(2) . . . . ?
O5 Ti1 O1 C11 157.0(2) . . . . ?
O2 Ti1 O1 C11 17.9(3) . . . . ?
O4 Ti1 O1 C11 66.3(2) . . . . ?
C1 Ti1 O1 C11 -22.6(2) . . . . ?
Ti2 Ti1 O1 C11 53.0(2) . . . . ?
O5 Ti1 O3 C16 161.6(3) . . . . ?
O1 Ti1 O3 C16 57.6(3) . . . . ?
O2 Ti1 O3 C16 -100.7(3) . . . . ?
O4 Ti1 O3 C16 -71.3(5) . . . . ?
C1 Ti1 O3 C16 -23.2(3) . . . . ?
Ti2 Ti1 O3 C16 -94.3(3) . . . . ?
O3 Ti1 O5 C22 75.2(3) . . . . ?
O1 Ti1 O5 C22 175.5(3) . . . . ?
O2 Ti1 O5 C22 -21.2(3) . . . . ?
O4 Ti1 O5 C22 -95.6(3) . . . . ?
Ti2 Ti1 O5 C22 -62.1(3) . . . . ?
O3 Ti1 O5 C22A 28.8(5) . . . . ?
O1 Ti1 O5 C22A 129.1(5) . . . . ?
O2 Ti1 O5 C22A -67.6(5) . . . . ?
O4 Ti1 O5 C22A -142.0(5) . . . . ?
Ti2 Ti1 O5 C22A -108.5(5) . . . . ?
O8 Ti2 O6 C35 87.2(2) . . . . ?
O7 Ti2 O6 C35 -20.1(4) . . . . ?
O4 Ti2 O6 C35 -164.1(2) . . . . ?
C25 Ti2 O6 C35 -8.5(2) . . . . ?
O2 Ti2 O6 C35 -91.7(2) . . . . ?
Ti1 Ti2 O6 C35 -127.5(2) . . . . ?
O8 Ti2 O7 C33 -94.2(2) . . . . ?
O6 Ti2 O7 C33 12.9(4) . . . . ?
O4 Ti2 O7 C33 156.9(2) . . . . ?
C25 Ti2 O7 C33 1.4(2) . . . . ?
O2 Ti2 O7 C33 85.1(2) . . . . ?
Ti1 Ti2 O7 C33 120.5(2) . . . . ?
O6 Ti2 O8 C40 -20.0(2) . . . . ?
O7 Ti2 O8 C40 143.9(2) . . . . ?
O4 Ti2 O8 C40 -117.7(2) . . . . ?
C25 Ti2 O8 C40 61.6(2) . . . . ?
Ti1 Ti2 O8 C40 -118.19(19) . . . . ?
C10 N1 C1 N2 -178.5(2) . . . . ?
C2 N1 C1 N2 -3.1(3) . . . . ?
C10 N1 C1 Ti1 9.5(3) . . . . ?
C2 N1 C1 Ti1 -175.11(16) . . . . ?
C4 N2 C1 N1 -176.18(19) . . . . ?
C3 N2 C1 N1 -2.5(3) . . . . ?
C4 N2 C1 Ti1 -4.2(3) . . . . ?
C3 N2 C1 Ti1 169.51(15) . . . . ?
C1 N1 C2 C3 7.1(3) . . . . ?
C10 N1 C2 C3 -177.24(19) . . . . ?
C1 N2 C3 C2 6.7(2) . . . . ?
C4 N2 C3 C2 -179.43(19) . . . . ?
N1 C2 C3 N2 -7.6(2) . . . . ?
C1 N2 C4 C5 165.2(2) . . . . ?
C3 N2 C4 C5 -8.0(3) . . . . ?
C1 N2 C4 C9 -15.8(3) . . . . ?
C3 N2 C4 C9 171.0(2) . . . . ?
C9 C4 C5 C6 3.0(3) . . . . ?
N2 C4 C5 C6 -178.0(2) . . . . ?
C4 C5 C6 C7 1.4(4) . . . . ?
C5 C6 C7 C8 -3.1(4) . . . . ?
C6 C7 C8 C9 0.2(4) . . . . ?
Ti1 O2 C9 C8 -128.51(19) . . . . ?
Ti2 O2 C9 C8 93.3(2) . . . . ?
Ti1 O2 C9 C4 54.4(3) . . . . ?
Ti2 O2 C9 C4 -83.8(2) . . . . ?
C7 C8 C9 O2 -173.0(2) . . . . ?
C7 C8 C9 C4 4.2(3) . . . . ?
C5 C4 C9 O2 171.4(2) . . . . ?
N2 C4 C9 O2 -7.6(3) . . . . ?
C5 C4 C9 C8 -5.7(3) . . . . ?
N2 C4 C9 C8 175.3(2) . . . . ?
C1 N1 C10 C15 168.4(2) . . . . ?
C2 N1 C10 C15 -6.6(3) . . . . ?
C1 N1 C10 C11 -12.0(3) . . . . ?
C2 N1 C10 C11 173.0(2) . . . . ?
Ti1 O1 C11 C12 -155.08(18) . . . . ?
Ti1 O1 C11 C10 26.3(3) . . . . ?
C15 C10 C11 O1 176.0(2) . . . . ?
N1 C10 C11 O1 -3.7(3) . . . . ?
C15 C10 C11 C12 -2.6(3) . . . . ?
N1 C10 C11 C12 177.7(2) . . . . ?
O1 C11 C12 C13 -176.8(2) . . . . ?
C10 C11 C12 C13 1.9(4) . . . . ?
C11 C12 C13 C14 -0.1(4) . . . . ?
C12 C13 C14 C15 -1.0(4) . . . . ?
C13 C14 C15 C10 0.2(4) . . . . ?
N1 C10 C15 C14 -178.7(2) . . . . ?
C11 C10 C15 C14 1.6(4) . . . . ?
Ti1 O3 C16 C18 166.8(2) . . . . ?
Ti1 O3 C16 C17 -69.3(3) . . . . ?
Ti2 O4 C19 C21 73.7(3) . . . . ?
Ti1 O4 C19 C21 -125.36(19) . . . . ?
Ti2 O4 C19 C20 -51.8(3) . . . . ?
Ti1 O4 C19 C20 109.1(2) . . . . ?
Ti1 O5 C22 C23 171.4(7) . . . . ?
Ti1 O5 C22 C24 -67.2(5) . . . . ?
Ti1 O5 C22A C24A 54.2(9) . . . . ?
Ti1 O5 C22A C23A 176.1(10) . . . . ?
C34 N3 C25 N4 -176.8(2) . . . . ?
C26 N3 C25 N4 0.5(3) . . . . ?
C34 N3 C25 Ti2 7.3(3) . . . . ?
C26 N3 C25 Ti2 -175.44(16) . . . . ?
C28 N4 C25 N3 -178.5(2) . . . . ?
C27 N4 C25 N3 -4.3(3) . . . . ?
C28 N4 C25 Ti2 -2.6(3) . . . . ?
C27 N4 C25 Ti2 171.56(16) . . . . ?
C25 N3 C26 C27 3.3(3) . . . . ?
C34 N3 C26 C27 -179.2(2) . . . . ?
C25 N4 C27 C26 6.2(3) . . . . ?
C28 N4 C27 C26 -179.2(2) . . . . ?
N3 C26 C27 N4 -5.3(2) . . . . ?
C25 N4 C28 C29 -175.5(2) . . . . ?
C27 N4 C28 C29 10.8(3) . . . . ?
C25 N4 C28 C33 4.4(4) . . . . ?
C27 N4 C28 C33 -169.3(2) . . . . ?
C33 C28 C29 C30 0.8(4) . . . . ?
N4 C28 C29 C30 -179.3(2) . . . . ?
C28 C29 C30 C31 1.2(4) . . . . ?
C29 C30 C31 C32 -1.5(4) . . . . ?
C30 C31 C32 C33 -0.1(4) . . . . ?
Ti2 O7 C33 C32 179.10(17) . . . . ?
Ti2 O7 C33 C28 -0.1(4) . . . . ?
C31 C32 C33 O7 -177.1(2) . . . . ?
C31 C32 C33 C28 2.1(3) . . . . ?
C29 C28 C33 O7 176.8(2) . . . . ?
N4 C28 C33 O7 -3.1(3) . . . . ?
C29 C28 C33 C32 -2.4(3) . . . . ?
N4 C28 C33 C32 177.7(2) . . . . ?
C25 N3 C34 C39 174.3(2) . . . . ?
C26 N3 C34 C39 -2.7(3) . . . . ?
C25 N3 C34 C35 -5.5(4) . . . . ?
C26 N3 C34 C35 177.4(2) . . . . ?
Ti2 O6 C35 C36 -167.68(18) . . . . ?
Ti2 O6 C35 C34 12.0(4) . . . . ?
C39 C34 C35 O6 177.1(2) . . . . ?
N3 C34 C35 O6 -3.1(3) . . . . ?
C39 C34 C35 C36 -3.2(3) . . . . ?
N3 C34 C35 C36 176.6(2) . . . . ?
O6 C35 C36 C37 -177.4(2) . . . . ?
C34 C35 C36 C37 2.8(4) . . . . ?
C35 C36 C37 C38 -0.3(4) . . . . ?
C36 C37 C38 C39 -1.7(4) . . . . ?
C37 C38 C39 C34 1.3(4) . . . . ?
C35 C34 C39 C38 1.2(4) . . . . ?
N3 C34 C39 C38 -178.6(2) . . . . ?
Ti2 O8 C40 C42 -96.1(2) . . . . ?
Ti2 O8 C40 C41 141.41(19) . . . . ?
C4S O1S C1S C2S -36.6(9) . . . . ?
O1S C1S C2S C3S 37.9(9) . . . . ?
C1S C2S C3S C4S -24.7(9) . . . . ?
C1S O1S C4S C3S 19.9(9) . . . . ?
C2S C3S C4S O1S 4.8(10) . . . . ?
C8S O2S C5S C6S -36.2(9) . . . . ?
O2S C5S C6S C7S 16.3(16) . . . . ?
C5S C6S C7S C8S 8(2) . . . . ?
C5S O2S C8S C7S 41.6(13) . . . . ?
C6S C7S C8S O2S -30(2) . . . . ?

_refine_diff_density_max         0.691
_refine_diff_density_min         -0.489
_refine_diff_density_rms         0.070


_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method 'THF/Pentane 1:5'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
####################################################################### 
# 
# 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_Compound3
_database_code_depnum_ccdc_archive 'CCDC 1476530'
_audit_update_record             
;
2016-04-26 deposited with the CCDC.
2016-06-14 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/7
_shelx_SHELXL_version_number     2014/7
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         '2(C33 H42 N2 O4 Ti), 2.5(C6 H14)'
_chemical_formula_sum            'C81 H119 N4 O8 Ti2'
_chemical_formula_weight         1372.59

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'
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'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   16.7643(16)
_cell_length_b                   27.625(3)
_cell_length_c                   17.7509(17)
_cell_angle_alpha                90
_cell_angle_beta                 112.6230(10)
_cell_angle_gamma                90
_cell_volume                     7588.2(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    103(2)
_cell_measurement_reflns_used    9958
_cell_measurement_theta_min      2.25
_cell_measurement_theta_max      25.21

_exptl_crystal_description       'long prism'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.201
_exptl_crystal_F_000             2964
_exptl_transmission_factor_min   0.4837
_exptl_transmission_factor_max   0.7452
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.252
_exptl_crystal_size_min          0.118
_exptl_absorpt_coefficient_mu    0.267
_shelx_estimated_absorpt_T_min   0.882
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   'SADABS 2012/1'
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      103(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Bruker TXS Rotating anode'
_diffrn_measurement_device_type  'Bruker APEX-II Pt135 CCD'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            88763
_diffrn_reflns_av_unetI/netI     0.0435
_diffrn_reflns_av_R_equivalents  0.0648
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.928
_diffrn_reflns_theta_max         25.290
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             13786
_reflns_number_gt                11119
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXT (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0915P)²+8.6884P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         13786
_refine_ls_number_parameters     879
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0739
_refine_ls_R_factor_gt           0.0587
_refine_ls_wR_factor_ref         0.1785
_refine_ls_wR_factor_gt          0.1672
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_restrained_S_all      1.089
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.62585(17) 0.25714(10) 0.52299(17) 0.0230(6) Uani 1 1 d . . . . .
N1 N 0.64547(15) 0.27789(8) 0.59622(14) 0.0241(5) Uani 1 1 d . . . . .
O1 O 0.68868(13) 0.33944(7) 0.49063(12) 0.0276(4) Uani 1 1 d . . . . .
Ti1 Ti 0.67169(3) 0.28206(2) 0.42816(3) 0.02145(14) Uani 1 1 d . . . . .
C2 C 0.6091(2) 0.25181(11) 0.64825(18) 0.0296(6) Uani 1 1 d . . . . .
H2A H 0.5657 0.2718 0.6592 0.036 Uiso 1 1 calc R U . . .
H2B H 0.6550 0.2422 0.7008 0.036 Uiso 1 1 calc R U . . .
N2 N 0.57823(15) 0.21724(8) 0.51945(14) 0.0238(5) Uani 1 1 d . . . . .
O2 O 0.60929(13) 0.22705(7) 0.37578(12) 0.0270(4) Uani 1 1 d . . . . .
Ti2 Ti 0.21672(3) 0.44260(2) 0.39683(3) 0.02213(14) Uani 1 1 d . . . . .
C3 C 0.5673(2) 0.20777(11) 0.59711(18) 0.0291(6) Uani 1 1 d . . . . .
H3A H 0.5972 0.1776 0.6231 0.035 Uiso 1 1 calc R U . . .
H3B H 0.5055 0.2054 0.5883 0.035 Uiso 1 1 calc R U . . .
N3 N 0.31847(16) 0.49439(9) 0.56892(15) 0.0304(6) Uani 1 1 d . . . . .
O3 O 0.77833(13) 0.25905(7) 0.46890(13) 0.0301(5) Uani 1 1 d . . . . .
C4 C 0.54268(18) 0.18482(10) 0.45353(18) 0.0253(6) Uani 1 1 d . . . . .
N4 N 0.37091(15) 0.51768(8) 0.48005(15) 0.0281(5) Uani 1 1 d . . . . .
O4 O 0.64647(12) 0.31708(6) 0.33226(11) 0.0213(4) Uani 1 1 d . . . . .
C5 C 0.4914(2) 0.14625(10) 0.4584(2) 0.0325(7) Uani 1 1 d . . . . .
H5 H 0.4817 0.1412 0.5071 0.039 Uiso 1 1 calc R U . . .
O5 O 0.18619(14) 0.42835(7) 0.48509(12) 0.0296(5) Uani 1 1 d . . . . .
C6 C 0.4545(2) 0.11539(11) 0.3932(2) 0.0381(8) Uani 1 1 d . . . . .
H6 H 0.4189 0.0895 0.3970 0.046 Uiso 1 1 calc R U . . .
O6 O 0.28927(12) 0.45910(7) 0.34157(12) 0.0269(4) Uani 1 1 d . . . . .
C7 C 0.4691(2) 0.12181(11) 0.3224(2) 0.0357(7) Uani 1 1 d . . . . .
H7 H 0.4432 0.1006 0.2774 0.043 Uiso 1 1 calc R U . . .
O7 O 0.12811(13) 0.48207(7) 0.34346(13) 0.0296(5) Uani 1 1 d . . . . .
C8 C 0.5214(2) 0.15933(11) 0.3173(2) 0.0319(7) Uani 1 1 d . . . . .
H8 H 0.5318 0.1634 0.2687 0.038 Uiso 1 1 calc R U . . .
O8 O 0.19689(12) 0.38093(7) 0.35451(11) 0.0225(4) Uani 1 1 d . . . . .
C9 C 0.55917(18) 0.19121(10) 0.38211(18) 0.0256(6) Uani 1 1 d . . . . .
C10 C 0.69338(18) 0.32083(10) 0.62419(17) 0.0249(6) Uani 1 1 d . . . . .
C11 C 0.71497(18) 0.35008(10) 0.56999(17) 0.0245(6) Uani 1 1 d . . . . .
C12 C 0.76332(19) 0.39192(10) 0.59979(18) 0.0277(6) Uani 1 1 d . . . . .
H12 H 0.7794 0.4115 0.5639 0.033 Uiso 1 1 calc R U . . .
C13 C 0.7884(2) 0.40556(11) 0.68069(19) 0.0333(7) Uani 1 1 d . . . . .
H13 H 0.8215 0.4341 0.7000 0.040 Uiso 1 1 calc R U . . .
C14 C 0.7650(2) 0.37741(12) 0.73320(19) 0.0374(7) Uani 1 1 d . . . . .
H14 H 0.7810 0.3870 0.7885 0.045 Uiso 1 1 calc R U . . .
C15 C 0.7182(2) 0.33528(11) 0.70531(18) 0.0332(7) Uani 1 1 d . . . . .
H15 H 0.7028 0.3160 0.7419 0.040 Uiso 1 1 calc R U . . .
C16 C 0.8320(2) 0.21722(11) 0.49556(19) 0.0327(7) Uani 1 1 d . . . . .
H16 H 0.8937 0.2279 0.5176 0.039 Uiso 1 1 calc R U . . .
C17 C 0.8175(2) 0.18455(13) 0.4239(2) 0.0403(8) Uani 1 1 d . . . . .
H17A H 0.8565 0.1567 0.4413 0.060 Uiso 1 1 calc R U . . .
H17B H 0.8292 0.2024 0.3815 0.060 Uiso 1 1 calc R U . . .
H17C H 0.7575 0.1733 0.4020 0.060 Uiso 1 1 calc R U . . .
C18 C 0.8138(2) 0.19293(13) 0.5638(2) 0.0405(8) Uani 1 1 d . . . . .
H18A H 0.8535 0.1656 0.5850 0.061 Uiso 1 1 calc R U . . .
H18B H 0.7541 0.1812 0.5428 0.061 Uiso 1 1 calc R U . . .
H18C H 0.8222 0.2163 0.6077 0.061 Uiso 1 1 calc R U . . .
C19 C 0.62113(17) 0.35381(9) 0.27820(16) 0.0199(5) Uani 1 1 d . . . . .
C20 C 0.53199(17) 0.36580(9) 0.24056(16) 0.0216(6) Uani 1 1 d . . . . .
C21 C 0.50861(19) 0.40333(10) 0.18355(17) 0.0269(6) Uani 1 1 d . . . . .
H21 H 0.4495 0.4124 0.1591 0.032 Uiso 1 1 calc R U . . .
C22 C 0.5681(2) 0.42803(10) 0.16109(17) 0.0276(6) Uani 1 1 d . . . . .
C23 C 0.65421(19) 0.41524(10) 0.19826(17) 0.0249(6) Uani 1 1 d . . . . .
H23 H 0.6952 0.4318 0.1827 0.030 Uiso 1 1 calc R U . . .
C24 C 0.68385(17) 0.37905(9) 0.25761(16) 0.0215(6) Uani 1 1 d . . . . .
C25 C 0.5399(2) 0.46820(12) 0.0986(2) 0.0402(8) Uani 1 1 d . . . . .
H25A H 0.5838 0.4729 0.0753 0.060 Uiso 1 1 calc R U . . .
H25B H 0.5329 0.4982 0.1248 0.060 Uiso 1 1 calc R U . . .
H25C H 0.4848 0.4595 0.0550 0.060 Uiso 1 1 calc R U . . .
C26 C 0.46121(18) 0.33883(10) 0.25931(17) 0.0237(6) Uani 1 1 d . . . . .
C27 C 0.45873(19) 0.28508(10) 0.23488(18) 0.0270(6) Uani 1 1 d . . . . .
H27A H 0.4211 0.2671 0.2557 0.040 Uiso 1 1 calc R U . . .
H27B H 0.5173 0.2716 0.2581 0.040 Uiso 1 1 calc R U . . .
H27C H 0.4362 0.2824 0.1753 0.040 Uiso 1 1 calc R U . . .
C28 C 0.4754(2) 0.34338(12) 0.34937(19) 0.0323(7) Uani 1 1 d . . . . .
H28A H 0.4369 0.3210 0.3618 0.048 Uiso 1 1 calc R U . . .
H28B H 0.4630 0.3766 0.3608 0.048 Uiso 1 1 calc R U . . .
H28C H 0.5356 0.3355 0.3833 0.048 Uiso 1 1 calc R U . . .
C29 C 0.37071(19) 0.35877(12) 0.2118(2) 0.0376(8) Uani 1 1 d . . . . .
H29A H 0.3284 0.3401 0.2253 0.056 Uiso 1 1 calc R U . . .
H29B H 0.3574 0.3563 0.1531 0.056 Uiso 1 1 calc R U . . .
H29C H 0.3683 0.3928 0.2264 0.056 Uiso 1 1 calc R U . . .
C30 C 0.78144(18) 0.36859(11) 0.29895(18) 0.0276(6) Uani 1 1 d . . . . .
C31 C 0.8346(2) 0.39943(13) 0.2625(2) 0.0381(8) Uani 1 1 d . . . . .
H31A H 0.8961 0.3919 0.2906 0.057 Uiso 1 1 calc R U . . .
H31B H 0.8250 0.4338 0.2694 0.057 Uiso 1 1 calc R U . . .
H31C H 0.8163 0.3921 0.2042 0.057 Uiso 1 1 calc R U . . .
C32 C 0.8019(2) 0.31548(11) 0.2878(2) 0.0346(7) Uani 1 1 d . . . . .
H32A H 0.8647 0.3108 0.3099 0.052 Uiso 1 1 calc R U . . .
H32B H 0.7780 0.3074 0.2295 0.052 Uiso 1 1 calc R U . . .
H32C H 0.7761 0.2944 0.3167 0.052 Uiso 1 1 calc R U . . .
C33 C 0.8140(2) 0.38189(12) 0.38995(19) 0.0339(7) Uani 1 1 d . . . . .
H33A H 0.8759 0.3747 0.4161 0.051 Uiso 1 1 calc R U . . .
H33B H 0.7824 0.3630 0.4162 0.051 Uiso 1 1 calc R U . . .
H33C H 0.8045 0.4165 0.3955 0.051 Uiso 1 1 calc R U . . .
C34 C 0.31221(19) 0.48859(10) 0.49168(17) 0.0260(6) Uani 1 1 d . . . . .
C35 C 0.3851(2) 0.53006(12) 0.6152(2) 0.0389(8) Uani 1 1 d . . . . .
H35A H 0.4321 0.5146 0.6614 0.047 Uiso 1 1 calc R U . . .
H35B H 0.3598 0.5567 0.6361 0.047 Uiso 1 1 calc R U . . .
C36 C 0.4176(2) 0.54823(11) 0.5519(2) 0.0345(7) Uani 1 1 d . . . . .
H36A H 0.4035 0.5829 0.5397 0.041 Uiso 1 1 calc R U . . .
H36B H 0.4809 0.5438 0.5704 0.041 Uiso 1 1 calc R U . . .
C37 C 0.38578(18) 0.52350(10) 0.40759(19) 0.0292(6) Uani 1 1 d . . . . .
C38 C 0.4426(2) 0.55904(11) 0.4029(2) 0.0366(7) Uani 1 1 d . . . . .
H38 H 0.4718 0.5790 0.4490 0.044 Uiso 1 1 calc R U . . .
C39 C 0.4570(2) 0.56563(12) 0.3321(2) 0.0427(8) Uani 1 1 d . . . . .
H39 H 0.4961 0.5899 0.3297 0.051 Uiso 1 1 calc R U . . .
C40 C 0.4147(2) 0.53687(12) 0.2645(2) 0.0405(8) Uani 1 1 d . . . . .
H40 H 0.4238 0.5418 0.2154 0.049 Uiso 1 1 calc R U . . .
C41 C 0.35921(19) 0.50097(11) 0.26872(19) 0.0313(7) Uani 1 1 d . . . . .
H41 H 0.3311 0.4810 0.2225 0.038 Uiso 1 1 calc R U . . .
C42 C 0.34374(18) 0.49357(10) 0.33957(19) 0.0264(6) Uani 1 1 d . . . . .
C43 C 0.2720(2) 0.46922(11) 0.60791(18) 0.0322(7) Uani 1 1 d . . . . .
C44 C 0.2066(2) 0.43661(10) 0.56465(18) 0.0306(7) Uani 1 1 d . . . . .
C45 C 0.1615(2) 0.41249(11) 0.6050(2) 0.0364(7) Uani 1 1 d . . . . .
H45 H 0.1170 0.3904 0.5757 0.044 Uiso 1 1 calc R U . . .
C46 C 0.1806(3) 0.42031(12) 0.6872(2) 0.0415(8) Uani 1 1 d . . . . .
H46 H 0.1492 0.4038 0.7140 0.050 Uiso 1 1 calc R U . . .
C47 C 0.2453(3) 0.45216(13) 0.7296(2) 0.0470(9) Uani 1 1 d . . . . .
H47 H 0.2587 0.4575 0.7861 0.056 Uiso 1 1 calc R U . . .
C48 C 0.2910(3) 0.47644(12) 0.6914(2) 0.0430(8) Uani 1 1 d . . . . .
H48 H 0.3357 0.4982 0.7217 0.052 Uiso 1 1 calc R U . . .
C49 C 0.0437(2) 0.48848(11) 0.3449(2) 0.0348(7) Uani 1 1 d . . . . .
H49 H 0.0220 0.4564 0.3551 0.042 Uiso 1 1 calc R U . . .
C50 C -0.0157(2) 0.50678(14) 0.2618(2) 0.0467(9) Uani 1 1 d . . . . .
H50A H -0.0741 0.5110 0.2610 0.070 Uiso 1 1 calc R U . . .
H50B H -0.0172 0.4833 0.2199 0.070 Uiso 1 1 calc R U . . .
H50C H 0.0057 0.5379 0.2508 0.070 Uiso 1 1 calc R U . . .
C51 C 0.0494(2) 0.52263(14) 0.4132(2) 0.0495(9) Uani 1 1 d . . . . .
H51A H -0.0076 0.5257 0.4160 0.074 Uiso 1 1 calc R U . . .
H51B H 0.0689 0.5545 0.4030 0.074 Uiso 1 1 calc R U . . .
H51C H 0.0906 0.5098 0.4651 0.074 Uiso 1 1 calc R U . . .
C52 C 0.21267(17) 0.33790(9) 0.32608(17) 0.0225(6) Uani 1 1 d . . . . .
C53 C 0.27263(18) 0.30544(10) 0.38001(17) 0.0245(6) Uani 1 1 d . . . . .
C54 C 0.28789(19) 0.26176(10) 0.34865(19) 0.0281(6) Uani 1 1 d . . . . .
H54 H 0.3293 0.2400 0.3841 0.034 Uiso 1 1 calc R U . . .
C55 C 0.2448(2) 0.24892(11) 0.2677(2) 0.0304(7) Uani 1 1 d . . . . .
C56 C 0.18529(19) 0.28101(11) 0.21690(18) 0.0288(6) Uani 1 1 d . . . . .
H56 H 0.1552 0.2723 0.1613 0.035 Uiso 1 1 calc R U . . .
C57 C 0.16714(18) 0.32574(10) 0.24330(17) 0.0246(6) Uani 1 1 d . . . . .
C58 C 0.2632(2) 0.20099(12) 0.2364(2) 0.0419(8) Uani 1 1 d . . . . .
H58A H 0.2157 0.1930 0.1848 0.063 Uiso 1 1 calc R U . . .
H58B H 0.2685 0.1756 0.2766 0.063 Uiso 1 1 calc R U . . .
H58C H 0.3172 0.2033 0.2275 0.063 Uiso 1 1 calc R U . . .
C59 C 0.3162(2) 0.31620(11) 0.47193(18) 0.0292(6) Uani 1 1 d . . . . .
C60 C 0.2463(2) 0.31743(12) 0.50813(19) 0.0346(7) Uani 1 1 d . . . . .
H60A H 0.2726 0.3268 0.5658 0.052 Uiso 1 1 calc R U . . .
H60B H 0.2201 0.2853 0.5035 0.052 Uiso 1 1 calc R U . . .
H60C H 0.2017 0.3410 0.4782 0.052 Uiso 1 1 calc R U . . .
C61 C 0.3686(2) 0.36372(11) 0.48976(18) 0.0311(7) Uani 1 1 d . . . . .
H61A H 0.3637 0.3799 0.5369 0.047 Uiso 1 1 calc R U . . .
H61B H 0.3460 0.3850 0.4421 0.047 Uiso 1 1 calc R U . . .
H61C H 0.4295 0.3564 0.5016 0.047 Uiso 1 1 calc R U . . .
C62 C 0.3808(2) 0.27658(12) 0.5181(2) 0.0406(8) Uani 1 1 d . . . . .
H62A H 0.4088 0.2855 0.5758 0.061 Uiso 1 1 calc R U . . .
H62B H 0.4248 0.2731 0.4947 0.061 Uiso 1 1 calc R U . . .
H62C H 0.3502 0.2458 0.5134 0.061 Uiso 1 1 calc R U . . .
C63 C 0.09979(19) 0.35994(11) 0.18311(18) 0.0292(6) Uani 1 1 d . . . . .
C64 C 0.02810(19) 0.37163(12) 0.21367(19) 0.0322(7) Uani 1 1 d . . . . .
H64A H -0.0144 0.3931 0.1746 0.048 Uiso 1 1 calc R U . . .
H64B H 0.0532 0.3877 0.2669 0.048 Uiso 1 1 calc R U . . .
H64C H -0.0003 0.3416 0.2190 0.048 Uiso 1 1 calc R U . . .
C65 C 0.0552(2) 0.33671(14) 0.0983(2) 0.0409(8) Uani 1 1 d . . . . .
H65A H 0.0120 0.3591 0.0623 0.061 Uiso 1 1 calc R U . . .
H65B H 0.0268 0.3066 0.1035 0.061 Uiso 1 1 calc R U . . .
H65C H 0.0985 0.3296 0.0753 0.061 Uiso 1 1 calc R U . . .
C66 C 0.1429(2) 0.40650(12) 0.17028(19) 0.0341(7) Uani 1 1 d . . . . .
H66A H 0.0990 0.4277 0.1321 0.051 Uiso 1 1 calc R U . . .
H66B H 0.1863 0.3984 0.1479 0.051 Uiso 1 1 calc R U . . .
H66C H 0.1708 0.4232 0.2227 0.051 Uiso 1 1 calc R U . . .
C1S C 0.0225(12) 0.5807(6) 0.0995(11) 0.299(9) Uani 1 1 d . U . . .
H1SA H 0.0525 0.5970 0.1518 0.448 Uiso 1 1 calc R U . . .
H1SB H -0.0331 0.5682 0.0973 0.448 Uiso 1 1 calc R U . . .
H1SC H 0.0125 0.6037 0.0548 0.448 Uiso 1 1 calc R U . . .
C2S C 0.0767(9) 0.5396(4) 0.0913(8) 0.204(5) Uani 1 1 d . U . . .
H2SA H 0.0816 0.5154 0.1340 0.244 Uiso 1 1 calc R U . . .
H2SB H 0.1356 0.5521 0.1027 0.244 Uiso 1 1 calc R U . . .
C3S C 0.0442(7) 0.5125(5) 0.0059(8) 0.192(5) Uani 1 1 d . U . . .
H3SA H 0.0361 0.5359 -0.0387 0.230 Uiso 1 1 calc R U . . .
H3SB H 0.0870 0.4879 0.0055 0.230 Uiso 1 1 calc R U . . .
C7S C 0.2396(4) 0.3461(2) -0.0442(3) 0.0832(15) Uani 1 1 d . . . . .
H7SA H 0.2053 0.3237 -0.0873 0.100 Uiso 1 1 calc R U . . .
H7SB H 0.2272 0.3407 0.0047 0.100 Uiso 1 1 calc R U . . .
H7SC H 0.3012 0.3406 -0.0314 0.100 Uiso 1 1 calc R U . . .
C8S C 0.2175(4) 0.3954(2) -0.0720(3) 0.0914(19) Uani 1 1 d . . . . .
H8A H 0.1543 0.3996 -0.0894 0.110 Uiso 1 1 calc R U . . .
H8B H 0.2318 0.4006 -0.1206 0.110 Uiso 1 1 calc R U . . .
C9S C 0.2615(3) 0.4335(2) -0.0107(3) 0.0741(14) Uani 1 1 d . . . . .
H9SA H 0.2447 0.4287 0.0365 0.089 Uiso 1 1 calc R U . . .
H9SB H 0.3245 0.4276 0.0088 0.089 Uiso 1 1 calc R U . . .
C10S C 0.2462(4) 0.4845(2) -0.0351(3) 0.0910(17) Uani 1 1 d . . . . .
H10A H 0.1832 0.4905 -0.0561 0.109 Uiso 1 1 calc R U . . .
H10B H 0.2652 0.4900 -0.0807 0.109 Uiso 1 1 calc R U . . .
C11S C 0.2897(4) 0.5210(2) 0.0298(3) 0.0833(15) Uani 1 1 d . . . . .
H11A H 0.2678 0.5164 0.0737 0.100 Uiso 1 1 calc R U . . .
H11B H 0.3522 0.5132 0.0533 0.100 Uiso 1 1 calc R U . . .
C12S C 0.2817(5) 0.5706(2) 0.0092(4) 0.100(2) Uani 1 1 d . . . . .
H12A H 0.3155 0.5898 0.0573 0.120 Uiso 1 1 calc R U . . .
H12B H 0.2208 0.5801 -0.0099 0.120 Uiso 1 1 calc R U . . .
H12C H 0.3032 0.5763 -0.0342 0.120 Uiso 1 1 calc R U . . .
C13S C -0.0246(3) 0.17569(16) 0.1099(3) 0.0665(12) Uani 1 1 d . . . . .
H13A H -0.0707 0.1865 0.0593 0.100 Uiso 1 1 calc R U . . .
H13B H -0.0262 0.1403 0.1136 0.100 Uiso 1 1 calc R U . . .
H13C H 0.0316 0.1857 0.1100 0.100 Uiso 1 1 calc R U . . .
C14S C -0.0376(3) 0.19834(15) 0.1831(3) 0.0546(10) Uani 1 1 d . . . . .
H14A H -0.0299 0.2338 0.1820 0.065 Uiso 1 1 calc R U . . .
H14B H -0.0975 0.1921 0.1782 0.065 Uiso 1 1 calc R U . . .
C15S C 0.0245(3) 0.17869(16) 0.2638(3) 0.0590(11) Uani 1 1 d . . . . .
H15A H 0.0179 0.1431 0.2637 0.071 Uiso 1 1 calc R U . . .
H15B H 0.0843 0.1857 0.2688 0.071 Uiso 1 1 calc R U . . .
C16S C 0.0124(3) 0.19897(16) 0.3373(3) 0.0606(11) Uani 1 1 d . . . . .
H16A H -0.0488 0.1945 0.3299 0.073 Uiso 1 1 calc R U . . .
H16B H 0.0483 0.1799 0.3858 0.073 Uiso 1 1 calc R U . . .
C17S C 0.0350(3) 0.25146(15) 0.3544(3) 0.0544(10) Uani 1 1 d . . . . .
H17D H -0.0035 0.2709 0.3077 0.065 Uiso 1 1 calc R U . . .
H17E H 0.0951 0.2566 0.3587 0.065 Uiso 1 1 calc R U . . .
C18S C 0.0271(3) 0.26987(18) 0.4329(3) 0.0604(11) Uani 1 1 d . . . . .
H18D H 0.0423 0.3043 0.4403 0.091 Uiso 1 1 calc R U . . .
H18E H 0.0663 0.2515 0.4797 0.091 Uiso 1 1 calc R U . . .
H18F H -0.0325 0.2655 0.4288 0.091 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 N1 1.341(4) . ?
C1 N2 1.348(4) . ?
C1 Ti1 2.212(3) . ?
N1 C10 1.411(4) . ?
N1 C2 1.476(4) . ?
O1 C11 1.337(3) . ?
O1 Ti1 1.892(2) . ?
Ti1 O3 1.769(2) . ?
Ti1 O4 1.8598(18) . ?
Ti1 O2 1.876(2) . ?
C2 C3 1.518(4) . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
N2 C4 1.411(4) . ?
N2 C3 1.482(4) . ?
O2 C9 1.331(3) . ?
Ti2 O7 1.792(2) . ?
Ti2 O8 1.8397(19) . ?
Ti2 O5 1.868(2) . ?
Ti2 O6 1.889(2) . ?
Ti2 C34 2.222(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
N3 C34 1.344(4) . ?
N3 C43 1.409(4) . ?
N3 C35 1.479(4) . ?
O3 C16 1.429(4) . ?
C4 C5 1.393(4) . ?
C4 C9 1.409(4) . ?
N4 C34 1.347(4) . ?
N4 C37 1.410(4) . ?
N4 C36 1.478(4) . ?
O4 C19 1.348(3) . ?
C5 C6 1.377(5) . ?
C5 H5 0.9500 . ?
O5 C44 1.339(4) . ?
C6 C7 1.381(5) . ?
C6 H6 0.9500 . ?
O6 C42 1.329(3) . ?
C7 C8 1.384(4) . ?
C7 H7 0.9500 . ?
O7 C49 1.436(4) . ?
C8 C9 1.393(4) . ?
C8 H8 0.9500 . ?
O8 C52 1.357(3) . ?
C10 C15 1.395(4) . ?
C10 C11 1.406(4) . ?
C11 C12 1.394(4) . ?
C12 C13 1.384(4) . ?
C12 H12 0.9500 . ?
C13 C14 1.382(5) . ?
C13 H13 0.9500 . ?
C14 C15 1.384(5) . ?
C14 H14 0.9500 . ?
C15 H15 0.9500 . ?
C16 C17 1.502(5) . ?
C16 C18 1.514(4) . ?
C16 H16 1.0000 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 C24 1.422(4) . ?
C19 C20 1.422(4) . ?
C20 C21 1.395(4) . ?
C20 C26 1.542(4) . ?
C21 C22 1.388(4) . ?
C21 H21 0.9500 . ?
C22 C23 1.382(4) . ?
C22 C25 1.511(4) . ?
C23 C24 1.397(4) . ?
C23 H23 0.9500 . ?
C24 C30 1.541(4) . ?
C25 H25A 0.9800 . ?
C25 H25B 0.9800 . ?
C25 H25C 0.9800 . ?
C26 C29 1.527(4) . ?
C26 C28 1.528(4) . ?
C26 C27 1.543(4) . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9800 . ?
C28 H28B 0.9800 . ?
C28 H28C 0.9800 . ?
C29 H29A 0.9800 . ?
C29 H29B 0.9800 . ?
C29 H29C 0.9800 . ?
C30 C32 1.537(4) . ?
C30 C33 1.538(4) . ?
C30 C31 1.544(4) . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
C33 H33A 0.9800 . ?
C33 H33B 0.9800 . ?
C33 H33C 0.9800 . ?
C35 C36 1.510(5) . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C37 C38 1.393(4) . ?
C37 C42 1.408(4) . ?
C38 C39 1.381(5) . ?
C38 H38 0.9500 . ?
C39 C40 1.386(5) . ?
C39 H39 0.9500 . ?
C40 C41 1.381(4) . ?
C40 H40 0.9500 . ?
C41 C42 1.393(4) . ?
C41 H41 0.9500 . ?
C43 C44 1.399(5) . ?
C43 C48 1.406(4) . ?
C44 C45 1.394(5) . ?
C45 C46 1.385(5) . ?
C45 H45 0.9500 . ?
C46 C47 1.375(6) . ?
C46 H46 0.9500 . ?
C47 C48 1.377(5) . ?
C47 H47 0.9500 . ?
C48 H48 0.9500 . ?
C49 C51 1.511(5) . ?
C49 C50 1.514(5) . ?
C49 H49 1.0000 . ?
C50 H50A 0.9800 . ?
C50 H50B 0.9800 . ?
C50 H50C 0.9800 . ?
C51 H51A 0.9800 . ?
C51 H51B 0.9800 . ?
C51 H51C 0.9800 . ?
C52 C53 1.411(4) . ?
C52 C57 1.411(4) . ?
C53 C54 1.393(4) . ?
C53 C59 1.539(4) . ?
C54 C55 1.384(4) . ?
C54 H54 0.9500 . ?
C55 C56 1.379(4) . ?
C55 C58 1.513(4) . ?
C56 C57 1.396(4) . ?
C56 H56 0.9500 . ?
C57 C63 1.543(4) . ?
C58 H58A 0.9800 . ?
C58 H58B 0.9800 . ?
C58 H58C 0.9800 . ?
C59 C62 1.537(4) . ?
C59 C60 1.539(4) . ?
C59 C61 1.543(4) . ?
C60 H60A 0.9800 . ?
C60 H60B 0.9800 . ?
C60 H60C 0.9800 . ?
C61 H61A 0.9800 . ?
C61 H61B 0.9800 . ?
C61 H61C 0.9800 . ?
C62 H62A 0.9800 . ?
C62 H62B 0.9800 . ?
C62 H62C 0.9800 . ?
C63 C64 1.531(4) . ?
C63 C66 1.535(4) . ?
C63 C65 1.539(4) . ?
C64 H64A 0.9800 . ?
C64 H64B 0.9800 . ?
C64 H64C 0.9800 . ?
C65 H65A 0.9800 . ?
C65 H65B 0.9800 . ?
C65 H65C 0.9800 . ?
C66 H66A 0.9800 . ?
C66 H66B 0.9800 . ?
C66 H66C 0.9800 . ?
C1S C2S 1.497(15) . ?
C1S H1SA 0.9800 . ?
C1S H1SB 0.9800 . ?
C1S H1SC 0.9800 . ?
C2S C3S 1.586(15) . ?
C2S H2SA 0.9900 . ?
C2S H2SB 0.9900 . ?
C3S C3S 1.57(2) 3_565 ?
C3S H3SA 0.9900 . ?
C3S H3SB 0.9900 . ?
C7S C8S 1.448(8) . ?
C7S H7SA 0.9800 . ?
C7S H7SB 0.9800 . ?
C7S H7SC 0.9800 . ?
C8S C9S 1.488(7) . ?
C8S H8A 0.9900 . ?
C8S H8B 0.9900 . ?
C9S C10S 1.468(7) . ?
C9S H9SA 0.9900 . ?
C9S H9SB 0.9900 . ?
C10S C11S 1.493(7) . ?
C10S H10A 0.9900 . ?
C10S H10B 0.9900 . ?
C11S C12S 1.411(7) . ?
C11S H11A 0.9900 . ?
C11S H11B 0.9900 . ?
C12S H12A 0.9800 . ?
C12S H12B 0.9800 . ?
C12S H12C 0.9800 . ?
C13S C14S 1.531(6) . ?
C13S H13A 0.9800 . ?
C13S H13B 0.9800 . ?
C13S H13C 0.9800 . ?
C14S C15S 1.512(6) . ?
C14S H14A 0.9900 . ?
C14S H14B 0.9900 . ?
C15S C16S 1.504(6) . ?
C15S H15A 0.9900 . ?
C15S H15B 0.9900 . ?
C16S C17S 1.500(6) . ?
C16S H16A 0.9900 . ?
C16S H16B 0.9900 . ?
C17S C18S 1.536(6) . ?
C17S H17D 0.9900 . ?
C17S H17E 0.9900 . ?
C18S H18D 0.9800 . ?
C18S H18E 0.9800 . ?
C18S H18F 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
N1 C1 N2 108.3(2) . . ?
N1 C1 Ti1 125.26(19) . . ?
N2 C1 Ti1 126.3(2) . . ?
C1 N1 C10 126.5(2) . . ?
C1 N1 C2 113.1(2) . . ?
C10 N1 C2 120.4(2) . . ?
C11 O1 Ti1 135.71(18) . . ?
O3 Ti1 O4 113.53(9) . . ?
O3 Ti1 O2 101.23(9) . . ?
O4 Ti1 O2 94.62(8) . . ?
O3 Ti1 O1 99.26(10) . . ?
O4 Ti1 O1 91.76(8) . . ?
O2 Ti1 O1 153.96(9) . . ?
O3 Ti1 C1 99.75(10) . . ?
O4 Ti1 C1 146.64(9) . . ?
O2 Ti1 C1 80.46(9) . . ?
O1 Ti1 C1 80.38(9) . . ?
N1 C2 C3 102.9(2) . . ?
N1 C2 H2A 111.2 . . ?
C3 C2 H2A 111.2 . . ?
N1 C2 H2B 111.2 . . ?
C3 C2 H2B 111.2 . . ?
H2A C2 H2B 109.1 . . ?
C1 N2 C4 127.7(2) . . ?
C1 N2 C3 112.6(2) . . ?
C4 N2 C3 119.7(2) . . ?
C9 O2 Ti1 144.14(19) . . ?
O7 Ti2 O8 111.39(9) . . ?
O7 Ti2 O5 97.63(9) . . ?
O8 Ti2 O5 94.73(9) . . ?
O7 Ti2 O6 98.46(9) . . ?
O8 Ti2 O6 93.60(8) . . ?
O5 Ti2 O6 157.75(9) . . ?
O7 Ti2 C34 105.17(10) . . ?
O8 Ti2 C34 143.43(9) . . ?
O5 Ti2 C34 80.50(10) . . ?
O6 Ti2 C34 80.52(10) . . ?
N2 C3 C2 102.8(2) . . ?
N2 C3 H3A 111.2 . . ?
C2 C3 H3A 111.2 . . ?
N2 C3 H3B 111.2 . . ?
C2 C3 H3B 111.2 . . ?
H3A C3 H3B 109.1 . . ?
C34 N3 C43 127.0(3) . . ?
C34 N3 C35 113.0(3) . . ?
C43 N3 C35 119.9(3) . . ?
C16 O3 Ti1 146.57(19) . . ?
C5 C4 C9 119.4(3) . . ?
C5 C4 N2 120.6(3) . . ?
C9 C4 N2 120.0(2) . . ?
C34 N4 C37 127.1(2) . . ?
C34 N4 C36 112.6(3) . . ?
C37 N4 C36 120.1(2) . . ?
C19 O4 Ti1 160.30(17) . . ?
C6 C5 C4 120.7(3) . . ?
C6 C5 H5 119.7 . . ?
C4 C5 H5 119.7 . . ?
C44 O5 Ti2 143.9(2) . . ?
C5 C6 C7 120.4(3) . . ?
C5 C6 H6 119.8 . . ?
C7 C6 H6 119.8 . . ?
C42 O6 Ti2 140.63(19) . . ?
C6 C7 C8 119.6(3) . . ?
C6 C7 H7 120.2 . . ?
C8 C7 H7 120.2 . . ?
C49 O7 Ti2 133.47(19) . . ?
C7 C8 C9 121.2(3) . . ?
C7 C8 H8 119.4 . . ?
C9 C8 H8 119.4 . . ?
C52 O8 Ti2 158.87(17) . . ?
O2 C9 C8 120.1(3) . . ?
O2 C9 C4 121.2(3) . . ?
C8 C9 C4 118.7(3) . . ?
C15 C10 C11 119.3(3) . . ?
C15 C10 N1 120.5(3) . . ?
C11 C10 N1 120.2(2) . . ?
O1 C11 C12 119.3(3) . . ?
O1 C11 C10 121.8(3) . . ?
C12 C11 C10 118.8(3) . . ?
C13 C12 C11 121.3(3) . . ?
C13 C12 H12 119.3 . . ?
C11 C12 H12 119.3 . . ?
C14 C13 C12 119.7(3) . . ?
C14 C13 H13 120.2 . . ?
C12 C13 H13 120.2 . . ?
C13 C14 C15 120.1(3) . . ?
C13 C14 H14 120.0 . . ?
C15 C14 H14 120.0 . . ?
C14 C15 C10 120.9(3) . . ?
C14 C15 H15 119.6 . . ?
C10 C15 H15 119.6 . . ?
O3 C16 C17 109.2(3) . . ?
O3 C16 C18 109.2(3) . . ?
C17 C16 C18 113.3(3) . . ?
O3 C16 H16 108.3 . . ?
C17 C16 H16 108.3 . . ?
C18 C16 H16 108.3 . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C16 C18 H18A 109.5 . . ?
C16 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C16 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O4 C19 C24 119.4(2) . . ?
O4 C19 C20 119.8(2) . . ?
C24 C19 C20 120.8(2) . . ?
C21 C20 C19 117.7(2) . . ?
C21 C20 C26 119.4(2) . . ?
C19 C20 C26 122.9(2) . . ?
C22 C21 C20 122.8(3) . . ?
C22 C21 H21 118.6 . . ?
C20 C21 H21 118.6 . . ?
C23 C22 C21 118.1(3) . . ?
C23 C22 C25 120.9(3) . . ?
C21 C22 C25 121.0(3) . . ?
C22 C23 C24 123.1(3) . . ?
C22 C23 H23 118.5 . . ?
C24 C23 H23 118.5 . . ?
C23 C24 C19 117.5(2) . . ?
C23 C24 C30 119.8(2) . . ?
C19 C24 C30 122.7(2) . . ?
C22 C25 H25A 109.5 . . ?
C22 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C22 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C29 C26 C28 105.7(2) . . ?
C29 C26 C20 112.9(2) . . ?
C28 C26 C20 111.3(2) . . ?
C29 C26 C27 106.2(2) . . ?
C28 C26 C27 110.5(2) . . ?
C20 C26 C27 110.1(2) . . ?
C26 C27 H27A 109.5 . . ?
C26 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C26 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
C26 C28 H28A 109.5 . . ?
C26 C28 H28B 109.5 . . ?
H28A C28 H28B 109.5 . . ?
C26 C28 H28C 109.5 . . ?
H28A C28 H28C 109.5 . . ?
H28B C28 H28C 109.5 . . ?
C26 C29 H29A 109.5 . . ?
C26 C29 H29B 109.5 . . ?
H29A C29 H29B 109.5 . . ?
C26 C29 H29C 109.5 . . ?
H29A C29 H29C 109.5 . . ?
H29B C29 H29C 109.5 . . ?
C32 C30 C33 110.9(3) . . ?
C32 C30 C24 111.5(2) . . ?
C33 C30 C24 109.8(2) . . ?
C32 C30 C31 106.2(2) . . ?
C33 C30 C31 106.2(2) . . ?
C24 C30 C31 112.0(2) . . ?
C30 C31 H31A 109.5 . . ?
C30 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C30 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C30 C32 H32A 109.5 . . ?
C30 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C30 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C30 C33 H33A 109.5 . . ?
C30 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C30 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
N3 C34 N4 108.1(2) . . ?
N3 C34 Ti2 126.3(2) . . ?
N4 C34 Ti2 125.5(2) . . ?
N3 C35 C36 102.7(2) . . ?
N3 C35 H35A 111.2 . . ?
C36 C35 H35A 111.2 . . ?
N3 C35 H35B 111.2 . . ?
C36 C35 H35B 111.2 . . ?
H35A C35 H35B 109.1 . . ?
N4 C36 C35 103.2(2) . . ?
N4 C36 H36A 111.1 . . ?
C35 C36 H36A 111.1 . . ?
N4 C36 H36B 111.1 . . ?
C35 C36 H36B 111.1 . . ?
H36A C36 H36B 109.1 . . ?
C38 C37 C42 119.4(3) . . ?
C38 C37 N4 120.0(3) . . ?
C42 C37 N4 120.6(3) . . ?
C39 C38 C37 120.7(3) . . ?
C39 C38 H38 119.7 . . ?
C37 C38 H38 119.7 . . ?
C38 C39 C40 120.2(3) . . ?
C38 C39 H39 119.9 . . ?
C40 C39 H39 119.9 . . ?
C41 C40 C39 119.7(3) . . ?
C41 C40 H40 120.1 . . ?
C39 C40 H40 120.1 . . ?
C40 C41 C42 121.2(3) . . ?
C40 C41 H41 119.4 . . ?
C42 C41 H41 119.4 . . ?
O6 C42 C41 119.8(3) . . ?
O6 C42 C37 121.3(3) . . ?
C41 C42 C37 118.8(3) . . ?
C44 C43 C48 118.8(3) . . ?
C44 C43 N3 120.9(3) . . ?
C48 C43 N3 120.3(3) . . ?
O5 C44 C45 119.5(3) . . ?
O5 C44 C43 121.1(3) . . ?
C45 C44 C43 119.4(3) . . ?
C46 C45 C44 121.0(3) . . ?
C46 C45 H45 119.5 . . ?
C44 C45 H45 119.5 . . ?
C47 C46 C45 119.4(3) . . ?
C47 C46 H46 120.3 . . ?
C45 C46 H46 120.3 . . ?
C46 C47 C48 120.9(3) . . ?
C46 C47 H47 119.6 . . ?
C48 C47 H47 119.6 . . ?
C47 C48 C43 120.4(3) . . ?
C47 C48 H48 119.8 . . ?
C43 C48 H48 119.8 . . ?
O7 C49 C51 109.4(3) . . ?
O7 C49 C50 107.9(3) . . ?
C51 C49 C50 112.8(3) . . ?
O7 C49 H49 108.9 . . ?
C51 C49 H49 108.9 . . ?
C50 C49 H49 108.9 . . ?
C49 C50 H50A 109.5 . . ?
C49 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C49 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C49 C51 H51A 109.5 . . ?
C49 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C49 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
O8 C52 C53 119.6(2) . . ?
O8 C52 C57 119.4(2) . . ?
C53 C52 C57 120.9(2) . . ?
C54 C53 C52 118.2(3) . . ?
C54 C53 C59 120.4(3) . . ?
C52 C53 C59 121.4(2) . . ?
C55 C54 C53 122.3(3) . . ?
C55 C54 H54 118.9 . . ?
C53 C54 H54 118.9 . . ?
C56 C55 C54 118.1(3) . . ?
C56 C55 C58 121.4(3) . . ?
C54 C55 C58 120.5(3) . . ?
C55 C56 C57 123.1(3) . . ?
C55 C56 H56 118.5 . . ?
C57 C56 H56 118.5 . . ?
C56 C57 C52 117.4(3) . . ?
C56 C57 C63 120.4(3) . . ?
C52 C57 C63 122.3(2) . . ?
C55 C58 H58A 109.5 . . ?
C55 C58 H58B 109.5 . . ?
H58A C58 H58B 109.5 . . ?
C55 C58 H58C 109.5 . . ?
H58A C58 H58C 109.5 . . ?
H58B C58 H58C 109.5 . . ?
C62 C59 C60 106.7(3) . . ?
C62 C59 C53 112.2(2) . . ?
C60 C59 C53 108.7(2) . . ?
C62 C59 C61 105.5(3) . . ?
C60 C59 C61 111.2(2) . . ?
C53 C59 C61 112.5(2) . . ?
C59 C60 H60A 109.5 . . ?
C59 C60 H60B 109.5 . . ?
H60A C60 H60B 109.5 . . ?
C59 C60 H60C 109.5 . . ?
H60A C60 H60C 109.5 . . ?
H60B C60 H60C 109.5 . . ?
C59 C61 H61A 109.5 . . ?
C59 C61 H61B 109.5 . . ?
H61A C61 H61B 109.5 . . ?
C59 C61 H61C 109.5 . . ?
H61A C61 H61C 109.5 . . ?
H61B C61 H61C 109.5 . . ?
C59 C62 H62A 109.5 . . ?
C59 C62 H62B 109.5 . . ?
H62A C62 H62B 109.5 . . ?
C59 C62 H62C 109.5 . . ?
H62A C62 H62C 109.5 . . ?
H62B C62 H62C 109.5 . . ?
C64 C63 C66 110.7(3) . . ?
C64 C63 C65 106.4(2) . . ?
C66 C63 C65 106.5(3) . . ?
C64 C63 C57 110.4(2) . . ?
C66 C63 C57 110.8(2) . . ?
C65 C63 C57 111.9(3) . . ?
C63 C64 H64A 109.5 . . ?
C63 C64 H64B 109.5 . . ?
H64A C64 H64B 109.5 . . ?
C63 C64 H64C 109.5 . . ?
H64A C64 H64C 109.5 . . ?
H64B C64 H64C 109.5 . . ?
C63 C65 H65A 109.5 . . ?
C63 C65 H65B 109.5 . . ?
H65A C65 H65B 109.5 . . ?
C63 C65 H65C 109.5 . . ?
H65A C65 H65C 109.5 . . ?
H65B C65 H65C 109.5 . . ?
C63 C66 H66A 109.5 . . ?
C63 C66 H66B 109.5 . . ?
H66A C66 H66B 109.5 . . ?
C63 C66 H66C 109.5 . . ?
H66A C66 H66C 109.5 . . ?
H66B C66 H66C 109.5 . . ?
C2S C1S H1SA 109.5 . . ?
C2S C1S H1SB 109.5 . . ?
H1SA C1S H1SB 109.5 . . ?
C2S C1S H1SC 109.5 . . ?
H1SA C1S H1SC 109.5 . . ?
H1SB C1S H1SC 109.5 . . ?
C1S C2S C3S 116.9(13) . . ?
C1S C2S H2SA 108.1 . . ?
C3S C2S H2SA 108.1 . . ?
C1S C2S H2SB 108.1 . . ?
C3S C2S H2SB 108.1 . . ?
H2SA C2S H2SB 107.3 . . ?
C3S C3S C2S 107.2(12) 3_565 . ?
C3S C3S H3SA 110.3 3_565 . ?
C2S C3S H3SA 110.3 . . ?
C3S C3S H3SB 110.3 3_565 . ?
C2S C3S H3SB 110.3 . . ?
H3SA C3S H3SB 108.5 . . ?
C8S C7S H7SA 109.5 . . ?
C8S C7S H7SB 109.5 . . ?
H7SA C7S H7SB 109.5 . . ?
C8S C7S H7SC 109.5 . . ?
H7SA C7S H7SC 109.5 . . ?
H7SB C7S H7SC 109.5 . . ?
C7S C8S C9S 115.2(5) . . ?
C7S C8S H8A 108.5 . . ?
C9S C8S H8A 108.5 . . ?
C7S C8S H8B 108.5 . . ?
C9S C8S H8B 108.5 . . ?
H8A C8S H8B 107.5 . . ?
C10S C9S C8S 118.8(5) . . ?
C10S C9S H9SA 107.6 . . ?
C8S C9S H9SA 107.6 . . ?
C10S C9S H9SB 107.6 . . ?
C8S C9S H9SB 107.6 . . ?
H9SA C9S H9SB 107.1 . . ?
C9S C10S C11S 116.3(5) . . ?
C9S C10S H10A 108.2 . . ?
C11S C10S H10A 108.2 . . ?
C9S C10S H10B 108.2 . . ?
C11S C10S H10B 108.2 . . ?
H10A C10S H10B 107.4 . . ?
C12S C11S C10S 119.1(5) . . ?
C12S C11S H11A 107.5 . . ?
C10S C11S H11A 107.5 . . ?
C12S C11S H11B 107.5 . . ?
C10S C11S H11B 107.5 . . ?
H11A C11S H11B 107.0 . . ?
C11S C12S H12A 109.5 . . ?
C11S C12S H12B 109.5 . . ?
H12A C12S H12B 109.5 . . ?
C11S C12S H12C 109.5 . . ?
H12A C12S H12C 109.5 . . ?
H12B C12S H12C 109.5 . . ?
C14S C13S H13A 109.5 . . ?
C14S C13S H13B 109.5 . . ?
H13A C13S H13B 109.5 . . ?
C14S C13S H13C 109.5 . . ?
H13A C13S H13C 109.5 . . ?
H13B C13S H13C 109.5 . . ?
C15S C14S C13S 112.7(4) . . ?
C15S C14S H14A 109.0 . . ?
C13S C14S H14A 109.0 . . ?
C15S C14S H14B 109.0 . . ?
C13S C14S H14B 109.0 . . ?
H14A C14S H14B 107.8 . . ?
C16S C15S C14S 114.5(4) . . ?
C16S C15S H15A 108.6 . . ?
C14S C15S H15A 108.6 . . ?
C16S C15S H15B 108.6 . . ?
C14S C15S H15B 108.6 . . ?
H15A C15S H15B 107.6 . . ?
C17S C16S C15S 115.3(4) . . ?
C17S C16S H16A 108.4 . . ?
C15S C16S H16A 108.4 . . ?
C17S C16S H16B 108.4 . . ?
C15S C16S H16B 108.4 . . ?
H16A C16S H16B 107.5 . . ?
C16S C17S C18S 113.6(4) . . ?
C16S C17S H17D 108.8 . . ?
C18S C17S H17D 108.8 . . ?
C16S C17S H17E 108.8 . . ?
C18S C17S H17E 108.8 . . ?
H17D C17S H17E 107.7 . . ?
C17S C18S H18D 109.5 . . ?
C17S C18S H18E 109.5 . . ?
H18D C18S H18E 109.5 . . ?
C17S C18S H18F 109.5 . . ?
H18D C18S H18F 109.5 . . ?
H18E C18S H18F 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
N2 C1 N1 C10 -179.0(2) . . . . ?
Ti1 C1 N1 C10 4.7(4) . . . . ?
N2 C1 N1 C2 -0.7(3) . . . . ?
Ti1 C1 N1 C2 -177.09(19) . . . . ?
C11 O1 Ti1 O3 -60.6(3) . . . . ?
C11 O1 Ti1 O4 -174.7(3) . . . . ?
C11 O1 Ti1 O2 81.0(3) . . . . ?
C11 O1 Ti1 C1 37.9(3) . . . . ?
C1 N1 C2 C3 4.1(3) . . . . ?
C10 N1 C2 C3 -177.6(2) . . . . ?
N1 C1 N2 C4 179.1(2) . . . . ?
Ti1 C1 N2 C4 -4.6(4) . . . . ?
N1 C1 N2 C3 -3.2(3) . . . . ?
Ti1 C1 N2 C3 173.11(19) . . . . ?
O3 Ti1 O2 C9 101.2(3) . . . . ?
O4 Ti1 O2 C9 -143.7(3) . . . . ?
O1 Ti1 O2 C9 -40.0(4) . . . . ?
C1 Ti1 O2 C9 3.1(3) . . . . ?
C1 N2 C3 C2 5.5(3) . . . . ?
C4 N2 C3 C2 -176.6(2) . . . . ?
N1 C2 C3 N2 -5.3(3) . . . . ?
O4 Ti1 O3 C16 -124.1(3) . . . . ?
O2 Ti1 O3 C16 -24.0(4) . . . . ?
O1 Ti1 O3 C16 139.9(3) . . . . ?
C1 Ti1 O3 C16 58.1(4) . . . . ?
C1 N2 C4 C5 -177.0(3) . . . . ?
C3 N2 C4 C5 5.4(4) . . . . ?
C1 N2 C4 C9 3.1(4) . . . . ?
C3 N2 C4 C9 -174.4(2) . . . . ?
O3 Ti1 O4 C19 -125.1(5) . . . . ?
O2 Ti1 O4 C19 130.5(5) . . . . ?
O1 Ti1 O4 C19 -24.2(5) . . . . ?
C1 Ti1 O4 C19 50.8(6) . . . . ?
C9 C4 C5 C6 -2.1(4) . . . . ?
N2 C4 C5 C6 178.1(3) . . . . ?
O7 Ti2 O5 C44 -106.9(3) . . . . ?
O8 Ti2 O5 C44 140.8(3) . . . . ?
O6 Ti2 O5 C44 29.1(5) . . . . ?
C34 Ti2 O5 C44 -2.7(3) . . . . ?
C4 C5 C6 C7 1.0(5) . . . . ?
O7 Ti2 O6 C42 78.5(3) . . . . ?
O8 Ti2 O6 C42 -169.3(3) . . . . ?
O5 Ti2 O6 C42 -57.4(4) . . . . ?
C34 Ti2 O6 C42 -25.6(3) . . . . ?
C5 C6 C7 C8 0.4(5) . . . . ?
O8 Ti2 O7 C49 76.8(3) . . . . ?
O5 Ti2 O7 C49 -21.3(3) . . . . ?
O6 Ti2 O7 C49 174.1(3) . . . . ?
C34 Ti2 O7 C49 -103.5(3) . . . . ?
C6 C7 C8 C9 -0.7(5) . . . . ?
O7 Ti2 O8 C52 134.9(5) . . . . ?
O5 Ti2 O8 C52 -125.0(5) . . . . ?
O6 Ti2 O8 C52 34.4(5) . . . . ?
C34 Ti2 O8 C52 -44.6(6) . . . . ?
Ti1 O2 C9 C8 174.7(2) . . . . ?
Ti1 O2 C9 C4 -4.9(5) . . . . ?
C7 C8 C9 O2 -180.0(3) . . . . ?
C7 C8 C9 C4 -0.4(4) . . . . ?
C5 C4 C9 O2 -178.6(3) . . . . ?
N2 C4 C9 O2 1.2(4) . . . . ?
C5 C4 C9 C8 1.8(4) . . . . ?
N2 C4 C9 C8 -178.4(3) . . . . ?
C1 N1 C10 C15 -172.1(3) . . . . ?
C2 N1 C10 C15 9.8(4) . . . . ?
C1 N1 C10 C11 9.3(4) . . . . ?
C2 N1 C10 C11 -168.8(3) . . . . ?
Ti1 O1 C11 C12 145.4(2) . . . . ?
Ti1 O1 C11 C10 -36.3(4) . . . . ?
C15 C10 C11 O1 -176.2(3) . . . . ?
N1 C10 C11 O1 2.5(4) . . . . ?
C15 C10 C11 C12 2.2(4) . . . . ?
N1 C10 C11 C12 -179.2(2) . . . . ?
O1 C11 C12 C13 176.9(3) . . . . ?
C10 C11 C12 C13 -1.5(4) . . . . ?
C11 C12 C13 C14 -0.3(5) . . . . ?
C12 C13 C14 C15 1.3(5) . . . . ?
C13 C14 C15 C10 -0.6(5) . . . . ?
C11 C10 C15 C14 -1.2(5) . . . . ?
N1 C10 C15 C14 -179.8(3) . . . . ?
Ti1 O3 C16 C17 65.7(4) . . . . ?
Ti1 O3 C16 C18 -58.7(4) . . . . ?
Ti1 O4 C19 C24 109.6(5) . . . . ?
Ti1 O4 C19 C20 -72.5(6) . . . . ?
O4 C19 C20 C21 -178.5(2) . . . . ?
C24 C19 C20 C21 -0.6(4) . . . . ?
O4 C19 C20 C26 0.7(4) . . . . ?
C24 C19 C20 C26 178.6(2) . . . . ?
C19 C20 C21 C22 1.8(4) . . . . ?
C26 C20 C21 C22 -177.4(3) . . . . ?
C20 C21 C22 C23 -1.3(4) . . . . ?
C20 C21 C22 C25 179.5(3) . . . . ?
C21 C22 C23 C24 -0.6(4) . . . . ?
C25 C22 C23 C24 178.7(3) . . . . ?
C22 C23 C24 C19 1.7(4) . . . . ?
C22 C23 C24 C30 -177.2(3) . . . . ?
O4 C19 C24 C23 176.8(2) . . . . ?
C20 C19 C24 C23 -1.1(4) . . . . ?
O4 C19 C24 C30 -4.3(4) . . . . ?
C20 C19 C24 C30 177.8(2) . . . . ?
C21 C20 C26 C29 -1.4(4) . . . . ?
C19 C20 C26 C29 179.4(3) . . . . ?
C21 C20 C26 C28 -120.1(3) . . . . ?
C19 C20 C26 C28 60.8(3) . . . . ?
C21 C20 C26 C27 117.1(3) . . . . ?
C19 C20 C26 C27 -62.1(3) . . . . ?
C23 C24 C30 C32 -122.6(3) . . . . ?
C19 C24 C30 C32 58.5(3) . . . . ?
C23 C24 C30 C33 114.0(3) . . . . ?
C19 C24 C30 C33 -64.8(3) . . . . ?
C23 C24 C30 C31 -3.8(4) . . . . ?
C19 C24 C30 C31 177.4(3) . . . . ?
C43 N3 C34 N4 -176.7(3) . . . . ?
C35 N3 C34 N4 0.5(3) . . . . ?
C43 N3 C34 Ti2 6.7(4) . . . . ?
C35 N3 C34 Ti2 -176.1(2) . . . . ?
C37 N4 C34 N3 -179.1(3) . . . . ?
C36 N4 C34 N3 -3.9(3) . . . . ?
C37 N4 C34 Ti2 -2.5(4) . . . . ?
C36 N4 C34 Ti2 172.68(19) . . . . ?
C34 N3 C35 C36 2.9(3) . . . . ?
C43 N3 C35 C36 -179.7(2) . . . . ?
C34 N4 C36 C35 5.6(3) . . . . ?
C37 N4 C36 C35 -178.9(2) . . . . ?
N3 C35 C36 N4 -4.7(3) . . . . ?
C34 N4 C37 C38 173.0(3) . . . . ?
C36 N4 C37 C38 -1.9(4) . . . . ?
C34 N4 C37 C42 -7.2(4) . . . . ?
C36 N4 C37 C42 178.0(3) . . . . ?
C42 C37 C38 C39 1.0(5) . . . . ?
N4 C37 C38 C39 -179.2(3) . . . . ?
C37 C38 C39 C40 0.2(5) . . . . ?
C38 C39 C40 C41 -1.2(5) . . . . ?
C39 C40 C41 C42 1.1(5) . . . . ?
Ti2 O6 C42 C41 -155.4(2) . . . . ?
Ti2 O6 C42 C37 23.8(4) . . . . ?
C40 C41 C42 O6 179.2(3) . . . . ?
C40 C41 C42 C37 0.0(4) . . . . ?
C38 C37 C42 O6 179.7(3) . . . . ?
N4 C37 C42 O6 -0.1(4) . . . . ?
C38 C37 C42 C41 -1.1(4) . . . . ?
N4 C37 C42 C41 179.1(3) . . . . ?
C34 N3 C43 C44 -5.2(4) . . . . ?
C35 N3 C43 C44 177.7(3) . . . . ?
C34 N3 C43 C48 174.5(3) . . . . ?
C35 N3 C43 C48 -2.5(4) . . . . ?
Ti2 O5 C44 C45 -176.0(2) . . . . ?
Ti2 O5 C44 C43 4.3(5) . . . . ?
C48 C43 C44 O5 -179.8(3) . . . . ?
N3 C43 C44 O5 0.0(4) . . . . ?
C48 C43 C44 C45 0.6(4) . . . . ?
N3 C43 C44 C45 -179.7(3) . . . . ?
O5 C44 C45 C46 -179.7(3) . . . . ?
C43 C44 C45 C46 -0.1(4) . . . . ?
C44 C45 C46 C47 -0.4(5) . . . . ?
C45 C46 C47 C48 0.3(5) . . . . ?
C46 C47 C48 C43 0.2(5) . . . . ?
C44 C43 C48 C47 -0.7(5) . . . . ?
N3 C43 C48 C47 179.6(3) . . . . ?
Ti2 O7 C49 C51 85.2(3) . . . . ?
Ti2 O7 C49 C50 -151.6(2) . . . . ?
Ti2 O8 C52 C53 67.6(6) . . . . ?
Ti2 O8 C52 C57 -114.0(5) . . . . ?
O8 C52 C53 C54 -179.4(2) . . . . ?
C57 C52 C53 C54 2.2(4) . . . . ?
O8 C52 C53 C59 4.2(4) . . . . ?
C57 C52 C53 C59 -174.1(2) . . . . ?
C52 C53 C54 C55 -1.7(4) . . . . ?
C59 C53 C54 C55 174.7(3) . . . . ?
C53 C54 C55 C56 0.4(4) . . . . ?
C53 C54 C55 C58 -179.7(3) . . . . ?
C54 C55 C56 C57 0.5(4) . . . . ?
C58 C55 C56 C57 -179.4(3) . . . . ?
C55 C56 C57 C52 0.0(4) . . . . ?
C55 C56 C57 C63 179.9(3) . . . . ?
O8 C52 C57 C56 -179.7(2) . . . . ?
C53 C52 C57 C56 -1.4(4) . . . . ?
O8 C52 C57 C63 0.4(4) . . . . ?
C53 C52 C57 C63 178.7(2) . . . . ?
C54 C53 C59 C62 5.4(4) . . . . ?
C52 C53 C59 C62 -178.4(3) . . . . ?
C54 C53 C59 C60 -112.3(3) . . . . ?
C52 C53 C59 C60 63.9(3) . . . . ?
C54 C53 C59 C61 124.2(3) . . . . ?
C52 C53 C59 C61 -59.6(3) . . . . ?
C56 C57 C63 C64 122.2(3) . . . . ?
C52 C57 C63 C64 -57.9(3) . . . . ?
C56 C57 C63 C66 -114.7(3) . . . . ?
C52 C57 C63 C66 65.2(3) . . . . ?
C56 C57 C63 C65 3.9(4) . . . . ?
C52 C57 C63 C65 -176.2(3) . . . . ?
C1S C2S C3S C3S -64.7(19) . . . 3_565 ?
C7S C8S C9S C10S 177.0(6) . . . . ?
C8S C9S C10S C11S 178.0(6) . . . . ?
C9S C10S C11S C12S 176.4(6) . . . . ?
C13S C14S C15S C16S -178.4(4) . . . . ?
C14S C15S C16S C17S -68.2(5) . . . . ?
C15S C16S C17S C18S -176.4(4) . . . . ?

_refine_diff_density_max         0.990
_refine_diff_density_min         -0.773
_refine_diff_density_rms         0.081


_chemical_properties_physical    Air-sensitive,Moisture-sensitive,Hygroscopic
