# Electronic Supplementary Material (ESI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2023

####################################################################### 
# 
# 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_s21alj13
_database_code_depnum_ccdc_archive 'CCDC 2260244'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok Kohn'
;Material and Chemical Characterisation Facility, University of Bath
United Kingdom
;
_audit_update_record             
;
2023-05-02 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C24 H48 N2 O7 Ti2'
_chemical_formula_sum            'C24 H48 N2 O7 Ti2'
_chemical_formula_weight         572.44

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_H-M_alt        'P 2/c'
_space_group_name_Hall           '-P 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, -y, -z'
'x, -y, z-1/2'

_cell_length_a                   12.5296(6)
_cell_length_b                   9.5707(4)
_cell_length_c                   12.5976(6)
_cell_angle_alpha                90
_cell_angle_beta                 107.738(5)
_cell_angle_gamma                90
_cell_volume                     1438.85(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    2710
_cell_measurement_theta_min      4.6140
_cell_measurement_theta_max      68.1870

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.321
_exptl_crystal_F_000             612
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    5.068
_shelx_estimated_absorpt_T_min   0.702
_shelx_estimated_absorpt_T_max   0.863
_exptl_absorpt_correction_T_min  0.61508
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.697
_oxdiff_exptl_absorpt_empirical_full_max 1.718
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            8446
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         3.704
_diffrn_reflns_theta_max         68.238
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measured_fraction_theta_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.992
_reflns_number_total             2620
_reflns_number_gt                2142
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0381P)²+5.3591P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         2620
_refine_ls_number_parameters     165
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0539
_refine_ls_wR_factor_ref         0.1406
_refine_ls_wR_factor_gt          0.1334
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_restrained_S_all      1.101
_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 0.62432(6) 0.71956(7) 0.37087(6) 0.0151(2) Uani 1 1 d . . . . .
N1 N 0.7863(3) 0.7044(3) 0.5325(3) 0.0178(7) Uani 1 1 d . . . . .
O1 O 0.5801(2) 0.8036(3) 0.4808(2) 0.0201(6) Uani 1 1 d . . . . .
O2 O 0.7326(2) 0.8174(3) 0.3303(2) 0.0210(6) Uani 1 1 d . . . . .
O3 O 0.6542(2) 0.5326(3) 0.3883(2) 0.0231(7) Uani 1 1 d . . . . .
O4 O 0.500000 0.7313(4) 0.250000 0.0184(8) Uani 1 2 d S T P . .
C1 C 0.6502(3) 0.8602(4) 0.5839(3) 0.0210(9) Uani 1 1 d . . . . .
C2 C 0.5853(4) 0.8621(5) 0.6689(4) 0.0322(11) Uani 1 1 d . . . . .
H2A H 0.520631 0.924659 0.642718 0.048 Uiso 1 1 calc R U . . .
H2B H 0.634306 0.895382 0.740778 0.048 Uiso 1 1 calc R U . . .
H2C H 0.559266 0.767458 0.677553 0.048 Uiso 1 1 calc R U . . .
C3 C 0.6817(4) 1.0087(5) 0.5617(4) 0.0296(11) Uani 1 1 d . . . . .
H3A H 0.712037 1.008459 0.498591 0.044 Uiso 1 1 calc R U . . .
H3B H 0.738283 1.044878 0.628010 0.044 Uiso 1 1 calc R U . . .
H3C H 0.614929 1.068252 0.544076 0.044 Uiso 1 1 calc R U . . .
C4 C 0.7501(3) 0.7595(4) 0.6254(3) 0.0201(9) Uani 1 1 d . . . . .
H4A H 0.813471 0.809146 0.678465 0.024 Uiso 1 1 calc R U . . .
H4B H 0.728554 0.680694 0.665477 0.024 Uiso 1 1 calc R U . . .
C5 C 0.8505(3) 0.8055(4) 0.3800(3) 0.0209(9) Uani 1 1 d . . . . .
C6 C 0.9069(4) 0.9385(5) 0.3580(4) 0.0338(12) Uani 1 1 d . . . . .
H6A H 0.894989 0.948144 0.277742 0.051 Uiso 1 1 calc R U . . .
H6B H 0.987411 0.933785 0.397144 0.051 Uiso 1 1 calc R U . . .
H6C H 0.874511 1.019277 0.384855 0.051 Uiso 1 1 calc R U . . .
C7 C 0.8931(4) 0.6818(5) 0.3282(4) 0.0302(11) Uani 1 1 d . . . . .
H7A H 0.854279 0.596603 0.339142 0.045 Uiso 1 1 calc R U . . .
H7B H 0.973841 0.670821 0.363978 0.045 Uiso 1 1 calc R U . . .
H7C H 0.878429 0.698360 0.248287 0.045 Uiso 1 1 calc R U . . .
C8 C 0.8726(3) 0.7918(4) 0.5069(3) 0.0213(9) Uani 1 1 d . . . . .
H8A H 0.947326 0.749615 0.541090 0.026 Uiso 1 1 calc R U . . .
H8B H 0.872662 0.885879 0.539667 0.026 Uiso 1 1 calc R U . . .
C9 C 0.7188(3) 0.4599(4) 0.4858(3) 0.0228(9) Uani 1 1 d . . . . .
C10 C 0.6441(4) 0.4252(5) 0.5573(4) 0.0308(11) Uani 1 1 d . . . . .
H10A H 0.613202 0.511627 0.577587 0.046 Uiso 1 1 calc R U . . .
H10B H 0.688310 0.377003 0.625143 0.046 Uiso 1 1 calc R U . . .
H10C H 0.582761 0.364468 0.515381 0.046 Uiso 1 1 calc R U . . .
C11 C 0.7634(4) 0.3259(4) 0.4487(4) 0.0303(11) Uani 1 1 d . . . . .
H11A H 0.700779 0.262664 0.414646 0.046 Uiso 1 1 calc R U . . .
H11B H 0.815733 0.280266 0.513513 0.046 Uiso 1 1 calc R U . . .
H11C H 0.802294 0.348677 0.394225 0.046 Uiso 1 1 calc R U . . .
C12 C 0.8186(3) 0.5549(4) 0.5451(3) 0.0199(9) Uani 1 1 d . . . . .
H12A H 0.845645 0.530761 0.625314 0.024 Uiso 1 1 calc R U . . .
H12B H 0.880692 0.538518 0.513331 0.024 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
Ti1 O4 1.8200(7) . ?
Ti1 O1 1.827(3) . ?
Ti1 O3 1.827(3) . ?
Ti1 O2 1.845(3) . ?
Ti1 N1 2.402(3) . ?
N1 C4 1.475(5) . ?
N1 C8 1.478(5) . ?
N1 C12 1.482(5) . ?
O1 C1 1.435(5) . ?
O2 C5 1.423(5) . ?
O3 C9 1.430(5) . ?
C1 C3 1.523(6) . ?
C1 C2 1.529(6) . ?
C1 C4 1.540(6) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.521(6) . ?
C5 C7 1.524(6) . ?
C5 C8 1.544(6) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.520(6) . ?
C9 C11 1.528(6) . ?
C9 C12 1.543(5) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 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
O4 Ti1 O1 103.13(10) . . ?
O4 Ti1 O3 104.62(15) . . ?
O1 Ti1 O3 116.00(13) . . ?
O4 Ti1 O2 104.54(11) . . ?
O1 Ti1 O2 113.90(13) . . ?
O3 Ti1 O2 112.91(13) . . ?
O4 Ti1 N1 178.98(9) . . ?
O1 Ti1 N1 75.94(12) . . ?
O3 Ti1 N1 75.52(11) . . ?
O2 Ti1 N1 76.27(11) . . ?
C4 N1 C8 113.1(3) . . ?
C4 N1 C12 113.6(3) . . ?
C8 N1 C12 112.1(3) . . ?
C4 N1 Ti1 105.4(2) . . ?
C8 N1 Ti1 105.4(2) . . ?
C12 N1 Ti1 106.4(2) . . ?
C1 O1 Ti1 127.6(2) . . ?
C5 O2 Ti1 126.2(2) . . ?
C9 O3 Ti1 128.4(2) . . ?
Ti1 O4 Ti1 172.9(2) . 2_655 ?
O1 C1 C3 107.9(3) . . ?
O1 C1 C2 109.2(3) . . ?
C3 C1 C2 109.9(4) . . ?
O1 C1 C4 106.3(3) . . ?
C3 C1 C4 114.7(3) . . ?
C2 C1 C4 108.7(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C1 111.7(3) . . ?
N1 C4 H4A 109.3 . . ?
C1 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C1 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
O2 C5 C6 109.3(3) . . ?
O2 C5 C7 109.0(3) . . ?
C6 C5 C7 109.3(4) . . ?
O2 C5 C8 107.3(3) . . ?
C6 C5 C8 108.2(3) . . ?
C7 C5 C8 113.7(4) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C5 111.2(3) . . ?
N1 C8 H8A 109.4 . . ?
C5 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C5 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O3 C9 C10 109.0(3) . . ?
O3 C9 C11 108.1(3) . . ?
C10 C9 C11 110.3(4) . . ?
O3 C9 C12 107.0(3) . . ?
C10 C9 C12 113.3(4) . . ?
C11 C9 C12 109.0(3) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C9 111.3(3) . . ?
N1 C12 H12A 109.4 . . ?
C9 C12 H12A 109.4 . . ?
N1 C12 H12B 109.4 . . ?
C9 C12 H12B 109.4 . . ?
H12A C12 H12B 108.0 . . ?

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
O4 Ti1 O1 C1 -160.5(3) . . . . ?
O3 Ti1 O1 C1 85.8(3) . . . . ?
O2 Ti1 O1 C1 -47.8(3) . . . . ?
N1 Ti1 O1 C1 19.9(3) . . . . ?
O4 Ti1 O2 C5 -160.0(3) . . . . ?
O1 Ti1 O2 C5 88.2(3) . . . . ?
O3 Ti1 O2 C5 -46.9(3) . . . . ?
N1 Ti1 O2 C5 20.6(3) . . . . ?
O4 Ti1 O3 C9 -159.2(3) . . . . ?
O1 Ti1 O3 C9 -46.3(4) . . . . ?
O2 Ti1 O3 C9 87.8(3) . . . . ?
N1 Ti1 O3 C9 19.8(3) . . . . ?
Ti1 O1 C1 C3 84.6(4) . . . . ?
Ti1 O1 C1 C2 -156.0(3) . . . . ?
Ti1 O1 C1 C4 -38.9(4) . . . . ?
C8 N1 C4 C1 89.9(4) . . . . ?
C12 N1 C4 C1 -140.8(3) . . . . ?
Ti1 N1 C4 C1 -24.8(4) . . . . ?
O1 C1 C4 N1 37.7(4) . . . . ?
C3 C1 C4 N1 -81.4(4) . . . . ?
C2 C1 C4 N1 155.1(3) . . . . ?
Ti1 O2 C5 C6 -157.1(3) . . . . ?
Ti1 O2 C5 C7 83.6(4) . . . . ?
Ti1 O2 C5 C8 -40.0(4) . . . . ?
C4 N1 C8 C5 -139.1(3) . . . . ?
C12 N1 C8 C5 90.9(4) . . . . ?
Ti1 N1 C8 C5 -24.4(4) . . . . ?
O2 C5 C8 N1 38.5(4) . . . . ?
C6 C5 C8 N1 156.3(3) . . . . ?
C7 C5 C8 N1 -82.1(4) . . . . ?
Ti1 O3 C9 C10 85.5(4) . . . . ?
Ti1 O3 C9 C11 -154.6(3) . . . . ?
Ti1 O3 C9 C12 -37.4(5) . . . . ?
C4 N1 C12 C9 93.3(4) . . . . ?
C8 N1 C12 C9 -136.9(3) . . . . ?
Ti1 N1 C12 C9 -22.2(4) . . . . ?
O3 C9 C12 N1 34.7(5) . . . . ?
C10 C9 C12 N1 -85.6(4) . . . . ?
C11 C9 C12 N1 151.3(4) . . . . ?

_refine_diff_density_max         0.715
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.086


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_s21alj16
_database_code_depnum_ccdc_archive 'CCDC 2260245'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok Kohn'
;Material and Chemical Characterisation Facility, University of Bath
United Kingdom
;
_audit_update_record             
;
2023-05-02 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H29 N O4 Ti'
_chemical_formula_sum            'C14 H29 N O4 Ti'
_chemical_formula_weight         323.28

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

_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'

_cell_length_a                   9.4321(3)
_cell_length_b                   9.6745(4)
_cell_length_c                   19.0259(8)
_cell_angle_alpha                86.629(4)
_cell_angle_beta                 88.435(3)
_cell_angle_gamma                80.670(3)
_cell_volume                     1709.92(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    5240
_cell_measurement_theta_min      4.6550
_cell_measurement_theta_max      72.8670

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.256
_exptl_crystal_F_000             696
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.291
_exptl_crystal_size_mid          0.127
_exptl_crystal_size_min          0.104
_exptl_absorpt_coefficient_mu    4.343
_shelx_estimated_absorpt_T_min   0.365
_shelx_estimated_absorpt_T_max   0.661
_exptl_absorpt_correction_T_min  0.67937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.763
_oxdiff_exptl_absorpt_empirical_full_max 1.509
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            11952
_diffrn_reflns_av_unetI/netI     0.0497
_diffrn_reflns_av_R_equivalents  0.0324
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_theta_min         4.639
_diffrn_reflns_theta_max         73.252
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measured_fraction_theta_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.969
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.969
_diffrn_reflns_point_group_measured_fraction_full 0.995
_reflns_number_total             6637
_reflns_number_gt                5421
_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       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.102a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 one OEt group is disordered over two sites in the ratio 70:30
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0425P)²+1.1308P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         6637
_refine_ls_number_parameters     395
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1177
_refine_ls_wR_factor_gt          0.1107
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_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 0.64438(5) 0.57487(5) 0.34628(3) 0.02405(13) Uani 1 1 d . . . . .
N1 N 0.3007(2) -0.1630(2) 0.17743(12) 0.0248(5) Uani 1 1 d . . . . .
O1 O 0.1823(2) -0.01412(19) 0.06721(11) 0.0305(4) Uani 1 1 d . . . . .
O2 O 0.1261(2) 0.0541(2) 0.22569(11) 0.0346(5) Uani 1 1 d . . . . .
O3 O 0.4270(2) 0.0601(2) 0.15663(12) 0.0337(5) Uani 1 1 d . . . . .
O4 O 0.1828(2) 0.2555(2) 0.11514(12) 0.0347(5) Uani 1 1 d . . . . .
C1 C 0.1591(3) -0.1570(3) 0.06802(16) 0.0300(6) Uani 1 1 d . . . . .
C2 C 0.1811(4) -0.2083(3) -0.00613(17) 0.0413(8) Uani 1 1 d . . . . .
H2A H 0.110592 -0.151820 -0.037418 0.062 Uiso 1 1 calc R U . . .
H2B H 0.168456 -0.306929 -0.005636 0.062 Uiso 1 1 calc R U . . .
H2C H 0.278334 -0.199224 -0.023124 0.062 Uiso 1 1 calc R U . . .
C3 C 0.0048(3) -0.1639(3) 0.09279(19) 0.0394(7) Uani 1 1 d . . . . .
H3A H -0.013263 -0.120160 0.138021 0.059 Uiso 1 1 calc R U . . .
H3B H -0.009178 -0.262180 0.098385 0.059 Uiso 1 1 calc R U . . .
H3C H -0.062063 -0.113882 0.057841 0.059 Uiso 1 1 calc R U . . .
C4 C 0.2742(3) -0.2426(3) 0.11630(16) 0.0284(6) Uani 1 1 d . . . . .
H4A H 0.241913 -0.331330 0.133249 0.034 Uiso 1 1 calc R U . . .
H4B H 0.364846 -0.266535 0.089022 0.034 Uiso 1 1 calc R U . . .
C5 C 0.1540(3) -0.0588(3) 0.27777(16) 0.0320(6) Uani 1 1 d . . . . .
C6 C 0.2603(4) -0.0228(3) 0.32995(18) 0.0417(8) Uani 1 1 d . . . . .
H6A H 0.344626 0.002786 0.304325 0.063 Uiso 1 1 calc R U . . .
H6B H 0.290198 -0.104391 0.362263 0.063 Uiso 1 1 calc R U . . .
H6C H 0.214441 0.056230 0.356834 0.063 Uiso 1 1 calc R U . . .
C7 C 0.0132(4) -0.0782(4) 0.31586(19) 0.0454(8) Uani 1 1 d . . . . .
H7A H -0.022930 0.005276 0.341806 0.068 Uiso 1 1 calc R U . . .
H7B H 0.030107 -0.160581 0.348867 0.068 Uiso 1 1 calc R U . . .
H7C H -0.057850 -0.091743 0.281335 0.068 Uiso 1 1 calc R U . . .
C8 C 0.2091(3) -0.1929(3) 0.23972(15) 0.0278(6) Uani 1 1 d . . . . .
H8A H 0.265556 -0.262280 0.272657 0.033 Uiso 1 1 calc R U . . .
H8B H 0.126392 -0.233944 0.224222 0.033 Uiso 1 1 calc R U . . .
C9 C 0.5292(3) -0.0672(3) 0.15801(16) 0.0298(6) Uani 1 1 d . . . . .
C10 C 0.5787(3) -0.0986(3) 0.08305(17) 0.0379(7) Uani 1 1 d . . . . .
H10A H 0.495348 -0.105919 0.054682 0.057 Uiso 1 1 calc R U . . .
H10B H 0.645741 -0.187332 0.083424 0.057 Uiso 1 1 calc R U . . .
H10C H 0.626957 -0.022723 0.062731 0.057 Uiso 1 1 calc R U . . .
C11 C 0.6576(3) -0.0473(3) 0.20108(18) 0.0374(7) Uani 1 1 d . . . . .
H11A H 0.706628 0.024698 0.177285 0.056 Uiso 1 1 calc R U . . .
H11B H 0.724412 -0.136067 0.205709 0.056 Uiso 1 1 calc R U . . .
H11C H 0.624331 -0.017871 0.247946 0.056 Uiso 1 1 calc R U . . .
C12 C 0.4550(3) -0.1819(3) 0.19586(15) 0.0264(6) Uani 1 1 d . . . . .
H12A H 0.503502 -0.275297 0.182180 0.032 Uiso 1 1 calc R U . . .
H12B H 0.463571 -0.177866 0.247417 0.032 Uiso 1 1 calc R U . . .
C13 C 0.1950(4) 0.3613(4) 0.0637(2) 0.0448(8) Uani 1 1 d . . . . .
H13A H 0.139389 0.450491 0.079188 0.054 Uiso 1 1 calc R U . . .
H13B H 0.152223 0.338664 0.019735 0.054 Uiso 1 1 calc R U . . .
C14 C 0.3470(4) 0.3811(3) 0.04883(18) 0.0423(8) Uani 1 1 d . . . . .
H14A H 0.388827 0.407263 0.091718 0.063 Uiso 1 1 calc R U . . .
H14B H 0.349168 0.455577 0.011802 0.063 Uiso 1 1 calc R U . . .
H14C H 0.402546 0.293385 0.033182 0.063 Uiso 1 1 calc R U . . .
Ti2 Ti 0.23306(5) 0.07304(5) 0.14421(3) 0.02634(13) Uani 1 1 d . . . . .
N2 N 0.6894(2) 0.3363(2) 0.32653(12) 0.0267(5) Uani 1 1 d . . . . .
O21 O 0.7585(2) 0.5009(2) 0.42045(11) 0.0337(5) Uani 1 1 d . . . . .
O22 O 0.46256(19) 0.53084(19) 0.34456(11) 0.0285(4) Uani 1 1 d . . . . .
O23 O 0.7302(2) 0.5721(2) 0.25836(10) 0.0288(4) Uani 1 1 d . . . . .
O24 O 0.6127(2) 0.7583(2) 0.36546(11) 0.0331(5) Uani 1 1 d . . . . .
C21 C 0.7849(3) 0.3579(3) 0.44553(16) 0.0342(7) Uani 1 1 d . . . . .
C22 C 0.9303(4) 0.3281(4) 0.48166(19) 0.0476(9) Uani 1 1 d . . . . .
H22A H 1.005906 0.347448 0.447919 0.071 Uiso 1 1 calc R U . . .
H22B H 0.949554 0.229448 0.498786 0.071 Uiso 1 1 calc R U . . .
H22C H 0.928549 0.388288 0.521443 0.071 Uiso 1 1 calc R U . . .
C23 C 0.6669(4) 0.3305(4) 0.49802(17) 0.0435(8) Uani 1 1 d . . . . .
H23A H 0.671095 0.385727 0.539259 0.065 Uiso 1 1 calc R U . . .
H23B H 0.680401 0.230529 0.512719 0.065 Uiso 1 1 calc R U . . .
H23C H 0.573085 0.357655 0.475924 0.065 Uiso 1 1 calc R U . . .
C24 C 0.7941(3) 0.2699(3) 0.38009(16) 0.0319(6) Uani 1 1 d . . . . .
H24A H 0.892482 0.260715 0.359514 0.038 Uiso 1 1 calc R U . . .
H24B H 0.774281 0.174654 0.394173 0.038 Uiso 1 1 calc R U . . .
C25 C 0.4226(3) 0.4051(3) 0.32031(16) 0.0306(6) Uani 1 1 d . . . . .
C26 C 0.2907(3) 0.3763(4) 0.3627(2) 0.0449(8) Uani 1 1 d . . . . .
H26A H 0.314506 0.361606 0.412670 0.067 Uiso 1 1 calc R U . . .
H26B H 0.259128 0.292156 0.346447 0.067 Uiso 1 1 calc R U . . .
H26C H 0.213390 0.456627 0.356287 0.067 Uiso 1 1 calc R U . . .
C27 C 0.3873(3) 0.4264(3) 0.24283(17) 0.0368(7) Uani 1 1 d . . . . .
H27A H 0.297850 0.493020 0.236898 0.055 Uiso 1 1 calc R U . . .
H27B H 0.375556 0.336422 0.224464 0.055 Uiso 1 1 calc R U . . .
H27C H 0.465575 0.463393 0.217011 0.055 Uiso 1 1 calc R U . . .
C28 C 0.5493(3) 0.2859(3) 0.33613(17) 0.0322(6) Uani 1 1 d . . . . .
H28A H 0.539996 0.247852 0.385192 0.039 Uiso 1 1 calc R U . . .
H28B H 0.545871 0.209133 0.304353 0.039 Uiso 1 1 calc R U . . .
C29 C 0.8139(3) 0.4541(3) 0.22808(16) 0.0308(6) Uani 1 1 d . . . . .
C30 C 0.8047(4) 0.4723(4) 0.14831(17) 0.0417(8) Uani 1 1 d . . . . .
H30A H 0.704233 0.480783 0.134491 0.063 Uiso 1 1 calc R U . . .
H30B H 0.861394 0.390653 0.127157 0.063 Uiso 1 1 calc R U . . .
H30C H 0.842703 0.557256 0.131875 0.063 Uiso 1 1 calc R U . . .
C31 C 0.9699(3) 0.4472(4) 0.25011(19) 0.0407(8) Uani 1 1 d . . . . .
H31A H 1.006237 0.531437 0.231149 0.061 Uiso 1 1 calc R U . . .
H31B H 1.028903 0.363826 0.231667 0.061 Uiso 1 1 calc R U . . .
H31C H 0.974544 0.441989 0.301613 0.061 Uiso 1 1 calc R U . . .
C32 C 0.7485(3) 0.3234(3) 0.25355(15) 0.0305(6) Uani 1 1 d . . . . .
H32A H 0.670946 0.311390 0.221538 0.037 Uiso 1 1 calc R U . . .
H32B H 0.823461 0.239086 0.251994 0.037 Uiso 1 1 calc R U . . .
C33 C 0.6293(9) 0.8825(6) 0.3962(3) 0.0436(16) Uani 0.698(13) 1 d . . P A 1
H33A H 0.533362 0.938464 0.404445 0.052 Uiso 0.698(13) 1 calc R U P A 1
H33B H 0.683517 0.938290 0.363144 0.052 Uiso 0.698(13) 1 calc R U P A 1
C34 C 0.7053(9) 0.8557(7) 0.4632(3) 0.060(2) Uani 0.698(13) 1 d . . P A 1
H34A H 0.639787 0.827259 0.500121 0.090 Uiso 0.698(13) 1 calc R U P A 1
H34B H 0.739108 0.941372 0.475873 0.090 Uiso 0.698(13) 1 calc R U P A 1
H34C H 0.787626 0.780697 0.458209 0.090 Uiso 0.698(13) 1 calc R U P A 1
C33A C 0.6985(17) 0.8346(18) 0.4078(10) 0.046(5) Uani 0.302(13) 1 d . . P A 2
H33C H 0.747130 0.898592 0.376642 0.056 Uiso 0.302(13) 1 calc R U P A 2
H33D H 0.773219 0.767226 0.432781 0.056 Uiso 0.302(13) 1 calc R U P A 2
C34A C 0.6056(17) 0.9165(14) 0.4597(7) 0.047(4) Uani 0.302(13) 1 d . . P A 2
H34D H 0.536993 0.988616 0.434829 0.070 Uiso 0.302(13) 1 calc R U P A 2
H34E H 0.665139 0.961448 0.489886 0.070 Uiso 0.302(13) 1 calc R U P A 2
H34F H 0.553167 0.853808 0.488687 0.070 Uiso 0.302(13) 1 calc R U P A 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 O24 1.8083(19) . ?
Ti1 O22 1.8345(18) . ?
Ti1 O21 1.837(2) . ?
Ti1 O23 1.838(2) . ?
Ti1 N2 2.329(2) . ?
N1 C4 1.481(3) . ?
N1 C12 1.487(3) . ?
N1 C8 1.490(3) . ?
N1 Ti2 2.324(2) . ?
O1 C1 1.433(3) . ?
O1 Ti2 1.844(2) . ?
O2 C5 1.427(3) . ?
O2 Ti2 1.843(2) . ?
O3 C9 1.435(3) . ?
O3 Ti2 1.834(2) . ?
O4 C13 1.390(4) . ?
O4 Ti2 1.8098(19) . ?
C1 C2 1.521(4) . ?
C1 C3 1.528(4) . ?
C1 C4 1.543(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.523(4) . ?
C5 C7 1.529(4) . ?
C5 C8 1.533(4) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.521(4) . ?
C9 C11 1.524(4) . ?
C9 C12 1.539(4) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C13 C14 1.494(4) . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
N2 C24 1.483(4) . ?
N2 C28 1.484(3) . ?
N2 C32 1.487(4) . ?
O21 C21 1.422(3) . ?
O22 C25 1.435(3) . ?
O23 C29 1.421(3) . ?
O24 C33 1.399(5) . ?
O24 C33A 1.466(14) . ?
C21 C23 1.520(4) . ?
C21 C22 1.529(4) . ?
C21 C24 1.542(4) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C27 1.515(4) . ?
C25 C26 1.518(4) . ?
C25 C28 1.543(4) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C30 1.521(4) . ?
C29 C31 1.532(4) . ?
C29 C32 1.542(4) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C33 C34 1.468(9) . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C34 H34A 0.9800 . ?
C34 H34B 0.9800 . ?
C34 H34C 0.9800 . ?
C33A C34A 1.48(2) . ?
C33A H33C 0.9900 . ?
C33A H33D 0.9900 . ?
C34A H34D 0.9800 . ?
C34A H34E 0.9800 . ?
C34A H34F 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
O24 Ti1 O22 103.20(9) . . ?
O24 Ti1 O21 100.43(9) . . ?
O22 Ti1 O21 117.63(9) . . ?
O24 Ti1 O23 104.27(9) . . ?
O22 Ti1 O23 111.77(9) . . ?
O21 Ti1 O23 116.73(9) . . ?
O24 Ti1 N2 177.46(9) . . ?
O22 Ti1 N2 77.68(8) . . ?
O21 Ti1 N2 77.09(9) . . ?
O23 Ti1 N2 77.47(8) . . ?
C4 N1 C12 112.9(2) . . ?
C4 N1 C8 112.2(2) . . ?
C12 N1 C8 111.5(2) . . ?
C4 N1 Ti2 106.54(16) . . ?
C12 N1 Ti2 106.60(15) . . ?
C8 N1 Ti2 106.50(15) . . ?
C1 O1 Ti2 124.89(17) . . ?
C5 O2 Ti2 125.18(17) . . ?
C9 O3 Ti2 125.53(16) . . ?
C13 O4 Ti2 147.6(2) . . ?
O1 C1 C2 109.1(2) . . ?
O1 C1 C3 108.8(2) . . ?
C2 C1 C3 109.3(3) . . ?
O1 C1 C4 106.5(2) . . ?
C2 C1 C4 109.1(2) . . ?
C3 C1 C4 113.9(2) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C1 111.3(2) . . ?
N1 C4 H4A 109.4 . . ?
C1 C4 H4A 109.4 . . ?
N1 C4 H4B 109.4 . . ?
C1 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
O2 C5 C6 108.7(2) . . ?
O2 C5 C7 109.1(2) . . ?
C6 C5 C7 110.0(3) . . ?
O2 C5 C8 107.8(2) . . ?
C6 C5 C8 113.4(2) . . ?
C7 C5 C8 107.9(2) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C5 111.0(2) . . ?
N1 C8 H8A 109.4 . . ?
C5 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C5 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O3 C9 C10 109.0(2) . . ?
O3 C9 C11 108.8(2) . . ?
C10 C9 C11 109.5(2) . . ?
O3 C9 C12 106.9(2) . . ?
C10 C9 C12 113.9(2) . . ?
C11 C9 C12 108.6(2) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C9 110.8(2) . . ?
N1 C12 H12A 109.5 . . ?
C9 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
O4 C13 C14 113.0(3) . . ?
O4 C13 H13A 109.0 . . ?
C14 C13 H13A 109.0 . . ?
O4 C13 H13B 109.0 . . ?
C14 C13 H13B 109.0 . . ?
H13A C13 H13B 107.8 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 Ti2 O3 101.96(9) . . ?
O4 Ti2 O2 104.14(9) . . ?
O3 Ti2 O2 115.08(10) . . ?
O4 Ti2 O1 100.74(10) . . ?
O3 Ti2 O1 115.09(9) . . ?
O2 Ti2 O1 116.63(9) . . ?
O4 Ti2 N1 177.92(9) . . ?
O3 Ti2 N1 77.66(8) . . ?
O2 Ti2 N1 77.82(8) . . ?
O1 Ti2 N1 77.66(8) . . ?
C24 N2 C28 111.7(2) . . ?
C24 N2 C32 112.4(2) . . ?
C28 N2 C32 112.8(2) . . ?
C24 N2 Ti1 106.52(16) . . ?
C28 N2 Ti1 106.08(16) . . ?
C32 N2 Ti1 106.75(16) . . ?
C21 O21 Ti1 126.39(18) . . ?
C25 O22 Ti1 126.88(16) . . ?
C29 O23 Ti1 126.25(18) . . ?
C33 O24 Ti1 159.4(4) . . ?
C33A O24 Ti1 128.8(8) . . ?
O21 C21 C23 109.1(2) . . ?
O21 C21 C22 109.0(3) . . ?
C23 C21 C22 109.7(3) . . ?
O21 C21 C24 106.5(2) . . ?
C23 C21 C24 114.1(3) . . ?
C22 C21 C24 108.4(3) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N2 C24 C21 110.9(2) . . ?
N2 C24 H24A 109.5 . . ?
C21 C24 H24A 109.5 . . ?
N2 C24 H24B 109.5 . . ?
C21 C24 H24B 109.5 . . ?
H24A C24 H24B 108.0 . . ?
O22 C25 C27 109.5(2) . . ?
O22 C25 C26 107.5(2) . . ?
C27 C25 C26 109.9(3) . . ?
O22 C25 C28 106.8(2) . . ?
C27 C25 C28 113.3(3) . . ?
C26 C25 C28 109.7(3) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N2 C28 C25 111.4(2) . . ?
N2 C28 H28A 109.3 . . ?
C25 C28 H28A 109.3 . . ?
N2 C28 H28B 109.3 . . ?
C25 C28 H28B 109.3 . . ?
H28A C28 H28B 108.0 . . ?
O23 C29 C30 109.1(2) . . ?
O23 C29 C31 108.1(2) . . ?
C30 C29 C31 109.7(3) . . ?
O23 C29 C32 107.5(2) . . ?
C30 C29 C32 109.0(2) . . ?
C31 C29 C32 113.3(3) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N2 C32 C29 111.2(2) . . ?
N2 C32 H32A 109.4 . . ?
C29 C32 H32A 109.4 . . ?
N2 C32 H32B 109.4 . . ?
C29 C32 H32B 109.4 . . ?
H32A C32 H32B 108.0 . . ?
O24 C33 C34 112.2(6) . . ?
O24 C33 H33A 109.2 . . ?
C34 C33 H33A 109.2 . . ?
O24 C33 H33B 109.2 . . ?
C34 C33 H33B 109.2 . . ?
H33A C33 H33B 107.9 . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
O24 C33A C34A 110.3(12) . . ?
O24 C33A H33C 109.6 . . ?
C34A C33A H33C 109.6 . . ?
O24 C33A H33D 109.6 . . ?
C34A C33A H33D 109.6 . . ?
H33C C33A H33D 108.1 . . ?
C33A C34A H34D 109.5 . . ?
C33A C34A H34E 109.5 . . ?
H34D C34A H34E 109.5 . . ?
C33A C34A H34F 109.5 . . ?
H34D C34A H34F 109.5 . . ?
H34E C34A H34F 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
Ti2 O1 C1 C2 -156.56(19) . . . . ?
Ti2 O1 C1 C3 84.3(3) . . . . ?
Ti2 O1 C1 C4 -38.9(3) . . . . ?
C12 N1 C4 C1 -140.6(2) . . . . ?
C8 N1 C4 C1 92.3(3) . . . . ?
Ti2 N1 C4 C1 -23.9(2) . . . . ?
O1 C1 C4 N1 37.5(3) . . . . ?
C2 C1 C4 N1 155.1(2) . . . . ?
C3 C1 C4 N1 -82.4(3) . . . . ?
Ti2 O2 C5 C6 87.3(3) . . . . ?
Ti2 O2 C5 C7 -152.9(2) . . . . ?
Ti2 O2 C5 C8 -36.0(3) . . . . ?
C4 N1 C8 C5 -139.9(2) . . . . ?
C12 N1 C8 C5 92.2(3) . . . . ?
Ti2 N1 C8 C5 -23.7(3) . . . . ?
O2 C5 C8 N1 36.0(3) . . . . ?
C6 C5 C8 N1 -84.3(3) . . . . ?
C7 C5 C8 N1 153.7(2) . . . . ?
Ti2 O3 C9 C10 86.4(3) . . . . ?
Ti2 O3 C9 C11 -154.2(2) . . . . ?
Ti2 O3 C9 C12 -37.2(3) . . . . ?
C4 N1 C12 C9 92.0(3) . . . . ?
C8 N1 C12 C9 -140.5(2) . . . . ?
Ti2 N1 C12 C9 -24.6(3) . . . . ?
O3 C9 C12 N1 37.0(3) . . . . ?
C10 C9 C12 N1 -83.5(3) . . . . ?
C11 C9 C12 N1 154.2(2) . . . . ?
Ti2 O4 C13 C14 -56.5(5) . . . . ?
C13 O4 Ti2 O3 64.7(4) . . . . ?
C13 O4 Ti2 O2 -175.3(4) . . . . ?
C13 O4 Ti2 O1 -54.1(4) . . . . ?
C9 O3 Ti2 O4 -159.3(2) . . . . ?
C9 O3 Ti2 O2 88.7(2) . . . . ?
C9 O3 Ti2 O1 -51.3(2) . . . . ?
C9 O3 Ti2 N1 18.6(2) . . . . ?
C5 O2 Ti2 O4 -162.8(2) . . . . ?
C5 O2 Ti2 O3 -52.1(2) . . . . ?
C5 O2 Ti2 O1 87.2(2) . . . . ?
C5 O2 Ti2 N1 17.9(2) . . . . ?
C1 O1 Ti2 O4 -160.9(2) . . . . ?
C1 O1 Ti2 O3 90.4(2) . . . . ?
C1 O1 Ti2 O2 -49.0(2) . . . . ?
C1 O1 Ti2 N1 20.5(2) . . . . ?
O24 Ti1 O21 C21 160.8(2) . . . . ?
O22 Ti1 O21 C21 49.8(3) . . . . ?
O23 Ti1 O21 C21 -87.3(2) . . . . ?
N2 Ti1 O21 C21 -18.7(2) . . . . ?
O24 Ti1 O22 C25 168.9(2) . . . . ?
O21 Ti1 O22 C25 -81.7(2) . . . . ?
O23 Ti1 O22 C25 57.4(2) . . . . ?
N2 Ti1 O22 C25 -13.6(2) . . . . ?
O24 Ti1 O23 C29 160.0(2) . . . . ?
O22 Ti1 O23 C29 -89.2(2) . . . . ?
O21 Ti1 O23 C29 50.3(2) . . . . ?
N2 Ti1 O23 C29 -18.1(2) . . . . ?
O22 Ti1 O24 C33 136.8(10) . . . . ?
O21 Ti1 O24 C33 14.9(10) . . . . ?
O23 Ti1 O24 C33 -106.3(10) . . . . ?
O22 Ti1 O24 C33A 144.7(8) . . . . ?
O21 Ti1 O24 C33A 22.8(8) . . . . ?
O23 Ti1 O24 C33A -98.4(8) . . . . ?
Ti1 O21 C21 C23 -86.3(3) . . . . ?
Ti1 O21 C21 C22 154.0(2) . . . . ?
Ti1 O21 C21 C24 37.2(3) . . . . ?
C28 N2 C24 C21 -90.5(3) . . . . ?
C32 N2 C24 C21 141.5(2) . . . . ?
Ti1 N2 C24 C21 24.9(3) . . . . ?
O21 C21 C24 N2 -37.1(3) . . . . ?
C23 C21 C24 N2 83.3(3) . . . . ?
C22 C21 C24 N2 -154.2(3) . . . . ?
Ti1 O22 C25 C27 -91.2(3) . . . . ?
Ti1 O22 C25 C26 149.4(2) . . . . ?
Ti1 O22 C25 C28 31.8(3) . . . . ?
C24 N2 C28 C25 142.5(2) . . . . ?
C32 N2 C28 C25 -89.7(3) . . . . ?
Ti1 N2 C28 C25 26.8(3) . . . . ?
O22 C25 C28 N2 -35.9(3) . . . . ?
C27 C25 C28 N2 84.8(3) . . . . ?
C26 C25 C28 N2 -152.1(3) . . . . ?
Ti1 O23 C29 C30 153.26(19) . . . . ?
Ti1 O23 C29 C31 -87.6(3) . . . . ?
Ti1 O23 C29 C32 35.2(3) . . . . ?
C24 N2 C32 C29 -94.2(3) . . . . ?
C28 N2 C32 C29 138.3(2) . . . . ?
Ti1 N2 C32 C29 22.2(3) . . . . ?
O23 C29 C32 N2 -34.2(3) . . . . ?
C30 C29 C32 N2 -152.4(2) . . . . ?
C31 C29 C32 N2 85.2(3) . . . . ?
Ti1 O24 C33 C34 -21.2(15) . . . . ?
Ti1 O24 C33A C34A -130.1(12) . . . . ?

_refine_diff_density_max         0.406
_refine_diff_density_min         -0.387
_refine_diff_density_rms         0.057


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_s21alj20
_database_code_depnum_ccdc_archive 'CCDC 2260246'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok Kohn'
;Material and Chemical Characterisation Facility, University of Bath
United Kingdom
;
_audit_update_record             
;
2023-05-02 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C15 H31 N O4 Ti'
_chemical_formula_sum            'C15 H31 N O4 Ti'
_chemical_formula_weight         337.31

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.46549(10)
_cell_length_b                   13.05943(14)
_cell_length_c                   14.98051(15)
_cell_angle_alpha                90
_cell_angle_beta                 91.4818(9)
_cell_angle_gamma                90
_cell_volume                     1851.18(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    10259
_cell_measurement_theta_min      4.4950
_cell_measurement_theta_max      73.1190

_exptl_crystal_description       needle
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.210
_exptl_crystal_F_000             728
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.020
_exptl_absorpt_coefficient_mu    4.032
_shelx_estimated_absorpt_T_min   0.689
_shelx_estimated_absorpt_T_max   0.924
_exptl_absorpt_correction_T_min  0.65041
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.102a (Rigaku Oxford Diffraction, 2021)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.760
_oxdiff_exptl_absorpt_empirical_full_max 1.973
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.00(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            16233
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         4.492
_diffrn_reflns_theta_max         73.191
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             3689
_reflns_number_gt                3539
_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       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_data_reduction        'CrysAlisPro 1.171.41.112a (Rigaku OD, 2021)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_refine_special_details          
;
 the isopropyl group is disordered over two sites in the ratio 60:40
 and was refined with ADP restraints
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0524P)²+0.6047P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0040(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         3689
_refine_ls_number_parameters     229
_refine_ls_number_restraints     24
_refine_ls_R_factor_all          0.0328
_refine_ls_R_factor_gt           0.0317
_refine_ls_wR_factor_ref         0.0892
_refine_ls_wR_factor_gt          0.0882
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_restrained_S_all      1.049
_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 0.33918(3) 0.36008(2) 0.65501(2) 0.02005(11) Uani 1 1 d . . . . .
N1 N 0.35943(13) 0.21925(9) 0.75205(8) 0.0226(3) Uani 1 1 d . . . . .
O1 O 0.15566(11) 0.31774(8) 0.66528(7) 0.0284(2) Uani 1 1 d . . . . .
O2 O 0.41718(11) 0.41887(8) 0.75653(7) 0.0257(2) Uani 1 1 d . . . . .
O3 O 0.45637(11) 0.27220(8) 0.59579(7) 0.0270(2) Uani 1 1 d . . . . .
O4 O 0.31961(13) 0.46306(9) 0.57554(7) 0.0320(3) Uani 1 1 d . . . . .
C1 C 0.10153(16) 0.25504(12) 0.73416(10) 0.0284(3) Uani 1 1 d . . . . .
C2 C 0.06167(19) 0.32349(15) 0.81230(12) 0.0390(4) Uani 1 1 d . . . . .
H2A H 0.144303 0.363404 0.832205 0.059 Uiso 1 1 calc R U . . .
H2B H 0.029524 0.280882 0.861647 0.059 Uiso 1 1 calc R U . . .
H2C H -0.014401 0.370096 0.793153 0.059 Uiso 1 1 calc R U . . .
C3 C -0.03002(18) 0.20063(16) 0.69731(13) 0.0410(4) Uani 1 1 d . . . . .
H3A H -0.104826 0.251020 0.685237 0.062 Uiso 1 1 calc R U . . .
H3B H -0.062365 0.150748 0.741172 0.062 Uiso 1 1 calc R U . . .
H3C H -0.007429 0.165166 0.641820 0.062 Uiso 1 1 calc R U . . .
C4 C 0.21565(16) 0.17474(12) 0.75843(10) 0.0283(3) Uani 1 1 d . . . . .
H4A H 0.201668 0.149831 0.819988 0.034 Uiso 1 1 calc R U . . .
H4B H 0.206249 0.115566 0.717394 0.034 Uiso 1 1 calc R U . . .
C5 C 0.49318(16) 0.36307(11) 0.82425(10) 0.0249(3) Uani 1 1 d . . . . .
C6 C 0.64555(17) 0.34997(13) 0.79540(12) 0.0345(4) Uani 1 1 d . . . . .
H6A H 0.646321 0.318230 0.736130 0.052 Uiso 1 1 calc R U . . .
H6B H 0.696650 0.306134 0.838394 0.052 Uiso 1 1 calc R U . . .
H6C H 0.691538 0.417116 0.793130 0.052 Uiso 1 1 calc R U . . .
C7 C 0.49109(19) 0.42346(13) 0.91129(10) 0.0352(4) Uani 1 1 d . . . . .
H7A H 0.545159 0.486894 0.904738 0.053 Uiso 1 1 calc R U . . .
H7B H 0.533535 0.382220 0.959608 0.053 Uiso 1 1 calc R U . . .
H7C H 0.393237 0.440087 0.925470 0.053 Uiso 1 1 calc R U . . .
C8 C 0.41390(16) 0.26182(11) 0.83812(9) 0.0259(3) Uani 1 1 d . . . . .
H8A H 0.478462 0.211607 0.867248 0.031 Uiso 1 1 calc R U . . .
H8B H 0.333959 0.273633 0.878191 0.031 Uiso 1 1 calc R U . . .
C9 C 0.46973(17) 0.16518(12) 0.61069(10) 0.0273(3) Uani 1 1 d . . . . .
C10 C 0.35375(19) 0.11093(14) 0.55637(11) 0.0360(4) Uani 1 1 d . . . . .
H10A H 0.261397 0.137946 0.572811 0.054 Uiso 1 1 calc R U . . .
H10B H 0.357438 0.037284 0.568772 0.054 Uiso 1 1 calc R U . . .
H10C H 0.367833 0.122677 0.492604 0.054 Uiso 1 1 calc R U . . .
C11 C 0.6154(2) 0.13099(15) 0.58020(13) 0.0414(4) Uani 1 1 d . . . . .
H11A H 0.621587 0.141058 0.515595 0.062 Uiso 1 1 calc R U . . .
H11B H 0.629110 0.058358 0.594407 0.062 Uiso 1 1 calc R U . . .
H11C H 0.688655 0.171634 0.611069 0.062 Uiso 1 1 calc R U . . .
C12 C 0.46087(17) 0.14742(11) 0.71208(10) 0.0278(3) Uani 1 1 d . . . . .
H12A H 0.430606 0.076126 0.723376 0.033 Uiso 1 1 calc R U . . .
H12B H 0.555476 0.157175 0.740539 0.033 Uiso 1 1 calc R U . . .
C41 C 0.3151(6) 0.4992(3) 0.4865(2) 0.0366(11) Uani 0.548(9) 1 d . . P A 1
H41 H 0.414991 0.513599 0.470411 0.044 Uiso 0.548(9) 1 calc R U P A 1
C42 C 0.2412(8) 0.5889(3) 0.4728(3) 0.0568(16) Uani 0.548(9) 1 d . U P A 1
H42A H 0.166772 0.594438 0.516813 0.085 Uiso 0.548(9) 1 calc R U P A 1
H42B H 0.198456 0.588879 0.412506 0.085 Uiso 0.548(9) 1 calc R U P A 1
H42C H 0.305782 0.647236 0.479285 0.085 Uiso 0.548(9) 1 calc R U P A 1
C43 C 0.2650(14) 0.4069(7) 0.4277(6) 0.105(4) Uani 0.548(9) 1 d . U P A 1
H43A H 0.269830 0.425506 0.364502 0.158 Uiso 0.548(9) 1 calc R U P A 1
H43B H 0.167386 0.389419 0.441792 0.158 Uiso 0.548(9) 1 calc R U P A 1
H43C H 0.326322 0.347836 0.439952 0.158 Uiso 0.548(9) 1 calc R U P A 1
C41A C 0.2332(8) 0.4745(4) 0.4930(3) 0.0436(15) Uani 0.452(9) 1 d . . P A 2
H41A H 0.157455 0.421910 0.499459 0.052 Uiso 0.452(9) 1 calc R U P A 2
C42A C 0.1679(14) 0.5524(12) 0.4761(7) 0.131(5) Uani 0.452(9) 1 d . U P A 2
H42D H 0.092900 0.561174 0.519305 0.196 Uiso 0.452(9) 1 calc R U P A 2
H42E H 0.125889 0.547744 0.415724 0.196 Uiso 0.452(9) 1 calc R U P A 2
H42F H 0.232153 0.611210 0.479475 0.196 Uiso 0.452(9) 1 calc R U P A 2
C43A C 0.3338(8) 0.4258(7) 0.4194(5) 0.0504(18) Uani 0.452(9) 1 d . U P A 2
H43D H 0.298687 0.445062 0.359606 0.076 Uiso 0.452(9) 1 calc R U P A 2
H43E H 0.333741 0.351089 0.425069 0.076 Uiso 0.452(9) 1 calc R U P A 2
H43F H 0.430265 0.451689 0.428625 0.076 Uiso 0.452(9) 1 calc R U P A 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 O4 1.8024(11) . ?
Ti1 O1 1.8333(11) . ?
Ti1 O3 1.8400(10) . ?
Ti1 O2 1.8411(10) . ?
Ti1 N1 2.3491(12) . ?
N1 C12 1.4799(18) . ?
N1 C8 1.4843(17) . ?
N1 C4 1.4853(19) . ?
O1 C1 1.4231(18) . ?
O2 C5 1.4283(17) . ?
O3 C9 1.4205(19) . ?
O4 C41 1.414(3) . ?
O4 C41A 1.472(4) . ?
C1 C3 1.525(2) . ?
C1 C2 1.528(2) . ?
C1 C4 1.542(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C7 1.5243(19) . ?
C5 C6 1.526(2) . ?
C5 C8 1.537(2) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.524(2) . ?
C9 C11 1.530(2) . ?
C9 C12 1.541(2) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C41 C42 1.377(6) . ?
C41 C43 1.559(9) . ?
C41 H41 1.0000 . ?
C42 H42A 0.9800 . ?
C42 H42B 0.9800 . ?
C42 H42C 0.9800 . ?
C43 H43A 0.9800 . ?
C43 H43B 0.9800 . ?
C43 H43C 0.9800 . ?
C41A C42A 1.214(12) . ?
C41A C43A 1.607(9) . ?
C41A H41A 1.0000 . ?
C42A H42D 0.9800 . ?
C42A H42E 0.9800 . ?
C42A H42F 0.9800 . ?
C43A H43D 0.9800 . ?
C43A H43E 0.9800 . ?
C43A H43F 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
O4 Ti1 O1 101.48(5) . . ?
O4 Ti1 O3 101.53(5) . . ?
O1 Ti1 O3 115.89(5) . . ?
O4 Ti1 O2 105.47(5) . . ?
O1 Ti1 O2 114.65(5) . . ?
O3 Ti1 O2 115.12(5) . . ?
O4 Ti1 N1 176.61(5) . . ?
O1 Ti1 N1 76.95(5) . . ?
O3 Ti1 N1 76.67(4) . . ?
O2 Ti1 N1 77.92(4) . . ?
C12 N1 C8 111.99(11) . . ?
C12 N1 C4 112.53(11) . . ?
C8 N1 C4 112.89(11) . . ?
C12 N1 Ti1 106.82(9) . . ?
C8 N1 Ti1 105.39(8) . . ?
C4 N1 Ti1 106.62(9) . . ?
C1 O1 Ti1 126.45(9) . . ?
C5 O2 Ti1 123.91(8) . . ?
C9 O3 Ti1 126.18(9) . . ?
C41 O4 Ti1 150.70(17) . . ?
C41A O4 Ti1 132.5(3) . . ?
O1 C1 C3 108.15(13) . . ?
O1 C1 C2 108.64(13) . . ?
C3 C1 C2 109.54(13) . . ?
O1 C1 C4 107.40(12) . . ?
C3 C1 C4 109.21(14) . . ?
C2 C1 C4 113.75(13) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 C1 110.86(12) . . ?
N1 C4 H4A 109.5 . . ?
C1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
C1 C4 H4B 109.5 . . ?
H4A C4 H4B 108.1 . . ?
O2 C5 C7 109.04(12) . . ?
O2 C5 C6 108.57(13) . . ?
C7 C5 C6 109.49(13) . . ?
O2 C5 C8 107.22(11) . . ?
C7 C5 C8 108.19(13) . . ?
C6 C5 C8 114.21(12) . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C5 111.38(11) . . ?
N1 C8 H8A 109.4 . . ?
C5 C8 H8A 109.4 . . ?
N1 C8 H8B 109.4 . . ?
C5 C8 H8B 109.4 . . ?
H8A C8 H8B 108.0 . . ?
O3 C9 C10 108.27(13) . . ?
O3 C9 C11 108.52(14) . . ?
C10 C9 C11 110.30(13) . . ?
O3 C9 C12 107.22(11) . . ?
C10 C9 C12 113.54(14) . . ?
C11 C9 C12 108.83(13) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C9 110.84(12) . . ?
N1 C12 H12A 109.5 . . ?
C9 C12 H12A 109.5 . . ?
N1 C12 H12B 109.5 . . ?
C9 C12 H12B 109.5 . . ?
H12A C12 H12B 108.1 . . ?
C42 C41 O4 115.3(3) . . ?
C42 C41 C43 115.3(5) . . ?
O4 C41 C43 106.0(5) . . ?
C42 C41 H41 106.5 . . ?
O4 C41 H41 106.5 . . ?
C43 C41 H41 106.5 . . ?
C41 C42 H42A 109.5 . . ?
C41 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C41 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C41 C43 H43A 109.5 . . ?
C41 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C41 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
C42A C41A O4 122.0(6) . . ?
C42A C41A C43A 119.7(7) . . ?
O4 C41A C43A 102.1(5) . . ?
C42A C41A H41A 103.5 . . ?
O4 C41A H41A 103.5 . . ?
C43A C41A H41A 103.5 . . ?
C41A C42A H42D 109.5 . . ?
C41A C42A H42E 109.5 . . ?
H42D C42A H42E 109.5 . . ?
C41A C42A H42F 109.5 . . ?
H42D C42A H42F 109.5 . . ?
H42E C42A H42F 109.5 . . ?
C41A C43A H43D 109.5 . . ?
C41A C43A H43E 109.5 . . ?
H43D C43A H43E 109.5 . . ?
C41A C43A H43F 109.5 . . ?
H43D C43A H43F 109.5 . . ?
H43E C43A H43F 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
O4 Ti1 O1 C1 -163.85(11) . . . . ?
O3 Ti1 O1 C1 87.16(12) . . . . ?
O2 Ti1 O1 C1 -50.73(13) . . . . ?
N1 Ti1 O1 C1 19.22(11) . . . . ?
O4 Ti1 O2 C5 -158.13(11) . . . . ?
O1 Ti1 O2 C5 91.12(11) . . . . ?
O3 Ti1 O2 C5 -47.11(12) . . . . ?
N1 Ti1 O2 C5 21.75(11) . . . . ?
O4 Ti1 O3 C9 -156.83(11) . . . . ?
O1 Ti1 O3 C9 -47.87(12) . . . . ?
O2 Ti1 O3 C9 89.82(12) . . . . ?
N1 Ti1 O3 C9 20.23(11) . . . . ?
O1 Ti1 O4 C41 -90.1(5) . . . . ?
O3 Ti1 O4 C41 29.7(5) . . . . ?
O2 Ti1 O4 C41 150.1(5) . . . . ?
O1 Ti1 O4 C41A -41.6(4) . . . . ?
O3 Ti1 O4 C41A 78.2(4) . . . . ?
O2 Ti1 O4 C41A -161.4(3) . . . . ?
Ti1 O1 C1 C3 -154.85(11) . . . . ?
Ti1 O1 C1 C2 86.33(15) . . . . ?
Ti1 O1 C1 C4 -37.11(16) . . . . ?
C12 N1 C4 C1 -139.57(12) . . . . ?
C8 N1 C4 C1 92.46(14) . . . . ?
Ti1 N1 C4 C1 -22.79(13) . . . . ?
O1 C1 C4 N1 35.49(16) . . . . ?
C3 C1 C4 N1 152.55(13) . . . . ?
C2 C1 C4 N1 -84.75(16) . . . . ?
Ti1 O2 C5 C7 -157.84(10) . . . . ?
Ti1 O2 C5 C6 82.94(14) . . . . ?
Ti1 O2 C5 C8 -40.91(15) . . . . ?
C12 N1 C8 C5 91.98(14) . . . . ?
C4 N1 C8 C5 -139.77(12) . . . . ?
Ti1 N1 C8 C5 -23.78(13) . . . . ?
O2 C5 C8 N1 39.00(15) . . . . ?
C7 C5 C8 N1 156.47(12) . . . . ?
C6 C5 C8 N1 -81.33(15) . . . . ?
Ti1 O3 C9 C10 84.56(14) . . . . ?
Ti1 O3 C9 C11 -155.71(10) . . . . ?
Ti1 O3 C9 C12 -38.31(16) . . . . ?
C8 N1 C12 C9 -137.62(13) . . . . ?
C4 N1 C12 C9 93.94(15) . . . . ?
Ti1 N1 C12 C9 -22.73(14) . . . . ?
O3 C9 C12 N1 36.07(17) . . . . ?
C10 C9 C12 N1 -83.47(16) . . . . ?
C11 C9 C12 N1 153.26(13) . . . . ?
Ti1 O4 C41 C42 155.8(4) . . . . ?
Ti1 O4 C41 C43 26.9(10) . . . . ?
Ti1 O4 C41A C42A 135.8(9) . . . . ?
Ti1 O4 C41A C43A -87.1(6) . . . . ?

_refine_diff_density_max         0.266
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.045


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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_s21alj08
_database_code_depnum_ccdc_archive 'CCDC 2260247'
loop_
_audit_author_name
_audit_author_address
'Gabriele Kociok Kohn'
;Material and Chemical Characterisation Facility, University of Bath
United Kingdom
;
_audit_update_record             
;
2023-05-02 deposited with the CCDC.	2023-07-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H30 N2 O3 Ti'
_chemical_formula_sum            'C14 H30 N2 O3 Ti'
_chemical_formula_weight         322.30

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   9.52655(8)
_cell_length_b                   27.2580(2)
_cell_length_c                   13.59102(12)
_cell_angle_alpha                90
_cell_angle_beta                 99.3958(8)
_cell_angle_gamma                90
_cell_volume                     3481.90(5)
_cell_formula_units_Z            8
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    18335
_cell_measurement_theta_min      4.6230
_cell_measurement_theta_max      73.1180

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_F_000             1392
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.394
_exptl_crystal_size_mid          0.246
_exptl_crystal_size_min          0.134
_exptl_absorpt_coefficient_mu    4.236
_shelx_estimated_absorpt_T_min   0.286
_shelx_estimated_absorpt_T_max   0.601
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 1 -2 0.1669
1 -11 -7 0.1231
-3 -11 -4 0.1318
-2 11 7 0.1060
1 12 6 0.1196
5 2 -5 0.1430
-5 -2 -3 0.1937
-3 -2 8 0.0843
0 0 9 0.0636
5 2 5 0.1575
-1 17 0 0.1116
0 -18 1 0.1251
-3 -15 1 0.1420
0 -4 -9 0.0742
0 4 -9 0.0619
4 5 -7 0.1178
0 13 -6 0.0743
3 12 -5 0.1321
1 17 1 0.1134
1 -13 6 0.1130
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
6.1324 1.3518 -2.3546 0.0258 0.1119 0.9934
1.3490 -11.1517 -6.7948 0.2306 0.9637 0.1344
-3.4804 -10.6830 -4.0999 0.1802 0.7498 -0.6366
-1.5896 10.9713 6.8173 -0.2291 -0.9577 -0.1743
1.2585 11.9061 5.8920 -0.2232 -0.9309 0.2893
5.3502 2.4465 -5.4467 -0.2229 0.4082 0.8853
-5.4383 -2.3332 -2.7171 -0.2263 0.4181 -0.8798
-3.1752 -1.5438 8.1709 0.4033 -0.7406 -0.5374
0.0148 -0.1554 8.6996 0.4776 -0.8784 -0.0187
4.6453 1.9508 4.5833 0.3175 -0.5854 0.7460
-1.4823 17.0934 -0.4734 -0.9201 -0.3817 -0.0881
0.0429 -17.6050 0.8414 0.9136 0.3793 -0.1464
-3.0092 -15.3798 1.4615 0.7284 0.3029 -0.6146
-0.0211 -3.5714 -8.5181 -0.2846 0.9585 -0.0147
0.0835 3.9059 -8.5083 -0.6484 0.7584 0.0662
3.7392 4.5761 -7.4304 -0.4924 0.5770 0.6516
-0.4365 13.1934 -5.6669 -0.9709 0.2325 0.0567
3.1885 11.8938 -5.3709 -0.7613 0.1830 0.6221
1.1125 17.0429 1.4646 -0.7202 -0.6154 0.3202
0.9347 -12.9920 5.5441 0.9722 -0.2328 0.0246
_exptl_absorpt_correction_T_min  0.402
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.112a (Rigaku Oxford Diffraction, 2021)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.721
_oxdiff_exptl_absorpt_empirical_full_max 1.495
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_diffrn_ambient_temperature      150.01(10)
_diffrn_ambient_environment      N~2~
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_monochromator  mirror
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            EosS2
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            33405
_diffrn_reflns_av_unetI/netI     0.0199
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.674
_diffrn_reflns_theta_max         73.271
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             6946
_reflns_number_gt                6598
_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       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_structure_solution    
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_computing_structure_refinement  
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. Hübschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_molecular_graphics    
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'

_computing_publication_material  
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_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)+(0.0431P)²+1.0781P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     dual
_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         6946
_refine_ls_number_parameters     377
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0301
_refine_ls_R_factor_gt           0.0285
_refine_ls_wR_factor_ref         0.0776
_refine_ls_wR_factor_gt          0.0763
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_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 0.83277(2) 0.44187(2) 0.31369(2) 0.01900(7) Uani 1 1 d . . . . .
O1 O 1.01660(10) 0.45998(4) 0.30242(7) 0.0263(2) Uani 1 1 d . . . . .
O2 O 0.72700(10) 0.48140(3) 0.38087(7) 0.0251(2) Uani 1 1 d . . . . .
O3 O 0.73943(10) 0.41667(3) 0.19244(7) 0.0245(2) Uani 1 1 d . . . . .
N1 N 0.79701(12) 0.51312(4) 0.21328(8) 0.0230(2) Uani 1 1 d . . . . .
N2 N 0.86192(12) 0.38743(4) 0.40101(8) 0.0246(2) Uani 1 1 d . . . . .
C1 C 1.05675(15) 0.49299(5) 0.23137(11) 0.0282(3) Uani 1 1 d . . . . .
C2 C 1.19784(17) 0.51667(7) 0.27626(14) 0.0419(4) Uani 1 1 d . . . . .
H2A H 1.187286 0.533302 0.338554 0.063 Uiso 1 1 calc R U . . .
H2B H 1.225475 0.540596 0.229111 0.063 Uiso 1 1 calc R U . . .
H2C H 1.271377 0.491315 0.289937 0.063 Uiso 1 1 calc R U . . .
C1N C 0.80312(17) 0.37861(6) 0.49137(11) 0.0354(3) Uani 1 1 d . . . . .
H1N1 H 0.750944 0.347480 0.485332 0.053 Uiso 1 1 calc R U . . .
H1N2 H 0.738222 0.405374 0.501350 0.053 Uiso 1 1 calc R U . . .
H1N3 H 0.880475 0.377008 0.548464 0.053 Uiso 1 1 calc R U . . .
C3 C 1.07612(17) 0.46385(6) 0.13847(12) 0.0366(3) Uani 1 1 d . . . . .
H3A H 1.154834 0.440600 0.155376 0.055 Uiso 1 1 calc R U . . .
H3B H 1.097521 0.486421 0.086778 0.055 Uiso 1 1 calc R U . . .
H3C H 0.988439 0.445840 0.113672 0.055 Uiso 1 1 calc R U . . .
C2N C 0.95293(19) 0.34799(6) 0.37849(12) 0.0370(4) Uani 1 1 d . . . . .
H2N1 H 1.032977 0.344373 0.433275 0.056 Uiso 1 1 calc R U . . .
H2N2 H 0.989094 0.355501 0.316692 0.056 Uiso 1 1 calc R U . . .
H2N3 H 0.898433 0.317358 0.370209 0.056 Uiso 1 1 calc R U . . .
C4 C 0.94090(15) 0.53322(5) 0.21159(11) 0.0281(3) Uani 1 1 d . . . . .
H4A H 0.961419 0.559136 0.262962 0.034 Uiso 1 1 calc R U . . .
H4B H 0.943630 0.548404 0.145751 0.034 Uiso 1 1 calc R U . . .
C3N C 0.52864(18) 0.31807(6) 0.29808(12) 0.0358(3) Uani 1 1 d . . . . .
H3N1 H 0.460825 0.317242 0.235567 0.054 Uiso 1 1 calc R U . . .
H3N2 H 0.582452 0.287290 0.305892 0.054 Uiso 1 1 calc R U . . .
H3N3 H 0.594386 0.345616 0.296628 0.054 Uiso 1 1 calc R U . . .
C5 C 0.71444(15) 0.53355(5) 0.37410(10) 0.0253(3) Uani 1 1 d . . . . .
C4N C 0.3677(2) 0.36842(6) 0.37134(13) 0.0425(4) Uani 1 1 d . . . . .
H4N1 H 0.430344 0.396980 0.372124 0.064 Uiso 1 1 calc R U . . .
H4N2 H 0.314420 0.370670 0.427078 0.064 Uiso 1 1 calc R U . . .
H4N3 H 0.300959 0.367662 0.308312 0.064 Uiso 1 1 calc R U . . .
C6 C 0.84217(16) 0.55632(6) 0.44092(12) 0.0326(3) Uani 1 1 d . . . . .
H6A H 0.838236 0.548364 0.510736 0.049 Uiso 1 1 calc R U . . .
H6B H 0.840074 0.592014 0.432210 0.049 Uiso 1 1 calc R U . . .
H6C H 0.930205 0.543193 0.422709 0.049 Uiso 1 1 calc R U . . .
C7 C 0.57680(16) 0.54883(6) 0.40863(12) 0.0331(3) Uani 1 1 d . . . . .
H7A H 0.496461 0.531895 0.368480 0.050 Uiso 1 1 calc R U . . .
H7B H 0.564142 0.584373 0.400658 0.050 Uiso 1 1 calc R U . . .
H7C H 0.581128 0.540083 0.479000 0.050 Uiso 1 1 calc R U . . .
C8 C 0.70585(15) 0.54620(5) 0.26252(10) 0.0260(3) Uani 1 1 d . . . . .
H8A H 0.605962 0.543319 0.228696 0.031 Uiso 1 1 calc R U . . .
H8B H 0.736517 0.580581 0.255931 0.031 Uiso 1 1 calc R U . . .
C9 C 0.65020(14) 0.44596(5) 0.12158(10) 0.0237(3) Uani 1 1 d . . . . .
C10 C 0.63380(17) 0.42051(6) 0.02026(11) 0.0331(3) Uani 1 1 d . . . . .
H10A H 0.728075 0.414086 0.003066 0.050 Uiso 1 1 calc R U . . .
H10B H 0.579752 0.441687 -0.030625 0.050 Uiso 1 1 calc R U . . .
H10C H 0.583043 0.389415 0.023314 0.050 Uiso 1 1 calc R U . . .
C11 C 0.50425(15) 0.45089(6) 0.15394(11) 0.0300(3) Uani 1 1 d . . . . .
H11A H 0.459630 0.418488 0.153645 0.045 Uiso 1 1 calc R U . . .
H11B H 0.443877 0.472614 0.107550 0.045 Uiso 1 1 calc R U . . .
H11C H 0.515824 0.464735 0.221327 0.045 Uiso 1 1 calc R U . . .
C12 C 0.72610(15) 0.49567(5) 0.11436(10) 0.0254(3) Uani 1 1 d . . . . .
H12A H 0.797861 0.492094 0.069730 0.030 Uiso 1 1 calc R U . . .
H12B H 0.655602 0.520405 0.084679 0.030 Uiso 1 1 calc R U . . .
Ti2 Ti 0.45770(2) 0.28315(2) 0.49465(2) 0.02049(7) Uani 1 1 d . . . . .
N3 N 0.46325(12) 0.22882(4) 0.63083(8) 0.0233(2) Uani 1 1 d . . . . .
N4 N 0.45223(12) 0.32408(4) 0.38095(8) 0.0246(2) Uani 1 1 d . . . . .
O21 O 0.26646(10) 0.27236(4) 0.49560(7) 0.0274(2) Uani 1 1 d . . . . .
O22 O 0.53744(11) 0.32126(3) 0.60201(7) 0.0266(2) Uani 1 1 d . . . . .
O23 O 0.56757(11) 0.23212(4) 0.46270(8) 0.0298(2) Uani 1 1 d . . . . .
C21 C 0.20921(14) 0.25327(5) 0.57845(10) 0.0253(3) Uani 1 1 d . . . . .
C22 C 0.06697(15) 0.22909(6) 0.53926(11) 0.0311(3) Uani 1 1 d . . . . .
H22A H -0.000544 0.254004 0.508667 0.047 Uiso 1 1 calc R U . . .
H22B H 0.029756 0.213393 0.594548 0.047 Uiso 1 1 calc R U . . .
H22C H 0.080144 0.204306 0.489326 0.047 Uiso 1 1 calc R U . . .
C23 C 0.18573(16) 0.29568(6) 0.64800(11) 0.0321(3) Uani 1 1 d . . . . .
H23A H 0.274026 0.314501 0.664901 0.048 Uiso 1 1 calc R U . . .
H23B H 0.157932 0.282518 0.709103 0.048 Uiso 1 1 calc R U . . .
H23C H 0.110221 0.317141 0.614455 0.048 Uiso 1 1 calc R U . . .
C24 C 0.31308(15) 0.21356(5) 0.62754(11) 0.0260(3) Uani 1 1 d . . . . .
H24A H 0.295360 0.207357 0.696230 0.031 Uiso 1 1 calc R U . . .
H24B H 0.295822 0.182604 0.589394 0.031 Uiso 1 1 calc R U . . .
C25 C 0.60413(15) 0.30285(5) 0.69620(10) 0.0269(3) Uani 1 1 d . . . . .
C26 C 0.75929(16) 0.29055(6) 0.69169(12) 0.0341(3) Uani 1 1 d . . . . .
H26A H 0.763773 0.267837 0.636393 0.051 Uiso 1 1 calc R U . . .
H26B H 0.802796 0.275203 0.754518 0.051 Uiso 1 1 calc R U . . .
H26C H 0.810889 0.320711 0.681258 0.051 Uiso 1 1 calc R U . . .
C27 C 0.59637(18) 0.34247(6) 0.77436(11) 0.0346(3) Uani 1 1 d . . . . .
H27A H 0.650181 0.371333 0.758986 0.052 Uiso 1 1 calc R U . . .
H27B H 0.637134 0.329894 0.840415 0.052 Uiso 1 1 calc R U . . .
H27C H 0.496801 0.351646 0.773920 0.052 Uiso 1 1 calc R U . . .
C28 C 0.51877(15) 0.25746(5) 0.72158(10) 0.0267(3) Uani 1 1 d . . . . .
H28A H 0.581040 0.236268 0.769264 0.032 Uiso 1 1 calc R U . . .
H28B H 0.438321 0.268378 0.753989 0.032 Uiso 1 1 calc R U . . .
C29 C 0.57372(15) 0.18360(5) 0.50170(11) 0.0274(3) Uani 1 1 d . . . . .
C30 C 0.71829(17) 0.16133(6) 0.49351(14) 0.0396(4) Uani 1 1 d . . . . .
H30A H 0.729614 0.159716 0.423202 0.059 Uiso 1 1 calc R U . . .
H30B H 0.724262 0.128189 0.521852 0.059 Uiso 1 1 calc R U . . .
H30C H 0.793847 0.181772 0.530227 0.059 Uiso 1 1 calc R U . . .
C31 C 0.45718(16) 0.15318(6) 0.44021(12) 0.0330(3) Uani 1 1 d . . . . .
H31A H 0.364826 0.168951 0.440572 0.049 Uiso 1 1 calc R U . . .
H31B H 0.456261 0.120240 0.469000 0.049 Uiso 1 1 calc R U . . .
H31C H 0.475417 0.150754 0.371471 0.049 Uiso 1 1 calc R U . . .
C32 C 0.55783(15) 0.18762(5) 0.61316(11) 0.0279(3) Uani 1 1 d . . . . .
H32A H 0.518381 0.156544 0.634650 0.034 Uiso 1 1 calc R U . . .
H32B H 0.652817 0.192577 0.653904 0.034 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
Ti1 O2 1.8195(10) . ?
Ti1 O1 1.8498(9) . ?
Ti1 O3 1.8707(9) . ?
Ti1 N2 1.8921(11) . ?
Ti1 N1 2.3662(11) . ?
O1 C1 1.4175(17) . ?
O2 C5 1.4281(16) . ?
O3 C9 1.4214(15) . ?
N1 C4 1.4799(17) . ?
N1 C12 1.4811(17) . ?
N1 C8 1.4848(17) . ?
N2 C2N 1.4448(19) . ?
N2 C1N 1.4506(18) . ?
C1 C2 1.526(2) . ?
C1 C3 1.528(2) . ?
C1 C4 1.548(2) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C1N H1N1 0.9800 . ?
C1N H1N2 0.9800 . ?
C1N H1N3 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C2N H2N1 0.9800 . ?
C2N H2N2 0.9800 . ?
C2N H2N3 0.9800 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C3N N4 1.4467(17) . ?
C3N H3N1 0.9800 . ?
C3N H3N2 0.9800 . ?
C3N H3N3 0.9800 . ?
C5 C7 1.5212(19) . ?
C5 C6 1.5263(19) . ?
C5 C8 1.5444(19) . ?
C4N N4 1.447(2) . ?
C4N H4N1 0.9800 . ?
C4N H4N2 0.9800 . ?
C4N H4N3 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 C10 1.5270(19) . ?
C9 C11 1.5312(19) . ?
C9 C12 1.5463(19) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
Ti2 O23 1.8350(10) . ?
Ti2 O21 1.8476(10) . ?
Ti2 O22 1.8503(10) . ?
Ti2 N4 1.8999(11) . ?
Ti2 N3 2.3642(11) . ?
N3 C28 1.4826(17) . ?
N3 C24 1.4835(17) . ?
N3 C32 1.4835(18) . ?
O21 C21 1.4271(16) . ?
O22 C25 1.4242(16) . ?
O23 C29 1.4224(17) . ?
C21 C22 1.5228(19) . ?
C21 C23 1.533(2) . ?
C21 C24 1.5428(19) . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C23 H23A 0.9800 . ?
C23 H23B 0.9800 . ?
C23 H23C 0.9800 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C25 C27 1.525(2) . ?
C25 C26 1.527(2) . ?
C25 C28 1.5500(19) . ?
C26 H26A 0.9800 . ?
C26 H26B 0.9800 . ?
C26 H26C 0.9800 . ?
C27 H27A 0.9800 . ?
C27 H27B 0.9800 . ?
C27 H27C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C29 C31 1.522(2) . ?
C29 C30 1.526(2) . ?
C29 C32 1.551(2) . ?
C30 H30A 0.9800 . ?
C30 H30B 0.9800 . ?
C30 H30C 0.9800 . ?
C31 H31A 0.9800 . ?
C31 H31B 0.9800 . ?
C31 H31C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 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
O2 Ti1 O1 119.53(4) . . ?
O2 Ti1 O3 115.91(4) . . ?
O1 Ti1 O3 110.20(4) . . ?
O2 Ti1 N2 100.74(5) . . ?
O1 Ti1 N2 102.54(5) . . ?
O3 Ti1 N2 105.34(5) . . ?
O2 Ti1 N1 76.34(4) . . ?
O1 Ti1 N1 77.43(4) . . ?
O3 Ti1 N1 77.90(4) . . ?
N2 Ti1 N1 176.45(5) . . ?
C1 O1 Ti1 126.17(8) . . ?
C5 O2 Ti1 127.20(8) . . ?
C9 O3 Ti1 122.43(8) . . ?
C4 N1 C12 113.02(11) . . ?
C4 N1 C8 113.18(11) . . ?
C12 N1 C8 112.99(11) . . ?
C4 N1 Ti1 105.45(8) . . ?
C12 N1 Ti1 105.14(8) . . ?
C8 N1 Ti1 106.16(8) . . ?
C2N N2 C1N 112.59(12) . . ?
C2N N2 Ti1 118.83(9) . . ?
C1N N2 Ti1 128.58(10) . . ?
O1 C1 C2 108.32(12) . . ?
O1 C1 C3 108.39(12) . . ?
C2 C1 C3 109.45(13) . . ?
O1 C1 C4 107.70(11) . . ?
C2 C1 C4 109.04(13) . . ?
C3 C1 C4 113.80(13) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
H2A C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N2 C1N H1N1 109.5 . . ?
N2 C1N H1N2 109.5 . . ?
H1N1 C1N H1N2 109.5 . . ?
N2 C1N H1N3 109.5 . . ?
H1N1 C1N H1N3 109.5 . . ?
H1N2 C1N H1N3 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N2 C2N H2N1 109.5 . . ?
N2 C2N H2N2 109.5 . . ?
H2N1 C2N H2N2 109.5 . . ?
N2 C2N H2N3 109.5 . . ?
H2N1 C2N H2N3 109.5 . . ?
H2N2 C2N H2N3 109.5 . . ?
N1 C4 C1 111.77(11) . . ?
N1 C4 H4A 109.3 . . ?
C1 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C1 C4 H4B 109.3 . . ?
H4A C4 H4B 107.9 . . ?
N4 C3N H3N1 109.5 . . ?
N4 C3N H3N2 109.5 . . ?
H3N1 C3N H3N2 109.5 . . ?
N4 C3N H3N3 109.5 . . ?
H3N1 C3N H3N3 109.5 . . ?
H3N2 C3N H3N3 109.5 . . ?
O2 C5 C7 108.67(11) . . ?
O2 C5 C6 108.43(11) . . ?
C7 C5 C6 110.41(12) . . ?
O2 C5 C8 106.02(11) . . ?
C7 C5 C8 109.37(12) . . ?
C6 C5 C8 113.75(12) . . ?
N4 C4N H4N1 109.5 . . ?
N4 C4N H4N2 109.5 . . ?
H4N1 C4N H4N2 109.5 . . ?
N4 C4N H4N3 109.5 . . ?
H4N1 C4N H4N3 109.5 . . ?
H4N2 C4N H4N3 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N1 C8 C5 111.46(11) . . ?
N1 C8 H8A 109.3 . . ?
C5 C8 H8A 109.3 . . ?
N1 C8 H8B 109.3 . . ?
C5 C8 H8B 109.3 . . ?
H8A C8 H8B 108.0 . . ?
O3 C9 C10 108.52(11) . . ?
O3 C9 C11 108.99(11) . . ?
C10 C9 C11 109.56(12) . . ?
O3 C9 C12 107.52(10) . . ?
C10 C9 C12 108.72(12) . . ?
C11 C9 C12 113.41(11) . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C12 C9 111.87(10) . . ?
N1 C12 H12A 109.2 . . ?
C9 C12 H12A 109.2 . . ?
N1 C12 H12B 109.2 . . ?
C9 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
O23 Ti2 O21 118.83(5) . . ?
O23 Ti2 O22 115.83(5) . . ?
O21 Ti2 O22 111.23(5) . . ?
O23 Ti2 N4 101.17(5) . . ?
O21 Ti2 N4 101.71(5) . . ?
O22 Ti2 N4 105.36(5) . . ?
O23 Ti2 N3 76.69(4) . . ?
O21 Ti2 N3 77.93(4) . . ?
O22 Ti2 N3 77.32(4) . . ?
N4 Ti2 N3 177.17(5) . . ?
C28 N3 C24 112.58(11) . . ?
C28 N3 C32 112.94(11) . . ?
C24 N3 C32 113.03(11) . . ?
C28 N3 Ti2 106.30(8) . . ?
C24 N3 Ti2 104.70(8) . . ?
C32 N3 Ti2 106.49(8) . . ?
C4N N4 C3N 111.58(12) . . ?
C4N N4 Ti2 120.34(9) . . ?
C3N N4 Ti2 128.05(10) . . ?
C21 O21 Ti2 124.60(8) . . ?
C25 O22 Ti2 125.20(8) . . ?
C29 O23 Ti2 127.37(8) . . ?
O21 C21 C22 108.34(11) . . ?
O21 C21 C23 108.94(11) . . ?
C22 C21 C23 109.33(12) . . ?
O21 C21 C24 107.23(11) . . ?
C22 C21 C24 108.60(11) . . ?
C23 C21 C24 114.23(12) . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
N3 C24 C21 111.33(11) . . ?
N3 C24 H24A 109.4 . . ?
C21 C24 H24A 109.4 . . ?
N3 C24 H24B 109.4 . . ?
C21 C24 H24B 109.4 . . ?
H24A C24 H24B 108.0 . . ?
O22 C25 C27 108.15(12) . . ?
O22 C25 C26 109.51(11) . . ?
C27 C25 C26 109.93(12) . . ?
O22 C25 C28 107.94(11) . . ?
C27 C25 C28 108.86(12) . . ?
C26 C25 C28 112.34(12) . . ?
C25 C26 H26A 109.5 . . ?
C25 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C25 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 109.5 . . ?
C25 C27 H27A 109.5 . . ?
C25 C27 H27B 109.5 . . ?
H27A C27 H27B 109.5 . . ?
C25 C27 H27C 109.5 . . ?
H27A C27 H27C 109.5 . . ?
H27B C27 H27C 109.5 . . ?
N3 C28 C25 111.35(11) . . ?
N3 C28 H28A 109.4 . . ?
C25 C28 H28A 109.4 . . ?
N3 C28 H28B 109.4 . . ?
C25 C28 H28B 109.4 . . ?
H28A C28 H28B 108.0 . . ?
O23 C29 C31 108.67(12) . . ?
O23 C29 C30 109.00(12) . . ?
C31 C29 C30 109.23(13) . . ?
O23 C29 C32 107.08(11) . . ?
C31 C29 C32 113.34(12) . . ?
C30 C29 C32 109.43(12) . . ?
C29 C30 H30A 109.5 . . ?
C29 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C29 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C29 C31 H31A 109.5 . . ?
C29 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C29 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
N3 C32 C29 111.74(11) . . ?
N3 C32 H32A 109.3 . . ?
C29 C32 H32A 109.3 . . ?
N3 C32 H32B 109.3 . . ?
C29 C32 H32B 109.3 . . ?
H32A C32 H32B 107.9 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ti1 O1 C1 -82.49(11) . . . . ?
O3 Ti1 O1 C1 55.55(12) . . . . ?
N2 Ti1 O1 C1 167.30(11) . . . . ?
N1 Ti1 O1 C1 -16.34(11) . . . . ?
O1 Ti1 O2 C5 44.02(12) . . . . ?
O3 Ti1 O2 C5 -91.73(11) . . . . ?
N2 Ti1 O2 C5 155.21(10) . . . . ?
N1 Ti1 O2 C5 -22.71(10) . . . . ?
O2 Ti1 O3 C9 44.01(11) . . . . ?
O1 Ti1 O3 C9 -95.68(10) . . . . ?
N2 Ti1 O3 C9 154.39(10) . . . . ?
N1 Ti1 O3 C9 -24.11(9) . . . . ?
O2 Ti1 N2 C2N -175.25(11) . . . . ?
O1 Ti1 N2 C2N -51.46(12) . . . . ?
O3 Ti1 N2 C2N 63.87(11) . . . . ?
O2 Ti1 N2 C1N 5.24(13) . . . . ?
O1 Ti1 N2 C1N 129.03(12) . . . . ?
O3 Ti1 N2 C1N -115.64(12) . . . . ?
Ti1 O1 C1 C2 152.29(10) . . . . ?
Ti1 O1 C1 C3 -89.04(13) . . . . ?
Ti1 O1 C1 C4 34.50(15) . . . . ?
C12 N1 C4 C1 -89.43(14) . . . . ?
C8 N1 C4 C1 140.51(12) . . . . ?
Ti1 N1 C4 C1 24.89(13) . . . . ?
O1 C1 C4 N1 -36.40(15) . . . . ?
C2 C1 C4 N1 -153.73(12) . . . . ?
C3 C1 C4 N1 83.78(15) . . . . ?
Ti1 O2 C5 C7 157.93(9) . . . . ?
Ti1 O2 C5 C6 -82.03(13) . . . . ?
Ti1 O2 C5 C8 40.47(14) . . . . ?
C4 N1 C8 C5 -93.57(13) . . . . ?
C12 N1 C8 C5 136.35(11) . . . . ?
Ti1 N1 C8 C5 21.63(12) . . . . ?
O2 C5 C8 N1 -35.82(14) . . . . ?
C7 C5 C8 N1 -152.82(12) . . . . ?
C6 C5 C8 N1 83.23(14) . . . . ?
Ti1 O3 C9 C10 160.59(9) . . . . ?
Ti1 O3 C9 C11 -80.16(12) . . . . ?
Ti1 O3 C9 C12 43.16(13) . . . . ?
C4 N1 C12 C9 136.89(12) . . . . ?
C8 N1 C12 C9 -92.95(13) . . . . ?
Ti1 N1 C12 C9 22.39(12) . . . . ?
O3 C9 C12 N1 -39.75(14) . . . . ?
C10 C9 C12 N1 -157.05(11) . . . . ?
C11 C9 C12 N1 80.81(14) . . . . ?
O23 Ti2 N4 C4N 176.25(12) . . . . ?
O21 Ti2 N4 C4N 53.37(13) . . . . ?
O22 Ti2 N4 C4N -62.77(13) . . . . ?
O23 Ti2 N4 C3N -6.03(13) . . . . ?
O21 Ti2 N4 C3N -128.91(12) . . . . ?
O22 Ti2 N4 C3N 114.95(12) . . . . ?
O23 Ti2 O21 C21 85.45(11) . . . . ?
O22 Ti2 O21 C21 -52.92(11) . . . . ?
N4 Ti2 O21 C21 -164.68(10) . . . . ?
N3 Ti2 O21 C21 18.18(10) . . . . ?
O23 Ti2 O22 C25 -47.87(11) . . . . ?
O21 Ti2 O22 C25 91.85(11) . . . . ?
N4 Ti2 O22 C25 -158.73(10) . . . . ?
N3 Ti2 O22 C25 20.35(10) . . . . ?
O21 Ti2 O23 C29 -48.36(13) . . . . ?
O22 Ti2 O23 C29 88.17(12) . . . . ?
N4 Ti2 O23 C29 -158.54(11) . . . . ?
N3 Ti2 O23 C29 19.58(11) . . . . ?
Ti2 O21 C21 C22 -155.32(10) . . . . ?
Ti2 O21 C21 C23 85.83(13) . . . . ?
Ti2 O21 C21 C24 -38.28(15) . . . . ?
C28 N3 C24 C21 87.81(13) . . . . ?
C32 N3 C24 C21 -142.74(12) . . . . ?
Ti2 N3 C24 C21 -27.24(12) . . . . ?
O21 C21 C24 N3 40.45(15) . . . . ?
C22 C21 C24 N3 157.32(11) . . . . ?
C23 C21 C24 N3 -80.37(14) . . . . ?
Ti2 O22 C25 C27 -155.58(10) . . . . ?
Ti2 O22 C25 C26 84.63(13) . . . . ?
Ti2 O22 C25 C28 -37.95(15) . . . . ?
C24 N3 C28 C25 -135.71(12) . . . . ?
C32 N3 C28 C25 94.79(13) . . . . ?
Ti2 N3 C28 C25 -21.63(13) . . . . ?
O22 C25 C28 N3 35.58(15) . . . . ?
C27 C25 C28 N3 152.75(12) . . . . ?
C26 C25 C28 N3 -85.25(14) . . . . ?
Ti2 O23 C29 C31 86.62(14) . . . . ?
Ti2 O23 C29 C30 -154.43(10) . . . . ?
Ti2 O23 C29 C32 -36.15(15) . . . . ?
C28 N3 C32 C29 -137.16(12) . . . . ?
C24 N3 C32 C29 93.58(13) . . . . ?
Ti2 N3 C32 C29 -20.85(13) . . . . ?
O23 C29 C32 N3 33.40(15) . . . . ?
C31 C29 C32 N3 -86.42(14) . . . . ?
C30 C29 C32 N3 151.40(12) . . . . ?

_refine_diff_density_max         0.322
_refine_diff_density_min         -0.292
_refine_diff_density_rms         0.044


_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: Toluene'
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
