# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_sad
_database_code_depnum_ccdc_archive 'CCDC 783224'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;State Key Laboratory of Physical Chemistry of Solid Surfaces
China
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;
_audit_creation_date             2019-10-16
_audit_creation_method           
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C11 H15 N2 O10 Ti, H4 N, H2 O'
_chemical_formula_sum            'C11 H21 N3 O11 Ti'
_chemical_formula_weight         419.21
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.6948(3)
_cell_length_b                   7.5422(4)
_cell_length_c                   16.7297(8)
_cell_angle_alpha                83.398(4)
_cell_angle_beta                 85.937(4)
_cell_angle_gamma                77.802(4)
_cell_volume                     819.25(7)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1953
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      2.78
_shelx_estimated_absorpt_T_max   0.943
_shelx_estimated_absorpt_T_min   0.798
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_T_max  0.9434
_exptl_absorpt_correction_T_min  0.7983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             436
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_av_unetI/netI     0.1485
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            10186
_diffrn_reflns_point_group_measured_fraction_full 0.966
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.627
_diffrn_reflns_theta_min         2.778
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Oxford Gemini Diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2819
_reflns_number_total             5294
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  ShelXL
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.357
_refine_diff_density_rms         0.061
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.787
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         5294
_refine_ls_number_restraints     34
_refine_ls_R_factor_all          0.0816
_refine_ls_R_factor_gt           0.0348
_refine_ls_restrained_S_all      0.792
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0231P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0599
_refine_ls_wR_factor_ref         0.0651
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H3A = N3-H3B = N3-H3C = N3-H3D = O1W-H1WA = O1W-H1WB
 0.85 with sigma of 0.01
 H3A-H3B = H3A-H3C = H3A-H3D = H3B-H3C = H3B-H3D = H3C-H3D = H1WA-H1WB
 1.39 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C3 \\sim O4: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C3) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C3, O4
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 C9(H9)
5.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B), C10(H10A,H10B)
5.c Me refined with riding coordinates:
 C11(H11A,H11B,H11C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.75971(4) 0.35797(4) 0.21723(2) 0.01577(8) Uani 1 1 d . . . . .
C1 C 0.7707(2) 0.0962(2) 0.09881(10) 0.0176(3) Uani 1 1 d . . . . .
C2 C 0.9552(2) 0.0047(2) 0.14647(10) 0.0178(3) Uani 1 1 d . . . . .
H2A H 0.915208 -0.079998 0.191482 0.021 Uiso 1 1 calc R . . . .
H2B H 1.060585 -0.065877 0.111392 0.021 Uiso 1 1 calc R . . . .
C3 C 1.0835(2) 0.4462(2) 0.10337(10) 0.0170(3) Uani 1 1 d . U . . .
C4 C 1.1513(2) 0.2418(2) 0.11220(10) 0.0187(4) Uani 1 1 d . . . . .
H4A H 1.133274 0.195341 0.060738 0.022 Uiso 1 1 calc R . . . .
H4B H 1.298924 0.209831 0.122686 0.022 Uiso 1 1 calc R . . . .
C5 C 0.7532(2) 0.1375(2) 0.36807(11) 0.0222(4) Uani 1 1 d . . . . .
C6 C 0.8838(2) 0.2657(2) 0.38955(10) 0.0222(4) Uani 1 1 d . . . . .
H6A H 0.797507 0.362541 0.419347 0.027 Uiso 1 1 calc R . . . .
H6B H 0.991952 0.197043 0.425220 0.027 Uiso 1 1 calc R . . . .
C7 C 1.1593(3) 0.5488(2) 0.38718(11) 0.0225(4) Uani 1 1 d . . . . .
C8 C 1.0040(2) 0.5377(2) 0.32708(11) 0.0212(4) Uani 1 1 d . . . . .
H8A H 0.869315 0.608809 0.344547 0.025 Uiso 1 1 calc R . . . .
H8B H 1.044091 0.596660 0.274154 0.025 Uiso 1 1 calc R . . . .
C9 C 1.1595(2) 0.0756(2) 0.25085(10) 0.0173(3) Uani 1 1 d . . . . .
H9 H 1.076445 0.002683 0.288020 0.021 Uiso 1 1 calc R . . . .
C10 C 1.1837(2) 0.2350(2) 0.29337(10) 0.0187(4) Uani 1 1 d . . . . .
H10A H 1.260545 0.189125 0.342529 0.022 Uiso 1 1 calc R . . . .
H10B H 1.264084 0.310928 0.257691 0.022 Uiso 1 1 calc R . . . .
C11 C 1.3638(2) -0.0500(2) 0.23257(11) 0.0225(4) Uani 1 1 d . . . . .
H11A H 1.434655 -0.092266 0.282695 0.034 Uiso 1 1 calc R . . . .
H11B H 1.340032 -0.155200 0.208061 0.034 Uiso 1 1 calc R . . . .
H11C H 1.448261 0.016612 0.195211 0.034 Uiso 1 1 calc R . . . .
N1 N 1.03733(18) 0.14881(17) 0.17815(8) 0.0154(3) Uani 1 1 d . . . . .
N2 N 0.98006(18) 0.35060(17) 0.31630(8) 0.0169(3) Uani 1 1 d . . . . .
N3 N 0.5582(2) 0.69374(19) 0.04960(9) 0.0214(3) Uani 1 1 d D . . . .
O1 O 0.67508(15) 0.25157(15) 0.11920(7) 0.0190(3) Uani 1 1 d . . . . .
O2 O 0.71679(16) 0.02107(15) 0.04438(7) 0.0239(3) Uani 1 1 d . . . . .
O3 O 0.92408(15) 0.51250(14) 0.14725(7) 0.0180(3) Uani 1 1 d . . . . .
O4 O 1.17684(16) 0.53883(15) 0.05563(7) 0.0229(3) Uani 1 1 d . U . . .
O5 O 0.70485(15) 0.15617(15) 0.29283(7) 0.0196(3) Uani 1 1 d . . . . .
O6 O 0.6977(2) 0.02978(19) 0.41943(8) 0.0414(4) Uani 1 1 d . . . . .
O8 O 1.2431(2) 0.42137(18) 0.43116(9) 0.0416(4) Uani 1 1 d . . . . .
O7 O 1.18896(18) 0.71508(16) 0.38404(8) 0.0287(3) Uani 1 1 d . . . . .
O9 O 0.61124(16) 0.55070(15) 0.26879(7) 0.0228(3) Uani 1 1 d . . . . .
O10 O 0.49957(15) 0.50316(15) 0.20478(7) 0.0205(3) Uani 1 1 d . . . . .
O1W O 0.5312(2) 0.72627(18) 0.43869(8) 0.0349(3) Uani 1 1 d D . . . .
H7 H 1.284(3) 0.726(3) 0.4032(14) 0.042 Uiso 1 1 d R . . . .
H3A H 0.518(2) 0.642(2) 0.0932(7) 0.042 Uiso 1 1 d DR . . . .
H3B H 0.634(2) 0.6176(17) 0.0205(9) 0.042 Uiso 1 1 d DR . . . .
H3C H 0.4577(18) 0.7568(19) 0.0232(9) 0.042 Uiso 1 1 d DR . . . .
H3D H 0.633(2) 0.7697(18) 0.0595(10) 0.042 Uiso 1 1 d DR . . . .
H1WA H 0.574(3) 0.673(2) 0.4828(8) 0.042 Uiso 1 1 d DR . . . .
H1WB H 0.550(3) 0.8328(15) 0.4301(12) 0.042 Uiso 1 1 d DR . . . .


_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 N1 2.2796(13) . ?
Ti1 N2 2.2841(13) . ?
Ti1 O1 2.0690(12) . ?
Ti1 O3 1.9964(10) . ?
Ti1 O5 1.9439(11) . ?
Ti1 O9 1.8442(12) . ?
Ti1 O10 1.8624(10) . ?
C1 C2 1.513(2) . ?
C1 O1 1.2821(19) . ?
C1 O2 1.2376(19) . ?
C2 N1 1.480(2) . ?
C3 C4 1.505(2) . ?
C3 O3 1.2947(18) . ?
C3 O4 1.2256(17) . ?
C4 N1 1.4898(19) . ?
C5 C6 1.520(2) . ?
C5 O5 1.306(2) . ?
C5 O6 1.2074(19) . ?
C6 N2 1.486(2) . ?
C7 C8 1.517(2) . ?
C7 O8 1.203(2) . ?
C7 O7 1.305(2) . ?
C8 N2 1.486(2) . ?
C9 C10 1.507(2) . ?
C9 C11 1.524(2) . ?
C9 N1 1.4997(19) . ?
C10 N2 1.505(2) . ?
O9 O10 1.4660(15) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ti1 N2 77.96(5) . . ?
O1 Ti1 N1 73.66(4) . . ?
O1 Ti1 N2 151.00(5) . . ?
O3 Ti1 N1 77.53(4) . . ?
O3 Ti1 N2 87.42(4) . . ?
O3 Ti1 O1 92.19(4) . . ?
O5 Ti1 N1 83.72(5) . . ?
O5 Ti1 N2 77.51(5) . . ?
O5 Ti1 O1 93.39(5) . . ?
O5 Ti1 O3 158.06(4) . . ?
O9 Ti1 N1 158.38(5) . . ?
O9 Ti1 N2 81.92(5) . . ?
O9 Ti1 O1 127.00(5) . . ?
O9 Ti1 O3 93.84(5) . . ?
O9 Ti1 O5 99.64(5) . . ?
O9 Ti1 O10 46.59(5) . . ?
O10 Ti1 N1 153.79(5) . . ?
O10 Ti1 N2 128.18(5) . . ?
O10 Ti1 O1 80.48(5) . . ?
O10 Ti1 O3 99.56(5) . . ?
O10 Ti1 O5 102.28(5) . . ?
O1 C1 C2 116.11(15) . . ?
O2 C1 C2 120.70(15) . . ?
O2 C1 O1 123.19(15) . . ?
N1 C2 C1 107.96(13) . . ?
O3 C3 C4 116.20(14) . . ?
O4 C3 C4 119.71(14) . . ?
O4 C3 O3 124.08(15) . . ?
N1 C4 C3 113.63(13) . . ?
O5 C5 C6 115.65(14) . . ?
O6 C5 C6 120.15(16) . . ?
O6 C5 O5 124.18(16) . . ?
N2 C6 C5 111.35(14) . . ?
O8 C7 C8 124.42(15) . . ?
O8 C7 O7 125.12(16) . . ?
O7 C7 C8 110.46(14) . . ?
N2 C8 C7 115.42(13) . . ?
C10 C9 C11 112.37(13) . . ?
N1 C9 C10 108.05(12) . . ?
N1 C9 C11 114.12(14) . . ?
N2 C10 C9 111.83(12) . . ?
C2 N1 Ti1 105.98(8) . . ?
C2 N1 C4 109.71(13) . . ?
C2 N1 C9 111.53(12) . . ?
C4 N1 Ti1 107.50(9) . . ?
C4 N1 C9 113.84(11) . . ?
C9 N1 Ti1 107.89(9) . . ?
C6 N2 Ti1 104.45(9) . . ?
C6 N2 C10 111.35(12) . . ?
C8 N2 Ti1 110.71(9) . . ?
C8 N2 C6 111.46(13) . . ?
C8 N2 C10 110.18(12) . . ?
C10 N2 Ti1 108.52(10) . . ?
C1 O1 Ti1 120.86(10) . . ?
C3 O3 Ti1 123.34(10) . . ?
C5 O5 Ti1 122.11(11) . . ?
O10 O9 Ti1 67.36(6) . . ?
O9 O10 Ti1 66.05(6) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_sad_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 783227'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;State Key Laboratory of Physical Chemistry of Solid Surfaces
China
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2019-10-21 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         ?
_chemical_formula_sum            'C10 H21 N3 O10 Ti'
_chemical_formula_weight         391.20

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

_space_group_crystal_system      Monoclinic
_space_group_IT_number           ?
_space_group_name_H-M_alt        'P 21/a'
_space_group_name_Hall           ?

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

_cell_length_a                   7.96650(10)
_cell_length_b                   30.1390(3)
_cell_length_c                   13.21500(10)
_cell_angle_alpha                90
_cell_angle_beta                 104.7650(10)
_cell_angle_gamma                90
_cell_volume                     3068.18(6)
_cell_formula_units_Z            8
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    1035
_cell_measurement_theta_min      1.73
_cell_measurement_theta_max      23.75

_exptl_crystal_description       prism
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_F_000             1632
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.200
_exptl_absorpt_coefficient_mu    0.618
_shelx_estimated_absorpt_T_min   0.827
_shelx_estimated_absorpt_T_max   0.886
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8267
_exptl_absorpt_correction_T_max  0.8863
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Oxford Gemini Diffractometer'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            23075
_diffrn_reflns_av_unetI/netI     0.0129
_diffrn_reflns_av_R_equivalents  0.0203
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.731
_diffrn_reflns_theta_max         23.749
_diffrn_reflns_theta_full        23.749
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measured_fraction_theta_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_point_group_measured_fraction_full 0.980
_reflns_number_total             4575
_reflns_number_gt                4199
_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, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0446P)²+3.7992P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4575
_refine_ls_number_parameters     481
_refine_ls_number_restraints     29
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0341
_refine_ls_wR_factor_ref         0.0896
_refine_ls_wR_factor_gt          0.0881
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.009
_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 0.49833(5) 0.11897(2) -0.61590(3) 0.01383(13) Uani 1 1 d . . . . .
Ti2 Ti 0.45779(6) 0.11535(2) -0.13079(3) 0.01493(13) Uani 1 1 d . . . . .
N1 N 0.2742(3) 0.13281(7) -0.54136(16) 0.0212(5) Uani 1 1 d . . . . .
N2 N 0.6209(2) 0.16661(6) -0.48463(15) 0.0158(4) Uani 1 1 d . . . . .
N3 N 0.2659(3) 0.11122(7) -0.02718(15) 0.0193(4) Uani 1 1 d . . . . .
N4 N 0.5537(3) 0.16998(6) -0.01194(15) 0.0171(4) Uani 1 1 d . . . . .
N5 N 0.1839(3) -0.01607(7) -0.31565(19) 0.0313(5) Uani 1 1 d D . . . .
H5A H 0.244(3) -0.0399(5) -0.3040(18) 0.038 Uiso 1 1 d D U . . .
H5B H 0.105(2) -0.0190(8) -0.3720(11) 0.038 Uiso 1 1 d D U . . .
H5C H 0.140(3) -0.0113(7) -0.2648(13) 0.038 Uiso 1 1 d D U . . .
H5D H 0.251(2) 0.0052(5) -0.3222(18) 0.038 Uiso 1 1 d D U . . .
N6 N 0.6893(4) 0.00851(8) -0.2197(2) 0.0420(6) Uani 1 1 d D . . . .
H6C H 0.622(3) 0.0004(8) -0.1828(17) 0.050 Uiso 1 1 d D U . . .
H6D H 0.665(3) -0.0036(8) -0.2785(11) 0.050 Uiso 1 1 d D U . . .
H6E H 0.7946(15) 0.0032(8) -0.1868(18) 0.050 Uiso 1 1 d D U . . .
H6F H 0.681(3) 0.0370(3) -0.227(2) 0.050 Uiso 1 1 d D U . . .
O1 O 0.2829(2) 0.09007(6) -0.71144(13) 0.0267(4) Uani 1 1 d . . . . .
O1W O -0.1501(3) 0.02012(9) -0.4384(2) 0.0589(7) Uani 1 1 d D . . . .
H1WA H -0.253(2) 0.0279(12) -0.468(3) 0.071 Uiso 1 1 d D U . . .
H1WB H -0.108(4) 0.0371(11) -0.387(2) 0.071 Uiso 1 1 d D U . . .
O2 O -0.0004(3) 0.09736(13) -0.78368(19) 0.0787(10) Uani 1 1 d . . . . .
O2W O -0.0572(6) 0.02482(14) -0.8870(4) 0.0618(15) Uiso 0.684(8) 1 d D . P A 1
H2WA H -0.035(6) 0.0480(12) -0.849(4) 0.074 Uiso 0.684(8) 1 d D U P A 1
H2WB H -0.162(3) 0.0173(18) -0.895(5) 0.074 Uiso 0.684(8) 1 d D U P A 1
O2W' O 0.8994(11) 0.0311(3) 0.0378(8) 0.056(3) Uiso 0.316(8) 1 d D . P A 2
H2WC H 0.800(7) 0.042(4) 0.037(8) 0.068 Uiso 0.316(8) 1 d D U P A 2
H2WD H 0.903(13) 0.027(4) -0.025(3) 0.068 Uiso 0.316(8) 1 d D U P A 2
O3 O 0.5271(2) 0.07239(5) -0.50730(13) 0.0199(4) Uani 1 1 d . . . . .
O4 O 0.4200(3) 0.03060(6) -0.40074(14) 0.0316(5) Uani 1 1 d . . . . .
O5 O 0.4314(2) 0.17692(6) -0.68151(12) 0.0206(4) Uani 1 1 d . . . . .
O6 O 0.4673(3) 0.25014(6) -0.67949(16) 0.0429(5) Uani 1 1 d . . . . .
O7 O 0.9698(3) 0.21587(6) -0.37222(15) 0.0301(5) Uani 1 1 d . . . . .
H7 H 1.051(4) 0.2248(11) -0.323(3) 0.036 Uiso 1 1 d . U . . .
O8 O 0.6023(2) 0.09208(6) -0.71162(13) 0.0249(4) Uani 1 1 d . . . . .
O9 O 0.7249(2) 0.11564(6) -0.62704(14) 0.0251(4) Uani 1 1 d . . . . .
O11 O 0.2563(2) 0.07474(5) -0.20740(13) 0.0219(4) Uani 1 1 d . . . . .
O12 O -0.0283(3) 0.06296(8) -0.24936(17) 0.0433(5) Uani 1 1 d . . . . .
O13 O 0.5692(2) 0.07187(5) -0.02066(13) 0.0229(4) Uani 1 1 d . . . . .
O14 O 0.5541(3) 0.02472(6) 0.10637(14) 0.0305(4) Uani 1 1 d . . . . .
O15 O 0.3127(2) 0.16576(5) -0.19473(12) 0.0178(4) Uani 1 1 d . . . . .
O16 O 0.2492(2) 0.23759(6) -0.19842(13) 0.0247(4) Uani 1 1 d . . . . .
O17 O 0.7707(3) 0.23969(6) 0.11451(16) 0.0335(5) Uani 1 1 d . . . . .
H17 H 0.807(4) 0.2502(11) 0.174(3) 0.040 Uiso 1 1 d . U . . .
O18 O 0.5547(2) 0.09593(5) -0.23689(13) 0.0220(4) Uani 1 1 d . . . . .
O19 O 0.6616(2) 0.12864(6) -0.16717(13) 0.0225(4) Uani 1 1 d . . . . .
C1 C 0.1297(4) 0.10601(12) -0.7149(2) 0.0380(7) Uani 1 1 d . . . . .
C2 C 0.1192(3) 0.13826(11) -0.6305(2) 0.0339(7) Uani 1 1 d . . . . .
H2A H 0.114312 0.168956 -0.657752 0.041 Uiso 1 1 calc R U . . .
H2B H 0.012546 0.132737 -0.607019 0.041 Uiso 1 1 calc R U . . .
C3 C 0.4100(3) 0.06261(8) -0.45837(18) 0.0227(6) Uani 1 1 d . . . . .
C4 C 0.2562(3) 0.09354(9) -0.4765(2) 0.0258(6) Uani 1 1 d . . . . .
H4A H 0.149939 0.077013 -0.511652 0.031 Uiso 1 1 calc R U . . .
H4B H 0.242151 0.103891 -0.407996 0.031 Uiso 1 1 calc R U . . .
C5 C 0.5035(3) 0.21380(9) -0.6401(2) 0.0240(6) Uani 1 1 d . . . . .
C6 C 0.6415(3) 0.20897(8) -0.53822(19) 0.0210(5) Uani 1 1 d . . . . .
H6A H 0.757655 0.209741 -0.552412 0.025 Uiso 1 1 calc R U . . .
H6B H 0.633718 0.234221 -0.491723 0.025 Uiso 1 1 calc R U . . .
C7 C 0.8926(4) 0.17921(9) -0.3329(2) 0.0270(6) Uani 1 1 d . . . . .
H7A H 0.813050 0.190327 -0.292060 0.032 Uiso 1 1 calc R U . . .
H7B H 0.984426 0.161486 -0.285428 0.032 Uiso 1 1 calc R U . . .
C8 C 0.7932(3) 0.15013(8) -0.4206(2) 0.0229(6) Uani 1 1 d . . . . .
H8A H 0.868006 0.144651 -0.468737 0.028 Uiso 1 1 calc R U . . .
H8B H 0.773907 0.121140 -0.390168 0.028 Uiso 1 1 calc R U . . .
C9 C 0.3145(3) 0.17377(9) -0.4777(2) 0.0256(6) Uani 1 1 d . . . . .
H9A H 0.237161 0.176040 -0.429946 0.031 Uiso 1 1 calc R U . . .
H9B H 0.295072 0.200102 -0.523968 0.031 Uiso 1 1 calc R U . . .
C10 C 0.5010(3) 0.17235(8) -0.41508(19) 0.0212(5) Uani 1 1 d . . . . .
H10A H 0.529762 0.200242 -0.374804 0.025 Uiso 1 1 calc R U . . .
H10B H 0.517155 0.147453 -0.364654 0.025 Uiso 1 1 calc R U . . .
C11 C 0.1038(3) 0.07900(9) -0.1920(2) 0.0263(6) Uani 1 1 d . . . . .
C12 C 0.0905(3) 0.10629(9) -0.0983(2) 0.0244(6) Uani 1 1 d . . . . .
H12A H 0.041358 0.135862 -0.121414 0.029 Uiso 1 1 calc R U . . .
H12B H 0.012697 0.091353 -0.061243 0.029 Uiso 1 1 calc R U . . .
C13 C 0.4916(4) 0.05412(8) 0.04424(19) 0.0238(6) Uani 1 1 d . . . . .
C14 C 0.3106(4) 0.07086(8) 0.0384(2) 0.0253(6) Uani 1 1 d . . . . .
H14A H 0.225910 0.047174 0.009368 0.030 Uiso 1 1 calc R U . . .
H14B H 0.300786 0.077549 0.110048 0.030 Uiso 1 1 calc R U . . .
C15 C 0.3390(3) 0.20610(8) -0.15940(18) 0.0171(5) Uani 1 1 d . . . . .
C16 C 0.4933(3) 0.21266(8) -0.06630(18) 0.0185(5) Uani 1 1 d . . . . .
H16A H 0.589654 0.226240 -0.090245 0.022 Uiso 1 1 calc R U . . .
H16B H 0.460986 0.233378 -0.016281 0.022 Uiso 1 1 calc R U . . .
C17 C 0.8266(4) 0.19469(9) 0.1259(2) 0.0311(6) Uani 1 1 d . . . . .
H17A H 0.790750 0.180994 0.185180 0.037 Uiso 1 1 calc R U . . .
H17B H 0.954871 0.193507 0.141497 0.037 Uiso 1 1 calc R U . . .
C18 C 0.7486(3) 0.16889(9) 0.0264(2) 0.0250(6) Uani 1 1 d . . . . .
H18A H 0.798060 0.180614 -0.029798 0.030 Uiso 1 1 calc R U . . .
H18B H 0.785556 0.137541 0.038102 0.030 Uiso 1 1 calc R U . . .
C19 C 0.2845(3) 0.15202(8) 0.03847(19) 0.0227(5) Uani 1 1 d . . . . .
H19A H 0.233217 0.147054 0.098337 0.027 Uiso 1 1 calc R U . . .
H19B H 0.222431 0.177017 -0.003517 0.027 Uiso 1 1 calc R U . . .
C20 C 0.4750(3) 0.16307(8) 0.07795(18) 0.0212(5) Uani 1 1 d . . . . .
H20A H 0.488715 0.190319 0.121131 0.025 Uiso 1 1 calc R U . . .
H20B H 0.535621 0.138556 0.122422 0.025 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 O9 1.8505(17) . ?
Ti1 O8 1.8647(17) . ?
Ti1 O5 1.9623(17) . ?
Ti1 O3 1.9788(16) . ?
Ti1 O1 2.0479(17) . ?
Ti1 N2 2.272(2) . ?
Ti1 N1 2.286(2) . ?
Ti2 O19 1.8511(18) . ?
Ti2 O18 1.8591(17) . ?
Ti2 O15 1.9648(16) . ?
Ti2 O13 1.9913(16) . ?
Ti2 O11 2.0669(17) . ?
Ti2 N4 2.2693(19) . ?
Ti2 N3 2.301(2) . ?
N1 C9 1.483(3) . ?
N1 C2 1.483(3) . ?
N1 C4 1.490(3) . ?
N2 C6 1.489(3) . ?
N2 C10 1.495(3) . ?
N2 C8 1.502(3) . ?
N3 C12 1.479(3) . ?
N3 C14 1.483(3) . ?
N3 C19 1.490(3) . ?
N4 C16 1.492(3) . ?
N4 C20 1.493(3) . ?
N4 C18 1.505(3) . ?
O1 C1 1.302(4) . ?
O2 C1 1.220(4) . ?
O3 C3 1.297(3) . ?
O4 C3 1.219(3) . ?
O5 C5 1.306(3) . ?
O6 C5 1.215(3) . ?
O7 C7 1.425(3) . ?
O8 O9 1.467(2) . ?
O11 C11 1.288(3) . ?
O12 C11 1.229(3) . ?
O13 C13 1.294(3) . ?
O14 C13 1.224(3) . ?
O15 C15 1.300(3) . ?
O16 C15 1.221(3) . ?
O17 C17 1.423(3) . ?
O18 O19 1.465(2) . ?
C1 C2 1.498(4) . ?
C3 C4 1.510(4) . ?
C5 C6 1.512(4) . ?
C7 C8 1.507(4) . ?
C9 C10 1.505(4) . ?
C11 C12 1.513(4) . ?
C13 C14 1.511(4) . ?
C15 C16 1.514(3) . ?
C17 C18 1.518(4) . ?
C19 C20 1.511(4) . ?

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
O9 Ti1 O8 46.50(8) . . ?
O9 Ti1 O5 99.99(8) . . ?
O8 Ti1 O5 101.81(7) . . ?
O9 Ti1 O3 94.84(8) . . ?
O8 Ti1 O3 101.20(8) . . ?
O5 Ti1 O3 156.95(7) . . ?
O9 Ti1 O1 127.51(8) . . ?
O8 Ti1 O1 81.03(8) . . ?
O5 Ti1 O1 90.90(7) . . ?
O3 Ti1 O1 93.97(7) . . ?
O9 Ti1 N2 81.77(7) . . ?
O8 Ti1 N2 127.87(8) . . ?
O5 Ti1 N2 77.90(7) . . ?
O3 Ti1 N2 86.96(7) . . ?
O1 Ti1 N2 150.37(7) . . ?
O9 Ti1 N1 158.22(8) . . ?
O8 Ti1 N1 154.44(8) . . ?
O5 Ti1 N1 82.77(7) . . ?
O3 Ti1 N1 77.04(7) . . ?
O1 Ti1 N1 73.72(7) . . ?
N2 Ti1 N1 77.68(7) . . ?
O19 Ti2 O18 46.52(7) . . ?
O19 Ti2 O15 100.36(7) . . ?
O18 Ti2 O15 103.35(7) . . ?
O19 Ti2 O13 94.30(8) . . ?
O18 Ti2 O13 98.66(7) . . ?
O15 Ti2 O13 157.98(7) . . ?
O19 Ti2 O11 128.62(7) . . ?
O18 Ti2 O11 82.19(7) . . ?
O15 Ti2 O11 87.07(7) . . ?
O13 Ti2 O11 96.56(7) . . ?
O19 Ti2 N4 81.94(7) . . ?
O18 Ti2 N4 128.25(8) . . ?
O15 Ti2 N4 78.12(7) . . ?
O13 Ti2 N4 87.87(7) . . ?
O11 Ti2 N4 148.35(7) . . ?
O19 Ti2 N3 157.85(7) . . ?
O18 Ti2 N3 153.93(7) . . ?
O15 Ti2 N3 83.72(7) . . ?
O13 Ti2 N3 76.67(7) . . ?
O11 Ti2 N3 73.05(7) . . ?
N4 Ti2 N3 77.59(7) . . ?
C9 N1 C2 112.0(2) . . ?
C9 N1 C4 111.92(19) . . ?
C2 N1 C4 111.2(2) . . ?
C9 N1 Ti1 108.46(15) . . ?
C2 N1 Ti1 105.17(15) . . ?
C4 N1 Ti1 107.68(15) . . ?
C6 N2 C10 111.00(18) . . ?
C6 N2 C8 110.85(19) . . ?
C10 N2 C8 109.12(18) . . ?
C6 N2 Ti1 104.87(14) . . ?
C10 N2 Ti1 108.96(14) . . ?
C8 N2 Ti1 111.99(14) . . ?
C12 N3 C14 109.64(19) . . ?
C12 N3 C19 113.0(2) . . ?
C14 N3 C19 111.27(19) . . ?
C12 N3 Ti2 106.92(15) . . ?
C14 N3 Ti2 107.17(15) . . ?
C19 N3 Ti2 108.60(14) . . ?
C16 N4 C20 110.73(18) . . ?
C16 N4 C18 111.04(19) . . ?
C20 N4 C18 109.63(18) . . ?
C16 N4 Ti2 106.37(13) . . ?
C20 N4 Ti2 108.29(14) . . ?
C18 N4 Ti2 110.70(14) . . ?
C1 O1 Ti1 119.72(18) . . ?
C3 O3 Ti1 123.91(16) . . ?
C5 O5 Ti1 122.11(15) . . ?
O9 O8 Ti1 66.24(9) . . ?
O8 O9 Ti1 67.26(10) . . ?
C11 O11 Ti2 120.63(16) . . ?
C13 O13 Ti2 123.87(16) . . ?
C15 O15 Ti2 123.05(14) . . ?
O19 O18 Ti2 66.45(9) . . ?
O18 O19 Ti2 67.03(10) . . ?
O2 C1 O1 124.0(3) . . ?
O2 C1 C2 119.7(3) . . ?
O1 C1 C2 116.3(2) . . ?
N1 C2 C1 109.1(2) . . ?
O4 C3 O3 123.4(3) . . ?
O4 C3 C4 120.6(2) . . ?
O3 C3 C4 116.0(2) . . ?
N1 C4 C3 112.8(2) . . ?
O6 C5 O5 123.8(2) . . ?
O6 C5 C6 120.5(2) . . ?
O5 C5 C6 115.7(2) . . ?
N2 C6 C5 111.3(2) . . ?
O7 C7 C8 111.2(2) . . ?
N2 C8 C7 117.8(2) . . ?
N1 C9 C10 109.2(2) . . ?
N2 C10 C9 111.18(19) . . ?
O12 C11 O11 123.9(3) . . ?
O12 C11 C12 119.4(2) . . ?
O11 C11 C12 116.7(2) . . ?
N3 C12 C11 108.8(2) . . ?
O14 C13 O13 124.2(3) . . ?
O14 C13 C14 119.7(2) . . ?
O13 C13 C14 116.1(2) . . ?
N3 C14 C13 112.8(2) . . ?
O16 C15 O15 123.5(2) . . ?
O16 C15 C16 120.6(2) . . ?
O15 C15 C16 115.9(2) . . ?
N4 C16 C15 111.96(19) . . ?
O17 C17 C18 110.4(2) . . ?
N4 C18 C17 116.1(2) . . ?
N3 C19 C20 109.0(2) . . ?
N4 C20 C19 110.17(19) . . ?

_refine_diff_density_max         0.776
_refine_diff_density_min         -0.515
_refine_diff_density_rms         0.065

####################################################################### 
# 
# 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_sad_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 783226'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;State Key Laboratory of Physical Chemistry of Solid Surfaces
China
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2019-10-21 downloaded from the CCDC.
;
_audit_creation_date             2019-07-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C9 H12 N2 O8 Ti, H4 N, H2 O'
_chemical_formula_sum            'C9 H18 N3 O9 Ti'
_chemical_formula_weight         360.16
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   16.1839(6)
_cell_length_b                   11.1970(4)
_cell_length_c                   15.8291(6)
_cell_angle_alpha                90
_cell_angle_beta                 103.231(4)
_cell_angle_gamma                90
_cell_volume                     2792.27(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    897
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.99
_cell_measurement_theta_min      2.23
_shelx_estimated_absorpt_T_max   0.949
_shelx_estimated_absorpt_T_min   0.776
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_T_max  0.9486
_exptl_absorpt_correction_T_min  0.7764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flaky
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0443
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            10553
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         2.231
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Oxford Gemini Diffractometer'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed tube'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2354
_reflns_number_total             3195
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.761
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.064
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3195
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0565
_refine_ls_R_factor_gt           0.0346
_refine_ls_restrained_S_all      0.957
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0362P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0720
_refine_ls_wR_factor_ref         0.0759
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 N3-H1 = N3-H2 = N3-H3 = N3-H4 = O1W-H1W1 = O1W-H1W2
 0.85 with sigma of 0.01
 H1-H2 = H1-H3 = H1-H4 = H2-H3 = H2-H4 = H3-H4 = H1W1-H1W2
 1.39 with sigma of 0.01
3.a Ternary CH refined with riding coordinates:
 C7(H7A)
3.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C8(H8A,H8B)
3.c Me refined with riding coordinates:
 C9(H9A,H9B,H9C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 0.28776(2) 0.20380(3) 0.16575(2) 0.01293(10) Uani 1 1 d . . . . .
N1 N 0.16102(10) 0.13511(15) 0.18948(11) 0.0141(4) Uani 1 1 d . . . . .
N2 N 0.23849(10) 0.08999(15) 0.05179(11) 0.0139(4) Uani 1 1 d . . . . .
O1 O 0.20695(9) 0.32548(12) 0.10829(9) 0.0170(3) Uani 1 1 d . . . . .
O2 O 0.07713(9) 0.40249(13) 0.07201(11) 0.0252(4) Uani 1 1 d . . . . .
O3 O 0.29010(9) 0.24632(13) 0.28997(9) 0.0190(3) Uani 1 1 d . . . . .
O4 O 0.24884(10) 0.20792(14) 0.41159(9) 0.0237(3) Uani 1 1 d . . . . .
O5 O 0.33686(9) 0.04679(12) 0.20648(9) 0.0176(3) Uani 1 1 d . . . . .
O6 O 0.40477(9) -0.10724(13) 0.16373(10) 0.0245(4) Uani 1 1 d . . . . .
O7 O 0.36760(9) 0.24057(13) 0.09996(9) 0.0202(3) Uani 1 1 d . . . . .
O8 O 0.38605(9) 0.29476(14) 0.18699(10) 0.0240(3) Uani 1 1 d . . . . .
C1 C 0.12684(13) 0.32826(18) 0.11030(13) 0.0174(4) Uani 1 1 d . . . . .
C2 C 0.09918(13) 0.23451(18) 0.16616(14) 0.0168(4) Uani 1 1 d . . . . .
H2A H 0.090854 0.272481 0.220078 0.020 Uiso 1 1 calc R U . . .
H2B H 0.043869 0.201425 0.134956 0.020 Uiso 1 1 calc R U . . .
C3 C 0.24214(13) 0.19400(18) 0.33375(13) 0.0166(4) Uani 1 1 d . . . . .
C4 C 0.17665(14) 0.10885(19) 0.28330(13) 0.0192(5) Uani 1 1 d . . . . .
H4A H 0.197035 0.025669 0.294218 0.023 Uiso 1 1 calc R U . . .
H4B H 0.123050 0.116876 0.302903 0.023 Uiso 1 1 calc R U . . .
C5 C 0.35146(13) -0.02845(18) 0.14834(14) 0.0168(4) Uani 1 1 d . . . . .
C6 C 0.29847(14) -0.01151(19) 0.05769(14) 0.0181(4) Uani 1 1 d . . . . .
H6A H 0.336381 0.002782 0.017719 0.022 Uiso 1 1 calc R U . . .
H6B H 0.266022 -0.085553 0.038891 0.022 Uiso 1 1 calc R U . . .
C7 C 0.13653(13) 0.02490(18) 0.13579(13) 0.0153(4) Uani 1 1 d . . . . .
H7A H 0.178127 -0.038848 0.161127 0.018 Uiso 1 1 calc R U . . .
C8 C 0.14941(13) 0.05175(19) 0.04637(13) 0.0164(4) Uani 1 1 d . . . . .
H8A H 0.136738 -0.020390 0.009518 0.020 Uiso 1 1 calc R U . . .
H8B H 0.110007 0.115889 0.019382 0.020 Uiso 1 1 calc R U . . .
C9 C 0.04848(14) -0.0237(2) 0.13406(15) 0.0246(5) Uani 1 1 d . . . . .
H9A H 0.038349 -0.095330 0.097543 0.037 Uiso 1 1 calc R U . . .
H9B H 0.044470 -0.044194 0.193187 0.037 Uiso 1 1 calc R U . . .
H9C H 0.005851 0.036975 0.110343 0.037 Uiso 1 1 calc R U . . .
N3 N 0.03036(12) 0.63391(18) 0.11854(13) 0.0280(5) Uani 1 1 d D . . . .
H1 H -0.0198(7) 0.6579(16) 0.1182(13) 0.034 Uiso 1 1 d D U . . .
H2 H 0.0470(12) 0.6663(16) 0.0766(9) 0.034 Uiso 1 1 d D U . . .
H3 H 0.0315(12) 0.5586(7) 0.1147(13) 0.034 Uiso 1 1 d D U . . .
H4 H 0.0634(10) 0.6552(17) 0.1664(8) 0.034 Uiso 1 1 d D U . . .
O1W O 0.41198(10) 0.24811(16) 0.51334(12) 0.0294(4) Uani 1 1 d D . . . .
H1W1 H 0.4199(13) 0.213(2) 0.5615(9) 0.035 Uiso 1 1 d D U . . .
H1W2 H 0.3607(7) 0.254(2) 0.4895(14) 0.035 Uiso 1 1 d D 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 N1 2.3006(17) . ?
Ti1 N2 2.2035(17) . ?
Ti1 O1 1.9621(14) . ?
Ti1 O3 2.0150(14) . ?
Ti1 O5 1.9756(14) . ?
Ti1 O7 1.8813(15) . ?
Ti1 O8 1.8537(15) . ?
N1 C2 1.486(3) . ?
N1 C4 1.478(2) . ?
N1 C7 1.499(2) . ?
N2 C6 1.484(3) . ?
N2 C8 1.487(3) . ?
O1 C1 1.304(2) . ?
O2 C1 1.217(2) . ?
O3 C3 1.293(3) . ?
O4 C3 1.222(2) . ?
O5 C5 1.309(3) . ?
O6 C5 1.219(2) . ?
O7 O8 1.472(2) . ?
C1 C2 1.505(3) . ?
C3 C4 1.511(3) . ?
C5 C6 1.506(3) . ?
C7 C8 1.507(3) . ?
C7 C9 1.520(3) . ?

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
N2 Ti1 N1 76.77(6) . . ?
O1 Ti1 N1 77.48(6) . . ?
O1 Ti1 N2 86.80(6) . . ?
O1 Ti1 O3 98.62(6) . . ?
O1 Ti1 O5 160.88(6) . . ?
O3 Ti1 N1 74.81(6) . . ?
O3 Ti1 N2 149.09(6) . . ?
O5 Ti1 N1 87.49(6) . . ?
O5 Ti1 N2 78.22(6) . . ?
O5 Ti1 O3 88.59(6) . . ?
O7 Ti1 N1 156.14(6) . . ?
O7 Ti1 N2 80.74(6) . . ?
O7 Ti1 O1 93.49(6) . . ?
O7 Ti1 O3 128.79(6) . . ?
O7 Ti1 O5 95.71(6) . . ?
O8 Ti1 N1 156.10(6) . . ?
O8 Ti1 N2 126.94(7) . . ?
O8 Ti1 O1 98.97(6) . . ?
O8 Ti1 O3 82.50(6) . . ?
O8 Ti1 O5 99.52(6) . . ?
O8 Ti1 O7 46.42(6) . . ?
C2 N1 Ti1 106.50(12) . . ?
C2 N1 C7 113.58(15) . . ?
C4 N1 Ti1 106.06(12) . . ?
C4 N1 C2 110.45(16) . . ?
C4 N1 C7 111.60(15) . . ?
C7 N1 Ti1 108.21(12) . . ?
C6 N2 Ti1 106.41(12) . . ?
C6 N2 C8 113.25(16) . . ?
C8 N2 Ti1 112.21(12) . . ?
C1 O1 Ti1 124.48(13) . . ?
C3 O3 Ti1 122.44(12) . . ?
C5 O5 Ti1 117.85(13) . . ?
O8 O7 Ti1 65.80(8) . . ?
O7 O8 Ti1 67.78(8) . . ?
O1 C1 C2 115.37(17) . . ?
O2 C1 O1 123.5(2) . . ?
O2 C1 C2 121.14(19) . . ?
N1 C2 C1 113.23(16) . . ?
O3 C3 C4 115.92(17) . . ?
O4 C3 O3 123.85(19) . . ?
O4 C3 C4 120.21(19) . . ?
N1 C4 C3 110.10(16) . . ?
O5 C5 C6 115.72(18) . . ?
O6 C5 O5 124.0(2) . . ?
O6 C5 C6 120.29(19) . . ?
N2 C6 C5 112.23(17) . . ?
N1 C7 C8 107.01(16) . . ?
N1 C7 C9 115.48(17) . . ?
C8 C7 C9 112.65(17) . . ?
N2 C8 C7 110.11(16) . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_sad_CCDC3
_database_code_depnum_ccdc_archive 'CCDC 783225'
loop_
_audit_author_name
_audit_author_address
'Zhao-Hui Zhou'
;State Key Laboratory of Physical Chemistry of Solid Surfaces
China
;
_audit_update_record             
;
2019-10-17 deposited with the CCDC.	2019-10-21 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         ?
_chemical_formula_sum            'C22 H55 N7 O27 Ti2'
_chemical_formula_weight         945.53

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

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

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

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

_cell_length_a                   22.998(14)
_cell_length_b                   12.0774(13)
_cell_length_c                   16.442(9)
_cell_angle_alpha                90
_cell_angle_beta                 124.99(4)
_cell_angle_gamma                90
_cell_volume                     3741(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    985
_cell_measurement_theta_min      2.8534
_cell_measurement_theta_max      28.9777

_exptl_crystal_description       flaky
_exptl_crystal_colour            orange
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.679
_exptl_crystal_F_000             1984
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.130
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    0.537
_shelx_estimated_absorpt_T_min   0.924
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.94574
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            8458
_diffrn_reflns_av_unetI/netI     0.1679
_diffrn_reflns_av_R_equivalents  0.0975
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_theta_min         2.859
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.997
_reflns_number_total             4114
_reflns_number_gt                2419
_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, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_cell_refinement       
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_data_reduction        
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0214P)²] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4114
_refine_ls_number_parameters     302
_refine_ls_number_restraints     23
_refine_ls_R_factor_all          0.1521
_refine_ls_R_factor_gt           0.0849
_refine_ls_wR_factor_ref         0.1326
_refine_ls_wR_factor_gt          0.1097
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_restrained_S_all      1.046
_refine_ls_shift/su_max          0.006
_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 0.27895(4) 0.21539(7) 0.35452(7) 0.0119(2) Uani 1 1 d . . . . .
C1 C 0.2351(2) 0.1152(4) 0.1656(4) 0.0150(11) Uani 1 1 d . . . . .
C2 C 0.3138(2) 0.1036(4) 0.2172(4) 0.0163(12) Uani 1 1 d . . . . .
H2A H 0.324409 0.028315 0.205269 0.020 Uiso 1 1 calc R U . . .
H2B H 0.329895 0.157420 0.188643 0.020 Uiso 1 1 calc R U . . .
C3 C 0.3915(3) 0.3166(4) 0.3492(4) 0.0209(13) Uani 1 1 d . . . . .
C4 C 0.4143(2) 0.1980(4) 0.3596(4) 0.0213(13) Uani 1 1 d . . . . .
H4A H 0.433465 0.185183 0.319691 0.026 Uiso 1 1 calc R U . . .
H4B H 0.452463 0.182301 0.429920 0.026 Uiso 1 1 calc R U . . .
C5 C 0.3800(3) 0.1401(4) 0.5568(4) 0.0163(12) Uani 1 1 d . . . . .
C6 C 0.3253(2) 0.0487(4) 0.5189(3) 0.0146(11) Uani 1 1 d . . . . .
H6A H 0.349898 -0.022802 0.547210 0.018 Uiso 1 1 calc R U . . .
H6B H 0.294563 0.062466 0.541926 0.018 Uiso 1 1 calc R U . . .
C7 C 0.2005(3) -0.1150(4) 0.3995(4) 0.0139(11) Uani 1 1 d . . . . .
C8 C 0.2082(2) -0.0001(4) 0.3704(4) 0.0131(11) Uani 1 1 d . . . . .
H8A H 0.179751 0.002901 0.296961 0.016 Uiso 1 1 calc R U . . .
H8B H 0.186446 0.052694 0.391701 0.016 Uiso 1 1 calc R U . . .
C9 C 0.3775(2) 0.0192(4) 0.3858(4) 0.0163(12) Uani 1 1 d . . . . .
H9A H 0.410004 0.041757 0.456969 0.020 Uiso 1 1 calc R U . . .
C10 C 0.3136(2) -0.0341(4) 0.3731(4) 0.0127(11) Uani 1 1 d . . . . .
H10A H 0.278191 -0.051571 0.302089 0.015 Uiso 1 1 calc R U . . .
H10B H 0.327951 -0.104444 0.410789 0.015 Uiso 1 1 calc R U . . .
C11 C 0.4183(3) -0.0628(4) 0.3655(4) 0.0234(13) Uani 1 1 d . . . . .
H11A H 0.431430 -0.127576 0.408615 0.035 Uiso 1 1 calc R U . . .
H11B H 0.388240 -0.086270 0.295849 0.035 Uiso 1 1 calc R U . . .
H11C H 0.461253 -0.027308 0.378860 0.035 Uiso 1 1 calc R U . . .
N1 N 0.35369(19) 0.1225(3) 0.3256(3) 0.0116(9) Uani 1 1 d . . . . .
N2 N 0.28049(18) 0.0407(3) 0.4090(3) 0.0109(9) Uani 1 1 d . . . . .
N3 N 0.000000 -0.0346(6) 0.250000 0.0296(17) Uani 1 2 d DS T P . .
N4 N 0.0624(2) 0.1087(4) 0.0681(4) 0.0380(14) Uani 1 1 d D . . . .
O1 O 0.21538(15) 0.1629(3) 0.2179(2) 0.0156(8) Uani 1 1 d . . . . .
O2 O 0.19354(17) 0.0859(3) 0.0802(3) 0.0244(9) Uani 1 1 d . . . . .
O3 O 0.32886(17) 0.3351(3) 0.3254(3) 0.0195(8) Uani 1 1 d . . . . .
O4 O 0.43492(18) 0.3903(3) 0.3669(3) 0.0301(10) Uani 1 1 d . . . . .
O5 O 0.36485(16) 0.2184(3) 0.4930(2) 0.0176(8) Uani 1 1 d . . . . .
O6 O 0.43266(17) 0.1384(3) 0.6419(3) 0.0239(9) Uani 1 1 d . . . . .
O7 O 0.14009(16) -0.1524(3) 0.3583(3) 0.0198(9) Uani 1 1 d . . . . .
O8 O 0.25755(16) -0.1653(3) 0.4660(3) 0.0190(8) Uani 1 1 d . . . . .
O9 O 0.22966(17) 0.3365(3) 0.3518(3) 0.0232(9) Uani 1 1 d . . . . .
O10 O 0.20718(17) 0.2342(3) 0.3731(3) 0.0189(8) Uani 1 1 d . . . . .
O1W O 0.07448(19) -0.2835(4) 0.4256(3) 0.0467(13) Uani 1 1 d D . . . .
O2W O 0.0524(2) 0.1999(3) 0.2117(3) 0.0383(11) Uani 1 1 d D . . . .
O3W O 0.08403(18) 0.0607(3) 0.4431(3) 0.0309(10) Uani 1 1 d D . . . .
O4W O 0.500000 -0.0812(7) 0.750000 0.0569(19) Uani 1 2 d DS T P . .
H1W1 H 0.1117(14) -0.258(5) 0.432(4) 0.068 Uiso 1 1 d D U . . .
H1W2 H 0.0382(15) -0.257(5) 0.373(3) 0.068 Uiso 1 1 d D U . . .
H2W1 H 0.0912(13) 0.229(4) 0.257(3) 0.068 Uiso 1 1 d D U . . .
H2W2 H 0.0176(16) 0.240(4) 0.198(4) 0.068 Uiso 1 1 d D U . . .
H3W1 H 0.093(3) 0.1299(11) 0.451(5) 0.068 Uiso 1 1 d D U . . .
H3W2 H 0.1223(16) 0.025(4) 0.483(4) 0.068 Uiso 1 1 d D U . . .
H4W1 H 0.4601(19) -0.087(6) 0.695(3) 0.068 Uiso 1 1 d D U . . .
H1 H 0.029(2) -0.078(4) 0.250(5) 0.068 Uiso 1 1 d D U . . .
H2 H 0.023(2) 0.009(4) 0.299(3) 0.068 Uiso 1 1 d D U . . .
H3 H 0.068(2) 0.0406(14) 0.085(4) 0.068 Uiso 1 1 d D U . . .
H4 H 0.0253(14) 0.115(4) 0.0090(14) 0.068 Uiso 1 1 d D U . . .
H5 H 0.0983(15) 0.132(3) 0.070(3) 0.068 Uiso 1 1 d D U . . .
H6 H 0.058(2) 0.146(3) 0.108(3) 0.068 Uiso 1 1 d D U . . .
H8 H 0.250000 -0.250000 0.500000 0.068 Uiso 1 2 d S U P . .


_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 O9 1.835(3) . ?
Ti1 O10 1.856(3) . ?
Ti1 O1 1.954(4) . ?
Ti1 O5 1.982(4) . ?
Ti1 O3 2.066(3) . ?
Ti1 N2 2.285(4) . ?
Ti1 N1 2.318(4) . ?
C1 O2 1.214(6) . ?
C1 O1 1.313(5) . ?
C1 C2 1.501(6) . ?
C2 N1 1.482(6) . ?
C3 O4 1.242(5) . ?
C3 O3 1.277(6) . ?
C3 C4 1.500(7) . ?
C4 N1 1.481(5) . ?
C5 O6 1.217(6) . ?
C5 O5 1.302(6) . ?
C5 C6 1.513(6) . ?
C6 N2 1.483(6) . ?
C7 O7 1.231(5) . ?
C7 O8 1.280(6) . ?
C7 C8 1.512(6) . ?
C8 N2 1.483(5) . ?
C9 N1 1.488(6) . ?
C9 C10 1.506(6) . ?
C9 C11 1.526(6) . ?
C10 N2 1.503(5) . ?
O9 O10 1.457(4) . ?

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
O9 Ti1 O10 46.51(13) . . ?
O9 Ti1 O1 100.71(16) . . ?
O10 Ti1 O1 94.54(15) . . ?
O9 Ti1 O5 102.03(16) . . ?
O10 Ti1 O5 101.74(15) . . ?
O1 Ti1 O5 157.24(14) . . ?
O9 Ti1 O3 81.61(15) . . ?
O10 Ti1 O3 128.12(15) . . ?
O1 Ti1 O3 96.27(14) . . ?
O5 Ti1 O3 86.17(14) . . ?
O9 Ti1 N2 128.04(14) . . ?
O10 Ti1 N2 82.17(13) . . ?
O1 Ti1 N2 89.10(15) . . ?
O5 Ti1 N2 77.61(14) . . ?
O3 Ti1 N2 148.37(13) . . ?
O9 Ti1 N1 154.25(15) . . ?
O10 Ti1 N1 157.87(15) . . ?
O1 Ti1 N1 76.19(14) . . ?
O5 Ti1 N1 82.90(14) . . ?
O3 Ti1 N1 73.45(13) . . ?
N2 Ti1 N1 77.69(13) . . ?
O2 C1 O1 123.1(4) . . ?
O2 C1 C2 121.5(5) . . ?
O1 C1 C2 115.3(4) . . ?
N1 C2 C1 112.3(4) . . ?
O4 C3 O3 124.1(5) . . ?
O4 C3 C4 118.4(5) . . ?
O3 C3 C4 117.5(4) . . ?
N1 C4 C3 110.6(4) . . ?
O6 C5 O5 124.6(5) . . ?
O6 C5 C6 120.4(5) . . ?
O5 C5 C6 115.0(4) . . ?
N2 C6 C5 112.5(4) . . ?
O7 C7 O8 125.2(5) . . ?
O7 C7 C8 117.5(4) . . ?
O8 C7 C8 117.3(4) . . ?
N2 C8 C7 118.3(4) . . ?
N1 C9 C10 108.0(4) . . ?
N1 C9 C11 116.0(4) . . ?
C10 C9 C11 111.4(4) . . ?
N2 C10 C9 111.3(4) . . ?
C4 N1 C2 110.4(4) . . ?
C4 N1 C9 111.0(4) . . ?
C2 N1 C9 114.1(4) . . ?
C4 N1 Ti1 105.9(3) . . ?
C2 N1 Ti1 107.5(3) . . ?
C9 N1 Ti1 107.7(3) . . ?
C6 N2 C8 111.7(3) . . ?
C6 N2 C10 111.3(4) . . ?
C8 N2 C10 109.2(4) . . ?
C6 N2 Ti1 105.1(3) . . ?
C8 N2 Ti1 112.1(3) . . ?
C10 N2 Ti1 107.4(2) . . ?
C1 O1 Ti1 125.7(3) . . ?
C3 O3 Ti1 119.0(3) . . ?
C5 O5 Ti1 122.8(3) . . ?
O10 O9 Ti1 67.53(18) . . ?
O9 O10 Ti1 65.96(17) . . ?

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 C1 C2 N1 -168.2(5) . . . . ?
O1 C1 C2 N1 14.4(6) . . . . ?
O4 C3 C4 N1 -174.1(4) . . . . ?
O3 C3 C4 N1 7.9(7) . . . . ?
O6 C5 C6 N2 -159.0(4) . . . . ?
O5 C5 C6 N2 22.6(6) . . . . ?
O7 C7 C8 N2 -172.1(4) . . . . ?
O8 C7 C8 N2 8.6(6) . . . . ?
N1 C9 C10 N2 -60.9(5) . . . . ?
C11 C9 C10 N2 170.7(4) . . . . ?
C3 C4 N1 C2 86.9(5) . . . . ?
C3 C4 N1 C9 -145.6(4) . . . . ?
C3 C4 N1 Ti1 -29.1(5) . . . . ?
C1 C2 N1 C4 -133.1(4) . . . . ?
C1 C2 N1 C9 101.2(5) . . . . ?
C1 C2 N1 Ti1 -18.1(5) . . . . ?
C10 C9 N1 C4 160.7(4) . . . . ?
C11 C9 N1 C4 -73.6(5) . . . . ?
C10 C9 N1 C2 -74.0(5) . . . . ?
C11 C9 N1 C2 51.8(5) . . . . ?
C10 C9 N1 Ti1 45.2(4) . . . . ?
C11 C9 N1 Ti1 171.0(3) . . . . ?
C5 C6 N2 C8 -149.5(4) . . . . ?
C5 C6 N2 C10 88.2(5) . . . . ?
C5 C6 N2 Ti1 -27.7(4) . . . . ?
C7 C8 N2 C6 -62.7(5) . . . . ?
C7 C8 N2 C10 60.8(5) . . . . ?
C7 C8 N2 Ti1 179.6(3) . . . . ?
C9 C10 N2 C6 -71.9(5) . . . . ?
C9 C10 N2 C8 164.4(4) . . . . ?
C9 C10 N2 Ti1 42.6(4) . . . . ?
O2 C1 O1 Ti1 -178.6(4) . . . . ?
C2 C1 O1 Ti1 -1.3(6) . . . . ?
O4 C3 O3 Ti1 -154.7(4) . . . . ?
C4 C3 O3 Ti1 23.1(6) . . . . ?
O6 C5 O5 Ti1 179.0(4) . . . . ?
C6 C5 O5 Ti1 -2.7(5) . . . . ?
O1 Ti1 O9 O10 86.1(2) . . . . ?
O5 Ti1 O9 O10 -94.9(2) . . . . ?
O3 Ti1 O9 O10 -179.1(2) . . . . ?
N2 Ti1 O9 O10 -11.3(3) . . . . ?
N1 Ti1 O9 O10 166.5(3) . . . . ?
O1 Ti1 O10 O9 -100.5(2) . . . . ?
O5 Ti1 O10 O9 95.5(2) . . . . ?
O3 Ti1 O10 O9 1.2(3) . . . . ?
N2 Ti1 O10 O9 171.1(2) . . . . ?
N1 Ti1 O10 O9 -164.3(4) . . . . ?

_refine_diff_density_max         0.507
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.109

