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

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

data_kyj41-1
_database_code_depnum_ccdc_archive 'CCDC 1497957'
_audit_update_record             
;
2016-08-06 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C13 H22 N2 O2'
_chemical_formula_weight         238.33

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'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P2(1)/c  '

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

_cell_length_a                   12.9760(3)
_cell_length_b                   9.0107(2)
_cell_length_c                   12.2487(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 102.498(2)
_cell_angle_gamma                90.00
_cell_volume                     1398.22(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    2798
_cell_measurement_theta_min      2.77
_cell_measurement_theta_max      29.79

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             520
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_correction_T_min  0.9849
_exptl_absorpt_correction_T_max  0.9924
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            7785
_diffrn_reflns_av_R_equivalents  0.0249
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.77
_diffrn_reflns_theta_max         25.00
_reflns_number_total             2464
_reflns_number_gt                1970
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0443P)²+0.4397P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     SHELXL
_refine_ls_extinction_coef       0.0019(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         2464
_refine_ls_number_parameters     161
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0522
_refine_ls_R_factor_gt           0.0373
_refine_ls_wR_factor_ref         0.0947
_refine_ls_wR_factor_gt          0.0872
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
N2 N 0.22097(9) 0.08149(13) 0.12068(9) 0.0220(3) Uani 1 1 d . . .
N1 N 0.17086(9) -0.16295(13) 0.09169(9) 0.0204(3) Uani 1 1 d . . .
C10 C 0.20443(11) 0.22833(16) 0.16327(12) 0.0242(3) Uani 1 1 d . . .
H10A H 0.1906 0.2189 0.2394 0.029 Uiso 1 1 calc R . .
H10B H 0.1416 0.2742 0.1147 0.029 Uiso 1 1 calc R . .
C6 C 0.27837(10) -0.19811(16) 0.07818(11) 0.0204(3) Uani 1 1 d . . .
H6A H 0.2924 -0.3044 0.0956 0.024 Uiso 1 1 calc R . .
H6B H 0.3294 -0.1398 0.1335 0.024 Uiso 1 1 calc R . .
C2 C 0.00297(11) -0.25376(19) 0.10903(13) 0.0321(4) Uani 1 1 d . . .
H2 H -0.0465 -0.3327 0.1024 0.039 Uiso 1 1 calc R . .
C7 C 0.29834(11) -0.16695(15) -0.03847(11) 0.0213(3) Uani 1 1 d . . .
C1 C 0.09917(11) -0.27524(17) 0.08596(12) 0.0260(3) Uani 1 1 d . . .
H1 H 0.1175 -0.3716 0.0651 0.031 Uiso 1 1 calc R . .
C11 C 0.29997(11) 0.32839(16) 0.16741(12) 0.0245(3) Uani 1 1 d . . .
C3 C -0.02208(12) -0.11109(19) 0.14318(13) 0.0321(4) Uani 1 1 d . . .
H3 H -0.0890 -0.0938 0.1605 0.039 Uiso 1 1 calc R . .
C9 C 0.41292(12) -0.20419(19) -0.03765(13) 0.0341(4) Uani 1 1 d . . .
H9A H 0.4274 -0.1834 -0.1114 0.051 Uiso 1 1 calc R . .
H9B H 0.4257 -0.3095 -0.0199 0.051 Uiso 1 1 calc R . .
H9C H 0.4594 -0.1436 0.0189 0.051 Uiso 1 1 calc R . .
C8 C 0.22425(13) -0.25647(17) -0.12728(12) 0.0313(4) Uani 1 1 d . . .
H8A H 0.1510 -0.2330 -0.1251 0.047 Uiso 1 1 calc R . .
H8B H 0.2370 -0.3626 -0.1129 0.047 Uiso 1 1 calc R . .
H8C H 0.2369 -0.2316 -0.2012 0.047 Uiso 1 1 calc R . .
C4 C 0.04827(11) 0.00112(17) 0.15146(12) 0.0270(4) Uani 1 1 d . . .
H4 H 0.0307 0.0953 0.1772 0.032 Uiso 1 1 calc R . .
C12 C 0.39729(12) 0.26654(18) 0.24563(13) 0.0322(4) Uani 1 1 d . . .
H12A H 0.4569 0.3340 0.2478 0.048 Uiso 1 1 calc R . .
H12B H 0.4141 0.1690 0.2187 0.048 Uiso 1 1 calc R . .
H12C H 0.3837 0.2566 0.3209 0.048 Uiso 1 1 calc R . .
C13 C 0.32011(13) 0.35393(17) 0.05112(12) 0.0311(4) Uani 1 1 d . . .
H13A H 0.2560 0.3930 0.0021 0.047 Uiso 1 1 calc R . .
H13B H 0.3396 0.2598 0.0209 0.047 Uiso 1 1 calc R . .
H13C H 0.3777 0.4255 0.0554 0.047 Uiso 1 1 calc R . .
O1 O 0.28198(8) -0.01300(11) -0.06610(8) 0.0265(3) Uani 1 1 d . . .
H1A H 0.2687 0.0330 -0.0111 0.040 Uiso 1 1 calc R . .
O2 O 0.27426(9) 0.47162(11) 0.20504(8) 0.0321(3) Uani 1 1 d . . .
H2A H 0.2782 0.4691 0.2744 0.048 Uiso 1 1 calc R . .
C5 C 0.14932(11) -0.01820(15) 0.12231(11) 0.0211(3) Uani 1 1 d . . .


_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
N2 C5 1.2960(18) . ?
N2 C10 1.4551(17) . ?
N1 C1 1.3660(18) . ?
N1 C5 1.4019(18) . ?
N1 C6 1.4744(17) . ?
C10 C11 1.525(2) . ?
C6 C7 1.5323(18) . ?
C2 C1 1.352(2) . ?
C2 C3 1.411(2) . ?
C7 O1 1.4327(16) . ?
C7 C8 1.518(2) . ?
C7 C9 1.522(2) . ?
C11 O2 1.4339(17) . ?
C11 C12 1.516(2) . ?
C11 C13 1.5203(19) . ?
C3 C4 1.351(2) . ?
C4 C5 1.4422(19) . ?

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
C5 N2 C10 117.56(11) . . ?
C1 N1 C5 122.00(12) . . ?
C1 N1 C6 119.04(12) . . ?
C5 N1 C6 118.57(11) . . ?
N2 C10 C11 111.57(11) . . ?
N1 C6 C7 114.85(11) . . ?
C1 C2 C3 118.33(14) . . ?
O1 C7 C8 107.86(11) . . ?
O1 C7 C9 108.03(12) . . ?
C8 C7 C9 110.72(12) . . ?
O1 C7 C6 110.57(11) . . ?
C8 C7 C6 111.23(12) . . ?
C9 C7 C6 108.39(11) . . ?
C2 C1 N1 122.17(14) . . ?
O2 C11 C12 110.34(12) . . ?
O2 C11 C13 105.31(11) . . ?
C12 C11 C13 111.04(12) . . ?
O2 C11 C10 107.39(11) . . ?
C12 C11 C10 111.32(12) . . ?
C13 C11 C10 111.20(12) . . ?
C4 C3 C2 120.57(14) . . ?
C3 C4 C5 121.78(14) . . ?
N2 C5 N1 117.10(12) . . ?
N2 C5 C4 127.87(13) . . ?
N1 C5 C4 115.04(12) . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        25.00
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.199
_refine_diff_density_min         -0.167
_refine_diff_density_rms         0.034
####################################################################### 
# 
# 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_kyj40-1
_database_code_depnum_ccdc_archive 'CCDC 1497958'
_audit_update_record             
;
2016-08-06 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C19 H34 N2 O4 Ti'
_chemical_formula_weight         402.38

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           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                   10.1045(2)
_cell_length_b                   14.8386(3)
_cell_length_c                   14.7511(3)
_cell_angle_alpha                90
_cell_angle_beta                 103.9490(10)
_cell_angle_gamma                90
_cell_volume                     2146.51(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9924
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      30.59

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.423
_shelx_estimated_absorpt_T_min   0.920
_shelx_estimated_absorpt_T_max   0.959
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            25010
_diffrn_reflns_av_unetI/netI     0.0233
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         1.977
_diffrn_reflns_theta_max         30.689
_diffrn_reflns_theta_full        25.242
_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             6620
_reflns_number_gt                5490
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0419P)²+0.8343P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6620
_refine_ls_number_parameters     272
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0441
_refine_ls_R_factor_gt           0.0322
_refine_ls_wR_factor_ref         0.0876
_refine_ls_wR_factor_gt          0.0816
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_restrained_S_all      1.021
_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 0.71489(2) 0.24499(2) 0.07060(2) 0.01231(6) Uani 1 1 d . . . . .
N1 N 0.83094(10) 0.15251(6) 0.31557(6) 0.01523(18) Uani 1 1 d . . . . .
N2 N 0.64340(9) 0.19452(6) 0.19596(6) 0.01556(18) Uani 1 1 d . . . . .
O1 O 0.88379(8) 0.25438(6) 0.14740(6) 0.02191(18) Uani 1 1 d . . . . .
O2 O 0.53973(8) 0.29276(6) 0.05341(5) 0.01791(16) Uani 1 1 d . . . . .
O3 O 0.70610(10) 0.13570(6) 0.01536(7) 0.0266(2) Uani 1 1 d . . . . .
O4 O 0.75076(8) 0.32659(6) -0.01604(5) 0.01788(16) Uani 1 1 d . . . . .
C1 C 0.90013(12) 0.09115(8) 0.37918(8) 0.0193(2) Uani 1 1 d . . . . .
H1 H 0.9910 0.1043 0.4122 0.023 Uiso 1 1 calc R U . . .
C2 C 0.84300(13) 0.01256(8) 0.39637(8) 0.0213(2) Uani 1 1 d . . . . .
H2 H 0.8930 -0.0299 0.4395 0.026 Uiso 1 1 calc R U . . .
C3 C 0.70708(13) -0.00433(8) 0.34841(8) 0.0210(2) Uani 1 1 d . . . . .
H3 H 0.6634 -0.0581 0.3608 0.025 Uiso 1 1 calc R U . . .
C4 C 0.63773(12) 0.05543(8) 0.28464(8) 0.0195(2) Uani 1 1 d . . . . .
H4 H 0.5454 0.0432 0.2543 0.023 Uiso 1 1 calc R U . . .
C5 C 0.70020(11) 0.13654(7) 0.26189(7) 0.0151(2) Uani 1 1 d . . . . .
C6 C 0.89749(12) 0.23988(7) 0.31140(8) 0.0171(2) Uani 1 1 d . . . . .
H6A H 0.9611 0.2516 0.3727 0.021 Uiso 1 1 calc R U . . .
H6B H 0.8271 0.2877 0.3008 0.021 Uiso 1 1 calc R U . . .
C7 C 0.97652(12) 0.24654(8) 0.23514(8) 0.0184(2) Uani 1 1 d . . . . .
C8 C 1.06539(14) 0.33102(9) 0.25506(10) 0.0286(3) Uani 1 1 d . . . . .
H8A H 1.1082 0.3418 0.2031 0.043 Uiso 1 1 calc R U . . .
H8B H 1.1363 0.3225 0.3128 0.043 Uiso 1 1 calc R U . . .
H8C H 1.0087 0.3829 0.2621 0.043 Uiso 1 1 calc R U . . .
C9 C 1.06592(14) 0.16395(9) 0.23403(9) 0.0272(3) Uani 1 1 d . . . . .
H9A H 1.0082 0.1103 0.2193 0.041 Uiso 1 1 calc R U . . .
H9B H 1.1288 0.1566 0.2955 0.041 Uiso 1 1 calc R U . . .
H9C H 1.1182 0.1719 0.1866 0.041 Uiso 1 1 calc R U . . .
C10 C 0.49531(12) 0.18518(8) 0.15921(8) 0.0184(2) Uani 1 1 d . . . . .
H10A H 0.4500 0.1747 0.2108 0.022 Uiso 1 1 calc R U . . .
H10B H 0.4747 0.1338 0.1152 0.022 Uiso 1 1 calc R U . . .
C11 C 0.44590(12) 0.27346(8) 0.10906(8) 0.0182(2) Uani 1 1 d . . . . .
C12 C 0.44773(14) 0.34977(9) 0.17832(9) 0.0264(3) Uani 1 1 d . . . . .
H12A H 0.5393 0.3551 0.2196 0.040 Uiso 1 1 calc R U . . .
H12B H 0.3819 0.3369 0.2157 0.040 Uiso 1 1 calc R U . . .
H12C H 0.4232 0.4064 0.1443 0.040 Uiso 1 1 calc R U . . .
C13 C 0.30362(12) 0.26255(10) 0.04527(10) 0.0272(3) Uani 1 1 d . . . . .
H13A H 0.2737 0.3201 0.0145 0.041 Uiso 1 1 calc R U . . .
H13B H 0.2399 0.2439 0.0824 0.041 Uiso 1 1 calc R U . . .
H13C H 0.3058 0.2166 -0.0021 0.041 Uiso 1 1 calc R U . . .
C14 C 0.7996(2) 0.06053(11) 0.01864(12) 0.0293(5) Uani 0.810(4) 1 d . . P A 1
H14 H 0.8946 0.0827 0.0451 0.035 Uiso 0.810(4) 1 calc R U P A 1
C15 C 0.7910(3) 0.02560(17) -0.07839(17) 0.0337(5) Uani 0.810(4) 1 d . . P A 1
H15A H 0.6965 0.0089 -0.1077 0.051 Uiso 0.810(4) 1 calc R U P A 1
H15B H 0.8498 -0.0274 -0.0751 0.051 Uiso 0.810(4) 1 calc R U P A 1
H15C H 0.8210 0.0726 -0.1156 0.051 Uiso 0.810(4) 1 calc R U P A 1
C16 C 0.7690(4) -0.01155(16) 0.08165(18) 0.0537(8) Uani 0.810(4) 1 d . . P A 1
H16A H 0.7864 0.0115 0.1457 0.081 Uiso 0.810(4) 1 calc R U P A 1
H16B H 0.8275 -0.0639 0.0799 0.081 Uiso 0.810(4) 1 calc R U P A 1
H16C H 0.6731 -0.0294 0.0606 0.081 Uiso 0.810(4) 1 calc R U P A 1
C14A C 0.6963(10) 0.0484(5) -0.0097(6) 0.033(2) Uani 0.190(4) 1 d . . P A 2
H14A H 0.6171 0.0414 -0.0649 0.040 Uiso 0.190(4) 1 calc R U P A 2
C15A C 0.8217(17) 0.0340(10) -0.0406(9) 0.057(4) Uani 0.190(4) 1 d . . P A 2
C16A C 0.6750(15) -0.0127(5) 0.0664(7) 0.042(3) Uani 0.190(4) 1 d . . P A 2
H16D H 0.7444 -0.0002 0.1240 0.063 Uiso 0.190(4) 1 calc R U P A 2
H16E H 0.6826 -0.0755 0.0480 0.063 Uiso 0.190(4) 1 calc R U P A 2
H16F H 0.5842 -0.0022 0.0770 0.063 Uiso 0.190(4) 1 calc R U P A 2
C17 C 0.87678(12) 0.35637(8) -0.03234(8) 0.0188(2) Uani 1 1 d . . . . .
H17 H 0.9428 0.3650 0.0295 0.023 Uiso 1 1 calc R U . . .
C18 C 0.93414(13) 0.28522(10) -0.08644(9) 0.0271(3) Uani 1 1 d . . . . .
H18A H 0.9495 0.2292 -0.0502 0.041 Uiso 1 1 calc R U . . .
H18B H 1.0207 0.3065 -0.0976 0.041 Uiso 1 1 calc R U . . .
H18C H 0.8692 0.2741 -0.1464 0.041 Uiso 1 1 calc R U . . .
C19 C 0.85649(14) 0.44669(9) -0.08256(9) 0.0253(3) Uani 1 1 d . . . . .
H19A H 0.7988 0.4385 -0.1457 0.038 Uiso 1 1 calc R U . . .
H19B H 0.9452 0.4709 -0.0864 0.038 Uiso 1 1 calc R U . . .
H19C H 0.8124 0.4889 -0.0479 0.038 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 O3 1.8074(9) . ?
Ti1 O1 1.8119(8) . ?
Ti1 O4 1.8586(8) . ?
Ti1 O2 1.8663(8) . ?
Ti1 N2 2.2685(9) . ?
N1 C1 1.3719(14) . ?
N1 C5 1.3871(14) . ?
N1 C6 1.4685(14) . ?
N2 C5 1.3215(13) . ?
N2 C10 1.4701(14) . ?
O1 C7 1.4078(13) . ?
O2 C11 1.4247(13) . ?
O3 C14A 1.344(7) . ?
O3 C14 1.4553(19) . ?
O4 C17 1.4220(13) . ?
C1 C2 1.3520(17) . ?
C2 C3 1.4076(18) . ?
C3 C4 1.3582(16) . ?
C4 C5 1.4358(15) . ?
C6 C7 1.5317(16) . ?
C7 C9 1.5249(18) . ?
C7 C8 1.5287(17) . ?
C10 C11 1.5279(16) . ?
C11 C12 1.5224(18) . ?
C11 C13 1.5252(17) . ?
C14 C16 1.497(3) . ?
C14 C15 1.505(3) . ?
C14A C15A 1.461(18) . ?
C14A C16A 1.498(11) . ?
C17 C18 1.5200(18) . ?
C17 C19 1.5211(17) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O3 Ti1 O1 106.71(4) . . ?
O3 Ti1 O4 105.73(4) . . ?
O1 Ti1 O4 93.98(4) . . ?
O3 Ti1 O2 109.73(4) . . ?
O1 Ti1 O2 140.83(4) . . ?
O4 Ti1 O2 89.70(4) . . ?
O3 Ti1 N2 94.63(4) . . ?
O1 Ti1 N2 87.29(4) . . ?
O4 Ti1 N2 158.25(4) . . ?
O2 Ti1 N2 76.01(3) . . ?
C1 N1 C5 122.36(10) . . ?
C1 N1 C6 116.84(9) . . ?
C5 N1 C6 120.64(9) . . ?
C5 N2 C10 115.65(9) . . ?
C5 N2 Ti1 130.37(7) . . ?
C10 N2 Ti1 103.09(6) . . ?
C7 O1 Ti1 152.41(8) . . ?
C11 O2 Ti1 125.90(7) . . ?
C14A O3 Ti1 168.8(3) . . ?
C14 O3 Ti1 135.37(10) . . ?
C17 O4 Ti1 130.52(7) . . ?
C2 C1 N1 122.04(11) . . ?
C1 C2 C3 117.93(11) . . ?
C4 C3 C2 120.65(11) . . ?
C3 C4 C5 121.79(11) . . ?
N2 C5 N1 119.58(10) . . ?
N2 C5 C4 125.48(10) . . ?
N1 C5 C4 114.94(9) . . ?
N1 C6 C7 114.38(9) . . ?
O1 C7 C9 108.74(10) . . ?
O1 C7 C8 109.81(9) . . ?
C9 C7 C8 109.81(11) . . ?
O1 C7 C6 109.35(9) . . ?
C9 C7 C6 111.78(10) . . ?
C8 C7 C6 107.33(10) . . ?
N2 C10 C11 106.41(9) . . ?
O2 C11 C12 109.58(10) . . ?
O2 C11 C13 108.97(9) . . ?
C12 C11 C13 110.49(10) . . ?
O2 C11 C10 105.44(9) . . ?
C12 C11 C10 111.29(10) . . ?
C13 C11 C10 110.93(10) . . ?
O3 C14 C16 109.77(17) . . ?
O3 C14 C15 110.11(16) . . ?
C16 C14 C15 111.78(18) . . ?
O3 C14A C15A 102.4(8) . . ?
O3 C14A C16A 113.0(6) . . ?
C15A C14A C16A 115.9(9) . . ?
O4 C17 C18 110.08(10) . . ?
O4 C17 C19 109.58(10) . . ?
C18 C17 C19 112.33(10) . . ?

_refine_diff_density_max         0.375
_refine_diff_density_min         -0.423
_refine_diff_density_rms         0.052

_shelxl_version_number           2014-3

####################################################################### 
# 
# 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_kyj35-2
_database_code_depnum_ccdc_archive 'CCDC 1497959'
_audit_update_record             
;
2016-08-06 deposited with the CCDC.
2016-10-07 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C28 H42 Cl6 N4 O6 Ti2'
_chemical_formula_weight         839.15

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'
Cl Cl 0.1484 0.1585 '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                   9.5970(3)
_cell_length_b                   19.6755(6)
_cell_length_c                   9.9008(3)
_cell_angle_alpha                90
_cell_angle_beta                 105.588(2)
_cell_angle_gamma                90
_cell_volume                     1800.76(10)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    9959
_cell_measurement_theta_min      2.37
_cell_measurement_theta_max      26.43

_exptl_crystal_description       block
_exptl_crystal_colour            ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_F_000             864
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_absorpt_coefficient_mu    0.934
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            31380
_diffrn_reflns_av_unetI/netI     0.0224
_diffrn_reflns_av_R_equivalents  0.0297
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.070
_diffrn_reflns_theta_max         26.573
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             3738
_reflns_number_gt                3145
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_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)+(0.0436P)²+3.6450P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3738
_refine_ls_number_parameters     212
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0396
_refine_ls_wR_factor_ref         0.1022
_refine_ls_wR_factor_gt          0.0955
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_restrained_S_all      1.030
_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 0.95809(4) 0.08047(2) 0.49266(4) 0.01006(12) Uani 1 1 d . . . . .
N1 N 0.8292(2) 0.20578(10) 0.2189(2) 0.0139(4) Uani 1 1 d . . . . .
N2 N 1.0176(2) 0.13131(10) 0.3238(2) 0.0118(4) Uani 1 1 d . . . . .
O1 O 0.77350(17) 0.11537(8) 0.42886(18) 0.0132(4) Uani 1 1 d . . . . .
O2 O 1.08900(17) 0.00992(8) 0.43469(17) 0.0114(3) Uani 1 1 d . . . . .
O3 O 1.04836(18) 0.12707(8) 0.62825(18) 0.0162(4) Uani 1 1 d . . . . .
C1 C 0.7407(3) 0.23712(13) 0.1032(3) 0.0186(5) Uani 1 1 d . . . . .
H1 H 0.6701 0.2671 0.1154 0.022 Uiso 1 1 calc R U . . .
C2 C 0.7531(3) 0.22558(13) -0.0276(3) 0.0214(6) Uani 1 1 d . . . . .
H2 H 0.6920 0.2470 -0.1048 0.026 Uiso 1 1 calc R U . . .
C3 C 0.8603(3) 0.18061(13) -0.0441(3) 0.0201(5) Uani 1 1 d . . . . .
H3 H 0.8703 0.1716 -0.1333 0.024 Uiso 1 1 calc R U . . .
C4 C 0.9499(3) 0.14995(12) 0.0696(3) 0.0167(5) Uani 1 1 d . . . . .
H4 H 1.0224 0.1213 0.0567 0.020 Uiso 1 1 calc R U . . .
C5 C 0.9361(2) 0.16042(11) 0.2083(3) 0.0125(5) Uani 1 1 d . . . . .
C6 C 0.8144(3) 0.22746(12) 0.3573(3) 0.0145(5) Uani 1 1 d . . . . .
H6A H 0.7762 0.2734 0.3492 0.017 Uiso 1 1 calc R U . . .
H6B H 0.9097 0.2286 0.4231 0.017 Uiso 1 1 calc R U . . .
C7 C 0.7164(3) 0.18180(12) 0.4173(3) 0.0143(5) Uani 1 1 d . . . . .
C8 C 0.5622(3) 0.17913(14) 0.3219(3) 0.0219(6) Uani 1 1 d . . . . .
H8A H 0.5635 0.1608 0.2323 0.033 Uiso 1 1 calc R U . . .
H8B H 0.5223 0.2242 0.3097 0.033 Uiso 1 1 calc R U . . .
H8C H 0.5039 0.1507 0.3636 0.033 Uiso 1 1 calc R U . . .
C9 C 0.7177(3) 0.20945(13) 0.5615(3) 0.0208(6) Uani 1 1 d . . . . .
H9A H 0.6568 0.1818 0.6017 0.031 Uiso 1 1 calc R U . . .
H9B H 0.6824 0.2553 0.5523 0.031 Uiso 1 1 calc R U . . .
H9C H 0.8148 0.2087 0.6212 0.031 Uiso 1 1 calc R U . . .
C10 C 1.1593(2) 0.10401(12) 0.3208(3) 0.0132(5) Uani 1 1 d . . . . .
H10A H 1.2333 0.1225 0.3990 0.016 Uiso 1 1 calc R U . . .
H10B H 1.1810 0.1182 0.2349 0.016 Uiso 1 1 calc R U . . .
C11 C 1.1625(3) 0.02613(12) 0.3294(3) 0.0139(5) Uani 1 1 d . . . . .
C12 C 1.0814(3) -0.00719(13) 0.1921(3) 0.0223(6) Uani 1 1 d . . . . .
H12A H 1.0777 -0.0554 0.2053 0.033 Uiso 1 1 calc R U . . .
H12B H 1.1306 0.0022 0.1216 0.033 Uiso 1 1 calc R U . . .
H12C H 0.9848 0.0106 0.1629 0.033 Uiso 1 1 calc R U . . .
C13 C 1.3186(3) 0.00238(14) 0.3774(3) 0.0237(6) Uani 1 1 d . . . . .
H13A H 1.3632 0.0205 0.4688 0.036 Uiso 1 1 calc R U . . .
H13B H 1.3700 0.0180 0.3125 0.036 Uiso 1 1 calc R U . . .
H13C H 1.3212 -0.0464 0.3813 0.036 Uiso 1 1 calc R U . . .
C14 C 0.3243(3) 0.07708(14) 0.8296(3) 0.0233(6) Uani 1 1 d . . . . .
H14 H 0.2364 0.0972 0.7684 0.028 Uiso 1 1 calc R U . . .
Cl1 Cl 0.47398(11) 0.11608(5) 0.79143(13) 0.0582(3) Uani 1 1 d . . . . .
Cl2 Cl 0.32483(10) 0.09339(5) 1.00375(8) 0.0409(2) Uani 1 1 d . . . . .
Cl3 Cl 0.32334(9) -0.00929(4) 0.79257(11) 0.0433(2) Uani 1 1 d . . . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O3 1.6638(17) . ?
Ti1 O1 1.8459(17) . ?
Ti1 O2 2.0147(16) 3_756 ?
Ti1 O2 2.0549(16) . ?
Ti1 N2 2.153(2) . ?
Ti1 Ti1 3.2609(8) 3_756 ?
N1 C1 1.375(3) . ?
N1 C5 1.385(3) . ?
N1 C6 1.478(3) . ?
N2 C5 1.329(3) . ?
N2 C10 1.470(3) . ?
O1 C7 1.410(3) . ?
O2 C11 1.443(3) . ?
O2 Ti1 2.0148(16) 3_756 ?
C1 C2 1.352(4) . ?
C2 C3 1.399(4) . ?
C3 C4 1.360(4) . ?
C4 C5 1.430(3) . ?
C6 C7 1.531(3) . ?
C7 C9 1.525(4) . ?
C7 C8 1.528(3) . ?
C10 C11 1.535(3) . ?
C11 C13 1.518(3) . ?
C11 C12 1.521(4) . ?
C14 Cl3 1.738(3) . ?
C14 Cl2 1.753(3) . ?
C14 Cl1 1.757(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
O3 Ti1 O1 108.35(8) . . ?
O3 Ti1 O2 108.45(8) . 3_756 ?
O1 Ti1 O2 99.43(7) . 3_756 ?
O3 Ti1 O2 111.88(8) . . ?
O1 Ti1 O2 139.32(7) . . ?
O2 Ti1 O2 73.50(7) 3_756 . ?
O3 Ti1 N2 100.45(8) . . ?
O1 Ti1 N2 89.54(7) . . ?
O2 Ti1 N2 144.99(7) 3_756 . ?
O2 Ti1 N2 77.71(7) . . ?
O3 Ti1 Ti1 115.49(6) . 3_756 ?
O1 Ti1 Ti1 125.39(5) . 3_756 ?
O2 Ti1 Ti1 37.17(4) 3_756 3_756 ?
O2 Ti1 Ti1 36.33(4) . 3_756 ?
N2 Ti1 Ti1 111.84(6) . 3_756 ?
C1 N1 C5 122.0(2) . . ?
C1 N1 C6 116.8(2) . . ?
C5 N1 C6 120.9(2) . . ?
C5 N2 C10 118.3(2) . . ?
C5 N2 Ti1 130.60(16) . . ?
C10 N2 Ti1 106.60(14) . . ?
C7 O1 Ti1 133.55(15) . . ?
C11 O2 Ti1 130.79(14) . 3_756 ?
C11 O2 Ti1 120.45(13) . . ?
Ti1 O2 Ti1 106.50(7) 3_756 . ?
C2 C1 N1 121.9(2) . . ?
C1 C2 C3 118.4(2) . . ?
C4 C3 C2 120.3(2) . . ?
C3 C4 C5 122.0(2) . . ?
N2 C5 N1 119.3(2) . . ?
N2 C5 C4 125.4(2) . . ?
N1 C5 C4 115.3(2) . . ?
N1 C6 C7 114.3(2) . . ?
O1 C7 C9 110.4(2) . . ?
O1 C7 C8 108.0(2) . . ?
C9 C7 C8 110.7(2) . . ?
O1 C7 C6 108.04(19) . . ?
C9 C7 C6 107.6(2) . . ?
C8 C7 C6 112.0(2) . . ?
N2 C10 C11 111.63(19) . . ?
O2 C11 C13 109.8(2) . . ?
O2 C11 C12 108.6(2) . . ?
C13 C11 C12 111.8(2) . . ?
O2 C11 C10 104.74(18) . . ?
C13 C11 C10 109.1(2) . . ?
C12 C11 C10 112.5(2) . . ?
Cl3 C14 Cl2 112.64(17) . . ?
Cl3 C14 Cl1 109.88(15) . . ?
Cl2 C14 Cl1 110.19(15) . . ?

_refine_diff_density_max         1.137
_refine_diff_density_min         -1.010
_refine_diff_density_rms         0.079

_shelxl_version_number           2014-3

