# Electronic Supplementary Material (ESI) for New Journal of Chemistry.
# This journal is © The Royal Society of Chemistry and the Centre National de la Recherche Scientifique 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_Ti3
_database_code_depnum_ccdc_archive 'CCDC 1422869'

_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_publcif_datablock.id            {35068966-66c2-4a79-ab60-a9f99ebbb317}
# publcif _publ_body_element loop end

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Ti3
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C42 H64 N2 O7 Ti2'
_chemical_formula_sum            'C42 H64 N2 O7 Ti2'
_chemical_formula_weight         804.75

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'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P2(1)/c
_symmetry_space_group_name_Hall  '-P 2ybc'

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                   14.9452(5)
_cell_length_b                   18.7424(6)
_cell_length_c                   18.6507(5)
_cell_angle_alpha                90.00
_cell_angle_beta                 107.1600(10)
_cell_angle_gamma                90.00
_cell_volume                     4991.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7231
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      22.76

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.071
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1720
_exptl_absorpt_coefficient_mu    0.361
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9151
_exptl_absorpt_correction_T_max  0.9648
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(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 APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            32072
_diffrn_reflns_av_R_equivalents  0.0328
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         1.58
_diffrn_reflns_theta_max         24.43
_reflns_number_total             8217
_reflns_number_gt                5563
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0733P)²+0.3215P] 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     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         8217
_refine_ls_number_parameters     482
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0459
_refine_ls_wR_factor_ref         0.1347
_refine_ls_wR_factor_gt          0.1243
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_restrained_S_all      1.029
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
H2 H 0.3721(15) 0.5231(12) 0.9781(12) 0.035(6) Uiso 1 1 d . . .
Ti1 Ti 0.21953(3) 0.42697(2) 0.65057(2) 0.04248(15) Uani 1 1 d . . .
Ti2 Ti 0.38766(3) 0.43145(2) 0.78856(2) 0.04015(15) Uani 1 1 d . . .
O3 O 0.30394(11) 0.50697(9) 0.73473(8) 0.0451(4) Uani 1 1 d . . .
N2 N 0.37407(13) 0.50067(11) 0.87785(11) 0.0408(5) Uani 1 1 d . . .
N1 N 0.12618(15) 0.51351(12) 0.59339(11) 0.0472(5) Uani 1 1 d . . .
O4 O 0.32115(12) 0.37578(9) 0.71540(8) 0.0463(5) Uani 1 1 d . . .
C12 C 0.01610(18) 0.43573(14) 0.76975(14) 0.0472(7) Uani 1 1 d . . .
O6 O 0.41328(12) 0.36466(9) 0.86732(8) 0.0472(5) Uani 1 1 d . . .
O2 O 0.27963(12) 0.46172(10) 0.58364(9) 0.0518(5) Uani 1 1 d . . .
O7 O 0.15992(13) 0.35225(10) 0.59563(9) 0.0540(5) Uani 1 1 d . . .
O1 O 0.13557(12) 0.42957(9) 0.70992(9) 0.0491(5) Uani 1 1 d . . .
C26 C 0.39967(17) 0.41557(14) 0.97961(13) 0.0419(6) Uani 1 1 d . . .
C31 C 0.41414(16) 0.35630(14) 0.93890(12) 0.0396(6) Uani 1 1 d . . .
C24 C 0.35322(18) 0.57316(13) 0.84859(14) 0.0445(6) Uani 1 1 d . . .
H24 H 0.4091 0.5906 0.8369 0.053 Uiso 1 1 calc R . .
C8 C 0.02397(18) 0.52190(14) 0.67310(14) 0.0476(7) Uani 1 1 d . . .
C25 C 0.38107(18) 0.48550(15) 0.94648(15) 0.0447(7) Uani 1 1 d . . .
C30 C 0.42942(17) 0.28778(14) 0.97205(13) 0.0431(6) Uani 1 1 d . . .
C19 C 0.27638(19) 0.56429(13) 0.77359(15) 0.0493(7) Uani 1 1 d . . .
H19 H 0.2179 0.5512 0.7839 0.059 Uiso 1 1 calc R . .
C13 C 0.06019(18) 0.46191(14) 0.71712(13) 0.0450(6) Uani 1 1 d . . .
C27 C 0.40189(18) 0.40664(16) 1.05517(14) 0.0503(7) Uani 1 1 d . . .
H27 H 0.3935 0.4462 1.0826 0.060 Uiso 1 1 calc R . .
O5 O 0.49912(13) 0.44995(11) 0.77531(10) 0.0582(5) Uani 1 1 d . . .
C28 C 0.4161(2) 0.34139(16) 1.08891(14) 0.0528(7) Uani 1 1 d . . .
C14 C 0.0518(2) 0.36791(16) 0.81443(16) 0.0605(8) Uani 1 1 d . . .
C29 C 0.42963(19) 0.28361(15) 1.04623(14) 0.0511(7) Uani 1 1 d . . .
H29 H 0.4395 0.2391 1.0692 0.061 Uiso 1 1 calc R . .
C6 C 0.1513(2) 0.53550(16) 0.52576(15) 0.0562(8) Uani 1 1 d . . .
H6 H 0.1251 0.4991 0.4876 0.067 Uiso 1 1 calc R . .
C2 C 0.2908(2) 0.53612(17) 0.47923(15) 0.0664(9) Uani 1 1 d . . .
H2A H 0.2667 0.4979 0.4437 0.080 Uiso 1 1 calc R . .
H2B H 0.3586 0.5337 0.4946 0.080 Uiso 1 1 calc R . .
C7 C 0.05909(19) 0.54365(15) 0.61187(15) 0.0529(7) Uani 1 1 d . . .
H7 H 0.0306 0.5828 0.5836 0.063 Uiso 1 1 calc R . .
C9 C -0.0527(2) 0.55854(16) 0.68436(17) 0.0637(8) Uani 1 1 d . . .
H9 H -0.0754 0.5990 0.6560 0.076 Uiso 1 1 calc R . .
C1 C 0.2559(2) 0.52699(16) 0.54665(15) 0.0582(8) Uani 1 1 d . . .
H1 H 0.2839 0.5649 0.5824 0.070 Uiso 1 1 calc R . .
C5 C 0.1164(2) 0.60675(17) 0.48939(16) 0.0657(9) Uani 1 1 d . . .
H5A H 0.1368 0.6449 0.5257 0.079 Uiso 1 1 calc R . .
H5B H 0.0485 0.6069 0.4719 0.079 Uiso 1 1 calc R . .
C20 C 0.2616(2) 0.63434(15) 0.73111(16) 0.0644(8) Uani 1 1 d . . .
H20A H 0.2125 0.6289 0.6840 0.077 Uiso 1 1 calc R . .
H20B H 0.3187 0.6479 0.7200 0.077 Uiso 1 1 calc R . .
C32 C 0.4463(2) 0.22278(15) 0.92809(15) 0.0570(8) Uani 1 1 d . . .
C11 C -0.0598(2) 0.47383(18) 0.77644(16) 0.0650(9) Uani 1 1 d . . .
H11 H -0.0902 0.4572 0.8101 0.078 Uiso 1 1 calc R . .
C36 C 0.4185(3) 0.33112(18) 1.17041(15) 0.0771(10) Uani 1 1 d . . .
H36A H 0.4291 0.2817 1.1837 0.116 Uiso 1 1 calc R . .
H36B H 0.3598 0.3458 1.1768 0.116 Uiso 1 1 calc R . .
H36C H 0.4681 0.3593 1.2022 0.116 Uiso 1 1 calc R . .
C23 C 0.3269(2) 0.62928(14) 0.89744(15) 0.0595(8) Uani 1 1 d . . .
H23A H 0.3776 0.6351 0.9436 0.071 Uiso 1 1 calc R . .
H23B H 0.2716 0.6141 0.9104 0.071 Uiso 1 1 calc R . .
C22 C 0.3076(3) 0.70020(16) 0.85557(17) 0.0761(10) Uani 1 1 d . . .
H22A H 0.3654 0.7184 0.8489 0.091 Uiso 1 1 calc R . .
H22B H 0.2854 0.7345 0.8853 0.091 Uiso 1 1 calc R . .
C21 C 0.2343(3) 0.69224(17) 0.77839(18) 0.0825(10) Uani 1 1 d . . .
H21A H 0.1742 0.6804 0.7853 0.099 Uiso 1 1 calc R . .
H21B H 0.2278 0.7374 0.7519 0.099 Uiso 1 1 calc R . .
C3 C 0.2589(3) 0.6078(2) 0.44197(19) 0.0849(11) Uani 1 1 d . . .
H3A H 0.2905 0.6457 0.4753 0.102 Uiso 1 1 calc R . .
H3B H 0.2771 0.6111 0.3963 0.102 Uiso 1 1 calc R . .
C4 C 0.1556(3) 0.61838(19) 0.42342(17) 0.0794(10) Uani 1 1 d . . .
H4A H 0.1246 0.5857 0.3834 0.095 Uiso 1 1 calc R . .
H4B H 0.1406 0.6665 0.4047 0.095 Uiso 1 1 calc R . .
C10 C -0.0944(2) 0.53599(19) 0.73595(18) 0.0701(9) Uani 1 1 d . . .
C34 C 0.3611(2) 0.21094(17) 0.85776(16) 0.0732(9) Uani 1 1 d . . .
H34A H 0.3723 0.1701 0.8306 0.110 Uiso 1 1 calc R . .
H34B H 0.3524 0.2523 0.8261 0.110 Uiso 1 1 calc R . .
H34C H 0.3059 0.2031 0.8730 0.110 Uiso 1 1 calc R . .
C16 C 0.1547(2) 0.37841(19) 0.86345(17) 0.0774(10) Uani 1 1 d . . .
H16A H 0.1766 0.3356 0.8914 0.116 Uiso 1 1 calc R . .
H16B H 0.1579 0.4174 0.8975 0.116 Uiso 1 1 calc R . .
H16C H 0.1933 0.3887 0.8317 0.116 Uiso 1 1 calc R . .
C33 C 0.4602(3) 0.15446(17) 0.97604(18) 0.0891(12) Uani 1 1 d . . .
H33A H 0.4705 0.1147 0.9469 0.134 Uiso 1 1 calc R . .
H33B H 0.4054 0.1458 0.9915 0.134 Uiso 1 1 calc R . .
H33C H 0.5135 0.1602 1.0195 0.134 Uiso 1 1 calc R . .
C40 C 0.5485(3) 0.4437(2) 0.7226(2) 0.0998(13) Uani 1 1 d . . .
H40 H 0.6124 0.4570 0.7514 0.120 Uiso 1 1 calc R . .
C37 C 0.1957(3) 0.29786(17) 0.55888(18) 0.0753(9) Uani 1 1 d . . .
H37 H 0.2641 0.2994 0.5795 0.090 Uiso 1 1 calc R . .
C35 C 0.5346(2) 0.23382(18) 0.90399(18) 0.0782(10) Uani 1 1 d . . .
H35A H 0.5447 0.1928 0.8765 0.117 Uiso 1 1 calc R . .
H35B H 0.5875 0.2401 0.9476 0.117 Uiso 1 1 calc R . .
H35C H 0.5272 0.2754 0.8727 0.117 Uiso 1 1 calc R . .
C17 C 0.0452(3) 0.30510(17) 0.76103(19) 0.0847(11) Uani 1 1 d . . .
H17A H 0.0678 0.2627 0.7895 0.127 Uiso 1 1 calc R . .
H17B H 0.0826 0.3148 0.7282 0.127 Uiso 1 1 calc R . .
H17C H -0.0188 0.2983 0.7318 0.127 Uiso 1 1 calc R . .
C39 C 0.1740(3) 0.3125(2) 0.47874(19) 0.1113(15) Uani 1 1 d . . .
H39A H 0.1987 0.2750 0.4551 0.167 Uiso 1 1 calc R . .
H39B H 0.2017 0.3571 0.4715 0.167 Uiso 1 1 calc R . .
H39C H 0.1073 0.3151 0.4569 0.167 Uiso 1 1 calc R . .
C15 C -0.0066(3) 0.3488(2) 0.8669(2) 0.0955(13) Uani 1 1 d . . .
H15A H 0.0178 0.3061 0.8942 0.143 Uiso 1 1 calc R . .
H15B H -0.0706 0.3411 0.8379 0.143 Uiso 1 1 calc R . .
H15C H -0.0037 0.3872 0.9016 0.143 Uiso 1 1 calc R . .
C18 C -0.1781(3) 0.5747(2) 0.7481(2) 0.1235(17) Uani 1 1 d . . .
H18A H -0.1975 0.5510 0.7866 0.185 Uiso 1 1 calc R . .
H18B H -0.2287 0.5746 0.7023 0.185 Uiso 1 1 calc R . .
H18C H -0.1610 0.6231 0.7631 0.185 Uiso 1 1 calc R . .
C42 C 0.5239(3) 0.4968(3) 0.6654(2) 0.1292(17) Uani 1 1 d . . .
H42A H 0.5598 0.4897 0.6309 0.194 Uiso 1 1 calc R . .
H42B H 0.5371 0.5432 0.6877 0.194 Uiso 1 1 calc R . .
H42C H 0.4584 0.4932 0.6390 0.194 Uiso 1 1 calc R . .
C41 C 0.5582(4) 0.3699(3) 0.7031(3) 0.156(2) Uani 1 1 d . . .
H41A H 0.5922 0.3676 0.6668 0.233 Uiso 1 1 calc R . .
H41B H 0.4973 0.3492 0.6823 0.233 Uiso 1 1 calc R . .
H41C H 0.5916 0.3440 0.7473 0.233 Uiso 1 1 calc R . .
C38 C 0.1657(4) 0.2270(2) 0.5785(3) 0.1262(17) Uani 1 1 d . . .
H38A H 0.1902 0.1904 0.5536 0.189 Uiso 1 1 calc R . .
H38B H 0.0985 0.2246 0.5628 0.189 Uiso 1 1 calc R . .
H38C H 0.1888 0.2201 0.6318 0.189 Uiso 1 1 calc R . .


_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 O7 1.8072(18) . ?
Ti1 O2 1.8576(17) . ?
Ti1 O4 1.8988(16) . ?
Ti1 O1 1.9031(17) . ?
Ti1 N1 2.199(2) . ?
Ti1 O3 2.2660(17) . ?
Ti1 Ti2 3.0213(6) . ?
Ti2 O4 1.7716(16) . ?
Ti2 O5 1.7885(19) . ?
Ti2 O6 1.8815(16) . ?
Ti2 O3 1.9585(17) . ?
Ti2 N2 2.167(2) . ?
O3 C19 1.423(3) . ?
N2 C25 1.285(3) . ?
N2 C24 1.463(3) . ?
N1 C7 1.283(3) . ?
N1 C6 1.477(3) . ?
C12 C11 1.377(4) . ?
C12 C13 1.421(4) . ?
C12 C14 1.527(4) . ?
O6 C31 1.340(3) . ?
O2 C1 1.398(3) . ?
O7 C37 1.419(4) . ?
O1 C13 1.321(3) . ?
C26 C31 1.398(3) . ?
C26 C27 1.410(3) . ?
C26 C25 1.441(4) . ?
C31 C30 1.414(3) . ?
C24 C23 1.517(4) . ?
C24 C19 1.535(3) . ?
C24 H24 0.9800 . ?
C8 C13 1.403(3) . ?
C8 C9 1.404(4) . ?
C8 C7 1.449(4) . ?
C25 H2 0.95(2) . ?
C30 C29 1.385(3) . ?
C30 C32 1.530(4) . ?
C19 C20 1.516(4) . ?
C19 H19 0.9800 . ?
C27 C28 1.363(4) . ?
C27 H27 0.9300 . ?
O5 C40 1.397(4) . ?
C28 C29 1.394(4) . ?
C28 C36 1.522(3) . ?
C14 C17 1.526(4) . ?
C14 C15 1.535(4) . ?
C14 C16 1.553(4) . ?
C29 H29 0.9300 . ?
C6 C1 1.503(4) . ?
C6 C5 1.519(4) . ?
C6 H6 0.9800 . ?
C2 C1 1.506(4) . ?
C2 C3 1.523(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C7 H7 0.9300 . ?
C9 C10 1.359(4) . ?
C9 H9 0.9300 . ?
C1 H1 0.9800 . ?
C5 C4 1.526(4) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C20 C21 1.528(4) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C32 C35 1.530(4) . ?
C32 C33 1.540(4) . ?
C32 C34 1.550(4) . ?
C11 C10 1.402(4) . ?
C11 H11 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C23 C22 1.525(4) . ?
C23 H23A 0.9700 . ?
C23 H23B 0.9700 . ?
C22 C21 1.537(4) . ?
C22 H22A 0.9700 . ?
C22 H22B 0.9700 . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C3 C4 1.493(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C10 C18 1.520(4) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C33 H33A 0.9600 . ?
C33 H33B 0.9600 . ?
C33 H33C 0.9600 . ?
C40 C42 1.427(5) . ?
C40 C41 1.448(5) . ?
C40 H40 0.9800 . ?
C37 C39 1.459(4) . ?
C37 C38 1.482(5) . ?
C37 H37 0.9800 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C15 H15A 0.9600 . ?
C15 H15B 0.9600 . ?
C15 H15C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?

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
O7 Ti1 O2 98.39(8) . . ?
O7 Ti1 O4 97.89(8) . . ?
O2 Ti1 O4 98.66(8) . . ?
O7 Ti1 O1 92.88(8) . . ?
O2 Ti1 O1 156.12(8) . . ?
O4 Ti1 O1 100.56(7) . . ?
O7 Ti1 N1 99.24(8) . . ?
O2 Ti1 N1 77.23(8) . . ?
O4 Ti1 N1 162.79(8) . . ?
O1 Ti1 N1 80.23(8) . . ?
O7 Ti1 O3 170.41(7) . . ?
O2 Ti1 O3 87.29(7) . . ?
O4 Ti1 O3 73.51(7) . . ?
O1 Ti1 O3 84.72(7) . . ?
N1 Ti1 O3 89.53(7) . . ?
O7 Ti1 Ti2 130.65(6) . . ?
O2 Ti1 Ti2 96.73(6) . . ?
O4 Ti1 Ti2 33.25(5) . . ?
O1 Ti1 Ti2 91.68(5) . . ?
N1 Ti1 Ti2 129.92(6) . . ?
O3 Ti1 Ti2 40.40(4) . . ?
O4 Ti2 O5 109.98(9) . . ?
O4 Ti2 O6 98.52(8) . . ?
O5 Ti2 O6 104.69(8) . . ?
O4 Ti2 O3 84.40(7) . . ?
O5 Ti2 O3 105.62(8) . . ?
O6 Ti2 O3 146.42(8) . . ?
O4 Ti2 N2 141.80(8) . . ?
O5 Ti2 N2 107.00(8) . . ?
O6 Ti2 N2 80.91(7) . . ?
O3 Ti2 N2 76.74(7) . . ?
O4 Ti2 Ti1 35.99(5) . . ?
O5 Ti2 Ti1 117.53(6) . . ?
O6 Ti2 Ti1 124.97(6) . . ?
O3 Ti2 Ti1 48.58(5) . . ?
N2 Ti2 Ti1 115.35(5) . . ?
C19 O3 Ti2 121.44(14) . . ?
C19 O3 Ti1 131.81(15) . . ?
Ti2 O3 Ti1 91.02(7) . . ?
C25 N2 C24 121.5(2) . . ?
C25 N2 Ti2 129.38(18) . . ?
C24 N2 Ti2 109.10(15) . . ?
C7 N1 C6 121.5(2) . . ?
C7 N1 Ti1 128.94(18) . . ?
C6 N1 Ti1 109.57(17) . . ?
Ti2 O4 Ti1 110.76(9) . . ?
C11 C12 C13 116.5(2) . . ?
C11 C12 C14 123.1(2) . . ?
C13 C12 C14 120.4(2) . . ?
C31 O6 Ti2 142.69(16) . . ?
C1 O2 Ti1 122.40(16) . . ?
C37 O7 Ti1 129.62(19) . . ?
C13 O1 Ti1 143.09(16) . . ?
C31 C26 C27 119.1(2) . . ?
C31 C26 C25 122.1(2) . . ?
C27 C26 C25 118.8(2) . . ?
O6 C31 C26 119.4(2) . . ?
O6 C31 C30 119.6(2) . . ?
C26 C31 C30 121.0(2) . . ?
N2 C24 C23 119.0(2) . . ?
N2 C24 C19 105.01(19) . . ?
C23 C24 C19 111.4(2) . . ?
N2 C24 H24 106.9 . . ?
C23 C24 H24 106.9 . . ?
C19 C24 H24 106.9 . . ?
C13 C8 C9 119.7(2) . . ?
C13 C8 C7 121.3(2) . . ?
C9 C8 C7 118.8(2) . . ?
N2 C25 C26 125.3(2) . . ?
N2 C25 H2 117.9(13) . . ?
C26 C25 H2 116.8(13) . . ?
C29 C30 C31 116.1(2) . . ?
C29 C30 C32 122.6(2) . . ?
C31 C30 C32 121.3(2) . . ?
O3 C19 C20 114.0(2) . . ?
O3 C19 C24 107.1(2) . . ?
C20 C19 C24 109.7(2) . . ?
O3 C19 H19 108.6 . . ?
C20 C19 H19 108.6 . . ?
C24 C19 H19 108.6 . . ?
O1 C13 C8 120.1(2) . . ?
O1 C13 C12 119.7(2) . . ?
C8 C13 C12 120.2(2) . . ?
C28 C27 C26 121.5(2) . . ?
C28 C27 H27 119.2 . . ?
C26 C27 H27 119.2 . . ?
C40 O5 Ti2 141.9(2) . . ?
C27 C28 C29 117.5(2) . . ?
C27 C28 C36 122.0(3) . . ?
C29 C28 C36 120.5(3) . . ?
C17 C14 C12 109.9(2) . . ?
C17 C14 C15 107.3(3) . . ?
C12 C14 C15 111.7(2) . . ?
C17 C14 C16 110.1(3) . . ?
C12 C14 C16 110.0(2) . . ?
C15 C14 C16 107.8(3) . . ?
C30 C29 C28 124.7(3) . . ?
C30 C29 H29 117.7 . . ?
C28 C29 H29 117.7 . . ?
N1 C6 C1 104.8(2) . . ?
N1 C6 C5 119.1(2) . . ?
C1 C6 C5 113.8(2) . . ?
N1 C6 H6 106.1 . . ?
C1 C6 H6 106.1 . . ?
C5 C6 H6 106.1 . . ?
C1 C2 C3 110.0(3) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
N1 C7 C8 125.5(2) . . ?
N1 C7 H7 117.2 . . ?
C8 C7 H7 117.2 . . ?
C10 C9 C8 121.3(3) . . ?
C10 C9 H9 119.4 . . ?
C8 C9 H9 119.4 . . ?
O2 C1 C6 108.3(2) . . ?
O2 C1 C2 114.3(3) . . ?
C6 C1 C2 111.2(2) . . ?
O2 C1 H1 107.6 . . ?
C6 C1 H1 107.6 . . ?
C2 C1 H1 107.6 . . ?
C6 C5 C4 108.8(3) . . ?
C6 C5 H5A 109.9 . . ?
C4 C5 H5A 109.9 . . ?
C6 C5 H5B 109.9 . . ?
C4 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
C19 C20 C21 109.6(3) . . ?
C19 C20 H20A 109.7 . . ?
C21 C20 H20A 109.7 . . ?
C19 C20 H20B 109.7 . . ?
C21 C20 H20B 109.7 . . ?
H20A C20 H20B 108.2 . . ?
C35 C32 C30 110.0(2) . . ?
C35 C32 C33 107.6(3) . . ?
C30 C32 C33 111.5(2) . . ?
C35 C32 C34 109.6(2) . . ?
C30 C32 C34 110.1(2) . . ?
C33 C32 C34 108.0(3) . . ?
C12 C11 C10 124.4(3) . . ?
C12 C11 H11 117.8 . . ?
C10 C11 H11 117.8 . . ?
C28 C36 H36A 109.5 . . ?
C28 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C28 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C24 C23 C22 109.9(2) . . ?
C24 C23 H23A 109.7 . . ?
C22 C23 H23A 109.7 . . ?
C24 C23 H23B 109.7 . . ?
C22 C23 H23B 109.7 . . ?
H23A C23 H23B 108.2 . . ?
C23 C22 C21 111.7(3) . . ?
C23 C22 H22A 109.3 . . ?
C21 C22 H22A 109.3 . . ?
C23 C22 H22B 109.3 . . ?
C21 C22 H22B 109.3 . . ?
H22A C22 H22B 107.9 . . ?
C20 C21 C22 111.8(3) . . ?
C20 C21 H21A 109.3 . . ?
C22 C21 H21A 109.3 . . ?
C20 C21 H21B 109.3 . . ?
C22 C21 H21B 109.3 . . ?
H21A C21 H21B 107.9 . . ?
C4 C3 C2 112.7(3) . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 114.2(3) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C9 C10 C11 117.8(3) . . ?
C9 C10 C18 121.8(3) . . ?
C11 C10 C18 120.4(3) . . ?
C32 C34 H34A 109.5 . . ?
C32 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C32 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C32 C33 H33A 109.5 . . ?
C32 C33 H33B 109.5 . . ?
H33A C33 H33B 109.5 . . ?
C32 C33 H33C 109.5 . . ?
H33A C33 H33C 109.5 . . ?
H33B C33 H33C 109.5 . . ?
O5 C40 C42 113.3(3) . . ?
O5 C40 C41 111.7(3) . . ?
C42 C40 C41 120.1(4) . . ?
O5 C40 H40 103.1 . . ?
C42 C40 H40 103.1 . . ?
C41 C40 H40 103.1 . . ?
O7 C37 C39 111.0(3) . . ?
O7 C37 C38 109.8(3) . . ?
C39 C37 C38 115.5(3) . . ?
O7 C37 H37 106.7 . . ?
C39 C37 H37 106.7 . . ?
C38 C37 H37 106.7 . . ?
C32 C35 H35A 109.5 . . ?
C32 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C32 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C14 C17 H17A 109.5 . . ?
C14 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C14 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C37 C39 H39A 109.5 . . ?
C37 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C37 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C10 C18 H18A 109.5 . . ?
C10 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C10 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C40 C42 H42A 109.5 . . ?
C40 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C40 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C40 C41 H41A 109.5 . . ?
C40 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C40 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C37 C38 H38A 109.5 . . ?
C37 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C37 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O7 Ti1 Ti2 O4 11.61(12) . . . . ?
O2 Ti1 Ti2 O4 -95.55(11) . . . . ?
O1 Ti1 Ti2 O4 106.85(11) . . . . ?
N1 Ti1 Ti2 O4 -174.50(12) . . . . ?
O3 Ti1 Ti2 O4 -173.31(12) . . . . ?
O7 Ti1 Ti2 O5 98.06(11) . . . . ?
O2 Ti1 Ti2 O5 -9.10(10) . . . . ?
O4 Ti1 Ti2 O5 86.45(12) . . . . ?
O1 Ti1 Ti2 O5 -166.70(9) . . . . ?
N1 Ti1 Ti2 O5 -88.05(11) . . . . ?
O3 Ti1 Ti2 O5 -86.86(10) . . . . ?
O7 Ti1 Ti2 O6 -37.46(10) . . . . ?
O2 Ti1 Ti2 O6 -144.61(9) . . . . ?
O4 Ti1 Ti2 O6 -49.07(12) . . . . ?
O1 Ti1 Ti2 O6 57.78(9) . . . . ?
N1 Ti1 Ti2 O6 136.43(10) . . . . ?
O3 Ti1 Ti2 O6 137.63(10) . . . . ?
O7 Ti1 Ti2 O3 -175.09(10) . . . . ?
O2 Ti1 Ti2 O3 77.76(9) . . . . ?
O4 Ti1 Ti2 O3 173.31(12) . . . . ?
O1 Ti1 Ti2 O3 -79.84(9) . . . . ?
N1 Ti1 Ti2 O3 -1.19(10) . . . . ?
O7 Ti1 Ti2 N2 -134.23(10) . . . . ?
O2 Ti1 Ti2 N2 118.61(9) . . . . ?
O4 Ti1 Ti2 N2 -145.84(12) . . . . ?
O1 Ti1 Ti2 N2 -38.99(8) . . . . ?
N1 Ti1 Ti2 N2 39.66(10) . . . . ?
O3 Ti1 Ti2 N2 40.85(9) . . . . ?
O4 Ti2 O3 C19 146.36(19) . . . . ?
O5 Ti2 O3 C19 -104.43(19) . . . . ?
O6 Ti2 O3 C19 49.4(2) . . . . ?
N2 Ti2 O3 C19 -0.19(18) . . . . ?
Ti1 Ti2 O3 C19 142.4(2) . . . . ?
O4 Ti2 O3 Ti1 3.95(7) . . . . ?
O5 Ti2 O3 Ti1 113.16(8) . . . . ?
O6 Ti2 O3 Ti1 -93.03(13) . . . . ?
N2 Ti2 O3 Ti1 -142.60(8) . . . . ?
O7 Ti1 O3 C19 -112.8(5) . . . . ?
O2 Ti1 O3 C19 120.6(2) . . . . ?
O4 Ti1 O3 C19 -139.5(2) . . . . ?
O1 Ti1 O3 C19 -36.9(2) . . . . ?
N1 Ti1 O3 C19 43.4(2) . . . . ?
Ti2 Ti1 O3 C19 -135.7(2) . . . . ?
O7 Ti1 O3 Ti2 23.0(5) . . . . ?
O2 Ti1 O3 Ti2 -103.68(8) . . . . ?
O4 Ti1 O3 Ti2 -3.82(7) . . . . ?
O1 Ti1 O3 Ti2 98.85(7) . . . . ?
N1 Ti1 O3 Ti2 179.08(7) . . . . ?
O4 Ti2 N2 C25 90.1(2) . . . . ?
O5 Ti2 N2 C25 -104.9(2) . . . . ?
O6 Ti2 N2 C25 -2.2(2) . . . . ?
O3 Ti2 N2 C25 152.6(2) . . . . ?
Ti1 Ti2 N2 C25 122.3(2) . . . . ?
O4 Ti2 N2 C24 -89.33(19) . . . . ?
O5 Ti2 N2 C24 75.73(16) . . . . ?
O6 Ti2 N2 C24 178.42(16) . . . . ?
O3 Ti2 N2 C24 -26.82(15) . . . . ?
Ti1 Ti2 N2 C24 -57.08(16) . . . . ?
O7 Ti1 N1 C7 97.4(2) . . . . ?
O2 Ti1 N1 C7 -166.0(3) . . . . ?
O4 Ti1 N1 C7 -88.1(4) . . . . ?
O1 Ti1 N1 C7 6.1(2) . . . . ?
O3 Ti1 N1 C7 -78.7(2) . . . . ?
Ti2 Ti1 N1 C7 -77.9(3) . . . . ?
O7 Ti1 N1 C6 -82.91(18) . . . . ?
O2 Ti1 N1 C6 13.67(17) . . . . ?
O4 Ti1 N1 C6 91.5(3) . . . . ?
O1 Ti1 N1 C6 -174.27(18) . . . . ?
O3 Ti1 N1 C6 101.00(17) . . . . ?
Ti2 Ti1 N1 C6 101.78(16) . . . . ?
O5 Ti2 O4 Ti1 -109.65(10) . . . . ?
O6 Ti2 O4 Ti1 141.24(9) . . . . ?
O3 Ti2 O4 Ti1 -5.04(9) . . . . ?
N2 Ti2 O4 Ti1 55.15(16) . . . . ?
O7 Ti1 O4 Ti2 -171.14(9) . . . . ?
O2 Ti1 O4 Ti2 89.07(10) . . . . ?
O1 Ti1 O4 Ti2 -76.69(10) . . . . ?
N1 Ti1 O4 Ti2 14.4(3) . . . . ?
O3 Ti1 O4 Ti2 4.52(8) . . . . ?
O4 Ti2 O6 C31 -134.3(3) . . . . ?
O5 Ti2 O6 C31 112.3(3) . . . . ?
O3 Ti2 O6 C31 -41.6(3) . . . . ?
N2 Ti2 O6 C31 7.0(3) . . . . ?
Ti1 Ti2 O6 C31 -107.6(3) . . . . ?
O7 Ti1 O2 C1 111.7(2) . . . . ?
O4 Ti1 O2 C1 -148.90(19) . . . . ?
O1 Ti1 O2 C1 -5.6(3) . . . . ?
N1 Ti1 O2 C1 14.09(19) . . . . ?
O3 Ti1 O2 C1 -76.04(19) . . . . ?
Ti2 Ti1 O2 C1 -115.40(18) . . . . ?
O2 Ti1 O7 C37 49.8(2) . . . . ?
O4 Ti1 O7 C37 -50.2(2) . . . . ?
O1 Ti1 O7 C37 -151.3(2) . . . . ?
N1 Ti1 O7 C37 128.1(2) . . . . ?
O3 Ti1 O7 C37 -76.1(5) . . . . ?
Ti2 Ti1 O7 C37 -56.6(2) . . . . ?
O7 Ti1 O1 C13 -97.7(3) . . . . ?
O2 Ti1 O1 C13 20.6(4) . . . . ?
O4 Ti1 O1 C13 163.7(3) . . . . ?
N1 Ti1 O1 C13 1.2(3) . . . . ?
O3 Ti1 O1 C13 91.6(3) . . . . ?
Ti2 Ti1 O1 C13 131.4(3) . . . . ?
Ti2 O6 C31 C26 -7.9(4) . . . . ?
Ti2 O6 C31 C30 171.94(19) . . . . ?
C27 C26 C31 O6 -179.2(2) . . . . ?
C25 C26 C31 O6 1.8(4) . . . . ?
C27 C26 C31 C30 1.0(4) . . . . ?
C25 C26 C31 C30 -178.0(2) . . . . ?
C25 N2 C24 C23 -8.1(4) . . . . ?
Ti2 N2 C24 C23 171.4(2) . . . . ?
C25 N2 C24 C19 -133.6(2) . . . . ?
Ti2 N2 C24 C19 45.9(2) . . . . ?
C24 N2 C25 C26 178.8(2) . . . . ?
Ti2 N2 C25 C26 -0.5(4) . . . . ?
C31 C26 C25 N2 1.4(4) . . . . ?
C27 C26 C25 N2 -177.6(2) . . . . ?
O6 C31 C30 C29 179.8(2) . . . . ?
C26 C31 C30 C29 -0.4(4) . . . . ?
O6 C31 C30 C32 0.7(4) . . . . ?
C26 C31 C30 C32 -179.4(2) . . . . ?
Ti2 O3 C19 C20 147.07(19) . . . . ?
Ti1 O3 C19 C20 -87.8(3) . . . . ?
Ti2 O3 C19 C24 25.5(3) . . . . ?
Ti1 O3 C19 C24 150.59(16) . . . . ?
N2 C24 C19 O3 -45.3(3) . . . . ?
C23 C24 C19 O3 -175.4(2) . . . . ?
N2 C24 C19 C20 -169.5(2) . . . . ?
C23 C24 C19 C20 60.4(3) . . . . ?
Ti1 O1 C13 C8 -8.2(4) . . . . ?
Ti1 O1 C13 C12 171.9(2) . . . . ?
C9 C8 C13 O1 -176.1(2) . . . . ?
C7 C8 C13 O1 9.0(4) . . . . ?
C9 C8 C13 C12 3.8(4) . . . . ?
C7 C8 C13 C12 -171.1(2) . . . . ?
C11 C12 C13 O1 177.4(2) . . . . ?
C14 C12 C13 O1 -3.8(4) . . . . ?
C11 C12 C13 C8 -2.5(4) . . . . ?
C14 C12 C13 C8 176.4(2) . . . . ?
C31 C26 C27 C28 -1.2(4) . . . . ?
C25 C26 C27 C28 177.8(2) . . . . ?
O4 Ti2 O5 C40 11.5(4) . . . . ?
O6 Ti2 O5 C40 116.4(3) . . . . ?
O3 Ti2 O5 C40 -78.2(3) . . . . ?
N2 Ti2 O5 C40 -158.8(3) . . . . ?
Ti1 Ti2 O5 C40 -27.1(4) . . . . ?
C26 C27 C28 C29 0.9(4) . . . . ?
C26 C27 C28 C36 -179.9(3) . . . . ?
C11 C12 C14 C17 118.6(3) . . . . ?
C13 C12 C14 C17 -60.2(3) . . . . ?
C11 C12 C14 C15 -0.4(4) . . . . ?
C13 C12 C14 C15 -179.2(3) . . . . ?
C11 C12 C14 C16 -120.0(3) . . . . ?
C13 C12 C14 C16 61.2(3) . . . . ?
C31 C30 C29 C28 0.0(4) . . . . ?
C32 C30 C29 C28 179.0(3) . . . . ?
C27 C28 C29 C30 -0.2(4) . . . . ?
C36 C28 C29 C30 -179.4(3) . . . . ?
C7 N1 C6 C1 145.3(3) . . . . ?
Ti1 N1 C6 C1 -34.4(3) . . . . ?
C7 N1 C6 C5 16.7(4) . . . . ?
Ti1 N1 C6 C5 -163.0(2) . . . . ?
C6 N1 C7 C8 174.3(2) . . . . ?
Ti1 N1 C7 C8 -6.0(4) . . . . ?
C13 C8 C7 N1 -2.4(4) . . . . ?
C9 C8 C7 N1 -177.3(3) . . . . ?
C13 C8 C9 C10 -1.7(5) . . . . ?
C7 C8 C9 C10 173.3(3) . . . . ?
Ti1 O2 C1 C6 -38.4(3) . . . . ?
Ti1 O2 C1 C2 -162.86(18) . . . . ?
N1 C6 C1 O2 44.5(3) . . . . ?
C5 C6 C1 O2 176.3(2) . . . . ?
N1 C6 C1 C2 170.9(2) . . . . ?
C5 C6 C1 C2 -57.4(3) . . . . ?
C3 C2 C1 O2 178.4(2) . . . . ?
C3 C2 C1 C6 55.5(3) . . . . ?
N1 C6 C5 C4 177.3(2) . . . . ?
C1 C6 C5 C4 52.9(3) . . . . ?
O3 C19 C20 C21 -178.8(2) . . . . ?
C24 C19 C20 C21 -58.7(3) . . . . ?
C29 C30 C32 C35 -117.8(3) . . . . ?
C31 C30 C32 C35 61.2(3) . . . . ?
C29 C30 C32 C33 1.5(4) . . . . ?
C31 C30 C32 C33 -179.5(3) . . . . ?
C29 C30 C32 C34 121.3(3) . . . . ?
C31 C30 C32 C34 -59.7(3) . . . . ?
C13 C12 C11 C10 -0.9(5) . . . . ?
C14 C12 C11 C10 -179.7(3) . . . . ?
N2 C24 C23 C22 -179.6(2) . . . . ?
C19 C24 C23 C22 -57.2(3) . . . . ?
C24 C23 C22 C21 53.8(4) . . . . ?
C19 C20 C21 C22 56.4(4) . . . . ?
C23 C22 C21 C20 -54.3(4) . . . . ?
C1 C2 C3 C4 -53.7(4) . . . . ?
C2 C3 C4 C5 52.7(4) . . . . ?
C6 C5 C4 C3 -50.5(4) . . . . ?
C8 C9 C10 C11 -1.5(5) . . . . ?
C8 C9 C10 C18 -179.4(3) . . . . ?
C12 C11 C10 C9 2.9(5) . . . . ?
C12 C11 C10 C18 -179.3(3) . . . . ?
Ti2 O5 C40 C42 78.1(5) . . . . ?
Ti2 O5 C40 C41 -61.3(5) . . . . ?
Ti1 O7 C37 C39 -100.4(3) . . . . ?
Ti1 O7 C37 C38 130.7(3) . . . . ?

_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_theta_full        24.43
_diffrn_measured_fraction_theta_full 0.998
_refine_diff_density_max         0.353
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.043
# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.500 429 98 ' '
2 0.000 0.500 0.000 429 98 ' '
3 0.062 0.694 0.649 6 0 ' '
4 0.062 0.806 0.149 6 0 ' '
5 0.937 0.194 0.851 6 0 ' '
6 0.937 0.306 0.351 6 0 ' '
_platon_squeeze_details          ?

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?

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

data_Ti2
_database_code_depnum_ccdc_archive 'CCDC 1422870'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        Ti2
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C26 H26 Cl4 N2 O4 Ti'
_chemical_formula_sum            'C26 H26 Cl4 N2 O4 Ti'
_chemical_formula_weight         620.19

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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   10.3126(3)
_cell_length_b                   12.8248(5)
_cell_length_c                   12.9776(4)
_cell_angle_alpha                63.2283(19)
_cell_angle_beta                 68.1217(13)
_cell_angle_gamma                66.2981(14)
_cell_volume                     1364.07(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7548
_cell_measurement_theta_min      2.22
_cell_measurement_theta_max      25.58

_exptl_crystal_description       Block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.510
_exptl_crystal_F_000             636
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.100
_exptl_absorpt_coefficient_mu    0.741
_shelx_estimated_absorpt_T_min   0.836
_shelx_estimated_absorpt_T_max   0.930
_exptl_absorpt_correction_type   none
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            18344
_diffrn_reflns_av_unetI/netI     0.0221
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_theta_min         1.854
_diffrn_reflns_theta_max         24.985
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 0.967
_reflns_number_total             4790
_reflns_number_gt                3986
_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-2013 (Sheldrick, 2013)'
_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)+(0.0316P)²+0.9027P] 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         4790
_refine_ls_number_parameters     334
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0439
_refine_ls_R_factor_gt           0.0336
_refine_ls_wR_factor_ref         0.0831
_refine_ls_wR_factor_gt          0.0776
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_restrained_S_all      1.032
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.6140(3) 0.6783(2) -0.0949(2) 0.0424(6) Uani 1 1 d . . . . .
H1 H 0.5373 0.6460 -0.0299 0.051 Uiso 1 1 calc R U . . .
C2 C 0.5742(3) 0.7175(2) -0.2106(2) 0.0498(6) Uani 1 1 d . . . . .
H2A H 0.6444 0.7558 -0.2762 0.060 Uiso 1 1 calc R U . . .
H2B H 0.4789 0.7765 -0.2103 0.060 Uiso 1 1 calc R U . . .
C3 C 0.5726(4) 0.6071(3) -0.2265(3) 0.0687(9) Uani 1 1 d . . . . .
H3A H 0.4912 0.5779 -0.1684 0.082 Uiso 1 1 calc R U . . .
H3B H 0.5579 0.6320 -0.3048 0.082 Uiso 1 1 calc R U . . .
C4 C 0.7102(3) 0.5053(3) -0.2130(3) 0.0630(8) Uani 1 1 d . . . . .
H4A H 0.7880 0.5295 -0.2807 0.076 Uiso 1 1 calc R U . . .
H4B H 0.6975 0.4350 -0.2143 0.076 Uiso 1 1 calc R U . . .
C5 C 0.7561(3) 0.4683(2) -0.0999(2) 0.0443(6) Uani 1 1 d . . . . .
H5A H 0.6896 0.4279 -0.0319 0.053 Uiso 1 1 calc R U . . .
H5B H 0.8531 0.4118 -0.1030 0.053 Uiso 1 1 calc R U . . .
C6 C 0.7550(2) 0.5796(2) -0.0869(2) 0.0379(5) Uani 1 1 d . . . . .
H6 H 0.8287 0.6132 -0.1547 0.045 Uiso 1 1 calc R U . . .
C7 C 0.8393(2) 0.46348(19) 0.09336(19) 0.0326(5) Uani 1 1 d . . . . .
H7 H 0.8580 0.3951 0.0761 0.039 Uiso 1 1 calc R U . . .
C8 C 0.8701(2) 0.44465(19) 0.20144(18) 0.0309(5) Uani 1 1 d . . . . .
C9 C 0.9168(2) 0.3248(2) 0.2773(2) 0.0403(5) Uani 1 1 d . . . . .
H9 H 0.9275 0.2601 0.2574 0.048 Uiso 1 1 calc R U . . .
C10 C 0.9467(3) 0.3026(2) 0.3807(2) 0.0467(6) Uani 1 1 d . . . . .
C11 C 0.9273(3) 0.3974(2) 0.4138(2) 0.0478(6) Uani 1 1 d . . . . .
H11 H 0.9445 0.3815 0.4856 0.057 Uiso 1 1 calc R U . . .
C12 C 0.8822(2) 0.5154(2) 0.3394(2) 0.0394(5) Uani 1 1 d . . . . .
C13 C 0.8569(2) 0.54332(19) 0.22920(19) 0.0331(5) Uani 1 1 d . . . . .
C14 C 0.9109(2) 0.90739(19) -0.08926(19) 0.0363(5) Uani 1 1 d . . . . .
H14 H 0.9572 0.8852 -0.0258 0.044 Uiso 1 1 calc R U . . .
C15 C 1.0092(3) 0.9598(2) -0.2071(2) 0.0481(6) Uani 1 1 d . . . . .
H15A H 0.9688 0.9763 -0.2713 0.058 Uiso 1 1 calc R U . . .
H15B H 1.1045 0.9012 -0.2148 0.058 Uiso 1 1 calc R U . . .
C16 C 1.0240(3) 1.0774(2) -0.2156(2) 0.0508(6) Uani 1 1 d . . . . .
H16A H 1.0772 1.0585 -0.1586 0.061 Uiso 1 1 calc R U . . .
H16B H 1.0797 1.1141 -0.2943 0.061 Uiso 1 1 calc R U . . .
C17 C 0.8770(3) 1.1679(2) -0.1918(2) 0.0541(7) Uani 1 1 d . . . . .
H17A H 0.8300 1.1954 -0.2555 0.065 Uiso 1 1 calc R U . . .
H17B H 0.8918 1.2382 -0.1923 0.065 Uiso 1 1 calc R U . . .
C18 C 0.7768(3) 1.11515(19) -0.0740(2) 0.0429(6) Uani 1 1 d . . . . .
H18A H 0.8167 1.0967 -0.0088 0.052 Uiso 1 1 calc R U . . .
H18B H 0.6816 1.1738 -0.0661 0.052 Uiso 1 1 calc R U . . .
C19 C 0.7632(2) 0.99993(18) -0.07018(19) 0.0344(5) Uani 1 1 d . . . . .
H19 H 0.7208 1.0232 -0.1363 0.041 Uiso 1 1 calc R U . . .
C20 C 0.6056(2) 0.9611(2) 0.1263(2) 0.0365(5) Uani 1 1 d . . . . .
H20 H 0.6013 1.0378 0.1194 0.044 Uiso 1 1 calc R U . . .
C21 C 0.5306(2) 0.8878(2) 0.2374(2) 0.0362(5) Uani 1 1 d . . . . .
C22 C 0.4789(3) 0.9240(2) 0.3356(2) 0.0452(6) Uani 1 1 d . . . . .
H22 H 0.4890 0.9962 0.3281 0.054 Uiso 1 1 calc R U . . .
C23 C 0.4134(3) 0.8533(2) 0.4429(2) 0.0481(6) Uani 1 1 d . . . . .
C24 C 0.3963(3) 0.7460(2) 0.4563(2) 0.0488(6) Uani 1 1 d . . . . .
H24 H 0.3536 0.6977 0.5301 0.059 Uiso 1 1 calc R U . . .
C25 C 0.4432(3) 0.7115(2) 0.3594(2) 0.0419(6) Uani 1 1 d . . . . .
C26 C 0.5102(2) 0.7812(2) 0.2472(2) 0.0369(5) Uani 1 1 d . . . . .
Cl1 Cl 1.01102(11) 0.15341(7) 0.47132(7) 0.0854(3) Uani 1 1 d . . . . .
Cl2 Cl 0.85553(9) 0.63498(7) 0.38048(7) 0.0679(2) Uani 1 1 d . . . . .
Cl3 Cl 0.34846(9) 0.89895(8) 0.56543(6) 0.0727(2) Uani 1 1 d . . . . .
Cl4 Cl 0.42091(8) 0.57853(6) 0.37391(6) 0.0615(2) Uani 1 1 d . . . . .
N1 N 0.78796(18) 0.56804(15) 0.01969(15) 0.0317(4) Uani 1 1 d . . . . .
N2 N 0.67752(18) 0.92698(15) 0.03704(15) 0.0314(4) Uani 1 1 d . . . . .
O1 O 0.62614(17) 0.77365(13) -0.07658(14) 0.0421(4) Uani 1 1 d . . . . .
O2 O 0.82698(17) 0.65565(13) 0.15573(14) 0.0414(4) Uani 1 1 d . . . . .
O3 O 0.55004(17) 0.74798(14) 0.15493(13) 0.0403(4) Uani 1 1 d . . . . .
O4 O 0.88293(17) 0.80332(13) -0.07812(14) 0.0423(4) Uani 1 1 d . . . . .
Ti1 Ti 0.72497(4) 0.74870(3) 0.02909(3) 0.03207(11) 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
C1 O1 1.406(3) . ?
C1 C6 1.497(3) . ?
C1 C2 1.513(3) . ?
C1 H1 0.9800 . ?
C2 C3 1.527(4) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.496(4) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.521(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.505(3) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 N1 1.476(3) . ?
C6 H6 0.9800 . ?
C7 N1 1.282(3) . ?
C7 C8 1.446(3) . ?
C7 H7 0.9300 . ?
C8 C9 1.400(3) . ?
C8 C13 1.409(3) . ?
C9 C10 1.368(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.383(4) . ?
C10 Cl1 1.737(2) . ?
C11 C12 1.375(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.409(3) . ?
C12 Cl2 1.732(2) . ?
C13 O2 1.305(2) . ?
C14 O4 1.411(2) . ?
C14 C15 1.511(3) . ?
C14 C19 1.523(3) . ?
C14 H14 0.9800 . ?
C15 C16 1.528(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.516(4) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.522(3) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 C19 1.517(3) . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 N2 1.472(3) . ?
C19 H19 0.9800 . ?
C20 N2 1.281(3) . ?
C20 C21 1.446(3) . ?
C20 H20 0.9300 . ?
C21 C22 1.398(3) . ?
C21 C26 1.409(3) . ?
C22 C23 1.368(3) . ?
C22 H22 0.9300 . ?
C23 C24 1.383(4) . ?
C23 Cl3 1.746(2) . ?
C24 C25 1.373(3) . ?
C24 H24 0.9300 . ?
C25 C26 1.404(3) . ?
C25 Cl4 1.730(2) . ?
C26 O3 1.317(3) . ?
N1 Ti1 2.1887(17) . ?
N2 Ti1 2.1801(17) . ?
O1 Ti1 1.8455(15) . ?
O2 Ti1 1.9350(15) . ?
O3 Ti1 1.9302(16) . ?
O4 Ti1 1.8521(16) . ?

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
O1 C1 C6 107.58(18) . . ?
O1 C1 C2 113.53(19) . . ?
C6 C1 C2 111.7(2) . . ?
O1 C1 H1 108.0 . . ?
C6 C1 H1 108.0 . . ?
C2 C1 H1 108.0 . . ?
C1 C2 C3 109.9(2) . . ?
C1 C2 H2A 109.7 . . ?
C3 C2 H2A 109.7 . . ?
C1 C2 H2B 109.7 . . ?
C3 C2 H2B 109.7 . . ?
H2A C2 H2B 108.2 . . ?
C4 C3 C2 112.9(2) . . ?
C4 C3 H3A 109.0 . . ?
C2 C3 H3A 109.0 . . ?
C4 C3 H3B 109.0 . . ?
C2 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 114.3(2) . . ?
C3 C4 H4A 108.7 . . ?
C5 C4 H4A 108.7 . . ?
C3 C4 H4B 108.7 . . ?
C5 C4 H4B 108.7 . . ?
H4A C4 H4B 107.6 . . ?
C6 C5 C4 109.6(2) . . ?
C6 C5 H5A 109.7 . . ?
C4 C5 H5A 109.7 . . ?
C6 C5 H5B 109.7 . . ?
C4 C5 H5B 109.7 . . ?
H5A C5 H5B 108.2 . . ?
N1 C6 C1 103.92(17) . . ?
N1 C6 C5 119.89(19) . . ?
C1 C6 C5 113.66(19) . . ?
N1 C6 H6 106.1 . . ?
C1 C6 H6 106.1 . . ?
C5 C6 H6 106.1 . . ?
N1 C7 C8 124.5(2) . . ?
N1 C7 H7 117.8 . . ?
C8 C7 H7 117.8 . . ?
C9 C8 C13 120.5(2) . . ?
C9 C8 C7 118.1(2) . . ?
C13 C8 C7 121.44(19) . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C9 C10 C11 120.9(2) . . ?
C9 C10 Cl1 119.6(2) . . ?
C11 C10 Cl1 119.55(19) . . ?
C12 C11 C10 119.3(2) . . ?
C12 C11 H11 120.3 . . ?
C10 C11 H11 120.3 . . ?
C11 C12 C13 122.1(2) . . ?
C11 C12 Cl2 119.80(18) . . ?
C13 C12 Cl2 118.08(17) . . ?
O2 C13 C8 122.30(19) . . ?
O2 C13 C12 120.8(2) . . ?
C8 C13 C12 116.91(19) . . ?
O4 C14 C15 113.49(18) . . ?
O4 C14 C19 106.47(17) . . ?
C15 C14 C19 111.24(18) . . ?
O4 C14 H14 108.5 . . ?
C15 C14 H14 108.5 . . ?
C19 C14 H14 108.5 . . ?
C14 C15 C16 110.1(2) . . ?
C14 C15 H15A 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C14 C15 H15B 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.2 . . ?
C17 C16 C15 112.0(2) . . ?
C17 C16 H16A 109.2 . . ?
C15 C16 H16A 109.2 . . ?
C17 C16 H16B 109.2 . . ?
C15 C16 H16B 109.2 . . ?
H16A C16 H16B 107.9 . . ?
C16 C17 C18 113.1(2) . . ?
C16 C17 H17A 109.0 . . ?
C18 C17 H17A 109.0 . . ?
C16 C17 H17B 109.0 . . ?
C18 C17 H17B 109.0 . . ?
H17A C17 H17B 107.8 . . ?
C19 C18 C17 108.7(2) . . ?
C19 C18 H18A 110.0 . . ?
C17 C18 H18A 110.0 . . ?
C19 C18 H18B 110.0 . . ?
C17 C18 H18B 110.0 . . ?
H18A C18 H18B 108.3 . . ?
N2 C19 C18 120.00(19) . . ?
N2 C19 C14 102.87(16) . . ?
C18 C19 C14 112.08(18) . . ?
N2 C19 H19 107.1 . . ?
C18 C19 H19 107.1 . . ?
C14 C19 H19 107.1 . . ?
N2 C20 C21 124.1(2) . . ?
N2 C20 H20 118.0 . . ?
C21 C20 H20 118.0 . . ?
C22 C21 C26 120.2(2) . . ?
C22 C21 C20 118.9(2) . . ?
C26 C21 C20 120.8(2) . . ?
C23 C22 C21 120.0(2) . . ?
C23 C22 H22 120.0 . . ?
C21 C22 H22 120.0 . . ?
C22 C23 C24 121.1(2) . . ?
C22 C23 Cl3 119.9(2) . . ?
C24 C23 Cl3 119.0(2) . . ?
C25 C24 C23 119.2(2) . . ?
C25 C24 H24 120.4 . . ?
C23 C24 H24 120.4 . . ?
C24 C25 C26 121.9(2) . . ?
C24 C25 Cl4 119.97(19) . . ?
C26 C25 Cl4 118.10(18) . . ?
O3 C26 C25 120.7(2) . . ?
O3 C26 C21 121.9(2) . . ?
C25 C26 C21 117.5(2) . . ?
C7 N1 C6 121.23(18) . . ?
C7 N1 Ti1 129.22(15) . . ?
C6 N1 Ti1 109.48(13) . . ?
C20 N2 C19 122.10(18) . . ?
C20 N2 Ti1 127.23(15) . . ?
C19 N2 Ti1 109.84(13) . . ?
C1 O1 Ti1 123.26(13) . . ?
C13 O2 Ti1 136.67(14) . . ?
C26 O3 Ti1 130.12(14) . . ?
C14 O4 Ti1 123.49(13) . . ?
O1 Ti1 O4 99.14(7) . . ?
O1 Ti1 O3 91.44(7) . . ?
O4 Ti1 O3 156.71(7) . . ?
O1 Ti1 O2 156.36(7) . . ?
O4 Ti1 O2 92.81(7) . . ?
O3 Ti1 O2 85.25(7) . . ?
O1 Ti1 N2 105.83(6) . . ?
O4 Ti1 N2 76.59(6) . . ?
O3 Ti1 N2 80.59(7) . . ?
O2 Ti1 N2 96.73(6) . . ?
O1 Ti1 N1 76.77(6) . . ?
O4 Ti1 N1 100.33(7) . . ?
O3 Ti1 N1 102.28(7) . . ?
O2 Ti1 N1 81.08(6) . . ?
N2 Ti1 N1 176.18(6) . . ?

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
O1 C1 C2 C3 176.5(2) . . . . ?
C6 C1 C2 C3 54.7(3) . . . . ?
C1 C2 C3 C4 -52.3(4) . . . . ?
C2 C3 C4 C5 51.4(4) . . . . ?
C3 C4 C5 C6 -50.1(3) . . . . ?
O1 C1 C6 N1 45.6(2) . . . . ?
C2 C1 C6 N1 170.82(19) . . . . ?
O1 C1 C6 C5 177.64(19) . . . . ?
C2 C1 C6 C5 -57.2(3) . . . . ?
C4 C5 C6 N1 176.7(2) . . . . ?
C4 C5 C6 C1 53.0(3) . . . . ?
N1 C7 C8 C9 175.8(2) . . . . ?
N1 C7 C8 C13 -5.6(3) . . . . ?
C13 C8 C9 C10 1.6(3) . . . . ?
C7 C8 C9 C10 -179.8(2) . . . . ?
C8 C9 C10 C11 2.0(4) . . . . ?
C8 C9 C10 Cl1 -177.63(18) . . . . ?
C9 C10 C11 C12 -2.3(4) . . . . ?
Cl1 C10 C11 C12 177.29(19) . . . . ?
C10 C11 C12 C13 -0.9(4) . . . . ?
C10 C11 C12 Cl2 179.29(19) . . . . ?
C9 C8 C13 O2 173.5(2) . . . . ?
C7 C8 C13 O2 -5.1(3) . . . . ?
C9 C8 C13 C12 -4.5(3) . . . . ?
C7 C8 C13 C12 176.84(19) . . . . ?
C11 C12 C13 O2 -173.8(2) . . . . ?
Cl2 C12 C13 O2 6.0(3) . . . . ?
C11 C12 C13 C8 4.3(3) . . . . ?
Cl2 C12 C13 C8 -175.93(16) . . . . ?
O4 C14 C15 C16 175.53(19) . . . . ?
C19 C14 C15 C16 55.5(3) . . . . ?
C14 C15 C16 C17 -53.6(3) . . . . ?
C15 C16 C17 C18 54.4(3) . . . . ?
C16 C17 C18 C19 -54.5(3) . . . . ?
C17 C18 C19 N2 177.09(18) . . . . ?
C17 C18 C19 C14 56.3(2) . . . . ?
O4 C14 C19 N2 47.0(2) . . . . ?
C15 C14 C19 N2 171.13(18) . . . . ?
O4 C14 C19 C18 177.27(17) . . . . ?
C15 C14 C19 C18 -58.6(2) . . . . ?
N2 C20 C21 C22 168.2(2) . . . . ?
N2 C20 C21 C26 -11.5(3) . . . . ?
C26 C21 C22 C23 2.6(3) . . . . ?
C20 C21 C22 C23 -177.1(2) . . . . ?
C21 C22 C23 C24 -0.4(4) . . . . ?
C21 C22 C23 Cl3 -179.79(18) . . . . ?
C22 C23 C24 C25 -1.4(4) . . . . ?
Cl3 C23 C24 C25 178.01(19) . . . . ?
C23 C24 C25 C26 1.0(4) . . . . ?
C23 C24 C25 Cl4 -179.27(19) . . . . ?
C24 C25 C26 O3 -177.9(2) . . . . ?
Cl4 C25 C26 O3 2.4(3) . . . . ?
C24 C25 C26 C21 1.1(3) . . . . ?
Cl4 C25 C26 C21 -178.59(16) . . . . ?
C22 C21 C26 O3 176.1(2) . . . . ?
C20 C21 C26 O3 -4.3(3) . . . . ?
C22 C21 C26 C25 -2.9(3) . . . . ?
C20 C21 C26 C25 176.72(19) . . . . ?
C8 C7 N1 C6 -178.03(19) . . . . ?
C8 C7 N1 Ti1 -1.6(3) . . . . ?
C1 C6 N1 C7 139.1(2) . . . . ?
C5 C6 N1 C7 10.8(3) . . . . ?
C1 C6 N1 Ti1 -37.98(19) . . . . ?
C5 C6 N1 Ti1 -166.25(17) . . . . ?
C21 C20 N2 C19 -174.30(19) . . . . ?
C21 C20 N2 Ti1 -5.8(3) . . . . ?
C18 C19 N2 C20 4.3(3) . . . . ?
C14 C19 N2 C20 129.5(2) . . . . ?
C18 C19 N2 Ti1 -165.96(16) . . . . ?
C14 C19 N2 Ti1 -40.71(17) . . . . ?
C6 C1 O1 Ti1 -36.7(3) . . . . ?
C2 C1 O1 Ti1 -160.76(17) . . . . ?
C8 C13 O2 Ti1 27.7(3) . . . . ?
C12 C13 O2 Ti1 -154.36(17) . . . . ?
C25 C26 O3 Ti1 -138.29(18) . . . . ?
C21 C26 O3 Ti1 42.7(3) . . . . ?
C15 C14 O4 Ti1 -159.23(16) . . . . ?
C19 C14 O4 Ti1 -36.5(2) . . . . ?
C1 O1 Ti1 O4 109.79(18) . . . . ?
C1 O1 Ti1 O3 -91.04(18) . . . . ?
C1 O1 Ti1 O2 -9.6(3) . . . . ?
C1 O1 Ti1 N2 -171.66(17) . . . . ?
C1 O1 Ti1 N1 11.24(17) . . . . ?
C14 O4 Ti1 O1 114.48(16) . . . . ?
C14 O4 Ti1 O3 -1.5(3) . . . . ?
C14 O4 Ti1 O2 -85.99(16) . . . . ?
C14 O4 Ti1 N2 10.26(16) . . . . ?
C14 O4 Ti1 N1 -167.43(16) . . . . ?

_refine_diff_density_max         0.416
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.044

_shelxl_version_number           2013-4


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

data_Ti1
_database_code_depnum_ccdc_archive 'CCDC 1422871'

_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;
_publcif_datablock.id            {1ca9f957-dee2-423c-8aa0-77e1010ccb34}
# publcif _publ_body_element loop end

_audit_creation_method           'APEX2 v2010.1-2'
_chemical_name_systematic        Ti1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C36 H50 N2 O4 Ti'
_chemical_formula_sum            'C36 H50 N2 O4 Ti'
_chemical_formula_weight         622.68

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

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   I2/a
_symmetry_space_group_name_Hall  '-I 2ya'

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

_cell_length_a                   14.4864(9)
_cell_length_b                   17.4311(13)
_cell_length_c                   16.5711(16)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.720(3)
_cell_angle_gamma                90.00
_cell_volume                     4047.1(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7841
_cell_measurement_theta_min      2.34
_cell_measurement_theta_max      27.80

_exptl_crystal_description       prism
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.15
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1336
_exptl_absorpt_coefficient_mu    0.245
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9193
_exptl_absorpt_correction_T_max  0.9642
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'

_exptl_special_details           ?

_diffrn_ambient_temperature      296(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 APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            19126
_diffrn_reflns_av_R_equivalents  0.0210
_diffrn_reflns_av_sigmaI/netI    0.0243
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         1.73
_diffrn_reflns_theta_max         28.34
_reflns_number_total             5037
_reflns_number_gt                3664
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0754P)²+0.6354P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5037
_refine_ls_number_parameters     199
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0626
_refine_ls_R_factor_gt           0.0451
_refine_ls_wR_factor_ref         0.1426
_refine_ls_wR_factor_gt          0.1357
_refine_ls_goodness_of_fit_ref   1.103
_refine_ls_restrained_S_all      1.103
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.2500 0.01259(2) 0.0000 0.04692(15) Uani 1 2 d S . .
O2 O 0.30253(10) -0.05784(8) 0.08246(9) 0.0777(4) Uani 1 1 d . . .
C13 C 0.30626(18) -0.13523(13) 0.20492(15) 0.0848(7) Uani 1 1 d . . .
H13A H 0.3754 -0.1379 0.2204 0.102 Uiso 1 1 calc R . .
H13B H 0.2821 -0.1794 0.1704 0.102 Uiso 1 1 calc R . .
C4 C 0.00507(12) 0.25282(11) -0.07150(11) 0.0598(4) Uani 1 1 d . . .
H4 H -0.0117 0.2973 -0.1028 0.072 Uiso 1 1 calc R . .
C10 C 0.11072(18) 0.16044(17) -0.22328(14) 0.0921(7) Uani 1 1 d . . .
H10A H 0.0440 0.1524 -0.2483 0.138 Uiso 1 1 calc R . .
H10B H 0.1380 0.1144 -0.1953 0.138 Uiso 1 1 calc R . .
H10C H 0.1424 0.1732 -0.2658 0.138 Uiso 1 1 calc R . .
C16 C 0.12930(16) -0.05388(13) 0.21063(12) 0.0752(6) Uani 1 1 d . . .
H16A H 0.0601 -0.0523 0.1944 0.090 Uiso 1 1 calc R . .
H16B H 0.1521 -0.0083 0.2432 0.090 Uiso 1 1 calc R . .
C15 C 0.16300(19) -0.12550(15) 0.26282(14) 0.0903(7) Uani 1 1 d . . .
H15A H 0.1437 -0.1219 0.3146 0.108 Uiso 1 1 calc R . .
H15B H 0.1319 -0.1701 0.2328 0.108 Uiso 1 1 calc R . .
C14 C 0.26961(18) -0.13659(15) 0.28262(14) 0.0885(7) Uani 1 1 d . . .
H14A H 0.2860 -0.1853 0.3109 0.106 Uiso 1 1 calc R . .
H14B H 0.3007 -0.0963 0.3202 0.106 Uiso 1 1 calc R . .
C1 C 0.05324(9) 0.12204(9) 0.02208(9) 0.0435(3) Uani 1 1 d . . .
C7 C -0.11360(17) 0.29275(16) 0.00952(15) 0.0920(8) Uani 1 1 d . . .
H7A H -0.1762 0.2775 -0.0216 0.138 Uiso 1 1 calc R . .
H7B H -0.1005 0.3436 -0.0067 0.138 Uiso 1 1 calc R . .
H7C H -0.1106 0.2921 0.0681 0.138 Uiso 1 1 calc R . .
C8 C 0.12305(13) 0.22670(12) -0.15976(11) 0.0639(5) Uani 1 1 d . . .
C9 C 0.22843(15) 0.23949(16) -0.12136(15) 0.0928(8) Uani 1 1 d . . .
H9A H 0.2596 0.2511 -0.1645 0.139 Uiso 1 1 calc R . .
H9B H 0.2558 0.1939 -0.0924 0.139 Uiso 1 1 calc R . .
H9C H 0.2366 0.2816 -0.0828 0.139 Uiso 1 1 calc R . .
C12 C 0.27445(13) -0.06279(11) 0.15660(12) 0.0616(5) Uani 1 1 d . . .
H12 H 0.3017 -0.0190 0.1918 0.074 Uiso 1 1 calc R . .
C2 C 0.09912(9) 0.13884(9) -0.04178(9) 0.0452(4) Uani 1 1 d . . .
C3 C 0.07342(10) 0.20579(10) -0.09055(10) 0.0516(4) Uani 1 1 d . . .
C5 C -0.04043(12) 0.23771(11) -0.00812(10) 0.0578(4) Uani 1 1 d . . .
C6 C -0.01665(10) 0.17204(10) 0.03677(9) 0.0502(4) Uani 1 1 d . . .
H6 H -0.0474 0.1600 0.0781 0.060 Uiso 1 1 calc R . .
C11 C 0.08082(19) 0.29811(16) -0.20791(16) 0.1030(9) Uani 1 1 d . . .
H11A H 0.0142 0.2899 -0.2332 0.154 Uiso 1 1 calc R . .
H11B H 0.1133 0.3085 -0.2505 0.154 Uiso 1 1 calc R . .
H11C H 0.0883 0.3410 -0.1704 0.154 Uiso 1 1 calc R . .
C17 C 0.07815(10) 0.05599(10) 0.07491(9) 0.0470(4) Uani 1 1 d . . .
H17 H 0.0408 0.0458 0.1118 0.056 Uiso 1 1 calc R . .
C18 C 0.16707(11) -0.05559(10) 0.13440(10) 0.0509(4) Uani 1 1 d . . .
H18 H 0.1410 -0.1016 0.1027 0.061 Uiso 1 1 calc R . .
N1 N 0.14724(9) 0.00981(7) 0.07582(8) 0.0438(3) Uani 1 1 d . . .
O1 O 0.16482(8) 0.09134(7) -0.05460(7) 0.0580(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
Ti1 O2 1.8506(13) 2 ?
Ti1 O2 1.8507(13) . ?
Ti1 O1 1.9126(11) 2 ?
Ti1 O1 1.9127(11) . ?
Ti1 N1 2.1789(12) 2 ?
Ti1 N1 2.1789(12) . ?
O2 C12 1.391(2) . ?
C13 C12 1.503(3) . ?
C13 C14 1.512(3) . ?
C13 H13A 0.9700 . ?
C13 H13B 0.9700 . ?
C4 C3 1.382(2) . ?
C4 C5 1.399(2) . ?
C4 H4 0.9300 . ?
C10 C8 1.542(3) . ?
C10 H10A 0.9600 . ?
C10 H10B 0.9600 . ?
C10 H10C 0.9600 . ?
C16 C18 1.499(2) . ?
C16 C15 1.526(3) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C15 C14 1.508(3) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C14 H14A 0.9700 . ?
C14 H14B 0.9700 . ?
C1 C6 1.403(2) . ?
C1 C2 1.4159(18) . ?
C1 C17 1.436(2) . ?
C7 C5 1.512(2) . ?
C7 H7A 0.9600 . ?
C7 H7B 0.9600 . ?
C7 H7C 0.9600 . ?
C8 C9 1.514(3) . ?
C8 C11 1.521(3) . ?
C8 C3 1.544(2) . ?
C9 H9A 0.9600 . ?
C9 H9B 0.9600 . ?
C9 H9C 0.9600 . ?
C12 C18 1.510(2) . ?
C12 H12 0.9800 . ?
C2 O1 1.3188(18) . ?
C2 C3 1.414(2) . ?
C5 C6 1.361(2) . ?
C6 H6 0.9300 . ?
C11 H11A 0.9600 . ?
C11 H11B 0.9600 . ?
C11 H11C 0.9600 . ?
C17 N1 1.282(2) . ?
C17 H17 0.9300 . ?
C18 N1 1.477(2) . ?
C18 H18 0.9800 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Ti1 O2 96.89(10) 2 . ?
O2 Ti1 O1 156.95(5) 2 2 ?
O2 Ti1 O1 91.83(7) . 2 ?
O2 Ti1 O1 91.83(7) 2 . ?
O2 Ti1 O1 156.95(5) . . ?
O1 Ti1 O1 88.27(8) 2 . ?
O2 Ti1 N1 76.85(5) 2 2 ?
O2 Ti1 N1 101.42(5) . 2 ?
O1 Ti1 N1 80.53(4) 2 2 ?
O1 Ti1 N1 101.33(4) . 2 ?
O2 Ti1 N1 101.42(5) 2 . ?
O2 Ti1 N1 76.85(5) . . ?
O1 Ti1 N1 101.33(4) 2 . ?
O1 Ti1 N1 80.53(4) . . ?
N1 Ti1 N1 177.45(7) 2 . ?
C12 O2 Ti1 122.38(11) . . ?
C12 C13 C14 109.89(19) . . ?
C12 C13 H13A 109.7 . . ?
C14 C13 H13A 109.7 . . ?
C12 C13 H13B 109.7 . . ?
C14 C13 H13B 109.7 . . ?
H13A C13 H13B 108.2 . . ?
C3 C4 C5 124.13(16) . . ?
C3 C4 H4 117.9 . . ?
C5 C4 H4 117.9 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
H10A C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C18 C16 C15 109.18(18) . . ?
C18 C16 H16A 109.8 . . ?
C15 C16 H16A 109.8 . . ?
C18 C16 H16B 109.8 . . ?
C15 C16 H16B 109.8 . . ?
H16A C16 H16B 108.3 . . ?
C14 C15 C16 112.99(19) . . ?
C14 C15 H15A 109.0 . . ?
C16 C15 H15A 109.0 . . ?
C14 C15 H15B 109.0 . . ?
C16 C15 H15B 109.0 . . ?
H15A C15 H15B 107.8 . . ?
C15 C14 C13 111.99(18) . . ?
C15 C14 H14A 109.2 . . ?
C13 C14 H14A 109.2 . . ?
C15 C14 H14B 109.2 . . ?
C13 C14 H14B 109.2 . . ?
H14A C14 H14B 107.9 . . ?
C6 C1 C2 119.84(14) . . ?
C6 C1 C17 118.22(13) . . ?
C2 C1 C17 121.91(13) . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C8 C11 109.16(19) . . ?
C9 C8 C10 109.07(18) . . ?
C11 C8 C10 107.06(18) . . ?
C9 C8 C3 109.43(15) . . ?
C11 C8 C3 112.45(15) . . ?
C10 C8 C3 109.59(16) . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C12 C13 113.81(17) . . ?
O2 C12 C18 107.10(14) . . ?
C13 C12 C18 110.91(16) . . ?
O2 C12 H12 108.3 . . ?
C13 C12 H12 108.3 . . ?
C18 C12 H12 108.3 . . ?
O1 C2 C3 121.46(12) . . ?
O1 C2 C1 119.05(14) . . ?
C3 C2 C1 119.49(13) . . ?
C4 C3 C2 117.30(14) . . ?
C4 C3 C8 121.69(15) . . ?
C2 C3 C8 120.96(14) . . ?
C6 C5 C4 117.80(15) . . ?
C6 C5 C7 121.36(16) . . ?
C4 C5 C7 120.84(17) . . ?
C5 C6 C1 121.41(14) . . ?
C5 C6 H6 119.3 . . ?
C1 C6 H6 119.3 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N1 C17 C1 125.83(12) . . ?
N1 C17 H17 117.1 . . ?
C1 C17 H17 117.1 . . ?
N1 C18 C16 119.12(15) . . ?
N1 C18 C12 103.92(12) . . ?
C16 C18 C12 111.74(15) . . ?
N1 C18 H18 107.1 . . ?
C16 C18 H18 107.1 . . ?
C12 C18 H18 107.1 . . ?
C17 N1 C18 120.89(12) . . ?
C17 N1 Ti1 128.69(10) . . ?
C18 N1 Ti1 110.41(9) . . ?
C2 O1 Ti1 141.23(10) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
O2 Ti1 O2 C12 -117.64(17) 2 . . . ?
O1 Ti1 O2 C12 83.74(15) 2 . . . ?
O1 Ti1 O2 C12 -6.2(3) . . . . ?
N1 Ti1 O2 C12 164.45(15) 2 . . . ?
N1 Ti1 O2 C12 -17.47(14) . . . . ?
C18 C16 C15 C14 53.2(3) . . . . ?
C16 C15 C14 C13 -53.3(3) . . . . ?
C12 C13 C14 C15 54.2(3) . . . . ?
Ti1 O2 C12 C13 165.22(15) . . . . ?
Ti1 O2 C12 C18 42.3(2) . . . . ?
C14 C13 C12 O2 -178.06(18) . . . . ?
C14 C13 C12 C18 -57.2(2) . . . . ?
C6 C1 C2 O1 179.82(13) . . . . ?
C17 C1 C2 O1 1.9(2) . . . . ?
C6 C1 C2 C3 -0.4(2) . . . . ?
C17 C1 C2 C3 -178.36(14) . . . . ?
C5 C4 C3 C2 -0.8(3) . . . . ?
C5 C4 C3 C8 -178.33(17) . . . . ?
O1 C2 C3 C4 -178.85(15) . . . . ?
C1 C2 C3 C4 1.4(2) . . . . ?
O1 C2 C3 C8 -1.3(2) . . . . ?
C1 C2 C3 C8 178.98(15) . . . . ?
C9 C8 C3 C4 115.6(2) . . . . ?
C11 C8 C3 C4 -5.9(3) . . . . ?
C10 C8 C3 C4 -124.88(19) . . . . ?
C9 C8 C3 C2 -61.9(2) . . . . ?
C11 C8 C3 C2 176.59(19) . . . . ?
C10 C8 C3 C2 57.6(2) . . . . ?
C3 C4 C5 C6 -0.9(3) . . . . ?
C3 C4 C5 C7 179.16(19) . . . . ?
C4 C5 C6 C1 1.9(2) . . . . ?
C7 C5 C6 C1 -178.12(18) . . . . ?
C2 C1 C6 C5 -1.3(2) . . . . ?
C17 C1 C6 C5 176.70(15) . . . . ?
C6 C1 C17 N1 -171.78(15) . . . . ?
C2 C1 C17 N1 6.2(2) . . . . ?
C15 C16 C18 N1 -177.36(16) . . . . ?
C15 C16 C18 C12 -56.1(2) . . . . ?
O2 C12 C18 N1 -45.78(18) . . . . ?
C13 C12 C18 N1 -170.50(16) . . . . ?
O2 C12 C18 C16 -175.47(15) . . . . ?
C13 C12 C18 C16 59.8(2) . . . . ?
C1 C17 N1 C18 178.78(14) . . . . ?
C1 C17 N1 Ti1 -0.4(2) . . . . ?
C16 C18 N1 C17 -20.2(2) . . . . ?
C12 C18 N1 C17 -145.29(15) . . . . ?
C16 C18 N1 Ti1 159.10(14) . . . . ?
C12 C18 N1 Ti1 34.01(15) . . . . ?
O2 Ti1 N1 C17 -98.33(14) 2 . . . ?
O2 Ti1 N1 C17 167.17(15) . . . . ?
O1 Ti1 N1 C17 77.93(14) 2 . . . ?
O1 Ti1 N1 C17 -8.36(13) . . . . ?
N1 Ti1 N1 C17 -145.38(13) 2 . . . ?
O2 Ti1 N1 C18 82.44(11) 2 . . . ?
O2 Ti1 N1 C18 -12.06(10) . . . . ?
O1 Ti1 N1 C18 -101.30(10) 2 . . . ?
O1 Ti1 N1 C18 172.40(11) . . . . ?
N1 Ti1 N1 C18 35.39(9) 2 . . . ?
C3 C2 O1 Ti1 159.40(13) . . . . ?
C1 C2 O1 Ti1 -20.8(3) . . . . ?
O2 Ti1 O1 C2 122.07(17) 2 . . . ?
O2 Ti1 O1 C2 9.6(3) . . . . ?
O1 Ti1 O1 C2 -80.99(17) 2 . . . ?
N1 Ti1 O1 C2 -160.98(16) 2 . . . ?
N1 Ti1 O1 C2 20.79(17) . . . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        28.34
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.265
_refine_diff_density_min         -0.164
_refine_diff_density_rms         0.039
# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 -0.015 0.500 0.000 471 102 ' '
2 0.049 0.000 0.500 471 102 ' '
_platon_squeeze_details          ?

loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max

loop_
_publcif_info_exptl_table_header_item
?

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

data_Zr1
_database_code_depnum_ccdc_archive 'CCDC 1422873'
_audit_update_record             
;
2016-04-24 deposited with the CCDC.
2016-09-30 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        Zr1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C72 H100 N4 O8 Zr2'
_chemical_formula_sum            'C72 H100 N4 O8 Zr2'
_chemical_formula_weight         1332.00

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'
Zr Zr -2.9673 0.5597 '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)/n
_symmetry_space_group_name_Hall  '-P 2yn'

loop_
_symmetry_equiv_pos_as_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                   20.5673(8)
_cell_length_b                   13.9216(5)
_cell_length_c                   29.0288(10)
_cell_angle_alpha                90.00
_cell_angle_beta                 108.3780(10)
_cell_angle_gamma                90.00
_cell_volume                     7887.9(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    7527
_cell_measurement_theta_min      2.53
_cell_measurement_theta_max      21.88

_exptl_crystal_description       prism
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2816
_exptl_absorpt_coefficient_mu    0.313
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9344
_exptl_absorpt_correction_T_max  0.9694
_exptl_absorpt_process_details   'SADABS (Bruker,2004)'

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(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 APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            37053
_diffrn_reflns_av_R_equivalents  0.0525
_diffrn_reflns_av_sigmaI/netI    0.0492
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         1.46
_diffrn_reflns_theta_max         21.97
_reflns_number_total             9605
_reflns_number_gt                7640
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'APEXII (Bruker, 2004)'
_computing_cell_refinement       'APEXII/SAINT (Bruker, 2004)'
_computing_data_reduction        'SAINT/XPREP (Bruker, 2004)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'ORTEP3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'

_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)+(0.0734P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         9605
_refine_ls_number_parameters     791
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0402
_refine_ls_wR_factor_ref         0.1153
_refine_ls_wR_factor_gt          0.1089
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.56354(12) 0.60149(15) 0.26808(8) 0.0300(6) Uani 1 1 d . . .
Zr1 Zr 0.462864(18) 0.59011(2) 0.213562(12) 0.02705(13) Uani 1 1 d . . .
Zr2 Zr 0.509112(19) 0.51834(2) 0.317327(12) 0.02811(13) Uani 1 1 d . . .
O3 O 0.40540(13) 0.51306(15) 0.25423(8) 0.0298(6) Uani 1 1 d . . .
O2 O 0.46559(12) 0.65658(15) 0.28799(8) 0.0308(6) Uani 1 1 d . . .
O4 O 0.51152(12) 0.44684(15) 0.25111(8) 0.0278(6) Uani 1 1 d . . .
C6 C 0.4164(2) 0.4750(3) 0.11123(13) 0.0360(10) Uani 1 1 d . . .
C7 C 0.61598(19) 0.5903(3) 0.20574(13) 0.0334(9) Uani 1 1 d . . .
H7 H 0.6158 0.6606 0.2033 0.040 Uiso 1 1 calc R . .
O6 O 0.47225(13) 0.72398(16) 0.18511(9) 0.0336(6) Uani 1 1 d . . .
O7 O 0.41038(13) 0.51606(17) 0.15100(9) 0.0354(6) Uani 1 1 d . . .
N2 N 0.35181(16) 0.6579(2) 0.19497(11) 0.0332(8) Uani 1 1 d . . .
O5 O 0.45819(13) 0.51776(16) 0.36815(9) 0.0359(7) Uani 1 1 d . . .
N3 N 0.47316(17) 0.3557(2) 0.31851(11) 0.0338(8) Uani 1 1 d . . .
C14 C 0.4240(2) 0.4637(3) 0.39078(13) 0.0328(9) Uani 1 1 d . . .
C15 C 0.4386(2) 0.8039(2) 0.16579(13) 0.0309(9) Uani 1 1 d . . .
C16 C 0.4793(2) 0.4767(3) 0.10183(14) 0.0396(10) Uani 1 1 d . . .
C17 C 0.4827(2) 0.3550(2) 0.23797(13) 0.0326(9) Uani 1 1 d . . .
H17 H 0.4332 0.3619 0.2222 0.039 Uiso 1 1 calc R . .
C18 C 0.4948(2) 0.2963(2) 0.28384(14) 0.0377(10) Uani 1 1 d . . .
H18 H 0.5445 0.2879 0.2977 0.045 Uiso 1 1 calc R . .
C19 C 0.6606(2) 0.4681(3) 0.39059(14) 0.0389(10) Uani 1 1 d . . .
N4 N 0.54739(16) 0.5573(2) 0.17601(11) 0.0295(7) Uani 1 1 d . . .
C21 C 0.2596(2) 0.5196(3) 0.08546(16) 0.0574(13) Uani 1 1 d . . .
H21A H 0.2476 0.5456 0.0532 0.086 Uiso 1 1 calc R . .
H21B H 0.2930 0.5603 0.1073 0.086 Uiso 1 1 calc R . .
H21C H 0.2195 0.5162 0.0955 0.086 Uiso 1 1 calc R . .
C22 C 0.5403(2) 0.5173(3) 0.13519(15) 0.0386(10) Uani 1 1 d . . .
H22 H 0.5795 0.5141 0.1258 0.046 Uiso 1 1 calc R . .
C23 C 0.5315(2) 0.7323(2) 0.36112(13) 0.0391(10) Uani 1 1 d . . .
H23 H 0.4938 0.7227 0.3745 0.047 Uiso 1 1 calc R . .
N1 N 0.57111(18) 0.6423(2) 0.36898(11) 0.0356(8) Uani 1 1 d . . .
C25 C 0.4137(2) 0.3654(3) 0.37927(13) 0.0342(10) Uani 1 1 d . . .
C26 C 0.4725(2) 0.8814(2) 0.15083(13) 0.0316(9) Uani 1 1 d . . .
C27 C 0.34186(19) 0.5485(3) 0.25653(14) 0.0341(9) Uani 1 1 d . . .
H27 H 0.3503 0.5985 0.2815 0.041 Uiso 1 1 calc R . .
C28 C 0.62286(19) 0.5665(3) 0.25809(13) 0.0331(9) Uani 1 1 d . . .
H28 H 0.6248 0.4965 0.2620 0.040 Uiso 1 1 calc R . .
C29 C 0.7429(3) 0.5757(4) 0.44457(16) 0.0600(13) Uani 1 1 d . . .
H29 H 0.7540 0.6365 0.4580 0.072 Uiso 1 1 calc R . .
C30 C 0.3680(2) 0.8126(3) 0.15996(13) 0.0335(9) Uani 1 1 d . . .
C31 C 0.4395(2) 0.3189(3) 0.34385(14) 0.0382(10) Uani 1 1 d . . .
H31 H 0.4300 0.2536 0.3391 0.046 Uiso 1 1 calc R . .
C32 C 0.3964(2) 0.5035(3) 0.42573(13) 0.0356(10) Uani 1 1 d . . .
C33 C 0.6773(2) 0.5552(4) 0.19241(15) 0.0516(12) Uani 1 1 d . . .
H33A H 0.6732 0.5755 0.1596 0.062 Uiso 1 1 calc R . .
H33B H 0.6785 0.4855 0.1932 0.062 Uiso 1 1 calc R . .
C34 C 0.3326(2) 0.8953(3) 0.14027(14) 0.0410(10) Uani 1 1 d . . .
H34 H 0.2861 0.8992 0.1366 0.049 Uiso 1 1 calc R . .
C35 C 0.3758(2) 0.3096(3) 0.40158(13) 0.0403(10) Uani 1 1 d . . .
H35 H 0.3688 0.2450 0.3932 0.048 Uiso 1 1 calc R . .
C36 C 0.4070(2) 0.6100(3) 0.44080(14) 0.0405(10) Uani 1 1 d . . .
O8 O 0.59975(14) 0.45386(17) 0.35720(9) 0.0385(7) Uani 1 1 d . . .
C38 C 0.3595(2) 0.4428(3) 0.44619(14) 0.0420(10) Uani 1 1 d . . .
H38 H 0.3409 0.4686 0.4688 0.050 Uiso 1 1 calc R . .
C39 C 0.30421(19) 0.5915(3) 0.20779(14) 0.0364(10) Uani 1 1 d . . .
H39 H 0.2959 0.5386 0.1843 0.044 Uiso 1 1 calc R . .
C40 C 0.6778(2) 0.5594(3) 0.41140(14) 0.0425(10) Uani 1 1 d . . .
C41 C 0.3485(2) 0.3456(3) 0.43499(14) 0.0421(10) Uani 1 1 d . . .
C42 C 0.2897(2) 0.4181(3) 0.08597(15) 0.0488(11) Uani 1 1 d . . .
C43 C 0.5479(2) 0.8756(3) 0.15461(15) 0.0423(10) Uani 1 1 d . . .
C44 C 0.3598(2) 0.4252(3) 0.07800(14) 0.0424(11) Uani 1 1 d . . .
C45 C 0.4334(2) 0.9615(3) 0.13194(14) 0.0414(10) Uani 1 1 d . . .
H45 H 0.4551 1.0128 0.1224 0.050 Uiso 1 1 calc R . .
C46 C 0.3715(2) 0.6730(3) 0.39659(16) 0.0540(12) Uani 1 1 d . . .
H46A H 0.3230 0.6624 0.3869 0.081 Uiso 1 1 calc R . .
H46B H 0.3883 0.6565 0.3703 0.081 Uiso 1 1 calc R . .
H46C H 0.3811 0.7394 0.4049 0.081 Uiso 1 1 calc R . .
C47 C 0.3637(2) 0.9709(3) 0.12615(15) 0.0455(11) Uani 1 1 d . . .
C48 C 0.6321(2) 0.6402(3) 0.39948(14) 0.0408(10) Uani 1 1 d . . .
H48 H 0.6484 0.6973 0.4156 0.049 Uiso 1 1 calc R . .
C51 C 0.7093(2) 0.3932(3) 0.40453(15) 0.0478(11) Uani 1 1 d . . .
C52 C 0.7499(2) 0.5727(3) 0.28025(17) 0.0575(13) Uani 1 1 d . . .
H52A H 0.7541 0.5039 0.2857 0.069 Uiso 1 1 calc R . .
H52B H 0.7909 0.6029 0.3015 0.069 Uiso 1 1 calc R . .
C53 C 0.2975(3) 0.3663(3) 0.13468(16) 0.0589(13) Uani 1 1 d . . .
H53A H 0.2539 0.3647 0.1403 0.088 Uiso 1 1 calc R . .
H53B H 0.3300 0.4002 0.1607 0.088 Uiso 1 1 calc R . .
H53C H 0.3133 0.3018 0.1332 0.088 Uiso 1 1 calc R . .
C54 C 0.3707(3) 0.3860(3) 0.03709(17) 0.0621(14) Uani 1 1 d . . .
H54 H 0.3340 0.3549 0.0149 0.075 Uiso 1 1 calc R . .
C55 C 0.4877(3) 0.9202(3) 0.31628(18) 0.0664(15) Uani 1 1 d . . .
H55A H 0.4556 0.9735 0.3093 0.080 Uiso 1 1 calc R . .
H55B H 0.5232 0.9343 0.3018 0.080 Uiso 1 1 calc R . .
C58 C 0.4994(2) 0.7438(2) 0.30628(14) 0.0358(10) Uani 1 1 d . . .
H58 H 0.5359 0.7546 0.2919 0.043 Uiso 1 1 calc R . .
C56 C 0.3301(2) 0.7394(3) 0.17550(13) 0.0376(10) Uani 1 1 d . . .
H56 H 0.2842 0.7528 0.1709 0.045 Uiso 1 1 calc R . .
C60 C 0.5199(3) 0.9092(3) 0.37144(19) 0.0781(17) Uani 1 1 d . . .
H60A H 0.5447 0.9674 0.3847 0.094 Uiso 1 1 calc R . .
H60B H 0.4839 0.9005 0.3861 0.094 Uiso 1 1 calc R . .
C57 C 0.4504(2) 0.8286(3) 0.29412(16) 0.0471(11) Uani 1 1 d . . .
H57A H 0.4126 0.8170 0.3067 0.057 Uiso 1 1 calc R . .
H57B H 0.4318 0.8357 0.2592 0.057 Uiso 1 1 calc R . .
C59 C 0.5687(3) 0.8239(3) 0.38415(17) 0.0658(14) Uani 1 1 d . . .
H59A H 0.5862 0.8164 0.4191 0.079 Uiso 1 1 calc R . .
H59B H 0.6073 0.8354 0.3724 0.079 Uiso 1 1 calc R . .
C74 C 0.5134(2) 0.3053(3) 0.20340(15) 0.0453(11) Uani 1 1 d . . .
H74A H 0.5628 0.3013 0.2180 0.054 Uiso 1 1 calc R . .
H74B H 0.5038 0.3423 0.1737 0.054 Uiso 1 1 calc R . .
C65 C 0.6877(2) 0.6096(3) 0.29231(14) 0.0447(11) Uani 1 1 d . . .
H65A H 0.6857 0.6791 0.2896 0.054 Uiso 1 1 calc R . .
H65B H 0.6916 0.5927 0.3255 0.054 Uiso 1 1 calc R . .
C72 C 0.2997(2) 0.4685(3) 0.26860(16) 0.0485(11) Uani 1 1 d . . .
H72A H 0.3234 0.4440 0.3008 0.058 Uiso 1 1 calc R . .
H72B H 0.2950 0.4163 0.2457 0.058 Uiso 1 1 calc R . .
C67 C 0.6935(2) 0.2922(3) 0.38241(16) 0.0536(12) Uani 1 1 d . . .
C71 C 0.2339(2) 0.6297(3) 0.20571(18) 0.0566(13) Uani 1 1 d . . .
H71A H 0.2104 0.6544 0.1735 0.068 Uiso 1 1 calc R . .
H71B H 0.2389 0.6817 0.2288 0.068 Uiso 1 1 calc R . .
C73 C 0.4641(3) 0.1958(3) 0.27251(16) 0.0555(13) Uani 1 1 d . . .
H73A H 0.4740 0.1589 0.3023 0.067 Uiso 1 1 calc R . .
H73B H 0.4148 0.2003 0.2582 0.067 Uiso 1 1 calc R . .
C70 C 0.3760(3) 0.6353(3) 0.48090(16) 0.0611(13) Uani 1 1 d . . .
H70A H 0.3847 0.7018 0.4896 0.092 Uiso 1 1 calc R . .
H70B H 0.3965 0.5959 0.5088 0.092 Uiso 1 1 calc R . .
H70C H 0.3275 0.6243 0.4694 0.092 Uiso 1 1 calc R . .
C63 C 0.5917(2) 0.8643(3) 0.20818(16) 0.0531(12) Uani 1 1 d . . .
H63A H 0.5895 0.9223 0.2255 0.080 Uiso 1 1 calc R . .
H63B H 0.6384 0.8518 0.2101 0.080 Uiso 1 1 calc R . .
H63C H 0.5746 0.8117 0.2223 0.080 Uiso 1 1 calc R . .
C64 C 0.7435(2) 0.5944(4) 0.22731(17) 0.0624(14) Uani 1 1 d . . .
H64A H 0.7451 0.6634 0.2230 0.075 Uiso 1 1 calc R . .
H64B H 0.7821 0.5663 0.2198 0.075 Uiso 1 1 calc R . .
C68 C 0.7909(3) 0.5032(4) 0.45760(18) 0.0666(14) Uani 1 1 d . . .
C69 C 0.4844(2) 0.6311(3) 0.46111(15) 0.0496(11) Uani 1 1 d . . .
H69A H 0.4914 0.6990 0.4662 0.074 Uiso 1 1 calc R . .
H69B H 0.5065 0.6095 0.4384 0.074 Uiso 1 1 calc R . .
H69C H 0.5035 0.5980 0.4914 0.074 Uiso 1 1 calc R . .
C62 C 0.5738(3) 0.9672(3) 0.1354(2) 0.0657(14) Uani 1 1 d . . .
H62A H 0.5475 0.9770 0.1019 0.099 Uiso 1 1 calc R . .
H62B H 0.6213 0.9594 0.1381 0.099 Uiso 1 1 calc R . .
H62C H 0.5687 1.0217 0.1542 0.099 Uiso 1 1 calc R . .
C75 C 0.4853(3) 0.4364(3) 0.05917(16) 0.0585(13) Uani 1 1 d . . .
H75 H 0.5267 0.4415 0.0527 0.070 Uiso 1 1 calc R . .
C61 C 0.3251(3) 1.0623(3) 0.1052(2) 0.0693(15) Uani 1 1 d . . .
H61A H 0.2918 1.0484 0.0743 0.104 Uiso 1 1 calc R . .
H61B H 0.3568 1.1095 0.1010 0.104 Uiso 1 1 calc R . .
H61C H 0.3024 1.0867 0.1270 0.104 Uiso 1 1 calc R . .
C66 C 0.6828(3) 0.2989(3) 0.32726(16) 0.0599(13) Uani 1 1 d . . .
H66A H 0.6482 0.3460 0.3129 0.090 Uiso 1 1 calc R . .
H66B H 0.6685 0.2375 0.3124 0.090 Uiso 1 1 calc R . .
H66C H 0.7250 0.3173 0.3222 0.090 Uiso 1 1 calc R . .
C110 C 0.5588(2) 0.7916(3) 0.12380(15) 0.0509(12) Uani 1 1 d . . .
H11A H 0.5389 0.7345 0.1322 0.076 Uiso 1 1 calc R . .
H11B H 0.6070 0.7819 0.1299 0.076 Uiso 1 1 calc R . .
H11C H 0.5373 0.8059 0.0900 0.076 Uiso 1 1 calc R . .
C108 C 0.7719(3) 0.4138(4) 0.43776(18) 0.0634(14) Uani 1 1 d . . .
H108 H 0.8035 0.3641 0.4475 0.076 Uiso 1 1 calc R . .
C101 C 0.4319(3) 0.3897(4) 0.02682(17) 0.0686(15) Uani 1 1 d . . .
C106 C 0.6310(2) 0.2510(3) 0.39324(17) 0.0598(13) Uani 1 1 d . . .
H10A H 0.6423 0.2387 0.4274 0.090 Uiso 1 1 calc R . .
H10B H 0.6174 0.1921 0.3756 0.090 Uiso 1 1 calc R . .
H10C H 0.5940 0.2963 0.3835 0.090 Uiso 1 1 calc R . .
C100 C 0.2376(3) 0.3596(4) 0.04617(18) 0.0765(16) Uani 1 1 d . . .
H10D H 0.2541 0.2950 0.0462 0.115 Uiso 1 1 calc R . .
H10E H 0.2318 0.3885 0.0151 0.115 Uiso 1 1 calc R . .
H10F H 0.1944 0.3586 0.0524 0.115 Uiso 1 1 calc R . .
C104 C 0.2286(2) 0.5043(3) 0.26673(19) 0.0630(14) Uani 1 1 d . . .
H10G H 0.2018 0.4511 0.2726 0.076 Uiso 1 1 calc R . .
H10H H 0.2330 0.5518 0.2920 0.076 Uiso 1 1 calc R . .
C105 C 0.3076(3) 0.2841(3) 0.45865(17) 0.0633(14) Uani 1 1 d . . .
H10I H 0.2984 0.2231 0.4425 0.095 Uiso 1 1 calc R . .
H10J H 0.2652 0.3156 0.4563 0.095 Uiso 1 1 calc R . .
H10K H 0.3334 0.2745 0.4922 0.095 Uiso 1 1 calc R . .
C107 C 0.7525(3) 0.2210(4) 0.4036(2) 0.0825(17) Uani 1 1 d . . .
H10L H 0.7921 0.2417 0.3955 0.124 Uiso 1 1 calc R . .
H10M H 0.7390 0.1583 0.3901 0.124 Uiso 1 1 calc R . .
H10N H 0.7632 0.2185 0.4382 0.124 Uiso 1 1 calc R . .
C103 C 0.1924(2) 0.5483(4) 0.2178(2) 0.0674(14) Uani 1 1 d . . .
H10O H 0.1482 0.5729 0.2177 0.081 Uiso 1 1 calc R . .
H10P H 0.1844 0.4991 0.1930 0.081 Uiso 1 1 calc R . .
C109 C 0.8621(3) 0.5221(5) 0.4929(2) 0.098(2) Uani 1 1 d . . .
H10Q H 0.8793 0.4646 0.5109 0.147 Uiso 1 1 calc R . .
H10R H 0.8596 0.5724 0.5150 0.147 Uiso 1 1 calc R . .
H10S H 0.8922 0.5413 0.4752 0.147 Uiso 1 1 calc R . .
C102 C 0.4379(3) 0.3422(5) -0.0187(2) 0.117(3) Uani 1 1 d . . .
H10T H 0.4064 0.3719 -0.0468 0.176 Uiso 1 1 calc R . .
H10U H 0.4273 0.2751 -0.0184 0.176 Uiso 1 1 calc R . .
H10V H 0.4838 0.3496 -0.0198 0.176 Uiso 1 1 calc R . .
C111 C 0.4837(3) 0.2048(3) 0.19173(16) 0.0629(14) Uani 1 1 d . . .
H11D H 0.5055 0.1726 0.1709 0.075 Uiso 1 1 calc R . .
H11E H 0.4351 0.2094 0.1743 0.075 Uiso 1 1 calc R . .
C112 C 0.4942(3) 0.1458(3) 0.23761(17) 0.0699(16) Uani 1 1 d . . .
H11F H 0.4726 0.0835 0.2291 0.084 Uiso 1 1 calc R . .
H11G H 0.5428 0.1355 0.2533 0.084 Uiso 1 1 calc R . .


_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
O1 C28 1.426(4) . ?
O1 Zr1 2.180(2) . ?
O1 Zr2 2.376(2) . ?
Zr1 O6 2.072(2) . ?
Zr1 O7 2.071(2) . ?
Zr1 O3 2.196(2) . ?
Zr1 O2 2.335(2) . ?
Zr1 O4 2.341(2) . ?
Zr1 N4 2.369(3) . ?
Zr1 N2 2.371(3) . ?
Zr1 Zr2 3.0281(5) . ?
Zr2 O5 2.061(2) . ?
Zr2 O8 2.064(3) . ?
Zr2 O4 2.179(2) . ?
Zr2 O2 2.179(2) . ?
Zr2 O3 2.334(2) . ?
Zr2 N1 2.377(3) . ?
Zr2 N3 2.385(3) . ?
O3 C27 1.418(4) . ?
O2 C58 1.417(4) . ?
O4 C17 1.411(4) . ?
C6 O7 1.328(4) . ?
C6 C16 1.406(6) . ?
C6 C44 1.434(6) . ?
C7 N4 1.476(5) . ?
C7 C28 1.518(5) . ?
C7 C33 1.513(5) . ?
O6 C15 1.336(4) . ?
N2 C56 1.283(5) . ?
N2 C39 1.478(5) . ?
O5 C14 1.336(4) . ?
N3 C31 1.268(5) . ?
N3 C18 1.476(4) . ?
C14 C25 1.408(5) . ?
C14 C32 1.422(5) . ?
C15 C30 1.414(5) . ?
C15 C26 1.424(5) . ?
C16 C75 1.400(6) . ?
C16 C22 1.436(6) . ?
C17 C74 1.512(5) . ?
C17 C18 1.514(5) . ?
C18 C73 1.527(5) . ?
C19 O8 1.335(5) . ?
C19 C40 1.403(6) . ?
C19 C51 1.414(6) . ?
N4 C22 1.275(5) . ?
C21 C42 1.541(6) . ?
C23 N1 1.472(5) . ?
C23 C58 1.528(5) . ?
C23 C59 1.528(5) . ?
N1 C48 1.288(5) . ?
C25 C35 1.398(5) . ?
C25 C31 1.449(5) . ?
C26 C45 1.383(5) . ?
C26 C43 1.523(6) . ?
C27 C39 1.506(5) . ?
C27 C72 1.517(5) . ?
C28 C65 1.513(5) . ?
C29 C68 1.379(7) . ?
C29 C40 1.401(6) . ?
C30 C34 1.386(5) . ?
C30 C56 1.439(5) . ?
C32 C38 1.389(5) . ?
C32 C36 1.542(5) . ?
C33 C64 1.519(6) . ?
C34 C47 1.360(5) . ?
C35 C41 1.360(5) . ?
C36 C70 1.534(5) . ?
C36 C46 1.535(6) . ?
C36 C69 1.541(6) . ?
C38 C41 1.393(6) . ?
C39 C71 1.524(5) . ?
C40 C48 1.436(6) . ?
C41 C105 1.508(5) . ?
C42 C44 1.533(6) . ?
C42 C100 1.539(6) . ?
C42 C53 1.550(6) . ?
C43 C110 1.530(5) . ?
C43 C63 1.540(6) . ?
C43 C62 1.552(5) . ?
C44 C54 1.388(6) . ?
C45 C47 1.396(6) . ?
C47 C61 1.521(6) . ?
C51 C108 1.373(7) . ?
C51 C67 1.537(6) . ?
C52 C65 1.519(6) . ?
C52 C64 1.531(6) . ?
C54 C101 1.382(7) . ?
C55 C57 1.523(6) . ?
C55 C60 1.535(7) . ?
C58 C57 1.520(5) . ?
C60 C59 1.524(7) . ?
C74 C111 1.521(5) . ?
C72 C104 1.530(6) . ?
C67 C106 1.528(6) . ?
C67 C107 1.537(6) . ?
C67 C66 1.549(6) . ?
C71 C103 1.524(6) . ?
C73 C112 1.513(6) . ?
C68 C108 1.375(7) . ?
C68 C109 1.523(7) . ?
C75 C101 1.365(6) . ?
C101 C102 1.518(6) . ?
C104 C103 1.510(7) . ?
C111 C112 1.522(6) . ?

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
C28 O1 Zr1 120.3(2) . . ?
C28 O1 Zr2 123.5(2) . . ?
Zr1 O1 Zr2 83.20(8) . . ?
O6 Zr1 O7 100.74(9) . . ?
O6 Zr1 O1 92.15(9) . . ?
O7 Zr1 O1 141.81(9) . . ?
O6 Zr1 O3 141.93(9) . . ?
O7 Zr1 O3 90.47(9) . . ?
O1 Zr1 O3 101.20(9) . . ?
O6 Zr1 O2 91.97(8) . . ?
O7 Zr1 O2 149.60(9) . . ?
O1 Zr1 O2 63.84(8) . . ?
O3 Zr1 O2 63.64(8) . . ?
O6 Zr1 O4 150.70(9) . . ?
O7 Zr1 O4 90.71(9) . . ?
O1 Zr1 O4 63.58(8) . . ?
O3 Zr1 O4 63.70(8) . . ?
O2 Zr1 O4 91.42(8) . . ?
O6 Zr1 N4 79.38(9) . . ?
O7 Zr1 N4 75.87(10) . . ?
O1 Zr1 N4 71.41(9) . . ?
O3 Zr1 N4 138.65(9) . . ?
O2 Zr1 N4 134.04(10) . . ?
O4 Zr1 N4 77.42(9) . . ?
O6 Zr1 N2 75.83(10) . . ?
O7 Zr1 N2 78.48(10) . . ?
O1 Zr1 N2 139.70(9) . . ?
O3 Zr1 N2 70.96(9) . . ?
O2 Zr1 N2 78.06(9) . . ?
O4 Zr1 N2 133.23(9) . . ?
N4 Zr1 N2 139.98(10) . . ?
O6 Zr1 Zr2 130.83(7) . . ?
O7 Zr1 Zr2 128.42(7) . . ?
O1 Zr1 Zr2 51.18(6) . . ?
O3 Zr1 Zr2 50.02(6) . . ?
O2 Zr1 Zr2 45.73(6) . . ?
O4 Zr1 Zr2 45.70(5) . . ?
N4 Zr1 Zr2 110.38(7) . . ?
N2 Zr1 Zr2 109.62(7) . . ?
O5 Zr2 O8 99.78(10) . . ?
O5 Zr2 O4 141.97(9) . . ?
O8 Zr2 O4 91.62(9) . . ?
O5 Zr2 O2 92.54(9) . . ?
O8 Zr2 O2 142.21(10) . . ?
O4 Zr2 O2 100.34(8) . . ?
O5 Zr2 O3 90.96(9) . . ?
O8 Zr2 O3 150.10(9) . . ?
O4 Zr2 O3 64.07(8) . . ?
O2 Zr2 O3 63.89(8) . . ?
O5 Zr2 N1 81.02(10) . . ?
O8 Zr2 N1 75.65(11) . . ?
O4 Zr2 N1 137.01(10) . . ?
O2 Zr2 N1 71.20(10) . . ?
O3 Zr2 N1 133.93(10) . . ?
O5 Zr2 O1 151.00(8) . . ?
O8 Zr2 O1 92.05(9) . . ?
O4 Zr2 O1 62.99(8) . . ?
O2 Zr2 O1 63.13(8) . . ?
O3 Zr2 O1 91.75(8) . . ?
N1 Zr2 O1 76.40(9) . . ?
O5 Zr2 N3 75.89(10) . . ?
O8 Zr2 N3 78.96(11) . . ?
O4 Zr2 N3 70.88(9) . . ?
O2 Zr2 N3 138.83(10) . . ?
O3 Zr2 N3 76.74(9) . . ?
N1 Zr2 N3 141.95(10) . . ?
O1 Zr2 N3 132.70(9) . . ?
O5 Zr2 Zr1 129.96(7) . . ?
O8 Zr2 Zr1 130.26(7) . . ?
O4 Zr2 Zr1 50.25(6) . . ?
O2 Zr2 Zr1 50.09(6) . . ?
O3 Zr2 Zr1 46.13(6) . . ?
N1 Zr2 Zr1 109.00(7) . . ?
O1 Zr2 Zr1 45.62(6) . . ?
N3 Zr2 Zr1 109.02(7) . . ?
C27 O3 Zr1 121.1(2) . . ?
C27 O3 Zr2 125.5(2) . . ?
Zr1 O3 Zr2 83.85(8) . . ?
C58 O2 Zr2 121.2(2) . . ?
C58 O2 Zr1 123.5(2) . . ?
Zr2 O2 Zr1 84.18(7) . . ?
C17 O4 Zr2 121.87(19) . . ?
C17 O4 Zr1 124.4(2) . . ?
Zr2 O4 Zr1 84.05(7) . . ?
O7 C6 C16 120.3(4) . . ?
O7 C6 C44 121.0(3) . . ?
C16 C6 C44 118.6(3) . . ?
N4 C7 C28 106.7(3) . . ?
N4 C7 C33 118.0(3) . . ?
C28 C7 C33 111.3(3) . . ?
C15 O6 Zr1 144.6(2) . . ?
C6 O7 Zr1 144.2(2) . . ?
C56 N2 C39 119.9(3) . . ?
C56 N2 Zr1 129.0(3) . . ?
C39 N2 Zr1 111.1(2) . . ?
C14 O5 Zr2 145.0(2) . . ?
C31 N3 C18 120.4(3) . . ?
C31 N3 Zr2 128.4(2) . . ?
C18 N3 Zr2 111.2(2) . . ?
O5 C14 C25 119.6(3) . . ?
O5 C14 C32 121.4(3) . . ?
C25 C14 C32 119.0(3) . . ?
O6 C15 C30 119.9(3) . . ?
O6 C15 C26 121.4(3) . . ?
C30 C15 C26 118.7(3) . . ?
C75 C16 C6 120.6(4) . . ?
C75 C16 C22 116.9(4) . . ?
C6 C16 C22 122.5(3) . . ?
O4 C17 C74 111.5(3) . . ?
O4 C17 C18 108.2(3) . . ?
C74 C17 C18 110.4(3) . . ?
N3 C18 C17 107.2(3) . . ?
N3 C18 C73 117.9(3) . . ?
C17 C18 C73 111.3(3) . . ?
O8 C19 C40 119.9(4) . . ?
O8 C19 C51 121.1(4) . . ?
C40 C19 C51 119.0(4) . . ?
C22 N4 C7 119.2(3) . . ?
C22 N4 Zr1 128.7(3) . . ?
C7 N4 Zr1 112.1(2) . . ?
N4 C22 C16 128.2(4) . . ?
N1 C23 C58 106.7(3) . . ?
N1 C23 C59 117.8(4) . . ?
C58 C23 C59 111.2(3) . . ?
C48 N1 C23 119.9(3) . . ?
C48 N1 Zr2 129.0(3) . . ?
C23 N1 Zr2 111.1(2) . . ?
C35 C25 C14 119.6(3) . . ?
C35 C25 C31 117.5(3) . . ?
C14 C25 C31 122.8(3) . . ?
C45 C26 C15 116.9(4) . . ?
C45 C26 C43 121.6(3) . . ?
C15 C26 C43 121.5(3) . . ?
O3 C27 C39 107.6(3) . . ?
O3 C27 C72 111.0(3) . . ?
C39 C27 C72 110.3(3) . . ?
O1 C28 C7 108.3(3) . . ?
O1 C28 C65 111.4(3) . . ?
C7 C28 C65 110.8(3) . . ?
C68 C29 C40 121.1(5) . . ?
C34 C30 C15 120.5(3) . . ?
C34 C30 C56 116.8(4) . . ?
C15 C30 C56 122.7(3) . . ?
N3 C31 C25 128.3(3) . . ?
C38 C32 C14 117.5(3) . . ?
C38 C32 C36 120.8(3) . . ?
C14 C32 C36 121.7(3) . . ?
C7 C33 C64 110.9(3) . . ?
C47 C34 C30 122.1(4) . . ?
C41 C35 C25 122.8(4) . . ?
C70 C36 C46 107.6(3) . . ?
C70 C36 C32 112.4(3) . . ?
C46 C36 C32 108.9(3) . . ?
C70 C36 C69 107.0(3) . . ?
C46 C36 C69 111.9(3) . . ?
C32 C36 C69 109.2(3) . . ?
C19 O8 Zr2 144.8(2) . . ?
C32 C38 C41 124.2(4) . . ?
N2 C39 C27 107.5(3) . . ?
N2 C39 C71 117.8(3) . . ?
C27 C39 C71 112.1(3) . . ?
C19 C40 C29 120.0(4) . . ?
C19 C40 C48 123.3(4) . . ?
C29 C40 C48 116.7(4) . . ?
C35 C41 C38 116.9(4) . . ?
C35 C41 C105 122.0(4) . . ?
C38 C41 C105 121.2(4) . . ?
C44 C42 C21 109.5(3) . . ?
C44 C42 C100 112.7(3) . . ?
C21 C42 C100 107.2(4) . . ?
C44 C42 C53 109.6(4) . . ?
C21 C42 C53 111.2(4) . . ?
C100 C42 C53 106.6(4) . . ?
C110 C43 C26 109.4(3) . . ?
C110 C43 C63 111.5(3) . . ?
C26 C43 C63 109.7(3) . . ?
C110 C43 C62 106.7(3) . . ?
C26 C43 C62 112.8(3) . . ?
C63 C43 C62 106.8(4) . . ?
C54 C44 C6 116.8(4) . . ?
C54 C44 C42 121.1(4) . . ?
C6 C44 C42 122.1(3) . . ?
C26 C45 C47 124.8(4) . . ?
C34 C47 C45 116.9(4) . . ?
C34 C47 C61 122.2(4) . . ?
C45 C47 C61 120.9(4) . . ?
N1 C48 C40 127.2(4) . . ?
C108 C51 C19 118.0(4) . . ?
C108 C51 C67 120.9(4) . . ?
C19 C51 C67 121.1(4) . . ?
C65 C52 C64 110.6(4) . . ?
C44 C54 C101 125.0(4) . . ?
C57 C55 C60 110.6(4) . . ?
O2 C58 C57 111.5(3) . . ?
O2 C58 C23 107.5(3) . . ?
C57 C58 C23 111.1(3) . . ?
N2 C56 C30 128.0(4) . . ?
C59 C60 C55 111.4(4) . . ?
C58 C57 C55 110.1(4) . . ?
C60 C59 C23 110.1(4) . . ?
C17 C74 C111 110.2(3) . . ?
C52 C65 C28 110.3(3) . . ?
C27 C72 C104 111.2(3) . . ?
C106 C67 C51 109.8(3) . . ?
C106 C67 C107 106.6(4) . . ?
C51 C67 C107 112.7(4) . . ?
C106 C67 C66 112.4(4) . . ?
C51 C67 C66 108.6(3) . . ?
C107 C67 C66 106.8(4) . . ?
C39 C71 C103 109.0(3) . . ?
C112 C73 C18 109.7(4) . . ?
C33 C64 C52 112.0(4) . . ?
C108 C68 C29 117.6(5) . . ?
C108 C68 C109 121.7(5) . . ?
C29 C68 C109 120.7(5) . . ?
C101 C75 C16 121.5(4) . . ?
C68 C108 C51 124.3(5) . . ?
C75 C101 C54 117.4(4) . . ?
C75 C101 C102 122.5(5) . . ?
C54 C101 C102 120.1(5) . . ?
C103 C104 C72 110.4(4) . . ?
C104 C103 C71 111.9(4) . . ?
C74 C111 C112 111.4(4) . . ?
C73 C112 C111 111.2(4) . . ?

_diffrn_measured_fraction_theta_max 0.996
_diffrn_reflns_theta_full        21.97
_diffrn_measured_fraction_theta_full 0.996
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.449
_refine_diff_density_rms         0.067
# SQUEEZE RESULTS
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.000 0.500 834 150 ' '
2 1.000 0.500 0.000 835 149 ' '
3 0.711 0.222 0.697 9 1 ' '
4 0.211 0.278 0.197 9 1 ' '
5 0.789 0.722 0.803 9 1 ' '
6 0.289 0.778 0.303 9 1 ' '
_platon_squeeze_details          ?
# start Validation Reply Form
_vrf_THETM01_I                   
;
PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550
RESPONSE: The crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.

;
_vrf_PLAT023_I                   
;
PROBLEM: Resolution (too) Low [sin(theta)/Lambda < 0.6]..      21.97 Degree
RESPONSE: The crystal (the largest available) still 
diffracted quite weakly at high angle. On repeated recrystallisation
we could get only small sized crystals.

;
# end Validation Reply Form
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_solvent_exptl_crystal_recrystallization_method Toluene
