# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

####################################################################### 
# 
# 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_a
_database_code_depnum_ccdc_archive 'CCDC 1572540'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H164 O44 Ti10'
_chemical_formula_weight         2597.34

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

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

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

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

_cell_length_a                   17.2643(4)
_cell_length_b                   18.9646(4)
_cell_length_c                   19.8713(4)
_cell_angle_alpha                90
_cell_angle_beta                 99.975(2)
_cell_angle_gamma                90
_cell_volume                     6407.7(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10958
_cell_measurement_theta_min      74.3570
_cell_measurement_theta_max      4.366

_exptl_crystal_description       block
_exptl_crystal_colour            pale
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_F_000             2720
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.675
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.35937
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.653
_oxdiff_exptl_absorpt_empirical_full_max 2.023
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_reflns_number            25972
_diffrn_reflns_av_unetI/netI     0.0473
_diffrn_reflns_av_R_equivalents  0.0436
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         3.491
_diffrn_reflns_theta_max         74.598
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             12728
_reflns_number_gt                10572
_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1221P)²+12.6746P] 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         12728
_refine_ls_number_parameters     712
_refine_ls_number_restraints     13
_refine_ls_R_factor_all          0.0856
_refine_ls_R_factor_gt           0.0737
_refine_ls_wR_factor_ref         0.2181
_refine_ls_wR_factor_gt          0.2034
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.057
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.18211(4) 0.30116(4) 0.38494(4) 0.02701(17) Uani 1 1 d . . . . .
Ti2 Ti 0.17225(4) 0.13557(4) 0.32514(4) 0.02933(18) Uani 1 1 d . . . . .
Ti3 Ti 0.29417(4) -0.01679(4) 0.40418(4) 0.03001(18) Uani 1 1 d . . . . .
Ti4 Ti 0.33425(4) 0.08079(4) 0.30252(4) 0.03183(19) Uani 1 1 d . . . . .
Ti5 Ti 0.28921(4) -0.18065(4) 0.34298(4) 0.0339(2) Uani 1 1 d . . . . .
O1 O 0.23999(15) 0.06235(14) 0.35549(14) 0.0282(6) Uani 1 1 d . . . . .
O2 O 0.37678(16) 0.01545(15) 0.36230(15) 0.0325(6) Uani 1 1 d . . . . .
O3 O 0.25517(15) 0.21027(14) 0.38374(14) 0.0267(5) Uani 1 1 d . . . . .
O4 O 0.13105(16) 0.23765(14) 0.45488(14) 0.0306(6) Uani 1 1 d . . . . .
O5 O 0.26069(16) -0.07579(14) 0.30772(15) 0.0311(6) Uani 1 1 d . . . . .
O6 O 0.18633(18) -0.05505(15) 0.41901(17) 0.0378(7) Uani 1 1 d . . . . .
O7 O 0.28102(18) 0.00679(15) 0.23431(15) 0.0343(6) Uani 1 1 d . . . . .
O8 O 0.26109(17) 0.32425(16) 0.46202(16) 0.0359(6) Uani 1 1 d . . . . .
O9 O 0.33390(18) -0.11484(15) 0.42168(16) 0.0352(6) Uani 1 1 d . . . . .
O10 O 0.24312(18) 0.14651(15) 0.25870(15) 0.0340(6) Uani 1 1 d . . . . .
O11 O 0.12314(17) 0.12919(15) 0.41064(16) 0.0360(7) Uani 1 1 d . . . . .
O12 O 0.36858(17) 0.16315(15) 0.36752(15) 0.0330(6) Uani 1 1 d . . . . .
O13 O 0.18395(18) -0.16736(16) 0.38353(17) 0.0380(7) Uani 1 1 d . . . . .
O14 O 0.22072(18) -0.20454(16) 0.25924(18) 0.0398(7) Uani 1 1 d . . . . .
O15 O 0.11269(18) 0.36678(15) 0.40157(15) 0.0342(6) Uani 1 1 d . . . . .
O16 O 0.3169(2) 0.01849(16) 0.48670(16) 0.0388(7) Uani 1 1 d . . . . .
O17 O 0.12544(17) 0.23374(15) 0.31373(15) 0.0344(6) Uani 1 1 d . . . . .
O18 O 0.40877(19) 0.09762(17) 0.25338(17) 0.0417(7) Uani 1 1 d . . . . .
O19 O 0.3000(2) -0.26475(17) 0.3828(2) 0.0486(8) Uani 1 1 d . . . . .
O20 O 0.2301(2) 0.34870(16) 0.32543(18) 0.0441(8) Uani 1 1 d . . . . .
C21 C 0.3309(2) 0.2114(2) 0.3911(2) 0.0287(8) Uani 1 1 d . . . . .
O22 O 0.37692(18) -0.17754(17) 0.30633(18) 0.0426(7) Uani 1 1 d . . . . .
C23 C -0.0470(3) 0.1940(2) 0.5656(2) 0.0327(8) Uani 1 1 d . . . . .
H23A H -0.0625 0.2271 0.5951 0.039 Uiso 1 1 calc R U . . .
C24 C -0.0879(3) 0.1309(2) 0.5537(2) 0.0363(9) Uani 1 1 d . . . . .
C25 C 0.0170(2) 0.2080(2) 0.5337(2) 0.0321(8) Uani 1 1 d . . . . .
H25A H 0.0448 0.2499 0.5425 0.039 Uiso 1 1 calc R U . . .
C26 C 0.0391(3) 0.1591(2) 0.4888(2) 0.0360(9) Uani 1 1 d . . . . .
O27 O 0.0943(2) 0.09370(19) 0.2709(2) 0.0507(9) Uani 1 1 d . . . . .
C28 C 0.0907(3) 0.3910(2) 0.4640(2) 0.0359(9) Uani 1 1 d . . . . .
H28A H 0.1108 0.3574 0.5003 0.043 Uiso 1 1 calc R U . . .
C29 C 0.2612(2) -0.0551(2) 0.2467(2) 0.0325(9) Uani 1 1 d . . . . .
C30 C 0.2187(2) -0.1753(2) 0.1987(3) 0.0403(10) Uani 1 1 d . . . . .
C31 C 0.1031(2) 0.1769(2) 0.4494(2) 0.0314(8) Uani 1 1 d . . . . .
C32 C 0.3379(3) 0.3215(3) 0.4636(3) 0.0428(11) Uani 1 1 d . . . . .
C33 C 0.2356(3) -0.0783(3) 0.1224(3) 0.0435(11) Uani 1 1 d . . . . .
H33A H 0.2486 -0.0314 0.1164 0.052 Uiso 1 1 calc R U . . .
C34 C 0.3892(3) -0.1426(2) 0.4793(2) 0.0389(9) Uani 1 1 d . . . . .
H34A H 0.4113 -0.1861 0.4638 0.047 Uiso 1 1 calc R U . . .
C35 C 0.1581(3) -0.1168(2) 0.4134(2) 0.0362(9) Uani 1 1 d . . . . .
C36 C 0.1298(3) 0.4619(3) 0.4820(3) 0.0473(11) Uani 1 1 d . . . . .
H36A H 0.1158 0.4790 0.5238 0.071 Uiso 1 1 calc R U . . .
H36B H 0.1859 0.4566 0.4878 0.071 Uiso 1 1 calc R U . . .
H36C H 0.1126 0.4949 0.4459 0.071 Uiso 1 1 calc R U . . .
C37 C 0.2385(2) -0.1044(2) 0.1887(2) 0.0371(9) Uani 1 1 d . . . . .
C38 C 0.2141(4) -0.1203(3) 0.0663(3) 0.0555(14) Uani 1 1 d . . . . .
H38A H 0.2128 -0.1024 0.0225 0.067 Uiso 1 1 calc R U . . .
C39 C 0.3751(3) 0.2696(2) 0.4290(3) 0.0401(10) Uani 1 1 d . . . . .
C40 C -0.0015(4) 0.0960(3) 0.4765(4) 0.0621(18) Uani 1 1 d . . . . .
H40A H 0.0133 0.0633 0.4462 0.075 Uiso 1 1 calc R U . . .
C41 C 0.1941(3) -0.1908(3) 0.0759(3) 0.0583(15) Uani 1 1 d . . . . .
H41A H 0.1790 -0.2198 0.0381 0.070 Uiso 1 1 calc R U . . .
C42 C 0.1963(3) -0.2175(3) 0.1401(3) 0.0496(12) Uani 1 1 d . . . . .
H42A H 0.1829 -0.2645 0.1452 0.060 Uiso 1 1 calc R U . . .
C43 C 0.0022(3) 0.3927(3) 0.4560(3) 0.0471(11) Uani 1 1 d . . . . .
H43A H -0.0127 0.4089 0.4977 0.071 Uiso 1 1 calc R U . . .
H43B H -0.0187 0.4241 0.4194 0.071 Uiso 1 1 calc R U . . .
H43C H -0.0184 0.3461 0.4457 0.071 Uiso 1 1 calc R U . . .
C44 C 0.3184(4) 0.0535(3) 0.5509(3) 0.0504(12) Uani 1 1 d . . . . .
H44A H 0.3633 0.0364 0.5839 0.061 Uiso 1 1 calc R U . . .
C45 C 0.4564(3) 0.2725(3) 0.4309(3) 0.0559(15) Uani 1 1 d . . . . .
H45A H 0.4806 0.2378 0.4088 0.067 Uiso 1 1 calc R U . . .
C46 C 0.3263(3) 0.1308(3) 0.5410(3) 0.0507(12) Uani 1 1 d . . . . .
H46A H 0.3273 0.1545 0.5838 0.076 Uiso 1 1 calc R U . . .
H46B H 0.3742 0.1402 0.5243 0.076 Uiso 1 1 calc R U . . .
H46C H 0.2824 0.1474 0.5084 0.076 Uiso 1 1 calc R U . . .
C47 C -0.0644(3) 0.0820(3) 0.5093(4) 0.0592(17) Uani 1 1 d . . . . .
H47A H -0.0912 0.0394 0.5015 0.071 Uiso 1 1 calc R U . . .
C48 C 0.2834(5) -0.3330(3) 0.3990(4) 0.0704(19) Uani 1 1 d . . . . .
H48A H 0.2908 -0.3367 0.4489 0.084 Uiso 1 1 calc R U . . .
C49 C 0.4773(3) 0.0801(4) 0.2279(3) 0.0589(15) Uani 1 1 d . . . . .
H49A H 0.4942 0.1218 0.2052 0.071 Uiso 1 1 calc R U . . .
C50 C 0.4573(3) -0.0928(3) 0.5018(3) 0.0494(12) Uani 1 1 d . . . . .
H50A H 0.4922 -0.1130 0.5397 0.074 Uiso 1 1 calc R U . . .
H50B H 0.4851 -0.0852 0.4646 0.074 Uiso 1 1 calc R U . . .
H50C H 0.4376 -0.0486 0.5153 0.074 Uiso 1 1 calc R U . . .
C51 C 0.4648(4) 0.3762(4) 0.4991(6) 0.100(3) Uani 1 1 d . . . . .
H51A H 0.4946 0.4128 0.5216 0.120 Uiso 1 1 calc R U . . .
C52 C 0.3455(3) -0.1627(3) 0.5358(3) 0.0571(14) Uani 1 1 d . . . . .
H52A H 0.3819 -0.1810 0.5738 0.086 Uiso 1 1 calc R U . . .
H52B H 0.3198 -0.1218 0.5500 0.086 Uiso 1 1 calc R U . . .
H52C H 0.3070 -0.1980 0.5195 0.086 Uiso 1 1 calc R U . . .
C53 C -0.0168(3) 0.2360(4) 0.3054(4) 0.076(2) Uani 1 1 d . . . . .
H53A H -0.0653 0.2456 0.2752 0.115 Uiso 1 1 calc R U . . .
H53B H -0.0164 0.1878 0.3204 0.115 Uiso 1 1 calc R U . . .
H53C H -0.0120 0.2667 0.3443 0.115 Uiso 1 1 calc R U . . .
C57 C 0.0538(5) 0.3212(4) 0.2373(3) 0.080(2) Uani 1 1 d . . . . .
H57A H 0.0050 0.3304 0.2074 0.120 Uiso 1 1 calc R U . . .
H57B H 0.0617 0.3557 0.2732 0.120 Uiso 1 1 calc R U . . .
H57C H 0.0963 0.3237 0.2119 0.120 Uiso 1 1 calc R U . . .
C59 C 0.2593(4) 0.4198(3) 0.3249(3) 0.0577(15) Uani 1 1 d . . . . .
H59A H 0.2675 0.4390 0.3714 0.069 Uiso 1 1 calc R U . . .
C60 C 0.2336(3) 0.1902(3) 0.1987(3) 0.0510(12) Uani 1 1 d . . . . .
H60A H 0.1829 0.2145 0.1936 0.061 Uiso 1 1 calc R U . . .
C62 C 0.0515(3) 0.2482(3) 0.2681(3) 0.0566(15) Uani 1 1 d . . . . .
H62A H 0.0466 0.2142 0.2305 0.068 Uiso 1 1 calc R U . . .
C63 C 0.2421(5) 0.0350(4) 0.5760(4) 0.078(2) Uani 1 1 d . . . . .
H63A H 0.2414 0.0578 0.6191 0.118 Uiso 1 1 calc R U . . .
H63B H 0.1981 0.0509 0.5432 0.118 Uiso 1 1 calc R U . . .
H63C H 0.2390 -0.0151 0.5816 0.118 Uiso 1 1 calc R U . . .
C64 C 0.1982(5) 0.4634(4) 0.2794(4) 0.076(2) Uani 1 1 d . . . . .
H64A H 0.2163 0.5111 0.2782 0.114 Uiso 1 1 calc R U . . .
H64B H 0.1895 0.4442 0.2340 0.114 Uiso 1 1 calc R U . . .
H64C H 0.1498 0.4625 0.2971 0.114 Uiso 1 1 calc R U . . .
C65 C 0.3852(3) 0.3732(4) 0.5003(4) 0.073(2) Uani 1 1 d . . . . .
H65A H 0.3628 0.4061 0.5259 0.087 Uiso 1 1 calc R U . . .
C66 C 0.5013(4) 0.3255(4) 0.4648(5) 0.086(3) Uani 1 1 d . . . . .
H66A H 0.5551 0.3275 0.4649 0.103 Uiso 1 1 calc R U . . .
C69 C 0.1993(4) -0.3494(4) 0.3711(5) 0.083(2) Uani 1 1 d . . . . .
H69A H 0.1880 -0.3971 0.3825 0.125 Uiso 1 1 calc R U . . .
H69B H 0.1659 -0.3177 0.3905 0.125 Uiso 1 1 calc R U . . .
H69C H 0.1901 -0.3441 0.3223 0.125 Uiso 1 1 calc R U . . .
C72 C 0.4602(5) 0.0217(5) 0.1755(4) 0.090(3) Uani 1 1 d . . . . .
H72A H 0.5073 0.0101 0.1585 0.136 Uiso 1 1 calc R U . . .
H72B H 0.4418 -0.0192 0.1965 0.136 Uiso 1 1 calc R U . . .
H72C H 0.4205 0.0371 0.1384 0.136 Uiso 1 1 calc R U . . .
C75 C 0.2350(6) 0.1441(4) 0.1362(3) 0.083(2) Uani 1 1 d . . . . .
H75A H 0.2287 0.1731 0.0960 0.124 Uiso 1 1 calc R U . . .
H75B H 0.2844 0.1196 0.1412 0.124 Uiso 1 1 calc R U . . .
H75C H 0.1929 0.1105 0.1321 0.124 Uiso 1 1 calc R U . . .
C79 C 0.5409(4) 0.0620(5) 0.2875(4) 0.085(2) Uani 1 1 d . . . . .
H79A H 0.5882 0.0498 0.2710 0.127 Uiso 1 1 calc R U . . .
H79B H 0.5506 0.1018 0.3175 0.127 Uiso 1 1 calc R U . . .
H79C H 0.5243 0.0226 0.3119 0.127 Uiso 1 1 calc R U . . .
C85 C 0.3361(5) 0.4181(4) 0.2994(5) 0.092(3) Uani 1 1 d . . . . .
H85A H 0.3564 0.4652 0.2987 0.138 Uiso 1 1 calc R U . . .
H85B H 0.3728 0.3893 0.3292 0.138 Uiso 1 1 calc R U . . .
H85C H 0.3281 0.3989 0.2541 0.138 Uiso 1 1 calc R U . . .
C117 C 0.2982(5) 0.2440(4) 0.2062(4) 0.078(2) Uani 1 1 d . . . . .
H11A H 0.2919 0.2732 0.1661 0.117 Uiso 1 1 calc R U . . .
H11B H 0.2960 0.2728 0.2456 0.117 Uiso 1 1 calc R U . . .
H11C H 0.3482 0.2205 0.2117 0.117 Uiso 1 1 calc R U . . .
C7 C 0.4400(6) -0.2126(7) 0.2904(6) 0.118(3) Uani 1 1 d . U . . .
H7A H 0.4450 -0.2596 0.3112 0.142 Uiso 1 1 calc R U . . .
C8 C 0.0527(7) -0.0140(8) 0.2511(7) 0.157(6) Uani 1 1 d D . . . .
H8A H 0.0985 -0.0269 0.2834 0.236 Uiso 1 1 calc R U . . .
H8B H 0.0100 -0.0044 0.2749 0.236 Uiso 1 1 calc R U . . .
H8C H 0.0384 -0.0521 0.2196 0.236 Uiso 1 1 calc R U . . .
C9 C 0.0689(8) 0.0461(6) 0.2154(6) 0.127(4) Uani 1 1 d D U . . .
H9A H 0.1127 0.0364 0.1913 0.152 Uiso 1 1 calc R U . . .
C12 C 0.3367(6) -0.3810(4) 0.3754(9) 0.177(8) Uani 1 1 d . . . . .
H12A H 0.3243 -0.4283 0.3870 0.266 Uiso 1 1 calc R U . . .
H12B H 0.3318 -0.3770 0.3266 0.266 Uiso 1 1 calc R U . . .
H12C H 0.3896 -0.3699 0.3965 0.266 Uiso 1 1 calc R U . . .
C14 C 0.5108(5) -0.1652(10) 0.3199(9) 0.201(9) Uani 1 1 d . . . . .
H14A H 0.5584 -0.1863 0.3108 0.301 Uiso 1 1 calc R U . . .
H14B H 0.5042 -0.1195 0.2988 0.301 Uiso 1 1 calc R U . . .
H14C H 0.5135 -0.1604 0.3683 0.301 Uiso 1 1 calc R U . . .
C1 C 0.4368(8) -0.2164(11) 0.2184(5) 0.207(10) Uani 1 1 d . . . . .
H1A H 0.4820 -0.2414 0.2088 0.311 Uiso 1 1 calc R U . . .
H1B H 0.3899 -0.2408 0.1979 0.311 Uiso 1 1 calc R U . . .
H1C H 0.4364 -0.1696 0.1999 0.311 Uiso 1 1 calc R U . . .
C11 C 0.0062(9) 0.0641(12) 0.1710(8) 0.258(13) Uani 1 1 d . . . . .
H11D H 0.0177 0.1054 0.1466 0.387 Uiso 1 1 calc R U . . .
H11E H -0.0081 0.0261 0.1393 0.387 Uiso 1 1 calc R U . . .
H11F H -0.0365 0.0738 0.1947 0.387 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O15 1.798(3) . ?
Ti1 O20 1.799(3) . ?
Ti1 O8 1.917(3) . ?
Ti1 O17 2.029(3) . ?
Ti1 O3 2.139(3) . ?
Ti1 O4 2.141(3) . ?
Ti1 Ti2 3.3516(9) . ?
Ti2 O27 1.760(3) . ?
Ti2 O1 1.848(3) . ?
Ti2 O10 1.960(3) . ?
Ti2 O17 2.027(3) . ?
Ti2 O11 2.030(3) . ?
Ti2 O3 2.199(3) . ?
Ti2 Ti4 3.0886(10) . ?
Ti3 O16 1.751(3) . ?
Ti3 O2 1.874(3) . ?
Ti3 O1 1.937(3) . ?
Ti3 O9 1.992(3) . ?
Ti3 O6 2.066(3) . ?
Ti3 O5 2.208(3) . ?
Ti3 Ti4 2.9102(10) . ?
Ti3 Ti5 3.3327(10) . ?
Ti4 O18 1.774(3) . ?
Ti4 O2 1.784(3) . ?
Ti4 O12 2.048(3) . ?
Ti4 O7 2.054(3) . ?
Ti4 O10 2.077(3) . ?
Ti4 O1 2.115(3) . ?
Ti5 O19 1.776(3) . ?
Ti5 O22 1.791(3) . ?
Ti5 O14 1.921(3) . ?
Ti5 O9 2.045(3) . ?
Ti5 O13 2.127(3) . ?
Ti5 O5 2.137(3) . ?
O3 C21 1.290(5) . ?
O4 C31 1.246(5) . ?
O5 C29 1.276(5) . ?
O6 C35 1.266(5) . ?
O7 C29 1.260(5) . ?
O8 C32 1.321(5) . ?
O9 C34 1.457(6) . ?
O10 C60 1.439(6) . ?
O11 C31 1.274(5) . ?
O12 C21 1.259(5) . ?
O13 C35 1.251(5) . ?
O14 C30 1.319(6) . ?
O15 C28 1.435(5) . ?
O16 C44 1.434(5) . ?
O17 C62 1.458(6) . ?
O18 C49 1.404(6) . ?
O19 C48 1.376(6) . ?
O20 C59 1.440(6) . ?
C21 C39 1.471(6) . ?
O22 C7 1.358(10) . ?
C23 C24 1.388(6) . ?
C23 C25 1.392(5) . ?
C24 C47 1.388(6) . ?
C24 C35 1.497(5) 3_556 ?
C25 C26 1.386(6) . ?
C26 C40 1.386(7) . ?
C26 C31 1.500(5) . ?
O27 C9 1.435(11) . ?
C28 C43 1.509(7) . ?
C28 C36 1.520(6) . ?
C29 C37 1.482(6) . ?
C30 C37 1.410(7) . ?
C30 C42 1.412(7) . ?
C32 C65 1.399(7) . ?
C32 C39 1.418(6) . ?
C33 C38 1.369(7) . ?
C33 C37 1.401(7) . ?
C34 C52 1.505(7) . ?
C34 C50 1.513(7) . ?
C35 C24 1.498(5) 3_556 ?
C38 C41 1.402(9) . ?
C39 C45 1.399(6) . ?
C40 C47 1.386(6) . ?
C41 C42 1.367(9) . ?
C44 C46 1.489(8) . ?
C44 C63 1.527(9) . ?
C45 C66 1.373(8) . ?
C48 C12 1.430(13) . ?
C48 C69 1.495(11) . ?
C49 C79 1.509(9) . ?
C49 C72 1.514(10) . ?
C51 C65 1.379(9) . ?
C51 C66 1.390(10) . ?
C53 C62 1.516(10) . ?
C57 C62 1.516(10) . ?
C59 C85 1.498(8) . ?
C59 C64 1.511(9) . ?
C60 C117 1.500(10) . ?
C60 C75 1.522(8) . ?
C7 C1 1.424(14) . ?
C7 C14 1.548(17) . ?
C8 C9 1.396(13) . ?
C9 C11 1.317(19) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O15 Ti1 O20 99.89(15) . . ?
O15 Ti1 O8 95.72(13) . . ?
O20 Ti1 O8 93.77(16) . . ?
O15 Ti1 O17 107.95(13) . . ?
O20 Ti1 O17 94.52(15) . . ?
O8 Ti1 O17 153.11(13) . . ?
O15 Ti1 O3 166.75(12) . . ?
O20 Ti1 O3 93.25(13) . . ?
O8 Ti1 O3 81.59(12) . . ?
O17 Ti1 O3 72.44(11) . . ?
O15 Ti1 O4 84.69(13) . . ?
O20 Ti1 O4 175.42(13) . . ?
O8 Ti1 O4 85.74(13) . . ?
O17 Ti1 O4 83.98(12) . . ?
O3 Ti1 O4 82.17(10) . . ?
O15 Ti1 Ti2 135.99(10) . . ?
O20 Ti1 Ti2 103.73(11) . . ?
O8 Ti1 Ti2 118.87(10) . . ?
O17 Ti1 Ti2 34.24(8) . . ?
O3 Ti1 Ti2 40.06(7) . . ?
O4 Ti1 Ti2 72.65(8) . . ?
O27 Ti2 O1 103.54(15) . . ?
O27 Ti2 O10 97.79(16) . . ?
O1 Ti2 O10 82.28(12) . . ?
O27 Ti2 O17 95.64(15) . . ?
O1 Ti2 O17 160.79(12) . . ?
O10 Ti2 O17 96.36(13) . . ?
O27 Ti2 O11 95.73(16) . . ?
O1 Ti2 O11 90.83(12) . . ?
O10 Ti2 O11 165.94(13) . . ?
O17 Ti2 O11 86.11(12) . . ?
O27 Ti2 O3 166.69(15) . . ?
O1 Ti2 O3 89.66(11) . . ?
O10 Ti2 O3 82.15(11) . . ?
O17 Ti2 O3 71.21(11) . . ?
O11 Ti2 O3 85.59(11) . . ?
O27 Ti2 Ti4 111.99(11) . . ?
O1 Ti2 Ti4 42.01(8) . . ?
O10 Ti2 Ti4 41.49(9) . . ?
O17 Ti2 Ti4 130.26(9) . . ?
O11 Ti2 Ti4 128.45(10) . . ?
O3 Ti2 Ti4 76.75(7) . . ?
O27 Ti2 Ti1 128.77(12) . . ?
O1 Ti2 Ti1 126.72(9) . . ?
O10 Ti2 Ti1 98.07(9) . . ?
O17 Ti2 Ti1 34.28(8) . . ?
O11 Ti2 Ti1 76.23(8) . . ?
O3 Ti2 Ti1 38.75(7) . . ?
Ti4 Ti2 Ti1 112.03(3) . . ?
O16 Ti3 O2 103.11(14) . . ?
O16 Ti3 O1 100.50(14) . . ?
O2 Ti3 O1 82.19(12) . . ?
O16 Ti3 O9 100.30(14) . . ?
O2 Ti3 O9 96.69(12) . . ?
O1 Ti3 O9 158.87(13) . . ?
O16 Ti3 O6 93.55(14) . . ?
O2 Ti3 O6 162.13(14) . . ?
O1 Ti3 O6 88.52(12) . . ?
O9 Ti3 O6 86.49(12) . . ?
O16 Ti3 O5 171.40(13) . . ?
O2 Ti3 O5 83.38(11) . . ?
O1 Ti3 O5 85.86(11) . . ?
O9 Ti3 O5 73.08(12) . . ?
O6 Ti3 O5 80.74(12) . . ?
O16 Ti3 Ti4 111.43(11) . . ?
O2 Ti3 Ti4 36.24(9) . . ?
O1 Ti3 Ti4 46.58(8) . . ?
O9 Ti3 Ti4 126.78(9) . . ?
O6 Ti3 Ti4 130.60(10) . . ?
O5 Ti3 Ti4 77.15(8) . . ?
O16 Ti3 Ti5 133.26(11) . . ?
O2 Ti3 Ti5 96.63(9) . . ?
O1 Ti3 Ti5 124.10(9) . . ?
O9 Ti3 Ti5 34.86(9) . . ?
O6 Ti3 Ti5 75.98(8) . . ?
O5 Ti3 Ti5 39.14(8) . . ?
Ti4 Ti3 Ti5 109.50(3) . . ?
O18 Ti4 O2 103.73(14) . . ?
O18 Ti4 O12 92.96(14) . . ?
O2 Ti4 O12 93.96(13) . . ?
O18 Ti4 O7 92.52(14) . . ?
O2 Ti4 O7 92.88(13) . . ?
O12 Ti4 O7 169.98(12) . . ?
O18 Ti4 O10 103.31(14) . . ?
O2 Ti4 O10 152.94(12) . . ?
O12 Ti4 O10 85.54(12) . . ?
O7 Ti4 O10 85.04(12) . . ?
O18 Ti4 O1 176.31(15) . . ?
O2 Ti4 O1 79.47(12) . . ?
O12 Ti4 O1 88.62(11) . . ?
O7 Ti4 O1 85.44(11) . . ?
O10 Ti4 O1 73.47(11) . . ?
O18 Ti4 Ti3 141.17(11) . . ?
O2 Ti4 Ti3 38.38(9) . . ?
O12 Ti4 Ti3 97.17(9) . . ?
O7 Ti4 Ti3 83.72(9) . . ?
O10 Ti4 Ti3 114.76(9) . . ?
O1 Ti4 Ti3 41.69(8) . . ?
O18 Ti4 Ti2 141.36(12) . . ?
O2 Ti4 Ti2 114.54(9) . . ?
O12 Ti4 Ti2 79.76(8) . . ?
O7 Ti4 Ti2 90.74(9) . . ?
O10 Ti4 Ti2 38.71(8) . . ?
O1 Ti4 Ti2 35.79(8) . . ?
Ti3 Ti4 Ti2 77.45(3) . . ?
O19 Ti5 O22 100.34(16) . . ?
O19 Ti5 O14 100.13(16) . . ?
O22 Ti5 O14 95.31(15) . . ?
O19 Ti5 O9 102.15(16) . . ?
O22 Ti5 O9 93.28(14) . . ?
O14 Ti5 O9 154.23(13) . . ?
O19 Ti5 O13 88.19(14) . . ?
O22 Ti5 O13 171.17(14) . . ?
O14 Ti5 O13 85.30(13) . . ?
O9 Ti5 O13 82.64(12) . . ?
O19 Ti5 O5 169.15(14) . . ?
O22 Ti5 O5 89.95(13) . . ?
O14 Ti5 O5 82.14(13) . . ?
O9 Ti5 O5 73.61(12) . . ?
O13 Ti5 O5 81.40(11) . . ?
O19 Ti5 Ti3 132.89(13) . . ?
O22 Ti5 Ti3 98.48(11) . . ?
O14 Ti5 Ti3 120.60(10) . . ?
O9 Ti5 Ti3 33.83(9) . . ?
O13 Ti5 Ti3 73.79(8) . . ?
O5 Ti5 Ti3 40.71(8) . . ?
Ti2 O1 Ti3 165.69(15) . . ?
Ti2 O1 Ti4 102.20(12) . . ?
Ti3 O1 Ti4 91.73(11) . . ?
Ti4 O2 Ti3 105.38(14) . . ?
C21 O3 Ti1 125.0(2) . . ?
C21 O3 Ti2 128.7(2) . . ?
Ti1 O3 Ti2 101.19(11) . . ?
C31 O4 Ti1 131.3(3) . . ?
C29 O5 Ti5 123.9(2) . . ?
C29 O5 Ti3 128.7(3) . . ?
Ti5 O5 Ti3 100.15(13) . . ?
C35 O6 Ti3 130.9(3) . . ?
C29 O7 Ti4 127.8(3) . . ?
C32 O8 Ti1 125.6(3) . . ?
C34 O9 Ti3 129.3(3) . . ?
C34 O9 Ti5 119.3(3) . . ?
Ti3 O9 Ti5 111.31(15) . . ?
C60 O10 Ti2 128.7(3) . . ?
C60 O10 Ti4 131.5(3) . . ?
Ti2 O10 Ti4 99.79(13) . . ?
C31 O11 Ti2 131.3(3) . . ?
C21 O12 Ti4 132.6(3) . . ?
C35 O13 Ti5 132.1(3) . . ?
C30 O14 Ti5 127.3(3) . . ?
C28 O15 Ti1 131.7(3) . . ?
C44 O16 Ti3 167.5(3) . . ?
C62 O17 Ti2 122.1(3) . . ?
C62 O17 Ti1 125.4(3) . . ?
Ti2 O17 Ti1 111.49(14) . . ?
C49 O18 Ti4 153.2(4) . . ?
C48 O19 Ti5 159.9(4) . . ?
C59 O20 Ti1 132.5(3) . . ?
O12 C21 O3 121.6(4) . . ?
O12 C21 C39 118.7(4) . . ?
O3 C21 C39 119.7(3) . . ?
C7 O22 Ti5 147.8(6) . . ?
C24 C23 C25 120.4(4) . . ?
C47 C24 C23 119.3(4) . . ?
C47 C24 C35 120.4(4) . 3_556 ?
C23 C24 C35 120.3(4) . 3_556 ?
C26 C25 C23 119.7(4) . . ?
C25 C26 C40 120.2(4) . . ?
C25 C26 C31 119.7(4) . . ?
C40 C26 C31 119.9(4) . . ?
C9 O27 Ti2 148.7(6) . . ?
O15 C28 C43 109.3(4) . . ?
O15 C28 C36 108.3(4) . . ?
C43 C28 C36 114.0(4) . . ?
O7 C29 O5 121.3(4) . . ?
O7 C29 C37 118.7(4) . . ?
O5 C29 C37 120.1(4) . . ?
O14 C30 C37 124.1(4) . . ?
O14 C30 C42 118.3(4) . . ?
C37 C30 C42 117.6(5) . . ?
O4 C31 O11 124.6(3) . . ?
O4 C31 C26 118.1(3) . . ?
O11 C31 C26 117.2(4) . . ?
O8 C32 C65 118.6(4) . . ?
O8 C32 C39 123.6(4) . . ?
C65 C32 C39 117.8(4) . . ?
C38 C33 C37 121.4(5) . . ?
O9 C34 C52 109.4(4) . . ?
O9 C34 C50 112.1(4) . . ?
C52 C34 C50 113.7(5) . . ?
O13 C35 O6 125.9(4) . . ?
O13 C35 C24 117.0(4) . 3_556 ?
O6 C35 C24 117.1(4) . 3_556 ?
C33 C37 C30 120.0(4) . . ?
C33 C37 C29 118.0(4) . . ?
C30 C37 C29 122.0(4) . . ?
C33 C38 C41 118.9(5) . . ?
C45 C39 C32 119.7(4) . . ?
C45 C39 C21 118.2(4) . . ?
C32 C39 C21 122.0(4) . . ?
C47 C40 C26 119.8(4) . . ?
C42 C41 C38 120.8(5) . . ?
C41 C42 C30 121.3(5) . . ?
O16 C44 C46 109.0(4) . . ?
O16 C44 C63 107.5(5) . . ?
C46 C44 C63 111.9(5) . . ?
C66 C45 C39 121.4(5) . . ?
C40 C47 C24 120.6(4) . . ?
O19 C48 C12 110.5(8) . . ?
O19 C48 C69 109.7(6) . . ?
C12 C48 C69 112.5(7) . . ?
O18 C49 C79 108.4(5) . . ?
O18 C49 C72 110.2(5) . . ?
C79 C49 C72 113.7(6) . . ?
C65 C51 C66 121.2(6) . . ?
O20 C59 C85 108.3(5) . . ?
O20 C59 C64 107.9(5) . . ?
C85 C59 C64 112.1(6) . . ?
O10 C60 C117 109.5(5) . . ?
O10 C60 C75 109.2(5) . . ?
C117 C60 C75 110.9(6) . . ?
O17 C62 C53 109.8(5) . . ?
O17 C62 C57 110.0(5) . . ?
C53 C62 C57 114.5(5) . . ?
C51 C65 C32 120.9(5) . . ?
C45 C66 C51 118.8(6) . . ?
O22 C7 C1 111.5(10) . . ?
O22 C7 C14 103.9(9) . . ?
C1 C7 C14 107.4(13) . . ?
C11 C9 C8 109.8(14) . . ?
C11 C9 O27 117.3(12) . . ?
C8 C9 O27 100.6(11) . . ?

_refine_diff_density_max         2.810
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.109

_shelxl_version_number           2014-3

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

data_a_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1572541'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C104 H174 N2 O44 Ti10'
_chemical_formula_weight         2635.44

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

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

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

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

_cell_length_a                   18.6395(4)
_cell_length_b                   17.7825(3)
_cell_length_c                   19.4352(4)
_cell_angle_alpha                90
_cell_angle_beta                 95.404(2)
_cell_angle_gamma                90
_cell_volume                     6413.3(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    9189
_cell_measurement_theta_min      3.9640
_cell_measurement_theta_max      74.3930

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_F_000             2768
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.681
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.41291
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.635
_oxdiff_exptl_absorpt_empirical_full_max 2.373
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_reflns_number            27029
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_theta_min         3.375
_diffrn_reflns_theta_max         74.398
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             12744
_reflns_number_gt                10115
_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0767P)²+7.3399P] 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         12744
_refine_ls_number_parameters     725
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0495
_refine_ls_wR_factor_ref         0.1459
_refine_ls_wR_factor_gt          0.1266
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_restrained_S_all      1.017
_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
Ti01 Ti 0.21506(3) 0.46939(3) 0.59523(3) 0.02347(12) Uani 1 1 d . . . . .
Ti02 Ti 0.32588(3) 0.62057(3) 0.68913(3) 0.02332(12) Uani 1 1 d . . . . .
Ti03 Ti 0.31296(3) 0.79950(3) 0.63460(3) 0.02398(12) Uani 1 1 d . . . . .
Ti04 Ti 0.17848(3) 0.55334(3) 0.71550(3) 0.02535(13) Uani 1 1 d . . . . .
Ti05 Ti 0.21523(3) 0.28571(3) 0.62888(3) 0.02619(13) Uani 1 1 d . . . . .
O1 O 0.26582(11) 0.54379(11) 0.65441(11) 0.0249(4) Uani 1 1 d . . . . .
O2 O 0.24975(11) 0.69922(12) 0.63404(11) 0.0245(4) Uani 1 1 d . . . . .
O3 O 0.68555(11) 0.56656(12) 0.43109(11) 0.0276(4) Uani 1 1 d . . . . .
O4 O 0.36338(11) 0.72690(12) 0.70422(11) 0.0252(4) Uani 1 1 d . . . . .
O5 O 0.14621(11) 0.64727(12) 0.65801(11) 0.0281(4) Uani 1 1 d . . . . .
O6 O 0.24163(11) 0.39109(12) 0.68060(11) 0.0253(4) Uani 1 1 d . . . . .
O7 O 0.37647(11) 0.62083(12) 0.60133(11) 0.0285(5) Uani 1 1 d . . . . .
O8 O 0.13866(11) 0.49404(12) 0.64770(11) 0.0260(4) Uani 1 1 d . . . . .
O9 O 0.24386(11) 0.82404(12) 0.55834(11) 0.0288(4) Uani 1 1 d . . . . .
O10 O 0.17659(11) 0.37002(12) 0.56333(11) 0.0258(4) Uani 1 1 d . . . . .
O11 O 0.36967(11) 0.73818(12) 0.56124(11) 0.0283(4) Uani 1 1 d . . . . .
O12 O 0.22630(11) 0.46515(12) 0.77009(11) 0.0285(4) Uani 1 1 d . . . . .
O13 O 0.37442(12) 0.87516(12) 0.61977(12) 0.0299(5) Uani 1 1 d . . . . .
O14 O 0.68775(11) 0.69062(12) 0.41158(12) 0.0299(5) Uani 1 1 d . . . . .
O15 O 0.27442(13) 0.24668(13) 0.70612(12) 0.0342(5) Uani 1 1 d . . . . .
O16 O 0.25846(12) 0.62256(12) 0.76042(11) 0.0279(4) Uani 1 1 d . . . . .
O17 O 0.20430(12) 0.20498(12) 0.57268(12) 0.0320(5) Uani 1 1 d . . . . .
O18 O 0.26135(12) 0.84311(12) 0.69795(12) 0.0307(5) Uani 1 1 d . . . . .
O19 O 0.19831(12) 0.52511(13) 0.52081(12) 0.0310(5) Uani 1 1 d . . . . .
O20 O 0.39771(12) 0.57531(13) 0.73808(12) 0.0318(5) Uani 1 1 d . . . . .
O21 O 0.13242(12) 0.28102(13) 0.66705(12) 0.0314(5) Uani 1 1 d . . . . .
O22 O 0.11045(12) 0.56529(13) 0.77229(12) 0.0336(5) Uani 1 1 d . . . . .
C01 C 0.18015(16) 0.69862(17) 0.63030(16) 0.0258(6) Uani 1 1 d . . . . .
C02 C 0.17295(16) 0.81557(18) 0.55545(16) 0.0276(6) Uani 1 1 d . . . . .
C03 C 0.39748(16) 0.67430(18) 0.56469(16) 0.0267(6) Uani 1 1 d . . . . .
C04 C 0.13916(16) 0.75781(17) 0.59136(16) 0.0263(6) Uani 1 1 d . . . . .
C05 C 0.65899(16) 0.63181(18) 0.43234(16) 0.0265(6) Uani 1 1 d . . . . .
C06 C 0.58780(16) 0.64081(18) 0.46120(16) 0.0267(6) Uani 1 1 d . . . . .
C07 C 0.46183(16) 0.65950(18) 0.52597(16) 0.0285(6) Uani 1 1 d . . . . .
C08 C 0.24530(16) 0.40293(18) 0.74622(16) 0.0272(6) Uani 1 1 d . . . . .
C10 C 0.50322(18) 0.59480(18) 0.53913(19) 0.0337(7) Uani 1 1 d . . . . .
C11 C 0.42643(16) 0.74458(18) 0.75216(17) 0.0289(6) Uani 1 1 d . . . . .
H11A H 0.4321 0.7043 0.7867 0.035 Uiso 1 1 calc R U . . .
C12 C 0.48269(17) 0.71401(19) 0.48003(17) 0.0297(6) Uani 1 1 d . . . . .
H12A H 0.4539 0.7561 0.4706 0.036 Uiso 1 1 calc R U . . .
C13 C 0.54640(17) 0.7058(2) 0.44822(16) 0.0306(7) Uani 1 1 d . . . . .
C14 C 0.27493(17) 0.34397(19) 0.79371(17) 0.0310(7) Uani 1 1 d . . . . .
C15 C 0.28965(17) 0.2709(2) 0.77057(18) 0.0333(7) Uani 1 1 d . . . . .
C16 C 0.06359(17) 0.75485(19) 0.58782(18) 0.0322(7) Uani 1 1 d . . . . .
H16A H 0.0415 0.7167 0.6109 0.039 Uiso 1 1 calc R U . . .
C17 C 0.56590(18) 0.58617(18) 0.50552(18) 0.0325(7) Uani 1 1 d . . . . .
H17A H 0.5934 0.5428 0.5131 0.039 Uiso 1 1 calc R U . . .
C18 C 0.49371(18) 0.7459(2) 0.71386(19) 0.0368(7) Uani 1 1 d . . . . .
H18A H 0.5348 0.7575 0.7457 0.055 Uiso 1 1 calc R U . . .
H18B H 0.5003 0.6975 0.6934 0.055 Uiso 1 1 calc R U . . .
H18C H 0.4886 0.7835 0.6783 0.055 Uiso 1 1 calc R U . . .
C19 C 0.41394(19) 0.81762(19) 0.78984(19) 0.0354(7) Uani 1 1 d . . . . .
H19A H 0.4555 0.8289 0.8212 0.053 Uiso 1 1 calc R U . . .
H19B H 0.4060 0.8577 0.7569 0.053 Uiso 1 1 calc R U . . .
H19C H 0.3725 0.8124 0.8153 0.053 Uiso 1 1 calc R U . . .
C09 C 0.2273(2) 0.91475(19) 0.70159(19) 0.0366(7) Uani 1 1 d . . . . .
H09A H 0.2167 0.9340 0.6545 0.044 Uiso 1 1 calc R U . . .
C20 C 0.26888(19) 0.6569(2) 0.82832(17) 0.0355(7) Uani 1 1 d . . . . .
H20A H 0.3157 0.6825 0.8327 0.043 Uiso 1 1 calc R U . . .
C21 C 0.12886(19) 0.8674(2) 0.51674(18) 0.0357(7) Uani 1 1 d . . . . .
H21A H 0.1499 0.9049 0.4921 0.043 Uiso 1 1 calc R U . . .
C22 C 0.15391(19) 0.14539(19) 0.5636(2) 0.0359(7) Uani 1 1 d . . . . .
H22A H 0.1051 0.1659 0.5635 0.043 Uiso 1 1 calc R U . . .
C23 C 0.39630(19) 0.9059(2) 0.55708(19) 0.0362(7) Uani 1 1 d . . . . .
H23A H 0.3778 0.8734 0.5188 0.043 Uiso 1 1 calc R U . . .
C24 C 0.3222(2) 0.2195(2) 0.8189(2) 0.0421(8) Uani 1 1 d . . . . .
H24A H 0.3327 0.1712 0.8047 0.051 Uiso 1 1 calc R U . . .
C25 C 0.02166(18) 0.8072(2) 0.5509(2) 0.0405(8) Uani 1 1 d . . . . .
H25A H -0.0283 0.8052 0.5499 0.049 Uiso 1 1 calc R U . . .
C26 C 0.12255(19) 0.3522(2) 0.50725(18) 0.0350(7) Uani 1 1 d . . . . .
H26A H 0.1018 0.3033 0.5176 0.042 Uiso 1 1 calc R U . . .
C27 C 0.04034(19) 0.5633(2) 0.7941(2) 0.0424(9) Uani 1 1 d . . . . .
H27A H 0.0332 0.6084 0.8216 0.051 Uiso 1 1 calc R U . . .
C28 C 0.0548(2) 0.8634(2) 0.5148(2) 0.0426(8) Uani 1 1 d . . . . .
H28A H 0.0266 0.8985 0.4892 0.051 Uiso 1 1 calc R U . . .
C29 C 0.0744(2) 0.3120(2) 0.6996(2) 0.0424(9) Uani 1 1 d . . . . .
H29A H 0.0772 0.3670 0.6979 0.051 Uiso 1 1 calc R U . . .
C30 C 0.4779(2) 0.9070(2) 0.5597(2) 0.0440(9) Uani 1 1 d . . . . .
H30A H 0.4922 0.9278 0.5175 0.066 Uiso 1 1 calc R U . . .
H30B H 0.4971 0.9374 0.5980 0.066 Uiso 1 1 calc R U . . .
H30C H 0.4961 0.8567 0.5654 0.066 Uiso 1 1 calc R U . . .
C31 C 0.0619(2) 0.4094(2) 0.5026(2) 0.0437(9) Uani 1 1 d . . . . .
H31A H 0.0268 0.3963 0.4651 0.065 Uiso 1 1 calc R U . . .
H31B H 0.0394 0.4095 0.5451 0.065 Uiso 1 1 calc R U . . .
H31C H 0.0809 0.4584 0.4946 0.065 Uiso 1 1 calc R U . . .
C32 C 0.3616(2) 0.9830(2) 0.5464(2) 0.0483(9) Uani 1 1 d . . . . .
H32A H 0.3756 1.0048 0.5044 0.072 Uiso 1 1 calc R U . . .
H32B H 0.3102 0.9780 0.5432 0.072 Uiso 1 1 calc R U . . .
H32C H 0.3772 1.0150 0.5847 0.072 Uiso 1 1 calc R U . . .
C33 C 0.2912(2) 0.3627(2) 0.86337(19) 0.0442(9) Uani 1 1 d . . . . .
H33A H 0.2805 0.4107 0.8786 0.053 Uiso 1 1 calc R U . . .
C34 C 0.2776(2) 0.9692(2) 0.7415(2) 0.0475(9) Uani 1 1 d . . . . .
H34A H 0.2543 1.0172 0.7437 0.071 Uiso 1 1 calc R U . . .
H34B H 0.2895 0.9505 0.7875 0.071 Uiso 1 1 calc R U . . .
H34C H 0.3208 0.9746 0.7187 0.071 Uiso 1 1 calc R U . . .
C35 C 0.3387(2) 0.2396(3) 0.8868(2) 0.0530(10) Uani 1 1 d . . . . .
H35A H 0.3607 0.2048 0.9177 0.064 Uiso 1 1 calc R U . . .
C36 C 0.2700(2) 0.5965(2) 0.88295(19) 0.0456(9) Uani 1 1 d . . . . .
H36A H 0.2769 0.6192 0.9279 0.068 Uiso 1 1 calc R U . . .
H36B H 0.2251 0.5698 0.8784 0.068 Uiso 1 1 calc R U . . .
H36C H 0.3087 0.5622 0.8773 0.068 Uiso 1 1 calc R U . . .
C37 C 0.3231(3) 0.3109(3) 0.9101(2) 0.0551(11) Uani 1 1 d . . . . .
H37A H 0.3338 0.3238 0.9563 0.066 Uiso 1 1 calc R U . . .
C38 C 0.1613(2) 0.1077(2) 0.4950(2) 0.0471(9) Uani 1 1 d . . . . .
H38A H 0.1272 0.0673 0.4886 0.071 Uiso 1 1 calc R U . . .
H38B H 0.1520 0.1437 0.4584 0.071 Uiso 1 1 calc R U . . .
H38C H 0.2092 0.0882 0.4944 0.071 Uiso 1 1 calc R U . . .
C39 C 0.1568(2) 0.9044(2) 0.7334(2) 0.0503(10) Uani 1 1 d . . . . .
H39A H 0.1333 0.9522 0.7361 0.075 Uiso 1 1 calc R U . . .
H39B H 0.1263 0.8708 0.7052 0.075 Uiso 1 1 calc R U . . .
H39C H 0.1662 0.8836 0.7789 0.075 Uiso 1 1 calc R U . . .
C40 C 0.2108(3) 0.7149(2) 0.8349(2) 0.0552(11) Uani 1 1 d . . . . .
H40A H 0.2175 0.7378 0.8797 0.083 Uiso 1 1 calc R U . . .
H40B H 0.2135 0.7528 0.8000 0.083 Uiso 1 1 calc R U . . .
H40C H 0.1644 0.6911 0.8290 0.083 Uiso 1 1 calc R U . . .
C41 C 0.1583(3) 0.3436(3) 0.4410(2) 0.0520(10) Uani 1 1 d . . . . .
H41A H 0.1225 0.3318 0.4038 0.078 Uiso 1 1 calc R U . . .
H41B H 0.1819 0.3898 0.4310 0.078 Uiso 1 1 calc R U . . .
H41C H 0.1932 0.3038 0.4462 0.078 Uiso 1 1 calc R U . . .
C42 C 0.1673(3) 0.0910(2) 0.6230(3) 0.0550(11) Uani 1 1 d . . . . .
H42A H 0.1333 0.0503 0.6172 0.082 Uiso 1 1 calc R U . . .
H42B H 0.2153 0.0714 0.6240 0.082 Uiso 1 1 calc R U . . .
H42C H 0.1616 0.1166 0.6657 0.082 Uiso 1 1 calc R U . . .
C43 C 0.1391(2) 0.6124(3) 0.4426(2) 0.0544(11) Uani 1 1 d . . . . .
H43A H 0.1456 0.6559 0.4146 0.082 Uiso 1 1 calc R U . . .
H43B H 0.1205 0.5717 0.4137 0.082 Uiso 1 1 calc R U . . .
H43C H 0.1057 0.6240 0.4758 0.082 Uiso 1 1 calc R U . . .
C44 C 0.4414(2) 0.5159(2) 0.7671(3) 0.0530(10) Uani 1 1 d . . . . .
H44A H 0.4256 0.5054 0.8128 0.064 Uiso 1 1 calc R U . . .
C45 C 0.2113(2) 0.5896(3) 0.4803(2) 0.0529(11) Uani 1 1 d . . . . .
H45A H 0.2265 0.6303 0.5123 0.064 Uiso 1 1 calc R U . . .
C46 C 0.5180(2) 0.5424(3) 0.7784(3) 0.0661(14) Uani 1 1 d . . . . .
H46A H 0.5478 0.5024 0.7981 0.099 Uiso 1 1 calc R U . . .
H46B H 0.5343 0.5572 0.7350 0.099 Uiso 1 1 calc R U . . .
H46C H 0.5209 0.5846 0.8093 0.099 Uiso 1 1 calc R U . . .
C47 C 0.0046(2) 0.2865(3) 0.6606(3) 0.0666(14) Uani 1 1 d . . . . .
H47A H -0.0354 0.3071 0.6822 0.100 Uiso 1 1 calc R U . . .
H47B H 0.0027 0.3036 0.6136 0.100 Uiso 1 1 calc R U . . .
H47C H 0.0020 0.2326 0.6614 0.100 Uiso 1 1 calc R U . . .
C48 C -0.0135(2) 0.5640(3) 0.7315(3) 0.0652(14) Uani 1 1 d . . . . .
H48A H -0.0614 0.5626 0.7458 0.098 Uiso 1 1 calc R U . . .
H48B H -0.0075 0.6090 0.7053 0.098 Uiso 1 1 calc R U . . .
H48C H -0.0061 0.5208 0.7033 0.098 Uiso 1 1 calc R U . . .
C49 C 0.0340(2) 0.4951(3) 0.8393(3) 0.0655(14) Uani 1 1 d . . . . .
H49A H -0.0136 0.4931 0.8545 0.098 Uiso 1 1 calc R U . . .
H49B H 0.0424 0.4505 0.8134 0.098 Uiso 1 1 calc R U . . .
H49C H 0.0689 0.4982 0.8787 0.098 Uiso 1 1 calc R U . . .
C50 C 0.4305(2) 0.4469(2) 0.7265(4) 0.0751(17) Uani 1 1 d . . . . .
H50A H 0.4607 0.4078 0.7473 0.113 Uiso 1 1 calc R U . . .
H50B H 0.3809 0.4318 0.7252 0.113 Uiso 1 1 calc R U . . .
H50C H 0.4427 0.4558 0.6803 0.113 Uiso 1 1 calc R U . . .
C51 C 0.0800(3) 0.2868(3) 0.7739(2) 0.0626(13) Uani 1 1 d . . . . .
H51A H 0.0408 0.3077 0.7963 0.094 Uiso 1 1 calc R U . . .
H51B H 0.0780 0.2329 0.7758 0.094 Uiso 1 1 calc R U . . .
H51C H 0.1249 0.3039 0.7970 0.094 Uiso 1 1 calc R U . . .
C52 C 0.2706(2) 0.5756(3) 0.4373(2) 0.0619(13) Uani 1 1 d . . . . .
H52A H 0.2785 0.6197 0.4105 0.093 Uiso 1 1 calc R U . . .
H52B H 0.3137 0.5641 0.4664 0.093 Uiso 1 1 calc R U . . .
H52C H 0.2584 0.5341 0.4069 0.093 Uiso 1 1 calc R U . . .
N1 N 0.5650(3) 0.7682(3) 0.4073(3) 0.0451(14) Uani 0.56 1 d . . P . .
H1A H 0.5377 0.8072 0.4036 0.054 Uiso 0.56 1 calc R U P . .
H1B H 0.6036 0.7667 0.3863 0.054 Uiso 0.56 1 calc R U P . .
N2 N 0.4958(5) 0.5414(5) 0.5931(4) 0.0504(18) Uiso 0.44 1 d . . P . .
H2A H 0.4633 0.5478 0.6212 0.060 Uiso 0.44 1 calc R U P . .
H2B H 0.5237 0.5029 0.5975 0.060 Uiso 0.44 1 calc R U P . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti01 O19 1.757(2) . ?
Ti01 O8 1.880(2) . ?
Ti01 O1 1.940(2) . ?
Ti01 O10 1.984(2) . ?
Ti01 O3 2.069(2) 3_666 ?
Ti01 O6 2.187(2) . ?
Ti01 Ti04 2.9082(8) . ?
Ti01 Ti05 3.3312(7) . ?
Ti02 O20 1.762(2) . ?
Ti02 O1 1.852(2) . ?
Ti02 O16 1.957(2) . ?
Ti02 O7 2.026(2) . ?
Ti02 O4 2.028(2) . ?
Ti02 O2 2.198(2) . ?
Ti02 Ti04 3.0831(7) . ?
Ti02 Ti03 3.3552(7) . ?
Ti03 O18 1.807(2) . ?
Ti03 O13 1.808(2) . ?
Ti03 O9 1.920(2) . ?
Ti03 O4 2.035(2) . ?
Ti03 O2 2.137(2) . ?
Ti03 O11 2.150(2) . ?
Ti04 O22 1.771(2) . ?
Ti04 O8 1.793(2) . ?
Ti04 O12 2.050(2) . ?
Ti04 O16 2.063(2) . ?
Ti04 O5 2.067(2) . ?
Ti04 O1 2.110(2) . ?
Ti05 O21 1.776(2) . ?
Ti05 O17 1.804(2) . ?
Ti05 O15 1.908(2) . ?
Ti05 O10 2.054(2) . ?
Ti05 O14 2.082(2) 3_666 ?
Ti05 O6 2.161(2) . ?
O2 C01 1.293(4) . ?
O3 C05 1.263(4) . ?
O3 Ti01 2.069(2) 3_666 ?
O4 C11 1.463(4) . ?
O5 C01 1.260(4) . ?
O6 C08 1.288(4) . ?
O7 C03 1.272(4) . ?
O9 C02 1.326(4) . ?
O10 C26 1.448(4) . ?
O11 C03 1.248(4) . ?
O12 C08 1.263(4) . ?
O13 C23 1.430(4) . ?
O14 C05 1.259(4) . ?
O14 Ti05 2.082(2) 3_666 ?
O15 C15 1.329(4) . ?
O16 C20 1.451(4) . ?
O17 C22 1.416(4) . ?
O18 C09 1.428(4) . ?
O19 C45 1.425(4) . ?
O20 C44 1.418(4) . ?
O21 C29 1.415(4) . ?
O22 C27 1.412(4) . ?
C01 C04 1.468(4) . ?
C02 C21 1.405(5) . ?
C02 C04 1.422(4) . ?
C03 C07 1.498(4) . ?
C04 C16 1.405(4) . ?
C05 C06 1.497(4) . ?
C06 C17 1.385(5) . ?
C06 C13 1.400(5) . ?
C07 C10 1.395(5) . ?
C07 C12 1.398(5) . ?
C08 C14 1.470(4) . ?
C10 C17 1.400(4) . ?
C10 N2 1.432(9) . ?
C11 C18 1.518(4) . ?
C11 C19 1.520(4) . ?
C11 H11A 0.9800 . ?
C12 C13 1.397(4) . ?
C12 H12A 0.9300 . ?
C13 N1 1.426(7) . ?
C14 C33 1.400(5) . ?
C14 C15 1.411(5) . ?
C15 C24 1.406(5) . ?
C16 C25 1.373(5) . ?
C16 H16A 0.9300 . ?
C17 H17A 0.9300 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C09 C34 1.510(5) . ?
C09 C39 1.515(5) . ?
C09 H09A 0.9800 . ?
C20 C36 1.509(5) . ?
C20 C40 1.509(5) . ?
C20 H20A 0.9800 . ?
C21 C28 1.379(5) . ?
C21 H21A 0.9300 . ?
C22 C38 1.508(5) . ?
C22 C42 1.510(5) . ?
C22 H22A 0.9800 . ?
C23 C30 1.518(5) . ?
C23 C32 1.522(5) . ?
C23 H23A 0.9800 . ?
C24 C35 1.374(6) . ?
C24 H24A 0.9300 . ?
C25 C28 1.398(5) . ?
C25 H25A 0.9300 . ?
C26 C41 1.512(5) . ?
C26 C31 1.517(5) . ?
C26 H26A 0.9800 . ?
C27 C48 1.504(6) . ?
C27 C49 1.509(6) . ?
C27 H27A 0.9800 . ?
C28 H28A 0.9300 . ?
C29 C51 1.507(6) . ?
C29 C47 1.513(6) . ?
C29 H29A 0.9800 . ?
C30 H30A 0.9600 . ?
C30 H30B 0.9600 . ?
C30 H30C 0.9600 . ?
C31 H31A 0.9600 . ?
C31 H31B 0.9600 . ?
C31 H31C 0.9600 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C37 1.388(6) . ?
C33 H33A 0.9300 . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
C35 C37 1.386(7) . ?
C35 H35A 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C37 H37A 0.9300 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C40 H40A 0.9600 . ?
C40 H40B 0.9600 . ?
C40 H40C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C43 C45 1.526(6) . ?
C43 H43A 0.9600 . ?
C43 H43B 0.9600 . ?
C43 H43C 0.9600 . ?
C44 C50 1.463(7) . ?
C44 C46 1.500(6) . ?
C44 H44A 0.9800 . ?
C45 C52 1.468(6) . ?
C45 H45A 0.9800 . ?
C46 H46A 0.9600 . ?
C46 H46B 0.9600 . ?
C46 H46C 0.9600 . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C49 H49A 0.9600 . ?
C49 H49B 0.9600 . ?
C49 H49C 0.9600 . ?
C50 H50A 0.9600 . ?
C50 H50B 0.9600 . ?
C50 H50C 0.9600 . ?
C51 H51A 0.9600 . ?
C51 H51B 0.9600 . ?
C51 H51C 0.9600 . ?
C52 H52A 0.9600 . ?
C52 H52B 0.9600 . ?
C52 H52C 0.9600 . ?
N1 H1A 0.8600 . ?
N1 H1B 0.8600 . ?
N2 H2A 0.8600 . ?
N2 H2B 0.8600 . ?

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
O19 Ti01 O8 103.30(10) . . ?
O19 Ti01 O1 98.19(10) . . ?
O8 Ti01 O1 82.61(9) . . ?
O19 Ti01 O10 102.36(10) . . ?
O8 Ti01 O10 96.16(9) . . ?
O1 Ti01 O10 159.11(9) . . ?
O19 Ti01 O3 93.70(10) . 3_666 ?
O8 Ti01 O3 161.42(9) . 3_666 ?
O1 Ti01 O3 87.66(9) . 3_666 ?
O10 Ti01 O3 87.32(9) . 3_666 ?
O19 Ti01 O6 173.61(10) . . ?
O8 Ti01 O6 82.29(8) . . ?
O1 Ti01 O6 85.49(9) . . ?
O10 Ti01 O6 73.71(8) . . ?
O3 Ti01 O6 81.18(8) 3_666 . ?
O19 Ti01 Ti04 109.59(8) . . ?
O8 Ti01 Ti04 36.61(7) . . ?
O1 Ti01 Ti04 46.49(6) . . ?
O10 Ti01 Ti04 127.09(6) . . ?
O3 Ti01 Ti04 129.83(7) 3_666 . ?
O6 Ti01 Ti04 76.73(6) . . ?
O19 Ti01 Ti05 135.36(8) . . ?
O8 Ti01 Ti05 96.25(7) . . ?
O1 Ti01 Ti05 124.12(7) . . ?
O10 Ti01 Ti05 35.09(6) . . ?
O3 Ti01 Ti05 76.19(6) 3_666 . ?
O6 Ti01 Ti05 39.71(6) . . ?
Ti04 Ti01 Ti05 109.97(2) . . ?
O20 Ti02 O1 105.22(10) . . ?
O20 Ti02 O16 97.59(10) . . ?
O1 Ti02 O16 82.23(9) . . ?
O20 Ti02 O7 93.76(10) . . ?
O1 Ti02 O7 90.47(9) . . ?
O16 Ti02 O7 167.79(10) . . ?
O20 Ti02 O4 96.53(10) . . ?
O1 Ti02 O4 158.19(9) . . ?
O16 Ti02 O4 96.68(9) . . ?
O7 Ti02 O4 86.46(9) . . ?
O20 Ti02 O2 167.56(10) . . ?
O1 Ti02 O2 87.21(9) . . ?
O16 Ti02 O2 84.56(9) . . ?
O7 Ti02 O2 85.33(8) . . ?
O4 Ti02 O2 71.03(8) . . ?
O20 Ti02 Ti04 112.14(8) . . ?
O1 Ti02 Ti04 42.03(6) . . ?
O16 Ti02 Ti04 41.19(7) . . ?
O7 Ti02 Ti04 129.32(7) . . ?
O4 Ti02 Ti04 129.64(6) . . ?
O2 Ti02 Ti04 77.48(6) . . ?
O20 Ti02 Ti03 129.19(8) . . ?
O1 Ti02 Ti03 124.13(7) . . ?
O16 Ti02 Ti03 100.06(7) . . ?
O7 Ti02 Ti03 75.94(6) . . ?
O4 Ti02 Ti03 34.39(6) . . ?
O2 Ti02 Ti03 38.62(5) . . ?
Ti04 Ti02 Ti03 112.43(2) . . ?
O18 Ti03 O13 100.09(10) . . ?
O18 Ti03 O9 93.84(10) . . ?
O13 Ti03 O9 95.56(10) . . ?
O18 Ti03 O4 93.52(9) . . ?
O13 Ti03 O4 108.55(9) . . ?
O9 Ti03 O4 153.08(9) . . ?
O18 Ti03 O2 91.89(9) . . ?
O13 Ti03 O2 167.89(9) . . ?
O9 Ti03 O2 81.74(9) . . ?
O4 Ti03 O2 72.17(8) . . ?
O18 Ti03 O11 174.81(10) . . ?
O13 Ti03 O11 85.02(9) . . ?
O9 Ti03 O11 86.52(9) . . ?
O4 Ti03 O11 83.92(8) . . ?
O2 Ti03 O11 83.03(8) . . ?
O18 Ti03 Ti02 102.63(7) . . ?
O13 Ti03 Ti02 136.76(7) . . ?
O9 Ti03 Ti02 118.84(7) . . ?
O4 Ti03 Ti02 34.25(6) . . ?
O2 Ti03 Ti02 39.94(6) . . ?
O11 Ti03 Ti02 72.74(6) . . ?
O22 Ti04 O8 104.92(11) . . ?
O22 Ti04 O12 94.08(10) . . ?
O8 Ti04 O12 93.45(9) . . ?
O22 Ti04 O16 101.31(10) . . ?
O8 Ti04 O16 153.47(9) . . ?
O12 Ti04 O16 88.62(9) . . ?
O22 Ti04 O5 92.92(10) . . ?
O8 Ti04 O5 89.93(9) . . ?
O12 Ti04 O5 171.18(9) . . ?
O16 Ti04 O5 84.75(9) . . ?
O22 Ti04 O1 174.98(10) . . ?
O8 Ti04 O1 80.04(9) . . ?
O12 Ti04 O1 84.77(8) . . ?
O16 Ti04 O1 73.80(8) . . ?
O5 Ti04 O1 87.80(8) . . ?
O22 Ti04 Ti01 142.99(8) . . ?
O8 Ti04 Ti01 38.70(7) . . ?
O12 Ti04 Ti01 84.25(6) . . ?
O16 Ti04 Ti01 115.58(6) . . ?
O5 Ti04 Ti01 93.36(6) . . ?
O1 Ti04 Ti01 41.82(6) . . ?
O22 Ti04 Ti02 139.36(8) . . ?
O8 Ti04 Ti02 114.81(7) . . ?
O12 Ti04 Ti02 91.83(6) . . ?
O16 Ti04 Ti02 38.66(6) . . ?
O5 Ti04 Ti02 79.36(6) . . ?
O1 Ti04 Ti02 35.99(6) . . ?
Ti01 Ti04 Ti02 77.609(19) . . ?
O21 Ti05 O17 99.35(11) . . ?
O21 Ti05 O15 96.62(11) . . ?
O17 Ti05 O15 102.17(11) . . ?
O21 Ti05 O10 91.46(10) . . ?
O17 Ti05 O10 101.09(10) . . ?
O15 Ti05 O10 153.73(10) . . ?
O21 Ti05 O14 170.80(10) . 3_666 ?
O17 Ti05 O14 89.13(10) . 3_666 ?
O15 Ti05 O14 84.97(10) . 3_666 ?
O10 Ti05 O14 83.36(9) . 3_666 ?
O21 Ti05 O6 90.88(9) . . ?
O17 Ti05 O6 168.37(9) . . ?
O15 Ti05 O6 81.95(9) . . ?
O10 Ti05 O6 72.94(8) . . ?
O14 Ti05 O6 80.35(8) 3_666 . ?
O21 Ti05 Ti01 98.23(8) . . ?
O17 Ti05 Ti01 131.57(8) . . ?
O15 Ti05 Ti01 120.06(8) . . ?
O10 Ti05 Ti01 33.74(6) . . ?
O14 Ti05 Ti01 73.28(6) 3_666 . ?
O6 Ti05 Ti01 40.28(6) . . ?
Ti02 O1 Ti01 164.37(12) . . ?
Ti02 O1 Ti04 101.98(9) . . ?
Ti01 O1 Ti04 91.69(8) . . ?
C01 O2 Ti03 123.87(19) . . ?
C01 O2 Ti02 128.4(2) . . ?
Ti03 O2 Ti02 101.43(8) . . ?
C05 O3 Ti01 130.58(19) . 3_666 ?
C11 O4 Ti02 122.52(18) . . ?
C11 O4 Ti03 125.45(18) . . ?
Ti02 O4 Ti03 111.35(10) . . ?
C01 O5 Ti04 133.2(2) . . ?
C08 O6 Ti05 126.21(19) . . ?
C08 O6 Ti01 129.4(2) . . ?
Ti05 O6 Ti01 100.01(9) . . ?
C03 O7 Ti02 131.7(2) . . ?
Ti04 O8 Ti01 104.69(10) . . ?
C02 O9 Ti03 126.9(2) . . ?
C26 O10 Ti01 129.45(19) . . ?
C26 O10 Ti05 119.06(19) . . ?
Ti01 O10 Ti05 111.16(10) . . ?
C03 O11 Ti03 130.8(2) . . ?
C08 O12 Ti04 127.1(2) . . ?
C23 O13 Ti03 131.0(2) . . ?
C05 O14 Ti05 134.5(2) . 3_666 ?
C15 O15 Ti05 132.8(2) . . ?
C20 O16 Ti02 127.73(19) . . ?
C20 O16 Ti04 131.76(19) . . ?
Ti02 O16 Ti04 100.15(9) . . ?
C22 O17 Ti05 135.0(2) . . ?
C09 O18 Ti03 133.2(2) . . ?
C45 O19 Ti01 152.0(3) . . ?
C44 O20 Ti02 159.0(3) . . ?
C29 O21 Ti05 154.0(2) . . ?
C27 O22 Ti04 157.2(3) . . ?
O5 C01 O2 121.6(3) . . ?
O5 C01 C04 118.8(3) . . ?
O2 C01 C04 119.6(3) . . ?
O9 C02 C21 118.6(3) . . ?
O9 C02 C04 123.2(3) . . ?
C21 C02 C04 118.2(3) . . ?
O11 C03 O7 124.2(3) . . ?
O11 C03 C07 118.8(3) . . ?
O7 C03 C07 117.0(3) . . ?
C16 C04 C02 119.4(3) . . ?
C16 C04 C01 118.0(3) . . ?
C02 C04 C01 122.5(3) . . ?
O14 C05 O3 125.3(3) . . ?
O14 C05 C06 116.8(3) . . ?
O3 C05 C06 117.9(3) . . ?
C17 C06 C13 120.1(3) . . ?
C17 C06 C05 118.8(3) . . ?
C13 C06 C05 120.9(3) . . ?
C10 C07 C12 120.4(3) . . ?
C10 C07 C03 120.5(3) . . ?
C12 C07 C03 118.9(3) . . ?
O12 C08 O6 121.1(3) . . ?
O12 C08 C14 119.7(3) . . ?
O6 C08 C14 119.1(3) . . ?
C07 C10 C17 118.4(3) . . ?
C07 C10 N2 126.2(4) . . ?
C17 C10 N2 114.3(5) . . ?
O4 C11 C18 110.0(3) . . ?
O4 C11 C19 109.9(2) . . ?
C18 C11 C19 113.2(3) . . ?
O4 C11 H11A 107.8 . . ?
C18 C11 H11A 107.8 . . ?
C19 C11 H11A 107.8 . . ?
C13 C12 C07 120.7(3) . . ?
C13 C12 H12A 119.7 . . ?
C07 C12 H12A 119.7 . . ?
C12 C13 C06 118.9(3) . . ?
C12 C13 N1 115.3(4) . . ?
C06 C13 N1 125.7(3) . . ?
C33 C14 C15 119.8(3) . . ?
C33 C14 C08 118.1(3) . . ?
C15 C14 C08 122.0(3) . . ?
O15 C15 C24 117.4(3) . . ?
O15 C15 C14 124.6(3) . . ?
C24 C15 C14 118.0(3) . . ?
C25 C16 C04 121.3(3) . . ?
C25 C16 H16A 119.4 . . ?
C04 C16 H16A 119.4 . . ?
C06 C17 C10 121.4(3) . . ?
C06 C17 H17A 119.3 . . ?
C10 C17 H17A 119.3 . . ?
C11 C18 H18A 109.5 . . ?
C11 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C11 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C11 C19 H19A 109.5 . . ?
C11 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C11 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O18 C09 C34 109.9(3) . . ?
O18 C09 C39 108.5(3) . . ?
C34 C09 C39 112.9(3) . . ?
O18 C09 H09A 108.5 . . ?
C34 C09 H09A 108.5 . . ?
C39 C09 H09A 108.5 . . ?
O16 C20 C36 109.4(3) . . ?
O16 C20 C40 109.2(3) . . ?
C36 C20 C40 112.9(3) . . ?
O16 C20 H20A 108.4 . . ?
C36 C20 H20A 108.4 . . ?
C40 C20 H20A 108.4 . . ?
C28 C21 C02 121.0(3) . . ?
C28 C21 H21A 119.5 . . ?
C02 C21 H21A 119.5 . . ?
O17 C22 C38 109.2(3) . . ?
O17 C22 C42 108.9(3) . . ?
C38 C22 C42 111.7(3) . . ?
O17 C22 H22A 109.0 . . ?
C38 C22 H22A 109.0 . . ?
C42 C22 H22A 109.0 . . ?
O13 C23 C30 110.0(3) . . ?
O13 C23 C32 108.1(3) . . ?
C30 C23 C32 113.8(3) . . ?
O13 C23 H23A 108.3 . . ?
C30 C23 H23A 108.3 . . ?
C32 C23 H23A 108.3 . . ?
C35 C24 C15 121.1(4) . . ?
C35 C24 H24A 119.4 . . ?
C15 C24 H24A 119.4 . . ?
C16 C25 C28 119.3(3) . . ?
C16 C25 H25A 120.3 . . ?
C28 C25 H25A 120.3 . . ?
O10 C26 C41 109.4(3) . . ?
O10 C26 C31 111.1(3) . . ?
C41 C26 C31 113.8(3) . . ?
O10 C26 H26A 107.4 . . ?
C41 C26 H26A 107.4 . . ?
C31 C26 H26A 107.4 . . ?
O22 C27 C48 108.8(3) . . ?
O22 C27 C49 108.7(3) . . ?
C48 C27 C49 113.3(4) . . ?
O22 C27 H27A 108.6 . . ?
C48 C27 H27A 108.6 . . ?
C49 C27 H27A 108.6 . . ?
C21 C28 C25 120.8(3) . . ?
C21 C28 H28A 119.6 . . ?
C25 C28 H28A 119.6 . . ?
O21 C29 C51 109.0(3) . . ?
O21 C29 C47 108.5(4) . . ?
C51 C29 C47 111.7(3) . . ?
O21 C29 H29A 109.2 . . ?
C51 C29 H29A 109.2 . . ?
C47 C29 H29A 109.2 . . ?
C23 C30 H30A 109.5 . . ?
C23 C30 H30B 109.5 . . ?
H30A C30 H30B 109.5 . . ?
C23 C30 H30C 109.5 . . ?
H30A C30 H30C 109.5 . . ?
H30B C30 H30C 109.5 . . ?
C26 C31 H31A 109.5 . . ?
C26 C31 H31B 109.5 . . ?
H31A C31 H31B 109.5 . . ?
C26 C31 H31C 109.5 . . ?
H31A C31 H31C 109.5 . . ?
H31B C31 H31C 109.5 . . ?
C23 C32 H32A 109.5 . . ?
C23 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C23 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C37 C33 C14 121.0(4) . . ?
C37 C33 H33A 119.5 . . ?
C14 C33 H33A 119.5 . . ?
C09 C34 H34A 109.5 . . ?
C09 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C09 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 109.5 . . ?
C24 C35 C37 121.1(4) . . ?
C24 C35 H35A 119.5 . . ?
C37 C35 H35A 119.5 . . ?
C20 C36 H36A 109.5 . . ?
C20 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C20 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C35 C37 C33 119.0(4) . . ?
C35 C37 H37A 120.5 . . ?
C33 C37 H37A 120.5 . . ?
C22 C38 H38A 109.5 . . ?
C22 C38 H38B 109.5 . . ?
H38A C38 H38B 109.5 . . ?
C22 C38 H38C 109.5 . . ?
H38A C38 H38C 109.5 . . ?
H38B C38 H38C 109.5 . . ?
C09 C39 H39A 109.5 . . ?
C09 C39 H39B 109.5 . . ?
H39A C39 H39B 109.5 . . ?
C09 C39 H39C 109.5 . . ?
H39A C39 H39C 109.5 . . ?
H39B C39 H39C 109.5 . . ?
C20 C40 H40A 109.5 . . ?
C20 C40 H40B 109.5 . . ?
H40A C40 H40B 109.5 . . ?
C20 C40 H40C 109.5 . . ?
H40A C40 H40C 109.5 . . ?
H40B C40 H40C 109.5 . . ?
C26 C41 H41A 109.5 . . ?
C26 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C26 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C22 C42 H42A 109.5 . . ?
C22 C42 H42B 109.5 . . ?
H42A C42 H42B 109.5 . . ?
C22 C42 H42C 109.5 . . ?
H42A C42 H42C 109.5 . . ?
H42B C42 H42C 109.5 . . ?
C45 C43 H43A 109.5 . . ?
C45 C43 H43B 109.5 . . ?
H43A C43 H43B 109.5 . . ?
C45 C43 H43C 109.5 . . ?
H43A C43 H43C 109.5 . . ?
H43B C43 H43C 109.5 . . ?
O20 C44 C50 111.4(4) . . ?
O20 C44 C46 109.1(4) . . ?
C50 C44 C46 115.1(4) . . ?
O20 C44 H44A 106.9 . . ?
C50 C44 H44A 106.9 . . ?
C46 C44 H44A 106.9 . . ?
O19 C45 C52 110.8(4) . . ?
O19 C45 C43 106.9(3) . . ?
C52 C45 C43 116.7(4) . . ?
O19 C45 H45A 107.3 . . ?
C52 C45 H45A 107.3 . . ?
C43 C45 H45A 107.3 . . ?
C44 C46 H46A 109.5 . . ?
C44 C46 H46B 109.5 . . ?
H46A C46 H46B 109.5 . . ?
C44 C46 H46C 109.5 . . ?
H46A C46 H46C 109.5 . . ?
H46B C46 H46C 109.5 . . ?
C29 C47 H47A 109.5 . . ?
C29 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C29 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C27 C48 H48A 109.5 . . ?
C27 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C27 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C27 C49 H49A 109.5 . . ?
C27 C49 H49B 109.5 . . ?
H49A C49 H49B 109.5 . . ?
C27 C49 H49C 109.5 . . ?
H49A C49 H49C 109.5 . . ?
H49B C49 H49C 109.5 . . ?
C44 C50 H50A 109.5 . . ?
C44 C50 H50B 109.5 . . ?
H50A C50 H50B 109.5 . . ?
C44 C50 H50C 109.5 . . ?
H50A C50 H50C 109.5 . . ?
H50B C50 H50C 109.5 . . ?
C29 C51 H51A 109.5 . . ?
C29 C51 H51B 109.5 . . ?
H51A C51 H51B 109.5 . . ?
C29 C51 H51C 109.5 . . ?
H51A C51 H51C 109.5 . . ?
H51B C51 H51C 109.5 . . ?
C45 C52 H52A 109.5 . . ?
C45 C52 H52B 109.5 . . ?
H52A C52 H52B 109.5 . . ?
C45 C52 H52C 109.5 . . ?
H52A C52 H52C 109.5 . . ?
H52B C52 H52C 109.5 . . ?
C13 N1 H1A 120.0 . . ?
C13 N1 H1B 120.0 . . ?
H1A N1 H1B 120.0 . . ?
C10 N2 H2A 120.0 . . ?
C10 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?

_refine_diff_density_max         1.086
_refine_diff_density_min         -0.537
_refine_diff_density_rms         0.083

_shelxl_version_number           2014-3

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

data_b
_database_code_depnum_ccdc_archive 'CCDC 1572543'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H160 N2 O44 Ti10'
_chemical_formula_weight         2813.49

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

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   36.5052(9)
_cell_length_b                   36.5052(9)
_cell_length_c                   26.8206(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     30953.4(17)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5466
_cell_measurement_theta_min      4.9410
_cell_measurement_theta_max      59.8400

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             13194
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.339
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.20506
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'four-circle diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_reflns_number            19672
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_av_R_equivalents  0.0375
_diffrn_reflns_limit_h_min       -41
_diffrn_reflns_limit_h_max       41
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_theta_min         3.580
_diffrn_reflns_theta_max         62.292
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measured_fraction_theta_full 0.837
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_Laue_measured_fraction_full 0.837
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_point_group_measured_fraction_full 0.837
_reflns_number_total             10435
_reflns_number_gt                4389
_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2000P)²] 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         10435
_refine_ls_number_parameters     783
_refine_ls_number_restraints     5
_refine_ls_R_factor_all          0.1963
_refine_ls_R_factor_gt           0.1127
_refine_ls_wR_factor_ref         0.3559
_refine_ls_wR_factor_gt          0.3094
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.190
_refine_ls_shift/su_mean         0.009

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
Ti4 Ti 0.77160(2) 0.10234(2) 0.47056(2) 0.10879(17) Uani 1 1 d . . . . .
Ti3 Ti 0.74903(2) 0.15078(2) 0.40151(2) 0.1220(2) Uani 1 1 d . . . . .
Ti2 Ti 0.77275(2) 0.20394(2) 0.49585(2) 0.10558(16) Uani 1 1 d . . . . .
Ti1 Ti 0.69047(2) 0.21273(2) 0.53563(2) 0.12397(18) Uani 1 1 d . . . . .
Ti5 Ti 0.85073(2) 0.09411(2) 0.42368(2) 0.1659(2) Uani 1 1 d . . . . .
O5 O 0.70236(4) 0.16930(3) 0.49726(4) 0.0954(5) Uani 1 1 d . . . . .
O8 O 0.76653(4) 0.18603(4) 0.56775(4) 0.1004(5) Uani 1 1 d . . . . .
O1 O 0.77066(3) 0.15429(3) 0.47574(4) 0.0891(5) Uani 1 1 d . . . . .
O4 O 0.63558(4) 0.16325(4) 0.54394(5) 0.1193(6) Uani 1 1 d . . . . .
O6 O 0.69033(4) 0.12875(4) 0.43011(4) 0.1012(5) Uani 1 1 d . . . . .
O17 O 0.81586(4) 0.12340(4) 0.52805(4) 0.0992(5) Uani 1 1 d . . . . .
O13 O 0.74461(4) 0.09823(4) 0.40922(4) 0.1075(6) Uani 1 1 d . . . . .
C10 C 0.63092(5) 0.11968(5) 0.47604(6) 0.0867(7) Uani 1 1 d . . . . .
O10 O 0.76265(4) 0.20743(4) 0.42607(5) 0.1198(6) Uani 1 1 d . . . . .
O14 O 0.81086(5) 0.17777(5) 0.38192(5) 0.1253(7) Uani 1 1 d . . . . .
O18 O 0.86890(5) 0.11715(5) 0.49739(5) 0.1368(7) Uani 1 1 d . . . . .
O9 O 0.82736(5) 0.23982(4) 0.49894(5) 0.1244(6) Uani 1 1 d . . . . .
O19 O 0.79204(5) 0.06234(5) 0.45325(5) 0.1409(7) Uani 1 1 d . . . . .
O22 O 0.90295(5) 0.14486(6) 0.40482(5) 0.1492(8) Uani 1 1 d . . . . .
O16 O 0.72934(5) 0.07013(4) 0.50846(4) 0.1185(6) Uani 1 1 d . . . . .
C20 C 0.67662(6) 0.13925(5) 0.46637(7) 0.0934(7) Uani 1 1 d . . . . .
O7 O 0.71234(4) 0.19191(4) 0.59778(5) 0.1111(6) Uani 1 1 d . . . . .
O3 O 0.75274(5) 0.24383(4) 0.51804(5) 0.1242(6) Uani 1 1 d . . . . .
O15 O 0.82864(4) 0.13796(5) 0.42623(5) 0.1243(7) Uani 1 1 d . . . . .
C19 C 0.60383(6) 0.08421(6) 0.44420(7) 0.0979(8) Uani 1 1 d . . . . .
H19A H 0.6155 0.0766 0.4182 0.117 Uiso 1 1 calc R U . . .
C22 C 0.76082(6) 0.19087(6) 0.65533(7) 0.0984(8) Uani 1 1 d . . . . .
C11 C 0.61276(6) 0.13117(5) 0.51304(6) 0.0941(7) Uani 1 1 d . . . . .
C12 C 0.56780(5) 0.10877(6) 0.51968(7) 0.0959(7) Uani 1 1 d . . . . .
O11 O 0.73396(4) 0.15153(6) 0.33991(5) 0.1464(8) Uani 1 1 d . . . . .
C21 C 0.74448(6) 0.18896(6) 0.60391(7) 0.0993(8) Uani 1 1 d . . . . .
C27 C 0.80039(6) 0.19525(6) 0.66161(7) 0.1100(8) Uani 1 1 d . . . . .
H27A H 0.8153 0.1946 0.6339 0.132 Uiso 1 1 calc R U . . .
C18 C 0.56216(6) 0.06241(7) 0.45208(7) 0.1095(9) Uani 1 1 d . . . . .
H18A H 0.5455 0.0392 0.4319 0.131 Uiso 1 1 calc R U . . .
C26 C 0.81802(7) 0.20049(7) 0.70821(7) 0.1191(9) Uani 1 1 d . . . . .
H26A H 0.8448 0.2036 0.7115 0.143 Uiso 1 1 calc R U . . .
C49 C 0.83785(6) 0.16700(8) 0.39419(7) 0.1254(11) Uani 1 1 d . . . . .
C25 C 0.79644(6) 0.20122(6) 0.75052(7) 0.1004(8) Uani 1 1 d . . . . .
C23 C 0.73975(7) 0.19164(6) 0.69694(7) 0.1119(9) Uani 1 1 d . . . . .
H23A H 0.7130 0.1885 0.6937 0.134 Uiso 1 1 calc R U . . .
C1 C 0.84992(6) 0.12375(6) 0.53277(7) 0.1075(8) Uani 1 1 d . . . . .
O20 O 0.83269(6) 0.08007(6) 0.36252(6) 0.1844(9) Uani 1 1 d . . . . .
O2 O 0.67630(4) 0.22932(4) 0.48094(6) 0.1389(7) Uani 1 1 d . . . . .
C24 C 0.75754(7) 0.19706(7) 0.74390(7) 0.1163(10) Uani 1 1 d . . . . .
O23 O 0.68459(5) 0.24612(5) 0.58026(7) 0.1619(8) Uani 1 1 d . . . . .
C17 C 0.54251(6) 0.07315(6) 0.48956(7) 0.1032(8) Uani 1 1 d . . . . .
C16 C 0.49858(6) 0.05004(6) 0.49913(8) 0.1129(9) Uani 1 1 d . . . . .
H16A H 0.4816 0.0261 0.4802 0.136 Uiso 1 1 calc R U . . .
C15 C 0.48092(7) 0.06162(7) 0.53440(9) 0.1250(10) Uani 1 1 d . . . . .
H15A H 0.4519 0.0457 0.5394 0.150 Uiso 1 1 calc R U . . .
C51 C 0.88745(9) 0.22752(9) 0.34128(8) 0.1509(14) Uani 1 1 d . . . . .
H51A H 0.8656 0.2332 0.3361 0.181 Uiso 1 1 calc R U . . .
C50 C 0.88030(7) 0.19157(9) 0.37110(7) 0.1432(13) Uani 1 1 d . . . . .
C14 C 0.50485(6) 0.09680(6) 0.56385(8) 0.1151(8) Uani 1 1 d . . . . .
H14A H 0.4920 0.1048 0.5880 0.138 Uiso 1 1 calc R U . . .
C13 C 0.54866(6) 0.12013(6) 0.55687(8) 0.1109(8) Uani 1 1 d . . . . .
H13A H 0.5651 0.1433 0.5771 0.133 Uiso 1 1 calc R U . . .
C58 C 0.95418(7) 0.20759(9) 0.35685(7) 0.1445(12) Uani 1 1 d . . . . .
C59 C 0.90863(8) 0.17850(9) 0.38084(8) 0.1477(12) Uani 1 1 d . . . . .
C57 C 0.98175(7) 0.19289(11) 0.36786(9) 0.2251(16) Uani 1 1 d . . . . .
H57A H 0.9698 0.1643 0.3552 0.270 Uiso 1 1 calc R U . . .
H57B H 0.9839 0.1917 0.4038 0.270 Uiso 1 1 calc R U . . .
C53 C 0.95868(8) 0.24145(9) 0.33069(10) 0.1490(13) Uani 1 1 d . . . . .
C52 C 0.92727(9) 0.25373(10) 0.32025(9) 0.1698(16) Uani 1 1 d . . . . .
H52A H 0.9378 0.2823 0.3324 0.204 Uiso 1 1 calc R U . . .
H52B H 0.9240 0.2542 0.2844 0.204 Uiso 1 1 calc R U . . .
C28 C 0.87511(10) 0.24944(13) 0.49045(11) 0.273(2) Uani 1 1 d . . . . .
H28A H 0.8802 0.2452 0.4556 0.328 Uiso 1 1 calc R U . . .
O21 O 0.86772(7) 0.05599(7) 0.43637(7) 0.2599(10) Uani 1 1 d . . . . .
C45 C 0.81350(7) 0.10260(8) 0.28806(9) 0.1367(11) Uani 1 1 d . . . . .
H45A H 0.8324 0.1292 0.3035 0.205 Uiso 1 1 calc R U . . .
H45B H 0.8222 0.1028 0.2542 0.205 Uiso 1 1 calc R U . . .
H45C H 0.7853 0.0982 0.2884 0.205 Uiso 1 1 calc R U . . .
C44 C 0.79347(14) 0.02990(8) 0.30513(12) 0.270(2) Uani 1 1 d . . . . .
H44A H 0.7824 0.0259 0.2719 0.405 Uiso 1 1 calc R U . . .
H44B H 0.8117 0.0180 0.3078 0.405 Uiso 1 1 calc R U . . .
H44C H 0.7705 0.0161 0.3284 0.405 Uiso 1 1 calc R U . . .
C29 C 0.88783(13) 0.23123(12) 0.5202(2) 0.394(3) Uani 1 1 d . . . . .
H29A H 0.9164 0.2390 0.5121 0.591 Uiso 1 1 calc R U . . .
H29B H 0.8867 0.2398 0.5537 0.591 Uiso 1 1 calc R U . . .
H29C H 0.8700 0.2011 0.5173 0.591 Uiso 1 1 calc R U . . .
C41 C 0.7368(2) -0.00508(13) 0.43301(13) 0.324(3) Uani 1 1 d . U . . .
H41A H 0.7246 -0.0346 0.4403 0.487 Uiso 1 1 calc R U . . .
H41B H 0.7164 0.0036 0.4400 0.487 Uiso 1 1 calc R U . . .
H41C H 0.7445 -0.0002 0.3984 0.487 Uiso 1 1 calc R U . . .
C42 C 0.77901(14) 0.00900(10) 0.51342(12) 0.258(2) Uani 1 1 d . . . . .
H42A H 0.8068 0.0310 0.5227 0.387 Uiso 1 1 calc R U . . .
H42B H 0.7585 0.0094 0.5355 0.387 Uiso 1 1 calc R U . . .
H42C H 0.7776 -0.0179 0.5156 0.387 Uiso 1 1 calc R U . . .
C56 C 1.02418(10) 0.21857(12) 0.34739(10) 0.205(2) Uani 1 1 d . . . . .
H56A H 1.0307 0.2011 0.3261 0.246 Uiso 1 1 calc R U . . .
H56B H 1.0445 0.2290 0.3745 0.246 Uiso 1 1 calc R U . . .
C55 C 1.02820(9) 0.25432(12) 0.31855(12) 0.1924(18) Uani 1 1 d . . . . .
H55A H 1.0547 0.2712 0.3044 0.231 Uiso 1 1 calc R U . . .
C54 C 1.00111(8) 0.26666(12) 0.30922(11) 0.1970(18) Uani 1 1 d . . . . .
H54A H 1.0083 0.2904 0.2898 0.236 Uiso 1 1 calc R U . . .
C35 C 0.71316(9) 0.16523(10) 0.26067(9) 0.1739(15) Uani 1 1 d . . . . .
H35A H 0.7354 0.1933 0.2685 0.261 Uiso 1 1 calc R U . . .
H35B H 0.7119 0.1611 0.2252 0.261 Uiso 1 1 calc R U . . .
H35C H 0.6866 0.1615 0.2723 0.261 Uiso 1 1 calc R U . . .
C7 C 0.78471(8) 0.28901(6) 0.52745(10) 0.1878(15) Uani 1 1 d D . . . .
C5 C 0.61919(10) 0.21555(13) 0.42823(13) 0.227(2) Uani 1 1 d . . . . .
H5A H 0.6100 0.1863 0.4344 0.340 Uiso 1 1 calc R U . . .
H5B H 0.5955 0.2201 0.4311 0.340 Uiso 1 1 calc R U . . .
H5C H 0.6309 0.2230 0.3953 0.340 Uiso 1 1 calc R U . . .
C37 C 0.69594(10) 0.06143(11) 0.54186(10) 0.1807(17) Uani 1 1 d . . . . .
H37A H 0.6965 0.0882 0.5479 0.217 Uiso 1 1 calc R U . . .
C9 C 0.79821(9) 0.29468(8) 0.57972(10) 0.1672(14) Uani 1 1 d . . . . .
H9A H 0.8035 0.2724 0.5894 0.251 Uiso 1 1 calc R U . . .
H9B H 0.8236 0.3215 0.5836 0.251 Uiso 1 1 calc R U . . .
H9C H 0.7764 0.2939 0.6004 0.251 Uiso 1 1 calc R U . . .
C30 C 0.89272(11) 0.30036(12) 0.50287(19) 0.247(3) Uani 1 1 d . . . . .
H30A H 0.8816 0.3117 0.4787 0.370 Uiso 1 1 calc R U . . .
H30B H 0.8836 0.3030 0.5356 0.370 Uiso 1 1 calc R U . . .
H30C H 0.9231 0.3158 0.5015 0.370 Uiso 1 1 calc R U . . .
C38 C 0.65370(12) 0.03133(10) 0.5204(2) 0.288(3) Uani 1 1 d . . . . .
H38A H 0.6320 0.0263 0.5442 0.433 Uiso 1 1 calc R U . . .
H38B H 0.6493 0.0432 0.4905 0.433 Uiso 1 1 calc R U . . .
H38C H 0.6525 0.0051 0.5126 0.433 Uiso 1 1 calc R U . . .
C34 C 0.72229(11) 0.13193(14) 0.28699(10) 0.306(2) Uani 1 1 d . . . . .
H34A H 0.7497 0.1384 0.2730 0.368 Uiso 1 1 calc R U . . .
C8 C 0.77402(10) 0.31804(7) 0.50067(13) 0.355(4) Uani 1 1 d D . . . .
H8A H 0.7952 0.3468 0.5075 0.533 Uiso 1 1 calc R U . . .
H8B H 0.7730 0.3129 0.4655 0.533 Uiso 1 1 calc R U . . .
H8C H 0.7469 0.3132 0.5117 0.533 Uiso 1 1 calc R U . . .
C43 C 0.81441(13) 0.06916(12) 0.31490(11) 0.213(2) Uani 1 1 d . . . . .
C33 C 0.80342(13) 0.25897(12) 0.35838(13) 0.216(2) Uani 1 1 d . . . . .
H33A H 0.8057 0.2823 0.3394 0.324 Uiso 1 1 calc R U . . .
H33B H 0.8294 0.2678 0.3761 0.324 Uiso 1 1 calc R U . . .
H33C H 0.7981 0.2361 0.3363 0.324 Uiso 1 1 calc R U . . .
C2 C 0.66829(15) 0.25328(12) 0.62298(13) 0.316(2) Uani 1 1 d . U . . .
C36 C 0.69900(16) 0.08731(12) 0.2866(3) 0.366(4) Uani 1 1 d . . . . .
H36A H 0.6929 0.0774 0.2527 0.548 Uiso 1 1 calc R U . . .
H36B H 0.7152 0.0764 0.3023 0.548 Uiso 1 1 calc R U . . .
H36C H 0.6730 0.0777 0.3044 0.548 Uiso 1 1 calc R U . . .
C46 C 0.9039(3) 0.07158(10) 0.45680(11) 0.439(5) Uani 1 1 d D . . . .
N14 N 0.73327(14) 0.19905(16) 0.78087(14) 0.331(4) Uani 1 1 d . . . . .
H14B H 0.7422 0.2032 0.8111 0.397 Uiso 1 1 calc R U . . .
H14C H 0.7089 0.1962 0.7740 0.397 Uiso 1 1 calc R U . . .
C32 C 0.72228(15) 0.23329(14) 0.37599(16) 0.300(2) Uani 1 1 d . U . . .
H32A H 0.7254 0.2574 0.3580 0.450 Uiso 1 1 calc R U . . .
H32B H 0.7123 0.2096 0.3538 0.450 Uiso 1 1 calc R U . . .
H32C H 0.7023 0.2266 0.4026 0.450 Uiso 1 1 calc R U . . .
C4 C 0.64996(12) 0.24058(11) 0.46309(17) 0.290(2) Uani 1 1 d . . . . .
H4A H 0.6321 0.2356 0.4924 0.348 Uiso 1 1 calc R U . . .
C31 C 0.76502(12) 0.24334(11) 0.39769(12) 0.2145(16) Uani 1 1 d . U . . .
H31A H 0.7731 0.2665 0.4215 0.257 Uiso 1 1 calc R U . . .
C39 C 0.70546(13) 0.04866(17) 0.58775(15) 0.402(3) Uani 1 1 d . . . . .
H39A H 0.6833 0.0425 0.6114 0.603 Uiso 1 1 calc R U . . .
H39B H 0.7077 0.0238 0.5825 0.603 Uiso 1 1 calc R U . . .
H39C H 0.7318 0.0710 0.6004 0.603 Uiso 1 1 calc R U . . .
C40 C 0.76962(13) 0.01622(9) 0.45998(11) 0.2220(17) Uani 1 1 d . U . . .
C3 C 0.69858(19) 0.27710(14) 0.65971(16) 0.330(3) Uani 1 1 d . U . . .
H3A H 0.6847 0.2806 0.6881 0.495 Uiso 1 1 calc R U . . .
H3B H 0.7132 0.2625 0.6696 0.495 Uiso 1 1 calc R U . . .
H3C H 0.7185 0.3043 0.6464 0.495 Uiso 1 1 calc R U . . .
C47 C 0.91592(15) 0.03697(17) 0.4346(2) 0.519(3) Uani 1 1 d . . . . .
H47A H 0.9453 0.0440 0.4349 0.623 Uiso 1 1 calc R U . . .
H47B H 0.8984 0.0178 0.4085 0.623 Uiso 1 1 calc R U . . .
C6 C 0.66195(17) 0.27899(15) 0.4548(3) 0.536(5) Uani 1 1 d . . . . .
H6A H 0.6387 0.2814 0.4419 0.804 Uiso 1 1 calc R U . . .
H6B H 0.6717 0.2947 0.4854 0.804 Uiso 1 1 calc R U . . .
H6C H 0.6846 0.2901 0.4309 0.804 Uiso 1 1 calc R U . . .
C60 C 0.8896(2) 0.03777(10) 0.49693(12) 0.351(3) Uiso 1 1 d D . . . .
H60A H 0.8596 0.0184 0.5009 0.421 Uiso 1 1 calc R U . . .
H60B H 0.9063 0.0444 0.5272 0.421 Uiso 1 1 calc R U . . .
C61 C 0.6219(2) 0.2193(2) 0.6343(3) 0.400(4) Uiso 1 1 d . . . . .
H61A H 0.6129 0.2266 0.6645 0.600 Uiso 1 1 calc R U . . .
H61B H 0.6041 0.2181 0.6073 0.600 Uiso 1 1 calc R U . . .
H61C H 0.6200 0.1923 0.6381 0.600 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti4 O16 1.7267(13) . ?
Ti4 O13 1.8847(13) . ?
Ti4 O1 1.9188(15) . ?
Ti4 O19 1.999(2) . ?
Ti4 O17 2.0826(12) . ?
Ti4 O15 2.1755(13) . ?
Ti4 Ti3 2.9484(7) . ?
Ti4 Ti5 3.2993(8) . ?
Ti3 O11 1.7459(14) . ?
Ti3 O13 1.8547(17) . ?
Ti3 O10 1.9822(16) . ?
Ti3 O6 2.0256(13) . ?
Ti3 O14 2.0294(16) . ?
Ti3 O1 2.1217(12) . ?
Ti3 Ti2 3.0392(5) . ?
Ti2 O9 1.7567(14) . ?
Ti2 O1 1.8558(14) . ?
Ti2 O10 1.9240(13) . ?
Ti2 O8 2.0124(12) . ?
Ti2 O3 2.0176(18) . ?
Ti2 O5 2.2256(12) . ?
Ti2 Ti1 3.3507(7) . ?
Ti1 O2 1.7603(18) . ?
Ti1 O23 1.796(2) . ?
Ti1 O4 1.9255(12) . ?
Ti1 O3 2.0247(15) . ?
Ti1 O5 2.1095(15) . ?
Ti1 O7 2.1448(16) . ?
Ti5 O20 1.7463(16) . ?
Ti5 O21 1.816(3) . ?
Ti5 O22 1.9468(15) . ?
Ti5 O19 2.0200(16) . ?
Ti5 O18 2.1206(14) . ?
Ti5 O15 2.124(2) . ?
Ti5 C46 2.612(9) . ?
O5 C20 1.3199(19) . ?
O8 C21 1.299(3) . ?
O4 C11 1.333(2) . ?
O6 C20 1.239(2) . ?
O17 C1 1.243(3) . ?
C10 C11 1.370(3) . ?
C10 C19 1.450(2) . ?
C10 C20 1.473(3) . ?
O10 C31 1.480(4) . ?
O14 C49 1.273(4) . ?
O18 C1 1.267(3) . ?
O9 C28 1.613(4) . ?
O19 C40 1.469(3) . ?
O22 C59 1.308(4) . ?
O16 C37 1.415(4) . ?
O7 C21 1.241(3) . ?
O3 C7 1.490(2) . ?
O15 C49 1.272(3) . ?
C19 C18 1.335(3) . ?
C22 C23 1.363(3) . ?
C22 C27 1.382(3) . ?
C22 C21 1.490(3) . ?
C11 C12 1.433(3) . ?
C12 C17 1.413(2) . ?
C12 C13 1.395(3) . ?
O11 C34 1.550(3) . ?
C27 C26 1.375(3) . ?
C18 C17 1.400(3) . ?
C26 C25 1.389(3) . ?
C49 C50 1.483(3) . ?
C25 C24 1.362(4) . ?
C25 C1 1.489(3) 13_656 ?
C23 C24 1.385(3) . ?
C1 C25 1.489(3) 13_656 ?
O20 C43 1.403(3) . ?
O2 C4 1.311(5) . ?
C24 N14 1.356(5) . ?
O23 C2 1.375(5) . ?
C17 C16 1.413(3) . ?
C16 C15 1.327(4) . ?
C15 C14 1.384(3) . ?
C51 C52 1.398(3) . ?
C51 C50 1.445(4) . ?
C50 C59 1.363(5) . ?
C14 C13 1.399(3) . ?
C58 C57 1.389(5) . ?
C58 C53 1.358(4) . ?
C58 C59 1.594(3) . ?
C57 C56 1.459(4) . ?
C53 C52 1.452(5) . ?
C53 C54 1.467(4) . ?
C28 C29 1.266(7) . ?
C28 C30 1.669(6) . ?
O21 C46 1.270(8) . ?
C45 C43 1.432(5) . ?
C44 C43 1.269(4) . ?
C41 C40 1.278(6) . ?
C42 C40 1.527(5) . ?
C56 C55 1.460(6) . ?
C55 C54 1.300(6) . ?
C35 C34 1.579(6) . ?
C7 C8 1.485(4) . ?
C7 C9 1.466(4) . ?
C5 C4 1.394(5) . ?
C37 C39 1.420(6) . ?
C37 C38 1.491(5) . ?
C34 C36 1.411(6) . ?
C33 C31 1.613(6) . ?
C2 C3 1.410(6) . ?
C2 C61 1.547(8) . ?
C46 C60 1.520(4) . ?
C46 C47 1.643(10) . ?
C32 C31 1.528(7) . ?
C4 C6 1.262(7) . ?
C47 C60 1.934(8) . ?

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
O16 Ti4 O13 101.91(6) . . ?
O16 Ti4 O1 100.33(7) . . ?
O13 Ti4 O1 82.81(6) . . ?
O16 Ti4 O19 99.89(7) . . ?
O13 Ti4 O19 96.33(7) . . ?
O1 Ti4 O19 159.49(5) . . ?
O16 Ti4 O17 94.56(5) . . ?
O13 Ti4 O17 162.53(5) . . ?
O1 Ti4 O17 88.60(5) . . ?
O19 Ti4 O17 86.42(6) . . ?
O16 Ti4 O15 172.28(9) . . ?
O13 Ti4 O15 82.91(5) . . ?
O1 Ti4 O15 86.18(6) . . ?
O19 Ti4 O15 73.40(7) . . ?
O17 Ti4 O15 81.37(5) . . ?
O16 Ti4 Ti3 110.85(7) . . ?
O13 Ti4 Ti3 37.60(5) . . ?
O1 Ti4 Ti3 45.91(3) . . ?
O19 Ti4 Ti3 127.64(4) . . ?
O17 Ti4 Ti3 129.91(4) . . ?
O15 Ti4 Ti3 76.66(5) . . ?
O16 Ti4 Ti5 133.39(7) . . ?
O13 Ti4 Ti5 96.13(5) . . ?
O1 Ti4 Ti5 124.52(4) . . ?
O19 Ti4 Ti5 35.02(4) . . ?
O17 Ti4 Ti5 76.27(4) . . ?
O15 Ti4 Ti5 39.30(5) . . ?
Ti3 Ti4 Ti5 109.592(16) . . ?
O11 Ti3 O13 104.85(8) . . ?
O11 Ti3 O10 102.41(9) . . ?
O13 Ti3 O10 152.73(6) . . ?
O11 Ti3 O6 94.92(6) . . ?
O13 Ti3 O6 91.11(6) . . ?
O10 Ti3 O6 87.26(6) . . ?
O11 Ti3 O14 91.71(6) . . ?
O13 Ti3 O14 91.79(7) . . ?
O10 Ti3 O14 86.66(7) . . ?
O6 Ti3 O14 171.84(5) . . ?
O11 Ti3 O1 176.05(6) . . ?
O13 Ti3 O1 78.18(5) . . ?
O10 Ti3 O1 74.55(6) . . ?
O6 Ti3 O1 87.51(5) . . ?
O14 Ti3 O1 85.62(5) . . ?
O11 Ti3 Ti4 142.03(8) . . ?
O13 Ti3 Ti4 38.32(4) . . ?
O10 Ti3 Ti4 114.68(4) . . ?
O6 Ti3 Ti4 94.66(4) . . ?
O14 Ti3 Ti4 82.95(5) . . ?
O1 Ti3 Ti4 40.51(4) . . ?
O11 Ti3 Ti2 140.30(8) . . ?
O13 Ti3 Ti2 114.67(4) . . ?
O10 Ti3 Ti2 38.23(4) . . ?
O6 Ti3 Ti2 81.11(3) . . ?
O14 Ti3 Ti2 90.75(4) . . ?
O1 Ti3 Ti2 37.04(4) . . ?
Ti4 Ti3 Ti2 77.540(15) . . ?
O9 Ti2 O1 102.64(7) . . ?
O9 Ti2 O10 100.38(6) . . ?
O1 Ti2 O10 82.32(6) . . ?
O9 Ti2 O8 95.66(6) . . ?
O1 Ti2 O8 91.05(6) . . ?
O10 Ti2 O8 163.63(5) . . ?
O9 Ti2 O3 97.67(7) . . ?
O1 Ti2 O3 159.66(5) . . ?
O10 Ti2 O3 95.08(7) . . ?
O8 Ti2 O3 85.94(6) . . ?
O9 Ti2 O5 168.61(8) . . ?
O1 Ti2 O5 88.74(5) . . ?
O10 Ti2 O5 81.32(5) . . ?
O8 Ti2 O5 83.60(5) . . ?
O3 Ti2 O5 70.94(5) . . ?
O9 Ti2 Ti3 111.72(5) . . ?
O1 Ti2 Ti3 43.53(4) . . ?
O10 Ti2 Ti3 39.61(5) . . ?
O8 Ti2 Ti3 129.83(4) . . ?
O3 Ti2 Ti3 128.02(5) . . ?
O5 Ti2 Ti3 76.81(3) . . ?
O9 Ti2 Ti1 130.63(6) . . ?
O1 Ti2 Ti1 125.81(4) . . ?
O10 Ti2 Ti1 95.32(6) . . ?
O8 Ti2 Ti1 76.42(5) . . ?
O3 Ti2 Ti1 34.08(3) . . ?
O5 Ti2 Ti1 38.14(4) . . ?
Ti3 Ti2 Ti1 110.082(17) . . ?
O2 Ti1 O23 99.59(9) . . ?
O2 Ti1 O4 94.15(6) . . ?
O23 Ti1 O4 97.94(7) . . ?
O2 Ti1 O3 93.07(7) . . ?
O23 Ti1 O3 104.86(6) . . ?
O4 Ti1 O3 154.55(8) . . ?
O2 Ti1 O5 93.34(7) . . ?
O23 Ti1 O5 167.04(8) . . ?
O4 Ti1 O5 81.96(6) . . ?
O3 Ti1 O5 73.28(5) . . ?
O2 Ti1 O7 174.20(8) . . ?
O23 Ti1 O7 85.10(8) . . ?
O4 Ti1 O7 88.55(6) . . ?
O3 Ti1 O7 82.37(6) . . ?
O5 Ti1 O7 81.94(6) . . ?
O2 Ti1 Ti2 101.48(6) . . ?
O23 Ti1 Ti2 133.96(6) . . ?
O4 Ti1 Ti2 120.61(6) . . ?
O3 Ti1 Ti2 33.95(5) . . ?
O5 Ti1 Ti2 40.66(3) . . ?
O7 Ti1 Ti2 72.73(4) . . ?
O20 Ti5 O21 100.04(11) . . ?
O20 Ti5 O22 94.67(7) . . ?
O21 Ti5 O22 103.35(10) . . ?
O20 Ti5 O19 93.67(7) . . ?
O21 Ti5 O19 99.04(9) . . ?
O22 Ti5 O19 154.31(9) . . ?
O20 Ti5 O18 171.59(11) . . ?
O21 Ti5 O18 88.30(8) . . ?
O22 Ti5 O18 84.35(6) . . ?
O19 Ti5 O18 83.88(6) . . ?
O20 Ti5 O15 91.25(10) . . ?
O21 Ti5 O15 167.24(8) . . ?
O22 Ti5 O15 81.44(8) . . ?
O19 Ti5 O15 74.12(7) . . ?
O18 Ti5 O15 80.34(7) . . ?
O20 Ti5 C46 117.23(12) . . ?
O21 Ti5 C46 26.28(9) . . ?
O22 Ti5 C46 81.96(12) . . ?
O19 Ti5 C46 115.30(12) . . ?
O18 Ti5 C46 70.96(10) . . ?
O15 Ti5 C46 148.01(8) . . ?
O20 Ti5 Ti4 99.54(8) . . ?
O21 Ti5 Ti4 130.41(7) . . ?
O22 Ti5 Ti4 119.84(7) . . ?
O19 Ti5 Ti4 34.60(5) . . ?
O18 Ti5 Ti4 73.92(5) . . ?
O15 Ti5 Ti4 40.46(4) . . ?
C46 Ti5 Ti4 136.13(10) . . ?
C20 O5 Ti1 127.04(14) . . ?
C20 O5 Ti2 126.98(13) . . ?
Ti1 O5 Ti2 101.20(4) . . ?
C21 O8 Ti2 131.51(15) . . ?
Ti2 O1 Ti4 166.91(7) . . ?
Ti2 O1 Ti3 99.43(6) . . ?
Ti4 O1 Ti3 93.59(5) . . ?
C11 O4 Ti1 130.72(12) . . ?
C20 O6 Ti3 133.25(10) . . ?
C1 O17 Ti4 131.79(12) . . ?
Ti3 O13 Ti4 104.08(6) . . ?
C11 C10 C19 118.78(16) . . ?
C11 C10 C20 125.67(15) . . ?
C19 C10 C20 115.51(17) . . ?
C31 O10 Ti2 129.08(16) . . ?
C31 O10 Ti3 128.76(15) . . ?
Ti2 O10 Ti3 102.15(7) . . ?
C49 O14 Ti3 128.89(13) . . ?
C1 O18 Ti5 132.95(14) . . ?
C28 O9 Ti2 148.85(19) . . ?
C40 O19 Ti4 127.7(2) . . ?
C40 O19 Ti5 122.0(2) . . ?
Ti4 O19 Ti5 110.38(7) . . ?
C59 O22 Ti5 129.91(17) . . ?
C37 O16 Ti4 154.4(2) . . ?
O6 C20 O5 121.33(16) . . ?
O6 C20 C10 121.54(14) . . ?
O5 C20 C10 117.10(17) . . ?
C21 O7 Ti1 132.00(12) . . ?
C7 O3 Ti2 118.88(15) . . ?
C7 O3 Ti1 128.27(16) . . ?
Ti2 O3 Ti1 111.97(6) . . ?
C49 O15 Ti5 124.37(16) . . ?
C49 O15 Ti4 129.98(17) . . ?
Ti5 O15 Ti4 100.24(7) . . ?
C18 C19 C10 120.3(2) . . ?
C23 C22 C27 117.74(18) . . ?
C23 C22 C21 122.8(2) . . ?
C27 C22 C21 119.28(18) . . ?
O4 C11 C10 122.25(17) . . ?
O4 C11 C12 117.29(18) . . ?
C10 C11 C12 120.45(15) . . ?
C17 C12 C13 119.25(16) . . ?
C17 C12 C11 119.30(19) . . ?
C13 C12 C11 121.37(16) . . ?
C34 O11 Ti3 151.1(3) . . ?
O7 C21 O8 124.05(18) . . ?
O7 C21 C22 119.48(19) . . ?
O8 C21 C22 116.4(2) . . ?
C26 C27 C22 121.1(2) . . ?
C19 C18 C17 122.52(18) . . ?
C27 C26 C25 121.0(2) . . ?
O15 C49 O14 120.59(19) . . ?
O15 C49 C50 123.2(3) . . ?
O14 C49 C50 116.2(2) . . ?
C24 C25 C26 117.44(19) . . ?
C24 C25 C1 121.7(2) . 13_656 ?
C26 C25 C1 120.7(2) . 13_656 ?
C22 C23 C24 121.2(2) . . ?
O17 C1 O18 124.11(17) . . ?
O17 C1 C25 119.11(19) . 13_656 ?
O18 C1 C25 116.8(2) . 13_656 ?
C43 O20 Ti5 173.8(3) . . ?
C4 O2 Ti1 143.1(2) . . ?
C25 C24 N14 124.8(3) . . ?
C25 C24 C23 121.5(2) . . ?
N14 C24 C23 113.6(3) . . ?
C2 O23 Ti1 153.4(2) . . ?
C12 C17 C18 118.53(17) . . ?
C12 C17 C16 118.0(2) . . ?
C18 C17 C16 123.42(18) . . ?
C15 C16 C17 121.76(19) . . ?
C16 C15 C14 121.4(2) . . ?
C52 C51 C50 119.9(3) . . ?
C59 C50 C51 126.8(2) . . ?
C59 C50 C49 117.0(2) . . ?
C51 C50 C49 116.1(3) . . ?
C15 C14 C13 119.2(2) . . ?
C12 C13 C14 120.34(17) . . ?
C57 C58 C53 132.9(2) . . ?
C57 C58 C59 111.9(2) . . ?
C53 C58 C59 115.2(3) . . ?
O22 C59 C50 129.1(2) . . ?
O22 C59 C58 116.5(3) . . ?
C50 C59 C58 114.3(2) . . ?
C58 C57 C56 114.4(3) . . ?
C58 C53 C52 128.8(2) . . ?
C58 C53 C54 112.5(3) . . ?
C52 C53 C54 118.6(3) . . ?
C51 C52 C53 114.9(3) . . ?
C29 C28 O9 115.9(3) . . ?
C29 C28 C30 114.9(3) . . ?
O9 C28 C30 89.2(3) . . ?
C46 O21 Ti5 114.4(3) . . ?
C57 C56 C55 111.9(4) . . ?
C54 C55 C56 131.2(3) . . ?
C55 C54 C53 117.0(3) . . ?
C8 C7 O3 111.6(2) . . ?
C8 C7 C9 123.5(3) . . ?
O3 C7 C9 109.89(18) . . ?
O16 C37 C39 107.3(3) . . ?
O16 C37 C38 112.2(3) . . ?
C39 C37 C38 115.2(3) . . ?
C36 C34 O11 114.1(4) . . ?
C36 C34 C35 130.4(4) . . ?
O11 C34 C35 99.7(3) . . ?
C44 C43 O20 116.1(3) . . ?
C44 C43 C45 127.0(3) . . ?
O20 C43 C45 115.2(3) . . ?
O23 C2 C3 114.8(5) . . ?
O23 C2 C61 114.5(4) . . ?
C3 C2 C61 124.3(4) . . ?
O21 C46 C60 94.9(4) . . ?
O21 C46 C47 96.7(3) . . ?
C60 C46 C47 75.3(4) . . ?
O21 C46 Ti5 39.3(3) . . ?
C60 C46 Ti5 119.4(6) . . ?
C47 C46 Ti5 130.2(3) . . ?
C6 C4 O2 120.7(4) . . ?
C6 C4 C5 109.2(5) . . ?
O2 C4 C5 121.1(4) . . ?
O10 C31 C32 112.5(3) . . ?
O10 C31 C33 107.8(4) . . ?
C32 C31 C33 116.0(3) . . ?
C41 C40 O19 116.3(4) . . ?
C41 C40 C42 130.5(3) . . ?
O19 C40 C42 105.6(2) . . ?
C46 C47 C60 49.5(2) . . ?
C46 C60 C47 55.2(4) . . ?

_refine_diff_density_max         0.842
_refine_diff_density_min         -0.391
_refine_diff_density_rms         0.097

_shelxl_version_number           2014-3

# SQUEEZE RESULTS (APPEND TO CIF)
# 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 0.000 185 11 ' '
2 0.000 0.000 0.231 57 6 ' '
3 0.000 0.000 0.501 365 31 ' '
4 0.000 0.000 0.771 57 6 ' '
5 -0.016 0.318 0.956 28 4 ' '
6 0.016 0.333 0.622 27 4 ' '
7 0.000 0.349 0.289 28 4 ' '
8 -0.011 0.374 0.776 21 1 ' '
9 -0.017 0.415 0.974 21 1 ' '
10 0.017 0.585 0.026 21 1 ' '
11 0.010 0.626 0.224 20 1 ' '
12 0.000 0.651 0.711 28 4 ' '
13 -0.016 0.667 0.378 27 4 ' '
14 0.016 0.682 0.044 28 4 ' '
15 0.041 0.718 0.557 20 1 ' '
16 0.051 0.344 0.109 20 1 ' '
17 0.082 0.766 0.359 20 1 ' '
18 0.099 0.351 0.307 20 1 ' '
19 0.333 0.667 0.167 372 32 ' '
20 0.333 0.667 0.667 181 11 ' '
21 0.234 0.316 0.359 20 1 ' '
22 0.251 0.901 0.307 20 1 ' '
23 0.282 0.323 0.557 20 1 ' '
24 0.333 0.667 0.895 55 5 ' '
25 0.333 0.667 0.438 56 5 ' '
26 0.293 0.949 0.109 20 1 ' '
27 0.317 0.984 0.622 28 4 ' '
28 0.316 0.082 0.640 20 1 ' '
29 0.323 0.041 0.443 20 1 ' '
30 0.333 0.317 0.378 27 4 ' '
31 0.318 0.333 0.044 28 4 ' '
32 0.333 0.016 0.956 28 4 ' '
33 0.344 0.293 0.891 20 1 ' '
34 0.349 0.349 0.711 28 4 ' '
35 0.349 0.000 0.289 28 4 ' '
36 0.351 0.251 0.693 21 1 ' '
37 0.374 0.384 0.224 20 1 ' '
38 0.384 1.010 0.776 21 1 ' '
39 0.415 0.432 0.026 20 1 ' '
40 0.432 0.017 0.974 21 1 ' '
41 0.667 0.333 0.833 372 32 ' '
42 0.667 0.333 0.333 181 11 ' '
43 0.567 0.983 0.026 21 1 ' '
44 0.585 0.567 0.974 20 1 ' '
45 0.616 0.989 0.224 21 1 ' '
46 0.667 0.333 0.562 56 5 ' '
47 0.667 0.333 0.105 55 5 ' '
48 0.626 0.616 0.776 20 1 ' '
49 0.651 0.651 0.289 28 4 ' '
50 0.649 0.749 0.307 21 1 ' '
51 0.651 0.000 0.711 28 4 ' '
52 0.656 0.707 0.109 20 1 ' '
53 0.667 0.984 0.044 28 4 ' '
54 0.667 0.682 0.622 27 4 ' '
55 0.682 0.016 0.378 28 4 ' '
56 0.677 0.959 0.557 20 1 ' '
57 0.682 0.666 0.956 28 4 ' '
58 0.684 0.918 0.360 20 1 ' '
59 0.707 0.051 0.891 20 1 ' '
60 0.718 0.677 0.443 20 1 ' '
61 0.749 0.099 0.693 20 1 ' '
62 0.766 0.684 0.640 20 1 ' '
63 0.901 0.649 0.693 20 1 ' '
64 0.918 0.234 0.640 20 1 ' '
65 0.949 0.656 0.891 20 1 ' '
66 0.959 0.282 0.443 20 1 ' '
_platon_squeeze_details          
;
;

####################################################################### 
# 
# 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_b_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 1572542'
_audit_update_record             
;
2017-10-17 deposited with the CCDC.
2017-10-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C120 H158 O44 Ti10'
_chemical_formula_weight         2783.45

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

_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_H-M_alt        'R -3 :H'
_space_group_name_Hall           '-R 3'

_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'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'

_cell_length_a                   36.3512(11)
_cell_length_b                   36.3512(11)
_cell_length_c                   26.7591(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     30622(2)
_cell_formula_units_Z            9
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    5200
_cell_measurement_theta_min      4.8520
_cell_measurement_theta_max      72.7520

_exptl_crystal_description       polyhedron
_exptl_crystal_colour            yellow
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_density_diffrn    1.358
_exptl_crystal_F_000             13050
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_exptl_absorpt_coefficient_mu    5.386
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54125
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_oxdiff_exptl_absorpt_empirical_full_min 0.669
_oxdiff_exptl_absorpt_empirical_full_max 1.877
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_type           CuK\a
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 10.3503
_diffrn_reflns_number            21495
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_k_min       -41
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         3.589
_diffrn_reflns_theta_max         74.306
_diffrn_reflns_theta_full        67.679
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             13397
_reflns_number_gt                8249
_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 FRAMBO'
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.2800P)²] 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         13397
_refine_ls_number_parameters     784
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.1343
_refine_ls_R_factor_gt           0.1054
_refine_ls_wR_factor_ref         0.3797
_refine_ls_wR_factor_gt          0.3356
_refine_ls_goodness_of_fit_ref   1.006
_refine_ls_restrained_S_all      1.011
_refine_ls_shift/su_max          0.726
_refine_ls_shift/su_mean         0.017

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ti1 Ti 0.56059(2) 0.09933(2) 0.66970(2) 0.09417(9) Uani 1 1 d . . . . .
Ti2 Ti 0.56041(2) -0.00205(2) 0.69793(2) 0.09474(10) Uani 1 1 d . . . . .
Ti3 Ti 0.58399(2) 0.06986(2) 0.76545(2) 0.10669(12) Uani 1 1 d . . . . .
Ti4 Ti 0.47855(2) -0.08786(2) 0.74518(2) 0.12361(16) Uani 1 1 d . . . . .
Ti5 Ti 0.64362(2) 0.19039(2) 0.62919(2) 0.11041(11) Uani 1 1 d . . . . .
O6 O 0.56771(3) 0.08650(3) 0.59782(3) 0.0889(3) Uani 1 1 d . . . . .
O4 O 0.63132(3) 0.13473(3) 0.66823(4) 0.0889(3) Uani 1 1 d . . . . .
O12 O 0.56276(3) 0.05183(3) 0.69102(3) 0.0833(3) Uani 1 1 d . . . . .
O9 O 0.64342(3) 0.10679(3) 0.73582(4) 0.0905(3) Uani 1 1 d . . . . .
O14 O 0.51674(3) -0.02513(3) 0.63932(3) 0.0938(4) Uani 1 1 d . . . . .
O15 O 0.58716(3) 0.02195(3) 0.75938(3) 0.0927(4) Uani 1 1 d . . . . .
O3 O 0.69897(3) 0.19625(3) 0.62251(4) 0.1040(4) Uani 1 1 d . . . . .
O17 O 0.52198(3) 0.03685(4) 0.78477(4) 0.1054(4) Uani 1 1 d . . . . .
O10 O 0.56993(3) 0.11430(4) 0.73955(5) 0.1090(4) Uani 1 1 d . . . . .
O22 O 0.46202(4) -0.08431(4) 0.67055(4) 0.1158(5) Uani 1 1 d . . . . .
C10 C 0.70291(4) 0.15640(4) 0.69060(5) 0.0802(4) Uani 1 1 d . . . . .
O19 O 0.50229(3) -0.02166(4) 0.74139(4) 0.1051(5) Uani 1 1 d . . . . .
O5 O 0.62183(3) 0.14657(3) 0.56668(4) 0.1017(4) Uani 1 1 d . . . . .
C8 C 0.76599(4) 0.20786(4) 0.64648(5) 0.0813(4) Uani 1 1 d . . . . .
C9 C 0.72140(4) 0.18611(4) 0.65275(5) 0.0844(4) Uani 1 1 d . . . . .
O8 O 0.50584(3) 0.08073(4) 0.66650(5) 0.1071(4) Uani 1 1 d . . . . .
C6 C 0.72921(4) 0.14739(5) 0.72122(5) 0.0847(5) Uani 1 1 d . . . . .
H6A H 0.7169 0.1275 0.7468 0.102 Uiso 1 1 calc R U . . .
C33 C 0.53396(5) 0.06008(5) 0.50471(5) 0.0947(5) Uani 1 1 d . . . . .
H33A H 0.5191 0.0443 0.5325 0.114 Uiso 1 1 calc R U . . .
C28 C 0.57297(4) 0.09564(5) 0.51030(5) 0.0903(4) Uani 1 1 d . . . . .
O13 O 0.60311(3) 0.00713(4) 0.66003(4) 0.1036(4) Uani 1 1 d . . . . .
C5 C 0.77188(5) 0.16696(5) 0.71423(5) 0.0903(5) Uani 1 1 d . . . . .
H5A H 0.7885 0.1601 0.7343 0.108 Uiso 1 1 calc R U . . .
O20 O 0.42685(4) -0.08801(5) 0.76231(4) 0.1278(6) Uani 1 1 d . . . . .
C11 C 0.65712(4) 0.13179(4) 0.69866(5) 0.0840(4) Uani 1 1 d . . . . .
O16 O 0.53860(4) -0.06200(4) 0.71613(4) 0.1146(5) Uani 1 1 d . . . . .
C4 C 0.79088(4) 0.19784(4) 0.67628(5) 0.0844(4) Uani 1 1 d . . . . .
O11 O 0.60007(4) 0.08688(5) 0.82740(4) 0.1339(6) Uani 1 1 d . . . . .
O7 O 0.58074(3) 0.15932(3) 0.64630(5) 0.1127(4) Uani 1 1 d . . . . .
C31 C 0.53829(5) 0.07117(5) 0.41564(6) 0.0933(5) Uani 1 1 d . . . . .
C27 C 0.58923(4) 0.11113(5) 0.56251(6) 0.0923(5) Uani 1 1 d . . . . .
C32 C 0.51645(5) 0.04753(5) 0.45692(5) 0.0989(6) Uani 1 1 d . . . . .
H32A H 0.4901 0.0232 0.4530 0.119 Uiso 1 1 calc R U . . .
O23 O 0.49676(5) -0.08318(5) 0.80733(5) 0.1312(6) Uani 1 1 d . . . . .
C2 C 0.85397(5) 0.24799(5) 0.63019(7) 0.1056(6) Uani 1 1 d . . . . .
H2A H 0.8830 0.2608 0.6244 0.127 Uiso 1 1 calc R U . . .
O21 O 0.45670(6) -0.14309(5) 0.73474(5) 0.1574(6) Uani 1 1 d . U . . .
C49 C 0.49534(5) 0.00096(6) 0.77455(6) 0.1058(7) Uani 1 1 d . . . . .
C3AA C 0.48193(5) -0.05885(5) 0.63550(6) 0.0955(6) Uani 1 1 d . . . . .
C29 C 0.59446(5) 0.11848(5) 0.46910(6) 0.1020(6) Uani 1 1 d . . . . .
H29A H 0.6210 0.1427 0.4729 0.122 Uiso 1 1 calc R U . . .
C60 C 0.45240(6) -0.01824(7) 0.79612(6) 0.1173(8) Uani 1 1 d . . . . .
C48 C 0.51935(6) -0.04123(6) 0.87971(6) 0.1076(7) Uani 1 1 d . . . . .
H48A H 0.5047 -0.0293 0.8623 0.161 Uiso 1 1 calc R U . . .
H48B H 0.5053 -0.0531 0.9108 0.161 Uiso 1 1 calc R U . . .
H48C H 0.5481 -0.0194 0.8861 0.161 Uiso 1 1 calc R U . . .
C3 C 0.83549(5) 0.21830(5) 0.66684(6) 0.0999(6) Uani 1 1 d . . . . .
H3A H 0.8523 0.2112 0.6862 0.120 Uiso 1 1 calc R U . . .
C1 C 0.82858(6) 0.25925(5) 0.60081(7) 0.1054(7) Uani 1 1 d . . . . .
H1A H 0.8410 0.2798 0.5760 0.127 Uiso 1 1 calc R U . . .
C7 C 0.78631(5) 0.24009(4) 0.60901(6) 0.0920(5) Uani 1 1 d . . . . .
H7A H 0.7700 0.2480 0.5899 0.110 Uiso 1 1 calc R U . . .
O2 O 0.65753(4) 0.22214(4) 0.68362(7) 0.1335(6) Uani 1 1 d . . . . .
C59 C 0.44394(6) 0.00936(8) 0.82558(6) 0.1276(9) Uani 1 1 d . . . . .
H59A H 0.4653 0.0373 0.8308 0.153 Uiso 1 1 calc R U . . .
O1 O 0.65026(5) 0.22940(4) 0.58353(7) 0.1492(6) Uani 1 1 d . . . . .
C30 C 0.57722(5) 0.10604(6) 0.42176(6) 0.1037(6) Uani 1 1 d . . . . .
H30A H 0.5924 0.1217 0.3940 0.124 Uiso 1 1 calc R U . . .
C58 C 0.40421(6) -0.00497(8) 0.84652(7) 0.1320(9) Uani 1 1 d . . . . .
H58A H 0.3991 0.0131 0.8661 0.158 Uiso 1 1 calc R U . . .
C52 C 0.37842(6) -0.07677(8) 0.80874(6) 0.1324(9) Uani 1 1 d . . . . .
C54 C 0.30651(8) -0.13190(11) 0.82018(8) 0.1717(15) Uani 1 1 d . . . . .
H54A H 0.2847 -0.1594 0.8135 0.206 Uiso 1 1 calc R U . . .
C51 C 0.42157(6) -0.06106(7) 0.78762(6) 0.1219(9) Uani 1 1 d . . . . .
C19 C 0.53597(6) 0.16492(7) 0.58273(9) 0.1401(8) Uani 1 1 d . . . . .
H19A H 0.5388 0.1416 0.5704 0.210 Uiso 1 1 calc R U . . .
H19B H 0.5066 0.1574 0.5820 0.210 Uiso 1 1 calc R U . . .
H19C H 0.5522 0.1894 0.5621 0.210 Uiso 1 1 calc R U . . .
C34 C 0.60337(9) 0.07954(9) 0.87939(8) 0.1466(12) Uani 1 1 d . . . . .
H34A H 0.5751 0.0590 0.8919 0.176 Uiso 1 1 calc R U . . .
C24 C 0.46241(7) 0.05558(9) 0.67998(11) 0.1476(11) Uani 1 1 d . . . . .
H24A H 0.4615 0.0536 0.7165 0.177 Uiso 1 1 calc R U . . .
C55 C 0.30044(8) -0.10471(13) 0.84890(10) 0.199(2) Uani 1 1 d . . . . .
H55A H 0.2737 -0.1149 0.8629 0.239 Uiso 1 1 calc R U . . .
C56 C 0.33070(7) -0.06314(13) 0.85906(9) 0.1820(17) Uani 1 1 d . . . . .
H56A H 0.3244 -0.0461 0.8792 0.218 Uiso 1 1 calc R U . . .
C36 C 0.61878(8) 0.12397(8) 0.90640(8) 0.1506(12) Uani 1 1 d . . . . .
H36A H 0.6216 0.1210 0.9416 0.226 Uiso 1 1 calc R U . . .
H36B H 0.6457 0.1448 0.8930 0.226 Uiso 1 1 calc R U . . .
H36C H 0.5983 0.1329 0.9009 0.226 Uiso 1 1 calc R U . . .
C57 C 0.37145(6) -0.04727(9) 0.83798(7) 0.1400(11) Uani 1 1 d . . . . .
C18 C 0.55174(6) 0.17454(6) 0.63411(9) 0.1506(7) Uani 1 1 d D . . . .
C47 C 0.53676(9) -0.09539(7) 0.86339(9) 0.1658(11) Uani 1 1 d . . . . .
H47A H 0.5516 -0.0844 0.8944 0.249 Uiso 1 1 calc R U . . .
H47B H 0.5152 -0.1246 0.8677 0.249 Uiso 1 1 calc R U . . .
H47C H 0.5564 -0.0934 0.8382 0.249 Uiso 1 1 calc R U . . .
C53 C 0.34747(7) -0.11618(9) 0.80129(7) 0.1464(11) Uani 1 1 d . . . . .
H53A H 0.3533 -0.1343 0.7826 0.176 Uiso 1 1 calc R U . . .
C25 C 0.44591(7) 0.01382(8) 0.66178(11) 0.1481(11) Uani 1 1 d . . . . .
H25A H 0.4166 -0.0029 0.6711 0.222 Uiso 1 1 calc R U . . .
H25B H 0.4484 0.0145 0.6260 0.222 Uiso 1 1 calc R U . . .
H25C H 0.4616 0.0015 0.6759 0.222 Uiso 1 1 calc R U . . .
C40 C 0.55823(9) -0.08892(8) 0.71186(10) 0.1634(11) Uani 1 1 d . . . . .
H40A H 0.5405 -0.1138 0.7327 0.196 Uiso 1 1 calc R U . . .
C37 C 0.63776(7) 0.03303(9) 0.62617(9) 0.1520(10) Uani 1 1 d . . . . .
H37A H 0.6378 0.0597 0.6209 0.182 Uiso 1 1 calc R U . . .
C14 C 0.71731(10) 0.26503(10) 0.73571(11) 0.1850(15) Uani 1 1 d . . . . .
H14A H 0.7227 0.2423 0.7286 0.277 Uiso 1 1 calc R U . . .
H14B H 0.7413 0.2915 0.7256 0.277 Uiso 1 1 calc R U . . .
H14C H 0.7127 0.2658 0.7709 0.277 Uiso 1 1 calc R U . . .
C41 C 0.54796(10) -0.10587(8) 0.65695(10) 0.1818(13) Uani 1 1 d . . . . .
H41A H 0.5182 -0.1174 0.6506 0.273 Uiso 1 1 calc R U . . .
H41B H 0.5641 -0.0830 0.6341 0.273 Uiso 1 1 calc R U . . .
H41C H 0.5553 -0.1276 0.6524 0.273 Uiso 1 1 calc R U . . .
C22 C 0.53019(9) 0.12514(9) 0.80652(11) 0.1689(11) Uani 1 1 d . . . . .
H22A H 0.5282 0.1465 0.8254 0.253 Uiso 1 1 calc R U . . .
H22B H 0.5040 0.1079 0.7891 0.253 Uiso 1 1 calc R U . . .
H22C H 0.5356 0.1076 0.8287 0.253 Uiso 1 1 calc R U . . .
C26 C 0.43847(7) 0.07703(8) 0.66596(13) 0.1851(13) Uani 1 1 d . . . . .
H26A H 0.4092 0.0595 0.6754 0.278 Uiso 1 1 calc R U . . .
H26B H 0.4503 0.1038 0.6829 0.278 Uiso 1 1 calc R U . . .
H26C H 0.4403 0.0816 0.6305 0.278 Uiso 1 1 calc R U . . .
C42 C 0.59845(8) -0.06990(8) 0.73441(11) 0.1892(10) Uani 1 1 d . . . . .
H42A H 0.6102 -0.0882 0.7309 0.284 Uiso 1 1 calc R U . . .
H42B H 0.6168 -0.0432 0.7185 0.284 Uiso 1 1 calc R U . . .
H42C H 0.5958 -0.0653 0.7692 0.284 Uiso 1 1 calc R U . . .
C39 C 0.67876(7) 0.04351(9) 0.6523(2) 0.241(3) Uani 1 1 d . . . . .
H39A H 0.6808 0.0580 0.6832 0.362 Uiso 1 1 calc R U . . .
H39B H 0.6791 0.0177 0.6592 0.362 Uiso 1 1 calc R U . . .
H39C H 0.7024 0.0615 0.6313 0.362 Uiso 1 1 calc R U . . .
C35 C 0.63242(8) 0.05997(9) 0.88384(12) 0.1610(12) Uani 1 1 d . . . . .
H35A H 0.6352 0.0547 0.9184 0.242 Uiso 1 1 calc R U . . .
H35B H 0.6201 0.0337 0.8656 0.242 Uiso 1 1 calc R U . . .
H35C H 0.6599 0.0793 0.8703 0.242 Uiso 1 1 calc R U . . .
C23 C 0.61230(13) 0.17818(10) 0.78753(16) 0.260(2) Uani 1 1 d . . . . .
H23A H 0.6116 0.2002 0.8066 0.391 Uiso 1 1 calc R U . . .
H23B H 0.6220 0.1632 0.8084 0.391 Uiso 1 1 calc R U . . .
H23C H 0.6313 0.1906 0.7598 0.391 Uiso 1 1 calc R U . . .
C21 C 0.56720(9) 0.14684(9) 0.76797(11) 0.1814(11) Uani 1 1 d . . . . .
H21A H 0.5595 0.1626 0.7444 0.218 Uiso 1 1 calc R U . . .
C46 C 0.51944(10) -0.07367(10) 0.84993(11) 0.2159(13) Uani 1 1 d . . . . .
C20 C 0.55295(8) 0.20404(8) 0.66278(15) 0.4382(12) Uani 1 1 d D . . . .
H20A H 0.5326 0.2116 0.6513 0.657 Uiso 1 1 calc R U . . .
H20B H 0.5463 0.1937 0.6965 0.657 Uiso 1 1 calc R U . . .
H20C H 0.5809 0.2286 0.6617 0.657 Uiso 1 1 calc R U . . .
C38 C 0.62835(13) 0.01119(13) 0.57904(11) 0.338(2) Uani 1 1 d . . . . .
H38A H 0.6508 0.0276 0.5557 0.507 Uiso 1 1 calc R U . . .
H38B H 0.6260 -0.0161 0.5836 0.507 Uiso 1 1 calc R U . . .
H38C H 0.6020 0.0075 0.5663 0.507 Uiso 1 1 calc R U . . .
C12 C 0.67915(14) 0.25815(11) 0.7080(2) 0.374(2) Uani 1 1 d . . . . .
C15 C 0.66311(11) 0.24306(11) 0.53377(13) 0.2656(15) Uani 1 1 d . . . . .
C16 C 0.63733(13) 0.24975(16) 0.50321(19) 0.312(2) Uani 1 1 d . . . . .
H16A H 0.6086 0.2339 0.5152 0.468 Uiso 1 1 calc R U . . .
H16B H 0.6463 0.2795 0.5028 0.468 Uiso 1 1 calc R U . . .
H16C H 0.6388 0.2406 0.4700 0.468 Uiso 1 1 calc R U . . .
C43 C 0.4258(2) -0.17676(12) 0.70113(15) 0.3866(11) Uani 1 1 d . U . . .
H43A H 0.4273 -0.1700 0.6655 0.464 Uiso 1 1 calc R U . . .
C45 C 0.4401(2) -0.2141(2) 0.7190(4) 0.435(6) Uani 1 1 d . . . . .
H45A H 0.4232 -0.2400 0.7010 0.652 Uiso 1 1 calc R U . . .
H45B H 0.4696 -0.2033 0.7117 0.652 Uiso 1 1 calc R U . . .
H45C H 0.4353 -0.2194 0.7542 0.652 Uiso 1 1 calc R U . . .
C44 C 0.37484(18) -0.19224(16) 0.7341(3) 0.576(4) Uani 1 1 d . . . . .
H44A H 0.3517 -0.2144 0.7157 0.864 Uiso 1 1 calc R U . . .
H44B H 0.3757 -0.2022 0.7670 0.864 Uiso 1 1 calc R U . . .
H44C H 0.3710 -0.1680 0.7364 0.864 Uiso 1 1 calc R U . . .
C17 C 0.70758(18) 0.2618(2) 0.5267(2) 0.406(4) Uani 1 1 d . . . . .
H17A H 0.7193 0.2526 0.5527 0.609 Uiso 1 1 calc R U . . .
H17B H 0.7130 0.2534 0.4948 0.609 Uiso 1 1 calc R U . . .
H17C H 0.7205 0.2922 0.5277 0.609 Uiso 1 1 calc R U . . .
C13 C 0.6706(2) 0.28635(16) 0.7156(5) 0.683(8) Uani 1 1 d . . . . .
H13A H 0.6930 0.3087 0.7347 1.025 Uiso 1 1 calc R U . . .
H13B H 0.6678 0.2975 0.6842 1.025 Uiso 1 1 calc R U . . .
H13C H 0.6444 0.2749 0.7337 1.025 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ti1 O8 1.7550(10) . ?
Ti1 O12 1.8573(12) . ?
Ti1 O10 1.9287(12) . ?
Ti1 O7 2.0215(13) . ?
Ti1 O6 2.0260(10) . ?
Ti1 O4 2.2270(9) . ?
Ti1 Ti3 3.0571(5) . ?
Ti1 Ti5 3.3542(4) . ?
Ti2 O13 1.7409(12) . ?
Ti2 O15 1.8875(9) . ?
Ti2 O12 1.9260(12) . ?
Ti2 O16 1.9715(13) . ?
Ti2 O14 2.0860(10) . ?
Ti2 O19 2.1950(12) . ?
Ti2 Ti3 2.9311(5) . ?
Ti2 Ti4 3.3019(4) . ?
Ti3 O11 1.7638(12) . ?
Ti3 O15 1.8094(14) . ?
Ti3 O17 2.0206(10) . ?
Ti3 O10 2.0436(15) . ?
Ti3 O9 2.0488(9) . ?
Ti3 O12 2.1181(9) . ?
Ti4 O23 1.7666(13) . ?
Ti4 O21 1.7732(18) . ?
Ti4 O20 1.9316(19) . ?
Ti4 O16 2.0496(14) . ?
Ti4 O22 2.1078(12) . ?
Ti4 O19 2.1143(15) . ?
Ti5 O2 1.7680(17) . ?
Ti5 O1 1.7944(18) . ?
Ti5 O3 1.9229(14) . ?
Ti5 O7 2.0318(11) . ?
Ti5 O4 2.1166(11) . ?
Ti5 O5 2.1682(11) . ?
O6 C27 1.2673(16) . ?
O4 C11 1.2860(19) . ?
O9 C11 1.2689(16) . ?
O14 C3AA 1.2503(16) . ?
O3 C9 1.325(2) . ?
O17 C49 1.205(2) . ?
O10 C21 1.451(4) . ?
O22 C3AA 1.2610(18) . ?
C10 C9 1.3849(18) . ?
C10 C6 1.416(2) . ?
C10 C11 1.4592(18) . ?
O19 C49 1.317(3) . ?
O5 C27 1.2449(15) . ?
C8 C4 1.384(2) . ?
C8 C9 1.4141(19) . ?
C8 C7 1.4346(19) . ?
O8 C24 1.420(2) . ?
C6 C5 1.358(2) . ?
C6 H6A 0.9300 . ?
C33 C28 1.3681(17) . ?
C33 C32 1.399(2) . ?
C33 H33A 0.9300 . ?
C28 C29 1.366(2) . ?
C28 C27 1.512(2) . ?
O13 C37 1.452(2) . ?
C5 C4 1.412(2) . ?
C5 H5A 0.9300 . ?
O20 C51 1.282(3) . ?
O16 C40 1.476(4) . ?
C4 C3 1.428(2) . ?
O11 C34 1.433(3) . ?
O7 C18 1.452(3) . ?
C31 C30 1.3575(19) . ?
C31 C32 1.381(2) . ?
C31 C3AA 1.512(2) 10_656 ?
C32 H32A 0.9300 . ?
O23 C46 1.347(3) . ?
C2 C3 1.361(2) . ?
C2 C1 1.419(3) . ?
C2 H2A 0.9300 . ?
O21 C43 1.481(4) . ?
C49 C60 1.472(2) . ?
C3AA C31 1.511(2) 10_656 ?
C29 C30 1.385(2) . ?
C29 H29A 0.9300 . ?
C60 C51 1.409(3) . ?
C60 C59 1.425(4) . ?
C48 C46 1.425(4) . ?
C48 H48A 0.9600 . ?
C48 H48B 0.9600 . ?
C48 H48C 0.9600 . ?
C3 H3A 0.9300 . ?
C1 C7 1.351(2) . ?
C1 H1A 0.9300 . ?
C7 H7A 0.9300 . ?
O2 C12 1.314(4) . ?
C59 C58 1.385(3) . ?
C59 H59A 0.9300 . ?
O1 C15 1.416(4) . ?
C30 H30A 0.9300 . ?
C58 C57 1.416(3) . ?
C58 H58A 0.9300 . ?
C52 C53 1.321(3) . ?
C52 C57 1.448(4) . ?
C52 C51 1.487(3) . ?
C54 C53 1.396(4) . ?
C54 C55 1.354(6) . ?
C54 H54A 0.9300 . ?
C19 C18 1.463(3) . ?
C19 H19A 0.9600 . ?
C19 H19B 0.9600 . ?
C19 H19C 0.9600 . ?
C34 C35 1.545(5) . ?
C34 C36 1.594(4) . ?
C34 H34A 0.9800 . ?
C24 C25 1.411(4) . ?
C24 C26 1.478(5) . ?
C24 H24A 0.9800 . ?
C55 C56 1.380(5) . ?
C55 H55A 0.9300 . ?
C56 C57 1.411(3) . ?
C56 H56A 0.9300 . ?
C36 H36A 0.9600 . ?
C36 H36B 0.9600 . ?
C36 H36C 0.9600 . ?
C18 C20 1.301(4) . ?
C47 C46 1.283(5) . ?
C47 H47A 0.9600 . ?
C47 H47B 0.9600 . ?
C47 H47C 0.9600 . ?
C53 H53A 0.9300 . ?
C25 H25A 0.9600 . ?
C25 H25B 0.9600 . ?
C25 H25C 0.9600 . ?
C40 C42 1.403(4) . ?
C40 C41 1.564(4) . ?
C40 H40A 0.9800 . ?
C37 C38 1.437(4) . ?
C37 C39 1.513(4) . ?
C37 H37A 0.9800 . ?
C14 C12 1.480(6) . ?
C14 H14A 0.9600 . ?
C14 H14B 0.9600 . ?
C14 H14C 0.9600 . ?
C41 H41A 0.9600 . ?
C41 H41B 0.9600 . ?
C41 H41C 0.9600 . ?
C22 C21 1.560(4) . ?
C22 H22A 0.9600 . ?
C22 H22B 0.9600 . ?
C22 H22C 0.9600 . ?
C26 H26A 0.9600 . ?
C26 H26B 0.9600 . ?
C26 H26C 0.9600 . ?
C42 H42A 0.9600 . ?
C42 H42B 0.9600 . ?
C42 H42C 0.9600 . ?
C39 H39A 0.9600 . ?
C39 H39B 0.9600 . ?
C39 H39C 0.9600 . ?
C35 H35A 0.9600 . ?
C35 H35B 0.9600 . ?
C35 H35C 0.9600 . ?
C23 C21 1.547(5) . ?
C23 H23A 0.9600 . ?
C23 H23B 0.9600 . ?
C23 H23C 0.9600 . ?
C21 H21A 0.9800 . ?
C20 H20A 0.9600 . ?
C20 H20B 0.9600 . ?
C20 H20C 0.9600 . ?
C38 H38A 0.9600 . ?
C38 H38B 0.9600 . ?
C38 H38C 0.9600 . ?
C12 C13 1.227(9) . ?
C15 C17 1.418(7) . ?
C15 C16 1.354(7) . ?
C16 H16A 0.9600 . ?
C16 H16B 0.9600 . ?
C16 H16C 0.9600 . ?
C43 C44 1.866(10) . ?
C43 C45 1.744(11) . ?
C43 H43A 0.9800 . ?
C45 H45A 0.9600 . ?
C45 H45B 0.9600 . ?
C45 H45C 0.9600 . ?
C44 H44A 0.9600 . ?
C44 H44B 0.9600 . ?
C44 H44C 0.9600 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C13 H13A 0.9600 . ?
C13 H13B 0.9600 . ?
C13 H13C 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
O8 Ti1 O12 102.94(5) . . ?
O8 Ti1 O10 99.31(6) . . ?
O12 Ti1 O10 83.19(5) . . ?
O8 Ti1 O7 97.46(6) . . ?
O12 Ti1 O7 159.57(4) . . ?
O10 Ti1 O7 94.49(6) . . ?
O8 Ti1 O6 96.64(5) . . ?
O12 Ti1 O6 90.45(5) . . ?
O10 Ti1 O6 163.79(5) . . ?
O7 Ti1 O6 86.27(5) . . ?
O8 Ti1 O4 168.82(6) . . ?
O12 Ti1 O4 88.23(4) . . ?
O10 Ti1 O4 82.22(4) . . ?
O7 Ti1 O4 71.36(5) . . ?
O6 Ti1 O4 82.69(4) . . ?
O8 Ti1 Ti3 111.50(4) . . ?
O12 Ti1 Ti3 42.97(3) . . ?
O10 Ti1 Ti3 41.08(5) . . ?
O7 Ti1 Ti3 128.57(4) . . ?
O6 Ti1 Ti3 128.69(4) . . ?
O4 Ti1 Ti3 76.95(3) . . ?
O8 Ti1 Ti5 130.69(5) . . ?
O12 Ti1 Ti5 125.53(3) . . ?
O10 Ti1 Ti5 95.18(3) . . ?
O7 Ti1 Ti5 34.25(4) . . ?
O6 Ti1 Ti5 76.40(2) . . ?
O4 Ti1 Ti5 38.27(3) . . ?
Ti3 Ti1 Ti5 110.239(11) . . ?
O13 Ti2 O15 102.41(5) . . ?
O13 Ti2 O12 99.62(5) . . ?
O15 Ti2 O12 82.13(5) . . ?
O13 Ti2 O16 100.55(6) . . ?
O15 Ti2 O16 97.19(5) . . ?
O12 Ti2 O16 159.47(5) . . ?
O13 Ti2 O14 93.76(5) . . ?
O15 Ti2 O14 162.45(6) . . ?
O12 Ti2 O14 88.55(5) . . ?
O16 Ti2 O14 86.36(5) . . ?
O13 Ti2 O19 172.73(5) . . ?
O15 Ti2 O19 83.01(4) . . ?
O12 Ti2 O19 85.83(5) . . ?
O16 Ti2 O19 73.76(6) . . ?
O14 Ti2 O19 81.51(4) . . ?
O13 Ti2 Ti3 110.67(4) . . ?
O15 Ti2 Ti3 36.63(4) . . ?
O12 Ti2 Ti3 46.20(3) . . ?
O16 Ti2 Ti3 127.60(4) . . ?
O14 Ti2 Ti3 130.28(4) . . ?
O19 Ti2 Ti3 76.57(3) . . ?
O13 Ti2 Ti4 134.44(5) . . ?
O15 Ti2 Ti4 96.64(3) . . ?
O12 Ti2 Ti4 123.94(3) . . ?
O16 Ti2 Ti4 35.58(5) . . ?
O14 Ti2 Ti4 76.27(3) . . ?
O19 Ti2 Ti4 39.09(4) . . ?
Ti3 Ti2 Ti4 109.272(12) . . ?
O11 Ti3 O15 104.62(8) . . ?
O11 Ti3 O17 92.49(5) . . ?
O15 Ti3 O17 92.32(5) . . ?
O11 Ti3 O10 102.21(8) . . ?
O15 Ti3 O10 153.12(5) . . ?
O17 Ti3 O10 84.87(5) . . ?
O11 Ti3 O9 94.47(5) . . ?
O15 Ti3 O9 92.42(5) . . ?
O17 Ti3 O9 170.33(5) . . ?
O10 Ti3 O9 87.10(5) . . ?
O11 Ti3 O12 176.31(8) . . ?
O15 Ti3 O12 78.84(5) . . ?
O17 Ti3 O12 86.06(4) . . ?
O10 Ti3 O12 74.30(5) . . ?
O9 Ti3 O12 86.59(3) . . ?
O11 Ti3 Ti2 142.19(7) . . ?
O15 Ti3 Ti2 38.49(3) . . ?
O17 Ti3 Ti2 83.47(4) . . ?
O10 Ti3 Ti2 114.75(3) . . ?
O9 Ti3 Ti2 95.06(3) . . ?
O12 Ti3 Ti2 41.02(3) . . ?
O11 Ti3 Ti1 140.02(7) . . ?
O15 Ti3 Ti1 115.15(3) . . ?
O17 Ti3 Ti1 89.96(4) . . ?
O10 Ti3 Ti1 38.33(3) . . ?
O9 Ti3 Ti1 80.39(3) . . ?
O12 Ti3 Ti1 36.70(3) . . ?
Ti2 Ti3 Ti1 77.724(11) . . ?
O23 Ti4 O21 101.04(8) . . ?
O23 Ti4 O20 95.39(7) . . ?
O21 Ti4 O20 98.61(9) . . ?
O23 Ti4 O16 92.93(6) . . ?
O21 Ti4 O16 103.36(9) . . ?
O20 Ti4 O16 154.53(7) . . ?
O23 Ti4 O22 172.14(7) . . ?
O21 Ti4 O22 86.57(7) . . ?
O20 Ti4 O22 85.32(6) . . ?
O16 Ti4 O22 83.31(5) . . ?
O23 Ti4 O19 90.88(6) . . ?
O21 Ti4 O19 167.96(6) . . ?
O20 Ti4 O19 81.81(6) . . ?
O16 Ti4 O19 74.01(6) . . ?
O22 Ti4 O19 81.46(5) . . ?
O23 Ti4 Ti2 98.75(4) . . ?
O21 Ti4 Ti2 133.73(7) . . ?
O20 Ti4 Ti2 120.63(5) . . ?
O16 Ti4 Ti2 34.04(4) . . ?
O22 Ti4 Ti2 74.29(3) . . ?
O19 Ti4 Ti2 40.89(4) . . ?
O2 Ti5 O1 99.40(8) . . ?
O2 Ti5 O3 93.58(6) . . ?
O1 Ti5 O3 97.43(7) . . ?
O2 Ti5 O7 93.00(6) . . ?
O1 Ti5 O7 105.19(7) . . ?
O3 Ti5 O7 155.04(6) . . ?
O2 Ti5 O4 94.15(6) . . ?
O1 Ti5 O4 166.44(7) . . ?
O3 Ti5 O4 82.01(5) . . ?
O7 Ti5 O4 73.52(5) . . ?
O2 Ti5 O5 174.49(5) . . ?
O1 Ti5 O5 84.88(7) . . ?
O3 Ti5 O5 89.28(5) . . ?
O7 Ti5 O5 82.48(5) . . ?
O4 Ti5 O5 81.58(4) . . ?
O2 Ti5 Ti1 101.57(4) . . ?
O1 Ti5 Ti1 134.35(5) . . ?
O3 Ti5 Ti1 120.99(4) . . ?
O7 Ti5 Ti1 34.06(4) . . ?
O4 Ti5 Ti1 40.66(3) . . ?
O5 Ti5 Ti1 72.93(3) . . ?
C27 O6 Ti1 130.55(10) . . ?
C11 O4 Ti5 125.28(7) . . ?
C11 O4 Ti1 128.31(8) . . ?
Ti5 O4 Ti1 101.07(5) . . ?
Ti1 O12 Ti2 166.89(5) . . ?
Ti1 O12 Ti3 100.33(5) . . ?
Ti2 O12 Ti3 92.78(4) . . ?
C11 O9 Ti3 132.85(10) . . ?
C3AA O14 Ti2 130.50(10) . . ?
Ti3 O15 Ti2 104.89(6) . . ?
C9 O3 Ti5 131.89(10) . . ?
C49 O17 Ti3 129.73(14) . . ?
C21 O10 Ti1 131.58(16) . . ?
C21 O10 Ti3 127.80(15) . . ?
Ti1 O10 Ti3 100.60(6) . . ?
C3AA O22 Ti4 132.30(10) . . ?
C9 C10 C6 118.89(12) . . ?
C9 C10 C11 123.10(14) . . ?
C6 C10 C11 117.90(12) . . ?
C49 O19 Ti4 125.57(10) . . ?
C49 O19 Ti2 127.46(9) . . ?
Ti4 O19 Ti2 100.01(7) . . ?
C27 O5 Ti5 129.68(10) . . ?
C4 C8 C9 120.12(12) . . ?
C4 C8 C7 118.69(13) . . ?
C9 C8 C7 121.18(15) . . ?
O3 C9 C10 122.52(13) . . ?
O3 C9 C8 117.69(12) . . ?
C10 C9 C8 119.76(15) . . ?
C24 O8 Ti1 156.57(16) . . ?
C5 C6 C10 121.70(13) . . ?
C5 C6 H6A 119.1 . . ?
C10 C6 H6A 119.1 . . ?
C28 C33 C32 119.71(13) . . ?
C28 C33 H33A 120.1 . . ?
C32 C33 H33A 120.1 . . ?
C29 C28 C33 119.57(13) . . ?
C29 C28 C27 121.42(11) . . ?
C33 C28 C27 118.72(12) . . ?
C37 O13 Ti2 152.75(17) . . ?
C6 C5 C4 119.50(16) . . ?
C6 C5 H5A 120.3 . . ?
C4 C5 H5A 120.3 . . ?
C51 O20 Ti4 129.84(12) . . ?
O9 C11 O4 120.96(11) . . ?
O9 C11 C10 118.28(14) . . ?
O4 C11 C10 120.75(12) . . ?
C40 O16 Ti2 130.79(12) . . ?
C40 O16 Ti4 118.83(11) . . ?
Ti2 O16 Ti4 110.38(8) . . ?
C8 C4 C5 119.95(13) . . ?
C8 C4 C3 118.84(13) . . ?
C5 C4 C3 121.19(16) . . ?
C34 O11 Ti3 153.01(17) . . ?
C18 O7 Ti1 122.70(9) . . ?
C18 O7 Ti5 124.55(10) . . ?
Ti1 O7 Ti5 111.69(7) . . ?
C30 C31 C32 119.43(14) . . ?
C30 C31 C3AA 120.74(13) . 10_656 ?
C32 C31 C3AA 119.80(12) . 10_656 ?
O5 C27 O6 126.59(13) . . ?
O5 C27 C28 117.45(12) . . ?
O6 C27 C28 115.96(10) . . ?
C31 C32 C33 120.13(13) . . ?
C31 C32 H32A 119.9 . . ?
C33 C32 H32A 119.9 . . ?
C46 O23 Ti4 166.77(16) . . ?
C3 C2 C1 119.55(17) . . ?
C3 C2 H2A 120.2 . . ?
C1 C2 H2A 120.2 . . ?
C43 O21 Ti4 139.2(3) . . ?
O17 C49 O19 121.83(15) . . ?
O17 C49 C60 120.8(2) . . ?
O19 C49 C60 117.19(15) . . ?
O14 C3AA O22 125.93(14) . . ?
O14 C3AA C31 117.92(13) . 10_656 ?
O22 C3AA C31 116.14(12) . 10_656 ?
C28 C29 C30 120.79(13) . . ?
C28 C29 H29A 119.6 . . ?
C30 C29 H29A 119.6 . . ?
C51 C60 C59 122.30(18) . . ?
C51 C60 C49 122.0(2) . . ?
C59 C60 C49 115.71(17) . . ?
C46 C48 H48A 109.5 . . ?
C46 C48 H48B 109.5 . . ?
H48A C48 H48B 109.5 . . ?
C46 C48 H48C 109.5 . . ?
H48A C48 H48C 109.5 . . ?
H48B C48 H48C 109.5 . . ?
C2 C3 C4 121.46(19) . . ?
C2 C3 H3A 119.3 . . ?
C4 C3 H3A 119.3 . . ?
C7 C1 C2 119.84(16) . . ?
C7 C1 H1A 120.1 . . ?
C2 C1 H1A 120.1 . . ?
C1 C7 C8 121.54(18) . . ?
C1 C7 H7A 119.2 . . ?
C8 C7 H7A 119.2 . . ?
C12 O2 Ti5 153.2(3) . . ?
C58 C59 C60 120.7(2) . . ?
C58 C59 H59A 119.7 . . ?
C60 C59 H59A 119.7 . . ?
C15 O1 Ti5 143.9(2) . . ?
C31 C30 C29 120.35(14) . . ?
C31 C30 H30A 119.8 . . ?
C29 C30 H30A 119.8 . . ?
C59 C58 C57 119.7(3) . . ?
C59 C58 H58A 120.1 . . ?
C57 C58 H58A 120.1 . . ?
C53 C52 C57 121.0(2) . . ?
C53 C52 C51 121.4(3) . . ?
C57 C52 C51 117.55(18) . . ?
C53 C54 C55 115.9(3) . . ?
C53 C54 H54A 122.1 . . ?
C55 C54 H54A 122.1 . . ?
O20 C51 C60 126.08(19) . . ?
O20 C51 C52 116.09(18) . . ?
C60 C51 C52 117.8(2) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O11 C34 C35 107.5(2) . . ?
O11 C34 C36 105.7(2) . . ?
C35 C34 C36 117.2(2) . . ?
O11 C34 H34A 108.7 . . ?
C35 C34 H34A 108.7 . . ?
C36 C34 H34A 108.7 . . ?
O8 C24 C25 110.0(2) . . ?
O8 C24 C26 110.8(2) . . ?
C25 C24 C26 115.7(2) . . ?
O8 C24 H24A 106.6 . . ?
C25 C24 H24A 106.6 . . ?
C26 C24 H24A 106.6 . . ?
C56 C55 C54 125.4(3) . . ?
C56 C55 H55A 117.3 . . ?
C54 C55 H55A 117.3 . . ?
C55 C56 C57 117.9(4) . . ?
C55 C56 H56A 121.0 . . ?
C57 C56 H56A 121.0 . . ?
C34 C36 H36A 109.5 . . ?
C34 C36 H36B 109.5 . . ?
H36A C36 H36B 109.5 . . ?
C34 C36 H36C 109.5 . . ?
H36A C36 H36C 109.5 . . ?
H36B C36 H36C 109.5 . . ?
C56 C57 C52 116.7(2) . . ?
C56 C57 C58 121.4(3) . . ?
C52 C57 C58 121.9(2) . . ?
C20 C18 O7 116.7(2) . . ?
C20 C18 C19 126.8(3) . . ?
O7 C18 C19 113.1(2) . . ?
C46 C47 H47A 109.5 . . ?
C46 C47 H47B 109.5 . . ?
H47A C47 H47B 109.5 . . ?
C46 C47 H47C 109.5 . . ?
H47A C47 H47C 109.5 . . ?
H47B C47 H47C 109.5 . . ?
C52 C53 C54 123.0(3) . . ?
C52 C53 H53A 118.5 . . ?
C54 C53 H53A 118.5 . . ?
C24 C25 H25A 109.5 . . ?
C24 C25 H25B 109.5 . . ?
H25A C25 H25B 109.5 . . ?
C24 C25 H25C 109.5 . . ?
H25A C25 H25C 109.5 . . ?
H25B C25 H25C 109.5 . . ?
C42 C40 O16 111.7(2) . . ?
C42 C40 C41 125.6(3) . . ?
O16 C40 C41 103.6(2) . . ?
C42 C40 H40A 104.7 . . ?
O16 C40 H40A 104.7 . . ?
C41 C40 H40A 104.7 . . ?
C38 C37 O13 107.44(19) . . ?
C38 C37 C39 118.5(3) . . ?
O13 C37 C39 107.5(2) . . ?
C38 C37 H37A 107.7 . . ?
O13 C37 H37A 107.7 . . ?
C39 C37 H37A 107.7 . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 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 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
C24 C26 H26A 109.5 . . ?
C24 C26 H26B 109.5 . . ?
H26A C26 H26B 109.5 . . ?
C24 C26 H26C 109.5 . . ?
H26A C26 H26C 109.5 . . ?
H26B C26 H26C 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 . . ?
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 . . ?
C34 C35 H35A 109.5 . . ?
C34 C35 H35B 109.5 . . ?
H35A C35 H35B 109.5 . . ?
C34 C35 H35C 109.5 . . ?
H35A C35 H35C 109.5 . . ?
H35B C35 H35C 109.5 . . ?
C21 C23 H23A 109.5 . . ?
C21 C23 H23B 109.5 . . ?
H23A C23 H23B 109.5 . . ?
C21 C23 H23C 109.5 . . ?
H23A C23 H23C 109.5 . . ?
H23B C23 H23C 109.5 . . ?
O10 C21 C22 109.1(2) . . ?
O10 C21 C23 107.3(3) . . ?
C22 C21 C23 118.5(3) . . ?
O10 C21 H21A 107.1 . . ?
C22 C21 H21A 107.1 . . ?
C23 C21 H21A 107.1 . . ?
C47 C46 O23 120.4(3) . . ?
C47 C46 C48 123.9(3) . . ?
O23 C46 C48 115.5(3) . . ?
C18 C20 H20A 109.5 . . ?
C18 C20 H20B 109.4 . . ?
H20A C20 H20B 109.5 . . ?
C18 C20 H20C 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 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 . . ?
C13 C12 O2 129.7(6) . . ?
C13 C12 C14 112.5(6) . . ?
O2 C12 C14 117.4(4) . . ?
C17 C15 C16 123.9(4) . . ?
C17 C15 O1 113.0(4) . . ?
C16 C15 O1 119.6(4) . . ?
C15 C16 H16A 109.5 . . ?
C15 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C15 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O21 C43 C44 101.0(4) . . ?
O21 C43 C45 94.5(5) . . ?
C44 C43 C45 105.8(4) . . ?
O21 C43 H43A 117.4 . . ?
C44 C43 H43A 117.4 . . ?
C45 C43 H43A 117.4 . . ?
C43 C45 H45A 109.5 . . ?
C43 C45 H45B 109.5 . . ?
H45A C45 H45B 109.5 . . ?
C43 C45 H45C 109.5 . . ?
H45A C45 H45C 109.5 . . ?
H45B C45 H45C 109.5 . . ?
C43 C44 H44A 109.5 . . ?
C43 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
C43 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C15 C17 H17A 109.5 . . ?
C15 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C15 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?

_refine_diff_density_max         1.025
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.085

_shelxl_version_number           2014-3


# SQUEEZE RESULTS (APPEND TO CIF)
# 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 0.000 201 12 ' '
2 0.000 0.000 0.260 57 2 ' '
3 0.000 0.000 0.500 190 6 ' '
4 0.000 0.000 0.740 57 2 ' '
5 0.020 0.330 0.535 24 3 ' '
6 0.003 0.357 0.202 24 2 ' '
7 0.010 0.386 0.731 16 0 ' '
8 -0.010 0.614 0.269 16 0 ' '
9 -0.003 0.643 0.798 24 2 ' '
10 -0.020 0.670 0.465 24 3 ' '
11 0.019 0.433 0.530 19 0 ' '
12 0.023 0.687 0.131 24 3 ' '
13 0.043 0.323 0.064 16 0 ' '
14 0.053 0.709 0.602 15 0 ' '
15 0.048 0.888 0.905 26 1 ' '
16 0.080 0.314 0.863 18 0 ' '
17 0.111 0.159 0.905 26 1 ' '
18 0.100 0.747 0.804 19 0 ' '
19 0.159 0.048 0.095 26 1 ' '
20 0.176 0.619 0.572 26 1 ' '
21 0.223 0.509 0.761 27 1 ' '
22 0.333 0.667 0.167 185 6 ' '
23 0.233 0.920 0.863 18 0 ' '
24 0.253 0.353 0.804 19 0 ' '
25 0.334 0.667 0.667 200 12 ' '
26 0.281 0.957 0.064 16 0 ' '
27 0.333 0.667 0.927 56 2 ' '
28 0.285 0.778 0.762 26 1 ' '
29 0.313 0.337 0.131 24 3 ' '
30 0.291 0.343 0.602 15 0 ' '
31 0.333 0.667 0.407 56 2 ' '
32 0.314 0.233 0.137 18 0 ' '
33 0.323 0.281 0.936 16 0 ' '
34 0.310 0.980 0.535 24 3 ' '
35 0.330 0.310 0.465 24 3 ' '
36 0.337 0.023 0.869 24 3 ' '
37 0.343 0.053 0.398 15 0 ' '
38 0.353 0.997 0.202 24 2 ' '
39 0.353 0.100 0.196 19 0 ' '
40 0.357 0.353 0.798 24 2 ' '
41 0.376 0.990 0.731 16 0 ' '
42 0.386 0.376 0.269 16 0 ' '
43 0.381 0.555 0.571 26 1 ' '
44 0.414 0.981 0.530 19 0 ' '
45 0.445 0.826 0.571 26 1 ' '
46 0.433 0.414 0.470 19 0 ' '
47 0.493 0.715 0.762 27 1 ' '
48 0.509 0.286 0.239 27 1 ' '
49 0.557 0.176 0.428 27 1 ' '
50 0.667 0.333 0.833 185 6 ' '
51 0.567 0.586 0.530 19 0 ' '
52 0.586 0.019 0.470 19 0 ' '
53 0.667 0.334 0.333 200 12 ' '
54 0.614 0.624 0.731 16 0 ' '
55 0.667 0.333 0.593 56 2 ' '
56 0.619 0.445 0.429 26 1 ' '
57 0.624 0.010 0.269 16 0 ' '
58 0.667 0.333 0.073 55 2 ' '
59 0.646 1.003 0.798 24 3 ' '
60 0.643 0.647 0.202 24 3 ' '
61 0.647 0.900 0.804 19 0 ' '
62 0.657 0.947 0.602 15 0 ' '
63 0.663 0.976 0.131 24 3 ' '
64 0.670 0.690 0.535 24 3 ' '
65 0.676 0.719 0.064 16 0 ' '
66 0.687 0.663 0.869 24 3 ' '
67 0.686 0.766 0.863 18 0 ' '
68 0.690 0.020 0.465 24 3 ' '
69 0.709 0.657 0.398 15 0 ' '
70 0.719 0.043 0.936 16 0 ' '
71 0.715 0.222 0.238 26 1 ' '
72 0.747 0.647 0.196 19 0 ' '
73 0.778 0.493 0.238 27 1 ' '
74 0.766 0.080 0.137 18 0 ' '
75 0.826 0.381 0.429 26 1 ' '
76 0.841 0.952 0.905 25 1 ' '
77 0.888 0.840 0.095 25 1 ' '
78 0.900 0.253 0.196 19 0 ' '
79 0.920 0.686 0.137 18 0 ' '
80 0.947 0.291 0.398 15 0 ' '
81 0.952 0.111 0.095 26 1 ' '
82 0.957 0.676 0.936 16 0 ' '
83 0.976 0.313 0.869 24 3 ' '
84 0.980 0.567 0.470 19 0 ' '
_platon_squeeze_details          
;
;
