#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:50:16 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551219.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1551219
loop_
_publ_author_name
'Ding, Qing-Rong'
'Xu, Gui-Lan'
'Zhang, Lei'
'Zhang, Jian'
_publ_section_title
;
 Ligand-directed assembly engineering of trapezoidal {Ti₅}
 building blocks stabilized by dimethylglyoxime.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9916
_journal_page_last               9919
_journal_paper_doi               10.1039/c9dt02032b
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C111 H220 N4 O57 Ti16'
_chemical_formula_sum            'C111 H220 N4 O57 Ti16'
_chemical_formula_weight         3288.79
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2019-05-29 deposited with the CCDC.    2019-06-04 downloaded from the CCDC.
;
_cell_angle_alpha                109.617(3)
_cell_angle_beta                 96.107(3)
_cell_angle_gamma                95.889(3)
_cell_formula_units_Z            1
_cell_length_a                   15.4097(7)
_cell_length_b                   15.8879(6)
_cell_length_c                   17.9294(7)
_cell_measurement_reflns_used    6703
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.6570
_cell_measurement_theta_min      3.6990
_cell_volume                     4066.3(3)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 16.2083
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0369
_diffrn_reflns_av_unetI/netI     0.0719
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29913
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         3.553
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.812
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.78515
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.313
_exptl_crystal_description       polyhedron
_exptl_crystal_F_000             1674
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.004
_refine_diff_density_min         -2.184
_refine_diff_density_rms         0.155
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     855
_refine_ls_number_reflns         14264
_refine_ls_number_restraints     560
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1695
_refine_ls_R_factor_gt           0.1228
_refine_ls_shift/su_max          0.043
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.3000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3639
_refine_ls_wR_factor_ref         0.4190
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8534
_reflns_number_total             14264
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c9dt02032b2.cif
_cod_data_source_block           b
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code               1551219
_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.
;
_shelxl_version_number           2014-3
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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
Ti3 Ti 0.17901(8) 0.48431(9) 0.30848(8) 0.0408(4) Uani 1 1 d . .
Ti4 Ti 0.25631(9) 0.34771(9) 0.17164(8) 0.0419(4) Uani 1 1 d . U
Ti8 Ti 0.49449(9) 0.43341(10) 0.72574(8) 0.0441(4) Uani 1 1 d . .
Ti2 Ti 0.29719(9) 0.59982(9) 0.23643(8) 0.0446(4) Uani 1 1 d . .
Ti7 Ti 0.46371(9) 0.32834(10) 0.21591(8) 0.0458(4) Uani 1 1 d . U
Ti5 Ti 0.14633(11) 0.24022(10) 0.25333(10) 0.0568(5) Uani 1 1 d . .
Ti1 Ti 0.22794(10) 0.73031(10) 0.38505(10) 0.0552(5) Uani 1 1 d . .
Ti6 Ti 0.31550(12) 0.16084(10) 0.12895(10) 0.0611(5) Uani 1 1 d . U
O23 O 0.2943(3) 0.4669(3) 0.3770(3) 0.0404(11) Uani 1 1 d . .
O21 O 0.3507(3) 0.3678(3) 0.2821(3) 0.0412(12) Uani 1 1 d . .
O25 O 0.5923(3) 0.3861(3) 0.6629(3) 0.0423(12) Uani 1 1 d . .
O8 O 0.2685(3) 0.4762(3) 0.2173(3) 0.0453(13) Uani 1 1 d . .
O22 O 0.5155(3) 0.3477(4) 0.3208(3) 0.0509(13) Uani 1 1 d . .
O10 O 0.1708(3) 0.3580(3) 0.2431(3) 0.0460(13) Uani 1 1 d . .
O5 O 0.2211(3) 0.6045(3) 0.3127(3) 0.0463(13) Uani 1 1 d . .
O24 O 0.6535(4) 0.3044(3) 0.5603(3) 0.0516(13) Uani 1 1 d . .
O26 O 0.4373(4) 0.4262(4) 0.6262(3) 0.0551(14) Uani 1 1 d . .
O19 O 0.3597(3) 0.2965(3) 0.1374(3) 0.0463(13) Uani 1 1 d . .
O11 O 0.2219(4) 0.2170(4) 0.1706(3) 0.0545(14) Uani 1 1 d . .
O7 O 0.4158(4) 0.5950(4) 0.1983(3) 0.0552(15) Uani 1 1 d . .
O28 O 0.5112(4) 0.5497(4) 0.7767(3) 0.0536(14) Uani 1 1 d . .
O9 O 0.0695(3) 0.4880(4) 0.2686(3) 0.0565(15) Uani 1 1 d . .
O4 O 0.3055(4) 0.7356(3) 0.3023(3) 0.0552(15) Uani 1 1 d . .
O1 O 0.1750(4) 0.6668(4) 0.4507(4) 0.0646(16) Uani 1 1 d . .
O6 O 0.2356(4) 0.6110(5) 0.1524(4) 0.0718(18) Uani 1 1 d . U
O15 O 0.1948(4) 0.3304(4) 0.0763(3) 0.0629(15) Uani 1 1 d . U
O20 O 0.5546(4) 0.2956(4) 0.1648(4) 0.0665(16) Uani 1 1 d . U
O27 O 0.4010(4) 0.3773(5) 0.7508(3) 0.0699(19) Uani 1 1 d . .
O18 O 0.4225(4) 0.1936(4) 0.2009(4) 0.0673(17) Uani 1 1 d . .
N1 N 0.1617(4) 0.5779(4) 0.4289(4) 0.0478(16) Uani 1 1 d . .
O2 O 0.2595(4) 0.8359(4) 0.4670(4) 0.0733(18) Uani 1 1 d . .
N2 N 0.1275(5) 0.4075(5) 0.3823(4) 0.0529(17) Uani 1 1 d . .
C49 C 0.5304(6) 0.3691(6) 0.5291(6) 0.0624(7) Uani 1 1 d . U
O17 O 0.3152(5) 0.1269(4) 0.0230(4) 0.079(2) Uani 1 1 d . .
O3 O 0.1306(4) 0.7574(4) 0.3415(4) 0.0745(19) Uani 1 1 d . .
C45 C 0.4153(6) 0.4018(6) 0.4167(6) 0.0624(7) Uani 1 1 d . U
O16 O 0.2836(5) 0.0511(4) 0.1324(4) 0.088(2) Uani 1 1 d . U
C47 C 0.4931(6) 0.3636(6) 0.3931(6) 0.0628(7) Uani 1 1 d . U
O12 O 0.1140(5) 0.3169(4) 0.3553(4) 0.078(2) Uani 1 1 d . .
C50 C 0.4546(6) 0.4056(6) 0.5504(6) 0.0624(7) Uani 1 1 d . U
C51 C 0.5968(6) 0.3501(6) 0.5859(6) 0.0625(7) Uani 1 1 d . U
C48 C 0.5469(6) 0.3461(6) 0.4488(5) 0.0625(7) Uani 1 1 d . U
H48 H 0.5959 0.3184 0.4342 0.075 Uiso 1 1 calc R U
C46 C 0.3992(6) 0.4221(6) 0.4938(5) 0.0627(7) Uani 1 1 d . U
H46 H 0.3491 0.4479 0.5081 0.075 Uiso 1 1 calc R U
C44 C 0.3498(6) 0.4139(6) 0.3546(6) 0.0624(7) Uani 1 1 d . U
C20 C 0.1228(8) 0.4479(7) 0.4556(6) 0.0759(14) Uani 1 1 d . U
C19 C 0.1410(7) 0.5457(7) 0.4830(6) 0.0759(14) Uani 1 1 d . U
O14 O 0.0410(6) 0.1856(6) 0.2025(5) 0.124(4) Uani 1 1 d . .
O13 O 0.1905(7) 0.1745(6) 0.3036(5) 0.117(3) Uani 1 1 d . U
C13 C 0.4359(9) 0.5736(9) 0.1155(6) 0.101(2) Uani 1 1 d . U
H13 H 0.4972 0.5619 0.1179 0.121 Uiso 1 1 calc R U
C14 C 0.3827(9) 0.4882(9) 0.0606(6) 0.102(2) Uani 1 1 d . U
H14A H 0.3933 0.4401 0.0800 0.153 Uiso 1 1 calc R U
H14B H 0.3990 0.4746 0.0081 0.153 Uiso 1 1 calc R U
H14C H 0.3212 0.4943 0.0582 0.153 Uiso 1 1 calc R U
C21 C 0.1347(7) 0.6061(7) 0.5673(6) 0.0765(14) Uani 1 1 d . U
H21A H 0.1888 0.6116 0.6018 0.115 Uiso 1 1 calc R U
H21B H 0.0866 0.5801 0.5864 0.115 Uiso 1 1 calc R U
H21C H 0.1247 0.6647 0.5673 0.115 Uiso 1 1 calc R U
C22 C 0.1000(7) 0.3990(7) 0.5125(6) 0.0762(14) Uani 1 1 d . U
H22A H 0.0407 0.3675 0.4955 0.114 Uiso 1 1 calc R U
H22B H 0.1047 0.4422 0.5657 0.114 Uiso 1 1 calc R U
H22C H 0.1401 0.3566 0.5122 0.114 Uiso 1 1 calc R U
C23 C -0.0198(9) 0.4453(12) 0.2474(10) 0.129(3) Uani 1 1 d . U
H23 H -0.0313 0.4098 0.2815 0.155 Uiso 1 1 calc R U
C7 C 0.3500(10) 0.8088(8) 0.2842(10) 0.116(3) Uani 1 1 d . U
H7 H 0.3553 0.7874 0.2271 0.139 Uiso 1 1 calc R U
C35 C 0.3515(11) 0.1522(11) -0.0351(9) 0.129(3) Uani 1 1 d . U
H35 H 0.3427 0.2151 -0.0249 0.155 Uiso 1 1 calc R U
C15 C 0.4361(9) 0.6548(9) 0.0947(7) 0.102(2) Uani 1 1 d . U
H15A H 0.3884 0.6856 0.1148 0.153 Uiso 1 1 calc R U
H15B H 0.4290 0.6383 0.0375 0.153 Uiso 1 1 calc R U
H15C H 0.4911 0.6939 0.1180 0.153 Uiso 1 1 calc R U
C52 C 0.3134(15) 0.3343(17) 0.7291(14) 0.214(5) Uani 1 1 d D U
H52 H 0.2903 0.3768 0.7060 0.257 Uiso 1 1 calc R U
C41 C 0.4841(6) 0.1397(6) 0.2308(6) 0.0645(7) Uani 1 1 d . U
H41 H 0.5382 0.1816 0.2584 0.077 Uiso 1 1 calc R U
C9 C 0.4388(9) 0.8354(8) 0.3303(9) 0.116(3) Uani 1 1 d . U
H9A H 0.4350 0.8635 0.3861 0.175 Uiso 1 1 calc R U
H9B H 0.4723 0.8773 0.3124 0.175 Uiso 1 1 calc R U
H9C H 0.4675 0.7829 0.3227 0.175 Uiso 1 1 calc R U
C1 C 0.313(2) 0.8833(14) 0.5426(12) 0.216(5) Uani 1 1 d . U
H1 H 0.3693 0.8604 0.5392 0.259 Uiso 1 1 calc R U
C36 C 0.3013(11) 0.0980(10) -0.1176(8) 0.129(3) Uani 1 1 d . U
H36A H 0.2947 0.0349 -0.1248 0.194 Uiso 1 1 calc R U
H36B H 0.3332 0.1085 -0.1575 0.194 Uiso 1 1 calc R U
H36C H 0.2441 0.1162 -0.1227 0.194 Uiso 1 1 calc R U
C16 C 0.1462(10) 0.2825(11) 0.0040(8) 0.120(2) Uani 1 1 d . U
C4 C 0.0697(12) 0.8232(14) 0.3671(13) 0.162(4) Uani 1 1 d . U
H4 H 0.1043 0.8832 0.3947 0.195 Uiso 1 1 calc R U
C8 C 0.2955(10) 0.8844(8) 0.3007(9) 0.116(3) Uani 1 1 d . U
H8A H 0.2341 0.8597 0.2848 0.174 Uiso 1 1 calc R U
H8B H 0.3115 0.9223 0.2710 0.174 Uiso 1 1 calc R U
H8C H 0.3061 0.9194 0.3569 0.174 Uiso 1 1 calc R U
C17 C 0.0794(10) 0.2178(10) -0.0041(7) 0.120(2) Uani 1 1 d . U
H17A H 0.1009 0.1729 0.0148 0.180 Uiso 1 1 calc R U
H17B H 0.0541 0.1903 -0.0595 0.180 Uiso 1 1 calc R U
H17C H 0.0352 0.2438 0.0266 0.180 Uiso 1 1 calc R U
C37 C 0.4460(10) 0.1516(10) -0.0292(9) 0.129(3) Uani 1 1 d . U
H37A H 0.4747 0.1946 0.0214 0.194 Uiso 1 1 calc R U
H37B H 0.4675 0.1673 -0.0718 0.194 Uiso 1 1 calc R U
H37C H 0.4584 0.0923 -0.0332 0.194 Uiso 1 1 calc R U
C24 C -0.0743(9) 0.5237(11) 0.2673(9) 0.129(3) Uani 1 1 d . U
H24A H -0.0625 0.5572 0.3238 0.194 Uiso 1 1 calc R U
H24B H -0.1359 0.5000 0.2520 0.194 Uiso 1 1 calc R U
H24C H -0.0584 0.5628 0.2386 0.194 Uiso 1 1 calc R U
C43 C 0.4445(6) 0.1135(6) 0.2920(6) 0.0661(8) Uani 1 1 d . U
H43A H 0.4325 0.1664 0.3327 0.099 Uiso 1 1 calc R U
H43B H 0.4846 0.0839 0.3156 0.099 Uiso 1 1 calc R U
H43C H 0.3904 0.0730 0.2678 0.099 Uiso 1 1 calc R U
C5 C 0.0173(11) 0.8010(13) 0.4217(12) 0.163(4) Uani 1 1 d . U
H5A H -0.0231 0.7465 0.3934 0.244 Uiso 1 1 calc R U
H5B H -0.0152 0.8494 0.4446 0.244 Uiso 1 1 calc R U
H5C H 0.0554 0.7922 0.4637 0.244 Uiso 1 1 calc R U
C6 C 0.0156(11) 0.8232(13) 0.2898(12) 0.162(4) Uani 1 1 d . U
H6A H 0.0440 0.8689 0.2729 0.244 Uiso 1 1 calc R U
H6B H -0.0426 0.8354 0.2996 0.244 Uiso 1 1 calc R U
H6C H 0.0118 0.7651 0.2485 0.244 Uiso 1 1 calc R U
C25 C -0.0374(9) 0.3858(11) 0.1644(9) 0.130(3) Uani 1 1 d . U
H25A H -0.0142 0.4167 0.1314 0.194 Uiso 1 1 calc R U
H25B H -0.0999 0.3683 0.1482 0.194 Uiso 1 1 calc R U
H25C H -0.0097 0.3330 0.1586 0.194 Uiso 1 1 calc R U
C10 C 0.1653(9) 0.6303(13) 0.1166(10) 0.139(3) Uani 1 1 d D U
H10 H 0.1699 0.6918 0.1553 0.166 Uiso 1 1 calc R U
C18 C 0.1592(10) 0.3252(10) -0.0521(7) 0.120(2) Uani 1 1 d . U
H18A H 0.1830 0.3877 -0.0244 0.180 Uiso 1 1 calc R U
H18B H 0.1039 0.3208 -0.0843 0.180 Uiso 1 1 calc R U
H18C H 0.1998 0.2962 -0.0859 0.180 Uiso 1 1 calc R U
C32 C 0.2471(12) -0.0393(11) 0.0987(11) 0.145(3) Uani 1 1 d . U
H32 H 0.2775 -0.0649 0.1350 0.174 Uiso 1 1 calc R U
C30 C 0.2708(7) 0.1905(7) 0.4246(6) 0.0722(9) Uani 1 1 d . U
H30A H 0.3195 0.2170 0.4066 0.108 Uiso 1 1 calc R U
H30B H 0.2920 0.1549 0.4546 0.108 Uiso 1 1 calc R U
H30C H 0.2429 0.2375 0.4580 0.108 Uiso 1 1 calc R U
C34 C 0.1586(11) -0.0524(11) 0.1125(10) 0.146(3) Uani 1 1 d . U
H34A H 0.1557 -0.0235 0.1683 0.218 Uiso 1 1 calc R U
H34B H 0.1381 -0.1159 0.0966 0.218 Uiso 1 1 calc R U
H34C H 0.1221 -0.0266 0.0817 0.218 Uiso 1 1 calc R U
C42 C 0.5083(7) 0.0720(6) 0.1590(6) 0.0676(9) Uani 1 1 d . U
H42A H 0.4589 0.0255 0.1333 0.101 Uiso 1 1 calc R U
H42B H 0.5572 0.0458 0.1750 0.101 Uiso 1 1 calc R U
H42C H 0.5246 0.1010 0.1224 0.101 Uiso 1 1 calc R U
C31 C 0.1351(6) 0.0875(7) 0.3760(6) 0.0753(10) Uani 1 1 d D U
H31A H 0.1034 0.1292 0.4108 0.113 Uiso 1 1 calc R U
H31B H 0.1542 0.0464 0.4011 0.113 Uiso 1 1 calc R U
H31C H 0.0974 0.0541 0.3263 0.113 Uiso 1 1 calc R U
C38 C 0.6416(11) 0.3244(11) 0.1722(9) 0.131(3) Uani 1 1 d D U
C26 C -0.0390(17) 0.133(2) 0.1909(14) 0.273(7) Uani 1 1 d D U
C39 C 0.6601(10) 0.3733(11) 0.1174(9) 0.132(3) Uani 1 1 d D U
H39A H 0.7011 0.3448 0.0839 0.198 Uiso 1 1 calc R U
H39B H 0.6850 0.4348 0.1480 0.198 Uiso 1 1 calc R U
H39C H 0.6063 0.3721 0.0845 0.198 Uiso 1 1 calc R U
C3 C 0.3317(18) 0.9759(12) 0.5566(12) 0.216(5) Uani 1 1 d . U
H3A H 0.3630 0.9848 0.5157 0.325 Uiso 1 1 calc R U
H3B H 0.3676 1.0054 0.6080 0.325 Uiso 1 1 calc R U
H3C H 0.2777 1.0010 0.5558 0.325 Uiso 1 1 calc R U
C2 C 0.2772(19) 0.8599(13) 0.6021(12) 0.216(5) Uani 1 1 d . U
H2A H 0.2523 0.9106 0.6336 0.325 Uiso 1 1 d R U
H2B H 0.3227 0.8466 0.6355 0.325 Uiso 1 1 d R U
H2C H 0.2320 0.8083 0.5792 0.325 Uiso 1 1 d R U
C29 C 0.2118(6) 0.1371(7) 0.3605(6) 0.0750(10) Uani 1 1 d D U
H29 H 0.2448 0.0892 0.3332 0.090 Uiso 1 1 calc R U
C11 C 0.0779(9) 0.5995(12) 0.1323(9) 0.139(3) Uani 1 1 d D U
H11A H 0.0735 0.5672 0.1668 0.167 Uiso 1 1 calc R U
H11B H 0.0273 0.6123 0.1077 0.167 Uiso 1 1 calc R U
C12 C 0.1686(10) 0.6564(12) 0.0528(9) 0.139(3) Uani 1 1 d . U
H12A H 0.2171 0.7041 0.0644 0.208 Uiso 1 1 calc R U
H12B H 0.1145 0.6777 0.0410 0.208 Uiso 1 1 calc R U
H12C H 0.1765 0.6061 0.0074 0.208 Uiso 1 1 calc R U
C27 C -0.0881(15) 0.1634(19) 0.2596(13) 0.274(7) Uani 1 1 d D U
H27A H -0.0472 0.2045 0.3043 0.410 Uiso 1 1 d R U
H27B H -0.1105 0.1121 0.2724 0.410 Uiso 1 1 d R U
H27C H -0.1361 0.1934 0.2482 0.410 Uiso 1 1 d R U
C40 C 0.7028(10) 0.3321(11) 0.2368(9) 0.132(3) Uani 1 1 d . U
H40A H 0.6999 0.3867 0.2802 0.198 Uiso 1 1 calc R U
H40B H 0.7608 0.3339 0.2220 0.198 Uiso 1 1 calc R U
H40C H 0.6903 0.2811 0.2533 0.198 Uiso 1 1 calc R U
C33 C 0.2704(11) -0.0876(10) 0.0273(10) 0.146(3) Uani 1 1 d . U
H33A H 0.2800 -0.0489 -0.0032 0.219 Uiso 1 1 calc R U
H33B H 0.2240 -0.1364 -0.0019 0.219 Uiso 1 1 calc R U
H33C H 0.3237 -0.1114 0.0366 0.219 Uiso 1 1 calc R U
C53 C 0.3134(15) 0.2576(16) 0.6499(12) 0.215(5) Uani 1 1 d D U
H53A H 0.3727 0.2558 0.6381 0.322 Uiso 1 1 calc R U
H53B H 0.2771 0.2678 0.6078 0.322 Uiso 1 1 calc R U
H53C H 0.2906 0.2012 0.6543 0.322 Uiso 1 1 calc R U
C28 C -0.0549(16) 0.0628(18) 0.1097(13) 0.274(7) Uani 1 1 d D U
H28A H -0.0922 0.0132 0.1144 0.410 Uiso 1 1 d R U
H28B H -0.0842 0.0832 0.0704 0.410 Uiso 1 1 d R U
H28C H -0.0007 0.0434 0.0935 0.410 Uiso 1 1 d R U
C54 C 0.2648(15) 0.3568(16) 0.8003(12) 0.215(5) Uani 1 1 d D U
H54A H 0.2887 0.3305 0.8375 0.322 Uiso 1 1 calc R U
H54B H 0.2033 0.3331 0.7827 0.322 Uiso 1 1 calc R U
H54C H 0.2714 0.4212 0.8259 0.322 Uiso 1 1 calc R U
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O9 Ti3 O5 93.2(2) . .
O9 Ti3 O10 91.5(2) . .
O5 Ti3 O10 142.5(2) . .
O9 Ti3 O23 165.2(2) . .
O5 Ti3 O23 96.9(2) . .
O10 Ti3 O23 87.1(2) . .
O9 Ti3 N1 90.9(3) . .
O5 Ti3 N1 73.6(2) . .
O10 Ti3 N1 143.5(2) . .
O23 Ti3 N1 81.6(2) . .
O9 Ti3 O8 110.5(2) . .
O5 Ti3 O8 70.8(2) . .
O10 Ti3 O8 72.8(2) . .
O23 Ti3 O8 83.16(18) . .
N1 Ti3 O8 139.0(2) . .
O9 Ti3 N2 90.3(3) . .
O5 Ti3 N2 142.5(3) . .
O10 Ti3 N2 74.6(2) . .
O23 Ti3 N2 75.1(2) . .
N1 Ti3 N2 69.0(3) . .
O8 Ti3 N2 141.4(2) . .
O9 Ti3 Ti4 106.7(2) . .
O5 Ti3 Ti4 108.04(18) . .
O10 Ti3 Ti4 35.74(15) . .
O23 Ti3 Ti4 80.47(14) . .
N1 Ti3 Ti4 162.06(17) . .
O8 Ti3 Ti4 37.31(13) . .
N2 Ti3 Ti4 106.61(19) . .
O9 Ti3 Ti2 104.25(19) . .
O5 Ti3 Ti2 34.44(17) . .
O10 Ti3 Ti2 108.71(16) . .
O23 Ti3 Ti2 90.11(13) . .
N1 Ti3 Ti2 105.92(17) . .
O8 Ti3 Ti2 36.34(13) . .
N2 Ti3 Ti2 164.79(18) . .
Ti4 Ti3 Ti2 73.63(5) . .
O15 Ti4 O8 99.7(3) . .
O15 Ti4 O10 105.4(3) . .
O8 Ti4 O10 81.0(2) . .
O15 Ti4 O19 99.5(3) . .
O8 Ti4 O19 116.9(2) . .
O10 Ti4 O19 146.4(2) . .
O15 Ti4 O11 96.2(2) . .
O8 Ti4 O11 154.0(2) . .
O10 Ti4 O11 75.1(2) . .
O19 Ti4 O11 80.2(2) . .
O15 Ti4 O21 171.6(2) . .
O8 Ti4 O21 81.59(19) . .
O10 Ti4 O21 83.0(2) . .
O19 Ti4 O21 72.76(19) . .
O11 Ti4 O21 85.7(2) . .
O15 Ti4 Ti6 97.2(2) . .
O8 Ti4 Ti6 156.67(16) . .
O10 Ti4 Ti6 109.86(17) . .
O19 Ti4 Ti6 43.78(15) . .
O11 Ti4 Ti6 36.54(16) . .
O21 Ti4 Ti6 79.44(13) . .
O15 Ti4 Ti5 107.39(19) . .
O8 Ti4 Ti5 116.53(18) . .
O10 Ti4 Ti5 37.11(16) . .
O19 Ti4 Ti5 113.57(16) . .
O11 Ti4 Ti5 38.27(16) . .
O21 Ti4 Ti5 79.09(13) . .
Ti6 Ti4 Ti5 72.89(5) . .
O15 Ti4 Ti3 110.9(2) . .
O8 Ti4 Ti3 45.08(17) . .
O10 Ti4 Ti3 36.21(15) . .
O19 Ti4 Ti3 146.27(15) . .
O11 Ti4 Ti3 109.76(16) . .
O21 Ti4 Ti3 75.91(13) . .
Ti6 Ti4 Ti3 139.79(6) . .
Ti5 Ti4 Ti3 71.60(5) . .
O15 Ti4 Ti7 129.0(2) . .
O8 Ti4 Ti7 97.31(15) . .
O10 Ti4 Ti7 124.68(16) . .
O19 Ti4 Ti7 31.37(14) . .
O11 Ti4 Ti7 88.38(17) . .
O21 Ti4 Ti7 42.79(13) . .
Ti6 Ti4 Ti7 59.43(5) . .
Ti5 Ti4 Ti7 107.04(6) . .
Ti3 Ti4 Ti7 115.07(5) . .
O28 Ti8 O27 112.4(3) . .
O28 Ti8 O26 101.0(3) . .
O27 Ti8 O26 94.7(2) . .
O28 Ti8 O25 114.7(2) . .
O27 Ti8 O25 132.2(3) . .
O26 Ti8 O25 83.9(2) . .
O28 Ti8 O7 95.9(2) . 2_666
O27 Ti8 O7 94.7(3) . 2_666
O26 Ti8 O7 155.8(3) . 2_666
O25 Ti8 O7 73.3(2) . 2_666
O28 Ti8 Ti2 97.03(19) . 2_666
O27 Ti8 Ti2 124.6(2) . 2_666
O26 Ti8 Ti2 125.33(18) . 2_666
O25 Ti8 Ti2 42.00(13) . 2_666
O7 Ti8 Ti2 34.22(16) 2_666 2_666
O6 Ti2 O8 101.8(3) . .
O6 Ti2 O5 107.5(3) . .
O8 Ti2 O5 80.2(2) . .
O6 Ti2 O7 98.6(3) . .
O8 Ti2 O7 97.4(2) . .
O5 Ti2 O7 153.7(2) . .
O6 Ti2 O4 92.4(3) . .
O8 Ti2 O4 154.4(3) . .
O5 Ti2 O4 75.2(2) . .
O7 Ti2 O4 101.6(2) . .
O6 Ti2 O25 162.8(2) . 2_666
O8 Ti2 O25 91.27(19) . 2_666
O5 Ti2 O25 85.6(2) . 2_666
O7 Ti2 O25 68.3(2) . 2_666
O4 Ti2 O25 80.0(2) . 2_666
O6 Ti2 Ti3 109.7(2) . .
O8 Ti2 Ti3 44.80(17) . .
O5 Ti2 Ti3 35.35(15) . .
O7 Ti2 Ti3 135.70(17) . .
O4 Ti2 Ti3 110.29(17) . .
O25 Ti2 Ti3 87.48(13) 2_666 .
O6 Ti2 Ti1 104.9(3) . .
O8 Ti2 Ti1 115.68(18) . .
O5 Ti2 Ti1 36.18(15) . .
O7 Ti2 Ti1 133.62(17) . .
O4 Ti2 Ti1 39.14(16) . .
O25 Ti2 Ti1 78.89(14) 2_666 .
Ti3 Ti2 Ti1 71.16(5) . .
O6 Ti2 Ti8 132.7(2) . 2_666
O8 Ti2 Ti8 85.03(16) . 2_666
O5 Ti2 Ti8 119.76(16) . 2_666
O7 Ti2 Ti8 34.37(14) . 2_666
O4 Ti2 Ti8 101.05(16) . 2_666
O25 Ti2 Ti8 36.58(14) 2_666 2_666
Ti3 Ti2 Ti8 107.61(5) . 2_666
Ti1 Ti2 Ti8 114.07(5) . 2_666
O20 Ti7 O22 99.4(3) . .
O20 Ti7 O28 93.6(3) . 2_666
O22 Ti7 O28 95.5(2) . 2_666
O20 Ti7 O19 107.9(3) . .
O22 Ti7 O19 149.1(2) . .
O28 Ti7 O19 96.8(2) 2_666 .
O20 Ti7 O18 89.7(3) . .
O22 Ti7 O18 89.2(2) . .
O28 Ti7 O18 173.7(2) 2_666 .
O19 Ti7 O18 77.0(2) . .
O20 Ti7 O21 178.7(3) . .
O22 Ti7 O21 79.5(2) . .
O28 Ti7 O21 87.3(2) 2_666 .
O19 Ti7 O21 72.96(19) . .
O18 Ti7 O21 89.5(2) . .
O20 Ti7 Ti6 102.4(2) . .
O22 Ti7 Ti6 118.87(18) . .
O28 Ti7 Ti6 138.31(17) 2_666 .
O19 Ti7 Ti6 41.70(16) . .
O18 Ti7 Ti6 35.43(18) . .
O21 Ti7 Ti6 77.56(13) . .
O20 Ti7 Ti4 138.2(2) . .
O22 Ti7 Ti4 122.23(17) . .
O28 Ti7 Ti4 85.75(18) 2_666 .
O19 Ti7 Ti4 31.54(16) . .
O18 Ti7 Ti4 88.20(18) . .
O21 Ti7 Ti4 42.83(12) . .
Ti6 Ti7 Ti4 56.91(5) . .
O13 Ti5 O14 108.5(5) . .
O13 Ti5 O11 97.2(4) . .
O14 Ti5 O11 104.7(3) . .
O13 Ti5 O10 140.6(4) . .
O14 Ti5 O10 110.6(4) . .
O11 Ti5 O10 77.7(2) . .
O13 Ti5 O12 88.6(4) . .
O14 Ti5 O12 99.7(4) . .
O11 Ti5 O12 151.6(3) . .
O10 Ti5 O12 80.2(2) . .
O13 Ti5 Ti4 123.7(3) . .
O14 Ti5 Ti4 116.9(3) . .
O11 Ti5 Ti4 41.56(16) . .
O10 Ti5 Ti4 36.50(16) . .
O12 Ti5 Ti4 113.39(17) . .
O3 Ti1 O2 97.5(3) . .
O3 Ti1 O5 99.0(3) . .
O2 Ti1 O5 163.4(3) . .
O3 Ti1 O1 99.2(3) . .
O2 Ti1 O1 94.3(3) . .
O5 Ti1 O1 80.4(2) . .
O3 Ti1 O4 98.7(3) . .
O2 Ti1 O4 105.7(3) . .
O5 Ti1 O4 74.5(2) . .
O1 Ti1 O4 151.0(2) . .
O3 Ti1 O24 179.0(3) . 2_666
O2 Ti1 O24 82.7(3) . 2_666
O5 Ti1 O24 80.8(2) . 2_666
O1 Ti1 O24 79.8(2) . 2_666
O4 Ti1 O24 82.2(2) . 2_666
O3 Ti1 Ti2 103.2(2) . .
O2 Ti1 Ti2 142.0(2) . .
O5 Ti1 Ti2 34.37(16) . .
O1 Ti1 Ti2 112.99(19) . .
O4 Ti1 Ti2 40.18(15) . .
O24 Ti1 Ti2 77.19(15) 2_666 .
O16 Ti6 O17 97.2(3) . .
O16 Ti6 O11 99.5(3) . .
O17 Ti6 O11 117.8(3) . .
O16 Ti6 O18 98.8(3) . .
O17 Ti6 O18 121.0(3) . .
O11 Ti6 O18 114.7(3) . .
O16 Ti6 O19 174.1(3) . .
O17 Ti6 O19 88.2(3) . .
O11 Ti6 O19 80.0(2) . .
O18 Ti6 O19 76.3(2) . .
O16 Ti6 Ti4 141.1(3) . .
O17 Ti6 Ti4 103.2(3) . .
O11 Ti6 Ti4 41.65(17) . .
O18 Ti6 Ti4 98.5(2) . .
O19 Ti6 Ti4 38.52(14) . .
O16 Ti6 Ti7 138.2(3) . .
O17 Ti6 Ti7 109.0(2) . .
O11 Ti6 Ti7 96.32(17) . .
O18 Ti6 Ti7 39.79(19) . .
O19 Ti6 Ti7 36.57(14) . .
Ti4 Ti6 Ti7 63.65(5) . .
C44 O23 Ti3 129.1(5) . .
C44 O21 Ti7 130.5(5) . .
C44 O21 Ti4 131.1(6) . .
Ti7 O21 Ti4 94.38(18) . .
C51 O25 Ti8 133.7(5) . .
C51 O25 Ti2 124.8(5) . 2_666
Ti8 O25 Ti2 101.4(2) . 2_666
Ti2 O8 Ti4 163.3(3) . .
Ti2 O8 Ti3 98.9(2) . .
Ti4 O8 Ti3 97.6(2) . .
C47 O22 Ti7 139.8(6) . .
Ti4 O10 Ti3 108.0(2) . .
Ti4 O10 Ti5 106.4(3) . .
Ti3 O10 Ti5 138.7(3) . .
Ti2 O5 Ti3 110.2(3) . .
Ti2 O5 Ti1 109.4(2) . .
Ti3 O5 Ti1 138.9(3) . .
C51 O24 Ti1 134.8(6) . 2_666
C50 O26 Ti8 138.2(6) . .
Ti7 O19 Ti4 117.1(2) . .
Ti7 O19 Ti6 101.7(2) . .
Ti4 O19 Ti6 97.7(2) . .
Ti6 O11 Ti5 147.5(3) . .
Ti6 O11 Ti4 101.8(3) . .
Ti5 O11 Ti4 100.2(2) . .
C13 O7 Ti2 128.6(6) . .
C13 O7 Ti8 115.1(7) . 2_666
Ti2 O7 Ti8 111.4(2) . 2_666
Ti8 O28 Ti7 153.8(3) . 2_666
C23 O9 Ti3 147.0(9) . .
C7 O4 Ti1 133.2(8) . .
C7 O4 Ti2 125.9(8) . .
Ti1 O4 Ti2 100.7(2) . .
N1 O1 Ti1 122.8(5) . .
C10 O6 Ti2 152.2(9) . .
C16 O15 Ti4 156.6(9) . .
C38 O20 Ti7 138.4(8) . .
C52 O27 Ti8 148.7(11) . .
C41 O18 Ti6 133.2(5) . .
C41 O18 Ti7 120.7(5) . .
Ti6 O18 Ti7 104.8(3) . .
C19 N1 O1 116.2(8) . .
C19 N1 Ti3 119.9(6) . .
O1 N1 Ti3 123.8(5) . .
C1 O2 Ti1 146.8(12) . .
C20 N2 O12 117.2(7) . .
C20 N2 Ti3 120.4(6) . .
O12 N2 Ti3 121.5(5) . .
C50 C49 C48 119.7(9) . .
C50 C49 C51 123.9(9) . .
C48 C49 C51 116.4(9) . .
C35 O17 Ti6 142.6(7) . .
C4 O3 Ti1 137.0(10) . .
C46 C45 C47 120.4(9) . .
C46 C45 C44 120.5(9) . .
C47 C45 C44 119.0(9) . .
C32 O16 Ti6 153.6(10) . .
O22 C47 C48 118.9(9) . .
O22 C47 C45 123.4(8) . .
C48 C47 C45 117.6(9) . .
N2 O12 Ti5 124.2(5) . .
O26 C50 C46 120.8(9) . .
O26 C50 C49 120.3(8) . .
C46 C50 C49 118.9(9) . .
O24 C51 O25 122.9(8) . .
O24 C51 C49 119.9(9) . .
O25 C51 C49 117.3(8) . .
C47 C48 C49 121.4(10) . .
C50 C46 C45 121.8(10) . .
O21 C44 O23 123.0(8) . .
O21 C44 C45 118.1(9) . .
O23 C44 C45 118.8(8) . .
N2 C20 C19 115.4(9) . .
N2 C20 C22 123.4(9) . .
C19 C20 C22 121.1(9) . .
N1 C19 C20 114.5(9) . .
N1 C19 C21 122.2(9) . .
C20 C19 C21 123.3(9) . .
C26 O14 Ti5 155.9(16) . .
C29 O13 Ti5 162.8(8) . .
C15 C13 C14 119.2(11) . .
C15 C13 O7 108.6(11) . .
C14 C13 O7 111.3(8) . .
O9 C23 C25 111.1(13) . .
O9 C23 C24 104.6(13) . .
C25 C23 C24 114.3(14) . .
O4 C7 C9 108.9(10) . .
O4 C7 C8 109.1(12) . .
C9 C7 C8 113.4(12) . .
O17 C35 C37 112.7(15) . .
O17 C35 C36 110.7(12) . .
C37 C35 C36 113.7(14) . .
O27 C52 C54 111.1(16) . .
O27 C52 C53 104.2(16) . .
C54 C52 C53 139.9(18) . .
C43 C41 C42 122.0(8) . .
C43 C41 O18 107.6(8) . .
C42 C41 O18 107.0(7) . .
C2 C1 C3 116(2) . .
C2 C1 O2 110.1(19) . .
C3 C1 O2 112.0(18) . .
C17 C16 O15 121.5(13) . .
C17 C16 C18 125.2(12) . .
O15 C16 C18 111.2(11) . .
C5 C4 O3 110.4(14) . .
C5 C4 C6 114.3(15) . .
O3 C4 C6 106.0(16) . .
O6 C10 C12 121.7(14) . .
O6 C10 C11 118.3(13) . .
C12 C10 C11 117.9(14) . .
C33 C32 O16 116.9(15) . .
C33 C32 C34 120.1(15) . .
O16 C32 C34 111.1(15) . .
C40 C38 O20 124.4(13) . .
C40 C38 C39 121.2(14) . .
O20 C38 C39 111.8(13) . .
O14 C26 C28 109.9(15) . .
O14 C26 C27 113.2(15) . .
C28 C26 C27 136.9(19) . .
C30 C29 O13 115.3(9) . .
C30 C29 C31 117.4(9) . .
O13 C29 C31 112.5(9) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti3 O9 1.776(5) .
Ti3 O5 1.926(5) .
Ti3 O10 1.938(5) .
Ti3 O23 2.147(5) .
Ti3 N1 2.235(7) .
Ti3 O8 2.228(6) .
Ti3 N2 2.232(7) .
Ti3 Ti4 3.119(2) .
Ti3 Ti2 3.1241(19) .
Ti4 O15 1.783(5) .
Ti4 O8 1.907(5) .
Ti4 O10 1.916(5) .
Ti4 O19 1.928(5) .
Ti4 O11 2.083(5) .
Ti4 O21 2.237(5) .
Ti4 Ti6 3.068(2) .
Ti4 Ti5 3.0900(19) .
Ti4 Ti7 3.2810(19) .
Ti8 O28 1.741(6) .
Ti8 O27 1.794(5) .
Ti8 O26 1.866(5) .
Ti8 O25 2.032(5) .
Ti8 O7 2.027(5) 2_666
Ti8 Ti2 3.3421(19) 2_666
Ti2 O6 1.763(5) .
Ti2 O8 1.874(5) .
Ti2 O5 1.883(6) .
Ti2 O7 2.019(6) .
Ti2 O4 2.065(6) .
Ti2 O25 2.281(5) 2_666
Ti2 Ti1 3.144(2) .
Ti2 Ti8 3.3420(19) 2_666
Ti7 O20 1.782(6) .
Ti7 O22 1.873(5) .
Ti7 O28 1.893(6) 2_666
Ti7 O19 1.918(5) .
Ti7 O18 2.087(6) .
Ti7 O21 2.235(5) .
Ti7 Ti6 3.152(2) .
Ti5 O13 1.735(8) .
Ti5 O14 1.756(7) .
Ti5 O11 1.944(6) .
Ti5 O10 1.943(5) .
Ti5 O12 1.974(7) .
Ti1 O3 1.776(6) .
Ti1 O2 1.799(6) .
Ti1 O5 1.969(5) .
Ti1 O1 1.974(6) .
Ti1 O4 2.020(6) .
Ti1 O24 2.189(5) 2_666
Ti6 O16 1.786(7) .
Ti6 O17 1.791(7) .
Ti6 O11 1.866(6) .
Ti6 O18 1.890(6) .
Ti6 O19 2.142(5) .
O23 C44 1.263(11) .
O21 C44 1.262(10) .
O25 C51 1.318(11) .
O25 Ti2 2.281(5) 2_666
O22 C47 1.325(10) .
O24 C51 1.222(11) .
O24 Ti1 2.189(5) 2_666
O26 C50 1.350(11) .
O7 C13 1.482(12) .
O7 Ti8 2.027(5) 2_666
O28 Ti7 1.893(6) 2_666
O9 C23 1.421(14) .
O4 C7 1.437(12) .
O1 N1 1.320(8) .
O6 C10 1.318(15) .
O15 C16 1.355(13) .
O20 C38 1.348(16) .
O27 C52 1.40(2) .
O18 C41 1.513(11) .
N1 C19 1.292(11) .
O2 C1 1.423(19) .
N2 C20 1.267(11) .
N2 O12 1.342(9) .
C49 C50 1.390(13) .
C49 C48 1.421(13) .
C49 C51 1.491(12) .
O17 C35 1.386(17) .
O3 C4 1.467(17) .
C45 C46 1.366(13) .
C45 C47 1.438(13) .
C45 C44 1.497(12) .
O16 C32 1.386(15) .
C47 C48 1.349(12) .
C50 C46 1.367(12) .
C20 C19 1.450(14) .
C20 C22 1.525(13) .
C19 C21 1.515(13) .
O14 C26 1.37(2) .
O13 C29 1.370(12) .
C13 C15 1.458(17) .
C13 C14 1.479(15) .
C23 C25 1.448(19) .
C23 C24 1.54(2) .
C7 C9 1.463(18) .
C7 C8 1.50(2) .
C35 C37 1.45(2) .
C35 C36 1.514(16) .
C52 C54 1.506(15) .
C52 C53 1.528(15) .
C41 C43 1.465(13) .
C41 C42 1.486(13) .
C1 C2 1.39(3) .
C1 C3 1.40(2) .
C16 C17 1.337(17) .
C16 C18 1.410(17) .
C4 C5 1.44(2) .
C4 C6 1.54(2) .
C10 C12 1.345(18) .
C10 C11 1.473(9) .
C32 C33 1.36(2) .
C32 C34 1.42(2) .
C30 C29 1.354(12) .
C31 C29 1.456(8) .
C38 C40 1.377(18) .
C38 C39 1.475(9) .
C26 C28 1.486(10) .
C26 C27 1.482(10) .
