#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:50:16 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551218.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_1551218
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 'C82 H171 N5 O36 Ti10'
_chemical_formula_sum 'C82 H171 N5 O36 Ti10'
_chemical_formula_weight 2281.91
_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 85.923(8)
_cell_angle_beta 85.061(7)
_cell_angle_gamma 66.484(9)
_cell_formula_units_Z 1
_cell_length_a 12.2992(10)
_cell_length_b 14.3904(15)
_cell_length_c 19.0996(17)
_cell_measurement_reflns_used 4796
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 3.9760
_cell_measurement_theta_min 67.5090
_cell_volume 3085.7(5)
_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 10.3503
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54178
_diffrn_reflns_av_R_equivalents 0.0386
_diffrn_reflns_av_unetI/netI 0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -14
_diffrn_reflns_limit_k_max 17
_diffrn_reflns_limit_k_min -17
_diffrn_reflns_limit_l_max 18
_diffrn_reflns_limit_l_min -23
_diffrn_reflns_number 21312
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full 67.679
_diffrn_reflns_theta_max 74.445
_diffrn_reflns_theta_min 3.352
_diffrn_source 'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 5.778
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.39623
_exptl_absorpt_correction_type multi-scan
_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.
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.228
_exptl_crystal_description block
_exptl_crystal_F_000 1205
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.2
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.015
_refine_diff_density_min -1.022
_refine_diff_density_rms 0.116
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.065
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 565
_refine_ls_number_reflns 12141
_refine_ls_number_restraints 379
_refine_ls_restrained_S_all 1.071
_refine_ls_R_factor_all 0.1869
_refine_ls_R_factor_gt 0.1334
_refine_ls_shift/su_max 0.001
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2900P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3760
_refine_ls_wR_factor_ref 0.4470
_reflns_Friedel_coverage 0.000
_reflns_number_gt 5930
_reflns_number_total 12141
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9dt02032b2.cif
_cod_data_source_block a_CCDC3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'multi-scan ' changed to
'multi-scan' according to
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.
Automatic conversion script
Id: cif_fix_values 4973 2017-02-22 13:04:09Z antanas
Adding full bibliography for 1551215--1551222.cif.
;
_cod_database_code 1551218
_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
_shelx_res_file
;
TITL a_a.res in P-1
REM Old TITL a in P-1
REM SHELXT solution in P-1
REM R1 0.293, Rweak 0.022, Alpha 0.114, Orientation as input
REM Formula found by SHELXT: C23 N7 O10 Ti5
CELL 1.54178 12.2992 14.3904 19.0996 85.923 85.061 66.484
ZERR 1 0.001 0.0015 0.0017 0.008 0.007 0.009
LATT 1
SFAC C H N O Ti
UNIT 82 170 5 36 10
DFIX 1.52 0.01 C27 C29
DFIX 1.52 0.01 C5 C6
DFIX 1.52 0.01 C33 C34
DFIX 1.52 0.01 C33 C35
DFIX 1.45 C44 C42 C43 C42
DFIX 2.2 C43 C44
DFIX 1.45 C44 C42
DFIX 1.45 C7 C5
DFIX 1.5 0.01 C8 C10
DFIX 1.5 0.01 C24 C25
DELU O17
DELU C11 C12
DELU C39 C41
SIMU 0.01 0.02 1.7 C21 C22 C23 C20 C1 C3 C2 C4 C17 C39 C14 C19 C24 C13 C7 =
C41 C11 C40 C5 C30 C18 C33 C8 C27 C16 C35 C26 C32 C25 C28 C12 C29 C10 C9 =
C31 C15 C6 C34 C42 C43 C44
ISOR 0.001 0.002 O15 C41
ISOR 0.001 0.002 O15 C40
ISOR 0.001 0.002 O17
ISOR 0.001 0.002 C44 C43
ISOR 0.001 0.002 C34
ISOR 0.001 0.002 O3 C5 C7 C6
ISOR 0.001 0.002 C24 C25
ISOR 0.001 0.002 C33 C35
ISOR 0.001 0.002 O12 C14 C15 C16
ISOR 0.001 0.002 O5 C11 C13 C12
ISOR 0.001 0.002 O9 C30 C31 C32
ISOR 0.001 0.002 C22 N3
ISOR 0.001 0.002 O13 C27 C28 C29
EADP O17 C44
EADP O4 C10
EADP O4 C9
EADP O4 C8
EADP O17 C42
EADP O15 C39
EADP O16 C33
L.S. 40
PLAN 10
BOND $H
list 4
ABIN
fmap 2
acta
SHEL 999 0.8
OMIT -4 2 2
OMIT 4 -2 4
OMIT 2 -1 1
OMIT 0 -4 3
OMIT 2 -1 7
OMIT 1 5 5
OMIT -3 3 3
OMIT -2 4 1
OMIT -2 1 7
OMIT -2 4 4
OMIT -4 -2 2
OMIT -2 2 5
OMIT 0 6 1
OMIT 1 -1 9
OMIT 0 2 1
OMIT 2 11 2
OMIT 2 -1 3
OMIT -1 4 6
REM
REM
REM
WGHT 0.290000
FVAR 0.42820
TI01 5 0.399994 0.384680 0.781043 11.00000 0.08991 0.11659 =
0.04689 0.00653 -0.00818 -0.05175
TI02 5 0.149205 0.483188 0.720997 11.00000 0.07961 0.13578 =
0.06161 0.00322 -0.00055 -0.04808
TI03 5 0.341648 0.209932 0.728732 11.00000 0.11140 0.12201 =
0.08565 0.00756 -0.02181 -0.06364
TI04 5 0.230644 0.651618 0.762554 11.00000 0.10834 0.11874 =
0.08556 -0.00107 0.00078 -0.04518
TI05 5 0.611033 0.123118 0.762817 11.00000 0.10997 0.11667 =
0.09507 0.01207 -0.01948 -0.04668
O10 4 0.451392 0.411024 0.677452 11.00000 0.07956 0.12624 =
0.04989 0.01053 0.00295 -0.04327
O7 4 0.266711 0.349319 0.742619 11.00000 0.08850 0.13188 =
0.06204 0.00821 -0.00836 -0.05459
O11 4 0.273431 0.487246 0.632372 11.00000 0.07382 0.15183 =
0.05605 0.01754 0.00070 -0.04693
O6 4 0.262498 0.512115 0.775368 11.00000 0.08574 0.11668 =
0.06046 -0.00087 0.00189 -0.03996
O8 4 0.468643 0.238526 0.760611 11.00000 0.10407 0.10839 =
0.08588 0.00650 -0.02003 -0.04709
O15 4 0.384229 0.364524 0.873426 11.00000 0.12348 0.12517 =
0.11955 -0.00302 -0.00826 -0.04885
O5 4 0.103147 0.636429 0.715020 11.00000 0.10919 0.11090 =
0.10930 -0.00310 -0.00732 -0.04245
O12 4 0.060102 0.468319 0.655333 11.00000 0.10277 0.10789 =
0.10366 -0.00387 -0.00743 -0.04222
C21 1 0.443294 0.478974 0.561452 11.00000 0.07854 0.10010 =
0.04963 0.00151 -0.00303 -0.04435
N1 3 0.466044 0.508235 0.795260 11.00000 0.10521 0.11901 =
0.08478 -0.00664 -0.00803 -0.05884
C22 1 0.379233 0.522098 0.503848 11.00000 0.07855 0.08189 =
0.07767 -0.00232 -0.00522 -0.03209
C23 1 0.434909 0.543239 0.442252 11.00000 0.07841 0.11821 =
0.05177 0.01293 -0.00939 -0.04217
AFIX 43
H23 2 0.391075 0.572298 0.403266 11.00000 -1.20000
AFIX 0
O18 4 0.043462 0.488586 0.793368 11.00000 0.09690 0.18666 =
0.07254 -0.00443 0.00954 -0.06585
O2 4 0.664270 0.222776 0.796960 11.00000 0.11804 0.12217 =
0.13788 0.01864 -0.05133 -0.04937
N2 3 0.597862 0.322504 0.793827 11.00000 0.09692 0.11383 =
0.07501 0.01206 -0.01443 -0.04735
C20 1 0.385312 0.456772 0.628871 11.00000 0.08283 0.11409 =
0.04213 0.00388 0.00174 -0.04950
O1 4 0.396647 0.603694 0.785654 11.00000 0.11878 0.12406 =
0.18759 -0.02918 -0.00337 -0.05798
O14 4 0.248872 0.165716 0.785109 11.00000 0.12677 0.15881 =
0.19060 0.02415 -0.00459 -0.08698
O4 4 0.165232 0.715435 0.840369 11.00000 0.23267 0.23747 =
0.14895 -0.05540 0.02044 -0.10147
O9 4 0.488497 0.077503 0.735862 11.00000 0.12455 0.12361 =
0.12475 -0.00546 -0.00860 -0.04929
C1 1 0.576132 0.487505 0.803459 11.00000 0.10487 0.14124 =
0.10214 -0.00097 -0.02276 -0.07368
O3 4 0.249106 0.739241 0.700940 11.00000 0.15937 0.15937 =
0.15974 -0.00508 -0.00928 -0.06390
O13 4 0.325800 0.198835 0.640041 11.00000 0.14483 0.14449 =
0.14302 -0.00636 -0.01075 -0.05683
C3 1 0.651666 0.379539 0.806918 11.00000 0.10014 0.14316 =
0.09393 0.00003 -0.02377 -0.06408
O17 4 0.713918 0.089391 0.688780 11.00000 0.19167 0.19225 =
0.19169 -0.00755 -0.01155 -0.07627
O16 4 0.668911 0.035753 0.833018 11.00000 0.17730 0.17711 =
0.17650 -0.00587 -0.01216 -0.06998
C2 1 0.625489 0.568168 0.806732 11.00000 0.11732 0.15829 =
0.19984 -0.02597 -0.01939 -0.07229
AFIX 33
H2A 2 0.709200 0.536274 0.813039 11.00000 -1.50000
H2B 2 0.612292 0.608749 0.763712 11.00000 -1.50000
H2C 2 0.586225 0.610553 0.845518 11.00000 -1.50000
AFIX 0
C4 1 0.776350 0.341658 0.828063 11.00000 0.10611 0.16166 =
0.16798 -0.00489 -0.03940 -0.05829
AFIX 33
H4A 2 0.796487 0.398198 0.834865 11.00000 -1.50000
H4B 2 0.783758 0.301524 0.871123 11.00000 -1.50000
H4C 2 0.829136 0.300845 0.791826 11.00000 -1.50000
AFIX 0
C17 1 0.027270 0.512490 0.864506 11.00000 0.14210 0.24240 =
0.06904 -0.01723 0.01473 -0.10367
AFIX 13
H17 2 0.090239 0.532970 0.876415 11.00000 -1.20000
AFIX 0
C39 1 0.423861 0.337737 0.940614 11.00000 0.12348 0.12517 =
0.11955 -0.00302 -0.00826 -0.04885
AFIX 13
H39 2 0.506323 0.291563 0.929503 11.00000 -1.20000
AFIX 0
C14 1 -0.049045 0.462252 0.655706 11.00000 0.21564 0.21585 =
0.21575 -0.00869 -0.01382 -0.08542
AFIX 13
H14 2 -0.095174 0.485092 0.700213 11.00000 -1.20000
AFIX 0
C19 1 -0.087776 0.595290 0.876931 11.00000 0.17160 0.24699 =
0.12949 -0.05773 0.04292 -0.03587
AFIX 33
H19A 2 -0.099002 0.611745 0.925580 11.00000 -1.50000
H19B 2 -0.090865 0.653641 0.848130 11.00000 -1.50000
H19C 2 -0.149400 0.575140 0.865286 11.00000 -1.50000
AFIX 0
C24 1 0.139058 0.169802 0.809557 11.00000 0.22913 0.22926 =
0.22899 -0.00914 -0.01433 -0.09090
AFIX 13
H24 2 0.080048 0.239554 0.804544 11.00000 -1.20000
AFIX 0
C13 1 0.019647 0.722532 0.604503 11.00000 0.18812 0.18810 =
0.18720 -0.00690 -0.01319 -0.07373
AFIX 33
H13A 2 -0.050255 0.772151 0.584580 11.00000 -1.50000
H13B 2 0.084570 0.743506 0.594888 11.00000 -1.50000
H13C 2 0.039260 0.658294 0.584104 11.00000 -1.50000
AFIX 0
C7 1 0.255573 0.884710 0.629590 11.00000 0.25666 0.25592 =
0.25702 -0.01003 -0.01585 -0.10195
AFIX 33
H7A 2 0.298725 0.903519 0.590826 11.00000 -1.50000
H7B 2 0.174409 0.904835 0.618559 11.00000 -1.50000
H7C 2 0.258333 0.917931 0.670843 11.00000 -1.50000
AFIX 0
C41 1 0.441359 0.411813 0.970236 11.00000 0.20070 0.19849 =
0.19922 -0.01008 -0.01369 -0.07979
AFIX 3
H41A 2 0.361969 0.462893 0.973846 11.00000 -1.50000
H41B 2 0.493539 0.440493 0.946576 11.00000 -1.50000
H41C 2 0.467219 0.387073 1.016526 11.00000 -1.50000
AFIX 0
C11 1 -0.002476 0.712925 0.680001 11.00000 0.19308 0.19327 =
0.19326 -0.00732 -0.01222 -0.07630
AFIX 13
H11 2 -0.067937 0.690249 0.688404 11.00000 -1.20000
AFIX 0
C40 1 0.380868 0.271208 0.976305 11.00000 0.19905 0.19840 =
0.19803 -0.00585 -0.01122 -0.07793
AFIX 137
H40A 2 0.417940 0.249163 1.020127 11.00000 -1.50000
H40B 2 0.398360 0.213544 0.948310 11.00000 -1.50000
H40C 2 0.296442 0.304704 0.985271 11.00000 -1.50000
AFIX 0
C5 1 0.307353 0.778723 0.642140 11.00000 0.25014 0.25017 =
0.25021 -0.00965 -0.01558 -0.09893
AFIX 13
H5 2 0.281277 0.756130 0.601901 11.00000 -1.20000
AFIX 0
C30 1 0.492894 -0.023474 0.722384 11.00000 0.18953 0.18920 =
0.18951 -0.00773 -0.01201 -0.07527
AFIX 13
H30 2 0.415963 -0.011204 0.704277 11.00000 -1.20000
AFIX 0
C18 1 0.039048 0.412870 0.905958 11.00000 0.24309 0.27011 =
0.09868 -0.00520 0.00507 -0.09211
AFIX 33
H18A 2 0.028779 0.424151 0.955473 11.00000 -1.50000
H18B 2 -0.020672 0.391400 0.892833 11.00000 -1.50000
H18C 2 0.116344 0.361268 0.895278 11.00000 -1.50000
AFIX 0
C33 1 0.713740 0.005966 0.895686 11.00000 0.17730 0.17711 =
0.17650 -0.00587 -0.01216 -0.06998
AFIX 13
H33 2 0.643143 0.039320 0.926981 11.00000 -1.20000
AFIX 0
C8 1 0.153629 0.781394 0.891175 11.00000 0.23267 0.23747 =
0.14895 -0.05540 0.02044 -0.10147
AFIX 13
H8 2 0.083573 0.844497 0.884682 11.00000 -1.20000
AFIX 0
C27 1 0.290382 0.238999 0.569375 11.00000 0.22439 0.22446 =
0.22431 -0.00936 -0.01432 -0.08897
AFIX 13
H27 2 0.223149 0.305006 0.567757 11.00000 -1.20000
AFIX 0
C16 1 -0.113278 0.523821 0.595866 11.00000 0.24518 0.24563 =
0.24584 -0.00928 -0.01653 -0.09685
AFIX 33
H16A 2 -0.189353 0.519820 0.595916 11.00000 -1.50000
H16B 2 -0.124234 0.593153 0.599938 11.00000 -1.50000
H16C 2 -0.068124 0.498629 0.552731 11.00000 -1.50000
AFIX 0
C35 1 0.800131 0.042480 0.923250 11.00000 0.23378 0.23316 =
0.23332 -0.00893 -0.01513 -0.09204
AFIX 33
H35A 2 0.821187 0.011923 0.969126 11.00000 -1.50000
H35B 2 0.870258 0.023900 0.892003 11.00000 -1.50000
H35C 2 0.764075 0.114917 0.926208 11.00000 -1.50000
AFIX 0
C26 1 0.103849 0.100828 0.770407 11.00000 0.22131 0.27161 =
0.26593 0.01452 0.03800 -0.11734
AFIX 33
H26A 2 0.026796 0.105016 0.788445 11.00000 -1.50000
H26B 2 0.101329 0.120844 0.721343 11.00000 -1.50000
H26C 2 0.160819 0.032345 0.776300 11.00000 -1.50000
AFIX 0
C32 1 0.578285 -0.059118 0.664247 11.00000 0.22685 0.22654 =
0.22732 -0.01004 -0.01382 -0.08942
AFIX 33
H32A 2 0.556440 -0.010320 0.625543 11.00000 -1.50000
H32B 2 0.655353 -0.068325 0.677910 11.00000 -1.50000
H32C 2 0.580323 -0.122612 0.650302 11.00000 -1.50000
AFIX 0
C25 1 0.137346 0.133041 0.884507 11.00000 0.27833 0.27860 =
0.27854 -0.01057 -0.01732 -0.11001
AFIX 33
H25A 2 0.059075 0.137160 0.899490 11.00000 -1.50000
H25B 2 0.193176 0.063898 0.888971 11.00000 -1.50000
H25C 2 0.158687 0.174411 0.913290 11.00000 -1.50000
AFIX 0
C28 1 0.267085 0.150724 0.540968 11.00000 0.25210 0.25155 =
0.25161 -0.01080 -0.01635 -0.09960
AFIX 33
H28A 2 0.242564 0.167829 0.493730 11.00000 -1.50000
H28B 2 0.338618 0.090184 0.541325 11.00000 -1.50000
H28C 2 0.205654 0.139518 0.570267 11.00000 -1.50000
AFIX 0
C12 1 -0.038254 0.814321 0.718976 11.00000 0.21875 0.21824 =
0.21835 -0.00940 -0.01449 -0.08555
AFIX 33
H12A 2 -0.051454 0.802364 0.768449 11.00000 -1.50000
H12B 2 0.024518 0.838259 0.711384 11.00000 -1.50000
H12C 2 -0.109712 0.864371 0.700936 11.00000 -1.50000
AFIX 0
C29 1 0.401383 0.235420 0.527280 11.00000 0.25356 0.25301 =
0.25319 -0.01073 -0.01551 -0.10024
AFIX 33
H29A 2 0.382241 0.261256 0.480191 11.00000 -1.50000
H29B 2 0.433915 0.276140 0.548775 11.00000 -1.50000
H29C 2 0.458664 0.166586 0.526073 11.00000 -1.50000
AFIX 0
C10 1 0.142867 0.731111 0.960377 11.00000 0.23267 0.23747 =
0.14895 -0.05540 0.02044 -0.10147
AFIX 3
H10A 2 0.091487 0.794571 0.980037 11.00000 -1.50000
H10B 2 0.203747 0.694351 0.991987 11.00000 -1.50000
H10C 2 0.097427 0.691941 0.953447 11.00000 -1.50000
AFIX 0
N3 3 0.266985 0.549095 0.503012 10.50000 0.17470 0.17598 =
0.17491 -0.00636 -0.01103 -0.06919
AFIX 93
H3A 2 0.226866 0.540540 0.540231 10.50000 -1.20000
H3B 2 0.231542 0.575822 0.465230 10.50000 -1.20000
AFIX 0
C9 1 0.258902 0.802204 0.892553 11.00000 0.23267 0.23747 =
0.14895 -0.05540 0.02044 -0.10147
AFIX 33
H9A 2 0.247670 0.848713 0.928788 11.00000 -1.50000
H9B 2 0.325702 0.740151 0.901928 11.00000 -1.50000
H9C 2 0.273353 0.831590 0.847861 11.00000 -1.50000
AFIX 0
C31 1 0.493191 -0.070851 0.785985 11.00000 0.22721 0.22695 =
0.22778 -0.00893 -0.01479 -0.09006
AFIX 33
H31A 2 0.425511 -0.029923 0.814948 11.00000 -1.50000
H31B 2 0.489621 -0.135308 0.780319 11.00000 -1.50000
H31C 2 0.564651 -0.081021 0.807927 11.00000 -1.50000
AFIX 0
C15 1 -0.032709 0.360654 0.644005 11.00000 0.23410 0.23489 =
0.23525 -0.00870 -0.01488 -0.09330
AFIX 33
H15A 2 -0.108773 0.356576 0.644282 11.00000 -1.50000
H15B 2 0.009589 0.340756 0.599284 11.00000 -1.50000
H15C 2 0.012059 0.316212 0.680570 11.00000 -1.50000
AFIX 0
C6 1 0.438576 0.714701 0.635731 11.00000 0.25310 0.25239 =
0.25294 -0.00993 -0.01506 -0.10046
AFIX 33
H6A 2 0.452065 0.645005 0.646861 11.00000 -1.50000
H6B 2 0.469099 0.721165 0.588481 11.00000 -1.50000
H6C 2 0.478287 0.737086 0.667762 11.00000 -1.50000
AFIX 0
C34 1 0.740633 -0.104527 0.915073 11.00000 0.22685 0.22660 =
0.22675 -0.00834 -0.01433 -0.08961
AFIX 33
H34A 2 0.772554 -0.121164 0.960596 11.00000 -1.50000
H34B 2 0.668856 -0.116121 0.916116 11.00000 -1.50000
H34C 2 0.797540 -0.146353 0.880801 11.00000 -1.50000
AFIX 0
C42 1 0.770270 0.123761 0.627236 11.00000 0.19167 0.19225 =
0.19169 -0.00755 -0.01155 -0.07627
AFIX 13
H42 2 0.721365 0.186336 0.602032 11.00000 -1.20000
AFIX 0
C43 1 0.817753 0.029056 0.588207 11.00000 0.26459 0.26519 =
0.26500 -0.01056 -0.01625 -0.10415
AFIX 137
H43A 2 0.846306 -0.028166 0.620743 11.00000 -1.50000
H43B 2 0.881863 0.028992 0.555739 11.00000 -1.50000
H43C 2 0.755905 0.024884 0.562813 11.00000 -1.50000
AFIX 0
C44 1 0.882782 0.116371 0.648589 11.00000 0.19167 0.19225 =
0.19169 -0.00755 -0.01155 -0.07627
AFIX 137
H44A 2 0.869791 0.164376 0.684062 11.00000 -1.50000
H44B 2 0.927507 0.130757 0.608722 11.00000 -1.50000
H44C 2 0.926191 0.049043 0.667246 11.00000 -1.50000
AFIX 0
HKLF 4
REM a_a.res in P-1
REM R1 = 0.1334 for 5930 Fo > 4sig(Fo) and 0.1869 for all 12141 data
REM 565 parameters refined using 379 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.015, deepest hole -1.022, 1-sigma level 0.116
Q1 1 0.3554 0.5884 0.3889 11.00000 0.05 0.69
Q2 1 0.0816 0.4176 0.6518 11.00000 0.05 0.63
Q3 1 0.0468 0.5201 0.6571 11.00000 0.05 0.62
Q4 1 0.3166 0.8043 0.6776 11.00000 0.05 0.61
Q5 1 0.3072 0.4768 0.9705 11.00000 0.05 0.59
Q6 1 0.7505 0.2159 0.6245 11.00000 0.05 0.59
Q7 1 0.7029 0.0204 0.8199 11.00000 0.05 0.56
Q8 1 0.5989 -0.1021 0.7291 11.00000 0.05 0.56
Q9 1 0.3787 0.2084 0.6216 11.00000 0.05 0.55
Q10 1 0.6335 -0.0161 0.9544 11.00000 0.05 0.54
;
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14 6 8 -0.1805 -0.0178
14 6 9 0.2869 -0.0368
14 6 10 -0.0633 -0.0178
14 7 0 -0.3359 -0.0039
14 7 1 -0.2984 0.0585
14 7 2 -0.0440 0.0364
14 7 3 0.0419 0.0229
14 7 4 -0.1794 0.0436
14 7 5 0.1762 -0.0055
14 7 6 -0.0540 -0.0303
14 7 7 -0.0127 -0.0036
14 7 8 -0.2009 -0.0197
14 7 9 0.2684 0.0067
14 7 10 -0.1217 0.0065
14 8 0 -0.3564 0.0989
14 8 1 0.0479 0.0627
14 8 2 -0.3193 0.0277
14 8 3 -0.0016 0.0188
14 8 4 -0.0389 -0.0147
14 8 5 0.1888 -0.0298
14 8 6 -0.3974 -0.0035
14 8 7 0.0872 0.0318
14 8 8 -0.0820 0.0019
14 8 9 0.0988 0.0508
14 8 10 -0.0824 0.0100
14 9 0 -0.1808 0.0744
14 9 1 -0.2184 0.0140
14 9 2 -0.6166 -0.0106
14 9 3 0.2870 -0.0180
14 9 4 -0.2386 -0.0258
14 9 5 0.0310 0.0324
14 9 6 -0.1003 0.0233
14 9 7 0.2007 0.0441
14 9 8 -0.2146 0.0109
14 9 9 0.0430 0.0548
14 10 0 -0.6607 -0.0127
14 10 1 -0.4727 -0.0325
14 10 2 -0.3267 -0.0285
14 10 3 0.2261 0.0132
14 10 4 -0.2914 0.0264
14 10 5 0.3415 0.0450
14 10 6 -0.0069 -0.0044
14 10 7 -0.0724 0.0344
14 10 8 -0.0404 -0.0062
14 10 9 -0.1407 0.0279
14 11 0 -0.8215 -0.0700
14 11 1 -0.0337 -0.0130
14 11 2 -0.0646 0.0254
14 11 3 0.0434 0.0403
14 11 4 -0.0553 0.0027
14 11 5 0.1482 -0.0083
14 11 6 -0.1014 -0.0181
14 11 7 0.0378 0.0081
14 11 8 -0.0346 -0.0217
14 12 0 -0.0258 -0.0187
14 12 1 0.2629 0.0467
14 12 2 -0.2360 0.0286
14 12 3 -0.1535 -0.0285
14 12 4 -0.1080 -0.0354
14 12 5 -0.0040 -0.0253
14 12 6 0.1244 -0.0151
14 13 0 0.3330 0.0589
14 13 1 -0.1955 0.0056
14 13 2 -0.4473 -0.0405
15 5 2 -0.2408 -0.0084
15 5 3 -0.1932 -0.0266
15 5 4 0.2879 0.0021
15 5 5 0.1983 -0.0006
15 6 0 0.2966 0.0308
15 6 1 -0.3463 0.0218
15 6 2 0.0800 -0.0262
15 6 3 0.2514 -0.0137
15 6 4 0.1460 -0.0091
15 6 5 0.0407 -0.0390
15 6 6 0.0092 -0.0187
15 7 0 0.1648 0.0281
15 7 1 0.1332 -0.0356
15 7 2 0.2825 -0.0282
15 7 3 0.0050 -0.0251
15 7 4 0.0171 -0.0382
15 7 5 0.1365 -0.0370
15 7 6 -0.1292 -0.0044
15 8 0 0.4457 -0.0382
15 8 1 0.1797 -0.0594
15 8 2 -0.2037 -0.0171
15 8 3 0.1343 -0.0340
15 8 4 -0.0548 -0.0175
15 8 5 -0.0074 0.0155
15 8 6 -0.0435 0.0045
15 9 0 0.0501 -0.0547
15 9 1 -0.0760 -0.0253
15 9 2 -0.0909 -0.0028
15 9 3 0.2885 0.0121
15 9 4 -0.3630 0.0360
15 9 5 0.2263 0.0285
15 10 1 0.3112 0.0207
15 10 2 0.0577 0.0355
15 10 3 0.0662 0.0556
15 10 4 -0.2652 0.0081
0 0 0 0.0 0.0
;
_shelx_fab_checksum 9624
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
_atom_site_refinement_flags_occupancy
Ti01 Ti 0.39999(13) 0.38468(12) 0.78104(6) 0.0813(4) Uani 1 1 d . . .
Ti02 Ti 0.14920(14) 0.48319(14) 0.72100(7) 0.0912(5) Uani 1 1 d . . .
Ti03 Ti 0.34165(17) 0.20993(14) 0.72873(9) 0.1004(5) Uani 1 1 d . . .
Ti04 Ti 0.23064(17) 0.65162(14) 0.76255(9) 0.1047(6) Uani 1 1 d . . .
Ti05 Ti 0.61103(18) 0.12312(14) 0.76282(9) 0.1067(6) Uani 1 1 d . . .
O10 O 0.4514(5) 0.4110(4) 0.6775(2) 0.0856(14) Uani 1 1 d . . .
O7 O 0.2667(5) 0.3493(5) 0.7426(3) 0.0910(15) Uani 1 1 d . . .
O11 O 0.2734(5) 0.4872(5) 0.6324(2) 0.0946(16) Uani 1 1 d . . .
O6 O 0.2625(5) 0.5121(4) 0.7754(3) 0.0882(14) Uani 1 1 d . . .
O8 O 0.4686(6) 0.2385(5) 0.7606(3) 0.0975(16) Uani 1 1 d . . .
O15 O 0.3842(7) 0.3645(6) 0.8734(4) 0.1229(17) Uani 1 1 d . U .
O5 O 0.1031(6) 0.6364(5) 0.7150(4) 0.1102(18) Uani 1 1 d . U .
O12 O 0.0601(6) 0.4683(5) 0.6553(3) 0.1046(17) Uani 1 1 d . U .
C21 C 0.4433(6) 0.4790(6) 0.5615(3) 0.0735(15) Uani 1 1 d . U .
N1 N 0.4660(8) 0.5082(6) 0.7953(4) 0.098(2) Uani 1 1 d . . .
C22 C 0.3792(7) 0.5221(5) 0.5038(4) 0.0793(16) Uani 1 1 d . U .
C23 C 0.4349(7) 0.5432(6) 0.4423(3) 0.0823(18) Uani 1 1 d . U .
H23 H 0.3911 0.5723 0.4033 0.099 Uiso 1 1 calc R U .
O18 O 0.0435(6) 0.4886(6) 0.7934(3) 0.117(2) Uani 1 1 d . . .
O2 O 0.6643(7) 0.2228(6) 0.7970(4) 0.124(2) Uani 1 1 d . . .
N2 N 0.5979(7) 0.3225(6) 0.7938(4) 0.0937(19) Uani 1 1 d . . .
C20 C 0.3853(7) 0.4568(6) 0.6289(3) 0.0770(16) Uani 1 1 d . U .
O1 O 0.3966(8) 0.6037(6) 0.7857(5) 0.140(3) Uani 1 1 d . . .
O14 O 0.2489(8) 0.1657(7) 0.7851(6) 0.151(3) Uani 1 1 d . . .
O4 O 0.1652(13) 0.7154(11) 0.8404(6) 0.203(3) Uani 1 1 d . . .
O9 O 0.4885(7) 0.0775(6) 0.7359(4) 0.124(2) Uani 1 1 d . U .
C1 C 0.5761(9) 0.4875(9) 0.8035(5) 0.107(2) Uani 1 1 d . U .
O3 O 0.2491(9) 0.7392(8) 0.7009(6) 0.159(3) Uani 1 1 d . U .
O13 O 0.3258(8) 0.1988(7) 0.6400(5) 0.144(3) Uani 1 1 d . U .
C3 C 0.6517(9) 0.3795(9) 0.8069(5) 0.106(2) Uani 1 1 d . U .
O17 O 0.7139(12) 0.0894(10) 0.6888(7) 0.192(3) Uani 1 1 d . U .
O16 O 0.6689(11) 0.0358(8) 0.8330(7) 0.177(3) Uani 1 1 d . . .
C2 C 0.6255(12) 0.5682(11) 0.8067(9) 0.151(4) Uani 1 1 d . U .
H2A H 0.7092 0.5363 0.8130 0.227 Uiso 1 1 calc R U .
H2B H 0.6123 0.6087 0.7637 0.227 Uiso 1 1 calc R U .
H2C H 0.5862 0.6106 0.8455 0.227 Uiso 1 1 calc R U .
C4 C 0.7763(11) 0.3417(10) 0.8281(8) 0.142(4) Uani 1 1 d . U .
H4A H 0.7965 0.3982 0.8349 0.213 Uiso 1 1 calc R U .
H4B H 0.7838 0.3015 0.8711 0.213 Uiso 1 1 calc R U .
H4C H 0.8291 0.3008 0.7918 0.213 Uiso 1 1 calc R U .
C17 C 0.0273(12) 0.5125(13) 0.8645(5) 0.143(4) Uani 1 1 d . U .
H17 H 0.0902 0.5330 0.8764 0.172 Uiso 1 1 calc R U .
C39 C 0.4239(12) 0.3377(9) 0.9406(6) 0.1229(17) Uani 1 1 d . U .
H39 H 0.5063 0.2916 0.9295 0.147 Uiso 1 1 calc R U .
C14 C -0.049(2) 0.4623(18) 0.6557(13) 0.216(6) Uani 1 1 d . U .
H14 H -0.0952 0.4851 0.7002 0.259 Uiso 1 1 calc R U .
C19 C -0.0878(16) 0.5953(15) 0.8769(8) 0.198(7) Uani 1 1 d . U .
H19A H -0.0990 0.6117 0.9256 0.297 Uiso 1 1 calc R U .
H19B H -0.0909 0.6536 0.8481 0.297 Uiso 1 1 calc R U .
H19C H -0.1494 0.5751 0.8653 0.297 Uiso 1 1 calc R U .
C24 C 0.139(2) 0.170(2) 0.8096(13) 0.229(7) Uani 1 1 d D U .
H24 H 0.0800 0.2396 0.8045 0.275 Uiso 1 1 calc R U .
C13 C 0.0196(18) 0.7225(14) 0.6045(10) 0.188(6) Uani 1 1 d . U .
H13A H -0.0503 0.7722 0.5846 0.282 Uiso 1 1 calc R U .
H13B H 0.0846 0.7435 0.5949 0.282 Uiso 1 1 calc R U .
H13C H 0.0393 0.6583 0.5841 0.282 Uiso 1 1 calc R U .
C7 C 0.256(2) 0.8847(19) 0.6296(14) 0.256(9) Uani 1 1 d D U .
H7A H 0.2987 0.9035 0.5908 0.385 Uiso 1 1 calc R U .
H7B H 0.1744 0.9048 0.6186 0.385 Uiso 1 1 calc R U .
H7C H 0.2583 0.9179 0.6708 0.385 Uiso 1 1 calc R U .
C41 C 0.4414(18) 0.4118(14) 0.9702(10) 0.199(5) Uani 1 1 d . U .
H41A H 0.3620 0.4629 0.9738 0.299 Uiso 1 1 d R U .
H41B H 0.4935 0.4405 0.9466 0.299 Uiso 1 1 d R U .
H41C H 0.4672 0.3871 1.0165 0.299 Uiso 1 1 d R U .
C11 C -0.0025(19) 0.7129(15) 0.6800(11) 0.193(5) Uani 1 1 d . U .
H11 H -0.0679 0.6902 0.6884 0.232 Uiso 1 1 calc R U .
C40 C 0.3809(19) 0.2712(15) 0.9763(11) 0.199(6) Uani 1 1 d . U .
H40A H 0.4179 0.2492 1.0201 0.298 Uiso 1 1 calc R U .
H40B H 0.3984 0.2135 0.9483 0.298 Uiso 1 1 calc R U .
H40C H 0.2964 0.3047 0.9853 0.298 Uiso 1 1 calc R U .
C5 C 0.307(2) 0.7787(19) 0.6421(16) 0.250(8) Uani 1 1 d D U .
H5 H 0.2813 0.7561 0.6019 0.300 Uiso 1 1 calc R U .
C30 C 0.493(2) -0.0235(15) 0.7224(12) 0.189(6) Uani 1 1 d . U .
H30 H 0.4160 -0.0112 0.7043 0.227 Uiso 1 1 calc R U .
C18 C 0.039(2) 0.4129(16) 0.9060(8) 0.208(7) Uani 1 1 d . U .
H18A H 0.0288 0.4242 0.9555 0.312 Uiso 1 1 calc R U .
H18B H -0.0207 0.3914 0.8928 0.312 Uiso 1 1 calc R U .
H18C H 0.1163 0.3613 0.8953 0.312 Uiso 1 1 calc R U .
C33 C 0.7137(17) 0.0060(13) 0.8957(10) 0.177(3) Uani 1 1 d D U .
H33 H 0.6431 0.0393 0.9270 0.212 Uiso 1 1 calc R U .
C8 C 0.154(2) 0.7814(16) 0.8912(8) 0.203(3) Uani 1 1 d D U .
H8 H 0.0836 0.8445 0.8847 0.244 Uiso 1 1 calc R U .
C27 C 0.290(2) 0.2390(19) 0.5694(13) 0.224(7) Uani 1 1 d D U .
H27 H 0.2231 0.3050 0.5678 0.269 Uiso 1 1 calc R U .
C16 C -0.113(2) 0.5238(19) 0.5959(14) 0.246(8) Uani 1 1 d . U .
H16A H -0.1894 0.5198 0.5959 0.368 Uiso 1 1 calc R U .
H16B H -0.1242 0.5932 0.5999 0.368 Uiso 1 1 calc R U .
H16C H -0.0681 0.4986 0.5527 0.368 Uiso 1 1 calc R U .
C35 C 0.8001(19) 0.0425(16) 0.9232(12) 0.233(7) Uani 1 1 d D U .
H35A H 0.8212 0.0119 0.9691 0.350 Uiso 1 1 calc R U .
H35B H 0.8703 0.0239 0.8920 0.350 Uiso 1 1 calc R U .
H35C H 0.7641 0.1149 0.9262 0.350 Uiso 1 1 calc R U .
C26 C 0.104(2) 0.1008(19) 0.7704(14) 0.251(9) Uani 1 1 d . U .
H26A H 0.0268 0.1050 0.7884 0.377 Uiso 1 1 calc R U .
H26B H 0.1013 0.1208 0.7213 0.377 Uiso 1 1 calc R U .
H26C H 0.1608 0.0323 0.7763 0.377 Uiso 1 1 calc R U .
C32 C 0.578(2) -0.0591(16) 0.6642(12) 0.227(7) Uani 1 1 d . U .
H32A H 0.5564 -0.0103 0.6255 0.340 Uiso 1 1 calc R U .
H32B H 0.6554 -0.0683 0.6779 0.340 Uiso 1 1 calc R U .
H32C H 0.5803 -0.1226 0.6503 0.340 Uiso 1 1 calc R U .
C25 C 0.137(3) 0.133(2) 0.8845(14) 0.279(9) Uani 1 1 d D U .
H25A H 0.0591 0.1372 0.8995 0.418 Uiso 1 1 calc R U .
H25B H 0.1932 0.0639 0.8890 0.418 Uiso 1 1 calc R U .
H25C H 0.1587 0.1744 0.9133 0.418 Uiso 1 1 calc R U .
C28 C 0.267(2) 0.1507(19) 0.5410(14) 0.252(8) Uani 1 1 d . U .
H28A H 0.2426 0.1678 0.4937 0.378 Uiso 1 1 calc R U .
H28B H 0.3386 0.0902 0.5413 0.378 Uiso 1 1 calc R U .
H28C H 0.2057 0.1395 0.5703 0.378 Uiso 1 1 calc R U .
C12 C -0.038(2) 0.8143(16) 0.7190(12) 0.219(6) Uani 1 1 d . U .
H12A H -0.0515 0.8024 0.7684 0.328 Uiso 1 1 calc R U .
H12B H 0.0245 0.8383 0.7114 0.328 Uiso 1 1 calc R U .
H12C H -0.1097 0.8644 0.7009 0.328 Uiso 1 1 calc R U .
C29 C 0.401(2) 0.2354(19) 0.5273(13) 0.253(8) Uani 1 1 d D U .
H29A H 0.3822 0.2613 0.4802 0.380 Uiso 1 1 calc R U .
H29B H 0.4339 0.2761 0.5488 0.380 Uiso 1 1 calc R U .
H29C H 0.4587 0.1666 0.5261 0.380 Uiso 1 1 calc R U .
C10 C 0.1429(19) 0.7311(14) 0.9604(8) 0.203(3) Uani 1 1 d D U .
H10A H 0.0915 0.7946 0.9800 0.305 Uiso 1 1 d R U .
H10B H 0.2037 0.6944 0.9920 0.305 Uiso 1 1 d R U .
H10C H 0.0974 0.6919 0.9534 0.305 Uiso 1 1 d R U .
N3 N 0.267(3) 0.5491(19) 0.5030(15) 0.175(9) Uani 0.5 1 d . U P
H3A H 0.2269 0.5405 0.5402 0.210 Uiso 0.5 1 calc R U P
H3B H 0.2315 0.5758 0.4652 0.210 Uiso 0.5 1 calc R U P
C9 C 0.259(2) 0.8022(16) 0.8926(9) 0.203(3) Uani 1 1 d . U .
H9A H 0.2477 0.8487 0.9288 0.305 Uiso 1 1 calc R U .
H9B H 0.3257 0.7402 0.9019 0.305 Uiso 1 1 calc R U .
H9C H 0.2734 0.8316 0.8479 0.305 Uiso 1 1 calc R U .
C31 C 0.493(2) -0.0709(17) 0.7860(13) 0.227(7) Uani 1 1 d . U .
H31A H 0.4255 -0.0299 0.8149 0.341 Uiso 1 1 calc R U .
H31B H 0.4896 -0.1353 0.7803 0.341 Uiso 1 1 calc R U .
H31C H 0.5647 -0.0810 0.8079 0.341 Uiso 1 1 calc R U .
C15 C -0.033(2) 0.3607(18) 0.6440(13) 0.235(8) Uani 1 1 d . U .
H15A H -0.1088 0.3566 0.6443 0.352 Uiso 1 1 calc R U .
H15B H 0.0096 0.3408 0.5993 0.352 Uiso 1 1 calc R U .
H15C H 0.0121 0.3162 0.6806 0.352 Uiso 1 1 calc R U .
C6 C 0.439(2) 0.7147(18) 0.6357(13) 0.253(9) Uani 1 1 d D U .
H6A H 0.4521 0.6450 0.6469 0.379 Uiso 1 1 calc R U .
H6B H 0.4691 0.7212 0.5885 0.379 Uiso 1 1 calc R U .
H6C H 0.4783 0.7371 0.6678 0.379 Uiso 1 1 calc R U .
C34 C 0.741(2) -0.1045(13) 0.9151(12) 0.227(7) Uani 1 1 d D U .
H34A H 0.7726 -0.1212 0.9606 0.340 Uiso 1 1 calc R U .
H34B H 0.6689 -0.1161 0.9161 0.340 Uiso 1 1 calc R U .
H34C H 0.7975 -0.1464 0.8808 0.340 Uiso 1 1 calc R U .
C42 C 0.7703(16) 0.1238(15) 0.6272(11) 0.192(3) Uani 1 1 d D U .
H42 H 0.7214 0.1863 0.6020 0.230 Uiso 1 1 calc R U .
C43 C 0.818(2) 0.0291(17) 0.5882(13) 0.265(8) Uani 1 1 d D U .
H43A H 0.8463 -0.0282 0.6207 0.398 Uiso 1 1 calc R U .
H43B H 0.8819 0.0290 0.5557 0.398 Uiso 1 1 calc R U .
H43C H 0.7559 0.0249 0.5628 0.398 Uiso 1 1 calc R U .
C44 C 0.8828(16) 0.1164(13) 0.6486(10) 0.192(3) Uani 1 1 d D U .
H44A H 0.8698 0.1644 0.6841 0.288 Uiso 1 1 calc R U .
H44B H 0.9275 0.1308 0.6087 0.288 Uiso 1 1 calc R U .
H44C H 0.9262 0.0490 0.6672 0.288 Uiso 1 1 calc R U .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ti01 0.0899(9) 0.1166(10) 0.0469(6) 0.0065(5) -0.0082(5) -0.0517(8)
Ti02 0.0796(9) 0.1358(12) 0.0616(7) 0.0032(7) -0.0005(6) -0.0481(8)
Ti03 0.1114(12) 0.1220(12) 0.0856(10) 0.0076(8) -0.0218(8) -0.0636(10)
Ti04 0.1083(12) 0.1187(12) 0.0856(10) -0.0011(8) 0.0008(8) -0.0452(10)
Ti05 0.1100(13) 0.1167(12) 0.0951(11) 0.0121(9) -0.0195(9) -0.0467(10)
O10 0.080(3) 0.126(4) 0.050(2) 0.011(2) 0.003(2) -0.043(3)
O7 0.089(3) 0.132(4) 0.062(3) 0.008(3) -0.008(2) -0.055(3)
O11 0.074(3) 0.152(5) 0.056(2) 0.018(3) 0.001(2) -0.047(3)
O6 0.086(3) 0.117(4) 0.060(2) -0.001(2) 0.002(2) -0.040(3)
O8 0.104(4) 0.108(4) 0.086(3) 0.006(3) -0.020(3) -0.047(3)
O15 0.1235(19) 0.1252(19) 0.1195(19) -0.0030(10) -0.0083(10) -0.0488(11)
O5 0.109(2) 0.111(2) 0.109(2) -0.0031(10) -0.0073(10) -0.0425(11)
O12 0.1028(19) 0.1079(19) 0.1037(19) -0.0039(10) -0.0074(10) -0.0422(11)
C21 0.079(4) 0.100(4) 0.050(3) 0.002(3) -0.003(2) -0.044(3)
N1 0.105(5) 0.119(6) 0.085(4) -0.007(4) -0.008(4) -0.059(5)
C22 0.0786(18) 0.0819(18) 0.0777(18) -0.0023(10) -0.0052(10) -0.0321(11)
C23 0.078(4) 0.118(5) 0.052(3) 0.013(3) -0.009(3) -0.042(4)
O18 0.097(4) 0.187(7) 0.073(3) -0.004(4) 0.010(3) -0.066(4)
O2 0.118(5) 0.122(5) 0.138(6) 0.019(4) -0.051(4) -0.049(4)
N2 0.097(5) 0.114(5) 0.075(4) 0.012(3) -0.014(3) -0.047(4)
C20 0.083(4) 0.114(5) 0.042(3) 0.004(3) 0.002(3) -0.049(4)
O1 0.119(6) 0.124(6) 0.188(8) -0.029(5) -0.003(5) -0.058(5)
O14 0.127(6) 0.159(7) 0.191(9) 0.024(6) -0.005(6) -0.087(6)
O4 0.233(8) 0.237(7) 0.149(5) -0.055(5) 0.020(6) -0.101(6)
O9 0.125(2) 0.124(2) 0.125(2) -0.0055(10) -0.0086(10) -0.0493(12)
C1 0.105(6) 0.141(6) 0.102(5) -0.001(5) -0.023(4) -0.074(5)
O3 0.159(3) 0.159(3) 0.160(3) -0.0051(10) -0.0093(10) -0.0639(15)
O13 0.145(3) 0.144(3) 0.143(3) -0.0064(10) -0.0108(10) -0.0568(14)
C3 0.100(5) 0.143(6) 0.094(5) 0.000(5) -0.024(4) -0.064(5)
O17 0.192(3) 0.192(3) 0.192(3) -0.0075(9) -0.0115(9) -0.0763(14)
O16 0.177(3) 0.177(3) 0.176(3) -0.0059(10) -0.0122(10) -0.0700(15)
C2 0.117(8) 0.158(9) 0.200(12) -0.026(9) -0.019(8) -0.072(7)
C4 0.106(7) 0.162(9) 0.168(10) -0.005(8) -0.039(7) -0.058(7)
C17 0.142(8) 0.242(12) 0.069(5) -0.017(6) 0.015(5) -0.104(9)
C39 0.1235(19) 0.1252(19) 0.1195(19) -0.0030(10) -0.0083(10) -0.0488(11)
C14 0.216(7) 0.216(7) 0.216(7) -0.0087(10) -0.0138(11) -0.085(3)
C19 0.172(12) 0.247(15) 0.129(9) -0.058(10) 0.043(9) -0.036(11)
C24 0.229(7) 0.229(7) 0.229(7) -0.0091(11) -0.0143(11) -0.091(3)
C13 0.188(6) 0.188(6) 0.187(6) -0.007(2) -0.013(2) -0.074(3)
C7 0.257(9) 0.256(9) 0.257(9) -0.010(2) -0.016(2) -0.102(4)
C41 0.201(6) 0.198(6) 0.199(6) -0.010(2) -0.014(2) -0.080(3)
C11 0.193(5) 0.193(5) 0.193(5) -0.0073(10) -0.0122(11) -0.076(2)
C40 0.199(6) 0.198(6) 0.198(6) -0.006(2) -0.011(2) -0.078(3)
C5 0.250(8) 0.250(8) 0.250(8) -0.0096(11) -0.0156(11) -0.099(3)
C30 0.190(6) 0.189(6) 0.190(6) -0.0077(10) -0.0120(11) -0.075(2)
C18 0.243(15) 0.270(17) 0.099(8) -0.005(10) 0.005(10) -0.092(13)
C33 0.177(3) 0.177(3) 0.176(3) -0.0059(10) -0.0122(10) -0.0700(15)
C8 0.233(8) 0.237(7) 0.149(5) -0.055(5) 0.020(6) -0.101(6)
C27 0.224(7) 0.224(7) 0.224(7) -0.0094(11) -0.0143(11) -0.089(3)
C16 0.245(8) 0.246(8) 0.246(8) -0.009(2) -0.017(2) -0.097(4)
C35 0.234(8) 0.233(8) 0.233(8) -0.009(2) -0.015(2) -0.092(3)
C26 0.221(15) 0.272(16) 0.266(17) 0.015(15) 0.038(14) -0.117(13)
C32 0.227(8) 0.227(8) 0.227(8) -0.010(2) -0.014(2) -0.089(3)
C25 0.278(9) 0.279(9) 0.279(9) -0.011(2) -0.017(2) -0.110(4)
C28 0.252(9) 0.252(9) 0.252(9) -0.011(2) -0.016(2) -0.100(4)
C12 0.219(7) 0.218(7) 0.218(7) -0.009(2) -0.014(2) -0.086(3)
C29 0.254(9) 0.253(9) 0.253(9) -0.011(2) -0.016(2) -0.100(4)
C10 0.233(8) 0.237(7) 0.149(5) -0.055(5) 0.020(6) -0.101(6)
N3 0.175(9) 0.176(9) 0.175(9) -0.006(2) -0.011(2) -0.069(4)
C9 0.233(8) 0.237(7) 0.149(5) -0.055(5) 0.020(6) -0.101(6)
C31 0.227(8) 0.227(8) 0.228(8) -0.009(2) -0.015(2) -0.090(3)
C15 0.234(8) 0.235(8) 0.235(8) -0.009(2) -0.015(2) -0.093(4)
C6 0.253(9) 0.252(9) 0.253(9) -0.010(2) -0.015(2) -0.100(4)
C34 0.227(7) 0.227(7) 0.227(7) -0.008(2) -0.014(2) -0.090(3)
C42 0.192(3) 0.192(3) 0.192(3) -0.0075(9) -0.0115(9) -0.0763(14)
C43 0.265(8) 0.265(8) 0.265(8) -0.011(2) -0.016(2) -0.104(4)
C44 0.192(3) 0.192(3) 0.192(3) -0.0075(9) -0.0115(9) -0.0763(14)
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'
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
O15 Ti01 O6 96.1(3) . .
O15 Ti01 O8 94.9(3) . .
O6 Ti01 O8 146.1(3) . .
O15 Ti01 O10 167.9(3) . .
O6 Ti01 O10 89.0(2) . .
O8 Ti01 O10 86.9(2) . .
O15 Ti01 O7 103.8(3) . .
O6 Ti01 O7 74.4(2) . .
O8 Ti01 O7 71.8(3) . .
O10 Ti01 O7 88.2(2) . .
O15 Ti01 N2 86.4(3) . .
O6 Ti01 N2 141.2(3) . .
O8 Ti01 N2 71.5(3) . .
O10 Ti01 N2 82.8(2) . .
O7 Ti01 N2 142.6(3) . .
O15 Ti01 N1 91.3(3) . .
O6 Ti01 N1 73.8(3) . .
O8 Ti01 N1 137.9(3) . .
O10 Ti01 N1 79.6(2) . .
O7 Ti01 N1 146.1(3) . .
N2 Ti01 N1 67.4(3) . .
O15 Ti01 Ti02 109.4(3) . .
O6 Ti01 Ti02 38.09(17) . .
O8 Ti01 Ti02 108.09(18) . .
O10 Ti01 Ti02 81.31(15) . .
O7 Ti01 Ti02 37.45(17) . .
N2 Ti01 Ti02 164.10(18) . .
N1 Ti01 Ti02 108.9(2) . .
O15 Ti01 Ti03 100.4(2) . .
O6 Ti01 Ti03 110.04(18) . .
O8 Ti01 Ti03 36.19(18) . .
O10 Ti01 Ti03 88.04(17) . .
O7 Ti01 Ti03 35.61(17) . .
N2 Ti01 Ti03 107.5(2) . .
N1 Ti01 Ti03 167.0(2) . .
Ti02 Ti01 Ti03 72.53(6) . .
O18 Ti02 O12 94.7(3) . .
O18 Ti02 O7 97.9(3) . .
O12 Ti02 O7 106.6(3) . .
O18 Ti02 O6 96.8(3) . .
O12 Ti02 O6 167.4(3) . .
O7 Ti02 O6 77.1(2) . .
O18 Ti02 O5 93.9(3) . .
O12 Ti02 O5 101.6(3) . .
O7 Ti02 O5 148.3(3) . .
O6 Ti02 O5 72.3(3) . .
O18 Ti02 O11 176.3(3) . .
O12 Ti02 O11 85.7(3) . .
O7 Ti02 O11 85.5(2) . .
O6 Ti02 O11 82.5(2) . .
O5 Ti02 O11 82.4(3) . .
O18 Ti02 Ti01 106.6(2) . .
O12 Ti02 Ti01 142.6(2) . .
O7 Ti02 Ti01 41.34(16) . .
O6 Ti02 Ti01 36.93(17) . .
O5 Ti02 Ti01 107.0(2) . .
O11 Ti02 Ti01 74.98(15) . .
O18 Ti02 Ti04 99.9(2) . .
O12 Ti02 Ti04 137.1(2) . .
O7 Ti02 Ti04 110.94(17) . .
O6 Ti02 Ti04 34.87(17) . .
O5 Ti02 Ti04 37.7(2) . .
O11 Ti02 Ti04 77.43(18) . .
Ti01 Ti02 Ti04 69.63(5) . .
O13 Ti03 O14 112.1(5) . .
O13 Ti03 O7 104.2(3) . .
O14 Ti03 O7 100.2(4) . .
O13 Ti03 O8 123.0(4) . .
O14 Ti03 O8 123.6(4) . .
O7 Ti03 O8 78.3(3) . .
O13 Ti03 O9 94.5(4) . .
O14 Ti03 O9 94.6(4) . .
O7 Ti03 O9 149.4(3) . .
O8 Ti03 O9 71.2(3) . .
O13 Ti03 Ti01 122.2(3) . .
O14 Ti03 Ti01 117.5(4) . .
O7 Ti03 Ti01 40.81(17) . .
O8 Ti03 Ti01 37.54(19) . .
O9 Ti03 Ti01 108.7(2) . .
O13 Ti03 Ti05 111.5(3) . .
O14 Ti03 Ti05 115.9(3) . .
O7 Ti03 Ti05 111.74(18) . .
O8 Ti03 Ti05 33.43(19) . .
O9 Ti03 Ti05 37.9(2) . .
Ti01 Ti03 Ti05 70.98(6) . .
O3 Ti04 O4 107.7(6) . .
O3 Ti04 O6 141.6(4) . .
O4 Ti04 O6 110.6(5) . .
O3 Ti04 O1 91.0(5) . .
O4 Ti04 O1 97.7(6) . .
O6 Ti04 O1 81.7(3) . .
O3 Ti04 O5 94.9(4) . .
O4 Ti04 O5 107.0(5) . .
O6 Ti04 O5 76.2(3) . .
O1 Ti04 O5 151.3(3) . .
O3 Ti04 Ti02 121.7(4) . .
O4 Ti04 Ti02 117.7(5) . .
O6 Ti04 Ti02 37.11(17) . .
O1 Ti04 Ti02 115.4(2) . .
O5 Ti04 Ti02 39.4(2) . .
O16 Ti05 O17 109.1(6) . .
O16 Ti05 O8 129.2(4) . .
O17 Ti05 O8 121.7(5) . .
O16 Ti05 O2 93.1(4) . .
O17 Ti05 O2 96.1(5) . .
O8 Ti05 O2 80.4(3) . .
O16 Ti05 O9 99.7(5) . .
O17 Ti05 O9 101.3(5) . .
O8 Ti05 O9 73.5(3) . .
O2 Ti05 O9 153.6(3) . .
O16 Ti05 Ti03 123.2(4) . .
O17 Ti05 Ti03 115.2(4) . .
O8 Ti05 Ti03 34.42(19) . .
O2 Ti05 Ti03 114.9(2) . .
O9 Ti05 Ti03 39.2(2) . .
C20 O10 Ti01 127.4(5) . .
Ti03 O7 Ti02 152.1(3) . .
Ti03 O7 Ti01 103.6(3) . .
Ti02 O7 Ti01 101.2(3) . .
C20 O11 Ti02 130.4(4) . .
Ti04 O6 Ti01 138.0(3) . .
Ti04 O6 Ti02 108.0(3) . .
Ti01 O6 Ti02 105.0(3) . .
Ti05 O8 Ti03 112.1(3) . .
Ti05 O8 Ti01 141.6(3) . .
Ti03 O8 Ti01 106.3(3) . .
C39 O15 Ti01 155.2(8) . .
C11 O5 Ti04 131.6(9) . .
C11 O5 Ti02 125.5(9) . .
Ti04 O5 Ti02 102.9(3) . .
C14 O12 Ti02 135.6(12) . .
C22 C21 C23 119.5(6) . 2_666
C22 C21 C20 121.4(7) . .
C23 C21 C20 119.1(6) 2_666 .
C1 N1 O1 117.1(8) . .
C1 N1 Ti01 121.7(7) . .
O1 N1 Ti01 120.6(6) . .
N3 C22 C21 124.2(15) . .
N3 C22 C23 115.5(15) . .
C21 C22 C23 120.2(7) . .
C22 C23 C21 120.2(7) . 2_666
C22 C23 H23 119.9 . .
C21 C23 H23 119.9 2_666 .
C17 O18 Ti02 137.0(7) . .
N2 O2 Ti05 122.2(5) . .
C3 N2 O2 115.2(8) . .
C3 N2 Ti01 122.4(7) . .
O2 N2 Ti01 122.0(6) . .
O10 C20 O11 125.5(6) . .
O10 C20 C21 117.4(6) . .
O11 C20 C21 117.1(6) . .
N1 O1 Ti04 124.0(6) . .
C24 O14 Ti03 151.6(13) . .
C8 O4 Ti04 153.5(14) . .
C30 O9 Ti05 132.1(10) . .
C30 O9 Ti03 125.0(10) . .
Ti05 O9 Ti03 102.9(3) . .
N1 C1 C3 114.7(8) . .
N1 C1 C2 123.2(11) . .
C3 C1 C2 122.1(10) . .
C5 O3 Ti04 157.6(12) . .
C27 O13 Ti03 153.9(12) . .
N2 C3 C1 113.5(8) . .
N2 C3 C4 124.8(11) . .
C1 C3 C4 121.6(9) . .
C42 O17 Ti05 147.5(12) . .
C33 O16 Ti05 155.2(11) . .
C1 C2 H2A 109.5 . .
C1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
C1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
C3 C4 H4A 109.5 . .
C3 C4 H4B 109.5 . .
H4A C4 H4B 109.5 . .
C3 C4 H4C 109.5 . .
H4A C4 H4C 109.5 . .
H4B C4 H4C 109.5 . .
O18 C17 C19 109.4(12) . .
O18 C17 C18 105.3(12) . .
C19 C17 C18 113.5(14) . .
O18 C17 H17 109.5 . .
C19 C17 H17 109.5 . .
C18 C17 H17 109.5 . .
C41 C39 C40 124.8(16) . .
C41 C39 O15 113.0(13) . .
C40 C39 O15 112.9(13) . .
C41 C39 H39 100.2 . .
C40 C39 H39 100.2 . .
O15 C39 H39 100.2 . .
O12 C14 C15 110(2) . .
O12 C14 C16 109(2) . .
C15 C14 C16 106(2) . .
O12 C14 H14 110.8 . .
C15 C14 H14 110.8 . .
C16 C14 H14 110.8 . .
C17 C19 H19A 109.5 . .
C17 C19 H19B 109.5 . .
H19A C19 H19B 109.5 . .
C17 C19 H19C 109.5 . .
H19A C19 H19C 109.5 . .
H19B C19 H19C 109.5 . .
O14 C24 C25 112(2) . .
O14 C24 C26 111(2) . .
C25 C24 C26 105(2) . .
O14 C24 H24 109.6 . .
C25 C24 H24 109.6 . .
C26 C24 H24 109.6 . .
C11 C13 H13A 109.5 . .
C11 C13 H13B 109.5 . .
H13A C13 H13B 109.5 . .
C11 C13 H13C 109.5 . .
H13A C13 H13C 109.5 . .
H13B C13 H13C 109.5 . .
C5 C7 H7A 109.5 . .
C5 C7 H7B 109.5 . .
H7A C7 H7B 109.5 . .
C5 C7 H7C 109.5 . .
H7A C7 H7C 109.5 . .
H7B C7 H7C 109.5 . .
C39 C41 H41A 101.2 . .
C39 C41 H41B 119.7 . .
H41A C41 H41B 109.5 . .
C39 C41 H41C 107.1 . .
H41A C41 H41C 109.5 . .
H41B C41 H41C 109.5 . .
C13 C11 O5 112.6(17) . .
C13 C11 C12 114.0(18) . .
O5 C11 C12 106.3(16) . .
C13 C11 H11 107.9 . .
O5 C11 H11 107.9 . .
C12 C11 H11 107.9 . .
C39 C40 H40A 109.5 . .
C39 C40 H40B 109.5 . .
H40A C40 H40B 109.5 . .
C39 C40 H40C 109.5 . .
H40A C40 H40C 109.5 . .
H40B C40 H40C 109.5 . .
C7 C5 O3 115(2) . .
C7 C5 C6 125(3) . .
O3 C5 C6 110(2) . .
C7 C5 H5 100.4 . .
O3 C5 H5 100.4 . .
C6 C5 H5 100.4 . .
C31 C30 C32 127(2) . .
C31 C30 O9 106.2(18) . .
C32 C30 O9 105.5(17) . .
C31 C30 H30 105.5 . .
C32 C30 H30 105.5 . .
O9 C30 H30 105.5 . .
C17 C18 H18A 109.5 . .
C17 C18 H18B 109.5 . .
H18A C18 H18B 109.5 . .
C17 C18 H18C 109.5 . .
H18A C18 H18C 109.5 . .
H18B C18 H18C 109.5 . .
O16 C33 C35 122.9(17) . .
O16 C33 C34 113.6(16) . .
C35 C33 C34 113.0(18) . .
O16 C33 H33 100.9 . .
C35 C33 H33 100.9 . .
C34 C33 H33 100.9 . .
O4 C8 C9 111.7(17) . .
O4 C8 C10 107.8(16) . .
C9 C8 C10 105.4(18) . .
O4 C8 H8 110.6 . .
C9 C8 H8 110.6 . .
C10 C8 H8 110.6 . .
O13 C27 C29 107(2) . .
O13 C27 C28 101.0(19) . .
C29 C27 C28 103(2) . .
O13 C27 H27 114.8 . .
C29 C27 H27 114.8 . .
C28 C27 H27 114.8 . .
C14 C16 H16A 109.5 . .
C14 C16 H16B 109.5 . .
H16A C16 H16B 109.5 . .
C14 C16 H16C 109.5 . .
H16A C16 H16C 109.5 . .
H16B C16 H16C 109.5 . .
C33 C35 H35A 109.5 . .
C33 C35 H35B 109.5 . .
H35A C35 H35B 109.5 . .
C33 C35 H35C 109.5 . .
H35A C35 H35C 109.5 . .
H35B C35 H35C 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 . .
C30 C32 H32A 109.5 . .
C30 C32 H32B 109.5 . .
H32A C32 H32B 109.5 . .
C30 C32 H32C 109.5 . .
H32A C32 H32C 109.5 . .
H32B C32 H32C 109.5 . .
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 . .
C27 C28 H28A 109.5 . .
C27 C28 H28B 109.5 . .
H28A C28 H28B 109.5 . .
C27 C28 H28C 109.5 . .
H28A C28 H28C 109.5 . .
H28B C28 H28C 109.5 . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
C11 C12 H12C 109.5 . .
H12A C12 H12C 109.5 . .
H12B C12 H12C 109.5 . .
C27 C29 H29A 109.5 . .
C27 C29 H29B 109.5 . .
H29A C29 H29B 109.5 . .
C27 C29 H29C 109.5 . .
H29A C29 H29C 109.5 . .
H29B C29 H29C 109.5 . .
C8 C10 H10A 91.8 . .
C8 C10 H10B 128.8 . .
H10A C10 H10B 109.5 . .
C8 C10 H10C 105.9 . .
H10A C10 H10C 109.5 . .
H10B C10 H10C 109.5 . .
C22 N3 H3A 120.0 . .
C22 N3 H3B 120.0 . .
H3A N3 H3B 120.0 . .
C8 C9 H9A 109.5 . .
C8 C9 H9B 109.5 . .
H9A C9 H9B 109.5 . .
C8 C9 H9C 109.5 . .
H9A C9 H9C 109.5 . .
H9B C9 H9C 109.5 . .
C30 C31 H31A 109.5 . .
C30 C31 H31B 109.5 . .
H31A C31 H31B 109.5 . .
C30 C31 H31C 109.5 . .
H31A C31 H31C 109.5 . .
H31B C31 H31C 109.5 . .
C14 C15 H15A 109.5 . .
C14 C15 H15B 109.5 . .
H15A C15 H15B 109.5 . .
C14 C15 H15C 109.5 . .
H15A C15 H15C 109.5 . .
H15B C15 H15C 109.5 . .
C5 C6 H6A 109.5 . .
C5 C6 H6B 109.5 . .
H6A C6 H6B 109.5 . .
C5 C6 H6C 109.5 . .
H6A C6 H6C 109.5 . .
H6B C6 H6C 109.5 . .
C33 C34 H34A 109.5 . .
C33 C34 H34B 109.5 . .
H34A C34 H34B 109.5 . .
C33 C34 H34C 109.5 . .
H34A C34 H34C 109.5 . .
H34B C34 H34C 109.5 . .
C44 C42 O17 105.9(17) . .
C44 C42 C43 96.2(12) . .
O17 C42 C43 98.7(18) . .
C44 C42 H42 117.5 . .
O17 C42 H42 117.5 . .
C43 C42 H42 117.5 . .
C42 C43 H43A 109.5 . .
C42 C43 H43B 109.5 . .
H43A C43 H43B 109.5 . .
C42 C43 H43C 109.5 . .
H43A C43 H43C 109.5 . .
H43B C43 H43C 109.5 . .
C42 C44 H44A 109.5 . .
C42 C44 H44B 109.5 . .
H44A C44 H44B 109.5 . .
C42 C44 H44C 109.5 . .
H44A C44 H44C 109.5 . .
H44B C44 H44C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ti01 O15 1.774(8) .
Ti01 O6 1.940(6) .
Ti01 O8 1.983(6) .
Ti01 O10 2.080(4) .
Ti01 O7 2.100(5) .
Ti01 N2 2.262(8) .
Ti01 N1 2.270(8) .
Ti01 Ti02 3.119(2) .
Ti01 Ti03 3.124(2) .
Ti02 O18 1.798(6) .
Ti02 O12 1.812(7) .
Ti02 O7 1.933(6) .
Ti02 O6 1.992(6) .
Ti02 O5 2.043(7) .
Ti02 O11 2.194(5) .
Ti02 Ti04 3.139(3) .
Ti03 O13 1.747(10) .
Ti03 O14 1.771(8) .
Ti03 O7 1.871(6) .
Ti03 O8 1.921(6) .
Ti03 O9 2.042(8) .
Ti03 Ti05 3.149(3) .
Ti04 O3 1.731(11) .
Ti04 O4 1.760(11) .
Ti04 O6 1.887(6) .
Ti04 O1 1.956(9) .
Ti04 O5 1.969(7) .
Ti05 O16 1.759(12) .
Ti05 O17 1.771(14) .
Ti05 O8 1.873(7) .
Ti05 O2 1.966(8) .
Ti05 O9 1.985(8) .
O10 C20 1.253(8) .
O11 C20 1.264(9) .
O15 C39 1.386(13) .
O5 C11 1.50(2) .
O12 C14 1.38(2) .
C21 C22 1.371(10) .
C21 C23 1.398(10) 2_666
C21 C20 1.495(9) .
N1 C1 1.286(12) .
N1 O1 1.306(11) .
C22 N3 1.28(3) .
C22 C23 1.386(10) .
C23 C21 1.398(10) 2_666
C23 H23 0.9300 .
O18 C17 1.403(11) .
O2 N2 1.338(10) .
N2 C3 1.290(12) .
O14 C24 1.37(3) .
O4 C8 1.365(19) .
O9 C30 1.473(19) .
C1 C3 1.458(15) .
C1 C2 1.516(15) .
O3 C5 1.48(3) .
O13 C27 1.46(2) .
C3 C4 1.490(14) .
O17 C42 1.47(2) .
O16 C33 1.331(19) .
C2 H2A 0.9600 .
C2 H2B 0.9600 .
C2 H2C 0.9600 .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C17 C19 1.45(2) .
C17 C18 1.55(2) .
C17 H17 0.9800 .
C39 C41 1.339(19) .
C39 C40 1.38(2) .
C39 H39 0.9800 .
C14 C15 1.43(3) .
C14 C16 1.47(3) .
C14 H14 0.9800 .
C19 H19A 0.9600 .
C19 H19B 0.9600 .
C19 H19C 0.9600 .
C24 C25 1.492(10) .
C24 C26 1.50(3) .
C24 H24 0.9800 .
C13 C11 1.45(2) .
C13 H13A 0.9600 .
C13 H13B 0.9600 .
C13 H13C 0.9600 .
C7 C5 1.410(17) .
C7 H7A 0.9600 .
C7 H7B 0.9600 .
C7 H7C 0.9600 .
C41 H41A 0.9599 .
C41 H41B 0.9599 .
C41 H41C 0.9607 .
C11 C12 1.57(2) .
C11 H11 0.9800 .
C40 H40A 0.9600 .
C40 H40B 0.9600 .
C40 H40C 0.9600 .
C5 C6 1.505(10) .
C5 H5 0.9800 .
C30 C31 1.35(2) .
C30 C32 1.43(2) .
C30 H30 0.9800 .
C18 H18A 0.9600 .
C18 H18B 0.9600 .
C18 H18C 0.9600 .
C33 C35 1.504(10) .
C33 C34 1.514(9) .
C33 H33 0.9800 .
C8 C9 1.44(3) .
C8 C10 1.483(9) .
C8 H8 0.9800 .
C27 C29 1.508(10) .
C27 C28 1.55(3) .
C27 H27 0.9800 .
C16 H16A 0.9600 .
C16 H16B 0.9600 .
C16 H16C 0.9600 .
C35 H35A 0.9600 .
C35 H35B 0.9600 .
C35 H35C 0.9600 .
C26 H26A 0.9600 .
C26 H26B 0.9600 .
C26 H26C 0.9600 .
C32 H32A 0.9600 .
C32 H32B 0.9600 .
C32 H32C 0.9600 .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
C28 H28A 0.9600 .
C28 H28B 0.9600 .
C28 H28C 0.9600 .
C12 H12A 0.9600 .
C12 H12B 0.9600 .
C12 H12C 0.9600 .
C29 H29A 0.9600 .
C29 H29B 0.9600 .
C29 H29C 0.9600 .
C10 H10A 0.9600 .
C10 H10B 0.9599 .
C10 H10C 0.9604 .
N3 H3A 0.8600 .
N3 H3B 0.8600 .
C9 H9A 0.9600 .
C9 H9B 0.9600 .
C9 H9C 0.9600 .
C31 H31A 0.9600 .
C31 H31B 0.9600 .
C31 H31C 0.9600 .
C15 H15A 0.9600 .
C15 H15B 0.9600 .
C15 H15C 0.9600 .
C6 H6A 0.9600 .
C6 H6B 0.9600 .
C6 H6C 0.9600 .
C34 H34A 0.9600 .
C34 H34B 0.9600 .
C34 H34C 0.9600 .
C42 C44 1.437(12) .
C42 C43 1.479(16) .
C42 H42 0.9800 .
C43 H43A 0.9600 .
C43 H43B 0.9600 .
C43 H43C 0.9600 .
C44 H44A 0.9600 .
C44 H44B 0.9600 .
C44 H44C 0.9600 .