#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:50:16 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551221.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_1551221
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 'C86 H174 N4 O38 S2 Ti10'
_chemical_formula_sum 'C86 H174 N4 O38 S2 Ti10'
_chemical_formula_weight 2415.10
_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 63.957(4)
_cell_angle_beta 78.283(3)
_cell_angle_gamma 82.357(3)
_cell_formula_units_Z 2
_cell_length_a 13.1346(4)
_cell_length_b 23.0388(10)
_cell_length_c 24.0200(11)
_cell_measurement_reflns_used 9133
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 25.3890
_cell_measurement_theta_min 3.7320
_cell_volume 6386.5(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 16.2083
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type 'Xcalibur, Eos'
_diffrn_measurement_method '\w scans'
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_reflns_av_R_equivalents 0.0434
_diffrn_reflns_av_unetI/netI 0.1062
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max 15
_diffrn_reflns_limit_h_min -15
_diffrn_reflns_limit_k_max 24
_diffrn_reflns_limit_k_min -27
_diffrn_reflns_limit_l_max 28
_diffrn_reflns_limit_l_min -28
_diffrn_reflns_number 43304
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 25.350
_diffrn_reflns_theta_min 3.401
_diffrn_source 'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu 0.691
_exptl_absorpt_correction_T_max 1.00000
_exptl_absorpt_correction_T_min 0.74479
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46c (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.252
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 2534
_exptl_crystal_size_max 0.3
_exptl_crystal_size_mid 0.3
_exptl_crystal_size_min 0.1
_refine_diff_density_max 1.317
_refine_diff_density_min -1.117
_refine_diff_density_rms 0.123
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.174
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 1287
_refine_ls_number_reflns 22977
_refine_ls_number_restraints 1317
_refine_ls_restrained_S_all 1.198
_refine_ls_R_factor_all 0.2051
_refine_ls_R_factor_gt 0.1219
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.3269
_refine_ls_wR_factor_ref 0.4041
_reflns_Friedel_coverage 0.000
_reflns_number_gt 10792
_reflns_number_total 22977
_reflns_threshold_expression 'I > 2\s(I)'
_cod_data_source_file c9dt02032b2.cif
_cod_data_source_block ccc
_cod_depositor_comments
'Adding full bibliography for 1551215--1551222.cif.'
_cod_database_code 1551221
_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 ccc_a.res in P-1
REM Old TITL ccc in P-1
REM SHELXT solution in P-1
REM R1 0.280, Rweak 0.023, Alpha 0.075, Orientation as input
REM Formula found by SHELXT: C63 N13 O36 Ti9 S3
CELL 0.71073 13.1346 23.0388 24.02 63.957 78.283 82.357
ZERR 2 0.0004 0.001 0.0011 0.004 0.003 0.003
LATT 1
SFAC C H N O S Ti
UNIT 172 334 8 76 4 20
DFIX 1.5 0.001 C81 C82
DFIX 1.5 0.001 C23 C24
DFIX 1.5 0.01 C80 C81
DFIX 1.5 0.01 C57 C58
DFIX 1.5 0.01 C69 C70
DFIX 1.5 0.01 C11 C12
DFIX 1.5 0.01 C66 C67
DFIX 1.5 0.01 C11 C13
DFIX 1.5 0.01 C32 C33
SIMU 0.005 0.01 3.8 C1 C44 C47 C2 C38 C43 C39 C45 C46 C50 C42 C40 C41 C49 =
C48 C4 C3 C51 C60 C35 C53 C61 C62 C8 C32 C52 C36 C57 C77 C22 C17 C26 C29 =
C37 C9 C55 C85 C63 C20 C28 C5 C10 C78 C71 C14 C83 C23 C27 C7 C64 C33 C16 =
C79 C13 C21 C34 C19 C65 C15 C18 C30 C59 C6 C84 C81 C68 C73 C75 C56 C69 C74 =
C54 C70 C67 C58 C80 C31 C76 C25 C66 C24 C72 C86 C82 C11
SIMU 0.01 0.02 3.8 O19 Ti1 C54
SIMU 0.01 0.02 3.8 O27 Ti3 C69
SIMU 0.01 0.02 3.8 O39 Ti8 C23
ISOR 0.001 0.002 C1 C44 C47 C2 C38 C43 C39 C45 C46 C50 C42 C40 C41 C49 C48 =
C4 C3 C51 C60 C35 C53 C61 C62 C8 C32 C52 C36 C57 C77 C22 C17 C26 C29 C37 C9 =
C55 C85 C63 C20 C28 C5 C10 C78 C71 C14 C83 C23 C27 C7 C64 C33 C16 C79 C13 =
C21 C34 C19 C65 C15 C18 C30 C59 C6 C84 C81 C68 C73 C75 C56 C69 C74 C54 C70 =
C67 C58 C80 C31 C76 C25 C66 C24 C72 C86 C82
ISOR 0.001 0.002 O31
EADP O23 C66
L.S. 20
PLAN 20
list 4
fmap 2
acta
OMIT 0 4 4
OMIT 0 -4 2
OMIT 1 0 4
OMIT -3 1 0
OMIT 2 -1 5
OMIT 1 5 3
OMIT 3 1 1
OMIT -1 1 5
OMIT 3 4 7
OMIT 6 3 3
OMIT -2 3 1
OMIT 2 5 4
OMIT 1 -1 3
OMIT -1 -3 3
OMIT 0 5 2
OMIT 1 8 8
OMIT 1 -5 1
OMIT -2 4 1
OMIT -1 4 1
OMIT 2 2 5
OMIT -2 -3 3
OMIT 0 -1 5
OMIT -3 5 0
OMIT -3 5 7
OMIT 1 9 6
OMIT -2 6 3
OMIT 2 -5 5
OMIT 3 4 11
OMIT -4 -7 1
OMIT 3 6 3
OMIT 3 11 5
OMIT 4 -5 5
OMIT 4 6 1
OMIT -2 -3 4
OMIT -3 2 2
OMIT 1 -6 5
OMIT -3 1 1
OMIT -3 8 2
OMIT -1 -2 8
OMIT -1 -7 5
OMIT -2 -2 3
OMIT 4 0 0
REM
REM
REM
WGHT 0.200000
FVAR 0.29617
TI8 6 0.678310 0.679745 0.513481 11.00000 0.06076 0.05893 =
0.05306 -0.03386 0.00379 -0.00814
TI3 6 -0.179372 0.820901 0.935095 11.00000 0.05366 0.06177 =
0.06441 -0.02967 -0.00184 -0.00808
TI1 6 -0.244016 0.657650 1.042596 11.00000 0.05542 0.07246 =
0.05490 -0.02500 0.00247 -0.01842
TI2 6 -0.034402 0.721115 1.025008 11.00000 0.05877 0.07723 =
0.05442 -0.02991 -0.00728 -0.01563
TI9 6 0.728641 0.685801 0.632311 11.00000 0.05777 0.08938 =
0.07022 -0.05163 -0.00476 -0.00716
TI7 6 0.584178 0.812346 0.512626 11.00000 0.09135 0.06430 =
0.07014 -0.04165 -0.00607 0.00098
TI6 6 0.520687 0.795598 0.401227 11.00000 0.08483 0.06671 =
0.06645 -0.03283 -0.01127 0.00161
TI10 6 0.775276 0.544339 0.641385 11.00000 0.05208 0.07580 =
0.07246 -0.03551 -0.00733 0.00221
TI4 6 0.042104 0.877824 0.892620 11.00000 0.06945 0.07993 =
0.08105 -0.02785 -0.00098 -0.02738
S1 5 0.510545 0.575979 0.623075 11.00000 0.04445 0.06607 =
0.06066 -0.03461 0.00379 -0.00528
S2 5 -0.155432 0.708708 0.881542 11.00000 0.04693 0.07464 =
0.05471 -0.03532 0.00279 -0.00684
TI5 6 -0.109688 0.971487 0.801385 11.00000 0.09746 0.06721 =
0.09487 -0.01391 -0.01155 -0.01848
O17 4 0.538570 0.639536 0.570507 11.00000 0.05307 0.06099 =
0.05086 -0.02819 0.00147 -0.00552
O21 4 -0.173714 0.738678 1.006750 11.00000 0.05094 0.06009 =
0.04945 -0.02455 0.00261 -0.01071
O33 4 -0.162897 0.660137 0.945621 11.00000 0.06075 0.06912 =
0.05436 -0.02934 0.00711 -0.01277
O32 4 -0.128936 0.770825 0.876927 11.00000 0.05877 0.06839 =
0.04616 -0.02337 0.00597 -0.00385
O15 4 0.589422 0.550035 0.663087 11.00000 0.04792 0.06691 =
0.06489 -0.01789 -0.00151 -0.00051
O9 4 0.745645 0.634310 0.586009 11.00000 0.04683 0.06879 =
0.05384 -0.03461 0.00907 -0.00633
O24 4 -0.025721 0.805735 0.957973 11.00000 0.06395 0.08091 =
0.06864 -0.03233 -0.00334 -0.02436
O8 4 0.666896 0.740916 0.560341 11.00000 0.07778 0.07389 =
0.07467 -0.04626 -0.00496 0.00165
O16 4 0.479947 0.532800 0.601311 11.00000 0.06334 0.08801 =
0.10112 -0.06263 0.01133 -0.01695
O5 4 0.589354 0.756908 0.472769 11.00000 0.08859 0.05846 =
0.05551 -0.03632 -0.00498 0.00255
O12 4 0.749691 0.531001 0.569998 11.00000 0.06730 0.06962 =
0.08255 -0.04598 -0.00855 0.01167
O25 4 -0.350890 0.714707 0.993739 11.00000 0.04930 0.07881 =
0.06220 -0.02485 0.00166 -0.01121
O20 4 -0.097683 0.634421 1.060989 11.00000 0.06533 0.07231 =
0.06249 -0.02060 -0.01211 -0.00832
O18 4 -0.294703 0.586409 1.051207 11.00000 0.07620 0.07768 =
0.07164 -0.03173 -0.00412 -0.02564
O34 4 -0.240368 0.715803 0.850019 11.00000 0.04806 0.14882 =
0.08338 -0.07294 -0.01346 -0.00012
O11 4 0.581346 0.717204 0.391630 11.00000 0.10631 0.07762 =
0.06950 -0.04577 -0.02073 -0.00062
O10 4 0.757977 0.592910 0.694406 11.00000 0.06311 0.11815 =
0.05928 -0.04814 -0.01403 0.00206
N2 3 0.710610 0.578213 0.520903 11.00000 0.05431 0.05304 =
0.05984 -0.02601 0.00025 0.00137
O28 4 -0.094656 0.890876 0.871631 11.00000 0.07393 0.07274 =
0.09185 -0.02860 -0.01535 -0.01352
O2 4 0.519184 0.862314 0.432665 11.00000 0.09555 0.06298 =
0.09047 -0.04210 -0.02431 0.01451
O39 4 0.792631 0.707252 0.457736 11.00000 0.08249 0.08526 =
0.07084 -0.04357 0.01077 -0.02311
O27 4 -0.243526 0.864625 0.976722 11.00000 0.09088 0.08083 =
0.08371 -0.05151 0.00199 -0.00631
O14 4 0.760444 0.461575 0.695645 11.00000 0.06658 0.06875 =
0.07984 -0.01152 -0.01338 -0.00981
N1 3 0.616508 0.667455 0.438600 11.00000 0.07427 0.05158 =
0.04818 -0.02133 -0.00421 -0.00501
O13 4 0.913608 0.542868 0.625352 11.00000 0.05304 0.10975 =
0.11854 -0.06549 -0.00926 0.01467
O19 4 -0.303436 0.656842 1.115932 11.00000 0.08161 0.11785 =
0.06141 -0.03435 0.01180 -0.02963
N3 3 -0.328150 0.774598 0.948305 11.00000 0.04973 0.06090 =
0.07325 -0.03890 0.00562 -0.00354
O36 4 0.637720 0.702167 0.691086 11.00000 0.08456 0.12694 =
0.08358 -0.07797 -0.01314 0.02264
O29 4 0.031269 0.967845 0.820289 11.00000 0.11360 0.07512 =
0.09843 -0.01164 0.00523 -0.05167
O22 4 0.090441 0.689395 1.002197 11.00000 0.05501 0.09039 =
0.09413 -0.02432 -0.00853 -0.00656
O23 4 -0.028337 0.732386 1.091771 11.00000 0.13919 0.13974 =
0.13775 -0.06033 -0.02403 -0.00895
O37 4 0.844040 0.723429 0.621181 11.00000 0.09281 0.10951 =
0.08297 -0.04070 -0.00361 -0.03331
O26 4 -0.250640 0.939975 0.816738 11.00000 0.08540 0.07797 =
0.11330 -0.00839 -0.02664 -0.00958
O38 4 0.141561 0.844849 0.853858 11.00000 0.08496 0.10564 =
0.10441 -0.03039 0.02055 -0.02858
N4 3 -0.278011 0.882236 0.861194 11.00000 0.05656 0.06555 =
0.08409 -0.02736 -0.01026 -0.00610
C1 1 0.629197 0.612363 0.434324 11.00000 0.06707 0.06642 =
0.06685 -0.02915 -0.01006 -0.00349
O1 4 0.557980 0.843873 0.320639 11.00000 0.16508 0.07577 =
0.05497 -0.02759 -0.01147 0.01350
C44 1 0.132596 0.648772 0.773824 11.00000 0.06623 0.06617 =
0.06579 -0.02871 -0.01032 -0.00322
C47 1 -0.043648 0.685184 0.839671 11.00000 0.06397 0.06520 =
0.06425 -0.02787 -0.01088 -0.00321
O7 4 0.476192 0.817623 0.566149 11.00000 0.11189 0.13151 =
0.09898 -0.06838 -0.01044 0.03442
C2 1 0.674565 0.561205 0.484853 11.00000 0.06494 0.06440 =
0.06488 -0.02844 -0.00961 -0.00338
C38 1 0.397946 0.594903 0.669984 11.00000 0.06328 0.06363 =
0.06358 -0.02769 -0.01008 -0.00335
C43 1 0.226580 0.628801 0.738414 11.00000 0.06512 0.06586 =
0.06536 -0.02827 -0.01065 -0.00336
C39 1 0.300951 0.585202 0.664118 11.00000 0.06527 0.06593 =
0.06562 -0.02874 -0.00983 -0.00337
AFIX 43
H39 2 0.293286 0.567624 0.637065 11.00000 -1.20000
AFIX 0
C45 1 0.128019 0.640214 0.833345 11.00000 0.06694 0.06799 =
0.06689 -0.02890 -0.01077 -0.00231
AFIX 43
H45 2 0.185932 0.621123 0.852778 11.00000 -1.20000
AFIX 0
O3 4 0.391823 0.779617 0.415984 11.00000 0.10204 0.11085 =
0.15908 -0.07135 -0.02170 -0.02506
C46 1 0.041727 0.658276 0.867358 11.00000 0.07203 0.07300 =
0.07172 -0.03072 -0.01150 -0.00323
AFIX 43
H46 2 0.042364 0.652083 0.908244 11.00000 -1.20000
AFIX 0
O6 4 0.667833 0.875390 0.491725 11.00000 0.15465 0.07619 =
0.15007 -0.05691 -0.04775 -0.01449
C50 1 -0.396191 0.803493 0.910930 11.00000 0.07520 0.07626 =
0.07590 -0.03274 -0.01259 -0.00374
C42 1 0.324616 0.634862 0.744358 11.00000 0.06615 0.06668 =
0.06575 -0.02875 -0.01057 -0.00304
AFIX 43
H42 2 0.333246 0.650252 0.772915 11.00000 -1.20000
AFIX 0
C40 1 0.216923 0.601285 0.697761 11.00000 0.06612 0.06712 =
0.06694 -0.02849 -0.01028 -0.00343
AFIX 43
H40 2 0.150997 0.594135 0.694186 11.00000 -1.20000
AFIX 0
C41 1 0.411213 0.619350 0.710238 11.00000 0.06996 0.07087 =
0.07034 -0.03051 -0.01137 -0.00352
AFIX 43
H41 2 0.477471 0.625313 0.714367 11.00000 -1.20000
AFIX 0
C49 1 0.041614 0.672148 0.748486 11.00000 0.06837 0.06953 =
0.06810 -0.02897 -0.01069 -0.00268
AFIX 43
H49 2 0.037648 0.673162 0.709848 11.00000 -1.20000
AFIX 0
C48 1 -0.042881 0.693867 0.779934 11.00000 0.06890 0.07008 =
0.06842 -0.02925 -0.01092 -0.00255
AFIX 43
H48 2 -0.099828 0.714634 0.760092 11.00000 -1.20000
AFIX 0
O35 4 0.096384 0.905997 0.936328 11.00000 0.17642 0.12979 =
0.11973 -0.03295 -0.05213 -0.08037
C4 1 0.603580 0.606514 0.380878 11.00000 0.07918 0.07603 =
0.07690 -0.03396 -0.01231 -0.00373
AFIX 3
H4A 2 0.530930 0.598614 0.388928 11.00000 -1.50000
H4B 2 0.617890 0.645744 0.343528 11.00000 -1.50000
H4C 2 0.644210 0.571044 0.375228 11.00000 -1.50000
AFIX 0
C3 1 0.676654 0.491508 0.494889 11.00000 0.07986 0.07558 =
0.07878 -0.03551 -0.00892 -0.00221
AFIX 137
H3A 2 0.745913 0.472517 0.499049 11.00000 -1.50000
H3B 2 0.655758 0.489830 0.459596 11.00000 -1.50000
H3C 2 0.629618 0.467946 0.532391 11.00000 -1.50000
AFIX 0
C51 1 -0.368326 0.864893 0.863861 11.00000 0.08204 0.08199 =
0.08226 -0.03486 -0.01346 -0.00363
C60 1 -0.047469 0.573213 1.095925 11.00000 0.08152 0.08184 =
0.08159 -0.03438 -0.01360 -0.00389
AFIX 13
H60 2 0.017531 0.581306 1.104807 11.00000 -1.20000
AFIX 0
O30 4 -0.077984 0.978221 0.723301 11.00000 0.15720 0.23396 =
0.08778 -0.03928 0.00318 -0.08391
C35 1 0.763598 0.572328 0.758548 11.00000 0.11209 0.11279 =
0.11203 -0.04772 -0.01902 -0.00572
AFIX 13
H35 2 0.761902 0.611294 0.765548 11.00000 -1.20000
AFIX 0
C53 1 -0.493823 0.771378 0.918867 11.00000 0.08741 0.09112 =
0.09153 -0.03708 -0.01644 -0.00689
AFIX 137
H53A 2 -0.477978 0.739992 0.901746 11.00000 -1.50000
H53B 2 -0.544016 0.803361 0.897215 11.00000 -1.50000
H53C 2 -0.521856 0.750260 0.962710 11.00000 -1.50000
AFIX 0
O31 4 -0.154751 1.046354 0.800178 11.00000 0.14286 0.14177 =
0.14413 -0.06031 -0.02302 -0.00736
C61 1 -0.113781 0.534663 1.157026 11.00000 0.09699 0.09684 =
0.09574 -0.03964 -0.01601 -0.00348
AFIX 137
H61A 2 -0.139742 0.561547 1.178580 11.00000 -1.50000
H61B 2 -0.072908 0.498597 1.182513 11.00000 -1.50000
H61C 2 -0.171197 0.519139 1.149147 11.00000 -1.50000
AFIX 0
C62 1 -0.021308 0.537729 1.055100 11.00000 0.10221 0.10147 =
0.10249 -0.04121 -0.01519 -0.00294
AFIX 137
H62A 2 -0.080606 0.515140 1.058999 11.00000 -1.50000
H62B 2 0.036174 0.507256 1.067956 11.00000 -1.50000
H62C 2 -0.002715 0.568031 1.012160 11.00000 -1.50000
AFIX 0
C8 1 0.482861 0.930378 0.405685 11.00000 0.11076 0.11013 =
0.11056 -0.04743 -0.01750 -0.00509
AFIX 13
H8 2 0.472186 0.943442 0.440248 11.00000 -1.20000
AFIX 0
C32 1 0.708045 0.406720 0.720569 11.00000 0.14592 0.14626 =
0.14603 -0.06211 -0.02420 -0.00724
AFIX 13
H32 2 0.643371 0.415734 0.744738 11.00000 -1.20000
AFIX 0
C52 1 -0.437073 0.908057 0.815581 11.00000 0.09648 0.09883 =
0.09854 -0.03863 -0.01768 -0.00372
AFIX 3
H52A 2 -0.495693 0.924027 0.836951 11.00000 -1.50000
H52B 2 -0.460993 0.883247 0.797871 11.00000 -1.50000
H52C 2 -0.399833 0.943817 0.782671 11.00000 -1.50000
AFIX 0
C36 1 0.861918 0.536137 0.774504 11.00000 0.12551 0.12838 =
0.12560 -0.05303 -0.02177 -0.00563
AFIX 137
H36A 2 0.868754 0.499290 0.765029 11.00000 -1.50000
H36B 2 0.862584 0.521861 0.818472 11.00000 -1.50000
H36C 2 0.918881 0.563532 0.750474 11.00000 -1.50000
AFIX 0
C57 1 -0.326862 0.545785 1.027603 11.00000 0.16831 0.16888 =
0.16889 -0.07154 -0.02792 -0.00900
AFIX 13
H57 2 -0.261938 0.528583 1.010672 11.00000 -1.20000
AFIX 0
C77 1 0.111545 1.016462 0.793998 11.00000 0.16493 0.16474 =
0.16502 -0.07006 -0.02678 -0.00872
AFIX 13
H77 2 0.173873 0.992358 0.810957 11.00000 -1.20000
AFIX 0
C22 1 0.544797 0.692221 0.790595 11.00000 0.13450 0.13523 =
0.13360 -0.05776 -0.01962 -0.00665
AFIX 137
H22A 2 0.492502 0.664207 0.795426 11.00000 -1.50000
H22B 2 0.517296 0.718553 0.812542 11.00000 -1.50000
H22C 2 0.604353 0.666648 0.807590 11.00000 -1.50000
AFIX 0
C17 1 0.375252 0.810706 0.601834 11.00000 0.15395 0.15372 =
0.15396 -0.06569 -0.02489 -0.00780
AFIX 13
H17 2 0.382557 0.780481 0.645072 11.00000 -1.20000
AFIX 0
C26 1 0.922517 0.751488 0.570815 11.00000 0.15157 0.15152 =
0.15194 -0.06433 -0.02492 -0.00766
AFIX 13
H26 2 0.890958 0.776070 0.532887 11.00000 -1.20000
AFIX 0
C29 1 0.994063 0.495988 0.615313 11.00000 0.19098 0.19133 =
0.19141 -0.08125 -0.03128 -0.00965
AFIX 13
H29 2 0.971534 0.452786 0.626613 11.00000 -1.20000
AFIX 0
C37 1 0.672540 0.534749 0.800645 11.00000 0.12988 0.13030 =
0.12840 -0.05434 -0.01993 -0.00600
AFIX 137
H37A 2 0.609687 0.561193 0.791804 11.00000 -1.50000
H37B 2 0.679270 0.521773 0.843615 11.00000 -1.50000
H37C 2 0.669966 0.497059 0.793650 11.00000 -1.50000
AFIX 0
C9 1 0.560203 0.969641 0.360427 11.00000 0.12791 0.12496 =
0.12694 -0.05245 -0.01993 -0.00573
AFIX 137
H9A 2 0.620792 0.964708 0.379027 11.00000 -1.50000
H9B 2 0.534703 1.014023 0.344928 11.00000 -1.50000
H9C 2 0.578090 0.957083 0.326328 11.00000 -1.50000
AFIX 0
C55 1 -0.498177 0.681456 1.135554 11.00000 0.18333 0.18424 =
0.18278 -0.07542 -0.02874 -0.00853
AFIX 137
H55A 2 -0.505371 0.715310 1.149347 11.00000 -1.50000
H55B 2 -0.559084 0.656470 1.153330 11.00000 -1.50000
H55C 2 -0.490272 0.700102 1.090569 11.00000 -1.50000
AFIX 0
C85 1 0.297846 0.818646 0.800667 11.00000 0.14805 0.15007 =
0.14823 -0.06230 -0.02211 -0.00500
AFIX 137
H85A 2 0.314235 0.863290 0.777486 11.00000 -1.50000
H85B 2 0.329504 0.795032 0.776594 11.00000 -1.50000
H85C 2 0.323935 0.800948 0.839731 11.00000 -1.50000
AFIX 0
C63 1 0.195132 0.688066 0.999478 11.00000 0.15137 0.15193 =
0.15135 -0.06463 -0.02511 -0.00738
C20 1 0.576388 0.734766 0.722268 11.00000 0.10895 0.10847 =
0.10833 -0.04559 -0.01693 -0.00468
AFIX 13
H20 2 0.512756 0.750438 0.703571 11.00000 -1.20000
AFIX 0
C28 1 0.978536 0.800837 0.584451 11.00000 0.15513 0.15515 =
0.15620 -0.06611 -0.02624 -0.00885
AFIX 137
H28A 2 0.931886 0.837449 0.581733 11.00000 -1.50000
H28B 2 1.040347 0.815168 0.553980 11.00000 -1.50000
H28C 2 0.996799 0.779338 0.625777 11.00000 -1.50000
AFIX 0
C5 1 0.599179 0.845901 0.261958 11.00000 0.20183 0.20160 =
0.20155 -0.08562 -0.03313 -0.01051
AFIX 13
H5 2 0.673370 0.832577 0.259780 11.00000 -1.20000
AFIX 0
C10 1 0.382832 0.939882 0.386941 11.00000 0.12045 0.11897 =
0.12009 -0.05103 -0.02057 -0.00467
AFIX 137
H10A 2 0.377241 0.909787 0.370101 11.00000 -1.50000
H10B 2 0.374943 0.983253 0.355471 11.00000 -1.50000
H10C 2 0.329310 0.932972 0.422695 11.00000 -1.50000
AFIX 0
C78 1 0.085641 1.064925 0.820882 11.00000 0.17230 0.17180 =
0.17252 -0.07339 -0.02733 -0.00977
AFIX 137
H78A 2 0.022334 1.054163 0.850639 11.00000 -1.50000
H78B 2 0.076746 1.107175 0.787760 11.00000 -1.50000
H78C 2 0.141160 1.064646 0.841561 11.00000 -1.50000
AFIX 0
C71 1 -0.267129 0.923484 1.040213 11.00000 0.17155 0.17097 =
0.17004 -0.07215 -0.02571 -0.00890
AFIX 137
H71A 2 -0.195291 0.918409 1.045119 11.00000 -1.50000
H71B 2 -0.310178 0.924405 1.077274 11.00000 -1.50000
H71C 2 -0.278427 0.963242 1.004538 11.00000 -1.50000
AFIX 0
C14 1 0.731811 0.906062 0.508800 11.00000 0.20685 0.20703 =
0.20708 -0.08796 -0.03337 -0.01026
AFIX 13
H14 2 0.759466 0.872237 0.545245 11.00000 -1.20000
AFIX 0
C83 1 0.177938 0.813257 0.813911 11.00000 0.10458 0.10487 =
0.10481 -0.04403 -0.01661 -0.00488
AFIX 13
H83 2 0.165338 0.767317 0.839672 11.00000 -1.20000
AFIX 0
C23 1 0.849113 0.735337 0.390820 11.00000 0.13367 0.13368 =
0.13386 -0.05684 -0.02111 -0.00722
AFIX 13
H23 2 0.806387 0.741383 0.359463 11.00000 -1.20000
AFIX 0
C27 1 1.001582 0.702059 0.559782 11.00000 0.16075 0.16100 =
0.16141 -0.06845 -0.02393 -0.00846
AFIX 137
H27A 2 1.038697 0.681002 0.594679 11.00000 -1.50000
H27B 2 1.049741 0.723275 0.522022 11.00000 -1.50000
H27C 2 0.966531 0.670504 0.555637 11.00000 -1.50000
AFIX 0
C7 1 0.582425 0.919771 0.210071 11.00000 0.20848 0.20749 =
0.20742 -0.08834 -0.03318 -0.01003
AFIX 137
H7A 2 0.520203 0.939445 0.224705 11.00000 -1.50000
H7B 2 0.576122 0.919428 0.171094 11.00000 -1.50000
H7C 2 0.641064 0.944025 0.203801 11.00000 -1.50000
AFIX 0
C64 1 0.249703 0.653417 0.966757 11.00000 0.16238 0.16326 =
0.16342 -0.06969 -0.02738 -0.00812
AFIX 137
H64A 2 0.244228 0.607916 0.992834 11.00000 -1.50000
H64B 2 0.321617 0.663760 0.955442 11.00000 -1.50000
H64C 2 0.220888 0.664684 0.929436 11.00000 -1.50000
AFIX 0
C33 1 0.674452 0.384649 0.678483 11.00000 0.17071 0.16854 =
0.16962 -0.07168 -0.02573 -0.00837
AFIX 137
H33A 2 0.633329 0.418650 0.650891 11.00000 -1.50000
H33B 2 0.633603 0.347398 0.703006 11.00000 -1.50000
H33C 2 0.734519 0.373506 0.654109 11.00000 -1.50000
AFIX 0
C16 1 0.668511 0.952469 0.531725 11.00000 0.21056 0.20896 =
0.20993 -0.08925 -0.03306 -0.01043
AFIX 137
H16A 2 0.681165 0.995959 0.500980 11.00000 -1.50000
H16B 2 0.687733 0.946369 0.570489 11.00000 -1.50000
H16C 2 0.595960 0.944900 0.538435 11.00000 -1.50000
AFIX 0
C79 1 0.135858 1.032504 0.729479 11.00000 0.17545 0.17607 =
0.17595 -0.07433 -0.02836 -0.01050
AFIX 137
H79A 2 0.156162 0.993873 0.723319 11.00000 -1.50000
H79B 2 0.192128 1.061284 0.711000 11.00000 -1.50000
H79C 2 0.075922 1.053332 0.709964 11.00000 -1.50000
AFIX 0
C13 1 0.318099 0.676551 0.475147 11.00000 0.18938 0.18936 =
0.19071 -0.08022 -0.03094 -0.01050
AFIX 137
H13A 2 0.371433 0.650104 0.462269 11.00000 -1.50000
H13B 2 0.251651 0.658680 0.483748 11.00000 -1.50000
H13C 2 0.331789 0.677805 0.512363 11.00000 -1.50000
AFIX 0
C21 1 0.634010 0.791640 0.707640 11.00000 0.14531 0.14291 =
0.14292 -0.06110 -0.02145 -0.00589
AFIX 137
H21A 2 0.704734 0.778310 0.714049 11.00000 -1.50000
H21B 2 0.601898 0.811960 0.734666 11.00000 -1.50000
H21C 2 0.632997 0.821761 0.664660 11.00000 -1.50000
AFIX 0
C34 1 0.768262 0.352222 0.770666 11.00000 0.17155 0.17037 =
0.17085 -0.06999 -0.02890 -0.00871
AFIX 137
H34A 2 0.832219 0.340029 0.749985 11.00000 -1.50000
H34B 2 0.726248 0.315312 0.793750 11.00000 -1.50000
H34C 2 0.783284 0.367869 0.799014 11.00000 -1.50000
AFIX 0
C19 1 0.338931 0.869232 0.602999 11.00000 0.17138 0.17097 =
0.17114 -0.07261 -0.02519 -0.00659
AFIX 137
H19A 2 0.394885 0.889733 0.606453 11.00000 -1.50000
H19B 2 0.284554 0.862150 0.638377 11.00000 -1.50000
H19C 2 0.312078 0.896541 0.564977 11.00000 -1.50000
AFIX 0
C65 1 0.228802 0.678003 1.056663 11.00000 0.16655 0.16811 =
0.16672 -0.07069 -0.02740 -0.00828
AFIX 3
H65A 2 0.259191 0.716823 1.049593 11.00000 -1.50000
H65B 2 0.170732 0.668883 1.090273 11.00000 -1.50000
H65C 2 0.279861 0.642613 1.067663 11.00000 -1.50000
AFIX 0
C15 1 0.819366 0.934128 0.463786 11.00000 0.21223 0.21233 =
0.21197 -0.08949 -0.03426 -0.01053
AFIX 137
H15A 2 0.843214 0.909078 0.440131 11.00000 -1.50000
H15B 2 0.873897 0.934905 0.484651 11.00000 -1.50000
H15C 2 0.800591 0.977508 0.435931 11.00000 -1.50000
AFIX 0
C18 1 0.311484 0.779850 0.580007 11.00000 0.17331 0.17422 =
0.17380 -0.07250 -0.02790 -0.00829
AFIX 137
H18A 2 0.283453 0.812015 0.544173 11.00000 -1.50000
H18B 2 0.255508 0.759099 0.613014 11.00000 -1.50000
H18C 2 0.353700 0.748213 0.568528 11.00000 -1.50000
AFIX 0
C30 1 1.077099 0.499469 0.646649 11.00000 0.19724 0.19913 =
0.19801 -0.08384 -0.03257 -0.00819
AFIX 137
H30A 2 1.120880 0.534172 0.618030 11.00000 -1.50000
H30B 2 1.117976 0.459382 0.659497 11.00000 -1.50000
H30C 2 1.046528 0.507121 0.682831 11.00000 -1.50000
AFIX 0
C59 1 -0.377094 0.483932 1.088031 11.00000 0.18214 0.18235 =
0.18220 -0.07720 -0.03013 -0.01029
AFIX 137
H59A 2 -0.354945 0.480745 1.125025 11.00000 -1.50000
H59B 2 -0.354496 0.445308 1.082211 11.00000 -1.50000
H59C 2 -0.451646 0.489043 1.092714 11.00000 -1.50000
AFIX 0
C6 1 0.548160 0.811009 0.244659 11.00000 0.21128 0.21021 =
0.20927 -0.08867 -0.03374 -0.01119
AFIX 137
H6A 2 0.494175 0.788673 0.278387 11.00000 -1.50000
H6B 2 0.596088 0.780127 0.235062 11.00000 -1.50000
H6C 2 0.517889 0.839383 0.208211 11.00000 -1.50000
AFIX 0
C84 1 0.123118 0.832772 0.765006 11.00000 0.13961 0.13991 =
0.13901 -0.05894 -0.02194 -0.00708
AFIX 137
H84A 2 0.052425 0.844458 0.777996 11.00000 -1.50000
H84B 2 0.124159 0.798018 0.753035 11.00000 -1.50000
H84C 2 0.154531 0.869451 0.729875 11.00000 -1.50000
AFIX 0
C81 1 -0.088597 0.972184 0.660490 11.00000 0.29588 0.29589 =
0.29594 -0.12565 -0.04828 -0.01478
AFIX 13
H81 2 -0.017729 0.958807 0.646615 11.00000 -1.20000
AFIX 0
C68 1 0.024272 0.760577 1.162274 11.00000 0.19332 0.19226 =
0.19149 -0.08176 -0.03129 -0.01034
AFIX 137
H68A 2 0.085693 0.767494 1.131075 11.00000 -1.50000
H68B 2 0.043470 0.738869 1.203356 11.00000 -1.50000
H68C 2 -0.010704 0.801488 1.157267 11.00000 -1.50000
AFIX 0
C73 1 -0.312512 1.067211 0.863923 11.00000 0.26234 0.26231 =
0.26231 -0.11180 -0.04271 -0.01312
AFIX 137
H73A 2 -0.333025 1.025100 0.872979 11.00000 -1.50000
H73B 2 -0.372925 1.096268 0.860568 11.00000 -1.50000
H73C 2 -0.279206 1.064461 0.897131 11.00000 -1.50000
AFIX 0
C75 1 0.095017 0.911160 1.029526 11.00000 0.22985 0.22987 =
0.22896 -0.09712 -0.03722 -0.01197
AFIX 137
H75A 2 0.125818 0.946450 1.029966 11.00000 -1.50000
H75B 2 0.101193 0.873198 1.067783 11.00000 -1.50000
H75C 2 0.022783 0.922112 1.025948 11.00000 -1.50000
AFIX 0
C56 1 -0.382525 0.591590 1.222385 11.00000 0.17327 0.17480 =
0.17287 -0.07215 -0.02756 -0.00833
AFIX 137
H56A 2 -0.313356 0.571886 1.222653 11.00000 -1.50000
H56B 2 -0.432252 0.558595 1.239681 11.00000 -1.50000
H56C 2 -0.393126 0.615761 1.247192 11.00000 -1.50000
AFIX 0
C69 1 -0.296572 0.863557 1.029623 11.00000 0.12951 0.12898 =
0.12932 -0.05510 -0.02050 -0.00698
AFIX 13
H69 2 -0.285413 0.822124 1.065204 11.00000 -1.20000
AFIX 0
C74 1 -0.205029 1.148739 0.795589 11.00000 0.26285 0.26210 =
0.26271 -0.11151 -0.04290 -0.01321
AFIX 137
H74A 2 -0.216209 1.154125 0.833840 11.00000 -1.50000
H74B 2 -0.240640 1.183625 0.765179 11.00000 -1.50000
H74C 2 -0.131835 1.148826 0.779603 11.00000 -1.50000
AFIX 0
C54 1 -0.395885 0.634703 1.158351 11.00000 0.13037 0.13143 =
0.13016 -0.05505 -0.02048 -0.00656
C70 1 -0.407746 0.880677 1.027539 11.00000 0.16448 0.16405 =
0.16353 -0.07025 -0.02505 -0.00662
AFIX 137
H70A 2 -0.416393 0.924161 0.996441 11.00000 -1.50000
H70B 2 -0.442655 0.877534 1.067890 11.00000 -1.50000
H70C 2 -0.436985 0.851546 1.016922 11.00000 -1.50000
AFIX 0
C67 1 -0.152804 0.704318 1.187615 11.00000 0.18387 0.18431 =
0.18317 -0.07796 -0.02846 -0.00949
AFIX 137
H67A 2 -0.198260 0.742394 1.173811 11.00000 -1.50000
H67B 2 -0.154666 0.687795 1.232092 11.00000 -1.50000
H67C 2 -0.175289 0.672095 1.178226 11.00000 -1.50000
AFIX 0
C58 1 -0.383114 0.580322 0.973857 11.00000 0.18895 0.18703 =
0.18812 -0.07953 -0.03054 -0.01128
AFIX 137
H58A 2 -0.450117 0.596199 0.987727 11.00000 -1.50000
H58B 2 -0.391959 0.551255 0.956491 11.00000 -1.50000
H58C 2 -0.343884 0.615995 0.942364 11.00000 -1.50000
AFIX 0
C80 1 -0.093481 1.043019 0.620815 11.00000 0.29907 0.29988 =
0.29909 -0.12649 -0.04924 -0.01538
AFIX 137
H80A 2 -0.148216 1.063307 0.640345 11.00000 -1.50000
H80B 2 -0.107134 1.051109 0.580189 11.00000 -1.50000
H80C 2 -0.028248 1.060415 0.616270 11.00000 -1.50000
AFIX 0
C31 1 1.030877 0.541428 0.539765 11.00000 0.19916 0.19862 =
0.19882 -0.08446 -0.03105 -0.00875
C76 1 0.254278 0.893825 0.970885 11.00000 0.23931 0.23999 =
0.24013 -0.10180 -0.03890 -0.01191
AFIX 137
H76A 2 0.281035 0.895307 0.930025 11.00000 -1.50000
H76B 2 0.276436 0.853489 1.002423 11.00000 -1.50000
H76C 2 0.280043 0.928921 0.974476 11.00000 -1.50000
AFIX 0
C25 1 0.888258 0.793824 0.383574 11.00000 0.18387 0.18338 =
0.18346 -0.07641 -0.02695 -0.00857
AFIX 137
H25A 2 0.832450 0.819197 0.396159 11.00000 -1.50000
H25B 2 0.917452 0.818050 0.340387 11.00000 -1.50000
H25C 2 0.941104 0.783419 0.409320 11.00000 -1.50000
AFIX 0
C66 1 -0.045321 0.720750 1.154841 11.00000 0.13919 0.13974 =
0.13775 -0.06033 -0.02403 -0.00895
C24 1 0.916932 0.674258 0.409291 11.00000 0.18916 0.18916 =
0.18913 -0.07941 -0.02909 -0.00987
AFIX 137
H24A 2 0.987758 0.684478 0.404078 11.00000 -1.50000
H24B 2 0.912472 0.653202 0.383184 11.00000 -1.50000
H24C 2 0.893976 0.645996 0.452434 11.00000 -1.50000
AFIX 0
C72 1 -0.243347 1.090166 0.807412 11.00000 0.26147 0.26141 =
0.26149 -0.11099 -0.04241 -0.01320
AFIX 13
H72 2 -0.283606 1.099149 0.774091 11.00000 -1.20000
AFIX 0
C86 1 0.145509 0.899300 0.979232 11.00000 0.23585 0.23599 =
0.23596 -0.10029 -0.03820 -0.01175
AFIX 13
H86 2 0.137747 0.852484 1.001523 11.00000 -1.20000
AFIX 0
C82 1 -0.142787 0.909685 0.693277 11.00000 0.30011 0.30037 =
0.29926 -0.12746 -0.04882 -0.01452
AFIX 3
H82A 2 -0.157467 0.899385 0.661167 11.00000 -1.50000
H82B 2 -0.206537 0.912465 0.720037 11.00000 -1.50000
H82C 2 -0.096807 0.876485 0.717737 11.00000 -1.50000
AFIX 0
C11 1 0.317215 0.742815 0.424463 11.00000 0.18615
C12 1 0.222863 0.768309 0.394590 11.00000 0.29176
AFIX 3
H12A 2 0.166443 0.739839 0.409880 11.00000 -1.50000
H12B 2 0.246003 0.779529 0.350720 11.00000 -1.50000
H12C 2 0.199653 0.806829 0.400470 11.00000 -1.50000
AFIX 0
HKLF 4
REM ccc_a.res in P-1
REM R1 = 0.1219 for 10792 Fo > 4sig(Fo) and 0.2051 for all 22977 data
REM 1287 parameters refined using 1317 restraints
END
WGHT 0.2000 0.0000
REM Highest difference peak 1.317, deepest hole -1.117, 1-sigma level 0.123
Q1 1 -0.4298 0.6898 1.1804 11.00000 0.05 0.90
Q2 1 0.8779 0.7095 0.3546 11.00000 0.05 0.88
Q3 1 -0.0953 0.7613 1.1405 11.00000 0.05 0.85
Q4 1 0.5338 0.7303 0.7699 11.00000 0.05 0.81
Q5 1 -0.0647 0.6638 1.2048 11.00000 0.05 0.81
Q6 1 -0.1727 1.0401 0.8400 11.00000 0.05 0.73
Q7 1 0.6425 0.7277 0.7326 11.00000 0.05 0.72
Q8 1 -0.4598 0.5721 1.0299 11.00000 0.05 0.71
Q9 1 0.2844 0.7407 0.4520 11.00000 0.05 0.70
Q10 1 -0.2302 0.8770 1.0694 11.00000 0.05 0.69
Q11 1 0.6967 0.3759 0.7884 11.00000 0.05 0.68
Q12 1 0.5558 0.8601 0.2578 11.00000 0.05 0.68
Q13 1 -0.1573 1.1599 0.7549 11.00000 0.05 0.66
Q14 1 -0.1412 0.9667 0.6792 11.00000 0.05 0.64
Q15 1 1.0325 0.4585 0.6726 11.00000 0.05 0.64
Q16 1 0.6579 0.8129 0.2432 11.00000 0.05 0.64
Q17 1 -0.2962 0.5445 0.9772 11.00000 0.05 0.63
Q18 1 0.8407 0.7908 0.3466 11.00000 0.05 0.62
Q19 1 0.7630 0.3686 0.6815 11.00000 0.05 0.62
Q20 1 -0.3151 0.9134 0.9912 11.00000 0.05 0.60
;
_shelx_res_checksum 67422
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
Ti8 Ti 0.67831(11) 0.67975(7) 0.51348(7) 0.0554(4) Uani 1 1 d . U
Ti3 Ti -0.17937(11) 0.82090(8) 0.93509(8) 0.0596(4) Uani 1 1 d . U
Ti1 Ti -0.24402(12) 0.65765(8) 1.04260(8) 0.0619(5) Uani 1 1 d . U
Ti2 Ti -0.03440(12) 0.72111(8) 1.02501(8) 0.0618(5) Uani 1 1 d . .
Ti9 Ti 0.72864(12) 0.68580(9) 0.63231(8) 0.0665(5) Uani 1 1 d . .
Ti7 Ti 0.58418(14) 0.81235(8) 0.51263(9) 0.0720(5) Uani 1 1 d . .
Ti6 Ti 0.52069(14) 0.79560(8) 0.40123(9) 0.0717(5) Uani 1 1 d . .
Ti10 Ti 0.77528(12) 0.54434(8) 0.64139(8) 0.0663(5) Uani 1 1 d . .
Ti4 Ti 0.04210(14) 0.87782(9) 0.89262(9) 0.0785(6) Uani 1 1 d . .
S1 S 0.51055(15) 0.57598(11) 0.62308(11) 0.0559(6) Uani 1 1 d . .
S2 S -0.15543(15) 0.70871(11) 0.88154(10) 0.0572(6) Uani 1 1 d . .
Ti5 Ti -0.10969(16) 0.97149(9) 0.80138(11) 0.0932(7) Uani 1 1 d . .
O17 O 0.5386(4) 0.6395(3) 0.5705(3) 0.0546(13) Uani 1 1 d . .
O21 O -0.1737(4) 0.7387(3) 1.0067(2) 0.0539(13) Uani 1 1 d . .
O33 O -0.1629(4) 0.6601(3) 0.9456(3) 0.0619(15) Uani 1 1 d . .
O32 O -0.1289(4) 0.7708(3) 0.8769(3) 0.0603(14) Uani 1 1 d . .
O15 O 0.5894(4) 0.5500(3) 0.6631(3) 0.0651(16) Uani 1 1 d . .
O9 O 0.7456(4) 0.6343(3) 0.5860(3) 0.0557(14) Uani 1 1 d . .
O24 O -0.0257(4) 0.8057(3) 0.9580(3) 0.0700(17) Uani 1 1 d . .
O8 O 0.6669(5) 0.7409(3) 0.5603(3) 0.0717(17) Uani 1 1 d . .
O16 O 0.4799(4) 0.5328(3) 0.6013(3) 0.0784(18) Uani 1 1 d . .
O5 O 0.5894(5) 0.7569(3) 0.4728(3) 0.0647(15) Uani 1 1 d . .
O12 O 0.7497(4) 0.5310(3) 0.5700(3) 0.0702(17) Uani 1 1 d . .
O25 O -0.3509(4) 0.7147(3) 0.9937(3) 0.0662(16) Uani 1 1 d . .
O20 O -0.0977(4) 0.6344(3) 1.0610(3) 0.0689(16) Uani 1 1 d . .
O18 O -0.2947(5) 0.5864(3) 1.0512(3) 0.0742(17) Uani 1 1 d . .
O34 O -0.2404(4) 0.7158(4) 0.8500(3) 0.085(2) Uani 1 1 d . .
O11 O 0.5813(5) 0.7172(3) 0.3916(3) 0.0785(18) Uani 1 1 d . .
O10 O 0.7580(4) 0.5929(3) 0.6944(3) 0.0764(18) Uani 1 1 d . .
N2 N 0.7106(5) 0.5782(3) 0.5209(3) 0.0569(17) Uani 1 1 d . .
O28 O -0.0947(5) 0.8909(3) 0.8716(3) 0.0806(19) Uani 1 1 d . .
O2 O 0.5192(5) 0.8623(3) 0.4327(3) 0.0799(19) Uani 1 1 d . .
O39 O 0.7926(5) 0.7073(3) 0.4577(3) 0.0774(16) Uani 1 1 d . U
O27 O -0.2435(5) 0.8646(3) 0.9767(3) 0.0814(17) Uani 1 1 d . U
O14 O 0.7604(5) 0.4616(3) 0.6956(3) 0.0782(19) Uani 1 1 d . .
N1 N 0.6165(5) 0.6675(3) 0.4386(3) 0.0587(17) Uani 1 1 d . .
O13 O 0.9136(5) 0.5429(4) 0.6254(4) 0.090(2) Uani 1 1 d . .
O19 O -0.3034(5) 0.6568(4) 1.1159(3) 0.0895(19) Uani 1 1 d . U
N3 N -0.3281(5) 0.7746(3) 0.9483(4) 0.0598(18) Uani 1 1 d . .
O36 O 0.6377(5) 0.7022(4) 0.6911(3) 0.089(2) Uani 1 1 d . .
O29 O 0.0313(6) 0.9678(3) 0.8203(4) 0.104(3) Uani 1 1 d . .
O22 O 0.0904(5) 0.6894(3) 1.0022(3) 0.086(2) Uani 1 1 d . .
O23 O -0.0283(8) 0.7324(5) 1.0918(5) 0.138(3) Uani 1 1 d . .
O37 O 0.8440(6) 0.7234(4) 0.6212(4) 0.094(2) Uani 1 1 d . .
O26 O -0.2506(5) 0.9400(4) 0.8167(4) 0.102(2) Uani 1 1 d . .
O38 O 0.1416(6) 0.8448(4) 0.8539(4) 0.107(3) Uani 1 1 d . .
N4 N -0.2780(5) 0.8822(4) 0.8612(4) 0.070(2) Uani 1 1 d . .
C1 C 0.6292(7) 0.6124(4) 0.4343(4) 0.0666(18) Uani 1 1 d . U
O1 O 0.5580(7) 0.8439(3) 0.3206(3) 0.102(2) Uani 1 1 d . .
C44 C 0.1326(7) 0.6488(4) 0.7738(4) 0.0659(11) Uani 1 1 d . U
C47 C -0.0436(7) 0.6852(4) 0.8397(4) 0.0643(13) Uani 1 1 d . U
O7 O 0.4762(6) 0.8176(4) 0.5661(4) 0.112(3) Uani 1 1 d . .
C2 C 0.6746(7) 0.5612(4) 0.4849(4) 0.0645(18) Uani 1 1 d . U
C38 C 0.3979(7) 0.5949(4) 0.6700(4) 0.0633(13) Uani 1 1 d . U
C43 C 0.2266(7) 0.6288(4) 0.7384(4) 0.0653(11) Uani 1 1 d . U
C39 C 0.3010(7) 0.5852(4) 0.6641(4) 0.0654(12) Uani 1 1 d . U
H39 H 0.2933 0.5676 0.6371 0.079 Uiso 1 1 calc R U
C45 C 0.1280(7) 0.6402(4) 0.8333(4) 0.0673(12) Uani 1 1 d . U
H45 H 0.1859 0.6211 0.8528 0.081 Uiso 1 1 calc R U
O3 O 0.3918(6) 0.7796(4) 0.4160(5) 0.117(3) Uani 1 1 d . .
C46 C 0.0417(7) 0.6583(4) 0.8674(5) 0.0723(12) Uani 1 1 d . U
H46 H 0.0424 0.6521 0.9082 0.087 Uiso 1 1 calc R U
O6 O 0.6678(7) 0.8754(4) 0.4917(4) 0.119(3) Uani 1 1 d . .
C50 C -0.3962(8) 0.8035(5) 0.9109(5) 0.076(2) Uani 1 1 d . U
C42 C 0.3246(7) 0.6349(4) 0.7444(4) 0.0660(12) Uani 1 1 d . U
H42 H 0.3332 0.6503 0.7729 0.079 Uiso 1 1 calc R U
C40 C 0.2169(7) 0.6013(4) 0.6978(4) 0.0668(12) Uani 1 1 d . U
H40 H 0.1510 0.5941 0.6942 0.080 Uiso 1 1 calc R U
C41 C 0.4112(7) 0.6193(4) 0.7102(4) 0.0702(12) Uani 1 1 d . U
H41 H 0.4775 0.6253 0.7144 0.084 Uiso 1 1 calc R U
C49 C 0.0416(7) 0.6721(4) 0.7485(5) 0.0689(12) Uani 1 1 d . U
H49 H 0.0376 0.6732 0.7098 0.083 Uiso 1 1 calc R U
C48 C -0.0429(7) 0.6939(4) 0.7799(4) 0.0693(13) Uani 1 1 d . U
H48 H -0.0998 0.7146 0.7601 0.083 Uiso 1 1 calc R U
O35 O 0.0964(8) 0.9060(4) 0.9363(4) 0.138(4) Uani 1 1 d . .
C4 C 0.6036(7) 0.6065(5) 0.3809(5) 0.077(2) Uani 1 1 d . U
H4A H 0.5309 0.5986 0.3889 0.115 Uiso 1 1 d R U
H4B H 0.6179 0.6457 0.3435 0.115 Uiso 1 1 d R U
H4C H 0.6442 0.5710 0.3752 0.115 Uiso 1 1 d R U
C3 C 0.6767(7) 0.4915(4) 0.4949(5) 0.078(2) Uani 1 1 d . U
H3A H 0.7459 0.4725 0.4990 0.117 Uiso 1 1 calc R U
H3B H 0.6558 0.4898 0.4596 0.117 Uiso 1 1 calc R U
H3C H 0.6296 0.4679 0.5324 0.117 Uiso 1 1 calc R U
C51 C -0.3683(8) 0.8649(5) 0.8639(5) 0.082(2) Uani 1 1 d . U
C60 C -0.0475(8) 0.5732(5) 1.0959(5) 0.082(2) Uani 1 1 d . U
H60 H 0.0175 0.5813 1.1048 0.098 Uiso 1 1 calc R U
O30 O -0.0780(8) 0.9782(6) 0.7233(5) 0.166(5) Uani 1 1 d . .
C35 C 0.7636(10) 0.5723(7) 0.7585(6) 0.112(3) Uani 1 1 d . U
H35 H 0.7619 0.6113 0.7655 0.135 Uiso 1 1 calc R U
C53 C -0.4938(8) 0.7714(5) 0.9189(5) 0.090(2) Uani 1 1 d . U
H53A H -0.4780 0.7400 0.9017 0.135 Uiso 1 1 calc R U
H53B H -0.5440 0.8034 0.8972 0.135 Uiso 1 1 calc R U
H53C H -0.5219 0.7503 0.9627 0.135 Uiso 1 1 calc R U
O31 O -0.1548(8) 1.0464(5) 0.8002(5) 0.143(3) Uani 1 1 d . U
C61 C -0.1138(9) 0.5347(6) 1.1570(6) 0.097(3) Uani 1 1 d . U
H61A H -0.1397 0.5615 1.1786 0.146 Uiso 1 1 calc R U
H61B H -0.0729 0.4986 1.1825 0.146 Uiso 1 1 calc R U
H61C H -0.1712 0.5191 1.1491 0.146 Uiso 1 1 calc R U
C62 C -0.0213(9) 0.5377(6) 1.0551(6) 0.103(3) Uani 1 1 d . U
H62A H -0.0806 0.5151 1.0590 0.155 Uiso 1 1 calc R U
H62B H 0.0362 0.5073 1.0680 0.155 Uiso 1 1 calc R U
H62C H -0.0027 0.5680 1.0122 0.155 Uiso 1 1 calc R U
C8 C 0.4829(10) 0.9304(6) 0.4057(7) 0.110(3) Uani 1 1 d . U
H8 H 0.4722 0.9434 0.4402 0.132 Uiso 1 1 calc R U
C32 C 0.7080(13) 0.4067(8) 0.7206(8) 0.146(4) Uani 1 1 d D U
H32 H 0.6434 0.4157 0.7447 0.175 Uiso 1 1 calc R U
C52 C -0.4371(9) 0.9081(5) 0.8156(5) 0.099(3) Uani 1 1 d . U
H52A H -0.4957 0.9240 0.8370 0.148 Uiso 1 1 d R U
H52B H -0.4610 0.8832 0.7979 0.148 Uiso 1 1 d R U
H52C H -0.3998 0.9438 0.7827 0.148 Uiso 1 1 d R U
C36 C 0.8619(10) 0.5361(7) 0.7745(7) 0.127(3) Uani 1 1 d . U
H36A H 0.8688 0.4993 0.7650 0.190 Uiso 1 1 calc R U
H36B H 0.8626 0.5219 0.8185 0.190 Uiso 1 1 calc R U
H36C H 0.9189 0.5635 0.7505 0.190 Uiso 1 1 calc R U
C57 C -0.3269(15) 0.5458(9) 1.0276(8) 0.169(5) Uani 1 1 d D U
H57 H -0.2619 0.5286 1.0107 0.202 Uiso 1 1 calc R U
C77 C 0.1115(14) 1.0165(9) 0.7940(10) 0.165(5) Uani 1 1 d . U
H77 H 0.1739 0.9924 0.8110 0.198 Uiso 1 1 calc R U
C22 C 0.5448(11) 0.6922(7) 0.7906(7) 0.135(3) Uani 1 1 d . U
H22A H 0.4925 0.6642 0.7954 0.202 Uiso 1 1 calc R U
H22B H 0.5173 0.7186 0.8125 0.202 Uiso 1 1 calc R U
H22C H 0.6044 0.6666 0.8076 0.202 Uiso 1 1 calc R U
C17 C 0.3753(14) 0.8107(9) 0.6018(9) 0.154(4) Uani 1 1 d . U
H17 H 0.3826 0.7805 0.6451 0.184 Uiso 1 1 calc R U
C26 C 0.9225(14) 0.7515(8) 0.5708(9) 0.152(4) Uani 1 1 d . U
H26 H 0.8910 0.7761 0.5329 0.182 Uiso 1 1 calc R U
C29 C 0.9941(17) 0.4960(11) 0.6153(11) 0.191(5) Uani 1 1 d . U
H29 H 0.9715 0.4528 0.6266 0.229 Uiso 1 1 calc R U
C37 C 0.6725(11) 0.5347(7) 0.8006(7) 0.130(3) Uani 1 1 d . U
H37A H 0.6097 0.5612 0.7918 0.195 Uiso 1 1 calc R U
H37B H 0.6793 0.5218 0.8436 0.195 Uiso 1 1 calc R U
H37C H 0.6700 0.4971 0.7937 0.195 Uiso 1 1 calc R U
C9 C 0.5602(11) 0.9696(7) 0.3604(7) 0.127(3) Uani 1 1 d . U
H9A H 0.6208 0.9647 0.3790 0.191 Uiso 1 1 calc R U
H9B H 0.5347 1.0140 0.3449 0.191 Uiso 1 1 calc R U
H9C H 0.5781 0.9571 0.3263 0.191 Uiso 1 1 calc R U
C55 C -0.4982(14) 0.6815(9) 1.1356(9) 0.185(4) Uani 1 1 d . U
H55A H -0.5054 0.7153 1.1493 0.277 Uiso 1 1 calc R U
H55B H -0.5591 0.6565 1.1533 0.277 Uiso 1 1 calc R U
H55C H -0.4903 0.7001 1.0906 0.277 Uiso 1 1 calc R U
C85 C 0.2978(12) 0.8186(8) 0.8007(8) 0.150(4) Uani 1 1 d . U
H85A H 0.3142 0.8633 0.7775 0.225 Uiso 1 1 calc R U
H85B H 0.3295 0.7950 0.7766 0.225 Uiso 1 1 calc R U
H85C H 0.3239 0.8009 0.8397 0.225 Uiso 1 1 calc R U
C63 C 0.1951(14) 0.6881(8) 0.9995(9) 0.151(4) Uani 1 1 d . U
C20 C 0.5764(10) 0.7348(6) 0.7223(7) 0.109(2) Uani 1 1 d . U
H20 H 0.5128 0.7504 0.7036 0.131 Uiso 1 1 calc R U
C28 C 0.9785(13) 0.8008(8) 0.5845(8) 0.155(4) Uani 1 1 d . U
H28A H 0.9319 0.8374 0.5817 0.233 Uiso 1 1 calc R U
H28B H 1.0403 0.8152 0.5540 0.233 Uiso 1 1 calc R U
H28C H 0.9968 0.7793 0.6258 0.233 Uiso 1 1 calc R U
C5 C 0.5992(18) 0.8459(11) 0.2620(11) 0.202(6) Uani 1 1 d . U
H5 H 0.6734 0.8326 0.2598 0.242 Uiso 1 1 calc R U
C10 C 0.3828(10) 0.9399(6) 0.3869(7) 0.120(3) Uani 1 1 d . U
H10A H 0.3772 0.9098 0.3701 0.180 Uiso 1 1 calc R U
H10B H 0.3749 0.9833 0.3555 0.180 Uiso 1 1 calc R U
H10C H 0.3293 0.9330 0.4227 0.180 Uiso 1 1 calc R U
C78 C 0.0856(14) 1.0649(9) 0.8209(9) 0.172(5) Uani 1 1 d . U
H78A H 0.0223 1.0542 0.8506 0.258 Uiso 1 1 calc R U
H78B H 0.0767 1.1072 0.7878 0.258 Uiso 1 1 calc R U
H78C H 0.1412 1.0646 0.8416 0.258 Uiso 1 1 calc R U
C71 C -0.2671(14) 0.9235(9) 1.0402(9) 0.171(4) Uani 1 1 d . U
H71A H -0.1953 0.9184 1.0451 0.257 Uiso 1 1 calc R U
H71B H -0.3102 0.9244 1.0773 0.257 Uiso 1 1 calc R U
H71C H -0.2784 0.9632 1.0045 0.257 Uiso 1 1 calc R U
C14 C 0.7318(19) 0.9061(12) 0.5088(12) 0.207(6) Uani 1 1 d . U
H14 H 0.7595 0.8722 0.5452 0.248 Uiso 1 1 calc R U
C83 C 0.1779(10) 0.8133(6) 0.8139(6) 0.105(2) Uani 1 1 d . U
H83 H 0.1653 0.7673 0.8397 0.126 Uiso 1 1 calc R U
C23 C 0.8491(11) 0.7353(7) 0.3908(8) 0.134(3) Uani 1 1 d D U
H23 H 0.8064 0.7414 0.3595 0.161 Uiso 1 1 calc R U
C27 C 1.0016(13) 0.7021(8) 0.5598(8) 0.161(4) Uani 1 1 d . U
H27A H 1.0387 0.6810 0.5947 0.242 Uiso 1 1 calc R U
H27B H 1.0497 0.7233 0.5220 0.242 Uiso 1 1 calc R U
H27C H 0.9665 0.6705 0.5556 0.242 Uiso 1 1 calc R U
C7 C 0.5824(16) 0.9198(10) 0.2101(10) 0.208(6) Uani 1 1 d . U
H7A H 0.5202 0.9394 0.2247 0.312 Uiso 1 1 calc R U
H7B H 0.5761 0.9194 0.1711 0.312 Uiso 1 1 calc R U
H7C H 0.6411 0.9440 0.2038 0.312 Uiso 1 1 calc R U
C64 C 0.2497(13) 0.6534(8) 0.9668(8) 0.163(4) Uani 1 1 d . U
H64A H 0.2442 0.6079 0.9928 0.244 Uiso 1 1 calc R U
H64B H 0.3216 0.6638 0.9554 0.244 Uiso 1 1 calc R U
H64C H 0.2209 0.6647 0.9294 0.244 Uiso 1 1 calc R U
C33 C 0.6745(14) 0.3846(8) 0.6785(8) 0.170(4) Uani 1 1 d D U
H33A H 0.6333 0.4186 0.6509 0.255 Uiso 1 1 calc R U
H33B H 0.6336 0.3474 0.7030 0.255 Uiso 1 1 calc R U
H33C H 0.7345 0.3735 0.6541 0.255 Uiso 1 1 calc R U
C16 C 0.6685(17) 0.9525(11) 0.5317(10) 0.210(6) Uani 1 1 d . U
H16A H 0.6812 0.9960 0.5010 0.315 Uiso 1 1 calc R U
H16B H 0.6877 0.9464 0.5705 0.315 Uiso 1 1 calc R U
H16C H 0.5960 0.9449 0.5384 0.315 Uiso 1 1 calc R U
C79 C 0.1359(14) 1.0325(9) 0.7295(9) 0.176(5) Uani 1 1 d . U
H79A H 0.1562 0.9939 0.7233 0.264 Uiso 1 1 calc R U
H79B H 0.1921 1.0613 0.7110 0.264 Uiso 1 1 calc R U
H79C H 0.0759 1.0533 0.7100 0.264 Uiso 1 1 calc R U
C13 C 0.3181(15) 0.6766(9) 0.4751(9) 0.190(6) Uani 1 1 d D U
H13A H 0.3714 0.6501 0.4623 0.285 Uiso 1 1 calc R U
H13B H 0.2517 0.6587 0.4837 0.285 Uiso 1 1 calc R U
H13C H 0.3318 0.6778 0.5124 0.285 Uiso 1 1 calc R U
C21 C 0.6340(12) 0.7916(7) 0.7076(8) 0.144(4) Uani 1 1 d . U
H21A H 0.7047 0.7783 0.7140 0.216 Uiso 1 1 calc R U
H21B H 0.6019 0.8120 0.7347 0.216 Uiso 1 1 calc R U
H21C H 0.6330 0.8218 0.6647 0.216 Uiso 1 1 calc R U
C34 C 0.7683(14) 0.3522(9) 0.7707(9) 0.172(5) Uani 1 1 d . U
H34A H 0.8322 0.3400 0.7500 0.257 Uiso 1 1 calc R U
H34B H 0.7262 0.3153 0.7937 0.257 Uiso 1 1 calc R U
H34C H 0.7833 0.3679 0.7990 0.257 Uiso 1 1 calc R U
C19 C 0.3389(14) 0.8692(9) 0.6030(9) 0.172(4) Uani 1 1 d . U
H19A H 0.3949 0.8897 0.6065 0.258 Uiso 1 1 calc R U
H19B H 0.2846 0.8621 0.6384 0.258 Uiso 1 1 calc R U
H19C H 0.3121 0.8965 0.5650 0.258 Uiso 1 1 calc R U
C65 C 0.2288(13) 0.6780(8) 1.0567(8) 0.167(4) Uani 1 1 d . U
H65A H 0.2592 0.7168 1.0496 0.251 Uiso 1 1 d R U
H65B H 0.1707 0.6689 1.0903 0.251 Uiso 1 1 d R U
H65C H 0.2799 0.6426 1.0677 0.251 Uiso 1 1 d R U
C15 C 0.8194(17) 0.9341(11) 0.4638(11) 0.212(6) Uani 1 1 d . U
H15A H 0.8432 0.9091 0.4401 0.319 Uiso 1 1 calc R U
H15B H 0.8739 0.9349 0.4847 0.319 Uiso 1 1 calc R U
H15C H 0.8006 0.9775 0.4359 0.319 Uiso 1 1 calc R U
C18 C 0.3115(14) 0.7798(9) 0.5800(9) 0.174(5) Uani 1 1 d . U
H18A H 0.2835 0.8120 0.5442 0.262 Uiso 1 1 calc R U
H18B H 0.2555 0.7591 0.6130 0.262 Uiso 1 1 calc R U
H18C H 0.3537 0.7482 0.5685 0.262 Uiso 1 1 calc R U
C30 C 1.0771(16) 0.4995(10) 0.6466(10) 0.198(5) Uani 1 1 d . U
H30A H 1.1209 0.5342 0.6180 0.298 Uiso 1 1 calc R U
H30B H 1.1180 0.4594 0.6595 0.298 Uiso 1 1 calc R U
H30C H 1.0465 0.5071 0.6828 0.298 Uiso 1 1 calc R U
C59 C -0.3771(14) 0.4839(9) 1.0880(9) 0.182(5) Uani 1 1 d . U
H59A H -0.3549 0.4807 1.1250 0.273 Uiso 1 1 calc R U
H59B H -0.3545 0.4453 1.0822 0.273 Uiso 1 1 calc R U
H59C H -0.4516 0.4890 1.0927 0.273 Uiso 1 1 calc R U
C6 C 0.5482(17) 0.8110(10) 0.2447(10) 0.210(6) Uani 1 1 d . U
H6A H 0.4942 0.7887 0.2784 0.316 Uiso 1 1 calc R U
H6B H 0.5961 0.7801 0.2351 0.316 Uiso 1 1 calc R U
H6C H 0.5179 0.8394 0.2082 0.316 Uiso 1 1 calc R U
C84 C 0.1231(11) 0.8328(7) 0.7650(7) 0.140(4) Uani 1 1 d . U
H84A H 0.0524 0.8445 0.7780 0.210 Uiso 1 1 calc R U
H84B H 0.1242 0.7980 0.7530 0.210 Uiso 1 1 calc R U
H84C H 0.1545 0.8695 0.7299 0.210 Uiso 1 1 calc R U
C81 C -0.089(2) 0.9722(11) 0.6605(15) 0.296(8) Uani 1 1 d D U
H81 H -0.0177 0.9588 0.6466 0.355 Uiso 1 1 calc R U
C68 C 0.0243(15) 0.7606(9) 1.1623(10) 0.192(4) Uani 1 1 d . U
H68A H 0.0857 0.7675 1.1311 0.288 Uiso 1 1 calc R U
H68B H 0.0435 0.7389 1.2034 0.288 Uiso 1 1 calc R U
H68C H -0.0107 0.8015 1.1573 0.288 Uiso 1 1 calc R U
C73 C -0.313(2) 1.0672(13) 0.8639(14) 0.262(7) Uani 1 1 d . U
H73A H -0.3330 1.0251 0.8730 0.393 Uiso 1 1 calc R U
H73B H -0.3729 1.0963 0.8606 0.393 Uiso 1 1 calc R U
H73C H -0.2792 1.0645 0.8971 0.393 Uiso 1 1 calc R U
C75 C 0.0950(19) 0.9112(12) 1.0295(12) 0.230(5) Uani 1 1 d . U
H75A H 0.1258 0.9464 1.0300 0.344 Uiso 1 1 calc R U
H75B H 0.1012 0.8732 1.0678 0.344 Uiso 1 1 calc R U
H75C H 0.0228 0.9221 1.0259 0.344 Uiso 1 1 calc R U
C56 C -0.3825(14) 0.5916(9) 1.2224(9) 0.174(4) Uani 1 1 d . U
H56A H -0.3134 0.5719 1.2227 0.262 Uiso 1 1 calc R U
H56B H -0.4323 0.5586 1.2397 0.262 Uiso 1 1 calc R U
H56C H -0.3931 0.6158 1.2472 0.262 Uiso 1 1 calc R U
C69 C -0.2966(10) 0.8636(7) 1.0296(8) 0.129(3) Uani 1 1 d D U
H69 H -0.2854 0.8221 1.0652 0.155 Uiso 1 1 calc R U
C74 C -0.205(2) 1.1487(14) 0.7956(13) 0.262(7) Uani 1 1 d . U
H74A H -0.2162 1.1541 0.8338 0.394 Uiso 1 1 calc R U
H74B H -0.2406 1.1836 0.7652 0.394 Uiso 1 1 calc R U
H74C H -0.1318 1.1488 0.7796 0.394 Uiso 1 1 calc R U
C54 C -0.3959(12) 0.6347(7) 1.1584(8) 0.131(3) Uani 1 1 d . U
C70 C -0.4077(11) 0.8807(8) 1.0275(8) 0.164(4) Uani 1 1 d D U
H70A H -0.4164 0.9242 0.9964 0.246 Uiso 1 1 calc R U
H70B H -0.4427 0.8775 1.0679 0.246 Uiso 1 1 calc R U
H70C H -0.4370 0.8515 1.0169 0.246 Uiso 1 1 calc R U
C67 C -0.1528(12) 0.7043(9) 1.1876(9) 0.184(4) Uani 1 1 d D U
H67A H -0.1983 0.7424 1.1738 0.276 Uiso 1 1 calc R U
H67B H -0.1547 0.6878 1.2321 0.276 Uiso 1 1 calc R U
H67C H -0.1753 0.6721 1.1782 0.276 Uiso 1 1 calc R U
C58 C -0.3831(15) 0.5803(9) 0.9739(8) 0.188(5) Uani 1 1 d D U
H58A H -0.4501 0.5962 0.9877 0.282 Uiso 1 1 calc R U
H58B H -0.3920 0.5513 0.9565 0.282 Uiso 1 1 calc R U
H58C H -0.3439 0.6160 0.9424 0.282 Uiso 1 1 calc R U
C80 C -0.093(2) 1.0430(12) 0.6208(14) 0.299(9) Uani 1 1 d D U
H80A H -0.1482 1.0633 0.6403 0.449 Uiso 1 1 calc R U
H80B H -0.1071 1.0511 0.5802 0.449 Uiso 1 1 calc R U
H80C H -0.0282 1.0604 0.6163 0.449 Uiso 1 1 calc R U
C31 C 1.0309(16) 0.5414(11) 0.5398(11) 0.199(4) Uani 1 1 d . U
C76 C 0.254(2) 0.8938(12) 0.9709(12) 0.240(6) Uani 1 1 d . U
H76A H 0.2810 0.8953 0.9300 0.360 Uiso 1 1 calc R U
H76B H 0.2764 0.8535 1.0024 0.360 Uiso 1 1 calc R U
H76C H 0.2800 0.9289 0.9745 0.360 Uiso 1 1 calc R U
C25 C 0.8883(15) 0.7938(9) 0.3836(9) 0.185(4) Uani 1 1 d . U
H25A H 0.8325 0.8192 0.3962 0.277 Uiso 1 1 calc R U
H25B H 0.9175 0.8180 0.3404 0.277 Uiso 1 1 calc R U
H25C H 0.9411 0.7834 0.4093 0.277 Uiso 1 1 calc R U
C66 C -0.0453(12) 0.7208(8) 1.1548(8) 0.138(3) Uani 1 1 d D U
C24 C 0.9169(13) 0.6743(7) 0.4093(9) 0.190(4) Uani 1 1 d D U
H24A H 0.9878 0.6845 0.4041 0.285 Uiso 1 1 calc R U
H24B H 0.9125 0.6532 0.3832 0.285 Uiso 1 1 calc R U
H24C H 0.8940 0.6460 0.4524 0.285 Uiso 1 1 calc R U
C72 C -0.243(2) 1.0902(15) 0.8074(15) 0.261(7) Uani 1 1 d . U
H72 H -0.2836 1.0991 0.7741 0.314 Uiso 1 1 calc R U
C86 C 0.146(2) 0.8993(13) 0.9792(14) 0.236(6) Uani 1 1 d . U
H86 H 0.1377 0.8525 1.0015 0.283 Uiso 1 1 calc R U
C82 C -0.143(2) 0.9097(11) 0.6933(13) 0.300(8) Uani 1 1 d D U
H82A H -0.1575 0.8994 0.6612 0.450 Uiso 1 1 d R U
H82B H -0.2065 0.9125 0.7200 0.450 Uiso 1 1 d R U
H82C H -0.0968 0.8765 0.7177 0.450 Uiso 1 1 d R U
C11 C 0.3172(18) 0.7428(10) 0.4245(10) 0.186(6) Uiso 1 1 d D U
C12 C 0.2229(19) 0.7683(14) 0.3946(14) 0.292(14) Uiso 1 1 d D .
H12A H 0.1664 0.7398 0.4099 0.438 Uiso 1 1 d R U
H12B H 0.2460 0.7795 0.3507 0.438 Uiso 1 1 d R U
H12C H 0.1997 0.8068 0.4005 0.438 Uiso 1 1 d 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
Ti8 0.0608(9) 0.0589(9) 0.0531(10) -0.0339(8) 0.0038(7) -0.0081(7)
Ti3 0.0537(9) 0.0618(10) 0.0644(11) -0.0297(9) -0.0018(7) -0.0081(7)
Ti1 0.0554(9) 0.0725(11) 0.0549(10) -0.0250(9) 0.0025(7) -0.0184(8)
Ti2 0.0588(9) 0.0772(11) 0.0544(10) -0.0299(9) -0.0073(7) -0.0156(8)
Ti9 0.0578(9) 0.0894(12) 0.0702(12) -0.0516(10) -0.0048(8) -0.0072(8)
Ti7 0.0913(12) 0.0643(11) 0.0701(12) -0.0417(10) -0.0061(9) 0.0010(9)
Ti6 0.0848(12) 0.0667(11) 0.0664(12) -0.0328(10) -0.0113(9) 0.0016(9)
Ti10 0.0521(9) 0.0758(11) 0.0725(12) -0.0355(10) -0.0073(8) 0.0022(8)
Ti4 0.0695(11) 0.0799(12) 0.0811(14) -0.0279(11) -0.0010(9) -0.0274(9)
S1 0.0444(11) 0.0661(14) 0.0607(14) -0.0346(12) 0.0038(10) -0.0053(10)
S2 0.0469(11) 0.0746(15) 0.0547(14) -0.0353(12) 0.0028(9) -0.0068(10)
Ti5 0.0975(14) 0.0672(12) 0.0949(17) -0.0139(11) -0.0116(12) -0.0185(11)
O17 0.053(3) 0.061(3) 0.051(3) -0.028(3) 0.001(2) -0.006(3)
O21 0.051(3) 0.060(3) 0.049(3) -0.025(3) 0.003(2) -0.011(2)
O33 0.061(3) 0.069(4) 0.054(4) -0.029(3) 0.007(3) -0.013(3)
O32 0.059(3) 0.068(4) 0.046(3) -0.023(3) 0.006(3) -0.004(3)
O15 0.048(3) 0.067(4) 0.065(4) -0.018(3) -0.002(3) -0.001(3)
O9 0.047(3) 0.069(4) 0.054(3) -0.035(3) 0.009(2) -0.006(3)
O24 0.064(4) 0.081(4) 0.069(4) -0.032(4) -0.003(3) -0.024(3)
O8 0.078(4) 0.074(4) 0.075(4) -0.046(4) -0.005(3) 0.002(3)
O16 0.063(4) 0.088(5) 0.101(5) -0.063(4) 0.011(3) -0.017(3)
O5 0.089(4) 0.058(3) 0.056(4) -0.036(3) -0.005(3) 0.003(3)
O12 0.067(4) 0.070(4) 0.083(5) -0.046(4) -0.009(3) 0.012(3)
O25 0.049(3) 0.079(4) 0.062(4) -0.025(4) 0.002(3) -0.011(3)
O20 0.065(4) 0.072(4) 0.062(4) -0.021(3) -0.012(3) -0.008(3)
O18 0.076(4) 0.078(4) 0.072(4) -0.032(4) -0.004(3) -0.026(3)
O34 0.048(3) 0.149(6) 0.083(5) -0.073(5) -0.013(3) 0.000(4)
O11 0.106(5) 0.078(4) 0.070(5) -0.046(4) -0.021(4) -0.001(4)
O10 0.063(4) 0.118(5) 0.059(4) -0.048(4) -0.014(3) 0.002(3)
N2 0.054(4) 0.053(4) 0.060(5) -0.026(4) 0.000(3) 0.001(3)
O28 0.074(4) 0.073(4) 0.092(5) -0.029(4) -0.015(4) -0.014(3)
O2 0.096(5) 0.063(4) 0.090(5) -0.042(4) -0.024(4) 0.015(3)
O39 0.082(4) 0.085(4) 0.071(4) -0.044(3) 0.011(3) -0.023(3)
O27 0.091(4) 0.081(4) 0.084(4) -0.052(3) 0.002(3) -0.006(3)
O14 0.067(4) 0.069(4) 0.080(5) -0.012(4) -0.013(3) -0.010(3)
N1 0.074(5) 0.052(4) 0.048(4) -0.021(4) -0.004(4) -0.005(3)
O13 0.053(4) 0.110(5) 0.119(6) -0.065(5) -0.009(4) 0.015(4)
O19 0.082(4) 0.118(4) 0.061(4) -0.034(3) 0.012(3) -0.030(3)
N3 0.050(4) 0.061(4) 0.073(5) -0.039(4) 0.006(4) -0.004(3)
O36 0.085(4) 0.127(6) 0.084(5) -0.078(5) -0.013(4) 0.023(4)
O29 0.114(6) 0.075(5) 0.098(6) -0.012(4) 0.005(4) -0.052(4)
O22 0.055(4) 0.090(5) 0.094(5) -0.024(4) -0.009(3) -0.007(3)
O23 0.139(3) 0.140(3) 0.138(3) -0.0603(14) -0.0240(11) -0.0090(10)
O37 0.093(5) 0.110(6) 0.083(5) -0.041(5) -0.004(4) -0.033(4)
O26 0.085(5) 0.078(5) 0.113(6) -0.008(5) -0.027(4) -0.010(4)
O38 0.085(5) 0.106(6) 0.104(6) -0.030(5) 0.021(4) -0.029(4)
N4 0.057(4) 0.066(5) 0.084(6) -0.027(5) -0.010(4) -0.006(4)
C1 0.067(2) 0.066(2) 0.067(2) -0.0291(11) -0.0101(10) -0.0035(10)
O1 0.165(7) 0.076(5) 0.055(5) -0.028(4) -0.011(4) 0.014(5)
C44 0.0662(13) 0.0662(13) 0.0658(13) -0.0287(8) -0.0103(8) -0.0032(8)
C47 0.0640(15) 0.0652(15) 0.0643(15) -0.0279(9) -0.0109(9) -0.0032(9)
O7 0.112(6) 0.132(7) 0.099(6) -0.068(6) -0.010(5) 0.034(5)
C2 0.0649(19) 0.0644(19) 0.065(2) -0.0284(11) -0.0096(10) -0.0034(10)
C38 0.0633(15) 0.0636(15) 0.0636(15) -0.0277(9) -0.0101(9) -0.0033(9)
C43 0.0651(13) 0.0659(13) 0.0654(13) -0.0283(8) -0.0106(8) -0.0034(8)
C39 0.0653(14) 0.0659(14) 0.0656(14) -0.0287(9) -0.0098(9) -0.0034(9)
C45 0.0669(13) 0.0680(13) 0.0669(13) -0.0289(9) -0.0108(9) -0.0023(9)
O3 0.102(6) 0.111(6) 0.159(8) -0.071(6) -0.022(5) -0.025(5)
C46 0.0720(14) 0.0730(14) 0.0717(14) -0.0307(9) -0.0115(9) -0.0032(9)
O6 0.155(7) 0.076(5) 0.150(8) -0.057(5) -0.048(6) -0.014(5)
C50 0.075(2) 0.076(2) 0.076(2) -0.0327(12) -0.0126(10) -0.0037(10)
C42 0.0661(13) 0.0667(13) 0.0658(13) -0.0288(9) -0.0106(9) -0.0030(9)
C40 0.0661(13) 0.0671(13) 0.0669(13) -0.0285(9) -0.0103(9) -0.0034(9)
C41 0.0700(14) 0.0709(14) 0.0703(14) -0.0305(9) -0.0114(9) -0.0035(9)
C49 0.0684(13) 0.0695(13) 0.0681(13) -0.0290(9) -0.0107(9) -0.0027(9)
C48 0.0689(14) 0.0701(14) 0.0684(14) -0.0293(9) -0.0109(9) -0.0026(9)
O35 0.176(9) 0.130(7) 0.120(7) -0.033(6) -0.052(7) -0.080(7)
C4 0.079(3) 0.076(3) 0.077(3) -0.0340(18) -0.0123(18) -0.0037(18)
C3 0.080(3) 0.076(3) 0.079(3) -0.0355(18) -0.0089(18) -0.0022(18)
C51 0.082(2) 0.082(2) 0.082(2) -0.0349(12) -0.0135(10) -0.0036(10)
C60 0.082(3) 0.082(3) 0.082(3) -0.0344(13) -0.0136(11) -0.0039(10)
O30 0.157(9) 0.234(13) 0.088(7) -0.039(8) 0.003(6) -0.084(9)
C35 0.112(3) 0.113(3) 0.112(3) -0.0477(16) -0.0190(11) -0.0057(10)
C53 0.087(3) 0.091(3) 0.092(3) -0.0371(18) -0.0164(18) -0.0069(18)
O31 0.143(3) 0.142(3) 0.144(3) -0.0603(17) -0.0230(11) -0.0074(10)
C61 0.097(3) 0.097(3) 0.096(3) -0.040(2) -0.0160(19) -0.0035(19)
C62 0.102(3) 0.101(3) 0.102(3) -0.041(2) -0.0152(19) -0.0029(19)
C8 0.111(3) 0.110(3) 0.111(3) -0.0474(16) -0.0175(11) -0.0051(10)
C32 0.146(4) 0.146(4) 0.146(4) -0.062(2) -0.0242(12) -0.0072(10)
C52 0.096(3) 0.099(3) 0.099(3) -0.0386(19) -0.0177(19) -0.0037(18)
C36 0.126(4) 0.128(4) 0.126(4) -0.053(2) -0.022(2) -0.0056(19)
C57 0.168(5) 0.169(5) 0.169(5) -0.072(2) -0.0279(13) -0.0090(10)
C77 0.165(5) 0.165(5) 0.165(5) -0.070(2) -0.0268(12) -0.0087(10)
C22 0.134(3) 0.135(3) 0.134(3) -0.058(2) -0.0196(19) -0.0066(19)
C17 0.154(4) 0.154(4) 0.154(4) -0.066(2) -0.0249(12) -0.0078(10)
C26 0.152(4) 0.152(4) 0.152(4) -0.0643(19) -0.0249(12) -0.0077(10)
C29 0.191(5) 0.191(5) 0.191(5) -0.081(2) -0.0313(13) -0.0097(10)
C37 0.130(3) 0.130(3) 0.128(3) -0.054(2) -0.0199(19) -0.0060(19)
C9 0.128(4) 0.125(4) 0.127(4) -0.052(2) -0.020(2) -0.0057(19)
C55 0.183(5) 0.184(5) 0.183(5) -0.075(2) -0.029(2) -0.009(2)
C85 0.148(4) 0.150(4) 0.148(4) -0.062(2) -0.022(2) -0.0050(19)
C63 0.151(4) 0.152(4) 0.151(4) -0.0646(19) -0.0251(12) -0.0074(10)
C20 0.109(2) 0.108(2) 0.108(2) -0.0456(12) -0.0169(10) -0.0047(10)
C28 0.155(4) 0.155(4) 0.156(4) -0.066(2) -0.026(2) -0.0089(19)
C5 0.202(6) 0.202(6) 0.202(6) -0.086(3) -0.0331(13) -0.0105(10)
C10 0.120(4) 0.119(4) 0.120(4) -0.051(2) -0.021(2) -0.0047(19)
C78 0.172(5) 0.172(5) 0.173(5) -0.073(3) -0.027(2) -0.010(2)
C71 0.172(4) 0.171(4) 0.170(4) -0.072(2) -0.026(2) -0.0089(19)
C14 0.207(6) 0.207(6) 0.207(6) -0.088(3) -0.0334(14) -0.0103(10)
C83 0.105(2) 0.105(2) 0.105(2) -0.0440(12) -0.0166(10) -0.0049(10)
C23 0.134(3) 0.134(3) 0.134(3) -0.0568(14) -0.0211(11) -0.0072(10)
C27 0.161(5) 0.161(5) 0.161(5) -0.068(2) -0.024(2) -0.0085(19)
C7 0.208(6) 0.207(6) 0.207(6) -0.088(3) -0.033(2) -0.010(2)
C64 0.162(5) 0.163(5) 0.163(5) -0.070(2) -0.027(2) -0.0081(19)
C33 0.171(5) 0.169(5) 0.170(5) -0.072(2) -0.026(2) -0.0084(19)
C16 0.211(6) 0.209(6) 0.210(6) -0.089(3) -0.033(2) -0.010(2)
C79 0.175(5) 0.176(5) 0.176(5) -0.074(3) -0.028(2) -0.010(2)
C13 0.189(6) 0.189(6) 0.191(6) -0.080(3) -0.031(2) -0.010(2)
C21 0.145(4) 0.143(4) 0.143(4) -0.061(2) -0.021(2) -0.0059(19)
C34 0.172(5) 0.170(5) 0.171(5) -0.070(2) -0.029(2) -0.0087(19)
C19 0.171(5) 0.171(5) 0.171(5) -0.073(2) -0.025(2) -0.007(2)
C65 0.167(5) 0.168(5) 0.167(5) -0.071(2) -0.027(2) -0.0083(19)
C15 0.212(6) 0.212(6) 0.212(6) -0.089(3) -0.034(2) -0.011(2)
C18 0.173(5) 0.174(5) 0.174(5) -0.073(2) -0.028(2) -0.008(2)
C30 0.197(5) 0.199(5) 0.198(5) -0.084(3) -0.033(2) -0.008(2)
C59 0.182(5) 0.182(5) 0.182(5) -0.077(3) -0.030(2) -0.010(2)
C6 0.211(6) 0.210(6) 0.209(6) -0.089(3) -0.034(2) -0.011(2)
C84 0.140(4) 0.140(4) 0.139(4) -0.059(2) -0.022(2) -0.0071(19)
C81 0.296(8) 0.296(8) 0.296(8) -0.126(4) -0.0483(17) -0.0148(11)
C68 0.193(4) 0.192(4) 0.191(4) -0.082(2) -0.031(2) -0.0103(19)
C73 0.262(7) 0.262(7) 0.262(7) -0.112(3) -0.043(2) -0.013(2)
C75 0.230(5) 0.230(5) 0.229(5) -0.097(3) -0.037(2) -0.0120(19)
C56 0.173(4) 0.175(4) 0.173(4) -0.072(2) -0.028(2) -0.0083(19)
C69 0.130(3) 0.129(3) 0.129(3) -0.0551(14) -0.0205(11) -0.0070(10)
C74 0.263(7) 0.262(7) 0.263(7) -0.112(3) -0.043(2) -0.013(2)
C54 0.130(3) 0.131(3) 0.130(3) -0.0550(15) -0.0205(11) -0.0066(10)
C70 0.164(4) 0.164(4) 0.164(4) -0.070(2) -0.025(2) -0.0066(19)
C67 0.184(4) 0.184(4) 0.183(4) -0.078(2) -0.028(2) -0.009(2)
C58 0.189(5) 0.187(5) 0.188(5) -0.080(3) -0.031(2) -0.011(2)
C80 0.299(9) 0.300(9) 0.299(9) -0.126(4) -0.049(2) -0.015(2)
C31 0.199(5) 0.199(5) 0.199(5) -0.084(2) -0.031(2) -0.0088(19)
C76 0.239(6) 0.240(6) 0.240(6) -0.102(3) -0.039(2) -0.012(2)
C25 0.184(4) 0.183(4) 0.183(4) -0.076(2) -0.027(2) -0.009(2)
C66 0.139(3) 0.140(3) 0.138(3) -0.0603(14) -0.0240(11) -0.0090(10)
C24 0.189(4) 0.189(4) 0.189(4) -0.079(2) -0.029(2) -0.0099(19)
C72 0.261(7) 0.261(7) 0.261(7) -0.111(3) -0.0424(15) -0.0132(11)
C86 0.236(6) 0.236(6) 0.236(6) -0.100(3) -0.0382(14) -0.0118(10)
C82 0.300(9) 0.300(9) 0.299(9) -0.127(4) -0.049(2) -0.015(2)
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'
S S 0.1246 0.1234 '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
O39 Ti8 O9 96.9(3)
O39 Ti8 O5 95.9(3)
O9 Ti8 O5 142.7(2)
O39 Ti8 O17 170.5(3)
O9 Ti8 O17 88.0(2)
O5 Ti8 O17 84.8(2)
O39 Ti8 O8 100.7(3)
O9 Ti8 O8 72.2(2)
O5 Ti8 O8 71.0(2)
O17 Ti8 O8 88.5(2)
O39 Ti8 N1 86.8(3)
O9 Ti8 N1 143.4(2)
O5 Ti8 N1 72.1(2)
O17 Ti8 N1 84.4(2)
O8 Ti8 N1 142.9(2)
O39 Ti8 N2 92.2(3)
O9 Ti8 N2 75.1(2)
O5 Ti8 N2 139.0(2)
O17 Ti8 N2 81.2(2)
O8 Ti8 N2 146.1(3)
N1 Ti8 N2 68.3(3)
O39 Ti8 Ti9 103.1(2)
O9 Ti8 Ti9 35.59(16)
O5 Ti8 Ti9 107.26(17)
O17 Ti8 Ti9 85.68(15)
O8 Ti8 Ti9 36.76(17)
N1 Ti8 Ti9 170.06(19)
N2 Ti8 Ti9 109.81(19)
O39 Ti8 Ti7 98.9(2)
O9 Ti8 Ti7 108.31(17)
O5 Ti8 Ti7 34.91(16)
O17 Ti8 Ti7 87.15(15)
O8 Ti8 Ti7 36.17(17)
N1 Ti8 Ti7 106.99(19)
N2 Ti8 Ti7 167.80(18)
Ti9 Ti8 Ti7 72.73(6)
O27 Ti3 O21 96.5(3)
O27 Ti3 O28 95.9(3)
O21 Ti3 O28 143.3(3)
O27 Ti3 O32 168.6(3)
O21 Ti3 O32 87.9(2)
O28 Ti3 O32 86.7(3)
O27 Ti3 O24 102.2(3)
O21 Ti3 O24 72.5(2)
O28 Ti3 O24 71.2(2)
O32 Ti3 O24 89.1(2)
O27 Ti3 N3 90.5(3)
O21 Ti3 N3 74.5(3)
O28 Ti3 N3 139.7(3)
O32 Ti3 N3 80.5(2)
O24 Ti3 N3 145.8(3)
O27 Ti3 N4 85.8(3)
O21 Ti3 N4 142.1(3)
O28 Ti3 N4 73.1(3)
O32 Ti3 N4 84.3(3)
O24 Ti3 N4 144.0(3)
N3 Ti3 N4 67.6(3)
O27 Ti3 Ti2 103.7(2)
O21 Ti3 Ti2 35.69(15)
O28 Ti3 Ti2 107.70(19)
O32 Ti3 Ti2 85.97(15)
O24 Ti3 Ti2 36.95(16)
N3 Ti3 Ti2 109.3(2)
N4 Ti3 Ti2 170.2(2)
O27 Ti3 Ti4 100.7(2)
O21 Ti3 Ti4 108.35(16)
O28 Ti3 Ti4 35.24(19)
O32 Ti3 Ti4 87.79(15)
O24 Ti3 Ti4 35.92(16)
N3 Ti3 Ti4 167.9(2)
N4 Ti3 Ti4 108.3(2)
Ti2 Ti3 Ti4 72.66(5)
O18 Ti1 O19 98.4(3)
O18 Ti1 O21 162.2(3)
O19 Ti1 O21 99.2(3)
O18 Ti1 O25 93.5(3)
O19 Ti1 O25 96.9(3)
O21 Ti1 O25 81.8(2)
O18 Ti1 O20 106.8(3)
O19 Ti1 O20 97.5(3)
O21 Ti1 O20 73.4(2)
O25 Ti1 O20 153.0(2)
O18 Ti1 O33 82.7(3)
O19 Ti1 O33 178.8(3)
O21 Ti1 O33 79.7(2)
O25 Ti1 O33 83.5(2)
O20 Ti1 O33 81.8(2)
O18 Ti1 Ti2 142.9(2)
O19 Ti1 Ti2 99.2(2)
O21 Ti1 Ti2 35.01(15)
O25 Ti1 Ti2 116.42(18)
O20 Ti1 Ti2 38.45(17)
O33 Ti1 Ti2 79.60(14)
O23 Ti2 O22 107.5(4)
O23 Ti2 O24 104.6(4)
O22 Ti2 O24 97.5(3)
O23 Ti2 O21 110.4(4)
O22 Ti2 O21 141.7(3)
O24 Ti2 O21 78.2(2)
O23 Ti2 O20 103.3(4)
O22 Ti2 O20 92.4(3)
O24 Ti2 O20 145.9(2)
O21 Ti2 O20 74.0(2)
O23 Ti2 Ti3 115.4(3)
O22 Ti2 Ti3 126.3(2)
O24 Ti2 Ti3 42.50(16)
O21 Ti2 Ti3 35.87(16)
O20 Ti2 Ti3 106.91(16)
O23 Ti2 Ti1 110.1(3)
O22 Ti2 Ti1 123.0(2)
O24 Ti2 Ti1 112.23(17)
O21 Ti2 Ti1 35.69(16)
O20 Ti2 Ti1 38.33(16)
Ti3 Ti2 Ti1 70.06(5)
O37 Ti9 O36 107.1(4)
O37 Ti9 O8 103.8(3)
O36 Ti9 O8 99.2(3)
O37 Ti9 O9 111.6(3)
O36 Ti9 O9 140.8(3)
O8 Ti9 O9 77.6(2)
O37 Ti9 O10 102.9(3)
O36 Ti9 O10 92.1(3)
O8 Ti9 O10 146.4(3)
O9 Ti9 O10 73.8(2)
O37 Ti9 Ti8 115.6(3)
O36 Ti9 Ti8 126.8(2)
O8 Ti9 Ti8 42.06(17)
O9 Ti9 Ti8 35.64(16)
O10 Ti9 Ti8 107.03(18)
O37 Ti9 Ti10 111.6(3)
O36 Ti9 Ti10 121.6(3)
O8 Ti9 Ti10 111.62(18)
O9 Ti9 Ti10 35.65(17)
O10 Ti9 Ti10 38.18(17)
Ti8 Ti9 Ti10 69.86(5)
O7 Ti7 O6 110.1(4)
O7 Ti7 O8 105.0(3)
O6 Ti7 O8 99.7(3)
O7 Ti7 O5 121.5(4)
O6 Ti7 O5 127.2(4)
O8 Ti7 O5 78.2(3)
O7 Ti7 O2 97.6(3)
O6 Ti7 O2 91.9(3)
O8 Ti7 O2 149.0(3)
O5 Ti7 O2 72.0(2)
O7 Ti7 Ti8 122.2(3)
O6 Ti7 Ti8 119.5(3)
O8 Ti7 Ti8 41.71(18)
O5 Ti7 Ti8 36.52(17)
O2 Ti7 Ti8 107.90(18)
O7 Ti7 Ti6 112.0(3)
O6 Ti7 Ti6 116.5(3)
O8 Ti7 Ti6 112.28(19)
O5 Ti7 Ti6 34.17(18)
O2 Ti7 Ti6 38.01(17)
Ti8 Ti7 Ti6 70.58(5)
O3 Ti6 O1 109.6(4)
O3 Ti6 O5 114.9(4)
O1 Ti6 O5 135.4(3)
O3 Ti6 O11 98.6(3)
O1 Ti6 O11 91.4(3)
O5 Ti6 O11 81.0(2)
O3 Ti6 O2 102.8(4)
O1 Ti6 O2 98.6(3)
O5 Ti6 O2 73.2(2)
O11 Ti6 O2 151.6(3)
O3 Ti6 Ti7 111.4(3)
O1 Ti6 Ti7 126.3(3)
O5 Ti6 Ti7 33.88(16)
O11 Ti6 Ti7 114.6(2)
O2 Ti6 Ti7 39.52(18)
O13 Ti10 O14 98.2(3)
O13 Ti10 O9 99.2(3)
O14 Ti10 O9 162.6(2)
O13 Ti10 O12 98.9(3)
O14 Ti10 O12 94.1(3)
O9 Ti10 O12 81.9(2)
O13 Ti10 O10 96.3(3)
O14 Ti10 O10 105.2(3)
O9 Ti10 O10 74.2(3)
O12 Ti10 O10 153.4(3)
O13 Ti10 O15 177.9(3)
O14 Ti10 O15 83.4(2)
O9 Ti10 O15 79.3(2)
O12 Ti10 O15 82.4(2)
O10 Ti10 O15 81.9(2)
O13 Ti10 Ti9 99.5(2)
O14 Ti10 Ti9 141.7(2)
O9 Ti10 Ti9 35.05(16)
O12 Ti10 Ti9 116.19(19)
O10 Ti10 Ti9 39.15(19)
O15 Ti10 Ti9 78.38(15)
O38 Ti4 O35 108.6(5)
O38 Ti4 O24 104.5(3)
O35 Ti4 O24 100.1(4)
O38 Ti4 O28 119.2(4)
O35 Ti4 O28 131.2(5)
O24 Ti4 O28 77.8(3)
O38 Ti4 O29 97.6(4)
O35 Ti4 O29 93.5(4)
O24 Ti4 O29 148.5(3)
O28 Ti4 O29 72.0(3)
O38 Ti4 Ti3 119.3(3)
O35 Ti4 Ti3 123.3(4)
O24 Ti4 Ti3 41.83(18)
O28 Ti4 Ti3 35.9(2)
O29 Ti4 Ti3 107.5(2)
O38 Ti4 Ti5 111.3(3)
O35 Ti4 Ti5 118.9(4)
O24 Ti4 Ti5 111.94(19)
O28 Ti4 Ti5 34.3(2)
O29 Ti4 Ti5 37.7(2)
Ti3 Ti4 Ti5 70.15(6)
O16 S1 O15 115.6(4)
O16 S1 O17 111.7(4)
O15 S1 O17 111.3(3)
O16 S1 C38 107.6(4)
O15 S1 C38 105.5(4)
O17 S1 C38 104.1(4)
O34 S2 O33 116.7(4)
O34 S2 O32 112.1(4)
O33 S2 O32 110.5(3)
O34 S2 C47 107.1(4)
O33 S2 C47 105.7(4)
O32 S2 C47 103.5(4)
O31 Ti5 O30 109.7(6)
O31 Ti5 O28 129.0(4)
O30 Ti5 O28 121.3(5)
O31 Ti5 O29 99.1(4)
O30 Ti5 O29 100.3(4)
O28 Ti5 O29 73.8(3)
O31 Ti5 O26 94.7(4)
O30 Ti5 O26 94.8(4)
O28 Ti5 O26 81.1(3)
O29 Ti5 O26 154.8(3)
O31 Ti5 Ti4 122.4(4)
O30 Ti5 Ti4 114.7(4)
O28 Ti5 Ti4 34.53(18)
O29 Ti5 Ti4 39.4(2)
O26 Ti5 Ti4 115.6(2)
S1 O17 Ti8 134.7(3)
Ti2 O21 Ti3 108.4(2)
Ti2 O21 Ti1 109.3(3)
Ti3 O21 Ti1 136.6(3)
S2 O33 Ti1 134.2(4)
S2 O32 Ti3 132.7(3)
S1 O15 Ti10 132.7(4)
Ti9 O9 Ti8 108.8(3)
Ti9 O9 Ti10 109.3(3)
Ti8 O9 Ti10 136.5(3)
Ti4 O24 Ti2 155.8(3)
Ti4 O24 Ti3 102.2(3)
Ti2 O24 Ti3 100.5(2)
Ti7 O8 Ti9 155.4(4)
Ti7 O8 Ti8 102.1(3)
Ti9 O8 Ti8 101.2(3)
Ti7 O5 Ti6 112.0(3)
Ti7 O5 Ti8 108.6(3)
Ti6 O5 Ti8 139.0(3)
N2 O12 Ti10 122.8(5)
N3 O25 Ti1 120.7(4)
C60 O20 Ti1 131.2(6)
C60 O20 Ti2 125.4(5)
Ti1 O20 Ti2 103.2(3)
C57 O18 Ti1 153.4(9)
N1 O11 Ti6 120.9(5)
C35 O10 Ti10 131.7(7)
C35 O10 Ti9 125.6(7)
Ti10 O10 Ti9 102.7(3)
C2 N2 O12 117.3(7)
C2 N2 Ti8 120.2(6)
O12 N2 Ti8 121.3(5)
Ti5 O28 Ti4 111.2(3)
Ti5 O28 Ti3 139.6(3)
Ti4 O28 Ti3 108.8(3)
C8 O2 Ti6 129.3(7)
C8 O2 Ti7 128.2(7)
Ti6 O2 Ti7 102.5(3)
C23 O39 Ti8 151.3(7)
C69 O27 Ti3 147.8(9)
C32 O14 Ti10 150.5(8)
C1 N1 O11 116.4(7)
C1 N1 Ti8 120.9(6)
O11 N1 Ti8 121.8(5)
C29 O13 Ti10 133.4(10)
C54 O19 Ti1 136.6(8)
C50 N3 O25 116.1(7)
C50 N3 Ti3 121.2(6)
O25 N3 Ti3 122.7(5)
C20 O36 Ti9 161.2(8)
C77 O29 Ti5 131.6(9)
C77 O29 Ti4 125.4(9)
Ti5 O29 Ti4 102.9(3)
C63 O22 Ti2 146.5(10)
C66 O23 Ti2 158.4(10)
C26 O37 Ti9 135.0(9)
N4 O26 Ti5 122.2(5)
C83 O38 Ti4 151.7(8)
C51 N4 O26 116.8(8)
C51 N4 Ti3 120.5(7)
O26 N4 Ti3 122.4(5)
N1 C1 C2 113.6(8)
N1 C1 C4 121.3(8)
C2 C1 C4 125.1(9)
C5 O1 Ti6 147.1(12)
C45 C44 C49 116.3(9)
C45 C44 C43 122.4(8)
C49 C44 C43 121.1(9)
C46 C47 C48 119.8(9)
C46 C47 S2 119.9(8)
C48 C47 S2 120.3(7)
C17 O7 Ti7 161.8(10)
N2 C2 C1 116.1(8)
N2 C2 C3 122.7(8)
C1 C2 C3 121.2(8)
C41 C38 C39 121.4(9)
C41 C38 S1 119.1(7)
C39 C38 S1 119.5(7)
C42 C43 C40 116.8(9)
C42 C43 C44 122.3(8)
C40 C43 C44 120.9(8)
C40 C39 C38 119.4(9)
C44 C45 C46 123.6(9)
C11 O3 Ti6 152.0(12)
C47 C46 C45 118.5(9)
C14 O6 Ti7 149.8(13)
N3 C50 C51 114.0(9)
N3 C50 C53 120.9(9)
C51 C50 C53 125.1(9)
C43 C42 C41 122.8(9)
C39 C40 C43 121.3(8)
C38 C41 C42 118.2(9)
C48 C49 C44 120.7(9)
C47 C48 C49 120.5(9)
C86 O35 Ti4 154.0(16)
N4 C51 C50 116.3(9)
N4 C51 C52 120.4(9)
C50 C51 C52 123.2(9)
O20 C60 C62 107.7(8)
O20 C60 C61 112.0(9)
C62 C60 C61 111.6(9)
C81 O30 Ti5 159.3(12)
O10 C35 C36 111.5(11)
O10 C35 C37 112.1(11)
C36 C35 C37 111.4(12)
C72 O31 Ti5 148.7(15)
C9 C8 C10 115.4(13)
C9 C8 O2 111.7(11)
C10 C8 O2 113.0(11)
O14 C32 C33 119.4(15)
O14 C32 C34 108.6(13)
C33 C32 C34 112.7(14)
O18 C57 C58 114.5(15)
O18 C57 C59 106.6(13)
C58 C57 C59 119.6(16)
C79 C77 O29 106.6(16)
C79 C77 C78 124.1(19)
O29 C77 C78 110.7(16)
C19 C17 O7 108.8(15)
C19 C17 C18 118.1(17)
O7 C17 C18 109.3(16)
O37 C26 C27 112.6(14)
O37 C26 C28 108.1(14)
C27 C26 C28 110.2(14)
O13 C29 C30 102.8(17)
O13 C29 C31 95.5(15)
C30 C29 C31 105.3(18)
O22 C63 C64 112.2(16)
O22 C63 C65 115.6(16)
C64 C63 C65 117.3(17)
O36 C20 C21 105.4(12)
O36 C20 C22 112.4(11)
C21 C20 C22 116.1(13)
C6 C5 O1 114(2)
C6 C5 C7 103.5(19)
O1 C5 C7 107.7(18)
O6 C14 C15 116(2)
O6 C14 C16 110(2)
C15 C14 C16 113(2)
C84 C83 O38 113.1(12)
C84 C83 C85 120.3(13)
O38 C83 C85 104.0(10)
C25 C23 C24 119.8(15)
C25 C23 O39 103.8(14)
C24 C23 O39 86.7(11)
C80 C81 C82 149(3)
C80 C81 O30 95(2)
C82 C81 O30 96(2)
O27 C69 C70 113.4(13)
O27 C69 C71 109.9(12)
C70 C69 C71 98.4(13)
O19 C54 C56 115.5(13)
O19 C54 C55 113.2(13)
C56 C54 C55 126.8(16)
O23 C66 C68 107.8(14)
O23 C66 C67 114.6(14)
C68 C66 C67 128.0(18)
C74 C72 C73 111(3)
C74 C72 O31 108(3)
C73 C72 O31 117(3)
O35 C86 C75 120(3)
O35 C86 C76 121(3)
C75 C86 C76 117(3)
O3 C11 C13 117.7(18)
O3 C11 C12 122.7(19)
C13 C11 C12 119(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Ti8 O39 1.772(6)
Ti8 O9 1.921(6)
Ti8 O5 1.966(6)
Ti8 O17 2.102(5)
Ti8 O8 2.132(6)
Ti8 N1 2.253(7)
Ti8 N2 2.255(7)
Ti8 Ti9 3.122(2)
Ti8 Ti7 3.132(2)
Ti3 O27 1.744(7)
Ti3 O21 1.926(5)
Ti3 O28 1.947(7)
Ti3 O32 2.135(6)
Ti3 O24 2.143(6)
Ti3 N3 2.250(7)
Ti3 N4 2.252(8)
Ti3 Ti2 3.118(2)
Ti3 Ti4 3.140(2)
Ti1 O18 1.765(6)
Ti1 O19 1.769(7)
Ti1 O21 1.950(5)
Ti1 O25 1.975(6)
Ti1 O20 2.010(6)
Ti1 O33 2.336(6)
Ti1 Ti2 3.155(2)
Ti2 O23 1.752(11)
Ti2 O22 1.786(7)
Ti2 O24 1.906(6)
Ti2 O21 1.918(5)
Ti2 O20 2.015(6)
Ti9 O37 1.761(7)
Ti9 O36 1.796(7)
Ti9 O8 1.904(6)
Ti9 O9 1.919(5)
Ti9 O10 2.041(7)
Ti9 Ti10 3.153(2)
Ti7 O7 1.741(8)
Ti7 O6 1.769(8)
Ti7 O8 1.891(6)
Ti7 O5 1.891(5)
Ti7 O2 2.051(6)
Ti7 Ti6 3.147(2)
Ti6 O3 1.713(8)
Ti6 O1 1.759(8)
Ti6 O5 1.906(6)
Ti6 O11 1.964(6)
Ti6 O2 1.984(6)
Ti10 O13 1.778(6)
Ti10 O14 1.785(6)
Ti10 O9 1.947(6)
Ti10 O12 1.968(6)
Ti10 O10 1.998(6)
Ti10 O15 2.389(5)
Ti4 O38 1.736(9)
Ti4 O35 1.749(8)
Ti4 O24 1.885(6)
Ti4 O28 1.914(6)
Ti4 O29 2.049(7)
Ti4 Ti5 3.148(3)
S1 O16 1.440(6)
S1 O15 1.446(6)
S1 O17 1.485(6)
S1 C38 1.797(9)
S2 O34 1.425(6)
S2 O33 1.444(6)
S2 O32 1.469(6)
S2 C47 1.769(9)
Ti5 O31 1.737(11)
Ti5 O30 1.778(11)
Ti5 O28 1.903(7)
Ti5 O29 1.977(8)
Ti5 O26 1.984(7)
O12 N2 1.345(8)
O25 N3 1.356(8)
O20 C60 1.437(11)
O18 C57 1.430(18)
O11 N1 1.317(8)
O10 C35 1.414(14)
N2 C2 1.281(10)
O2 C8 1.463(13)
O39 C23 1.511(16)
O27 C69 1.311(15)
O14 C32 1.352(16)
N1 C1 1.304(11)
O13 C29 1.47(2)
O19 C54 1.407(16)
N3 C50 1.300(11)
O36 C20 1.365(14)
O29 C77 1.479(18)
O22 C63 1.360(18)
O23 C66 1.392(17)
O37 C26 1.389(18)
O26 N4 1.328(9)
O38 C83 1.419(14)
N4 C51 1.282(11)
C1 C2 1.438(12)
C1 C4 1.456(12)
O1 C5 1.39(2)
C44 C45 1.344(12)
C44 C49 1.387(11)
C44 C43 1.492(13)
C47 C46 1.356(11)
C47 C48 1.357(12)
O7 C17 1.412(18)
C2 C3 1.513(12)
C38 C41 1.362(12)
C38 C39 1.367(11)
C43 C42 1.356(11)
C43 C40 1.410(12)
C39 C40 1.342(12)
C45 C46 1.386(12)
O3 C11 1.31(2)
O6 C14 1.39(2)
C50 C51 1.407(13)
C50 C53 1.502(13)
C42 C41 1.365(12)
C49 C48 1.377(12)
O35 C86 1.27(3)
C51 C52 1.524(14)
C60 C62 1.497(15)
C60 C61 1.498(14)
O30 C81 1.61(3)
C35 C36 1.464(16)
C35 C37 1.489(17)
O31 C72 1.47(3)
C8 C9 1.402(17)
C8 C10 1.433(15)
C32 C33 1.472(9)
C32 C34 1.56(2)
C57 C58 1.475(9)
C57 C59 1.62(2)
C77 C79 1.40(2)
C77 C78 1.49(2)
C22 C20 1.499(17)
C17 C19 1.38(2)
C17 C18 1.46(2)
C26 C27 1.51(2)
C26 C28 1.61(2)
C29 C30 1.47(2)
C29 C31 1.65(3)
C55 C54 1.63(2)
C85 C83 1.553(17)
C63 C64 1.39(2)
C63 C65 1.44(2)
C20 C21 1.471(16)
C5 C6 1.35(2)
C5 C7 1.63(2)
C71 C69 1.62(2)
C14 C15 1.41(2)
C14 C16 1.49(3)
C83 C84 1.376(16)
C23 C25 1.43(2)
C23 C24 1.4998(10)
C13 C11 1.477(9)
C81 C80 1.486(10)
C81 C82 1.4998(10)
C68 C66 1.46(2)
C73 C72 1.39(3)
C75 C86 1.37(3)
C56 C54 1.45(2)
C69 C70 1.466(9)
C74 C72 1.39(3)
C67 C66 1.478(9)
C76 C86 1.40(3)
C11 C12 1.481(10)