#------------------------------------------------------------------------------ #$Date: 2019-11-07 22:50:16 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223870 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551222.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_1551222 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 'C96 H198 N4 O46 Ti12' _chemical_formula_sum 'C96 H198 N4 O46 Ti12' _chemical_formula_weight 2718.99 _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 geom _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 93.516(4) _cell_angle_beta 111.982(4) _cell_angle_gamma 100.404(4) _cell_formula_units_Z 1 _cell_length_a 14.7714(7) _cell_length_b 15.1120(7) _cell_length_c 16.8580(7) _cell_measurement_reflns_used 5232 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 25.8420 _cell_measurement_theta_min 3.6500 _cell_volume 3397.7(3) _computing_cell_refinement 'Bruker FRAMBO' _computing_data_collection 'Bruker FRAMBO' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_structure_solution 'Bruker SHELXTL' _diffrn_ambient_temperature 293(2) _diffrn_detector_area_resol_mean 16.2083 _diffrn_measured_fraction_theta_full 0.968 _diffrn_measured_fraction_theta_max 0.996 _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 0.0528 _diffrn_reflns_av_unetI/netI 0.1360 _diffrn_reflns_Laue_measured_fraction_full 0.968 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 24431 _diffrn_reflns_point_group_measured_fraction_full 0.968 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.442 _diffrn_source 'fine-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 0.735 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.68263 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.269 _exptl_crystal_description block _exptl_crystal_F_000 1364 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.488 _refine_diff_density_min -1.678 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.090 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 676 _refine_ls_number_reflns 11911 _refine_ls_number_restraints 410 _refine_ls_restrained_S_all 1.132 _refine_ls_R_factor_all 0.1663 _refine_ls_R_factor_gt 0.1115 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1910P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3081 _refine_ls_wR_factor_ref 0.3594 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6247 _reflns_number_total 11911 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt02032b2.cif _cod_data_source_block a_CCDC4 _cod_depositor_comments 'Adding full bibliography for 1551215--1551222.cif.' _cod_database_code 1551222 _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. ; _oxdiff_exptl_absorpt_empirical_full_min 0.599 _oxdiff_exptl_absorpt_empirical_full_max 1.606 _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _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 0.220, Rweak 0.027, Alpha 0.073, Orientation as input REM Formula found by SHELXT: C37 N6 O19 Ti6 CELL 0.71073 14.7714 15.112 16.858 93.516 111.982 100.404 ZERR 1 0.0007 0.0007 0.0007 0.004 0.004 0.004 LATT 1 SFAC C H N O Ti UNIT 90 180 4 44 12 DFIX 1.5 0.01 C4 C5 DFIX 1.5 0.01 C22 C23 DFIX 1.5 0.01 C19 C21 DFIX 1.5 0.01 C40 C42 DFIX 1.5 0.01 C40 C41 DELU C22 C23 DELU 0.02 0.01 C4 C5 DELU C4 C6 DELU C19 C21 DELU C19 C20 DELU 0.02 0.01 O2 C4 DELU 0.008 0.004 O2 O2 C4 C4 DELU 0.008 0.004 O7 C14 DELU 0.008 0.004 O18 C43 DELU 0.0002 0.0001 O8 C14 DELU 0.0002 0.0001 O9 C16 DELU 0.0002 0.0001 O10 C16 DELU 0.0002 0.0001 O13 C31 DELU 0.0002 0.0001 O16 C28 DELU 0.0002 0.0001 O17 C25 DELU 0.0002 0.0001 O20 C22 SIMU 0.01 0.02 2 O16 Ti4 C28 SIMU 0.01 0.02 2 O19 Ti2 C19 SIMU 0.01 0.02 2 C1 O1 C2 C3 SIMU 0.01 0.02 2 C22 O20 C23 C24 SIMU 0.01 0.02 3.8 $C SIMU 0.01 0.02 3.8 C15 C15 C18 C18 C17 C17 C16 C16 C14 C14 C11 C11 C10 C10 = C12 C12 C31 C31 C37 C37 C7 C7 C13 C13 C43 C43 C34 C34 C32 C32 C25 C25 C33 = C33 C27 C27 C36 C36 C38 C38 C26 C26 C35 C35 C8 C8 C9 C9 C44 C44 C40 C40 C30 = C30 C22 C22 C1 C1 C4 C4 C28 C28 C39 C39 C45 C45 C41 C41 C6 C6 C29 C29 C24 = C24 C42 C42 C5 C5 C19 C19 C23 C23 C3 C3 C2 C2 C20 C20 C21 C21 SIMU 0.005 0.01 3.8 C29 C28 C30 C24 C23 C3 C2 C5 C6 C4 C42 C41 C40 C20 C19 C21 SIMU 0.0005 0.001 3.8 C23 C24 C6 C4 C5 C21 C20 C19 C3 C2 C42 C40 C41 C29 = C28 C30 SIMU 0.005 0.01 3.8 C11 C10 C12 C31 C37 C7 C13 C43 C34 C32 C25 C33 C27 C36 = C38 C26 C35 C8 C9 C44 C40 C30 C22 C1 C4 C28 C39 C45 C41 C6 C29 C24 C42 C5 = C19 C23 C3 C2 C20 C21 SIMU 0.0005 0.001 3.8 C15 C18 C17 C16 C14 C11 C10 C12 C31 C37 C7 C13 C43 = C34 C32 C25 C33 C27 C36 C38 C26 C35 C8 C9 C44 C40 C30 C22 C1 C4 C28 C39 C45 = C41 C6 C29 C24 C42 C5 C19 C23 C3 C2 C20 C21 ISOR 0.01 0.02 C5 ISOR 0.01 0.02 C21 L.S. 20 PLAN 4 BOND $H list 4 ABIN fmap 2 acta OMIT 0 50 OMIT 1 1 5 OMIT -1 -5 6 OMIT 0 4 3 OMIT -6 -1 7 OMIT -6 -4 3 OMIT -5 4 0 OMIT -1 -7 6 OMIT -6 -6 3 OMIT -4 -3 8 OMIT -4 8 4 OMIT -4 2 5 OMIT -2 -4 5 OMIT -5 4 4 OMIT -14 -3 6 OMIT -3 4 6 REM REM REM WGHT 0.191000 FVAR 4.72847 TI3 5 0.214032 0.819016 0.720656 11.00000 0.04335 0.03442 = 0.03267 0.00228 0.01141 0.00480 TI5 5 0.196420 0.871781 0.504539 11.00000 0.04513 0.03171 = 0.04039 0.01251 0.01702 0.00679 TI4 5 0.358590 0.786869 0.633803 11.00000 0.03570 0.03858 = 0.04531 0.00678 0.01332 0.00317 TI6 5 0.332664 0.565619 0.631222 11.00000 0.04463 0.04375 = 0.04758 0.00862 0.01720 0.01444 TI2 5 0.318568 0.669017 0.804602 11.00000 0.05001 0.04556 = 0.03736 0.01199 0.01127 0.01218 TI1 5 0.142764 0.677432 0.862742 11.00000 0.06367 0.05139 = 0.03331 0.01023 0.01973 0.01252 O10 4 0.123246 0.725038 0.485074 11.00000 0.03028 0.04606 = 0.03721 -0.00237 0.00842 -0.00283 O8 4 0.122553 0.703540 0.649216 11.00000 0.04019 0.04800 = 0.02953 -0.00283 0.01293 0.01003 O9 4 0.242636 0.663658 0.570027 11.00000 0.05181 0.02683 = 0.04600 0.01307 0.02750 0.00495 O11 4 0.338122 0.759083 0.733553 11.00000 0.04499 0.04016 = 0.03147 0.00858 0.00876 0.00346 O6 4 0.236171 0.745770 0.817463 11.00000 0.04381 0.04039 = 0.02826 0.00317 0.00991 0.00604 O12 4 0.259468 0.849811 0.627105 11.00000 0.04333 0.02678 = 0.03745 0.00845 0.01605 0.00563 O13 4 0.316583 0.817493 0.512272 11.00000 0.03307 0.03610 = 0.05807 0.01136 0.01136 -0.00395 O7 4 0.060679 0.608068 0.722073 11.00000 0.05889 0.04247 = 0.03359 0.00206 0.01814 -0.01144 O5 4 0.095975 0.896207 0.546579 11.00000 0.06040 0.04080 = 0.03680 0.01544 0.02197 0.01654 O17 4 0.419897 0.676941 0.621735 11.00000 0.05386 0.04537 = 0.06143 0.01911 0.02196 0.00736 O22 4 0.267682 0.924738 0.788873 11.00000 0.06414 0.03665 = 0.05072 -0.00910 0.01396 0.00011 O15 4 0.120122 0.860020 0.390766 11.00000 0.05945 0.04843 = 0.04756 0.02379 0.01916 0.02172 O21 4 0.292514 0.574073 0.719238 11.00000 0.06143 0.04051 = 0.05236 0.00986 0.02174 0.00898 O3 4 0.235833 0.596856 0.859181 11.00000 0.07620 0.04258 = 0.03698 0.01588 0.01754 0.01174 O4 4 0.072667 0.775331 0.823185 11.00000 0.06438 0.05749 = 0.04984 0.01718 0.03099 0.02070 O16 4 0.474622 0.866029 0.678193 11.00000 0.05226 0.06327 = 0.07265 0.02364 0.02766 0.01012 O18 4 0.251242 0.484884 0.536865 11.00000 0.05278 0.04763 = 0.06314 0.00386 0.01037 0.02160 O14 4 0.259956 0.986286 0.515748 11.00000 0.05059 0.03508 = 0.06927 0.01317 0.02072 0.00146 N1 3 0.093075 0.873224 0.621516 11.00000 0.04551 0.03212 = 0.04671 0.00240 0.01749 0.00742 N2 3 0.079200 0.814427 0.754921 11.00000 0.05793 0.04194 = 0.03244 0.00887 0.01843 0.01759 O2 4 0.209569 0.725640 0.974883 11.00000 0.07818 0.07038 = 0.04010 0.00695 0.01472 0.01341 O1 4 0.039803 0.604435 0.873813 11.00000 0.07209 0.08429 = 0.07248 0.02598 0.04476 0.01022 C15 1 0.037330 0.557131 0.577061 11.00000 0.05106 0.05823 = 0.06804 0.01632 0.03351 0.01669 O20 4 0.424701 0.501265 0.673928 11.00000 0.05760 0.06193 = 0.09406 0.00346 0.02312 0.02142 C18 1 0.030032 0.519624 0.433230 11.00000 0.05133 0.05849 = 0.06834 0.01616 0.03327 0.01666 AFIX 43 H18 2 0.049081 0.533712 0.387996 11.00000 -1.20000 AFIX 0 O19 4 0.438485 0.678805 0.886239 11.00000 0.07316 0.09584 = 0.05520 0.02104 -0.00097 0.02909 C17 1 0.071995 0.578732 0.511022 11.00000 0.05108 0.05825 = 0.06802 0.01629 0.03349 0.01669 C16 1 0.151177 0.661475 0.524259 11.00000 0.05126 0.05862 = 0.06832 0.01637 0.03328 0.01675 C14 1 0.076213 0.626736 0.657374 11.00000 0.05108 0.05817 = 0.06803 0.01640 0.03357 0.01653 C11 1 0.016102 0.884864 0.636007 11.00000 0.05731 0.04977 = 0.05727 0.01019 0.02664 0.02089 C10 1 0.010324 0.851911 0.714991 11.00000 0.05734 0.04989 = 0.05729 0.01015 0.02663 0.02091 C12 1 -0.065117 0.923676 0.573941 11.00000 0.05768 0.05014 = 0.05768 0.01046 0.02590 0.02080 AFIX 33 H12A 2 -0.115506 0.926842 0.596415 11.00000 -1.50000 H12B 2 -0.036989 0.983558 0.566751 11.00000 -1.50000 H12C 2 -0.094632 0.885369 0.519090 11.00000 -1.50000 AFIX 0 C31 1 0.353875 0.796350 0.447491 11.00000 0.05707 0.07556 = 0.07822 0.01315 0.03084 0.01544 AFIX 13 H31 2 0.420637 0.784298 0.476677 11.00000 -1.20000 AFIX 0 C37 1 0.036644 0.807293 0.321539 11.00000 0.09334 0.12235 = 0.04845 -0.00289 0.01175 0.00140 AFIX 13 H37 2 0.041627 0.743819 0.325713 11.00000 -1.20000 AFIX 0 C7 1 0.243983 0.509446 0.882766 11.00000 0.12565 0.07128 = 0.10459 0.04285 0.05875 0.03849 AFIX 13 H7 2 0.310666 0.502648 0.888082 11.00000 -1.20000 AFIX 0 C13 1 -0.077624 0.856368 0.738567 11.00000 0.05773 0.05046 = 0.05765 0.01008 0.02648 0.02062 AFIX 33 H13A 2 -0.120965 0.888392 0.698948 11.00000 -1.50000 H13B 2 -0.113795 0.795864 0.735553 11.00000 -1.50000 H13C 2 -0.054211 0.887691 0.796238 11.00000 -1.50000 AFIX 0 C43 1 0.244805 0.391799 0.512028 11.00000 0.05707 0.06268 = 0.07607 0.01241 0.02724 0.01643 AFIX 13 H43 2 0.311146 0.377523 0.535797 11.00000 -1.20000 AFIX 0 C34 1 0.341168 1.056192 0.572612 11.00000 0.08046 0.07194 = 0.11904 0.01513 0.02362 0.00238 AFIX 13 H34 2 0.400254 1.030441 0.598142 11.00000 -1.20000 AFIX 0 C32 1 0.287614 0.712281 0.387639 11.00000 0.05553 0.06983 = 0.07451 0.01424 0.03166 0.01579 AFIX 33 H32A 2 0.313123 0.698771 0.344697 11.00000 -1.50000 H32B 2 0.286176 0.662298 0.419978 11.00000 -1.50000 H32C 2 0.221082 0.721902 0.359889 11.00000 -1.50000 AFIX 0 C25 1 0.520276 0.688181 0.620623 11.00000 0.05808 0.07776 = 0.08035 0.01280 0.02945 0.01503 AFIX 13 H25 2 0.537485 0.748354 0.604748 11.00000 -1.20000 AFIX 0 C33 1 0.363570 0.875517 0.400607 11.00000 0.05680 0.07330 = 0.07663 0.01403 0.03112 0.01542 AFIX 33 H33A 2 0.388482 0.860773 0.357552 11.00000 -1.50000 H33B 2 0.299248 0.889905 0.373246 11.00000 -1.50000 H33C 2 0.409233 0.926935 0.440783 11.00000 -1.50000 AFIX 0 C27 1 0.596724 0.685250 0.709600 11.00000 0.06382 0.08309 = 0.08630 0.01188 0.02336 0.01366 AFIX 33 H27A 2 0.661848 0.692675 0.707844 11.00000 -1.50000 H27B 2 0.597000 0.733397 0.749637 11.00000 -1.50000 H27C 2 0.579871 0.627816 0.727823 11.00000 -1.50000 AFIX 0 C36 1 0.310366 1.090327 0.645419 11.00000 0.08109 0.07233 = 0.11921 0.01499 0.02351 0.00211 AFIX 33 H36A 2 0.363556 1.137679 0.685100 11.00000 -1.50000 H36B 2 0.251012 1.113570 0.620634 11.00000 -1.50000 H36C 2 0.297461 1.040865 0.675595 11.00000 -1.50000 AFIX 0 C38 1 -0.056271 0.815949 0.333305 11.00000 0.09353 0.12272 = 0.04908 -0.00290 0.01150 0.00119 AFIX 33 H38A 2 -0.113255 0.779854 0.285913 11.00000 -1.50000 H38B 2 -0.054423 0.795127 0.386443 11.00000 -1.50000 H38C 2 -0.061195 0.878462 0.335162 11.00000 -1.50000 AFIX 0 C26 1 0.515336 0.617489 0.549949 11.00000 0.06106 0.08102 = 0.08363 0.01209 0.02661 0.01468 AFIX 33 H26A 2 0.580303 0.623612 0.548067 11.00000 -1.50000 H26B 2 0.494216 0.557752 0.561986 11.00000 -1.50000 H26C 2 0.468372 0.626516 0.495217 11.00000 -1.50000 AFIX 0 C35 1 0.365458 1.132537 0.524449 11.00000 0.08056 0.07213 = 0.11935 0.01503 0.02374 0.00206 AFIX 33 H35A 2 0.420258 1.178742 0.563956 11.00000 -1.50000 H35B 2 0.383591 1.109034 0.479634 11.00000 -1.50000 H35C 2 0.307890 1.158136 0.499285 11.00000 -1.50000 AFIX 0 C8 1 0.171749 0.437452 0.813135 11.00000 0.12602 0.07168 = 0.10504 0.04232 0.05868 0.03828 AFIX 33 H8A 2 0.178785 0.378976 0.830699 11.00000 -1.50000 H8B 2 0.104914 0.444443 0.801859 11.00000 -1.50000 H8C 2 0.184652 0.442195 0.761641 11.00000 -1.50000 AFIX 0 C9 1 0.241010 0.501435 0.968332 11.00000 0.12587 0.07174 = 0.10480 0.04272 0.05864 0.03834 AFIX 33 H9A 2 0.246727 0.441385 0.981895 11.00000 -1.50000 H9B 2 0.295561 0.545269 1.011098 11.00000 -1.50000 H9C 2 0.178801 0.512424 0.967839 11.00000 -1.50000 AFIX 0 C44 1 0.204280 0.378914 0.414409 11.00000 0.05630 0.06237 = 0.07464 0.01313 0.02832 0.01594 AFIX 33 H44A 2 0.198071 0.316734 0.393283 11.00000 -1.50000 H44B 2 0.139787 0.393991 0.392082 11.00000 -1.50000 H44C 2 0.249247 0.417835 0.395874 11.00000 -1.50000 AFIX 0 C40 1 0.278861 0.977194 0.860102 11.00000 0.24056 0.13170 = 0.07915 -0.01154 0.04192 0.07913 AFIX 13 H40 2 0.225140 0.938274 0.870840 11.00000 -1.20000 AFIX 0 C30 1 0.650838 0.936414 0.748271 11.00000 0.06630 0.08688 = 0.08994 0.00821 0.01999 0.00982 AFIX 33 H30A 2 0.651228 0.896909 0.701635 11.00000 -1.50000 H30B 2 0.678619 0.998053 0.745305 11.00000 -1.50000 H30C 2 0.690201 0.919412 0.802372 11.00000 -1.50000 AFIX 0 C22 1 0.480036 0.457178 0.743693 11.00000 0.06952 0.08588 = 0.09015 0.01418 0.01865 0.01524 AFIX 13 H22 2 0.526365 0.500670 0.794330 11.00000 -1.20000 AFIX 0 C1 1 -0.064415 0.570388 0.831208 11.00000 0.11673 0.14506 = 0.15961 0.01131 0.05757 0.00071 AFIX 13 H1 2 -0.080850 0.589434 0.773850 11.00000 -1.20000 AFIX 0 C4 1 0.192445 0.731315 1.047670 11.00000 0.19138 0.21069 = 0.07396 0.00640 0.05707 0.02412 AFIX 13 H4 2 0.141608 0.677700 1.043653 11.00000 -1.20000 AFIX 0 C28 1 0.548907 0.928667 0.741481 11.00000 0.06679 0.08802 = 0.09091 0.00618 0.01887 0.00814 C39 1 0.041926 0.826065 0.240119 11.00000 0.09388 0.12295 = 0.04894 -0.00269 0.01136 0.00104 AFIX 33 H39A 2 -0.015555 0.789581 0.193443 11.00000 -1.50000 H39B 2 0.043212 0.889211 0.235320 11.00000 -1.50000 H39C 2 0.101626 0.811867 0.237533 11.00000 -1.50000 AFIX 0 C45 1 0.172584 0.332425 0.544092 11.00000 0.05792 0.06314 = 0.07681 0.01285 0.02649 0.01569 AFIX 33 H45A 2 0.168158 0.269412 0.527328 11.00000 -1.50000 H45B 2 0.197181 0.345055 0.605912 11.00000 -1.50000 H45C 2 0.107480 0.345866 0.518987 11.00000 -1.50000 AFIX 0 C41 1 0.231381 1.055416 0.844546 11.00000 0.24067 0.13175 = 0.07943 -0.01177 0.04194 0.07916 AFIX 33 H41A 2 0.243018 1.089208 0.898852 11.00000 -1.50000 H41B 2 0.259412 1.093829 0.812410 11.00000 -1.50000 H41C 2 0.160683 1.034330 0.812209 11.00000 -1.50000 AFIX 0 C6 1 0.269598 0.740224 1.124105 11.00000 0.19152 0.21078 = 0.07429 0.00635 0.05675 0.02414 AFIX 33 H6A 2 0.245934 0.743388 1.169821 11.00000 -1.50000 H6B 2 0.299864 0.688821 1.126176 11.00000 -1.50000 H6C 2 0.318183 0.794837 1.130993 11.00000 -1.50000 AFIX 0 C29 1 0.519792 0.974740 0.796534 11.00000 0.06733 0.08847 = 0.09124 0.00681 0.01904 0.00822 AFIX 33 H29A 2 0.576841 1.016958 0.838482 11.00000 -1.50000 H29B 2 0.471009 1.007221 0.764418 11.00000 -1.50000 H29C 2 0.491026 0.932484 0.825467 11.00000 -1.50000 AFIX 0 C24 1 0.533092 0.397644 0.709192 11.00000 0.07227 0.08773 = 0.09209 0.01434 0.01703 0.01518 AFIX 33 H24A 2 0.570795 0.367222 0.754478 11.00000 -1.50000 H24B 2 0.484573 0.353372 0.662446 11.00000 -1.50000 H24C 2 0.577538 0.434602 0.688782 11.00000 -1.50000 AFIX 0 C42 1 0.359784 0.969182 0.941211 11.00000 0.24081 0.13210 = 0.07944 -0.01157 0.04171 0.07889 AFIX 33 H42A 2 0.360363 1.009902 0.987489 11.00000 -1.50000 H42B 2 0.348997 0.907903 0.953573 11.00000 -1.50000 H42C 2 0.422825 0.984508 0.935527 11.00000 -1.50000 AFIX 0 C5 1 0.150313 0.812013 1.049203 11.00000 0.19152 0.21086 = 0.07442 0.00629 0.05688 0.02410 AFIX 33 H5A 2 0.094527 0.808741 0.995539 11.00000 -1.50000 H5B 2 0.128293 0.814388 1.095977 11.00000 -1.50000 H5C 2 0.200582 0.865654 1.057094 11.00000 -1.50000 AFIX 0 C19 1 0.509960 0.718129 0.961000 11.00000 0.12821 0.18522 = 0.11492 -0.01134 -0.00378 0.03632 AFIX 13 H19 2 0.529970 0.777839 0.945491 11.00000 -1.20000 AFIX 0 C23 1 0.411066 0.388629 0.764951 11.00000 0.07228 0.08770 = 0.09209 0.01446 0.01714 0.01500 AFIX 33 H23A 2 0.448928 0.359758 0.811553 11.00000 -1.50000 H23B 2 0.367203 0.417706 0.781963 11.00000 -1.50000 H23C 2 0.372193 0.343826 0.715167 11.00000 -1.50000 AFIX 0 C3 1 -0.095218 0.479011 0.814761 11.00000 0.11707 0.14556 = 0.16029 0.01106 0.05733 0.00073 AFIX 33 H3A 2 -0.166801 0.462828 0.785839 11.00000 -1.50000 H3B 2 -0.065671 0.455114 0.778601 11.00000 -1.50000 H3C 2 -0.075087 0.454110 0.868147 11.00000 -1.50000 AFIX 0 C2 1 -0.119601 0.620147 0.870850 11.00000 0.11684 0.14543 = 0.16011 0.01122 0.05754 0.00078 AFIX 33 H2A 2 -0.091885 0.684256 0.879785 11.00000 -1.50000 H2B 2 -0.189047 0.607875 0.832877 11.00000 -1.50000 H2C 2 -0.113236 0.600196 0.925290 11.00000 -1.50000 AFIX 0 C20 1 0.479919 0.745889 1.030993 11.00000 0.12850 0.18557 = 0.11528 -0.01133 -0.00377 0.03608 AFIX 33 H20A 2 0.538478 0.773418 1.081508 11.00000 -1.50000 H20B 2 0.438211 0.788854 1.013072 11.00000 -1.50000 H20C 2 0.443463 0.693511 1.044080 11.00000 -1.50000 AFIX 0 C21 1 0.606967 0.690890 0.991334 11.00000 0.12847 0.18555 = 0.11533 -0.01143 -0.00378 0.03632 AFIX 33 H21A 2 0.650259 0.725762 1.046370 11.00000 -1.50000 H21B 2 0.596618 0.627431 0.997028 11.00000 -1.50000 H21C 2 0.637176 0.701745 0.950351 11.00000 -1.50000 AFIX 0 HKLF 4 REM a_a.res in P-1 REM R1 = 0.1115 for 6247 Fo > 4sig(Fo) and 0.1663 for all 11911 data REM 676 parameters refined using 410 restraints END WGHT 0.1905 0.0000 REM Highest difference peak 1.488, deepest hole -1.678, 1-sigma level 0.128 Q1 1 0.5581 0.9249 0.8164 11.00000 0.05 0.86 Q2 1 0.4944 0.4715 0.8215 11.00000 0.05 0.77 Q3 1 0.1931 0.3358 0.4415 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12 -10 1 0.7345 -0.0147 12 -10 2 1.2865 -0.0008 12 -10 3 2.0773 0.0054 12 -10 4 2.2384 0.0023 12 -10 5 1.4638 0.0004 12 -10 6 0.6273 0.0064 12 -9 0 -0.2072 -0.0266 12 -9 1 0.2536 -0.0199 12 -9 2 0.7110 0.0049 12 -9 3 0.8095 0.0166 12 -9 4 0.6755 0.0023 12 -9 5 0.3254 -0.0185 12 -9 6 -0.1643 -0.0228 12 -9 7 -0.3416 -0.0100 12 -8 0 0.0562 0.0050 12 -8 1 0.5959 -0.0051 12 -8 2 0.8945 -0.0041 12 -8 3 0.2093 0.0039 12 -8 4 -0.4453 0.0084 12 -8 5 -0.1552 0.0104 12 -8 6 0.4895 0.0153 12 -8 7 0.5951 0.0190 12 -7 0 0.2166 0.0246 12 -7 1 0.0635 0.0260 12 -7 2 0.0106 0.0055 12 -7 3 -0.5734 -0.0166 12 -7 4 -1.2717 -0.0190 12 -7 5 -0.8358 0.0029 12 -7 6 0.9594 0.0334 12 -7 7 2.6946 0.0488 12 -7 8 2.9613 0.0376 12 -6 0 1.0259 -0.0023 12 -6 1 0.0403 0.0178 12 -6 2 -0.1839 0.0159 12 -6 3 0.2684 -0.0063 12 -6 4 0.2281 -0.0208 12 -6 5 -0.4034 -0.0095 12 -6 6 -0.3901 0.0160 12 -6 7 0.7317 0.0314 12 -6 8 1.7967 0.0246 12 -5 0 -1.1333 -0.0077 12 -5 1 -1.9349 -0.0009 12 -5 2 -1.7227 0.0038 12 -5 3 0.0062 -0.0008 12 -5 4 2.0186 -0.0035 12 -5 5 2.5754 0.0048 12 -5 6 1.4673 0.0160 12 -5 7 -0.0170 0.0174 12 -5 8 -0.8289 0.0081 12 -4 0 -2.1964 -0.0009 12 -4 1 -2.3304 -0.0020 12 -4 2 -2.4111 -0.0006 12 -4 3 -2.0925 0.0040 12 -4 4 -0.6709 0.0094 12 -4 5 1.2905 0.0125 12 -4 6 2.2981 0.0090 12 -4 7 1.8410 -0.0019 12 -4 8 0.8287 -0.0128 12 -3 0 0.1369 -0.0040 12 -3 1 0.5396 -0.0110 12 -3 2 0.6620 -0.0075 12 -3 3 -0.0975 0.0036 12 -3 4 -0.9388 0.0077 12 -3 5 -0.8642 -0.0029 12 -3 6 -0.0077 -0.0237 12 -3 7 0.8665 -0.0445 12 -3 8 1.4324 -0.0540 12 -2 0 0.5053 0.0055 12 -2 1 -0.1251 -0.0026 12 -2 2 0.1449 -0.0027 12 -2 3 0.9060 0.0017 12 -2 4 1.1430 -0.0004 12 -2 5 0.6037 -0.0143 12 -2 6 -0.0838 -0.0339 12 -2 7 -0.3770 -0.0494 12 -2 8 -0.2886 -0.0544 12 -1 0 -0.0161 -0.0084 12 -1 1 -1.4660 -0.0007 12 -1 2 -1.8554 0.0024 12 -1 3 -0.8248 0.0019 12 -1 4 0.4841 0.0020 12 -1 5 0.8649 0.0017 12 -1 6 0.2971 0.0006 12 -1 7 -0.5002 0.0027 12 -1 8 -1.0519 0.0094 12 0 0 -0.2831 -0.0185 12 0 1 -0.3057 -0.0056 12 0 2 -0.1756 0.0037 12 0 3 0.0813 0.0057 12 0 4 0.4445 0.0084 12 0 5 0.5925 0.0139 12 0 6 0.2288 0.0179 12 0 7 -0.4680 0.0212 12 1 0 -1.2787 -0.0097 12 1 1 -0.1586 -0.0016 12 1 2 0.7152 0.0098 12 1 3 1.0140 0.0119 12 1 4 1.0773 0.0077 12 1 5 1.0898 0.0077 12 1 6 0.8099 0.0110 12 1 7 0.2039 0.0098 12 2 0 -0.6946 0.0025 12 2 1 -0.2981 0.0030 12 2 2 0.0112 0.0009 12 2 3 0.3402 -0.0058 12 2 4 0.6318 -0.0118 12 2 5 0.6725 -0.0051 12 2 6 0.3294 0.0126 12 3 0 0.5761 0.0293 12 3 1 0.3996 0.0292 12 3 2 0.3239 0.0178 12 3 3 0.5074 0.0153 12 3 4 0.6673 0.0293 12 3 5 0.4664 0.0488 12 3 6 -0.0765 0.0591 12 4 0 -1.0342 0.0094 12 4 1 -0.7733 0.0083 12 4 2 -0.2569 0.0106 12 4 3 0.2083 0.0380 12 4 4 0.5030 0.0852 12 4 5 0.5540 0.1153 12 5 0 -1.7000 -0.0182 12 5 1 -1.4041 -0.0280 12 5 2 -0.9418 -0.0234 12 5 3 -0.6022 0.0018 12 5 4 -0.2730 0.0364 12 6 0 0.2784 0.0072 12 6 1 0.4944 0.0054 12 6 2 0.5887 0.0054 12 6 3 0.4611 0.0036 12 6 4 0.2125 -0.0031 12 7 0 0.9934 0.0118 12 7 1 0.9451 0.0103 12 7 2 1.0094 0.0057 12 8 0 0.9285 0.0103 12 8 1 0.5810 -0.0088 13 -13 0 -0.4470 -0.0532 13 -13 1 0.2364 -0.0231 13 -12 0 0.1112 -0.0373 13 -12 1 0.1420 -0.0080 13 -12 2 0.1714 0.0290 13 -12 3 0.3306 0.0448 13 -11 0 1.3893 -0.0291 13 -11 1 1.9490 -0.0240 13 -11 2 2.2273 0.0066 13 -11 3 2.0457 0.0356 13 -11 4 1.5819 0.0418 13 -10 0 -0.5365 -0.0045 13 -10 1 1.0779 -0.0090 13 -10 2 2.4434 -0.0130 13 -10 3 2.2121 -0.0162 13 -10 4 1.0476 -0.0181 13 -10 5 0.4299 -0.0134 13 -9 0 -1.1088 -0.0034 13 -9 1 -0.3821 0.0152 13 -9 2 0.7458 0.0145 13 -9 3 0.8410 -0.0025 13 -9 4 -0.2003 -0.0169 13 -9 5 -0.9957 -0.0149 13 -8 0 0.5961 -0.0084 13 -8 1 -0.0479 0.0027 13 -8 2 -0.5997 0.0102 13 -8 3 -0.4032 0.0080 13 -8 4 0.0363 0.0109 13 -8 5 0.1415 0.0281 13 -8 6 0.2641 0.0471 13 -7 0 1.3172 0.0112 13 -7 1 0.8221 0.0055 13 -7 2 -0.5178 -0.0003 13 -7 3 -1.0764 -0.0082 13 -7 4 -0.3013 -0.0062 13 -7 5 0.7821 0.0140 13 -7 6 1.2888 0.0381 13 -6 0 -0.5243 0.0120 13 -6 1 0.3052 0.0062 13 -6 2 1.1565 -0.0029 13 -6 3 1.3435 -0.0068 13 -6 4 1.3492 -0.0011 13 -6 5 1.5328 0.0100 13 -6 6 1.3995 0.0154 13 -5 0 -3.2214 0.0146 13 -5 1 -2.6203 0.0038 13 -5 2 -0.4145 -0.0115 13 -5 3 1.3994 -0.0085 13 -5 4 2.0446 0.0118 13 -5 5 2.1761 0.0275 13 -5 6 2.1093 0.0218 13 -4 0 -0.5437 0.0064 13 -4 1 -1.2913 0.0078 13 -4 2 -1.3996 0.0037 13 -4 3 -0.9560 0.0030 13 -4 4 -0.6127 0.0049 13 -4 5 -0.4056 0.0017 13 -4 6 0.2003 -0.0087 13 -3 0 2.8962 -0.0192 13 -3 1 2.0423 -0.0026 13 -3 2 0.6153 0.0172 13 -3 3 -0.0939 0.0175 13 -3 4 -0.1819 -0.0046 13 -3 5 -0.4825 -0.0350 13 -3 6 -0.8794 -0.0540 13 -2 0 1.3129 -0.0139 13 -2 1 0.5412 0.0014 13 -2 2 -0.1183 0.0162 13 -2 3 -0.0713 0.0118 13 -2 4 0.6787 -0.0050 13 -2 5 1.2605 -0.0175 13 -2 6 0.9597 -0.0184 13 -1 0 -0.1631 0.0007 13 -1 1 -0.6535 0.0055 13 -1 2 -0.5926 -0.0022 13 -1 3 -0.4274 -0.0179 13 -1 4 -0.1105 -0.0232 13 -1 5 0.4542 -0.0041 13 -1 6 0.7931 0.0304 13 0 0 0.2481 0.0136 13 0 1 0.5055 0.0078 13 0 2 0.8458 -0.0089 13 0 3 1.0713 -0.0261 13 0 4 1.0605 -0.0355 13 0 5 0.8890 -0.0278 13 0 6 0.5849 -0.0020 13 1 0 -0.0138 0.0002 13 1 1 0.4340 -0.0090 13 1 2 0.5878 -0.0204 13 1 3 1.0415 -0.0205 13 1 4 1.6082 -0.0107 13 1 5 1.6643 -0.0024 13 2 0 -0.1675 -0.0036 13 2 1 -0.0566 -0.0175 13 2 2 0.0738 -0.0345 13 2 3 0.3978 -0.0294 13 2 4 0.6980 0.0066 13 2 5 0.5565 0.0457 13 3 0 -0.4086 0.0185 13 3 1 -0.0533 0.0179 13 3 2 0.4997 0.0195 13 3 3 0.7328 0.0336 13 3 4 0.5287 0.0617 13 4 0 -1.8870 -0.0230 13 4 1 -0.9870 -0.0170 13 4 2 -0.2056 0.0184 13 4 3 0.1298 0.0647 13 5 0 -0.8623 -0.0333 13 5 1 -0.5430 -0.0481 13 5 2 -0.4588 -0.0363 13 5 3 -0.4075 -0.0076 13 6 0 1.3590 0.0130 13 6 1 1.1044 0.0031 13 7 0 0.9082 -0.0066 14 -12 0 0.0007 -0.0105 14 -11 0 0.0879 -0.0290 14 -11 1 0.8124 -0.0203 14 -11 2 1.6108 -0.0049 14 -10 0 -1.2740 -0.0194 14 -10 1 -0.1049 -0.0186 14 -10 2 0.3707 -0.0202 14 -10 3 0.3694 -0.0286 14 -9 0 -0.9577 -0.0233 14 -9 1 0.0795 -0.0068 14 -9 2 -0.0126 0.0120 14 -9 3 -0.4645 0.0200 14 -8 0 -0.0926 -0.0056 14 -8 1 0.5326 -0.0083 14 -8 2 0.7910 -0.0051 14 -8 3 0.4564 0.0099 14 -8 4 0.1863 0.0319 14 -7 0 -0.0918 0.0346 14 -7 1 0.3686 0.0275 14 -7 2 1.6864 -0.0046 14 -7 3 2.2758 -0.0269 14 -7 4 1.4935 -0.0169 14 -6 0 -0.5926 0.0093 14 -6 1 0.0796 0.0163 14 -6 2 1.7464 0.0068 14 -6 3 3.3103 -0.0028 14 -6 4 3.3314 0.0007 14 -6 5 1.8297 0.0095 14 -5 0 0.1845 -0.0090 14 -5 1 0.4407 -0.0203 14 -5 2 0.0258 -0.0070 14 -5 3 0.0623 0.0187 14 -5 4 0.7537 0.0350 14 -5 5 1.0961 0.0286 14 -4 0 2.8342 -0.0011 14 -4 1 2.6130 -0.0064 14 -4 2 0.8038 0.0041 14 -4 3 -1.3771 0.0126 14 -4 4 -2.3139 0.0068 14 -4 5 -1.8213 -0.0075 14 -3 0 2.9646 0.0033 14 -3 1 1.9561 0.0247 14 -3 2 1.5091 0.0251 14 -3 3 0.9559 -0.0023 14 -3 4 0.1457 -0.0377 14 -3 5 -0.3282 -0.0523 14 -2 0 1.6332 0.0213 14 -2 1 -0.1740 0.0294 14 -2 2 -0.4104 0.0066 14 -2 3 0.5260 -0.0266 14 -2 4 1.3478 -0.0445 14 -2 5 1.5577 -0.0358 14 -1 0 1.4936 0.0242 14 -1 1 0.8134 -0.0051 14 -1 2 0.0000 -0.0521 14 -1 3 -0.0657 -0.0789 14 -1 4 0.4782 -0.0681 14 0 0 1.1976 0.0036 14 0 1 1.4725 -0.0248 14 0 2 1.1057 -0.0591 14 0 3 0.8440 -0.0804 14 0 4 1.0186 -0.0755 14 1 0 0.3936 -0.0422 14 1 1 0.3443 -0.0494 14 1 2 0.4349 -0.0437 14 1 3 0.6055 -0.0329 14 2 0 -0.1198 -0.0252 14 2 1 -0.2105 -0.0433 14 2 2 0.0008 -0.0375 14 2 3 0.1354 -0.0102 14 3 0 -0.5797 0.0207 14 3 1 -0.1658 0.0091 14 3 2 -0.0636 0.0116 14 4 0 -1.1864 -0.0344 14 4 1 -0.6410 -0.0325 14 5 0 -0.0371 -0.0421 15 -10 0 -1.2968 -0.0235 15 -9 0 -0.2471 -0.0168 15 -9 1 0.0779 0.0183 15 -8 0 0.9339 0.0075 15 -8 1 0.6891 0.0124 15 -8 2 0.8704 0.0054 15 -7 0 0.8312 0.0283 15 -7 1 2.0405 0.0048 15 -7 2 2.1722 -0.0154 15 -6 0 0.1607 -0.0095 15 -6 1 1.8456 -0.0286 15 -6 2 2.4743 -0.0202 15 -6 3 1.6947 0.0106 15 -5 0 1.5022 -0.0133 15 -5 1 0.7960 -0.0178 15 -5 2 0.3230 -0.0028 15 -5 3 -0.3174 0.0167 15 -4 0 2.7761 0.0057 15 -4 1 0.9014 0.0289 15 -4 2 -0.0931 0.0224 15 -4 3 -0.1815 -0.0087 15 -3 0 1.5626 0.0268 15 -3 1 0.3193 0.0361 15 -3 2 -0.0530 0.0016 15 -3 3 0.6698 -0.0467 15 -2 0 1.0135 0.0353 15 -2 1 0.6351 -0.0058 15 -2 2 0.0689 -0.0529 15 -2 3 -0.2303 -0.0743 15 -1 0 0.6570 -0.0035 15 -1 1 0.8612 -0.0600 15 -1 2 0.7208 -0.0926 15 0 0 0.4355 -0.0316 15 0 1 -0.2089 -0.0498 15 0 2 -0.2118 -0.0522 15 1 0 0.5617 -0.0359 15 1 1 -0.1161 -0.0298 15 2 0 -0.2378 0.0112 15 2 1 0.0025 -0.0062 15 3 0 -0.6220 0.0310 16 -7 0 -0.1473 -0.0043 16 -6 0 0.4762 -0.0530 16 -5 0 0.4344 -0.0070 16 -4 0 -1.3679 0.0391 16 -3 0 -1.4250 0.0476 16 -2 0 0.7766 0.0132 16 -1 0 0.0047 -0.0358 0 0 0 0.0 0.0 ; _shelx_fab_checksum 16467 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ti3 Ti 0.21403(11) 0.81902(8) 0.72066(9) 0.0385(4) Uani 1 1 d . . Ti5 Ti 0.19642(10) 0.87178(8) 0.50454(9) 0.0389(4) Uani 1 1 d . . Ti4 Ti 0.35859(10) 0.78687(9) 0.63380(9) 0.0413(4) Uani 1 1 d . U Ti6 Ti 0.33266(11) 0.56562(9) 0.63122(10) 0.0448(4) Uani 1 1 d . . Ti2 Ti 0.31857(12) 0.66902(9) 0.80460(9) 0.0456(4) Uani 1 1 d . U Ti1 Ti 0.14276(12) 0.67743(10) 0.86274(9) 0.0491(4) Uani 1 1 d . . O10 O 0.1232(4) 0.7250(3) 0.4851(3) 0.0412(11) Uani 1 1 d . U O8 O 0.1226(4) 0.7035(3) 0.6492(3) 0.0398(11) Uani 1 1 d . U O9 O 0.2426(4) 0.6637(3) 0.5700(3) 0.0392(10) Uani 1 1 d . U O11 O 0.3381(4) 0.7591(3) 0.7336(3) 0.0414(12) Uani 1 1 d . . O6 O 0.2362(4) 0.7458(3) 0.8175(3) 0.0393(12) Uani 1 1 d . . O12 O 0.2595(4) 0.8498(3) 0.6271(3) 0.0359(12) Uani 1 1 d . . O13 O 0.3166(4) 0.8175(3) 0.5123(4) 0.0457(11) Uani 1 1 d . U O7 O 0.0607(4) 0.6081(3) 0.7221(3) 0.0482(14) Uani 1 1 d . U O5 O 0.0960(4) 0.8962(3) 0.5466(3) 0.0439(13) Uani 1 1 d . . O17 O 0.4199(4) 0.6769(3) 0.6217(4) 0.0537(13) Uani 1 1 d . U O22 O 0.2677(4) 0.9247(3) 0.7889(4) 0.0553(15) Uani 1 1 d . . O15 O 0.1201(4) 0.8600(3) 0.3908(4) 0.0502(14) Uani 1 1 d . . O21 O 0.2925(4) 0.5741(3) 0.7192(4) 0.0518(15) Uani 1 1 d . . O3 O 0.2358(5) 0.5969(3) 0.8592(3) 0.0530(15) Uani 1 1 d . . O4 O 0.0727(4) 0.7753(4) 0.8232(4) 0.0532(15) Uani 1 1 d . . O16 O 0.4746(4) 0.8660(4) 0.6782(4) 0.0615(14) Uani 1 1 d . U O18 O 0.2512(4) 0.4849(4) 0.5369(4) 0.0570(16) Uani 1 1 d . U O14 O 0.2600(4) 0.9863(3) 0.5157(4) 0.0533(15) Uani 1 1 d . . N1 N 0.0931(5) 0.8732(4) 0.6215(4) 0.0419(15) Uani 1 1 d . . N2 N 0.0792(5) 0.8144(4) 0.7549(4) 0.0428(16) Uani 1 1 d . . O2 O 0.2096(5) 0.7256(4) 0.9749(4) 0.0659(17) Uani 1 1 d . U O1 O 0.0398(5) 0.6044(5) 0.8738(4) 0.0716(18) Uani 1 1 d . U C15 C 0.0373(7) 0.5571(6) 0.5771(6) 0.0551(7) Uani 1 1 d . U O20 O 0.4247(5) 0.5013(4) 0.6739(5) 0.0724(16) Uani 1 1 d . U C18 C 0.0300(6) 0.5196(6) 0.4332(6) 0.0555(7) Uani 1 1 d . U H18 H 0.0491 0.5337 0.3880 0.067 Uiso 1 1 calc R U O19 O 0.4385(6) 0.6788(5) 0.8862(4) 0.0807(19) Uani 1 1 d . U C17 C 0.0720(7) 0.5787(6) 0.5110(6) 0.0551(7) Uani 1 1 d . U C16 C 0.1512(7) 0.6615(6) 0.5243(6) 0.0555(7) Uani 1 1 d . U C14 C 0.0762(7) 0.6267(6) 0.6574(6) 0.0551(7) Uani 1 1 d . U C11 C 0.0161(7) 0.8849(5) 0.6360(6) 0.0522(11) Uani 1 1 d . U C10 C 0.0103(7) 0.8519(5) 0.7150(6) 0.0522(11) Uani 1 1 d . U C12 C -0.0651(7) 0.9237(5) 0.5739(6) 0.0528(11) Uani 1 1 d . U H12A H -0.1155 0.9268 0.5964 0.079 Uiso 1 1 calc R U H12B H -0.0370 0.9836 0.5668 0.079 Uiso 1 1 calc R U H12C H -0.0946 0.8854 0.5191 0.079 Uiso 1 1 calc R U C31 C 0.3539(8) 0.7964(6) 0.4475(7) 0.0688(7) Uani 1 1 d . U H31 H 0.4206 0.7843 0.4767 0.083 Uiso 1 1 calc R U C37 C 0.0366(10) 0.8073(9) 0.3215(7) 0.097(2) Uani 1 1 d . U H37 H 0.0416 0.7438 0.3257 0.116 Uiso 1 1 calc R U C7 C 0.2440(10) 0.5094(7) 0.8828(8) 0.093(2) Uani 1 1 d . U H7 H 0.3107 0.5026 0.8881 0.111 Uiso 1 1 calc R U C13 C -0.0776(6) 0.8564(5) 0.7386(6) 0.0528(11) Uani 1 1 d . U H13A H -0.1210 0.8884 0.6989 0.079 Uiso 1 1 calc R U H13B H -0.1138 0.7959 0.7356 0.079 Uiso 1 1 calc R U H13C H -0.0542 0.8877 0.7962 0.079 Uiso 1 1 calc R U C43 C 0.2448(7) 0.3918(6) 0.5120(7) 0.0644(10) Uani 1 1 d . U H43 H 0.3111 0.3775 0.5358 0.077 Uiso 1 1 calc R U C34 C 0.3412(9) 1.0562(8) 0.5726(9) 0.097(2) Uani 1 1 d . U H34 H 0.4003 1.0304 0.5981 0.116 Uiso 1 1 calc R U C32 C 0.2876(7) 0.7123(6) 0.3876(7) 0.0643(8) Uani 1 1 d . U H32A H 0.3131 0.6988 0.3447 0.096 Uiso 1 1 calc R U H32B H 0.2862 0.6623 0.4200 0.096 Uiso 1 1 calc R U H32C H 0.2211 0.7219 0.3599 0.096 Uiso 1 1 calc R U C25 C 0.5203(8) 0.6882(7) 0.6206(7) 0.0713(8) Uani 1 1 d . U H25 H 0.5375 0.7484 0.6047 0.086 Uiso 1 1 calc R U C33 C 0.3636(7) 0.8755(6) 0.4006(7) 0.0671(8) Uani 1 1 d . U H33A H 0.3885 0.8608 0.3576 0.101 Uiso 1 1 calc R U H33B H 0.2992 0.8899 0.3732 0.101 Uiso 1 1 calc R U H33C H 0.4092 0.9269 0.4408 0.101 Uiso 1 1 calc R U C27 C 0.5967(8) 0.6852(7) 0.7096(7) 0.0799(8) Uani 1 1 d . U H27A H 0.6618 0.6927 0.7078 0.120 Uiso 1 1 calc R U H27B H 0.5970 0.7334 0.7496 0.120 Uiso 1 1 calc R U H27C H 0.5799 0.6278 0.7278 0.120 Uiso 1 1 calc R U C36 C 0.3104(9) 1.0903(8) 0.6454(8) 0.098(2) Uani 1 1 d . U H36A H 0.3636 1.1377 0.6851 0.146 Uiso 1 1 calc R U H36B H 0.2510 1.1136 0.6206 0.146 Uiso 1 1 calc R U H36C H 0.2975 1.0409 0.6756 0.146 Uiso 1 1 calc R U C38 C -0.0563(9) 0.8159(9) 0.3333(7) 0.097(2) Uani 1 1 d . U H38A H -0.1133 0.7799 0.2859 0.146 Uiso 1 1 calc R U H38B H -0.0544 0.7951 0.3864 0.146 Uiso 1 1 calc R U H38C H -0.0612 0.8785 0.3352 0.146 Uiso 1 1 calc R U C26 C 0.5153(8) 0.6175(7) 0.5499(7) 0.0759(9) Uani 1 1 d . U H26A H 0.5803 0.6236 0.5481 0.114 Uiso 1 1 calc R U H26B H 0.4942 0.5578 0.5620 0.114 Uiso 1 1 calc R U H26C H 0.4684 0.6265 0.4952 0.114 Uiso 1 1 calc R U C35 C 0.3655(9) 1.1325(7) 0.5244(9) 0.097(2) Uani 1 1 d . U H35A H 0.4203 1.1787 0.5640 0.146 Uiso 1 1 calc R U H35B H 0.3836 1.1090 0.4796 0.146 Uiso 1 1 calc R U H35C H 0.3079 1.1581 0.4993 0.146 Uiso 1 1 calc R U C8 C 0.1717(10) 0.4375(7) 0.8131(8) 0.093(2) Uani 1 1 d . U H8A H 0.1788 0.3790 0.8307 0.140 Uiso 1 1 calc R U H8B H 0.1049 0.4444 0.8019 0.140 Uiso 1 1 calc R U H8C H 0.1847 0.4422 0.7616 0.140 Uiso 1 1 calc R U C9 C 0.2410(10) 0.5014(7) 0.9683(8) 0.093(2) Uani 1 1 d . U H9A H 0.2467 0.4414 0.9819 0.140 Uiso 1 1 calc R U H9B H 0.2956 0.5453 1.0111 0.140 Uiso 1 1 calc R U H9C H 0.1788 0.5124 0.9678 0.140 Uiso 1 1 calc R U C44 C 0.2043(7) 0.3789(6) 0.4144(6) 0.0631(9) Uani 1 1 d . U H44A H 0.1981 0.3167 0.3933 0.095 Uiso 1 1 calc R U H44B H 0.1398 0.3940 0.3921 0.095 Uiso 1 1 calc R U H44C H 0.2492 0.4178 0.3959 0.095 Uiso 1 1 calc R U C40 C 0.2789(14) 0.9772(10) 0.8601(8) 0.153(4) Uani 1 1 d D U H40 H 0.2251 0.9383 0.8708 0.183 Uiso 1 1 calc R U C30 C 0.6508(8) 0.9364(7) 0.7483(7) 0.0854(10) Uani 1 1 d . U H30A H 0.6512 0.8969 0.7016 0.128 Uiso 1 1 calc R U H30B H 0.6786 0.9981 0.7453 0.128 Uiso 1 1 calc R U H30C H 0.6902 0.9194 0.8024 0.128 Uiso 1 1 calc R U C22 C 0.4800(8) 0.4572(7) 0.7437(8) 0.0858(10) Uani 1 1 d D U H22 H 0.5264 0.5007 0.7943 0.103 Uiso 1 1 calc R U C1 C -0.0644(13) 0.5704(12) 0.8312(13) 0.144(3) Uani 1 1 d . U H1 H -0.0808 0.5894 0.7739 0.173 Uiso 1 1 calc R U C4 C 0.1924(16) 0.7313(13) 1.0477(10) 0.161(4) Uani 1 1 d D U H4 H 0.1416 0.6777 1.0437 0.193 Uiso 1 1 calc R U C28 C 0.5489(9) 0.9287(8) 0.7415(8) 0.0870(11) Uani 1 1 d . U C39 C 0.0419(9) 0.8261(9) 0.2401(7) 0.097(2) Uani 1 1 d . U H39A H -0.0156 0.7896 0.1934 0.146 Uiso 1 1 calc R U H39B H 0.0432 0.8892 0.2353 0.146 Uiso 1 1 calc R U H39C H 0.1016 0.8119 0.2375 0.146 Uiso 1 1 calc R U C45 C 0.1726(7) 0.3324(6) 0.5441(7) 0.0655(10) Uani 1 1 d . U H45A H 0.1682 0.2694 0.5273 0.098 Uiso 1 1 calc R U H45B H 0.1972 0.3451 0.6059 0.098 Uiso 1 1 calc R U H45C H 0.1075 0.3459 0.5190 0.098 Uiso 1 1 calc R U C41 C 0.2314(14) 1.0554(9) 0.8445(9) 0.153(4) Uani 1 1 d D U H41A H 0.2430 1.0892 0.8989 0.229 Uiso 1 1 calc R U H41B H 0.2594 1.0938 0.8124 0.229 Uiso 1 1 calc R U H41C H 0.1607 1.0343 0.8122 0.229 Uiso 1 1 calc R U C6 C 0.2696(14) 0.7402(13) 1.1241(10) 0.161(4) Uani 1 1 d . U H6A H 0.2459 0.7434 1.1698 0.241 Uiso 1 1 calc R U H6B H 0.2999 0.6888 1.1262 0.241 Uiso 1 1 calc R U H6C H 0.3182 0.7948 1.1310 0.241 Uiso 1 1 calc R U C29 C 0.5198(8) 0.9747(8) 0.7965(8) 0.0875(11) Uani 1 1 d . U H29A H 0.5768 1.0170 0.8385 0.131 Uiso 1 1 calc R U H29B H 0.4710 1.0072 0.7644 0.131 Uiso 1 1 calc R U H29C H 0.4910 0.9325 0.8255 0.131 Uiso 1 1 calc R U C24 C 0.5331(9) 0.3976(7) 0.7092(8) 0.0889(11) Uani 1 1 d . U H24A H 0.5708 0.3672 0.7545 0.133 Uiso 1 1 calc R U H24B H 0.4846 0.3534 0.6624 0.133 Uiso 1 1 calc R U H24C H 0.5775 0.4346 0.6888 0.133 Uiso 1 1 calc R U C42 C 0.3598(13) 0.9692(10) 0.9412(8) 0.153(4) Uani 1 1 d D U H42A H 0.3604 1.0099 0.9875 0.230 Uiso 1 1 calc R U H42B H 0.3490 0.9079 0.9536 0.230 Uiso 1 1 calc R U H42C H 0.4228 0.9845 0.9355 0.230 Uiso 1 1 calc R U C5 C 0.1503(14) 0.8120(12) 1.0492(9) 0.161(4) Uani 1 1 d D U H5A H 0.0945 0.8087 0.9955 0.241 Uiso 1 1 calc R U H5B H 0.1283 0.8144 1.0960 0.241 Uiso 1 1 calc R U H5C H 0.2006 0.8657 1.0571 0.241 Uiso 1 1 calc R U C19 C 0.5100(12) 0.7181(13) 0.9610(12) 0.159(3) Uani 1 1 d D U H19 H 0.5300 0.7778 0.9455 0.191 Uiso 1 1 calc R U C23 C 0.4111(8) 0.3886(7) 0.7650(8) 0.0888(11) Uani 1 1 d D U H23A H 0.4489 0.3598 0.8116 0.133 Uiso 1 1 calc R U H23B H 0.3672 0.4177 0.7820 0.133 Uiso 1 1 calc R U H23C H 0.3722 0.3438 0.7152 0.133 Uiso 1 1 calc R U C3 C -0.0952(12) 0.4790(12) 0.8148(12) 0.144(3) Uani 1 1 d . U H3A H -0.1668 0.4628 0.7858 0.217 Uiso 1 1 calc R U H3B H -0.0657 0.4551 0.7786 0.217 Uiso 1 1 calc R U H3C H -0.0751 0.4541 0.8681 0.217 Uiso 1 1 calc R U C2 C -0.1196(12) 0.6201(11) 0.8708(11) 0.144(3) Uani 1 1 d . U H2A H -0.0919 0.6843 0.8798 0.216 Uiso 1 1 calc R U H2B H -0.1890 0.6079 0.8329 0.216 Uiso 1 1 calc R U H2C H -0.1132 0.6002 0.9253 0.216 Uiso 1 1 calc R U C20 C 0.4799(13) 0.7459(12) 1.0310(11) 0.160(3) Uani 1 1 d . U H20A H 0.5385 0.7734 1.0815 0.240 Uiso 1 1 calc R U H20B H 0.4382 0.7889 1.0131 0.240 Uiso 1 1 calc R U H20C H 0.4435 0.6935 1.0441 0.240 Uiso 1 1 calc R U C21 C 0.6070(12) 0.6909(12) 0.9913(11) 0.160(3) Uani 1 1 d D U H21A H 0.6503 0.7258 1.0464 0.240 Uiso 1 1 calc R U H21B H 0.5966 0.6274 0.9970 0.240 Uiso 1 1 calc R U H21C H 0.6372 0.7017 0.9504 0.240 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 Ti3 0.0434(9) 0.0344(7) 0.0327(8) 0.0023(6) 0.0114(7) 0.0048(6) Ti5 0.0451(9) 0.0317(7) 0.0404(9) 0.0125(6) 0.0170(7) 0.0068(6) Ti4 0.0357(8) 0.0386(7) 0.0453(9) 0.0068(6) 0.0133(7) 0.0032(6) Ti6 0.0446(9) 0.0437(8) 0.0476(9) 0.0086(7) 0.0172(8) 0.0144(7) Ti2 0.0500(10) 0.0456(8) 0.0374(9) 0.0120(6) 0.0113(8) 0.0122(7) Ti1 0.0637(11) 0.0514(9) 0.0333(9) 0.0102(7) 0.0197(8) 0.0125(7) O10 0.030(3) 0.046(2) 0.037(3) -0.0024(18) 0.008(2) -0.003(2) O8 0.040(3) 0.048(2) 0.030(3) -0.003(2) 0.013(2) 0.0100(19) O9 0.0518(17) 0.027(2) 0.046(3) 0.013(2) 0.0275(19) 0.005(2) O11 0.045(3) 0.040(3) 0.031(3) 0.009(2) 0.009(3) 0.003(2) O6 0.044(3) 0.040(3) 0.028(3) 0.003(2) 0.010(3) 0.006(2) O12 0.043(3) 0.027(2) 0.037(3) 0.008(2) 0.016(3) 0.006(2) O13 0.033(3) 0.036(3) 0.058(3) 0.011(2) 0.011(2) -0.004(2) O7 0.059(4) 0.042(3) 0.034(3) 0.002(2) 0.018(3) -0.011(2) O5 0.060(4) 0.041(3) 0.037(3) 0.015(2) 0.022(3) 0.017(3) O17 0.054(2) 0.045(3) 0.061(4) 0.019(3) 0.022(3) 0.007(3) O22 0.064(4) 0.037(3) 0.051(4) -0.009(3) 0.014(3) 0.000(3) O15 0.059(4) 0.048(3) 0.048(3) 0.024(3) 0.019(3) 0.022(3) O21 0.061(4) 0.041(3) 0.052(4) 0.010(3) 0.022(3) 0.009(3) O3 0.076(4) 0.043(3) 0.037(3) 0.016(2) 0.018(3) 0.012(3) O4 0.064(4) 0.057(3) 0.050(4) 0.017(3) 0.031(3) 0.021(3) O16 0.052(3) 0.063(3) 0.073(3) 0.024(2) 0.028(2) 0.010(2) O18 0.053(4) 0.048(3) 0.063(4) 0.004(3) 0.010(3) 0.022(3) O14 0.051(4) 0.035(3) 0.069(4) 0.013(3) 0.021(3) 0.001(2) N1 0.046(4) 0.032(3) 0.047(4) 0.002(3) 0.017(3) 0.007(3) N2 0.058(5) 0.042(3) 0.032(4) 0.009(3) 0.018(3) 0.018(3) O2 0.078(5) 0.070(4) 0.040(3) 0.007(3) 0.015(3) 0.013(3) O1 0.072(4) 0.084(4) 0.072(5) 0.026(3) 0.045(4) 0.010(3) C15 0.0511(13) 0.0582(13) 0.0680(15) 0.0163(12) 0.0335(12) 0.0167(11) O20 0.058(4) 0.062(3) 0.094(4) 0.003(3) 0.023(3) 0.021(3) C18 0.0513(13) 0.0585(13) 0.0683(15) 0.0162(11) 0.0333(12) 0.0167(11) O19 0.073(4) 0.096(4) 0.055(4) 0.021(3) -0.001(3) 0.029(3) C17 0.0511(13) 0.0583(13) 0.0680(15) 0.0163(12) 0.0335(12) 0.0167(11) C16 0.0513(13) 0.0586(13) 0.0683(15) 0.0164(11) 0.0333(12) 0.0168(11) C14 0.0511(13) 0.0582(13) 0.0680(15) 0.0164(12) 0.0336(12) 0.0165(11) C11 0.057(3) 0.050(2) 0.057(3) 0.010(2) 0.027(2) 0.021(2) C10 0.057(3) 0.050(2) 0.057(3) 0.010(2) 0.027(2) 0.021(2) C12 0.058(3) 0.050(2) 0.058(3) 0.010(2) 0.026(2) 0.021(2) C31 0.0571(13) 0.0756(14) 0.0782(15) 0.0131(12) 0.0308(12) 0.0154(12) C37 0.093(5) 0.122(5) 0.048(4) -0.003(4) 0.012(4) 0.001(4) C7 0.126(6) 0.071(4) 0.105(6) 0.043(4) 0.059(5) 0.038(4) C13 0.058(3) 0.050(2) 0.058(3) 0.010(2) 0.026(2) 0.021(2) C43 0.0571(17) 0.0627(17) 0.0761(19) 0.0124(16) 0.0272(16) 0.0164(15) C34 0.080(5) 0.072(4) 0.119(6) 0.015(4) 0.024(4) 0.002(3) C32 0.0555(13) 0.0698(14) 0.0745(15) 0.0142(12) 0.0317(12) 0.0158(12) C25 0.0581(13) 0.0778(14) 0.0804(16) 0.0128(13) 0.0294(12) 0.0150(12) C33 0.0568(14) 0.0733(15) 0.0766(16) 0.0140(14) 0.0311(13) 0.0154(13) C27 0.0638(14) 0.0831(15) 0.0863(16) 0.0119(13) 0.0234(13) 0.0137(13) C36 0.081(5) 0.072(4) 0.119(6) 0.015(4) 0.024(4) 0.002(3) C38 0.094(5) 0.123(5) 0.049(4) -0.003(4) 0.011(4) 0.001(4) C26 0.0611(15) 0.0810(16) 0.0836(17) 0.0121(14) 0.0266(14) 0.0147(14) C35 0.081(5) 0.072(4) 0.119(6) 0.015(4) 0.024(4) 0.002(3) C8 0.126(6) 0.072(4) 0.105(6) 0.042(4) 0.059(5) 0.038(4) C9 0.126(6) 0.072(4) 0.105(6) 0.043(4) 0.059(5) 0.038(4) C44 0.0563(15) 0.0624(15) 0.0746(17) 0.0131(14) 0.0283(14) 0.0159(13) C40 0.241(10) 0.132(7) 0.079(5) -0.012(5) 0.042(6) 0.079(7) C30 0.0663(16) 0.0869(17) 0.0899(18) 0.0082(15) 0.0200(15) 0.0098(15) C22 0.0695(17) 0.0859(17) 0.0901(18) 0.0142(15) 0.0186(15) 0.0152(15) C1 0.117(6) 0.145(6) 0.160(6) 0.011(6) 0.058(5) 0.001(5) C4 0.191(9) 0.211(9) 0.074(5) 0.006(7) 0.057(6) 0.024(7) C28 0.0668(18) 0.0880(19) 0.091(2) 0.0062(17) 0.0189(17) 0.0081(16) C39 0.094(5) 0.123(5) 0.049(4) -0.003(4) 0.011(4) 0.001(4) C45 0.0579(17) 0.0631(17) 0.0768(19) 0.0128(16) 0.0265(16) 0.0157(15) C41 0.241(10) 0.132(7) 0.079(5) -0.012(5) 0.042(6) 0.079(7) C6 0.192(9) 0.211(9) 0.074(5) 0.006(7) 0.057(6) 0.024(7) C29 0.0673(18) 0.0885(19) 0.091(2) 0.0068(17) 0.0190(17) 0.0082(17) C24 0.0723(18) 0.0877(19) 0.092(2) 0.0143(17) 0.0170(17) 0.0152(16) C42 0.241(10) 0.132(7) 0.079(5) -0.012(5) 0.042(6) 0.079(7) C5 0.192(9) 0.211(9) 0.074(5) 0.006(7) 0.057(6) 0.024(7) C19 0.128(6) 0.185(6) 0.115(6) -0.011(5) -0.004(5) 0.036(5) C23 0.0723(18) 0.0877(19) 0.092(2) 0.0145(17) 0.0171(17) 0.0150(16) C3 0.117(6) 0.146(6) 0.160(7) 0.011(6) 0.057(5) 0.001(5) C2 0.117(6) 0.145(6) 0.160(7) 0.011(6) 0.058(5) 0.001(5) C20 0.128(6) 0.186(6) 0.115(6) -0.011(6) -0.004(5) 0.036(5) C21 0.128(6) 0.186(6) 0.115(6) -0.011(5) -0.004(5) 0.036(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 O22 Ti3 O12 98.2(2) . O22 Ti3 O6 94.5(2) . O12 Ti3 O6 142.8(2) . O22 Ti3 O8 165.3(2) . O12 Ti3 O8 91.8(2) . O6 Ti3 O8 83.9(2) . O22 Ti3 O11 104.6(2) . O12 Ti3 O11 71.30(19) . O6 Ti3 O11 71.64(19) . O8 Ti3 O11 88.78(19) . O22 Ti3 N1 93.7(2) . O12 Ti3 N1 72.3(2) . O6 Ti3 N1 141.6(2) . O8 Ti3 N1 79.0(2) . O11 Ti3 N1 141.1(2) . O22 Ti3 N2 87.2(3) . O12 Ti3 N2 140.3(2) . O6 Ti3 N2 75.0(2) . O8 Ti3 N2 78.2(2) . O11 Ti3 N2 145.2(2) . N1 Ti3 N2 68.1(2) . O22 Ti3 Ti2 110.9(2) . O12 Ti3 Ti2 107.19(14) . O6 Ti3 Ti2 35.91(14) . O8 Ti3 Ti2 76.00(15) . O11 Ti3 Ti2 37.85(13) . N1 Ti3 Ti2 154.94(16) . N2 Ti3 Ti2 107.38(16) . O22 Ti3 Ti4 107.2(2) . O12 Ti3 Ti4 35.00(13) . O6 Ti3 Ti4 107.75(15) . O8 Ti3 Ti4 87.13(14) . O11 Ti3 Ti4 36.55(13) . N1 Ti3 Ti4 105.40(17) . N2 Ti3 Ti4 164.80(17) . Ti2 Ti3 Ti4 72.40(5) . O14 Ti5 O15 96.9(3) . O14 Ti5 O5 97.4(2) . O15 Ti5 O5 97.2(2) . O14 Ti5 O12 98.9(2) . O15 Ti5 O12 164.1(2) . O5 Ti5 O12 80.0(2) . O14 Ti5 O13 95.0(2) . O15 Ti5 O13 105.4(2) . O5 Ti5 O13 152.7(2) . O12 Ti5 O13 74.0(2) . O14 Ti5 O10 175.7(2) . O15 Ti5 O10 81.7(2) . O5 Ti5 O10 86.85(19) . O12 Ti5 O10 82.47(19) . O13 Ti5 O10 81.44(18) . O14 Ti5 Ti4 103.0(2) . O15 Ti5 Ti4 140.45(17) . O5 Ti5 Ti4 113.39(16) . O12 Ti5 Ti4 34.75(13) . O13 Ti5 Ti4 39.69(16) . O10 Ti5 Ti4 75.85(14) . O16 Ti4 O12 107.5(2) . O16 Ti4 O11 101.6(3) . O12 Ti4 O11 80.1(2) . O16 Ti4 O13 97.0(2) . O12 Ti4 O13 77.9(2) . O11 Ti4 O13 154.6(2) . O16 Ti4 O17 94.7(3) . O12 Ti4 O17 157.8(2) . O11 Ti4 O17 95.4(2) . O13 Ti4 O17 100.1(2) . O16 Ti4 O9 162.8(2) . O12 Ti4 O9 89.3(2) . O11 Ti4 O9 84.7(2) . O13 Ti4 O9 82.55(19) . O17 Ti4 O9 68.5(2) . O16 Ti4 Ti3 113.1(2) . O12 Ti4 Ti3 37.69(14) . O11 Ti4 Ti3 42.66(16) . O13 Ti4 Ti3 113.58(16) . O17 Ti4 Ti3 131.88(16) . O9 Ti4 Ti3 82.44(13) . O16 Ti4 Ti5 110.4(2) . O12 Ti4 Ti5 37.85(15) . O11 Ti4 Ti5 115.57(17) . O13 Ti4 Ti5 40.51(15) . O17 Ti4 Ti5 133.69(18) . O9 Ti4 Ti5 80.50(14) . Ti3 Ti4 Ti5 73.25(5) . O16 Ti4 Ti6 124.3(2) . O12 Ti4 Ti6 124.83(15) . O11 Ti4 Ti6 72.90(15) . O13 Ti4 Ti6 110.15(15) . O17 Ti4 Ti6 34.68(16) . O9 Ti4 Ti6 41.89(13) . Ti3 Ti4 Ti6 99.32(5) . Ti5 Ti4 Ti6 122.03(6) . O20 Ti6 O21 99.2(3) . O20 Ti6 O18 97.4(3) . O21 Ti6 O18 116.9(3) . O20 Ti6 O17 98.8(3) . O21 Ti6 O17 115.6(2) . O18 Ti6 O17 121.2(3) . O20 Ti6 O9 167.6(3) . O21 Ti6 O9 89.7(2) . O18 Ti6 O9 86.1(2) . O17 Ti6 O9 69.4(2) . O20 Ti6 Ti4 129.6(2) . O21 Ti6 Ti4 88.97(17) . O18 Ti6 Ti4 122.79(19) . O17 Ti6 Ti4 36.38(16) . O9 Ti6 Ti4 41.26(13) . O20 Ti6 Ti2 104.2(2) . O21 Ti6 Ti2 24.61(17) . O18 Ti6 Ti2 137.8(2) . O17 Ti6 Ti2 91.01(18) . O9 Ti6 Ti2 80.49(13) . Ti4 Ti6 Ti2 67.02(4) . O19 Ti2 O21 110.1(3) . O19 Ti2 O6 119.6(3) . O21 Ti2 O6 130.2(2) . O19 Ti2 O11 104.3(3) . O21 Ti2 O11 92.8(2) . O6 Ti2 O11 78.8(2) . O19 Ti2 O3 99.4(3) . O21 Ti2 O3 93.4(2) . O6 Ti2 O3 76.1(2) . O11 Ti2 O3 151.7(2) . O19 Ti2 Ti3 129.6(2) . O21 Ti2 Ti3 108.64(18) . O6 Ti2 Ti3 38.21(15) . O11 Ti2 Ti3 42.98(16) . O3 Ti2 Ti3 109.13(17) . O19 Ti2 Ti1 117.4(2) . O21 Ti2 Ti1 114.82(19) . O6 Ti2 Ti1 37.25(15) . O11 Ti2 Ti1 114.27(16) . O3 Ti2 Ti1 39.02(15) . Ti3 Ti2 Ti1 71.39(5) . O19 Ti2 Ti6 103.8(2) . O21 Ti2 Ti6 23.92(17) . O6 Ti2 Ti6 132.21(16) . O11 Ti2 Ti6 71.70(15) . O3 Ti2 Ti6 117.37(16) . Ti3 Ti2 Ti6 98.72(5) . Ti1 Ti2 Ti6 133.56(6) . O1 Ti1 O2 97.6(3) . O1 Ti1 O4 95.7(3) . O2 Ti1 O4 98.0(3) . O1 Ti1 O6 164.7(3) . O2 Ti1 O6 97.6(3) . O4 Ti1 O6 81.2(2) . O1 Ti1 O3 105.2(3) . O2 Ti1 O3 96.6(3) . O4 Ti1 O3 152.6(2) . O6 Ti1 O3 73.9(2) . O1 Ti1 O7 81.4(3) . O2 Ti1 O7 176.6(3) . O4 Ti1 O7 85.4(2) . O6 Ti1 O7 83.42(19) . O3 Ti1 O7 80.5(2) . O1 Ti1 Ti2 140.7(2) . O2 Ti1 Ti2 101.5(2) . O4 Ti1 Ti2 114.98(17) . O6 Ti1 Ti2 35.16(14) . O3 Ti1 Ti2 38.90(15) . O7 Ti1 Ti2 77.50(15) . C16 O10 Ti5 131.4(6) . C14 O8 Ti3 140.6(6) . C16 O9 Ti4 125.4(5) . C16 O9 Ti6 136.9(5) . Ti4 O9 Ti6 96.9(2) . Ti4 O11 Ti2 148.3(3) . Ti4 O11 Ti3 100.8(2) . Ti2 O11 Ti3 99.2(2) . Ti2 O6 Ti1 107.6(2) . Ti2 O6 Ti3 105.9(2) . Ti1 O6 Ti3 131.9(3) . Ti4 O12 Ti3 107.3(2) . Ti4 O12 Ti5 107.4(2) . Ti3 O12 Ti5 136.8(3) . C31 O13 Ti4 129.0(5) . C31 O13 Ti5 130.8(5) . Ti4 O13 Ti5 99.8(2) . C14 O7 Ti1 129.3(6) . N1 O5 Ti5 123.4(4) . C25 O17 Ti6 128.5(5) . C25 O17 Ti4 121.9(5) . Ti6 O17 Ti4 108.9(3) . C40 O22 Ti3 148.4(10) . C37 O15 Ti5 145.4(6) . Ti6 O21 Ti2 131.5(3) . C7 O3 Ti2 125.2(6) . C7 O3 Ti1 132.7(7) . Ti2 O3 Ti1 102.1(2) . N2 O4 Ti1 120.1(4) . C28 O16 Ti4 154.1(7) . C43 O18 Ti6 133.2(6) . C34 O14 Ti5 143.9(7) . C11 N1 O5 116.0(7) . C11 N1 Ti3 119.9(6) . O5 N1 Ti3 124.1(4) . C10 N2 O4 116.8(7) . C10 N2 Ti3 121.8(6) . O4 N2 Ti3 121.3(5) . C4 O2 Ti1 138.4(10) . C1 O1 Ti1 141.8(9) . C18 C15 C17 121.2(9) 2_566 C18 C15 C14 121.8(8) 2_566 C17 C15 C14 117.0(8) . C22 O20 Ti6 149.4(7) . C15 C18 C17 120.8(9) 2_566 C15 C18 H18 119.6 2_566 C17 C18 H18 119.6 . C19 O19 Ti2 150.9(9) . C18 C17 C15 117.9(8) . C18 C17 C16 120.8(8) . C15 C17 C16 121.3(9) . O10 C16 O9 122.8(8) . O10 C16 C17 116.3(8) . O9 C16 C17 120.8(8) . O7 C14 O8 125.7(8) . O7 C14 C15 120.7(8) . O8 C14 C15 113.5(8) . N1 C11 C10 115.0(8) . N1 C11 C12 122.3(8) . C10 C11 C12 122.6(7) . N2 C10 C11 114.3(7) . N2 C10 C13 124.1(8) . C11 C10 C13 121.4(8) . 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 . O13 C31 C33 110.1(7) . O13 C31 C32 110.1(7) . C33 C31 C32 112.2(9) . O13 C31 H31 108.1 . C33 C31 H31 108.1 . C32 C31 H31 108.1 . O15 C37 C39 110.4(10) . O15 C37 C38 109.6(9) . C39 C37 C38 117.1(11) . O15 C37 H37 106.4 . C39 C37 H37 106.4 . C38 C37 H37 106.4 . O3 C7 C9 112.0(9) . O3 C7 C8 111.1(10) . C9 C7 C8 114.5(11) . O3 C7 H7 106.2 . C9 C7 H7 106.2 . C8 C7 H7 106.2 . C10 C13 H13A 109.5 . C10 C13 H13B 109.5 . H13A C13 H13B 109.5 . C10 C13 H13C 109.5 . H13A C13 H13C 109.5 . H13B C13 H13C 109.5 . O18 C43 C44 105.3(7) . O18 C43 C45 109.4(7) . C44 C43 C45 110.9(8) . O18 C43 H43 110.4 . C44 C43 H43 110.4 . C45 C43 H43 110.4 . O14 C34 C35 110.9(10) . O14 C34 C36 107.2(10) . C35 C34 C36 111.6(10) . O14 C34 H34 109.0 . C35 C34 H34 109.0 . C36 C34 H34 109.0 . C31 C32 H32A 109.5 . C31 C32 H32B 109.5 . H32A C32 H32B 109.5 . C31 C32 H32C 109.5 . H32A C32 H32C 109.5 . H32B C32 H32C 109.5 . O17 C25 C27 110.4(8) . O17 C25 C26 108.1(8) . C27 C25 C26 114.8(9) . O17 C25 H25 107.8 . C27 C25 H25 107.8 . C26 C25 H25 107.8 . C31 C33 H33A 109.5 . C31 C33 H33B 109.5 . H33A C33 H33B 109.5 . C31 C33 H33C 109.5 . H33A C33 H33C 109.5 . H33B C33 H33C 109.5 . C25 C27 H27A 109.5 . C25 C27 H27B 109.5 . H27A C27 H27B 109.5 . C25 C27 H27C 109.5 . H27A C27 H27C 109.5 . H27B C27 H27C 109.5 . C34 C36 H36A 109.5 . C34 C36 H36B 109.5 . H36A C36 H36B 109.5 . C34 C36 H36C 109.5 . H36A C36 H36C 109.5 . H36B C36 H36C 109.5 . C37 C38 H38A 109.5 . C37 C38 H38B 109.5 . H38A C38 H38B 109.5 . C37 C38 H38C 109.5 . H38A C38 H38C 109.5 . H38B C38 H38C 109.5 . C25 C26 H26A 109.5 . C25 C26 H26B 109.5 . H26A C26 H26B 109.5 . C25 C26 H26C 109.5 . H26A C26 H26C 109.5 . H26B C26 H26C 109.5 . C34 C35 H35A 109.5 . C34 C35 H35B 109.5 . H35A C35 H35B 109.5 . C34 C35 H35C 109.5 . H35A C35 H35C 109.5 . H35B C35 H35C 109.5 . C7 C8 H8A 109.5 . C7 C8 H8B 109.5 . H8A C8 H8B 109.5 . C7 C8 H8C 109.5 . H8A C8 H8C 109.5 . H8B C8 H8C 109.5 . C7 C9 H9A 109.5 . C7 C9 H9B 109.5 . H9A C9 H9B 109.5 . C7 C9 H9C 109.5 . H9A C9 H9C 109.5 . H9B C9 H9C 109.5 . C43 C44 H44A 109.5 . C43 C44 H44B 109.5 . H44A C44 H44B 109.5 . C43 C44 H44C 109.5 . H44A C44 H44C 109.5 . H44B C44 H44C 109.5 . O22 C40 C41 115.0(10) . O22 C40 C42 117.1(11) . C41 C40 C42 124.9(13) . O22 C40 H40 95.8 . C41 C40 H40 95.8 . C42 C40 H40 95.8 . C28 C30 H30A 109.5 . C28 C30 H30B 109.5 . H30A C30 H30B 109.5 . C28 C30 H30C 109.5 . H30A C30 H30C 109.5 . H30B C30 H30C 109.5 . O20 C22 C23 110.3(9) . O20 C22 C24 107.6(9) . C23 C22 C24 101.3(9) . O20 C22 H22 112.3 . C23 C22 H22 112.3 . C24 C22 H22 112.3 . C3 C1 O1 115.9(16) . C3 C1 C2 116.3(15) . O1 C1 C2 110.5(14) . C3 C1 H1 104.1 . O1 C1 H1 104.1 . C2 C1 H1 104.1 . C6 C4 O2 119.0(17) . C6 C4 C5 106.4(17) . O2 C4 C5 106.4(13) . C6 C4 H4 108.2 . O2 C4 H4 108.2 . C5 C4 H4 108.2 . C29 C28 O16 115.6(10) . C29 C28 C30 125.8(11) . O16 C28 C30 118.4(10) . C37 C39 H39A 109.5 . C37 C39 H39B 109.5 . H39A C39 H39B 109.5 . C37 C39 H39C 109.5 . H39A C39 H39C 109.5 . H39B C39 H39C 109.5 . C43 C45 H45A 109.5 . C43 C45 H45B 109.5 . H45A C45 H45B 109.5 . C43 C45 H45C 109.5 . H45A C45 H45C 109.5 . H45B C45 H45C 109.5 . C40 C41 H41A 109.5 . C40 C41 H41B 109.5 . H41A C41 H41B 109.5 . C40 C41 H41C 109.5 . H41A C41 H41C 109.5 . H41B C41 H41C 109.5 . C4 C6 H6A 109.5 . C4 C6 H6B 109.5 . H6A C6 H6B 109.5 . C4 C6 H6C 109.5 . H6A C6 H6C 109.5 . H6B C6 H6C 109.5 . C28 C29 H29A 109.5 . C28 C29 H29B 109.5 . H29A C29 H29B 109.5 . C28 C29 H29C 109.5 . H29A C29 H29C 109.5 . H29B C29 H29C 109.5 . C22 C24 H24A 109.5 . C22 C24 H24B 109.5 . H24A C24 H24B 109.5 . C22 C24 H24C 109.5 . H24A C24 H24C 109.5 . H24B C24 H24C 109.5 . C40 C42 H42A 109.5 . C40 C42 H42B 109.5 . H42A C42 H42B 109.5 . C40 C42 H42C 109.5 . H42A C42 H42C 109.5 . H42B C42 H42C 109.5 . C4 C5 H5A 109.5 . C4 C5 H5B 109.5 . H5A C5 H5B 109.5 . C4 C5 H5C 109.5 . H5A C5 H5C 109.5 . H5B C5 H5C 109.5 . O19 C19 C20 117.7(15) . O19 C19 C21 120.0(15) . C20 C19 C21 113.9(16) . O19 C19 H19 99.7 . C20 C19 H19 99.7 . C21 C19 H19 99.7 . C22 C23 H23A 109.5 . C22 C23 H23B 109.5 . H23A C23 H23B 109.5 . C22 C23 H23C 109.5 . H23A C23 H23C 109.5 . H23B C23 H23C 109.5 . C1 C3 H3A 109.5 . C1 C3 H3B 109.5 . H3A C3 H3B 109.5 . C1 C3 H3C 109.5 . H3A C3 H3C 109.5 . H3B C3 H3C 109.5 . 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 . C19 C20 H20A 109.5 . C19 C20 H20B 109.5 . H20A C20 H20B 109.5 . C19 C20 H20C 109.5 . H20A C20 H20C 109.5 . H20B C20 H20C 109.5 . C19 C21 H21A 109.5 . C19 C21 H21B 109.5 . H21A C21 H21B 109.5 . C19 C21 H21C 109.5 . H21A C21 H21C 109.5 . H21B C21 H21C 109.5 . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ti3 O22 1.771(5) . Ti3 O12 1.981(5) . Ti3 O6 1.987(5) . Ti3 O8 1.998(5) . Ti3 O11 2.134(5) . Ti3 N1 2.262(7) . Ti3 N2 2.263(7) . Ti3 Ti2 3.0898(19) . Ti3 Ti4 3.0931(19) . Ti5 O14 1.775(5) . Ti5 O15 1.802(6) . Ti5 O5 1.948(5) . Ti5 O12 2.001(5) . Ti5 O13 2.051(5) . Ti5 O10 2.230(5) . Ti5 Ti4 3.1111(19) . Ti4 O16 1.766(6) . Ti4 O12 1.858(5) . Ti4 O11 1.875(5) . Ti4 O13 2.016(6) . Ti4 O17 2.064(5) . Ti4 O9 2.186(5) . Ti4 Ti6 3.2916(19) . Ti6 O20 1.773(6) . Ti6 O21 1.798(6) . Ti6 O18 1.807(6) . Ti6 O17 1.980(5) . Ti6 O9 2.214(5) . Ti6 Ti2 3.323(2) . Ti2 O19 1.763(7) . Ti2 O21 1.847(5) . Ti2 O6 1.884(5) . Ti2 O11 1.920(5) . Ti2 O3 2.003(6) . Ti2 Ti1 3.119(2) . Ti1 O1 1.788(6) . Ti1 O2 1.804(6) . Ti1 O4 1.965(6) . Ti1 O6 1.981(5) . Ti1 O3 2.008(6) . Ti1 O7 2.297(5) . O10 C16 1.243(9) . O8 C14 1.280(9) . O9 C16 1.274(10) . O13 C31 1.438(10) . O7 C14 1.234(10) . O5 N1 1.344(8) . O17 C25 1.469(11) . O22 C40 1.336(13) . O15 C37 1.404(12) . O3 C7 1.415(11) . O4 N2 1.352(8) . O16 C28 1.365(13) . O18 C43 1.419(10) . O14 C34 1.425(12) . N1 C11 1.288(10) . N2 C10 1.246(10) . O2 C4 1.343(15) . O1 C1 1.411(17) . C15 C18 1.340(11) 2_566 C15 C17 1.421(12) . C15 C14 1.515(13) . O20 C22 1.438(12) . C18 C15 1.340(11) 2_566 C18 C17 1.396(12) . C18 H18 0.9300 . O19 C19 1.320(17) . C17 C16 1.491(12) . C11 C10 1.476(11) . C11 C12 1.506(12) . C10 C13 1.505(11) . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C31 C33 1.488(12) . C31 C32 1.498(13) . C31 H31 0.9800 . C37 C39 1.446(14) . C37 C38 1.485(16) . C37 H37 0.9800 . C7 C9 1.471(14) . C7 C8 1.479(16) . C7 H7 0.9800 . C13 H13A 0.9600 . C13 H13B 0.9600 . C13 H13C 0.9600 . C43 C44 1.512(13) . C43 C45 1.543(12) . C43 H43 0.9800 . C34 C35 1.517(15) . C34 C36 1.551(16) . C34 H34 0.9800 . C32 H32A 0.9600 . C32 H32B 0.9600 . C32 H32C 0.9600 . C25 C27 1.512(14) . C25 C26 1.522(13) . C25 H25 0.9800 . C33 H33A 0.9600 . C33 H33B 0.9600 . C33 H33C 0.9600 . C27 H27A 0.9600 . C27 H27B 0.9600 . C27 H27C 0.9600 . C36 H36A 0.9600 . C36 H36B 0.9600 . C36 H36C 0.9600 . C38 H38A 0.9600 . C38 H38B 0.9600 . C38 H38C 0.9600 . C26 H26A 0.9600 . C26 H26B 0.9600 . C26 H26C 0.9600 . C35 H35A 0.9600 . C35 H35B 0.9600 . C35 H35C 0.9600 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C9 H9A 0.9600 . C9 H9B 0.9600 . C9 H9C 0.9600 . C44 H44A 0.9600 . C44 H44B 0.9600 . C44 H44C 0.9600 . C40 C41 1.469(9) . C40 C42 1.470(9) . C40 H40 0.9800 . C30 C28 1.449(14) . C30 H30A 0.9600 . C30 H30B 0.9600 . C30 H30C 0.9600 . C22 C23 1.476(8) . C22 C24 1.514(15) . C22 H22 0.9800 . C1 C3 1.35(2) . C1 C2 1.50(2) . C1 H1 0.9800 . C4 C6 1.34(2) . C4 C5 1.469(9) . C4 H4 0.9800 . C28 C29 1.363(14) . C39 H39A 0.9600 . C39 H39B 0.9600 . C39 H39C 0.9600 . C45 H45A 0.9600 . C45 H45B 0.9600 . C45 H45C 0.9600 . C41 H41A 0.9600 . C41 H41B 0.9600 . C41 H41C 0.9600 . C6 H6A 0.9600 . C6 H6B 0.9600 . C6 H6C 0.9600 . C29 H29A 0.9600 . C29 H29B 0.9600 . C29 H29C 0.9600 . C24 H24A 0.9600 . C24 H24B 0.9600 . C24 H24C 0.9600 . C42 H42A 0.9600 . C42 H42B 0.9600 . C42 H42C 0.9600 . C5 H5A 0.9600 . C5 H5B 0.9600 . C5 H5C 0.9600 . C19 C20 1.471(19) . C19 C21 1.475(9) . C19 H19 0.9800 . C23 H23A 0.9600 . C23 H23B 0.9600 . C23 H23C 0.9600 . C3 H3A 0.9600 . C3 H3B 0.9600 . C3 H3C 0.9600 . C2 H2A 0.9600 . C2 H2B 0.9600 . C2 H2C 0.9600 . C20 H20A 0.9600 . C20 H20B 0.9600 . C20 H20C 0.9600 . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 .