#------------------------------------------------------------------------------ #$Date: 2019-06-05 04:04:15 +0300 (Wed, 05 Jun 2019) $ #$Revision: 215695 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/12/1551217.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_1551217 _journal_paper_doi 10.1039/C9DT02032B _chemical_formula_moiety 'C82 H169 N5 O36 Ti10' _chemical_formula_sum 'C82 H169 N5 O36 Ti10' _chemical_formula_weight 2311.89 _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 82.343(4) _cell_angle_beta 85.367(3) _cell_angle_gamma 70.160(4) _cell_formula_units_Z 1 _cell_length_a 11.8011(4) _cell_length_b 13.8482(7) _cell_length_c 18.9934(7) _cell_measurement_reflns_used 6798 _cell_measurement_temperature 99.98(13) _cell_measurement_theta_max 74.3000 _cell_measurement_theta_min 4.3020 _cell_volume 2891.6(2) _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 99.98(13) _diffrn_detector_area_resol_mean 10.3503 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.966 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0326 _diffrn_reflns_av_unetI/netI 0.0439 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.966 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 20280 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.966 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 74.491 _diffrn_reflns_theta_min 3.415 _diffrn_source 'micro-focus sealed X-ray tube' _exptl_absorpt_coefficient_mu 6.187 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.20321 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour yellow _exptl_crystal_density_diffrn 1.324 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 1213 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.446 _refine_diff_density_min -1.085 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 622 _refine_ls_number_reflns 11438 _refine_ls_number_restraints 358 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.1234 _refine_ls_R_factor_gt 0.0991 _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^)+(0.2412P)^2^+6.2584P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2935 _refine_ls_wR_factor_ref 0.3370 _reflns_Friedel_coverage 0.000 _reflns_number_gt 8505 _reflns_number_total 11438 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9dt02032b2.cif _cod_data_source_block a_CCDC2 _cod_database_code 1551217 _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 0.688 _oxdiff_exptl_absorpt_empirical_full_max 3.541 _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 0.210, Rweak 0.005, Alpha 0.042, Orientation as input REM Formula found by SHELXT: C40 N5 O18 Ti5 CELL 1.54178 11.8011 13.8482 18.9934 82.343 85.367 70.16 ZERR 1 0.0004 0.0007 0.0007 0.004 0.003 0.004 LATT 1 SFAC C H N O Ti UNIT 82 162 5 38 10 DFIX 1.52 0.01 C36 C37 DELU C27 C29 DELU O16 C27 DELU C8 C10 SIMU 0.02 0.04 C39 C40 C41 O19 SIMU 0.01 0.02 C20 C21 C22 O10 ISOR 0.01 0.02 C27 C39 SIMU 0.005 0.01 3.8 $C DELU 0.0008 0.0004 O16 C27 L.S. 60 PLAN 20 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.241200 6.258400 FVAR 0.27137 TI3 5 0.587247 0.646413 0.212097 11.00000 0.05576 0.03890 = 0.03311 -0.00318 -0.01262 -0.01940 TI1 5 0.764977 0.376514 0.226233 11.00000 0.05228 0.04594 = 0.03979 -0.00617 -0.00692 -0.01173 TI5 5 0.371534 0.903063 0.236841 11.00000 0.07275 0.03539 = 0.04439 -0.00556 -0.01340 -0.01835 TI2 5 0.847270 0.551880 0.271617 11.00000 0.05142 0.06275 = 0.03610 -0.01012 -0.00785 -0.02245 TI4 5 0.650342 0.825521 0.265287 11.00000 0.07959 0.04577 = 0.04336 0.00245 -0.02603 -0.03223 O13 4 0.541743 0.603411 0.316838 11.00000 0.04788 0.03822 = 0.03694 -0.00329 -0.01139 -0.01419 O6 4 0.726366 0.521296 0.217454 11.00000 0.04951 0.04975 = 0.03560 -0.00777 -0.00584 -0.01732 O12 4 0.724875 0.534103 0.363626 11.00000 0.04567 0.05061 = 0.03343 -0.00453 -0.00586 -0.01204 O8 4 0.518328 0.790189 0.236413 11.00000 0.07200 0.04063 = 0.04418 -0.00236 -0.01440 -0.02678 O7 4 0.725395 0.685862 0.250857 11.00000 0.06226 0.05575 = 0.03759 -0.00673 -0.01025 -0.02630 O5 4 0.891909 0.393959 0.280271 11.00000 0.04442 0.06480 = 0.04590 -0.00780 -0.00647 -0.01082 O21 4 0.595319 0.681180 0.118770 11.00000 0.08720 0.05217 = 0.03642 -0.00395 -0.01430 -0.02822 O1 4 0.595353 0.416018 0.202970 11.00000 0.05186 0.03585 = 0.06607 -0.01732 -0.00706 -0.00896 O11 4 0.949918 0.556360 0.195628 11.00000 0.05790 0.08047 = 0.04485 -0.01503 -0.00202 -0.03299 O20 4 0.298956 1.001374 0.169046 11.00000 0.05669 0.04055 = 0.06928 0.00272 -0.00984 -0.01210 O2 4 0.316636 0.801053 0.201308 11.00000 0.08000 0.02941 = 0.08821 -0.00900 -0.05137 -0.00309 O4 4 0.839811 0.326386 0.146814 11.00000 0.06816 0.06090 = 0.06013 -0.01872 -0.01089 0.00054 O18 4 0.503692 0.956337 0.255998 11.00000 0.09806 0.03925 = 0.08114 -0.00654 -0.03847 -0.02729 O10 4 0.940699 0.568454 0.336837 11.00000 0.05780 0.11286 = 0.04637 -0.01866 -0.00842 -0.03879 N1 3 0.520039 0.516314 0.198873 11.00000 0.05411 0.03508 = 0.03935 -0.00846 -0.01174 -0.01066 N2 3 0.384648 0.699905 0.203243 11.00000 0.06378 0.03455 = 0.04814 -0.00457 -0.02670 -0.00836 O16 4 0.673431 0.827442 0.356389 11.00000 0.12457 0.05677 = 0.07618 -0.01711 -0.04863 -0.01899 O3 4 0.748600 0.269835 0.286372 11.00000 0.07791 0.07277 = 0.07631 0.01817 -0.02179 -0.02861 C24 1 0.553605 0.528916 0.435380 11.00000 0.04904 0.03639 = 0.03858 -0.00656 -0.00769 -0.01466 O17 4 0.744989 0.883327 0.207982 11.00000 0.08609 0.07812 = 0.10096 0.02875 -0.03578 -0.04929 C23 1 0.612242 0.557486 0.366762 11.00000 0.05233 0.03796 = 0.03825 -0.00772 -0.00591 -0.01661 C26 1 0.570342 0.456700 0.558246 11.00000 0.04780 0.03923 = 0.03807 -0.00533 -0.00803 -0.01188 C25 1 0.623438 0.484907 0.494627 11.00000 0.04525 0.03921 = 0.03917 -0.00477 -0.00801 -0.01247 AFIX 43 H25 2 0.705720 0.474450 0.491490 11.00000 -1.20000 AFIX 0 O19 4 0.287780 0.917416 0.317602 11.00000 0.15577 0.08482 = 0.06086 -0.02892 0.02452 -0.07230 C1 1 0.408112 0.528231 0.194767 11.00000 0.05805 0.03769 = 0.05644 -0.01349 -0.01362 -0.01414 C3 1 0.328273 0.637469 0.194200 11.00000 0.05704 0.03907 = 0.06126 -0.01403 -0.01998 -0.01083 C14 1 0.946583 0.547618 0.121724 11.00000 0.06680 0.07870 = 0.04295 -0.01299 -0.00511 -0.03737 AFIX 13 H14 2 0.882411 0.520192 0.114722 11.00000 -1.20000 AFIX 0 C8 1 0.984540 0.313455 0.317776 11.00000 0.05298 0.06850 = 0.05373 -0.00364 -0.01597 -0.01766 AFIX 13 H8 2 0.989878 0.248378 0.300519 11.00000 -1.20000 AFIX 0 C2 1 0.359798 0.442174 0.193298 11.00000 0.05876 0.04411 = 0.08362 -0.01574 -0.01690 -0.01611 AFIX 33 H2A 2 0.273735 0.469715 0.190079 11.00000 -1.50000 H2B 2 0.394395 0.405954 0.152846 11.00000 -1.50000 H2C 2 0.380125 0.395391 0.236021 11.00000 -1.50000 AFIX 0 C11 1 0.835591 0.312416 0.076540 11.00000 0.06728 0.07284 = 0.06451 -0.02936 0.00326 -0.01946 AFIX 13 H11 2 0.911958 0.314485 0.053108 11.00000 -1.20000 AFIX 0 C4 1 0.195795 0.670936 0.185679 11.00000 0.06385 0.05066 = 0.08913 -0.02229 -0.02948 -0.00689 AFIX 33 H4A 2 0.173210 0.612232 0.179676 11.00000 -1.50000 H4B 2 0.154489 0.701106 0.227201 11.00000 -1.50000 H4C 2 0.174217 0.721062 0.144660 11.00000 -1.50000 AFIX 0 C15 1 1.063523 0.475260 0.098433 11.00000 0.07405 0.09089 = 0.04956 -0.02380 -0.00530 -0.02677 AFIX 33 H15A 2 1.062109 0.468905 0.048820 11.00000 -1.50000 H15B 2 1.126948 0.501100 0.105979 11.00000 -1.50000 H15C 2 1.077459 0.408785 0.125372 11.00000 -1.50000 AFIX 0 C16 1 0.918043 0.654000 0.082617 11.00000 0.06847 0.08514 = 0.05372 -0.00838 -0.00101 -0.03027 AFIX 33 H16A 2 0.915207 0.650506 0.032678 11.00000 -1.50000 H16B 2 0.841311 0.697484 0.099641 11.00000 -1.50000 H16C 2 0.979335 0.682133 0.090489 11.00000 -1.50000 AFIX 0 C9 1 0.950050 0.305412 0.395579 11.00000 0.06163 0.09801 = 0.06624 0.00497 -0.01831 -0.01927 AFIX 33 H9A 2 1.012622 0.251140 0.420649 11.00000 -1.50000 H9B 2 0.939372 0.369703 0.413472 11.00000 -1.50000 H9C 2 0.876088 0.290247 0.402391 11.00000 -1.50000 AFIX 0 C38 1 0.550513 0.844769 0.048294 11.00000 0.16855 0.05999 = 0.06230 0.01577 -0.03392 -0.05038 AFIX 33 H38A 2 0.555020 0.864601 0.094255 11.00000 -1.50000 H38B 2 0.619814 0.848181 0.019261 11.00000 -1.50000 H38C 2 0.478682 0.890853 0.026151 11.00000 -1.50000 AFIX 0 C17 1 0.871812 0.868700 0.186995 11.00000 0.07007 0.07411 = 0.06442 -0.00926 -0.00377 -0.03285 AFIX 13 H17 2 0.919109 0.794999 0.194211 11.00000 -1.20000 AFIX 0 C13 1 0.735332 0.403073 0.040472 11.00000 0.08416 0.07339 = 0.06877 -0.00610 -0.01320 -0.02903 AFIX 33 H13A 2 0.732647 0.393121 -0.008349 11.00000 -1.50000 H13B 2 0.659362 0.406817 0.064380 11.00000 -1.50000 H13C 2 0.751049 0.466189 0.042744 11.00000 -1.50000 AFIX 0 C5 1 0.662977 0.229535 0.324356 11.00000 0.10816 0.06739 = 0.07041 -0.00712 -0.00495 -0.04737 AFIX 13 H5 2 0.614312 0.216602 0.289594 11.00000 -1.20000 AFIX 0 C30 1 0.511626 1.058970 0.256269 11.00000 0.09617 0.05461 = 0.11498 -0.02533 -0.01110 -0.03644 AFIX 13 H30 2 0.581983 1.053723 0.282562 11.00000 -1.20000 AFIX 0 C39 1 0.187766 0.910195 0.358200 11.00000 0.08504 0.13125 = 0.08679 -0.04704 -0.00118 -0.01720 AFIX 13 H39 2 0.156138 0.858479 0.344937 11.00000 -1.20000 AFIX 0 C35 1 0.171157 0.989660 0.082522 11.00000 0.08487 0.08682 = 0.10145 0.03878 -0.04408 -0.03438 AFIX 33 H35A 2 0.127816 1.028447 0.041569 11.00000 -1.50000 H35B 2 0.228700 0.926236 0.069334 11.00000 -1.50000 H35C 2 0.115599 0.974548 0.118428 11.00000 -1.50000 AFIX 0 C19 1 0.879718 0.908750 0.108430 11.00000 0.09240 0.07813 = 0.06695 -0.00253 -0.01007 -0.03491 AFIX 33 H19A 2 0.962311 0.899527 0.094190 11.00000 -1.50000 H19B 2 0.848884 0.871051 0.080446 11.00000 -1.50000 H19C 2 0.832925 0.980832 0.101297 11.00000 -1.50000 AFIX 0 O15 4 0.659636 0.474980 0.654706 10.50000 0.05277 0.07812 = 0.04207 -0.00211 -0.00507 -0.03562 C18 1 0.918980 0.926780 0.232094 11.00000 0.08369 0.08229 = 0.06986 -0.01166 -0.00634 -0.03112 AFIX 33 H18A 2 1.001859 0.917566 0.218667 11.00000 -1.50000 H18B 2 0.872389 0.998931 0.225220 11.00000 -1.50000 H18C 2 0.912846 0.900974 0.281227 11.00000 -1.50000 AFIX 0 C33 1 0.236490 1.052452 0.111332 11.00000 0.11150 0.06816 = 0.10321 0.03028 -0.05003 -0.00949 O14 4 0.696607 0.321611 0.625867 10.50000 0.04966 0.06301 = 0.05019 -0.00111 -0.00677 0.00393 C36 1 0.547574 0.741752 0.056046 11.00000 0.21306 0.06337 = 0.05697 0.01377 -0.05963 -0.04968 C32 1 0.524365 1.107883 0.178756 11.00000 0.08994 0.05904 = 0.12049 -0.01102 -0.00006 -0.03217 AFIX 33 H32A 2 0.529536 1.175463 0.179393 11.00000 -1.50000 H32B 2 0.596048 1.065140 0.156025 11.00000 -1.50000 H32C 2 0.455376 1.113253 0.152981 11.00000 -1.50000 AFIX 0 C34 1 0.184088 1.161071 0.108204 11.00000 0.08196 0.07163 = 0.13602 0.04117 -0.03609 -0.02455 AFIX 33 H34A 2 0.142526 1.187594 0.064666 11.00000 -1.50000 H34B 2 0.128023 1.178439 0.147822 11.00000 -1.50000 H34C 2 0.246137 1.190928 0.110001 11.00000 -1.50000 AFIX 0 C6 1 0.584160 0.299493 0.368890 11.00000 0.11420 0.06657 = 0.07393 -0.00211 0.00398 -0.03113 AFIX 33 H6A 2 0.527937 0.269168 0.393487 11.00000 -1.50000 H6B 2 0.629996 0.314633 0.402836 11.00000 -1.50000 H6C 2 0.541028 0.362181 0.340587 11.00000 -1.50000 AFIX 0 C31 1 0.401832 1.123177 0.291570 11.00000 0.10217 0.07524 = 0.13456 -0.04205 0.00736 -0.03958 AFIX 33 H31A 2 0.405852 1.191155 0.292127 11.00000 -1.50000 H31B 2 0.332761 1.127697 0.266185 11.00000 -1.50000 H31C 2 0.395089 1.092662 0.339480 11.00000 -1.50000 AFIX 0 N3 3 0.643636 0.414899 0.617942 10.50000 0.02828 0.05350 = 0.04363 0.00239 -0.00479 -0.01095 C7 1 0.728266 0.127590 0.365785 11.00000 0.12728 0.06809 = 0.08470 0.00092 -0.00875 -0.04090 AFIX 33 H7A 2 0.670629 0.100001 0.391598 11.00000 -1.50000 H7B 2 0.775799 0.080134 0.333602 11.00000 -1.50000 H7C 2 0.779977 0.137669 0.398554 11.00000 -1.50000 AFIX 0 C10 1 1.107209 0.331215 0.298860 11.00000 0.07774 0.10661 = 0.08573 -0.00965 -0.00728 -0.01982 AFIX 33 H10A 2 1.170006 0.277220 0.323965 11.00000 -1.50000 H10B 2 1.124333 0.330602 0.248611 11.00000 -1.50000 H10C 2 1.102999 0.396783 0.312327 11.00000 -1.50000 AFIX 0 C20 1 0.967767 0.596465 0.401106 11.00000 0.09531 0.13171 = 0.08499 -0.03054 -0.01885 -0.04652 AFIX 13 H20 2 0.902701 0.600140 0.437221 11.00000 -1.20000 AFIX 0 C37 1 0.540882 0.682439 0.000306 11.00000 0.20808 0.07862 = 0.07449 0.00727 -0.06855 -0.04629 AFIX 33 H37A 2 0.507517 0.728533 -0.040920 11.00000 -1.50000 H37B 2 0.620287 0.637791 -0.011638 11.00000 -1.50000 H37C 2 0.490399 0.641615 0.016470 11.00000 -1.50000 AFIX 0 C12 1 0.826148 0.214162 0.067725 11.00000 0.10638 0.07896 = 0.11733 -0.03426 -0.02933 -0.01739 AFIX 33 H12A 2 0.823590 0.208889 0.018031 11.00000 -1.50000 H12B 2 0.894741 0.159876 0.087448 11.00000 -1.50000 H12C 2 0.753794 0.207978 0.091799 11.00000 -1.50000 AFIX 0 C21 1 0.988603 0.697237 0.385313 11.00000 0.13337 0.14415 = 0.10527 -0.02630 -0.02342 -0.05932 AFIX 33 H21A 2 1.007055 0.717354 0.428283 11.00000 -1.50000 H21B 2 1.054856 0.690767 0.351360 11.00000 -1.50000 H21C 2 0.917361 0.748703 0.366091 11.00000 -1.50000 AFIX 0 C28 1 0.556818 0.798331 0.442250 11.00000 0.12845 0.11125 = 0.08506 -0.01251 -0.00446 -0.02797 AFIX 33 H28A 2 0.544672 0.774305 0.491126 11.00000 -1.50000 H28B 2 0.507827 0.869531 0.432718 11.00000 -1.50000 H28C 2 0.534614 0.757775 0.412110 11.00000 -1.50000 AFIX 0 C27 1 0.688283 0.787893 0.427731 11.00000 0.14938 0.13458 = 0.07125 -0.00737 -0.01695 -0.05089 C29 1 0.728488 0.857956 0.465181 11.00000 0.15485 0.13603 = 0.08872 -0.02285 -0.02753 -0.05208 AFIX 33 H29A 2 0.738989 0.831360 0.514420 11.00000 -1.50000 H29B 2 0.803589 0.862008 0.443920 11.00000 -1.50000 H29C 2 0.668771 0.925607 0.461313 11.00000 -1.50000 AFIX 0 C22 1 1.088481 0.514657 0.426690 11.00000 0.11024 0.15199 = 0.10805 -0.02337 -0.03316 -0.02994 AFIX 33 H22A 2 1.109147 0.531652 0.470213 11.00000 -1.50000 H22B 2 1.079649 0.447605 0.434557 11.00000 -1.50000 H22C 2 1.151161 0.514216 0.391091 11.00000 -1.50000 AFIX 0 C40 1 0.104305 1.021286 0.341947 11.00000 0.12727 0.16054 = 0.13684 -0.02997 0.00226 -0.01363 AFIX 33 H40A 2 0.028098 1.029749 0.366904 11.00000 -1.50000 H40B 2 0.140007 1.067594 0.356960 11.00000 -1.50000 H40C 2 0.092275 1.036441 0.291748 11.00000 -1.50000 AFIX 0 C41 1 0.199673 0.905289 0.431549 11.00000 0.13532 0.15813 = 0.12005 -0.02369 0.00467 -0.02040 AFIX 33 H41A 2 0.251348 0.837648 0.449027 11.00000 -1.50000 H41B 2 0.234049 0.955904 0.440580 11.00000 -1.50000 H41C 2 0.121775 0.918955 0.455270 11.00000 -1.50000 AFIX 0 HKLF 4 REM a_a.res in P-1 REM R1 = 0.0991 for 8505 Fo > 4sig(Fo) and 0.1234 for all 11438 data REM 622 parameters refined using 358 restraints END WGHT 0.1893 7.8663 REM Highest difference peak 1.446, deepest hole -1.085, 1-sigma level 0.133 Q1 1 0.6182 0.8675 0.4156 11.00000 0.05 1.45 Q2 1 1.0323 0.2069 0.2745 11.00000 0.05 1.42 Q3 1 0.0807 0.9618 0.4024 11.00000 0.05 1.38 Q4 1 0.2755 0.8134 0.4164 11.00000 0.05 1.37 Q5 1 0.5952 0.8367 0.2859 11.00000 0.05 1.23 Q6 1 0.4049 1.0649 0.3746 11.00000 0.05 1.12 Q7 1 1.0625 0.5542 0.3386 11.00000 0.05 1.08 Q8 1 1.0270 0.6284 0.3446 11.00000 0.05 1.06 Q9 1 0.6225 0.7535 0.4836 11.00000 0.05 1.06 Q10 1 0.1792 1.0373 0.1304 11.00000 0.05 1.02 Q11 1 0.4838 0.7103 0.0222 11.00000 0.05 1.01 Q12 1 0.9864 0.7434 0.3105 11.00000 0.05 1.01 Q13 1 0.4540 1.0581 0.2992 11.00000 0.05 0.93 Q14 1 0.3079 0.9197 0.2500 11.00000 0.05 0.91 Q15 1 0.2120 0.9447 0.3072 11.00000 0.05 0.85 Q16 1 0.7883 0.2078 0.1060 11.00000 0.05 0.78 Q17 1 0.7321 0.9792 0.1794 11.00000 0.05 0.76 Q18 1 0.5012 0.7436 0.0537 11.00000 0.05 0.76 Q19 1 0.6049 0.7209 0.0420 11.00000 0.05 0.76 Q20 1 1.1484 0.4679 0.3844 11.00000 0.05 0.73 ; _shelx_res_checksum 57273 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy Ti3 Ti 0.58725(10) 0.64641(7) 0.21210(5) 0.0411(3) Uani 1 1 d . . . Ti1 Ti 0.76498(10) 0.37651(8) 0.22623(6) 0.0468(3) Uani 1 1 d . . . Ti5 Ti 0.37153(12) 0.90306(8) 0.23684(6) 0.0500(3) Uani 1 1 d . . . Ti2 Ti 0.84727(10) 0.55188(9) 0.27162(5) 0.0484(3) Uani 1 1 d . . . Ti4 Ti 0.65034(12) 0.82552(9) 0.26529(6) 0.0527(3) Uani 1 1 d . . . O13 O 0.5417(3) 0.6034(3) 0.3168(2) 0.0406(8) Uani 1 1 d . . . O6 O 0.7264(4) 0.5213(3) 0.2175(2) 0.0442(8) Uani 1 1 d . . . O12 O 0.7249(4) 0.5341(3) 0.3636(2) 0.0440(8) Uani 1 1 d . . . O8 O 0.5183(4) 0.7902(3) 0.2364(2) 0.0497(10) Uani 1 1 d . . . O7 O 0.7254(4) 0.6859(3) 0.2509(2) 0.0495(9) Uani 1 1 d . . . O5 O 0.8919(4) 0.3940(4) 0.2803(2) 0.0532(10) Uani 1 1 d . . . O21 O 0.5953(5) 0.6812(4) 0.1188(2) 0.0567(11) Uani 1 1 d . . . O1 O 0.5954(4) 0.4160(3) 0.2030(3) 0.0513(10) Uani 1 1 d . . . O11 O 0.9499(4) 0.5564(4) 0.1956(2) 0.0577(11) Uani 1 1 d . . . O20 O 0.2990(4) 1.0014(3) 0.1690(3) 0.0570(11) Uani 1 1 d . . . O2 O 0.3166(5) 0.8011(3) 0.2013(3) 0.0667(15) Uani 1 1 d . . . O4 O 0.8398(5) 0.3264(4) 0.1468(3) 0.0671(13) Uani 1 1 d . . . O18 O 0.5037(5) 0.9563(4) 0.2560(3) 0.0697(14) Uani 1 1 d . . . O10 O 0.9407(4) 0.5685(5) 0.3368(3) 0.0684(14) Uani 1 1 d . U . N1 N 0.5200(5) 0.5163(4) 0.1989(2) 0.0429(10) Uani 1 1 d . . . N2 N 0.3846(5) 0.6999(4) 0.2032(3) 0.0495(12) Uani 1 1 d . . . O16 O 0.6734(7) 0.8274(4) 0.3564(3) 0.0852(19) Uani 1 1 d . U . O3 O 0.7486(5) 0.2698(5) 0.2864(3) 0.0762(15) Uani 1 1 d . . . C24 C 0.5536(5) 0.5289(4) 0.4354(3) 0.0406(9) Uani 1 1 d . U . O17 O 0.7450(6) 0.8833(5) 0.2080(4) 0.0846(19) Uani 1 1 d . . . C23 C 0.6122(5) 0.5575(4) 0.3668(3) 0.0419(10) Uani 1 1 d . U . C26 C 0.5703(5) 0.4567(4) 0.5582(3) 0.0419(10) Uani 1 1 d . U . C25 C 0.6234(5) 0.4849(4) 0.4946(3) 0.0412(10) Uani 1 1 d . U . H25 H 0.7057 0.4744 0.4915 0.049 Uiso 1 1 calc R U . O19 O 0.2878(8) 0.9174(5) 0.3176(3) 0.092(2) Uani 1 1 d . U . C1 C 0.4081(6) 0.5282(4) 0.1948(4) 0.0497(12) Uani 1 1 d . U . C3 C 0.3283(6) 0.6375(5) 0.1942(4) 0.0520(12) Uani 1 1 d . U . C14 C 0.9466(7) 0.5476(6) 0.1217(3) 0.0587(15) Uani 1 1 d . U . H14 H 0.8824 0.5202 0.1147 0.070 Uiso 1 1 calc R U . C8 C 0.9845(6) 0.3135(6) 0.3178(4) 0.0586(15) Uani 1 1 d . U . H8 H 0.9899 0.2484 0.3005 0.070 Uiso 1 1 calc R U . C2 C 0.3598(7) 0.4422(5) 0.1933(4) 0.0608(15) Uani 1 1 d . U . H2A H 0.2737 0.4697 0.1901 0.091 Uiso 1 1 calc R U . H2B H 0.3944 0.4060 0.1528 0.091 Uiso 1 1 calc R U . H2C H 0.3801 0.3954 0.2360 0.091 Uiso 1 1 calc R U . C11 C 0.8356(7) 0.3124(6) 0.0765(4) 0.0675(17) Uani 1 1 d . U . H11 H 0.9120 0.3145 0.0531 0.081 Uiso 1 1 calc R U . C4 C 0.1958(7) 0.6709(6) 0.1857(5) 0.0681(17) Uani 1 1 d . U . H4A H 0.1732 0.6122 0.1797 0.102 Uiso 1 1 calc R U . H4B H 0.1545 0.7011 0.2272 0.102 Uiso 1 1 calc R U . H4C H 0.1742 0.7211 0.1447 0.102 Uiso 1 1 calc R U . C15 C 1.0635(7) 0.4753(7) 0.0984(4) 0.0700(18) Uani 1 1 d . U . H15A H 1.0621 0.4689 0.0488 0.105 Uiso 1 1 calc R U . H15B H 1.1269 0.5011 0.1060 0.105 Uiso 1 1 calc R U . H15C H 1.0775 0.4088 0.1254 0.105 Uiso 1 1 calc R U . C16 C 0.9180(7) 0.6540(7) 0.0826(4) 0.0679(16) Uani 1 1 d . U . H16A H 0.9152 0.6505 0.0327 0.102 Uiso 1 1 calc R U . H16B H 0.8413 0.6975 0.0996 0.102 Uiso 1 1 calc R U . H16C H 0.9793 0.6821 0.0905 0.102 Uiso 1 1 calc R U . C9 C 0.9500(8) 0.3054(8) 0.3956(5) 0.078(2) Uani 1 1 d . U . H9A H 1.0126 0.2511 0.4206 0.116 Uiso 1 1 calc R U . H9B H 0.9394 0.3697 0.4135 0.116 Uiso 1 1 calc R U . H9C H 0.8761 0.2902 0.4024 0.116 Uiso 1 1 calc R U . C38 C 0.5505(12) 0.8448(7) 0.0483(5) 0.094(3) Uani 1 1 d . U . H38A H 0.5550 0.8646 0.0943 0.141 Uiso 1 1 calc R U . H38B H 0.6198 0.8482 0.0193 0.141 Uiso 1 1 calc R U . H38C H 0.4787 0.8909 0.0262 0.141 Uiso 1 1 calc R U . C17 C 0.8718(7) 0.8687(7) 0.1870(4) 0.0670(16) Uani 1 1 d . U . H17 H 0.9191 0.7950 0.1942 0.080 Uiso 1 1 calc R U . C13 C 0.7353(8) 0.4031(7) 0.0405(5) 0.0743(19) Uani 1 1 d . U . H13A H 0.7326 0.3931 -0.0083 0.111 Uiso 1 1 calc R U . H13B H 0.6594 0.4068 0.0644 0.111 Uiso 1 1 calc R U . H13C H 0.7510 0.4662 0.0427 0.111 Uiso 1 1 calc R U . C5 C 0.6630(9) 0.2295(7) 0.3244(5) 0.0773(19) Uani 1 1 d . U . H5 H 0.6143 0.2166 0.2896 0.093 Uiso 1 1 calc R U . C30 C 0.5116(9) 1.0590(6) 0.2563(6) 0.084(2) Uani 1 1 d . U . H30 H 0.5820 1.0537 0.2826 0.100 Uiso 1 1 calc R U . C39 C 0.1878(10) 0.9102(11) 0.3582(6) 0.103(3) Uani 1 1 d . U . H39 H 0.1561 0.8585 0.3449 0.123 Uiso 1 1 calc R U . C35 C 0.1712(9) 0.9897(8) 0.0825(6) 0.092(3) Uani 1 1 d . U . H35A H 0.1278 1.0284 0.0416 0.138 Uiso 1 1 calc R U . H35B H 0.2287 0.9262 0.0693 0.138 Uiso 1 1 calc R U . H35C H 0.1156 0.9745 0.1184 0.138 Uiso 1 1 calc R U . C19 C 0.8797(9) 0.9088(7) 0.1084(5) 0.0776(19) Uani 1 1 d . U . H19A H 0.9623 0.8995 0.0942 0.116 Uiso 1 1 calc R U . H19B H 0.8489 0.8711 0.0804 0.116 Uiso 1 1 calc R U . H19C H 0.8329 0.9808 0.1013 0.116 Uiso 1 1 calc R U . O15 O 0.6596(8) 0.4750(8) 0.6547(5) 0.054(2) Uani 0.5 1 d . . P C18 C 0.9190(9) 0.9268(7) 0.2321(5) 0.077(2) Uani 1 1 d . U . H18A H 1.0019 0.9176 0.2187 0.116 Uiso 1 1 calc R U . H18B H 0.8724 0.9989 0.2252 0.116 Uiso 1 1 calc R U . H18C H 0.9128 0.9010 0.2812 0.116 Uiso 1 1 calc R U . C33 C 0.2365(11) 1.0525(8) 0.1113(6) 0.101(3) Uani 1 1 d . U . O14 O 0.6966(8) 0.3216(8) 0.6259(5) 0.060(2) Uani 0.5 1 d . . P C36 C 0.5476(14) 0.7418(7) 0.0560(5) 0.109(3) Uani 1 1 d D U . C32 C 0.5244(9) 1.1079(7) 0.1788(6) 0.088(2) Uani 1 1 d . U . H32A H 0.5295 1.1755 0.1794 0.132 Uiso 1 1 calc R U . H32B H 0.5960 1.0651 0.1560 0.132 Uiso 1 1 calc R U . H32C H 0.4554 1.1133 0.1530 0.132 Uiso 1 1 calc R U . C34 C 0.1841(9) 1.1611(7) 0.1082(7) 0.100(3) Uani 1 1 d . U . H34A H 0.1425 1.1876 0.0647 0.150 Uiso 1 1 calc R U . H34B H 0.1280 1.1784 0.1478 0.150 Uiso 1 1 calc R U . H34C H 0.2461 1.1909 0.1100 0.150 Uiso 1 1 calc R U . C6 C 0.5842(10) 0.2995(7) 0.3689(5) 0.086(2) Uani 1 1 d . U . H6A H 0.5279 0.2692 0.3935 0.128 Uiso 1 1 calc R U . H6B H 0.6300 0.3146 0.4028 0.128 Uiso 1 1 calc R U . H6C H 0.5410 0.3622 0.3406 0.128 Uiso 1 1 calc R U . C31 C 0.4018(10) 1.1232(8) 0.2916(7) 0.099(3) Uani 1 1 d . U . H31A H 0.4059 1.1912 0.2921 0.149 Uiso 1 1 calc R U . H31B H 0.3328 1.1277 0.2662 0.149 Uiso 1 1 calc R U . H31C H 0.3951 1.0927 0.3395 0.149 Uiso 1 1 calc R U . N3 N 0.6436(8) 0.4149(8) 0.6179(5) 0.043(2) Uani 0.5 1 d . . P C7 C 0.7283(11) 0.1276(7) 0.3658(6) 0.092(2) Uani 1 1 d . U . H7A H 0.6706 0.1000 0.3916 0.138 Uiso 1 1 calc R U . H7B H 0.7758 0.0801 0.3336 0.138 Uiso 1 1 calc R U . H7C H 0.7800 0.1377 0.3986 0.138 Uiso 1 1 calc R U . C10 C 1.1072(9) 0.3312(9) 0.2989(6) 0.093(2) Uani 1 1 d . U . H10A H 1.1700 0.2772 0.3240 0.139 Uiso 1 1 calc R U . H10B H 1.1243 0.3306 0.2486 0.139 Uiso 1 1 calc R U . H10C H 1.1030 0.3968 0.3123 0.139 Uiso 1 1 calc R U . C20 C 0.9678(10) 0.5965(10) 0.4011(6) 0.099(2) Uani 1 1 d . U . H20 H 0.9027 0.6001 0.4372 0.119 Uiso 1 1 calc R U . C37 C 0.5409(15) 0.6824(8) 0.0003(5) 0.119(3) Uani 1 1 d D U . H37A H 0.5075 0.7285 -0.0409 0.178 Uiso 1 1 calc R U . H37B H 0.6203 0.6378 -0.0116 0.178 Uiso 1 1 calc R U . H37C H 0.4904 0.6416 0.0165 0.178 Uiso 1 1 calc R U . C12 C 0.8261(11) 0.2142(8) 0.0677(7) 0.101(3) Uani 1 1 d . U . H12A H 0.8236 0.2089 0.0180 0.151 Uiso 1 1 calc R U . H12B H 0.8947 0.1599 0.0874 0.151 Uiso 1 1 calc R U . H12C H 0.7538 0.2080 0.0918 0.151 Uiso 1 1 calc R U . C21 C 0.9886(14) 0.6972(12) 0.3853(7) 0.122(3) Uani 1 1 d . U . H21A H 1.0071 0.7174 0.4283 0.183 Uiso 1 1 calc R U . H21B H 1.0549 0.6908 0.3514 0.183 Uiso 1 1 calc R U . H21C H 0.9174 0.7487 0.3661 0.183 Uiso 1 1 calc R U . C28 C 0.5568(12) 0.7983(11) 0.4422(6) 0.111(2) Uani 1 1 d . U . H28A H 0.5447 0.7743 0.4911 0.167 Uiso 1 1 calc R U . H28B H 0.5078 0.8695 0.4327 0.167 Uiso 1 1 calc R U . H28C H 0.5346 0.7578 0.4121 0.167 Uiso 1 1 calc R U . C27 C 0.6883(14) 0.7879(12) 0.4277(6) 0.117(3) Uani 1 1 d . U . C29 C 0.7285(15) 0.8580(12) 0.4652(7) 0.123(3) Uani 1 1 d . U . H29A H 0.7390 0.8314 0.5144 0.185 Uiso 1 1 calc R U . H29B H 0.8036 0.8620 0.4439 0.185 Uiso 1 1 calc R U . H29C H 0.6688 0.9256 0.4613 0.185 Uiso 1 1 calc R U . C22 C 1.0885(12) 0.5147(12) 0.4267(7) 0.124(3) Uani 1 1 d . U . H22A H 1.1091 0.5317 0.4702 0.187 Uiso 1 1 calc R U . H22B H 1.0796 0.4476 0.4346 0.187 Uiso 1 1 calc R U . H22C H 1.1512 0.5142 0.3911 0.187 Uiso 1 1 calc R U . C40 C 0.1043(15) 1.0213(14) 0.3419(9) 0.150(4) Uani 1 1 d . U . H40A H 0.0281 1.0297 0.3669 0.224 Uiso 1 1 calc R U . H40B H 0.1400 1.0676 0.3570 0.224 Uiso 1 1 calc R U . H40C H 0.0923 1.0364 0.2917 0.224 Uiso 1 1 calc R U . C41 C 0.1997(15) 0.9053(14) 0.4315(8) 0.145(4) Uani 1 1 d . U . H41A H 0.2513 0.8376 0.4490 0.217 Uiso 1 1 calc R U . H41B H 0.2340 0.9559 0.4406 0.217 Uiso 1 1 calc R U . H41C H 0.1218 0.9190 0.4553 0.217 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 0.0558(6) 0.0389(5) 0.0331(5) -0.0032(4) -0.0126(4) -0.0194(4) Ti1 0.0523(6) 0.0459(6) 0.0398(5) -0.0062(4) -0.0069(4) -0.0117(4) Ti5 0.0728(7) 0.0354(5) 0.0444(6) -0.0056(4) -0.0134(5) -0.0183(5) Ti2 0.0514(6) 0.0627(7) 0.0361(5) -0.0101(4) -0.0078(4) -0.0224(5) Ti4 0.0796(8) 0.0458(6) 0.0434(6) 0.0024(4) -0.0260(5) -0.0322(5) O13 0.048(2) 0.0382(18) 0.0369(18) -0.0033(14) -0.0114(15) -0.0142(15) O6 0.050(2) 0.050(2) 0.0356(18) -0.0078(16) -0.0058(15) -0.0173(17) O12 0.046(2) 0.051(2) 0.0334(18) -0.0045(15) -0.0059(15) -0.0120(17) O8 0.072(3) 0.041(2) 0.044(2) -0.0024(16) -0.0144(19) -0.0268(19) O7 0.062(2) 0.056(2) 0.038(2) -0.0067(17) -0.0102(18) -0.026(2) O5 0.044(2) 0.065(3) 0.046(2) -0.0078(19) -0.0065(17) -0.0108(19) O21 0.087(3) 0.052(2) 0.036(2) -0.0040(18) -0.014(2) -0.028(2) O1 0.052(2) 0.0358(19) 0.066(3) -0.0173(18) -0.0071(19) -0.0090(17) O11 0.058(3) 0.080(3) 0.045(2) -0.015(2) -0.0020(19) -0.033(2) O20 0.057(2) 0.041(2) 0.069(3) 0.003(2) -0.010(2) -0.0121(19) O2 0.080(3) 0.0294(19) 0.088(4) -0.009(2) -0.051(3) -0.0031(19) O4 0.068(3) 0.061(3) 0.060(3) -0.019(2) -0.011(2) 0.001(2) O18 0.098(4) 0.039(2) 0.081(3) -0.007(2) -0.038(3) -0.027(2) O10 0.058(3) 0.113(4) 0.046(2) -0.019(3) -0.008(2) -0.039(3) N1 0.054(3) 0.035(2) 0.039(2) -0.0085(18) -0.0117(19) -0.0107(19) N2 0.064(3) 0.035(2) 0.048(3) -0.0046(19) -0.027(2) -0.008(2) O16 0.125(5) 0.057(3) 0.076(3) -0.017(2) -0.049(4) -0.019(3) O3 0.078(3) 0.073(3) 0.076(4) 0.018(3) -0.022(3) -0.029(3) C24 0.049(2) 0.0364(19) 0.039(2) -0.0066(16) -0.0077(17) -0.0147(17) O17 0.086(4) 0.078(4) 0.101(4) 0.029(3) -0.036(3) -0.049(3) C23 0.052(2) 0.0380(19) 0.038(2) -0.0077(17) -0.0059(18) -0.0166(17) C26 0.048(2) 0.039(2) 0.038(2) -0.0053(17) -0.0080(17) -0.0119(17) C25 0.045(2) 0.039(2) 0.039(2) -0.0048(17) -0.0080(18) -0.0125(17) O19 0.156(6) 0.085(4) 0.061(3) -0.029(3) 0.025(4) -0.072(4) C1 0.058(3) 0.038(2) 0.056(3) -0.013(2) -0.014(2) -0.014(2) C3 0.057(3) 0.039(2) 0.061(3) -0.014(2) -0.020(2) -0.011(2) C14 0.067(3) 0.079(4) 0.043(3) -0.013(3) -0.005(3) -0.037(3) C8 0.053(3) 0.068(4) 0.054(3) -0.004(3) -0.016(3) -0.018(3) C2 0.059(3) 0.044(3) 0.084(4) -0.016(3) -0.017(3) -0.016(2) C11 0.067(4) 0.073(4) 0.065(4) -0.029(3) 0.003(3) -0.019(3) C4 0.064(3) 0.051(3) 0.089(4) -0.022(3) -0.029(3) -0.007(3) C15 0.074(4) 0.091(5) 0.050(3) -0.024(3) -0.005(3) -0.027(4) C16 0.068(3) 0.085(4) 0.054(3) -0.008(3) -0.001(3) -0.030(3) C9 0.062(4) 0.098(5) 0.066(4) 0.005(4) -0.018(3) -0.019(4) C38 0.169(8) 0.060(4) 0.062(4) 0.016(3) -0.034(5) -0.050(5) C17 0.070(4) 0.074(4) 0.064(4) -0.009(3) -0.004(3) -0.033(3) C13 0.084(4) 0.073(4) 0.069(4) -0.006(3) -0.013(4) -0.029(4) C5 0.108(5) 0.067(4) 0.070(4) -0.007(3) -0.005(4) -0.047(4) C30 0.096(5) 0.055(4) 0.115(6) -0.025(4) -0.011(4) -0.036(4) C39 0.085(5) 0.131(6) 0.087(5) -0.047(5) -0.001(4) -0.017(4) C35 0.085(5) 0.087(5) 0.101(6) 0.039(4) -0.044(4) -0.034(4) C19 0.092(4) 0.078(4) 0.067(4) -0.003(3) -0.010(3) -0.035(4) O15 0.053(5) 0.078(6) 0.042(4) -0.002(4) -0.005(4) -0.036(4) C18 0.084(4) 0.082(5) 0.070(4) -0.012(4) -0.006(4) -0.031(4) C33 0.112(6) 0.068(5) 0.103(6) 0.030(4) -0.050(5) -0.009(4) O14 0.050(5) 0.063(6) 0.050(5) -0.001(4) -0.007(4) 0.004(4) C36 0.213(8) 0.063(4) 0.057(4) 0.014(3) -0.060(5) -0.050(5) C32 0.090(5) 0.059(4) 0.120(6) -0.011(4) 0.000(5) -0.032(4) C34 0.082(5) 0.072(5) 0.136(6) 0.041(5) -0.036(5) -0.025(4) C6 0.114(4) 0.067(4) 0.074(4) -0.002(3) 0.004(4) -0.031(4) C31 0.102(5) 0.075(5) 0.135(6) -0.042(5) 0.007(5) -0.040(4) N3 0.028(4) 0.053(5) 0.044(5) 0.002(4) -0.005(3) -0.011(4) C7 0.127(6) 0.068(4) 0.085(5) 0.001(4) -0.009(5) -0.041(4) C10 0.078(4) 0.107(5) 0.086(5) -0.010(4) -0.007(4) -0.020(4) C20 0.095(5) 0.132(5) 0.085(5) -0.031(4) -0.019(4) -0.047(4) C37 0.208(8) 0.079(5) 0.074(5) 0.007(4) -0.069(5) -0.046(5) C12 0.106(5) 0.079(5) 0.117(6) -0.034(4) -0.029(5) -0.017(4) C21 0.133(5) 0.144(5) 0.105(5) -0.026(5) -0.023(5) -0.059(5) C28 0.128(5) 0.111(4) 0.085(4) -0.013(4) -0.004(4) -0.028(4) C27 0.149(5) 0.135(5) 0.071(3) -0.007(4) -0.017(4) -0.051(5) C29 0.155(6) 0.136(6) 0.089(5) -0.023(5) -0.028(5) -0.052(5) C22 0.110(5) 0.152(6) 0.108(5) -0.023(5) -0.033(5) -0.030(5) C40 0.127(7) 0.161(8) 0.137(7) -0.030(7) 0.002(6) -0.014(7) C41 0.135(6) 0.158(7) 0.120(6) -0.024(6) 0.005(5) -0.020(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2191 1.8069 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 O21 Ti3 O6 97.7(2) . . O21 Ti3 O8 95.3(2) . . O6 Ti3 O8 145.79(18) . . O21 Ti3 O13 167.5(2) . . O6 Ti3 O13 88.17(16) . . O8 Ti3 O13 85.66(17) . . O21 Ti3 O7 104.2(2) . . O6 Ti3 O7 74.32(17) . . O8 Ti3 O7 71.86(18) . . O13 Ti3 O7 88.02(16) . . O21 Ti3 N1 92.36(19) . . O6 Ti3 N1 73.34(17) . . O8 Ti3 N1 137.53(19) . . O13 Ti3 N1 78.75(16) . . O7 Ti3 N1 145.30(18) . . O21 Ti3 N2 86.9(2) . . O6 Ti3 N2 140.81(18) . . O8 Ti3 N2 71.21(18) . . O13 Ti3 N2 81.58(18) . . O7 Ti3 N2 142.22(18) . . N1 Ti3 N2 67.59(18) . . O21 Ti3 Ti4 99.78(15) . . O6 Ti3 Ti4 110.16(12) . . O8 Ti3 Ti4 36.15(13) . . O13 Ti3 Ti4 88.38(11) . . O7 Ti3 Ti4 35.84(13) . . N1 Ti3 Ti4 166.64(13) . . N2 Ti3 Ti4 107.26(13) . . O21 Ti3 Ti2 110.26(18) . . O6 Ti3 Ti2 38.14(12) . . O8 Ti3 Ti2 107.66(13) . . O13 Ti3 Ti2 81.13(11) . . O7 Ti3 Ti2 37.14(13) . . N1 Ti3 Ti2 108.55(13) . . N2 Ti3 Ti2 162.71(14) . . Ti4 Ti3 Ti2 72.51(4) . . O4 Ti1 O3 107.6(3) . . O4 Ti1 O6 110.5(2) . . O3 Ti1 O6 141.9(3) . . O4 Ti1 O1 101.6(2) . . O3 Ti1 O1 89.4(2) . . O6 Ti1 O1 81.46(17) . . O4 Ti1 O5 105.2(2) . . O3 Ti1 O5 94.6(2) . . O6 Ti1 O5 77.25(19) . . O1 Ti1 O5 150.24(18) . . O4 Ti1 Ti2 113.7(2) . . O3 Ti1 Ti2 124.0(2) . . O6 Ti1 Ti2 37.56(12) . . O1 Ti1 Ti2 116.22(12) . . O5 Ti1 Ti2 39.70(14) . . O19 Ti5 O20 111.3(3) . . O19 Ti5 O8 116.8(3) . . O20 Ti5 O8 132.0(2) . . O19 Ti5 O2 99.7(3) . . O20 Ti5 O2 92.5(2) . . O8 Ti5 O2 79.87(19) . . O19 Ti5 O18 100.7(3) . . O20 Ti5 O18 98.7(2) . . O8 Ti5 O18 72.9(2) . . O2 Ti5 O18 151.2(2) . . O19 Ti5 Ti4 110.0(3) . . O20 Ti5 Ti4 125.16(17) . . O8 Ti5 Ti4 34.36(12) . . O2 Ti5 Ti4 114.20(15) . . O18 Ti5 Ti4 38.88(15) . . O10 Ti2 O11 96.3(2) . . O10 Ti2 O7 105.8(2) . . O11 Ti2 O7 99.1(2) . . O10 Ti2 O6 167.7(2) . . O11 Ti2 O6 95.27(18) . . O7 Ti2 O6 76.43(17) . . O10 Ti2 O5 102.2(2) . . O11 Ti2 O5 93.8(2) . . O7 Ti2 O5 147.61(18) . . O6 Ti2 O5 72.86(17) . . O10 Ti2 O12 85.21(19) . . O11 Ti2 O12 175.8(2) . . O7 Ti2 O12 84.25(17) . . O6 Ti2 O12 82.94(16) . . O5 Ti2 O12 82.01(17) . . O10 Ti2 Ti3 141.8(2) . . O11 Ti2 Ti3 105.72(16) . . O7 Ti2 Ti3 40.85(12) . . O6 Ti2 Ti3 36.57(12) . . O5 Ti2 Ti3 106.99(13) . . O12 Ti2 Ti3 75.10(10) . . O10 Ti2 Ti1 138.9(2) . . O11 Ti2 Ti1 96.17(16) . . O7 Ti2 Ti1 110.68(13) . . O6 Ti2 Ti1 34.91(12) . . O5 Ti2 Ti1 37.96(12) . . O12 Ti2 Ti1 80.15(11) . . Ti3 Ti2 Ti1 69.89(3) . . O16 Ti4 O17 111.2(3) . . O16 Ti4 O7 103.6(2) . . O17 Ti4 O7 100.3(3) . . O16 Ti4 O8 121.6(3) . . O17 Ti4 O8 126.1(2) . . O7 Ti4 O8 78.08(19) . . O16 Ti4 O18 96.4(3) . . O17 Ti4 O18 93.4(3) . . O7 Ti4 O18 149.6(2) . . O8 Ti4 O18 71.92(19) . . O16 Ti4 Ti3 122.1(2) . . O17 Ti4 Ti3 117.9(2) . . O7 Ti4 Ti3 40.78(13) . . O8 Ti4 Ti3 37.44(13) . . O18 Ti4 Ti3 108.90(14) . . O16 Ti4 Ti5 110.4(3) . . O17 Ti4 Ti5 118.11(19) . . O7 Ti4 Ti5 111.97(14) . . O8 Ti4 Ti5 33.90(13) . . O18 Ti4 Ti5 38.38(14) . . Ti3 Ti4 Ti5 71.33(4) . . C23 O13 Ti3 127.8(4) . . Ti1 O6 Ti3 140.3(2) . . Ti1 O6 Ti2 107.52(19) . . Ti3 O6 Ti2 105.29(19) . . C23 O12 Ti2 129.6(4) . . Ti5 O8 Ti4 111.7(2) . . Ti5 O8 Ti3 141.8(2) . . Ti4 O8 Ti3 106.4(2) . . Ti4 O7 Ti2 151.9(2) . . Ti4 O7 Ti3 103.4(2) . . Ti2 O7 Ti3 102.01(19) . . C8 O5 Ti1 126.3(4) . . C8 O5 Ti2 131.3(4) . . Ti1 O5 Ti2 102.34(19) . . C36 O21 Ti3 151.8(7) . . N1 O1 Ti1 122.1(3) . . C14 O11 Ti2 133.9(4) . . C33 O20 Ti5 163.0(6) . . N2 O2 Ti5 122.7(4) . . C11 O4 Ti1 149.8(5) . . C30 O18 Ti5 134.2(6) . . C30 O18 Ti4 122.7(5) . . Ti5 O18 Ti4 102.7(2) . . C20 O10 Ti2 157.1(6) . . C1 N1 O1 114.8(5) . . C1 N1 Ti3 123.2(4) . . O1 N1 Ti3 121.6(3) . . C3 N2 O2 116.0(5) . . C3 N2 Ti3 122.2(4) . . O2 N2 Ti3 121.6(4) . . C27 O16 Ti4 155.9(8) . . C5 O3 Ti1 143.7(6) . . C25 C24 C26 118.6(5) . 2_666 C25 C24 C23 119.6(5) . . C26 C24 C23 121.8(5) 2_666 . C17 O17 Ti4 142.2(5) . . O12 C23 O13 126.2(5) . . O12 C23 C24 118.0(5) . . O13 C23 C24 115.8(5) . . N3 C26 C25 118.5(6) . . N3 C26 C24 120.2(6) . 2_666 C25 C26 C24 121.3(5) . 2_666 C26 C25 C24 120.1(5) . . C26 C25 H25 120.0 . . C24 C25 H25 120.0 . . C39 O19 Ti5 149.0(7) . . N1 C1 C3 113.4(5) . . N1 C1 C2 124.4(6) . . C3 C1 C2 122.2(6) . . N2 C3 C1 113.5(5) . . N2 C3 C4 123.5(6) . . C1 C3 C4 123.0(6) . . O11 C14 C15 108.9(6) . . O11 C14 C16 107.6(6) . . C15 C14 C16 113.0(7) . . O11 C14 H14 109.1 . . C15 C14 H14 109.1 . . C16 C14 H14 109.1 . . O5 C8 C9 109.7(6) . . O5 C8 C10 109.1(7) . . C9 C8 C10 115.3(7) . . O5 C8 H8 107.5 . . C9 C8 H8 107.5 . . C10 C8 H8 107.5 . . 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 . . O4 C11 C12 113.2(8) . . O4 C11 C13 109.7(6) . . C12 C11 C13 112.6(8) . . O4 C11 H11 107.0 . . C12 C11 H11 107.0 . . C13 C11 H11 107.0 . . C3 C4 H4A 109.5 . . C3 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . C3 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . C14 C15 H15A 109.5 . . C14 C15 H15B 109.5 . . H15A C15 H15B 109.5 . . C14 C15 H15C 109.5 . . H15A C15 H15C 109.5 . . H15B C15 H15C 109.5 . . C14 C16 H16A 109.5 . . C14 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . C14 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . C8 C9 H9A 109.5 . . C8 C9 H9B 109.5 . . H9A C9 H9B 109.5 . . C8 C9 H9C 109.5 . . H9A C9 H9C 109.5 . . H9B C9 H9C 109.5 . . C36 C38 H38A 109.5 . . C36 C38 H38B 109.5 . . H38A C38 H38B 109.5 . . C36 C38 H38C 109.5 . . H38A C38 H38C 109.5 . . H38B C38 H38C 109.5 . . O17 C17 C19 108.8(7) . . O17 C17 C18 109.0(7) . . C19 C17 C18 110.6(7) . . O17 C17 H17 109.5 . . C19 C17 H17 109.5 . . C18 C17 H17 109.5 . . C11 C13 H13A 109.5 . . C11 C13 H13B 109.5 . . H13A C13 H13B 109.5 . . C11 C13 H13C 109.5 . . H13A C13 H13C 109.5 . . H13B C13 H13C 109.5 . . O3 C5 C6 112.3(8) . . O3 C5 C7 109.2(8) . . C6 C5 C7 111.6(8) . . O3 C5 H5 107.9 . . C6 C5 H5 107.9 . . C7 C5 H5 107.9 . . O18 C30 C31 108.6(8) . . O18 C30 C32 110.0(7) . . C31 C30 C32 110.1(9) . . O18 C30 H30 109.4 . . C31 C30 H30 109.4 . . C32 C30 H30 109.4 . . C40 C39 O19 98.7(12) . . C40 C39 C41 100.9(12) . . O19 C39 C41 114.0(12) . . C40 C39 H39 113.9 . . O19 C39 H39 113.9 . . C41 C39 H39 113.9 . . C33 C35 H35A 109.5 . . C33 C35 H35B 109.5 . . H35A C35 H35B 109.5 . . C33 C35 H35C 109.5 . . H35A C35 H35C 109.5 . . H35B C35 H35C 109.5 . . C17 C19 H19A 109.5 . . C17 C19 H19B 109.5 . . H19A C19 H19B 109.5 . . C17 C19 H19C 109.5 . . H19A C19 H19C 109.5 . . H19B C19 H19C 109.5 . . C17 C18 H18A 109.5 . . C17 C18 H18B 109.5 . . H18A C18 H18B 109.5 . . C17 C18 H18C 109.5 . . H18A C18 H18C 109.5 . . H18B C18 H18C 109.5 . . O20 C33 C34 118.0(11) . . O20 C33 C35 111.9(8) . . C34 C33 C35 120.3(9) . . C37 C36 O21 113.9(7) . . C37 C36 C38 127.4(9) . . O21 C36 C38 115.2(7) . . C30 C32 H32A 109.5 . . C30 C32 H32B 109.5 . . H32A C32 H32B 109.5 . . C30 C32 H32C 109.5 . . H32A C32 H32C 109.5 . . H32B C32 H32C 109.5 . . C33 C34 H34A 109.5 . . C33 C34 H34B 109.5 . . H34A C34 H34B 109.5 . . C33 C34 H34C 109.5 . . H34A C34 H34C 109.5 . . H34B C34 H34C 109.5 . . C5 C6 H6A 109.5 . . C5 C6 H6B 109.5 . . H6A C6 H6B 109.5 . . C5 C6 H6C 109.5 . . H6A C6 H6C 109.5 . . H6B C6 H6C 109.5 . . C30 C31 H31A 109.5 . . C30 C31 H31B 109.5 . . H31A C31 H31B 109.5 . . C30 C31 H31C 109.5 . . H31A C31 H31C 109.5 . . H31B C31 H31C 109.5 . . O14 N3 O15 123.4(10) . . O14 N3 C26 118.1(9) . . O15 N3 C26 118.1(9) . . C5 C7 H7A 109.5 . . C5 C7 H7B 109.5 . . H7A C7 H7B 109.5 . . C5 C7 H7C 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . C8 C10 H10A 109.5 . . C8 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C8 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . O10 C20 C21 108.4(10) . . O10 C20 C22 107.6(10) . . C21 C20 C22 107.3(11) . . O10 C20 H20 111.1 . . C21 C20 H20 111.1 . . C22 C20 H20 111.1 . . C36 C37 H37A 109.5 . . C36 C37 H37B 109.5 . . H37A C37 H37B 109.5 . . C36 C37 H37C 109.5 . . H37A C37 H37C 109.5 . . H37B C37 H37C 109.5 . . C11 C12 H12A 109.5 . . C11 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C11 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . C20 C21 H21A 109.5 . . C20 C21 H21B 109.5 . . H21A C21 H21B 109.5 . . C20 C21 H21C 109.5 . . H21A C21 H21C 109.5 . . H21B C21 H21C 109.5 . . C27 C28 H28A 109.5 . . C27 C28 H28B 109.5 . . H28A C28 H28B 109.5 . . C27 C28 H28C 109.5 . . H28A C28 H28C 109.5 . . H28B C28 H28C 109.5 . . O16 C27 C28 94.3(10) . . O16 C27 C29 108.8(12) . . C28 C27 C29 113.9(13) . . C27 C29 H29A 109.5 . . C27 C29 H29B 109.5 . . H29A C29 H29B 109.5 . . C27 C29 H29C 109.5 . . H29A C29 H29C 109.5 . . H29B C29 H29C 109.5 . . C20 C22 H22A 109.5 . . C20 C22 H22B 109.5 . . H22A C22 H22B 109.5 . . C20 C22 H22C 109.5 . . H22A C22 H22C 109.5 . . H22B C22 H22C 109.5 . . C39 C40 H40A 109.5 . . C39 C40 H40B 109.5 . . H40A C40 H40B 109.5 . . C39 C40 H40C 109.5 . . H40A C40 H40C 109.5 . . H40B C40 H40C 109.5 . . C39 C41 H41A 109.5 . . C39 C41 H41B 109.5 . . H41A C41 H41B 109.5 . . C39 C41 H41C 109.5 . . H41A C41 H41C 109.5 . . H41B C41 H41C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ti3 O21 1.777(4) . Ti3 O6 1.938(4) . Ti3 O8 1.981(4) . Ti3 O13 2.081(4) . Ti3 O7 2.099(4) . Ti3 N1 2.250(5) . Ti3 N2 2.263(6) . Ti3 Ti4 3.1257(14) . Ti3 Ti2 3.1380(15) . Ti1 O4 1.785(5) . Ti1 O3 1.798(6) . Ti1 O6 1.886(4) . Ti1 O1 1.959(4) . Ti1 O5 1.979(4) . Ti1 Ti2 3.1429(16) . Ti5 O19 1.753(6) . Ti5 O20 1.779(5) . Ti5 O8 1.899(5) . Ti5 O2 1.954(4) . Ti5 O18 2.013(5) . Ti5 Ti4 3.1631(18) . Ti2 O10 1.809(5) . Ti2 O11 1.816(5) . Ti2 O7 1.937(5) . Ti2 O6 2.009(4) . Ti2 O5 2.055(5) . Ti2 O12 2.218(4) . Ti4 O16 1.778(6) . Ti4 O17 1.803(6) . Ti4 O7 1.881(5) . Ti4 O8 1.922(4) . Ti4 O18 2.036(6) . O13 C23 1.266(7) . O12 C23 1.255(7) . O5 C8 1.426(8) . O21 C36 1.401(9) . O1 N1 1.367(6) . O11 C14 1.430(8) . O20 C33 1.347(10) . O2 N2 1.355(6) . O4 C11 1.381(9) . O18 C30 1.456(8) . O10 C20 1.420(11) . N1 C1 1.282(8) . N2 C3 1.292(8) . O16 C27 1.394(13) . O3 C5 1.418(10) . C24 C25 1.394(8) . C24 C26 1.405(8) 2_666 C24 C23 1.496(8) . O17 C17 1.469(10) . C26 N3 1.419(10) . C26 C25 1.387(8) . C26 C24 1.405(8) 2_666 C25 H25 0.9300 . O19 C39 1.382(13) . C1 C3 1.485(8) . C1 C2 1.490(9) . C3 C4 1.488(10) . C14 C15 1.478(11) . C14 C16 1.499(11) . C14 H14 0.9800 . C8 C9 1.501(11) . C8 C10 1.555(13) . C8 H8 0.9800 . C2 H2A 0.9600 . C2 H2B 0.9600 . C2 H2C 0.9600 . C11 C12 1.435(13) . C11 C13 1.529(12) . C11 H11 0.9800 . C4 H4A 0.9600 . C4 H4B 0.9600 . C4 H4C 0.9600 . C15 H15A 0.9600 . C15 H15B 0.9600 . C15 H15C 0.9600 . C16 H16A 0.9600 . C16 H16B 0.9600 . C16 H16C 0.9600 . C9 H9A 0.9600 . C9 H9B 0.9600 . C9 H9C 0.9600 . C38 C36 1.426(12) . C38 H38A 0.9600 . C38 H38B 0.9600 . C38 H38C 0.9600 . C17 C19 1.528(11) . C17 C18 1.502(11) . C17 H17 0.9800 . C13 H13A 0.9600 . C13 H13B 0.9600 . C13 H13C 0.9600 . C5 C6 1.414(13) . C5 C7 1.506(13) . C5 H5 0.9800 . C30 C31 1.468(14) . C30 C32 1.555(15) . C30 H30 0.9800 . C39 C40 1.525(19) . C39 C41 1.402(18) . C39 H39 0.9800 . C35 C33 1.517(15) . C35 H35A 0.9600 . C35 H35B 0.9600 . C35 H35C 0.9600 . C19 H19A 0.9600 . C19 H19B 0.9600 . C19 H19C 0.9600 . O15 N3 1.224(14) . C18 H18A 0.9600 . C18 H18B 0.9600 . C18 H18C 0.9600 . C33 C34 1.414(14) . O14 N3 1.224(14) . C36 C37 1.446(8) . C32 H32A 0.9600 . C32 H32B 0.9600 . C32 H32C 0.9600 . C34 H34A 0.9600 . C34 H34B 0.9600 . C34 H34C 0.9600 . C6 H6A 0.9600 . C6 H6B 0.9600 . C6 H6C 0.9600 . C31 H31A 0.9600 . C31 H31B 0.9600 . C31 H31C 0.9600 . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 . C10 H10A 0.9600 . C10 H10B 0.9600 . C10 H10C 0.9600 . C20 C21 1.486(18) . C20 C22 1.555(17) . C20 H20 0.9800 . C37 H37A 0.9600 . C37 H37B 0.9600 . C37 H37C 0.9600 . C12 H12A 0.9600 . C12 H12B 0.9600 . C12 H12C 0.9600 . C21 H21A 0.9600 . C21 H21B 0.9600 . C21 H21C 0.9600 . C28 C27 1.514(19) . C28 H28A 0.9600 . C28 H28B 0.9600 . C28 H28C 0.9600 . C27 C29 1.491(19) . C29 H29A 0.9600 . C29 H29B 0.9600 . C29 H29C 0.9600 . C22 H22A 0.9600 . C22 H22B 0.9600 . C22 H22C 0.9600 . C40 H40A 0.9600 . C40 H40B 0.9600 . C40 H40C 0.9600 . C41 H41A 0.9600 . C41 H41B 0.9600 . C41 H41C 0.9600 .