#------------------------------------------------------------------------------ #$Date: 2021-01-15 04:47:57 +0200 (Fri, 15 Jan 2021) $ #$Revision: 260968 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/64/7706424.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_7706424 loop_ _publ_author_name 'Neto, Antonio de Brito Santiago' 'Alves da Cruz, Marcia Gabriely' 'Jeanneau, Erwann' 'Oliveira, Alcineia Concei\,c\~ao' 'Essayem, Nadine' 'Mishra, Shashank' _publ_section_title ; Designed sol-gel precursors for atomically dispersed Nb and Pb within TiO2 as catalysts for dihydroxyacetone transformation ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT03726E _journal_year 2021 _chemical_formula_moiety '2(C18 H42 N2 O8 Ti2), C2 H6 O' _chemical_formula_sum 'C38 H90 N4 O17 Ti4' _chemical_formula_weight 1066.62 _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary direct _audit_update_record ; 2017-06-27 deposited with the CCDC. 2021-01-14 downloaded from the CCDC. ; _cell_angle_alpha 78.159(3) _cell_angle_beta 80.220(3) _cell_angle_gamma 79.813(3) _cell_formula_units_Z 1 _cell_length_a 9.7305(3) _cell_length_b 10.3706(4) _cell_length_c 13.6626(5) _cell_measurement_reflns_used 8324 _cell_measurement_temperature 150.00(10) _cell_measurement_theta_max 29.0180 _cell_measurement_theta_min 4.0340 _cell_volume 1315.27(8) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) ; _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _diffrn_ambient_temperature 150.00(10) _diffrn_detector_area_resol_mean 10.4678 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.879 _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_reflns_av_R_equivalents 0.034 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 27521 _diffrn_reflns_theta_full 26.620 _diffrn_reflns_theta_max 29.828 _diffrn_reflns_theta_min 3.164 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.651 _exptl_absorpt_correction_T_max 0.905 _exptl_absorpt_correction_T_min 0.750 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 570 _exptl_crystal_size_max 0.558 _exptl_crystal_size_mid 0.318 _exptl_crystal_size_min 0.190 _refine_diff_density_max 1.96 _refine_diff_density_min -0.69 _refine_ls_extinction_method None _refine_ls_goodness_of_fit_ref 1.0280 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 293 _refine_ls_number_reflns 6645 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0586 _refine_ls_shift/su_max 0.0004664 _refine_ls_shift/su_mean 0.0000208 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; Method= Modified Sheldrick w=1/[\s^2^(F^2^) + ( 0.06P)^2^ + 3.40P] ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all 0.1635 _refine_ls_wR_factor_gt 0.1397 _refine_ls_wR_factor_ref 0.1635 _reflns_limit_h_max 13 _reflns_limit_h_min -13 _reflns_limit_k_max 14 _reflns_limit_k_min -13 _reflns_limit_l_max 18 _reflns_limit_l_min 0 _reflns_number_gt 5197 _reflns_number_total 6645 _reflns_threshold_expression I>2.0\s(I) _oxford_diffrn_Wilson_B_factor 2.11 _oxford_diffrn_Wilson_scale 0.07 _oxford_refine_ls_r_factor_ref 0.0781 _oxford_refine_ls_scale 4.60(9) _oxford_reflns_number_all 6645 _oxford_reflns_threshold_expression_ref I>-10.0\s(I) _iucr_refine_instructions_details ; # # Punched on 27/06/17 at 10:36:41 # #LIST 12 BLOCK CONT SCALE CONT TI ( 1 ,X'S,U'S) UNTIL O ( 10 ) CONT C ( 11 ,X'S,U'S) CONT O ( 12 ,X'S,U'S) UNTIL O ( 18 ) CONT C ( 19 ,X'S,U'S) CONT O ( 20 ,X'S,U'S) UNTIL C ( 22 ) CONT C ( 23 ,X'S,U'S) UNTIL C ( 24 ) CONT O ( 25 ,X'S,U'S) UNTIL C ( 27 ) CONT O ( 28 ,X'S,U'S) UNTIL C ( 30 ) CONT O ( 31 ,X'S,U'S) UNTIL C ( 32 ) CONT H ( 312 ,X'S,U[ISO]) END # # Punched on 27/06/17 at 10:36:41 # #LIST 16 NO DISTANCE 1.350000 , 0.0010000 = C(32) TO O(31) U(IJ)'S 0.0, 0.010000 = C(32) TO O(31) REM HREST START (DO NOT REMOVE THIS LINE) REM NO H NO #H U MULT DIST REM C-H REM >4 1.5 .96 DISORDER REM 1 1 1.2 .93 C C-H (ACETYLENE) REM 1 2 1.2 .93 C-C(H)-C REM 1 3 1.2 .98 (C)3-C-H REM 2 1 1.2 .93 C=C-H(2) REM 2 2 1.2 .97 (C)2-C-(H)2 REM 3 1 1.5 .96 C-C-(H)3 REM N-H REM >4 1.5 .89 DISORDER REM 1 1 1.2 .86 N-N/H REM 1 2 1.2 .86 (C)2-N-H REM 1 3 1.2 .89 (C)3-N-H REM 2 1 1.2 .86 C-N-(H)2 REM 2 2 1.2 .89 (C)2-N-(H)2 REM 3 1 1.2 .89 C-H-(H)3 REM O-H REM 1 1 1.5 .82 O-H REM REM DIST ESD = 0.02 REM VIB ESD = 0.002 REM ANGLE ESD = 2.0 REM REM TO ACTIVATE THE VIB RESTRAINTS, REMOVE LEADING REM REM H ON O-HETRO ATOM DIST 0.82, 0.02 = CONT O ( 31) TO H(312) REST 0.097, 0.002 = H(312,U[ISO]) REM HREST END (DO NOT REMOVE THIS LINE) DISTANCE 1.5500000 , 0.010000 = C(32) TO C(32,-1,1,1,1) END ; _cod_data_source_file d0dt03726e2.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P -1 ' _cod_database_code 7706424 loop_ _symmetry_equiv_pos_as_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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Ti1 Ti 0.23143(5) 0.72760(5) 0.27271(4) 0.0249 1.0000 Uani . . . . . . O2 O 0.0239(2) 0.7299(2) 0.33537(16) 0.0281 1.0000 Uani . . . . . . Ti3 Ti -0.10129(5) 0.78059(5) 0.22572(4) 0.0279 1.0000 Uani . . . . . . O4 O 0.1058(2) 0.7516(2) 0.16156(15) 0.0253 1.0000 Uani . . . . . . C5 C 0.1557(3) 0.8286(3) 0.0676(2) 0.0339 1.0000 Uani . . . . . . C6 C 0.1751(4) 0.9627(3) 0.0875(3) 0.0368 1.0000 Uani . . . . . . N7 N 0.2402(3) 0.9475(3) 0.1811(2) 0.0327 1.0000 Uani . . . . . . C8 C 0.3939(4) 0.9483(4) 0.1600(3) 0.0406 1.0000 Uani . . . . . . C9 C 0.4632(3) 0.8225(4) 0.1220(3) 0.0421 1.0000 Uani . . . . . . O10 O 0.3998(2) 0.7142(2) 0.17961(18) 0.0351 1.0000 Uani . . . . . . H92 H 0.5611 0.8084 0.1257 0.0501 1.0000 Uiso . . . . . . H91 H 0.4518 0.8308 0.0518 0.0496 1.0000 Uiso . . . . . . H81 H 0.4274 0.9532 0.2222 0.0489 1.0000 Uiso . . . . . . H82 H 0.4138 1.0247 0.1095 0.0489 1.0000 Uiso . . . . . . C11 C 0.1735(4) 1.0564(4) 0.2369(3) 0.0457 1.0000 Uani . . . . . . H112 H 0.2192 1.0503 0.2942 0.0681 1.0000 Uiso . . . . . . H111 H 0.1811 1.1398 0.1934 0.0675 1.0000 Uiso . . . . . . H113 H 0.0778 1.0446 0.2585 0.0666 1.0000 Uiso . . . . . . H62 H 0.2339 1.0049 0.0314 0.0439 1.0000 Uiso . . . . . . H61 H 0.0829 1.0157 0.0957 0.0439 1.0000 Uiso . . . . . . H52 H 0.2460 0.7849 0.0390 0.0406 1.0000 Uiso . . . . . . H51 H 0.0892 0.8420 0.0204 0.0412 1.0000 Uiso . . . . . . O12 O -0.2617(2) 0.7477(2) 0.3170(2) 0.0375 1.0000 Uani . . . . . . C13 C -0.3192(4) 0.6285(4) 0.3424(3) 0.0410 1.0000 Uani . . . . . . C14 C -0.2043(4) 0.5151(4) 0.3221(3) 0.0422 1.0000 Uani . . . . . . N15 N -0.1138(3) 0.5564(3) 0.2261(2) 0.0288 1.0000 Uani . . . . . . C16 C -0.1846(4) 0.5599(4) 0.1374(3) 0.0412 1.0000 Uani . . . . . . C17 C -0.1363(4) 0.6710(4) 0.0553(3) 0.0453 1.0000 Uani . . . . . . O18 O -0.1542(3) 0.7855(2) 0.09876(19) 0.0388 1.0000 Uani . . . . . . H171 H -0.0352 0.6474 0.0303 0.0536 1.0000 Uiso . . . . . . H172 H -0.1909 0.6861 0.0009 0.0541 1.0000 Uiso . . . . . . H162 H -0.2871 0.5778 0.1567 0.0504 1.0000 Uiso . . . . . . H161 H -0.1578 0.4735 0.1150 0.0498 1.0000 Uiso . . . . . . C19 C 0.0211(4) 0.4658(4) 0.2222(4) 0.0534 1.0000 Uani . . . . . . H193 H 0.0867 0.4974 0.1617 0.0792 1.0000 Uiso . . . . . . H192 H 0.0630 0.4635 0.2808 0.0786 1.0000 Uiso . . . . . . H191 H 0.0062 0.3759 0.2221 0.0782 1.0000 Uiso . . . . . . H142 H -0.1458 0.4911 0.3761 0.0511 1.0000 Uiso . . . . . . H141 H -0.2463 0.4369 0.3180 0.0508 1.0000 Uiso . . . . . . H131 H -0.3546 0.6122 0.4149 0.0493 1.0000 Uiso . . . . . . H132 H -0.3951 0.6335 0.3041 0.0494 1.0000 Uiso . . . . . . O20 O -0.1400(2) 0.9594(2) 0.2188(2) 0.0420 1.0000 Uani . . . . . . C21 C -0.2657(4) 1.0515(4) 0.2163(3) 0.0444 1.0000 Uani . . . . . . C22 C -0.2366(5) 1.1855(4) 0.2229(4) 0.0573 1.0000 Uani . . . . . . H222 H -0.3241 1.2443 0.2231 0.0877 1.0000 Uiso . . . . . . H221 H -0.1968 1.1769 0.2858 0.0875 1.0000 Uiso . . . . . . H223 H -0.1711 1.2155 0.1659 0.0878 1.0000 Uiso . . . . . . H212 H -0.3298 1.0228 0.2760 0.0540 1.0000 Uiso . . . . . . H211 H -0.3077 1.0585 0.1547 0.0542 1.0000 Uiso . . . . . . C23 C -0.0188(4) 0.7132(4) 0.4419(3) 0.0385 1.0000 Uani . . . . . . C24 C -0.0634(5) 0.8460(5) 0.4754(4) 0.0607 1.0000 Uani . . . . . . H243 H -0.0865 0.8299 0.5478 0.0916 1.0000 Uiso . . . . . . H242 H -0.1452 0.8903 0.4468 0.0916 1.0000 Uiso . . . . . . H241 H 0.0097 0.8975 0.4543 0.0918 1.0000 Uiso . . . . . . H232 H 0.0595 0.6652 0.4750 0.0470 1.0000 Uiso . . . . . . H231 H -0.0970 0.6637 0.4605 0.0467 1.0000 Uiso . . . . . . O25 O 0.2747(3) 0.8022(2) 0.37082(17) 0.0355 1.0000 Uani . . . . . . C26 C 0.3232(4) 0.7699(4) 0.4655(3) 0.0461 1.0000 Uani . . . . . . C27 C 0.4197(4) 0.8661(5) 0.4726(3) 0.0548 1.0000 Uani . . . . . . H271 H 0.4477 0.8454 0.5390 0.0820 1.0000 Uiso . . . . . . H273 H 0.3718 0.9546 0.4603 0.0817 1.0000 Uiso . . . . . . H272 H 0.5011 0.8543 0.4234 0.0813 1.0000 Uiso . . . . . . H261 H 0.2443 0.7783 0.5182 0.0559 1.0000 Uiso . . . . . . H262 H 0.3719 0.6788 0.4767 0.0560 1.0000 Uiso . . . . . . O28 O 0.2722(2) 0.5513(2) 0.32372(18) 0.0336 1.0000 Uani . . . . . . C29 C 0.3900(4) 0.4503(3) 0.3226(3) 0.0376 1.0000 Uani . . . . . . C30 C 0.3488(4) 0.3200(4) 0.3131(4) 0.0578 1.0000 Uani . . . . . . H302 H 0.4320 0.2530 0.3144 0.0877 1.0000 Uiso . . . . . . H301 H 0.2777 0.2937 0.3700 0.0882 1.0000 Uiso . . . . . . H303 H 0.3115 0.3307 0.2503 0.0881 1.0000 Uiso . . . . . . H292 H 0.4259 0.4359 0.3873 0.0448 1.0000 Uiso . . . . . . H291 H 0.4607 0.4755 0.2674 0.0447 1.0000 Uiso . . . . . . O31 O 0.3388(6) 0.5246(7) 0.0615(6) 0.0648 0.5000 Uani D U . . . . C32 C 0.4601(6) 0.4479(5) 0.0330(4) 0.0924 1.0000 Uani D U . . . . H325 H 0.3738 0.4811 0.0618 0.1123 0.5000 Uiso . . . . . . H324 H 0.5155 0.4031 0.0921 0.1129 0.5000 Uiso . . . . . . H323 H 0.5195 0.4041 0.0861 0.1123 0.5000 Uiso . . . . . . H322 H 0.4444 0.3811 -0.0038 0.1128 0.5000 Uiso . . . . . . H321 H 0.4564 0.3810 -0.0048 0.1123 0.5000 Uiso . . . . . . H312 H 0.377(12) 0.560(12) 0.095(8) 0.097(2) 0.5000 Uiso D . . . . . 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 Ti1 0.0228(3) 0.0246(3) 0.0270(3) -0.00258(19) -0.00251(19) -0.00598(19) O2 0.0252(10) 0.0311(11) 0.0281(11) -0.0061(8) 0.0013(8) -0.0078(8) Ti3 0.0212(3) 0.0212(3) 0.0397(3) -0.0034(2) -0.0029(2) -0.00285(19) O4 0.0228(10) 0.0281(10) 0.0238(10) -0.0018(8) -0.0021(8) -0.0050(8) C5 0.0321(16) 0.0411(18) 0.0260(15) 0.0020(13) -0.0039(12) -0.0081(13) C6 0.0332(17) 0.0312(16) 0.0382(18) 0.0076(13) -0.0021(13) -0.0030(13) N7 0.0305(13) 0.0258(13) 0.0401(15) -0.0008(11) -0.0008(11) -0.0090(10) C8 0.0328(17) 0.0376(18) 0.049(2) 0.0050(15) -0.0028(15) -0.0172(14) C9 0.0243(15) 0.044(2) 0.048(2) 0.0073(16) 0.0043(14) -0.0074(14) O10 0.0247(11) 0.0343(12) 0.0390(13) 0.0032(10) 0.0021(9) -0.0026(9) C11 0.046(2) 0.0280(17) 0.063(2) -0.0135(16) 0.0001(18) -0.0063(15) O12 0.0243(11) 0.0334(12) 0.0544(15) -0.0110(11) 0.0046(10) -0.0090(9) C13 0.0354(18) 0.0392(19) 0.049(2) -0.0067(15) 0.0037(15) -0.0167(15) C14 0.049(2) 0.0330(17) 0.046(2) 0.0021(15) -0.0123(16) -0.0158(15) N15 0.0244(12) 0.0258(12) 0.0373(14) -0.0057(10) -0.0083(10) -0.0034(10) C16 0.045(2) 0.0368(18) 0.046(2) -0.0079(15) -0.0116(16) -0.0114(15) C17 0.048(2) 0.053(2) 0.0383(19) -0.0053(16) -0.0116(16) -0.0137(17) O18 0.0338(12) 0.0351(12) 0.0462(14) 0.0049(10) -0.0153(10) -0.0067(10) C19 0.039(2) 0.0289(18) 0.097(3) -0.0174(19) -0.021(2) 0.0015(15) O20 0.0288(12) 0.0215(11) 0.0710(18) -0.0064(11) 0.0003(11) -0.0005(9) C21 0.0312(17) 0.0340(18) 0.064(2) -0.0085(16) -0.0014(16) -0.0009(14) C22 0.051(2) 0.034(2) 0.082(3) -0.016(2) 0.001(2) 0.0040(17) C23 0.0364(18) 0.049(2) 0.0323(17) -0.0100(14) 0.0065(13) -0.0198(15) C24 0.066(3) 0.065(3) 0.057(3) -0.036(2) 0.023(2) -0.028(2) O25 0.0385(13) 0.0411(13) 0.0313(12) -0.0061(10) -0.0049(9) -0.0178(10) C26 0.045(2) 0.065(3) 0.0321(18) -0.0064(17) -0.0071(15) -0.0206(18) C27 0.045(2) 0.074(3) 0.058(3) -0.030(2) -0.0129(19) -0.018(2) O28 0.0287(11) 0.0273(11) 0.0412(13) 0.0019(9) -0.0067(9) -0.0024(9) C29 0.0302(16) 0.0310(16) 0.049(2) 0.0008(14) -0.0100(14) -0.0023(13) C30 0.038(2) 0.0310(19) 0.099(4) -0.006(2) -0.004(2) -0.0033(15) O31 0.058(4) 0.072(4) 0.077(4) -0.030(3) -0.015(3) -0.018(3) C32 0.109(5) 0.087(4) 0.094(4) -0.031(3) -0.031(4) -0.013(3) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Ti 0.2776 0.4457 9.7595 7.8508 7.3558 0.5000 1.6991 35.6338 1.9021 116.1050 1.2807 'International Tables Vol C 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O2 . Ti1 . O4 . 69.78(8) yes O2 . Ti1 . N7 . 103.84(9) yes O4 . Ti1 . N7 . 74.07(9) yes O2 . Ti1 . O10 . 161.66(10) yes O4 . Ti1 . O10 . 92.69(9) yes N7 . Ti1 . O10 . 75.25(10) yes O2 . Ti1 . O25 . 93.29(10) yes O4 . Ti1 . O25 . 145.06(10) yes N7 . Ti1 . O25 . 81.18(10) yes O10 . Ti1 . O25 . 104.55(11) yes O2 . Ti1 . O28 . 91.42(9) yes O4 . Ti1 . O28 . 109.18(10) yes N7 . Ti1 . O28 . 164.42(10) yes O10 . Ti1 . O28 . 89.29(10) yes O25 . Ti1 . O28 . 101.32(11) yes Ti1 . O2 . Ti3 . 110.02(10) yes Ti1 . O2 . C23 . 122.12(19) yes Ti3 . O2 . C23 . 127.4(2) yes O2 . Ti3 . O4 . 70.53(8) yes O2 . Ti3 . O12 . 92.46(10) yes O4 . Ti3 . O12 . 157.65(10) yes O2 . Ti3 . N15 . 91.85(9) yes O4 . Ti3 . N15 . 89.24(9) yes O12 . Ti3 . N15 . 76.56(10) yes O2 . Ti3 . O18 . 156.53(10) yes O4 . Ti3 . O18 . 88.61(10) yes O12 . Ti3 . O18 . 104.47(11) yes N15 . Ti3 . O18 . 76.79(10) yes O2 . Ti3 . O20 . 100.65(11) yes O4 . Ti3 . O20 . 103.31(10) yes O12 . Ti3 . O20 . 93.82(11) yes N15 . Ti3 . O20 . 164.61(10) yes O18 . Ti3 . O20 . 94.41(12) yes Ti1 . O4 . Ti3 . 108.53(9) yes Ti1 . O4 . C5 . 114.88(18) yes Ti3 . O4 . C5 . 121.95(18) yes O4 . C5 . C6 . 107.7(3) yes O4 . C5 . H52 . 110.5 no C6 . C5 . H52 . 108.8 no O4 . C5 . H51 . 111.0 no C6 . C5 . H51 . 109.4 no H52 . C5 . H51 . 109.3 no C5 . C6 . N7 . 111.4(2) yes C5 . C6 . H62 . 109.1 no N7 . C6 . H62 . 109.4 no C5 . C6 . H61 . 107.8 no N7 . C6 . H61 . 108.9 no H62 . C6 . H61 . 110.4 no Ti1 . N7 . C6 . 108.64(19) yes Ti1 . N7 . C8 . 100.69(19) yes C6 . N7 . C8 . 112.6(3) yes Ti1 . N7 . C11 . 115.8(2) yes C6 . N7 . C11 . 109.7(3) yes C8 . N7 . C11 . 109.3(3) yes N7 . C8 . C9 . 108.7(3) yes N7 . C8 . H81 . 108.5 no C9 . C8 . H81 . 110.8 no N7 . C8 . H82 . 109.4 no C9 . C8 . H82 . 109.8 no H81 . C8 . H82 . 109.6 no C8 . C9 . O10 . 109.3(3) yes C8 . C9 . H92 . 110.3 no O10 . C9 . H92 . 110.7 no C8 . C9 . H91 . 109.7 no O10 . C9 . H91 . 109.3 no H92 . C9 . H91 . 107.5 no C9 . O10 . Ti1 . 125.3(2) yes N7 . C11 . H112 . 109.7 no N7 . C11 . H111 . 109.2 no H112 . C11 . H111 . 109.9 no N7 . C11 . H113 . 107.1 no H112 . C11 . H113 . 109.4 no H111 . C11 . H113 . 111.4 no Ti3 . O12 . C13 . 126.5(2) yes O12 . C13 . C14 . 108.9(3) yes O12 . C13 . H131 . 109.5 no C14 . C13 . H131 . 107.6 no O12 . C13 . H132 . 110.2 no C14 . C13 . H132 . 110.9 no H131 . C13 . H132 . 109.6 no C13 . C14 . N15 . 109.6(3) yes C13 . C14 . H142 . 110.1 no N15 . C14 . H142 . 108.3 no C13 . C14 . H141 . 109.9 no N15 . C14 . H141 . 109.9 no H142 . C14 . H141 . 109.0 no Ti3 . N15 . C14 . 103.8(2) yes Ti3 . N15 . C16 . 104.61(19) yes C14 . N15 . C16 . 111.6(3) yes Ti3 . N15 . C19 . 116.3(2) yes C14 . N15 . C19 . 109.4(3) yes C16 . N15 . C19 . 110.9(3) yes N15 . C16 . C17 . 107.6(3) yes N15 . C16 . H162 . 109.0 no C17 . C16 . H162 . 110.0 no N15 . C16 . H161 . 108.9 no C17 . C16 . H161 . 110.8 no H162 . C16 . H161 . 110.5 no C16 . C17 . O18 . 107.3(3) yes C16 . C17 . H171 . 109.7 no O18 . C17 . H171 . 109.1 no C16 . C17 . H172 . 110.2 no O18 . C17 . H172 . 110.6 no H171 . C17 . H172 . 110.0 no C17 . O18 . Ti3 . 122.2(2) yes N15 . C19 . H193 . 110.5 no N15 . C19 . H192 . 109.2 no H193 . C19 . H192 . 108.6 no N15 . C19 . H191 . 110.7 no H193 . C19 . H191 . 110.2 no H192 . C19 . H191 . 107.5 no Ti3 . O20 . C21 . 133.5(2) yes O20 . C21 . C22 . 109.8(3) yes O20 . C21 . H212 . 107.3 no C22 . C21 . H212 . 107.3 no O20 . C21 . H211 . 112.3 no C22 . C21 . H211 . 108.9 no H212 . C21 . H211 . 111.2 no C21 . C22 . H222 . 107.4 no C21 . C22 . H221 . 107.7 no H222 . C22 . H221 . 111.4 no C21 . C22 . H223 . 109.3 no H222 . C22 . H223 . 110.4 no H221 . C22 . H223 . 110.4 no O2 . C23 . C24 . 111.1(3) yes O2 . C23 . H232 . 108.4 no C24 . C23 . H232 . 109.3 no O2 . C23 . H231 . 109.9 no C24 . C23 . H231 . 108.6 no H232 . C23 . H231 . 109.6 no C23 . C24 . H243 . 108.1 no C23 . C24 . H242 . 109.2 no H243 . C24 . H242 . 108.7 no C23 . C24 . H241 . 109.6 no H243 . C24 . H241 . 111.2 no H242 . C24 . H241 . 110.1 no Ti1 . O25 . C26 . 142.3(2) yes O25 . C26 . C27 . 110.2(3) yes O25 . C26 . H261 . 109.6 no C27 . C26 . H261 . 107.4 no O25 . C26 . H262 . 110.8 no C27 . C26 . H262 . 110.3 no H261 . C26 . H262 . 108.5 no C26 . C27 . H271 . 108.9 no C26 . C27 . H273 . 109.6 no H271 . C27 . H273 . 110.3 no C26 . C27 . H272 . 107.8 no H271 . C27 . H272 . 109.4 no H273 . C27 . H272 . 110.8 no Ti1 . O28 . C29 . 138.1(2) yes O28 . C29 . C30 . 111.1(3) yes O28 . C29 . H292 . 108.2 no C30 . C29 . H292 . 107.1 no O28 . C29 . H291 . 110.1 no C30 . C29 . H291 . 109.3 no H292 . C29 . H291 . 111.1 no C29 . C30 . H302 . 108.5 no C29 . C30 . H301 . 109.1 no H302 . C30 . H301 . 109.6 no C29 . C30 . H303 . 109.5 no H302 . C30 . H303 . 110.1 no H301 . C30 . H303 . 110.1 no C32 . O31 . H312 . 92(9) no C32 2_665 C32 . O31 . 100.0(6) yes C32 2_665 C32 . H325 . 113.6 no C32 2_665 C32 . H324 . 108.2 no O31 . C32 . H324 . 113.3 no H325 . C32 . H324 . 105.7 no C32 2_665 C32 . H323 . 105.5 no O31 . C32 . H323 . 117.2 no H325 . C32 . H323 . 109.8 no C32 2_665 C32 . H322 . 112.7 no O31 . C32 . H322 . 111.8 no H325 . C32 . H322 . 106.0 no H324 . C32 . H322 . 110.4 no H323 . C32 . H322 . 109.3 no C32 2_665 C32 . H321 . 109.0 no O31 . C32 . H321 . 118.3 no H325 . C32 . H321 . 112.6 no H324 . C32 . H321 . 107.4 no H323 . C32 . H321 . 105.9 no loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 . O2 . 2.053(2) yes Ti1 . O4 . 2.057(2) yes Ti1 . N7 . 2.374(3) yes Ti1 . O10 . 1.899(2) yes Ti1 . O25 . 1.818(2) yes Ti1 . O28 . 1.817(2) yes O2 . Ti3 . 2.018(2) yes O2 . C23 . 1.427(4) yes Ti3 . O4 . 2.053(2) yes Ti3 . O12 . 1.860(2) yes Ti3 . N15 . 2.349(3) yes Ti3 . O18 . 1.880(3) yes Ti3 . O20 . 1.812(2) yes O4 . C5 . 1.423(4) yes C5 . C6 . 1.519(5) yes C5 . H52 . 0.972 no C5 . H51 . 0.964 no C6 . N7 . 1.489(5) yes C6 . H62 . 0.953 no C6 . H61 . 0.967 no N7 . C8 . 1.476(4) yes N7 . C11 . 1.485(5) yes C8 . C9 . 1.508(5) yes C8 . H81 . 0.974 no C8 . H82 . 0.962 no C9 . O10 . 1.406(4) yes C9 . H92 . 0.946 no C9 . H91 . 0.970 no C11 . H112 . 0.950 no C11 . H111 . 0.951 no C11 . H113 . 0.949 no O12 . C13 . 1.402(4) yes C13 . C14 . 1.508(5) yes C13 . H131 . 0.982 no C13 . H132 . 0.963 no C14 . N15 . 1.480(5) yes C14 . H142 . 0.974 no C14 . H141 . 0.985 no N15 . C16 . 1.484(4) yes N15 . C19 . 1.472(4) yes C16 . C17 . 1.513(5) yes C16 . H162 . 0.982 no C16 . H161 . 0.983 no C17 . O18 . 1.405(5) yes C17 . H171 . 0.991 no C17 . H172 . 0.956 no C19 . H193 . 0.991 no C19 . H192 . 0.953 no C19 . H191 . 0.969 no O20 . C21 . 1.413(4) yes C21 . C22 . 1.490(6) yes C21 . H212 . 0.967 no C21 . H211 . 0.981 no C22 . H222 . 0.956 no C22 . H221 . 0.983 no C22 . H223 . 0.955 no C23 . C24 . 1.508(6) yes C23 . H232 . 0.962 no C23 . H231 . 0.962 no C24 . H243 . 0.964 no C24 . H242 . 0.948 no C24 . H241 . 0.936 no O25 . C26 . 1.408(4) yes C26 . C27 . 1.513(6) yes C26 . H261 . 0.965 no C26 . H262 . 0.973 no C27 . H271 . 0.963 no C27 . H273 . 0.948 no C27 . H272 . 0.955 no O28 . C29 . 1.409(4) yes C29 . C30 . 1.510(5) yes C29 . H292 . 0.979 no C29 . H291 . 0.958 no C30 . H302 . 0.969 no C30 . H301 . 0.977 no C30 . H303 . 0.966 no O31 . C32 . 1.3484(10) yes O31 . H312 . 0.81(2) no C32 . C32 2_665 1.498(8) yes C32 . H325 . 0.905 no C32 . H324 . 1.031 no C32 . H323 . 0.990 no C32 . H322 . 0.980 no C32 . H321 . 0.954 no loop_ _geom_hbond_atom_site_label_D _geom_hbond_site_symmetry_D _geom_hbond_atom_site_label_H _geom_hbond_site_symmetry_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_angle_DHA _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_publ_flag C6 . H61 . O20 . 129 0.97 2.58 3.281(6) yes C19 . H192 . O28 . 137 0.95 2.57 3.332(6) yes O31 . H312 . O10 . 156(12) 0.809 2.218 2.977(6) yes