# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L6Ti(O2Ar1) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H68 Cl4 N4 O8 Ti2' _chemical_formula_weight 1186.76 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' O O 0.0106 0.0060 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 12.2350(4) _cell_length_b 17.2330(8) _cell_length_c 13.4000(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.642(2) _cell_angle_gamma 90.00 _cell_volume 2806.37(19) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30575 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 26.73 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.533 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48977 _diffrn_reflns_av_R_equivalents 0.1302 _diffrn_reflns_av_sigmaI/netI 0.0723 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 26.76 _reflns_number_total 5929 _reflns_number_gt 3841 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0887P)^2^+5.3837P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5929 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1199 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.2017 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.54140(6) 0.14340(4) 0.77179(5) 0.0230(2) Uani 1 1 d . . . Cl1 Cl 0.3690(2) -0.25050(15) 0.7971(2) 0.1204(9) Uani 1 1 d . . . O1 O 0.6177(2) 0.04607(16) 0.7604(2) 0.0276(6) Uani 1 1 d . . . N1 N 0.4027(3) 0.08771(19) 0.8359(2) 0.0252(7) Uani 1 1 d . . . C1 C 0.6928(3) 0.0256(2) 0.8384(3) 0.0285(9) Uani 1 1 d . . . Cl2 Cl 0.5999(2) -0.24821(15) 0.77091(18) 0.1108(8) Uani 1 1 d . . . O2 O 0.6475(2) 0.14623(16) 0.8946(2) 0.0273(6) Uani 1 1 d . . . N2 N 0.4515(3) 0.2220(2) 0.8665(2) 0.0254(7) Uani 1 1 d . . . C2 C 0.7095(3) 0.0828(3) 0.9142(3) 0.0287(9) Uani 1 1 d . . . O3 O 0.4528(2) 0.11580(16) 0.6546(2) 0.0259(6) Uani 1 1 d . . . C3 C 0.7857(3) 0.0705(3) 0.9981(3) 0.0333(10) Uani 1 1 d . . . H3 H 0.7979 0.1087 1.0493 0.040 Uiso 1 1 calc R . . O4 O 0.5944(2) 0.23333(16) 0.7184(2) 0.0265(6) Uani 1 1 d . . . C4 C 0.8439(4) 0.0002(3) 1.0053(4) 0.0401(12) Uani 1 1 d . . . H4 H 0.8966 -0.0088 1.0619 0.048 Uiso 1 1 calc R . . C5 C 0.8263(4) -0.0562(3) 0.9320(4) 0.0406(12) Uani 1 1 d . . . H5 H 0.8663 -0.1035 0.9392 0.049 Uiso 1 1 calc R . . C6 C 0.7499(4) -0.0442(3) 0.8470(3) 0.0341(10) Uani 1 1 d . . . H6 H 0.7376 -0.0829 0.7964 0.041 Uiso 1 1 calc R . . C7 C 0.3945(3) 0.0517(2) 0.6223(3) 0.0261(8) Uani 1 1 d . . . C8 C 0.3678(3) 0.0410(3) 0.5188(3) 0.0307(9) Uani 1 1 d . . . C9 C 0.3060(4) -0.0240(3) 0.4851(3) 0.0349(10) Uani 1 1 d . . . H9 H 0.2896 -0.0321 0.4148 0.042 Uiso 1 1 calc R . . C10 C 0.2678(3) -0.0772(3) 0.5506(4) 0.0344(10) Uani 1 1 d . . . C11 C 0.2942(3) -0.0647(3) 0.6529(3) 0.0321(9) Uani 1 1 d . . . H11 H 0.2676 -0.1001 0.6987 0.039 Uiso 1 1 calc R . . C12 C 0.3583(3) -0.0020(2) 0.6908(3) 0.0288(9) Uani 1 1 d . . . C13 C 0.1983(4) -0.1457(3) 0.5122(4) 0.0461(12) Uani 1 1 d . . . H13A H 0.1202 -0.1318 0.5081 0.069 Uiso 1 1 calc R . . H13B H 0.2131 -0.1896 0.5583 0.069 Uiso 1 1 calc R . . H13C H 0.2164 -0.1603 0.4454 0.069 Uiso 1 1 calc R . . C14 C 0.4076(4) 0.0983(3) 0.4466(3) 0.0350(10) Uani 1 1 d . . . H14A H 0.3703 0.1481 0.4526 0.052 Uiso 1 1 calc R . . H14B H 0.3913 0.0787 0.3778 0.052 Uiso 1 1 calc R . . H14C H 0.4872 0.1055 0.4622 0.052 Uiso 1 1 calc R . . C15 C 0.3852(3) 0.0062(2) 0.8039(3) 0.0295(9) Uani 1 1 d . . . H15A H 0.3241 -0.0159 0.8372 0.035 Uiso 1 1 calc R . . H15B H 0.4523 -0.0241 0.8260 0.035 Uiso 1 1 calc R . . C16 C 0.3021(3) 0.1362(2) 0.8069(3) 0.0269(9) Uani 1 1 d . . . H16A H 0.2464 0.1264 0.8535 0.032 Uiso 1 1 calc R . . H16B H 0.2694 0.1232 0.7379 0.032 Uiso 1 1 calc R . . C17 C 0.3377(3) 0.2215(2) 0.8126(3) 0.0273(9) Uani 1 1 d . . . H17A H 0.3371 0.2435 0.7444 0.033 Uiso 1 1 calc R . . H17B H 0.2876 0.2523 0.8499 0.033 Uiso 1 1 calc R . . C18 C 0.4294(3) 0.0960(2) 0.9465(3) 0.0291(9) Uani 1 1 d . . . H18A H 0.4974 0.0672 0.9703 0.035 Uiso 1 1 calc R . . H18B H 0.3685 0.0759 0.9818 0.035 Uiso 1 1 calc R . . C19 C 0.4453(3) 0.1834(2) 0.9652(3) 0.0291(9) Uani 1 1 d . . . H19A H 0.3828 0.2046 0.9973 0.035 Uiso 1 1 calc R . . H19B H 0.5139 0.1928 1.0104 0.035 Uiso 1 1 calc R . . C20 C 0.4971(4) 0.3011(2) 0.8808(3) 0.0284(9) Uani 1 1 d . . . H20A H 0.5705 0.2977 0.9203 0.034 Uiso 1 1 calc R . . H20B H 0.4490 0.3315 0.9207 0.034 Uiso 1 1 calc R . . C21 C 0.5085(3) 0.3447(2) 0.7840(3) 0.0262(9) Uani 1 1 d . . . C22 C 0.4781(3) 0.4211(2) 0.7741(3) 0.0296(9) Uani 1 1 d . . . H22 H 0.4393 0.4444 0.8238 0.036 Uiso 1 1 calc R . . C23 C 0.5030(3) 0.4658(2) 0.6922(3) 0.0310(9) Uani 1 1 d . . . C24 C 0.5572(3) 0.4291(2) 0.6190(3) 0.0307(9) Uani 1 1 d . . . H24 H 0.5763 0.4587 0.5638 0.037 Uiso 1 1 calc R . . C25 C 0.5842(3) 0.3509(2) 0.6245(3) 0.0275(9) Uani 1 1 d . . . C26 C 0.5612(3) 0.3087(2) 0.7087(3) 0.0257(8) Uani 1 1 d . . . C27 C 0.6441(4) 0.3120(3) 0.5453(3) 0.0335(10) Uani 1 1 d . . . H27A H 0.7194 0.2995 0.5739 0.050 Uiso 1 1 calc R . . H27B H 0.6463 0.3472 0.4882 0.050 Uiso 1 1 calc R . . H27C H 0.6055 0.2643 0.5227 0.050 Uiso 1 1 calc R . . C28 C 0.4723(4) 0.5503(3) 0.6832(4) 0.0412(11) Uani 1 1 d . . . H28A H 0.5165 0.5757 0.6362 0.062 Uiso 1 1 calc R . . H28B H 0.4864 0.5750 0.7493 0.062 Uiso 1 1 calc R . . H28C H 0.3941 0.5550 0.6583 0.062 Uiso 1 1 calc R . . C29 C 0.4645(8) -0.2288(6) 0.7182(6) 0.112(3) Uani 1 1 d . . . H29A H 0.4583 -0.1731 0.7002 0.135 Uiso 1 1 calc R . . H29B H 0.4484 -0.2593 0.6557 0.135 Uiso 1 1 calc R . . 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 0.0221(4) 0.0262(4) 0.0208(4) 0.0015(3) 0.0027(3) 0.0020(3) Cl1 0.1194(19) 0.1014(17) 0.133(2) 0.0418(15) -0.0157(16) -0.0226(14) O1 0.0276(14) 0.0290(15) 0.0261(14) 0.0009(12) 0.0030(11) 0.0038(12) N1 0.0230(16) 0.0293(18) 0.0234(17) 0.0021(14) 0.0033(13) 0.0014(14) C1 0.026(2) 0.035(2) 0.025(2) 0.0066(17) 0.0055(16) -0.0003(18) Cl2 0.144(2) 0.0995(17) 0.0898(15) -0.0036(12) 0.0173(14) -0.0146(15) O2 0.0250(14) 0.0318(15) 0.0250(14) 0.0019(12) 0.0027(11) 0.0015(12) N2 0.0244(17) 0.0310(18) 0.0207(16) 0.0016(14) 0.0025(13) 0.0004(14) C2 0.023(2) 0.037(2) 0.027(2) 0.0075(18) 0.0050(16) 0.0035(17) O3 0.0245(14) 0.0305(15) 0.0226(14) 0.0018(11) 0.0022(11) 0.0020(12) C3 0.027(2) 0.043(3) 0.030(2) 0.0082(19) 0.0040(18) -0.0018(19) O4 0.0262(14) 0.0273(15) 0.0267(14) 0.0025(11) 0.0058(11) 0.0020(11) C4 0.025(2) 0.060(3) 0.035(2) 0.022(2) 0.0008(18) 0.003(2) C5 0.032(2) 0.045(3) 0.046(3) 0.022(2) 0.013(2) 0.014(2) C6 0.032(2) 0.034(2) 0.040(2) 0.0063(19) 0.0144(19) 0.0048(18) C7 0.0227(19) 0.028(2) 0.027(2) -0.0017(16) 0.0011(16) 0.0037(16) C8 0.027(2) 0.036(2) 0.028(2) -0.0034(18) 0.0024(17) 0.0080(18) C9 0.033(2) 0.040(3) 0.031(2) -0.0083(19) -0.0016(18) 0.0107(19) C10 0.029(2) 0.028(2) 0.045(3) -0.010(2) -0.0009(19) 0.0051(18) C11 0.027(2) 0.031(2) 0.037(2) -0.0029(19) 0.0018(18) 0.0054(18) C12 0.026(2) 0.032(2) 0.028(2) 0.0016(17) 0.0011(16) 0.0040(17) C13 0.039(3) 0.040(3) 0.057(3) -0.013(2) -0.002(2) 0.003(2) C14 0.037(2) 0.043(3) 0.024(2) -0.0015(19) 0.0000(18) 0.004(2) C15 0.026(2) 0.032(2) 0.030(2) 0.0037(18) 0.0057(17) -0.0033(17) C16 0.0200(18) 0.033(2) 0.028(2) 0.0048(17) 0.0050(15) 0.0059(16) C17 0.0209(19) 0.033(2) 0.028(2) 0.0011(17) 0.0040(16) 0.0051(16) C18 0.030(2) 0.036(2) 0.022(2) 0.0075(17) 0.0045(16) 0.0000(18) C19 0.030(2) 0.037(2) 0.021(2) 0.0010(17) 0.0067(16) 0.0034(18) C20 0.033(2) 0.027(2) 0.025(2) -0.0056(17) 0.0029(17) -0.0005(17) C21 0.0235(19) 0.029(2) 0.026(2) -0.0027(16) 0.0024(16) -0.0028(16) C22 0.026(2) 0.030(2) 0.032(2) -0.0044(18) 0.0020(17) -0.0008(17) C23 0.030(2) 0.027(2) 0.036(2) 0.0004(18) 0.0009(18) 0.0003(17) C24 0.031(2) 0.030(2) 0.030(2) 0.0032(18) 0.0007(17) -0.0040(18) C25 0.0236(19) 0.031(2) 0.028(2) -0.0006(17) 0.0023(16) 0.0008(17) C26 0.0216(19) 0.026(2) 0.028(2) -0.0006(17) -0.0016(15) -0.0017(16) C27 0.043(2) 0.031(2) 0.029(2) 0.0032(18) 0.0102(19) 0.0036(19) C28 0.053(3) 0.026(2) 0.045(3) 0.003(2) 0.011(2) 0.002(2) C29 0.156(9) 0.111(7) 0.068(5) 0.023(5) 0.007(5) 0.047(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.855(3) . ? Ti1 O3 1.864(3) . ? Ti1 O1 1.934(3) . ? Ti1 O2 1.975(3) . ? Ti1 N1 2.207(3) . ? Ti1 N2 2.230(3) . ? Cl1 C29 1.705(10) . ? O1 C1 1.356(5) . ? N1 C15 1.477(5) . ? N1 C18 1.487(5) . ? N1 C16 1.501(5) . ? C1 C6 1.389(6) . ? C1 C2 1.413(6) . ? Cl2 C29 1.756(10) . ? O2 C2 1.339(5) . ? N2 C20 1.478(5) . ? N2 C19 1.490(5) . ? N2 C17 1.492(5) . ? C2 C3 1.391(6) . ? O3 C7 1.359(5) . ? C3 C4 1.403(7) . ? C3 H3 0.9500 . ? O4 C26 1.363(5) . ? C4 C5 1.381(7) . ? C4 H4 0.9500 . ? C5 C6 1.403(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.400(6) . ? C7 C12 1.412(6) . ? C8 C9 1.397(6) . ? C8 C14 1.502(6) . ? C9 C10 1.387(7) . ? C9 H9 0.9500 . ? C10 C11 1.388(6) . ? C10 C13 1.511(6) . ? C11 C12 1.396(6) . ? C11 H11 0.9500 . ? C12 C15 1.519(6) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.532(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.535(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.519(6) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.371(6) . ? C21 C26 1.404(5) . ? C22 C23 1.403(6) . ? C22 H22 0.9500 . ? C23 C24 1.396(6) . ? C23 C28 1.505(6) . ? C24 C25 1.388(6) . ? C24 H24 0.9500 . ? C25 C26 1.397(6) . ? C25 C27 1.514(6) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 _geom_angle_publ_flag O4 Ti1 O3 94.79(12) . . ? O4 Ti1 O1 120.04(12) . . ? O3 Ti1 O1 87.19(12) . . ? O4 Ti1 O2 94.31(12) . . ? O3 Ti1 O2 166.03(12) . . ? O1 Ti1 O2 79.07(12) . . ? O4 Ti1 N1 146.30(12) . . ? O3 Ti1 N1 79.56(12) . . ? O1 Ti1 N1 93.05(12) . . ? O2 Ti1 N1 98.47(12) . . ? O4 Ti1 N2 85.96(12) . . ? O3 Ti1 N2 110.94(12) . . ? O1 Ti1 N2 147.72(12) . . ? O2 Ti1 N2 80.26(12) . . ? N1 Ti1 N2 65.87(12) . . ? C1 O1 Ti1 117.1(2) . . ? C15 N1 C18 112.8(3) . . ? C15 N1 C16 111.5(3) . . ? C18 N1 C16 106.4(3) . . ? C15 N1 Ti1 113.2(2) . . ? C18 N1 Ti1 104.9(2) . . ? C16 N1 Ti1 107.6(2) . . ? O1 C1 C6 125.4(4) . . ? O1 C1 C2 113.7(4) . . ? C6 C1 C2 120.9(4) . . ? C2 O2 Ti1 116.5(2) . . ? C20 N2 C19 110.7(3) . . ? C20 N2 C17 112.7(3) . . ? C19 N2 C17 106.6(3) . . ? C20 N2 Ti1 115.5(2) . . ? C19 N2 Ti1 108.2(2) . . ? C17 N2 Ti1 102.4(2) . . ? O2 C2 C3 126.5(4) . . ? O2 C2 C1 113.3(3) . . ? C3 C2 C1 120.2(4) . . ? C7 O3 Ti1 135.2(2) . . ? C2 C3 C4 118.3(4) . . ? C2 C3 H3 120.8 . . ? C4 C3 H3 120.8 . . ? C26 O4 Ti1 136.0(2) . . ? C5 C4 C3 121.5(4) . . ? C5 C4 H4 119.2 . . ? C3 C4 H4 119.2 . . ? C4 C5 C6 120.5(4) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C1 C6 C5 118.5(4) . . ? C1 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? O3 C7 C8 118.5(4) . . ? O3 C7 C12 121.2(4) . . ? C8 C7 C12 120.3(4) . . ? C9 C8 C7 118.8(4) . . ? C9 C8 C14 121.5(4) . . ? C7 C8 C14 119.7(4) . . ? C10 C9 C8 122.4(4) . . ? C10 C9 H9 118.8 . . ? C8 C9 H9 118.8 . . ? C9 C10 C11 117.7(4) . . ? C9 C10 C13 121.3(4) . . ? C11 C10 C13 121.0(4) . . ? C10 C11 C12 122.5(4) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C11 C12 C7 118.4(4) . . ? C11 C12 C15 118.9(4) . . ? C7 C12 C15 122.7(4) . . ? 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 . . ? C8 C14 H14A 109.5 . . ? C8 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C8 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C12 112.7(3) . . ? N1 C15 H15A 109.1 . . ? C12 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C12 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N1 C16 C17 107.5(3) . . ? N1 C16 H16A 110.2 . . ? C17 C16 H16A 110.2 . . ? N1 C16 H16B 110.2 . . ? C17 C16 H16B 110.2 . . ? H16A C16 H16B 108.5 . . ? N2 C17 C16 105.9(3) . . ? N2 C17 H17A 110.6 . . ? C16 C17 H17A 110.6 . . ? N2 C17 H17B 110.6 . . ? C16 C17 H17B 110.6 . . ? H17A C17 H17B 108.7 . . ? N1 C18 C19 105.4(3) . . ? N1 C18 H18A 110.7 . . ? C19 C18 H18A 110.7 . . ? N1 C18 H18B 110.7 . . ? C19 C18 H18B 110.7 . . ? H18A C18 H18B 108.8 . . ? N2 C19 C18 108.2(3) . . ? N2 C19 H19A 110.1 . . ? C18 C19 H19A 110.1 . . ? N2 C19 H19B 110.1 . . ? C18 C19 H19B 110.1 . . ? H19A C19 H19B 108.4 . . ? N2 C20 C21 114.5(3) . . ? N2 C20 H20A 108.6 . . ? C21 C20 H20A 108.6 . . ? N2 C20 H20B 108.6 . . ? C21 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C22 C21 C26 119.8(4) . . ? C22 C21 C20 120.5(4) . . ? C26 C21 C20 119.4(4) . . ? C21 C22 C23 121.5(4) . . ? C21 C22 H22 119.3 . . ? C23 C22 H22 119.3 . . ? C24 C23 C22 117.7(4) . . ? C24 C23 C28 121.1(4) . . ? C22 C23 C28 121.2(4) . . ? C25 C24 C23 122.1(4) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C24 C25 C26 118.6(4) . . ? C24 C25 C27 121.6(4) . . ? C26 C25 C27 119.6(4) . . ? O4 C26 C25 119.2(4) . . ? O4 C26 C21 120.6(4) . . ? C25 C26 C21 120.2(4) . . ? 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 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Cl1 C29 Cl2 113.0(4) . . ? Cl1 C29 H29A 109.0 . . ? Cl2 C29 H29A 109.0 . . ? Cl1 C29 H29B 109.0 . . ? Cl2 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.76 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.556 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.145 _database_code_depnum_ccdc_archive 'CCDC 961388' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L6(TiO2Ar2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28.50 H32 Cl N3 O6 Ti' _chemical_formula_weight 595.92 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' O O 0.0106 0.0060 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7780(2) _cell_length_b 13.3090(2) _cell_length_c 16.4640(3) _cell_angle_alpha 90.00 _cell_angle_beta 101.0970(10) _cell_angle_gamma 90.00 _cell_volume 2747.56(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 42158 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.441 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1244 _exptl_absorpt_coefficient_mu 0.457 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 40787 _diffrn_reflns_av_R_equivalents 0.0700 _diffrn_reflns_av_sigmaI/netI 0.0408 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.58 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6270 _reflns_number_gt 5144 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0681P)^2^+6.5769P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6270 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0785 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1664 _refine_ls_wR_factor_gt 0.1533 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.22533(4) 0.87870(3) 0.32084(3) 0.01925(14) Uani 1 1 d . . . Cl1 Cl 0.01529(16) 0.4827(2) 0.41704(9) 0.1304(9) Uani 1 1 d . . . O1 O 0.33263(15) 0.80689(15) 0.39867(12) 0.0251(4) Uani 1 1 d . . . N1 N 0.26798(18) 1.02936(17) 0.37260(14) 0.0226(5) Uani 1 1 d . . . C1 C 0.4273(2) 0.7912(2) 0.37680(18) 0.0242(6) Uani 1 1 d . . . O2 O 0.34183(16) 0.86552(15) 0.25681(12) 0.0262(4) Uani 1 1 d . . . N2 N 0.17958(18) 1.00247(17) 0.23150(14) 0.0211(5) Uani 1 1 d . . . C2 C 0.5157(2) 0.7473(2) 0.42621(19) 0.0287(6) Uani 1 1 d . . . H2 H 0.5149 0.7264 0.4813 0.034 Uiso 1 1 calc R . . O3 O 0.14382(15) 0.88413(14) 0.40287(11) 0.0225(4) Uani 1 1 d . . . N3 N 0.7027(2) 0.6938(2) 0.4425(2) 0.0392(7) Uani 1 1 d . . . C3 C 0.6065(2) 0.7353(2) 0.3908(2) 0.0304(6) Uani 1 1 d . . . O4 O 0.12840(15) 0.80244(14) 0.24951(12) 0.0228(4) Uani 1 1 d . . . C4 C 0.6117(2) 0.7636(2) 0.3111(2) 0.0313(6) Uani 1 1 d . . . H4 H 0.6746 0.7520 0.2897 0.038 Uiso 1 1 calc R . . O5 O 0.7042(2) 0.6835(3) 0.51729(19) 0.0646(9) Uani 1 1 d . . . C5 C 0.5235(2) 0.8092(2) 0.2625(2) 0.0302(6) Uani 1 1 d . . . H5 H 0.5256 0.8303 0.2077 0.036 Uiso 1 1 calc R . . O6 O 0.7786(2) 0.6734(2) 0.41000(19) 0.0557(7) Uani 1 1 d . . . C6 C 0.4315(2) 0.8237(2) 0.29554(18) 0.0249(6) Uani 1 1 d . . . C7 C 0.1636(2) 0.9131(2) 0.48332(16) 0.0226(5) Uani 1 1 d . . . C8 C 0.0957(2) 0.8764(2) 0.53417(18) 0.0252(6) Uani 1 1 d . . . C9 C 0.1152(2) 0.9049(2) 0.61701(18) 0.0283(6) Uani 1 1 d . . . H9 H 0.0712 0.8784 0.6523 0.034 Uiso 1 1 calc R . . C10 C 0.1972(2) 0.9711(2) 0.65014(18) 0.0286(6) Uani 1 1 d . . . C11 C 0.2612(2) 1.0077(2) 0.59783(17) 0.0278(6) Uani 1 1 d . . . H11 H 0.3170 1.0531 0.6193 0.033 Uiso 1 1 calc R . . C12 C 0.2464(2) 0.9801(2) 0.51458(17) 0.0243(6) Uani 1 1 d . . . C13 C 0.0035(3) 0.8097(3) 0.4973(2) 0.0326(7) Uani 1 1 d . . . H13A H -0.0255 0.7777 0.5418 0.049 Uiso 1 1 calc R . . H13B H 0.0282 0.7579 0.4631 0.049 Uiso 1 1 calc R . . H13C H -0.0521 0.8502 0.4629 0.049 Uiso 1 1 calc R . . C14 C 0.2129(3) 1.0043(3) 0.73929(19) 0.0364(7) Uani 1 1 d . . . H14A H 0.2861 1.0287 0.7574 0.055 Uiso 1 1 calc R . . H14B H 0.2003 0.9474 0.7739 0.055 Uiso 1 1 calc R . . H14C H 0.1627 1.0585 0.7445 0.055 Uiso 1 1 calc R . . C15 C 0.3188(2) 1.0251(2) 0.46148(17) 0.0263(6) Uani 1 1 d . . . H15A H 0.3391 1.0940 0.4813 0.032 Uiso 1 1 calc R . . H15B H 0.3848 0.9846 0.4678 0.032 Uiso 1 1 calc R . . C16 C 0.3385(2) 1.0732(2) 0.32005(18) 0.0276(6) Uani 1 1 d . . . H16A H 0.4060 1.0349 0.3262 0.033 Uiso 1 1 calc R . . H16B H 0.3554 1.1441 0.3355 0.033 Uiso 1 1 calc R . . C17 C 0.2752(2) 1.0660(2) 0.23043(18) 0.0265(6) Uani 1 1 d . . . H17A H 0.2532 1.1339 0.2090 0.032 Uiso 1 1 calc R . . H17B H 0.3200 1.0355 0.1942 0.032 Uiso 1 1 calc R . . C18 C 0.1685(2) 1.0914(2) 0.35812(18) 0.0264(6) Uani 1 1 d . . . H18A H 0.1863 1.1639 0.3594 0.032 Uiso 1 1 calc R . . H18B H 0.1261 1.0778 0.4013 0.032 Uiso 1 1 calc R . . C19 C 0.1051(2) 1.0614(2) 0.27205(17) 0.0248(6) Uani 1 1 d . . . H19A H 0.0423 1.0202 0.2776 0.030 Uiso 1 1 calc R . . H19B H 0.0801 1.1220 0.2391 0.030 Uiso 1 1 calc R . . C20 C 0.1295(2) 0.9710(2) 0.14586(16) 0.0245(6) Uani 1 1 d . . . H20A H 0.1825 0.9332 0.1213 0.029 Uiso 1 1 calc R . . H20B H 0.1094 1.0317 0.1116 0.029 Uiso 1 1 calc R . . C21 C 0.0319(2) 0.9066(2) 0.14337(16) 0.0234(5) Uani 1 1 d . . . C22 C 0.0361(2) 0.8229(2) 0.19555(16) 0.0223(5) Uani 1 1 d . . . C23 C -0.0526(2) 0.7608(2) 0.19346(17) 0.0249(6) Uani 1 1 d . . . C24 C -0.1441(2) 0.7813(2) 0.13430(19) 0.0291(6) Uani 1 1 d . . . H24 H -0.2038 0.7378 0.1302 0.035 Uiso 1 1 calc R . . C25 C -0.1507(2) 0.8636(2) 0.08104(18) 0.0291(6) Uani 1 1 d . . . C26 C -0.0627(2) 0.9268(2) 0.08741(17) 0.0267(6) Uani 1 1 d . . . H26 H -0.0670 0.9846 0.0531 0.032 Uiso 1 1 calc R . . C27 C -0.0508(3) 0.6767(2) 0.2545(2) 0.0320(6) Uani 1 1 d . . . H27A H 0.0215 0.6693 0.2872 0.048 Uiso 1 1 calc R . . H27B H -0.0722 0.6139 0.2247 0.048 Uiso 1 1 calc R . . H27C H -0.1004 0.6918 0.2914 0.048 Uiso 1 1 calc R . . C28 C -0.2516(3) 0.8826(3) 0.0185(2) 0.0384(7) Uani 1 1 d . . . H28A H -0.2528 0.9525 -0.0001 0.058 Uiso 1 1 calc R . . H28B H -0.3136 0.8698 0.0441 0.058 Uiso 1 1 calc R . . H28C H -0.2539 0.8377 -0.0290 0.058 Uiso 1 1 calc R . . C29 C 0.0250(7) 0.4619(6) 0.5204(6) 0.057(2) Uani 0.50 1 d P . . H29A H 0.1035 0.4616 0.5258 0.068 Uiso 0.50 1 calc PR . . H29B H -0.0073 0.3950 0.5065 0.068 Uiso 0.50 1 calc PR . . 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 0.0214(2) 0.0174(2) 0.0183(2) -0.00023(17) 0.00236(17) 0.00007(17) Cl1 0.1214(14) 0.218(2) 0.0457(7) 0.0031(10) 0.0015(8) -0.1100(15) O1 0.0255(10) 0.0256(10) 0.0234(9) 0.0027(8) 0.0029(8) 0.0018(8) N1 0.0248(11) 0.0206(11) 0.0217(11) -0.0002(9) 0.0029(9) -0.0033(9) C1 0.0238(13) 0.0190(13) 0.0287(14) -0.0009(10) 0.0020(11) -0.0006(10) O2 0.0253(10) 0.0290(10) 0.0243(10) 0.0022(8) 0.0044(8) 0.0024(8) N2 0.0249(11) 0.0186(11) 0.0194(10) -0.0001(8) 0.0029(9) -0.0009(9) C2 0.0296(15) 0.0243(14) 0.0304(15) 0.0028(11) 0.0010(12) -0.0012(11) O3 0.0244(9) 0.0233(9) 0.0196(9) -0.0020(7) 0.0040(7) -0.0015(7) N3 0.0294(14) 0.0375(15) 0.0484(17) 0.0078(13) 0.0017(12) 0.0042(11) C3 0.0229(14) 0.0229(14) 0.0429(17) -0.0015(12) 0.0000(12) 0.0021(11) O4 0.0253(10) 0.0194(9) 0.0222(9) -0.0003(7) 0.0007(8) 0.0007(7) C4 0.0266(14) 0.0280(15) 0.0405(17) -0.0050(13) 0.0093(13) -0.0009(12) O5 0.0411(15) 0.094(2) 0.0571(18) 0.0404(17) 0.0064(13) 0.0184(15) C5 0.0295(15) 0.0306(15) 0.0314(15) -0.0031(12) 0.0082(12) -0.0026(12) O6 0.0280(12) 0.078(2) 0.0602(17) -0.0038(15) 0.0052(12) 0.0186(13) C6 0.0256(14) 0.0192(13) 0.0292(14) -0.0035(10) 0.0032(11) -0.0014(10) C7 0.0245(13) 0.0222(13) 0.0207(12) -0.0003(10) 0.0035(10) 0.0026(10) C8 0.0249(13) 0.0243(14) 0.0269(14) -0.0002(11) 0.0059(11) 0.0034(11) C9 0.0294(15) 0.0313(15) 0.0264(14) 0.0019(11) 0.0105(12) 0.0063(12) C10 0.0352(15) 0.0282(15) 0.0218(13) -0.0022(11) 0.0037(11) 0.0086(12) C11 0.0338(15) 0.0262(14) 0.0218(13) -0.0023(11) 0.0013(11) 0.0032(11) C12 0.0281(14) 0.0224(13) 0.0215(13) -0.0002(10) 0.0027(11) 0.0008(11) C13 0.0303(15) 0.0375(17) 0.0316(15) -0.0027(13) 0.0100(12) -0.0048(13) C14 0.0463(19) 0.0401(18) 0.0232(14) -0.0044(13) 0.0077(13) 0.0035(14) C15 0.0292(14) 0.0258(14) 0.0221(13) -0.0025(11) 0.0006(11) -0.0048(11) C16 0.0314(15) 0.0247(14) 0.0255(14) 0.0010(11) 0.0029(11) -0.0079(11) C17 0.0317(15) 0.0225(13) 0.0252(13) 0.0025(11) 0.0051(11) -0.0048(11) C18 0.0318(15) 0.0200(13) 0.0266(14) -0.0026(10) 0.0033(11) 0.0033(11) C19 0.0283(14) 0.0191(13) 0.0259(13) -0.0003(10) 0.0025(11) 0.0043(10) C20 0.0300(14) 0.0246(13) 0.0185(12) 0.0004(10) 0.0038(11) 0.0001(11) C21 0.0264(13) 0.0248(13) 0.0187(12) -0.0034(10) 0.0035(10) 0.0014(11) C22 0.0222(13) 0.0233(13) 0.0209(12) -0.0039(10) 0.0027(10) 0.0027(10) C23 0.0261(14) 0.0251(14) 0.0237(13) -0.0041(11) 0.0054(11) 0.0004(11) C24 0.0251(14) 0.0298(15) 0.0318(15) -0.0059(12) 0.0043(12) -0.0038(11) C25 0.0249(14) 0.0368(16) 0.0243(14) -0.0059(12) 0.0013(11) 0.0044(12) C26 0.0298(14) 0.0284(14) 0.0209(13) -0.0001(11) 0.0024(11) 0.0034(11) C27 0.0315(15) 0.0289(15) 0.0359(16) 0.0021(12) 0.0074(13) -0.0053(12) C28 0.0296(16) 0.0460(19) 0.0353(17) 0.0000(14) -0.0042(13) 0.0028(14) C29 0.049(4) 0.044(4) 0.071(6) 0.025(4) -0.004(4) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.8395(19) . ? Ti1 O3 1.8589(19) . ? Ti1 O1 1.939(2) . ? Ti1 O2 1.990(2) . ? Ti1 N1 2.206(2) . ? Ti1 N2 2.211(2) . ? Cl1 C29 1.440(11) 3_566 ? O1 C1 1.343(3) . ? N1 C15 1.483(3) . ? N1 C16 1.483(4) . ? N1 C18 1.496(4) . ? C1 C2 1.388(4) . ? C1 C6 1.417(4) . ? O2 C6 1.322(3) . ? N2 C19 1.487(3) . ? N2 C17 1.489(4) . ? N2 C20 1.492(3) . ? C2 C3 1.404(4) . ? C2 H2 0.9500 . ? O3 C7 1.356(3) . ? N3 O6 1.225(4) . ? N3 O5 1.236(4) . ? N3 C3 1.462(4) . ? C3 C4 1.378(5) . ? O4 C22 1.360(3) . ? C4 C5 1.390(4) . ? C4 H4 0.9500 . ? C5 C6 1.400(4) . ? C5 H5 0.9500 . ? C7 C12 1.404(4) . ? C7 C8 1.404(4) . ? C8 C9 1.391(4) . ? C8 C13 1.506(4) . ? C9 C10 1.397(4) . ? C9 H9 0.9500 . ? C10 C11 1.385(4) . ? C10 C14 1.509(4) . ? C11 C12 1.396(4) . ? C11 H11 0.9500 . ? C12 C15 1.513(4) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.543(4) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.543(4) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.508(4) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C26 1.398(4) . ? C21 C22 1.401(4) . ? C22 C23 1.398(4) . ? C23 C24 1.397(4) . ? C23 C27 1.501(4) . ? C24 C25 1.395(4) . ? C24 H24 0.9500 . ? C25 C26 1.392(4) . ? C25 C28 1.508(4) . ? C26 H26 0.9500 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C29 1.313(15) 3_566 ? C29 Cl1 1.440(11) 3_566 ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 _geom_angle_publ_flag O4 Ti1 O3 94.74(9) . . ? O4 Ti1 O1 116.97(9) . . ? O3 Ti1 O1 87.87(8) . . ? O4 Ti1 O2 95.37(9) . . ? O3 Ti1 O2 165.67(9) . . ? O1 Ti1 O2 78.50(8) . . ? O4 Ti1 N1 146.54(9) . . ? O3 Ti1 N1 79.36(8) . . ? O1 Ti1 N1 95.86(9) . . ? O2 Ti1 N1 97.49(9) . . ? O4 Ti1 N2 85.82(8) . . ? O3 Ti1 N2 109.94(9) . . ? O1 Ti1 N2 150.44(9) . . ? O2 Ti1 N2 80.93(8) . . ? N1 Ti1 N2 66.03(8) . . ? C1 O1 Ti1 117.29(17) . . ? C15 N1 C16 113.0(2) . . ? C15 N1 C18 112.0(2) . . ? C16 N1 C18 106.4(2) . . ? C15 N1 Ti1 112.04(17) . . ? C16 N1 Ti1 105.35(17) . . ? C18 N1 Ti1 107.53(16) . . ? O1 C1 C2 125.6(3) . . ? O1 C1 C6 113.9(2) . . ? C2 C1 C6 120.5(3) . . ? C6 O2 Ti1 116.67(18) . . ? C19 N2 C17 107.7(2) . . ? C19 N2 C20 112.2(2) . . ? C17 N2 C20 110.6(2) . . ? C19 N2 Ti1 101.79(16) . . ? C17 N2 Ti1 108.58(16) . . ? C20 N2 Ti1 115.49(16) . . ? C1 C2 C3 116.7(3) . . ? C1 C2 H2 121.7 . . ? C3 C2 H2 121.7 . . ? C7 O3 Ti1 134.08(18) . . ? O6 N3 O5 123.3(3) . . ? O6 N3 C3 118.5(3) . . ? O5 N3 C3 118.2(3) . . ? C4 C3 C2 124.0(3) . . ? C4 C3 N3 117.9(3) . . ? C2 C3 N3 118.0(3) . . ? C22 O4 Ti1 134.33(17) . . ? C3 C4 C5 119.0(3) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 119.0(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? O2 C6 C5 125.8(3) . . ? O2 C6 C1 113.4(2) . . ? C5 C6 C1 120.8(3) . . ? O3 C7 C12 121.6(2) . . ? O3 C7 C8 117.6(2) . . ? C12 C7 C8 120.7(3) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 C13 122.3(3) . . ? C7 C8 C13 119.3(3) . . ? C8 C9 C10 122.3(3) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C11 C10 C9 117.8(3) . . ? C11 C10 C14 121.1(3) . . ? C9 C10 C14 121.0(3) . . ? C10 C11 C12 122.3(3) . . ? C10 C11 H11 118.9 . . ? C12 C11 H11 118.9 . . ? C11 C12 C7 118.5(3) . . ? C11 C12 C15 118.8(3) . . ? C7 C12 C15 122.8(2) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C12 112.7(2) . . ? N1 C15 H15A 109.1 . . ? C12 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? C12 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N1 C16 C17 105.5(2) . . ? N1 C16 H16A 110.6 . . ? C17 C16 H16A 110.6 . . ? N1 C16 H16B 110.6 . . ? C17 C16 H16B 110.6 . . ? H16A C16 H16B 108.8 . . ? N2 C17 C16 107.7(2) . . ? N2 C17 H17A 110.2 . . ? C16 C17 H17A 110.2 . . ? N2 C17 H17B 110.2 . . ? C16 C17 H17B 110.2 . . ? H17A C17 H17B 108.5 . . ? N1 C18 C19 106.4(2) . . ? N1 C18 H18A 110.4 . . ? C19 C18 H18A 110.4 . . ? N1 C18 H18B 110.4 . . ? C19 C18 H18B 110.4 . . ? H18A C18 H18B 108.6 . . ? N2 C19 C18 106.3(2) . . ? N2 C19 H19A 110.5 . . ? C18 C19 H19A 110.5 . . ? N2 C19 H19B 110.5 . . ? C18 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? N2 C20 C21 112.8(2) . . ? N2 C20 H20A 109.0 . . ? C21 C20 H20A 109.0 . . ? N2 C20 H20B 109.0 . . ? C21 C20 H20B 109.0 . . ? H20A C20 H20B 107.8 . . ? C26 C21 C22 118.9(3) . . ? C26 C21 C20 121.0(3) . . ? C22 C21 C20 120.1(2) . . ? O4 C22 C23 119.6(2) . . ? O4 C22 C21 119.1(2) . . ? C23 C22 C21 121.3(3) . . ? C24 C23 C22 117.8(3) . . ? C24 C23 C27 121.0(3) . . ? C22 C23 C27 121.1(3) . . ? C25 C24 C23 122.2(3) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26 C25 C24 118.4(3) . . ? C26 C25 C28 121.5(3) . . ? C24 C25 C28 120.1(3) . . ? C25 C26 C21 121.2(3) . . ? C25 C26 H26 119.4 . . ? C21 C26 H26 119.4 . . ? C23 C27 H27A 109.5 . . ? C23 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C23 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C29 C29 Cl1 76.4(9) 3_566 3_566 ? C29 C29 H29A 115.8 3_566 . ? Cl1 C29 H29A 115.8 3_566 . ? C29 C29 H29B 115.8 3_566 . ? Cl1 C29 H29B 115.8 3_566 . ? H29A C29 H29B 112.8 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.768 _refine_diff_density_min -1.596 _refine_diff_density_rms 0.092 _database_code_depnum_ccdc_archive 'CCDC 961389' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L6Ti(O2Ar4) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C37 H50 Cl2 N2 O4 Ti' _chemical_formula_weight 705.59 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.8000(2) _cell_length_b 12.5740(2) _cell_length_c 30.7360(5) _cell_angle_alpha 90 _cell_angle_beta 103.8080(10) _cell_angle_gamma 90 _cell_volume 7431.05(18) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 290302 _cell_measurement_theta_min 3.513 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.261 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.414 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 98628 _diffrn_reflns_av_R_equivalents 0.1423 _diffrn_reflns_av_sigmaI/netI 0.0789 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 3.53 _diffrn_reflns_theta_max 27.52 _reflns_number_total 16983 _reflns_number_gt 12004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Bruker AXS BV 1997-2004)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'Denzo & Scalepack (Otwinowski, Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97/2 (Sheldrick 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0934P)^2^+20.2606P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16983 _refine_ls_number_parameters 874 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0867 _refine_ls_wR_factor_ref 0.2455 _refine_ls_wR_factor_gt 0.2228 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.039 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.59160(3) 0.26293(6) 0.26641(2) 0.02888(17) Uani 1 1 d . . . Cl1 Cl 0.54213(14) 0.1041(2) 0.42443(7) 0.1110(7) Uani 1 1 d . . . O1 O 0.61197(13) 0.3435(2) 0.32106(9) 0.0303(6) Uani 1 1 d . . . N1 N 0.62244(16) 0.1067(3) 0.29867(11) 0.0329(7) Uani 1 1 d . . . C1 C 0.56114(18) 0.3514(3) 0.34381(12) 0.0280(8) Uani 1 1 d . . . Ti2 Ti 0.91910(3) -0.18999(6) 0.25971(2) 0.02794(17) Uani 1 1 d . . . Cl2 Cl 0.6378(2) -0.0184(3) 0.49408(9) 0.1732(16) Uani 1 1 d . . . O2 O 0.50088(13) 0.2639(2) 0.28038(9) 0.0325(6) Uani 1 1 d . . . N2 N 0.54713(16) 0.1223(3) 0.22506(11) 0.0332(7) Uani 1 1 d . . . C2 C 0.49801(18) 0.3056(3) 0.32010(12) 0.0287(8) Uani 1 1 d . . . Cl3 Cl 1.04655(12) -0.04746(19) 0.44056(8) 0.1116(7) Uani 1 1 d . . . O3 O 0.68814(13) 0.2629(2) 0.27004(9) 0.0340(6) Uani 1 1 d . . . N3 N 0.93649(16) -0.0512(3) 0.21816(11) 0.0323(7) Uani 1 1 d . . . C3 C 0.43961(18) 0.3065(3) 0.33766(13) 0.0291(8) Uani 1 1 d . . . H3 H 0.3975 0.2748 0.3215 0.035 Uiso 1 1 calc R . . Cl4 Cl 1.15635(12) 0.03603(17) 0.51175(7) 0.0985(6) Uani 1 1 d . . . O4 O 0.56609(14) 0.3413(2) 0.21367(9) 0.0341(6) Uani 1 1 d . . . N4 N 0.89952(16) -0.0327(3) 0.28689(11) 0.0305(7) Uani 1 1 d . . . C4 C 0.44309(19) 0.3540(3) 0.37901(13) 0.0311(8) Uani 1 1 d . . . O5 O 1.01931(13) -0.1852(2) 0.28297(9) 0.0326(6) Uani 1 1 d . . . C5 C 0.5064(2) 0.3978(3) 0.40225(13) 0.0317(8) Uani 1 1 d . . . H5 H 0.5086 0.4296 0.4306 0.038 Uiso 1 1 calc R . . O6 O 0.92915(13) -0.2671(2) 0.31496(9) 0.0320(6) Uani 1 1 d . . . C6 C 0.56726(19) 0.3974(3) 0.38585(12) 0.0288(8) Uani 1 1 d . . . O7 O 0.91895(14) -0.2719(2) 0.20888(9) 0.0335(6) Uani 1 1 d . . . C7 C 0.6369(2) 0.4430(3) 0.41290(13) 0.0340(9) Uani 1 1 d . . . O8 O 0.82298(13) -0.1997(2) 0.25572(9) 0.0311(6) Uani 1 1 d . . . C8 C 0.6902(2) 0.3516(4) 0.42346(17) 0.0499(12) Uani 1 1 d . . . H8A H 0.7348 0.3793 0.4408 0.075 Uiso 1 1 calc R . . H8B H 0.6965 0.3208 0.3954 0.075 Uiso 1 1 calc R . . H8C H 0.6733 0.2968 0.4409 0.075 Uiso 1 1 calc R . . C9 C 0.6635(2) 0.5298(4) 0.38608(15) 0.0446(11) Uani 1 1 d . . . H9A H 0.6316 0.5905 0.3818 0.067 Uiso 1 1 calc R . . H9B H 0.6661 0.5013 0.3568 0.067 Uiso 1 1 calc R . . H9C H 0.7099 0.5529 0.4025 0.067 Uiso 1 1 calc R . . C10 C 0.6307(2) 0.4915(4) 0.45716(14) 0.0418(10) Uani 1 1 d . . . H10A H 0.6764 0.5174 0.4736 0.063 Uiso 1 1 calc R . . H10B H 0.6141 0.4374 0.4751 0.063 Uiso 1 1 calc R . . H10C H 0.5978 0.5509 0.4513 0.063 Uiso 1 1 calc R . . C11 C 0.3782(2) 0.3536(4) 0.39855(14) 0.0361(9) Uani 1 1 d . . . C12 C 0.3677(3) 0.2422(5) 0.4147(2) 0.0695(17) Uani 1 1 d . . . H12A H 0.3602 0.1926 0.3894 0.104 Uiso 1 1 calc R . . H12B H 0.3271 0.2413 0.4278 0.104 Uiso 1 1 calc R . . H12C H 0.4091 0.2206 0.4375 0.104 Uiso 1 1 calc R . . C13 C 0.3851(2) 0.4313(5) 0.43747(18) 0.0591(15) Uani 1 1 d . . . H13A H 0.3413 0.4337 0.4470 0.089 Uiso 1 1 calc R . . H13B H 0.3958 0.5024 0.4279 0.089 Uiso 1 1 calc R . . H13C H 0.4226 0.4078 0.4626 0.089 Uiso 1 1 calc R . . C14 C 0.3129(2) 0.3869(5) 0.36284(16) 0.0564(14) Uani 1 1 d . . . H14A H 0.3046 0.3359 0.3380 0.085 Uiso 1 1 calc R . . H14B H 0.3200 0.4580 0.3516 0.085 Uiso 1 1 calc R . . H14C H 0.2727 0.3881 0.3762 0.085 Uiso 1 1 calc R . . C15 C 0.7421(2) 0.2458(3) 0.30572(15) 0.0359(9) Uani 1 1 d . . . C16 C 0.7361(2) 0.1810(3) 0.34174(15) 0.0361(9) Uani 1 1 d . . . C17 C 0.7925(2) 0.1710(4) 0.37880(16) 0.0440(10) Uani 1 1 d . . . H17 H 0.7879 0.1288 0.4035 0.053 Uiso 1 1 calc R . . C18 C 0.8558(2) 0.2222(4) 0.38011(18) 0.0507(12) Uani 1 1 d . . . C19 C 0.8616(2) 0.2804(4) 0.34276(19) 0.0515(12) Uani 1 1 d . . . H19 H 0.9050 0.3124 0.3427 0.062 Uiso 1 1 calc R . . C20 C 0.8064(2) 0.2937(4) 0.30548(17) 0.0422(10) Uani 1 1 d . . . C21 C 0.9164(3) 0.2121(6) 0.4206(2) 0.080(2) Uani 1 1 d . . . H21A H 0.9157 0.2718 0.4410 0.121 Uiso 1 1 calc R . . H21B H 0.9601 0.2130 0.4109 0.121 Uiso 1 1 calc R . . H21C H 0.9126 0.1451 0.4361 0.121 Uiso 1 1 calc R . . C22 C 0.8137(2) 0.3583(5) 0.26594(19) 0.0566(13) Uani 1 1 d . . . H22A H 0.7911 0.4275 0.2665 0.085 Uiso 1 1 calc R . . H22B H 0.7917 0.3207 0.2383 0.085 Uiso 1 1 calc R . . H22C H 0.8631 0.3691 0.2671 0.085 Uiso 1 1 calc R . . C23 C 0.6705(2) 0.1220(3) 0.34334(14) 0.0362(9) Uani 1 1 d . . . H23A H 0.6833 0.0514 0.3572 0.043 Uiso 1 1 calc R . . H23B H 0.6460 0.1617 0.3627 0.043 Uiso 1 1 calc R . . C24 C 0.6540(2) 0.0431(3) 0.26769(14) 0.0358(9) Uani 1 1 d . . . H24A H 0.6528 -0.0336 0.2747 0.043 Uiso 1 1 calc R . . H24B H 0.7030 0.0645 0.2706 0.043 Uiso 1 1 calc R . . C25 C 0.6104(2) 0.0656(3) 0.21965(14) 0.0359(9) Uani 1 1 d . . . H25A H 0.6369 0.1102 0.2030 0.043 Uiso 1 1 calc R . . H25B H 0.5976 -0.0018 0.2031 0.043 Uiso 1 1 calc R . . C26 C 0.5570(2) 0.0514(3) 0.30089(15) 0.0367(9) Uani 1 1 d . . . H26A H 0.5333 0.0892 0.3213 0.044 Uiso 1 1 calc R . . H26B H 0.5666 -0.0226 0.3116 0.044 Uiso 1 1 calc R . . C27 C 0.5118(2) 0.0532(3) 0.25210(15) 0.0388(9) Uani 1 1 d . . . H27A H 0.5066 -0.0197 0.2396 0.047 Uiso 1 1 calc R . . H27B H 0.4650 0.0816 0.2515 0.047 Uiso 1 1 calc R . . C28 C 0.4993(2) 0.1485(4) 0.18147(14) 0.0361(9) Uani 1 1 d . . . H28A H 0.4572 0.1830 0.1871 0.043 Uiso 1 1 calc R . . H28B H 0.4845 0.0817 0.1649 0.043 Uiso 1 1 calc R . . C29 C 0.53078(19) 0.2208(3) 0.15259(14) 0.0342(9) Uani 1 1 d . . . C30 C 0.56248(19) 0.3157(3) 0.17005(14) 0.0343(9) Uani 1 1 d . . . C31 C 0.5906(2) 0.3855(4) 0.14378(14) 0.0366(9) Uani 1 1 d . . . C33 C 0.5844(2) 0.3587(4) 0.09894(14) 0.0405(10) Uani 1 1 d . . . H33 H 0.6024 0.4062 0.0805 0.049 Uiso 1 1 calc R . . C34 C 0.5526(2) 0.2644(4) 0.08010(15) 0.0410(10) Uani 1 1 d . . . C35 C 0.5267(2) 0.1971(4) 0.10773(14) 0.0379(9) Uani 1 1 d . . . H35 H 0.5054 0.1323 0.0957 0.046 Uiso 1 1 calc R . . C36 C 0.6261(3) 0.4857(4) 0.16378(16) 0.0463(11) Uani 1 1 d . . . H36A H 0.5911 0.5374 0.1679 0.069 Uiso 1 1 calc R . . H36B H 0.6528 0.5156 0.1436 0.069 Uiso 1 1 calc R . . H36C H 0.6575 0.4696 0.1928 0.069 Uiso 1 1 calc R . . C37 C 0.5482(3) 0.2368(5) 0.03170(15) 0.0543(13) Uani 1 1 d . . . H37A H 0.5463 0.1594 0.0280 0.082 Uiso 1 1 calc R . . H37B H 0.5892 0.2646 0.0229 0.082 Uiso 1 1 calc R . . H37C H 0.5061 0.2685 0.0127 0.082 Uiso 1 1 calc R . . C38 C 1.04445(19) -0.2274(3) 0.32379(13) 0.0311(8) Uani 1 1 d . . . C39 C 0.99403(19) -0.2737(3) 0.34274(13) 0.0299(8) Uani 1 1 d . . . C40 C 1.0110(2) -0.3197(3) 0.38511(14) 0.0361(9) Uani 1 1 d . . . C41 C 1.0822(2) -0.3207(4) 0.40652(14) 0.0401(10) Uani 1 1 d . . . H41 H 1.0959 -0.3521 0.4354 0.048 Uiso 1 1 calc R . . C42 C 1.1341(2) -0.2783(3) 0.38790(15) 0.0397(10) Uani 1 1 d . A . C43 C 1.1145(2) -0.2290(3) 0.34619(14) 0.0358(9) Uani 1 1 d . . . H43 H 1.1485 -0.1968 0.3332 0.043 Uiso 1 1 calc R . . C44 C 0.9552(2) -0.3650(4) 0.40769(15) 0.0422(10) Uani 1 1 d . . . C45 C 0.9868(3) -0.4118(6) 0.4539(2) 0.078(2) Uani 1 1 d . . . H45A H 1.0188 -0.3600 0.4718 0.118 Uiso 1 1 calc R . . H45B H 1.0123 -0.4769 0.4507 0.118 Uiso 1 1 calc R . . H45C H 0.9497 -0.4284 0.4690 0.118 Uiso 1 1 calc R . . C46 C 0.9141(3) -0.4519(5) 0.3791(2) 0.0696(17) Uani 1 1 d . . . H46A H 0.8776 -0.4775 0.3930 0.104 Uiso 1 1 calc R . . H46B H 0.9453 -0.5108 0.3764 0.104 Uiso 1 1 calc R . . H46C H 0.8930 -0.4237 0.3492 0.104 Uiso 1 1 calc R . . C47 C 0.9063(3) -0.2766(5) 0.41339(19) 0.0596(14) Uani 1 1 d . . . H47A H 0.8816 -0.2502 0.3839 0.089 Uiso 1 1 calc R . . H47B H 0.9329 -0.2185 0.4307 0.089 Uiso 1 1 calc R . . H47C H 0.8725 -0.3038 0.4293 0.089 Uiso 1 1 calc R . . C48 C 1.2109(2) -0.2824(3) 0.41274(15) 0.0512(12) Uani 1 1 d D . . C49 C 1.2315(16) -0.1822(12) 0.4416(8) 0.106(11) Uani 0.50 1 d PD A 1 H49A H 1.2807 -0.1864 0.4572 0.159 Uiso 0.50 1 calc PR A 1 H49B H 1.2031 -0.1773 0.4637 0.159 Uiso 0.50 1 calc PR A 1 H49C H 1.2237 -0.1191 0.4223 0.159 Uiso 0.50 1 calc PR A 1 C50 C 1.2269(9) -0.3855(8) 0.4403(5) 0.065(4) Uani 0.50 1 d PD A 1 H50A H 1.2762 -0.3868 0.4559 0.098 Uiso 0.50 1 calc PR A 1 H50B H 1.2163 -0.4471 0.4203 0.098 Uiso 0.50 1 calc PR A 1 H50C H 1.1984 -0.3883 0.4624 0.098 Uiso 0.50 1 calc PR A 1 C51 C 1.2550(8) -0.2928(19) 0.3779(5) 0.082(7) Uani 0.50 1 d PD A 1 H51A H 1.3044 -0.2956 0.3933 0.123 Uiso 0.50 1 calc PR A 1 H51B H 1.2466 -0.2312 0.3578 0.123 Uiso 0.50 1 calc PR A 1 H51C H 1.2421 -0.3581 0.3605 0.123 Uiso 0.50 1 calc PR A 1 C52 C 0.8946(2) -0.2502(3) 0.16488(13) 0.0340(9) Uani 1 1 d . . . C53 C 0.9131(2) -0.1540(4) 0.14744(14) 0.0374(9) Uani 1 1 d . . . C54 C 0.8871(2) -0.1320(4) 0.10209(15) 0.0458(11) Uani 1 1 d . . . H54 H 0.8998 -0.0674 0.0901 0.055 Uiso 1 1 calc R . . C55 C 0.8431(2) -0.2023(5) 0.07391(15) 0.0498(12) Uani 1 1 d . . . C56 C 0.8255(2) -0.2955(4) 0.09193(15) 0.0464(11) Uani 1 1 d . . . H56 H 0.7955 -0.3440 0.0729 0.056 Uiso 1 1 calc R . . C57 C 0.8500(2) -0.3218(4) 0.13716(15) 0.0400(10) Uani 1 1 d . . . C58 C 0.8288(3) -0.4232(4) 0.15696(17) 0.0497(11) Uani 1 1 d . . . H58A H 0.7919 -0.4586 0.1347 0.075 Uiso 1 1 calc R . . H58B H 0.8117 -0.4060 0.1835 0.075 Uiso 1 1 calc R . . H58C H 0.8691 -0.4706 0.1655 0.075 Uiso 1 1 calc R . . C59 C 0.8143(3) -0.1753(5) 0.02468(17) 0.0662(16) Uani 1 1 d . . . H59A H 0.8436 -0.2080 0.0068 0.099 Uiso 1 1 calc R . . H59B H 0.8140 -0.0979 0.0208 0.099 Uiso 1 1 calc R . . H59C H 0.7667 -0.2026 0.0148 0.099 Uiso 1 1 calc R . . C60 C 0.9611(2) -0.0784(4) 0.17804(14) 0.0388(9) Uani 1 1 d . . . H60A H 1.0079 -0.1111 0.1874 0.047 Uiso 1 1 calc R . . H60B H 0.9656 -0.0124 0.1614 0.047 Uiso 1 1 calc R . . C61 C 0.86750(19) 0.0023(3) 0.20654(14) 0.0353(9) Uani 1 1 d . . . H61A H 0.8326 -0.0439 0.1870 0.042 Uiso 1 1 calc R . . H61B H 0.8704 0.0700 0.1906 0.042 Uiso 1 1 calc R . . C62 C 0.8472(2) 0.0234(3) 0.25095(15) 0.0360(9) Uani 1 1 d . . . H62A H 0.8477 0.1007 0.2571 0.043 Uiso 1 1 calc R . . H62B H 0.7999 -0.0041 0.2496 0.043 Uiso 1 1 calc R . . C63 C 0.98582(19) 0.0235(3) 0.24810(14) 0.0362(9) Uani 1 1 d . . . H63A H 0.9828 0.0951 0.2344 0.043 Uiso 1 1 calc R . . H63B H 1.0342 -0.0024 0.2525 0.043 Uiso 1 1 calc R . . C64 C 0.9657(2) 0.0285(4) 0.29294(15) 0.0378(9) Uani 1 1 d . . . H64A H 1.0025 -0.0037 0.3169 0.045 Uiso 1 1 calc R . . H64B H 0.9588 0.1032 0.3011 0.045 Uiso 1 1 calc R . . C65 C 0.8749(2) -0.0425(3) 0.32836(14) 0.0355(9) Uani 1 1 d . . . H65A H 0.8637 0.0293 0.3379 0.043 Uiso 1 1 calc R . . H65B H 0.9131 -0.0717 0.3523 0.043 Uiso 1 1 calc R . . C66 C 0.81130(19) -0.1132(3) 0.32367(14) 0.0328(8) Uani 1 1 d . . . C67 C 0.78927(19) -0.1867(3) 0.28875(13) 0.0308(8) Uani 1 1 d . . . C68 C 0.7323(2) -0.2535(3) 0.28859(14) 0.0360(9) Uani 1 1 d . . . C69 C 0.6984(2) -0.2448(4) 0.32319(16) 0.0421(10) Uani 1 1 d . . . H69 H 0.6597 -0.2897 0.3230 0.050 Uiso 1 1 calc R . . C70 C 0.7193(2) -0.1727(4) 0.35807(16) 0.0426(10) Uani 1 1 d . . . C71 C 0.7758(2) -0.1084(3) 0.35756(15) 0.0368(9) Uani 1 1 d . . . H71 H 0.7910 -0.0591 0.3813 0.044 Uiso 1 1 calc R . . C72 C 0.6833(3) -0.1686(5) 0.39660(19) 0.0601(14) Uani 1 1 d . . . H72A H 0.6328 -0.1654 0.3846 0.090 Uiso 1 1 calc R . . H72B H 0.6988 -0.1053 0.4149 0.090 Uiso 1 1 calc R . . H72C H 0.6951 -0.2325 0.4151 0.090 Uiso 1 1 calc R . . C73 C 0.7117(2) -0.3366(4) 0.25272(16) 0.0459(11) Uani 1 1 d . . . H73A H 0.7472 -0.3925 0.2573 0.069 Uiso 1 1 calc R . . H73B H 0.7074 -0.3038 0.2233 0.069 Uiso 1 1 calc R . . H73C H 0.6669 -0.3677 0.2542 0.069 Uiso 1 1 calc R . . C74 C 0.5687(5) -0.0178(9) 0.4566(6) 0.198(8) Uani 1 1 d . . . H74A H 0.5305 -0.0380 0.4707 0.237 Uiso 1 1 calc R . . H74B H 0.5722 -0.0747 0.4350 0.237 Uiso 1 1 calc R . . C75 C 1.0780(3) 0.0604(6) 0.4740(2) 0.0778(18) Uani 1 1 d . . . H75A H 1.0432 0.0815 0.4908 0.093 Uiso 1 1 calc R . . H75B H 1.0840 0.1208 0.4546 0.093 Uiso 1 1 calc R . . C50' C 1.2216(11) -0.3375(19) 0.4586(4) 0.122(11) Uani 0.50 1 d PD A 2 H50D H 1.2712 -0.3386 0.4734 0.184 Uiso 0.50 1 calc PR A 2 H50E H 1.2039 -0.4105 0.4544 0.184 Uiso 0.50 1 calc PR A 2 H50F H 1.1963 -0.2983 0.4773 0.184 Uiso 0.50 1 calc PR A 2 C49' C 1.2359(11) -0.1672(7) 0.4231(7) 0.064(5) Uani 0.50 1 d PD A 2 H49D H 1.2851 -0.1674 0.4391 0.096 Uiso 0.50 1 calc PR A 2 H49E H 1.2083 -0.1334 0.4419 0.096 Uiso 0.50 1 calc PR A 2 H49F H 1.2302 -0.1275 0.3951 0.096 Uiso 0.50 1 calc PR A 2 C51' C 1.2572(8) -0.3294(16) 0.3838(5) 0.085(8) Uani 0.50 1 d PD A 2 H51D H 1.3057 -0.3305 0.4011 0.128 Uiso 0.50 1 calc PR A 2 H51E H 1.2534 -0.2854 0.3570 0.128 Uiso 0.50 1 calc PR A 2 H51F H 1.2420 -0.4020 0.3749 0.128 Uiso 0.50 1 calc PR A 2 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 0.0231(3) 0.0306(4) 0.0335(4) -0.0053(3) 0.0078(3) -0.0002(3) Cl1 0.146(2) 0.1176(18) 0.0727(12) -0.0100(11) 0.0326(12) -0.0031(15) O1 0.0228(12) 0.0341(15) 0.0335(14) -0.0038(11) 0.0060(10) -0.0006(11) N1 0.0269(15) 0.0317(18) 0.0411(19) -0.0039(14) 0.0102(13) 0.0012(13) C1 0.0231(16) 0.0305(19) 0.0315(19) -0.0008(15) 0.0083(14) 0.0038(14) Ti2 0.0205(3) 0.0307(4) 0.0317(4) 0.0014(3) 0.0044(2) 0.0023(3) Cl2 0.258(4) 0.151(3) 0.0938(18) -0.0312(17) 0.009(2) 0.073(3) O2 0.0251(12) 0.0359(15) 0.0363(15) -0.0090(12) 0.0072(11) -0.0008(11) N2 0.0243(15) 0.0361(19) 0.0411(19) -0.0090(15) 0.0114(13) -0.0048(13) C2 0.0245(17) 0.0302(19) 0.0306(19) -0.0023(15) 0.0049(14) 0.0019(15) Cl3 0.0967(14) 0.0986(16) 0.1277(18) -0.0338(13) 0.0032(12) -0.0075(12) O3 0.0274(13) 0.0360(15) 0.0400(15) -0.0058(12) 0.0106(11) -0.0019(11) N3 0.0228(15) 0.0345(18) 0.0386(18) 0.0037(14) 0.0055(13) -0.0009(13) C3 0.0226(16) 0.0290(19) 0.036(2) -0.0012(16) 0.0066(14) 0.0009(14) Cl4 0.1101(15) 0.0940(14) 0.0778(12) 0.0099(10) -0.0048(10) 0.0028(11) O4 0.0342(14) 0.0377(16) 0.0300(14) -0.0058(12) 0.0067(11) -0.0027(12) N4 0.0249(15) 0.0255(16) 0.0409(18) -0.0011(14) 0.0077(13) -0.0006(12) C4 0.0291(18) 0.030(2) 0.035(2) 0.0025(16) 0.0095(15) 0.0012(15) O5 0.0239(12) 0.0408(16) 0.0318(14) 0.0065(12) 0.0040(10) 0.0022(11) C5 0.0337(19) 0.034(2) 0.0276(19) -0.0003(16) 0.0067(15) 0.0053(16) O6 0.0255(12) 0.0363(15) 0.0329(14) 0.0028(12) 0.0044(10) 0.0015(11) C6 0.0285(18) 0.0256(19) 0.0299(19) -0.0001(15) 0.0023(14) 0.0021(14) O7 0.0343(14) 0.0327(15) 0.0330(14) 0.0006(12) 0.0068(11) 0.0035(12) C7 0.0286(18) 0.037(2) 0.033(2) -0.0026(17) -0.0001(15) 0.0029(16) O8 0.0244(12) 0.0332(15) 0.0348(14) -0.0013(11) 0.0055(10) 0.0017(11) C8 0.037(2) 0.051(3) 0.052(3) -0.012(2) -0.009(2) 0.013(2) C9 0.038(2) 0.052(3) 0.041(2) -0.003(2) 0.0036(18) -0.013(2) C10 0.039(2) 0.049(3) 0.034(2) -0.0072(19) 0.0020(17) 0.0029(19) C11 0.034(2) 0.041(2) 0.036(2) -0.0035(18) 0.0153(17) 0.0007(17) C12 0.061(3) 0.058(3) 0.107(5) 0.015(3) 0.054(3) 0.002(3) C13 0.036(2) 0.091(4) 0.055(3) -0.029(3) 0.021(2) -0.006(3) C14 0.033(2) 0.093(4) 0.046(3) -0.004(3) 0.015(2) 0.012(2) C15 0.0255(18) 0.035(2) 0.047(2) -0.0081(18) 0.0088(16) 0.0044(16) C16 0.0277(18) 0.030(2) 0.050(2) -0.0080(18) 0.0080(17) 0.0046(16) C17 0.039(2) 0.035(2) 0.053(3) -0.006(2) 0.0013(19) 0.0053(18) C18 0.036(2) 0.041(3) 0.067(3) -0.009(2) -0.006(2) 0.0016(19) C19 0.028(2) 0.045(3) 0.076(4) -0.010(3) 0.003(2) -0.0040(19) C20 0.030(2) 0.036(2) 0.061(3) -0.008(2) 0.0108(19) -0.0016(17) C21 0.052(3) 0.072(4) 0.097(5) 0.005(4) -0.024(3) -0.011(3) C22 0.035(2) 0.060(3) 0.076(4) 0.000(3) 0.016(2) -0.016(2) C23 0.0319(19) 0.036(2) 0.040(2) -0.0007(18) 0.0072(16) 0.0053(17) C24 0.0275(18) 0.032(2) 0.050(2) -0.0083(18) 0.0124(17) 0.0014(16) C25 0.037(2) 0.032(2) 0.043(2) -0.0084(18) 0.0167(18) -0.0018(17) C26 0.0310(19) 0.034(2) 0.047(2) -0.0014(18) 0.0149(17) -0.0048(16) C27 0.035(2) 0.035(2) 0.049(2) -0.0082(19) 0.0154(18) -0.0089(17) C28 0.0263(18) 0.041(2) 0.040(2) -0.0090(18) 0.0057(16) -0.0084(17) C29 0.0259(18) 0.038(2) 0.038(2) -0.0055(17) 0.0047(15) -0.0009(16) C30 0.0252(17) 0.041(2) 0.036(2) -0.0050(18) 0.0061(15) 0.0027(16) C31 0.032(2) 0.039(2) 0.036(2) 0.0013(18) 0.0031(16) 0.0018(17) C33 0.043(2) 0.044(3) 0.034(2) 0.0074(19) 0.0095(18) 0.0063(19) C34 0.037(2) 0.046(3) 0.038(2) -0.0051(19) 0.0037(17) 0.0043(19) C35 0.0310(19) 0.046(2) 0.034(2) -0.0092(18) 0.0013(16) -0.0020(18) C36 0.053(3) 0.041(3) 0.044(3) 0.001(2) 0.009(2) -0.009(2) C37 0.066(3) 0.062(3) 0.034(2) -0.006(2) 0.009(2) 0.002(3) C38 0.0268(18) 0.032(2) 0.033(2) 0.0025(16) 0.0044(15) 0.0056(15) C39 0.0279(18) 0.030(2) 0.0298(19) -0.0008(15) 0.0022(14) 0.0019(15) C40 0.037(2) 0.034(2) 0.037(2) 0.0004(17) 0.0077(17) 0.0022(17) C41 0.046(2) 0.037(2) 0.032(2) 0.0043(18) -0.0020(17) 0.0032(19) C42 0.034(2) 0.033(2) 0.044(2) -0.0013(18) -0.0069(17) -0.0013(17) C43 0.0268(18) 0.036(2) 0.041(2) -0.0008(18) 0.0009(16) 0.0006(16) C44 0.048(2) 0.044(3) 0.037(2) 0.0096(19) 0.0139(19) 0.011(2) C45 0.069(4) 0.103(5) 0.070(4) 0.048(4) 0.029(3) 0.025(4) C46 0.076(4) 0.064(4) 0.083(4) -0.013(3) 0.048(3) -0.029(3) C47 0.067(3) 0.060(3) 0.062(3) 0.010(3) 0.036(3) 0.016(3) C48 0.036(2) 0.047(3) 0.056(3) 0.007(2) -0.017(2) -0.002(2) C49 0.082(15) 0.073(11) 0.12(2) -0.044(11) -0.050(15) 0.020(9) C50 0.030(6) 0.082(10) 0.073(9) 0.026(8) -0.009(7) 0.010(7) C51 0.016(5) 0.116(19) 0.103(12) 0.032(11) -0.005(6) 0.031(7) C52 0.0279(18) 0.041(2) 0.033(2) -0.0009(17) 0.0063(15) 0.0079(16) C53 0.0253(18) 0.048(3) 0.040(2) 0.0039(19) 0.0090(16) 0.0058(17) C54 0.045(2) 0.055(3) 0.039(2) 0.005(2) 0.0127(19) 0.006(2) C55 0.046(3) 0.066(3) 0.036(2) -0.001(2) 0.0081(19) 0.018(2) C56 0.041(2) 0.055(3) 0.040(2) -0.010(2) 0.0038(19) 0.012(2) C57 0.037(2) 0.043(2) 0.040(2) -0.0058(19) 0.0092(17) 0.0078(18) C58 0.049(3) 0.045(3) 0.052(3) -0.009(2) 0.007(2) -0.004(2) C59 0.079(4) 0.078(4) 0.035(3) 0.001(3) 0.002(2) 0.023(3) C60 0.0297(19) 0.046(3) 0.042(2) 0.0080(19) 0.0105(17) 0.0016(18) C61 0.0234(17) 0.035(2) 0.045(2) 0.0084(18) 0.0031(16) 0.0037(16) C62 0.0255(18) 0.028(2) 0.052(3) 0.0031(18) 0.0055(17) 0.0050(15) C63 0.0252(18) 0.035(2) 0.047(2) 0.0052(18) 0.0043(17) -0.0052(16) C64 0.0256(18) 0.036(2) 0.050(2) -0.0032(19) 0.0043(17) -0.0062(16) C65 0.0299(19) 0.036(2) 0.042(2) -0.0050(18) 0.0098(16) -0.0002(16) C66 0.0257(18) 0.030(2) 0.042(2) 0.0017(17) 0.0077(16) 0.0037(15) C67 0.0253(17) 0.032(2) 0.036(2) 0.0028(16) 0.0083(15) 0.0029(15) C68 0.0272(18) 0.036(2) 0.043(2) 0.0047(18) 0.0049(16) -0.0029(16) C69 0.033(2) 0.041(2) 0.055(3) 0.005(2) 0.0159(19) -0.0031(18) C70 0.040(2) 0.042(3) 0.051(3) 0.005(2) 0.020(2) 0.0007(19) C71 0.036(2) 0.030(2) 0.045(2) -0.0011(18) 0.0115(17) 0.0050(17) C72 0.069(3) 0.057(3) 0.066(3) -0.001(3) 0.040(3) -0.008(3) C73 0.043(2) 0.045(3) 0.048(3) -0.003(2) 0.007(2) -0.015(2) C74 0.080(6) 0.112(8) 0.42(2) -0.147(12) 0.106(10) -0.056(6) C75 0.064(4) 0.076(4) 0.097(5) -0.001(4) 0.026(3) -0.009(3) C50' 0.064(12) 0.16(2) 0.105(15) 0.081(15) -0.057(12) -0.050(14) C49' 0.027(5) 0.078(11) 0.074(11) -0.031(8) -0.012(7) -0.004(6) C51' 0.056(9) 0.064(11) 0.101(12) -0.042(10) -0.048(8) 0.042(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O4 1.861(3) . ? Ti1 O3 1.888(3) . ? Ti1 O1 1.920(3) . ? Ti1 O2 1.944(3) . ? Ti1 N1 2.219(3) . ? Ti1 N2 2.232(3) . ? Cl1 C74 1.831(16) . ? O1 C1 1.359(4) . ? N1 C23 1.485(5) . ? N1 C24 1.490(5) . ? N1 C26 1.487(5) . ? C1 C6 1.394(5) . ? C1 C2 1.411(5) . ? Ti2 O7 1.870(3) . ? Ti2 O8 1.882(3) . ? Ti2 O6 1.924(3) . ? Ti2 O5 1.943(3) . ? Ti2 N4 2.217(3) . ? Ti2 N3 2.237(3) . ? Cl2 C74 1.566(14) . ? O2 C2 1.343(5) . ? N2 C25 1.484(5) . ? N2 C28 1.482(5) . ? N2 C27 1.487(5) . ? C2 C3 1.388(5) . ? Cl3 C75 1.726(7) . ? O3 C15 1.354(5) . ? N3 C60 1.470(5) . ? N3 C61 1.488(5) . ? N3 C63 1.501(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? Cl4 C75 1.728(7) . ? O4 C30 1.364(5) . ? N4 C65 1.474(5) . ? N4 C64 1.493(5) . ? N4 C62 1.499(5) . ? C4 C5 1.400(5) . ? C4 C11 1.543(5) . ? O5 C38 1.344(5) . ? C5 C6 1.413(5) . ? C5 H5 0.9500 . ? O6 C39 1.365(4) . ? C6 C7 1.540(5) . ? O7 C52 1.351(5) . ? C7 C10 1.522(6) . ? C7 C9 1.535(6) . ? C7 C8 1.542(6) . ? O8 C67 1.351(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.518(7) . ? C11 C14 1.541(6) . ? C11 C13 1.525(6) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.402(6) . ? C15 C20 1.410(6) . ? C16 C17 1.398(6) . ? C16 C23 1.506(6) . ? C17 C18 1.401(7) . ? C17 H17 0.9500 . ? C18 C19 1.389(8) . ? C18 C21 1.513(7) . ? C19 C20 1.392(7) . ? C19 H19 0.9500 . ? C20 C22 1.497(7) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.548(6) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C27 1.552(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.506(6) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.395(6) . ? C29 C35 1.394(6) . ? C30 C31 1.395(6) . ? C31 C33 1.396(6) . ? C31 C36 1.501(6) . ? C33 C34 1.401(7) . ? C33 H33 0.9500 . ? C34 C35 1.381(6) . ? C34 C37 1.510(6) . ? C35 H35 0.9500 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 C43 1.394(5) . ? C38 C39 1.397(5) . ? C39 C40 1.391(6) . ? C40 C41 1.408(6) . ? C40 C44 1.547(6) . ? C41 C42 1.395(6) . ? C41 H41 0.9500 . ? C42 C43 1.393(6) . ? C42 C48 1.531(5) . ? C43 H43 0.9500 . ? C44 C46 1.512(7) . ? C44 C47 1.511(7) . ? C44 C45 1.528(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.539(2) . ? C48 C51' 1.539(2) . ? C48 C49' 1.540(2) . ? C48 C51 1.540(2) . ? C48 C50' 1.540(2) . ? C48 C50 1.540(2) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C57 1.398(6) . ? C52 C53 1.407(6) . ? C53 C54 1.393(6) . ? C53 C60 1.505(6) . ? C54 C55 1.389(7) . ? C54 H54 0.9500 . ? C55 C56 1.376(8) . ? C55 C59 1.523(7) . ? C56 C57 1.398(6) . ? C56 H56 0.9500 . ? C57 C58 1.515(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.535(6) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.524(6) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.520(5) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 C71 1.390(6) . ? C66 C67 1.405(6) . ? C67 C68 1.405(5) . ? C68 C69 1.391(6) . ? C68 C73 1.503(6) . ? C69 C70 1.389(7) . ? C69 H69 0.9500 . ? C70 C71 1.384(6) . ? C70 C72 1.521(6) . ? C71 H71 0.9500 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C50' H50D 0.9800 . ? C50' H50E 0.9800 . ? C50' H50F 0.9800 . ? C49' H49D 0.9800 . ? C49' H49E 0.9800 . ? C49' H49F 0.9800 . ? C51' H51D 0.9800 . ? C51' H51E 0.9800 . ? C51' H51F 0.9800 . ? 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 _geom_angle_publ_flag O4 Ti1 O3 96.44(12) . . ? O4 Ti1 O1 116.07(12) . . ? O3 Ti1 O1 87.15(11) . . ? O4 Ti1 O2 96.68(12) . . ? O3 Ti1 O2 164.32(12) . . ? O1 Ti1 O2 79.39(11) . . ? O4 Ti1 N1 147.81(13) . . ? O3 Ti1 N1 78.84(12) . . ? O1 Ti1 N1 95.63(12) . . ? O2 Ti1 N1 94.40(12) . . ? O4 Ti1 N2 86.27(13) . . ? O3 Ti1 N2 106.83(12) . . ? O1 Ti1 N2 152.62(12) . . ? O2 Ti1 N2 82.58(11) . . ? N1 Ti1 N2 65.32(13) . . ? C1 O1 Ti1 117.5(2) . . ? C23 N1 C24 112.7(3) . . ? C23 N1 C26 113.1(3) . . ? C24 N1 C26 106.3(3) . . ? C23 N1 Ti1 110.3(2) . . ? C24 N1 Ti1 107.6(3) . . ? C26 N1 Ti1 106.5(2) . . ? O1 C1 C6 126.6(3) . . ? O1 C1 C2 112.2(3) . . ? C6 C1 C2 121.2(3) . . ? O7 Ti2 O8 96.31(12) . . ? O7 Ti2 O6 116.04(13) . . ? O8 Ti2 O6 85.12(11) . . ? O7 Ti2 O5 97.03(12) . . ? O8 Ti2 O5 162.61(12) . . ? O6 Ti2 O5 79.03(11) . . ? O7 Ti2 N4 147.17(13) . . ? O8 Ti2 N4 79.46(12) . . ? O6 Ti2 N4 96.17(12) . . ? O5 Ti2 N4 95.08(12) . . ? O7 Ti2 N3 85.55(13) . . ? O8 Ti2 N3 107.72(12) . . ? O6 Ti2 N3 154.07(12) . . ? O5 Ti2 N3 84.43(11) . . ? N4 Ti2 N3 65.41(12) . . ? C2 O2 Ti1 116.4(2) . . ? C25 N2 C28 112.4(3) . . ? C25 N2 C27 107.7(3) . . ? C28 N2 C27 110.5(3) . . ? C25 N2 Ti1 102.5(2) . . ? C28 N2 Ti1 114.8(3) . . ? C27 N2 Ti1 108.6(2) . . ? O2 C2 C3 125.2(3) . . ? O2 C2 C1 113.9(3) . . ? C3 C2 C1 120.9(3) . . ? C15 O3 Ti1 129.9(3) . . ? C60 N3 C61 111.9(3) . . ? C60 N3 C63 111.2(3) . . ? C61 N3 C63 106.8(3) . . ? C60 N3 Ti2 115.1(3) . . ? C61 N3 Ti2 103.4(2) . . ? C63 N3 Ti2 107.7(2) . . ? C2 C3 C4 119.6(3) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C30 O4 Ti1 132.2(3) . . ? C65 N4 C64 113.4(3) . . ? C65 N4 C62 111.3(3) . . ? C64 N4 C62 106.3(3) . . ? C65 N4 Ti2 112.0(2) . . ? C64 N4 Ti2 106.2(2) . . ? C62 N4 Ti2 107.1(2) . . ? C3 C4 C5 118.6(3) . . ? C3 C4 C11 119.4(3) . . ? C5 C4 C11 122.0(4) . . ? C38 O5 Ti2 116.7(2) . . ? C4 C5 C6 123.6(4) . . ? C4 C5 H5 118.2 . . ? C6 C5 H5 118.2 . . ? C39 O6 Ti2 117.8(2) . . ? C1 C6 C5 116.1(3) . . ? C1 C6 C7 121.6(3) . . ? C5 C6 C7 122.4(3) . . ? C52 O7 Ti2 130.9(3) . . ? C10 C7 C9 107.8(4) . . ? C10 C7 C6 112.3(3) . . ? C9 C7 C6 110.7(3) . . ? C10 C7 C8 107.9(3) . . ? C9 C7 C8 109.6(4) . . ? C6 C7 C8 108.4(3) . . ? C67 O8 Ti2 128.0(2) . . ? 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 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C14 109.1(4) . . ? C12 C11 C4 108.8(4) . . ? C14 C11 C4 110.9(3) . . ? C12 C11 C13 109.2(4) . . ? C14 C11 C13 106.7(4) . . ? C4 C11 C13 112.1(4) . . ? 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 . . ? 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 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C16 122.1(4) . . ? O3 C15 C20 117.9(4) . . ? C16 C15 C20 120.0(4) . . ? C17 C16 C15 119.6(4) . . ? C17 C16 C23 117.2(4) . . ? C15 C16 C23 123.3(4) . . ? C16 C17 C18 121.2(5) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C19 C18 C17 117.9(4) . . ? C19 C18 C21 121.2(5) . . ? C17 C18 C21 120.9(5) . . ? C18 C19 C20 122.7(4) . . ? C18 C19 H19 118.6 . . ? C20 C19 H19 118.6 . . ? C19 C20 C15 118.5(5) . . ? C19 C20 C22 121.6(4) . . ? C15 C20 C22 119.9(4) . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 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 . . ? N1 C23 C16 113.6(3) . . ? N1 C23 H23A 108.8 . . ? C16 C23 H23A 108.8 . . ? N1 C23 H23B 108.8 . . ? C16 C23 H23B 108.8 . . ? H23A C23 H23B 107.7 . . ? N1 C24 C25 106.8(3) . . ? N1 C24 H24A 110.4 . . ? C25 C24 H24A 110.4 . . ? N1 C24 H24B 110.4 . . ? C25 C24 H24B 110.4 . . ? H24A C24 H24B 108.6 . . ? N2 C25 C24 105.9(3) . . ? N2 C25 H25A 110.6 . . ? C24 C25 H25A 110.6 . . ? N2 C25 H25B 110.6 . . ? C24 C25 H25B 110.6 . . ? H25A C25 H25B 108.7 . . ? N1 C26 C27 104.9(3) . . ? N1 C26 H26A 110.8 . . ? C27 C26 H26A 110.8 . . ? N1 C26 H26B 110.8 . . ? C27 C26 H26B 110.8 . . ? H26A C26 H26B 108.8 . . ? N2 C27 C26 108.0(3) . . ? N2 C27 H27A 110.1 . . ? C26 C27 H27A 110.1 . . ? N2 C27 H27B 110.1 . . ? C26 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? N2 C28 C29 113.7(3) . . ? N2 C28 H28A 108.8 . . ? C29 C28 H28A 108.8 . . ? N2 C28 H28B 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C30 C29 C35 118.6(4) . . ? C30 C29 C28 120.1(4) . . ? C35 C29 C28 121.3(4) . . ? O4 C30 C29 119.5(4) . . ? O4 C30 C31 119.1(4) . . ? C29 C30 C31 121.4(4) . . ? C30 C31 C33 117.8(4) . . ? C30 C31 C36 120.2(4) . . ? C33 C31 C36 121.9(4) . . ? C34 C33 C31 122.5(4) . . ? C34 C33 H33 118.8 . . ? C31 C33 H33 118.8 . . ? C35 C34 C33 117.5(4) . . ? C35 C34 C37 121.5(4) . . ? C33 C34 C37 121.1(4) . . ? C29 C35 C34 122.3(4) . . ? C29 C35 H35 118.9 . . ? C34 C35 H35 118.9 . . ? C31 C36 H36A 109.5 . . ? C31 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C31 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C34 C37 H37A 109.5 . . ? C34 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C34 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O5 C38 C43 124.7(4) . . ? O5 C38 C39 114.3(3) . . ? C43 C38 C39 120.9(4) . . ? O6 C39 C40 126.3(4) . . ? O6 C39 C38 111.9(3) . . ? C40 C39 C38 121.8(3) . . ? C39 C40 C41 115.6(4) . . ? C39 C40 C44 122.3(4) . . ? C41 C40 C44 122.1(4) . . ? C42 C41 C40 124.0(4) . . ? C42 C41 H41 118.0 . . ? C40 C41 H41 118.0 . . ? C43 C42 C41 118.6(4) . . ? C43 C42 C48 119.9(4) . . ? C41 C42 C48 121.5(4) . . ? C42 C43 C38 119.0(4) . . ? C42 C43 H43 120.5 . . ? C38 C43 H43 120.5 . . ? C46 C44 C47 109.2(5) . . ? C46 C44 C45 107.9(5) . . ? C47 C44 C45 107.9(4) . . ? C46 C44 C40 110.3(4) . . ? C47 C44 C40 109.1(4) . . ? C45 C44 C40 112.4(4) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C42 C48 C49 110.7(12) . . ? C42 C48 C51' 112.5(8) . . ? C49 C48 C51' 122.3(15) . . ? C42 C48 C49' 107.7(8) . . ? C49 C48 C49' 23.4(14) . . ? C51' C48 C49' 105.9(12) . . ? C42 C48 C51 108.5(7) . . ? C49 C48 C51 110.7(15) . . ? C51' C48 C51 18.4(13) . . ? C49' C48 C51 90.9(13) . . ? C42 C48 C50' 112.0(8) . . ? C49 C48 C50' 83.1(13) . . ? C51' C48 C50' 112.8(13) . . ? C49' C48 C50' 105.4(12) . . ? C51 C48 C50' 128.5(13) . . ? C42 C48 C50 110.7(7) . . ? C49 C48 C50 112.4(12) . . ? C51' C48 C50 85.6(10) . . ? C49' C48 C50 131.6(10) . . ? C51 C48 C50 103.6(11) . . ? C50' C48 C50 32.0(11) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O7 C52 C57 120.2(4) . . ? O7 C52 C53 119.4(4) . . ? C57 C52 C53 120.3(4) . . ? C54 C53 C52 118.9(4) . . ? C54 C53 C60 121.8(4) . . ? C52 C53 C60 119.2(4) . . ? C53 C54 C55 121.6(5) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C56 C55 C54 118.2(4) . . ? C56 C55 C59 121.2(5) . . ? C54 C55 C59 120.6(5) . . ? C55 C56 C57 122.7(5) . . ? C55 C56 H56 118.7 . . ? C57 C56 H56 118.7 . . ? C56 C57 C52 118.2(4) . . ? C56 C57 C58 122.3(4) . . ? C52 C57 C58 119.5(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C55 C59 H59A 109.5 . . ? C55 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C55 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N3 C60 C53 112.6(3) . . ? N3 C60 H60A 109.1 . . ? C53 C60 H60A 109.1 . . ? N3 C60 H60B 109.1 . . ? C53 C60 H60B 109.1 . . ? H60A C60 H60B 107.8 . . ? N3 C61 C62 106.6(3) . . ? N3 C61 H61A 110.4 . . ? C62 C61 H61A 110.4 . . ? N3 C61 H61B 110.4 . . ? C62 C61 H61B 110.4 . . ? H61A C61 H61B 108.6 . . ? N4 C62 C61 107.0(3) . . ? N4 C62 H62A 110.3 . . ? C61 C62 H62A 110.3 . . ? N4 C62 H62B 110.3 . . ? C61 C62 H62B 110.3 . . ? H62A C62 H62B 108.6 . . ? N3 C63 C64 107.9(3) . . ? N3 C63 H63A 110.1 . . ? C64 C63 H63A 110.1 . . ? N3 C63 H63B 110.1 . . ? C64 C63 H63B 110.1 . . ? H63A C63 H63B 108.4 . . ? N4 C64 C63 106.1(3) . . ? N4 C64 H64A 110.5 . . ? C63 C64 H64A 110.5 . . ? N4 C64 H64B 110.5 . . ? C63 C64 H64B 110.5 . . ? H64A C64 H64B 108.7 . . ? N4 C65 C66 113.9(3) . . ? N4 C65 H65A 108.8 . . ? C66 C65 H65A 108.8 . . ? N4 C65 H65B 108.8 . . ? C66 C65 H65B 108.8 . . ? H65A C65 H65B 107.7 . . ? C71 C66 C67 118.7(4) . . ? C71 C66 C65 117.4(4) . . ? C67 C66 C65 123.8(3) . . ? O8 C67 C68 117.7(4) . . ? O8 C67 C66 122.3(3) . . ? C68 C67 C66 119.9(4) . . ? C69 C68 C67 118.9(4) . . ? C69 C68 C73 121.2(4) . . ? C67 C68 C73 119.7(4) . . ? C70 C69 C68 122.1(4) . . ? C70 C69 H69 118.9 . . ? C68 C69 H69 118.9 . . ? C71 C70 C69 117.7(4) . . ? C71 C70 C72 121.3(4) . . ? C69 C70 C72 121.0(4) . . ? C70 C71 C66 122.6(4) . . ? C70 C71 H71 118.7 . . ? C66 C71 H71 118.7 . . ? C70 C72 H72A 109.5 . . ? C70 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C70 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C68 C73 H73A 109.5 . . ? C68 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C68 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? Cl2 C74 Cl1 119.3(5) . . ? Cl2 C74 H74A 107.5 . . ? Cl1 C74 H74A 107.5 . . ? Cl2 C74 H74B 107.5 . . ? Cl1 C74 H74B 107.5 . . ? H74A C74 H74B 107.0 . . ? Cl3 C75 Cl4 113.6(4) . . ? Cl3 C75 H75A 108.9 . . ? Cl4 C75 H75A 108.9 . . ? Cl3 C75 H75B 108.9 . . ? Cl4 C75 H75B 108.9 . . ? H75A C75 H75B 107.7 . . ? C48 C50' H50D 109.5 . . ? C48 C50' H50E 109.5 . . ? H50D C50' H50E 109.5 . . ? C48 C50' H50F 109.5 . . ? H50D C50' H50F 109.5 . . ? H50E C50' H50F 109.5 . . ? C48 C49' H49D 109.5 . . ? C48 C49' H49E 109.5 . . ? H49D C49' H49E 109.5 . . ? C48 C49' H49F 109.5 . . ? H49D C49' H49F 109.5 . . ? H49E C49' H49F 109.5 . . ? C48 C51' H51D 109.5 . . ? C48 C51' H51E 109.5 . . ? H51D C51' H51E 109.5 . . ? C48 C51' H51F 109.5 . . ? H51D C51' H51F 109.5 . . ? H51E C51' H51F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.155 _refine_diff_density_min -1.307 _refine_diff_density_rms 0.097 _database_code_depnum_ccdc_archive 'CCDC 961390' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_L7Ti(O2Ar2) _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H49 N3 O6 Ti' _chemical_formula_weight 751.75 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' O O 0.0106 0.0060 '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' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.0540(5) _cell_length_b 18.6670(5) _cell_length_c 22.6240(6) _cell_angle_alpha 90.00 _cell_angle_beta 113.361(2) _cell_angle_gamma 90.00 _cell_volume 7775.0(4) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 122826 _cell_measurement_theta_min 3.51 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.284 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3184 _exptl_absorpt_coefficient_mu 0.272 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'nonius kappa ccd' _diffrn_measurement_method ccd _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 153652 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 27.49 _reflns_number_total 17724 _reflns_number_gt 12372 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction 'HKL Denzo & Scalepack (Otwinski & Minor 1997)' _computing_structure_solution ; SIR97- Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C. , Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. (1999) J. Appl. Cryst. 32, 115-119. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0515P)^2^+5.6798P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 17724 _refine_ls_number_parameters 1020 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0830 _refine_ls_R_factor_gt 0.0508 _refine_ls_wR_factor_ref 0.1378 _refine_ls_wR_factor_gt 0.1209 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.717933(19) 1.00655(2) 0.746827(17) 0.02554(9) Uani 1 1 d . . . O1 O 0.64869(8) 0.93345(8) 0.74892(7) 0.0324(3) Uani 1 1 d . . . N1 N 0.78077(9) 0.93014(9) 0.71134(8) 0.0291(4) Uani 1 1 d . . . C1 C 0.58805(12) 0.92646(12) 0.69578(10) 0.0311(5) Uani 1 1 d . C . Ti2 Ti 0.785464(19) 0.450490(19) 0.757864(17) 0.02507(9) Uani 1 1 d . . . O2 O 0.63904(8) 1.01967(8) 0.66206(7) 0.0315(3) Uani 1 1 d . . . N2 N 0.79119(9) 1.06834(9) 0.71016(8) 0.0278(4) Uani 1 1 d . . . C2 C 0.58222(12) 0.97537(12) 0.64675(10) 0.0319(5) Uani 1 1 d . . . O3 O 0.77959(8) 0.96812(8) 0.82464(7) 0.0291(3) Uani 1 1 d . . . N3 N 0.4223(2) 0.8223(3) 0.6129(2) 0.0505(12) Uani 0.50 1 d P A 1 C3 C 0.52127(13) 0.97600(14) 0.58957(12) 0.0427(6) Uani 1 1 d . C . H3 H 0.5167 1.0095 0.5565 0.051 Uiso 1 1 calc R . . O4 O 0.70518(7) 1.09236(8) 0.78228(7) 0.0294(3) Uani 1 1 d . . . N4 N 0.72309(9) 0.52981(9) 0.79040(8) 0.0288(4) Uani 1 1 d . . . C4 C 0.46648(14) 0.92570(16) 0.58188(14) 0.0528(7) Uani 1 1 d . . . O5 O 0.4288(2) 0.7789(2) 0.6554(2) 0.0645(12) Uani 0.50 1 d P A 1 N5 N 0.71036(9) 0.39257(9) 0.79503(8) 0.0273(4) Uani 1 1 d . . . C5 C 0.47352(14) 0.87624(15) 0.62889(14) 0.0496(7) Uani 1 1 d . A . O6 O 0.3696(2) 0.8217(3) 0.5602(2) 0.0714(14) Uani 0.50 1 d P A 1 N6 N 1.0857(2) 0.6317(3) 0.8976(2) 0.0448(11) Uani 0.50 1 d P B 1 C6 C 0.53363(13) 0.87643(13) 0.68709(12) 0.0403(5) Uani 1 1 d . . . H6 H 0.5375 0.8432 0.7201 0.048 Uiso 1 1 calc R C . O7 O 0.72542(8) 0.48754(8) 0.67879(7) 0.0304(3) Uani 1 1 d . . . C7 C 0.76016(11) 1.13585(11) 0.82051(10) 0.0276(4) Uani 1 1 d . . . O8 O 0.79656(8) 0.36280(8) 0.72434(7) 0.0297(3) Uani 1 1 d . . . C8 C 0.76568(12) 1.15465(12) 0.88204(10) 0.0312(5) Uani 1 1 d . . . O9 O 0.86410(8) 0.43800(8) 0.84308(7) 0.0333(3) Uani 1 1 d . . . C9 C 0.82300(12) 1.19948(12) 0.91877(11) 0.0349(5) Uani 1 1 d . . . H9 H 0.8273 1.2130 0.9606 0.042 Uiso 1 1 calc R . . O10 O 0.85601(8) 0.52146(8) 0.75501(7) 0.0338(3) Uani 1 1 d . . . C10 C 0.87385(12) 1.22505(12) 0.89655(11) 0.0347(5) Uani 1 1 d . . . O11 O 1.0813(2) 0.6739(2) 0.8557(2) 0.0573(11) Uani 0.50 1 d P B 1 C11 C 0.86648(12) 1.20556(12) 0.83491(11) 0.0325(5) Uani 1 1 d . . . H11 H 0.9006 1.2227 0.8187 0.039 Uiso 1 1 calc R . . O12 O 1.1361(2) 0.6350(3) 0.9506(2) 0.0643(13) Uani 0.50 1 d P B 1 C12 C 0.80989(11) 1.16125(11) 0.79648(10) 0.0289(4) Uani 1 1 d . . . C13 C 0.70988(14) 1.12942(15) 0.90608(12) 0.0444(6) Uani 1 1 d . . . H13A H 0.6619 1.1470 0.8774 0.067 Uiso 1 1 calc R . . H13B H 0.7219 1.1478 0.9497 0.067 Uiso 1 1 calc R . . H13C H 0.7094 1.0769 0.9068 0.067 Uiso 1 1 calc R . . C14 C 0.93534(14) 1.27280(15) 0.93798(13) 0.0476(6) Uani 1 1 d . . . H14A H 0.9272 1.2877 0.9761 0.071 Uiso 1 1 calc R . . H14B H 0.9375 1.3152 0.9133 0.071 Uiso 1 1 calc R . . H14C H 0.9813 1.2465 0.9515 0.071 Uiso 1 1 calc R . . C15 C 0.79589(12) 1.14631(12) 0.72735(10) 0.0322(5) Uani 1 1 d . . . H15A H 0.7498 1.1698 0.6997 0.039 Uiso 1 1 calc R . . H15B H 0.8353 1.1683 0.7176 0.039 Uiso 1 1 calc R . . C16 C 0.86437(11) 1.03511(12) 0.74155(11) 0.0318(5) Uani 1 1 d . . . H16A H 0.8874 1.0513 0.7869 0.038 Uiso 1 1 calc R . . H16B H 0.8954 1.0507 0.7191 0.038 Uiso 1 1 calc R . . C17 C 0.85862(11) 0.95264(12) 0.73959(11) 0.0316(5) Uani 1 1 d . . . H17A H 0.8838 0.9331 0.7134 0.038 Uiso 1 1 calc R . . H17B H 0.8826 0.9332 0.7838 0.038 Uiso 1 1 calc R . . C18 C 0.76534(13) 1.06577(12) 0.63803(10) 0.0341(5) Uani 1 1 d . . . H18A H 0.7907 1.1035 0.6241 0.041 Uiso 1 1 calc R . . H18B H 0.7127 1.0767 0.6186 0.041 Uiso 1 1 calc R . . C19 C 0.77801(14) 0.99377(13) 0.61254(11) 0.0377(5) Uani 1 1 d . . . H19A H 0.8306 0.9887 0.6227 0.045 Uiso 1 1 calc R . . H19B H 0.7523 0.9937 0.5651 0.045 Uiso 1 1 calc R . . C20 C 0.75305(13) 0.92883(12) 0.63937(10) 0.0341(5) Uani 1 1 d . . . H20A H 0.6993 0.9275 0.6211 0.041 Uiso 1 1 calc R . . H20B H 0.7703 0.8846 0.6257 0.041 Uiso 1 1 calc R . . C21 C 0.77361(12) 0.85595(11) 0.73310(10) 0.0323(5) Uani 1 1 d . . . H21A H 0.7996 0.8225 0.7156 0.039 Uiso 1 1 calc R . . H21B H 0.7216 0.8424 0.7144 0.039 Uiso 1 1 calc R . . C22 C 0.80247(11) 0.84615(11) 0.80521(10) 0.0300(5) Uani 1 1 d . . . C23 C 0.80120(11) 0.90091(11) 0.84711(10) 0.0286(4) Uani 1 1 d . . . C24 C 0.82464(11) 0.88822(12) 0.91361(10) 0.0318(5) Uani 1 1 d . . . C25 C 0.85193(12) 0.82049(12) 0.93681(11) 0.0343(5) Uani 1 1 d . . . H25 H 0.8685 0.8115 0.9817 0.041 Uiso 1 1 calc R . . C26 C 0.85580(12) 0.76577(12) 0.89672(11) 0.0354(5) Uani 1 1 d . . . C27 C 0.83048(12) 0.77942(12) 0.83106(11) 0.0336(5) Uani 1 1 d . . . H27 H 0.8323 0.7423 0.8030 0.040 Uiso 1 1 calc R . . C28 C 0.81862(14) 0.94697(14) 0.95683(11) 0.0400(6) Uani 1 1 d . . . H28A H 0.8398 0.9307 1.0017 0.060 Uiso 1 1 calc R . . H28B H 0.7673 0.9590 0.9449 0.060 Uiso 1 1 calc R . . H28C H 0.8448 0.9894 0.9521 0.060 Uiso 1 1 calc R . . C29 C 0.88589(15) 0.69280(13) 0.92320(13) 0.0476(6) Uani 1 1 d . . . H29A H 0.9213 0.6978 0.9677 0.071 Uiso 1 1 calc R . . H29B H 0.9097 0.6718 0.8969 0.071 Uiso 1 1 calc R . . H29C H 0.8462 0.6615 0.9221 0.071 Uiso 1 1 calc R . . C30 C 0.70513(11) 0.55403(12) 0.65495(10) 0.0308(5) Uani 1 1 d . . . C31 C 0.70372(12) 0.61044(12) 0.69505(11) 0.0325(5) Uani 1 1 d . . . C32 C 0.67595(12) 0.67699(13) 0.66782(12) 0.0397(5) Uani 1 1 d . . . H32 H 0.6739 0.7150 0.6950 0.048 Uiso 1 1 calc R . . C33 C 0.65123(13) 0.68862(14) 0.60183(13) 0.0450(6) Uani 1 1 d . . . C34 C 0.65611(13) 0.63201(15) 0.56352(12) 0.0441(6) Uani 1 1 d . . . H34 H 0.6405 0.6396 0.5185 0.053 Uiso 1 1 calc R . . C35 C 0.68274(12) 0.56503(13) 0.58833(11) 0.0366(5) Uani 1 1 d . . . C36 C 0.61991(17) 0.76021(16) 0.57302(15) 0.0634(8) Uani 1 1 d . . . H36A H 0.5911 0.7797 0.5956 0.095 Uiso 1 1 calc R . . H36B H 0.5888 0.7541 0.5273 0.095 Uiso 1 1 calc R . . H36C H 0.6595 0.7934 0.5775 0.095 Uiso 1 1 calc R . . C37 C 0.68770(14) 0.50443(15) 0.54639(11) 0.0454(6) Uani 1 1 d . . . H37A H 0.6625 0.5178 0.5010 0.068 Uiso 1 1 calc R . . H37B H 0.6650 0.4615 0.5552 0.068 Uiso 1 1 calc R . . H37C H 0.7389 0.4944 0.5557 0.068 Uiso 1 1 calc R . . C38 C 0.73168(12) 0.60298(11) 0.76745(11) 0.0331(5) Uani 1 1 d . . . H38A H 0.7838 0.6158 0.7863 0.040 Uiso 1 1 calc R . . H38B H 0.7057 0.6377 0.7838 0.040 Uiso 1 1 calc R . . C39 C 0.64465(12) 0.50870(12) 0.76180(12) 0.0347(5) Uani 1 1 d . . . H39A H 0.6216 0.5267 0.7171 0.042 Uiso 1 1 calc R . . H39B H 0.6192 0.5304 0.7870 0.042 Uiso 1 1 calc R . . C40 C 0.63768(11) 0.42646(12) 0.76214(11) 0.0322(5) Uani 1 1 d . . . H40A H 0.6061 0.4129 0.7846 0.039 Uiso 1 1 calc R . . H40B H 0.6148 0.4087 0.7173 0.039 Uiso 1 1 calc R . . C41 C 0.74969(14) 0.53350(12) 0.86227(11) 0.0361(5) Uani 1 1 d . . . H41A H 0.7326 0.5787 0.8744 0.043 Uiso 1 1 calc R . . H41B H 0.8035 0.5343 0.8811 0.043 Uiso 1 1 calc R . . C42 C 0.72376(15) 0.47087(13) 0.89035(12) 0.0422(6) Uani 1 1 d . . . H42A H 0.6712 0.4770 0.8797 0.051 Uiso 1 1 calc R . . H42B H 0.7492 0.4724 0.9378 0.051 Uiso 1 1 calc R . . C43 C 0.73559(13) 0.39743(12) 0.86705(10) 0.0351(5) Uani 1 1 d . . . H43A H 0.7880 0.3857 0.8871 0.042 Uiso 1 1 calc R . . H43B H 0.7093 0.3612 0.8816 0.042 Uiso 1 1 calc R . . C44 C 0.70438(12) 0.31402(11) 0.77977(10) 0.0302(5) Uani 1 1 d . . . H44A H 0.7501 0.2902 0.8080 0.036 Uiso 1 1 calc R . . H44B H 0.6646 0.2936 0.7899 0.036 Uiso 1 1 calc R . . C45 C 0.69019(12) 0.29728(11) 0.71109(10) 0.0287(4) Uani 1 1 d . . . C46 C 0.74055(11) 0.32067(11) 0.68658(10) 0.0275(4) Uani 1 1 d . . . C47 C 0.73429(12) 0.30021(12) 0.62518(10) 0.0314(5) Uani 1 1 d . . . C48 C 0.67538(12) 0.25705(12) 0.58877(11) 0.0356(5) Uani 1 1 d . . . H48 H 0.6703 0.2430 0.5468 0.043 Uiso 1 1 calc R . . C49 C 0.62413(12) 0.23391(12) 0.61103(11) 0.0349(5) Uani 1 1 d . . . C50 C 0.63252(12) 0.25436(12) 0.67291(11) 0.0331(5) Uani 1 1 d . . . H50 H 0.5981 0.2386 0.6893 0.040 Uiso 1 1 calc R . . C51 C 0.79123(14) 0.32194(14) 0.60106(12) 0.0431(6) Uani 1 1 d . . . H51A H 0.7813 0.2987 0.5596 0.065 Uiso 1 1 calc R . . H51B H 0.8392 0.3072 0.6322 0.065 Uiso 1 1 calc R . . H51C H 0.7903 0.3741 0.5956 0.065 Uiso 1 1 calc R . . C52 C 0.56184(14) 0.18625(14) 0.57047(13) 0.0459(6) Uani 1 1 d . . . H52A H 0.5541 0.1909 0.5251 0.069 Uiso 1 1 calc R . . H52B H 0.5176 0.2006 0.5760 0.069 Uiso 1 1 calc R . . H52C H 0.5734 0.1363 0.5841 0.069 Uiso 1 1 calc R . . C53 C 0.92126(12) 0.48188(12) 0.85819(11) 0.0353(5) Uani 1 1 d . . . C54 C 0.98169(14) 0.48226(15) 0.91591(14) 0.0506(7) Uani 1 1 d . D . H54 H 0.9860 0.4493 0.9492 0.061 Uiso 1 1 calc R . . C55 C 1.03589(15) 0.53233(18) 0.92362(19) 0.0700(10) Uani 1 1 d . . . C56 C 1.02970(14) 0.58082(17) 0.87615(19) 0.0644(9) Uani 1 1 d . B . C57 C 0.97055(13) 0.57976(14) 0.81680(14) 0.0480(7) Uani 1 1 d . . . H57 H 0.9675 0.6122 0.7834 0.058 Uiso 1 1 calc R D . C58 C 0.91619(12) 0.52955(13) 0.80823(12) 0.0358(5) Uani 1 1 d . D . C100 C 1.01929(16) 0.84422(17) 0.72399(16) 0.0607(8) Uani 1 1 d . . . H10C H 1.0416 0.8186 0.7650 0.091 Uiso 1 1 calc R . . H10D H 1.0079 0.8934 0.7321 0.091 Uiso 1 1 calc R . . H10E H 1.0532 0.8452 0.7025 0.091 Uiso 1 1 calc R . . C101 C 0.95077(14) 0.80669(14) 0.68181(14) 0.0462(6) Uani 1 1 d . . . C102 C 0.92124(18) 0.75127(15) 0.70376(18) 0.0619(8) Uani 1 1 d . . . H102 H 0.9448 0.7361 0.7472 0.074 Uiso 1 1 calc R . . C103 C 0.8578(2) 0.71717(17) 0.6638(3) 0.0807(13) Uani 1 1 d . . . H103 H 0.8381 0.6795 0.6801 0.097 Uiso 1 1 calc R . . C104 C 0.8236(2) 0.7381(2) 0.6007(2) 0.0834(13) Uani 1 1 d . . . H104 H 0.7809 0.7140 0.5730 0.100 Uiso 1 1 calc R . . C105 C 0.85095(16) 0.7934(2) 0.57764(17) 0.0674(9) Uani 1 1 d . . . H105 H 0.8269 0.8083 0.5341 0.081 Uiso 1 1 calc R . . C106 C 0.91412(15) 0.82779(16) 0.61802(14) 0.0508(7) Uani 1 1 d . . . H106 H 0.9326 0.8664 0.6017 0.061 Uiso 1 1 calc R . . C200 C 0.48631(16) 0.61200(17) 0.78202(16) 0.0611(8) Uani 1 1 d . . . H20D H 0.4648 0.6347 0.7395 0.092 Uiso 1 1 calc R . . H20E H 0.4515 0.6135 0.8025 0.092 Uiso 1 1 calc R . . H20C H 0.4983 0.5621 0.7772 0.092 Uiso 1 1 calc R . . C201 C 0.55432(14) 0.65156(14) 0.82321(15) 0.0483(6) Uani 1 1 d . . . C202 C 0.59186(16) 0.63383(17) 0.88762(15) 0.0548(7) Uani 1 1 d . . . H202 H 0.5746 0.5957 0.9055 0.066 Uiso 1 1 calc R . . C203 C 0.65362(17) 0.6703(2) 0.92619(18) 0.0682(9) Uani 1 1 d . . . H203 H 0.6783 0.6572 0.9701 0.082 Uiso 1 1 calc R . . C204 C 0.67936(17) 0.72528(19) 0.9011(2) 0.0716(10) Uani 1 1 d . . . H204 H 0.7214 0.7511 0.9277 0.086 Uiso 1 1 calc R . . C205 C 0.64392(18) 0.74307(16) 0.8370(2) 0.0679(10) Uani 1 1 d . . . H205 H 0.6623 0.7806 0.8193 0.082 Uiso 1 1 calc R . . C206 C 0.58168(17) 0.70658(15) 0.79799(17) 0.0566(7) Uani 1 1 d . . . H206 H 0.5577 0.7193 0.7539 0.068 Uiso 1 1 calc R . . C300 C 0.51559(16) 1.09620(16) 0.89992(16) 0.0600(8) Uani 1 1 d . . . H30A H 0.5456 1.1198 0.8805 0.090 Uiso 1 1 calc R . . H30B H 0.5335 1.1088 0.9457 0.090 Uiso 1 1 calc R . . H30C H 0.4651 1.1120 0.8780 0.090 Uiso 1 1 calc R . . C301 C 0.51967(13) 1.01606(14) 0.89317(12) 0.0422(6) Uani 1 1 d . . . C302 C 0.56220(13) 0.98579(15) 0.86387(12) 0.0425(6) Uani 1 1 d . . . H302 H 0.5880 1.0160 0.8465 0.051 Uiso 1 1 calc R . . C303 C 0.56734(14) 0.91225(15) 0.85978(12) 0.0433(6) Uani 1 1 d . . . H303 H 0.5971 0.8925 0.8401 0.052 Uiso 1 1 calc R . . C304 C 0.52962(14) 0.86719(16) 0.88409(12) 0.0469(6) Uani 1 1 d . . . H304 H 0.5334 0.8167 0.8814 0.056 Uiso 1 1 calc R . . C305 C 0.48603(14) 0.89702(16) 0.91259(12) 0.0479(6) Uani 1 1 d . . . H305 H 0.4592 0.8668 0.9289 0.058 Uiso 1 1 calc R . . C306 C 0.48177(13) 0.97022(16) 0.91710(12) 0.0462(6) Uani 1 1 d . . . H306 H 0.4522 0.9899 0.9371 0.055 Uiso 1 1 calc R . . C400 C 0.97652(16) 0.36477(15) 0.59620(15) 0.0550(7) Uani 1 1 d . . . H40C H 0.9456 0.3415 0.6149 0.082 Uiso 1 1 calc R . . H40D H 1.0266 0.3477 0.6182 0.082 Uiso 1 1 calc R . . H40E H 0.9588 0.3531 0.5503 0.082 Uiso 1 1 calc R . . C401 C 0.97442(13) 0.44484(14) 0.60431(11) 0.0387(5) Uani 1 1 d . . . C402 C 0.93295(13) 0.47607(14) 0.63430(12) 0.0394(5) Uani 1 1 d . . . H402 H 0.9058 0.4465 0.6508 0.047 Uiso 1 1 calc R . . C403 C 0.93086(14) 0.54961(14) 0.64038(12) 0.0419(6) Uani 1 1 d . . . H403 H 0.9020 0.5700 0.6607 0.050 Uiso 1 1 calc R . . C404 C 0.97021(14) 0.59376(14) 0.61727(12) 0.0429(6) Uani 1 1 d . . . H404 H 0.9684 0.6443 0.6214 0.052 Uiso 1 1 calc R . . C405 C 1.01252(14) 0.56348(14) 0.58795(12) 0.0429(6) Uani 1 1 d . . . H405 H 1.0403 0.5933 0.5723 0.051 Uiso 1 1 calc R . . C406 C 1.01422(13) 0.48957(14) 0.58152(11) 0.0400(6) Uani 1 1 d . . . H406 H 1.0431 0.4693 0.5612 0.048 Uiso 1 1 calc R . . N3' N 0.3949(2) 0.9318(3) 0.5310(2) 0.0467(11) Uani 0.50 1 d P C 2 O5' O 0.3849(2) 0.9831(3) 0.49414(19) 0.0665(12) Uani 0.50 1 d P C 2 O6' O 0.3471(2) 0.8849(3) 0.52280(19) 0.0580(11) Uani 0.50 1 d P C 2 N6' N 1.1056(3) 0.5335(3) 0.9685(2) 0.0586(13) Uani 0.50 1 d P D 2 O11' O 1.1208(2) 0.4796(3) 1.0029(2) 0.0766(14) Uani 0.50 1 d P D 2 O12' O 1.1479(2) 0.5874(3) 0.9768(3) 0.0737(15) Uani 0.50 1 d P D 2 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 0.02221(18) 0.02844(19) 0.02698(19) -0.00265(15) 0.01082(15) -0.00009(15) O1 0.0283(8) 0.0370(8) 0.0326(8) -0.0011(6) 0.0127(6) -0.0030(6) N1 0.0270(9) 0.0305(9) 0.0296(9) -0.0038(7) 0.0110(7) 0.0005(7) C1 0.0272(11) 0.0327(11) 0.0343(11) -0.0086(9) 0.0133(9) -0.0004(9) Ti2 0.02234(18) 0.02825(19) 0.02620(19) -0.00291(15) 0.01129(15) -0.00269(15) O2 0.0275(8) 0.0352(8) 0.0301(8) -0.0026(6) 0.0096(6) -0.0026(6) N2 0.0284(9) 0.0287(9) 0.0289(9) -0.0013(7) 0.0142(7) 0.0015(7) C2 0.0275(11) 0.0353(12) 0.0329(11) -0.0086(9) 0.0118(9) 0.0000(9) O3 0.0271(7) 0.0299(8) 0.0295(7) -0.0023(6) 0.0105(6) 0.0012(6) N3 0.034(2) 0.071(3) 0.057(3) -0.037(3) 0.029(2) -0.023(2) C3 0.0378(13) 0.0454(14) 0.0368(13) -0.0082(11) 0.0061(10) -0.0016(11) O4 0.0241(7) 0.0329(8) 0.0326(8) -0.0060(6) 0.0127(6) -0.0016(6) N4 0.0278(9) 0.0286(9) 0.0332(9) -0.0022(7) 0.0155(8) -0.0016(7) C4 0.0331(13) 0.0562(17) 0.0540(16) -0.0196(13) 0.0011(12) -0.0066(12) O5 0.054(2) 0.065(3) 0.089(3) -0.029(2) 0.043(2) -0.036(2) N5 0.0285(9) 0.0285(9) 0.0284(9) -0.0007(7) 0.0150(7) -0.0016(7) C5 0.0393(14) 0.0476(15) 0.0565(16) -0.0184(13) 0.0133(12) -0.0106(12) O6 0.049(2) 0.108(4) 0.067(3) -0.047(3) 0.033(2) -0.042(3) N6 0.025(2) 0.057(3) 0.063(3) -0.033(2) 0.028(2) -0.0205(19) C6 0.0356(13) 0.0423(13) 0.0456(14) -0.0088(11) 0.0189(11) -0.0064(11) O7 0.0300(8) 0.0334(8) 0.0276(7) -0.0021(6) 0.0112(6) -0.0022(6) C7 0.0240(10) 0.0264(10) 0.0304(10) -0.0015(8) 0.0086(8) 0.0009(8) O8 0.0256(7) 0.0319(8) 0.0331(8) -0.0066(6) 0.0133(6) -0.0033(6) C8 0.0313(11) 0.0320(11) 0.0304(11) -0.0008(9) 0.0123(9) -0.0009(9) O9 0.0274(8) 0.0389(9) 0.0321(8) -0.0044(6) 0.0102(6) -0.0033(7) C9 0.0365(12) 0.0369(12) 0.0286(11) -0.0045(9) 0.0100(9) -0.0006(10) O10 0.0285(8) 0.0386(9) 0.0371(8) -0.0060(7) 0.0158(7) -0.0093(7) C10 0.0316(12) 0.0312(11) 0.0357(12) -0.0021(9) 0.0075(9) -0.0014(9) O11 0.041(2) 0.051(2) 0.087(3) -0.025(2) 0.033(2) -0.0285(18) C11 0.0280(11) 0.0294(11) 0.0403(12) 0.0022(9) 0.0139(10) -0.0010(9) O12 0.040(2) 0.092(4) 0.061(3) -0.033(3) 0.020(2) -0.032(3) C12 0.0301(11) 0.0245(10) 0.0321(11) 0.0004(8) 0.0124(9) 0.0023(9) C13 0.0457(14) 0.0542(15) 0.0407(13) -0.0109(11) 0.0249(12) -0.0110(12) C14 0.0413(14) 0.0498(15) 0.0453(14) -0.0078(12) 0.0101(12) -0.0118(12) C15 0.0340(12) 0.0315(11) 0.0342(11) 0.0006(9) 0.0167(10) -0.0016(9) C16 0.0252(10) 0.0373(12) 0.0360(11) -0.0014(9) 0.0153(9) 0.0014(9) C17 0.0243(10) 0.0358(12) 0.0377(12) -0.0026(9) 0.0155(9) 0.0040(9) C18 0.0394(13) 0.0369(12) 0.0302(11) 0.0007(9) 0.0183(10) -0.0012(10) C19 0.0413(13) 0.0455(13) 0.0311(11) -0.0046(10) 0.0194(10) 0.0006(11) C20 0.0387(12) 0.0370(12) 0.0299(11) -0.0073(9) 0.0171(10) 0.0021(10) C21 0.0349(12) 0.0281(11) 0.0346(11) -0.0061(9) 0.0143(10) -0.0003(9) C22 0.0259(10) 0.0314(11) 0.0321(11) -0.0045(9) 0.0109(9) -0.0041(9) C23 0.0230(10) 0.0296(11) 0.0324(11) 0.0009(9) 0.0100(9) -0.0002(8) C24 0.0237(10) 0.0379(12) 0.0339(11) -0.0026(9) 0.0114(9) -0.0021(9) C25 0.0298(11) 0.0390(12) 0.0323(11) 0.0034(9) 0.0102(9) -0.0004(10) C26 0.0282(11) 0.0319(12) 0.0440(13) 0.0013(10) 0.0121(10) -0.0034(9) C27 0.0302(11) 0.0293(11) 0.0412(12) -0.0045(9) 0.0140(10) -0.0022(9) C28 0.0413(13) 0.0476(14) 0.0308(12) -0.0009(10) 0.0142(10) 0.0068(11) C29 0.0511(15) 0.0340(13) 0.0471(14) 0.0025(11) 0.0083(12) 0.0002(11) C30 0.0229(10) 0.0354(12) 0.0334(11) 0.0020(9) 0.0102(9) -0.0045(9) C31 0.0257(11) 0.0313(11) 0.0382(12) 0.0041(9) 0.0103(9) -0.0019(9) C32 0.0297(12) 0.0355(12) 0.0510(14) 0.0052(11) 0.0129(11) -0.0026(10) C33 0.0286(12) 0.0446(14) 0.0561(16) 0.0176(12) 0.0109(11) -0.0015(11) C34 0.0291(12) 0.0592(16) 0.0393(13) 0.0161(12) 0.0084(10) -0.0073(11) C35 0.0256(11) 0.0483(14) 0.0335(12) 0.0047(10) 0.0092(9) -0.0074(10) C36 0.0572(18) 0.0552(18) 0.068(2) 0.0271(15) 0.0145(15) 0.0077(15) C37 0.0399(14) 0.0637(17) 0.0320(12) -0.0001(11) 0.0136(11) -0.0066(12) C38 0.0340(12) 0.0262(11) 0.0395(12) -0.0022(9) 0.0149(10) -0.0017(9) C39 0.0270(11) 0.0339(12) 0.0481(13) -0.0029(10) 0.0200(10) -0.0004(9) C40 0.0251(11) 0.0341(12) 0.0413(12) -0.0030(9) 0.0173(9) -0.0020(9) C41 0.0439(13) 0.0345(12) 0.0353(12) -0.0072(9) 0.0215(10) -0.0007(10) C42 0.0581(16) 0.0414(13) 0.0389(13) -0.0080(11) 0.0318(12) -0.0072(12) C43 0.0432(13) 0.0381(12) 0.0293(11) -0.0028(9) 0.0200(10) -0.0074(10) C44 0.0341(11) 0.0258(10) 0.0360(11) -0.0009(9) 0.0194(10) -0.0022(9) C45 0.0310(11) 0.0248(10) 0.0324(11) -0.0021(8) 0.0147(9) 0.0008(9) C46 0.0251(10) 0.0252(10) 0.0320(11) -0.0035(8) 0.0111(9) 0.0004(8) C47 0.0322(11) 0.0330(11) 0.0307(11) -0.0017(9) 0.0143(9) 0.0008(9) C48 0.0368(12) 0.0375(12) 0.0294(11) -0.0048(9) 0.0099(10) 0.0012(10) C49 0.0307(11) 0.0326(12) 0.0380(12) -0.0048(9) 0.0101(10) -0.0017(9) C50 0.0293(11) 0.0309(11) 0.0407(12) -0.0011(9) 0.0156(10) -0.0019(9) C51 0.0481(14) 0.0502(15) 0.0396(13) -0.0078(11) 0.0266(12) -0.0075(12) C52 0.0373(13) 0.0485(15) 0.0478(14) -0.0130(12) 0.0124(11) -0.0066(11) C53 0.0251(11) 0.0362(12) 0.0425(13) -0.0136(10) 0.0113(10) -0.0005(9) C54 0.0344(13) 0.0490(15) 0.0540(16) -0.0160(12) 0.0022(12) 0.0003(12) C55 0.0289(14) 0.0574(19) 0.099(3) -0.0309(19) -0.0003(15) -0.0008(13) C56 0.0263(13) 0.0522(18) 0.105(3) -0.0380(18) 0.0155(15) -0.0093(12) C57 0.0316(13) 0.0445(14) 0.0728(18) -0.0191(13) 0.0261(13) -0.0080(11) C58 0.0255(11) 0.0382(12) 0.0478(13) -0.0135(10) 0.0188(10) -0.0046(9) C100 0.0476(16) 0.0641(19) 0.071(2) -0.0125(15) 0.0242(15) -0.0066(14) C101 0.0429(14) 0.0420(14) 0.0646(17) -0.0135(12) 0.0330(13) -0.0017(11) C102 0.074(2) 0.0429(16) 0.096(2) -0.0024(15) 0.063(2) 0.0051(15) C103 0.084(3) 0.0405(17) 0.163(4) -0.026(2) 0.097(3) -0.0140(17) C104 0.054(2) 0.080(3) 0.139(4) -0.062(3) 0.063(2) -0.0209(19) C105 0.0451(16) 0.085(2) 0.078(2) -0.0367(18) 0.0304(16) -0.0018(16) C106 0.0443(15) 0.0518(16) 0.0688(18) -0.0137(14) 0.0358(14) -0.0031(12) C200 0.0503(17) 0.0600(19) 0.074(2) -0.0092(15) 0.0262(16) -0.0088(14) C201 0.0410(14) 0.0433(14) 0.0706(18) -0.0108(13) 0.0326(14) -0.0018(12) C202 0.0488(16) 0.0575(17) 0.0698(19) -0.0042(15) 0.0358(15) 0.0030(14) C203 0.0438(16) 0.088(2) 0.078(2) -0.0215(19) 0.0302(16) 0.0050(17) C204 0.0442(17) 0.068(2) 0.111(3) -0.038(2) 0.040(2) -0.0093(16) C205 0.062(2) 0.0447(16) 0.123(3) -0.0166(18) 0.064(2) -0.0066(15) C206 0.0600(18) 0.0444(15) 0.082(2) -0.0031(14) 0.0463(17) 0.0021(14) C300 0.0475(16) 0.0586(18) 0.077(2) -0.0083(16) 0.0282(15) 0.0045(14) C301 0.0282(12) 0.0525(15) 0.0419(13) -0.0054(11) 0.0094(10) 0.0040(11) C302 0.0319(12) 0.0554(16) 0.0396(13) -0.0017(11) 0.0135(10) -0.0006(11) C303 0.0372(13) 0.0544(15) 0.0396(13) -0.0074(12) 0.0166(11) 0.0029(12) C304 0.0431(14) 0.0530(16) 0.0420(14) -0.0034(12) 0.0140(12) -0.0007(12) C305 0.0387(14) 0.0616(17) 0.0445(14) -0.0005(12) 0.0176(12) -0.0061(13) C306 0.0286(12) 0.0699(18) 0.0413(13) -0.0066(12) 0.0150(11) 0.0015(12) C400 0.0508(16) 0.0466(16) 0.074(2) -0.0051(14) 0.0316(15) 0.0036(13) C401 0.0296(12) 0.0483(14) 0.0367(12) -0.0028(10) 0.0116(10) 0.0015(10) C402 0.0343(12) 0.0458(14) 0.0410(13) 0.0015(11) 0.0180(10) -0.0011(11) C403 0.0388(13) 0.0504(15) 0.0392(13) -0.0038(11) 0.0184(11) 0.0038(11) C404 0.0421(14) 0.0430(14) 0.0413(13) -0.0035(11) 0.0141(11) -0.0029(11) C405 0.0383(13) 0.0513(15) 0.0403(13) 0.0003(11) 0.0167(11) -0.0084(11) C406 0.0297(12) 0.0556(15) 0.0351(12) -0.0054(11) 0.0134(10) 0.0000(11) N3' 0.041(2) 0.067(3) 0.035(2) -0.016(2) 0.0177(19) -0.009(2) O5' 0.045(2) 0.103(4) 0.039(2) 0.002(2) 0.0029(17) -0.010(2) O6' 0.034(2) 0.086(3) 0.053(2) -0.032(2) 0.0152(17) -0.021(2) N6' 0.045(3) 0.072(3) 0.046(3) -0.010(3) 0.004(2) -0.005(3) O11' 0.057(3) 0.104(4) 0.049(2) 0.012(3) 0.000(2) -0.009(3) O12' 0.038(2) 0.104(4) 0.065(3) -0.033(3) 0.006(2) -0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O3 1.8484(15) . ? Ti1 O4 1.8541(15) . ? Ti1 O2 1.9583(15) . ? Ti1 O1 1.9607(15) . ? Ti1 N1 2.2515(18) . ? Ti1 N2 2.2679(18) . ? O1 C1 1.335(3) . ? N1 C17 1.494(3) . ? N1 C21 1.496(3) . ? N1 C20 1.498(3) . ? C1 C6 1.390(3) . ? C1 C2 1.405(3) . ? Ti2 O7 1.8494(15) . ? Ti2 O8 1.8543(15) . ? Ti2 O10 1.9579(15) . ? Ti2 O9 1.9614(15) . ? Ti2 N4 2.2426(18) . ? Ti2 N5 2.2690(17) . ? O2 C2 1.338(3) . ? N2 C16 1.489(3) . ? N2 C15 1.500(3) . ? N2 C18 1.504(3) . ? C2 C3 1.383(3) . ? O3 C23 1.359(3) . ? N3 O5 1.224(6) . ? N3 O6 1.240(6) . ? N3 C5 1.380(5) . ? C3 C4 1.403(4) . ? C3 H3 0.9500 . ? O4 C7 1.366(2) . ? N4 C38 1.495(3) . ? N4 C39 1.497(3) . ? N4 C41 1.498(3) . ? C4 C5 1.373(4) . ? C4 N3' 1.446(5) . ? N5 C40 1.489(3) . ? N5 C44 1.500(3) . ? N5 C43 1.505(3) . ? C5 C6 1.389(4) . ? N6 O11 1.207(6) . ? N6 O12 1.226(6) . ? N6 C56 1.402(5) . ? C6 H6 0.9500 . ? O7 C30 1.350(3) . ? C7 C12 1.395(3) . ? C7 C8 1.397(3) . ? O8 C46 1.360(2) . ? C8 C9 1.398(3) . ? C8 C13 1.501(3) . ? O9 C53 1.338(3) . ? C9 C10 1.388(3) . ? C9 H9 0.9500 . ? O10 C58 1.333(3) . ? C10 C11 1.391(3) . ? C10 C14 1.509(3) . ? C11 C12 1.395(3) . ? C11 H11 0.9500 . ? C12 C15 1.501(3) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.543(3) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.523(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.526(3) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.510(3) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C27 1.396(3) . ? C22 C23 1.401(3) . ? C23 C24 1.407(3) . ? C24 C25 1.395(3) . ? C24 C28 1.506(3) . ? C25 C26 1.389(3) . ? C25 H25 0.9500 . ? C26 C27 1.390(3) . ? C26 C29 1.514(3) . ? C27 H27 0.9500 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.398(3) . ? C30 C35 1.407(3) . ? C31 C32 1.400(3) . ? C31 C38 1.513(3) . ? C32 C33 1.391(4) . ? C32 H32 0.9500 . ? C33 C34 1.394(4) . ? C33 C36 1.510(4) . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C37 1.505(4) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.542(3) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.518(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.521(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.497(3) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C50 1.390(3) . ? C45 C46 1.401(3) . ? C46 C47 1.397(3) . ? C47 C48 1.397(3) . ? C47 C51 1.504(3) . ? C48 C49 1.381(3) . ? C48 H48 0.9500 . ? C49 C50 1.396(3) . ? C49 C52 1.512(3) . ? C50 H50 0.9500 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.385(3) . ? C53 C58 1.410(4) . ? C54 C55 1.391(4) . ? C54 H54 0.9500 . ? C55 N6' 1.363(5) . ? C55 C56 1.372(5) . ? C56 C57 1.395(4) . ? C57 C58 1.392(3) . ? C57 H57 0.9500 . ? C100 C101 1.500(4) . ? C100 H10C 0.9800 . ? C100 H10D 0.9800 . ? C100 H10E 0.9800 . ? C101 C102 1.378(4) . ? C101 C106 1.392(4) . ? C102 C103 1.389(5) . ? C102 H102 0.9500 . ? C103 C104 1.373(6) . ? C103 H103 0.9500 . ? C104 C105 1.365(5) . ? C104 H104 0.9500 . ? C105 C106 1.391(4) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C200 C201 1.505(4) . ? C200 H20D 0.9800 . ? C200 H20E 0.9800 . ? C200 H20C 0.9800 . ? C201 C206 1.389(4) . ? C201 C202 1.389(4) . ? C202 C203 1.379(4) . ? C202 H202 0.9500 . ? C203 C204 1.370(5) . ? C203 H203 0.9500 . ? C204 C205 1.379(5) . ? C204 H204 0.9500 . ? C205 C206 1.388(5) . ? C205 H205 0.9500 . ? C206 H206 0.9500 . ? C300 C301 1.509(4) . ? C300 H30A 0.9800 . ? C300 H30B 0.9800 . ? C300 H30C 0.9800 . ? C301 C306 1.389(4) . ? C301 C302 1.391(3) . ? C302 C303 1.383(4) . ? C302 H302 0.9500 . ? C303 C304 1.383(4) . ? C303 H303 0.9500 . ? C304 C305 1.392(4) . ? C304 H304 0.9500 . ? C305 C306 1.375(4) . ? C305 H305 0.9500 . ? C306 H306 0.9500 . ? C400 C401 1.509(4) . ? C400 H40C 0.9800 . ? C400 H40D 0.9800 . ? C400 H40E 0.9800 . ? C401 C406 1.388(4) . ? C401 C402 1.393(3) . ? C402 C403 1.382(4) . ? C402 H402 0.9500 . ? C403 C404 1.380(4) . ? C403 H403 0.9500 . ? C404 C405 1.388(4) . ? C404 H404 0.9500 . ? C405 C406 1.389(4) . ? C405 H405 0.9500 . ? C406 H406 0.9500 . ? N3' O5' 1.233(6) . ? N3' O6' 1.256(6) . ? N6' O11' 1.234(7) . ? N6' O12' 1.281(7) . ? 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 _geom_angle_publ_flag O3 Ti1 O4 94.48(6) . . ? O3 Ti1 O2 163.12(7) . . ? O4 Ti1 O2 96.84(6) . . ? O3 Ti1 O1 85.39(6) . . ? O4 Ti1 O1 111.73(7) . . ? O2 Ti1 O1 78.80(6) . . ? O3 Ti1 N1 80.57(6) . . ? O4 Ti1 N1 153.42(7) . . ? O2 Ti1 N1 94.54(6) . . ? O1 Ti1 N1 93.99(7) . . ? O3 Ti1 N2 105.07(7) . . ? O4 Ti1 N2 86.52(6) . . ? O2 Ti1 N2 88.11(6) . . ? O1 Ti1 N2 158.51(6) . . ? N1 Ti1 N2 69.91(6) . . ? C1 O1 Ti1 116.57(14) . . ? C17 N1 C21 109.87(17) . . ? C17 N1 C20 110.13(17) . . ? C21 N1 C20 107.46(16) . . ? C17 N1 Ti1 107.89(12) . . ? C21 N1 Ti1 109.20(13) . . ? C20 N1 Ti1 112.28(13) . . ? O1 C1 C6 125.2(2) . . ? O1 C1 C2 114.10(19) . . ? C6 C1 C2 120.7(2) . . ? O7 Ti2 O8 94.13(7) . . ? O7 Ti2 O10 85.23(7) . . ? O8 Ti2 O10 112.23(7) . . ? O7 Ti2 O9 163.06(7) . . ? O8 Ti2 O9 96.72(7) . . ? O10 Ti2 O9 78.64(6) . . ? O7 Ti2 N4 80.60(7) . . ? O8 Ti2 N4 152.89(7) . . ? O10 Ti2 N4 93.93(7) . . ? O9 Ti2 N4 95.25(6) . . ? O7 Ti2 N5 105.27(7) . . ? O8 Ti2 N5 86.32(6) . . ? O10 Ti2 N5 158.30(6) . . ? O9 Ti2 N5 88.41(6) . . ? N4 Ti2 N5 69.78(6) . . ? C2 O2 Ti1 116.79(13) . . ? C16 N2 C15 109.38(17) . . ? C16 N2 C18 110.77(17) . . ? C15 N2 C18 105.75(16) . . ? C16 N2 Ti1 105.82(13) . . ? C15 N2 Ti1 112.46(12) . . ? C18 N2 Ti1 112.71(13) . . ? O2 C2 C3 125.7(2) . . ? O2 C2 C1 113.67(19) . . ? C3 C2 C1 120.6(2) . . ? C23 O3 Ti1 135.10(13) . . ? O5 N3 O6 122.2(5) . . ? O5 N3 C5 116.1(4) . . ? O6 N3 C5 121.4(5) . . ? C2 C3 C4 117.9(2) . . ? C2 C3 H3 121.0 . . ? C4 C3 H3 121.0 . . ? C7 O4 Ti1 124.90(13) . . ? C38 N4 C39 109.65(17) . . ? C38 N4 C41 107.11(16) . . ? C39 N4 C41 110.00(17) . . ? C38 N4 Ti2 109.45(13) . . ? C39 N4 Ti2 108.16(13) . . ? C41 N4 Ti2 112.44(13) . . ? C5 C4 C3 121.3(2) . . ? C5 C4 N3' 115.7(3) . . ? C3 C4 N3' 121.9(3) . . ? C40 N5 C44 109.09(16) . . ? C40 N5 C43 110.95(17) . . ? C44 N5 C43 105.66(16) . . ? C40 N5 Ti2 105.92(12) . . ? C44 N5 Ti2 112.63(12) . . ? C43 N5 Ti2 112.64(13) . . ? C4 C5 N3 116.7(3) . . ? C4 C5 C6 121.1(2) . . ? N3 C5 C6 121.8(3) . . ? O11 N6 O12 120.7(5) . . ? O11 N6 C56 111.8(4) . . ? O12 N6 C56 127.5(5) . . ? C5 C6 C1 118.3(2) . . ? C5 C6 H6 120.9 . . ? C1 C6 H6 120.9 . . ? C30 O7 Ti2 135.04(14) . . ? O4 C7 C12 118.52(18) . . ? O4 C7 C8 120.35(19) . . ? C12 C7 C8 121.12(19) . . ? C46 O8 Ti2 124.36(12) . . ? C7 C8 C9 117.7(2) . . ? C7 C8 C13 120.4(2) . . ? C9 C8 C13 121.9(2) . . ? C53 O9 Ti2 116.85(14) . . ? C10 C9 C8 122.6(2) . . ? C10 C9 H9 118.7 . . ? C8 C9 H9 118.7 . . ? C58 O10 Ti2 117.01(14) . . ? C9 C10 C11 118.1(2) . . ? C9 C10 C14 121.0(2) . . ? C11 C10 C14 120.9(2) . . ? C10 C11 C12 121.1(2) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C7 C12 C11 119.3(2) . . ? C7 C12 C15 118.41(19) . . ? C11 C12 C15 122.0(2) . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C10 C14 H14A 109.5 . . ? C10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 C12 114.64(17) . . ? N2 C15 H15A 108.6 . . ? C12 C15 H15A 108.6 . . ? N2 C15 H15B 108.6 . . ? C12 C15 H15B 108.6 . . ? H15A C15 H15B 107.6 . . ? N2 C16 C17 110.71(17) . . ? N2 C16 H16A 109.5 . . ? C17 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? C17 C16 H16B 109.5 . . ? H16A C16 H16B 108.1 . . ? N1 C17 C16 110.26(17) . . ? N1 C17 H17A 109.6 . . ? C16 C17 H17A 109.6 . . ? N1 C17 H17B 109.6 . . ? C16 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N2 C18 C19 113.67(18) . . ? N2 C18 H18A 108.8 . . ? C19 C18 H18A 108.8 . . ? N2 C18 H18B 108.8 . . ? C19 C18 H18B 108.8 . . ? H18A C18 H18B 107.7 . . ? C18 C19 C20 114.84(19) . . ? C18 C19 H19A 108.6 . . ? C20 C19 H19A 108.6 . . ? C18 C19 H19B 108.6 . . ? C20 C19 H19B 108.6 . . ? H19A C19 H19B 107.5 . . ? N1 C20 C19 112.36(18) . . ? N1 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? N1 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.9 . . ? N1 C21 C22 114.96(17) . . ? N1 C21 H21A 108.5 . . ? C22 C21 H21A 108.5 . . ? N1 C21 H21B 108.5 . . ? C22 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C27 C22 C23 118.7(2) . . ? C27 C22 C21 118.61(19) . . ? C23 C22 C21 122.71(19) . . ? O3 C23 C22 120.63(19) . . ? O3 C23 C24 118.51(19) . . ? C22 C23 C24 120.8(2) . . ? C25 C24 C23 118.0(2) . . ? C25 C24 C28 122.4(2) . . ? C23 C24 C28 119.5(2) . . ? C26 C25 C24 122.4(2) . . ? C26 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? C25 C26 C27 118.2(2) . . ? C25 C26 C29 121.3(2) . . ? C27 C26 C29 120.5(2) . . ? C26 C27 C22 121.8(2) . . ? C26 C27 H27 119.1 . . ? C22 C27 H27 119.1 . . ? C24 C28 H28A 109.5 . . ? C24 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C24 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O7 C30 C31 120.91(19) . . ? O7 C30 C35 118.7(2) . . ? C31 C30 C35 120.4(2) . . ? C30 C31 C32 119.3(2) . . ? C30 C31 C38 122.63(19) . . ? C32 C31 C38 118.0(2) . . ? C33 C32 C31 121.4(2) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 117.8(2) . . ? C32 C33 C36 120.8(3) . . ? C34 C33 C36 121.5(3) . . ? C35 C34 C33 122.8(2) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 C35 C30 118.2(2) . . ? C34 C35 C37 122.2(2) . . ? C30 C35 C37 119.5(2) . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 C31 114.58(17) . . ? N4 C38 H38A 108.6 . . ? C31 C38 H38A 108.6 . . ? N4 C38 H38B 108.6 . . ? C31 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? N4 C39 C40 109.97(17) . . ? N4 C39 H39A 109.7 . . ? C40 C39 H39A 109.7 . . ? N4 C39 H39B 109.7 . . ? C40 C39 H39B 109.7 . . ? H39A C39 H39B 108.2 . . ? N5 C40 C39 110.65(17) . . ? N5 C40 H40A 109.5 . . ? C39 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 108.1 . . ? N4 C41 C42 112.65(19) . . ? N4 C41 H41A 109.1 . . ? C42 C41 H41A 109.1 . . ? N4 C41 H41B 109.1 . . ? C42 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C41 C42 C43 115.02(19) . . ? C41 C42 H42A 108.5 . . ? C43 C42 H42A 108.5 . . ? C41 C42 H42B 108.5 . . ? C43 C42 H42B 108.5 . . ? H42A C42 H42B 107.5 . . ? N5 C43 C42 113.45(19) . . ? N5 C43 H43A 108.9 . . ? C42 C43 H43A 108.9 . . ? N5 C43 H43B 108.9 . . ? C42 C43 H43B 108.9 . . ? H43A C43 H43B 107.7 . . ? C45 C44 N5 114.06(17) . . ? C45 C44 H44A 108.7 . . ? N5 C44 H44A 108.7 . . ? C45 C44 H44B 108.7 . . ? N5 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C50 C45 C46 119.1(2) . . ? C50 C45 C44 122.3(2) . . ? C46 C45 C44 118.40(19) . . ? O8 C46 C47 120.59(19) . . ? O8 C46 C45 118.50(18) . . ? C47 C46 C45 120.91(19) . . ? C48 C47 C46 117.7(2) . . ? C48 C47 C51 121.9(2) . . ? C46 C47 C51 120.3(2) . . ? C49 C48 C47 122.9(2) . . ? C49 C48 H48 118.6 . . ? C47 C48 H48 118.6 . . ? C48 C49 C50 118.0(2) . . ? C48 C49 C52 121.2(2) . . ? C50 C49 C52 120.8(2) . . ? C45 C50 C49 121.4(2) . . ? C45 C50 H50 119.3 . . ? C49 C50 H50 119.3 . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? O9 C53 C54 125.8(2) . . ? O9 C53 C58 113.53(19) . . ? C54 C53 C58 120.7(2) . . ? C53 C54 C55 118.0(3) . . ? C53 C54 H54 121.0 . . ? C55 C54 H54 121.0 . . ? N6' C55 C56 108.6(4) . . ? N6' C55 C54 128.6(4) . . ? C56 C55 C54 121.4(3) . . ? C55 C56 C57 121.5(3) . . ? C55 C56 N6 111.4(4) . . ? C57 C56 N6 126.9(4) . . ? C58 C57 C56 117.6(3) . . ? C58 C57 H57 121.2 . . ? C56 C57 H57 121.2 . . ? O10 C58 C57 125.5(2) . . ? O10 C58 C53 113.84(19) . . ? C57 C58 C53 120.6(2) . . ? C101 C100 H10C 109.5 . . ? C101 C100 H10D 109.5 . . ? H10C C100 H10D 109.5 . . ? C101 C100 H10E 109.5 . . ? H10C C100 H10E 109.5 . . ? H10D C100 H10E 109.5 . . ? C102 C101 C106 117.4(3) . . ? C102 C101 C100 122.5(3) . . ? C106 C101 C100 120.1(3) . . ? C101 C102 C103 121.5(4) . . ? C101 C102 H102 119.2 . . ? C103 C102 H102 119.2 . . ? C104 C103 C102 119.8(3) . . ? C104 C103 H103 120.1 . . ? C102 C103 H103 120.1 . . ? C105 C104 C103 120.1(3) . . ? C105 C104 H104 120.0 . . ? C103 C104 H104 120.0 . . ? C104 C105 C106 119.8(4) . . ? C104 C105 H105 120.1 . . ? C106 C105 H105 120.1 . . ? C105 C106 C101 121.3(3) . . ? C105 C106 H106 119.4 . . ? C101 C106 H106 119.4 . . ? C201 C200 H20D 109.5 . . ? C201 C200 H20E 109.5 . . ? H20D C200 H20E 109.5 . . ? C201 C200 H20C 109.5 . . ? H20D C200 H20C 109.5 . . ? H20E C200 H20C 109.5 . . ? C206 C201 C202 118.0(3) . . ? C206 C201 C200 121.1(3) . . ? C202 C201 C200 120.9(3) . . ? C203 C202 C201 121.6(3) . . ? C203 C202 H202 119.2 . . ? C201 C202 H202 119.2 . . ? C204 C203 C202 119.9(4) . . ? C204 C203 H203 120.0 . . ? C202 C203 H203 120.0 . . ? C203 C204 C205 119.7(3) . . ? C203 C204 H204 120.2 . . ? C205 C204 H204 120.2 . . ? C204 C205 C206 120.6(3) . . ? C204 C205 H205 119.7 . . ? C206 C205 H205 119.7 . . ? C205 C206 C201 120.3(3) . . ? C205 C206 H206 119.9 . . ? C201 C206 H206 119.9 . . ? C301 C300 H30A 109.5 . . ? C301 C300 H30B 109.5 . . ? H30A C300 H30B 109.5 . . ? C301 C300 H30C 109.5 . . ? H30A C300 H30C 109.5 . . ? H30B C300 H30C 109.5 . . ? C306 C301 C302 118.0(2) . . ? C306 C301 C300 120.8(2) . . ? C302 C301 C300 121.3(3) . . ? C303 C302 C301 120.8(3) . . ? C303 C302 H302 119.6 . . ? C301 C302 H302 119.6 . . ? C302 C303 C304 120.7(2) . . ? C302 C303 H303 119.7 . . ? C304 C303 H303 119.7 . . ? C303 C304 C305 118.9(3) . . ? C303 C304 H304 120.5 . . ? C305 C304 H304 120.5 . . ? C306 C305 C304 120.1(3) . . ? C306 C305 H305 120.0 . . ? C304 C305 H305 120.0 . . ? C305 C306 C301 121.6(2) . . ? C305 C306 H306 119.2 . . ? C301 C306 H306 119.2 . . ? C401 C400 H40C 109.5 . . ? C401 C400 H40D 109.5 . . ? H40C C400 H40D 109.5 . . ? C401 C400 H40E 109.5 . . ? H40C C400 H40E 109.5 . . ? H40D C400 H40E 109.5 . . ? C406 C401 C402 118.1(2) . . ? C406 C401 C400 120.2(2) . . ? C402 C401 C400 121.7(2) . . ? C403 C402 C401 120.8(2) . . ? C403 C402 H402 119.6 . . ? C401 C402 H402 119.6 . . ? C404 C403 C402 120.7(2) . . ? C404 C403 H403 119.6 . . ? C402 C403 H403 119.6 . . ? C403 C404 C405 119.2(2) . . ? C403 C404 H404 120.4 . . ? C405 C404 H404 120.4 . . ? C404 C405 C406 120.0(2) . . ? C404 C405 H405 120.0 . . ? C406 C405 H405 120.0 . . ? C401 C406 C405 121.1(2) . . ? C401 C406 H406 119.4 . . ? C405 C406 H406 119.4 . . ? O5' N3' O6' 122.2(5) . . ? O5' N3' C4 116.3(4) . . ? O6' N3' C4 121.4(5) . . ? O11' N6' O12' 124.3(5) . . ? O11' N6' C55 112.4(5) . . ? O12' N6' C55 123.1(5) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.354 _refine_diff_density_min -0.447 _refine_diff_density_rms 0.052 #===END _database_code_depnum_ccdc_archive 'CCDC 961391'