Supplementary Material (ESI) for Chemical Communications This journal is (C) The Royal Society of Chemistry 2001 data_global _audit_creation_date 'Tue Sep 4 15:21:34 2001' _audit_creation_method 'by teXsan' _audit_update_record ? _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Hiratani, Kazuhisa' 'Houjou, Hirohiko' 'Rao, Maddali L. N.' #------------------------------------------------------------------------------ # SUBMISSION DETAILS _publ_contact_author_name 'Dr Kazuhisa Hiratani ' _publ_contact_author_address ; National Institute of Advanced Industrial Science and Technology Central 4 1-1-1 Higashi Tsukuba Ibaraki 305-8562 JAPAN ; _publ_contact_author_email 'K-HIRATANI@AIST.GO.JP' _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_contact_letter ; ? ; #------------------------------------------------------------------------------ # TITLE AND AUTHOR LIST _publ_section_title ; Self-assembly of double stranded dinuclear titanium (IV)-Schiff base complexes and formation of intramolecular u-Oxo bridges ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation, Rigaku Corporation. (1999). teXsan. Single Crystal Structure Analysis Software. Version 1.10. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Rigaku, 3-9-12 Akishima, Tokyo, Japan. ; data_complex_3 _database_code_CSD 170678 #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C72 H74 Cl4 N4 O11 Ti2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1409.01 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz x,y,z 1/2-x,1/2+y,1/2-z -x,-y,-z 1/2+x,1/2-y,1/2+z _cell_length_a 13.5241(5) _cell_length_b 21.6644(7) _cell_length_c 23.3745(7) _cell_angle_alpha 90 _cell_angle_beta 97.455(1) _cell_angle_gamma 90 _cell_volume 6790.6(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 53434 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'platelet' _exptl_crystal_colour 'Pale' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.100 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F000 2928 _exptl_absorpt_coefficient_mu 0.456 _exptl_absorpt_correction_type none #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 62324 _diffrn_reflns_av_R_equivalents 0.069 _diffrn_reflns_theta_max 27.48 _diffrn_measured_fraction_theta_max 0.9947 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.9947 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.5 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 15489 _reflns_number_gt 8670 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0686 _refine_ls_wR_factor_ref 0.1366 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 9634 _refine_ls_number_parameters 838 _refine_ls_goodness_of_fit_ref 1.740 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.03000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0007 _refine_diff_density_max ? _refine_diff_density_min ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ti' 'Ti' 0.278 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Cl' 'Cl' 0.148 0.159 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti1 Ti 0.09389(6) 0.52136(4) 0.78293(3) 0.0243(2) Uani 1.00 d . . . Ti2 Ti -0.05551(6) 0.38411(4) 0.76400(3) 0.0246(2) Uani 1.00 d . . . Cl1 Cl 0.3826(1) 0.45206(9) 0.56289(9) 0.0822(6) Uani 1.00 d . . . Cl2 Cl 0.3814(2) 0.3529(1) 0.47997(9) 0.131(1) Uani 1.00 d . . . Cl3 Cl 0.0924(1) 0.18139(9) 0.47127(7) 0.0720(6) Uani 1.00 d . . . Cl4 Cl -0.0967(1) 0.23086(7) 0.49707(7) 0.0578(5) Uani 1.00 d . . . O1 O -0.0021(2) 0.5712(1) 0.7369(1) 0.0280(8) Uani 1.00 d . . . O2 O 0.5855(3) 0.5998(2) 0.8754(2) 0.056(1) Uani 1.00 d . . . O3 O -0.1705(2) 0.4235(1) 0.7211(1) 0.0311(9) Uani 1.00 d . . . O4 O 0.3440(3) 0.2636(2) 0.6339(2) 0.044(1) Uani 1.00 d . . . O5 O 0.0540(2) 0.3296(1) 0.7894(1) 0.0281(8) Uani 1.00 d . . . O6 O -0.4381(3) 0.2635(2) 0.5664(2) 0.050(1) Uani 1.00 d . . . O7 O 0.2150(2) 0.4798(1) 0.8126(1) 0.0277(8) Uani 1.00 d . . . O8 O -0.0321(3) 0.6074(2) 0.4957(1) 0.044(1) Uani 1.00 d . . . O9 O 0.0646(3) 0.5419(2) 0.8527(1) 0.0394(10) Uani 1.00 d . . . O10 O -0.1062(2) 0.3863(1) 0.8313(1) 0.0331(9) Uani 1.00 d . . . O11 O 0.0246(2) 0.4512(1) 0.7651(1) 0.0273(8) Uani 1.00 d . . . N1 N 0.1829(3) 0.6125(2) 0.7826(2) 0.028(1) Uani 1.00 d . . . N2 N -0.0249(3) 0.3588(2) 0.6735(2) 0.028(1) Uani 1.00 d . . . N3 N -0.1332(3) 0.2887(2) 0.7492(2) 0.0254(10) Uani 1.00 d . . . N4 N 0.1732(3) 0.5154(2) 0.7005(2) 0.0257(10) Uani 1.00 d . . . C1 C -0.2457(4) 0.5973(3) 0.7691(2) 0.047(2) Uani 1.00 d . . . C2 C -0.2486(4) 0.5698(2) 0.7191(2) 0.034(1) Uani 1.00 d . . . C3 C -0.1875(3) 0.5902(2) 0.6730(2) 0.033(1) Uani 1.00 d . . . C4 C -0.1151(3) 0.6418(2) 0.6876(2) 0.029(1) Uani 1.00 d . . . C5 C -0.0212(3) 0.6283(2) 0.7194(2) 0.028(1) Uani 1.00 d . . . C6 C 0.0504(3) 0.6754(2) 0.7305(2) 0.029(1) Uani 1.00 d . . . C7 C 0.0265(4) 0.7359(2) 0.7117(2) 0.035(1) Uani 1.00 d . . . C8 C -0.0659(4) 0.7488(2) 0.6817(2) 0.040(2) Uani 1.00 d . . . C9 C -0.1345(4) 0.7018(2) 0.6703(2) 0.035(1) Uani 1.00 d . . . C10 C 0.1502(4) 0.6639(2) 0.7600(2) 0.031(1) Uani 1.00 d . . . C11 C 0.2867(3) 0.6114(2) 0.8073(2) 0.029(1) Uani 1.00 d . . . C12 C 0.3624(4) 0.6304(2) 0.7761(2) 0.036(1) Uani 1.00 d . . . C13 C 0.4612(4) 0.6255(2) 0.7996(2) 0.039(1) Uani 1.00 d . . . C14 C 0.4851(4) 0.6029(2) 0.8555(2) 0.039(2) Uani 1.00 d . . . C15 C 0.4098(4) 0.5844(2) 0.8867(2) 0.035(1) Uani 1.00 d . . . C16 C 0.3119(4) 0.5883(2) 0.8627(2) 0.031(1) Uani 1.00 d . . . C17 C 0.6149(4) 0.5701(3) 0.9285(3) 0.064(2) Uani 1.00 d . . . C18 C -0.3198(4) 0.5155(2) 0.7035(2) 0.042(2) Uani 1.00 d . . . C19 C -0.2931(3) 0.4733(2) 0.6561(2) 0.037(1) Uani 1.00 d . . . C20 C -0.2130(3) 0.4306(2) 0.6675(2) 0.032(1) Uani 1.00 d . . . C21 C -0.1815(4) 0.3984(2) 0.6216(2) 0.032(1) Uani 1.00 d . . . C22 C -0.2334(4) 0.4033(3) 0.5664(2) 0.044(2) Uani 1.00 d . . . C23 C -0.3163(5) 0.4399(3) 0.5565(3) 0.055(2) Uani 1.00 d . . . C24 C -0.3429(4) 0.4762(3) 0.6010(3) 0.047(2) Uani 1.00 d . . . C25 C -0.0867(4) 0.3656(2) 0.6276(2) 0.031(1) Uani 1.00 d . . . C26 C 0.0671(3) 0.3299(2) 0.6647(2) 0.026(1) Uani 1.00 d . . . C27 C 0.0720(4) 0.2781(2) 0.6308(2) 0.032(1) Uani 1.00 d . . . C28 C 0.1624(4) 0.2547(2) 0.6194(2) 0.034(1) Uani 1.00 d . . . C29 C 0.2497(4) 0.2820(2) 0.6427(2) 0.033(1) Uani 1.00 d . . . C30 C 0.2472(3) 0.3325(2) 0.6793(2) 0.032(1) Uani 1.00 d . . . C31 C 0.1569(4) 0.3563(2) 0.6908(2) 0.029(1) Uani 1.00 d . . . C32 C 0.3509(5) 0.2128(3) 0.5958(3) 0.060(2) Uani 1.00 d . . . C33 C 0.1623(4) 0.3792(2) 0.9219(2) 0.045(2) Uani 1.00 d . . . C34 C 0.2371(4) 0.3680(2) 0.8931(2) 0.030(1) Uani 1.00 d . . . C35 C 0.2415(3) 0.3128(2) 0.8548(2) 0.031(1) Uani 1.00 d . . . C36 C 0.1577(3) 0.2668(2) 0.8539(2) 0.029(1) Uani 1.00 d . . . C37 C 0.0646(3) 0.2783(2) 0.8194(2) 0.024(1) Uani 1.00 d . . . C38 C -0.0112(3) 0.2341(2) 0.8171(2) 0.026(1) Uani 1.00 d . . . C39 C 0.0035(4) 0.1798(2) 0.8501(2) 0.035(1) Uani 1.00 d . . . C40 C 0.0919(4) 0.1698(2) 0.8848(2) 0.038(1) Uani 1.00 d . . . C41 C 0.1683(4) 0.2134(2) 0.8859(2) 0.035(1) Uani 1.00 d . . . C42 C -0.1025(3) 0.2398(2) 0.7774(2) 0.028(1) Uani 1.00 d . . . C43 C -0.2140(3) 0.2782(2) 0.7042(2) 0.030(1) Uani 1.00 d . . . C44 C -0.3052(4) 0.3081(2) 0.7039(2) 0.032(1) Uani 1.00 d . . . C45 C -0.3790(4) 0.3001(3) 0.6587(2) 0.038(1) Uani 1.00 d . . . C46 C -0.3628(4) 0.2643(2) 0.6113(2) 0.036(1) Uani 1.00 d . . . C47 C -0.2735(4) 0.2331(2) 0.6119(2) 0.035(1) Uani 1.00 d . . . C48 C -0.2000(4) 0.2397(2) 0.6588(2) 0.033(1) Uani 1.00 d . . . C49 C -0.4220(5) 0.2316(3) 0.5161(2) 0.059(2) Uani 1.00 d . . . C50 C 0.3279(4) 0.4098(2) 0.8970(2) 0.035(1) Uani 1.00 d . . . C51 C 0.3639(4) 0.4255(2) 0.8405(2) 0.032(1) Uani 1.00 d . . . C52 C 0.3009(3) 0.4603(2) 0.7994(2) 0.028(1) Uani 1.00 d . . . C53 C 0.3319(3) 0.4730(2) 0.7451(2) 0.029(1) Uani 1.00 d . . . C54 C 0.4274(4) 0.4541(2) 0.7343(2) 0.037(1) Uani 1.00 d . . . C55 C 0.4891(4) 0.4219(2) 0.7750(2) 0.041(2) Uani 1.00 d . . . C56 C 0.4568(4) 0.4079(2) 0.8275(2) 0.037(1) Uani 1.00 d . . . C57 C 0.2656(4) 0.5011(2) 0.6989(2) 0.029(1) Uani 1.00 d . . . C58 C 0.1202(3) 0.5382(2) 0.6473(2) 0.027(1) Uani 1.00 d . . . C59 C 0.1577(4) 0.5868(2) 0.6178(2) 0.033(1) Uani 1.00 d . . . C60 C 0.1053(4) 0.6084(2) 0.5671(2) 0.037(1) Uani 1.00 d . . . C61 C 0.0137(4) 0.5820(2) 0.5459(2) 0.033(1) Uani 1.00 d . . . C62 C -0.0244(3) 0.5341(2) 0.5753(2) 0.030(1) Uani 1.00 d . . . C63 C 0.0289(3) 0.5130(2) 0.6268(2) 0.030(1) Uani 1.00 d . . . C64 C -0.1315(4) 0.5866(3) 0.4756(2) 0.047(2) Uani 1.00 d . . . C65 C 0.0176(4) 0.5323(2) 0.9017(2) 0.044(2) Uani 1.00 d . . . C66 C -0.0790(5) 0.5662(4) 0.8959(3) 0.081(3) Uani 1.00 d . . . C67 C 0.0871(5) 0.5512(3) 0.9548(2) 0.063(2) Uani 1.00 d . . . C68 C -0.1844(4) 0.3679(3) 0.8625(2) 0.051(2) Uani 1.00 d . . . C69 C -0.2457(5) 0.4222(3) 0.8738(3) 0.065(2) Uani 1.00 d . . . C70 C -0.1456(5) 0.3315(3) 0.9132(3) 0.061(2) Uani 1.00 d . . . C71 C 0.4216(5) 0.3768(3) 0.5500(3) 0.074(2) Uani 1.00 d . . . C72 C 0.0160(5) 0.2465(3) 0.4694(3) 0.062(2) Uani 1.00 d . . . H1 H -0.2874 0.5839 0.7963 0.0553 Uiso 1.00 calc . . . H2 H -0.2013 0.6313 0.7785 0.0553 Uiso 1.00 calc . . . H3 H -0.2410 0.5942 0.6408 0.0380 Uiso 1.00 calc . . . H4 H -0.1502 0.5580 0.6584 0.0380 Uiso 1.00 calc . . . H5 H 0.0739 0.7686 0.7197 0.0380 Uiso 1.00 calc . . . H6 H -0.0855 0.7924 0.6772 0.0380 Uiso 1.00 calc . . . H7 H -0.2008 0.7062 0.6460 0.0380 Uiso 1.00 calc . . . H8 H 0.1955 0.6977 0.7628 0.0367 Uiso 1.00 calc . . . H9 H 0.3462 0.6467 0.7382 0.0436 Uiso 1.00 calc . . . H10 H 0.5157 0.6223 0.7756 0.0380 Uiso 1.00 calc . . . H11 H 0.4236 0.5596 0.9212 0.0380 Uiso 1.00 calc . . . H12 H 0.2609 0.5753 0.8843 0.0360 Uiso 1.00 calc . . . H13 H 0.5891 0.5922 0.9583 0.0770 Uiso 1.00 calc . . . H14 H 0.6858 0.5695 0.9358 0.0770 Uiso 1.00 calc . . . H15 H 0.5903 0.5292 0.9267 0.0770 Uiso 1.00 calc . . . H16 H -0.3845 0.5316 0.6918 0.0508 Uiso 1.00 calc . . . H17 H -0.3209 0.4911 0.7373 0.0508 Uiso 1.00 calc . . . H18 H -0.2111 0.3812 0.5354 0.0516 Uiso 1.00 calc . . . H19 H -0.3504 0.4482 0.5187 0.0380 Uiso 1.00 calc . . . H20 H -0.4009 0.5020 0.5888 0.0380 Uiso 1.00 calc . . . H21 H -0.0687 0.3470 0.5935 0.0371 Uiso 1.00 calc . . . H22 H 0.0164 0.2617 0.6044 0.0380 Uiso 1.00 calc . . . H23 H 0.1641 0.2194 0.5954 0.0405 Uiso 1.00 calc . . . H24 H 0.3058 0.3562 0.6943 0.0380 Uiso 1.00 calc . . . H25 H 0.1554 0.3905 0.7162 0.0350 Uiso 1.00 calc . . . H26 H 0.3211 0.1774 0.6104 0.0721 Uiso 1.00 calc . . . H27 H 0.3170 0.2226 0.5587 0.0721 Uiso 1.00 calc . . . H28 H 0.4190 0.2045 0.5928 0.0721 Uiso 1.00 calc . . . H29 H 0.1634 0.4143 0.9464 0.0531 Uiso 1.00 calc . . . H30 H 0.1064 0.3521 0.9186 0.0531 Uiso 1.00 calc . . . H31 H 0.3024 0.2894 0.8632 0.0380 Uiso 1.00 calc . . . H32 H 0.2422 0.3290 0.8165 0.0380 Uiso 1.00 calc . . . H33 H -0.0462 0.1465 0.8490 0.0380 Uiso 1.00 calc . . . H34 H 0.1057 0.1337 0.9110 0.0380 Uiso 1.00 calc . . . H35 H 0.2301 0.1967 0.9059 0.0380 Uiso 1.00 calc . . . H36 H -0.1295 0.1982 0.7731 0.0380 Uiso 1.00 calc . . . H37 H -0.3137 0.3357 0.7351 0.0380 Uiso 1.00 calc . . . H38 H -0.4420 0.3189 0.6597 0.0446 Uiso 1.00 calc . . . H39 H -0.2730 0.2023 0.5815 0.0380 Uiso 1.00 calc . . . H40 H -0.1352 0.2226 0.6561 0.0380 Uiso 1.00 calc . . . H41 H -0.3661 0.2496 0.5011 0.0700 Uiso 1.00 calc . . . H42 H -0.4793 0.2353 0.4885 0.0700 Uiso 1.00 calc . . . H43 H -0.4085 0.1898 0.5250 0.0700 Uiso 1.00 calc . . . H44 H 0.3826 0.3882 0.9187 0.0380 Uiso 1.00 calc . . . H45 H 0.3108 0.4463 0.9177 0.0380 Uiso 1.00 calc . . . H46 H 0.4436 0.4599 0.6946 0.0380 Uiso 1.00 calc . . . H47 H 0.5535 0.4091 0.7672 0.0488 Uiso 1.00 calc . . . H48 H 0.4970 0.3877 0.8586 0.0380 Uiso 1.00 calc . . . H49 H 0.2963 0.5018 0.6642 0.0380 Uiso 1.00 calc . . . H50 H 0.2191 0.6093 0.6301 0.0380 Uiso 1.00 calc . . . H51 H 0.1355 0.6389 0.5444 0.0380 Uiso 1.00 calc . . . H52 H -0.0927 0.5213 0.5594 0.0380 Uiso 1.00 calc . . . H53 H 0.0017 0.4809 0.6479 0.0349 Uiso 1.00 calc . . . H54 H -0.1261 0.5430 0.4702 0.0380 Uiso 1.00 calc . . . H55 H -0.1622 0.5977 0.5085 0.0380 Uiso 1.00 calc . . . H56 H -0.1608 0.6131 0.4455 0.0380 Uiso 1.00 calc . . . H57 H 0.0040 0.4894 0.9045 0.0526 Uiso 1.00 calc . . . H58 H -0.1200 0.5527 0.8623 0.0964 Uiso 1.00 calc . . . H59 H -0.0668 0.6092 0.8933 0.0964 Uiso 1.00 calc . . . H60 H -0.1115 0.5583 0.9289 0.0964 Uiso 1.00 calc . . . H61 H 0.1460 0.5270 0.9575 0.0751 Uiso 1.00 calc . . . H62 H 0.1035 0.5936 0.9519 0.0751 Uiso 1.00 calc . . . H63 H 0.0549 0.5448 0.9881 0.0751 Uiso 1.00 calc . . . H64 H -0.2218 0.3403 0.8350 0.0380 Uiso 1.00 calc . . . H65 H -0.2495 0.4495 0.8421 0.0777 Uiso 1.00 calc . . . H66 H -0.2151 0.4428 0.9077 0.0777 Uiso 1.00 calc . . . H67 H -0.3102 0.4088 0.8797 0.0777 Uiso 1.00 calc . . . H68 H -0.1233 0.2926 0.9014 0.0732 Uiso 1.00 calc . . . H69 H -0.0911 0.3528 0.9346 0.0732 Uiso 1.00 calc . . . H70 H -0.1967 0.3257 0.9370 0.0732 Uiso 1.00 calc . . . H71 H 0.4923 0.3754 0.5562 0.0882 Uiso 1.00 calc . . . H72 H 0.3953 0.3495 0.5759 0.0882 Uiso 1.00 calc . . . H73 H 0.0507 0.2782 0.4919 0.0729 Uiso 1.00 calc . . . H74 H 0.0012 0.2600 0.4306 0.0729 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti1 0.0247(4) 0.0222(4) 0.0259(4) -0.0001(4) 0.0030(3) 0.0002(4) Ti2 0.0231(4) 0.0226(4) 0.0276(4) -0.0015(4) 0.0010(3) 0.0026(4) Cl1 0.068(1) 0.081(1) 0.093(1) 0.006(1) -0.003(1) 0.006(1) Cl2 0.156(2) 0.166(3) 0.068(1) 0.089(2) 0.007(1) -0.019(2) Cl3 0.071(1) 0.079(1) 0.063(1) 0.0181(10) -0.0029(9) -0.0167(10) Cl4 0.0565(10) 0.0582(9) 0.0572(9) -0.0066(8) 0.0013(7) -0.0044(8) O1 0.023(2) 0.021(2) 0.038(2) 0.001(1) 0.000(1) 0.003(1) O2 0.026(2) 0.076(3) 0.063(3) -0.005(2) -0.004(2) 0.009(2) O3 0.026(2) 0.030(2) 0.036(2) 0.004(1) -0.002(1) 0.001(2) O4 0.037(2) 0.035(2) 0.061(2) 0.002(2) 0.017(2) -0.003(2) O5 0.023(2) 0.025(2) 0.034(2) 0.001(1) -0.001(1) 0.006(1) O6 0.037(2) 0.068(3) 0.041(2) -0.003(2) -0.008(2) -0.012(2) O7 0.021(2) 0.028(2) 0.033(2) 0.001(1) -0.001(1) 0.003(2) O8 0.043(2) 0.053(2) 0.032(2) -0.009(2) -0.007(2) 0.015(2) O9 0.041(2) 0.050(2) 0.029(2) -0.002(2) 0.008(2) -0.003(2) O10 0.032(2) 0.035(2) 0.032(2) -0.004(2) 0.005(1) 0.001(2) O11 0.023(2) 0.023(1) 0.035(2) 0.000(1) -0.001(1) 0.004(1) N1 0.023(2) 0.030(2) 0.031(2) -0.003(2) -0.001(2) -0.003(2) N2 0.029(2) 0.024(2) 0.029(2) -0.004(2) -0.002(2) 0.002(2) N3 0.021(2) 0.027(2) 0.028(2) -0.002(2) 0.003(2) 0.003(2) N4 0.024(2) 0.023(2) 0.030(2) -0.003(2) 0.003(2) 0.002(2) C1 0.044(3) 0.049(3) 0.051(3) -0.001(3) 0.018(3) 0.002(3) C2 0.025(3) 0.028(3) 0.049(3) 0.008(2) 0.007(2) 0.010(2) C3 0.022(3) 0.039(3) 0.036(3) -0.001(2) 0.000(2) 0.003(2) C4 0.025(3) 0.029(2) 0.032(2) 0.001(2) 0.002(2) 0.002(2) C5 0.033(3) 0.023(2) 0.030(2) 0.004(2) 0.007(2) 0.003(2) C6 0.030(3) 0.024(2) 0.033(3) 0.001(2) 0.005(2) 0.001(2) C7 0.040(3) 0.023(2) 0.044(3) -0.002(2) 0.011(2) 0.001(2) C8 0.042(3) 0.024(3) 0.051(3) 0.007(2) 0.003(3) 0.005(2) C9 0.034(3) 0.034(3) 0.037(3) 0.004(2) 0.004(2) 0.007(2) C10 0.031(3) 0.023(2) 0.037(3) -0.006(2) 0.003(2) -0.004(2) C11 0.027(3) 0.025(2) 0.034(3) -0.001(2) 0.003(2) -0.003(2) C12 0.038(3) 0.034(3) 0.037(3) -0.008(2) 0.004(2) 0.000(2) C13 0.033(3) 0.044(3) 0.041(3) -0.007(2) 0.005(2) -0.001(3) C14 0.029(3) 0.037(3) 0.049(3) -0.004(2) -0.003(2) -0.001(3) C15 0.038(3) 0.030(3) 0.034(3) -0.002(2) -0.003(2) 0.003(2) C16 0.032(3) 0.026(2) 0.035(3) -0.003(2) 0.004(2) -0.002(2) C17 0.039(4) 0.080(5) 0.070(4) 0.001(3) -0.007(3) 0.012(4) C18 0.025(3) 0.038(3) 0.065(4) 0.004(2) 0.007(3) 0.013(3) C19 0.023(3) 0.031(3) 0.055(3) -0.001(2) -0.001(2) 0.013(3) C20 0.024(3) 0.032(3) 0.037(3) -0.009(2) -0.005(2) 0.012(2) C21 0.029(3) 0.032(3) 0.033(3) -0.006(2) -0.003(2) 0.004(2) C22 0.048(3) 0.048(3) 0.033(3) 0.001(3) -0.007(3) 0.005(3) C23 0.052(4) 0.059(4) 0.048(3) -0.003(3) -0.020(3) 0.016(3) C24 0.029(3) 0.045(3) 0.063(4) 0.000(3) -0.013(3) 0.017(3) C25 0.036(3) 0.028(2) 0.030(3) -0.005(2) 0.003(2) 0.001(2) C26 0.025(3) 0.029(2) 0.024(2) -0.001(2) 0.000(2) 0.004(2) C27 0.038(3) 0.030(3) 0.027(2) -0.005(2) 0.001(2) -0.002(2) C28 0.043(3) 0.029(3) 0.030(3) -0.003(2) 0.007(2) -0.009(2) C29 0.037(3) 0.028(2) 0.037(3) 0.001(2) 0.014(2) 0.004(2) C30 0.027(3) 0.026(2) 0.041(3) -0.003(2) 0.004(2) -0.003(2) C31 0.033(3) 0.023(2) 0.032(3) -0.002(2) 0.002(2) 0.000(2) C32 0.061(4) 0.040(3) 0.090(5) -0.001(3) 0.046(4) -0.018(3) C33 0.051(4) 0.031(3) 0.053(3) -0.004(3) 0.007(3) -0.007(3) C34 0.033(3) 0.025(2) 0.029(3) 0.001(2) -0.002(2) 0.005(2) C35 0.024(3) 0.030(2) 0.037(3) 0.002(2) 0.000(2) 0.004(2) C36 0.032(3) 0.027(2) 0.027(2) 0.004(2) 0.004(2) 0.002(2) C37 0.024(2) 0.023(2) 0.024(2) 0.004(2) 0.002(2) 0.001(2) C38 0.031(3) 0.023(2) 0.026(2) 0.004(2) 0.005(2) 0.002(2) C39 0.038(3) 0.027(2) 0.040(3) -0.002(2) 0.003(2) 0.002(2) C40 0.046(3) 0.027(3) 0.039(3) 0.005(2) 0.001(3) 0.008(2) C41 0.035(3) 0.031(3) 0.039(3) 0.011(2) -0.001(2) 0.001(2) C42 0.028(3) 0.022(2) 0.036(3) -0.004(2) 0.008(2) 0.000(2) C43 0.029(3) 0.027(2) 0.033(3) -0.007(2) 0.003(2) 0.005(2) C44 0.027(3) 0.034(3) 0.035(3) -0.001(2) 0.004(2) -0.003(2) C45 0.023(3) 0.051(3) 0.039(3) 0.001(2) 0.001(2) -0.003(3) C46 0.034(3) 0.037(3) 0.033(3) -0.011(2) -0.004(2) 0.004(2) C47 0.040(3) 0.031(3) 0.032(3) -0.001(2) 0.002(2) -0.004(2) C48 0.031(3) 0.031(3) 0.037(3) -0.001(2) 0.006(2) 0.001(2) C49 0.063(4) 0.073(4) 0.038(3) -0.007(4) -0.004(3) -0.006(3) C50 0.033(3) 0.028(2) 0.041(3) 0.004(2) -0.009(2) 0.000(2) C51 0.026(3) 0.026(2) 0.041(3) -0.003(2) -0.005(2) 0.005(2) C52 0.022(2) 0.022(2) 0.037(3) -0.004(2) -0.003(2) -0.001(2) C53 0.022(2) 0.025(2) 0.039(3) -0.001(2) 0.002(2) 0.002(2) C54 0.028(3) 0.037(3) 0.046(3) -0.006(2) 0.008(2) 0.000(3) C55 0.023(3) 0.038(3) 0.062(4) 0.008(2) 0.006(3) 0.004(3) C56 0.028(3) 0.032(3) 0.047(3) 0.003(2) -0.006(2) 0.006(2) C57 0.034(3) 0.026(2) 0.029(2) -0.005(2) 0.008(2) 0.001(2) C58 0.028(3) 0.028(2) 0.024(2) 0.001(2) 0.004(2) 0.000(2) C59 0.030(3) 0.033(3) 0.034(3) -0.009(2) -0.001(2) 0.004(2) C60 0.042(3) 0.040(3) 0.028(3) -0.008(2) 0.006(2) 0.011(2) C61 0.037(3) 0.036(3) 0.026(2) 0.001(2) 0.003(2) 0.002(2) C62 0.030(3) 0.032(3) 0.027(2) -0.001(2) 0.001(2) -0.003(2) C63 0.031(3) 0.028(3) 0.030(2) -0.003(2) 0.005(2) 0.003(2) C64 0.044(3) 0.055(3) 0.039(3) 0.008(3) -0.008(3) 0.006(3) C65 0.054(4) 0.042(3) 0.037(3) -0.006(3) 0.009(3) 0.000(3) C66 0.048(4) 0.103(6) 0.095(5) 0.013(4) 0.025(4) 0.001(5) C67 0.089(5) 0.062(4) 0.039(3) -0.026(4) 0.009(3) -0.003(3) C68 0.050(4) 0.059(4) 0.047(3) 0.001(3) 0.022(3) 0.006(3) C69 0.052(4) 0.070(4) 0.080(5) 0.018(4) 0.033(4) 0.018(4) C70 0.069(4) 0.065(4) 0.054(4) 0.010(4) 0.023(3) 0.018(3) C71 0.072(5) 0.076(5) 0.075(5) 0.017(4) 0.009(4) 0.024(4) C72 0.069(4) 0.061(4) 0.056(4) 0.005(4) 0.013(3) -0.002(3) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI1 O1 1.909(3) . . yes TI1 O7 1.918(3) . . yes TI1 O9 1.784(3) . . yes TI1 O11 1.806(3) . . yes TI1 N1 2.313(4) . . yes TI1 N4 2.326(4) . . yes TI2 O3 1.935(3) . . yes TI2 O5 1.927(3) . . yes TI2 O10 1.795(3) . . yes TI2 O11 1.811(3) . . yes TI2 N2 2.274(4) . . yes TI2 N3 2.324(4) . . yes CL1 C71 1.752(8) . . yes CL2 C71 1.734(8) . . yes CL3 C72 1.745(7) . . yes CL4 C72 1.764(7) . . yes O1 C5 1.318(5) . . yes O2 C14 1.379(6) . . yes O2 C17 1.408(7) . . yes O3 C20 1.318(5) . . yes O4 C29 1.377(6) . . yes O4 C32 1.425(6) . . yes O5 C37 1.313(5) . . yes O6 C46 1.364(6) . . yes O6 C49 1.407(7) . . yes O7 C52 1.309(5) . . yes O8 C61 1.368(6) . . yes O8 C64 1.439(6) . . yes O9 C65 1.395(6) . . yes O10 C68 1.418(6) . . yes N1 C10 1.286(6) . . yes N1 C11 1.446(6) . . yes N2 C25 1.280(6) . . yes N2 C26 1.432(6) . . yes N3 C42 1.288(6) . . yes N3 C43 1.433(6) . . yes N4 C57 1.294(6) . . yes N4 C58 1.439(6) . . yes C1 C2 1.308(7) . . yes C2 C3 1.506(7) . . yes C2 C18 1.534(7) . . yes C3 C4 1.496(6) . . yes C4 C5 1.416(6) . . yes C4 C9 1.378(6) . . yes C5 C6 1.407(6) . . yes C6 C7 1.406(6) . . yes C6 C10 1.455(6) . . yes C7 C8 1.381(7) . . yes C8 C9 1.378(7) . . yes C11 C12 1.395(6) . . yes C11 C16 1.389(6) . . yes C12 C13 1.381(7) . . yes C13 C14 1.393(7) . . yes C14 C15 1.387(7) . . yes C15 C16 1.373(6) . . yes C18 C19 1.515(8) . . yes C19 C20 1.424(6) . . yes C19 C24 1.374(7) . . yes C20 C21 1.393(7) . . yes C21 C22 1.391(7) . . yes C21 C25 1.456(7) . . yes C22 C23 1.368(8) . . yes C23 C24 1.388(8) . . yes C26 C27 1.380(6) . . yes C26 C31 1.409(6) . . yes C27 C28 1.380(7) . . yes C28 C29 1.371(7) . . yes C29 C30 1.392(7) . . yes C30 C31 1.384(6) . . yes C33 C34 1.308(7) . . yes C34 C35 1.501(7) . . yes C34 C50 1.518(7) . . yes C35 C36 1.507(6) . . yes C36 C37 1.426(6) . . yes C36 C41 1.376(6) . . yes C37 C38 1.399(6) . . yes C38 C39 1.406(6) . . yes C38 C42 1.451(6) . . yes C39 C40 1.372(7) . . yes C40 C41 1.398(7) . . yes C43 C44 1.394(6) . . yes C43 C48 1.382(6) . . yes C44 C45 1.366(6) . . yes C45 C46 1.394(7) . . yes C46 C47 1.383(7) . . yes C47 C48 1.388(6) . . yes C50 C51 1.505(7) . . yes C51 C52 1.417(6) . . yes C51 C56 1.385(7) . . yes C52 C53 1.414(6) . . yes C53 C54 1.408(6) . . yes C53 C57 1.445(6) . . yes C54 C55 1.372(7) . . yes C55 C56 1.387(7) . . yes C58 C59 1.391(6) . . yes C58 C63 1.379(6) . . yes C59 C60 1.381(7) . . yes C60 C61 1.396(7) . . yes C61 C62 1.382(6) . . yes C62 C63 1.396(6) . . yes C65 C66 1.490(8) . . yes C65 C67 1.513(8) . . yes C68 C69 1.482(8) . . yes C68 C70 1.463(8) . . yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O9 TI1 O11 104.5(1) . 1_555 1_555 yes O10 TI2 O11 105.2(1) . 1_555 1_555 yes C14 O2 C17 118.3(4) . 1_555 1_555 yes C29 O4 C32 117.0(4) . 1_555 1_555 yes C46 O6 C49 117.9(4) . 1_555 1_555 yes C61 O8 C64 117.0(4) . 1_555 1_555 yes TI1 O9 C65 153.2(3) . 1_555 1_555 yes TI2 O10 C68 147.0(3) . 1_555 1_555 yes TI1 O11 TI2 166.0(2) . 1_555 1_555 yes C10 N1 C11 116.3(4) . 1_555 1_555 yes C25 N2 C26 114.4(4) . 1_555 1_555 yes C42 N3 C43 114.1(4) . 1_555 1_555 yes C57 N4 C58 115.6(4) . 1_555 1_555 yes C1 C2 C3 123.3(5) . 1_555 1_555 yes C1 C2 C18 120.5(5) . 1_555 1_555 yes C3 C2 C18 116.1(4) . 1_555 1_555 yes C2 C3 C4 117.4(4) . 1_555 1_555 yes C3 C4 C5 118.8(4) . 1_555 1_555 yes C3 C4 C9 123.0(4) . 1_555 1_555 yes C5 C4 C9 118.2(4) . 1_555 1_555 yes O1 C5 C4 118.8(4) . 1_555 1_555 yes O1 C5 C6 121.4(4) . 1_555 1_555 yes C4 C5 C6 119.7(4) . 1_555 1_555 yes C5 C6 C7 119.6(4) . 1_555 1_555 yes C5 C6 C10 122.4(4) . 1_555 1_555 yes C7 C6 C10 117.9(4) . 1_555 1_555 yes C6 C7 C8 120.2(5) . 1_555 1_555 yes C7 C8 C9 119.4(4) . 1_555 1_555 yes C4 C9 C8 122.8(5) . 1_555 1_555 yes N1 C10 C6 126.3(4) . 1_555 1_555 yes N1 C11 C12 121.8(4) . 1_555 1_555 yes N1 C11 C16 119.1(4) . 1_555 1_555 yes C12 C11 C16 119.1(4) . 1_555 1_555 yes C11 C12 C13 120.5(5) . 1_555 1_555 yes C12 C13 C14 119.7(5) . 1_555 1_555 yes O2 C14 C13 115.6(5) . 1_555 1_555 yes O2 C14 C15 124.4(5) . 1_555 1_555 yes C13 C14 C15 119.9(5) . 1_555 1_555 yes C14 C15 C16 120.1(5) . 1_555 1_555 yes C11 C16 C15 120.7(4) . 1_555 1_555 yes C2 C18 C19 115.8(4) . 1_555 1_555 yes C18 C19 C20 120.1(4) . 1_555 1_555 yes C18 C19 C24 121.6(5) . 1_555 1_555 yes C20 C19 C24 118.2(5) . 1_555 1_555 yes O3 C20 C19 118.9(5) . 1_555 1_555 yes O3 C20 C21 122.3(4) . 1_555 1_555 yes C19 C20 C21 118.9(4) . 1_555 1_555 yes C20 C21 C22 120.5(5) . 1_555 1_555 yes C20 C21 C25 121.7(4) . 1_555 1_555 yes C22 C21 C25 117.3(5) . 1_555 1_555 yes C21 C22 C23 120.4(5) . 1_555 1_555 yes C22 C23 C24 119.1(5) . 1_555 1_555 yes C19 C24 C23 122.3(5) . 1_555 1_555 yes N2 C25 C21 127.3(4) . 1_555 1_555 yes N2 C26 C27 123.1(4) . 1_555 1_555 yes N2 C26 C31 118.4(4) . 1_555 1_555 yes C27 C26 C31 118.5(4) . 1_555 1_555 yes C26 C27 C28 121.3(4) . 1_555 1_555 yes C27 C28 C29 120.2(4) . 1_555 1_555 yes O4 C29 C28 125.6(4) . 1_555 1_555 yes O4 C29 C30 114.6(4) . 1_555 1_555 yes C28 C29 C30 119.7(4) . 1_555 1_555 yes C29 C30 C31 120.3(4) . 1_555 1_555 yes C26 C31 C30 119.8(4) . 1_555 1_555 yes C33 C34 C35 123.2(5) . 1_555 1_555 yes C33 C34 C50 122.1(4) . 1_555 1_555 yes C35 C34 C50 114.7(4) . 1_555 1_555 yes C34 C35 C36 116.6(4) . 1_555 1_555 yes C35 C36 C37 119.9(4) . 1_555 1_555 yes C35 C36 C41 121.7(4) . 1_555 1_555 yes C37 C36 C41 118.4(4) . 1_555 1_555 yes O5 C37 C36 118.5(4) . 1_555 1_555 yes O5 C37 C38 122.0(4) . 1_555 1_555 yes C36 C37 C38 119.5(4) . 1_555 1_555 yes C37 C38 C39 120.0(4) . 1_555 1_555 yes C37 C38 C42 121.7(4) . 1_555 1_555 yes C39 C38 C42 118.1(4) . 1_555 1_555 yes C38 C39 C40 120.5(4) . 1_555 1_555 yes C39 C40 C41 119.3(4) . 1_555 1_555 yes C36 C41 C40 122.3(5) . 1_555 1_555 yes N3 C42 C38 126.0(4) . 1_555 1_555 yes N3 C43 C44 121.3(4) . 1_555 1_555 yes N3 C43 C48 119.5(4) . 1_555 1_555 yes C44 C43 C48 119.1(4) . 1_555 1_555 yes C43 C44 C45 120.1(4) . 1_555 1_555 yes C44 C45 C46 120.7(4) . 1_555 1_555 yes O6 C46 C45 116.1(5) . 1_555 1_555 yes O6 C46 C47 124.4(5) . 1_555 1_555 yes C45 C46 C47 119.5(4) . 1_555 1_555 yes C46 C47 C48 119.5(4) . 1_555 1_555 yes C43 C48 C47 120.9(4) . 1_555 1_555 yes C34 C50 C51 115.7(4) . 1_555 1_555 yes C50 C51 C52 118.8(4) . 1_555 1_555 yes C50 C51 C56 122.5(4) . 1_555 1_555 yes C52 C51 C56 118.7(4) . 1_555 1_555 yes O7 C52 C51 119.0(4) . 1_555 1_555 yes O7 C52 C53 121.6(4) . 1_555 1_555 yes C51 C52 C53 119.3(4) . 1_555 1_555 yes C52 C53 C54 119.3(4) . 1_555 1_555 yes C52 C53 C57 121.7(4) . 1_555 1_555 yes C54 C53 C57 118.9(4) . 1_555 1_555 yes C53 C54 C55 120.9(5) . 1_555 1_555 yes C54 C55 C56 119.4(4) . 1_555 1_555 yes C51 C56 C55 122.2(4) . 1_555 1_555 yes N4 C57 C53 125.9(4) . 1_555 1_555 yes N4 C58 C59 121.1(4) . 1_555 1_555 yes N4 C58 C63 119.2(4) . 1_555 1_555 yes C59 C58 C63 119.7(4) . 1_555 1_555 yes C58 C59 C60 120.2(4) . 1_555 1_555 yes C59 C60 C61 120.0(4) . 1_555 1_555 yes O8 C61 C60 115.0(4) . 1_555 1_555 yes O8 C61 C62 124.9(4) . 1_555 1_555 yes C60 C61 C62 120.1(4) . 1_555 1_555 yes C61 C62 C63 119.4(4) . 1_555 1_555 yes C58 C63 C62 120.6(4) . 1_555 1_555 yes O9 C65 C66 109.9(5) . 1_555 1_555 yes O9 C65 C67 109.4(5) . 1_555 1_555 yes C66 C65 C67 112.6(5) . 1_555 1_555 yes O10 C68 C69 109.9(5) . 1_555 1_555 yes O10 C68 C70 110.8(5) . 1_555 1_555 yes C69 C68 C70 115.6(5) . 1_555 1_555 yes CL1 C71 CL2 112.1(4) . 1_555 1_555 yes CL3 C72 CL4 111.9(4) . 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag TI1 O1 C4 C5 36(1) 1_555 1_555 1_555 1_555 yes TI1 O1 C4 C9 35(2) 1_555 1_555 1_555 1_555 yes TI1 O1 C5 C6 8.1(8) 1_555 1_555 1_555 1_555 yes TI1 O1 C6 C7 -173.3(6) 1_555 1_555 1_555 1_555 yes TI1 O1 C6 C10 7.0(3) 1_555 1_555 1_555 1_555 yes TI1 O7 C51 C52 35(2) 1_555 1_555 1_555 1_555 yes TI1 O7 C51 C56 40(2) 1_555 1_555 1_555 1_555 yes TI1 O7 C52 C53 4.8(7) 1_555 1_555 1_555 1_555 yes TI1 O7 C53 C54 177.0(6) 1_555 1_555 1_555 1_555 yes TI1 O7 C53 C57 -3.8(3) 1_555 1_555 1_555 1_555 yes TI1 O9 C65 C66 -94.4(8) 1_555 1_555 1_555 1_555 yes TI1 O9 C65 C67 141.4(6) 1_555 1_555 1_555 1_555 yes TI1 N1 C10 C11 -176.6(6) 1_555 1_555 1_555 1_555 yes TI1 N1 C11 C12 124.6(4) 1_555 1_555 1_555 1_555 yes TI1 N1 C11 C16 -52.5(5) 1_555 1_555 1_555 1_555 yes TI1 N4 C57 C58 -170.5(6) 1_555 1_555 1_555 1_555 yes TI1 N4 C58 C59 118.9(4) 1_555 1_555 1_555 1_555 yes TI1 N4 C58 C63 -58.4(5) 1_555 1_555 1_555 1_555 yes TI2 O3 C19 C20 38(1) 1_555 1_555 1_555 1_555 yes TI2 O3 C19 C24 48(1) 1_555 1_555 1_555 1_555 yes TI2 O3 C20 C21 8.9(7) 1_555 1_555 1_555 1_555 yes TI2 O3 C21 C22 177.3(7) 1_555 1_555 1_555 1_555 yes TI2 O3 C21 C25 -5.9(3) 1_555 1_555 1_555 1_555 yes TI2 O5 C36 C37 70.2(6) 1_555 1_555 1_555 1_555 yes TI2 O5 C36 C41 68.9(9) 1_555 1_555 1_555 1_555 yes TI2 O5 C37 C38 33.2(6) 1_555 1_555 1_555 1_555 yes TI2 O5 C38 C39 -155.8(6) 1_555 1_555 1_555 1_555 yes TI2 O5 C38 C42 28.9(3) 1_555 1_555 1_555 1_555 yes TI2 O10 C68 C69 -110.3(6) 1_555 1_555 1_555 1_555 yes TI2 O10 C68 C70 120.7(6) 1_555 1_555 1_555 1_555 yes TI2 N2 C25 C26 -176.5(6) 1_555 1_555 1_555 1_555 yes TI2 N2 C26 C27 131.8(4) 1_555 1_555 1_555 1_555 yes TI2 N2 C26 C31 -49.7(5) 1_555 1_555 1_555 1_555 yes TI2 N3 C42 C43 -174.6(5) 1_555 1_555 1_555 1_555 yes TI2 N3 C43 C44 -64.5(5) 1_555 1_555 1_555 1_555 yes TI2 N3 C43 C48 112.6(4) 1_555 1_555 1_555 1_555 yes O1 C4 C5 C6 178.4(7) 1_555 1_555 1_555 1_555 yes O1 C5 C6 C7 -179.1(4) 1_555 1_555 1_555 1_555 yes O1 C5 C6 C10 2.0(7) 1_555 1_555 1_555 1_555 yes O1 C6 C7 C8 -2.1(10) 1_555 1_555 1_555 1_555 yes O1 C6 C7 C9 -2.0(7) 1_555 1_555 1_555 1_555 yes O1 C6 C10 C11 0(1) 1_555 1_555 1_555 1_555 yes O2 C13 C14 C15 -178.9(8) 1_555 1_555 1_555 1_555 yes O2 C14 C15 C16 -178.9(5) 1_555 1_555 1_555 1_555 yes O3 C19 C20 C21 -179.3(7) 1_555 1_555 1_555 1_555 yes O3 C20 C21 C22 174.7(4) 1_555 1_555 1_555 1_555 yes O3 C20 C21 C25 -14.1(7) 1_555 1_555 1_555 1_555 yes O3 C21 C22 C23 4(1) 1_555 1_555 1_555 1_555 yes O3 C21 C22 C24 7.5(7) 1_555 1_555 1_555 1_555 yes O3 C21 C25 C26 -13(1) 1_555 1_555 1_555 1_555 yes O4 C29 C30 C31 178.8(4) 1_555 1_555 1_555 1_555 yes O5 C36 C37 C38 178.1(7) 1_555 1_555 1_555 1_555 yes O5 C37 C38 C39 -179.9(4) 1_555 1_555 1_555 1_555 yes O5 C37 C38 C42 5.8(6) 1_555 1_555 1_555 1_555 yes O5 C38 C39 C40 -0.1(9) 1_555 1_555 1_555 1_555 yes O5 C38 C42 C43 8(1) 1_555 1_555 1_555 1_555 yes O6 C45 C46 C47 179.2(7) 1_555 1_555 1_555 1_555 yes O6 C45 C46 C49 4.3(5) 1_555 1_555 1_555 1_555 yes O6 C46 C47 C48 176.8(5) 1_555 1_555 1_555 1_555 yes O7 C51 C52 C53 -179.8(7) 1_555 1_555 1_555 1_555 yes O7 C52 C53 C54 176.2(4) 1_555 1_555 1_555 1_555 yes O7 C52 C53 C57 -8.1(7) 1_555 1_555 1_555 1_555 yes O7 C53 C54 C55 5.5(9) 1_555 1_555 1_555 1_555 yes O7 C53 C54 C56 5.4(7) 1_555 1_555 1_555 1_555 yes O7 C53 C57 C58 -14(1) 1_555 1_555 1_555 1_555 yes O8 C60 C61 C62 -179.7(8) 1_555 1_555 1_555 1_555 yes O8 C61 C62 C63 -178.8(4) 1_555 1_555 1_555 1_555 yes N1 C10 C11 C12 136.7(5) 1_555 1_555 1_555 1_555 yes N1 C10 C11 C16 -69.2(6) 1_555 1_555 1_555 1_555 yes N1 C11 C12 C13 -176.2(5) 1_555 1_555 1_555 1_555 yes N2 C25 C26 C27 143.2(5) 1_555 1_555 1_555 1_555 yes N2 C25 C26 C31 -66.3(6) 1_555 1_555 1_555 1_555 yes N2 C26 C27 C28 174.4(4) 1_555 1_555 1_555 1_555 yes N2 C26 C27 C29 175.0(4) 1_555 1_555 1_555 1_555 yes N3 C42 C43 C44 -81.6(6) 1_555 1_555 1_555 1_555 yes N3 C42 C43 C48 128.1(5) 1_555 1_555 1_555 1_555 yes N3 C43 C44 C45 176.1(4) 1_555 1_555 1_555 1_555 yes N4 C57 C58 C59 136.3(5) 1_555 1_555 1_555 1_555 yes N4 C57 C58 C63 -70.1(6) 1_555 1_555 1_555 1_555 yes N4 C58 C59 C60 -179.4(4) 1_555 1_555 1_555 1_555 yes C1 C2 C3 C4 4.5(7) 1_555 1_555 1_555 1_555 yes C1 C2 C18 C19 -159.1(5) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C5 81.1(5) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C9 -100.5(6) 1_555 1_555 1_555 1_555 yes C2 C18 C19 C20 74.8(6) 1_555 1_555 1_555 1_555 yes C2 C18 C19 C24 -103.4(6) 1_555 1_555 1_555 1_555 yes C3 C4 C5 C6 176.0(4) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C7 2.5(7) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C10 -176.4(4) 1_555 1_555 1_555 1_555 yes C5 C6 C7 C8 -1.3(7) 1_555 1_555 1_555 1_555 yes C5 C6 C7 C9 -1.3(5) 1_555 1_555 1_555 1_555 yes C5 C6 C10 C11 0(1) 1_555 1_555 1_555 1_555 yes C6 C7 C8 C9 0.1(8) 1_555 1_555 1_555 1_555 yes C6 C10 C11 C12 130(1) 1_555 1_555 1_555 1_555 yes C6 C10 C11 C16 -75(1) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C13 160.2(4) 1_555 1_555 1_555 1_555 yes C11 C12 C13 C14 -1.8(8) 1_555 1_555 1_555 1_555 yes C12 C13 C14 C15 1.3(8) 1_555 1_555 1_555 1_555 yes C13 C14 C15 C16 -0.1(8) 1_555 1_555 1_555 1_555 yes C18 C19 C20 C21 -171.5(4) 1_555 1_555 1_555 1_555 yes C19 C20 C21 C22 -6.1(7) 1_555 1_555 1_555 1_555 yes C19 C20 C21 C25 165.2(4) 1_555 1_555 1_555 1_555 yes C20 C21 C22 C23 -0.1(8) 1_555 1_555 1_555 1_555 yes C20 C21 C22 C24 2.7(5) 1_555 1_555 1_555 1_555 yes C20 C21 C25 C26 -7(1) 1_555 1_555 1_555 1_555 yes C21 C22 C23 C24 5.6(8) 1_555 1_555 1_555 1_555 yes C21 C25 C26 C27 159(1) 1_555 1_555 1_555 1_555 yes C21 C25 C26 C31 -50(1) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C28 152.9(4) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C29 153.6(2) 1_555 1_555 1_555 1_555 yes C26 C27 C28 C29 1.3(7) 1_555 1_555 1_555 1_555 yes C26 C27 C28 C30 2.2(5) 1_555 1_555 1_555 1_555 yes C26 C27 C29 C30 2.7(4) 1_555 1_555 1_555 1_555 yes C26 C27 C29 C32 -176.5(4) 1_555 1_555 1_555 1_555 yes C27 C28 C29 C30 1.9(7) 1_555 1_555 1_555 1_555 yes C27 C28 C29 C32 -178.0(4) 1_555 1_555 1_555 1_555 yes C27 C28 C30 C31 -0.1(4) 1_555 1_555 1_555 1_555 yes C27 C29 C30 C31 -1.0(5) 1_555 1_555 1_555 1_555 yes C28 C29 C30 C31 -2.0(7) 1_555 1_555 1_555 1_555 yes C33 C34 C35 C36 -4.5(7) 1_555 1_555 1_555 1_555 yes C33 C34 C50 C51 -135.0(5) 1_555 1_555 1_555 1_555 yes C34 C35 C36 C37 80.8(5) 1_555 1_555 1_555 1_555 yes C34 C35 C36 C41 -99.2(5) 1_555 1_555 1_555 1_555 yes C34 C50 C51 C52 64.3(5) 1_555 1_555 1_555 1_555 yes C34 C50 C51 C56 -116.5(5) 1_555 1_555 1_555 1_555 yes C35 C36 C37 C38 177.3(4) 1_555 1_555 1_555 1_555 yes C36 C37 C38 C39 2.1(6) 1_555 1_555 1_555 1_555 yes C36 C37 C38 C42 -172.2(4) 1_555 1_555 1_555 1_555 yes C37 C38 C39 C40 0.0(7) 1_555 1_555 1_555 1_555 yes C37 C38 C42 C43 6(1) 1_555 1_555 1_555 1_555 yes C38 C39 C40 C41 -1.5(7) 1_555 1_555 1_555 1_555 yes C38 C42 C43 C44 -111.2(10) 1_555 1_555 1_555 1_555 yes C38 C42 C43 C48 98.6(10) 1_555 1_555 1_555 1_555 yes C42 C43 C44 C45 -147.3(4) 1_555 1_555 1_555 1_555 yes C43 C44 C45 C46 -3.0(7) 1_555 1_555 1_555 1_555 yes C44 C45 C46 C47 4.6(7) 1_555 1_555 1_555 1_555 yes C44 C45 C46 C49 -170.2(6) 1_555 1_555 1_555 1_555 yes C45 C46 C47 C48 -2.3(7) 1_555 1_555 1_555 1_555 yes C50 C51 C52 C53 -177.1(4) 1_555 1_555 1_555 1_555 yes C51 C52 C53 C54 -4.0(6) 1_555 1_555 1_555 1_555 yes C51 C52 C53 C57 171.7(4) 1_555 1_555 1_555 1_555 yes C52 C53 C54 C55 2.2(7) 1_555 1_555 1_555 1_555 yes C52 C53 C54 C56 2.2(5) 1_555 1_555 1_555 1_555 yes C52 C53 C57 C58 -10(1) 1_555 1_555 1_555 1_555 yes C53 C54 C55 C56 -0.1(8) 1_555 1_555 1_555 1_555 yes C53 C57 C58 C59 148.1(10) 1_555 1_555 1_555 1_555 yes C53 C57 C58 C63 -58(1) 1_555 1_555 1_555 1_555 yes C57 C58 C59 C60 156.6(4) 1_555 1_555 1_555 1_555 yes C58 C59 C60 C61 0.9(8) 1_555 1_555 1_555 1_555 yes C59 C60 C61 C62 -0.3(8) 1_555 1_555 1_555 1_555 yes C60 C61 C62 C63 0.9(7) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------ data_complex_4 _database_code_CSD 170679 _audit_creation_date 'Wed Dec 5 11:22:52 2001' _audit_creation_method 'by teXsan' _audit_update_record ? #------------------------------------------------------------------------------ # CHEMICAL DATA _chemical_formula_sum 'C72 H72 N4 O12 Ti2 ' _chemical_formula_moiety '?' _chemical_formula_weight 1281.18 _chemical_melting_point ? #------------------------------------------------------------------------------ # CRYSTAL DATA _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1 ' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z _cell_length_a 12.115(2) _cell_length_b 14.049(3) _cell_length_c 9.924(1) _cell_angle_alpha 98.118(9) _cell_angle_beta 93.263(4) _cell_angle_gamma 71.151(6) _cell_volume 1582.2(5) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9205 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.5 _cell_measurement_temperature 193.2 #------------------------------------------------------------------------------ _exptl_crystal_description 'prism' _exptl_crystal_colour 'yellow' _exptl_crystal_size_max 0.700 _exptl_crystal_size_mid 0.600 _exptl_crystal_size_min 0.300 _exptl_crystal_size_rad ? _exptl_crystal_density_diffrn 1.344 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F000 718 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(Higashi, 1995)' _exptl_absorpt_correction_T_min 0.469 _exptl_absorpt_correction_T_max 0.908 #------------------------------------------------------------------------------ # EXPERIMENTAL DATA _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.7107 _diffrn_measurement_device_type 'Rigaku RAXIS-RAPID Imaging Plate' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12844 _diffrn_reflns_av_R_equivalents 0.075 _diffrn_reflns_theta_max 27.49 _diffrn_measured_fraction_theta_max 0.9399 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.9399 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 #------------------------------------------------------------------------------ # REFINEMENT DATA _refine_special_details ; Refinement using reflections with F^2^ > 1.5 sigma(F^2^). The weighted R-factor (wR) and goodness of fit (S) are based on F^2^. R-factor (gt) are based on F. The threshold expression of F^2^ > 2.0 sigma(F^2^) is used only for calculating R-factor (gt). ; _reflns_number_total 6810 _reflns_number_gt 4857 _reflns_threshold_expression F^2^>2.0\s(F^2^) _refine_ls_structure_factor_coef Fsqd _refine_ls_R_factor_gt 0.0803 _refine_ls_wR_factor_ref 0.1834 _refine_ls_hydrogen_treatment noref _refine_ls_number_reflns 5173 _refine_ls_number_parameters 417 _refine_ls_goodness_of_fit_ref 2.434 _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^) + (0.04000(Max(Fo^2^,0) + 2Fc^2^)/3)^2^]' _refine_ls_shift/su_max 0.0071 _refine_diff_density_max 0.63 _refine_diff_density_min -0.64 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ? _refine_ls_abs_structure_Flack ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.003 0.002 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'H' 'H' 0.000 0.000 ;International Tables for Crystallography (1992, Vol. C, Table 6.1.1.2) ; 'N' 'N' 0.006 0.003 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'O' 'O' 0.011 0.006 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; 'Ti' 'Ti' 0.278 0.446 ;International Tables for Crystallography (1992, Vol. C, Tables 4.2.6.8 and 6.1.1.1) ; #------------------------------------------------------------------------------ # ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.60845(7) 0.00520(4) 0.03620(7) 0.0436(2) Uani 1.00 d . . . O1 O 0.6875(2) -0.1319(2) 0.0659(3) 0.0474(8) Uani 1.00 d . . . O2 O 0.7881(4) 0.2582(3) -0.4224(4) 0.089(1) Uani 1.00 d . . . O3 O 0.5852(2) 0.1445(2) 0.0252(3) 0.0512(8) Uani 1.00 d . . . O4 O 0.8055(4) -0.2064(2) 0.6396(3) 0.080(1) Uani 1.00 d . . . O5 O 0.4731(2) 0.0177(2) 0.1220(2) 0.0431(7) Uani 1.00 d . . . O6 O 0.403(2) 0.457(1) 0.440(2) 0.204(8) Uani 0.62 d P . . O7 O 0.9093(8) 0.4790(5) 0.3686(8) 0.100(3) Uani 0.55 d P . . N1 N 0.7755(3) -0.0241(2) -0.0833(3) 0.0475(9) Uani 1.00 d . . . N2 N 0.7025(3) 0.0454(2) 0.2313(3) 0.0491(9) Uani 1.00 d . . . C1 C 0.6559(4) -0.3815(3) -0.0680(5) 0.056(1) Uani 1.00 d . . . C2 C 0.6233(4) -0.3399(2) 0.0561(4) 0.050(1) Uani 1.00 d . . . C3 C 0.7043(5) -0.3122(3) 0.1630(4) 0.062(1) Uani 1.00 d . . . C4 C 0.8077(4) -0.2949(3) 0.1078(4) 0.055(1) Uani 1.00 d . . . C5 C 0.7906(4) -0.2016(2) 0.0545(4) 0.050(1) Uani 1.00 d . . . C6 C 0.8827(4) -0.1889(3) -0.0108(4) 0.052(1) Uani 1.00 d . . . C7 C 0.9912(4) -0.2665(3) -0.0209(5) 0.067(1) Uani 1.00 d . . . C8 C 1.0086(5) -0.3539(3) 0.0345(6) 0.075(2) Uani 1.00 d . . . C9 C 0.9169(5) -0.3676(3) 0.0978(5) 0.067(1) Uani 1.00 d . . . C10 C 0.8689(4) -0.1013(3) -0.0811(4) 0.054(1) Uani 1.00 d . . . C11 C 0.7818(4) 0.0482(3) -0.1685(4) 0.054(1) Uani 1.00 d . . . C12 C 0.6977(4) 0.0778(3) -0.2688(4) 0.054(1) Uani 1.00 d . . . C13 C 0.7023(4) 0.1466(3) -0.3516(4) 0.058(1) Uani 1.00 d . . . C14 C 0.7912(5) 0.1903(3) -0.3354(5) 0.068(2) Uani 1.00 d . . . C15 C 0.8707(5) 0.1639(4) -0.2359(5) 0.069(2) Uani 1.00 d . . . C16 C 0.8709(4) 0.0921(3) -0.1543(5) 0.067(2) Uani 1.00 d . . . C17 C 0.8498(7) 0.3283(5) -0.3803(7) 0.112(3) Uani 1.00 d . . . C18 C 0.4988(4) -0.3177(3) 0.1036(5) 0.061(1) Uani 1.00 d . . . C19 C 0.5917(4) 0.3080(2) 0.0067(5) 0.056(1) Uani 1.00 d . . . C20 C 0.6289(4) 0.2182(2) 0.0700(4) 0.051(1) Uani 1.00 d . . . C21 C 0.7075(4) 0.2096(3) 0.1804(4) 0.050(1) Uani 1.00 d . . . C22 C 0.7510(4) 0.2915(3) 0.2274(5) 0.065(1) Uani 1.00 d . . . C23 C 0.7200(5) 0.3755(3) 0.1592(6) 0.074(2) Uani 1.00 d . . . C24 C 0.6413(4) 0.3842(3) 0.0538(6) 0.068(2) Uani 1.00 d . . . C25 C 0.7344(4) 0.1265(3) 0.2580(4) 0.052(1) Uani 1.00 d . . . C26 C 0.7304(4) -0.0210(3) 0.3347(4) 0.053(1) Uani 1.00 d . . . C27 C 0.8408(4) -0.0552(3) 0.3893(5) 0.066(1) Uani 1.00 d . . . C28 C 0.8627(5) -0.1178(3) 0.4904(5) 0.073(2) Uani 1.00 d . . . C29 C 0.7744(5) -0.1473(3) 0.5379(5) 0.063(1) Uani 1.00 d . . . C30 C 0.6636(5) -0.1153(3) 0.4809(4) 0.062(1) Uani 1.00 d . . . C31 C 0.6426(4) -0.0533(3) 0.3786(4) 0.059(1) Uani 1.00 d . . . C32 C 0.7147(6) -0.2330(4) 0.6956(6) 0.093(2) Uani 1.00 d . . . C33 C 0.466(2) 0.424(1) 0.521(2) 0.219(7) Uani 1.00 d . . . C34 C 0.458(1) 0.525(1) 0.401(1) 0.179(6) Uani 1.00 d . . . C35 C 1.0249(8) 0.4432(6) 0.385(1) 0.142(4) Uani 1.00 d . . . C36 C 0.9078(7) 0.5582(5) 0.4803(9) 0.118(3) Uani 1.00 d . . . H1 H 0.5989 -0.3962 -0.1315 0.0380 Uiso 1.00 calc . . . H2 H 0.7363 -0.3994 -0.0935 0.0380 Uiso 1.00 calc . . . H3 H 0.7290 -0.3598 0.2295 0.0380 Uiso 1.00 calc . . . H4 H 0.6734 -0.2514 0.2291 0.0380 Uiso 1.00 calc . . . H5 H 1.0537 -0.2649 -0.0783 0.0380 Uiso 1.00 calc . . . H6 H 1.0856 -0.4076 0.0271 0.0380 Uiso 1.00 calc . . . H7 H 0.9261 -0.4301 0.1317 0.0380 Uiso 1.00 calc . . . H8 H 0.9273 -0.1101 -0.1500 0.0380 Uiso 1.00 calc . . . H9 H 0.6342 0.0491 -0.2680 0.0380 Uiso 1.00 calc . . . H10 H 0.6386 0.1744 -0.4179 0.0380 Uiso 1.00 calc . . . H11 H 0.9379 0.1883 -0.2343 0.0380 Uiso 1.00 calc . . . H12 H 0.9222 0.0852 -0.0742 0.0380 Uiso 1.00 calc . . . H13 H 0.8415 0.3721 -0.4479 0.1352 Uiso 1.00 calc . . . H14 H 0.9306 0.2921 -0.3692 0.1352 Uiso 1.00 calc . . . H15 H 0.8201 0.3673 -0.2967 0.1352 Uiso 1.00 calc . . . H16 H 0.4719 -0.2545 0.1635 0.0380 Uiso 1.00 calc . . . H17 H 0.4962 -0.3685 0.1571 0.0380 Uiso 1.00 calc . . . H18 H 0.8078 0.2833 0.3036 0.0380 Uiso 1.00 calc . . . H19 H 0.7540 0.4277 0.1855 0.0874 Uiso 1.00 calc . . . H20 H 0.6264 0.4435 0.0060 0.0380 Uiso 1.00 calc . . . H21 H 0.7944 0.1206 0.3313 0.0380 Uiso 1.00 calc . . . H22 H 0.8979 -0.0226 0.3650 0.0380 Uiso 1.00 calc . . . H23 H 0.9391 -0.1406 0.5284 0.0878 Uiso 1.00 calc . . . H24 H 0.6063 -0.1452 0.5056 0.0380 Uiso 1.00 calc . . . H25 H 0.5669 -0.0324 0.3381 0.0716 Uiso 1.00 calc . . . H26 H 0.6564 -0.1731 0.7325 0.1122 Uiso 1.00 calc . . . H27 H 0.6819 -0.2695 0.6262 0.1122 Uiso 1.00 calc . . . H28 H 0.7467 -0.2741 0.7658 0.1122 Uiso 1.00 calc . . . H29 H 0.5440 0.3889 0.4895 0.2563 Uiso 1.00 calc . . . H30 H 0.4398 0.3750 0.5592 0.2563 Uiso 1.00 calc . . . H31 H 0.4121 0.5582 0.3248 0.2179 Uiso 1.00 calc . . . H32 H 0.5354 0.4902 0.3634 0.2179 Uiso 1.00 calc . . . H33 H 1.0621 0.4945 0.3686 0.1740 Uiso 1.00 calc . . . H34 H 1.0618 0.3847 0.3196 0.1740 Uiso 1.00 calc . . . H35 H 0.9494 0.6017 0.4565 0.1398 Uiso 1.00 calc . . . H36 H 0.8273 0.6012 0.4949 0.1398 Uiso 1.00 calc . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti 0.0650(5) 0.0234(3) 0.0457(4) -0.0181(3) -0.0007(3) 0.0062(2) O1 0.065(2) 0.027(1) 0.052(2) -0.016(1) 0.000(1) 0.008(1) O2 0.137(3) 0.084(2) 0.078(2) -0.071(2) -0.008(2) 0.029(2) O3 0.077(2) 0.025(1) 0.056(2) -0.023(1) -0.003(1) 0.006(1) O4 0.127(3) 0.055(2) 0.060(2) -0.029(2) -0.008(2) 0.016(2) O5 0.060(2) 0.025(1) 0.045(1) -0.015(1) 0.005(1) 0.0028(10) O6 0.27(2) 0.18(1) 0.20(2) -0.13(1) -0.04(1) 0.070(10) O7 0.123(8) 0.077(5) 0.102(6) -0.042(5) -0.036(5) 0.012(4) N1 0.059(2) 0.034(1) 0.054(2) -0.020(2) -0.008(2) 0.010(1) N2 0.068(2) 0.039(2) 0.049(2) -0.027(2) -0.002(2) 0.010(1) C1 0.065(3) 0.040(2) 0.067(3) -0.024(2) 0.000(2) 0.005(2) C2 0.079(3) 0.021(1) 0.055(2) -0.018(2) 0.006(2) 0.010(2) C3 0.108(4) 0.029(2) 0.050(2) -0.022(2) -0.004(2) 0.008(2) C4 0.083(3) 0.030(2) 0.052(2) -0.020(2) -0.008(2) 0.005(2) C5 0.071(3) 0.026(2) 0.048(2) -0.012(2) -0.011(2) 0.002(2) C6 0.060(3) 0.038(2) 0.057(3) -0.016(2) -0.005(2) 0.005(2) C7 0.058(3) 0.048(2) 0.090(4) -0.014(2) 0.001(3) 0.006(2) C8 0.071(3) 0.040(2) 0.103(4) -0.005(2) -0.015(3) 0.009(2) C9 0.087(4) 0.030(2) 0.076(3) -0.011(2) -0.024(3) 0.009(2) C10 0.063(3) 0.046(2) 0.055(3) -0.025(2) -0.001(2) 0.001(2) C11 0.071(3) 0.044(2) 0.052(2) -0.027(2) -0.001(2) 0.005(2) C12 0.065(3) 0.043(2) 0.058(3) -0.024(2) -0.004(2) 0.004(2) C13 0.077(3) 0.049(2) 0.053(2) -0.028(2) 0.001(2) 0.002(2) C14 0.088(4) 0.060(3) 0.068(3) -0.042(3) 0.000(3) 0.011(2) C15 0.079(3) 0.072(3) 0.076(3) -0.047(3) -0.002(3) 0.018(2) C16 0.079(3) 0.066(3) 0.072(3) -0.043(3) -0.020(3) 0.018(2) C17 0.163(6) 0.088(4) 0.126(5) -0.086(4) -0.018(5) 0.042(4) C18 0.091(4) 0.028(2) 0.065(3) -0.015(2) 0.014(3) 0.013(2) C19 0.078(3) 0.025(2) 0.068(3) -0.018(2) 0.022(2) 0.007(2) C20 0.070(3) 0.025(2) 0.060(3) -0.020(2) 0.016(2) 0.000(2) C21 0.063(3) 0.033(2) 0.060(3) -0.024(2) 0.010(2) 0.000(2) C22 0.072(3) 0.042(2) 0.087(3) -0.028(2) -0.001(3) 0.004(2) C23 0.078(3) 0.035(2) 0.117(4) -0.031(2) 0.013(3) 0.004(2) C24 0.077(3) 0.029(2) 0.105(4) -0.022(2) 0.021(3) 0.014(2) C25 0.067(3) 0.042(2) 0.052(2) -0.025(2) -0.007(2) 0.006(2) C26 0.074(3) 0.039(2) 0.050(2) -0.025(2) 0.000(2) 0.003(2) C27 0.074(3) 0.050(2) 0.074(3) -0.021(2) -0.005(3) 0.013(2) C28 0.084(4) 0.051(2) 0.075(3) -0.012(2) -0.006(3) 0.011(2) C29 0.090(4) 0.039(2) 0.057(3) -0.018(2) -0.001(3) 0.000(2) C30 0.102(4) 0.045(2) 0.048(2) -0.035(2) 0.001(3) 0.004(2) C31 0.080(3) 0.047(2) 0.056(3) -0.028(2) -0.006(2) 0.006(2) C32 0.160(6) 0.057(3) 0.070(3) -0.044(3) -0.002(4) 0.014(2) C33 0.25(2) 0.19(1) 0.19(1) -0.04(1) -0.10(1) 0.05(1) C34 0.18(1) 0.22(1) 0.16(1) -0.082(9) -0.010(8) 0.046(9) C35 0.097(6) 0.141(7) 0.175(9) -0.005(5) -0.028(6) 0.073(6) C36 0.138(6) 0.071(4) 0.142(7) -0.031(4) 0.034(5) -0.008(4) #------------------------------------------------------------------------------ _computing_data_collection 'PROCESS-AUTO' _computing_cell_refinement 'PROCESS-AUTO' _computing_data_reduction 'teXsan Ver. 1.10' _computing_structure_solution SIR92 _computing_structure_refinement 'teXsan Ver. 1.10' _computing_publication_material 'teXsan Ver. 1.10' _computing_molecular_graphics ? #------------------------------------------------------------------------------ _geom_special_details ; ? ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag TI O1 1.910(2) . . yes TI O3 1.903(2) . . yes TI O5 1.837(3) . . yes TI O5 1.852(2) . 2_655 yes TI N1 2.295(4) . . yes TI N2 2.285(3) . . yes O1 C5 1.314(4) . . yes O2 C14 1.365(5) . . yes O2 C17 1.424(6) . . yes O3 C20 1.322(4) . . yes O4 C29 1.357(5) . . yes O4 C32 1.432(7) . . yes O6 C33 1.12(1) . . yes O6 C34 1.43(2) . . yes O7 C35 1.34(1) . . yes O7 C36 1.452(10) . . yes N1 C10 1.291(5) . . yes N1 C11 1.433(5) . . yes N2 C25 1.306(4) . . yes N2 C26 1.436(5) . . yes C1 C2 1.311(6) . . yes C2 C3 1.501(6) . . yes C2 C18 1.527(7) . . yes C3 C4 1.497(7) . . yes C4 C5 1.431(5) . . yes C4 C9 1.384(6) . . yes C5 C6 1.394(6) . . yes C6 C7 1.408(6) . . yes C6 C10 1.457(6) . . yes C7 C8 1.366(7) . . yes C8 C9 1.385(7) . . yes C11 C12 1.390(6) . . yes C11 C16 1.399(6) . . yes C12 C13 1.370(6) . . yes C13 C14 1.393(6) . . yes C14 C15 1.344(7) . . yes C15 C16 1.378(6) . . yes C18 C19 1.492(6) . 2_655 yes C19 C20 1.419(5) . . yes C19 C24 1.403(6) . . yes C20 C21 1.402(6) . . yes C21 C22 1.426(5) . . yes C21 C25 1.428(5) . . yes C22 C23 1.379(6) . . yes C23 C24 1.366(7) . . yes C26 C27 1.375(6) . . yes C26 C31 1.395(6) . . yes C27 C28 1.385(6) . . yes C28 C29 1.391(7) . . yes C29 C30 1.386(7) . . yes C30 C31 1.390(6) . . yes C33 C34 1.46(2) . 2_666 yes C35 C36 1.52(1) . 2_766 yes #------------------------------------------------------------------------------ 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 O2 C17 116.7(4) . 1_555 1_555 yes C29 O4 C32 116.8(4) . 1_555 1_555 yes C33 O6 C34 99(1) . 1_555 1_555 yes C35 O7 C36 87.9(6) . 1_555 1_555 yes C10 N1 C11 114.5(4) . 1_555 1_555 yes C25 N2 C26 115.6(3) . 1_555 1_555 yes C1 C2 C3 123.4(4) . 1_555 1_555 yes C1 C2 C18 121.9(4) . 1_555 1_555 yes C3 C2 C18 114.7(4) . 1_555 1_555 yes C2 C3 C4 114.3(4) . 1_555 1_555 yes C3 C4 C5 118.3(4) . 1_555 1_555 yes C3 C4 C9 122.9(4) . 1_555 1_555 yes C5 C4 C9 118.7(4) . 1_555 1_555 yes O1 C5 C4 118.7(4) . 1_555 1_555 yes O1 C5 C6 122.2(3) . 1_555 1_555 yes C4 C5 C6 119.0(4) . 1_555 1_555 yes C5 C6 C7 119.8(4) . 1_555 1_555 yes C5 C6 C10 122.4(4) . 1_555 1_555 yes C7 C6 C10 117.6(4) . 1_555 1_555 yes C6 C7 C8 121.1(5) . 1_555 1_555 yes C7 C8 C9 119.3(4) . 1_555 1_555 yes C4 C9 C8 122.1(4) . 1_555 1_555 yes N1 C10 C6 125.6(4) . 1_555 1_555 yes N1 C11 C12 120.5(4) . 1_555 1_555 yes N1 C11 C16 122.1(4) . 1_555 1_555 yes C12 C11 C16 117.4(4) . 1_555 1_555 yes C11 C12 C13 121.4(4) . 1_555 1_555 yes C12 C13 C14 120.5(4) . 1_555 1_555 yes O2 C14 C13 116.1(4) . 1_555 1_555 yes O2 C14 C15 125.7(4) . 1_555 1_555 yes C13 C14 C15 118.2(4) . 1_555 1_555 yes C14 C15 C16 122.7(4) . 1_555 1_555 yes C11 C16 C15 119.8(4) . 1_555 1_555 yes C2 C18 C19 115.4(4) . 1_555 2_655 yes C18 C19 C20 119.0(3) . 2_655 2_655 yes C18 C19 C24 123.5(4) . 2_655 2_655 yes C20 C19 C24 117.5(4) . 1_555 1_555 yes O3 C20 C19 118.5(4) . 1_555 1_555 yes O3 C20 C21 121.0(3) . 1_555 1_555 yes C19 C20 C21 120.5(3) . 1_555 1_555 yes C20 C21 C22 119.3(3) . 1_555 1_555 yes C20 C21 C25 121.8(3) . 1_555 1_555 yes C22 C21 C25 118.4(4) . 1_555 1_555 yes C21 C22 C23 119.5(4) . 1_555 1_555 yes C22 C23 C24 120.6(4) . 1_555 1_555 yes C19 C24 C23 122.4(4) . 1_555 1_555 yes N2 C25 C21 127.2(4) . 1_555 1_555 yes N2 C26 C27 122.3(4) . 1_555 1_555 yes N2 C26 C31 118.6(4) . 1_555 1_555 yes C27 C26 C31 119.1(4) . 1_555 1_555 yes C26 C27 C28 120.0(5) . 1_555 1_555 yes C27 C28 C29 121.0(5) . 1_555 1_555 yes O4 C29 C28 115.7(5) . 1_555 1_555 yes O4 C29 C30 124.9(5) . 1_555 1_555 yes C28 C29 C30 119.4(4) . 1_555 1_555 yes C29 C30 C31 119.2(4) . 1_555 1_555 yes C26 C31 C30 121.2(4) . 1_555 1_555 yes O6 C33 C34 124(1) . 1_555 2_666 yes O6 C34 C33 130(1) . 1_555 2_666 yes O7 C35 C36 126.6(9) . 1_555 2_766 yes O7 C36 C35 132.0(7) . 1_555 2_766 yes #------------------------------------------------------------------------------ loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag TI O1 C4 C5 -35(1) 1_555 1_555 1_555 1_555 yes TI O1 C4 C9 -33(1) 1_555 1_555 1_555 1_555 yes TI O1 C5 C6 -8.8(6) 1_555 1_555 1_555 1_555 yes TI O1 C6 C7 174.9(5) 1_555 1_555 1_555 1_555 yes TI O1 C6 C10 -10.4(3) 1_555 1_555 1_555 1_555 yes TI O3 C19 C20 -55(1) 1_555 1_555 1_555 1_555 yes TI O3 C19 C24 -53(1) 1_555 1_555 1_555 1_555 yes TI O3 C20 C21 -15.2(7) 1_555 1_555 1_555 1_555 yes TI O3 C21 C22 171.8(6) 1_555 1_555 1_555 1_555 yes TI O3 C21 C25 -15.8(3) 1_555 1_555 1_555 1_555 yes TI O5 TI O1 99.0(1) 1_555 2_655 2_655 2_655 yes TI O5 TI O3 -95.4(1) 1_555 2_655 2_655 2_655 yes TI O5 TI O5 0.0 1_555 2_655 2_655 1_555 yes TI O5 TI N1 46(1) 1_555 2_655 2_655 2_655 yes TI O5 TI N2 -176.0(1) 1_555 2_655 2_655 2_655 yes TI N1 C10 C11 -179.2(5) 1_555 1_555 1_555 1_555 yes TI N1 C11 C12 -54.7(5) 1_555 1_555 1_555 1_555 yes TI N1 C11 C16 124.8(4) 1_555 1_555 1_555 1_555 yes TI N2 C25 C26 -179.9(6) 1_555 1_555 1_555 1_555 yes TI N2 C26 C27 128.7(4) 1_555 1_555 1_555 1_555 yes TI N2 C26 C28 129.9(5) 1_555 1_555 1_555 1_555 yes TI N2 C26 C31 -49.9(5) 1_555 1_555 1_555 1_555 yes O1 C4 C5 C6 -178.3(6) 1_555 1_555 1_555 1_555 yes O1 C5 C6 C7 -179.5(4) 1_555 1_555 1_555 1_555 yes O1 C5 C6 C10 -5.3(6) 1_555 1_555 1_555 1_555 yes O1 C6 C7 C8 -1.6(9) 1_555 1_555 1_555 1_555 yes O1 C6 C7 C9 -0.5(6) 1_555 1_555 1_555 1_555 yes O1 C6 C10 C11 -5.0(9) 1_555 1_555 1_555 1_555 yes O2 C13 C14 C15 179.0(8) 1_555 1_555 1_555 1_555 yes O2 C13 C14 C16 -179.4(5) 1_555 1_555 1_555 1_555 yes O2 C13 C14 C17 19.8(5) 1_555 1_555 1_555 1_555 yes O2 C13 C15 C16 -177.8(4) 1_555 1_555 1_555 1_555 yes O2 C14 C15 C16 -177.8(5) 1_555 1_555 1_555 1_555 yes O3 C19 C20 C21 -178.0(7) 1_555 1_555 1_555 1_555 yes O3 C20 C21 C22 -178.8(4) 1_555 1_555 1_555 1_555 yes O3 C20 C21 C25 -6.6(6) 1_555 1_555 1_555 1_555 yes O3 C21 C22 C23 -4.5(9) 1_555 1_555 1_555 1_555 yes O3 C21 C22 C24 -2.0(7) 1_555 1_555 1_555 1_555 yes O3 C21 C25 C26 -6(1) 1_555 1_555 1_555 1_555 yes O4 C28 C29 C30 179.8(7) 1_555 1_555 1_555 1_555 yes O4 C28 C29 C32 3.5(4) 1_555 1_555 1_555 1_555 yes O4 C29 C30 C31 178.9(4) 1_555 1_555 1_555 1_555 yes O6 C33 C34 C34 159(2) 1_555 1_555 1_555 2_666 yes O6 C34 C34 O6 -180.0 1_555 1_555 2_666 2_666 yes O6 C34 C34 C33 11(1) 1_555 1_555 2_666 1_555 yes O6 C34 O6 C33 13(1) 1_555 2_666 2_666 2_666 yes O6 C34 C33 C34 17(2) 1_555 2_666 1_555 1_555 yes O7 C35 C36 C36 151.6(9) 1_555 1_555 1_555 2_766 yes O7 C36 C36 O7 180.0 1_555 1_555 2_766 2_766 yes O7 C36 C36 C35 19.4(6) 1_555 1_555 2_766 1_555 yes N1 C10 C11 C12 -75.9(5) 1_555 1_555 1_555 1_555 yes N1 C10 C11 C16 135.3(5) 1_555 1_555 1_555 1_555 yes N1 C11 C12 C13 -179.8(4) 1_555 1_555 1_555 1_555 yes N1 C11 C12 C16 179.5(7) 1_555 1_555 1_555 1_555 yes N2 C25 C26 C27 137.8(5) 1_555 1_555 1_555 1_555 yes N2 C25 C26 C28 153.3(5) 1_555 1_555 1_555 1_555 yes N2 C25 C26 C31 -69.9(6) 1_555 1_555 1_555 1_555 yes N2 C26 C27 C28 178.9(4) 1_555 1_555 1_555 1_555 yes N2 C26 C27 C31 -178.6(6) 1_555 1_555 1_555 1_555 yes N2 C26 C28 C29 178.2(6) 1_555 1_555 1_555 1_555 yes C1 C2 C3 C4 23.9(5) 1_555 1_555 1_555 1_555 yes C1 C2 C18 C19 -22.5(5) 1_555 1_555 1_555 2_655 yes C2 C3 C4 C5 76.3(4) 1_555 1_555 1_555 1_555 yes C2 C3 C4 C9 -99.3(5) 1_555 1_555 1_555 1_555 yes C2 C18 C19 C20 -75.4(5) 1_555 1_555 2_655 2_655 yes C2 C18 C19 C24 103.4(5) 1_555 1_555 2_655 2_655 yes C3 C4 C5 C6 -173.0(4) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C7 -1.3(6) 1_555 1_555 1_555 1_555 yes C4 C5 C6 C10 172.9(4) 1_555 1_555 1_555 1_555 yes C5 C6 C7 C8 -1.2(7) 1_555 1_555 1_555 1_555 yes C5 C6 C7 C9 -0.1(4) 1_555 1_555 1_555 1_555 yes C5 C6 C10 C11 -2(1) 1_555 1_555 1_555 1_555 yes C6 C7 C8 C9 2.1(8) 1_555 1_555 1_555 1_555 yes C6 C10 C11 C12 -64(1) 1_555 1_555 1_555 1_555 yes C6 C10 C11 C16 146.2(9) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C13 -144.5(4) 1_555 1_555 1_555 1_555 yes C10 C11 C12 C16 -145.2(7) 1_555 1_555 1_555 1_555 yes C11 C12 C13 C14 -1.2(7) 1_555 1_555 1_555 1_555 yes C11 C12 C13 C15 -1.6(5) 1_555 1_555 1_555 1_555 yes C12 C13 C14 C15 -0.8(7) 1_555 1_555 1_555 1_555 yes C12 C13 C14 C16 0.8(5) 1_555 1_555 1_555 1_555 yes C12 C13 C14 C17 -159.9(6) 1_555 1_555 1_555 1_555 yes C12 C13 C15 C16 2.1(4) 1_555 1_555 1_555 1_555 yes C13 C14 C15 C16 3.3(8) 1_555 1_555 1_555 1_555 yes C18 C19 C20 C21 175.4(4) 1_555 2_655 2_655 2_655 yes C18 C19 C24 C23 -176.8(5) 1_555 2_655 2_655 2_655 yes C19 C20 C21 C22 -0.9(6) 1_555 1_555 1_555 1_555 yes C19 C20 C21 C25 171.3(4) 1_555 1_555 1_555 1_555 yes C20 C21 C22 C23 -3.4(7) 1_555 1_555 1_555 1_555 yes C20 C21 C22 C24 -0.9(4) 1_555 1_555 1_555 1_555 yes C20 C21 C25 C26 -3(1) 1_555 1_555 1_555 1_555 yes C21 C22 C23 C24 5.0(8) 1_555 1_555 1_555 1_555 yes C21 C25 C26 C27 154(1) 1_555 1_555 1_555 1_555 yes C21 C25 C26 C28 169.9(9) 1_555 1_555 1_555 1_555 yes C21 C25 C26 C31 -53(1) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C28 155.1(4) 1_555 1_555 1_555 1_555 yes C25 C26 C27 C31 157.6(5) 1_555 1_555 1_555 1_555 yes C25 C26 C28 C29 148.7(3) 1_555 1_555 1_555 1_555 yes C26 C27 C28 C29 0.3(7) 1_555 1_555 1_555 1_555 yes C26 C28 C29 C30 1.6(4) 1_555 1_555 1_555 1_555 yes C26 C28 C29 C32 -174.7(6) 1_555 1_555 1_555 1_555 yes C27 C28 C29 C30 1.4(7) 1_555 1_555 1_555 1_555 yes C27 C28 C29 C32 -174.8(5) 1_555 1_555 1_555 1_555 yes C28 C29 C30 C31 -0.8(6) 1_555 1_555 1_555 1_555 yes #------------------------------------------------------------------------------ loop_ _geom_contact_atom_site_label_1 _geom_contact_atom_site_label_2 _geom_contact_distance _geom_contact_site_symmetry_1 _geom_contact_site_symmetry_2 _geom_contact_publ_flag #------------------------------------------------------------------------------