Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'K. Molloy' _publ_contact_author_address ; School of Chemistry University of Bath Claverton Down BATH BA2 7AY UNITED KINGDOM ; _publ_contact_author_email CHSKCM@BATH.AC.UK _publ_section_title ; Synthesis and Characterisation of New Titanium Amino-alkoxides: Precursors for the formation of TiO2 Materials ; loop_ _publ_author_name 'K. Molloy' 'Nathan Hollingsworth' 'Miki Kanna' 'Garbriele I. Kociok-Kohn' 'Sumpun Wongnawa' data_h06kcm24_compound1 _database_code_depnum_ccdc_archive 'CCDC 657058' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C26 H64 N4 O8 Ti2' _chemical_formula_sum 'C26 H64 N4 O8 Ti2' _chemical_formula_weight 656.61 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 triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1309(2) _cell_length_b 12.6399(3) _cell_length_c 17.1215(6) _cell_angle_alpha 69.9053(10) _cell_angle_beta 76.8434(10) _cell_angle_gamma 81.660(2) _cell_volume 1802.30(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 35246 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 26.373 _exptl_crystal_description 'irregular shape' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.210 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8674 _exptl_absorpt_correction_T_max 0.9760 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '\f and \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23383 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.90 _diffrn_reflns_theta_max 26.16 _reflns_number_total 7052 _reflns_number_gt 5058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _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 ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0559P)^2^+1.1854P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7052 _refine_ls_number_parameters 410 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0799 _refine_ls_R_factor_gt 0.0493 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1180 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.001 _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 0.98296(5) 0.36473(4) 0.01492(3) 0.02880(14) Uani 1 1 d . . . O1 O 1.0212(2) 0.24311(15) 0.10891(12) 0.0347(4) Uani 1 1 d . . . O2 O 0.8582(2) 0.30712(17) -0.02861(13) 0.0390(5) Uani 1 1 d . . . O3 O 1.1588(2) 0.33379(16) -0.05043(13) 0.0390(5) Uani 1 1 d . . . O4 O 0.92195(19) 0.52460(15) -0.05192(11) 0.0298(4) Uani 1 1 d . . . N1 N 0.7556(2) 0.35636(19) 0.12283(15) 0.0319(5) Uani 1 1 d . . . N2 N 0.8272(3) -0.0065(2) 0.25931(16) 0.0416(6) Uani 1 1 d . . . C1 C 0.7629(3) 0.4125(3) 0.18453(19) 0.0383(7) Uani 1 1 d . . . H1A H 0.7640 0.4942 0.1561 0.057 Uiso 1 1 calc R . . H1B H 0.8549 0.3842 0.2078 0.057 Uiso 1 1 calc R . . H1C H 0.6746 0.3962 0.2305 0.057 Uiso 1 1 calc R . . C2 C 0.6133(3) 0.3972(3) 0.0917(2) 0.0419(7) Uani 1 1 d . . . H2A H 0.6082 0.3637 0.0487 0.063 Uiso 1 1 calc R . . H2B H 0.6091 0.4797 0.0667 0.063 Uiso 1 1 calc R . . H2C H 0.5280 0.3755 0.1390 0.063 Uiso 1 1 calc R . . C3 C 0.7573(3) 0.2331(2) 0.16372(18) 0.0338(6) Uani 1 1 d . . . H3A H 0.7274 0.1980 0.1267 0.041 Uiso 1 1 calc R . . H3B H 0.6841 0.2150 0.2181 0.041 Uiso 1 1 calc R . . C4 C 0.9150(3) 0.1858(2) 0.17983(18) 0.0340(6) Uani 1 1 d . . . H4 H 0.9308 0.1987 0.2317 0.041 Uiso 1 1 calc R . . C5 C 0.9387(3) 0.0605(2) 0.19099(19) 0.0384(7) Uani 1 1 d . . . H5A H 0.9337 0.0493 0.1372 0.046 Uiso 1 1 calc R . . H5B H 1.0409 0.0326 0.2032 0.046 Uiso 1 1 calc R . . C6 C 0.8398(4) -0.1211(3) 0.2564(3) 0.0547(9) Uani 1 1 d . . . H6A H 0.9406 -0.1562 0.2644 0.082 Uiso 1 1 calc R . . H6B H 0.8236 -0.1192 0.2013 0.082 Uiso 1 1 calc R . . H6C H 0.7637 -0.1649 0.3015 0.082 Uiso 1 1 calc R . . C7 C 0.8471(5) -0.0093(3) 0.3416(2) 0.0686(11) Uani 1 1 d . . . H7A H 0.9504 -0.0381 0.3489 0.103 Uiso 1 1 calc R . . H7B H 0.7758 -0.0588 0.3861 0.103 Uiso 1 1 calc R . . H7C H 0.8286 0.0672 0.3456 0.103 Uiso 1 1 calc R . . C8 C 0.8634(4) 0.2635(3) -0.0940(2) 0.0469(8) Uani 1 1 d . . . H8A H 0.9617 0.2772 -0.1335 0.056 Uiso 1 1 calc R . . H8B H 0.7830 0.3032 -0.1261 0.056 Uiso 1 1 calc R . . C9 C 0.8432(4) 0.1400(3) -0.0607(3) 0.0635(10) Uani 1 1 d . . . H9A H 0.9251 0.1001 -0.0309 0.095 Uiso 1 1 calc R . . H9B H 0.8449 0.1124 -0.1078 0.095 Uiso 1 1 calc R . . H9C H 0.7463 0.1262 -0.0213 0.095 Uiso 1 1 calc R . . C10 C 1.2581(4) 0.2377(3) -0.0521(3) 0.0579(9) Uani 1 1 d . . . H10A H 1.2479 0.2138 -0.0997 0.069 Uiso 1 1 calc R . . H10B H 1.2296 0.1751 0.0011 0.069 Uiso 1 1 calc R . . C11 C 1.4165(4) 0.2596(4) -0.0615(3) 0.0671(11) Uani 1 1 d . . . H11A H 1.4442 0.3233 -0.1131 0.101 Uiso 1 1 calc R . . H11B H 1.4819 0.1922 -0.0656 0.101 Uiso 1 1 calc R . . H11C H 1.4287 0.2777 -0.0123 0.101 Uiso 1 1 calc R . . C12 C 0.7993(3) 0.5593(2) -0.09699(18) 0.0336(6) Uani 1 1 d . . . H12A H 0.7440 0.6274 -0.0855 0.040 Uiso 1 1 calc R . . H12B H 0.7286 0.4986 -0.0752 0.040 Uiso 1 1 calc R . . C13 C 0.8486(3) 0.5849(3) -0.19101(19) 0.0421(7) Uani 1 1 d . . . H13A H 0.9094 0.6505 -0.2142 0.063 Uiso 1 1 calc R . . H13B H 0.7596 0.6015 -0.2174 0.063 Uiso 1 1 calc R . . H13C H 0.9089 0.5195 -0.2029 0.063 Uiso 1 1 calc R . . Ti2 Ti 0.57021(5) 0.36653(4) 0.51769(3) 0.03099(15) Uani 1 1 d . . . O5 O 0.4977(2) 0.24416(16) 0.61043(13) 0.0378(5) Uani 1 1 d . A . O7 O 0.7647(2) 0.31644(17) 0.48275(13) 0.0413(5) Uani 1 1 d . . . O6 O 0.4855(2) 0.32767(17) 0.44619(13) 0.0426(5) Uani 1 1 d . . . O8 O 0.61561(19) 0.52852(15) 0.45250(12) 0.0313(4) Uani 1 1 d . . . N3 N 0.6823(3) 0.3680(2) 0.63322(15) 0.0360(6) Uani 1 1 d . . . N4 N 0.6547(3) 0.0008(2) 0.76898(18) 0.0467(7) Uani 1 1 d . . . C21 C 0.5852(4) 0.4238(3) 0.6916(2) 0.0429(7) Uani 1 1 d . A . H21A H 0.4878 0.3901 0.7128 0.064 Uiso 1 1 calc R . . H21B H 0.5692 0.5046 0.6614 0.064 Uiso 1 1 calc R . . H21C H 0.6341 0.4136 0.7393 0.064 Uiso 1 1 calc R . . C22 C 0.8309(3) 0.4158(3) 0.6085(2) 0.0486(8) Uani 1 1 d . A . H22A H 0.8758 0.3976 0.6588 0.073 Uiso 1 1 calc R . . H22B H 0.8182 0.4979 0.5828 0.073 Uiso 1 1 calc R . . H22C H 0.8972 0.3833 0.5674 0.073 Uiso 1 1 calc R . . C23 C 0.7015(3) 0.2450(2) 0.6760(2) 0.0404(7) Uani 1 1 d . A . H23A H 0.7240 0.2301 0.7329 0.048 Uiso 1 1 calc R . . H23B H 0.7871 0.2116 0.6427 0.048 Uiso 1 1 calc R . . C24 C 0.5577(3) 0.1913(2) 0.68424(19) 0.0377(7) Uani 1 1 d . . . H24 H 0.4828 0.2026 0.7338 0.045 Uiso 1 1 calc R A . C25 C 0.5856(3) 0.0652(2) 0.6966(2) 0.0414(7) Uani 1 1 d . A . H25A H 0.4881 0.0342 0.7035 0.050 Uiso 1 1 calc R . . H25B H 0.6515 0.0548 0.6448 0.050 Uiso 1 1 calc R . . C26 C 0.7019(4) -0.1140(3) 0.7669(3) 0.0605(10) Uani 1 1 d . . . H26A H 0.7502 -0.1561 0.8154 0.091 Uiso 1 1 calc R . . H26B H 0.7735 -0.1110 0.7142 0.091 Uiso 1 1 calc R . . H26C H 0.6134 -0.1519 0.7699 0.091 Uiso 1 1 calc R . . C27 C 0.5512(5) -0.0051(3) 0.8481(2) 0.0709(11) Uani 1 1 d . . . H27A H 0.4591 -0.0378 0.8498 0.106 Uiso 1 1 calc R . . H27B H 0.5258 0.0711 0.8522 0.106 Uiso 1 1 calc R . . H27C H 0.5988 -0.0525 0.8956 0.106 Uiso 1 1 calc R . . C28 C 0.3890(10) 0.2465(8) 0.4503(7) 0.052(2) Uani 0.65 1 d P A 1 H28A H 0.3190 0.2824 0.4104 0.062 Uiso 0.65 1 calc PR A 1 H28B H 0.3279 0.2200 0.5082 0.062 Uiso 0.65 1 calc PR A 1 C29 C 0.4743(14) 0.1499(9) 0.4290(8) 0.136(5) Uani 0.65 1 d P A 1 H29A H 0.4043 0.0965 0.4313 0.203 Uiso 0.65 1 calc PR A 1 H29B H 0.5408 0.1124 0.4697 0.203 Uiso 0.65 1 calc PR A 1 H29C H 0.5350 0.1759 0.3717 0.203 Uiso 0.65 1 calc PR A 1 C30 C 0.8566(13) 0.2761(8) 0.4186(7) 0.047(2) Uani 0.65 1 d P B 1 H30A H 0.9328 0.3304 0.3836 0.056 Uiso 0.65 1 calc PR B 1 H30B H 0.7940 0.2674 0.3813 0.056 Uiso 0.65 1 calc PR B 1 C31 C 0.9351(13) 0.1615(8) 0.4617(7) 0.093(4) Uani 0.65 1 d P B 1 H31A H 1.0016 0.1332 0.4185 0.139 Uiso 0.65 1 calc PR B 1 H31B H 0.8590 0.1076 0.4946 0.139 Uiso 0.65 1 calc PR B 1 H31C H 0.9947 0.1707 0.4996 0.139 Uiso 0.65 1 calc PR B 1 C28A C 0.456(2) 0.217(2) 0.4491(16) 0.076(6) Uani 0.35 1 d P A 2 H28C H 0.5487 0.1792 0.4238 0.092 Uiso 0.35 1 calc PR A 2 H28D H 0.4230 0.1688 0.5084 0.092 Uiso 0.35 1 calc PR A 2 C29A C 0.341(3) 0.2332(18) 0.4020(15) 0.167(11) Uani 0.35 1 d P A 2 H29D H 0.3132 0.1597 0.4051 0.251 Uiso 0.35 1 calc PR A 2 H29E H 0.3781 0.2768 0.3427 0.251 Uiso 0.35 1 calc PR A 2 H29F H 0.2530 0.2744 0.4256 0.251 Uiso 0.35 1 calc PR A 2 C30A C 0.837(3) 0.2401(16) 0.4431(12) 0.048(4) Uani 0.35 1 d P B 2 H30C H 0.8088 0.1633 0.4795 0.058 Uiso 0.35 1 calc PR B 2 H30D H 0.8017 0.2569 0.3893 0.058 Uiso 0.35 1 calc PR B 2 C31A C 0.989(2) 0.241(3) 0.4263(15) 0.141(11) Uani 0.35 1 d P B 2 H31D H 1.0332 0.1889 0.3946 0.212 Uiso 0.35 1 calc PR B 2 H31E H 1.0259 0.2173 0.4796 0.212 Uiso 0.35 1 calc PR B 2 H31F H 1.0179 0.3175 0.3925 0.212 Uiso 0.35 1 calc PR B 2 C32 C 0.7615(3) 0.5688(2) 0.41093(18) 0.0346(6) Uani 1 1 d . A . H32A H 0.8394 0.5145 0.4379 0.041 Uiso 1 1 calc R . . H32B H 0.7677 0.6419 0.4188 0.041 Uiso 1 1 calc R . . C33 C 0.7948(3) 0.5844(3) 0.31727(19) 0.0430(7) Uani 1 1 d . . . H33A H 0.7790 0.5144 0.3087 0.064 Uiso 1 1 calc R A . H33B H 0.8997 0.6029 0.2935 0.064 Uiso 1 1 calc R . . H33C H 0.7272 0.6459 0.2888 0.064 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 0.0285(3) 0.0228(3) 0.0312(3) -0.0042(2) -0.0044(2) -0.00285(18) O1 0.0306(10) 0.0266(10) 0.0376(11) -0.0002(8) -0.0035(8) -0.0036(7) O2 0.0424(11) 0.0364(12) 0.0408(12) -0.0137(10) -0.0075(9) -0.0085(8) O3 0.0367(11) 0.0304(11) 0.0395(12) -0.0061(9) 0.0021(9) 0.0024(8) O4 0.0280(9) 0.0257(10) 0.0321(10) -0.0035(8) -0.0082(8) -0.0012(7) N1 0.0296(12) 0.0270(12) 0.0340(13) -0.0042(10) -0.0052(10) -0.0015(9) N2 0.0422(14) 0.0268(13) 0.0441(15) 0.0008(11) -0.0011(11) -0.0076(10) C1 0.0387(16) 0.0350(16) 0.0374(17) -0.0099(13) -0.0026(13) -0.0021(12) C2 0.0296(15) 0.0455(18) 0.0432(18) -0.0073(15) -0.0053(13) -0.0002(12) C3 0.0323(14) 0.0266(15) 0.0353(16) -0.0025(12) -0.0017(12) -0.0060(11) C4 0.0334(15) 0.0267(15) 0.0329(15) -0.0009(12) -0.0003(12) -0.0050(11) C5 0.0378(16) 0.0288(15) 0.0416(17) -0.0043(13) -0.0029(13) -0.0058(11) C6 0.0471(19) 0.0298(17) 0.078(3) -0.0067(17) -0.0051(17) -0.0105(13) C7 0.095(3) 0.050(2) 0.044(2) -0.0018(18) 0.008(2) -0.021(2) C8 0.0485(18) 0.048(2) 0.052(2) -0.0239(17) -0.0122(15) -0.0036(14) C9 0.073(2) 0.049(2) 0.072(3) -0.029(2) -0.004(2) -0.0113(18) C10 0.049(2) 0.052(2) 0.065(2) -0.0200(19) -0.0063(17) 0.0154(16) C11 0.055(2) 0.073(3) 0.072(3) -0.030(2) -0.0101(19) 0.0126(18) C12 0.0273(14) 0.0350(16) 0.0348(16) -0.0041(13) -0.0111(12) -0.0003(11) C13 0.0385(16) 0.0472(19) 0.0390(17) -0.0094(15) -0.0130(13) -0.0005(13) Ti2 0.0316(3) 0.0252(3) 0.0334(3) -0.0037(2) -0.0088(2) -0.00361(19) O5 0.0387(11) 0.0306(11) 0.0395(12) 0.0017(9) -0.0164(9) -0.0067(8) O7 0.0377(11) 0.0366(12) 0.0452(12) -0.0113(10) -0.0074(9) 0.0048(8) O6 0.0554(13) 0.0334(12) 0.0422(12) -0.0082(10) -0.0173(10) -0.0110(9) O8 0.0271(9) 0.0284(10) 0.0334(10) -0.0023(8) -0.0049(8) -0.0065(7) N3 0.0360(13) 0.0293(13) 0.0392(14) -0.0023(11) -0.0113(11) -0.0072(9) N4 0.0538(16) 0.0266(14) 0.0559(18) 0.0006(12) -0.0258(13) -0.0014(11) C21 0.0537(19) 0.0368(17) 0.0399(18) -0.0075(14) -0.0181(14) -0.0056(13) C22 0.0463(18) 0.048(2) 0.051(2) -0.0036(16) -0.0197(15) -0.0179(14) C23 0.0402(16) 0.0349(17) 0.0414(17) -0.0009(13) -0.0161(13) -0.0027(12) C24 0.0388(16) 0.0287(15) 0.0388(17) 0.0006(13) -0.0118(13) -0.0030(11) C25 0.0428(17) 0.0308(16) 0.0459(18) -0.0031(14) -0.0139(14) -0.0018(12) C26 0.057(2) 0.0336(19) 0.086(3) -0.0056(18) -0.0286(19) 0.0019(15) C27 0.110(3) 0.048(2) 0.047(2) 0.0000(18) -0.027(2) 0.000(2) C28 0.062(5) 0.045(5) 0.057(4) -0.018(4) -0.015(4) -0.021(4) C29 0.167(10) 0.088(7) 0.174(11) -0.101(8) 0.050(8) -0.063(7) C30 0.049(5) 0.040(6) 0.034(6) -0.002(4) -0.002(4) 0.014(4) C31 0.113(9) 0.090(6) 0.081(7) -0.049(5) -0.046(6) 0.070(6) C28A 0.094(15) 0.063(14) 0.088(11) -0.029(9) -0.033(13) -0.018(11) C29A 0.28(3) 0.101(15) 0.19(2) -0.045(14) -0.15(2) -0.075(17) C30A 0.075(11) 0.034(10) 0.025(10) 0.003(6) -0.016(8) 0.006(8) C31A 0.071(13) 0.27(3) 0.107(18) -0.12(2) -0.029(12) 0.066(18) C32 0.0286(14) 0.0336(16) 0.0369(16) -0.0045(13) -0.0049(12) -0.0073(11) C33 0.0369(16) 0.051(2) 0.0376(17) -0.0100(15) -0.0025(13) -0.0099(13) _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 1.8122(18) . ? Ti1 O2 1.839(2) . ? Ti1 O1 1.8641(19) . ? Ti1 O4 2.0194(18) . ? Ti1 O4 2.0793(19) 2_765 ? Ti1 N1 2.432(2) . ? Ti1 Ti1 3.3298(9) 2_765 ? O1 C4 1.415(3) . ? O2 C8 1.398(4) . ? O3 C10 1.410(4) . ? O4 C12 1.435(3) . ? O4 Ti1 2.0793(19) 2_765 ? N1 C3 1.472(3) . ? N1 C2 1.474(3) . ? N1 C1 1.478(4) . ? N2 C7 1.450(5) . ? N2 C6 1.453(4) . ? N2 C5 1.466(4) . ? C3 C4 1.524(4) . ? C4 C5 1.518(4) . ? C8 C9 1.490(5) . ? C10 C11 1.474(5) . ? C12 C13 1.501(4) . ? Ti2 O6 1.815(2) . ? Ti2 O7 1.8338(19) . ? Ti2 O5 1.8662(19) . ? Ti2 O8 2.0187(18) . ? Ti2 O8 2.0778(18) 2_666 ? Ti2 N3 2.432(2) . ? Ti2 Ti2 3.3301(10) 2_666 ? O5 C24 1.404(3) . ? O7 C30A 1.37(3) . ? O7 C30 1.418(12) . ? O6 C28 1.421(10) . ? O6 C28A 1.45(2) . ? O8 C32 1.434(3) . ? O8 Ti2 2.0778(18) 2_666 ? N3 C21 1.476(4) . ? N3 C22 1.478(4) . ? N3 C23 1.478(4) . ? N4 C27 1.449(5) . ? N4 C25 1.453(4) . ? N4 C26 1.463(4) . ? C23 C24 1.521(4) . ? C24 C25 1.525(4) . ? C28 C29 1.460(13) . ? C30 C31 1.536(12) . ? C28A C29A 1.42(3) . ? C30A C31A 1.35(3) . ? C32 C33 1.510(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ti1 O2 97.19(9) . . ? O3 Ti1 O1 92.42(8) . . ? O2 Ti1 O1 102.56(9) . . ? O3 Ti1 O4 102.65(8) . . ? O2 Ti1 O4 91.53(8) . . ? O1 Ti1 O4 157.96(9) . . ? O3 Ti1 O4 93.01(8) . 2_765 ? O2 Ti1 O4 161.68(8) . 2_765 ? O1 Ti1 O4 92.13(8) . 2_765 ? O4 Ti1 O4 71.35(8) . 2_765 ? O3 Ti1 N1 165.60(8) . . ? O2 Ti1 N1 80.50(8) . . ? O1 Ti1 N1 74.38(8) . . ? O4 Ti1 N1 91.64(7) . . ? O4 Ti1 N1 93.21(7) 2_765 . ? O3 Ti1 Ti1 99.53(7) . 2_765 ? O2 Ti1 Ti1 127.52(7) . 2_765 ? O1 Ti1 Ti1 125.83(7) . 2_765 ? O4 Ti1 Ti1 36.27(5) . 2_765 ? O4 Ti1 Ti1 35.07(5) 2_765 2_765 ? N1 Ti1 Ti1 93.00(6) . 2_765 ? C4 O1 Ti1 127.57(16) . . ? C8 O2 Ti1 140.11(19) . . ? C10 O3 Ti1 136.6(2) . . ? C12 O4 Ti1 126.15(16) . . ? C12 O4 Ti1 122.64(16) . 2_765 ? Ti1 O4 Ti1 108.65(8) . 2_765 ? C3 N1 C2 108.9(2) . . ? C3 N1 C1 110.4(2) . . ? C2 N1 C1 108.0(2) . . ? C3 N1 Ti1 98.93(15) . . ? C2 N1 Ti1 116.06(18) . . ? C1 N1 Ti1 114.06(16) . . ? C7 N2 C6 109.5(3) . . ? C7 N2 C5 111.4(3) . . ? C6 N2 C5 109.9(2) . . ? N1 C3 C4 109.8(2) . . ? O1 C4 C5 108.4(2) . . ? O1 C4 C3 108.3(2) . . ? C5 C4 C3 111.5(2) . . ? N2 C5 C4 113.1(2) . . ? O2 C8 C9 111.5(3) . . ? O3 C10 C11 112.2(3) . . ? O4 C12 C13 113.5(2) . . ? O6 Ti2 O7 97.05(10) . . ? O6 Ti2 O5 92.78(9) . . ? O7 Ti2 O5 103.16(9) . . ? O6 Ti2 O8 102.79(9) . . ? O7 Ti2 O8 91.37(8) . . ? O5 Ti2 O8 157.29(9) . . ? O6 Ti2 O8 93.85(9) . 2_666 ? O7 Ti2 O8 161.21(9) . 2_666 ? O5 Ti2 O8 91.52(8) . 2_666 ? O8 Ti2 O8 71.25(8) . 2_666 ? O6 Ti2 N3 165.54(9) . . ? O7 Ti2 N3 80.20(9) . . ? O5 Ti2 N3 74.23(8) . . ? O8 Ti2 N3 91.50(8) . . ? O8 Ti2 N3 92.83(8) 2_666 . ? O6 Ti2 Ti2 100.14(7) . 2_666 ? O7 Ti2 Ti2 127.25(7) . 2_666 ? O5 Ti2 Ti2 125.15(7) . 2_666 ? O8 Ti2 Ti2 36.22(5) . 2_666 ? O8 Ti2 Ti2 35.03(5) 2_666 2_666 ? N3 Ti2 Ti2 92.67(6) . 2_666 ? C24 O5 Ti2 127.38(17) . . ? C30A O7 Ti2 137.6(11) . . ? C30 O7 Ti2 141.9(6) . . ? C28 O6 Ti2 138.5(5) . . ? C28A O6 Ti2 129.1(9) . . ? C32 O8 Ti2 126.31(16) . . ? C32 O8 Ti2 122.98(16) . 2_666 ? Ti2 O8 Ti2 108.75(8) . 2_666 ? C21 N3 C22 107.1(2) . . ? C21 N3 C23 110.6(2) . . ? C22 N3 C23 109.1(2) . . ? C21 N3 Ti2 114.75(17) . . ? C22 N3 Ti2 115.98(19) . . ? C23 N3 Ti2 99.03(17) . . ? C27 N4 C25 111.3(3) . . ? C27 N4 C26 108.9(3) . . ? C25 N4 C26 110.2(3) . . ? N3 C23 C24 109.5(2) . . ? O5 C24 C23 109.1(2) . . ? O5 C24 C25 108.5(2) . . ? C23 C24 C25 112.1(2) . . ? N4 C25 C24 114.2(3) . . ? O6 C28 C29 111.7(8) . . ? O7 C30 C31 108.2(7) . . ? C29A C28A O6 106.5(17) . . ? C31A C30A O7 114(2) . . ? O8 C32 C33 112.9(2) . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 26.16 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 0.948 _refine_diff_density_min -0.481 _refine_diff_density_rms 0.065 # Attachment 'compound 7.cif' data_k06kcm8_COMPOUND7 _database_code_depnum_ccdc_archive 'CCDC 657059' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H68 N8 O6 Ti2' _chemical_formula_sum 'C28 H68 N8 O6 Ti2' _chemical_formula_weight 708.70 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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 13.0770(3) _cell_length_b 15.9297(4) _cell_length_c 19.8605(6) _cell_angle_alpha 90.00 _cell_angle_beta 108.4600(10) _cell_angle_gamma 90.00 _cell_volume 3924.24(18) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 30126 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1536 _exptl_absorpt_coefficient_mu 0.452 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8763 _exptl_absorpt_correction_T_max 0.8953 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements Sortav (Blessing 1995) ; _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '163 2.0 degree images with \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 24881 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0362 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 5.56 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4448 _reflns_number_gt 3635 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _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 ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0460P)^2^+4.4429P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4448 _refine_ls_number_parameters 237 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0582 _refine_ls_R_factor_gt 0.0441 _refine_ls_wR_factor_ref 0.1146 _refine_ls_wR_factor_gt 0.1059 _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.001 _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 0.49509(3) 0.63559(2) 0.818945(18) 0.02625(11) Uani 1 1 d . . . O1 O 0.59772(10) 0.63673(8) 0.77315(7) 0.0281(3) Uani 1 1 d . . . O2 O 0.48211(11) 0.52626(8) 0.85060(8) 0.0322(3) Uani 1 1 d . . . O3 O 0.50114(11) 0.74385(9) 0.85804(8) 0.0346(3) Uani 1 1 d . . . N1 N 0.65143(13) 0.61472(10) 0.92040(9) 0.0310(4) Uani 1 1 d . . . N2 N 0.48469(15) 0.33387(11) 0.88585(10) 0.0379(4) Uani 1 1 d . . . N3 N 0.32658(14) 0.65356(12) 0.84683(10) 0.0379(4) Uani 1 1 d . . . N4 N 0.5168(9) 0.9294(6) 0.8981(4) 0.0423(15) Uani 0.65 1 d P A 1 N4A N 0.491(2) 0.9288(16) 0.8861(13) 0.088(8) Uani 0.35 1 d P A 2 C1 C 0.56067(16) 0.47907(12) 0.90143(11) 0.0316(4) Uani 1 1 d . . . H1 H 0.5419 0.4779 0.9465 0.038 Uiso 1 1 calc R . . C2 C 0.66873(16) 0.52365(13) 0.91540(12) 0.0340(4) Uani 1 1 d . . . H2A H 0.7208 0.5030 0.9602 0.041 Uiso 1 1 calc R . . H2B H 0.6985 0.5121 0.8763 0.041 Uiso 1 1 calc R . . C3 C 0.74664(17) 0.66191(14) 0.91845(12) 0.0389(5) Uani 1 1 d . . . H3A H 0.8080 0.6475 0.9601 0.058 Uiso 1 1 calc R . . H3B H 0.7320 0.7222 0.9188 0.058 Uiso 1 1 calc R . . H3C H 0.7635 0.6476 0.8751 0.058 Uiso 1 1 calc R . . C4 C 0.62799(19) 0.63516(14) 0.98654(11) 0.0370(4) Uani 1 1 d . . . H4A H 0.6142 0.6955 0.9879 0.056 Uiso 1 1 calc R . . H4B H 0.6899 0.6198 1.0275 0.056 Uiso 1 1 calc R . . H4C H 0.5643 0.6038 0.9881 0.056 Uiso 1 1 calc R . . C5 C 0.56926(18) 0.38897(13) 0.87777(13) 0.0371(5) Uani 1 1 d . . . H5A H 0.5660 0.3893 0.8273 0.045 Uiso 1 1 calc R . . H5B H 0.6403 0.3659 0.9058 0.045 Uiso 1 1 calc R . . C6 C 0.5117(3) 0.24608(15) 0.8806(2) 0.0649(8) Uani 1 1 d . . . H6A H 0.5817 0.2338 0.9159 0.097 Uiso 1 1 calc R . . H6B H 0.5155 0.2348 0.8329 0.097 Uiso 1 1 calc R . . H6C H 0.4562 0.2105 0.8894 0.097 Uiso 1 1 calc R . . C7 C 0.3802(2) 0.35235(17) 0.83422(15) 0.0508(6) Uani 1 1 d . . . H7A H 0.3833 0.3423 0.7862 0.076 Uiso 1 1 calc R . . H7B H 0.3616 0.4112 0.8388 0.076 Uiso 1 1 calc R . . H7C H 0.3253 0.3159 0.8429 0.076 Uiso 1 1 calc R . . C8 C 0.42145(19) 0.78797(14) 0.87658(14) 0.0411(5) Uani 1 1 d . A . H8 H 0.4369 0.7834 0.9291 0.049 Uiso 1 1 calc R . . C9 C 0.31421(18) 0.74523(15) 0.84006(15) 0.0457(5) Uani 1 1 d . . . H9A H 0.2598 0.7642 0.8619 0.055 Uiso 1 1 calc R . . H9B H 0.2886 0.7609 0.7892 0.055 Uiso 1 1 calc R . . C10 C 0.23582(19) 0.61132(18) 0.79540(14) 0.0483(6) Uani 1 1 d . . . H10A H 0.1697 0.6223 0.8072 0.072 Uiso 1 1 calc R . . H10B H 0.2494 0.5507 0.7968 0.072 Uiso 1 1 calc R . . H10C H 0.2275 0.6327 0.7477 0.072 Uiso 1 1 calc R . . C11 C 0.3336(2) 0.62576(16) 0.91801(13) 0.0456(5) Uani 1 1 d . . . H11A H 0.3463 0.5651 0.9219 0.068 Uiso 1 1 calc R . . H11B H 0.2660 0.6387 0.9272 0.068 Uiso 1 1 calc R . . H11C H 0.3934 0.6548 0.9529 0.068 Uiso 1 1 calc R . . C12 C 0.4168(2) 0.88010(16) 0.8571(2) 0.0597(8) Uani 1 1 d . . . H12A H 0.3531 0.9057 0.8658 0.072 Uiso 0.65 1 calc PR A 1 H12B H 0.4068 0.8850 0.8057 0.072 Uiso 0.65 1 calc PR A 1 H12C H 0.4056 0.8830 0.8055 0.072 Uiso 0.35 1 calc PR A 2 H12D H 0.3509 0.9033 0.8645 0.072 Uiso 0.35 1 calc PR A 2 C13 C 0.4904(6) 1.0162(4) 0.9057(4) 0.0673(17) Uani 0.65 1 d P A 1 H13A H 0.5548 1.0457 0.9352 0.101 Uiso 0.65 1 calc PR A 1 H13B H 0.4339 1.0192 0.9283 0.101 Uiso 0.65 1 calc PR A 1 H13C H 0.4648 1.0426 0.8588 0.101 Uiso 0.65 1 calc PR A 1 C14 C 0.5981(5) 0.9214(3) 0.8652(4) 0.0398(11) Uani 0.65 1 d P A 1 H14A H 0.5739 0.9483 0.8184 0.060 Uiso 0.65 1 calc PR A 1 H14B H 0.6121 0.8617 0.8596 0.060 Uiso 0.65 1 calc PR A 1 H14C H 0.6643 0.9485 0.8947 0.060 Uiso 0.65 1 calc PR A 1 C13A C 0.4687(15) 1.0196(9) 0.8582(12) 0.116(7) Uani 0.35 1 d P A 2 H13D H 0.4785 1.0235 0.8114 0.174 Uiso 0.35 1 calc PR A 2 H13E H 0.5189 1.0579 0.8912 0.174 Uiso 0.35 1 calc PR A 2 H13F H 0.3945 1.0349 0.8543 0.174 Uiso 0.35 1 calc PR A 2 C14A C 0.587(3) 0.9134(19) 0.8665(19) 0.154(11) Uani 0.35 1 d P A 2 H14D H 0.6146 0.8570 0.8821 0.231 Uiso 0.35 1 calc PR A 2 H14E H 0.6423 0.9551 0.8894 0.231 Uiso 0.35 1 calc PR A 2 H14F H 0.5695 0.9176 0.8149 0.231 Uiso 0.35 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 0.02739(18) 0.02246(18) 0.03122(19) 0.00098(13) 0.01257(13) 0.00060(12) O1 0.0261(6) 0.0287(7) 0.0312(7) -0.0027(5) 0.0114(5) -0.0015(5) O2 0.0289(7) 0.0249(7) 0.0407(8) 0.0045(6) 0.0080(6) -0.0023(5) O3 0.0365(8) 0.0284(7) 0.0416(8) -0.0029(6) 0.0164(6) 0.0047(6) N1 0.0315(8) 0.0289(8) 0.0342(9) -0.0032(6) 0.0125(7) -0.0029(6) N2 0.0471(11) 0.0215(8) 0.0532(11) -0.0026(7) 0.0274(9) -0.0045(7) N3 0.0341(9) 0.0397(10) 0.0428(10) 0.0052(8) 0.0163(8) 0.0011(7) N4 0.046(4) 0.024(2) 0.060(2) -0.0053(17) 0.021(2) 0.001(2) N4A 0.059(12) 0.038(6) 0.18(2) -0.026(9) 0.056(12) -0.003(6) C1 0.0352(10) 0.0256(9) 0.0363(10) 0.0019(7) 0.0145(8) 0.0013(7) C2 0.0325(10) 0.0283(10) 0.0405(11) 0.0012(8) 0.0107(8) 0.0022(8) C3 0.0335(11) 0.0367(11) 0.0457(12) -0.0015(9) 0.0113(9) -0.0064(8) C4 0.0435(12) 0.0354(11) 0.0325(10) -0.0029(8) 0.0126(9) -0.0005(9) C5 0.0406(11) 0.0284(10) 0.0494(13) -0.0034(9) 0.0242(10) -0.0030(8) C6 0.0706(18) 0.0239(11) 0.116(3) -0.0069(13) 0.0518(18) -0.0059(11) C7 0.0499(14) 0.0458(14) 0.0577(15) -0.0035(11) 0.0186(12) -0.0131(11) C8 0.0446(12) 0.0302(11) 0.0554(14) -0.0010(9) 0.0257(10) 0.0068(9) C9 0.0385(12) 0.0396(12) 0.0645(15) 0.0073(11) 0.0241(11) 0.0104(9) C10 0.0331(11) 0.0627(16) 0.0526(14) -0.0037(11) 0.0185(10) -0.0079(10) C11 0.0476(13) 0.0516(14) 0.0465(13) 0.0084(10) 0.0275(11) 0.0040(10) C12 0.0498(15) 0.0333(13) 0.102(2) 0.0060(13) 0.0334(15) 0.0087(11) C13 0.077(4) 0.025(2) 0.097(4) -0.012(3) 0.023(3) 0.008(2) C14 0.030(2) 0.0241(19) 0.064(3) -0.0025(19) 0.014(2) -0.0032(16) C13A 0.077(9) 0.047(6) 0.22(2) 0.001(12) 0.048(13) 0.000(6) C14A 0.12(2) 0.13(2) 0.17(3) 0.016(18) -0.01(2) -0.024(15) _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 O1 1.8445(13) . ? Ti1 O1 1.8474(14) 2_656 ? Ti1 O2 1.8774(14) . ? Ti1 O3 1.8826(14) . ? Ti1 N1 2.3962(18) . ? Ti1 N3 2.4529(18) . ? Ti1 Ti1 2.7820(7) 2_656 ? O1 Ti1 1.8474(14) 2_656 ? O2 C1 1.408(2) . ? O3 C8 1.399(2) . ? N1 C3 1.465(3) . ? N1 C2 1.476(3) . ? N1 C4 1.477(3) . ? N2 C6 1.454(3) . ? N2 C7 1.455(3) . ? N2 C5 1.460(3) . ? N3 C11 1.456(3) . ? N3 C10 1.462(3) . ? N3 C9 1.471(3) . ? N4 C14 1.419(11) . ? N4 C13 1.444(12) . ? N4 C12 1.522(11) . ? N4A C12 1.23(2) . ? N4A C14A 1.45(4) . ? N4A C13A 1.54(3) . ? C1 C5 1.525(3) . ? C1 C2 1.526(3) . ? C1 H1 1.0000 . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C12 1.514(3) . ? C8 C9 1.521(3) . ? C8 H8 1.0000 . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C12 H12C 0.9900 . ? C12 H12D 0.9900 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 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 O1 Ti1 O1 82.19(6) . 2_656 ? O1 Ti1 O2 109.35(6) . . ? O1 Ti1 O2 103.88(6) 2_656 . ? O1 Ti1 O3 104.61(6) . . ? O1 Ti1 O3 109.15(6) 2_656 . ? O2 Ti1 O3 135.08(7) . . ? O1 Ti1 N1 81.70(6) . . ? O1 Ti1 N1 162.18(6) 2_656 . ? O2 Ti1 N1 74.53(6) . . ? O3 Ti1 N1 82.36(6) . . ? O1 Ti1 N3 162.97(6) . . ? O1 Ti1 N3 82.35(6) 2_656 . ? O2 Ti1 N3 81.36(6) . . ? O3 Ti1 N3 73.94(6) . . ? N1 Ti1 N3 114.50(6) . . ? O1 Ti1 Ti1 41.14(4) . 2_656 ? O1 Ti1 Ti1 41.06(4) 2_656 2_656 ? O2 Ti1 Ti1 111.52(5) . 2_656 ? O3 Ti1 Ti1 113.39(5) . 2_656 ? N1 Ti1 Ti1 122.32(4) . 2_656 ? N3 Ti1 Ti1 123.17(5) . 2_656 ? Ti1 O1 Ti1 97.80(6) . 2_656 ? C1 O2 Ti1 127.77(12) . . ? C8 O3 Ti1 129.12(13) . . ? C3 N1 C2 110.66(16) . . ? C3 N1 C4 109.13(17) . . ? C2 N1 C4 110.85(16) . . ? C3 N1 Ti1 114.36(13) . . ? C2 N1 Ti1 100.83(12) . . ? C4 N1 Ti1 110.81(13) . . ? C6 N2 C7 109.8(2) . . ? C6 N2 C5 111.13(18) . . ? C7 N2 C5 112.08(18) . . ? C11 N3 C10 109.04(19) . . ? C11 N3 C9 111.22(19) . . ? C10 N3 C9 110.6(2) . . ? C11 N3 Ti1 113.48(14) . . ? C10 N3 Ti1 112.16(14) . . ? C9 N3 Ti1 100.13(12) . . ? C14 N4 C13 111.9(7) . . ? C14 N4 C12 110.4(7) . . ? C13 N4 C12 110.9(8) . . ? C12 N4A C14A 113(2) . . ? C12 N4A C13A 112.9(19) . . ? C14A N4A C13A 98(2) . . ? O2 C1 C5 112.93(17) . . ? O2 C1 C2 107.78(15) . . ? C5 C1 C2 109.84(16) . . ? O2 C1 H1 108.7 . . ? C5 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? N1 C2 C1 108.45(16) . . ? N1 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? N1 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C1 113.55(17) . . ? N2 C5 H5A 108.9 . . ? C1 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O3 C8 C12 113.1(2) . . ? O3 C8 C9 107.50(18) . . ? C12 C8 C9 110.8(2) . . ? O3 C8 H8 108.4 . . ? C12 C8 H8 108.4 . . ? C9 C8 H8 108.4 . . ? N3 C9 C8 110.05(18) . . ? N3 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? N3 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N3 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N4A C12 C8 121.9(12) . . ? C8 C12 N4 113.9(4) . . ? N4A C12 H12A 104.0 . . ? C8 C12 H12A 108.8 . . ? N4 C12 H12A 108.8 . . ? N4A C12 H12B 105.0 . . ? C8 C12 H12B 108.8 . . ? N4 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? N4A C12 H12C 106.9 . . ? C8 C12 H12C 106.9 . . ? N4 C12 H12C 110.5 . . ? H12A C12 H12C 107.8 . . ? N4A C12 H12D 106.9 . . ? C8 C12 H12D 106.9 . . ? N4 C12 H12D 111.6 . . ? H12B C12 H12D 106.6 . . ? H12C C12 H12D 106.7 . . ? N4A C13A H13D 109.5 . . ? N4A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? N4A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? N4A C14A H14D 109.5 . . ? N4A C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? N4A C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.430 _refine_diff_density_min -0.351 _refine_diff_density_rms 0.050 data_h06kcm30_Compound9 _database_code_depnum_ccdc_archive 'CCDC 657060' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H89 N12 O6 Ti2,C6 H14' _chemical_formula_sum 'C43 H103 N12 O6 Ti2' _chemical_formula_weight 980.17 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 tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y+3/4, x+1/4, z+1/4' '-x, -y+1/2, z' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-y+5/4, x+3/4, z+3/4' '-x+1/2, -y+1, z+1/2' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'y-3/4, -x-1/4, -z-1/4' 'x, y-1/2, -z' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' 'x+1/2, y, -z+1/2' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 42.8710(6) _cell_length_b 42.8710(6) _cell_length_c 12.3339(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 22668.9(6) _cell_formula_units_Z 16 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 175585 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8592 _exptl_absorpt_coefficient_mu 0.332 _exptl_absorpt_correction_type none _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '353 1.8 degree images with \f and \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72564 _diffrn_reflns_av_R_equivalents 0.0839 _diffrn_reflns_av_sigmaI/netI 0.0824 _diffrn_reflns_limit_h_min -55 _diffrn_reflns_limit_h_max 55 _diffrn_reflns_limit_k_min -55 _diffrn_reflns_limit_k_max 55 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 27.45 _reflns_number_total 12742 _reflns_number_gt 8011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, Processing of X-ray Diffraction Data Collected in Oscillation Mode , Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _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 ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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. Five restraints had to be applied to idealise the bond lengths (C41-C46) of a molecule of hexane solvent, which is disordered about a mirror plane. ; _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^)+(0.0553P)^2^+29.7199P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12742 _refine_ls_number_parameters 619 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0535 _refine_ls_wR_factor_ref 0.1400 _refine_ls_wR_factor_gt 0.1152 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _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 0.158547(10) 0.153398(10) 0.12662(4) 0.02477(11) Uani 1 1 d . . . Ti2 Ti 0.159457(10) 0.170370(10) -0.09243(4) 0.02458(11) Uani 1 1 d . . . O1 O 0.13046(4) 0.16101(4) 0.01476(13) 0.0269(4) Uani 1 1 d . . . O2 O 0.18730(4) 0.16316(4) 0.01946(13) 0.0279(4) Uani 1 1 d . . . O3 O 0.16209(4) 0.10983(4) 0.14638(14) 0.0290(4) Uani 1 1 d . . . O4 O 0.15471(4) 0.18846(4) 0.21903(14) 0.0298(4) Uani 1 1 d . . . O5 O 0.16024(4) 0.21396(4) -0.11576(14) 0.0290(4) Uani 1 1 d . . . O6 O 0.15929(4) 0.13518(4) -0.18412(14) 0.0277(4) Uani 1 1 d . . . N1 N 0.20535(5) 0.14480(5) 0.22753(17) 0.0299(5) Uani 1 1 d . . . N2 N 0.22495(5) 0.06197(5) 0.02172(19) 0.0373(5) Uani 1 1 d . . . N3 N 0.17060(6) 0.03915(5) 0.1998(2) 0.0387(6) Uani 1 1 d . . . N4 N 0.11232(5) 0.14563(5) 0.22919(17) 0.0293(5) Uani 1 1 d . . . N5 N 0.08717(5) 0.24222(5) 0.18700(19) 0.0367(5) Uani 1 1 d . . . N6 N 0.14563(6) 0.24172(5) 0.38624(18) 0.0392(6) Uani 1 1 d . . . N7 N 0.20760(5) 0.18179(5) -0.18520(18) 0.0314(5) Uani 1 1 d . . . N8 N 0.21911(5) 0.26530(5) 0.0161(2) 0.0392(6) Uani 1 1 d . . . N9 N 0.16449(5) 0.28442(5) -0.18076(18) 0.0348(5) Uani 1 1 d . . . N10 N 0.11385(5) 0.17451(5) -0.20240(17) 0.0281(5) Uani 1 1 d . . . N11 N 0.09521(5) 0.07706(5) -0.16369(18) 0.0318(5) Uani 1 1 d . . . N12 N 0.15774(5) 0.08141(5) -0.35210(17) 0.0328(5) Uani 1 1 d . . . C1 C 0.19067(6) 0.09286(6) 0.1462(2) 0.0305(6) Uani 1 1 d . . . C2 C 0.21734(6) 0.11633(6) 0.1746(2) 0.0323(6) Uani 1 1 d . . . H2A H 0.2325 0.1060 0.2234 0.039 Uiso 1 1 calc R . . H2B H 0.2285 0.1222 0.1073 0.039 Uiso 1 1 calc R . . C3 C 0.19983(7) 0.14001(7) 0.3438(2) 0.0372(6) Uani 1 1 d . . . H3A H 0.2195 0.1347 0.3796 0.056 Uiso 1 1 calc R . . H3B H 0.1849 0.1230 0.3539 0.056 Uiso 1 1 calc R . . H3C H 0.1914 0.1592 0.3756 0.056 Uiso 1 1 calc R . . C4 C 0.22799(6) 0.17051(7) 0.2154(2) 0.0382(7) Uani 1 1 d . . . H4A H 0.2475 0.1650 0.2521 0.057 Uiso 1 1 calc R . . H4B H 0.2194 0.1895 0.2478 0.057 Uiso 1 1 calc R . . H4C H 0.2321 0.1741 0.1382 0.057 Uiso 1 1 calc R . . C5 C 0.19012(6) 0.06604(6) 0.2290(2) 0.0346(6) Uani 1 1 d . . . H5A H 0.2118 0.0586 0.2397 0.042 Uiso 1 1 calc R . . H5B H 0.1827 0.0744 0.2992 0.042 Uiso 1 1 calc R . . C6 C 0.13749(7) 0.04547(7) 0.2102(3) 0.0550(9) Uani 1 1 d . . . H6A H 0.1256 0.0271 0.1877 0.083 Uiso 1 1 calc R . . H6B H 0.1319 0.0632 0.1640 0.083 Uiso 1 1 calc R . . H6C H 0.1326 0.0504 0.2859 0.083 Uiso 1 1 calc R . . C7 C 0.17901(9) 0.01226(7) 0.2663(3) 0.0574(9) Uani 1 1 d . . . H7A H 0.1733 0.0163 0.3419 0.086 Uiso 1 1 calc R . . H7B H 0.2015 0.0086 0.2613 0.086 Uiso 1 1 calc R . . H7C H 0.1678 -0.0062 0.2403 0.086 Uiso 1 1 calc R . . C8 C 0.19583(6) 0.07987(6) 0.0318(2) 0.0318(6) Uani 1 1 d . . . H8A H 0.1780 0.0662 0.0124 0.038 Uiso 1 1 calc R . . H8B H 0.1963 0.0974 -0.0205 0.038 Uiso 1 1 calc R . . C9 C 0.24703(8) 0.07563(8) -0.0530(3) 0.0615(10) Uani 1 1 d . . . H9A H 0.2395 0.0730 -0.1274 0.092 Uiso 1 1 calc R . . H9B H 0.2673 0.0653 -0.0451 0.092 Uiso 1 1 calc R . . H9C H 0.2493 0.0979 -0.0372 0.092 Uiso 1 1 calc R . . C10 C 0.22023(9) 0.02960(8) -0.0058(3) 0.0690(11) Uani 1 1 d . . . H10A H 0.2068 0.0198 0.0487 0.103 Uiso 1 1 calc R . . H10B H 0.2404 0.0189 -0.0075 0.103 Uiso 1 1 calc R . . H10C H 0.2103 0.0281 -0.0772 0.103 Uiso 1 1 calc R . . C11 C 0.12576(6) 0.20232(6) 0.2490(2) 0.0297(6) Uani 1 1 d . . . C12 C 0.09957(6) 0.17752(6) 0.2345(2) 0.0321(6) Uani 1 1 d . . . H12A H 0.0848 0.1790 0.2960 0.038 Uiso 1 1 calc R . . H12B H 0.0879 0.1820 0.1671 0.038 Uiso 1 1 calc R . . C13 C 0.11906(7) 0.13348(7) 0.3382(2) 0.0372(6) Uani 1 1 d . . . H13A H 0.1347 0.1468 0.3734 0.056 Uiso 1 1 calc R . . H13B H 0.1271 0.1122 0.3324 0.056 Uiso 1 1 calc R . . H13C H 0.0999 0.1334 0.3814 0.056 Uiso 1 1 calc R . . C14 C 0.08996(6) 0.12457(6) 0.1764(2) 0.0354(6) Uani 1 1 d . . . H14A H 0.0985 0.1034 0.1748 0.053 Uiso 1 1 calc R . . H14B H 0.0861 0.1317 0.1022 0.053 Uiso 1 1 calc R . . H14C H 0.0703 0.1246 0.2172 0.053 Uiso 1 1 calc R . . C15 C 0.12660(7) 0.21392(6) 0.3676(2) 0.0363(6) Uani 1 1 d . . . H15A H 0.1050 0.2184 0.3910 0.044 Uiso 1 1 calc R . . H15B H 0.1346 0.1969 0.4140 0.044 Uiso 1 1 calc R . . C16 C 0.17883(8) 0.23538(8) 0.3827(3) 0.0541(9) Uani 1 1 d . . . H16A H 0.1841 0.2197 0.4374 0.081 Uiso 1 1 calc R . . H16B H 0.1904 0.2546 0.3977 0.081 Uiso 1 1 calc R . . H16C H 0.1845 0.2276 0.3107 0.081 Uiso 1 1 calc R . . C17 C 0.13741(9) 0.25648(8) 0.4897(3) 0.0597(10) Uani 1 1 d . . . H17A H 0.1485 0.2764 0.4965 0.089 Uiso 1 1 calc R . . H17B H 0.1433 0.2427 0.5496 0.089 Uiso 1 1 calc R . . H17C H 0.1149 0.2603 0.4920 0.089 Uiso 1 1 calc R . . C18 C 0.11885(6) 0.22955(6) 0.1708(2) 0.0326(6) Uani 1 1 d . . . H18A H 0.1343 0.2463 0.1824 0.039 Uiso 1 1 calc R . . H18B H 0.1210 0.2222 0.0951 0.039 Uiso 1 1 calc R . . C19 C 0.08698(8) 0.27170(7) 0.2455(3) 0.0533(9) Uani 1 1 d . . . H19A H 0.0999 0.2698 0.3107 0.080 Uiso 1 1 calc R . . H19B H 0.0656 0.2769 0.2665 0.080 Uiso 1 1 calc R . . H19C H 0.0953 0.2882 0.1988 0.080 Uiso 1 1 calc R . . C20 C 0.07041(8) 0.24610(8) 0.0861(3) 0.0575(9) Uani 1 1 d . . . H20A H 0.0496 0.2546 0.1010 0.086 Uiso 1 1 calc R . . H20B H 0.0684 0.2258 0.0500 0.086 Uiso 1 1 calc R . . H20C H 0.0819 0.2605 0.0391 0.086 Uiso 1 1 calc R . . C21 C 0.18747(6) 0.23294(6) -0.1134(2) 0.0303(6) Uani 1 1 d . . . C22 C 0.21636(6) 0.21155(6) -0.1327(2) 0.0335(6) Uani 1 1 d . . . H22A H 0.2316 0.2227 -0.1791 0.040 Uiso 1 1 calc R . . H22B H 0.2266 0.2071 -0.0624 0.040 Uiso 1 1 calc R . . C23 C 0.20379(7) 0.18573(7) -0.3035(2) 0.0369(6) Uani 1 1 d . . . H23A H 0.2235 0.1930 -0.3351 0.055 Uiso 1 1 calc R . . H23B H 0.1874 0.2011 -0.3178 0.055 Uiso 1 1 calc R . . H23C H 0.1980 0.1657 -0.3362 0.055 Uiso 1 1 calc R . . C24 C 0.23204(6) 0.15835(7) -0.1660(2) 0.0387(7) Uani 1 1 d . . . H24A H 0.2259 0.1386 -0.1997 0.058 Uiso 1 1 calc R . . H24B H 0.2347 0.1553 -0.0878 0.058 Uiso 1 1 calc R . . H24C H 0.2517 0.1656 -0.1977 0.058 Uiso 1 1 calc R . . C25 C 0.18613(6) 0.25861(6) -0.2008(2) 0.0335(6) Uani 1 1 d . . . H25A H 0.2073 0.2674 -0.2093 0.040 Uiso 1 1 calc R . . H25B H 0.1804 0.2487 -0.2705 0.040 Uiso 1 1 calc R . . C26 C 0.17089(8) 0.30971(7) -0.2563(3) 0.0486(8) Uani 1 1 d . . . H26A H 0.1923 0.3170 -0.2461 0.073 Uiso 1 1 calc R . . H26B H 0.1564 0.3269 -0.2429 0.073 Uiso 1 1 calc R . . H26C H 0.1683 0.3022 -0.3308 0.073 Uiso 1 1 calc R . . C27 C 0.13197(7) 0.27531(7) -0.1877(3) 0.0427(7) Uani 1 1 d . . . H27A H 0.1276 0.2673 -0.2606 0.064 Uiso 1 1 calc R . . H27B H 0.1187 0.2934 -0.1731 0.064 Uiso 1 1 calc R . . H27C H 0.1277 0.2590 -0.1341 0.064 Uiso 1 1 calc R . . C28 C 0.18991(6) 0.24758(6) 0.0002(2) 0.0336(6) Uani 1 1 d . . . H28A H 0.1719 0.2617 0.0115 0.040 Uiso 1 1 calc R . . H28B H 0.1887 0.2308 0.0553 0.040 Uiso 1 1 calc R . . C29 C 0.23498(9) 0.25634(8) 0.1151(3) 0.0655(11) Uani 1 1 d . . . H29A H 0.2539 0.2689 0.1235 0.098 Uiso 1 1 calc R . . H29B H 0.2406 0.2342 0.1115 0.098 Uiso 1 1 calc R . . H29C H 0.2212 0.2599 0.1771 0.098 Uiso 1 1 calc R . . C30 C 0.21403(8) 0.29886(7) 0.0180(3) 0.0561(9) Uani 1 1 d . . . H30A H 0.2022 0.3045 0.0832 0.084 Uiso 1 1 calc R . . H30B H 0.2022 0.3051 -0.0465 0.084 Uiso 1 1 calc R . . H30C H 0.2342 0.3096 0.0186 0.084 Uiso 1 1 calc R . . C31 C 0.13227(6) 0.11905(6) -0.2202(2) 0.0271(5) Uani 1 1 d . . . C32 C 0.10384(6) 0.14154(6) -0.2120(2) 0.0303(6) Uani 1 1 d . . . H32A H 0.0906 0.1391 -0.2773 0.036 Uiso 1 1 calc R . . H32B H 0.0911 0.1359 -0.1480 0.036 Uiso 1 1 calc R . . C33 C 0.08882(6) 0.19298(6) -0.1520(2) 0.0360(6) Uani 1 1 d . . . H33A H 0.0955 0.2147 -0.1454 0.054 Uiso 1 1 calc R . . H33B H 0.0842 0.1846 -0.0799 0.054 Uiso 1 1 calc R . . H33C H 0.0700 0.1919 -0.1972 0.054 Uiso 1 1 calc R . . C34 C 0.12101(7) 0.18771(7) -0.3093(2) 0.0367(6) Uani 1 1 d . . . H34A H 0.1024 0.1869 -0.3551 0.055 Uiso 1 1 calc R . . H34B H 0.1378 0.1756 -0.3432 0.055 Uiso 1 1 calc R . . H34C H 0.1277 0.2094 -0.3010 0.055 Uiso 1 1 calc R . . C35 C 0.13643(6) 0.10771(6) -0.3375(2) 0.0316(6) Uani 1 1 d . . . H35A H 0.1157 0.1017 -0.3662 0.038 Uiso 1 1 calc R . . H35B H 0.1441 0.1254 -0.3818 0.038 Uiso 1 1 calc R . . C36 C 0.19019(7) 0.08952(7) -0.3326(3) 0.0473(8) Uani 1 1 d . . . H36A H 0.2033 0.0712 -0.3447 0.071 Uiso 1 1 calc R . . H36B H 0.1926 0.0966 -0.2575 0.071 Uiso 1 1 calc R . . H36C H 0.1965 0.1062 -0.3822 0.071 Uiso 1 1 calc R . . C37 C 0.15438(8) 0.06847(7) -0.4604(2) 0.0472(8) Uani 1 1 d . . . H37A H 0.1592 0.0846 -0.5143 0.071 Uiso 1 1 calc R . . H37B H 0.1329 0.0612 -0.4707 0.071 Uiso 1 1 calc R . . H37C H 0.1688 0.0509 -0.4693 0.071 Uiso 1 1 calc R . . C38 C 0.12586(6) 0.09145(6) -0.1432(2) 0.0291(6) Uani 1 1 d . . . H38A H 0.1424 0.0755 -0.1527 0.035 Uiso 1 1 calc R . . H38B H 0.1267 0.0989 -0.0673 0.035 Uiso 1 1 calc R . . C39 C 0.09787(7) 0.04750(7) -0.2222(3) 0.0437(7) Uani 1 1 d . . . H39A H 0.1089 0.0323 -0.1768 0.066 Uiso 1 1 calc R . . H39B H 0.1095 0.0508 -0.2895 0.066 Uiso 1 1 calc R . . H39C H 0.0770 0.0396 -0.2393 0.066 Uiso 1 1 calc R . . C40 C 0.07766(7) 0.07226(7) -0.0639(3) 0.0449(7) Uani 1 1 d . . . H40A H 0.0584 0.0609 -0.0802 0.067 Uiso 1 1 calc R . . H40B H 0.0725 0.0925 -0.0317 0.067 Uiso 1 1 calc R . . H40C H 0.0903 0.0601 -0.0128 0.067 Uiso 1 1 calc R . . C41 C -0.0469(3) 0.2953(5) 0.5218(12) 0.103(6) Uani 0.50 1 d PD . . H41A H -0.0417 0.3150 0.5572 0.154 Uiso 0.50 1 calc PR . . H41B H -0.0461 0.2783 0.5750 0.154 Uiso 0.50 1 calc PR . . H41C H -0.0680 0.2966 0.4913 0.154 Uiso 0.50 1 calc PR . . C42 C -0.0245(5) 0.2890(5) 0.435(2) 0.144(10) Uani 0.50 1 d PD . . H42A H -0.0286 0.3039 0.3748 0.173 Uiso 0.50 1 calc PR . . H42B H -0.0016 0.2863 0.4405 0.173 Uiso 0.50 1 calc PR . . C43 C -0.0076(4) 0.2607(3) 0.4559(13) 0.154(7) Uani 0.50 1 d PD . . H43A H 0.0074 0.2652 0.5146 0.185 Uiso 0.50 1 calc PR . . H43B H -0.0228 0.2454 0.4850 0.185 Uiso 0.50 1 calc PR . . C44 C 0.0088(4) 0.2460(5) 0.3722(12) 0.147(7) Uani 0.50 1 d PD . . H44A H 0.0256 0.2613 0.3574 0.177 Uiso 0.50 1 calc PR . . H44B H 0.0105 0.2280 0.3225 0.177 Uiso 0.50 1 calc PR . . C45 C 0.0308(4) 0.2244(6) 0.4227(13) 0.136(10) Uani 0.50 1 d PD . . H45A H 0.0485 0.2384 0.4393 0.164 Uiso 0.50 1 calc PR . . H45B H 0.0378 0.2121 0.3593 0.164 Uiso 0.50 1 calc PR . . C46 C 0.0334(5) 0.2011(4) 0.511(2) 0.159(12) Uani 0.50 1 d PD . . H46A H 0.0523 0.1886 0.5002 0.239 Uiso 0.50 1 calc PR . . H46B H 0.0151 0.1874 0.5099 0.239 Uiso 0.50 1 calc PR . . H46C H 0.0346 0.2118 0.5809 0.239 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 0.0259(2) 0.0263(2) 0.0222(2) 0.00128(18) -0.00023(18) -0.00133(18) Ti2 0.0253(2) 0.0266(2) 0.0219(2) 0.00100(18) 0.00013(18) -0.00216(18) O1 0.0251(9) 0.0313(9) 0.0245(9) 0.0018(7) 0.0007(7) -0.0016(7) O2 0.0244(9) 0.0331(10) 0.0263(9) 0.0026(7) -0.0015(7) -0.0018(7) O3 0.0277(9) 0.0271(9) 0.0321(10) 0.0033(7) -0.0009(7) -0.0001(7) O4 0.0320(10) 0.0289(10) 0.0284(10) -0.0025(7) 0.0004(7) -0.0017(7) O5 0.0289(9) 0.0282(9) 0.0299(10) 0.0012(7) -0.0005(7) -0.0046(7) O6 0.0249(9) 0.0306(9) 0.0277(10) -0.0021(7) -0.0006(7) -0.0012(7) N1 0.0309(12) 0.0303(12) 0.0284(12) 0.0006(9) -0.0017(9) -0.0031(9) N2 0.0383(13) 0.0364(13) 0.0372(13) -0.0036(10) 0.0016(10) 0.0059(10) N3 0.0435(14) 0.0292(12) 0.0433(14) 0.0064(10) -0.0021(11) 0.0022(10) N4 0.0305(12) 0.0275(11) 0.0298(12) 0.0013(9) 0.0021(9) 0.0006(9) N5 0.0425(14) 0.0297(12) 0.0378(14) -0.0001(10) 0.0058(11) 0.0052(10) N6 0.0522(15) 0.0360(13) 0.0294(13) -0.0068(10) 0.0021(11) -0.0042(11) N7 0.0309(12) 0.0343(12) 0.0289(12) 0.0014(9) 0.0018(9) -0.0011(9) N8 0.0400(14) 0.0383(13) 0.0393(14) -0.0042(11) -0.0037(11) -0.0123(11) N9 0.0449(14) 0.0266(12) 0.0327(13) 0.0025(9) 0.0033(10) -0.0041(10) N10 0.0290(11) 0.0274(11) 0.0278(12) 0.0015(9) 0.0000(9) -0.0011(9) N11 0.0329(12) 0.0292(12) 0.0335(12) -0.0017(9) -0.0015(10) -0.0058(9) N12 0.0378(13) 0.0341(12) 0.0264(12) -0.0059(9) 0.0029(9) 0.0026(10) C1 0.0270(13) 0.0309(14) 0.0335(15) 0.0001(11) -0.0018(11) 0.0023(11) C2 0.0293(14) 0.0358(15) 0.0319(15) 0.0000(11) -0.0027(11) 0.0040(11) C3 0.0409(16) 0.0441(17) 0.0267(14) -0.0010(12) -0.0044(12) 0.0027(13) C4 0.0320(15) 0.0387(16) 0.0437(18) -0.0013(13) -0.0053(12) -0.0041(12) C5 0.0393(16) 0.0320(15) 0.0325(15) 0.0033(12) -0.0036(12) 0.0024(12) C6 0.0479(19) 0.0345(17) 0.083(3) 0.0016(16) 0.0043(17) -0.0086(14) C7 0.074(2) 0.0351(18) 0.064(2) 0.0119(16) -0.0082(18) -0.0012(16) C8 0.0298(14) 0.0344(15) 0.0312(15) 0.0027(11) -0.0042(11) -0.0014(11) C9 0.0445(19) 0.051(2) 0.089(3) -0.0038(19) 0.0194(19) 0.0042(16) C10 0.072(3) 0.042(2) 0.093(3) -0.0129(19) 0.029(2) 0.0016(17) C11 0.0352(14) 0.0284(14) 0.0255(14) 0.0001(10) 0.0059(11) 0.0002(11) C12 0.0348(15) 0.0293(14) 0.0321(15) -0.0021(11) 0.0059(11) 0.0021(11) C13 0.0392(16) 0.0381(16) 0.0342(16) 0.0073(12) 0.0060(12) 0.0005(12) C14 0.0319(15) 0.0334(15) 0.0409(17) -0.0007(12) 0.0023(12) -0.0025(12) C15 0.0484(17) 0.0334(15) 0.0270(14) -0.0007(11) 0.0054(12) -0.0004(12) C16 0.059(2) 0.0473(19) 0.056(2) -0.0113(16) -0.0105(17) -0.0090(16) C17 0.093(3) 0.048(2) 0.0373(19) -0.0124(15) 0.0029(17) -0.0076(18) C18 0.0391(15) 0.0300(14) 0.0288(14) -0.0001(11) 0.0059(12) -0.0008(12) C19 0.067(2) 0.0346(17) 0.058(2) -0.0039(15) 0.0002(17) 0.0091(15) C20 0.058(2) 0.062(2) 0.053(2) -0.0137(17) -0.0115(17) 0.0201(17) C21 0.0310(14) 0.0308(14) 0.0292(14) 0.0014(11) 0.0006(11) -0.0075(11) C22 0.0307(14) 0.0358(15) 0.0339(15) 0.0013(12) 0.0018(11) -0.0081(11) C23 0.0394(16) 0.0416(16) 0.0296(15) 0.0001(12) 0.0062(12) -0.0041(12) C24 0.0290(14) 0.0415(16) 0.0455(18) 0.0005(13) 0.0043(12) -0.0005(12) C25 0.0404(16) 0.0343(15) 0.0258(14) 0.0027(11) 0.0019(11) -0.0058(12) C26 0.069(2) 0.0332(16) 0.0432(19) 0.0085(13) 0.0097(16) 0.0000(15) C27 0.0490(18) 0.0336(16) 0.0454(18) 0.0005(13) -0.0006(14) 0.0011(13) C28 0.0353(15) 0.0350(15) 0.0305(15) 0.0001(11) 0.0002(11) -0.0060(12) C29 0.065(2) 0.055(2) 0.077(3) 0.0013(19) -0.030(2) -0.0185(18) C30 0.067(2) 0.0433(19) 0.058(2) -0.0059(16) -0.0132(17) -0.0158(16) C31 0.0254(13) 0.0316(14) 0.0243(13) -0.0019(10) -0.0015(10) -0.0024(10) C32 0.0325(14) 0.0285(14) 0.0298(15) -0.0018(11) -0.0007(11) -0.0036(11) C33 0.0335(15) 0.0312(15) 0.0435(17) -0.0015(12) 0.0007(12) 0.0026(12) C34 0.0395(16) 0.0392(16) 0.0315(15) 0.0064(12) -0.0030(12) -0.0006(12) C35 0.0371(15) 0.0317(14) 0.0259(14) -0.0004(11) -0.0028(11) 0.0000(11) C36 0.0365(17) 0.0486(19) 0.057(2) -0.0143(15) 0.0086(14) 0.0012(14) C37 0.067(2) 0.0463(18) 0.0281(16) -0.0079(13) -0.0003(14) 0.0082(15) C38 0.0335(14) 0.0282(14) 0.0257(14) -0.0013(10) -0.0007(11) -0.0017(11) C39 0.0512(19) 0.0334(16) 0.0465(19) -0.0068(13) 0.0016(14) -0.0071(13) C40 0.0415(17) 0.0491(18) 0.0441(18) -0.0061(14) 0.0088(14) -0.0138(14) C41 0.066(9) 0.165(15) 0.078(8) 0.049(8) -0.015(6) -0.027(8) C42 0.109(14) 0.080(11) 0.24(2) 0.040(11) 0.093(14) 0.040(10) C43 0.22(2) 0.106(11) 0.135(13) -0.045(9) -0.078(13) 0.075(10) C44 0.15(2) 0.152(16) 0.144(13) 0.013(15) 0.072(14) 0.054(14) C45 0.068(9) 0.25(3) 0.089(11) -0.033(14) 0.025(9) 0.012(14) C46 0.11(2) 0.096(13) 0.27(3) -0.045(15) 0.07(2) -0.009(14) _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 O2 1.8553(17) . ? Ti1 O1 1.8601(17) . ? Ti1 O3 1.8898(17) . ? Ti1 O4 1.8936(17) . ? Ti1 N4 2.374(2) . ? Ti1 N1 2.390(2) . ? Ti1 Ti2 2.7983(6) . ? Ti2 O2 1.8507(17) . ? Ti2 O1 1.8586(17) . ? Ti2 O6 1.8856(17) . ? Ti2 O5 1.8912(17) . ? Ti2 N10 2.386(2) . ? Ti2 N7 2.410(2) . ? O3 C1 1.425(3) . ? O4 C11 1.425(3) . ? O5 C21 1.423(3) . ? O6 C31 1.420(3) . ? N1 C3 1.468(3) . ? N1 C4 1.476(3) . ? N1 C2 1.476(3) . ? N2 C10 1.443(4) . ? N2 C9 1.445(4) . ? N2 C8 1.471(3) . ? N3 C6 1.451(4) . ? N3 C7 1.460(4) . ? N3 C5 1.469(3) . ? N4 C14 1.469(3) . ? N4 C13 1.470(3) . ? N4 C12 1.474(3) . ? N5 C20 1.446(4) . ? N5 C19 1.455(4) . ? N5 C18 1.476(3) . ? N6 C16 1.450(4) . ? N6 C15 1.463(3) . ? N6 C17 1.467(4) . ? N7 C24 1.471(3) . ? N7 C23 1.478(3) . ? N7 C22 1.479(3) . ? N8 C29 1.449(4) . ? N8 C30 1.455(4) . ? N8 C28 1.478(3) . ? N9 C27 1.450(4) . ? N9 C26 1.456(3) . ? N9 C25 1.465(3) . ? N10 C34 1.467(3) . ? N10 C33 1.471(3) . ? N10 C32 1.482(3) . ? N11 C40 1.457(4) . ? N11 C39 1.463(3) . ? N11 C38 1.473(3) . ? N12 C37 1.454(3) . ? N12 C36 1.454(4) . ? N12 C35 1.462(3) . ? C1 C8 1.533(4) . ? C1 C5 1.538(4) . ? C1 C2 1.563(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 C18 1.543(4) . ? C11 C15 1.545(4) . ? C11 C12 1.557(4) . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? 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 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C28 1.538(4) . ? C21 C25 1.542(4) . ? C21 C22 1.560(4) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C35 1.537(3) . ? C31 C38 1.542(3) . ? C31 C32 1.557(3) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? 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 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.468(16) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 C46 1.10(3) 3 ? C42 C43 1.436(15) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.400(13) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C43 1.072(16) 3 ? C44 C45 1.461(16) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.481(17) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 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 O2 Ti1 O1 82.08(7) . . ? O2 Ti1 O3 105.15(8) . . ? O1 Ti1 O3 108.73(7) . . ? O2 Ti1 O4 107.91(8) . . ? O1 Ti1 O4 104.53(8) . . ? O3 Ti1 O4 135.56(8) . . ? O2 Ti1 N4 164.96(8) . . ? O1 Ti1 N4 83.08(7) . . ? O3 Ti1 N4 81.94(7) . . ? O4 Ti1 N4 73.63(7) . . ? O2 Ti1 N1 81.25(7) . . ? O1 Ti1 N1 163.11(7) . . ? O3 Ti1 N1 73.31(7) . . ? O4 Ti1 N1 83.22(7) . . ? N4 Ti1 N1 113.68(7) . . ? O2 Ti1 Ti2 40.91(5) . . ? O1 Ti1 Ti2 41.17(5) . . ? O3 Ti1 Ti2 112.36(6) . . ? O4 Ti1 Ti2 112.08(6) . . ? N4 Ti1 Ti2 124.23(5) . . ? N1 Ti1 Ti2 122.09(5) . . ? O2 Ti2 O1 82.24(7) . . ? O2 Ti2 O6 108.42(8) . . ? O1 Ti2 O6 104.55(7) . . ? O2 Ti2 O5 105.50(7) . . ? O1 Ti2 O5 109.48(7) . . ? O6 Ti2 O5 134.39(8) . . ? O2 Ti2 N10 164.76(7) . . ? O1 Ti2 N10 82.67(7) . . ? O6 Ti2 N10 73.47(7) . . ? O5 Ti2 N10 81.63(7) . . ? O2 Ti2 N7 80.54(7) . . ? O1 Ti2 N7 162.62(8) . . ? O6 Ti2 N7 83.17(7) . . ? O5 Ti2 N7 73.25(7) . . ? N10 Ti2 N7 114.62(7) . . ? O2 Ti2 Ti1 41.03(5) . . ? O1 Ti2 Ti1 41.21(5) . . ? O6 Ti2 Ti1 111.77(6) . . ? O5 Ti2 Ti1 113.84(6) . . ? N10 Ti2 Ti1 123.83(5) . . ? N7 Ti2 Ti1 121.54(5) . . ? Ti2 O1 Ti1 97.62(8) . . ? Ti2 O2 Ti1 98.06(8) . . ? C1 O3 Ti1 125.00(15) . . ? C11 O4 Ti1 124.27(15) . . ? C21 O5 Ti2 125.19(15) . . ? C31 O6 Ti2 125.49(15) . . ? C3 N1 C4 108.0(2) . . ? C3 N1 C2 111.9(2) . . ? C4 N1 C2 110.1(2) . . ? C3 N1 Ti1 113.26(16) . . ? C4 N1 Ti1 112.59(16) . . ? C2 N1 Ti1 100.92(14) . . ? C10 N2 C9 109.4(3) . . ? C10 N2 C8 113.7(2) . . ? C9 N2 C8 113.5(2) . . ? C6 N3 C7 109.8(3) . . ? C6 N3 C5 112.9(2) . . ? C7 N3 C5 110.0(2) . . ? C14 N4 C13 108.4(2) . . ? C14 N4 C12 110.3(2) . . ? C13 N4 C12 111.2(2) . . ? C14 N4 Ti1 113.27(16) . . ? C13 N4 Ti1 111.89(16) . . ? C12 N4 Ti1 101.73(14) . . ? C20 N5 C19 108.9(2) . . ? C20 N5 C18 112.5(2) . . ? C19 N5 C18 113.1(2) . . ? C16 N6 C15 113.0(2) . . ? C16 N6 C17 110.0(3) . . ? C15 N6 C17 110.8(2) . . ? C24 N7 C23 108.4(2) . . ? C24 N7 C22 109.8(2) . . ? C23 N7 C22 111.2(2) . . ? C24 N7 Ti2 113.24(16) . . ? C23 N7 Ti2 113.41(16) . . ? C22 N7 Ti2 100.66(15) . . ? C29 N8 C30 108.6(2) . . ? C29 N8 C28 111.9(2) . . ? C30 N8 C28 112.6(2) . . ? C27 N9 C26 110.1(2) . . ? C27 N9 C25 113.3(2) . . ? C26 N9 C25 109.6(2) . . ? C34 N10 C33 109.0(2) . . ? C34 N10 C32 110.9(2) . . ? C33 N10 C32 109.6(2) . . ? C34 N10 Ti2 111.60(15) . . ? C33 N10 Ti2 113.42(16) . . ? C32 N10 Ti2 102.23(14) . . ? C40 N11 C39 109.5(2) . . ? C40 N11 C38 112.0(2) . . ? C39 N11 C38 112.2(2) . . ? C37 N12 C36 109.8(2) . . ? C37 N12 C35 110.2(2) . . ? C36 N12 C35 113.2(2) . . ? O3 C1 C8 108.1(2) . . ? O3 C1 C5 111.6(2) . . ? C8 C1 C5 110.0(2) . . ? O3 C1 C2 107.5(2) . . ? C8 C1 C2 109.5(2) . . ? C5 C1 C2 110.1(2) . . ? N1 C2 C1 112.1(2) . . ? N1 C2 H2A 109.2 . . ? C1 C2 H2A 109.2 . . ? N1 C2 H2B 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C1 115.6(2) . . ? N3 C5 H5A 108.4 . . ? C1 C5 H5A 108.4 . . ? N3 C5 H5B 108.4 . . ? C1 C5 H5B 108.4 . . ? H5A C5 H5B 107.4 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N3 C7 H7A 109.5 . . ? N3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 C1 112.9(2) . . ? N2 C8 H8A 109.0 . . ? C1 C8 H8A 109.0 . . ? N2 C8 H8B 109.0 . . ? C1 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? N2 C9 H9A 109.5 . . ? N2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N2 C10 H10A 109.5 . . ? N2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O4 C11 C18 108.7(2) . . ? O4 C11 C15 111.1(2) . . ? C18 C11 C15 110.7(2) . . ? O4 C11 C12 108.3(2) . . ? C18 C11 C12 107.8(2) . . ? C15 C11 C12 110.2(2) . . ? N4 C12 C11 111.8(2) . . ? N4 C12 H12A 109.3 . . ? C11 C12 H12A 109.3 . . ? N4 C12 H12B 109.3 . . ? C11 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N4 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N6 C15 C11 115.1(2) . . ? N6 C15 H15A 108.5 . . ? C11 C15 H15A 108.5 . . ? N6 C15 H15B 108.5 . . ? C11 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? N6 C16 H16A 109.5 . . ? N6 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N6 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N6 C17 H17A 109.5 . . ? N6 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N6 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N5 C18 C11 111.7(2) . . ? N5 C18 H18A 109.3 . . ? C11 C18 H18A 109.3 . . ? N5 C18 H18B 109.3 . . ? C11 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? N5 C19 H19A 109.5 . . ? N5 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N5 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N5 C20 H20A 109.5 . . ? N5 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N5 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O5 C21 C28 107.9(2) . . ? O5 C21 C25 111.3(2) . . ? C28 C21 C25 110.4(2) . . ? O5 C21 C22 108.2(2) . . ? C28 C21 C22 109.0(2) . . ? C25 C21 C22 110.0(2) . . ? N7 C22 C21 111.9(2) . . ? N7 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? N7 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? N7 C23 H23A 109.5 . . ? N7 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N7 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N7 C24 H24A 109.5 . . ? N7 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N7 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N9 C25 C21 116.4(2) . . ? N9 C25 H25A 108.2 . . ? C21 C25 H25A 108.2 . . ? N9 C25 H25B 108.2 . . ? C21 C25 H25B 108.2 . . ? H25A C25 H25B 107.3 . . ? N9 C26 H26A 109.5 . . ? N9 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N9 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N9 C27 H27A 109.5 . . ? N9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N8 C28 C21 112.8(2) . . ? N8 C28 H28A 109.0 . . ? C21 C28 H28A 109.0 . . ? N8 C28 H28B 109.0 . . ? C21 C28 H28B 109.0 . . ? H28A C28 H28B 107.8 . . ? N8 C29 H29A 109.5 . . ? N8 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N8 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N8 C30 H30A 109.5 . . ? N8 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N8 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O6 C31 C35 110.8(2) . . ? O6 C31 C38 109.03(19) . . ? C35 C31 C38 110.9(2) . . ? O6 C31 C32 108.47(19) . . ? C35 C31 C32 110.3(2) . . ? C38 C31 C32 107.2(2) . . ? N10 C32 C31 111.6(2) . . ? N10 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? N10 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? N10 C33 H33A 109.5 . . ? N10 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N10 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N10 C34 H34A 109.5 . . ? N10 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N10 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N12 C35 C31 115.6(2) . . ? N12 C35 H35A 108.4 . . ? C31 C35 H35A 108.4 . . ? N12 C35 H35B 108.4 . . ? C31 C35 H35B 108.4 . . ? H35A C35 H35B 107.4 . . ? N12 C36 H36A 109.5 . . ? N12 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N12 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N12 C37 H37A 109.5 . . ? N12 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N12 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N11 C38 C31 112.0(2) . . ? N11 C38 H38A 109.2 . . ? C31 C38 H38A 109.2 . . ? N11 C38 H38B 109.2 . . ? C31 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? N11 C39 H39A 109.5 . . ? N11 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N11 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N11 C40 H40A 109.5 . . ? N11 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N11 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C45 C42 C46 113(3) 3 3 ? C45 C42 C43 60(2) 3 . ? C46 C42 C43 110(2) 3 . ? C45 C42 C41 93(3) 3 . ? C43 C42 C41 110.5(18) . . ? C45 C42 C44 48(2) 3 3 ? C46 C42 C44 144(2) 3 3 ? C41 C42 C44 134.7(17) . 3 ? C45 C42 H42A 109.0 3 . ? C46 C42 H42A 109.0 3 . ? C43 C42 H42A 140.3 . . ? C41 C42 H42A 108.2 . . ? C44 C42 H42A 106.4 3 . ? C45 C42 H42B 109.0 3 . ? C46 C42 H42B 109.0 3 . ? C43 C42 H42B 52.5 . . ? C41 C42 H42B 128.0 . . ? C44 C42 H42B 64.5 3 . ? H42A C42 H42B 107.8 . . ? C44 C43 C42 120.0(16) . . ? C44 C43 H43A 107.3 . . ? C42 C43 H43A 107.3 . . ? C44 C43 H43B 107.3 . . ? C42 C43 H43B 107.3 . . ? H43A C43 H43B 106.9 . . ? C44 C44 C43 93.9(16) 3 3 ? C44 C44 C43 49.8(9) 3 . ? C43 C44 C43 52.3(12) 3 . ? C44 C44 C45 148(3) 3 . ? C43 C44 C45 56.6(12) 3 . ? C43 C44 C45 107.3(12) . . ? C44 C44 C42 133(4) 3 3 ? C43 C44 C42 52.2(12) 3 3 ? C43 C44 C42 104.3(13) . 3 ? C44 C44 H44A 112.9 3 . ? C43 C44 H44A 112.9 3 . ? C43 C44 H44A 101.8 . . ? C45 C44 H44A 91.7 . . ? C42 C44 H44A 110.9 3 . ? C44 C44 H44B 112.9 3 . ? C43 C44 H44B 112.9 3 . ? C43 C44 H44B 147.8 . . ? C45 C44 H44B 73.8 . . ? C42 C44 H44B 65.8 3 . ? H44A C44 H44B 110.4 . . ? C44 C45 C46 142.2(17) . . ? C44 C45 H45A 101.4 . . ? C46 C45 H45A 101.4 . . ? C44 C45 H45B 101.4 . . ? C46 C45 H45B 101.4 . . ? H45A C45 H45B 104.6 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.273 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.059 # Attachment 'compound 10.cif' data_h06kcm29 _database_code_depnum_ccdc_archive 'CCDC 657061' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H54 N6 O6 Zn2' _chemical_formula_sum 'C24 H54 N6 O6 Zn2' _chemical_formula_weight 653.47 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.6443(3) _cell_length_b 16.8905(6) _cell_length_c 10.4930(4) _cell_angle_alpha 90.00 _cell_angle_beta 111.741(2) _cell_angle_gamma 90.00 _cell_volume 1587.69(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 38176 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 27.485 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.367 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 696 _exptl_absorpt_coefficient_mu 1.555 _exptl_absorpt_correction_type none _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '297 1.9 degree images with \f and \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12765 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_av_sigmaI/netI 0.0539 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 4.13 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3482 _reflns_number_gt 2600 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _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 ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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^)+(0.0331P)^2^+0.1839P] 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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3482 _refine_ls_number_parameters 179 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0755 _refine_ls_wR_factor_gt 0.0691 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 Zn Zn -0.02403(3) 0.060956(14) -0.11374(2) 0.02117(9) Uani 1 1 d . . . O1 O 0.13384(16) 0.03251(8) 0.07377(14) 0.0204(3) Uani 1 1 d . . . O2 O 0.09381(17) 0.13049(9) -0.19684(15) 0.0304(4) Uani 1 1 d . . . O3 O 0.16168(18) 0.00812(10) -0.22254(17) 0.0361(4) Uani 1 1 d . . . N1 N -0.0762(2) 0.15638(10) 0.00259(18) 0.0245(4) Uani 1 1 d . . . N2 N 0.2008(2) -0.03067(11) 0.31953(18) 0.0281(4) Uani 1 1 d . . . N3 N 0.4359(2) 0.11335(11) 0.20894(19) 0.0304(5) Uani 1 1 d . . . C1 C 0.1638(2) 0.09298(13) 0.1724(2) 0.0232(5) Uani 1 1 d . . . C2 C 0.0174(2) 0.13943(13) 0.1485(2) 0.0267(5) Uani 1 1 d . . . H2A H -0.0433 0.1089 0.1894 0.032 Uiso 1 1 calc R . . H2B H 0.0436 0.1904 0.1984 0.032 Uiso 1 1 calc R . . C3 C -0.0415(3) 0.23489(13) -0.0415(2) 0.0331(6) Uani 1 1 d . . . H3A H -0.0489 0.2756 0.0222 0.050 Uiso 1 1 calc R . . H3B H -0.1126 0.2466 -0.1341 0.050 Uiso 1 1 calc R . . H3C H 0.0601 0.2343 -0.0416 0.050 Uiso 1 1 calc R . . C4 C -0.2333(3) 0.15764(14) -0.0081(3) 0.0344(6) Uani 1 1 d . . . H4A H -0.2613 0.1051 0.0140 0.052 Uiso 1 1 calc R . . H4B H -0.2980 0.1721 -0.1018 0.052 Uiso 1 1 calc R . . H4C H -0.2449 0.1966 0.0565 0.052 Uiso 1 1 calc R . . C5 C 0.2114(3) 0.05677(13) 0.3196(2) 0.0298(5) Uani 1 1 d . . . H5A H 0.3156 0.0726 0.3736 0.036 Uiso 1 1 calc R . . H5B H 0.1472 0.0791 0.3655 0.036 Uiso 1 1 calc R . . C6 C 0.3423(3) -0.06536(15) 0.3223(3) 0.0422(7) Uani 1 1 d . . . H6A H 0.4241 -0.0484 0.4058 0.063 Uiso 1 1 calc R . . H6B H 0.3619 -0.0475 0.2417 0.063 Uiso 1 1 calc R . . H6C H 0.3350 -0.1232 0.3212 0.063 Uiso 1 1 calc R . . C7 C 0.1752(3) -0.05724(16) 0.4426(2) 0.0467(7) Uani 1 1 d . . . H7A H 0.1685 -0.1151 0.4422 0.070 Uiso 1 1 calc R . . H7B H 0.0818 -0.0344 0.4426 0.070 Uiso 1 1 calc R . . H7C H 0.2582 -0.0399 0.5249 0.070 Uiso 1 1 calc R . . C8 C 0.2873(2) 0.14954(13) 0.1686(2) 0.0277(5) Uani 1 1 d . . . H8A H 0.2588 0.1708 0.0744 0.033 Uiso 1 1 calc R . . H8B H 0.2933 0.1948 0.2305 0.033 Uiso 1 1 calc R . . C9 C 0.4560(3) 0.07344(14) 0.0937(3) 0.0356(6) Uani 1 1 d . . . H9A H 0.3738 0.0361 0.0520 0.053 Uiso 1 1 calc R . . H9B H 0.5510 0.0446 0.1264 0.053 Uiso 1 1 calc R . . H9C H 0.4568 0.1128 0.0253 0.053 Uiso 1 1 calc R . . C10 C 0.5512(3) 0.17298(16) 0.2645(3) 0.0437(7) Uani 1 1 d . . . H10A H 0.6495 0.1488 0.2848 0.066 Uiso 1 1 calc R . . H10B H 0.5456 0.1948 0.3491 0.066 Uiso 1 1 calc R . . H10C H 0.5363 0.2156 0.1973 0.066 Uiso 1 1 calc R . . C11 C 0.1726(3) 0.08081(14) -0.2326(2) 0.0281(5) Uani 1 1 d . . . C12 C 0.2808(3) 0.11496(15) -0.2910(3) 0.0352(6) Uani 1 1 d . . . H12A H 0.3457 0.0728 -0.3012 0.053 Uiso 1 1 calc R . . H12B H 0.3418 0.1557 -0.2288 0.053 Uiso 1 1 calc R . . H12C H 0.2254 0.1386 -0.3808 0.053 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 Zn 0.02045(15) 0.01844(14) 0.02405(14) 0.00070(10) 0.00756(10) -0.00036(11) O1 0.0201(8) 0.0189(7) 0.0221(8) -0.0017(6) 0.0078(6) -0.0007(6) O2 0.0259(9) 0.0348(9) 0.0327(9) 0.0001(7) 0.0136(7) -0.0007(7) O3 0.0360(10) 0.0298(10) 0.0422(10) 0.0052(8) 0.0140(8) -0.0040(8) N1 0.0239(11) 0.0203(9) 0.0315(10) 0.0020(8) 0.0127(8) 0.0029(7) N2 0.0284(11) 0.0263(10) 0.0266(10) 0.0030(8) 0.0067(8) -0.0033(8) N3 0.0197(10) 0.0307(11) 0.0353(11) 0.0004(8) 0.0039(8) -0.0057(8) C1 0.0251(12) 0.0195(11) 0.0238(11) -0.0037(9) 0.0077(9) -0.0027(9) C2 0.0301(13) 0.0241(12) 0.0288(12) -0.0057(9) 0.0142(10) -0.0024(10) C3 0.0357(14) 0.0204(12) 0.0450(15) 0.0009(10) 0.0171(11) 0.0037(10) C4 0.0266(14) 0.0338(14) 0.0465(15) 0.0005(11) 0.0177(11) 0.0056(10) C5 0.0341(14) 0.0287(13) 0.0239(11) -0.0031(9) 0.0077(10) -0.0027(10) C6 0.0344(15) 0.0385(15) 0.0404(15) -0.0039(11) -0.0018(11) 0.0082(12) C7 0.0559(18) 0.0482(17) 0.0287(13) 0.0047(12) 0.0073(12) -0.0216(14) C8 0.0279(13) 0.0212(12) 0.0320(12) -0.0017(9) 0.0088(10) -0.0017(9) C9 0.0241(13) 0.0392(15) 0.0444(15) 0.0009(11) 0.0139(11) -0.0010(11) C10 0.0313(14) 0.0429(16) 0.0469(15) 0.0002(12) 0.0028(11) -0.0138(12) C11 0.0245(13) 0.0349(15) 0.0232(12) 0.0016(10) 0.0067(9) -0.0028(10) C12 0.0341(14) 0.0356(14) 0.0426(14) 0.0026(11) 0.0218(12) -0.0010(11) _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 Zn O1 2.0294(14) 3 ? Zn O2 2.0410(15) . ? Zn O1 2.0496(14) . ? Zn N1 2.1898(17) . ? Zn N2 2.2594(18) 3 ? Zn O3 2.6120(17) . ? O1 C1 1.406(2) . ? O1 Zn 2.0294(14) 3 ? O2 C11 1.278(3) . ? O3 C11 1.240(3) . ? N1 C4 1.478(3) . ? N1 C3 1.483(3) . ? N1 C2 1.489(3) . ? N2 C7 1.472(3) . ? N2 C6 1.475(3) . ? N2 C5 1.480(3) . ? N2 Zn 2.2594(18) 3 ? N3 C10 1.453(3) . ? N3 C9 1.458(3) . ? N3 C8 1.469(3) . ? C1 C8 1.539(3) . ? C1 C2 1.552(3) . ? C1 C5 1.563(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? 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 1.506(3) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 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 O1 Zn O2 162.12(6) 3 . ? O1 Zn O1 83.00(6) 3 . ? O2 Zn O1 102.23(6) . . ? O1 Zn N1 102.25(6) 3 . ? O2 Zn N1 95.38(6) . . ? O1 Zn N1 83.10(6) . . ? O1 Zn N2 75.79(6) 3 3 ? O2 Zn N2 93.70(6) . 3 ? O1 Zn N2 153.34(6) . 3 ? N1 Zn N2 116.84(7) . 3 ? O1 Zn O3 108.63(5) 3 . ? O2 Zn O3 55.21(6) . . ? O1 Zn O3 87.34(5) . . ? N1 Zn O3 146.24(6) . . ? N2 Zn O3 84.37(6) 3 . ? C1 O1 Zn 113.18(12) . 3 ? C1 O1 Zn 114.42(12) . . ? Zn O1 Zn 97.00(6) 3 . ? C11 O2 Zn 103.50(14) . . ? C11 O3 Zn 78.04(14) . . ? C4 N1 C3 107.88(17) . . ? C4 N1 C2 107.15(17) . . ? C3 N1 C2 111.81(17) . . ? C4 N1 Zn 114.15(13) . . ? C3 N1 Zn 111.06(13) . . ? C2 N1 Zn 104.75(12) . . ? C7 N2 C6 108.4(2) . . ? C7 N2 C5 109.75(19) . . ? C6 N2 C5 109.45(19) . . ? C7 N2 Zn 117.18(15) . 3 ? C6 N2 Zn 107.09(14) . 3 ? C5 N2 Zn 104.70(12) . 3 ? C10 N3 C9 109.7(2) . . ? C10 N3 C8 110.30(19) . . ? C9 N3 C8 111.65(18) . . ? O1 C1 C8 112.46(18) . . ? O1 C1 C2 108.76(16) . . ? C8 C1 C2 110.40(18) . . ? O1 C1 C5 110.37(17) . . ? C8 C1 C5 108.74(17) . . ? C2 C1 C5 105.92(18) . . ? N1 C2 C1 115.60(17) . . ? N1 C2 H2A 108.4 . . ? C1 C2 H2A 108.4 . . ? N1 C2 H2B 108.4 . . ? C1 C2 H2B 108.4 . . ? H2A C2 H2B 107.4 . . ? N1 C3 H3A 109.5 . . ? N1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 C1 113.26(17) . . ? N2 C5 H5A 108.9 . . ? C1 C5 H5A 108.9 . . ? N2 C5 H5B 108.9 . . ? C1 C5 H5B 108.9 . . ? H5A C5 H5B 107.7 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C1 114.60(18) . . ? N3 C8 H8A 108.6 . . ? C1 C8 H8A 108.6 . . ? N3 C8 H8B 108.6 . . ? C1 C8 H8B 108.6 . . ? H8A C8 H8B 107.6 . . ? N3 C9 H9A 109.5 . . ? N3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N3 C10 H10A 109.5 . . ? N3 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N3 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O3 C11 O2 123.1(2) . . ? O3 C11 C12 120.5(2) . . ? O2 C11 C12 116.4(2) . . ? 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 . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.379 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.068 # Attachment 'Compound 11 revised.cif' data_h05kcm24_Compound11 _database_code_depnum_ccdc_archive 'CCDC 657062' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H68 N4 O12 Ti4' _chemical_formula_sum 'C28 H68 N4 O12 Ti4' _chemical_formula_weight 844.46 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 'P 1 21/c 1' _symmetry_space_group_name_Hall '-P 2ybc' 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 9.8514(3) _cell_length_b 22.0293(8) _cell_length_c 10.8310(3) _cell_angle_alpha 90.00 _cell_angle_beta 117.830(2) _cell_angle_gamma 90.00 _cell_volume 2078.67(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21996 _cell_measurement_theta_min 2.910 _cell_measurement_theta_max 25.485 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type none _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 '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method '208 2.0 degree images with \v scans' _diffrn_standards_number 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22055 _diffrn_reflns_av_R_equivalents 0.1501 _diffrn_reflns_av_sigmaI/netI 0.0764 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 4.35 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3593 _reflns_number_gt 2710 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinski & Minor, 1997)' _computing_data_reduction ; DENZO-SCALEPACK Z. Otwinowski and W. Minor, " Processing of X-ray Diffraction Data Collected in Oscillation Mode ", Methods in Enzymology, Volume 276: Macromolecular Crystallography, part A, p.307-326, 1997,C.W. Carter, Jr. & R. M. Sweet, Eds., Academic Press. ; _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 ; SHELXL97 -Program for Crystal Structure Analysis (Release 97-2). Sheldrick, G.M., Instit\"ut f\"ur Anorganische Chemie der Universit\"at, Tammanstrasse 4, D-3400 G\"ottingen, Germany, 1998 ; _computing_molecular_graphics 'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565' _computing_publication_material ; WinGX publication routines, Farrugia, L. J., J. Appl. Crystallogr., 1999, 32, 837-838 ; _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. One iso-propoxyl group is disordered in a ratio 1:1 and as a result one of the bond lengths (C21-C23) in it had to be restrained. ; _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^)+(0.1216P)^2^+8.1901P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.019(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3593 _refine_ls_number_parameters 240 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1111 _refine_ls_R_factor_gt 0.0844 _refine_ls_wR_factor_ref 0.2420 _refine_ls_wR_factor_gt 0.2169 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _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 0.57303(13) 0.10106(5) 0.15574(12) 0.0275(4) Uani 1 1 d . . . Ti2 Ti 0.37694(12) 0.02961(5) -0.12588(11) 0.0257(4) Uani 1 1 d . . . N1 N 0.3551(6) 0.1618(2) 0.1076(6) 0.0329(12) Uani 1 1 d . . . N2 N 0.4200(6) 0.0616(2) -0.3060(6) 0.0322(12) Uani 1 1 d . . . O1 O 0.5687(5) 0.1067(2) 0.3268(5) 0.0340(10) Uani 1 1 d . . . O2 O 0.6834(5) 0.1711(2) 0.1685(5) 0.0348(11) Uani 1 1 d . B . C21 C 0.8259(10) 0.1908(4) 0.2733(10) 0.063(3) Uani 1 1 d D . . H21 H 0.8671 0.1564 0.3411 0.076 Uiso 0.50 1 calc PR A 1 H21A H 0.8163 0.1843 0.3603 0.076 Uiso 0.50 1 calc PR A 2 C22 C 0.836(2) 0.2408(12) 0.352(3) 0.073(7) Uani 0.50 1 d P B 1 H22A H 0.7685 0.2356 0.3949 0.109 Uiso 0.50 1 calc PR B 1 H22B H 0.8038 0.2769 0.2916 0.109 Uiso 0.50 1 calc PR B 1 H22C H 0.9419 0.2460 0.4247 0.109 Uiso 0.50 1 calc PR B 1 C23 C 0.930(4) 0.194(2) 0.199(4) 0.18(3) Uani 0.50 1 d PD B 1 H23A H 0.9173 0.1565 0.1457 0.275 Uiso 0.50 1 calc PR B 1 H23B H 1.0374 0.1983 0.2692 0.275 Uiso 0.50 1 calc PR B 1 H23C H 0.8992 0.2287 0.1354 0.275 Uiso 0.50 1 calc PR B 1 C22A C 0.824(2) 0.2611(8) 0.262(3) 0.059(5) Uani 0.50 1 d P B 2 H22D H 0.7237 0.2766 0.2450 0.089 Uiso 0.50 1 calc PR B 2 H22E H 0.8431 0.2728 0.1837 0.089 Uiso 0.50 1 calc PR B 2 H22F H 0.9043 0.2783 0.3485 0.089 Uiso 0.50 1 calc PR B 2 C23A C 0.957(2) 0.1608(9) 0.301(3) 0.073(6) Uani 0.50 1 d P B 2 H23D H 0.9410 0.1171 0.3066 0.110 Uiso 0.50 1 calc PR B 2 H23E H 1.0397 0.1749 0.3902 0.110 Uiso 0.50 1 calc PR B 2 H23F H 0.9841 0.1685 0.2263 0.110 Uiso 0.50 1 calc PR B 2 O3 O 0.7196(5) 0.04356(19) 0.2123(5) 0.0308(10) Uani 1 1 d . . . O4 O 0.5045(5) 0.10559(18) -0.0531(4) 0.0289(9) Uani 1 1 d . . . O5 O 0.4339(5) 0.02624(18) 0.0639(4) 0.0257(9) Uani 1 1 d . . . O6 O 0.1904(5) 0.0682(2) -0.2024(5) 0.0342(10) Uani 1 1 d . . . C61 C 0.0351(8) 0.0492(3) -0.2872(7) 0.0403(16) Uani 1 1 d . . . H61 H 0.0319 0.0218 -0.3623 0.048 Uiso 1 1 calc R . . C62 C -0.0209(9) 0.0139(4) -0.1998(9) 0.056(2) Uani 1 1 d . . . H62A H 0.0448 -0.0216 -0.1591 0.084 Uiso 1 1 calc R . . H62B H -0.1268 0.0006 -0.2589 0.084 Uiso 1 1 calc R . . H62C H -0.0171 0.0399 -0.1249 0.084 Uiso 1 1 calc R . . C63 C -0.0613(9) 0.1045(4) -0.3549(11) 0.066(3) Uani 1 1 d . . . H63A H -0.0201 0.1256 -0.4099 0.100 Uiso 1 1 calc R . . H63B H -0.0590 0.1318 -0.2825 0.100 Uiso 1 1 calc R . . H63C H -0.1673 0.0920 -0.4163 0.100 Uiso 1 1 calc R . . C1 C 0.3098(9) 0.2041(3) -0.0101(8) 0.0447(18) Uani 1 1 d . . . H1A H 0.2328 0.2326 -0.0109 0.067 Uiso 1 1 calc R . . H1B H 0.2663 0.1813 -0.0978 0.067 Uiso 1 1 calc R . . H1C H 0.4000 0.2268 0.0001 0.067 Uiso 1 1 calc R . . C2 C 0.2208(8) 0.1253(4) 0.0888(9) 0.0456(18) Uani 1 1 d . . . H2A H 0.2520 0.0963 0.1659 0.068 Uiso 1 1 calc R . . H2B H 0.1803 0.1032 0.0001 0.068 Uiso 1 1 calc R . . H2C H 0.1412 0.1522 0.0881 0.068 Uiso 1 1 calc R . . C3 C 0.4162(9) 0.1965(3) 0.2389(8) 0.0399(16) Uani 1 1 d . . . H3A H 0.3320 0.2187 0.2447 0.048 Uiso 1 1 calc R . . H3B H 0.4927 0.2265 0.2421 0.048 Uiso 1 1 calc R . . C4 C 0.4910(9) 0.1524(3) 0.3606(8) 0.0412(16) Uani 1 1 d . . . H4A H 0.5646 0.1744 0.4452 0.049 Uiso 1 1 calc R . . H4B H 0.4117 0.1338 0.3803 0.049 Uiso 1 1 calc R . . C5 C 0.2886(9) 0.0477(4) -0.4414(7) 0.0450(18) Uani 1 1 d . . . H5A H 0.1988 0.0708 -0.4516 0.067 Uiso 1 1 calc R . . H5B H 0.2661 0.0042 -0.4468 0.067 Uiso 1 1 calc R . . H5C H 0.3129 0.0589 -0.5165 0.067 Uiso 1 1 calc R . . C6 C 0.5614(8) 0.0351(3) -0.3048(8) 0.0391(16) Uani 1 1 d . . . H6A H 0.5455 -0.0083 -0.3263 0.059 Uiso 1 1 calc R . . H6B H 0.6494 0.0407 -0.2122 0.059 Uiso 1 1 calc R . . H6C H 0.5812 0.0557 -0.3750 0.059 Uiso 1 1 calc R . . C7 C 0.4383(9) 0.1287(3) -0.2854(7) 0.0363(15) Uani 1 1 d . . . H7A H 0.3380 0.1475 -0.3083 0.044 Uiso 1 1 calc R . . H7B H 0.4759 0.1462 -0.3480 0.044 Uiso 1 1 calc R . . C8 C 0.5508(8) 0.1415(3) -0.1361(7) 0.0339(15) Uani 1 1 d . . . H8A H 0.6561 0.1304 -0.1175 0.041 Uiso 1 1 calc R . . H8B H 0.5493 0.1851 -0.1148 0.041 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 0.0257(7) 0.0328(7) 0.0240(7) -0.0021(4) 0.0116(5) -0.0018(4) Ti2 0.0223(6) 0.0327(6) 0.0216(6) 0.0000(4) 0.0097(4) 0.0004(4) N1 0.032(3) 0.042(3) 0.025(3) -0.002(2) 0.013(2) 0.002(2) N2 0.030(3) 0.038(3) 0.028(3) 0.000(2) 0.013(2) 0.000(2) O1 0.041(3) 0.037(2) 0.027(2) -0.0007(17) 0.018(2) 0.0003(19) O2 0.029(2) 0.039(2) 0.035(3) -0.0029(19) 0.014(2) -0.0061(18) C21 0.040(5) 0.056(5) 0.064(6) -0.006(4) 0.000(4) -0.012(4) C22 0.043(10) 0.098(17) 0.083(16) -0.060(14) 0.033(12) -0.031(10) C23 0.11(2) 0.30(6) 0.21(4) -0.20(4) 0.13(3) -0.14(3) C22A 0.049(10) 0.042(9) 0.084(15) -0.015(9) 0.029(11) -0.011(7) C23A 0.043(10) 0.056(11) 0.11(2) -0.011(11) 0.030(12) -0.001(8) O3 0.021(2) 0.039(2) 0.027(2) -0.0049(17) 0.0069(18) -0.0024(17) O4 0.033(2) 0.033(2) 0.026(2) 0.0005(16) 0.018(2) -0.0036(17) O5 0.026(2) 0.033(2) 0.019(2) 0.0002(15) 0.0117(17) -0.0005(16) O6 0.026(2) 0.045(3) 0.029(2) -0.0003(18) 0.010(2) 0.0054(18) C61 0.026(3) 0.054(4) 0.032(4) -0.005(3) 0.007(3) 0.004(3) C62 0.034(4) 0.086(6) 0.054(5) -0.012(4) 0.026(4) -0.012(4) C63 0.030(4) 0.069(6) 0.067(6) 0.007(4) -0.005(4) 0.012(4) C1 0.052(5) 0.047(4) 0.033(4) 0.005(3) 0.019(3) 0.014(3) C2 0.036(4) 0.057(5) 0.047(5) -0.012(3) 0.021(4) -0.001(3) C3 0.046(4) 0.042(4) 0.038(4) -0.013(3) 0.025(3) -0.001(3) C4 0.049(4) 0.047(4) 0.036(4) -0.007(3) 0.027(4) 0.001(3) C5 0.044(4) 0.064(5) 0.024(4) 0.001(3) 0.014(3) -0.008(3) C6 0.042(4) 0.043(4) 0.043(4) 0.003(3) 0.029(3) 0.003(3) C7 0.052(4) 0.039(4) 0.025(4) 0.005(3) 0.024(3) -0.001(3) C8 0.037(4) 0.035(3) 0.031(4) 0.003(3) 0.017(3) -0.006(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 1.799(4) . ? Ti1 O2 1.855(4) . ? Ti1 O1 1.877(5) . ? Ti1 O4 2.039(4) . ? Ti1 O5 2.076(4) . ? Ti1 N1 2.372(5) . ? Ti1 Ti2 2.9635(15) 3_655 ? Ti1 Ti2 3.1641(15) . ? Ti2 O6 1.834(4) . ? Ti2 O5 1.863(4) . ? Ti2 O3 1.883(4) 3_655 ? Ti2 O4 2.019(4) . ? Ti2 O5 2.066(4) 3_655 ? Ti2 N2 2.292(6) . ? Ti2 Ti1 2.9635(15) 3_655 ? Ti2 Ti2 2.974(2) 3_655 ? N1 C1 1.470(9) . ? N1 C3 1.473(8) . ? N1 C2 1.479(9) . ? N2 C5 1.466(9) . ? N2 C7 1.492(8) . ? N2 C6 1.504(8) . ? O1 C4 1.412(8) . ? O2 C21 1.400(9) . ? C21 C23A 1.35(2) . ? C21 C22 1.37(2) . ? C21 C22A 1.554(19) . ? C21 C23 1.572(17) . ? C21 H21 1.0000 . ? C21 H21A 1.0000 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22A H22D 0.9800 . ? C22A H22E 0.9800 . ? C22A H22F 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? O3 Ti2 1.883(4) 3_655 ? O4 C8 1.423(7) . ? O5 Ti2 2.066(4) 3_655 ? O6 C61 1.432(8) . ? C61 C63 1.508(11) . ? C61 C62 1.514(11) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.523(10) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.500(9) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 H8A 0.9900 . ? C8 H8B 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 O3 Ti1 O2 102.2(2) . . ? O3 Ti1 O1 95.4(2) . . ? O2 Ti1 O1 98.9(2) . . ? O3 Ti1 O4 102.11(19) . . ? O2 Ti1 O4 85.48(19) . . ? O1 Ti1 O4 160.6(2) . . ? O3 Ti1 O5 81.35(18) . . ? O2 Ti1 O5 158.25(19) . . ? O1 Ti1 O5 102.18(18) . . ? O4 Ti1 O5 72.84(16) . . ? O3 Ti1 N1 166.4(2) . . ? O2 Ti1 N1 89.2(2) . . ? O1 Ti1 N1 75.2(2) . . ? O4 Ti1 N1 86.06(18) . . ? O5 Ti1 N1 90.88(18) . . ? O3 Ti1 Ti2 37.40(13) . 3_655 ? O2 Ti1 Ti2 133.98(15) . 3_655 ? O1 Ti1 Ti2 104.69(14) . 3_655 ? O4 Ti1 Ti2 84.97(12) . 3_655 ? O5 Ti1 Ti2 44.19(12) . 3_655 ? N1 Ti1 Ti2 134.72(14) . 3_655 ? O3 Ti1 Ti2 90.56(14) . . ? O2 Ti1 Ti2 123.95(15) . . ? O1 Ti1 Ti2 134.38(15) . . ? O4 Ti1 Ti2 38.54(12) . . ? O5 Ti1 Ti2 34.32(11) . . ? N1 Ti1 Ti2 89.21(13) . . ? Ti2 Ti1 Ti2 57.96(4) 3_655 . ? O6 Ti2 O5 103.8(2) . . ? O6 Ti2 O3 90.34(19) . 3_655 ? O5 Ti2 O3 109.66(19) . 3_655 ? O6 Ti2 O4 95.81(19) . . ? O5 Ti2 O4 77.90(17) . . ? O3 Ti2 O4 168.87(19) 3_655 . ? O6 Ti2 O5 169.81(19) . 3_655 ? O5 Ti2 O5 81.76(18) . 3_655 ? O3 Ti2 O5 79.70(17) 3_655 3_655 ? O4 Ti2 O5 93.69(17) . 3_655 ? O6 Ti2 N2 91.0(2) . . ? O5 Ti2 N2 150.61(19) . . ? O3 Ti2 N2 95.2(2) 3_655 . ? O4 Ti2 N2 75.42(18) . . ? O5 Ti2 N2 87.83(18) 3_655 . ? O6 Ti2 Ti1 125.72(15) . 3_655 ? O5 Ti2 Ti1 95.85(13) . 3_655 ? O3 Ti2 Ti1 35.47(13) 3_655 3_655 ? O4 Ti2 Ti1 137.98(13) . 3_655 ? O5 Ti2 Ti1 44.47(11) 3_655 3_655 ? N2 Ti2 Ti1 95.72(14) . 3_655 ? O6 Ti2 Ti2 146.47(16) . 3_655 ? O5 Ti2 Ti2 43.45(13) . 3_655 ? O3 Ti2 Ti2 94.96(14) 3_655 3_655 ? O4 Ti2 Ti2 85.03(13) . 3_655 ? O5 Ti2 Ti2 38.32(11) 3_655 3_655 ? N2 Ti2 Ti2 121.30(15) . 3_655 ? Ti1 Ti2 Ti2 64.41(4) 3_655 3_655 ? O6 Ti2 Ti1 103.68(15) . . ? O5 Ti2 Ti1 38.93(12) . . ? O3 Ti2 Ti1 147.58(15) 3_655 . ? O4 Ti2 Ti1 38.99(12) . . ? O5 Ti2 Ti1 86.04(12) 3_655 . ? N2 Ti2 Ti1 113.26(14) . . ? Ti1 Ti2 Ti1 122.04(4) 3_655 . ? Ti2 Ti2 Ti1 57.64(4) 3_655 . ? C1 N1 C3 109.3(6) . . ? C1 N1 C2 109.6(6) . . ? C3 N1 C2 110.5(6) . . ? C1 N1 Ti1 115.2(4) . . ? C3 N1 Ti1 99.2(4) . . ? C2 N1 Ti1 112.5(4) . . ? C5 N2 C7 110.1(5) . . ? C5 N2 C6 108.0(6) . . ? C7 N2 C6 109.7(5) . . ? C5 N2 Ti2 111.1(4) . . ? C7 N2 Ti2 103.6(4) . . ? C6 N2 Ti2 114.3(4) . . ? C4 O1 Ti1 124.6(4) . . ? C21 O2 Ti1 130.5(5) . . ? C23A C21 C22 118.3(15) . . ? C23A C21 O2 121.2(12) . . ? C22 C21 O2 120.5(11) . . ? C23A C21 C22A 118.7(13) . . ? O2 C21 C22A 105.9(9) . . ? C23A C21 C23 50(2) . . ? C22 C21 C23 114.2(17) . . ? O2 C21 C23 104.1(13) . . ? C22A C21 C23 84(2) . . ? C23A C21 H21 56.4 . . ? C22 C21 H21 105.6 . . ? O2 C21 H21 105.6 . . ? C22A C21 H21 143.3 . . ? C23 C21 H21 105.6 . . ? C23A C21 H21A 102.7 . . ? C22 C21 H21A 62.8 . . ? O2 C21 H21A 102.7 . . ? C22A C21 H21A 102.7 . . ? C23 C21 H21A 149.2 . . ? H21 C21 H21A 52.0 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22A H22D 109.5 . . ? C21 C22A H22E 109.5 . . ? H22D C22A H22E 109.5 . . ? C21 C22A H22F 109.5 . . ? H22D C22A H22F 109.5 . . ? H22E C22A H22F 109.5 . . ? C21 C23A H23D 109.5 . . ? C21 C23A H23E 109.5 . . ? H23D C23A H23E 109.5 . . ? C21 C23A H23F 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? Ti1 O3 Ti2 107.1(2) . 3_655 ? C8 O4 Ti2 122.6(4) . . ? C8 O4 Ti1 133.6(4) . . ? Ti2 O4 Ti1 102.47(18) . . ? Ti2 O5 Ti2 98.24(18) . 3_655 ? Ti2 O5 Ti1 106.75(19) . . ? Ti2 O5 Ti1 91.34(17) 3_655 . ? C61 O6 Ti2 134.3(4) . . ? O6 C61 C63 108.4(6) . . ? O6 C61 C62 110.0(6) . . ? C63 C61 C62 112.8(7) . . ? O6 C61 H61 108.5 . . ? C63 C61 H61 108.5 . . ? C62 C61 H61 108.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 108.6(6) . . ? N1 C3 H3A 110.0 . . ? C4 C3 H3A 110.0 . . ? N1 C3 H3B 110.0 . . ? C4 C3 H3B 110.0 . . ? H3A C3 H3B 108.3 . . ? O1 C4 C3 109.4(6) . . ? O1 C4 H4A 109.8 . . ? C3 C4 H4A 109.8 . . ? O1 C4 H4B 109.8 . . ? C3 C4 H4B 109.8 . . ? H4A C4 H4B 108.2 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 108.9(5) . . ? N2 C7 H7A 109.9 . . ? C8 C7 H7A 109.9 . . ? N2 C7 H7B 109.9 . . ? C8 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? O4 C8 C7 106.4(5) . . ? O4 C8 H8A 110.4 . . ? C7 C8 H8A 110.4 . . ? O4 C8 H8B 110.4 . . ? C7 C8 H8B 110.4 . . ? H8A C8 H8B 108.6 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.504 _refine_diff_density_min -0.637 _refine_diff_density_rms 0.136