# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2137 # Data for 4 and 5 only (2 is hard copy) data_pwn #compound 4 in "Chiral N2O2 Schiff-base complexes.." _audit_creation_method shelxl-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'c58 h68 n2 o2 ti' _chemical_formula_weight 873.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'c' 'c' 0.0033 0.0016 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'h' 'h' 0.0000 0.0000 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'n' 'n' 0.0061 0.0033 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'o' 'o' 0.0106 0.0060 'international tables vol c tables 4.2.6.8 and 6.1.1.4' 'ti' 'ti' 0.2776 0.4457 'international tables vol c tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_h-m p2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 19.7558(10) _cell_length_b 10.2159(5) _cell_length_c 26.3957(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.6850(10) _cell_angle_gamma 90.00 _cell_volume 5251.3(5) _cell_formula_units_z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5288 _cell_measurement_theta_min 1.50 _cell_measurement_theta_max 22.50 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.104 _exptl_crystal_density_method 'not measured' _exptl_crystal_f_000 1872 _exptl_absorpt_coefficient_mu 0.204 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_t_min 0.639356 _exptl_absorpt_correction_t_max 0.927989 _exptl_absorpt_process_details 'sadabs (sheldrick, 1996)' _exptl_special_details ; the temperature of the crystal was controlled using the oxford cryosystem cryostream cooler (cosier & glazer, 1986). the data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. the crystal-to-detector distance was 5.0 cm. coverage of the unique set is over 97% complete to at least 26\% in \q. crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. hydrogen atoms were added at calculated positions and refined using a riding model. anisotropic displacement parameters were used for all non-h atoms h-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type mok\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'siemens smart diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 20157 _diffrn_reflns_av_r_equivalents 0.1071 _diffrn_reflns_av_sigmai/neti 0.1308 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 22.50 _reflns_number_total 6819 _reflns_number_gt 3831 _reflns_threshold_expression >2sigma(i) _computing_data_collection 'siemens xscans' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'Siemens SHELXTL' _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^)+(0.1662P)^2^+3.1181P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6819 _refine_ls_number_parameters 582 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1729 _refine_ls_R_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.2960 _refine_ls_wR_factor_gt 0.2521 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.108 _refine_ls_shift/su_mean 0.011 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 0.30467(7) 0.79815(13) 0.15358(5) 0.0269(4) Uani 1 1 d . . . O1 O 0.3111(3) 0.7174(5) 0.09003(17) 0.0322(13) Uani 1 1 d . . . O2 O 0.2562(2) 0.9525(5) 0.13243(18) 0.0307(13) Uani 1 1 d . . . N1 N 0.3479(3) 0.6036(6) 0.1825(2) 0.0266(15) Uani 1 1 d . . . N2 N 0.2455(3) 0.7671(6) 0.2011(2) 0.0277(15) Uani 1 1 d . . . C1 C 0.3391(4) 0.6133(7) 0.0692(3) 0.0308(19) Uani 1 1 d . . . C2 C 0.3326(4) 0.6010(7) 0.0151(3) 0.033(2) Uani 1 1 d . . . C3 C 0.3621(4) 0.4908(8) -0.0021(3) 0.039(2) Uani 1 1 d . . . H3A H 0.3573 0.4798 -0.0382 0.047 Uiso 1 1 calc R . . C4 C 0.3984(4) 0.3930(7) 0.0287(3) 0.033(2) Uani 1 1 d . . . C5 C 0.4022(4) 0.4091(7) 0.0802(3) 0.036(2) Uani 1 1 d . . . H5A H 0.4260 0.3457 0.1028 0.044 Uiso 1 1 calc R . . C6 C 0.3718(4) 0.5173(7) 0.1012(3) 0.0275(18) Uani 1 1 d . . . C7 C 0.2946(5) 0.7027(8) -0.0212(3) 0.049(2) Uani 1 1 d . . . C8 C 0.3293(5) 0.8373(8) -0.0108(3) 0.054(3) Uani 1 1 d . . . H8A H 0.3061 0.9014 -0.0354 0.081 Uiso 1 1 calc R . . H8B H 0.3777 0.8307 -0.0147 0.081 Uiso 1 1 calc R . . H8C H 0.3262 0.8654 0.0242 0.081 Uiso 1 1 calc R . . C9 C 0.2194(5) 0.7084(9) -0.0151(4) 0.065(3) Uani 1 1 d . . . H9A H 0.1957 0.7751 -0.0383 0.097 Uiso 1 1 calc R . . H9B H 0.2161 0.7309 0.0205 0.097 Uiso 1 1 calc R . . H9C H 0.1980 0.6230 -0.0237 0.097 Uiso 1 1 calc R . . C10 C 0.2957(7) 0.6691(9) -0.0774(3) 0.091(4) Uani 1 1 d . . . H10A H 0.2730 0.7389 -0.0994 0.137 Uiso 1 1 calc R . . H10B H 0.2714 0.5863 -0.0860 0.137 Uiso 1 1 calc R . . H10C H 0.3434 0.6605 -0.0828 0.137 Uiso 1 1 calc R . . C11 C 0.4286(5) 0.2748(8) 0.0043(3) 0.045(2) Uani 1 1 d . . . C12 C 0.4709(6) 0.3174(9) -0.0350(4) 0.078(3) Uani 1 1 d . . . H12A H 0.4429 0.3726 -0.0608 0.116 Uiso 1 1 calc R . . H12B H 0.4866 0.2402 -0.0518 0.116 Uiso 1 1 calc R . . H12C H 0.5107 0.3673 -0.0181 0.116 Uiso 1 1 calc R . . C13 C 0.3702(5) 0.1869(9) -0.0224(4) 0.072(3) Uani 1 1 d . . . H13A H 0.3416 0.2363 -0.0498 0.108 Uiso 1 1 calc R . . H13B H 0.3420 0.1580 0.0027 0.108 Uiso 1 1 calc R . . H13C H 0.3896 0.1104 -0.0371 0.108 Uiso 1 1 calc R . . C14 C 0.4734(6) 0.1904(10) 0.0458(3) 0.077(3) Uani 1 1 d . . . H14A H 0.4933 0.1174 0.0292 0.115 Uiso 1 1 calc R . . H14B H 0.4449 0.1561 0.0697 0.115 Uiso 1 1 calc R . . H14C H 0.5103 0.2444 0.0646 0.115 Uiso 1 1 calc R . . C15 C 0.3742(4) 0.5171(7) 0.1561(3) 0.0292(19) Uani 1 1 d . . . H15A H 0.3975 0.4461 0.1746 0.035 Uiso 1 1 calc R . . C16 C 0.3555(4) 0.5759(7) 0.2371(3) 0.0259(18) Uani 1 1 d . . . C17 C 0.4193(4) 0.5794(7) 0.2666(3) 0.0319(19) Uani 1 1 d . . . H17A H 0.4588 0.5964 0.2515 0.038 Uiso 1 1 calc R . . C18 C 0.4253(4) 0.5574(7) 0.3194(3) 0.036(2) Uani 1 1 d . . . H18A H 0.4693 0.5582 0.3404 0.043 Uiso 1 1 calc R . . C19 C 0.3680(4) 0.5346(7) 0.3408(3) 0.035(2) Uani 1 1 d . . . H19A H 0.3728 0.5225 0.3769 0.042 Uiso 1 1 calc R . . C20 C 0.3023(4) 0.5286(7) 0.3107(3) 0.0317(19) Uani 1 1 d . . . C21 C 0.2953(4) 0.5479(6) 0.2571(3) 0.0245(18) Uani 1 1 d . . . C22 C 0.2413(4) 0.5096(8) 0.3365(3) 0.039(2) Uani 1 1 d . . . H22A H 0.2159 0.4317 0.3224 0.058 Uiso 1 1 calc R . . H22B H 0.2114 0.5865 0.3305 0.058 Uiso 1 1 calc R . . H22C H 0.2565 0.4981 0.3735 0.058 Uiso 1 1 calc R . . C23 C 0.2280(4) 0.5408(7) 0.2231(3) 0.0287(19) Uani 1 1 d . . . C24 C 0.1897(4) 0.4230(7) 0.2143(3) 0.0312(19) Uani 1 1 d . . . C25 C 0.1253(4) 0.4292(8) 0.1830(3) 0.044(2) Uani 1 1 d . . . H25A H 0.0993 0.3508 0.1767 0.053 Uiso 1 1 calc R . . C26 C 0.0979(5) 0.5424(9) 0.1609(3) 0.052(2) Uani 1 1 d . . . H26A H 0.0528 0.5431 0.1416 0.062 Uiso 1 1 calc R . . C27 C 0.1367(4) 0.6565(8) 0.1669(3) 0.041(2) Uani 1 1 d . . . H27A H 0.1192 0.7349 0.1503 0.049 Uiso 1 1 calc R . . C28 C 0.2013(4) 0.6552(7) 0.1974(3) 0.0301(19) Uani 1 1 d . . . C29 C 0.2166(5) 0.2935(7) 0.2358(3) 0.049(2) Uani 1 1 d . . . H29A H 0.2614 0.3061 0.2576 0.074 Uiso 1 1 calc R . . H29B H 0.2216 0.2341 0.2075 0.074 Uiso 1 1 calc R . . H29C H 0.1844 0.2557 0.2562 0.074 Uiso 1 1 calc R . . C30 C 0.2225(4) 0.8887(7) 0.2255(3) 0.0295(19) Uani 1 1 d . . . H30A H 0.2642 0.9455 0.2336 0.035 Uiso 1 1 calc R . . C31 C 0.1726(4) 0.9631(7) 0.1874(3) 0.0292(19) Uani 1 1 d . . . C32 C 0.1071(4) 0.9922(7) 0.1950(3) 0.036(2) Uani 1 1 d . . . H32A H 0.0928 0.9647 0.2259 0.043 Uiso 1 1 calc R . . C33 C 0.0603(4) 1.0623(7) 0.1579(3) 0.038(2) Uani 1 1 d . . . C34 C 0.0868(4) 1.1107(8) 0.1159(3) 0.040(2) Uani 1 1 d . . . H34A H 0.0577 1.1636 0.0919 0.048 Uiso 1 1 calc R . . C35 C 0.1540(4) 1.0862(7) 0.1067(3) 0.034(2) Uani 1 1 d . . . C36 C 0.1947(4) 1.0022(7) 0.1413(3) 0.0282(19) Uani 1 1 d . . . C37 C -0.0140(4) 1.0791(9) 0.1649(4) 0.052(3) Uani 1 1 d . . . C38 C -0.0174(6) 1.1392(14) 0.2170(4) 0.101(4) Uani 1 1 d . . . H38A H 0.0078 1.2223 0.2204 0.152 Uiso 1 1 calc R . . H38B H 0.0033 1.0791 0.2442 0.152 Uiso 1 1 calc R . . H38C H -0.0655 1.1550 0.2201 0.152 Uiso 1 1 calc R . . C39 C -0.0541(5) 1.1678(12) 0.1249(4) 0.088(4) Uani 1 1 d . . . H39A H -0.0313 1.2532 0.1257 0.132 Uiso 1 1 calc R . . H39B H -0.1007 1.1794 0.1322 0.132 Uiso 1 1 calc R . . H39C H -0.0563 1.1285 0.0908 0.132 Uiso 1 1 calc R . . C40 C -0.0473(5) 0.9453(11) 0.1618(7) 0.128(6) Uani 1 1 d . . . H40A H -0.0476 0.9084 0.1275 0.193 Uiso 1 1 calc R . . H40B H -0.0946 0.9533 0.1681 0.193 Uiso 1 1 calc R . . H40C H -0.0213 0.8876 0.1876 0.193 Uiso 1 1 calc R . . C41 C 0.1804(4) 1.1518(8) 0.0622(3) 0.046(2) Uani 1 1 d . . . C42 C 0.1312(5) 1.2543(9) 0.0345(4) 0.065(3) Uani 1 1 d . . . H42A H 0.0888 1.2114 0.0180 0.098 Uiso 1 1 calc R . . H42B H 0.1528 1.2985 0.0084 0.098 Uiso 1 1 calc R . . H42C H 0.1203 1.3188 0.0595 0.098 Uiso 1 1 calc R . . C43 C 0.2487(5) 1.2233(9) 0.0827(4) 0.063(3) Uani 1 1 d . . . H43A H 0.2819 1.1605 0.1006 0.095 Uiso 1 1 calc R . . H43B H 0.2403 1.2924 0.1066 0.095 Uiso 1 1 calc R . . H43C H 0.2671 1.2620 0.0539 0.095 Uiso 1 1 calc R . . C44 C 0.1926(5) 1.0486(9) 0.0219(3) 0.060(3) Uani 1 1 d . . . H44A H 0.1485 1.0123 0.0054 0.090 Uiso 1 1 calc R . . H44B H 0.2217 0.9782 0.0388 0.090 Uiso 1 1 calc R . . H44C H 0.2155 1.0899 -0.0042 0.090 Uiso 1 1 calc R . . C45 C 0.2014(4) 0.8556(7) 0.2774(3) 0.035(2) Uani 1 1 d . . . H45A H 0.1559 0.8122 0.2709 0.042 Uiso 1 1 calc R . . H45B H 0.2348 0.7922 0.2956 0.042 Uiso 1 1 calc R . . C46 C 0.1974(4) 0.9717(8) 0.3119(3) 0.037(2) Uani 1 1 d . . . C47 C 0.2540(5) 1.0553(8) 0.3243(3) 0.040(2) Uani 1 1 d . . . H47A H 0.2937 1.0425 0.3091 0.048 Uiso 1 1 calc R . . C48 C 0.2520(5) 1.1568(9) 0.3590(3) 0.053(3) Uani 1 1 d . . . H48A H 0.2909 1.2123 0.3676 0.063 Uiso 1 1 calc R . . C49 C 0.1958(6) 1.1780(9) 0.3808(4) 0.064(3) Uani 1 1 d . . . H49A H 0.1956 1.2470 0.4049 0.077 Uiso 1 1 calc R . . C50 C 0.1387(6) 1.0996(11) 0.3679(4) 0.071(3) Uani 1 1 d . . . H50A H 0.0986 1.1167 0.3823 0.085 Uiso 1 1 calc R . . C51 C 0.1395(5) 0.9951(9) 0.3339(4) 0.056(3) Uani 1 1 d . . . H51A H 0.1004 0.9400 0.3257 0.067 Uiso 1 1 calc R . . C52 C 0.3995(4) 0.8873(7) 0.1833(3) 0.0329(19) Uani 1 1 d . . . H52A H 0.4327 0.8157 0.1935 0.039 Uiso 1 1 calc R . . H52B H 0.4150 0.9335 0.1543 0.039 Uiso 1 1 calc R . . C53 C 0.4072(4) 0.9811(7) 0.2270(3) 0.033(2) Uani 1 1 d . . . C54 C 0.4306(4) 0.9399(8) 0.2779(3) 0.041(2) Uani 1 1 d . . . H54A H 0.4397 0.8496 0.2844 0.050 Uiso 1 1 calc R . . C55 C 0.4407(4) 1.0265(9) 0.3184(4) 0.049(2) Uani 1 1 d . . . H55A H 0.4563 0.9954 0.3523 0.059 Uiso 1 1 calc R . . C56 C 0.4283(4) 1.1579(9) 0.3100(3) 0.046(2) Uani 1 1 d . . . H56A H 0.4361 1.2180 0.3379 0.055 Uiso 1 1 calc R . . C57 C 0.4043(4) 1.2018(9) 0.2608(4) 0.046(2) Uani 1 1 d . . . H57A H 0.3957 1.2925 0.2548 0.056 Uiso 1 1 calc R . . C58 C 0.3928(4) 1.1149(8) 0.2203(3) 0.038(2) Uani 1 1 d . . . H58A H 0.3746 1.1465 0.1869 0.046 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 0.0343(8) 0.0194(8) 0.0289(8) 0.0007(6) 0.0107(6) 0.0018(6) O1 0.050(3) 0.022(3) 0.027(3) 0.001(2) 0.010(2) 0.004(3) O2 0.030(3) 0.023(3) 0.042(3) 0.007(2) 0.014(2) 0.012(2) N1 0.027(4) 0.030(4) 0.024(3) 0.002(3) 0.009(3) 0.002(3) N2 0.032(4) 0.018(4) 0.034(4) -0.001(3) 0.007(3) 0.000(3) C1 0.043(5) 0.019(5) 0.032(5) -0.002(4) 0.010(4) 0.002(4) C2 0.050(5) 0.023(5) 0.025(5) -0.008(4) 0.006(4) 0.003(4) C3 0.066(6) 0.031(5) 0.023(4) 0.000(4) 0.013(4) -0.004(4) C4 0.057(6) 0.021(5) 0.024(5) 0.002(4) 0.013(4) 0.005(4) C5 0.050(5) 0.025(5) 0.035(5) 0.005(4) 0.010(4) -0.001(4) C6 0.044(5) 0.014(4) 0.026(4) -0.002(4) 0.011(4) 0.001(4) C7 0.088(8) 0.035(6) 0.023(5) -0.001(4) 0.004(4) 0.008(5) C8 0.106(8) 0.023(5) 0.038(5) 0.005(4) 0.029(5) 0.013(5) C9 0.089(8) 0.030(6) 0.065(7) 0.005(5) -0.019(6) 0.004(5) C10 0.191(13) 0.040(6) 0.034(6) 0.002(5) -0.009(6) 0.036(7) C11 0.081(7) 0.027(5) 0.032(5) -0.005(4) 0.023(5) 0.000(5) C12 0.119(10) 0.048(7) 0.084(8) -0.012(6) 0.070(7) -0.004(6) C13 0.105(9) 0.035(6) 0.077(7) -0.025(5) 0.018(6) 0.008(6) C14 0.108(9) 0.074(8) 0.050(6) -0.013(6) 0.017(6) 0.053(7) C15 0.034(5) 0.025(5) 0.031(5) -0.002(4) 0.011(4) 0.011(4) C16 0.039(5) 0.011(4) 0.029(4) -0.002(3) 0.010(4) 0.004(3) C17 0.038(5) 0.024(5) 0.034(5) 0.003(4) 0.007(4) 0.004(4) C18 0.043(5) 0.031(5) 0.032(5) -0.002(4) 0.002(4) 0.004(4) C19 0.064(6) 0.023(5) 0.021(4) 0.004(4) 0.014(4) 0.006(4) C20 0.045(5) 0.015(4) 0.036(5) 0.001(4) 0.010(4) 0.003(4) C21 0.036(5) 0.012(4) 0.025(4) 0.000(3) 0.002(4) 0.003(3) C22 0.059(6) 0.027(5) 0.035(5) 0.002(4) 0.021(4) -0.002(4) C23 0.034(5) 0.021(5) 0.035(5) -0.003(4) 0.019(4) 0.004(4) C24 0.045(5) 0.020(5) 0.032(5) 0.000(4) 0.016(4) -0.001(4) C25 0.046(6) 0.029(5) 0.057(6) -0.009(5) 0.008(5) -0.016(4) C26 0.050(6) 0.040(6) 0.060(6) -0.010(5) -0.007(5) -0.006(5) C27 0.041(5) 0.026(5) 0.053(6) -0.002(4) 0.000(4) 0.006(4) C28 0.034(5) 0.025(5) 0.034(5) -0.005(4) 0.015(4) 0.002(4) C29 0.074(7) 0.018(5) 0.057(6) 0.003(4) 0.016(5) -0.008(4) C30 0.038(5) 0.016(4) 0.036(5) -0.007(4) 0.009(4) -0.001(4) C31 0.041(5) 0.012(4) 0.037(5) -0.004(4) 0.012(4) 0.004(4) C32 0.050(6) 0.018(4) 0.042(5) 0.006(4) 0.018(4) 0.000(4) C33 0.044(5) 0.023(5) 0.050(6) -0.002(4) 0.016(4) -0.004(4) C34 0.043(6) 0.026(5) 0.051(6) 0.003(4) 0.005(4) 0.012(4) C35 0.044(5) 0.017(4) 0.042(5) 0.002(4) 0.010(4) -0.002(4) C36 0.038(5) 0.014(4) 0.034(5) 0.002(4) 0.011(4) 0.004(4) C37 0.027(5) 0.049(6) 0.081(7) 0.013(5) 0.011(5) 0.012(4) C38 0.076(8) 0.147(12) 0.090(9) 0.010(9) 0.038(7) 0.057(8) C39 0.055(7) 0.110(10) 0.101(9) 0.005(8) 0.020(6) 0.029(7) C40 0.037(7) 0.069(9) 0.29(2) 0.005(10) 0.058(9) 0.000(6) C41 0.049(6) 0.036(5) 0.055(6) 0.015(5) 0.014(5) 0.014(5) C42 0.079(7) 0.050(6) 0.070(7) 0.037(5) 0.023(6) 0.028(5) C43 0.081(8) 0.038(6) 0.078(7) 0.023(5) 0.034(6) 0.000(5) C44 0.072(7) 0.065(7) 0.045(6) 0.013(5) 0.016(5) 0.018(6) C45 0.047(5) 0.030(5) 0.032(5) 0.009(4) 0.015(4) 0.000(4) C46 0.051(6) 0.026(5) 0.039(5) -0.003(4) 0.018(4) 0.011(4) C47 0.057(6) 0.032(5) 0.030(5) -0.005(4) 0.006(4) 0.003(4) C48 0.082(8) 0.032(6) 0.045(6) 0.002(5) 0.014(5) 0.002(5) C49 0.110(10) 0.036(6) 0.048(6) -0.014(5) 0.013(6) 0.003(6) C50 0.073(8) 0.078(8) 0.070(7) -0.016(6) 0.040(6) 0.012(7) C51 0.074(7) 0.037(6) 0.069(7) -0.012(5) 0.047(6) -0.011(5) C52 0.030(5) 0.023(5) 0.048(5) 0.000(4) 0.014(4) 0.001(4) C53 0.030(5) 0.022(5) 0.049(6) 0.003(4) 0.010(4) -0.009(4) C54 0.048(6) 0.027(5) 0.048(6) -0.001(4) 0.006(4) 0.002(4) C55 0.054(6) 0.038(6) 0.056(6) -0.001(5) 0.015(5) -0.009(5) C56 0.046(6) 0.051(7) 0.042(6) -0.019(5) 0.010(4) -0.009(5) C57 0.047(6) 0.030(5) 0.063(7) -0.004(5) 0.011(5) -0.002(4) C58 0.032(5) 0.036(6) 0.045(5) -0.001(4) 0.001(4) 0.000(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ti1 O2 1.880(5) . y Ti1 N2 1.881(6) . y Ti1 O1 1.893(5) . y Ti1 C52 2.112(7) . y Ti1 N1 2.246(6) . y O1 C1 1.357(8) . ? O2 C36 1.371(8) . ? N1 C15 1.288(8) . ? N1 C16 1.450(9) . ? N2 C28 1.431(9) . ? N2 C30 1.503(9) . y C1 C6 1.382(10) . ? C1 C2 1.418(10) . ? C2 C3 1.378(10) . ? C2 C7 1.525(11) . ? C3 C4 1.406(11) . ? C4 C5 1.359(10) . ? C4 C11 1.535(10) . ? C5 C6 1.416(10) . ? C6 C15 1.441(10) . ? C7 C9 1.521(13) . ? C7 C10 1.525(11) . ? C7 C8 1.541(12) . ? C11 C12 1.501(11) . ? C11 C13 1.537(12) . ? C11 C14 1.549(12) . ? C16 C17 1.367(10) . ? C16 C21 1.409(10) . ? C17 C18 1.397(10) . ? C18 C19 1.367(10) . ? C19 C20 1.404(11) . ? C20 C21 1.411(10) . ? C20 C22 1.494(10) . ? C21 C23 1.477(10) . ? C23 C28 1.408(10) . ? C23 C24 1.419(10) . ? C24 C25 1.399(11) . ? C24 C29 1.500(10) . ? C25 C26 1.365(12) . ? C26 C27 1.390(11) . ? C27 C28 1.389(10) . ? C30 C31 1.494(10) . ? C30 C45 1.535(9) . y C31 C32 1.375(10) . ? C31 C36 1.417(10) . ? C32 C33 1.421(11) . ? C33 C34 1.394(11) . ? C33 C37 1.519(11) . ? C34 C35 1.412(11) . ? C35 C36 1.404(10) . ? C35 C41 1.519(11) . ? C37 C39 1.511(13) . ? C37 C40 1.513(14) . ? C37 C38 1.517(13) . ? C41 C42 1.529(11) . ? C41 C44 1.545(12) . ? C41 C43 1.549(12) . ? C45 C46 1.506(10) . y C46 C51 1.387(11) . y C46 C47 1.402(11) . y C47 C48 1.388(11) . y C48 C49 1.352(12) . y C49 C50 1.379(13) . y C50 C51 1.398(13) . y C52 C53 1.488(10) . y C53 C58 1.401(11) . y C53 C54 1.408(11) . y C54 C55 1.377(11) . y C55 C56 1.376(12) . y C56 C57 1.381(11) . y C57 C58 1.379(11) . y 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 N2 89.8(2) . . y O2 Ti1 O1 102.1(2) . . y N2 Ti1 O1 131.3(2) . . y O2 Ti1 C52 97.2(3) . . y N2 Ti1 C52 115.9(3) . . y O1 Ti1 C52 109.2(3) . . y O2 Ti1 N1 171.4(2) . . y N2 Ti1 N1 82.4(2) . . y O1 Ti1 N1 80.6(2) . . y C52 Ti1 N1 89.6(3) . . y C1 O1 Ti1 142.5(5) . . ? C36 O2 Ti1 132.9(4) . . ? C15 N1 C16 114.9(6) . . y C15 N1 Ti1 126.0(5) . . y C16 N1 Ti1 118.7(4) . . y C28 N2 C30 117.8(5) . . y C28 N2 Ti1 121.9(4) . . y C30 N2 Ti1 114.3(4) . . y O1 C1 C6 119.3(6) . . ? O1 C1 C2 120.2(7) . . ? C6 C1 C2 120.4(7) . . ? C3 C2 C1 115.6(7) . . ? C3 C2 C7 122.7(7) . . ? C1 C2 C7 121.7(7) . . ? C2 C3 C4 126.4(7) . . ? C5 C4 C3 115.3(7) . . ? C5 C4 C11 123.7(7) . . ? C3 C4 C11 120.9(7) . . ? C4 C5 C6 122.1(7) . . ? C1 C6 C5 120.0(7) . . ? C1 C6 C15 123.3(7) . . ? C5 C6 C15 116.7(7) . . ? C9 C7 C2 110.3(7) . . ? C9 C7 C10 106.6(8) . . ? C2 C7 C10 111.8(7) . . ? C9 C7 C8 111.1(7) . . ? C2 C7 C8 109.8(7) . . ? C10 C7 C8 107.2(7) . . ? C12 C11 C4 111.2(7) . . ? C12 C11 C13 108.4(8) . . ? C4 C11 C13 109.7(7) . . ? C12 C11 C14 109.4(8) . . ? C4 C11 C14 110.9(6) . . ? C13 C11 C14 107.1(8) . . ? N1 C15 C6 126.6(7) . . ? C17 C16 C21 123.1(7) . . ? C17 C16 N1 119.4(6) . . ? C21 C16 N1 117.4(6) . . ? C16 C17 C18 118.6(7) . . ? C19 C18 C17 120.2(7) . . ? C18 C19 C20 121.6(7) . . ? C19 C20 C21 119.1(7) . . ? C19 C20 C22 119.3(7) . . ? C21 C20 C22 121.6(7) . . ? C16 C21 C20 117.3(7) . . ? C16 C21 C23 120.8(6) . . ? C20 C21 C23 121.9(7) . . ? C28 C23 C24 118.7(7) . . ? C28 C23 C21 118.5(7) . . ? C24 C23 C21 122.8(7) . . ? C25 C24 C23 117.7(7) . . ? C25 C24 C29 119.5(7) . . ? C23 C24 C29 122.8(7) . . ? C26 C25 C24 123.1(7) . . ? C25 C26 C27 119.4(8) . . ? C28 C27 C26 119.6(8) . . ? C27 C28 C23 121.3(7) . . ? C27 C28 N2 121.5(7) . . ? C23 C28 N2 117.1(7) . . ? C31 C30 N2 110.2(6) . . ? C31 C30 C45 117.7(6) . . ? N2 C30 C45 110.3(6) . . y C32 C31 C36 119.9(7) . . ? C32 C31 C30 122.9(7) . . ? C36 C31 C30 117.2(7) . . ? C31 C32 C33 121.9(7) . . ? C34 C33 C32 115.9(7) . . ? C34 C33 C37 123.8(8) . . ? C32 C33 C37 120.3(7) . . ? C33 C34 C35 124.4(7) . . ? C36 C35 C34 116.7(7) . . ? C36 C35 C41 122.6(7) . . ? C34 C35 C41 120.7(7) . . ? O2 C36 C35 122.8(6) . . ? O2 C36 C31 116.9(6) . . ? C35 C36 C31 120.3(7) . . ? C39 C37 C40 109.3(9) . . ? C39 C37 C38 107.1(8) . . ? C40 C37 C38 109.3(10) . . ? C39 C37 C33 112.7(8) . . ? C40 C37 C33 108.1(7) . . ? C38 C37 C33 110.3(8) . . ? C35 C41 C42 113.4(7) . . ? C35 C41 C44 110.2(7) . . ? C42 C41 C44 107.4(7) . . ? C35 C41 C43 109.2(7) . . ? C42 C41 C43 106.9(8) . . ? C44 C41 C43 109.6(7) . . ? C46 C45 C30 114.6(6) . . y C51 C46 C47 118.6(8) . . ? C51 C46 C45 121.3(8) . . ? C47 C46 C45 120.1(7) . . ? C48 C47 C46 120.0(8) . . ? C49 C48 C47 121.1(9) . . ? C48 C49 C50 120.0(9) . . ? C49 C50 C51 120.3(9) . . ? C46 C51 C50 120.0(9) . . ? C53 C52 Ti1 122.3(5) . . y C58 C53 C54 116.1(7) . . y C58 C53 C52 122.5(7) . . ? C54 C53 C52 121.4(7) . . ? C55 C54 C53 122.0(8) . . ? C56 C55 C54 120.3(9) . . ? C55 C56 C57 119.4(8) . . ? C58 C57 C56 120.4(8) . . ? C57 C58 C53 121.8(8) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.487 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.099 ####END data_p1 #compound 5 in "Chiral N2O2 Schiff-base complexes.." _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C53.50 H67 N2 O3 Ti' _chemical_formula_weight 833.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.270(3) _cell_length_b 16.917(3) _cell_length_c 22.645(4) _cell_angle_alpha 89.2150(10) _cell_angle_beta 86.8140(10) _cell_angle_gamma 79.7910(10) _cell_volume 5371.9(16) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4296 _cell_measurement_theta_min 0.990 _cell_measurement_theta_max 22.50 _exptl_crystal_description Block _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.031 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.198 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.687340 _exptl_absorpt_correction_T_max 0.927987 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; The temperature of the crystal was controlled using the Oxford Cryosystem Cryostream Cooler (Cosier & Glazer, 1986). The data collection nominally covered over a hemisphere of reciprocal space, by a combination of three sets of exposures with different \f angles for the crystal; each 10 s exposure covered 0.3\% in \w. The crystal-to-detector distance was 5.0 cm. Coverage of the unique set is over 97% complete to at least 26\% in \q. Crystal decay was found to be negligible by by repeating the initial frames at t data collection and analyzing the duplicate reflections. Hydrogen atoms were added at calculated positions and refined using a riding model. Anisotropic displacement parameters were used for all non-H atoms H-atoms were given isotropic displacement parameter equal to 1.2 (or 1.5 for met atoms) times the equivalent isotropic displacement parameter of the atom to which they are attached. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.192 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% nil _diffrn_reflns_number 21842 _diffrn_reflns_av_R_equivalents 0.0691 _diffrn_reflns_av_sigmaI/netI 0.1342 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.22 _diffrn_reflns_theta_max 22.50 _reflns_number_total 13915 _reflns_number_gt 7293 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1994)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997)' _computing_publication_material 'SHELXTL (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1630P)^2^+16.8899P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13915 _refine_ls_number_parameters 1102 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2064 _refine_ls_R_factor_gt 0.1109 _refine_ls_wR_factor_ref 0.3584 _refine_ls_wR_factor_gt 0.2739 _refine_ls_goodness_of_fit_ref 1.112 _refine_ls_restrained_S_all 1.112 _refine_ls_shift/su_max 0.687 _refine_ls_shift/su_mean 0.005 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 0.84741(12) 0.67682(9) 0.29549(7) 0.0321(5) Uani 1 1 d . . . Ti2 Ti 0.88059(12) 0.75790(9) 0.19098(7) 0.0318(5) Uani 1 1 d . . . O1 O 0.8224(4) 0.6975(4) 0.3788(3) 0.0384(16) Uani 1 1 d . . . O2 O 0.7316(4) 0.6460(3) 0.2804(3) 0.0362(15) Uani 1 1 d . . . O3 O 0.9734(4) 0.7571(3) 0.1261(2) 0.0355(15) Uani 1 1 d . . . O4 O 0.7804(4) 0.7311(3) 0.1489(2) 0.0362(16) Uani 1 1 d . . . O5 O 0.8178(4) 0.7777(3) 0.2681(2) 0.0338(15) Uani 1 1 d . . . O6 O 0.9189(4) 0.6604(3) 0.2207(2) 0.0315(14) Uani 1 1 d . . . N1 N 0.9009(5) 0.5345(4) 0.2962(3) 0.0317(18) Uani 1 1 d . . . N2 N 0.9992(5) 0.6567(4) 0.3291(3) 0.0341(19) Uani 1 1 d . . . N3 N 0.9717(5) 0.8417(4) 0.2261(3) 0.0335(19) Uani 1 1 d . . . N4 N 0.7940(5) 0.8948(4) 0.1752(3) 0.0339(19) Uani 1 1 d . . . C1' C 0.7966(9) 1.1144(6) 0.2763(6) 0.075(4) Uani 1 1 d . . . H1'A H 0.7720 1.1123 0.2378 0.112 Uiso 1 1 calc R . . H1'B H 0.8413 1.1507 0.2753 0.112 Uiso 1 1 calc R . . H1'C H 0.7450 1.1330 0.3046 0.112 Uiso 1 1 calc R . . C1 C 1.1838(8) 0.4622(7) 0.4172(5) 0.070(4) Uani 1 1 d . . . H1A H 1.1893 0.4734 0.4582 0.105 Uiso 1 1 calc R . . H1B H 1.2057 0.5032 0.3932 0.105 Uiso 1 1 calc R . . H1C H 1.2219 0.4110 0.4074 0.105 Uiso 1 1 calc R . . C2' C 0.8458(8) 1.0319(6) 0.2937(5) 0.053(3) Uani 1 1 d . . . C2 C 1.0827(7) 0.4608(6) 0.4062(4) 0.046(3) Uani 1 1 d . . . C3 C 1.0272(9) 0.4288(6) 0.4491(5) 0.059(3) Uani 1 1 d . . . H3A H 1.0549 0.4045 0.4826 0.071 Uiso 1 1 calc R . . C3' C 0.8455(8) 1.0085(7) 0.3533(5) 0.061(3) Uani 1 1 d . . . H3'A H 0.8157 1.0451 0.3817 0.073 Uiso 1 1 calc R . . C4 C 0.9324(9) 0.4327(6) 0.4426(4) 0.058(3) Uani 1 1 d . . . H4A H 0.8961 0.4122 0.4725 0.069 Uiso 1 1 calc R . . C4' C 0.8876(8) 0.9335(7) 0.3710(5) 0.058(3) Uani 1 1 d . . . H4'A H 0.8873 0.9200 0.4110 0.069 Uiso 1 1 calc R . . C5' C 0.9298(8) 0.8792(6) 0.3302(4) 0.048(3) Uani 1 1 d . . . H5'A H 0.9579 0.8281 0.3422 0.058 Uiso 1 1 calc R . . C5 C 0.8873(7) 0.4666(5) 0.3925(4) 0.045(3) Uani 1 1 d . . . H5A H 0.8220 0.4697 0.3894 0.054 Uiso 1 1 calc R . . C6' C 0.9315(6) 0.8991(5) 0.2703(4) 0.035(2) Uani 1 1 d . . . C6 C 0.9429(7) 0.4952(5) 0.3478(4) 0.036(2) Uani 1 1 d . . . C7' C 0.8915(7) 0.9757(6) 0.2521(4) 0.037(2) Uani 1 1 d . . . C7 C 1.0395(7) 0.4917(5) 0.3539(4) 0.040(2) Uani 1 1 d . . . C8' C 0.8957(7) 0.9938(5) 0.1867(5) 0.044(3) Uani 1 1 d . . . C8 C 1.0981(6) 0.5267(6) 0.3058(4) 0.040(2) Uani 1 1 d . . . C9 C 1.0762(7) 0.6101(6) 0.2943(4) 0.041(2) Uani 1 1 d . . . C9' C 0.8466(7) 0.9534(5) 0.1487(4) 0.040(2) Uani 1 1 d . . . C10' C 0.8526(7) 0.9660(6) 0.0876(4) 0.047(3) Uani 1 1 d . . . H10A H 0.8203 0.9382 0.0626 0.056 Uiso 1 1 calc R . . C10 C 1.1277(7) 0.6448(7) 0.2501(5) 0.049(3) Uani 1 1 d . . . H10B H 1.1114 0.6994 0.2419 0.059 Uiso 1 1 calc R . . C11 C 1.2015(8) 0.5993(8) 0.2188(5) 0.060(3) Uani 1 1 d . . . H11A H 1.2375 0.6229 0.1904 0.072 Uiso 1 1 calc R . . C11' C 0.9062(8) 1.0194(7) 0.0651(5) 0.066(3) Uani 1 1 d . . . H11B H 0.9084 1.0297 0.0247 0.079 Uiso 1 1 calc R . . C12' C 0.9577(9) 1.0586(7) 0.1015(6) 0.069(4) Uani 1 1 d . . . H12A H 0.9951 1.0939 0.0850 0.083 Uiso 1 1 calc R . . C12 C 1.2228(8) 0.5177(7) 0.2294(5) 0.059(3) Uani 1 1 d . . . H12B H 1.2721 0.4870 0.2069 0.071 Uiso 1 1 calc R . . C13 C 1.1735(7) 0.4800(6) 0.2724(5) 0.047(3) Uani 1 1 d . . . C13' C 0.9544(8) 1.0459(6) 0.1625(6) 0.059(3) Uani 1 1 d . . . C14 C 1.1975(8) 0.3898(6) 0.2798(5) 0.061(3) Uani 1 1 d . . . H14A H 1.2352 0.3668 0.2458 0.091 Uiso 1 1 calc R . . H14B H 1.1397 0.3681 0.2838 0.091 Uiso 1 1 calc R . . H14C H 1.2329 0.3772 0.3146 0.091 Uiso 1 1 calc R . . C14' C 1.0165(9) 1.0849(7) 0.2002(6) 0.075(4) Uani 1 1 d . . . H14D H 1.0776 1.0838 0.1799 0.112 Uiso 1 1 calc R . . H14E H 1.0247 1.0562 0.2370 0.112 Uiso 1 1 calc R . . H14F H 0.9869 1.1396 0.2079 0.112 Uiso 1 1 calc R . . C15 C 1.0213(7) 0.6770(6) 0.3799(4) 0.040(2) Uani 1 1 d . . . H15A H 1.0857 0.6653 0.3875 0.048 Uiso 1 1 calc R . . C15' C 1.0548(7) 0.8523(5) 0.2023(4) 0.040(3) Uani 1 1 d . . . H15B H 1.0840 0.8890 0.2214 0.049 Uiso 1 1 calc R . . C16 C 0.9592(8) 0.7154(6) 0.4264(4) 0.041(3) Uani 1 1 d . . . C16' C 1.1068(7) 0.8150(6) 0.1506(4) 0.043(3) Uani 1 1 d . . . C17 C 1.0039(9) 0.7434(6) 0.4747(5) 0.053(3) Uani 1 1 d . . . H17A H 1.0700 0.7376 0.4741 0.063 Uiso 1 1 calc R . . C17' C 1.1995(7) 0.8283(6) 0.1380(5) 0.045(3) Uani 1 1 d . . . H17B H 1.2278 0.8566 0.1648 0.054 Uiso 1 1 calc R . . C18 C 0.9493(10) 0.7792(6) 0.5226(5) 0.059(3) Uani 1 1 d . . . C18' C 1.2483(7) 0.8012(6) 0.0881(5) 0.047(3) Uani 1 1 d . . . C19' C 1.2016(8) 0.7606(6) 0.0485(4) 0.047(3) Uani 1 1 d . . . H19A H 1.2351 0.7419 0.0135 0.056 Uiso 1 1 calc R . . C19 C 0.8494(9) 0.7839(6) 0.5210(5) 0.059(3) Uani 1 1 d . . . H19B H 0.8121 0.8071 0.5533 0.071 Uiso 1 1 calc R . . C20' C 1.1089(7) 0.7461(5) 0.0575(4) 0.041(2) Uani 1 1 d . . . C20 C 0.8029(8) 0.7571(6) 0.4759(4) 0.051(3) Uani 1 1 d . . . C21 C 0.8602(8) 0.7230(6) 0.4258(4) 0.043(3) Uani 1 1 d . . . C21' C 1.0612(7) 0.7720(5) 0.1118(4) 0.038(2) Uani 1 1 d . . . C22' C 0.6984(6) 0.8892(5) 0.1525(4) 0.034(2) Uani 1 1 d . . . H22A H 0.6695 0.8571 0.1824 0.041 Uiso 1 1 calc R . . C22 C 0.8314(6) 0.4945(5) 0.2644(4) 0.036(2) Uani 1 1 d . . . H22B H 0.8251 0.5224 0.2263 0.043 Uiso 1 1 calc R . . C23' C 0.7014(7) 0.8421(5) 0.0953(4) 0.036(2) Uani 1 1 d . . . C23 C 0.7310(6) 0.5084(6) 0.2929(4) 0.036(2) Uani 1 1 d . . . C24 C 0.6813(6) 0.5873(5) 0.2939(4) 0.033(2) Uani 1 1 d . . . C24' C 0.7332(6) 0.7589(6) 0.1001(4) 0.033(2) Uani 1 1 d . . . C25' C 0.7176(6) 0.7058(5) 0.0558(4) 0.035(2) Uani 1 1 d . . . C25 C 0.5805(7) 0.6030(6) 0.3058(4) 0.044(3) Uani 1 1 d . . . C26' C 0.6853(6) 0.7424(5) 0.0028(4) 0.036(2) Uani 1 1 d . . . H26A H 0.6762 0.7093 -0.0281 0.043 Uiso 1 1 calc R . . C26 C 0.5405(7) 0.5373(6) 0.3263(5) 0.052(3) Uani 1 1 d . . . H26B H 0.4755 0.5462 0.3366 0.062 Uiso 1 1 calc R . . C27' C 0.6660(6) 0.8248(5) -0.0063(4) 0.035(2) Uani 1 1 d . . . C27 C 0.5901(8) 0.4612(6) 0.3323(5) 0.053(3) Uani 1 1 d . . . C28 C 0.6866(7) 0.4463(6) 0.3138(4) 0.045(3) Uani 1 1 d . . . H28A H 0.7213 0.3944 0.3156 0.054 Uiso 1 1 calc R . . C28' C 0.6683(6) 0.8741(6) 0.0424(4) 0.038(2) Uani 1 1 d . . . H28B H 0.6474 0.9292 0.0391 0.045 Uiso 1 1 calc R . . C29 C 0.8711(7) 0.4084(5) 0.2487(4) 0.041(2) Uani 1 1 d . . . H29A H 0.8215 0.3863 0.2304 0.050 Uiso 1 1 calc R . . H29B H 0.8843 0.3789 0.2852 0.050 Uiso 1 1 calc R . . C29' C 0.6317(7) 0.9695(5) 0.1529(4) 0.044(3) Uani 1 1 d . . . H29C H 0.6608 1.0059 0.1274 0.053 Uiso 1 1 calc R . . H29D H 0.5733 0.9620 0.1354 0.053 Uiso 1 1 calc R . . C30 C 0.9597(7) 0.3918(6) 0.2082(4) 0.037(2) Uani 1 1 d . . . C30' C 0.6050(7) 1.0099(6) 0.2116(4) 0.044(3) Uani 1 1 d . . . C31' C 0.5680(8) 1.0905(7) 0.2131(5) 0.065(3) Uani 1 1 d . . . H31A H 0.5636 1.1194 0.1778 0.078 Uiso 1 1 calc R . . C31 C 1.0141(8) 0.3148(6) 0.2049(5) 0.053(3) Uani 1 1 d . . . H31B H 0.9966 0.2746 0.2293 0.064 Uiso 1 1 calc R . . C32 C 1.0926(8) 0.2967(7) 0.1666(5) 0.059(3) Uani 1 1 d . . . H32A H 1.1271 0.2447 0.1652 0.071 Uiso 1 1 calc R . . C32' C 0.5371(10) 1.1302(8) 0.2660(6) 0.083(4) Uani 1 1 d . . . H32B H 0.5113 1.1846 0.2654 0.099 Uiso 1 1 calc R . . C33 C 1.1206(8) 0.3545(6) 0.1303(5) 0.055(3) Uani 1 1 d . . . H33A H 1.1731 0.3418 0.1038 0.066 Uiso 1 1 calc R . . C33' C 0.5444(10) 1.0893(8) 0.3197(6) 0.077(4) Uani 1 1 d . . . H33B H 0.5243 1.1159 0.3551 0.092 Uiso 1 1 calc R . . C34 C 1.0706(7) 0.4312(7) 0.1337(5) 0.055(3) Uani 1 1 d . . . H34A H 1.0903 0.4710 0.1098 0.066 Uiso 1 1 calc R . . C34' C 0.5819(10) 1.0086(8) 0.3193(5) 0.075(4) Uani 1 1 d . . . H34B H 0.5877 0.9801 0.3546 0.090 Uiso 1 1 calc R . . C35 C 0.9912(7) 0.4504(6) 0.1719(4) 0.043(3) Uani 1 1 d . . . H35A H 0.9582 0.5030 0.1735 0.052 Uiso 1 1 calc R . . C35' C 0.6115(8) 0.9691(7) 0.2651(5) 0.057(3) Uani 1 1 d . . . H35B H 0.6360 0.9144 0.2654 0.068 Uiso 1 1 calc R . . C37 C 0.9911(12) 0.8124(8) 0.5765(5) 0.080(4) Uani 1 1 d . . . C37' C 1.3513(8) 0.8100(7) 0.0718(6) 0.065(3) Uani 1 1 d . . . C38' C 1.4148(9) 0.7289(8) 0.0631(7) 0.099(5) Uani 1 1 d . . . H38A H 1.4220 0.7018 0.1005 0.149 Uiso 1 1 calc R . . H38B H 1.4762 0.7362 0.0467 0.149 Uiso 1 1 calc R . . H38C H 1.3865 0.6974 0.0365 0.149 Uiso 1 1 calc R . . C38 C 0.9547(12) 0.7738(9) 0.6340(5) 0.108(6) Uani 1 1 d . . . H13A H 0.9756 0.7167 0.6327 0.163 Uiso 1 1 calc R . . H13B H 0.8863 0.7856 0.6372 0.163 Uiso 1 1 calc R . . H13C H 0.9796 0.7953 0.6676 0.163 Uiso 1 1 calc R . . C39' C 1.3557(10) 0.8582(9) 0.0141(6) 0.098(5) Uani 1 1 d . . . H39A H 1.3219 0.9120 0.0202 0.148 Uiso 1 1 calc R . . H39B H 1.3268 0.8332 -0.0163 0.148 Uiso 1 1 calc R . . H39C H 1.4210 0.8595 0.0022 0.148 Uiso 1 1 calc R . . C39 C 0.9558(12) 0.9055(8) 0.5785(7) 0.112(6) Uani 1 1 d . . . H39D H 0.9750 0.9291 0.5420 0.168 Uiso 1 1 calc R . . H39E H 0.9831 0.9278 0.6108 0.168 Uiso 1 1 calc R . . H39F H 0.8875 0.9166 0.5838 0.168 Uiso 1 1 calc R . . C40' C 1.3919(9) 0.8547(8) 0.1202(6) 0.087(4) Uani 1 1 d . . . H40A H 1.3917 0.8247 0.1565 0.130 Uiso 1 1 calc R . . H40B H 1.3533 0.9068 0.1259 0.130 Uiso 1 1 calc R . . H40C H 1.4560 0.8604 0.1085 0.130 Uiso 1 1 calc R . . C40 C 1.0993(12) 0.7936(9) 0.5721(7) 0.114(6) Uani 1 1 d . . . H13D H 1.1225 0.8196 0.5377 0.170 Uiso 1 1 calc R . . H13E H 1.1201 0.7366 0.5689 0.170 Uiso 1 1 calc R . . H13F H 1.1236 0.8128 0.6068 0.170 Uiso 1 1 calc R . . C41 C 0.6936(8) 0.7682(7) 0.4766(5) 0.061(3) Uani 1 1 d . . . C41' C 1.0643(7) 0.6996(6) 0.0127(4) 0.048(3) Uani 1 1 d . . . C42' C 1.1217(9) 0.6898(8) -0.0475(5) 0.073(4) Uani 1 1 d . . . H42A H 1.1313 0.7416 -0.0619 0.110 Uiso 1 1 calc R . . H42B H 1.0870 0.6658 -0.0753 0.110 Uiso 1 1 calc R . . H42C H 1.1824 0.6561 -0.0426 0.110 Uiso 1 1 calc R . . C42 C 0.6617(8) 0.6875(7) 0.4636(5) 0.066(3) Uani 1 1 d . . . H46M H 0.6856 0.6483 0.4927 0.099 Uiso 1 1 calc R . . H46K H 0.6865 0.6690 0.4250 0.099 Uiso 1 1 calc R . . H46L H 0.5934 0.6951 0.4652 0.099 Uiso 1 1 calc R . . C43' C 1.0648(8) 0.6152(6) 0.0378(5) 0.060(3) Uani 1 1 d . . . H43A H 1.0280 0.6186 0.0748 0.090 Uiso 1 1 calc R . . H43B H 1.1292 0.5897 0.0440 0.090 Uiso 1 1 calc R . . H43C H 1.0374 0.5841 0.0104 0.090 Uiso 1 1 calc R . . C43 C 0.6463(10) 0.7983(9) 0.5361(5) 0.092(5) Uani 1 1 d . . . H43D H 0.6732 0.7636 0.5671 0.139 Uiso 1 1 calc R . . H43E H 0.5790 0.7983 0.5361 0.139 Uiso 1 1 calc R . . H43F H 0.6569 0.8519 0.5427 0.139 Uiso 1 1 calc R . . C44' C 0.9652(8) 0.7409(6) -0.0017(4) 0.054(3) Uani 1 1 d . . . H44A H 0.9675 0.7945 -0.0156 0.080 Uiso 1 1 calc R . . H44B H 0.9234 0.7432 0.0332 0.080 Uiso 1 1 calc R . . H44C H 0.9419 0.7114 -0.0319 0.080 Uiso 1 1 calc R . . C44 C 0.6574(9) 0.8315(7) 0.4293(5) 0.075(4) Uani 1 1 d . . . H44D H 0.6787 0.8809 0.4371 0.112 Uiso 1 1 calc R . . H44E H 0.5890 0.8406 0.4305 0.112 Uiso 1 1 calc R . . H44F H 0.6821 0.8123 0.3908 0.112 Uiso 1 1 calc R . . C45 C 0.5173(7) 0.6826(7) 0.2940(5) 0.056(3) Uani 1 1 d . . . C45' C 0.7306(7) 0.6162(5) 0.0653(4) 0.042(3) Uani 1 1 d . . . C46' C 0.6764(9) 0.5984(6) 0.1237(5) 0.064(3) Uani 1 1 d . . . H46D H 0.6092 0.6166 0.1204 0.096 Uiso 1 1 calc R . . H46E H 0.6981 0.6259 0.1557 0.096 Uiso 1 1 calc R . . H46F H 0.6882 0.5416 0.1314 0.096 Uiso 1 1 calc R . . C46 C 0.5575(12) 0.7398(12) 0.2587(15) 0.27(2) Uani 1 1 d . . . H46A H 0.5516 0.7294 0.2176 0.399 Uiso 1 1 calc R . . H46B H 0.6237 0.7357 0.2664 0.399 Uiso 1 1 calc R . . H46C H 0.5244 0.7929 0.2683 0.399 Uiso 1 1 calc R . . C47' C 0.8379(8) 0.5791(6) 0.0684(5) 0.063(3) Uani 1 1 d . . . H47D H 0.8706 0.5861 0.0311 0.094 Uiso 1 1 calc R . . H47E H 0.8442 0.5228 0.0774 0.094 Uiso 1 1 calc R . . H47F H 0.8651 0.6053 0.0988 0.094 Uiso 1 1 calc R . . C47 C 0.479(3) 0.7220(16) 0.3494(9) 0.34(3) Uani 1 1 d . . . H47G H 0.4669 0.6822 0.3780 0.504 Uiso 1 1 calc R . . H47H H 0.4211 0.7583 0.3426 0.504 Uiso 1 1 calc R . . H47I H 0.5250 0.7513 0.3639 0.504 Uiso 1 1 calc R . . C48' C 0.6924(8) 0.5733(6) 0.0151(5) 0.052(3) Uani 1 1 d . . . H48A H 0.7237 0.5849 -0.0218 0.079 Uiso 1 1 calc R . . H48B H 0.6249 0.5917 0.0135 0.079 Uiso 1 1 calc R . . H48C H 0.7045 0.5164 0.0221 0.079 Uiso 1 1 calc R . . C48 C 0.4308(13) 0.6738(11) 0.2662(13) 0.222(15) Uani 1 1 d . . . H48G H 0.3994 0.6366 0.2887 0.333 Uiso 1 1 calc R . . H48H H 0.4464 0.6539 0.2267 0.333 Uiso 1 1 calc R . . H48I H 0.3893 0.7250 0.2649 0.333 Uiso 1 1 calc R . . C49' C 0.6524(7) 0.8617(6) -0.0695(4) 0.039(2) Uani 1 1 d . . . C49 C 0.5383(9) 0.3959(7) 0.3609(7) 0.079(4) Uani 1 1 d . . . C50' C 0.7456(7) 0.8902(7) -0.0888(4) 0.056(3) Uani 1 1 d . . . H50A H 0.7415 0.9109 -0.1284 0.084 Uiso 1 1 calc R . . H50B H 0.7977 0.8458 -0.0875 0.084 Uiso 1 1 calc R . . H50C H 0.7558 0.9316 -0.0626 0.084 Uiso 1 1 calc R . . C50 C 0.4970(15) 0.4219(10) 0.4224(8) 0.164(10) Uani 1 1 d . . . H53A H 0.4710 0.4782 0.4220 0.245 Uiso 1 1 calc R . . H53B H 0.5463 0.4115 0.4501 0.245 Uiso 1 1 calc R . . H53C H 0.4474 0.3922 0.4339 0.245 Uiso 1 1 calc R . . C51' C 0.5708(7) 0.9342(6) -0.0686(4) 0.043(3) Uani 1 1 d . . . H51A H 0.5679 0.9590 -0.1070 0.065 Uiso 1 1 calc R . . H51B H 0.5818 0.9723 -0.0399 0.065 Uiso 1 1 calc R . . H51C H 0.5115 0.9167 -0.0584 0.065 Uiso 1 1 calc R . . C51 C 0.4564(12) 0.3834(11) 0.3210(10) 0.153(8) Uani 1 1 d . . . H15C H 0.4103 0.4321 0.3197 0.229 Uiso 1 1 calc R . . H15D H 0.4262 0.3408 0.3370 0.229 Uiso 1 1 calc R . . H15E H 0.4824 0.3695 0.2817 0.229 Uiso 1 1 calc R . . C52' C 0.6327(9) 0.8020(6) -0.1144(4) 0.063(3) Uani 1 1 d . . . H52A H 0.6177 0.8292 -0.1510 0.094 Uiso 1 1 calc R . . H52B H 0.5799 0.7779 -0.0999 0.094 Uiso 1 1 calc R . . H52C H 0.6882 0.7611 -0.1207 0.094 Uiso 1 1 calc R . . C52 C 0.6032(11) 0.3135(9) 0.3604(7) 0.113(6) Uani 1 1 d . . . H55A H 0.6576 0.3157 0.3831 0.169 Uiso 1 1 calc R . . H55B H 0.6242 0.2987 0.3204 0.169 Uiso 1 1 calc R . . H55C H 0.5686 0.2742 0.3775 0.169 Uiso 1 1 calc R . . C201 C 0.6918(15) 1.2816(16) 0.1712(8) 0.188(11) Uani 1 1 d . . . H20A H 0.7266 1.2350 0.1511 0.283 Uiso 1 1 calc R . . H20B H 0.6835 1.2698 0.2125 0.283 Uiso 1 1 calc R . . H20C H 0.7265 1.3252 0.1663 0.283 Uiso 1 1 calc R . . C202 C 0.5965(17) 1.3049(15) 0.1457(9) 0.159(8) Uani 1 1 d . . . H20D H 0.5991 1.2779 0.1080 0.191 Uiso 1 1 calc R . . H20E H 0.5505 1.2835 0.1716 0.191 Uiso 1 1 calc R . . C203 C 0.560(2) 1.3868(15) 0.1363(14) 0.214(15) Uani 1 1 d . . . H20K H 0.5759 1.4139 0.1709 0.257 Uiso 1 1 calc R . . H20L H 0.5996 1.4028 0.1037 0.257 Uiso 1 1 calc R . . C204 C 0.471(2) 1.4222(16) 0.1256(16) 0.249(19) Uani 1 1 d . . . H20F H 0.4321 1.4111 0.1600 0.299 Uiso 1 1 calc R . . H20G H 0.4527 1.3922 0.0933 0.299 Uiso 1 1 calc R . . C205 C 0.4409(16) 1.5006(13) 0.1124(10) 0.164(8) Uani 1 1 d . . . H20H H 0.3757 1.5082 0.1016 0.246 Uiso 1 1 calc R . . H20I H 0.4799 1.5163 0.0799 0.246 Uiso 1 1 calc R . . H20J H 0.4454 1.5329 0.1463 0.246 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 0.0364(10) 0.0333(10) 0.0291(10) 0.0080(8) -0.0079(8) -0.0117(8) Ti2 0.0369(10) 0.0310(10) 0.0302(10) 0.0090(8) -0.0097(8) -0.0117(8) O1 0.045(4) 0.048(4) 0.027(4) 0.008(3) -0.009(3) -0.019(3) O2 0.032(4) 0.035(4) 0.043(4) 0.010(3) -0.005(3) -0.010(3) O3 0.036(4) 0.043(4) 0.031(4) 0.005(3) -0.003(3) -0.017(3) O4 0.044(4) 0.033(4) 0.034(4) 0.012(3) -0.015(3) -0.011(3) O5 0.045(4) 0.026(3) 0.032(4) 0.001(3) -0.005(3) -0.008(3) O6 0.041(4) 0.027(3) 0.026(3) 0.005(3) -0.009(3) -0.006(3) N1 0.035(4) 0.027(4) 0.036(4) 0.006(3) -0.012(4) -0.010(3) N2 0.039(5) 0.034(5) 0.033(5) 0.018(4) -0.012(4) -0.017(4) N3 0.038(5) 0.032(5) 0.033(5) 0.009(4) -0.011(4) -0.010(4) N4 0.035(5) 0.029(4) 0.040(5) 0.007(4) -0.014(4) -0.010(4) C1' 0.093(10) 0.044(7) 0.089(10) -0.019(7) -0.028(8) -0.006(7) C1 0.062(8) 0.071(8) 0.073(8) 0.023(7) -0.034(7) 0.007(6) C2' 0.060(7) 0.043(7) 0.060(8) -0.008(6) -0.011(6) -0.019(6) C2 0.052(7) 0.044(6) 0.040(6) 0.010(5) -0.020(5) -0.002(5) C3 0.075(9) 0.049(7) 0.055(8) 0.015(6) -0.033(7) -0.009(6) C3' 0.072(8) 0.057(8) 0.061(8) -0.030(7) 0.007(6) -0.031(7) C4 0.090(10) 0.047(7) 0.036(6) 0.021(5) -0.002(6) -0.017(6) C4' 0.080(9) 0.055(8) 0.045(7) 0.000(6) -0.004(6) -0.029(7) C5' 0.069(8) 0.044(6) 0.038(7) -0.008(5) -0.009(6) -0.026(6) C5 0.054(7) 0.040(6) 0.042(6) 0.010(5) -0.010(5) -0.012(5) C6' 0.039(6) 0.032(6) 0.040(6) -0.007(5) -0.010(5) -0.015(5) C6 0.045(6) 0.034(6) 0.030(6) 0.012(4) -0.002(5) -0.006(5) C7' 0.039(6) 0.037(6) 0.040(6) 0.000(5) -0.009(5) -0.016(5) C7 0.056(7) 0.027(5) 0.038(6) 0.003(4) -0.011(5) -0.006(5) C8' 0.047(6) 0.025(5) 0.062(7) -0.004(5) -0.019(5) -0.006(5) C8 0.024(5) 0.050(7) 0.048(6) 0.015(5) -0.017(5) -0.007(5) C9 0.033(6) 0.054(7) 0.036(6) 0.008(5) -0.011(5) -0.006(5) C9' 0.043(6) 0.030(5) 0.046(6) 0.017(5) -0.005(5) -0.007(5) C10' 0.058(7) 0.045(6) 0.042(7) 0.018(5) -0.008(5) -0.020(5) C10 0.035(6) 0.057(7) 0.057(7) 0.020(6) -0.011(6) -0.015(6) C11 0.039(7) 0.082(9) 0.061(8) 0.026(7) 0.007(6) -0.019(6) C11' 0.073(9) 0.076(9) 0.053(7) 0.030(7) -0.013(7) -0.028(7) C12' 0.077(9) 0.056(8) 0.082(10) 0.034(7) -0.002(7) -0.036(7) C12 0.046(7) 0.069(9) 0.062(8) 0.006(7) -0.005(6) -0.005(6) C13 0.033(6) 0.055(7) 0.051(7) 0.001(6) -0.012(5) 0.000(5) C13' 0.061(8) 0.038(6) 0.084(9) 0.018(6) -0.014(7) -0.021(6) C14 0.058(7) 0.062(8) 0.059(7) -0.005(6) -0.014(6) 0.000(6) C14' 0.077(9) 0.049(7) 0.106(10) 0.004(7) -0.010(8) -0.032(7) C15 0.043(6) 0.046(6) 0.036(6) 0.015(5) -0.019(5) -0.023(5) C15' 0.046(7) 0.036(6) 0.046(6) 0.010(5) -0.019(5) -0.021(5) C16 0.060(7) 0.041(6) 0.030(6) 0.013(5) -0.022(5) -0.022(5) C16' 0.049(7) 0.038(6) 0.042(6) 0.002(5) 0.000(5) -0.010(5) C17 0.074(8) 0.048(7) 0.043(7) 0.010(6) -0.013(6) -0.027(6) C17' 0.036(6) 0.042(6) 0.060(7) 0.008(5) -0.006(5) -0.018(5) C18 0.092(10) 0.042(7) 0.050(8) 0.014(6) -0.028(7) -0.029(7) C18' 0.042(6) 0.044(6) 0.056(7) 0.005(6) -0.004(6) -0.012(5) C19' 0.065(8) 0.034(6) 0.036(6) 0.005(5) 0.012(5) 0.001(5) C19 0.096(10) 0.049(7) 0.037(7) 0.010(5) -0.015(6) -0.023(7) C20' 0.044(6) 0.037(6) 0.041(6) 0.008(5) 0.001(5) -0.010(5) C20 0.077(8) 0.054(7) 0.028(6) 0.006(5) -0.013(6) -0.023(6) C21 0.058(7) 0.037(6) 0.038(6) 0.016(5) -0.012(6) -0.019(5) C21' 0.044(6) 0.027(5) 0.041(6) 0.013(5) -0.008(5) -0.006(5) C22' 0.028(5) 0.031(5) 0.042(6) 0.005(4) -0.004(4) -0.003(4) C22 0.040(6) 0.027(5) 0.040(6) 0.003(4) 0.001(5) -0.007(4) C23' 0.042(6) 0.033(6) 0.033(6) 0.003(5) -0.006(5) -0.003(5) C23 0.037(6) 0.041(6) 0.033(6) 0.000(5) 0.003(4) -0.015(5) C24 0.028(6) 0.039(6) 0.031(5) -0.001(4) 0.001(4) -0.008(5) C24' 0.035(5) 0.048(6) 0.020(5) 0.005(5) -0.006(4) -0.013(5) C25' 0.030(5) 0.037(6) 0.040(6) 0.010(5) -0.014(4) -0.011(4) C25 0.042(6) 0.039(6) 0.053(7) 0.004(5) -0.009(5) -0.013(5) C26' 0.048(6) 0.023(5) 0.039(6) -0.002(4) -0.015(5) -0.011(4) C26 0.030(6) 0.048(7) 0.078(8) -0.009(6) 0.014(5) -0.014(5) C27' 0.032(5) 0.043(6) 0.036(6) 0.004(5) -0.004(4) -0.018(5) C27 0.048(7) 0.044(7) 0.071(8) 0.004(6) 0.008(6) -0.021(6) C28 0.042(7) 0.040(6) 0.053(7) 0.003(5) -0.009(5) -0.004(5) C28' 0.038(6) 0.037(6) 0.038(6) 0.015(5) -0.014(5) -0.003(5) C29 0.048(6) 0.039(6) 0.038(6) 0.003(5) -0.004(5) -0.010(5) C29' 0.040(6) 0.038(6) 0.053(7) 0.000(5) -0.016(5) -0.001(5) C30 0.044(6) 0.038(6) 0.031(6) 0.001(5) -0.008(5) -0.008(5) C30' 0.046(6) 0.045(7) 0.039(6) -0.009(5) -0.006(5) 0.004(5) C31' 0.082(9) 0.047(8) 0.061(8) -0.018(6) -0.011(7) 0.007(6) C31 0.074(8) 0.038(7) 0.051(7) 0.001(5) 0.006(6) -0.019(6) C32 0.073(8) 0.051(7) 0.047(7) -0.009(6) 0.010(6) 0.004(6) C32' 0.110(11) 0.048(8) 0.089(11) -0.016(8) -0.021(9) -0.002(7) C33 0.053(7) 0.050(7) 0.056(7) 0.002(6) 0.023(6) 0.000(6) C33' 0.104(11) 0.063(9) 0.059(9) -0.021(7) -0.010(8) -0.002(8) C34 0.045(7) 0.053(8) 0.063(8) 0.019(6) 0.008(6) -0.004(6) C34' 0.104(11) 0.074(10) 0.042(8) 0.002(7) -0.004(7) -0.004(8) C35 0.041(6) 0.036(6) 0.050(6) 0.007(5) -0.002(5) 0.002(5) C35' 0.059(8) 0.050(7) 0.060(8) -0.010(6) 0.001(6) -0.007(6) C37 0.128(13) 0.071(9) 0.054(8) 0.003(7) -0.041(8) -0.046(9) C37' 0.043(7) 0.062(8) 0.092(10) 0.007(7) 0.015(7) -0.020(6) C38' 0.053(9) 0.090(11) 0.152(15) 0.008(10) -0.002(9) -0.007(8) C38 0.166(16) 0.131(13) 0.043(8) -0.003(8) -0.039(9) -0.059(12) C39' 0.099(11) 0.113(12) 0.097(11) 0.011(9) 0.034(9) -0.068(10) C39 0.164(16) 0.072(10) 0.109(12) -0.026(9) -0.034(11) -0.034(10) C40' 0.052(8) 0.095(10) 0.119(12) 0.018(9) 0.011(8) -0.034(8) C40 0.147(16) 0.107(12) 0.104(12) -0.015(9) -0.081(11) -0.044(11) C41 0.069(8) 0.071(8) 0.041(7) 0.003(6) 0.008(6) -0.006(7) C41' 0.052(7) 0.054(7) 0.039(6) 0.004(5) 0.005(5) -0.017(6) C42' 0.074(9) 0.085(9) 0.061(8) -0.015(7) 0.017(7) -0.022(7) C42 0.059(8) 0.087(9) 0.054(7) 0.021(7) -0.010(6) -0.017(7) C43' 0.072(8) 0.041(7) 0.069(8) -0.005(6) 0.008(6) -0.016(6) C43 0.096(11) 0.119(12) 0.056(8) -0.025(8) 0.015(8) -0.007(9) C44' 0.070(8) 0.061(7) 0.032(6) 0.005(5) -0.001(5) -0.019(6) C44 0.075(9) 0.060(8) 0.084(9) 0.010(7) -0.001(7) 0.001(7) C45 0.033(6) 0.066(8) 0.071(8) -0.004(6) -0.019(6) -0.009(6) C45' 0.061(7) 0.026(5) 0.044(6) 0.006(5) -0.011(5) -0.016(5) C46' 0.089(9) 0.054(7) 0.060(8) 0.017(6) -0.023(7) -0.037(7) C46 0.058(11) 0.136(17) 0.58(6) 0.23(3) 0.003(19) 0.019(11) C47' 0.060(8) 0.041(7) 0.088(9) -0.002(6) -0.021(7) -0.004(6) C47 0.54(5) 0.23(3) 0.112(17) -0.100(19) -0.13(3) 0.31(4) C48' 0.066(7) 0.034(6) 0.061(7) 0.000(5) -0.020(6) -0.013(5) C48 0.117(15) 0.129(16) 0.45(4) 0.15(2) -0.16(2) -0.078(13) C49' 0.042(6) 0.041(6) 0.032(6) 0.003(5) -0.007(5) -0.004(5) C49 0.059(8) 0.057(8) 0.118(12) 0.016(8) 0.027(8) -0.015(7) C50' 0.054(7) 0.070(8) 0.043(7) 0.010(6) -0.003(5) -0.008(6) C50 0.25(2) 0.088(12) 0.156(18) 0.000(12) 0.129(17) -0.071(14) C51' 0.049(6) 0.046(6) 0.036(6) 0.016(5) -0.010(5) -0.011(5) C51 0.100(14) 0.132(16) 0.25(2) 0.037(15) -0.010(15) -0.077(12) C52' 0.097(9) 0.051(7) 0.041(7) -0.002(5) -0.026(6) -0.004(7) C52 0.107(12) 0.089(11) 0.150(15) 0.031(10) 0.034(11) -0.056(10) C201 0.143(19) 0.34(4) 0.113(16) 0.058(19) -0.012(14) -0.14(2) C202 0.18(2) 0.17(2) 0.141(18) 0.023(16) -0.053(16) -0.059(18) C203 0.27(4) 0.088(17) 0.27(3) 0.03(2) 0.09(3) -0.05(2) C204 0.24(4) 0.13(2) 0.32(4) 0.09(2) 0.03(3) 0.08(2) C205 0.17(2) 0.143(19) 0.19(2) 0.006(17) 0.012(17) -0.050(17) _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 O5 1.795(6) . y Ti1 O2 1.869(6) . y Ti1 O6 1.925(6) . y Ti1 O1 1.926(6) . y Ti1 N2 2.302(7) . y Ti1 N1 2.393(7) . y Ti1 Ti2 2.779(2) . y Ti2 O6 1.778(5) . y Ti2 O4 1.885(6) . y Ti2 O3 1.922(6) . y Ti2 O5 1.923(6) . y Ti2 N3 2.265(7) . y Ti2 N4 2.455(7) . y O1 C21 1.329(11) . y O2 C24 1.346(10) . y O3 C21' 1.342(11) . y O4 C24' 1.362(10) . y N1 C6 1.443(11) . y N1 C22 1.514(11) . y N2 C15 1.277(11) . y N2 C9 1.437(12) . y N3 C15' 1.316(11) . y N3 C6' 1.427(11) . y N4 C9' 1.451(11) . y N4 C22' 1.503(11) . y C1' C2' 1.505(15) . ? C1 C2 1.483(14) . ? C2' C7' 1.398(13) . ? C2' C3' 1.400(15) . ? C2 C3 1.384(14) . ? C2 C7 1.416(13) . ? C3 C4 1.359(15) . ? C3' C4' 1.370(15) . ? C4 C5 1.400(13) . ? C4' C5' 1.351(14) . ? C5' C6' 1.393(13) . ? C5 C6 1.387(13) . ? C6' C7' 1.389(12) . ? C6 C7 1.384(13) . ? C7' C8' 1.507(13) . ? C7 C8 1.515(13) . ? C8' C9' 1.395(13) . ? C8' C13' 1.406(14) . ? C8 C13 1.407(13) . ? C8 C9 1.414(13) . ? C9 C10 1.393(13) . ? C9' C10' 1.398(13) . ? C10' C11' 1.360(14) . ? C10 C11 1.361(14) . ? C11 C12 1.380(15) . ? C11' C12' 1.383(15) . ? C12' C13' 1.394(15) . ? C12 C13 1.384(14) . ? C13 C14 1.513(14) . ? C13' C14' 1.502(15) . ? C15 C16 1.422(13) . ? C15' C16' 1.442(13) . ? C16 C21 1.398(14) . ? C16 C17 1.424(13) . ? C16' C17' 1.393(13) . ? C16' C21' 1.405(13) . ? C17 C18 1.379(15) . ? C17' C18' 1.337(13) . ? C18 C19 1.415(16) . ? C18 C37 1.543(15) . ? C18' C19' 1.403(14) . ? C18' C37' 1.527(14) . ? C19' C20' 1.391(13) . ? C19 C20 1.373(14) . ? C20' C21' 1.408(13) . ? C20' C41' 1.524(14) . ? C20 C21 1.426(14) . ? C20 C41 1.536(15) . ? C22' C29' 1.514(12) . ? C22' C23' 1.525(12) . ? C22 C29 1.506(12) . ? C22 C23 1.518(12) . ? C23' C28' 1.381(12) . ? C23' C24' 1.405(12) . ? C23 C28 1.386(13) . ? C23 C24 1.396(12) . ? C24 C25 1.427(13) . ? C24' C25' 1.408(12) . ? C25' C26' 1.406(12) . ? C25' C45' 1.509(12) . ? C25 C26 1.400(13) . ? C25 C45 1.512(14) . ? C26' C27' 1.387(12) . ? C26 C27 1.364(14) . ? C27' C28' 1.397(12) . ? C27' C49' 1.562(12) . ? C27 C28 1.396(14) . ? C27 C49 1.550(15) . ? C29 C30 1.506(13) . ? C29' C30' 1.502(13) . ? C30 C31 1.394(13) . ? C30 C35 1.400(13) . ? C30' C31' 1.373(14) . ? C30' C35' 1.384(14) . ? C31' C32' 1.392(16) . ? C31 C32 1.371(14) . ? C32 C33 1.368(14) . ? C32' C33' 1.391(17) . ? C33 C34 1.366(13) . ? C33' C34' 1.374(16) . ? C34 C35 1.382(13) . ? C34' C35' 1.412(15) . ? C37 C40 1.52(2) . ? C37 C38 1.554(18) . ? C37 C39 1.567(18) . ? C37' C38' 1.513(16) . ? C37' C40' 1.536(17) . ? C37' C39' 1.536(17) . ? C41 C43 1.526(15) . ? C41 C44 1.548(15) . ? C41 C42 1.550(16) . ? C41' C44' 1.513(14) . ? C41' C43' 1.530(13) . ? C41' C42' 1.546(14) . ? C45 C46 1.42(2) . ? C45 C48 1.447(18) . ? C45 C47 1.46(2) . ? C45' C48' 1.532(12) . ? C45' C46' 1.550(14) . ? C45' C47' 1.553(14) . ? C49' C52' 1.513(13) . ? C49' C50' 1.532(13) . ? C49' C51' 1.534(12) . ? C49 C50 1.521(19) . ? C49 C52 1.531(18) . ? C49 C51 1.56(2) . ? C201 C202 1.49(2) . ? C202 C203 1.41(3) . ? C203 C204 1.34(4) . ? C204 C205 1.36(3) . ? 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 O5 Ti1 O2 96.5(3) . . y O5 Ti1 O6 82.6(2) . . y O2 Ti1 O6 103.3(3) . . y O5 Ti1 O1 99.1(3) . . y O2 Ti1 O1 97.8(3) . . y O6 Ti1 O1 158.5(3) . . y O5 Ti1 N2 109.3(3) . . y O2 Ti1 N2 154.3(3) . . y O6 Ti1 N2 81.1(3) . . y O1 Ti1 N2 78.2(3) . . y O5 Ti1 N1 160.0(3) . . y O2 Ti1 N1 82.1(2) . . y O6 Ti1 N1 78.3(2) . . y O1 Ti1 N1 100.8(3) . . y N2 Ti1 N1 73.9(2) . . y O5 Ti1 Ti2 43.42(19) . . y O2 Ti1 Ti2 100.18(19) . . y O6 Ti1 Ti2 39.40(16) . . y O1 Ti1 Ti2 139.85(19) . . y N2 Ti1 Ti2 98.88(18) . . y N1 Ti1 Ti2 116.97(18) . . y O6 Ti2 O4 96.2(2) . . y O6 Ti2 O3 100.0(3) . . y O4 Ti2 O3 98.5(3) . . y O6 Ti2 O5 83.1(3) . . y O4 Ti2 O5 100.4(3) . . y O3 Ti2 O5 160.4(3) . . y O6 Ti2 N3 108.3(3) . . y O4 Ti2 N3 155.3(3) . . y O3 Ti2 N3 79.6(3) . . y O5 Ti2 N3 81.1(3) . . y O6 Ti2 N4 163.1(3) . . y O4 Ti2 N4 82.1(2) . . y O3 Ti2 N4 96.9(3) . . y O5 Ti2 N4 80.6(2) . . y N3 Ti2 N4 73.8(2) . . y O6 Ti2 Ti1 43.41(19) . . y O4 Ti2 Ti1 97.99(18) . . y O3 Ti2 Ti1 141.30(19) . . y O5 Ti2 Ti1 39.90(17) . . y N3 Ti2 Ti1 98.50(19) . . y N4 Ti2 Ti1 119.92(19) . . y C21 O1 Ti1 142.3(6) . . ? C24 O2 Ti1 140.6(5) . . ? C21' O3 Ti2 142.8(6) . . ? C24' O4 Ti2 136.5(5) . . ? Ti1 O5 Ti2 96.7(3) . . y Ti2 O6 Ti1 97.2(3) . . y C6 N1 C22 118.2(7) . . ? C6 N1 Ti1 120.3(5) . . ? C22 N1 Ti1 109.1(5) . . ? C15 N2 C9 114.7(8) . . ? C15 N2 Ti1 125.5(7) . . ? C9 N2 Ti1 119.5(5) . . ? C15' N3 C6' 114.6(7) . . ? C15' N3 Ti2 125.0(6) . . ? C6' N3 Ti2 119.3(6) . . ? C9' N4 C22' 118.7(7) . . ? C9' N4 Ti2 118.1(5) . . ? C22' N4 Ti2 108.3(5) . . ? C7' C2' C3' 117.6(10) . . ? C7' C2' C1' 122.3(10) . . ? C3' C2' C1' 120.1(10) . . ? C3 C2 C7 118.2(10) . . ? C3 C2 C1 118.8(9) . . ? C7 C2 C1 123.0(10) . . ? C4 C3 C2 120.3(10) . . ? C4' C3' C2' 122.1(10) . . ? C3 C4 C5 122.4(10) . . ? C5' C4' C3' 119.6(11) . . ? C4' C5' C6' 120.6(10) . . ? C6 C5 C4 118.0(10) . . ? C7' C6' C5' 120.1(9) . . ? C7' C6' N3 118.2(8) . . ? C5' C6' N3 121.7(8) . . ? C7 C6 C5 120.1(9) . . ? C7 C6 N1 118.4(8) . . ? C5 C6 N1 121.3(8) . . ? C6' C7' C2' 119.8(9) . . ? C6' C7' C8' 117.7(8) . . ? C2' C7' C8' 122.4(9) . . ? C6 C7 C2 120.8(9) . . ? C6 C7 C8 119.4(8) . . ? C2 C7 C8 119.7(9) . . ? C9' C8' C13' 119.0(10) . . ? C9' C8' C7' 119.7(8) . . ? C13' C8' C7' 121.1(9) . . ? C13 C8 C9 118.7(9) . . ? C13 C8 C7 122.9(9) . . ? C9 C8 C7 118.4(9) . . ? C10 C9 C8 120.4(10) . . ? C10 C9 N2 121.9(9) . . ? C8 C9 N2 117.7(8) . . ? C8' C9' C10' 121.1(9) . . ? C8' C9' N4 117.1(8) . . ? C10' C9' N4 121.7(8) . . ? C11' C10' C9' 119.1(10) . . ? C11 C10 C9 120.3(10) . . ? C10 C11 C12 119.6(10) . . ? C10' C11' C12' 121.0(10) . . ? C11' C12' C13' 121.0(10) . . ? C11 C12 C13 122.5(11) . . ? C12 C13 C8 118.4(10) . . ? C12 C13 C14 119.8(10) . . ? C8 C13 C14 121.7(10) . . ? C12' C13' C8' 118.7(10) . . ? C12' C13' C14' 119.6(10) . . ? C8' C13' C14' 121.7(11) . . ? N2 C15 C16 127.8(9) . . ? N3 C15' C16' 129.0(9) . . ? C21 C16 C15 122.2(8) . . ? C21 C16 C17 121.6(10) . . ? C15 C16 C17 116.2(10) . . ? C17' C16' C21' 121.6(10) . . ? C17' C16' C15' 118.4(9) . . ? C21' C16' C15' 119.7(9) . . ? C18 C17 C16 120.1(11) . . ? C18' C17' C16' 121.2(10) . . ? C17 C18 C19 116.6(10) . . ? C17 C18 C37 123.8(12) . . ? C19 C18 C37 119.6(12) . . ? C17' C18' C19' 117.2(9) . . ? C17' C18' C37' 124.8(10) . . ? C19' C18' C37' 118.0(10) . . ? C20' C19' C18' 124.9(9) . . ? C20 C19 C18 125.7(11) . . ? C19' C20' C21' 116.4(9) . . ? C19' C20' C41' 121.5(9) . . ? C21' C20' C41' 122.0(9) . . ? C19 C20 C21 117.0(11) . . ? C19 C20 C41 122.2(10) . . ? C21 C20 C41 120.7(9) . . ? O1 C21 C16 118.9(9) . . ? O1 C21 C20 122.1(9) . . ? C16 C21 C20 119.0(9) . . ? O3 C21' C16' 120.5(9) . . ? O3 C21' C20' 121.0(8) . . ? C16' C21' C20' 118.5(9) . . ? N4 C22' C29' 112.5(7) . . ? N4 C22' C23' 115.2(7) . . ? C29' C22' C23' 114.2(7) . . ? C29 C22 N1 112.8(7) . . ? C29 C22 C23 114.7(7) . . ? N1 C22 C23 114.2(7) . . ? C28' C23' C24' 119.4(8) . . ? C28' C23' C22' 125.0(8) . . ? C24' C23' C22' 115.4(7) . . ? C28 C23 C24 120.1(9) . . ? C28 C23 C22 122.8(9) . . ? C24 C23 C22 117.0(8) . . ? O2 C24 C23 117.3(8) . . ? O2 C24 C25 122.5(8) . . ? C23 C24 C25 120.1(8) . . ? O4 C24' C23' 117.8(8) . . ? O4 C24' C25' 120.9(8) . . ? C23' C24' C25' 121.3(8) . . ? C26' C25' C24' 115.3(8) . . ? C26' C25' C45' 122.2(8) . . ? C24' C25' C45' 122.5(8) . . ? C26 C25 C24 115.5(9) . . ? C26 C25 C45 120.3(9) . . ? C24 C25 C45 124.1(9) . . ? C27' C26' C25' 124.0(8) . . ? C27 C26 C25 124.6(9) . . ? C26' C27' C28' 117.5(8) . . ? C26' C27' C49' 121.6(8) . . ? C28' C27' C49' 120.6(8) . . ? C26 C27 C28 118.1(9) . . ? C26 C27 C49 118.9(10) . . ? C28 C27 C49 122.9(10) . . ? C23 C28 C27 120.4(9) . . ? C23' C28' C27' 120.8(9) . . ? C22 C29 C30 118.0(8) . . ? C30' C29' C22' 117.5(8) . . ? C31 C30 C35 116.6(9) . . ? C31 C30 C29 120.3(9) . . ? C35 C30 C29 123.1(9) . . ? C31' C30' C35' 117.4(10) . . ? C31' C30' C29' 119.2(9) . . ? C35' C30' C29' 123.3(9) . . ? C30' C31' C32' 121.7(11) . . ? C32 C31 C30 121.7(10) . . ? C33 C32 C31 120.7(10) . . ? C33' C32' C31' 120.8(12) . . ? C34 C33 C32 119.1(10) . . ? C34' C33' C32' 118.4(11) . . ? C33 C34 C35 121.0(10) . . ? C33' C34' C35' 120.0(11) . . ? C34 C35 C30 120.8(9) . . ? C30' C35' C34' 121.6(10) . . ? C40 C37 C18 111.0(12) . . ? C40 C37 C38 108.9(12) . . ? C18 C37 C38 109.4(10) . . ? C40 C37 C39 110.2(12) . . ? C18 C37 C39 108.1(10) . . ? C38 C37 C39 109.3(12) . . ? C38' C37' C18' 111.3(9) . . ? C38' C37' C40' 108.1(11) . . ? C18' C37' C40' 111.1(10) . . ? C38' C37' C39' 108.4(11) . . ? C18' C37' C39' 109.8(10) . . ? C40' C37' C39' 108.0(10) . . ? C43 C41 C20 112.4(10) . . ? C43 C41 C44 107.6(10) . . ? C20 C41 C44 108.8(9) . . ? C43 C41 C42 107.5(10) . . ? C20 C41 C42 110.5(9) . . ? C44 C41 C42 110.1(10) . . ? C44' C41' C20' 112.6(9) . . ? C44' C41' C43' 112.0(9) . . ? C20' C41' C43' 107.4(8) . . ? C44' C41' C42' 105.0(9) . . ? C20' C41' C42' 112.9(9) . . ? C43' C41' C42' 107.0(9) . . ? C46 C45 C48 105.5(15) . . ? C46 C45 C47 107.4(19) . . ? C48 C45 C47 102(2) . . ? C46 C45 C25 117.5(11) . . ? C48 C45 C25 112.8(11) . . ? C47 C45 C25 110.7(11) . . ? C25' C45' C48' 112.4(8) . . ? C25' C45' C46' 109.2(8) . . ? C48' C45' C46' 108.1(8) . . ? C25' C45' C47' 110.9(8) . . ? C48' C45' C47' 106.8(8) . . ? C46' C45' C47' 109.4(9) . . ? C52' C49' C50' 108.8(9) . . ? C52' C49' C51' 108.5(8) . . ? C50' C49' C51' 108.7(8) . . ? C52' C49' C27' 113.1(8) . . ? C50' C49' C27' 106.6(7) . . ? C51' C49' C27' 111.0(7) . . ? C50 C49 C52 113.0(13) . . ? C50 C49 C27 110.3(11) . . ? C52 C49 C27 111.6(10) . . ? C50 C49 C51 109.7(14) . . ? C52 C49 C51 103.3(13) . . ? C27 C49 C51 108.7(11) . . ? C203 C202 C201 119(2) . . ? C204 C203 C202 129(3) . . ? C203 C204 C205 127(3) . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 1.436 _refine_diff_density_min -0.638 _refine_diff_density_rms 0.151