# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Moshe Kol' 'Geoffrey Coates' 'Israel Goldberg' 'Jacob Kopilov' 'Ayellet L. Zelikoff' _publ_contact_author_name 'Moshe Kol' _publ_contact_author_email MOSHEKOL@POST.TAU.AC.IL _publ_section_title ; New facets of an old ligand: titanium and zirconium complexes of phenylenediamine bis(phenolate) in lactide polymerisation catalysis ; # Attachment 'mk196-7-200.txt' data_mk196 _database_code_depnum_ccdc_archive 'CCDC 742351' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H88 N2 O8 Ti2, C5 H12' _chemical_formula_sum 'C57 H100 N2 O8 Ti2' _chemical_formula_weight 1037.19 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 'P 21/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 17.9559(2) _cell_length_b 19.0596(3) _cell_length_c 18.6149(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.5379(12) _cell_angle_gamma 90.00 _cell_volume 5965.70(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 13316 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2256 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48922 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.86 _reflns_number_total 14077 _reflns_number_gt 9651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The pentane solvent is partly disordered, and its geometry was refined with restrained bond distances and bond angles. Some of the propoxy substituents are partly disordered as well. ; _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^)+(0.0957P)^2^+4.8938P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14077 _refine_ls_number_parameters 637 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1842 _refine_ls_wR_factor_gt 0.1596 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.023 _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 0.33071(3) 0.35762(2) 0.15015(2) 0.02482(12) Uani 1 1 d . . . Ti2 Ti 0.28576(3) 0.52001(2) 0.08928(3) 0.02650(13) Uani 1 1 d . . . O3 O 0.29114(10) 0.45249(10) 0.17359(9) 0.0267(4) Uani 1 1 d . . . C4 C 0.30261(16) 0.46769(15) 0.25390(14) 0.0304(6) Uani 1 1 d . . . H4 H 0.3243 0.4245 0.2845 0.036 Uiso 1 1 calc R . . C5 C 0.22259(17) 0.48330(17) 0.26055(16) 0.0376(7) Uani 1 1 d . . . H5A H 0.1998 0.5254 0.2307 0.056 Uiso 1 1 calc R . . H5B H 0.2294 0.4912 0.3145 0.056 Uiso 1 1 calc R . . H5C H 0.1868 0.4434 0.2408 0.056 Uiso 1 1 calc R . . C6 C 0.36270(17) 0.52597(16) 0.28447(16) 0.0373(6) Uani 1 1 d . . . H6A H 0.4117 0.5144 0.2751 0.056 Uiso 1 1 calc R . . H6B H 0.3745 0.5313 0.3397 0.056 Uiso 1 1 calc R . . H6C H 0.3408 0.5700 0.2584 0.056 Uiso 1 1 calc R . . O7 O 0.32381(10) 0.42601(10) 0.06083(9) 0.0269(4) Uani 1 1 d . . . C8 C 0.36792(15) 0.42469(15) 0.00886(14) 0.0301(6) Uani 1 1 d . . . H8 H 0.3655 0.4728 -0.0133 0.036 Uiso 1 1 calc R . . C9 C 0.32894(17) 0.37414(16) -0.05717(15) 0.0329(6) Uani 1 1 d . . . H9A H 0.3295 0.3266 -0.0369 0.049 Uiso 1 1 calc R . . H9B H 0.3584 0.3746 -0.0926 0.049 Uiso 1 1 calc R . . H9C H 0.2739 0.3887 -0.0844 0.049 Uiso 1 1 calc R . . C10 C 0.45435(16) 0.40722(18) 0.05102(17) 0.0403(7) Uani 1 1 d . . . H10A H 0.4753 0.4373 0.0964 0.060 Uiso 1 1 calc R . . H10B H 0.4847 0.4151 0.0171 0.060 Uiso 1 1 calc R . . H10C H 0.4591 0.3579 0.0669 0.060 Uiso 1 1 calc R . . O11 O 0.29497(12) 0.31029(10) 0.21456(11) 0.0351(4) Uani 1 1 d . . . C12 C 0.29448(16) 0.25946(15) 0.27012(15) 0.0317(6) Uani 1 1 d . . . H12 H 0.3491 0.2568 0.3096 0.038 Uiso 1 1 calc R . . C13 C 0.27366(18) 0.18835(15) 0.23206(16) 0.0371(6) Uani 1 1 d . . . H13A H 0.2214 0.1908 0.1912 0.056 Uiso 1 1 calc R . . H13B H 0.2722 0.1535 0.2702 0.056 Uiso 1 1 calc R . . H13C H 0.3139 0.1748 0.2102 0.056 Uiso 1 1 calc R . . C14 C 0.23720(17) 0.28275(17) 0.30955(16) 0.0369(6) Uani 1 1 d . . . H14A H 0.2545 0.3280 0.3348 0.055 Uiso 1 1 calc R . . H14B H 0.2366 0.2477 0.3479 0.055 Uiso 1 1 calc R . . H14C H 0.1836 0.2875 0.2713 0.055 Uiso 1 1 calc R . . O15 O 0.43303(11) 0.36705(10) 0.20753(10) 0.0318(4) Uani 1 1 d . . . C16 C 0.4920(3) 0.3307(3) 0.2712(2) 0.0378(17) Uani 1 1 d . . . H16 H 0.4661 0.2875 0.2819 0.045 Uiso 1 1 calc R . . C17 C 0.5575(2) 0.3080(2) 0.2472(2) 0.0668(11) Uani 1 1 d . . . H17A H 0.5364 0.2800 0.2003 0.100 Uiso 1 1 calc R . . H17B H 0.5948 0.2795 0.2879 0.100 Uiso 1 1 calc R . . H17C H 0.5851 0.3492 0.2375 0.100 Uiso 1 1 calc R . . C18 C 0.5133(3) 0.3756(3) 0.3403(2) 0.0809(15) Uani 1 1 d . . . H18A H 0.5399 0.4181 0.3321 0.121 Uiso 1 1 calc R . . H18B H 0.5492 0.3498 0.3845 0.121 Uiso 1 1 calc R . . H18C H 0.4650 0.3885 0.3503 0.121 Uiso 1 1 calc R . . O19 O 0.22901(11) 0.58710(10) 0.12021(11) 0.0344(4) Uani 1 1 d . . . C20 C 0.2113(2) 0.65877(16) 0.10327(18) 0.0413(7) Uani 1 1 d . . . H20 H 0.2474 0.6771 0.0771 0.050 Uiso 1 1 calc R . . C21 C 0.2270(3) 0.69919(19) 0.1760(2) 0.0622(10) Uani 1 1 d . . . H21A H 0.1929 0.6814 0.2031 0.093 Uiso 1 1 calc R . . H21B H 0.2155 0.7490 0.1639 0.093 Uiso 1 1 calc R . . H21C H 0.2829 0.6937 0.2087 0.093 Uiso 1 1 calc R . . C22 C 0.1273(3) 0.6673(2) 0.0500(3) 0.0742(13) Uani 1 1 d . . . H22A H 0.1206 0.6440 0.0011 0.111 Uiso 1 1 calc R . . H22B H 0.1150 0.7173 0.0409 0.111 Uiso 1 1 calc R . . H22C H 0.0912 0.6461 0.0729 0.111 Uiso 1 1 calc R . . O23 O 0.37860(11) 0.56287(10) 0.11546(11) 0.0345(4) Uani 1 1 d . . . C24 C 0.4354(2) 0.6164(2) 0.1439(2) 0.0606(10) Uani 1 1 d . . . H24 H 0.4249 0.6399 0.1875 0.073 Uiso 1 1 calc R . . C25 C 0.4251(3) 0.6704(2) 0.0811(3) 0.0668(11) Uani 1 1 d . . . H25A H 0.4269 0.6469 0.0349 0.100 Uiso 1 1 calc R . . H25B H 0.4681 0.7051 0.0985 0.100 Uiso 1 1 calc R . . H25C H 0.3738 0.6940 0.0694 0.100 Uiso 1 1 calc R . . C26 C 0.5160(2) 0.5859(3) 0.1736(2) 0.0753(14) Uani 1 1 d . . . H26A H 0.5195 0.5525 0.2146 0.113 Uiso 1 1 calc R . . H26B H 0.5551 0.6234 0.1938 0.113 Uiso 1 1 calc R . . H26C H 0.5270 0.5615 0.1320 0.113 Uiso 1 1 calc R . . O27 O 0.34257(10) 0.27771(10) 0.09137(10) 0.0275(4) Uani 1 1 d . . . C28 C 0.28127(15) 0.23664(14) 0.05049(13) 0.0253(5) Uani 1 1 d . . . C29 C 0.29117(16) 0.16895(14) 0.02410(14) 0.0291(5) Uani 1 1 d . . . C30 C 0.22243(16) 0.13081(14) -0.01327(15) 0.0299(6) Uani 1 1 d . . . H30 H 0.2284 0.0849 -0.0303 0.036 Uiso 1 1 calc R . . C31 C 0.14505(16) 0.15524(14) -0.02754(14) 0.0279(5) Uani 1 1 d . . . C32 C 0.13727(15) 0.22361(14) -0.00545(14) 0.0261(5) Uani 1 1 d . . . H32 H 0.0859 0.2435 -0.0169 0.031 Uiso 1 1 calc R . . C33 C 0.20411(15) 0.26289(13) 0.03323(13) 0.0248(5) Uani 1 1 d . . . N34 N 0.20061(12) 0.33496(11) 0.05692(11) 0.0246(4) Uani 1 1 d . . . H34 H 0.1983 0.3618 0.0145 0.030 Uiso 1 1 calc R . . C35 C 0.13501(14) 0.35829(13) 0.07695(13) 0.0235(5) Uani 1 1 d . . . C36 C 0.09778(15) 0.31530(14) 0.11461(13) 0.0268(5) Uani 1 1 d . . . H36 H 0.1128 0.2674 0.1232 0.032 Uiso 1 1 calc R . . C37 C 0.03895(15) 0.34136(14) 0.13977(14) 0.0287(6) Uani 1 1 d . . . H37 H 0.0140 0.3113 0.1652 0.034 Uiso 1 1 calc R A . C38 C 0.01651(15) 0.41123(14) 0.12781(14) 0.0287(5) Uani 1 1 d . . . H38 H -0.0228 0.4295 0.1461 0.034 Uiso 1 1 calc R . . C39 C 0.05194(14) 0.45409(14) 0.08894(14) 0.0274(5) Uani 1 1 d . . . H39 H 0.0359 0.5017 0.0795 0.033 Uiso 1 1 calc R A . C40 C 0.11100(14) 0.42783(13) 0.06353(13) 0.0231(5) Uani 1 1 d . . . N41 N 0.15137(12) 0.47513(11) 0.02920(11) 0.0244(4) Uani 1 1 d . . . H41 H 0.1221 0.5159 0.0267 0.029 Uiso 1 1 calc R A . C42 C 0.14170(14) 0.46639(13) -0.05151(13) 0.0241(5) Uani 1 1 d . . . C43 C 0.08804(14) 0.42160(13) -0.10187(14) 0.0243(5) Uani 1 1 d . . . H43 H 0.0556 0.3918 -0.0843 0.029 Uiso 1 1 calc R . . C44 C 0.08163(14) 0.42033(13) -0.17888(14) 0.0253(5) Uani 1 1 d . . . C45 C 0.12892(15) 0.46706(14) -0.20144(15) 0.0289(6) Uani 1 1 d . . . H45 H 0.1235 0.4676 -0.2541 0.035 Uiso 1 1 calc R A . C46 C 0.18374(15) 0.51315(15) -0.15214(15) 0.0291(6) Uani 1 1 d . . . C47 C 0.19275(15) 0.50993(14) -0.07372(14) 0.0267(5) Uani 1 1 d . . . O48 O 0.24712(10) 0.54694(10) -0.01768(10) 0.0299(4) Uani 1 1 d . . . C49 C 0.37448(16) 0.13870(15) 0.03710(16) 0.0333(6) Uani 1 1 d . . . C50 C 0.37002(19) 0.06605(17) -0.0001(2) 0.0484(8) Uani 1 1 d . . . H50A H 0.3410 0.0337 0.0215 0.073 Uiso 1 1 calc R . . H50B H 0.4240 0.0482 0.0102 0.073 Uiso 1 1 calc R . . H50C H 0.3423 0.0700 -0.0556 0.073 Uiso 1 1 calc R . . C51 C 0.42065(18) 0.13107(18) 0.12334(17) 0.0418(7) Uani 1 1 d . . . H51A H 0.4242 0.1768 0.1483 0.063 Uiso 1 1 calc R . . H51B H 0.4743 0.1136 0.1314 0.063 Uiso 1 1 calc R . . H51C H 0.3929 0.0979 0.1455 0.063 Uiso 1 1 calc R . . C52 C 0.41983(17) 0.18749(17) 0.00140(17) 0.0388(7) Uani 1 1 d . . . H52A H 0.3895 0.1932 -0.0534 0.058 Uiso 1 1 calc R . . H52B H 0.4720 0.1671 0.0081 0.058 Uiso 1 1 calc R . . H52C H 0.4270 0.2334 0.0267 0.058 Uiso 1 1 calc R . . C53 C 0.07273(16) 0.10802(15) -0.06696(16) 0.0318(6) Uani 1 1 d . . . C54 C 0.06287(19) 0.09875(18) -0.15190(17) 0.0442(7) Uani 1 1 d . . . H54A H 0.0556 0.1448 -0.1769 0.066 Uiso 1 1 calc R . . H54B H 0.0163 0.0694 -0.1773 0.066 Uiso 1 1 calc R . . H54C H 0.1105 0.0762 -0.1556 0.066 Uiso 1 1 calc R . . C55 C 0.0852(2) 0.03635(17) -0.0276(2) 0.0510(8) Uani 1 1 d . . . H55A H 0.1344 0.0153 -0.0292 0.077 Uiso 1 1 calc R . . H55B H 0.0402 0.0057 -0.0543 0.077 Uiso 1 1 calc R . . H55C H 0.0891 0.0421 0.0259 0.077 Uiso 1 1 calc R . . C56 C -0.00417(17) 0.13936(17) -0.0625(2) 0.0437(7) Uani 1 1 d . . . H56A H 0.0028 0.1491 -0.0088 0.065 Uiso 1 1 calc R . . H56B H -0.0479 0.1059 -0.0838 0.065 Uiso 1 1 calc R . . H56C H -0.0166 0.1831 -0.0920 0.065 Uiso 1 1 calc R . . C57 C 0.01959(15) 0.37262(14) -0.23613(14) 0.0277(5) Uani 1 1 d . . . C58 C 0.02069(18) 0.29922(15) -0.20272(16) 0.0373(6) Uani 1 1 d . . . H58A H 0.0081 0.3024 -0.1557 0.056 Uiso 1 1 calc R . . H58B H 0.0736 0.2785 -0.1909 0.056 Uiso 1 1 calc R . . H58C H -0.0190 0.2697 -0.2402 0.056 Uiso 1 1 calc R . . C59 C 0.03394(19) 0.36535(17) -0.31213(16) 0.0406(7) Uani 1 1 d . . . H59A H -0.0029 0.3305 -0.3445 0.061 Uiso 1 1 calc R . . H59B H 0.0888 0.3501 -0.3020 0.061 Uiso 1 1 calc R . . H59C H 0.0250 0.4107 -0.3385 0.061 Uiso 1 1 calc R . . C60 C -0.06302(16) 0.40524(16) -0.25216(17) 0.0362(6) Uani 1 1 d . . . H60A H -0.1034 0.3761 -0.2893 0.054 Uiso 1 1 calc R . . H60B H -0.0642 0.4526 -0.2731 0.054 Uiso 1 1 calc R . . H60C H -0.0741 0.4078 -0.2043 0.054 Uiso 1 1 calc R . . C61 C 0.22852(17) 0.56812(17) -0.18165(16) 0.0377(7) Uani 1 1 d . . . C62 C 0.2126(2) 0.5590(2) -0.26768(18) 0.0560(10) Uani 1 1 d . . . H62A H 0.2423 0.5945 -0.2846 0.084 Uiso 1 1 calc R . . H62B H 0.1556 0.5644 -0.2964 0.084 Uiso 1 1 calc R . . H62C H 0.2298 0.5121 -0.2770 0.084 Uiso 1 1 calc R . . C63 C 0.31847(18) 0.5642(2) -0.14038(18) 0.0489(8) Uani 1 1 d . . . H63A H 0.3446 0.5993 -0.1620 0.073 Uiso 1 1 calc R . . H63B H 0.3374 0.5173 -0.1470 0.073 Uiso 1 1 calc R . . H63C H 0.3312 0.5736 -0.0856 0.073 Uiso 1 1 calc R . . C64 C 0.1979(2) 0.64071(18) -0.1693(2) 0.0555(9) Uani 1 1 d . . . H64A H 0.2106 0.6488 -0.1143 0.083 Uiso 1 1 calc R . . H64B H 0.1401 0.6428 -0.1955 0.083 Uiso 1 1 calc R . . H64C H 0.2233 0.6769 -0.1902 0.083 Uiso 1 1 calc R . . C65 C 0.7695(4) 0.1172(4) -0.0515(3) 0.134(2) Uiso 1 1 d . . . H65A H 0.7241 0.0864 -0.0570 0.201 Uiso 1 1 calc R . . H65B H 0.8095 0.0915 -0.0658 0.201 Uiso 1 1 calc R . . H65C H 0.7514 0.1580 -0.0853 0.201 Uiso 1 1 calc R . . C66 C 0.8051(4) 0.1414(5) 0.0299(3) 0.062(3) Uiso 1 1 d . . . H66A H 0.8162 0.0995 0.0635 0.074 Uiso 1 1 calc R . . H66B H 0.8568 0.1639 0.0367 0.074 Uiso 1 1 calc R . . C67 C 0.7567(6) 0.1914(3) 0.0573(6) 0.080(4) Uiso 1 1 d . . . H67A H 0.7945 0.2233 0.0946 0.097 Uiso 1 1 calc R . . H67B H 0.7258 0.2204 0.0128 0.097 Uiso 1 1 calc R . . C68 C 0.6999(5) 0.1656(4) 0.0938(6) 0.175(4) Uiso 1 1 d . . . H68A H 0.7327 0.1431 0.1426 0.210 Uiso 1 1 calc R . . H68B H 0.6689 0.1276 0.0604 0.210 Uiso 1 1 calc R . . C69 C 0.6406(3) 0.2107(2) 0.1125(3) 0.0712(11) Uiso 1 1 d . . . H69A H 0.6675 0.2368 0.1599 0.107 Uiso 1 1 calc R . . H69B H 0.5991 0.1810 0.1194 0.107 Uiso 1 1 calc R . . H69C H 0.6165 0.2438 0.0704 0.107 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 0.0234(2) 0.0273(3) 0.0242(2) -0.00217(18) 0.00881(18) 0.00033(18) Ti2 0.0258(2) 0.0259(3) 0.0280(2) -0.00298(18) 0.00968(19) -0.00297(18) O3 0.0271(9) 0.0287(10) 0.0254(8) -0.0038(7) 0.0106(7) -0.0017(7) C4 0.0322(14) 0.0335(15) 0.0256(12) -0.0054(11) 0.0104(11) 0.0005(11) C5 0.0376(16) 0.0440(18) 0.0349(14) -0.0029(13) 0.0175(12) 0.0035(13) C6 0.0372(15) 0.0407(17) 0.0325(14) -0.0080(12) 0.0104(12) -0.0091(13) O7 0.0263(9) 0.0300(10) 0.0266(8) -0.0034(7) 0.0119(7) -0.0014(7) C8 0.0314(14) 0.0348(15) 0.0284(12) -0.0035(11) 0.0157(11) -0.0019(11) C9 0.0353(14) 0.0382(16) 0.0265(12) -0.0031(11) 0.0125(11) 0.0028(12) C10 0.0311(15) 0.057(2) 0.0371(15) -0.0062(14) 0.0178(12) -0.0034(13) O11 0.0444(11) 0.0319(11) 0.0350(10) -0.0022(8) 0.0212(9) -0.0036(9) C12 0.0298(14) 0.0381(16) 0.0252(12) 0.0029(11) 0.0071(11) 0.0037(12) C13 0.0414(16) 0.0319(16) 0.0367(14) 0.0074(12) 0.0121(13) 0.0062(12) C14 0.0389(16) 0.0455(18) 0.0279(13) 0.0066(12) 0.0136(12) 0.0027(13) O15 0.0280(9) 0.0374(11) 0.0279(9) -0.0019(8) 0.0071(8) 0.0012(8) C16 0.029(2) 0.050(4) 0.032(2) 0.008(2) 0.0072(18) 0.004(2) C17 0.054(2) 0.083(3) 0.065(2) 0.022(2) 0.0227(19) 0.033(2) C18 0.067(3) 0.115(4) 0.0389(19) -0.013(2) -0.0086(18) 0.035(3) O19 0.0390(11) 0.0285(10) 0.0336(10) -0.0043(8) 0.0101(8) 0.0024(8) C20 0.0518(18) 0.0291(16) 0.0452(16) 0.0023(13) 0.0199(14) 0.0040(13) C21 0.092(3) 0.0327(19) 0.058(2) -0.0108(16) 0.020(2) 0.0003(19) C22 0.072(3) 0.043(2) 0.082(3) -0.007(2) -0.005(2) 0.019(2) O23 0.0314(10) 0.0344(11) 0.0354(10) -0.0028(8) 0.0090(8) -0.0104(8) C24 0.059(2) 0.060(2) 0.069(2) -0.0214(19) 0.030(2) -0.0314(19) C25 0.083(3) 0.040(2) 0.098(3) -0.005(2) 0.057(3) -0.017(2) C26 0.0372(19) 0.135(4) 0.0455(19) -0.002(2) 0.0046(16) -0.033(2) O27 0.0237(9) 0.0302(10) 0.0275(9) -0.0028(7) 0.0075(7) 0.0019(7) C28 0.0267(12) 0.0269(13) 0.0229(11) 0.0004(10) 0.0095(10) 0.0011(10) C29 0.0330(14) 0.0284(14) 0.0269(12) 0.0001(11) 0.0116(11) 0.0049(11) C30 0.0354(14) 0.0256(14) 0.0314(13) -0.0027(11) 0.0151(11) 0.0012(11) C31 0.0320(14) 0.0265(14) 0.0266(12) -0.0006(10) 0.0118(11) -0.0010(11) C32 0.0251(12) 0.0269(14) 0.0267(12) 0.0011(10) 0.0095(10) 0.0019(10) C33 0.0280(13) 0.0245(13) 0.0229(11) 0.0001(10) 0.0100(10) 0.0028(10) N34 0.0254(11) 0.0238(11) 0.0259(10) -0.0009(8) 0.0105(8) 0.0017(9) C35 0.0209(11) 0.0259(13) 0.0223(11) -0.0024(9) 0.0059(9) 0.0003(10) C36 0.0287(13) 0.0247(13) 0.0246(12) 0.0019(10) 0.0062(10) 0.0027(10) C37 0.0285(13) 0.0325(15) 0.0272(12) 0.0027(11) 0.0127(10) 0.0001(11) C38 0.0260(13) 0.0334(15) 0.0295(12) -0.0016(11) 0.0130(11) 0.0020(11) C39 0.0247(12) 0.0279(14) 0.0280(12) -0.0006(10) 0.0075(10) 0.0041(10) C40 0.0218(12) 0.0239(13) 0.0224(11) -0.0015(9) 0.0063(9) -0.0026(10) N41 0.0261(11) 0.0224(11) 0.0255(10) -0.0018(8) 0.0100(9) 0.0012(8) C42 0.0249(12) 0.0237(13) 0.0240(11) 0.0005(9) 0.0090(10) 0.0033(10) C43 0.0225(12) 0.0233(13) 0.0281(12) 0.0014(10) 0.0103(10) 0.0021(10) C44 0.0232(12) 0.0237(13) 0.0284(12) 0.0001(10) 0.0083(10) 0.0025(10) C45 0.0261(13) 0.0343(15) 0.0260(12) 0.0031(11) 0.0090(10) 0.0039(11) C46 0.0253(13) 0.0313(15) 0.0309(13) 0.0050(11) 0.0098(11) 0.0011(11) C47 0.0248(12) 0.0239(13) 0.0296(12) 0.0021(10) 0.0075(10) 0.0019(10) O48 0.0280(9) 0.0299(10) 0.0314(9) -0.0008(8) 0.0097(8) -0.0058(8) C49 0.0316(14) 0.0328(15) 0.0366(14) -0.0027(12) 0.0133(12) 0.0082(12) C50 0.0409(17) 0.0397(18) 0.065(2) -0.0141(16) 0.0190(16) 0.0111(14) C51 0.0396(16) 0.0458(19) 0.0393(15) 0.0062(13) 0.0129(13) 0.0147(14) C52 0.0315(15) 0.0473(19) 0.0404(15) -0.0004(13) 0.0161(12) 0.0076(13) C53 0.0322(14) 0.0280(15) 0.0369(14) -0.0056(11) 0.0143(12) -0.0056(11) C54 0.0459(18) 0.0478(19) 0.0397(16) -0.0142(14) 0.0159(14) -0.0129(15) C55 0.0498(19) 0.0343(18) 0.068(2) 0.0048(15) 0.0195(17) -0.0082(15) C56 0.0326(15) 0.0436(19) 0.0565(19) -0.0158(15) 0.0178(14) -0.0096(13) C57 0.0288(13) 0.0264(13) 0.0270(12) -0.0005(10) 0.0084(10) 0.0011(10) C58 0.0424(16) 0.0288(15) 0.0349(14) -0.0028(12) 0.0062(12) -0.0026(12) C59 0.0441(17) 0.0475(19) 0.0303(14) -0.0073(13) 0.0132(13) -0.0044(14) C60 0.0295(14) 0.0346(16) 0.0397(15) -0.0048(12) 0.0059(12) 0.0000(12) C61 0.0333(15) 0.0417(17) 0.0364(14) 0.0102(13) 0.0103(12) -0.0082(13) C62 0.052(2) 0.078(3) 0.0379(16) 0.0135(17) 0.0146(15) -0.0216(19) C63 0.0363(16) 0.066(2) 0.0444(17) 0.0157(16) 0.0137(14) -0.0136(15) C64 0.060(2) 0.0369(19) 0.069(2) 0.0170(16) 0.0222(19) -0.0058(16) _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 O15 1.7810(19) . ? Ti1 O11 1.7898(18) . ? Ti1 O27 1.9301(18) . ? Ti1 O3 2.0452(18) . ? Ti1 O7 2.0818(18) . ? Ti1 N34 2.411(2) . ? Ti1 Ti2 3.2975(7) . ? Ti2 O23 1.7647(18) . ? Ti2 O19 1.8484(19) . ? Ti2 O48 1.9338(18) . ? Ti2 O3 2.0055(18) . ? Ti2 O7 2.0521(18) . ? Ti2 N41 2.431(2) . ? O3 C4 1.465(3) . ? C4 C6 1.514(4) . ? C4 C5 1.514(4) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C8 1.450(3) . ? C8 C10 1.510(4) . ? C8 C9 1.525(4) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O11 C12 1.419(3) . ? C12 C13 1.514(4) . ? C12 C14 1.524(4) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O15 C16 1.458(5) . ? C16 C17 1.462(6) . ? C16 C18 1.480(6) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O19 C20 1.413(4) . ? C20 C22 1.495(5) . ? C20 C21 1.496(4) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O23 C24 1.408(4) . ? C24 C26 1.475(6) . ? C24 C25 1.520(6) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O27 C28 1.347(3) . ? C28 C33 1.400(3) . ? C28 C29 1.414(4) . ? C29 C30 1.390(4) . ? C29 C49 1.541(4) . ? C30 C31 1.400(4) . ? C30 H30 0.9500 . ? C31 C32 1.388(4) . ? C31 C53 1.538(4) . ? C32 C33 1.383(4) . ? C32 H32 0.9500 . ? C33 N34 1.451(3) . ? N34 C35 1.426(3) . ? N34 H34 0.9300 . ? C35 C40 1.389(4) . ? C35 C36 1.392(3) . ? C36 C37 1.389(4) . ? C36 H36 0.9500 . ? C37 C38 1.387(4) . ? C37 H37 0.9500 . ? C38 C39 1.385(4) . ? C38 H38 0.9500 . ? C39 C40 1.397(3) . ? C39 H39 0.9500 . ? C40 N41 1.439(3) . ? N41 C42 1.460(3) . ? N41 H41 0.9300 . ? C42 C43 1.379(4) . ? C42 C47 1.402(3) . ? C43 C44 1.398(3) . ? C43 H43 0.9500 . ? C44 C45 1.393(4) . ? C44 C57 1.540(4) . ? C45 C46 1.396(4) . ? C45 H45 0.9500 . ? C46 C47 1.412(3) . ? C46 C61 1.535(4) . ? C47 O48 1.351(3) . ? C49 C52 1.533(4) . ? C49 C51 1.534(4) . ? C49 C50 1.537(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C55 1.529(4) . ? C53 C56 1.533(4) . ? C53 C54 1.538(4) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.528(4) . ? C57 C59 1.531(4) . ? C57 C60 1.538(4) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.528(4) . ? C61 C62 1.535(4) . ? C61 C64 1.536(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.496(2) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.495(12) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.493(15) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.501(11) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 O15 Ti1 O11 100.72(9) . . ? O15 Ti1 O27 97.11(8) . . ? O11 Ti1 O27 96.83(8) . . ? O15 Ti1 O3 98.36(8) . . ? O11 Ti1 O3 93.99(8) . . ? O27 Ti1 O3 159.12(7) . . ? O15 Ti1 O7 100.12(8) . . ? O11 Ti1 O7 156.31(8) . . ? O27 Ti1 O7 91.65(7) . . ? O3 Ti1 O7 71.88(7) . . ? O15 Ti1 N34 170.11(8) . . ? O11 Ti1 N34 84.68(8) . . ? O27 Ti1 N34 73.88(7) . . ? O3 Ti1 N34 89.46(7) . . ? O7 Ti1 N34 76.47(7) . . ? O15 Ti1 Ti2 100.84(7) . . ? O11 Ti1 Ti2 126.96(7) . . ? O27 Ti1 Ti2 127.46(6) . . ? O3 Ti1 Ti2 35.11(5) . . ? O7 Ti1 Ti2 36.78(5) . . ? N34 Ti1 Ti2 82.08(5) . . ? O23 Ti2 O19 99.46(9) . . ? O23 Ti2 O48 97.15(8) . . ? O19 Ti2 O48 95.70(8) . . ? O23 Ti2 O3 107.42(8) . . ? O19 Ti2 O3 94.62(8) . . ? O48 Ti2 O3 151.33(8) . . ? O23 Ti2 O7 96.18(8) . . ? O19 Ti2 O7 162.59(8) . . ? O48 Ti2 O7 89.87(7) . . ? O3 Ti2 O7 73.30(7) . . ? O23 Ti2 N41 168.21(8) . . ? O19 Ti2 N41 79.63(8) . . ? O48 Ti2 N41 71.35(7) . . ? O3 Ti2 N41 84.37(7) . . ? O7 Ti2 N41 86.60(7) . . ? O23 Ti2 Ti1 104.23(7) . . ? O19 Ti2 Ti1 129.61(6) . . ? O48 Ti2 Ti1 123.99(6) . . ? O3 Ti2 Ti1 35.91(5) . . ? O7 Ti2 Ti1 37.40(5) . . ? N41 Ti2 Ti1 84.93(5) . . ? C4 O3 Ti2 128.52(16) . . ? C4 O3 Ti1 117.24(15) . . ? Ti2 O3 Ti1 108.98(8) . . ? O3 C4 C6 110.8(2) . . ? O3 C4 C5 108.9(2) . . ? C6 C4 C5 113.4(2) . . ? O3 C4 H4 107.8 . . ? C6 C4 H4 107.8 . . ? C5 C4 H4 107.8 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 O7 Ti2 119.78(16) . . ? C8 O7 Ti1 128.96(16) . . ? Ti2 O7 Ti1 105.82(7) . . ? O7 C8 C10 111.1(2) . . ? O7 C8 C9 110.2(2) . . ? C10 C8 C9 112.1(2) . . ? O7 C8 H8 107.7 . . ? C10 C8 H8 107.7 . . ? C9 C8 H8 107.7 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 O11 Ti1 158.06(18) . . ? O11 C12 C13 109.5(2) . . ? O11 C12 C14 109.3(2) . . ? C13 C12 C14 112.9(2) . . ? O11 C12 H12 108.4 . . ? C13 C12 H12 108.4 . . ? C14 C12 H12 108.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 O15 Ti1 137.9(3) . . ? O15 C16 C17 109.0(3) . . ? O15 C16 C18 108.9(4) . . ? C17 C16 C18 116.5(4) . . ? O15 C16 H16 107.4 . . ? C17 C16 H16 107.4 . . ? C18 C16 H16 107.4 . . ? C20 O19 Ti2 134.80(18) . . ? O19 C20 C22 110.4(3) . . ? O19 C20 C21 109.9(3) . . ? C22 C20 C21 111.7(3) . . ? O19 C20 H20 108.3 . . ? C22 C20 H20 108.3 . . ? C21 C20 H20 108.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 O23 Ti2 158.3(2) . . ? O23 C24 C26 110.0(3) . . ? O23 C24 C25 109.0(3) . . ? C26 C24 C25 113.1(3) . . ? O23 C24 H24 108.2 . . ? C26 C24 H24 108.2 . . ? C25 C24 H24 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 O27 Ti1 123.21(15) . . ? O27 C28 C33 117.9(2) . . ? O27 C28 C29 123.3(2) . . ? C33 C28 C29 118.8(2) . . ? C30 C29 C28 116.9(2) . . ? C30 C29 C49 121.7(2) . . ? C28 C29 C49 121.4(2) . . ? C29 C30 C31 124.7(2) . . ? C29 C30 H30 117.7 . . ? C31 C30 H30 117.7 . . ? C32 C31 C30 116.9(2) . . ? C32 C31 C53 122.3(2) . . ? C30 C31 C53 120.8(2) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C32 C33 C28 122.3(2) . . ? C32 C33 N34 123.3(2) . . ? C28 C33 N34 114.4(2) . . ? C35 N34 C33 120.2(2) . . ? C35 N34 Ti1 115.91(15) . . ? C33 N34 Ti1 104.72(14) . . ? C35 N34 H34 104.8 . . ? C33 N34 H34 104.8 . . ? Ti1 N34 H34 104.8 . . ? C40 C35 C36 118.6(2) . . ? C40 C35 N34 118.9(2) . . ? C36 C35 N34 122.3(2) . . ? C37 C36 C35 121.0(2) . . ? C37 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C38 C37 C36 120.1(2) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C39 C38 C37 119.3(2) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 120.5(2) . . ? C38 C39 H39 119.7 . . ? C40 C39 H39 119.7 . . ? C35 C40 C39 120.4(2) . . ? C35 C40 N41 120.3(2) . . ? C39 C40 N41 119.1(2) . . ? C40 N41 C42 119.27(19) . . ? C40 N41 Ti2 126.10(15) . . ? C42 N41 Ti2 104.71(14) . . ? C40 N41 H41 100.5 . . ? C42 N41 H41 100.5 . . ? Ti2 N41 H41 100.5 . . ? C43 C42 C47 122.6(2) . . ? C43 C42 N41 124.9(2) . . ? C47 C42 N41 112.5(2) . . ? C42 C43 C44 119.6(2) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C45 C44 C43 117.3(2) . . ? C45 C44 C57 122.6(2) . . ? C43 C44 C57 120.0(2) . . ? C44 C45 C46 124.6(2) . . ? C44 C45 H45 117.7 . . ? C46 C45 H45 117.7 . . ? C45 C46 C47 116.8(2) . . ? C45 C46 C61 122.1(2) . . ? C47 C46 C61 121.0(2) . . ? O48 C47 C42 116.8(2) . . ? O48 C47 C46 124.4(2) . . ? C42 C47 C46 118.7(2) . . ? C47 O48 Ti2 123.89(16) . . ? C52 C49 C51 109.7(2) . . ? C52 C49 C50 107.6(2) . . ? C51 C49 C50 108.0(3) . . ? C52 C49 C29 109.8(2) . . ? C51 C49 C29 109.8(2) . . ? C50 C49 C29 111.8(2) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C55 C53 C56 107.8(2) . . ? C55 C53 C31 109.7(2) . . ? C56 C53 C31 111.8(2) . . ? C55 C53 C54 109.5(3) . . ? C56 C53 C54 108.6(2) . . ? C31 C53 C54 109.3(2) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 C59 108.1(2) . . ? C58 C57 C60 108.8(2) . . ? C59 C57 C60 108.7(2) . . ? C58 C57 C44 110.9(2) . . ? C59 C57 C44 112.2(2) . . ? C60 C57 C44 108.1(2) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 C62 107.2(3) . . ? C63 C61 C46 112.4(2) . . ? C62 C61 C46 111.5(2) . . ? C63 C61 C64 109.9(3) . . ? C62 C61 C64 108.3(3) . . ? C46 C61 C64 107.5(2) . . ? 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 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C67 C66 C65 116.6(7) . . ? C67 C66 H66A 108.1 . . ? C65 C66 H66A 108.1 . . ? C67 C66 H66B 108.1 . . ? C65 C66 H66B 108.1 . . ? H66A C66 H66B 107.3 . . ? C68 C67 C66 121.2(2) . . ? C68 C67 H67A 107.0 . . ? C66 C67 H67A 107.0 . . ? C68 C67 H67B 107.0 . . ? C66 C67 H67B 107.0 . . ? H67A C67 H67B 106.8 . . ? C67 C68 C69 124.8(6) . . ? C67 C68 H68A 106.1 . . ? C69 C68 H68A 106.1 . . ? C67 C68 H68B 106.1 . . ? C69 C68 H68B 106.1 . . ? H68A C68 H68B 106.3 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.125 _refine_diff_density_min -0.682 _refine_diff_density_rms 0.071 #===============END================================ data_mk197 _database_code_depnum_ccdc_archive 'CCDC 742352' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H60 N2 O4 Ti' _chemical_formula_sum 'C40 H60 N2 O4 Ti' _chemical_formula_weight 680.80 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 'P 21/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 15.9917(4) _cell_length_b 50.3346(10) _cell_length_c 9.9634(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.3742(7) _cell_angle_gamma 90.00 _cell_volume 7984.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 8298 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 25.00 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.253 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '0.6 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24913 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1493 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -59 _diffrn_reflns_limit_k_max 0 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12703 _reflns_number_gt 5591 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. There are two molecules of the compound in the asymmetric unit. The four propoxy groups of the asymmetric unit are conformationally disorder. The disorder of three of them could not be resolved reliably by discrete atoms. ; _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^)+(0.1066P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12703 _refine_ls_number_parameters 895 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1862 _refine_ls_R_factor_gt 0.0748 _refine_ls_wR_factor_ref 0.2212 _refine_ls_wR_factor_gt 0.1662 _refine_ls_goodness_of_fit_ref 0.957 _refine_ls_restrained_S_all 0.957 _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 -0.03709(5) 0.183014(19) 0.28972(8) 0.0320(3) Uani 1 1 d . A . O2 O -0.0768(2) 0.15940(7) 0.1683(3) 0.0406(9) Uani 1 1 d . . . C3A C -0.0676(8) 0.1456(2) 0.0453(11) 0.045(4) Uani 0.576(18) 1 d P A 1 H3A H -0.0139 0.1515 0.0107 0.054 Uiso 0.576(18) 1 calc PR A 1 C4A C -0.0599(9) 0.1160(3) 0.0786(15) 0.069(4) Uani 0.576(18) 1 d P A 1 H4A1 H -0.0068 0.1127 0.1334 0.103 Uiso 0.576(18) 1 calc PR A 1 H4A2 H -0.0612 0.1057 -0.0052 0.103 Uiso 0.576(18) 1 calc PR A 1 H4A3 H -0.1069 0.1106 0.1290 0.103 Uiso 0.576(18) 1 calc PR A 1 C5A C -0.1392(10) 0.1529(2) -0.0583(14) 0.054(4) Uani 0.576(18) 1 d P A 1 H5A1 H -0.1927 0.1480 -0.0245 0.080 Uiso 0.576(18) 1 calc PR A 1 H5A2 H -0.1329 0.1433 -0.1425 0.080 Uiso 0.576(18) 1 calc PR A 1 H5A3 H -0.1383 0.1721 -0.0750 0.080 Uiso 0.576(18) 1 calc PR A 1 C3B C -0.1130(11) 0.1385(3) 0.0860(15) 0.039(5) Uiso 0.424(18) 1 d P A 2 H3B H -0.1430 0.1262 0.1441 0.047 Uiso 0.424(18) 1 calc PR A 2 C4B C -0.0436(13) 0.1229(5) 0.026(2) 0.062(7) Uiso 0.424(18) 1 d P A 2 H4B1 H -0.0123 0.1349 -0.0292 0.093 Uiso 0.424(18) 1 calc PR A 2 H4B2 H -0.0685 0.1085 -0.0308 0.093 Uiso 0.424(18) 1 calc PR A 2 H4B3 H -0.0052 0.1154 0.0985 0.093 Uiso 0.424(18) 1 calc PR A 2 C5B C -0.1753(12) 0.1494(5) -0.0206(19) 0.058(6) Uiso 0.424(18) 1 d P A 2 H5B1 H -0.2242 0.1562 0.0211 0.087 Uiso 0.424(18) 1 calc PR A 2 H5B2 H -0.1930 0.1354 -0.0851 0.087 Uiso 0.424(18) 1 calc PR A 2 H5B3 H -0.1495 0.1640 -0.0676 0.087 Uiso 0.424(18) 1 calc PR A 2 O6 O 0.0052(2) 0.16553(7) 0.4361(3) 0.0412(10) Uani 1 1 d . . . C7 C 0.0455(4) 0.14303(15) 0.4948(7) 0.081(2) Uani 1 1 d . A . H7 H 0.0565 0.1312 0.4179 0.097 Uiso 1 1 calc R . . C8 C 0.1275(4) 0.14846(13) 0.5665(6) 0.075(2) Uani 1 1 d . . . H8A H 0.1617 0.1586 0.5080 0.112 Uiso 1 1 calc R A . H8B H 0.1557 0.1316 0.5914 0.112 Uiso 1 1 calc R . . H8C H 0.1202 0.1587 0.6481 0.112 Uiso 1 1 calc R . . C9 C -0.0134(4) 0.12837(17) 0.5725(9) 0.145(4) Uani 1 1 d . . . H9A H -0.0274 0.1392 0.6488 0.218 Uiso 1 1 calc R A . H9B H 0.0129 0.1118 0.6060 0.218 Uiso 1 1 calc R . . H9C H -0.0647 0.1244 0.5143 0.218 Uiso 1 1 calc R . . O10 O 0.06525(19) 0.18828(6) 0.2022(3) 0.0292(8) Uani 1 1 d . . . C11 C 0.1318(3) 0.19782(10) 0.2831(5) 0.0285(12) Uani 1 1 d . A . C12 C 0.2154(3) 0.19028(10) 0.2725(4) 0.0286(13) Uani 1 1 d . . . C13 C 0.2758(3) 0.19933(10) 0.3739(5) 0.0320(13) Uani 1 1 d . A . H13 H 0.3327 0.1945 0.3681 0.038 Uiso 1 1 calc R . . C14 C 0.2571(3) 0.21496(10) 0.4820(5) 0.0312(13) Uani 1 1 d . . . C15 C 0.1743(3) 0.22258(10) 0.4892(5) 0.0325(13) Uani 1 1 d . A . H15 H 0.1595 0.2332 0.5620 0.039 Uiso 1 1 calc R . . C16 C 0.1132(3) 0.21453(10) 0.3893(5) 0.0272(12) Uani 1 1 d . . . N17 N 0.0236(2) 0.21974(8) 0.3914(4) 0.0274(10) Uani 1 1 d . A . H17 H 0.0111 0.2200 0.4807 0.033 Uiso 1 1 calc R . . C18 C -0.0046(3) 0.24472(10) 0.3287(5) 0.0272(12) Uani 1 1 d . . . C19 C 0.0232(3) 0.26910(11) 0.3809(5) 0.0312(13) Uani 1 1 d . A . H19 H 0.0617 0.2698 0.4593 0.037 Uiso 1 1 calc R . . C20 C -0.0055(3) 0.29224(11) 0.3182(5) 0.0371(14) Uani 1 1 d . . . H20 H 0.0143 0.3089 0.3533 0.044 Uiso 1 1 calc R A . C21 C -0.0624(3) 0.29162(11) 0.2053(5) 0.0368(14) Uani 1 1 d . A . H21 H -0.0827 0.3077 0.1645 0.044 Uiso 1 1 calc R . . C22 C -0.0895(3) 0.26772(10) 0.1526(5) 0.0316(13) Uani 1 1 d . . . H22 H -0.1284 0.2673 0.0745 0.038 Uiso 1 1 calc R A . C23 C -0.0604(3) 0.24383(10) 0.2127(5) 0.0273(12) Uani 1 1 d . A . N24 N -0.0870(2) 0.21793(8) 0.1575(3) 0.0273(10) Uani 1 1 d . . . H24 H -0.0687 0.2161 0.0720 0.033 Uiso 1 1 calc R A . C25 C -0.1780(3) 0.21352(10) 0.1490(4) 0.0235(12) Uani 1 1 d . A . C26 C -0.2309(3) 0.21968(10) 0.0375(4) 0.0285(12) Uani 1 1 d . . . H26 H -0.2101 0.2287 -0.0364 0.034 Uiso 1 1 calc R A . C27 C -0.3152(3) 0.21270(10) 0.0326(4) 0.0250(12) Uani 1 1 d . A . C28 C -0.3411(3) 0.20004(10) 0.1469(4) 0.0294(13) Uani 1 1 d . . . H28 H -0.3989 0.1957 0.1462 0.035 Uiso 1 1 calc R A . C29 C -0.2887(3) 0.19325(10) 0.2615(4) 0.0262(12) Uani 1 1 d . A . C30 C -0.2041(3) 0.20013(10) 0.2600(4) 0.0258(12) Uani 1 1 d . . . O31 O -0.14287(18) 0.19319(7) 0.3574(3) 0.0304(9) Uani 1 1 d . A . C32 C 0.2385(3) 0.17057(11) 0.1644(5) 0.0319(13) Uani 1 1 d . A . C33 C 0.3334(3) 0.16702(11) 0.1623(5) 0.0412(15) Uani 1 1 d . . . H33A H 0.3593 0.1843 0.1468 0.062 Uiso 1 1 calc R A . H33B H 0.3446 0.1547 0.0897 0.062 Uiso 1 1 calc R . . H33C H 0.3571 0.1598 0.2489 0.062 Uiso 1 1 calc R . . C34 C 0.2036(3) 0.18058(11) 0.0230(4) 0.0408(15) Uani 1 1 d . . . H34A H 0.1425 0.1826 0.0201 0.061 Uiso 1 1 calc R A . H34B H 0.2172 0.1677 -0.0455 0.061 Uiso 1 1 calc R . . H34C H 0.2291 0.1978 0.0049 0.061 Uiso 1 1 calc R . . C35 C 0.1989(3) 0.14348(10) 0.1920(5) 0.0395(14) Uani 1 1 d . . . H35A H 0.2165 0.1379 0.2846 0.059 Uiso 1 1 calc R A . H35B H 0.2174 0.1303 0.1288 0.059 Uiso 1 1 calc R . . H35C H 0.1376 0.1450 0.1800 0.059 Uiso 1 1 calc R . . C36 C 0.3250(3) 0.22225(11) 0.5969(5) 0.0374(14) Uani 1 1 d . A . C37 C 0.4134(3) 0.21513(13) 0.5628(5) 0.0579(18) Uani 1 1 d . . . H37A H 0.4242 0.2236 0.4776 0.087 Uiso 1 1 calc R A . H37B H 0.4181 0.1958 0.5542 0.087 Uiso 1 1 calc R . . H37C H 0.4545 0.2214 0.6349 0.087 Uiso 1 1 calc R . . C38 C 0.3249(4) 0.25238(13) 0.6190(6) 0.069(2) Uani 1 1 d . . . H38A H 0.2700 0.2579 0.6458 0.104 Uiso 1 1 calc R A . H38B H 0.3356 0.2614 0.5352 0.104 Uiso 1 1 calc R . . H38C H 0.3688 0.2571 0.6902 0.104 Uiso 1 1 calc R . . C39 C 0.3072(4) 0.20766(16) 0.7228(5) 0.088(3) Uani 1 1 d . . . H39A H 0.3519 0.2114 0.7945 0.132 Uiso 1 1 calc R A . H39B H 0.3049 0.1885 0.7047 0.132 Uiso 1 1 calc R . . H39C H 0.2532 0.2136 0.7512 0.132 Uiso 1 1 calc R . . C40 C -0.3776(3) 0.21726(10) -0.0905(4) 0.0323(13) Uani 1 1 d . . . C41 C -0.4084(3) 0.18984(10) -0.1461(5) 0.0395(14) Uani 1 1 d . A . H41A H -0.3601 0.1792 -0.1676 0.059 Uiso 1 1 calc R . . H41B H -0.4466 0.1924 -0.2279 0.059 Uiso 1 1 calc R . . H41C H -0.4380 0.1806 -0.0781 0.059 Uiso 1 1 calc R . . C42 C -0.3382(3) 0.23211(11) -0.2022(5) 0.0456(16) Uani 1 1 d . A . H42A H -0.3213 0.2499 -0.1705 0.068 Uiso 1 1 calc R . . H42B H -0.3791 0.2336 -0.2814 0.068 Uiso 1 1 calc R . . H42C H -0.2887 0.2224 -0.2265 0.068 Uiso 1 1 calc R . . C43 C -0.4529(3) 0.23339(12) -0.0522(5) 0.0489(16) Uani 1 1 d . A . H43A H -0.4818 0.2235 0.0148 0.073 Uiso 1 1 calc R . . H43B H -0.4918 0.2365 -0.1326 0.073 Uiso 1 1 calc R . . H43C H -0.4334 0.2505 -0.0140 0.073 Uiso 1 1 calc R . . C44 C -0.3203(3) 0.17781(11) 0.3790(5) 0.0348(14) Uani 1 1 d . . . C45 C -0.2952(3) 0.19263(11) 0.5129(4) 0.0455(16) Uani 1 1 d . A . H45A H -0.3155 0.1827 0.5879 0.068 Uiso 1 1 calc R . . H45B H -0.3203 0.2104 0.5089 0.068 Uiso 1 1 calc R . . H45C H -0.2339 0.1942 0.5265 0.068 Uiso 1 1 calc R . . C46 C -0.4164(3) 0.17491(12) 0.3650(5) 0.0494(17) Uani 1 1 d . A . H46A H -0.4340 0.1644 0.2846 0.074 Uiso 1 1 calc R . . H46B H -0.4424 0.1925 0.3565 0.074 Uiso 1 1 calc R . . H46C H -0.4342 0.1660 0.4450 0.074 Uiso 1 1 calc R . . C47 C -0.2817(3) 0.14998(11) 0.3843(5) 0.0490(16) Uani 1 1 d . A . H47A H -0.2963 0.1409 0.2982 0.073 Uiso 1 1 calc R . . H47B H -0.3035 0.1398 0.4572 0.073 Uiso 1 1 calc R . . H47C H -0.2205 0.1514 0.4008 0.073 Uiso 1 1 calc R . . Ti48 Ti -0.48748(5) 0.066998(19) 0.73848(8) 0.0325(3) Uani 1 1 d . . . O49 O -0.4427(2) 0.08731(7) 0.8711(3) 0.0415(10) Uani 1 1 d . . . C50 C -0.4069(4) 0.10556(17) 0.9608(7) 0.095(3) Uani 1 1 d . . . H50 H -0.3858 0.1194 0.9005 0.115 Uiso 1 1 calc R . . C51 C -0.3328(4) 0.09777(15) 1.0407(6) 0.082(2) Uani 1 1 d . . . H51A H -0.3471 0.0848 1.1083 0.123 Uiso 1 1 calc R . . H51B H -0.3068 0.1134 1.0861 0.123 Uiso 1 1 calc R . . H51C H -0.2934 0.0897 0.9829 0.123 Uiso 1 1 calc R . . C52 C -0.4718(4) 0.12046(15) 1.0313(6) 0.089(3) Uani 1 1 d . . . H52A H -0.5128 0.1285 0.9640 0.133 Uiso 1 1 calc R . . H52B H -0.4443 0.1344 1.0880 0.133 Uiso 1 1 calc R . . H52C H -0.5006 0.1081 1.0876 0.133 Uiso 1 1 calc R . . O53 O -0.5221(2) 0.08764(7) 0.5995(3) 0.0434(10) Uani 1 1 d . . . C54 C -0.5616(7) 0.10724(15) 0.5202(8) 0.142(4) Uani 1 1 d . . . H54 H -0.5121 0.1117 0.4702 0.171 Uiso 1 1 calc R . . C55 C -0.5658(5) 0.13265(13) 0.5864(6) 0.091(3) Uani 1 1 d . . . H55A H -0.6124 0.1326 0.6437 0.137 Uiso 1 1 calc R . . H55B H -0.5750 0.1467 0.5185 0.137 Uiso 1 1 calc R . . H55C H -0.5130 0.1359 0.6420 0.137 Uiso 1 1 calc R . . C56 C -0.6126(5) 0.10025(16) 0.4111(8) 0.138(4) Uani 1 1 d . . . H56A H -0.5949 0.0830 0.3777 0.207 Uiso 1 1 calc R . . H56B H -0.6097 0.1137 0.3405 0.207 Uiso 1 1 calc R . . H56C H -0.6705 0.0989 0.4354 0.207 Uiso 1 1 calc R . . O57 O -0.59393(18) 0.06247(7) 0.8174(3) 0.0328(9) Uani 1 1 d . . . C58 C -0.6600(3) 0.05552(10) 0.7292(4) 0.0268(12) Uani 1 1 d . . . C59 C -0.7431(3) 0.06395(10) 0.7384(5) 0.0304(13) Uani 1 1 d . . . C60 C -0.8020(3) 0.05741(10) 0.6298(5) 0.0303(13) Uani 1 1 d . . . H60 H -0.8586 0.0628 0.6349 0.036 Uiso 1 1 calc R . . C61 C -0.7831(3) 0.04365(10) 0.5155(5) 0.0286(12) Uani 1 1 d . . . C62 C -0.7015(3) 0.03434(10) 0.5133(4) 0.0293(13) Uani 1 1 d . . . H62 H -0.6865 0.0241 0.4392 0.035 Uiso 1 1 calc R . . C63 C -0.6430(3) 0.04000(10) 0.6182(5) 0.0250(12) Uani 1 1 d . . . N64 N -0.5536(2) 0.03269(8) 0.6216(3) 0.0272(10) Uani 1 1 d . . . H64 H -0.5381 0.0329 0.5339 0.033 Uiso 1 1 calc R . . C65 C -0.5343(3) 0.00675(10) 0.6796(4) 0.0264(12) Uani 1 1 d . . . C66 C -0.5657(3) -0.01674(10) 0.6226(5) 0.0294(13) Uani 1 1 d . . . H66 H -0.6039 -0.0161 0.5437 0.035 Uiso 1 1 calc R . . C67 C -0.5424(3) -0.04116(11) 0.6788(5) 0.0349(13) Uani 1 1 d . . . H67 H -0.5642 -0.0571 0.6382 0.042 Uiso 1 1 calc R . . C68 C -0.4874(3) -0.04218(11) 0.7942(5) 0.0343(13) Uani 1 1 d . . . H68 H -0.4713 -0.0589 0.8331 0.041 Uiso 1 1 calc R . . C69 C -0.4556(3) -0.01892(10) 0.8533(5) 0.0296(13) Uani 1 1 d . . . H69 H -0.4168 -0.0197 0.9316 0.036 Uiso 1 1 calc R . . C70 C -0.4800(3) 0.00545(10) 0.7988(5) 0.0266(12) Uani 1 1 d . . . N71 N -0.4481(2) 0.03027(8) 0.8605(3) 0.0283(10) Uani 1 1 d . . . H71 H -0.4675 0.0318 0.9453 0.034 Uiso 1 1 calc R . . C72 C -0.3569(3) 0.03243(10) 0.8751(5) 0.0264(12) Uani 1 1 d . . . C73 C -0.3079(3) 0.02433(10) 0.9883(4) 0.0281(12) Uani 1 1 d . . . H73 H -0.3325 0.0156 1.0596 0.034 Uiso 1 1 calc R . . C74 C -0.2218(3) 0.02905(10) 0.9975(4) 0.0285(12) Uani 1 1 d . . . C75 C -0.1898(3) 0.04134(10) 0.8876(4) 0.0283(13) Uani 1 1 d . . . H75 H -0.1308 0.0442 0.8923 0.034 Uiso 1 1 calc R . . C76 C -0.2379(3) 0.04979(10) 0.7713(4) 0.0286(12) Uani 1 1 d . . . C77 C -0.3260(3) 0.04575(10) 0.7676(5) 0.0282(12) Uani 1 1 d . . . O78 O -0.38291(19) 0.05500(7) 0.6692(3) 0.0322(9) Uani 1 1 d . . . C79 C -0.8519(3) 0.03929(11) 0.3983(5) 0.0338(13) Uani 1 1 d . . . C80 C -0.8186(3) 0.02435(11) 0.2816(4) 0.0444(15) Uani 1 1 d . . . H80A H -0.7737 0.0347 0.2462 0.067 Uiso 1 1 calc R . . H80B H -0.8642 0.0217 0.2102 0.067 Uiso 1 1 calc R . . H80C H -0.7965 0.0071 0.3134 0.067 Uiso 1 1 calc R . . C81 C -0.8825(3) 0.06683(11) 0.3453(5) 0.0473(15) Uani 1 1 d . . . H81A H -0.9081 0.0764 0.4167 0.071 Uiso 1 1 calc R . . H81B H -0.9242 0.0645 0.2675 0.071 Uiso 1 1 calc R . . H81C H -0.8347 0.0770 0.3180 0.071 Uiso 1 1 calc R . . C82 C -0.9259(3) 0.02396(12) 0.4469(5) 0.0437(15) Uani 1 1 d . . . H82A H -0.9066 0.0065 0.4806 0.065 Uiso 1 1 calc R . . H82B H -0.9694 0.0217 0.3718 0.065 Uiso 1 1 calc R . . H82C H -0.9490 0.0339 0.5194 0.065 Uiso 1 1 calc R . . C83 C -0.7649(3) 0.08057(11) 0.8589(5) 0.0335(13) Uani 1 1 d . . . C84 C -0.7205(3) 0.10716(10) 0.8555(5) 0.0411(14) Uani 1 1 d . . . H84A H -0.6600 0.1043 0.8541 0.062 Uiso 1 1 calc R . . H84B H -0.7308 0.1175 0.9357 0.062 Uiso 1 1 calc R . . H84C H -0.7419 0.1169 0.7745 0.062 Uiso 1 1 calc R . . C85 C -0.7367(3) 0.06580(11) 0.9914(4) 0.0425(15) Uani 1 1 d . . . H85A H -0.7647 0.0485 0.9917 0.064 Uiso 1 1 calc R . . H85B H -0.7517 0.0763 1.0682 0.064 Uiso 1 1 calc R . . H85C H -0.6757 0.0632 0.9983 0.064 Uiso 1 1 calc R . . C86 C -0.8599(3) 0.08560(12) 0.8571(5) 0.0470(16) Uani 1 1 d . . . H86A H -0.8790 0.0964 0.7783 0.071 Uiso 1 1 calc R . . H86B H -0.8715 0.0950 0.9394 0.071 Uiso 1 1 calc R . . H86C H -0.8898 0.0686 0.8526 0.071 Uiso 1 1 calc R . . C87 C -0.1637(3) 0.02291(11) 1.1260(4) 0.0327(13) Uani 1 1 d . . . C88 C -0.2116(3) 0.01005(11) 1.2346(4) 0.0396(14) Uani 1 1 d . . . H88A H -0.1722 0.0054 1.3123 0.059 Uiso 1 1 calc R . . H88B H -0.2398 -0.0060 1.1982 0.059 Uiso 1 1 calc R . . H88C H -0.2535 0.0226 1.2628 0.059 Uiso 1 1 calc R . . C89 C -0.1250(3) 0.04877(11) 1.1808(5) 0.0437(15) Uani 1 1 d . . . H89A H -0.0906 0.0453 1.2656 0.066 Uiso 1 1 calc R . . H89B H -0.1697 0.0613 1.1970 0.066 Uiso 1 1 calc R . . H89C H -0.0898 0.0564 1.1151 0.066 Uiso 1 1 calc R . . C90 C -0.0940(3) 0.00390(12) 1.0921(5) 0.0512(17) Uani 1 1 d . . . H90A H -0.0595 0.0125 1.0282 0.077 Uiso 1 1 calc R . . H90B H -0.1191 -0.0123 1.0516 0.077 Uiso 1 1 calc R . . H90C H -0.0587 -0.0006 1.1747 0.077 Uiso 1 1 calc R . . C91 C -0.1995(3) 0.06483(11) 0.6585(5) 0.0345(14) Uani 1 1 d . . . C92 C -0.2275(3) 0.09380(11) 0.6598(5) 0.0459(15) Uani 1 1 d . . . H92A H -0.2889 0.0947 0.6444 0.069 Uiso 1 1 calc R . . H92B H -0.2025 0.1036 0.5884 0.069 Uiso 1 1 calc R . . H92C H -0.2091 0.1017 0.7475 0.069 Uiso 1 1 calc R . . C93 C -0.1030(3) 0.06375(11) 0.6766(5) 0.0440(15) Uani 1 1 d . . . H93A H -0.0826 0.0729 0.7602 0.066 Uiso 1 1 calc R . . H93B H -0.0803 0.0725 0.6000 0.066 Uiso 1 1 calc R . . H93C H -0.0845 0.0452 0.6809 0.066 Uiso 1 1 calc R . . C94 C -0.2287(3) 0.05207(11) 0.5215(4) 0.0461(16) Uani 1 1 d . . . H94A H -0.2158 0.0330 0.5248 0.069 Uiso 1 1 calc R . . H94B H -0.1994 0.0605 0.4506 0.069 Uiso 1 1 calc R . . H94C H -0.2894 0.0546 0.5021 0.069 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 0.0301(6) 0.0302(6) 0.0350(6) 0.0013(5) -0.0012(4) 0.0006(5) O2 0.037(2) 0.037(2) 0.048(2) -0.014(2) 0.0011(17) -0.0042(18) C3A 0.054(8) 0.021(6) 0.065(8) 0.006(6) 0.030(6) -0.006(5) C4A 0.106(12) 0.038(9) 0.065(9) -0.007(8) 0.021(8) 0.000(8) C5A 0.076(11) 0.032(7) 0.049(8) -0.008(6) -0.011(8) -0.018(7) O6 0.037(2) 0.038(2) 0.047(2) 0.012(2) -0.0058(17) 0.0014(18) C7 0.057(5) 0.078(6) 0.102(6) 0.044(5) -0.014(4) -0.001(4) C8 0.050(4) 0.081(6) 0.088(5) 0.048(4) -0.018(4) -0.003(4) C9 0.049(5) 0.148(9) 0.233(10) 0.145(8) -0.017(6) -0.020(5) O10 0.0284(19) 0.036(2) 0.0222(18) -0.0066(17) -0.0055(15) 0.0087(17) C11 0.027(3) 0.030(3) 0.028(3) 0.003(3) -0.001(2) -0.001(2) C12 0.029(3) 0.031(3) 0.025(3) 0.009(3) 0.002(2) 0.003(3) C13 0.030(3) 0.034(3) 0.032(3) 0.005(3) 0.001(3) 0.002(3) C14 0.034(3) 0.028(3) 0.030(3) 0.003(3) 0.000(2) -0.004(3) C15 0.037(3) 0.029(3) 0.032(3) -0.004(3) 0.003(3) 0.001(3) C16 0.029(3) 0.024(3) 0.029(3) 0.000(3) 0.007(2) 0.002(2) N17 0.025(2) 0.034(3) 0.024(2) -0.003(2) 0.0049(18) 0.005(2) C18 0.026(3) 0.030(3) 0.027(3) 0.002(3) 0.011(2) 0.005(2) C19 0.033(3) 0.033(4) 0.027(3) -0.001(3) 0.001(2) 0.000(3) C20 0.043(3) 0.032(4) 0.036(3) -0.010(3) 0.004(3) -0.009(3) C21 0.036(3) 0.028(4) 0.046(3) -0.004(3) 0.006(3) 0.006(3) C22 0.033(3) 0.034(4) 0.028(3) 0.004(3) 0.002(2) 0.003(3) C23 0.023(3) 0.034(4) 0.026(3) -0.004(3) 0.008(2) -0.003(2) N24 0.026(2) 0.035(3) 0.021(2) -0.005(2) 0.0032(18) -0.002(2) C25 0.022(3) 0.026(3) 0.024(3) -0.005(3) 0.007(2) -0.001(2) C26 0.035(3) 0.027(3) 0.024(3) 0.000(2) 0.003(2) -0.003(2) C27 0.026(3) 0.028(3) 0.021(3) 0.002(2) -0.001(2) 0.002(2) C28 0.022(3) 0.037(3) 0.028(3) -0.011(3) -0.002(2) 0.002(2) C29 0.024(3) 0.032(3) 0.024(3) -0.005(3) 0.007(2) -0.003(2) C30 0.030(3) 0.029(3) 0.018(3) -0.002(2) 0.001(2) 0.004(2) O31 0.0259(19) 0.041(2) 0.0237(18) 0.0083(17) -0.0029(15) 0.0050(17) C32 0.029(3) 0.039(4) 0.029(3) -0.004(3) 0.007(2) 0.005(3) C33 0.034(3) 0.039(4) 0.053(4) -0.003(3) 0.015(3) 0.010(3) C34 0.049(4) 0.045(4) 0.030(3) -0.007(3) 0.010(3) 0.010(3) C35 0.047(4) 0.032(4) 0.041(3) -0.004(3) 0.014(3) 0.009(3) C36 0.038(3) 0.040(4) 0.032(3) -0.012(3) -0.008(3) 0.002(3) C37 0.042(4) 0.081(5) 0.049(4) -0.014(4) -0.008(3) -0.005(4) C38 0.064(4) 0.069(5) 0.069(4) -0.027(4) -0.024(4) 0.008(4) C39 0.064(5) 0.166(8) 0.030(3) 0.018(4) -0.009(3) -0.057(5) C40 0.035(3) 0.035(4) 0.025(3) -0.002(3) -0.007(2) 0.005(3) C41 0.044(3) 0.043(4) 0.031(3) 0.000(3) 0.001(3) -0.005(3) C42 0.055(4) 0.045(4) 0.035(3) 0.001(3) -0.006(3) 0.004(3) C43 0.049(4) 0.064(5) 0.032(3) 0.000(3) -0.007(3) 0.019(3) C44 0.033(3) 0.045(4) 0.027(3) 0.000(3) 0.004(2) -0.004(3) C45 0.057(4) 0.058(4) 0.024(3) -0.002(3) 0.013(3) -0.013(3) C46 0.043(4) 0.072(5) 0.035(3) 0.005(3) 0.016(3) -0.017(3) C47 0.064(4) 0.040(4) 0.044(3) 0.009(3) 0.008(3) -0.017(3) Ti48 0.0318(6) 0.0297(6) 0.0351(6) -0.0021(5) -0.0018(4) 0.0010(5) O49 0.035(2) 0.035(2) 0.053(2) -0.022(2) -0.0086(17) 0.0026(18) C50 0.061(5) 0.124(8) 0.096(6) -0.077(5) -0.021(4) 0.026(5) C51 0.057(5) 0.101(6) 0.082(5) -0.050(5) -0.020(4) 0.012(4) C52 0.082(5) 0.096(6) 0.088(5) -0.051(5) 0.003(4) 0.028(5) O53 0.047(2) 0.030(2) 0.051(2) 0.014(2) -0.0081(18) -0.0029(18) C54 0.273(12) 0.037(5) 0.095(6) -0.004(5) -0.098(7) 0.051(7) C55 0.157(8) 0.037(5) 0.085(5) 0.010(4) 0.041(5) 0.009(5) C56 0.164(9) 0.087(7) 0.144(8) 0.031(6) -0.084(7) 0.027(7) O57 0.0254(19) 0.048(3) 0.0242(18) -0.0085(17) -0.0033(15) 0.0098(17) C58 0.030(3) 0.027(3) 0.023(3) -0.002(3) -0.001(2) 0.007(2) C59 0.036(3) 0.025(3) 0.031(3) 0.005(3) 0.008(3) 0.007(3) C60 0.023(3) 0.036(3) 0.033(3) 0.000(3) 0.006(2) 0.003(2) C61 0.026(3) 0.031(3) 0.029(3) 0.005(3) 0.003(2) 0.002(2) C62 0.034(3) 0.031(3) 0.023(3) -0.003(3) 0.005(2) 0.000(3) C63 0.025(3) 0.023(3) 0.028(3) 0.001(3) 0.008(2) -0.001(2) N64 0.024(2) 0.034(3) 0.024(2) 0.003(2) 0.0017(18) 0.004(2) C65 0.023(3) 0.033(3) 0.024(3) -0.005(3) 0.007(2) -0.002(2) C66 0.025(3) 0.036(4) 0.029(3) -0.005(3) 0.006(2) 0.000(3) C67 0.033(3) 0.034(4) 0.039(3) -0.008(3) 0.008(3) -0.002(3) C68 0.037(3) 0.031(4) 0.035(3) 0.011(3) 0.003(3) 0.006(3) C69 0.027(3) 0.035(4) 0.028(3) 0.003(3) 0.006(2) 0.001(3) C70 0.026(3) 0.026(3) 0.029(3) -0.001(3) 0.009(2) -0.003(2) N71 0.027(2) 0.035(3) 0.023(2) -0.004(2) 0.0050(18) 0.000(2) C72 0.027(3) 0.025(3) 0.027(3) -0.003(3) -0.001(2) 0.001(2) C73 0.031(3) 0.026(3) 0.027(3) -0.004(3) 0.002(2) -0.005(2) C74 0.031(3) 0.032(3) 0.022(3) -0.003(3) 0.001(2) 0.001(3) C75 0.021(3) 0.033(3) 0.031(3) -0.008(3) 0.002(2) 0.003(2) C76 0.031(3) 0.030(3) 0.026(3) -0.008(3) 0.005(2) 0.001(2) C77 0.031(3) 0.027(3) 0.027(3) -0.009(3) 0.007(2) -0.001(2) O78 0.029(2) 0.044(2) 0.0225(18) 0.0071(17) -0.0034(15) -0.0048(17) C79 0.031(3) 0.040(4) 0.029(3) 0.002(3) -0.006(2) -0.001(3) C80 0.045(4) 0.050(4) 0.035(3) -0.003(3) -0.010(3) 0.001(3) C81 0.044(4) 0.048(4) 0.047(4) 0.001(3) -0.008(3) -0.001(3) C82 0.029(3) 0.061(4) 0.038(3) 0.006(3) -0.010(2) -0.009(3) C83 0.028(3) 0.043(4) 0.030(3) 0.002(3) 0.008(2) 0.009(3) C84 0.049(4) 0.034(4) 0.041(3) -0.005(3) 0.009(3) 0.009(3) C85 0.047(4) 0.054(4) 0.026(3) -0.005(3) 0.003(3) 0.012(3) C86 0.039(3) 0.064(4) 0.041(3) -0.006(3) 0.015(3) 0.015(3) C87 0.030(3) 0.043(4) 0.025(3) 0.001(3) -0.001(2) 0.004(3) C88 0.043(3) 0.046(4) 0.029(3) 0.008(3) -0.003(3) -0.001(3) C89 0.040(3) 0.057(4) 0.034(3) -0.002(3) -0.002(3) -0.002(3) C90 0.042(4) 0.075(5) 0.035(3) 0.001(3) -0.006(3) 0.024(3) C91 0.038(3) 0.041(4) 0.025(3) 0.005(3) 0.007(2) -0.007(3) C92 0.048(4) 0.039(4) 0.052(4) 0.000(3) 0.010(3) -0.009(3) C93 0.040(3) 0.052(4) 0.042(3) 0.010(3) 0.016(3) -0.003(3) C94 0.051(4) 0.061(4) 0.028(3) 0.000(3) 0.013(3) -0.014(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 O2 1.771(3) . ? Ti1 O6 1.782(3) . ? Ti1 O10 1.944(3) . ? Ti1 O31 1.947(3) . ? Ti1 N17 2.281(4) . ? Ti1 N24 2.295(4) . ? O2 C3B 1.424(14) . ? O2 C3A 1.428(11) . ? C3A C5A 1.513(14) . ? C3A C4A 1.529(19) . ? C3A H3A 1.0000 . ? C4A H4A1 0.9800 . ? C4A H4A2 0.9800 . ? C4A H4A3 0.9800 . ? C5A H5A1 0.9800 . ? C5A H5A2 0.9800 . ? C5A H5A3 0.9800 . ? C3B C5B 1.49(2) . ? C3B C4B 1.53(3) . ? C3B H3B 1.0000 . ? C4B H4B1 0.9800 . ? C4B H4B2 0.9800 . ? C4B H4B3 0.9800 . ? C5B H5B1 0.9800 . ? C5B H5B2 0.9800 . ? C5B H5B3 0.9800 . ? O6 C7 1.402(7) . ? C7 C8 1.459(7) . ? C7 C9 1.471(8) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? O10 C11 1.361(5) . ? C11 C12 1.403(6) . ? C11 C16 1.406(6) . ? C12 C13 1.407(6) . ? C12 C32 1.535(6) . ? C13 C14 1.388(6) . ? C13 H13 0.9500 . ? C14 C15 1.387(6) . ? C14 C36 1.547(6) . ? C15 C16 1.388(6) . ? C15 H15 0.9500 . ? C16 N17 1.460(6) . ? N17 C18 1.457(6) . ? N17 H17 0.9300 . ? C18 C19 1.389(7) . ? C18 C23 1.394(6) . ? C19 C20 1.379(7) . ? C19 H19 0.9500 . ? C20 C21 1.379(6) . ? C20 H20 0.9500 . ? C21 C22 1.367(7) . ? C21 H21 0.9500 . ? C22 C23 1.403(6) . ? C22 H22 0.9500 . ? C23 N24 1.462(6) . ? N24 C25 1.467(5) . ? N24 H24 0.9300 . ? C25 C26 1.368(6) . ? C25 C30 1.392(6) . ? C26 C27 1.390(6) . ? C26 H26 0.9500 . ? C27 C28 1.400(6) . ? C27 C40 1.525(6) . ? C28 C29 1.394(6) . ? C28 H28 0.9500 . ? C29 C30 1.399(6) . ? C29 C44 1.530(6) . ? C30 O31 1.358(5) . ? C32 C33 1.531(6) . ? C32 C35 1.539(7) . ? C32 C34 1.551(6) . ? 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 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C39 1.503(7) . ? C36 C37 1.527(7) . ? C36 C38 1.532(7) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C42 1.525(7) . ? C40 C43 1.531(7) . ? C40 C41 1.550(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C47 1.530(7) . ? C44 C46 1.537(6) . ? C44 C45 1.548(6) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? Ti48 O49 1.768(3) . ? Ti48 O53 1.777(3) . ? Ti48 O57 1.954(3) . ? Ti48 O78 1.963(3) . ? Ti48 N71 2.269(4) . ? Ti48 N64 2.286(4) . ? O49 C50 1.370(6) . ? C50 C51 1.418(8) . ? C50 C52 1.507(8) . ? C50 H50 1.0000 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O53 C54 1.380(7) . ? C54 C56 1.344(9) . ? C54 C55 1.443(9) . ? C54 H54 1.0000 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? O57 C58 1.356(5) . ? C58 C63 1.401(6) . ? C58 C59 1.406(6) . ? C59 C60 1.406(6) . ? C59 C83 1.530(7) . ? C60 C61 1.390(6) . ? C60 H60 0.9500 . ? C61 C62 1.389(6) . ? C61 C79 1.543(6) . ? C62 C63 1.366(6) . ? C62 H62 0.9500 . ? C63 N64 1.474(5) . ? N64 C65 1.449(6) . ? N64 H64 0.9300 . ? C65 C66 1.385(6) . ? C65 C70 1.405(6) . ? C66 C67 1.388(7) . ? C66 H66 0.9500 . ? C67 C68 1.382(6) . ? C67 H67 0.9500 . ? C68 C69 1.385(6) . ? C68 H68 0.9500 . ? C69 C70 1.383(6) . ? C69 H69 0.9500 . ? C70 N71 1.463(6) . ? N71 C72 1.456(5) . ? N71 H71 0.9300 . ? C72 C73 1.374(6) . ? C72 C77 1.393(6) . ? C73 C74 1.392(6) . ? C73 H73 0.9500 . ? C74 C75 1.396(6) . ? C74 C87 1.541(6) . ? C75 C76 1.396(6) . ? C75 H75 0.9500 . ? C76 C77 1.420(6) . ? C76 C91 1.530(6) . ? C77 O78 1.356(5) . ? C79 C80 1.522(7) . ? C79 C82 1.528(6) . ? C79 C81 1.546(7) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 C84 1.517(7) . ? C83 C86 1.539(6) . ? C83 C85 1.545(6) . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C89 1.520(7) . ? C87 C88 1.527(6) . ? C87 C90 1.530(7) . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 C92 1.525(7) . ? C91 C94 1.540(6) . ? C91 C93 1.539(6) . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 H94A 0.9800 . ? C94 H94B 0.9800 . ? C94 H94C 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 O6 108.18(17) . . ? O2 Ti1 O10 92.75(14) . . ? O6 Ti1 O10 99.41(14) . . ? O2 Ti1 O31 98.37(14) . . ? O6 Ti1 O31 97.02(14) . . ? O10 Ti1 O31 156.19(15) . . ? O2 Ti1 N17 163.35(15) . . ? O6 Ti1 N17 85.62(15) . . ? O10 Ti1 N17 75.40(13) . . ? O31 Ti1 N17 88.86(13) . . ? O2 Ti1 N24 92.22(15) . . ? O6 Ti1 N24 158.97(15) . . ? O10 Ti1 N24 84.25(13) . . ? O31 Ti1 N24 74.39(13) . . ? N17 Ti1 N24 75.21(14) . . ? C3B O2 C3A 38.3(6) . . ? C3B O2 Ti1 172.0(8) . . ? C3A O2 Ti1 148.6(6) . . ? O2 C3A C5A 109.6(9) . . ? O2 C3A C4A 107.5(10) . . ? C5A C3A C4A 115.1(10) . . ? O2 C3A H3A 108.1 . . ? C5A C3A H3A 108.1 . . ? C4A C3A H3A 108.1 . . ? O2 C3B C5B 110.2(13) . . ? O2 C3B C4B 109.5(14) . . ? C5B C3B C4B 111.8(14) . . ? O2 C3B H3B 108.4 . . ? C5B C3B H3B 108.4 . . ? C4B C3B H3B 108.4 . . ? C3B C4B H4B1 109.5 . . ? C3B C4B H4B2 109.5 . . ? H4B1 C4B H4B2 109.5 . . ? C3B C4B H4B3 109.5 . . ? H4B1 C4B H4B3 109.5 . . ? H4B2 C4B H4B3 109.5 . . ? C3B C5B H5B1 109.5 . . ? C3B C5B H5B2 109.5 . . ? H5B1 C5B H5B2 109.5 . . ? C3B C5B H5B3 109.5 . . ? H5B1 C5B H5B3 109.5 . . ? H5B2 C5B H5B3 109.5 . . ? C7 O6 Ti1 149.8(4) . . ? O6 C7 C8 114.2(6) . . ? O6 C7 C9 109.5(6) . . ? C8 C7 C9 115.2(6) . . ? O6 C7 H7 105.7 . . ? C8 C7 H7 105.7 . . ? C9 C7 H7 105.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 O10 Ti1 115.3(3) . . ? O10 C11 C12 123.9(4) . . ? O10 C11 C16 116.7(4) . . ? C12 C11 C16 119.2(4) . . ? C11 C12 C13 117.0(4) . . ? C11 C12 C32 121.4(4) . . ? C13 C12 C32 121.3(4) . . ? C14 C13 C12 123.9(5) . . ? C14 C13 H13 118.1 . . ? C12 C13 H13 118.1 . . ? C15 C14 C13 118.2(5) . . ? C15 C14 C36 120.2(4) . . ? C13 C14 C36 121.5(5) . . ? C14 C15 C16 119.6(5) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C15 C16 C11 122.0(5) . . ? C15 C16 N17 124.3(4) . . ? C11 C16 N17 113.3(4) . . ? C18 N17 C16 114.4(4) . . ? C18 N17 Ti1 114.1(3) . . ? C16 N17 Ti1 103.0(3) . . ? C18 N17 H17 108.4 . . ? C16 N17 H17 108.4 . . ? Ti1 N17 H17 108.4 . . ? C19 C18 C23 119.7(5) . . ? C19 C18 N17 121.8(4) . . ? C23 C18 N17 118.4(5) . . ? C20 C19 C18 119.7(5) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C21 C20 C19 121.0(5) . . ? C21 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C20 119.7(5) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C21 C22 C23 120.6(5) . . ? C21 C22 H22 119.7 . . ? C23 C22 H22 119.7 . . ? C18 C23 C22 119.2(5) . . ? C18 C23 N24 118.8(5) . . ? C22 C23 N24 122.0(4) . . ? C23 N24 C25 114.1(4) . . ? C23 N24 Ti1 113.2(3) . . ? C25 N24 Ti1 101.9(3) . . ? C23 N24 H24 109.1 . . ? C25 N24 H24 109.1 . . ? Ti1 N24 H24 109.1 . . ? C26 C25 C30 123.1(4) . . ? C26 C25 N24 123.2(4) . . ? C30 C25 N24 113.4(4) . . ? C25 C26 C27 119.7(4) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 116.5(4) . . ? C26 C27 C40 123.3(4) . . ? C28 C27 C40 120.1(4) . . ? C29 C28 C27 125.2(4) . . ? C29 C28 H28 117.4 . . ? C27 C28 H28 117.4 . . ? C28 C29 C30 116.0(4) . . ? C28 C29 C44 122.4(4) . . ? C30 C29 C44 121.5(4) . . ? O31 C30 C25 116.3(4) . . ? O31 C30 C29 124.2(4) . . ? C25 C30 C29 119.4(4) . . ? C30 O31 Ti1 114.3(3) . . ? C33 C32 C12 112.9(4) . . ? C33 C32 C35 108.9(4) . . ? C12 C32 C35 108.5(4) . . ? C33 C32 C34 107.3(4) . . ? C12 C32 C34 109.8(4) . . ? C35 C32 C34 109.3(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C39 C36 C37 108.8(5) . . ? C39 C36 C38 111.1(5) . . ? C37 C36 C38 106.1(5) . . ? C39 C36 C14 109.1(4) . . ? C37 C36 C14 112.3(4) . . ? C38 C36 C14 109.3(4) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C42 C40 C27 112.1(4) . . ? C42 C40 C43 108.1(4) . . ? C27 C40 C43 110.5(4) . . ? C42 C40 C41 108.3(4) . . ? C27 C40 C41 108.4(4) . . ? C43 C40 C41 109.3(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C29 C44 C47 109.3(4) . . ? C29 C44 C46 112.2(4) . . ? C47 C44 C46 108.3(5) . . ? C29 C44 C45 109.7(4) . . ? C47 C44 C45 109.9(4) . . ? C46 C44 C45 107.5(4) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C44 C46 H46A 109.5 . . ? C44 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C44 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C44 C47 H47A 109.5 . . ? C44 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C44 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O49 Ti48 O53 108.61(17) . . ? O49 Ti48 O57 94.21(14) . . ? O53 Ti48 O57 99.30(15) . . ? O49 Ti48 O78 98.18(14) . . ? O53 Ti48 O78 96.87(15) . . ? O57 Ti48 O78 155.30(15) . . ? O49 Ti48 N71 89.89(15) . . ? O53 Ti48 N71 160.75(15) . . ? O57 Ti48 N71 84.14(13) . . ? O78 Ti48 N71 74.64(13) . . ? O49 Ti48 N64 162.36(16) . . ? O53 Ti48 N64 87.08(15) . . ? O57 Ti48 N64 74.82(13) . . ? O78 Ti48 N64 87.54(13) . . ? N71 Ti48 N64 75.48(14) . . ? C50 O49 Ti48 172.3(5) . . ? O49 C50 C51 117.2(6) . . ? O49 C50 C52 111.9(5) . . ? C51 C50 C52 116.9(6) . . ? O49 C50 H50 102.7 . . ? C51 C50 H50 102.7 . . ? C52 C50 H50 102.7 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 O53 Ti48 163.1(5) . . ? C56 C54 O53 119.1(7) . . ? C56 C54 C55 123.5(8) . . ? O53 C54 C55 114.2(6) . . ? C56 C54 H54 95.9 . . ? O53 C54 H54 95.9 . . ? C55 C54 H54 95.9 . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C54 C56 H56A 109.5 . . ? C54 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C54 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 O57 Ti48 115.2(3) . . ? O57 C58 C63 117.3(4) . . ? O57 C58 C59 124.3(4) . . ? C63 C58 C59 118.3(4) . . ? C60 C59 C58 116.7(4) . . ? C60 C59 C83 123.1(4) . . ? C58 C59 C83 120.1(4) . . ? C61 C60 C59 124.4(4) . . ? C61 C60 H60 117.8 . . ? C59 C60 H60 117.8 . . ? C62 C61 C60 117.3(4) . . ? C62 C61 C79 123.0(4) . . ? C60 C61 C79 119.8(4) . . ? C63 C62 C61 119.6(4) . . ? C63 C62 H62 120.2 . . ? C61 C62 H62 120.2 . . ? C62 C63 C58 123.4(4) . . ? C62 C63 N64 124.0(4) . . ? C58 C63 N64 112.4(4) . . ? C65 N64 C63 113.8(4) . . ? C65 N64 Ti48 114.0(3) . . ? C63 N64 Ti48 103.0(3) . . ? C65 N64 H64 108.6 . . ? C63 N64 H64 108.6 . . ? Ti48 N64 H64 108.6 . . ? C66 C65 C70 118.6(5) . . ? C66 C65 N64 123.3(4) . . ? C70 C65 N64 118.1(4) . . ? C65 C66 C67 121.1(5) . . ? C65 C66 H66 119.4 . . ? C67 C66 H66 119.4 . . ? C68 C67 C66 119.6(5) . . ? C68 C67 H67 120.2 . . ? C66 C67 H67 120.2 . . ? C67 C68 C69 120.1(5) . . ? C67 C68 H68 119.9 . . ? C69 C68 H68 119.9 . . ? C70 C69 C68 120.2(5) . . ? C70 C69 H69 119.9 . . ? C68 C69 H69 119.9 . . ? C69 C70 C65 120.2(5) . . ? C69 C70 N71 121.2(4) . . ? C65 C70 N71 118.6(4) . . ? C72 N71 C70 114.3(4) . . ? C72 N71 Ti48 102.5(3) . . ? C70 N71 Ti48 113.7(3) . . ? C72 N71 H71 108.6 . . ? C70 N71 H71 108.6 . . ? Ti48 N71 H71 108.6 . . ? C73 C72 C77 123.9(5) . . ? C73 C72 N71 123.3(4) . . ? C77 C72 N71 112.6(4) . . ? C72 C73 C74 119.2(4) . . ? C72 C73 H73 120.4 . . ? C74 C73 H73 120.4 . . ? C73 C74 C75 117.2(4) . . ? C73 C74 C87 122.4(4) . . ? C75 C74 C87 120.2(4) . . ? C76 C75 C74 124.9(4) . . ? C76 C75 H75 117.6 . . ? C74 C75 H75 117.6 . . ? C75 C76 C77 116.5(4) . . ? C75 C76 C91 122.2(4) . . ? C77 C76 C91 121.1(4) . . ? O78 C77 C72 117.3(4) . . ? O78 C77 C76 124.5(4) . . ? C72 C77 C76 118.1(5) . . ? C77 O78 Ti48 112.8(3) . . ? C80 C79 C82 109.2(4) . . ? C80 C79 C61 111.9(4) . . ? C82 C79 C61 110.5(4) . . ? C80 C79 C81 107.7(4) . . ? C82 C79 C81 109.3(4) . . ? C61 C79 C81 108.2(4) . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C79 C82 H82A 109.5 . . ? C79 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C79 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 C59 108.9(4) . . ? C84 C83 C86 108.6(4) . . ? C59 C83 C86 112.2(4) . . ? C84 C83 C85 110.1(4) . . ? C59 C83 C85 109.8(4) . . ? C86 C83 C85 107.3(4) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C83 C86 H86A 109.5 . . ? C83 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C83 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C89 C87 C88 108.8(4) . . ? C89 C87 C90 109.5(4) . . ? C88 C87 C90 108.4(4) . . ? C89 C87 C74 108.7(4) . . ? C88 C87 C74 111.7(4) . . ? C90 C87 C74 109.7(4) . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C87 C90 H90A 109.5 . . ? C87 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C87 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C92 C91 C76 109.2(4) . . ? C92 C91 C94 110.0(4) . . ? C76 C91 C94 109.6(4) . . ? C92 C91 C93 108.9(4) . . ? C76 C91 C93 111.3(4) . . ? C94 C91 C93 107.8(4) . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C91 C94 H94A 109.5 . . ? C91 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C91 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? # start Validation Reply Form _vrf_PLAT029_mk197 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ..... 0.90 RESPONSE: Due to the poor diffraction of the analyzed crystal, and the very long b-axis of the unit-cell, it was difficult and impractical for technical reasons to measure a more complete set of data. ; _vrf_PLAT220_mk197 ; PROBLEM: Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.12 Rat RESPONSE: The propoxy groups in this structure are conformationally disordered. This disorder could not be reliably resolved by discrete atoms. ; _vrf_PLAT222_mk197 ; PROBLEM: Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.61 Rat RESPONSE: The propoxy groups in this structure are conformationally disordered. This disorder could not be reliably resolved by discrete atoms. ; _vrf_PLAT241_mk197 ; PROBLEM: Check High Ueq as Compared to Neighbors for C54 RESPONSE: The propoxy groups in this structure are conformationally disordered. This disorder could not be reliably resolved by discrete atoms. ; _vrf_PLAT242_mk197 ; PROBLEM: Check Low Ueq as Compared to Neighbors for ... O53 RESPONSE: The propoxy groups in this structure are conformationally disordered. This disorder could not be reliably resolved by discrete atoms. ; _vrf_PLAT213_mk197 ; PROBLEM: Atom C54 has ADP max/min Ration ...... 4.20 pro RESPONSE: The propoxy groups in this structure are conformationally disordered. This disorder could not be reliably resolved by discrete atoms. ; # end Validation Reply Form _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.904 _refine_diff_density_max 0.459 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.071 #=======================END======================================== data_mk200 _database_code_depnum_ccdc_archive 'CCDC 742353' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H88 N2 O8 Zr2, C5 H12' _chemical_formula_sum 'C57 H100 N2 O8 Zr2' _chemical_formula_weight 1123.83 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' Zr Zr -2.9673 0.5597 '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 14.4907(4) _cell_length_b 15.2879(3) _cell_length_c 15.5942(4) _cell_angle_alpha 66.3144(16) _cell_angle_beta 80.8334(10) _cell_angle_gamma 81.8588(11) _cell_volume 3111.68(13) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 10865 _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 25.98 _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.199 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1200 _exptl_absorpt_coefficient_mu 0.383 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method '1 deg. \f and \w scans' _diffrn_detector_area_resol_mean 12.8 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27999 _diffrn_reflns_av_R_equivalents 0.0510 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.41 _diffrn_reflns_theta_max 25.98 _reflns_number_total 11977 _reflns_number_gt 8576 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect, Nonius B.V.' _computing_cell_refinement Denzo _computing_data_reduction 'Denzo & Scalepack' _computing_structure_solution SIR-97 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Molecule of the pentane solvent is partly disordered. It was assigned isotropic ADP's, and the C-C bond lengths were restrained to 1.52A. Partial disorder was observed also in some of the propoxy substituents. ; _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^)+(0.0755P)^2^+2.9877P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11977 _refine_ls_number_parameters 623 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0845 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1513 _refine_ls_wR_factor_gt 0.1333 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Zr1 Zr 0.84273(3) -0.18482(3) 0.80199(3) 0.02777(11) Uani 1 1 d . . . Zr2 Zr 0.80486(3) 0.05656(3) 0.77948(3) 0.02843(12) Uani 1 1 d . . . O3 O 0.85340(19) -0.08428(19) 0.86583(19) 0.0306(6) Uani 1 1 d . . . C4 C 0.9151(3) -0.1140(3) 0.9403(3) 0.0366(10) Uani 1 1 d . . . H4 H 0.9440 -0.1801 0.9494 0.044 Uiso 1 1 calc R . . C5 C 0.9937(3) -0.0488(3) 0.9099(3) 0.0450(11) Uani 1 1 d . . . H5A H 1.0246 -0.0449 0.8479 0.067 Uiso 1 1 calc R . . H5B H 1.0395 -0.0746 0.9559 0.067 Uiso 1 1 calc R . . H5C H 0.9680 0.0153 0.9061 0.067 Uiso 1 1 calc R . . C6 C 0.8577(3) -0.1195(3) 1.0319(3) 0.0461(11) Uani 1 1 d . . . H6A H 0.8302 -0.0552 1.0259 0.069 Uiso 1 1 calc R . . H6B H 0.8983 -0.1451 1.0827 0.069 Uiso 1 1 calc R . . H6C H 0.8075 -0.1617 1.0465 0.069 Uiso 1 1 calc R . . O7 O 0.79258(19) -0.03994(18) 0.70935(18) 0.0290(6) Uani 1 1 d . . . C8 C 0.7841(3) -0.0025(3) 0.6094(3) 0.0317(9) Uani 1 1 d . . . H8 H 0.7791 0.0691 0.5859 0.038 Uiso 1 1 calc R . . C9 C 0.6958(3) -0.0311(3) 0.5910(3) 0.0361(9) Uani 1 1 d . . . H9A H 0.6996 -0.1010 0.6116 0.054 Uiso 1 1 calc R . . H9B H 0.6894 -0.0011 0.5234 0.054 Uiso 1 1 calc R . . H9C H 0.6412 -0.0099 0.6259 0.054 Uiso 1 1 calc R . . C10 C 0.8717(3) -0.0332(4) 0.5575(3) 0.0443(11) Uani 1 1 d . . . H10A H 0.9271 -0.0161 0.5742 0.066 Uiso 1 1 calc R . . H10B H 0.8689 -0.0006 0.4894 0.066 Uiso 1 1 calc R . . H10C H 0.8758 -0.1027 0.5754 0.066 Uiso 1 1 calc R . . O11 O 0.8420(2) -0.29061(19) 0.92243(19) 0.0340(6) Uani 1 1 d . . . C12 C 0.8443(3) -0.3768(3) 1.0033(3) 0.0378(10) Uani 1 1 d . . . H12 H 0.7926 -0.3708 1.0519 0.045 Uiso 1 1 calc R . . C13 C 0.8278(3) -0.4584(3) 0.9780(4) 0.0481(12) Uani 1 1 d . . . H13A H 0.7663 -0.4461 0.9549 0.072 Uiso 1 1 calc R . . H13B H 0.8297 -0.5184 1.0339 0.072 Uiso 1 1 calc R . . H13C H 0.8768 -0.4636 0.9287 0.072 Uiso 1 1 calc R . . C14 C 0.9370(4) -0.3932(3) 1.0429(4) 0.0514(12) Uani 1 1 d . . . H14A H 0.9886 -0.3938 0.9942 0.077 Uiso 1 1 calc R . . H14B H 0.9398 -0.4548 1.0969 0.077 Uiso 1 1 calc R . . H14C H 0.9426 -0.3415 1.0633 0.077 Uiso 1 1 calc R . . O15 O 0.96939(19) -0.1918(2) 0.7454(2) 0.0377(7) Uani 1 1 d . . . C16 C 1.0580(3) -0.2108(4) 0.7008(4) 0.0547(13) Uani 1 1 d . . . H16 H 1.0557 -0.1778 0.6312 0.066 Uiso 1 1 calc R . . C17 C 1.1307(4) -0.1693(5) 0.7256(6) 0.093(2) Uani 1 1 d . . . H17A H 1.1118 -0.1015 0.7129 0.139 Uiso 1 1 calc R . . H17B H 1.1904 -0.1751 0.6878 0.139 Uiso 1 1 calc R . . H17C H 1.1382 -0.2039 0.7927 0.139 Uiso 1 1 calc R . . C18 C 1.0775(4) -0.3148(4) 0.7228(6) 0.086(2) Uani 1 1 d . . . H18A H 1.0859 -0.3487 0.7897 0.128 Uiso 1 1 calc R . . H18B H 1.1349 -0.3260 0.6844 0.128 Uiso 1 1 calc R . . H18C H 1.0248 -0.3387 0.7088 0.128 Uiso 1 1 calc R . . O19 O 0.7926(2) 0.10822(19) 0.8769(2) 0.0357(7) Uani 1 1 d . . . C20 C 0.7753(3) 0.1755(3) 0.9207(3) 0.0434(11) Uani 1 1 d . . . H20 H 0.7848 0.1408 0.9887 0.052 Uiso 1 1 calc R . . C21 C 0.8443(5) 0.2512(4) 0.8755(4) 0.0690(17) Uani 1 1 d . . . H21A H 0.9084 0.2205 0.8810 0.104 Uiso 1 1 calc R . . H21B H 0.8336 0.2960 0.9074 0.104 Uiso 1 1 calc R . . H21C H 0.8355 0.2861 0.8088 0.104 Uiso 1 1 calc R . . C22 C 0.6735(4) 0.2166(4) 0.9143(4) 0.0648(15) Uani 1 1 d . . . H22A H 0.6621 0.2478 0.8480 0.097 Uiso 1 1 calc R . . H22B H 0.6607 0.2637 0.9436 0.097 Uiso 1 1 calc R . . H22C H 0.6322 0.1647 0.9473 0.097 Uiso 1 1 calc R . . O23 O 0.9111(2) 0.1139(2) 0.6965(2) 0.0415(7) Uani 1 1 d . . . C24 C 0.9876(4) 0.1603(4) 0.6323(4) 0.0602(14) Uani 1 1 d . . . H24 H 1.0281 0.1119 0.6120 0.072 Uiso 1 1 calc R . . C25 C 0.9486(6) 0.2368(6) 0.5468(5) 0.085(2) Uani 1 1 d . . . H25A H 0.9072 0.2088 0.5225 0.122 Uiso 1 1 calc R . . H25B H 1.0003 0.2635 0.4981 0.122 Uiso 1 1 calc R . . H25C H 0.9129 0.2879 0.5641 0.122 Uiso 1 1 calc R . . C26 C 1.0441(5) 0.1967(5) 0.6778(5) 0.084(2) Uani 1 1 d . . . H26A H 1.0061 0.2455 0.6969 0.126 Uiso 1 1 calc R . . H26B H 1.0981 0.2252 0.6336 0.126 Uiso 1 1 calc R . . H26C H 1.0662 0.1439 0.7335 0.126 Uiso 1 1 calc R . . O27 O 0.78692(18) -0.25132(19) 0.73309(19) 0.0305(6) Uani 1 1 d . . . C28 C 0.7023(3) -0.2858(3) 0.7581(3) 0.0273(8) Uani 1 1 d . . . C29 C 0.6780(3) -0.3561(3) 0.7299(3) 0.0297(8) Uani 1 1 d . . . C30 C 0.5878(3) -0.3858(3) 0.7605(3) 0.0307(9) Uani 1 1 d . . . H30 H 0.5710 -0.4338 0.7431 0.037 Uiso 1 1 calc R . . C31 C 0.5195(3) -0.3490(3) 0.8159(3) 0.0294(8) Uani 1 1 d . . . C32 C 0.5453(3) -0.2802(3) 0.8411(3) 0.0290(8) Uani 1 1 d . . . H32 H 0.5013 -0.2532 0.8777 0.035 Uiso 1 1 calc R . . C33 C 0.6353(3) -0.2499(3) 0.8135(3) 0.0261(8) Uani 1 1 d . . . N34 N 0.6664(2) -0.1757(2) 0.8368(2) 0.0246(7) Uani 1 1 d . . . H34 H 0.6444 -0.1173 0.7929 0.029 Uiso 1 1 calc R . . C35 C 0.6337(3) -0.1731(3) 0.9277(3) 0.0258(8) Uani 1 1 d . . . C36 C 0.6191(3) -0.2567(3) 1.0060(3) 0.0295(8) Uani 1 1 d . . . H36 H 0.6261 -0.3161 0.9986 0.035 Uiso 1 1 calc R . . C37 C 0.5944(3) -0.2555(3) 1.0956(3) 0.0319(9) Uani 1 1 d . . . H37 H 0.5845 -0.3135 1.1489 0.038 Uiso 1 1 calc R . . C38 C 0.5845(3) -0.1692(3) 1.1064(3) 0.0330(9) Uani 1 1 d . . . H38 H 0.5683 -0.1676 1.1672 0.040 Uiso 1 1 calc R . . C39 C 0.5981(3) -0.0855(3) 1.0288(3) 0.0299(8) Uani 1 1 d . . . H39 H 0.5902 -0.0264 1.0368 0.036 Uiso 1 1 calc R . . C40 C 0.6232(3) -0.0855(3) 0.9385(3) 0.0252(8) Uani 1 1 d . . . N41 N 0.6433(2) 0.0024(2) 0.8605(2) 0.0262(7) Uani 1 1 d . . . H41 H 0.6258 0.0453 0.8900 0.031 Uiso 1 1 calc R . . C42 C 0.5808(3) 0.0417(3) 0.7861(3) 0.0259(8) Uani 1 1 d . . . C43 C 0.4985(3) 0.0050(3) 0.7884(3) 0.0279(8) Uani 1 1 d . . . H43 H 0.4804 -0.0521 0.8392 0.034 Uiso 1 1 calc R . . C44 C 0.4418(3) 0.0518(3) 0.7157(3) 0.0300(8) Uani 1 1 d . . . C45 C 0.4691(3) 0.1379(3) 0.6455(3) 0.0316(9) Uani 1 1 d . . . H45 H 0.4285 0.1724 0.5985 0.038 Uiso 1 1 calc R . . C46 C 0.5531(3) 0.1769(3) 0.6399(3) 0.0308(9) Uani 1 1 d . . . C47 C 0.6126(3) 0.1240(3) 0.7096(3) 0.0285(8) Uani 1 1 d . . . O48 O 0.69858(19) 0.14764(18) 0.70840(18) 0.0308(6) Uani 1 1 d . . . C49 C 0.7496(3) -0.3997(3) 0.6710(3) 0.0343(9) Uani 1 1 d . . . C50 C 0.7777(3) -0.3193(3) 0.5753(3) 0.0458(11) Uani 1 1 d . . . H50A H 0.8101 -0.2727 0.5854 0.069 Uiso 1 1 calc R . . H50B H 0.7212 -0.2871 0.5447 0.069 Uiso 1 1 calc R . . H50C H 0.8195 -0.3469 0.5350 0.069 Uiso 1 1 calc R . . C51 C 0.7093(3) -0.4762(3) 0.6510(3) 0.0418(11) Uani 1 1 d . . . H51A H 0.7575 -0.5028 0.6143 0.063 Uiso 1 1 calc R . . H51B H 0.6553 -0.4471 0.6153 0.063 Uiso 1 1 calc R . . H51C H 0.6891 -0.5276 0.7108 0.063 Uiso 1 1 calc R . . C52 C 0.8361(3) -0.4467(4) 0.7229(4) 0.0502(13) Uani 1 1 d . . . H52A H 0.8654 -0.3982 0.7332 0.075 Uiso 1 1 calc R . . H52B H 0.8811 -0.4746 0.6849 0.075 Uiso 1 1 calc R . . H52C H 0.8173 -0.4972 0.7837 0.075 Uiso 1 1 calc R . . C53 C 0.4221(3) -0.3856(3) 0.8420(3) 0.0322(9) Uani 1 1 d . . . C54 C 0.3733(3) -0.3549(3) 0.7532(3) 0.0426(10) Uani 1 1 d . . . H54A H 0.3718 -0.2851 0.7199 0.064 Uiso 1 1 calc R . . H54B H 0.3090 -0.3741 0.7707 0.064 Uiso 1 1 calc R . . H54C H 0.4078 -0.3858 0.7120 0.064 Uiso 1 1 calc R . . C55 C 0.4282(3) -0.4952(3) 0.8908(3) 0.0416(10) Uani 1 1 d . . . H55A H 0.4695 -0.5232 0.8505 0.062 Uiso 1 1 calc R . . H55B H 0.3655 -0.5173 0.9020 0.062 Uiso 1 1 calc R . . H55C H 0.4536 -0.5153 0.9511 0.062 Uiso 1 1 calc R . . C56 C 0.3602(3) -0.3446(3) 0.9098(3) 0.0415(10) Uani 1 1 d . . . H56A H 0.3903 -0.3632 0.9673 0.062 Uiso 1 1 calc R . . H56B H 0.2986 -0.3700 0.9260 0.062 Uiso 1 1 calc R . . H56C H 0.3525 -0.2745 0.8791 0.062 Uiso 1 1 calc R . . C57 C 0.5789(3) 0.2730(3) 0.5626(3) 0.0359(9) Uani 1 1 d . . . C58 C 0.6689(3) 0.2575(3) 0.5006(3) 0.0438(11) Uani 1 1 d . . . H58A H 0.7215 0.2336 0.5388 0.066 Uiso 1 1 calc R . . H58B H 0.6826 0.3185 0.4486 0.066 Uiso 1 1 calc R . . H58C H 0.6596 0.2107 0.4752 0.066 Uiso 1 1 calc R . . C59 C 0.5016(3) 0.3214(3) 0.4978(3) 0.0426(11) Uani 1 1 d . . . H59A H 0.4916 0.2801 0.4662 0.064 Uiso 1 1 calc R . . H59B H 0.5205 0.3832 0.4505 0.064 Uiso 1 1 calc R . . H59C H 0.4433 0.3317 0.5353 0.064 Uiso 1 1 calc R . . C60 C 0.5952(4) 0.3412(3) 0.6078(3) 0.0477(12) Uani 1 1 d . . . H60A H 0.5368 0.3543 0.6437 0.072 Uiso 1 1 calc R . . H60B H 0.6153 0.4014 0.5584 0.072 Uiso 1 1 calc R . . H60C H 0.6440 0.3114 0.6502 0.072 Uiso 1 1 calc R . . C61 C 0.3546(3) 0.0072(3) 0.7121(3) 0.0368(9) Uani 1 1 d . . . C62 C 0.2889(3) 0.0793(3) 0.6446(4) 0.0507(12) Uani 1 1 d . . . H62A H 0.2663 0.1316 0.6658 0.076 Uiso 1 1 calc R . . H62B H 0.2353 0.0473 0.6434 0.076 Uiso 1 1 calc R . . H62C H 0.3226 0.1052 0.5812 0.076 Uiso 1 1 calc R . . C63 C 0.3007(4) -0.0360(4) 0.8105(3) 0.0577(14) Uani 1 1 d . . . H63A H 0.2803 0.0144 0.8348 0.087 Uiso 1 1 calc R . . H63B H 0.3416 -0.0858 0.8529 0.087 Uiso 1 1 calc R . . H63C H 0.2457 -0.0643 0.8066 0.087 Uiso 1 1 calc R . . C64 C 0.3884(4) -0.0733(3) 0.6767(4) 0.0502(12) Uani 1 1 d . . . H64A H 0.3342 -0.1029 0.6731 0.075 Uiso 1 1 calc R . . H64B H 0.4292 -0.1218 0.7204 0.075 Uiso 1 1 calc R . . H64C H 0.4235 -0.0468 0.6141 0.075 Uiso 1 1 calc R . . C65 C 0.9059(6) -0.4785(6) 1.4072(5) 0.106(3) Uiso 1 1 d D . . H65A H 0.9168 -0.4272 1.4260 0.159 Uiso 1 1 calc R . . H65B H 0.9620 -0.5237 1.4134 0.159 Uiso 1 1 calc R . . H65C H 0.8525 -0.5123 1.4479 0.159 Uiso 1 1 calc R . . C66 C 0.8846(8) -0.4354(7) 1.3052(6) 0.150(4) Uiso 1 1 d D . . H66A H 0.8617 -0.4871 1.2932 0.180 Uiso 1 1 calc R . . H66B H 0.9454 -0.4206 1.2656 0.180 Uiso 1 1 calc R . . C67 C 0.8164(5) -0.3469(6) 1.2668(7) 0.140(4) Uiso 1 1 d D . . H67A H 0.8403 -0.2909 1.2701 0.168 Uiso 1 1 calc R . . H67B H 0.8103 -0.3325 1.2000 0.168 Uiso 1 1 calc R . . C68 C 0.7212(6) -0.3656(6) 1.3252(7) 0.135(3) Uiso 1 1 d D . . H68A H 0.6758 -0.3094 1.2993 0.162 Uiso 1 1 calc R . . H68B H 0.7266 -0.3755 1.3910 0.162 Uiso 1 1 calc R . . C69 C 0.6863(7) -0.4541(7) 1.3234(9) 0.176(5) Uiso 1 1 d D . . H69A H 0.6677 -0.4392 1.2609 0.264 Uiso 1 1 calc R . . H69B H 0.6321 -0.4737 1.3711 0.264 Uiso 1 1 calc R . . H69C H 0.7365 -0.5064 1.3370 0.264 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 Zr1 0.0244(2) 0.0285(2) 0.0325(2) -0.01352(17) -0.00326(15) -0.00334(15) Zr2 0.0293(2) 0.0279(2) 0.0299(2) -0.01171(17) -0.00432(16) -0.00573(16) O3 0.0295(15) 0.0334(14) 0.0335(14) -0.0160(13) -0.0079(12) -0.0033(12) C4 0.039(2) 0.038(2) 0.037(2) -0.0136(19) -0.0171(19) -0.0019(19) C5 0.041(3) 0.053(3) 0.049(3) -0.024(2) -0.014(2) -0.007(2) C6 0.052(3) 0.051(3) 0.034(2) -0.013(2) -0.010(2) -0.004(2) O7 0.0324(15) 0.0297(14) 0.0269(13) -0.0128(12) -0.0018(11) -0.0058(11) C8 0.038(2) 0.030(2) 0.028(2) -0.0107(17) -0.0027(17) -0.0046(17) C9 0.040(2) 0.040(2) 0.032(2) -0.0173(19) -0.0090(18) 0.0000(19) C10 0.041(3) 0.057(3) 0.037(2) -0.023(2) 0.005(2) -0.007(2) O11 0.0360(16) 0.0288(14) 0.0357(15) -0.0113(13) -0.0060(12) 0.0002(12) C12 0.035(2) 0.032(2) 0.036(2) -0.0039(19) -0.0043(18) 0.0021(18) C13 0.038(3) 0.035(2) 0.060(3) -0.006(2) -0.007(2) -0.004(2) C14 0.051(3) 0.045(3) 0.050(3) -0.007(2) -0.018(2) 0.002(2) O15 0.0260(15) 0.0429(16) 0.0466(17) -0.0202(15) -0.0009(13) -0.0053(12) C16 0.029(2) 0.056(3) 0.077(4) -0.028(3) 0.007(2) -0.004(2) C17 0.035(3) 0.096(5) 0.170(8) -0.077(5) -0.007(4) -0.009(3) C18 0.043(3) 0.072(4) 0.158(7) -0.070(5) 0.003(4) 0.003(3) O19 0.0410(17) 0.0336(15) 0.0394(16) -0.0201(13) -0.0083(13) -0.0020(13) C20 0.059(3) 0.042(2) 0.039(2) -0.025(2) -0.007(2) -0.005(2) C21 0.088(4) 0.053(3) 0.081(4) -0.036(3) -0.003(3) -0.027(3) C22 0.066(4) 0.069(4) 0.076(4) -0.050(3) -0.010(3) 0.012(3) O23 0.0395(17) 0.0427(17) 0.0424(17) -0.0129(14) -0.0023(14) -0.0180(14) C24 0.053(3) 0.068(3) 0.054(3) -0.014(3) 0.005(3) -0.027(3) C25 0.075(6) 0.076(8) 0.069(4) 0.024(5) -0.021(4) -0.037(6) C26 0.067(4) 0.097(5) 0.084(5) -0.023(4) -0.004(3) -0.041(4) O27 0.0239(14) 0.0343(14) 0.0375(15) -0.0186(13) 0.0015(11) -0.0070(11) C28 0.026(2) 0.0297(19) 0.0263(19) -0.0098(17) -0.0029(16) -0.0053(16) C29 0.031(2) 0.0273(19) 0.031(2) -0.0115(17) -0.0045(17) -0.0018(16) C30 0.032(2) 0.028(2) 0.034(2) -0.0139(18) -0.0043(17) -0.0052(17) C31 0.029(2) 0.030(2) 0.030(2) -0.0098(17) -0.0076(16) -0.0036(16) C32 0.027(2) 0.030(2) 0.030(2) -0.0123(17) -0.0018(16) -0.0021(16) C33 0.0248(19) 0.0253(18) 0.031(2) -0.0137(17) -0.0038(16) -0.0031(15) N34 0.0252(16) 0.0239(15) 0.0261(16) -0.0107(14) -0.0033(13) -0.0032(13) C35 0.0215(19) 0.031(2) 0.0264(19) -0.0133(17) -0.0033(15) 0.0007(15) C36 0.029(2) 0.0253(19) 0.033(2) -0.0099(17) -0.0040(17) -0.0024(16) C37 0.034(2) 0.030(2) 0.0262(19) -0.0058(17) -0.0014(17) -0.0040(17) C38 0.037(2) 0.037(2) 0.027(2) -0.0141(18) -0.0045(17) -0.0018(18) C39 0.031(2) 0.029(2) 0.032(2) -0.0146(18) -0.0033(17) -0.0003(16) C40 0.0233(19) 0.0263(19) 0.0271(19) -0.0114(16) -0.0044(15) -0.0010(15) N41 0.0284(17) 0.0249(16) 0.0259(16) -0.0104(14) -0.0046(13) -0.0014(13) C42 0.029(2) 0.0264(19) 0.0241(18) -0.0119(16) -0.0053(16) 0.0012(16) C43 0.032(2) 0.0285(19) 0.0248(19) -0.0129(17) 0.0014(16) -0.0042(16) C44 0.031(2) 0.033(2) 0.029(2) -0.0160(18) -0.0049(17) 0.0003(17) C45 0.035(2) 0.032(2) 0.030(2) -0.0125(18) -0.0088(17) -0.0010(17) C46 0.034(2) 0.031(2) 0.0254(19) -0.0097(17) 0.0002(16) -0.0028(17) C47 0.033(2) 0.0267(19) 0.029(2) -0.0134(17) -0.0029(16) -0.0028(16) O48 0.0314(15) 0.0300(14) 0.0307(14) -0.0094(12) -0.0027(12) -0.0097(12) C49 0.031(2) 0.037(2) 0.040(2) -0.021(2) 0.0007(18) -0.0070(18) C50 0.051(3) 0.051(3) 0.043(3) -0.028(2) 0.011(2) -0.015(2) C51 0.042(3) 0.042(2) 0.053(3) -0.032(2) 0.005(2) -0.006(2) C52 0.030(2) 0.058(3) 0.078(4) -0.046(3) -0.004(2) 0.005(2) C53 0.029(2) 0.033(2) 0.035(2) -0.0122(18) 0.0006(17) -0.0093(17) C54 0.037(2) 0.043(2) 0.046(3) -0.011(2) -0.012(2) -0.008(2) C55 0.041(3) 0.031(2) 0.051(3) -0.012(2) -0.006(2) -0.0096(19) C56 0.032(2) 0.044(2) 0.053(3) -0.025(2) 0.006(2) -0.0122(19) C57 0.040(2) 0.033(2) 0.032(2) -0.0082(18) -0.0068(18) -0.0036(18) C58 0.042(3) 0.042(2) 0.037(2) -0.004(2) -0.004(2) -0.007(2) C59 0.046(3) 0.038(2) 0.032(2) 0.0002(19) -0.008(2) -0.002(2) C60 0.066(3) 0.027(2) 0.046(3) -0.006(2) -0.010(2) -0.011(2) C61 0.032(2) 0.040(2) 0.037(2) -0.011(2) -0.0067(18) -0.0086(18) C62 0.039(3) 0.048(3) 0.065(3) -0.018(3) -0.018(2) -0.003(2) C63 0.040(3) 0.089(4) 0.043(3) -0.018(3) -0.002(2) -0.029(3) C64 0.048(3) 0.046(3) 0.065(3) -0.024(3) -0.021(2) -0.006(2) _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 Zr1 O15 1.914(3) . ? Zr1 O11 1.924(3) . ? Zr1 O27 2.056(3) . ? Zr1 O3 2.173(2) . ? Zr1 O7 2.197(3) . ? Zr1 N34 2.522(3) . ? Zr1 Zr2 3.5341(5) . ? Zr2 O23 1.910(3) . ? Zr2 O19 1.949(3) . ? Zr2 O48 2.058(3) . ? Zr2 O3 2.118(3) . ? Zr2 O7 2.199(2) . ? Zr2 N41 2.556(3) . ? O3 C4 1.465(5) . ? C4 C6 1.511(6) . ? C4 C5 1.513(6) . ? C4 H4 1.0000 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? O7 C8 1.448(4) . ? C8 C9 1.513(6) . ? C8 C10 1.515(6) . ? C8 H8 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? O11 C12 1.412(5) . ? C12 C13 1.510(6) . ? C12 C14 1.514(6) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? O15 C16 1.411(5) . ? C16 C17 1.476(7) . ? C16 C18 1.480(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O19 C20 1.422(5) . ? C20 C21 1.511(7) . ? C20 C22 1.521(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? O23 C24 1.425(6) . ? C24 C26 1.454(8) . ? C24 C25 1.505(9) . ? C24 H24 1.0000 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O27 C28 1.341(5) . ? C28 C33 1.398(5) . ? C28 C29 1.417(5) . ? C29 C30 1.392(6) . ? C29 C49 1.536(5) . ? C30 C31 1.416(5) . ? C30 H30 0.9500 . ? C31 C32 1.375(5) . ? C31 C53 1.526(5) . ? C32 C33 1.390(5) . ? C32 H32 0.9500 . ? C33 N34 1.467(4) . ? N34 C35 1.435(5) . ? N34 H34 0.9300 . ? C35 C36 1.382(5) . ? C35 C40 1.401(5) . ? C36 C37 1.394(5) . ? C36 H36 0.9500 . ? C37 C38 1.381(5) . ? C37 H37 0.9500 . ? C38 C39 1.374(6) . ? C38 H38 0.9500 . ? C39 C40 1.397(5) . ? C39 H39 0.9500 . ? C40 N41 1.433(5) . ? N41 C42 1.465(5) . ? N41 H41 0.9300 . ? C42 C43 1.377(5) . ? C42 C47 1.414(5) . ? C43 C44 1.396(5) . ? C43 H43 0.9500 . ? C44 C45 1.393(6) . ? C44 C61 1.537(6) . ? C45 C46 1.404(6) . ? C45 H45 0.9500 . ? C46 C47 1.406(5) . ? C46 C57 1.531(6) . ? C47 O48 1.341(5) . ? C49 C52 1.531(6) . ? C49 C51 1.533(5) . ? C49 C50 1.542(6) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.528(6) . ? C53 C55 1.533(6) . ? C53 C56 1.545(6) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C59 1.532(6) . ? C57 C60 1.534(6) . ? C57 C58 1.544(6) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.523(6) . ? C61 C63 1.532(6) . ? C61 C64 1.533(6) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.522(13) . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.525(15) . ? C66 H66A 0.9900 . ? C66 H66B 0.9900 . ? C67 C68 1.522(13) . ? C67 H67A 0.9900 . ? C67 H67B 0.9900 . ? C68 C69 1.522(17) . ? C68 H68A 0.9900 . ? C68 H68B 0.9900 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 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 O15 Zr1 O11 103.86(12) . . ? O15 Zr1 O27 96.92(11) . . ? O11 Zr1 O27 97.07(11) . . ? O15 Zr1 O3 99.39(11) . . ? O11 Zr1 O3 91.34(11) . . ? O27 Zr1 O3 159.28(10) . . ? O15 Zr1 O7 100.29(11) . . ? O11 Zr1 O7 151.91(11) . . ? O27 Zr1 O7 94.02(10) . . ? O3 Zr1 O7 70.59(9) . . ? O15 Zr1 N34 165.05(11) . . ? O11 Zr1 N34 85.36(11) . . ? O27 Zr1 N34 69.94(10) . . ? O3 Zr1 N34 92.03(10) . . ? O7 Zr1 N34 74.36(10) . . ? O15 Zr1 Zr2 102.30(9) . . ? O11 Zr1 Zr2 122.50(8) . . ? O27 Zr1 Zr2 129.11(8) . . ? O3 Zr1 Zr2 34.06(7) . . ? O7 Zr1 Zr2 36.52(6) . . ? N34 Zr1 Zr2 81.86(7) . . ? O23 Zr2 O19 103.42(12) . . ? O23 Zr2 O48 99.83(12) . . ? O19 Zr2 O48 95.16(11) . . ? O23 Zr2 O3 106.53(12) . . ? O19 Zr2 O3 95.59(11) . . ? O48 Zr2 O3 148.27(10) . . ? O23 Zr2 O7 94.70(11) . . ? O19 Zr2 O7 160.30(11) . . ? O48 Zr2 O7 89.20(10) . . ? O3 Zr2 O7 71.56(10) . . ? O23 Zr2 N41 167.63(11) . . ? O19 Zr2 N41 81.54(11) . . ? O48 Zr2 N41 68.23(10) . . ? O3 Zr2 N41 83.98(10) . . ? O7 Zr2 N41 82.28(10) . . ? O23 Zr2 Zr1 103.41(9) . . ? O19 Zr2 Zr1 129.07(8) . . ? O48 Zr2 Zr1 121.52(7) . . ? O3 Zr2 Zr1 35.08(7) . . ? O7 Zr2 Zr1 36.49(7) . . ? N41 Zr2 Zr1 81.31(7) . . ? C4 O3 Zr2 128.3(2) . . ? C4 O3 Zr1 117.8(2) . . ? Zr2 O3 Zr1 110.86(11) . . ? O3 C4 C6 109.7(4) . . ? O3 C4 C5 110.1(3) . . ? C6 C4 C5 114.0(4) . . ? O3 C4 H4 107.6 . . ? C6 C4 H4 107.6 . . ? C5 C4 H4 107.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C8 O7 Zr1 129.0(2) . . ? C8 O7 Zr2 120.8(2) . . ? Zr1 O7 Zr2 106.99(11) . . ? O7 C8 C9 111.1(3) . . ? O7 C8 C10 110.1(3) . . ? C9 C8 C10 112.5(3) . . ? O7 C8 H8 107.6 . . ? C9 C8 H8 107.6 . . ? C10 C8 H8 107.6 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 O11 Zr1 171.7(3) . . ? O11 C12 C13 109.2(4) . . ? O11 C12 C14 109.7(4) . . ? C13 C12 C14 112.1(4) . . ? O11 C12 H12 108.6 . . ? C13 C12 H12 108.6 . . ? C14 C12 H12 108.6 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 O15 Zr1 169.6(3) . . ? O15 C16 C17 109.9(5) . . ? O15 C16 C18 110.5(4) . . ? C17 C16 C18 113.6(5) . . ? O15 C16 H16 107.5 . . ? C17 C16 H16 107.5 . . ? C18 C16 H16 107.5 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 O19 Zr2 159.9(3) . . ? O19 C20 C21 109.7(4) . . ? O19 C20 C22 108.5(4) . . ? C21 C20 C22 113.2(5) . . ? O19 C20 H20 108.4 . . ? C21 C20 H20 108.4 . . ? C22 C20 H20 108.4 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 O23 Zr2 177.4(3) . . ? O23 C24 C26 110.8(5) . . ? O23 C24 C25 108.2(5) . . ? C26 C24 C25 113.4(6) . . ? O23 C24 H24 108.1 . . ? C26 C24 H24 108.1 . . ? C25 C24 H24 108.1 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 O27 Zr1 124.8(2) . . ? O27 C28 C33 118.3(3) . . ? O27 C28 C29 122.8(3) . . ? C33 C28 C29 118.9(3) . . ? C30 C29 C28 117.1(3) . . ? C30 C29 C49 121.8(3) . . ? C28 C29 C49 121.1(3) . . ? C29 C30 C31 124.1(4) . . ? C29 C30 H30 118.0 . . ? C31 C30 H30 118.0 . . ? C32 C31 C30 117.1(4) . . ? C32 C31 C53 124.2(3) . . ? C30 C31 C53 118.7(3) . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32 119.7 . . ? C33 C32 H32 119.7 . . ? C32 C33 C28 122.1(3) . . ? C32 C33 N34 123.1(3) . . ? C28 C33 N34 114.7(3) . . ? C35 N34 C33 118.3(3) . . ? C35 N34 Zr1 113.3(2) . . ? C33 N34 Zr1 106.3(2) . . ? C35 N34 H34 106.0 . . ? C33 N34 H34 106.0 . . ? Zr1 N34 H34 106.0 . . ? C36 C35 C40 119.4(3) . . ? C36 C35 N34 120.9(3) . . ? C40 C35 N34 119.5(3) . . ? C35 C36 C37 121.2(3) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C38 C37 C36 119.3(4) . . ? C38 C37 H37 120.3 . . ? C36 C37 H37 120.3 . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? C38 C39 C40 121.5(3) . . ? C38 C39 H39 119.2 . . ? C40 C39 H39 119.2 . . ? C39 C40 C35 118.6(3) . . ? C39 C40 N41 119.7(3) . . ? C35 C40 N41 121.6(3) . . ? C40 N41 C42 118.8(3) . . ? C40 N41 Zr2 127.1(2) . . ? C42 N41 Zr2 105.6(2) . . ? C40 N41 H41 99.7 . . ? C42 N41 H41 99.7 . . ? Zr2 N41 H41 99.7 . . ? C43 C42 C47 121.9(3) . . ? C43 C42 N41 125.0(3) . . ? C47 C42 N41 113.1(3) . . ? C42 C43 C44 119.9(4) . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 117.6(4) . . ? C45 C44 C61 121.6(4) . . ? C43 C44 C61 120.7(4) . . ? C44 C45 C46 124.1(4) . . ? C44 C45 H45 118.0 . . ? C46 C45 H45 118.0 . . ? C45 C46 C47 116.9(4) . . ? C45 C46 C57 122.1(4) . . ? C47 C46 C57 121.0(4) . . ? O48 C47 C46 123.5(4) . . ? O48 C47 C42 117.5(3) . . ? C46 C47 C42 118.9(4) . . ? C47 O48 Zr2 125.8(2) . . ? C52 C49 C51 107.9(4) . . ? C52 C49 C29 110.2(3) . . ? C51 C49 C29 112.2(3) . . ? C52 C49 C50 110.3(4) . . ? C51 C49 C50 107.6(3) . . ? C29 C49 C50 108.6(3) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C31 C53 C54 109.7(3) . . ? C31 C53 C55 111.0(3) . . ? C54 C53 C55 108.9(3) . . ? C31 C53 C56 111.3(3) . . ? C54 C53 C56 108.0(4) . . ? C55 C53 C56 107.7(3) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C46 C57 C59 112.3(4) . . ? C46 C57 C60 109.5(3) . . ? C59 C57 C60 108.0(4) . . ? C46 C57 C58 109.8(3) . . ? C59 C57 C58 107.6(3) . . ? C60 C57 C58 109.7(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C63 109.4(4) . . ? C62 C61 C64 108.0(4) . . ? C63 C61 C64 108.6(4) . . ? C62 C61 C44 112.4(4) . . ? C63 C61 C44 110.9(3) . . ? C64 C61 C44 107.5(3) . . ? 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 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 H65A 109.5 . . ? C66 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C66 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C65 C66 C67 122.7(9) . . ? C65 C66 H66A 106.7 . . ? C67 C66 H66A 106.7 . . ? C65 C66 H66B 106.7 . . ? C67 C66 H66B 106.7 . . ? H66A C66 H66B 106.6 . . ? C68 C67 C66 109.0(8) . . ? C68 C67 H67A 109.9 . . ? C66 C67 H67A 109.9 . . ? C68 C67 H67B 109.9 . . ? C66 C67 H67B 109.9 . . ? H67A C67 H67B 108.3 . . ? C67 C68 C69 109.9(8) . . ? C67 C68 H68A 109.7 . . ? C69 C68 H68A 109.7 . . ? C67 C68 H68B 109.7 . . ? C69 C68 H68B 109.7 . . ? H68A C68 H68B 108.2 . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 1.151 _refine_diff_density_min -0.759 _refine_diff_density_rms 0.087 #========================END===================================