Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Piotr Sobota' _publ_contact_author_email plas@wchuwr.chem.uni.wroc.pl _publ_contact_author_phone '+48-(0-71) 375-7306' loop_ _publ_author_name _publ_author_address 'Katarzyna Krauzy-Dziedzic' ; Faculty of Chemistry University of Wroc\/aw 14 Joliot-Curie St 50-383 Wroc\/aw Poland ; 'Jolanta Ejfler' ; Faculty of Chemistry University of Wroc\/aw 14 Joliot-Curie St 50-383 Wroc\/aw Poland ; 'S\/awomir Szafert' ; Faculty of Chemistry University of Wroc\/aw 14 Joliot-Curie St 50-383 Wroc\/aw Poland ; 'Piotr Sobota' ; Faculty of Chemistry University of Wroc\/aw 14 Joliot-Curie St 50-383 Wroc\/aw Poland ; _publ_section_title ; Titanium and Zirconium Benzofuranoxides. Crystal Structures and Catalytic Properties. ; data_for_complex_1_kkr1 _database_code_depnum_ccdc_archive 'CCDC 629476' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H88 O16 Ti2' _chemical_formula_weight 1401.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1696(7) _cell_length_b 12.8552(6) _cell_length_c 13.0040(7) _cell_angle_alpha 73.920(4) _cell_angle_beta 81.944(4) _cell_angle_gamma 64.201(5) _cell_volume 1759.50(16) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5876 _cell_measurement_theta_min 3 _cell_measurement_theta_max 36 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.322 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 740 _exptl_absorpt_coefficient_mu 0.296 _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 100(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 'Kuma KM-4 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21465 _diffrn_reflns_av_R_equivalents 0.0406 _diffrn_reflns_av_sigmaI/netI 0.0632 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 28.47 _reflns_number_total 8172 _reflns_number_gt 6059 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 1995-2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0441P)^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 8172 _refine_ls_number_parameters 442 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.0994 _refine_ls_goodness_of_fit_ref 1.175 _refine_ls_restrained_S_all 1.175 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti 0.97301(3) 0.49753(3) 0.13081(3) 0.01288(10) Uani 1 1 d . . . O11 O 1.08609(12) 0.41252(11) 0.02443(10) 0.0134(3) Uani 1 1 d . . . O12 O 1.05809(12) 0.19834(11) 0.13219(11) 0.0185(3) Uani 1 1 d . . . O21 O 0.92083(12) 0.64356(11) 0.15952(11) 0.0156(3) Uani 1 1 d . . . O22 O 0.71210(13) 0.64819(12) 0.29572(12) 0.0214(3) Uani 1 1 d . . . O31 O 1.08733(12) 0.41267(11) 0.23275(11) 0.0166(3) Uani 1 1 d . . . O32 O 0.97918(12) 0.34233(12) 0.43554(11) 0.0187(3) Uani 1 1 d . . . O41 O 0.85933(12) 0.44335(12) 0.16796(11) 0.0171(3) Uani 1 1 d . . . O42 O 0.76621(13) 0.42162(12) -0.01074(11) 0.0191(3) Uani 1 1 d . . . C11 C 1.18518(18) 0.30291(16) 0.04670(15) 0.0134(4) Uani 1 1 d . . . C12 C 1.30309(18) 0.29099(17) 0.01475(16) 0.0161(4) Uani 1 1 d . . . H12A H 1.3171 0.3595 -0.0210 0.019 Uiso 1 1 calc R . . C13 C 1.40083(19) 0.17930(18) 0.03478(17) 0.0176(5) Uani 1 1 d . . . H13A H 1.4810 0.1728 0.0133 0.021 Uiso 1 1 calc R . . C14 C 1.38323(19) 0.07705(18) 0.08565(16) 0.0183(5) Uani 1 1 d . . . H14A H 1.4501 0.0009 0.0981 0.022 Uiso 1 1 calc R . . C15 C 1.26589(19) 0.08889(17) 0.11764(16) 0.0156(4) Uani 1 1 d . . . C16 C 1.16890(18) 0.20012(17) 0.09900(15) 0.0147(4) Uani 1 1 d . . . C17 C 1.21376(19) -0.00187(18) 0.16469(18) 0.0216(5) Uani 1 1 d . . . H17A H 1.2604 -0.0617 0.2274 0.026 Uiso 1 1 calc R . . H17B H 1.2132 -0.0431 0.1109 0.026 Uiso 1 1 calc R . . C18 C 1.08226(19) 0.07609(17) 0.19794(17) 0.0179(5) Uani 1 1 d . . . C19 C 1.0747(2) 0.08037(19) 0.31428(17) 0.0248(5) Uani 1 1 d . . . H19A H 0.9907 0.1302 0.3328 0.037 Uiso 1 1 calc R . . H19B H 1.1293 0.1141 0.3250 0.037 Uiso 1 1 calc R . . H19C H 1.0992 -0.0004 0.3601 0.037 Uiso 1 1 calc R . . C110 C 0.9864(2) 0.04400(19) 0.17092(18) 0.0229(5) Uani 1 1 d . . . H11A H 0.9058 0.0966 0.1939 0.034 Uiso 1 1 calc R . . H11B H 1.0034 -0.0388 0.2079 0.034 Uiso 1 1 calc R . . H11C H 0.9876 0.0533 0.0934 0.034 Uiso 1 1 calc R . . C21 C 0.83118(18) 0.74684(17) 0.17768(16) 0.0142(4) Uani 1 1 d . . . C22 C 0.83682(18) 0.85633(17) 0.13041(16) 0.0163(4) Uani 1 1 d . . . H22A H 0.9030 0.8589 0.0830 0.020 Uiso 1 1 calc R . . C23 C 0.74682(19) 0.96166(18) 0.15174(17) 0.0188(5) Uani 1 1 d . . . H23A H 0.7531 1.0349 0.1197 0.023 Uiso 1 1 calc R . . C24 C 0.64793(19) 0.96085(18) 0.21938(17) 0.0202(5) Uani 1 1 d . . . H24A H 0.5867 1.0327 0.2339 0.024 Uiso 1 1 calc R . . C25 C 0.64057(18) 0.85305(18) 0.26523(17) 0.0179(5) Uani 1 1 d . . . C26 C 0.73120(19) 0.74835(17) 0.24452(16) 0.0162(4) Uani 1 1 d . . . C27 C 0.5477(2) 0.82158(18) 0.34071(19) 0.0243(5) Uani 1 1 d . . . H27A H 0.4640 0.8714 0.3136 0.029 Uiso 1 1 calc R . . H27B H 0.5513 0.8312 0.4129 0.029 Uiso 1 1 calc R . . C28 C 0.58708(19) 0.68936(19) 0.34236(18) 0.0235(5) Uani 1 1 d . . . C29 C 0.5099(2) 0.6758(2) 0.2686(2) 0.0431(7) Uani 1 1 d . . . H29A H 0.5373 0.5913 0.2713 0.065 Uiso 1 1 calc R . . H29B H 0.5186 0.7189 0.1951 0.065 Uiso 1 1 calc R . . H29C H 0.4240 0.7087 0.2919 0.065 Uiso 1 1 calc R . . C210 C 0.5939(3) 0.6107(2) 0.4530(2) 0.0527(9) Uani 1 1 d . . . H21A H 0.6193 0.5286 0.4484 0.079 Uiso 1 1 calc R . . H21B H 0.5135 0.6383 0.4887 0.079 Uiso 1 1 calc R . . H21C H 0.6534 0.6140 0.4942 0.079 Uiso 1 1 calc R . . C31 C 1.15404(18) 0.32185(17) 0.31238(16) 0.0147(4) Uani 1 1 d . . . C32 C 1.27932(19) 0.25581(18) 0.29851(17) 0.0185(5) Uani 1 1 d . . . H32A H 1.3186 0.2761 0.2325 0.022 Uiso 1 1 calc R . . C33 C 1.3475(2) 0.16091(19) 0.37970(17) 0.0229(5) Uani 1 1 d . . . H33A H 1.4324 0.1172 0.3684 0.027 Uiso 1 1 calc R . . C34 C 1.2922(2) 0.12979(18) 0.47706(17) 0.0221(5) Uani 1 1 d . . . H34A H 1.3384 0.0648 0.5323 0.026 Uiso 1 1 calc R . . C35 C 1.16847(19) 0.19543(17) 0.49199(16) 0.0176(5) Uani 1 1 d . . . C36 C 1.10147(18) 0.28988(17) 0.41050(16) 0.0153(4) Uani 1 1 d . . . C37 C 1.0818(2) 0.18135(18) 0.58316(17) 0.0216(5) Uani 1 1 d . . . H37A H 1.1137 0.1742 0.6520 0.026 Uiso 1 1 calc R . . H37B H 1.0661 0.1107 0.5885 0.026 Uiso 1 1 calc R . . C38 C 0.9655(2) 0.29764(19) 0.55247(16) 0.0209(5) Uani 1 1 d . . . C39 C 0.9590(2) 0.39238(19) 0.60491(18) 0.0253(5) Uani 1 1 d . . . H39A H 0.8844 0.4648 0.5833 0.038 Uiso 1 1 calc R . . H39B H 1.0304 0.4104 0.5823 0.038 Uiso 1 1 calc R . . H39C H 0.9581 0.3629 0.6829 0.038 Uiso 1 1 calc R . . C310 C 0.8491(2) 0.2783(2) 0.57040(18) 0.0271(5) Uani 1 1 d . . . H31A H 0.7789 0.3551 0.5494 0.041 Uiso 1 1 calc R . . H31B H 0.8405 0.2421 0.6463 0.041 Uiso 1 1 calc R . . H31C H 0.8529 0.2254 0.5271 0.041 Uiso 1 1 calc R . . C41 C 0.78361(18) 0.38740(17) 0.18109(17) 0.0169(5) Uani 1 1 d . . . C42 C 0.74883(19) 0.33830(17) 0.28249(17) 0.0215(5) Uani 1 1 d . . . H42A H 0.7782 0.3434 0.3440 0.026 Uiso 1 1 calc R . . C43 C 0.6713(2) 0.28166(18) 0.29454(18) 0.0248(5) Uani 1 1 d . . . H43A H 0.6488 0.2480 0.3644 0.030 Uiso 1 1 calc R . . C44 C 0.6260(2) 0.27365(18) 0.20543(19) 0.0238(5) Uani 1 1 d . . . H44A H 0.5730 0.2351 0.2140 0.029 Uiso 1 1 calc R . . C45 C 0.66009(19) 0.32298(17) 0.10451(18) 0.0197(5) Uani 1 1 d . . . C46 C 0.73919(18) 0.37757(17) 0.09300(17) 0.0174(5) Uani 1 1 d . . . C47 C 0.6253(2) 0.33515(19) -0.00634(18) 0.0231(5) Uani 1 1 d . . . H47A H 0.5411 0.3964 -0.0225 0.028 Uiso 1 1 calc R . . H47B H 0.6319 0.2585 -0.0150 0.028 Uiso 1 1 calc R . . C48 C 0.72025(19) 0.37350(18) -0.07861(17) 0.0189(5) Uani 1 1 d . . . C49 C 0.8289(2) 0.26696(18) -0.10476(18) 0.0230(5) Uani 1 1 d . . . H49A H 0.8877 0.2937 -0.1501 0.035 Uiso 1 1 calc R . . H49B H 0.8014 0.2269 -0.1428 0.035 Uiso 1 1 calc R . . H49C H 0.8679 0.2114 -0.0383 0.035 Uiso 1 1 calc R . . C410 C 0.6696(2) 0.47212(19) -0.17725(18) 0.0266(5) Uani 1 1 d . . . H41A H 0.7356 0.4910 -0.2175 0.040 Uiso 1 1 calc R . . H41B H 0.6073 0.5431 -0.1561 0.040 Uiso 1 1 calc R . . H41C H 0.6328 0.4464 -0.2223 0.040 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 Ti 0.01435(19) 0.01162(18) 0.01194(18) -0.00320(14) -0.00033(14) -0.00454(15) O11 0.0146(7) 0.0095(6) 0.0123(7) -0.0020(5) -0.0015(6) -0.0017(6) O12 0.0137(7) 0.0115(7) 0.0251(8) 0.0006(6) -0.0018(6) -0.0032(6) O21 0.0154(7) 0.0121(7) 0.0189(8) -0.0064(6) -0.0032(6) -0.0031(6) O22 0.0171(8) 0.0167(7) 0.0286(9) -0.0053(6) 0.0033(6) -0.0068(6) O31 0.0199(8) 0.0140(7) 0.0120(7) -0.0014(6) -0.0018(6) -0.0043(6) O32 0.0180(8) 0.0209(8) 0.0131(7) -0.0023(6) 0.0001(6) -0.0055(7) O41 0.0192(8) 0.0173(7) 0.0179(8) -0.0044(6) 0.0011(6) -0.0107(6) O42 0.0238(8) 0.0215(8) 0.0184(8) -0.0061(6) -0.0002(6) -0.0147(7) C11 0.0149(10) 0.0097(9) 0.0120(10) -0.0037(8) -0.0023(8) -0.0007(8) C12 0.0183(11) 0.0146(10) 0.0158(10) -0.0038(8) -0.0009(8) -0.0072(9) C13 0.0118(10) 0.0197(11) 0.0205(11) -0.0047(9) 0.0017(8) -0.0064(9) C14 0.0175(11) 0.0129(10) 0.0194(11) -0.0032(8) -0.0037(9) -0.0013(9) C15 0.0185(11) 0.0110(10) 0.0166(11) -0.0026(8) -0.0031(9) -0.0053(9) C16 0.0132(10) 0.0173(10) 0.0134(10) -0.0044(8) -0.0007(8) -0.0055(9) C17 0.0184(11) 0.0132(10) 0.0287(12) -0.0015(9) -0.0033(9) -0.0038(9) C18 0.0200(11) 0.0096(9) 0.0217(11) 0.0001(8) -0.0010(9) -0.0061(9) C19 0.0335(13) 0.0175(11) 0.0239(12) -0.0010(9) -0.0054(10) -0.0120(10) C110 0.0233(12) 0.0203(11) 0.0263(12) -0.0032(9) -0.0035(10) -0.0108(10) C21 0.0123(10) 0.0138(10) 0.0168(11) -0.0072(8) -0.0042(8) -0.0023(8) C22 0.0158(11) 0.0180(10) 0.0156(11) -0.0049(8) -0.0017(8) -0.0066(9) C23 0.0202(11) 0.0133(10) 0.0229(12) -0.0043(9) -0.0051(9) -0.0056(9) C24 0.0167(11) 0.0156(10) 0.0260(12) -0.0102(9) -0.0050(9) -0.0003(9) C25 0.0146(11) 0.0202(11) 0.0208(11) -0.0096(9) -0.0018(9) -0.0057(9) C26 0.0176(11) 0.0136(10) 0.0173(11) -0.0043(8) -0.0044(9) -0.0049(9) C27 0.0206(12) 0.0234(12) 0.0290(13) -0.0100(10) 0.0045(10) -0.0085(10) C28 0.0163(11) 0.0216(11) 0.0310(13) -0.0067(10) 0.0062(10) -0.0080(10) C29 0.0251(14) 0.0388(15) 0.074(2) -0.0303(15) 0.0007(13) -0.0118(12) C210 0.0480(18) 0.0354(15) 0.0422(17) 0.0027(13) 0.0194(14) -0.0012(14) C31 0.0191(11) 0.0118(10) 0.0141(10) -0.0031(8) -0.0050(8) -0.0058(9) C32 0.0193(11) 0.0201(11) 0.0156(11) -0.0038(9) 0.0004(9) -0.0084(9) C33 0.0172(11) 0.0246(12) 0.0226(12) -0.0070(9) -0.0026(9) -0.0034(10) C34 0.0245(12) 0.0171(11) 0.0196(12) 0.0008(9) -0.0088(9) -0.0048(10) C35 0.0228(11) 0.0153(10) 0.0155(11) -0.0033(8) -0.0033(9) -0.0080(9) C36 0.0165(11) 0.0139(10) 0.0169(11) -0.0071(8) -0.0023(8) -0.0051(9) C37 0.0270(12) 0.0214(11) 0.0150(11) -0.0002(9) -0.0043(9) -0.0101(10) C38 0.0246(12) 0.0245(11) 0.0115(10) -0.0011(9) -0.0009(9) -0.0103(10) C39 0.0326(13) 0.0244(12) 0.0188(12) -0.0047(9) -0.0007(10) -0.0121(11) C310 0.0273(13) 0.0302(13) 0.0221(12) -0.0008(10) -0.0016(10) -0.0134(11) C41 0.0139(10) 0.0136(10) 0.0237(12) -0.0055(9) 0.0021(9) -0.0062(9) C42 0.0229(12) 0.0175(11) 0.0200(12) -0.0040(9) 0.0025(9) -0.0057(10) C43 0.0266(12) 0.0184(11) 0.0252(12) -0.0016(9) 0.0076(10) -0.0103(10) C44 0.0172(11) 0.0182(11) 0.0353(14) -0.0066(10) 0.0052(10) -0.0084(10) C45 0.0148(11) 0.0134(10) 0.0315(13) -0.0080(9) 0.0003(9) -0.0052(9) C46 0.0152(11) 0.0157(10) 0.0206(11) -0.0053(9) 0.0035(9) -0.0064(9) C47 0.0203(12) 0.0214(11) 0.0326(13) -0.0099(10) 0.0004(10) -0.0114(10) C48 0.0184(11) 0.0183(11) 0.0247(12) -0.0092(9) -0.0025(9) -0.0091(9) C49 0.0260(12) 0.0184(11) 0.0236(12) -0.0063(9) 0.0007(10) -0.0080(10) C410 0.0245(12) 0.0235(12) 0.0310(13) -0.0044(10) -0.0077(10) -0.0086(10) _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 Ti O41 1.7599(14) . ? Ti O31 1.8105(14) . ? Ti O21 1.8305(13) . ? Ti O11 1.9992(13) . ? Ti O11 2.0783(13) 2_765 ? Ti Ti 3.3615(7) 2_765 ? O11 C11 1.384(2) . ? O11 Ti 2.0783(13) 2_765 ? O12 C16 1.365(2) . ? O12 C18 1.487(2) . ? O21 C21 1.360(2) . ? O22 C26 1.377(2) . ? O22 C28 1.477(2) . ? O31 C31 1.355(2) . ? O32 C36 1.374(2) . ? O32 C38 1.483(2) . ? O41 C41 1.364(2) . ? O42 C46 1.365(2) . ? O42 C48 1.489(2) . ? C11 C12 1.390(3) . ? C11 C16 1.393(3) . ? C12 C13 1.392(3) . ? C13 C14 1.391(3) . ? C14 C15 1.384(3) . ? C15 C16 1.384(3) . ? C15 C17 1.509(3) . ? C17 C18 1.550(3) . ? C18 C110 1.506(3) . ? C18 C19 1.518(3) . ? C21 C26 1.389(3) . ? C21 C22 1.399(3) . ? C22 C23 1.394(3) . ? C23 C24 1.390(3) . ? C24 C25 1.385(3) . ? C25 C26 1.388(3) . ? C25 C27 1.507(3) . ? C27 C28 1.547(3) . ? C28 C210 1.501(3) . ? C28 C29 1.523(3) . ? C31 C36 1.384(3) . ? C31 C32 1.400(3) . ? C32 C33 1.394(3) . ? C33 C34 1.389(3) . ? C34 C35 1.386(3) . ? C35 C36 1.389(3) . ? C35 C37 1.499(3) . ? C37 C38 1.544(3) . ? C38 C310 1.518(3) . ? C38 C39 1.522(3) . ? C41 C42 1.390(3) . ? C41 C46 1.391(3) . ? C42 C43 1.393(3) . ? C43 C44 1.397(3) . ? C44 C45 1.383(3) . ? C45 C46 1.390(3) . ? C45 C47 1.507(3) . ? C47 C48 1.548(3) . ? C48 C410 1.508(3) . ? C48 C49 1.515(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O41 Ti O31 105.54(6) . . ? O41 Ti O21 110.40(6) . . ? O31 Ti O21 98.10(6) . . ? O41 Ti O11 108.02(6) . . ? O31 Ti O11 90.63(6) . . ? O21 Ti O11 136.46(6) . . ? O41 Ti O11 95.92(6) . 2_765 ? O31 Ti O11 154.25(6) . 2_765 ? O21 Ti O11 87.31(6) . 2_765 ? O11 Ti O11 68.96(6) . 2_765 ? O41 Ti Ti 104.34(5) . 2_765 ? O31 Ti Ti 124.29(5) . 2_765 ? O21 Ti Ti 113.71(5) . 2_765 ? O11 Ti Ti 35.24(4) . 2_765 ? O11 Ti Ti 33.71(4) 2_765 2_765 ? C11 O11 Ti 126.74(11) . . ? C11 O11 Ti 121.96(11) . 2_765 ? Ti O11 Ti 111.04(6) . 2_765 ? C16 O12 C18 106.92(14) . . ? C21 O21 Ti 151.95(13) . . ? C26 O22 C28 107.00(15) . . ? C31 O31 Ti 159.32(13) . . ? C36 O32 C38 106.72(15) . . ? C41 O41 Ti 167.77(13) . . ? C46 O42 C48 106.81(15) . . ? O11 C11 C12 121.43(17) . . ? O11 C11 C16 120.67(17) . . ? C12 C11 C16 117.86(17) . . ? C11 C12 C13 120.43(18) . . ? C14 C13 C12 121.19(19) . . ? C15 C14 C13 118.39(18) . . ? C14 C15 C16 120.42(18) . . ? C14 C15 C17 132.01(18) . . ? C16 C15 C17 107.33(17) . . ? O12 C16 C15 114.18(17) . . ? O12 C16 C11 124.08(17) . . ? C15 C16 C11 121.69(18) . . ? C15 C17 C18 102.36(16) . . ? O12 C18 C110 106.89(16) . . ? O12 C18 C19 106.89(16) . . ? C110 C18 C19 112.63(18) . . ? O12 C18 C17 104.52(16) . . ? C110 C18 C17 113.78(18) . . ? C19 C18 C17 111.44(18) . . ? O21 C21 C26 121.75(18) . . ? O21 C21 C22 121.09(18) . . ? C26 C21 C22 117.15(18) . . ? C23 C22 C21 121.01(19) . . ? C24 C23 C22 120.78(19) . . ? C25 C24 C23 118.61(19) . . ? C24 C25 C26 120.3(2) . . ? C24 C25 C27 131.89(19) . . ? C26 C25 C27 107.82(18) . . ? O22 C26 C25 113.91(18) . . ? O22 C26 C21 123.95(18) . . ? C25 C26 C21 122.14(19) . . ? C25 C27 C28 102.80(17) . . ? O22 C28 C210 106.80(18) . . ? O22 C28 C29 105.72(19) . . ? C210 C28 C29 112.6(2) . . ? O22 C28 C27 105.90(16) . . ? C210 C28 C27 113.6(2) . . ? C29 C28 C27 111.58(19) . . ? O31 C31 C36 121.63(18) . . ? O31 C31 C32 121.24(18) . . ? C36 C31 C32 117.14(18) . . ? C33 C32 C31 121.2(2) . . ? C34 C33 C32 120.5(2) . . ? C35 C34 C33 118.71(19) . . ? C34 C35 C36 120.28(19) . . ? C34 C35 C37 131.82(19) . . ? C36 C35 C37 107.80(18) . . ? O32 C36 C31 124.41(18) . . ? O32 C36 C35 113.36(18) . . ? C31 C36 C35 122.13(19) . . ? C35 C37 C38 102.71(16) . . ? O32 C38 C310 106.96(17) . . ? O32 C38 C39 106.84(16) . . ? C310 C38 C39 112.39(19) . . ? O32 C38 C37 104.77(16) . . ? C310 C38 C37 113.38(18) . . ? C39 C38 C37 111.86(18) . . ? O41 C41 C42 121.20(19) . . ? O41 C41 C46 120.77(18) . . ? C42 C41 C46 118.0(2) . . ? C41 C42 C43 120.5(2) . . ? C42 C43 C44 120.9(2) . . ? C45 C44 C43 118.6(2) . . ? C44 C45 C46 120.2(2) . . ? C44 C45 C47 132.6(2) . . ? C46 C45 C47 107.16(18) . . ? O42 C46 C45 114.25(19) . . ? O42 C46 C41 124.02(19) . . ? C45 C46 C41 121.72(19) . . ? C45 C47 C48 102.78(17) . . ? O42 C48 C410 106.48(16) . . ? O42 C48 C49 106.52(17) . . ? C410 C48 C49 112.10(18) . . ? O42 C48 C47 104.62(16) . . ? C410 C48 C47 115.14(18) . . ? C49 C48 C47 111.19(17) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O41 Ti O11 C11 -84.81(16) . . . . ? O31 Ti O11 C11 21.77(15) . . . . ? O21 Ti O11 C11 124.24(15) . . . . ? O11 Ti O11 C11 -174.30(19) 2_765 . . . ? Ti Ti O11 C11 -174.30(19) 2_765 . . . ? O41 Ti O11 Ti 89.49(7) . . . 2_765 ? O31 Ti O11 Ti -163.93(7) . . . 2_765 ? O21 Ti O11 Ti -61.46(11) . . . 2_765 ? O11 Ti O11 Ti 0.0 2_765 . . 2_765 ? O41 Ti O21 C21 -21.9(3) . . . . ? O31 Ti O21 C21 -131.9(3) . . . . ? O11 Ti O21 C21 128.5(3) . . . . ? O11 Ti O21 C21 73.4(3) 2_765 . . . ? Ti Ti O21 C21 94.9(3) 2_765 . . . ? O41 Ti O31 C31 23.7(4) . . . . ? O21 Ti O31 C31 137.6(4) . . . . ? O11 Ti O31 C31 -85.2(4) . . . . ? O11 Ti O31 C31 -121.7(4) 2_765 . . . ? Ti Ti O31 C31 -96.4(4) 2_765 . . . ? O31 Ti O41 C41 -98.7(6) . . . . ? O21 Ti O41 C41 156.3(6) . . . . ? O11 Ti O41 C41 -2.8(6) . . . . ? O11 Ti O41 C41 67.0(6) 2_765 . . . ? Ti Ti O41 C41 33.8(6) 2_765 . . . ? Ti O11 C11 C12 -118.34(17) . . . . ? Ti O11 C11 C12 67.9(2) 2_765 . . . ? Ti O11 C11 C16 63.8(2) . . . . ? Ti O11 C11 C16 -109.89(18) 2_765 . . . ? O11 C11 C12 C13 -177.78(18) . . . . ? C16 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 C14 0.9(3) . . . . ? C12 C13 C14 C15 -1.0(3) . . . . ? C13 C14 C15 C16 0.1(3) . . . . ? C13 C14 C15 C17 173.7(2) . . . . ? C18 O12 C16 C15 10.9(2) . . . . ? C18 O12 C16 C11 -171.66(19) . . . . ? C14 C15 C16 O12 178.37(18) . . . . ? C17 C15 C16 O12 3.3(2) . . . . ? C14 C15 C16 C11 0.9(3) . . . . ? C17 C15 C16 C11 -174.14(19) . . . . ? O11 C11 C16 O12 -0.3(3) . . . . ? C12 C11 C16 O12 -178.21(18) . . . . ? O11 C11 C16 C15 176.92(18) . . . . ? C12 C11 C16 C15 -1.0(3) . . . . ? C14 C15 C17 C18 170.5(2) . . . . ? C16 C15 C17 C18 -15.2(2) . . . . ? C16 O12 C18 C110 -140.84(17) . . . . ? C16 O12 C18 C19 98.33(19) . . . . ? C16 O12 C18 C17 -19.9(2) . . . . ? C15 C17 C18 O12 21.0(2) . . . . ? C15 C17 C18 C110 137.21(18) . . . . ? C15 C17 C18 C19 -94.1(2) . . . . ? Ti O21 C21 C26 43.8(4) . . . . ? Ti O21 C21 C22 -137.0(2) . . . . ? O21 C21 C22 C23 -177.97(18) . . . . ? C26 C21 C22 C23 1.3(3) . . . . ? C21 C22 C23 C24 -1.0(3) . . . . ? C22 C23 C24 C25 0.0(3) . . . . ? C23 C24 C25 C26 0.7(3) . . . . ? C23 C24 C25 C27 179.8(2) . . . . ? C28 O22 C26 C25 9.8(2) . . . . ? C28 O22 C26 C21 -170.05(19) . . . . ? C24 C25 C26 O22 179.79(19) . . . . ? C27 C25 C26 O22 0.5(2) . . . . ? C24 C25 C26 C21 -0.4(3) . . . . ? C27 C25 C26 C21 -179.68(19) . . . . ? O21 C21 C26 O22 -1.5(3) . . . . ? C22 C21 C26 O22 179.19(18) . . . . ? O21 C21 C26 C25 178.65(18) . . . . ? C22 C21 C26 C25 -0.6(3) . . . . ? C24 C25 C27 C28 170.9(2) . . . . ? C26 C25 C27 C28 -9.9(2) . . . . ? C26 O22 C28 C210 -136.9(2) . . . . ? C26 O22 C28 C29 103.0(2) . . . . ? C26 O22 C28 C27 -15.5(2) . . . . ? C25 C27 C28 O22 15.2(2) . . . . ? C25 C27 C28 C210 132.1(2) . . . . ? C25 C27 C28 C29 -99.3(2) . . . . ? Ti O31 C31 C36 -63.9(4) . . . . ? Ti O31 C31 C32 115.7(4) . . . . ? O31 C31 C32 C33 -178.74(19) . . . . ? C36 C31 C32 C33 0.9(3) . . . . ? C31 C32 C33 C34 -0.2(3) . . . . ? C32 C33 C34 C35 -0.5(3) . . . . ? C33 C34 C35 C36 0.4(3) . . . . ? C33 C34 C35 C37 176.3(2) . . . . ? C38 O32 C36 C31 -169.95(19) . . . . ? C38 O32 C36 C35 13.4(2) . . . . ? O31 C31 C36 O32 2.4(3) . . . . ? C32 C31 C36 O32 -177.27(18) . . . . ? O31 C31 C36 C35 178.70(18) . . . . ? C32 C31 C36 C35 -0.9(3) . . . . ? C34 C35 C36 O32 176.99(18) . . . . ? C37 C35 C36 O32 0.3(2) . . . . ? C34 C35 C36 C31 0.3(3) . . . . ? C37 C35 C36 C31 -176.45(19) . . . . ? C34 C35 C37 C38 170.7(2) . . . . ? C36 C35 C37 C38 -13.0(2) . . . . ? C36 O32 C38 C310 -141.48(17) . . . . ? C36 O32 C38 C39 97.96(18) . . . . ? C36 O32 C38 C37 -20.9(2) . . . . ? C35 C37 C38 O32 20.3(2) . . . . ? C35 C37 C38 C310 136.53(18) . . . . ? C35 C37 C38 C39 -95.1(2) . . . . ? Ti O41 C41 C42 134.2(6) . . . . ? Ti O41 C41 C46 -45.6(7) . . . . ? O41 C41 C42 C43 179.88(18) . . . . ? C46 C41 C42 C43 -0.3(3) . . . . ? C41 C42 C43 C44 -0.5(3) . . . . ? C42 C43 C44 C45 0.2(3) . . . . ? C43 C44 C45 C46 1.0(3) . . . . ? C43 C44 C45 C47 -177.0(2) . . . . ? C48 O42 C46 C45 -11.5(2) . . . . ? C48 O42 C46 C41 169.79(19) . . . . ? C44 C45 C46 O42 179.46(17) . . . . ? C47 C45 C46 O42 -2.1(2) . . . . ? C44 C45 C46 C41 -1.8(3) . . . . ? C47 C45 C46 C41 176.61(19) . . . . ? O41 C41 C46 O42 -0.1(3) . . . . ? C42 C41 C46 O42 -179.94(18) . . . . ? O41 C41 C46 C45 -178.73(17) . . . . ? C42 C41 C46 C45 1.5(3) . . . . ? C44 C45 C47 C48 -167.8(2) . . . . ? C46 C45 C47 C48 14.0(2) . . . . ? C46 O42 C48 C410 142.00(17) . . . . ? C46 O42 C48 C49 -98.19(18) . . . . ? C46 O42 C48 C47 19.65(19) . . . . ? C45 C47 C48 O42 -20.1(2) . . . . ? C45 C47 C48 C410 -136.65(19) . . . . ? C45 C47 C48 C49 94.5(2) . . . . ? _diffrn_measured_fraction_theta_max 0.918 _diffrn_reflns_theta_full 28.47 _diffrn_measured_fraction_theta_full 0.918 _refine_diff_density_max 0.324 _refine_diff_density_min -0.457 _refine_diff_density_rms 0.056 #===END data_for_complex_2_kkr4 _database_code_depnum_ccdc_archive 'CCDC 629477' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H88 O16 Zr2' _chemical_formula_weight 1343.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 11.1465(5) _cell_length_b 12.1096(7) _cell_length_c 13.1966(8) _cell_angle_alpha 93.782(5) _cell_angle_beta 111.460(5) _cell_angle_gamma 92.187(4) _cell_volume 1650.45(16) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3579 _cell_measurement_theta_min 3 _cell_measurement_theta_max 36 _exptl_crystal_description needles _exptl_crystal_colour colorless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.352 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 704 _exptl_absorpt_coefficient_mu 0.382 _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 100(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 'Kuma KM-4 CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19807 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 28.50 _reflns_number_total 7632 _reflns_number_gt 6169 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD (Oxford Diffraction, 1995-2003)' _computing_cell_refinement 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_data_reduction 'CrysAlis RED (Oxford Diffraction, 1995-2003)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0400P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7632 _refine_ls_number_parameters 411 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0457 _refine_ls_wR_factor_ref 0.0900 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.003 _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 Zr Zr 0.44372(2) 0.42182(2) 0.874620(19) 0.01797(8) Uani 1 1 d . . . O10 O 0.80286(16) 0.26930(17) 0.87371(14) 0.0358(5) Uani 1 1 d . . . O11 O 0.54072(15) 0.31958(13) 0.81645(13) 0.0223(4) Uani 1 1 d . . . O20 O 0.42731(16) 0.18752(13) 1.11862(13) 0.0239(4) Uani 1 1 d . . . O21 O 0.35189(16) 0.31126(14) 0.93276(14) 0.0267(4) Uani 1 1 d . . . O30 O 0.13590(17) 0.27872(15) 0.57829(13) 0.0327(4) Uani 1 1 d . . . O31 O 0.30639(16) 0.44343(13) 0.73445(13) 0.0240(4) Uani 1 1 d . . . O41 O 0.40420(15) 0.55990(13) 0.96349(13) 0.0216(4) Uani 1 1 d . . . O51 O 0.56333(18) 0.56234(16) 0.84256(16) 0.0313(5) Uani 1 1 d . . . C11 C 0.5813(2) 0.26182(19) 0.74496(19) 0.0190(5) Uani 1 1 d . . . C12 C 0.4972(2) 0.2210(2) 0.6414(2) 0.0289(6) Uani 1 1 d . . . H12 H 0.4101 0.2342 0.6198 0.035 Uiso 1 1 calc R . . C13 C 0.5399(2) 0.1610(2) 0.5695(2) 0.0327(7) Uani 1 1 d . . . H13 H 0.4812 0.1346 0.5008 0.039 Uiso 1 1 calc R . . C14 C 0.6697(2) 0.1396(2) 0.5988(2) 0.0276(6) Uani 1 1 d . . . H14 H 0.6984 0.0992 0.5507 0.033 Uiso 1 1 calc R . . C15 C 0.7543(2) 0.1801(2) 0.7012(2) 0.0254(6) Uani 1 1 d . . . C16 C 0.7102(2) 0.2388(2) 0.77305(19) 0.0209(5) Uani 1 1 d . . . C17 C 0.8970(3) 0.1699(3) 0.7587(2) 0.0521(9) Uani 1 1 d . . . H17 H 0.9455 0.2028 0.7191 0.063 Uiso 1 1 calc R . . H171 H 0.9164 0.0928 0.7665 0.063 Uiso 1 1 calc R . . C18 C 0.9290(2) 0.2348(2) 0.8724(2) 0.0288(6) Uani 1 1 d . . . C19 C 1.0109(3) 0.3400(3) 0.8857(3) 0.0517(9) Uani 1 1 d . . . H19 H 1.0276 0.3775 0.9563 0.078 Uiso 1 1 calc R . . H191 H 0.9663 0.3871 0.8300 0.078 Uiso 1 1 calc R . . H192 H 1.0913 0.3227 0.8792 0.078 Uiso 1 1 calc R . . C110 C 0.9828(3) 0.1630(2) 0.9642(2) 0.0369(7) Uani 1 1 d . . . H11A H 1.0010 0.2060 1.0325 0.055 Uiso 1 1 calc R . . H11B H 1.0610 0.1341 0.9622 0.055 Uiso 1 1 calc R . . H11C H 0.9209 0.1027 0.9569 0.055 Uiso 1 1 calc R . . C21 C 0.3202(2) 0.2016(2) 0.92247(19) 0.0211(5) Uani 1 1 d . . . C22 C 0.2466(2) 0.1438(2) 0.8226(2) 0.0279(6) Uani 1 1 d . . . H22 H 0.2182 0.1815 0.7598 0.034 Uiso 1 1 calc R . . C23 C 0.2152(3) 0.0311(2) 0.8156(2) 0.0348(7) Uani 1 1 d . . . H23 H 0.1642 -0.0053 0.7484 0.042 Uiso 1 1 calc R . . C24 C 0.2582(2) -0.0285(2) 0.9070(2) 0.0318(6) Uani 1 1 d . . . H24 H 0.2378 -0.1044 0.9015 0.038 Uiso 1 1 calc R . . C25 C 0.3324(2) 0.0279(2) 1.0069(2) 0.0237(5) Uani 1 1 d . . . C26 C 0.3585(2) 0.1406(2) 1.01370(19) 0.0206(5) Uani 1 1 d . . . C27 C 0.3997(3) -0.0095(2) 1.1195(2) 0.0295(6) Uani 1 1 d . . . H27 H 0.4794 -0.0431 1.1253 0.035 Uiso 1 1 calc R . . H271 H 0.3445 -0.0621 1.1377 0.035 Uiso 1 1 calc R . . C28 C 0.4268(2) 0.1004(2) 1.1938(2) 0.0274(6) Uani 1 1 d . . . C29 C 0.5559(3) 0.1117(3) 1.2862(2) 0.0376(7) Uani 1 1 d . . . H29 H 0.5654 0.1818 1.3277 0.056 Uiso 1 1 calc R . . H291 H 0.6233 0.1077 1.2573 0.056 Uiso 1 1 calc R . . H292 H 0.5615 0.0528 1.3326 0.056 Uiso 1 1 calc R . . C210 C 0.3161(3) 0.1208(2) 1.2325(2) 0.0330(6) Uani 1 1 d . . . H21A H 0.3347 0.1893 1.2780 0.049 Uiso 1 1 calc R . . H21B H 0.3060 0.0609 1.2736 0.049 Uiso 1 1 calc R . . H21C H 0.2377 0.1249 1.1705 0.049 Uiso 1 1 calc R . . C31 C 0.2462(2) 0.4628(2) 0.6278(2) 0.0259(6) Uani 1 1 d . . . C32 C 0.2643(3) 0.5625(2) 0.5877(2) 0.0392(7) Uani 1 1 d . . . H32 H 0.3188 0.6193 0.6348 0.047 Uiso 1 1 calc R . . C33 C 0.2013(4) 0.5787(3) 0.4771(3) 0.0536(9) Uani 1 1 d . . . H33 H 0.2167 0.6458 0.4519 0.064 Uiso 1 1 calc R . . C34 C 0.1175(3) 0.4984(3) 0.4049(3) 0.0478(8) Uani 1 1 d . . . H34 H 0.0742 0.5111 0.3321 0.057 Uiso 1 1 calc R . . C35 C 0.0995(3) 0.3987(3) 0.4433(2) 0.0356(7) Uani 1 1 d . . . C36 C 0.1633(2) 0.3821(2) 0.5522(2) 0.0262(6) Uani 1 1 d . . . C37 C 0.0167(3) 0.2946(3) 0.3876(2) 0.0447(8) Uani 1 1 d . . . H37 H 0.0310 0.2698 0.3218 0.054 Uiso 1 1 calc R . . H371 H -0.0743 0.3060 0.3690 0.054 Uiso 1 1 calc R . . C38 C 0.0628(3) 0.2118(2) 0.4743(2) 0.0365(7) Uani 1 1 d . . . C39 C -0.0462(3) 0.1485(3) 0.4934(2) 0.0465(8) Uani 1 1 d . . . H39 H -0.0107 0.0982 0.5484 0.070 Uiso 1 1 calc R . . H391 H -0.1008 0.1075 0.4266 0.070 Uiso 1 1 calc R . . H392 H -0.0959 0.1998 0.5173 0.070 Uiso 1 1 calc R . . C310 C 0.1559(3) 0.1352(2) 0.4508(2) 0.0424(8) Uani 1 1 d . . . H31A H 0.2221 0.1785 0.4380 0.064 Uiso 1 1 calc R . . H31B H 0.1099 0.0857 0.3872 0.064 Uiso 1 1 calc R . . H31C H 0.1947 0.0930 0.5123 0.064 Uiso 1 1 calc R . . C41 C 0.3189(2) 0.6472(2) 0.9192(2) 0.0265(6) Uani 1 1 d . . . H41 H 0.3324 0.6713 0.8553 0.032 Uiso 1 1 calc R . . H411 H 0.3391 0.7103 0.9732 0.032 Uiso 1 1 calc R . . C42 C 0.1809(2) 0.6066(2) 0.8884(2) 0.0341(7) Uani 1 1 d . . . H42 H 0.1260 0.6652 0.8594 0.051 Uiso 1 1 calc R . . H421 H 0.1673 0.5837 0.9519 0.051 Uiso 1 1 calc R . . H422 H 0.1606 0.5448 0.8341 0.051 Uiso 1 1 calc R . . C511 C 0.6630(12) 0.5580(11) 0.7945(9) 0.028(3) Uani 0.522(7) 1 d P A 1 H51A H 0.7140 0.4949 0.8183 0.034 Uiso 0.522(7) 1 calc PR A 1 H51B H 0.7202 0.6248 0.8189 0.034 Uiso 0.522(7) 1 calc PR A 1 C521 C 0.5991(6) 0.5477(5) 0.6694(5) 0.047(2) Uani 0.522(7) 1 d P A 1 H52A H 0.6647 0.5479 0.6384 0.070 Uiso 0.522(7) 1 calc PR A 1 H52B H 0.5466 0.6092 0.6463 0.070 Uiso 0.522(7) 1 calc PR A 1 H52C H 0.5460 0.4796 0.6453 0.070 Uiso 0.522(7) 1 calc PR A 1 C512 C 0.6231(15) 0.5655(14) 0.7616(11) 0.043(4) Uani 0.478(7) 1 d P A 2 H51C H 0.5912 0.6250 0.7151 0.052 Uiso 0.478(7) 1 calc PR A 2 H51D H 0.6039 0.4959 0.7162 0.052 Uiso 0.478(7) 1 calc PR A 2 C522 C 0.7673(7) 0.5849(6) 0.8246(6) 0.055(2) Uani 0.478(7) 1 d P A 2 H52D H 0.8118 0.5808 0.7745 0.082 Uiso 0.478(7) 1 calc PR A 2 H52E H 0.7960 0.5292 0.8751 0.082 Uiso 0.478(7) 1 calc PR A 2 H52F H 0.7856 0.6569 0.8640 0.082 Uiso 0.478(7) 1 calc PR A 2 HO51 H 0.571(4) 0.619(3) 0.871(3) 0.071(13) Uiso 1 1 d . . . 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 Zr 0.01496(12) 0.02048(13) 0.01781(13) -0.00190(8) 0.00578(9) 0.00208(8) O10 0.0173(9) 0.0646(14) 0.0224(10) -0.0097(9) 0.0050(8) 0.0111(9) O11 0.0195(9) 0.0241(9) 0.0238(9) -0.0046(7) 0.0095(8) 0.0020(7) O20 0.0263(9) 0.0254(10) 0.0197(9) -0.0003(7) 0.0087(8) -0.0022(7) O21 0.0267(10) 0.0233(10) 0.0350(10) 0.0077(8) 0.0157(8) 0.0059(8) O30 0.0367(11) 0.0321(11) 0.0215(10) -0.0016(8) 0.0032(8) -0.0055(9) O31 0.0249(9) 0.0243(9) 0.0197(9) -0.0004(7) 0.0047(7) 0.0051(7) O41 0.0172(9) 0.0220(9) 0.0232(9) -0.0020(7) 0.0046(7) 0.0079(7) O51 0.0349(11) 0.0234(11) 0.0403(12) -0.0084(9) 0.0220(9) -0.0045(9) C11 0.0203(13) 0.0180(13) 0.0215(13) 0.0005(10) 0.0110(10) 0.0040(10) C12 0.0199(13) 0.0365(16) 0.0276(14) -0.0057(11) 0.0069(11) 0.0013(11) C13 0.0252(15) 0.0425(17) 0.0254(14) -0.0131(12) 0.0068(12) -0.0036(12) C14 0.0283(15) 0.0288(15) 0.0287(15) -0.0051(11) 0.0151(12) 0.0039(11) C15 0.0227(13) 0.0296(15) 0.0265(14) 0.0010(11) 0.0119(11) 0.0058(11) C16 0.0204(13) 0.0237(13) 0.0195(13) 0.0023(10) 0.0081(11) 0.0022(10) C17 0.0279(16) 0.095(3) 0.0296(17) -0.0108(16) 0.0065(13) 0.0267(17) C18 0.0183(13) 0.0410(17) 0.0284(15) 0.0016(12) 0.0101(11) 0.0075(12) C19 0.0454(19) 0.0414(19) 0.088(3) 0.0196(17) 0.0436(19) 0.0164(15) C110 0.0383(17) 0.0352(17) 0.0432(18) 0.0066(13) 0.0208(14) 0.0096(13) C21 0.0168(12) 0.0243(14) 0.0254(14) 0.0004(10) 0.0116(11) 0.0053(10) C22 0.0226(14) 0.0399(17) 0.0228(14) 0.0031(11) 0.0092(11) 0.0104(12) C23 0.0282(15) 0.0433(18) 0.0282(15) -0.0123(13) 0.0077(13) 0.0021(13) C24 0.0279(15) 0.0216(14) 0.0448(18) -0.0093(12) 0.0145(13) -0.0025(11) C25 0.0219(13) 0.0211(13) 0.0307(15) 0.0011(10) 0.0127(11) 0.0028(10) C26 0.0170(12) 0.0254(14) 0.0198(13) -0.0009(10) 0.0078(10) 0.0021(10) C27 0.0328(15) 0.0245(14) 0.0360(16) 0.0076(11) 0.0173(13) 0.0046(11) C28 0.0313(15) 0.0305(15) 0.0242(14) 0.0059(11) 0.0138(12) 0.0034(12) C29 0.0344(16) 0.0522(19) 0.0267(15) 0.0065(13) 0.0106(13) 0.0107(14) C210 0.0334(16) 0.0385(17) 0.0320(16) 0.0056(12) 0.0173(13) 0.0035(13) C31 0.0262(14) 0.0300(15) 0.0231(14) 0.0039(11) 0.0100(12) 0.0077(11) C32 0.0513(19) 0.0291(16) 0.0401(18) 0.0045(13) 0.0200(15) 0.0030(14) C33 0.078(3) 0.043(2) 0.049(2) 0.0223(16) 0.030(2) 0.0148(18) C34 0.064(2) 0.055(2) 0.0282(17) 0.0176(15) 0.0170(16) 0.0208(18) C35 0.0300(15) 0.054(2) 0.0232(15) 0.0043(13) 0.0095(13) 0.0120(14) C36 0.0226(14) 0.0335(15) 0.0234(14) 0.0039(11) 0.0090(11) 0.0066(11) C37 0.0358(17) 0.068(2) 0.0244(16) -0.0002(15) 0.0048(13) 0.0052(16) C38 0.0320(16) 0.0491(19) 0.0222(15) -0.0105(12) 0.0059(12) -0.0067(14) C39 0.0380(17) 0.059(2) 0.0410(18) -0.0189(15) 0.0188(15) -0.0142(15) C310 0.0355(17) 0.051(2) 0.0383(18) -0.0122(14) 0.0140(14) -0.0054(14) C41 0.0265(14) 0.0242(14) 0.0262(14) -0.0010(11) 0.0066(12) 0.0071(11) C42 0.0237(14) 0.0401(17) 0.0335(16) -0.0035(12) 0.0052(12) 0.0085(12) C511 0.036(7) 0.020(4) 0.032(7) -0.001(4) 0.018(5) 0.000(4) C521 0.056(4) 0.047(4) 0.050(5) -0.006(3) 0.038(4) -0.001(3) C512 0.066(11) 0.037(6) 0.025(7) 0.001(4) 0.018(6) -0.021(6) C522 0.042(5) 0.052(5) 0.083(6) 0.006(4) 0.037(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr O31 1.9637(16) . ? Zr O11 1.9685(15) . ? Zr O21 2.0086(16) . ? Zr O41 2.1310(15) . ? Zr O41 2.1785(16) 2_667 ? Zr O51 2.2774(19) . ? Zr Zr 3.4734(5) 2_667 ? O10 C16 1.367(3) . ? O10 C18 1.488(3) . ? O11 C11 1.354(3) . ? O20 C26 1.384(3) . ? O20 C28 1.495(3) . ? O21 C21 1.346(3) . ? O30 C36 1.373(3) . ? O30 C38 1.479(3) . ? O31 C31 1.360(3) . ? O41 C41 1.454(3) . ? O41 Zr 2.1785(16) 2_667 ? O51 C512 1.453(18) . ? O51 C511 1.467(15) . ? C11 C12 1.389(3) . ? C11 C16 1.391(3) . ? C12 C13 1.386(3) . ? C13 C14 1.393(4) . ? C14 C15 1.379(3) . ? C15 C16 1.387(3) . ? C15 C17 1.505(4) . ? C17 C18 1.557(4) . ? C18 C110 1.494(4) . ? C18 C19 1.501(4) . ? C21 C26 1.394(3) . ? C21 C22 1.394(3) . ? C22 C23 1.385(4) . ? C23 C24 1.386(4) . ? C24 C25 1.389(3) . ? C25 C26 1.375(3) . ? C25 C27 1.509(3) . ? C27 C28 1.551(4) . ? C28 C29 1.502(4) . ? C28 C210 1.521(3) . ? C31 C32 1.387(4) . ? C31 C36 1.390(3) . ? C32 C33 1.400(4) . ? C33 C34 1.372(5) . ? C34 C35 1.376(4) . ? C35 C36 1.383(3) . ? C35 C37 1.508(4) . ? C37 C38 1.530(4) . ? C38 C39 1.518(4) . ? C38 C310 1.518(4) . ? C41 C42 1.495(3) . ? C511 C521 1.534(11) . ? C512 C522 1.516(15) . ? 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 O31 Zr O11 97.11(7) . . ? O31 Zr O21 100.38(7) . . ? O11 Zr O21 99.13(7) . . ? O31 Zr O41 95.66(6) . . ? O11 Zr O41 160.08(6) . . ? O21 Zr O41 93.53(7) . . ? O31 Zr O41 166.46(6) . 2_667 ? O11 Zr O41 92.59(6) . 2_667 ? O21 Zr O41 87.32(7) . 2_667 ? O41 Zr O41 72.59(7) . 2_667 ? O31 Zr O51 88.03(7) . . ? O11 Zr O51 86.86(7) . . ? O21 Zr O51 168.91(7) . . ? O41 Zr O51 78.35(7) . . ? O41 Zr O51 83.07(7) 2_667 . ? O31 Zr Zr 132.09(5) . 2_667 ? O11 Zr Zr 127.24(5) . 2_667 ? O21 Zr Zr 90.48(5) . 2_667 ? O41 Zr Zr 36.76(4) . 2_667 ? O41 Zr Zr 35.83(4) 2_667 2_667 ? O51 Zr Zr 78.49(5) . 2_667 ? C16 O10 C18 108.09(18) . . ? C11 O11 Zr 160.80(15) . . ? C26 O20 C28 106.40(18) . . ? C21 O21 Zr 139.91(15) . . ? C36 O30 C38 107.11(19) . . ? C31 O31 Zr 160.79(15) . . ? C41 O41 Zr 127.26(14) . . ? C41 O41 Zr 122.91(13) . 2_667 ? Zr O41 Zr 107.41(7) . 2_667 ? C512 O51 C511 20.2(7) . . ? C512 O51 Zr 129.5(7) . . ? C511 O51 Zr 129.8(6) . . ? O11 C11 C12 122.3(2) . . ? O11 C11 C16 121.1(2) . . ? C12 C11 C16 116.6(2) . . ? C13 C12 C11 121.6(2) . . ? C12 C13 C14 120.9(2) . . ? C15 C14 C13 118.1(2) . . ? C14 C15 C16 120.5(2) . . ? C14 C15 C17 131.6(2) . . ? C16 C15 C17 107.8(2) . . ? O10 C16 C15 114.5(2) . . ? O10 C16 C11 123.2(2) . . ? C15 C16 C11 122.2(2) . . ? C15 C17 C18 103.9(2) . . ? O10 C18 C110 107.1(2) . . ? O10 C18 C19 106.0(2) . . ? C110 C18 C19 113.2(2) . . ? O10 C18 C17 105.4(2) . . ? C110 C18 C17 112.2(2) . . ? C19 C18 C17 112.3(2) . . ? O21 C21 C26 120.6(2) . . ? O21 C21 C22 122.7(2) . . ? C26 C21 C22 116.7(2) . . ? C23 C22 C21 120.9(2) . . ? C22 C23 C24 121.3(2) . . ? C23 C24 C25 118.4(2) . . ? C26 C25 C24 119.8(2) . . ? C26 C25 C27 107.2(2) . . ? C24 C25 C27 132.9(2) . . ? C25 C26 O20 114.1(2) . . ? C25 C26 C21 122.7(2) . . ? O20 C26 C21 123.2(2) . . ? C25 C27 C28 102.6(2) . . ? O20 C28 C29 107.4(2) . . ? O20 C28 C210 107.2(2) . . ? C29 C28 C210 112.3(2) . . ? O20 C28 C27 103.67(19) . . ? C29 C28 C27 114.6(2) . . ? C210 C28 C27 110.9(2) . . ? O31 C31 C32 122.6(2) . . ? O31 C31 C36 121.3(2) . . ? C32 C31 C36 116.1(2) . . ? C31 C32 C33 120.8(3) . . ? C34 C33 C32 121.8(3) . . ? C33 C34 C35 118.0(3) . . ? C34 C35 C36 120.1(3) . . ? C34 C35 C37 131.8(3) . . ? C36 C35 C37 108.1(2) . . ? O30 C36 C35 113.4(2) . . ? O30 C36 C31 123.4(2) . . ? C35 C36 C31 123.1(3) . . ? C35 C37 C38 102.7(2) . . ? O30 C38 C39 105.9(2) . . ? O30 C38 C310 107.2(2) . . ? C39 C38 C310 112.3(3) . . ? O30 C38 C37 106.0(2) . . ? C39 C38 C37 113.8(3) . . ? C310 C38 C37 111.2(2) . . ? O41 C41 C42 110.6(2) . . ? O51 C511 C521 109.8(8) . . ? O51 C512 C522 106.5(8) . . ? _diffrn_measured_fraction_theta_max 0.912 _diffrn_reflns_theta_full 28.50 _diffrn_measured_fraction_theta_full 0.912 _refine_diff_density_max 0.418 _refine_diff_density_min -0.365 _refine_diff_density_rms 0.068