# Supplementary Material (ESI) for Journal of Materials Chemistry # This journal is © The Royal Society of Chemistry 2004 data_global _journal_name_full J.Mater.Chem. _journal_coden_Cambridge 1145 _publ_contact_author_name 'Prof Vadim Kessler' _publ_contact_author_address ; Chemistry SLU Box 7015 Uppsala 75007 SWEDEN ; _publ_contact_author_email VADIM.KESSLER@KEMI.SLU.SE _publ_section_title ; Influence of Heteroligands on the Composition, Structure and Properties of Homo- and Heterometallic Zirconium Alkoxides ; loop_ _publ_author_name 'Vadim Kessler' 'Surresh Gohil' 'Gulaim A. Seisenbaeva' data_zroipr1m _database_code_depnum_ccdc_archive 'CCDC 234684' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H72 O10 Zr2' _chemical_formula_weight 775.32 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 12.121(2) _cell_length_b 12.191(2) _cell_length_c 14.984(3) _cell_angle_alpha 80.335(4) _cell_angle_beta 84.806(3) _cell_angle_gamma 89.102(4) _cell_volume 2173.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 964(I>10sigma(I)) _cell_measurement_theta_min 1.38 _cell_measurement_theta_max 21.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.185 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 0.520 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7454 _exptl_absorpt_correction_T_max 0.8595 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7249 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4555 _reflns_number_gt 2783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1128P)^2^+1.4406P] 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 4555 _refine_ls_number_parameters 383 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1098 _refine_ls_R_factor_gt 0.0700 _refine_ls_wR_factor_ref 0.2139 _refine_ls_wR_factor_gt 0.1999 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.92084(8) 0.48415(9) 0.41175(7) 0.0832(5) Uani 1 1 d . . . Zr2 Zr 0.46404(9) 0.07767(9) 0.08573(7) 0.0888(5) Uani 1 1 d . . . O6 O 0.5123(5) -0.0865(5) 0.0597(4) 0.0660(16) Uani 1 1 d . . . O1 O 1.0833(5) 0.5291(5) 0.4417(4) 0.0657(16) Uani 1 1 d . . . O7 O 0.3015(5) 0.0203(6) 0.0648(5) 0.093(2) Uani 1 1 d . . . O2 O 0.9808(6) 0.3219(5) 0.4299(5) 0.092(2) Uani 1 1 d . . . O8 O 0.4482(6) 0.0386(6) 0.2165(5) 0.106(2) Uani 1 1 d . . . O3 O 0.8893(6) 0.6629(5) 0.4280(5) 0.094(2) Uani 1 1 d . . . O4 O 0.9519(6) 0.5239(6) 0.2814(5) 0.105(2) Uani 1 1 d . . . O9 O 0.4208(6) 0.2280(6) 0.0800(5) 0.102(2) Uani 1 1 d . . . O10 O 0.6384(5) 0.1043(6) 0.0720(5) 0.095(2) Uani 1 1 d . . . O5 O 0.7651(6) 0.4532(7) 0.4111(6) 0.113(3) Uani 1 1 d . . . C6 C 0.5319(13) -0.1819(11) 0.1294(10) 0.132(5) Uani 1 1 d . . . H15 H 0.5581 -0.2283 0.0844 0.158 Uiso 1 1 calc R . . C3 C 0.8236(13) 0.7456(12) 0.3795(10) 0.136(5) Uani 1 1 d . . . H16A H 0.7916 0.7130 0.3322 0.163 Uiso 1 1 calc R . . C5 C 0.6568(16) 0.440(2) 0.392(2) 0.238(12) Uani 1 1 d . . . H17 H 0.6238 0.4771 0.4417 0.285 Uiso 1 1 calc R . . C1 C 1.1771(12) 0.5611(12) 0.3799(10) 0.139(5) Uani 1 1 d D . . C7 C 0.1951(11) 0.0421(12) 0.1092(11) 0.134(5) Uani 1 1 d . . . H19A H 0.2078 0.0887 0.1546 0.161 Uiso 1 1 calc R . . C9 C 0.389(2) 0.3398(15) 0.0882(17) 0.217(11) Uani 1 1 d . . . H20 H 0.4343 0.3736 0.0334 0.261 Uiso 1 1 calc R . . C12 C 1.1882(14) 0.6774(12) 0.3494(13) 0.189(8) Uani 1 1 d D . . H21A H 1.1330 0.7161 0.3823 0.284 Uiso 1 1 calc R . . H21B H 1.1784 0.6938 0.2856 0.284 Uiso 1 1 calc R . . H21C H 1.2605 0.7009 0.3595 0.284 Uiso 1 1 calc R . . C2 C 0.9562(16) 0.2312(13) 0.3857(14) 0.159(6) Uani 1 1 d . . . H23A H 0.9050 0.2600 0.3403 0.190 Uiso 1 1 calc R . . C10 C 0.7113(15) 0.1772(15) 0.1064(13) 0.160(6) Uani 1 1 d . . . H25A H 0.6612 0.2126 0.1482 0.192 Uiso 1 1 calc R . . C62 C 0.4362(13) -0.2451(13) 0.1565(13) 0.194(8) Uani 1 1 d . . . H26A H 0.4530 -0.3096 0.1994 0.291 Uiso 1 1 calc R . . H26B H 0.4088 -0.2681 0.1044 0.291 Uiso 1 1 calc R . . H26C H 0.3809 -0.2013 0.1843 0.291 Uiso 1 1 calc R . . C11 C 1.2430(14) 0.4765(14) 0.3536(13) 0.223(10) Uani 1 1 d D . . H28A H 1.2165 0.4062 0.3868 0.334 Uiso 1 1 calc R . . H28B H 1.3181 0.4874 0.3660 0.334 Uiso 1 1 calc R . . H28C H 1.2403 0.4770 0.2897 0.334 Uiso 1 1 calc R . . C22 C 0.900(2) 0.1434(14) 0.4462(16) 0.257(13) Uani 1 1 d . . . H31A H 0.8345 0.1719 0.4752 0.385 Uiso 1 1 calc R . . H31B H 0.9479 0.1117 0.4915 0.385 Uiso 1 1 calc R . . H31C H 0.8799 0.0871 0.4129 0.385 Uiso 1 1 calc R . . C82 C 0.505(4) 0.084(3) 0.3478(18) 0.39(3) Uani 1 1 d . . . H32A H 0.4971 0.0718 0.4130 0.585 Uiso 1 1 calc R . . H32B H 0.4821 0.1583 0.3249 0.585 Uiso 1 1 calc R . . H32C H 0.5817 0.0746 0.3271 0.585 Uiso 1 1 calc R . . C61 C 0.6336(14) -0.1836(14) 0.1641(11) 0.177(7) Uani 1 1 d . . . H35A H 0.6826 -0.1320 0.1245 0.266 Uiso 1 1 calc R . . H35B H 0.6643 -0.2572 0.1685 0.266 Uiso 1 1 calc R . . H35C H 0.6248 -0.1628 0.2233 0.266 Uiso 1 1 calc R . . C52 C 0.616(2) 0.331(2) 0.432(2) 0.37(2) Uani 1 1 d . . . H36A H 0.6777 0.2831 0.4477 0.556 Uiso 1 1 calc R . . H36B H 0.5756 0.3015 0.3896 0.556 Uiso 1 1 calc R . . H36C H 0.5685 0.3359 0.4862 0.556 Uiso 1 1 calc R . . C81 C 0.345(3) 0.023(5) 0.3451(19) 0.50(4) Uani 1 1 d . . . H41A H 0.2974 -0.0178 0.3149 0.744 Uiso 1 1 calc R . . H41B H 0.3270 0.1008 0.3329 0.744 Uiso 1 1 calc R . . H41C H 0.3355 -0.0031 0.4094 0.744 Uiso 1 1 calc R . . C102 C 0.752(2) 0.271(2) 0.039(2) 0.35(2) Uani 1 1 d . . . H43A H 0.7932 0.3205 0.0671 0.529 Uiso 1 1 calc R . . H43B H 0.6910 0.3107 0.0119 0.529 Uiso 1 1 calc R . . H43C H 0.8000 0.2446 -0.0079 0.529 Uiso 1 1 calc R . . C21 C 1.0558(17) 0.1984(19) 0.3360(17) 0.283(16) Uani 1 1 d . . . H44A H 1.0829 0.2600 0.2911 0.424 Uiso 1 1 calc R . . H44B H 1.0395 0.1372 0.3065 0.424 Uiso 1 1 calc R . . H44C H 1.1112 0.1762 0.3774 0.424 Uiso 1 1 calc R . . C101 C 0.7818(17) 0.1168(18) 0.163(2) 0.278(15) Uani 1 1 d . . . H45A H 0.7395 0.0666 0.2094 0.417 Uiso 1 1 calc R . . H45B H 0.8228 0.1665 0.1910 0.417 Uiso 1 1 calc R . . H45C H 0.8322 0.0751 0.1286 0.417 Uiso 1 1 calc R . . C8 C 0.442(3) 0.010(3) 0.3170(15) 0.286(17) Uani 1 1 d . . . H55A H 0.4667 -0.0670 0.3364 0.343 Uiso 1 1 calc R . . C72 C 0.1289(13) 0.1109(18) 0.0389(15) 0.238(11) Uani 1 1 d . . . H51A H 0.0586 0.1300 0.0673 0.357 Uiso 1 1 calc R . . H51B H 0.1172 0.0687 -0.0081 0.357 Uiso 1 1 calc R . . H51C H 0.1689 0.1777 0.0128 0.357 Uiso 1 1 calc R . . C92 C 0.447(2) 0.3894(18) 0.1470(17) 0.266(13) Uani 1 1 d . . . H53A H 0.4243 0.4656 0.1443 0.399 Uiso 1 1 calc R . . H53B H 0.5251 0.3866 0.1291 0.399 Uiso 1 1 calc R . . H53C H 0.4322 0.3503 0.2079 0.399 Uiso 1 1 calc R . . C71 C 0.1453(15) -0.0533(16) 0.1548(18) 0.272(14) Uani 1 1 d . . . H50A H 0.1898 -0.0870 0.2019 0.407 Uiso 1 1 calc R . . H50B H 0.1377 -0.1041 0.1132 0.407 Uiso 1 1 calc R . . H50C H 0.0734 -0.0361 0.1813 0.407 Uiso 1 1 calc R . . C32 C 0.7276(15) 0.7745(17) 0.4464(13) 0.230(11) Uani 1 1 d . . . H10A H 0.6839 0.7091 0.4693 0.345 Uiso 1 1 calc R . . H10B H 0.6820 0.8310 0.4155 0.345 Uiso 1 1 calc R . . H10C H 0.7571 0.8013 0.4961 0.345 Uiso 1 1 calc R . . C31 C 0.8865(18) 0.8440(13) 0.3352(14) 0.235(12) Uani 1 1 d . . . H10D H 0.9410 0.8236 0.2904 0.352 Uiso 1 1 calc R . . H10E H 0.9227 0.8748 0.3798 0.352 Uiso 1 1 calc R . . H10F H 0.8371 0.8984 0.3065 0.352 Uiso 1 1 calc R . . C91 C 0.297(2) 0.3784(19) 0.059(2) 0.34(2) Uani 1 1 d . . . H10G H 0.2738 0.3346 0.0170 0.508 Uiso 1 1 calc R . . H10H H 0.3076 0.4542 0.0297 0.508 Uiso 1 1 calc R . . H10I H 0.2418 0.3754 0.1097 0.508 Uiso 1 1 calc R . . C51 C 0.613(2) 0.501(2) 0.332(2) 0.34(2) Uani 1 1 d . . . H10J H 0.6671 0.5510 0.2971 0.510 Uiso 1 1 calc R . . H10K H 0.5553 0.5437 0.3592 0.510 Uiso 1 1 calc R . . H10L H 0.5814 0.4572 0.2937 0.510 Uiso 1 1 calc R . . C42 C 0.960(3) 0.634(2) 0.1474(15) 0.294(16) Uani 1 1 d . . . H10M H 0.9753 0.6372 0.0830 0.441 Uiso 1 1 calc R . . H10N H 1.0116 0.6809 0.1685 0.441 Uiso 1 1 calc R . . H10O H 0.8860 0.6597 0.1602 0.441 Uiso 1 1 calc R . . C4 C 0.970(3) 0.534(2) 0.1876(17) 0.281(16) Uani 1 1 d . . . H22A H 1.0483 0.5158 0.1757 0.338 Uiso 1 1 calc R . . C41 C 0.916(4) 0.466(3) 0.1512(19) 0.54(5) Uani 1 1 d . . . H38A H 0.9312 0.4815 0.0863 0.817 Uiso 1 1 calc R . . H38B H 0.8383 0.4729 0.1671 0.817 Uiso 1 1 calc R . . H38C H 0.9393 0.3909 0.1731 0.817 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 0.0815(8) 0.1060(9) 0.0629(8) -0.0126(6) -0.0112(5) -0.0115(6) Zr2 0.1221(10) 0.0774(8) 0.0669(8) -0.0171(6) -0.0023(6) 0.0140(6) O6 0.072(4) 0.059(4) 0.062(4) 0.004(3) -0.006(3) 0.001(3) O1 0.064(4) 0.074(4) 0.055(4) -0.006(3) 0.009(3) -0.009(3) O7 0.053(4) 0.114(6) 0.110(6) -0.015(4) 0.003(4) 0.006(4) O2 0.120(6) 0.061(4) 0.101(6) -0.024(4) -0.020(4) -0.003(4) O8 0.127(6) 0.127(6) 0.063(5) -0.024(4) 0.005(4) 0.012(5) O3 0.113(6) 0.069(4) 0.098(6) -0.008(4) -0.026(4) 0.026(4) O4 0.142(7) 0.125(6) 0.048(5) -0.010(4) -0.030(4) -0.001(5) O9 0.127(6) 0.085(5) 0.097(6) -0.030(4) 0.004(4) 0.015(4) O10 0.080(5) 0.105(5) 0.109(6) -0.033(4) -0.025(4) -0.007(4) O5 0.079(5) 0.138(7) 0.133(7) -0.045(5) -0.033(5) -0.009(4) C6 0.135(12) 0.116(11) 0.121(12) 0.061(9) -0.029(10) -0.038(9) C3 0.171(14) 0.109(11) 0.136(13) -0.030(10) -0.047(11) 0.056(11) C5 0.144(17) 0.23(2) 0.34(3) 0.03(2) -0.154(19) -0.060(15) C1 0.125(12) 0.139(14) 0.133(13) 0.004(10) 0.050(10) -0.021(10) C7 0.085(10) 0.124(12) 0.179(15) 0.004(10) 0.008(10) 0.007(9) C9 0.27(3) 0.130(16) 0.29(3) -0.120(17) -0.11(2) 0.084(16) C12 0.179(16) 0.150(15) 0.205(19) 0.015(13) 0.084(13) -0.050(12) C2 0.189(17) 0.099(12) 0.207(19) -0.064(13) -0.059(14) 0.019(11) C10 0.158(15) 0.174(16) 0.161(17) -0.038(13) -0.067(12) -0.008(13) C62 0.145(14) 0.157(15) 0.23(2) 0.092(13) 0.018(13) -0.025(11) C11 0.150(15) 0.28(2) 0.22(2) -0.061(18) 0.110(14) 0.034(15) C22 0.40(4) 0.074(12) 0.29(3) -0.022(14) -0.01(2) -0.055(16) C82 0.63(8) 0.41(5) 0.14(2) -0.06(3) -0.04(3) -0.22(5) C61 0.149(14) 0.217(19) 0.146(15) 0.048(12) -0.055(12) 0.015(12) C52 0.28(3) 0.29(3) 0.53(6) 0.06(3) -0.21(4) -0.14(3) C81 0.31(4) 1.10(13) 0.12(2) -0.24(4) -0.03(2) 0.12(6) C102 0.42(4) 0.31(3) 0.31(3) 0.04(3) -0.05(3) -0.30(3) C21 0.21(2) 0.29(3) 0.39(4) -0.25(3) 0.07(2) 0.01(2) C101 0.19(2) 0.21(2) 0.47(5) -0.07(2) -0.18(3) 0.003(17) C8 0.33(4) 0.41(4) 0.15(2) -0.19(2) 0.10(2) -0.10(3) C72 0.104(13) 0.27(3) 0.31(3) 0.02(2) -0.013(15) 0.063(15) C92 0.33(3) 0.21(2) 0.31(3) -0.18(2) -0.06(2) 0.05(2) C71 0.139(16) 0.172(19) 0.45(4) 0.04(2) 0.11(2) -0.027(13) C32 0.188(18) 0.28(3) 0.22(2) -0.066(19) 0.004(15) 0.130(18) C31 0.31(3) 0.119(14) 0.25(2) 0.101(15) -0.12(2) -0.052(15) C91 0.31(3) 0.19(2) 0.56(6) -0.15(3) -0.17(3) 0.17(2) C51 0.22(2) 0.40(4) 0.37(4) 0.14(3) -0.23(3) -0.11(2) C42 0.55(5) 0.23(3) 0.097(17) 0.005(17) -0.06(2) 0.04(3) C4 0.48(5) 0.22(3) 0.14(2) 0.050(19) -0.17(3) -0.07(3) C41 1.10(12) 0.40(5) 0.16(3) -0.01(3) -0.18(4) -0.41(7) _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 O5 1.933(7) . ? Zr1 O4 1.935(7) . ? Zr1 O2 2.080(6) . ? Zr1 O1 2.158(6) . ? Zr1 O1 2.171(6) 2_766 ? Zr1 O3 2.256(6) . ? Zr1 Zr1 3.480(2) 2_766 ? Zr2 O9 1.889(7) . ? Zr2 O8 1.930(7) . ? Zr2 O10 2.129(7) . ? Zr2 O6 2.157(6) 2_655 ? Zr2 O6 2.164(6) . ? Zr2 O7 2.167(7) . ? Zr2 Zr2 3.482(2) 2_655 ? O6 C6 1.459(12) . ? O6 Zr2 2.157(6) 2_655 ? O1 C1 1.415(13) . ? O1 Zr1 2.171(6) 2_766 ? O7 C7 1.439(14) . ? O2 C2 1.429(15) . ? O8 C8 1.48(3) . ? O3 C3 1.418(13) . ? O4 C4 1.39(3) . ? O9 C9 1.433(16) . ? O10 C10 1.448(16) . ? O5 C5 1.383(17) . ? C6 C61 1.379(17) . ? C6 C62 1.394(18) . ? C3 C31 1.46(2) . ? C3 C32 1.54(2) . ? C5 C51 1.22(2) . ? C5 C52 1.44(3) . ? C1 C11 1.383(13) . ? C1 C12 1.419(13) . ? C7 C71 1.366(19) . ? C7 C72 1.51(2) . ? C9 C91 1.28(2) . ? C9 C92 1.39(2) . ? C2 C22 1.42(2) . ? C2 C21 1.45(2) . ? C10 C101 1.38(2) . ? C10 C102 1.46(3) . ? C82 C8 1.36(3) . ? C81 C8 1.23(4) . ? C42 C4 1.27(3) . ? C4 C41 1.29(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zr1 O4 96.7(3) . . ? O5 Zr1 O2 99.1(3) . . ? O4 Zr1 O2 99.6(3) . . ? O5 Zr1 O1 167.2(3) . . ? O4 Zr1 O1 94.5(3) . . ? O2 Zr1 O1 85.3(2) . . ? O5 Zr1 O1 95.1(3) . 2_766 ? O4 Zr1 O1 165.8(3) . 2_766 ? O2 Zr1 O1 86.4(3) . 2_766 ? O1 Zr1 O1 73.0(2) . 2_766 ? O5 Zr1 O3 93.0(3) . . ? O4 Zr1 O3 92.2(3) . . ? O2 Zr1 O3 161.9(3) . . ? O1 Zr1 O3 80.2(2) . . ? O1 Zr1 O3 79.2(2) 2_766 . ? O5 Zr1 Zr1 131.3(2) . 2_766 ? O4 Zr1 Zr1 130.8(2) . 2_766 ? O2 Zr1 Zr1 84.81(19) . 2_766 ? O1 Zr1 Zr1 36.62(15) . 2_766 ? O1 Zr1 Zr1 36.37(15) 2_766 2_766 ? O3 Zr1 Zr1 77.13(18) . 2_766 ? O9 Zr2 O8 96.7(3) . . ? O9 Zr2 O10 97.3(3) . . ? O8 Zr2 O10 96.7(3) . . ? O9 Zr2 O6 94.6(3) . 2_655 ? O8 Zr2 O6 168.6(3) . 2_655 ? O10 Zr2 O6 83.1(2) . 2_655 ? O9 Zr2 O6 167.1(3) . . ? O8 Zr2 O6 96.0(3) . . ? O10 Zr2 O6 82.9(2) . . ? O6 Zr2 O6 72.6(2) 2_655 . ? O9 Zr2 O7 94.6(3) . . ? O8 Zr2 O7 96.0(3) . . ? O10 Zr2 O7 161.5(3) . . ? O6 Zr2 O7 81.8(2) 2_655 . ? O6 Zr2 O7 82.3(2) . . ? O9 Zr2 Zr2 131.0(2) . 2_655 ? O8 Zr2 Zr2 132.3(2) . 2_655 ? O10 Zr2 Zr2 81.35(19) . 2_655 ? O6 Zr2 Zr2 36.38(14) 2_655 2_655 ? O6 Zr2 Zr2 36.24(15) . 2_655 ? O7 Zr2 Zr2 80.12(19) . 2_655 ? C6 O6 Zr2 127.5(8) . 2_655 ? C6 O6 Zr2 125.0(8) . . ? Zr2 O6 Zr2 107.4(2) 2_655 . ? C1 O1 Zr1 128.1(8) . . ? C1 O1 Zr1 124.9(8) . 2_766 ? Zr1 O1 Zr1 107.0(2) . 2_766 ? C7 O7 Zr2 129.4(8) . . ? C2 O2 Zr1 129.9(8) . . ? C8 O8 Zr2 177.1(15) . . ? C3 O3 Zr1 130.4(7) . . ? C4 O4 Zr1 170.6(13) . . ? C9 O9 Zr2 172.5(11) . . ? C10 O10 Zr2 134.5(9) . . ? C5 O5 Zr1 168.4(14) . . ? C61 C6 C62 132.4(13) . . ? C61 C6 O6 115.3(11) . . ? C62 C6 O6 111.6(12) . . ? O3 C3 C31 113.3(14) . . ? O3 C3 C32 107.6(13) . . ? C31 C3 C32 112.1(16) . . ? C51 C5 O5 124(2) . . ? C51 C5 C52 124(2) . . ? O5 C5 C52 111(2) . . ? O1 C1 C11 116.8(12) . . ? O1 C1 C12 114.9(12) . . ? C11 C1 C12 128.1(12) . . ? C71 C7 O7 111.8(13) . . ? C71 C7 C72 115.6(18) . . ? O7 C7 C72 107.6(13) . . ? C91 C9 C92 123.1(19) . . ? C91 C9 O9 120(2) . . ? C92 C9 O9 115.5(18) . . ? C22 C2 O2 112.3(17) . . ? C22 C2 C21 114.9(18) . . ? O2 C2 C21 109.4(16) . . ? C101 C10 O10 110.9(16) . . ? C101 C10 C102 121(2) . . ? O10 C10 C102 113.7(16) . . ? C81 C8 C82 108(3) . . ? C81 C8 O8 107(3) . . ? C82 C8 O8 108(3) . . ? C42 C4 C41 112(3) . . ? C42 C4 O4 113(3) . . ? C41 C4 O4 116(3) . . ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.523 _refine_diff_density_min -0.423 _refine_diff_density_rms 0.071 data_zropp2m _database_code_depnum_ccdc_archive 'CCDC 234685' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H36 O5 Zr' _chemical_formula_weight 387.66 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 10.153(4) _cell_length_b 10.774(4) _cell_length_c 11.872(4) _cell_angle_alpha 112.144(8) _cell_angle_beta 101.329(6) _cell_angle_gamma 104.345(5) _cell_volume 1102.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 964(I>2sigma(I)) _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 20.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 412 _exptl_absorpt_coefficient_mu 0.513 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6845 _exptl_absorpt_correction_T_max 0.9044 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3378 _diffrn_reflns_av_R_equivalents 0.0664 _diffrn_reflns_av_sigmaI/netI 0.0653 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 20.00 _reflns_number_total 2044 _reflns_number_gt 1362 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1344P)^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 SHELXL _refine_ls_extinction_coef 0.003(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2044 _refine_ls_number_parameters 195 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.1055 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1960 _refine_ls_wR_factor_gt 0.1761 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.07246(10) 0.14460(9) 0.15131(8) 0.1126(7) Uani 1 1 d D . . O1 O -0.0806(6) -0.0646(6) 0.0401(6) 0.0955(17) Uani 1 1 d D . . O2 O 0.2167(7) 0.3262(6) 0.2099(7) 0.130(2) Uani 1 1 d D . . O3 O 0.2144(8) 0.0349(9) 0.1764(8) 0.131(2) Uani 1 1 d D . . O4 O 0.0246(8) 0.1722(8) 0.3060(6) 0.141(2) Uani 1 1 d . . . O5 O -0.1025(7) 0.1957(7) 0.0646(7) 0.130(2) Uani 1 1 d . . . C4 C -0.002(3) 0.228(3) 0.4284(17) 0.330(15) Uani 1 1 d D . . H6A H -0.0036 0.3236 0.4450 0.395 Uiso 1 1 calc R . . C1 C -0.1624(19) -0.155(2) 0.0956(18) 0.279(13) Uani 1 1 d D . . H1A H -0.1599 -0.2502 0.0538 0.335 Uiso 1 1 calc R . . H1B H -0.1072 -0.1151 0.1856 0.335 Uiso 1 1 calc R . . C2 C 0.325(3) 0.453(3) 0.311(5) 0.23(2) Uiso 0.54(8) 1 d PD . . C3 C 0.332(2) 0.059(3) 0.283(2) 0.241(9) Uani 1 1 d . . . H3A H 0.3439 0.1536 0.3491 0.289 Uiso 1 1 calc R . . C12 C -0.3463(18) -0.2707(19) 0.1486(19) 0.262(11) Uani 1 1 d D . . H12A H -0.4418 -0.2853 0.1536 0.393 Uiso 1 1 calc R . . H12B H -0.2789 -0.2294 0.2335 0.393 Uiso 1 1 calc R . . H12C H -0.3401 -0.3609 0.0969 0.393 Uiso 1 1 calc R . . C31 C 0.283(3) -0.034(3) 0.335(3) 0.359(17) Uani 1 1 d . . . H31A H 0.3548 -0.0089 0.4133 0.539 Uiso 1 1 calc R . . H31B H 0.2640 -0.1305 0.2746 0.539 Uiso 1 1 calc R . . H31C H 0.1961 -0.0253 0.3522 0.539 Uiso 1 1 calc R . . C21 C 0.455(3) 0.482(3) 0.266(4) 0.47(3) Uani 1 1 d . . . C32 C 0.452(2) 0.078(4) 0.266(3) 0.43(3) Uani 1 1 d . . . H32A H 0.5233 0.0976 0.3431 0.648 Uiso 1 1 calc R . . H32B H 0.4768 0.1576 0.2464 0.648 Uiso 1 1 calc R . . H32C H 0.4480 -0.0068 0.1964 0.648 Uiso 1 1 calc R . . C22 C 0.271(3) 0.570(2) 0.315(4) 0.43(2) Uani 1 1 d D . . C5 C -0.148(2) 0.313(2) 0.120(2) 0.213(7) Uani 1 1 d . . . H5D H -0.0946 0.3647 0.2126 0.255 Uiso 1 1 calc R . . C51 C -0.296(3) 0.255(3) 0.106(3) 0.337(15) Uani 1 1 d . . . H51A H -0.3270 0.3308 0.1519 0.505 Uiso 1 1 calc R . . H51B H -0.3093 0.1859 0.1384 0.505 Uiso 1 1 calc R . . H51C H -0.3515 0.2100 0.0160 0.505 Uiso 1 1 calc R . . C52 C -0.131(3) 0.406(3) 0.073(3) 0.362(18) Uani 1 1 d . . . H52A H -0.0304 0.4538 0.0919 0.543 Uiso 1 1 calc R . . H52B H -0.1729 0.4756 0.1109 0.543 Uiso 1 1 calc R . . H52C H -0.1772 0.3570 -0.0184 0.543 Uiso 1 1 calc R . . C42 C 0.115(4) 0.249(5) 0.526(3) 0.52(3) Uani 1 1 d D . . H42A H 0.0898 0.2652 0.6028 0.783 Uiso 1 1 calc R . . H42B H 0.1946 0.3311 0.5424 0.783 Uiso 1 1 calc R . . H42C H 0.1424 0.1659 0.5007 0.783 Uiso 1 1 calc R . . C41 C -0.142(3) 0.146(5) 0.422(2) 0.51(3) Uani 1 1 d D . . H41A H -0.1454 0.1680 0.5078 0.764 Uiso 1 1 calc R . . H41B H -0.1598 0.0451 0.3767 0.764 Uiso 1 1 calc R . . H41C H -0.2147 0.1693 0.3782 0.764 Uiso 1 1 calc R . . C11 C -0.312(2) -0.171(2) 0.089(2) 0.329(17) Uani 1 1 d D . . H11A H -0.3744 -0.2131 0.0009 0.395 Uiso 1 1 calc R . . H11B H -0.3209 -0.0800 0.1377 0.395 Uiso 1 1 calc R . . C2A C 0.305(4) 0.466(2) 0.241(4) 0.17(2) Uiso 0.46(8) 1 d PD . . H1 H 0.211(15) -0.043(13) 0.107(5) 0.32(11) Uiso 1 1 d 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 Zr1 0.1127(10) 0.0968(9) 0.1021(9) 0.0310(6) 0.0433(6) 0.0101(6) O1 0.077(4) 0.095(4) 0.126(5) 0.059(4) 0.054(3) 0.015(3) O2 0.121(5) 0.081(4) 0.137(5) 0.028(4) 0.032(4) -0.004(4) O3 0.111(5) 0.132(6) 0.139(6) 0.056(5) 0.029(5) 0.043(4) O4 0.162(6) 0.144(6) 0.103(5) 0.041(4) 0.057(4) 0.045(5) O5 0.121(5) 0.115(5) 0.159(6) 0.055(4) 0.050(4) 0.060(5) C4 0.37(3) 0.48(4) 0.127(15) 0.14(2) 0.126(19) 0.09(3) C1 0.210(19) 0.25(2) 0.173(16) -0.062(15) 0.034(15) 0.021(18) C3 0.151(16) 0.34(3) 0.217(18) 0.157(18) 0.002(14) 0.067(17) C12 0.198(16) 0.29(2) 0.38(3) 0.25(2) 0.150(18) 0.021(15) C31 0.39(4) 0.45(4) 0.34(3) 0.30(3) 0.06(3) 0.15(3) C21 0.21(3) 0.32(4) 0.65(7) 0.08(3) 0.13(3) -0.07(2) C32 0.104(14) 0.70(7) 0.52(5) 0.37(5) 0.06(2) 0.07(3) C22 0.28(3) 0.150(17) 0.61(5) 0.00(2) 0.02(3) 0.049(18) C5 0.192(17) 0.226(18) 0.34(2) 0.181(18) 0.140(16) 0.143(15) C51 0.27(3) 0.33(3) 0.50(4) 0.17(3) 0.22(3) 0.18(3) C52 0.48(4) 0.27(2) 0.57(5) 0.31(3) 0.28(4) 0.24(3) C42 0.56(6) 0.89(9) 0.19(3) 0.21(4) 0.13(3) 0.42(7) C41 0.53(5) 0.88(9) 0.34(4) 0.35(5) 0.35(4) 0.32(6) C11 0.35(4) 0.37(4) 0.24(2) 0.08(2) 0.03(3) 0.24(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 Zr1 O2 1.900(6) . ? Zr1 O4 1.925(6) . ? Zr1 O1 2.110(6) . ? Zr1 O3 2.122(7) . ? Zr1 O1 2.133(6) 2 ? Zr1 O5 2.170(7) . ? Zr1 Zr1 3.4631(19) 2 ? O1 C1 1.54(3) . ? O1 Zr1 2.133(6) 2 ? O2 C2A 1.411(19) . ? O2 C2 1.42(2) . ? O3 C3 1.444(17) . ? O4 C4 1.455(19) . ? O5 C5 1.429(16) . ? C4 C42 1.390(18) . ? C4 C41 1.455(18) . ? C1 C11 1.469(13) . ? C2 C2A 0.89(4) . ? C2 C22 1.48(2) . ? C2 C21 1.52(5) . ? C3 C32 1.25(2) . ? C3 C31 1.41(3) . ? C12 C11 1.501(13) . ? C21 C2A 1.45(4) . ? C22 C2A 1.31(3) . ? C5 C52 1.31(2) . ? C5 C51 1.42(2) . ? 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 Zr1 O4 99.7(3) . . ? O2 Zr1 O1 165.2(2) . . ? O4 Zr1 O1 95.0(3) . . ? O2 Zr1 O3 96.5(3) . . ? O4 Zr1 O3 96.4(3) . . ? O1 Zr1 O3 83.4(3) . . ? O2 Zr1 O1 94.7(3) . 2 ? O4 Zr1 O1 165.5(2) . 2 ? O1 Zr1 O1 70.6(2) . 2 ? O3 Zr1 O1 83.5(3) . 2 ? O2 Zr1 O5 95.9(3) . . ? O4 Zr1 O5 95.3(3) . . ? O1 Zr1 O5 80.9(2) . . ? O3 Zr1 O5 161.2(3) . . ? O1 Zr1 O5 81.4(2) 2 . ? O2 Zr1 Zr1 129.7(2) . 2 ? O4 Zr1 Zr1 130.5(2) . 2 ? O1 Zr1 Zr1 35.51(15) . 2 ? O3 Zr1 Zr1 82.0(2) . 2 ? O1 Zr1 Zr1 35.08(14) 2 2 ? O5 Zr1 Zr1 79.18(18) . 2 ? C1 O1 Zr1 124.4(7) . . ? C1 O1 Zr1 125.1(7) . 2 ? Zr1 O1 Zr1 109.4(2) . 2 ? C2A O2 C2 36.7(18) . . ? C2A O2 Zr1 169.9(19) . . ? C2 O2 Zr1 151(3) . . ? C3 O3 Zr1 134.3(12) . . ? C4 O4 Zr1 166.6(12) . . ? C5 O5 Zr1 129.1(10) . . ? C42 C4 O4 110(3) . . ? C42 C4 C41 117(2) . . ? O4 C4 C41 112.3(18) . . ? C11 C1 O1 122(2) . . ? C2A C2 O2 71(2) . . ? C2A C2 C22 61(3) . . ? O2 C2 C22 105(2) . . ? C2A C2 C21 68(5) . . ? O2 C2 C21 107(3) . . ? C22 C2 C21 104(3) . . ? C32 C3 C31 120(3) . . ? C32 C3 O3 116(2) . . ? C31 C3 O3 109(2) . . ? C2A C21 C2 34.8(17) . . ? C2A C22 C2 36.6(19) . . ? C52 C5 C51 109(2) . . ? C52 C5 O5 115.9(19) . . ? C51 C5 O5 107.4(18) . . ? C1 C11 C12 102.2(18) . . ? C2 C2A C22 82(3) . . ? C2 C2A O2 72.2(19) . . ? C22 C2A O2 115(3) . . ? C2 C2A C21 77(5) . . ? C22 C2A C21 118(3) . . ? O2 C2A C21 112(3) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.373 _refine_diff_density_min -0.387 _refine_diff_density_rms 0.064 data_cozrpr1m _database_code_depnum_ccdc_archive 'CCDC 234686' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H84 Co2 O14 Zr2' _chemical_formula_weight 1089.37 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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.922(5) _cell_length_b 16.075(6) _cell_length_c 13.415(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.868(8) _cell_angle_gamma 90.00 _cell_volume 2772.1(17) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 996(I>10sigma(I)) _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 22.00 _exptl_crystal_description needle _exptl_crystal_colour 'bluish purple' _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.305 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.005 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5398 _exptl_absorpt_correction_T_max 0.9062 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8295 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 22.00 _reflns_number_total 3373 _reflns_number_gt 1992 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0761P)^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 3373 _refine_ls_number_parameters 252 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1038 _refine_ls_R_factor_gt 0.0494 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1186 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _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 Zr1 Zr 0.00188(5) 0.11031(4) 0.03203(5) 0.0652(3) Uani 1 1 d . . . Co1 Co 0.18027(8) 0.02139(6) -0.10423(7) 0.0795(4) Uani 1 1 d . . . O1 O 0.1551(3) 0.1073(3) -0.0076(3) 0.0799(14) Uani 1 1 d . . . O2 O -0.1557(3) 0.0895(3) 0.0528(3) 0.0747(13) Uani 1 1 d . . . O3 O -0.0094(3) 0.0187(3) -0.0919(3) 0.0675(12) Uani 1 1 d . . . O7 O 0.3352(4) 0.0216(3) -0.1038(4) 0.1004(17) Uani 1 1 d . . . O5 O 0.0417(4) 0.1575(3) 0.1604(4) 0.0936(15) Uani 1 1 d . . . O6 O 0.1590(4) 0.0301(4) -0.2475(4) 0.1030(17) Uani 1 1 d . . . O4 O -0.0357(4) 0.2075(3) -0.0468(4) 0.1011(16) Uani 1 1 d . . . C2 C -0.2444(6) 0.1437(5) 0.0331(6) 0.099(3) Uani 1 1 d . . . H2A H -0.3057 0.1114 0.0104 0.118 Uiso 1 1 calc R . . H2B H -0.2320 0.1832 -0.0190 0.118 Uiso 1 1 calc R . . C3 C -0.0594(6) 0.0404(5) -0.1907(5) 0.087(2) Uani 1 1 d . . . H3A H -0.0350 0.0026 -0.2395 0.105 Uiso 1 1 calc R . . H3B H -0.0378 0.0961 -0.2073 0.105 Uiso 1 1 calc R . . C31 C -0.1744(6) 0.0376(6) -0.1998(6) 0.113(3) Uani 1 1 d . . . H4A H -0.2003 0.0787 -0.1555 0.136 Uiso 1 1 calc R . . H4B H -0.1972 -0.0168 -0.1797 0.136 Uiso 1 1 calc R . . C102 C 0.3826(8) 0.0204(5) -0.1816(11) 0.113(3) Uani 1 1 d . . . C104 C 0.2307(10) 0.0268(6) -0.3058(7) 0.113(3) Uani 1 1 d . . . C103 C 0.3356(10) 0.0244(7) -0.2777(8) 0.122(3) Uani 1 1 d . . . H7A H 0.3791 0.0256 -0.3288 0.146 Uiso 1 1 calc R . . C21 C -0.2616(7) 0.1891(6) 0.1274(8) 0.135(4) Uani 1 1 d . . . H8A H -0.2038 0.2263 0.1461 0.162 Uiso 1 1 calc R . . H8B H -0.2664 0.1498 0.1816 0.162 Uiso 1 1 calc R . . C105 C 0.1933(9) 0.0248(7) -0.4152(7) 0.178(5) Uani 1 1 d . . . H9A H 0.1187 0.0262 -0.4236 0.266 Uiso 1 1 calc R . . H9B H 0.2172 -0.0252 -0.4445 0.266 Uiso 1 1 calc R . . H9C H 0.2201 0.0722 -0.4477 0.266 Uiso 1 1 calc R . . C52 C -0.0013(12) 0.1705(12) 0.3291(11) 0.296(11) Uani 1 1 d . . . H11A H 0.0246 0.1905 0.3944 0.445 Uiso 1 1 calc R . . H11B H -0.0106 0.1113 0.3316 0.445 Uiso 1 1 calc R . . H11C H -0.0668 0.1966 0.3083 0.445 Uiso 1 1 calc R . . C101 C 0.5008(7) 0.0161(6) -0.1571(8) 0.161(4) Uani 1 1 d . . . H12A H 0.5174 0.0136 -0.0857 0.242 Uiso 1 1 calc R . . H12B H 0.5320 0.0647 -0.1828 0.242 Uiso 1 1 calc R . . H12C H 0.5270 -0.0326 -0.1872 0.242 Uiso 1 1 calc R . . C1 C 0.2267(10) 0.1803(13) 0.0119(12) 0.233(9) Uani 1 1 d . . . H13A H 0.1897 0.2203 0.0504 0.280 Uiso 1 1 calc R . . C32 C -0.2183(7) 0.0551(8) -0.3065(6) 0.170(5) Uani 1 1 d . . . H16A H -0.2929 0.0535 -0.3111 0.255 Uiso 1 1 calc R . . H16B H -0.1938 0.0137 -0.3501 0.255 Uiso 1 1 calc R . . H16C H -0.1961 0.1091 -0.3261 0.255 Uiso 1 1 calc R . . C5 C 0.0702(16) 0.1897(9) 0.2604(11) 0.249(9) Uani 1 1 d . . . H17A H 0.1355 0.1621 0.2851 0.298 Uiso 1 1 calc R . . C22 C -0.3627(10) 0.2388(8) 0.1089(10) 0.207(6) Uani 1 1 d . . . H18A H -0.3764 0.2665 0.1696 0.311 Uiso 1 1 calc R . . H18B H -0.4191 0.2017 0.0882 0.311 Uiso 1 1 calc R . . H18C H -0.3561 0.2793 0.0574 0.311 Uiso 1 1 calc R . . C4 C -0.0619(18) 0.2886(14) -0.0830(17) 0.255(10) Uani 1 1 d . . . H19A H -0.1368 0.2889 -0.0767 0.305 Uiso 1 1 calc R . . C41 C -0.063(2) 0.2994(14) -0.1685(15) 0.329(14) Uani 1 1 d . . . H20A H -0.0874 0.3545 -0.1849 0.493 Uiso 1 1 calc R . . H20B H -0.1076 0.2594 -0.2040 0.493 Uiso 1 1 calc R . . H20C H 0.0067 0.2933 -0.1875 0.493 Uiso 1 1 calc R . . C51 C 0.0897(17) 0.2622(12) 0.2556(14) 0.307(11) Uiso 1 1 d . . . H24A H 0.1141 0.2825 0.3211 0.461 Uiso 1 1 calc R . . H24B H 0.0280 0.2920 0.2307 0.461 Uiso 1 1 calc R . . H24C H 0.1425 0.2703 0.2112 0.461 Uiso 1 1 calc R . . C12 C 0.2565(11) 0.2269(8) -0.0801(13) 0.243(8) Uani 1 1 d . . . H1A H 0.3001 0.2734 -0.0591 0.364 Uiso 1 1 calc R . . H1B H 0.1948 0.2465 -0.1188 0.364 Uiso 1 1 calc R . . H1C H 0.2936 0.1901 -0.1203 0.364 Uiso 1 1 calc R . . C11 C 0.3006(15) 0.1630(12) 0.0610(14) 0.283(10) Uiso 1 1 d . . . H10A H 0.3435 0.2115 0.0727 0.425 Uiso 1 1 calc R . . H10B H 0.3378 0.1213 0.0279 0.425 Uiso 1 1 calc R . . H10C H 0.2828 0.1416 0.1238 0.425 Uiso 1 1 calc R . . C42 C -0.0298(15) 0.3612(9) -0.0232(13) 0.279(11) Uani 1 1 d . . . H14A H -0.0602 0.4102 -0.0549 0.418 Uiso 1 1 calc R . . H14B H 0.0446 0.3658 -0.0175 0.418 Uiso 1 1 calc R . . H14C H -0.0527 0.3556 0.0424 0.418 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 0.0620(4) 0.0739(5) 0.0602(5) -0.0057(4) 0.0089(3) -0.0001(4) Co1 0.0774(7) 0.0934(8) 0.0700(7) -0.0029(6) 0.0186(5) 0.0006(6) O1 0.056(3) 0.096(3) 0.089(4) -0.020(3) 0.016(2) -0.014(3) O2 0.057(3) 0.090(3) 0.078(3) 0.005(3) 0.011(2) 0.013(3) O3 0.077(3) 0.075(3) 0.050(3) 0.000(2) 0.003(2) 0.004(2) O7 0.076(4) 0.113(4) 0.117(5) -0.008(4) 0.037(3) -0.005(3) O5 0.091(4) 0.110(4) 0.081(4) -0.036(3) 0.013(3) -0.010(3) O6 0.106(4) 0.133(5) 0.074(4) 0.006(3) 0.032(3) 0.000(4) O4 0.101(4) 0.091(4) 0.114(4) 0.020(3) 0.024(3) 0.008(3) C2 0.100(7) 0.101(6) 0.100(7) 0.010(5) 0.031(5) 0.018(5) C3 0.108(7) 0.099(6) 0.053(5) 0.000(4) 0.003(4) 0.009(5) C31 0.077(6) 0.175(9) 0.084(6) -0.005(6) -0.007(5) 0.021(6) C102 0.096(8) 0.092(6) 0.160(11) 0.003(7) 0.064(8) -0.001(5) C104 0.134(9) 0.123(8) 0.085(8) 0.008(6) 0.029(7) -0.005(7) C103 0.133(10) 0.155(9) 0.087(8) 0.007(7) 0.055(7) -0.002(8) C21 0.096(7) 0.113(7) 0.199(11) -0.022(8) 0.026(7) 0.033(6) C105 0.237(14) 0.235(13) 0.067(7) 0.016(8) 0.048(7) 0.003(10) C52 0.269(19) 0.47(3) 0.159(14) -0.145(18) 0.077(13) -0.096(19) C101 0.087(7) 0.194(11) 0.213(12) -0.008(9) 0.065(7) 0.006(7) C1 0.101(10) 0.40(3) 0.204(15) -0.170(16) 0.058(10) -0.034(13) C32 0.127(8) 0.287(14) 0.086(7) 0.002(8) -0.043(6) 0.057(9) C5 0.42(3) 0.168(14) 0.177(15) -0.075(12) 0.122(15) -0.075(15) C22 0.186(12) 0.207(13) 0.235(15) -0.010(11) 0.049(10) 0.068(10) C4 0.36(2) 0.190(18) 0.22(2) 0.106(19) 0.04(2) -0.032(17) C41 0.53(4) 0.24(2) 0.22(2) 0.07(2) 0.04(3) 0.01(2) C12 0.228(16) 0.161(12) 0.37(2) 0.031(14) 0.175(17) 0.015(11) C42 0.45(3) 0.101(10) 0.29(2) -0.014(12) 0.10(2) 0.032(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O5 1.904(5) . ? Zr1 O4 1.921(5) . ? Zr1 O1 2.102(4) . ? Zr1 O2 2.110(4) . ? Zr1 O3 2.215(4) . ? Zr1 O3 2.222(4) 3 ? Zr1 Zr1 3.6484(18) 3 ? Co1 O6 1.919(5) . ? Co1 O1 1.944(5) . ? Co1 O2 1.949(5) 3 ? Co1 O7 2.001(5) . ? O1 C1 1.501(17) . ? O2 C2 1.443(8) . ? O2 Co1 1.949(5) 3 ? O3 C3 1.456(7) . ? O3 Zr1 2.222(4) 3 ? O7 C102 1.263(11) . ? O5 C5 1.450(14) . ? O6 C104 1.273(10) . ? O4 C4 1.420(19) . ? C2 C21 1.496(10) . ? C3 C31 1.480(9) . ? C31 C32 1.511(10) . ? C102 C103 1.370(13) . ? C102 C101 1.531(12) . ? C104 C103 1.371(12) . ? C104 C105 1.498(12) . ? C21 C22 1.530(12) . ? C52 C5 1.404(16) . ? C1 C11 1.14(2) . ? C1 C12 1.53(2) . ? C5 C51 1.20(2) . ? C4 C41 1.16(2) . ? C4 C42 1.45(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zr1 O4 101.7(2) . . ? O5 Zr1 O1 93.67(19) . . ? O4 Zr1 O1 94.1(2) . . ? O5 Zr1 O2 96.81(18) . . ? O4 Zr1 O2 90.49(19) . . ? O1 Zr1 O2 167.47(18) . . ? O5 Zr1 O3 159.24(19) . . ? O4 Zr1 O3 97.7(2) . . ? O1 Zr1 O3 77.63(17) . . ? O2 Zr1 O3 90.21(16) . . ? O5 Zr1 O3 92.72(19) . 3 ? O4 Zr1 O3 163.17(19) . 3 ? O1 Zr1 O3 93.58(17) . 3 ? O2 Zr1 O3 79.13(16) . 3 ? O3 Zr1 O3 69.38(17) . 3 ? O5 Zr1 Zr1 126.62(16) . 3 ? O4 Zr1 Zr1 131.66(16) . 3 ? O1 Zr1 Zr1 84.72(13) . 3 ? O2 Zr1 Zr1 83.53(12) . 3 ? O3 Zr1 Zr1 34.76(11) . 3 ? O3 Zr1 Zr1 34.62(10) 3 3 ? O6 Co1 O1 126.9(2) . . ? O6 Co1 O2 114.1(2) . 3 ? O1 Co1 O2 111.7(2) . 3 ? O6 Co1 O7 92.5(2) . . ? O1 Co1 O7 103.4(2) . . ? O2 Co1 O7 101.5(2) 3 . ? C1 O1 Co1 122.0(5) . . ? C1 O1 Zr1 121.1(5) . . ? Co1 O1 Zr1 114.3(2) . . ? C2 O2 Co1 117.5(4) . 3 ? C2 O2 Zr1 129.7(4) . . ? Co1 O2 Zr1 112.7(2) 3 . ? C3 O3 Zr1 120.8(4) . . ? C3 O3 Zr1 123.5(4) . 3 ? Zr1 O3 Zr1 110.62(17) . 3 ? C102 O7 Co1 124.5(7) . . ? C5 O5 Zr1 177.1(7) . . ? C104 O6 Co1 125.0(6) . . ? C4 O4 Zr1 166.7(11) . . ? O2 C2 C21 108.9(7) . . ? O3 C3 C31 114.6(6) . . ? C3 C31 C32 110.4(7) . . ? O7 C102 C103 124.9(9) . . ? O7 C102 C101 112.4(11) . . ? C103 C102 C101 122.7(10) . . ? O6 C104 C103 126.4(9) . . ? O6 C104 C105 114.9(10) . . ? C103 C104 C105 118.7(10) . . ? C102 C103 C104 126.2(9) . . ? C2 C21 C22 108.4(9) . . ? C11 C1 O1 112(2) . . ? C11 C1 C12 108.7(17) . . ? O1 C1 C12 116.4(12) . . ? C51 C5 C52 113.9(19) . . ? C51 C5 O5 109.4(17) . . ? C52 C5 O5 114.0(14) . . ? C41 C4 O4 117(3) . . ? C41 C4 C42 114(2) . . ? O4 C4 C42 120.2(18) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.491 _refine_diff_density_min -0.465 _refine_diff_density_rms 0.068 data_zrprac1m _database_code_depnum_ccdc_archive 'CCDC 234687' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H56 O10 Zr2' _chemical_formula_weight 735.17 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 9.818(8) _cell_length_b 10.639(11) _cell_length_c 11.790(12) _cell_angle_alpha 87.86(4) _cell_angle_beta 68.83(3) _cell_angle_gamma 64.64(5) _cell_volume 1027.7(17) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 994(I>2sigma(I)) _cell_measurement_theta_min 1.87 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.188 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 384 _exptl_absorpt_coefficient_mu 0.547 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8109 _exptl_absorpt_correction_T_max 0.9224 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4918 _diffrn_reflns_av_R_equivalents 0.0219 _diffrn_reflns_av_sigmaI/netI 0.0673 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3491 _reflns_number_gt 2223 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0599P)^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 3491 _refine_ls_number_parameters 181 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0815 _refine_ls_R_factor_gt 0.0451 _refine_ls_wR_factor_ref 0.1104 _refine_ls_wR_factor_gt 0.1016 _refine_ls_goodness_of_fit_ref 0.890 _refine_ls_restrained_S_all 0.890 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr -0.13827(5) 0.07917(4) 0.15213(4) 0.06162(19) Uani 1 1 d . . . O1 O 0.1136(3) -0.0055(3) 0.0346(2) 0.0611(7) Uani 1 1 d . . . O2 O -0.1313(4) 0.1642(3) 0.2929(3) 0.0859(9) Uani 1 1 d . . . O3 O -0.4021(4) 0.1879(3) 0.2146(3) 0.0823(9) Uani 1 1 d . . . O4 O -0.1806(4) 0.2826(3) 0.0766(3) 0.0818(9) Uani 1 1 d . . . O5 O -0.1532(4) -0.0877(3) 0.2164(3) 0.0844(9) Uani 1 1 d . . . C2 C -0.5069(6) 0.3191(6) 0.2229(5) 0.0877(15) Uani 1 1 d . . . C3 C -0.4632(8) 0.4236(6) 0.1701(6) 0.1067(19) Uani 1 1 d . . . H2A H -0.5457 0.5146 0.1841 0.128 Uiso 1 1 calc R . . C6 C 0.2541(6) -0.0116(6) 0.0564(5) 0.0976(17) Uani 1 1 d . . . H3A H 0.3498 -0.0611 -0.0192 0.117 Uiso 1 1 calc R . . C4 C -0.3047(8) 0.4000(5) 0.0984(5) 0.0890(16) Uani 1 1 d . . . C62 C 0.2387(8) 0.1354(8) 0.0730(6) 0.146(3) Uani 1 1 d . . . H5A H 0.2222 0.1817 0.0044 0.219 Uiso 1 1 calc R . . H5B H 0.3367 0.1296 0.0780 0.219 Uiso 1 1 calc R . . H5C H 0.1475 0.1877 0.1473 0.219 Uiso 1 1 calc R . . C1 C -0.6846(7) 0.3498(7) 0.2994(6) 0.136(3) Uani 1 1 d . . . H6A H -0.6887 0.2646 0.3260 0.204 Uiso 1 1 calc R . . H6B H -0.7487 0.3860 0.2501 0.204 Uiso 1 1 calc R . . H6C H -0.7273 0.4178 0.3697 0.204 Uiso 1 1 calc R . . C5 C -0.2726(9) 0.5225(6) 0.0432(7) 0.139(3) Uani 1 1 d . . . H7A H -0.1581 0.4894 -0.0043 0.209 Uiso 1 1 calc R . . H7B H -0.3072 0.5945 0.1082 0.209 Uiso 1 1 calc R . . H7C H -0.3325 0.5603 -0.0087 0.209 Uiso 1 1 calc R . . C8 C -0.1508(11) 0.2380(8) 0.3997(7) 0.142(3) Uani 1 1 d . . . H8A H -0.0428 0.1999 0.4039 0.170 Uiso 1 1 calc R . . C61 C 0.2799(9) -0.1014(8) 0.1544(7) 0.158(3) Uani 1 1 d . . . H9A H 0.2891 -0.1914 0.1324 0.236 Uiso 1 1 calc R . . H9B H 0.1890 -0.0569 0.2309 0.236 Uiso 1 1 calc R . . H9C H 0.3782 -0.1134 0.1630 0.236 Uiso 1 1 calc R . . C7 C -0.1875(12) -0.1875(11) 0.2813(10) 0.197(4) Uani 1 1 d . . . H10 H -0.1505 -0.2543 0.2092 0.237 Uiso 1 1 calc R . . C82 C -0.1974(19) 0.3814(10) 0.3889(10) 0.306(9) Uani 1 1 d . . . H11A H -0.2100 0.4290 0.4623 0.459 Uiso 1 1 calc R . . H11B H -0.2989 0.4217 0.3776 0.459 Uiso 1 1 calc R . . H11C H -0.1149 0.3911 0.3196 0.459 Uiso 1 1 calc R . . C72 C -0.0715(15) -0.2745(13) 0.3268(13) 0.305(8) Uani 1 1 d . . . H12A H 0.0324 -0.2775 0.2783 0.457 Uiso 1 1 calc R . . H12B H -0.0633 -0.3676 0.3228 0.457 Uiso 1 1 calc R . . H12C H -0.1036 -0.2385 0.4105 0.457 Uiso 1 1 calc R . . C71 C -0.3499(13) -0.1651(12) 0.3261(11) 0.248(6) Uani 1 1 d . . . H13A H -0.4058 -0.1016 0.2801 0.372 Uiso 1 1 calc R . . H13B H -0.4020 -0.1254 0.4112 0.372 Uiso 1 1 calc R . . H13C H -0.3536 -0.2529 0.3179 0.372 Uiso 1 1 calc R . . C81 C -0.2502(18) 0.2121(16) 0.5044(8) 0.326(10) Uani 1 1 d . . . H14A H -0.2090 0.1126 0.5059 0.489 Uiso 1 1 calc R . . H14B H -0.3586 0.2497 0.5052 0.489 Uiso 1 1 calc R . . H14C H -0.2524 0.2559 0.5751 0.489 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 0.0545(3) 0.0579(3) 0.0691(3) 0.00415(18) -0.0194(2) -0.0252(2) O1 0.0506(17) 0.0618(16) 0.0729(18) 0.0023(14) -0.0257(14) -0.0246(14) O2 0.086(2) 0.094(2) 0.074(2) -0.0063(18) -0.0267(18) -0.0376(19) O3 0.057(2) 0.081(2) 0.091(2) -0.0087(17) -0.0162(17) -0.0230(18) O4 0.085(2) 0.0557(18) 0.100(2) 0.0097(16) -0.0343(19) -0.0276(18) O5 0.088(2) 0.077(2) 0.091(2) 0.0281(17) -0.0282(19) -0.0463(19) C2 0.058(3) 0.101(4) 0.086(4) -0.024(3) -0.025(3) -0.019(3) C3 0.094(5) 0.066(3) 0.135(5) -0.002(3) -0.047(4) -0.009(3) C6 0.057(3) 0.135(5) 0.104(4) -0.015(4) -0.035(3) -0.040(3) C4 0.104(5) 0.062(3) 0.106(4) 0.006(3) -0.055(4) -0.029(3) C62 0.132(6) 0.193(7) 0.159(6) -0.022(5) -0.038(5) -0.123(6) C1 0.068(4) 0.150(6) 0.140(6) -0.038(5) -0.017(4) -0.020(4) C5 0.173(7) 0.072(4) 0.179(7) 0.035(4) -0.080(6) -0.052(4) C8 0.166(8) 0.146(6) 0.098(5) -0.031(5) -0.036(5) -0.065(6) C61 0.116(6) 0.191(7) 0.176(7) 0.027(6) -0.108(6) -0.033(5) C7 0.169(9) 0.218(9) 0.302(12) 0.182(9) -0.135(9) -0.145(8) C82 0.56(3) 0.140(8) 0.220(11) -0.028(8) -0.194(14) -0.120(12) C72 0.236(13) 0.300(14) 0.44(2) 0.293(15) -0.174(14) -0.157(11) C71 0.184(11) 0.312(14) 0.312(14) 0.161(11) -0.087(10) -0.183(11) C81 0.45(2) 0.49(2) 0.094(7) -0.047(10) 0.025(10) -0.36(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 O5 1.947(3) . ? Zr1 O2 1.955(3) . ? Zr1 O1 2.134(3) . ? Zr1 O3 2.170(4) . ? Zr1 O4 2.236(4) . ? Zr1 O1 2.258(3) 2 ? Zr1 Zr1 3.546(4) 2 ? O1 C6 1.468(5) . ? O1 Zr1 2.258(3) 2 ? O2 C8 1.418(6) . ? O3 C2 1.313(6) . ? O4 C4 1.267(6) . ? O5 C7 1.373(7) . ? C2 C3 1.405(8) . ? C2 C1 1.536(7) . ? C3 C4 1.389(8) . ? C6 C61 1.494(8) . ? C6 C62 1.519(8) . ? C4 C5 1.537(8) . ? C8 C81 1.374(11) . ? C8 C82 1.407(11) . ? C7 C72 1.394(11) . ? C7 C71 1.398(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Zr1 O2 99.38(15) . . ? O5 Zr1 O1 101.38(14) . . ? O2 Zr1 O1 99.23(14) . . ? O5 Zr1 O3 89.77(14) . . ? O2 Zr1 O3 94.27(14) . . ? O1 Zr1 O3 160.76(11) . . ? O5 Zr1 O4 165.86(13) . . ? O2 Zr1 O4 87.56(15) . . ? O1 Zr1 O4 89.53(13) . . ? O3 Zr1 O4 77.37(13) . . ? O5 Zr1 O1 91.84(13) . 2 ? O2 Zr1 O1 167.22(12) . 2 ? O1 Zr1 O1 72.36(12) . 2 ? O3 Zr1 O1 91.86(12) . 2 ? O4 Zr1 O1 82.84(13) . 2 ? O5 Zr1 Zr1 98.00(12) . 2 ? O2 Zr1 Zr1 135.85(12) . 2 ? O1 Zr1 Zr1 37.36(7) . 2 ? O3 Zr1 Zr1 126.08(10) . 2 ? O4 Zr1 Zr1 85.16(11) . 2 ? O1 Zr1 Zr1 35.00(8) 2 2 ? C6 O1 Zr1 130.8(3) . . ? C6 O1 Zr1 121.4(3) . 2 ? Zr1 O1 Zr1 107.64(12) . 2 ? C8 O2 Zr1 171.7(4) . . ? C2 O3 Zr1 133.8(3) . . ? C4 O4 Zr1 133.8(4) . . ? C7 O5 Zr1 168.9(6) . . ? O3 C2 C3 124.1(5) . . ? O3 C2 C1 113.5(5) . . ? C3 C2 C1 122.4(5) . . ? C4 C3 C2 124.3(5) . . ? O1 C6 C61 109.3(5) . . ? O1 C6 C62 110.1(5) . . ? C61 C6 C62 117.8(6) . . ? O4 C4 C3 124.2(5) . . ? O4 C4 C5 116.3(6) . . ? C3 C4 C5 119.5(5) . . ? C81 C8 C82 114.5(10) . . ? C81 C8 O2 111.5(8) . . ? C82 C8 O2 111.0(7) . . ? O5 C7 C72 115.6(8) . . ? O5 C7 C71 116.6(8) . . ? C72 C7 C71 124.7(9) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.446 _refine_diff_density_min -0.665 _refine_diff_density_rms 0.063 data_zrcopr2m _database_code_depnum_ccdc_archive 'CCDC 234688' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H70 Co O12 Zr2' _chemical_formula_weight 912.27 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' Co Co 0.3494 0.9721 '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 Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.601(12) _cell_length_b 9.408(4) _cell_length_c 17.851(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.580(8) _cell_angle_gamma 90.00 _cell_volume 4871(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 658(I>2sigma(I)) _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 17.00 _exptl_crystal_description plate _exptl_crystal_colour purple _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1908 _exptl_absorpt_coefficient_mu 0.803 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6897 _exptl_absorpt_correction_T_max 0.9610 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4880 _diffrn_reflns_av_R_equivalents 0.1846 _diffrn_reflns_av_sigmaI/netI 0.1619 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 17.00 _reflns_number_total 1403 _reflns_number_gt 734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0000P)^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 1403 _refine_ls_number_parameters 222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1227 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.0822 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 0.809 _refine_ls_restrained_S_all 0.809 _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 Co1 Co 0.0000 0.1818(3) 0.2500 0.0961(10) Uani 1 2 d S . . Zr1 Zr 0.10834(4) 0.20523(18) 0.31299(8) 0.1071(8) Uani 1 1 d . . . O1 O 0.0499(3) 0.2782(11) 0.2270(6) 0.112(3) Uani 1 1 d . . . O2 O 0.0510(3) 0.0901(10) 0.3286(6) 0.100(3) Uani 1 1 d . . . O3 O 0.1527(3) 0.2909(12) 0.2709(5) 0.145(3) Uani 1 1 d . . . O5 O 0.1547(4) 0.0696(15) 0.3942(7) 0.153(5) Uani 1 1 d . . . O4 O 0.1122(3) 0.3424(11) 0.3963(6) 0.139(4) Uani 1 1 d . . . O6 O 0.1096(4) 0.0233(14) 0.2395(8) 0.146(5) Uani 1 1 d . . . C1 C 0.0501(9) 0.404(5) 0.1680(16) 0.28(2) Uani 1 1 d . . . C11 C 0.0363(15) 0.504(5) 0.186(2) 0.51(4) Uani 1 1 d . . . H11A H 0.0362 0.5788 0.1494 0.771 Uiso 1 1 calc R . . H11B H 0.0554 0.5317 0.2381 0.771 Uiso 1 1 calc R . . H11C H 0.0054 0.4885 0.1868 0.771 Uiso 1 1 calc R . . C12 C 0.0397(10) 0.337(2) 0.0997(15) 0.292(15) Uani 1 1 d . . . H1A H 0.0386 0.4045 0.0587 0.437 Uiso 1 1 calc R . . H1B H 0.0103 0.2920 0.0888 0.437 Uiso 1 1 calc R . . H1C H 0.0628 0.2668 0.1019 0.437 Uiso 1 1 calc R . . C2 C 0.0478(7) -0.020(3) 0.3791(13) 0.201(12) Uani 1 1 d . . . H2A H 0.0682 -0.0957 0.3724 0.241 Uiso 1 1 calc R . . C21 C 0.0657(7) 0.025(2) 0.4599(14) 0.254(11) Uani 1 1 d . . . H17A H 0.0659 -0.0536 0.4941 0.381 Uiso 1 1 calc R . . H17B H 0.0467 0.0998 0.4693 0.381 Uiso 1 1 calc R . . H17C H 0.0966 0.0597 0.4703 0.381 Uiso 1 1 calc R . . C22 C 0.0081(9) -0.078(3) 0.3684(13) 0.308(17) Uani 1 1 d . . . H28A H -0.0037 -0.1135 0.3153 0.461 Uiso 1 1 calc R . . H28B H -0.0128 -0.0090 0.3771 0.461 Uiso 1 1 calc R . . H28C H 0.0113 -0.1555 0.4049 0.461 Uiso 1 1 calc R . . C3 C 0.1870(7) 0.345(4) 0.246(2) 0.311(19) Uani 1 1 d . . . H24A H 0.1749 0.4292 0.2136 0.374 Uiso 1 1 calc R . . C31 C 0.1958(10) 0.223(4) 0.1899(18) 0.38(2) Uani 1 1 d . . . H40A H 0.2177 0.2558 0.1655 0.572 Uiso 1 1 calc R . . H40B H 0.1674 0.1999 0.1498 0.572 Uiso 1 1 calc R . . H40C H 0.2077 0.1397 0.2209 0.572 Uiso 1 1 calc R . . C32 C 0.2264(9) 0.378(4) 0.2961(18) 0.53(4) Uani 1 1 d . . . H38A H 0.2463 0.4132 0.2682 0.790 Uiso 1 1 calc R . . H38B H 0.2399 0.2955 0.3259 0.790 Uiso 1 1 calc R . . H38C H 0.2223 0.4504 0.3312 0.790 Uiso 1 1 calc R . . C4 C 0.1300(11) 0.426(4) 0.4674(18) 0.305(17) Uani 1 1 d . . . H20A H 0.1099 0.4009 0.4986 0.366 Uiso 1 1 calc R . . C41 C 0.1716(10) 0.386(4) 0.5128(14) 0.42(3) Uani 1 1 d . . . H3A H 0.1800 0.4379 0.5615 0.636 Uiso 1 1 calc R . . H3B H 0.1936 0.4038 0.4858 0.636 Uiso 1 1 calc R . . H3C H 0.1712 0.2858 0.5238 0.636 Uiso 1 1 calc R . . C42 C 0.1174(12) 0.571(4) 0.4439(19) 0.40(2) Uani 1 1 d . . . H19A H 0.1260 0.6311 0.4898 0.598 Uiso 1 1 calc R . . H19B H 0.0847 0.5768 0.4183 0.598 Uiso 1 1 calc R . . H19C H 0.1331 0.6016 0.4080 0.598 Uiso 1 1 calc R . . C51 C 0.2120(8) -0.086(4) 0.4733(17) 0.39(3) Uani 1 1 d . . . H35A H 0.2140 -0.0201 0.5153 0.581 Uiso 1 1 calc R . . H35B H 0.2418 -0.0970 0.4671 0.581 Uiso 1 1 calc R . . H35C H 0.2015 -0.1764 0.4859 0.581 Uiso 1 1 calc R . . C52 C 0.1827(15) -0.038(5) 0.407(3) 0.29(2) Uani 1 1 d . . . C53 C 0.1709(9) -0.101(4) 0.336(2) 0.237(17) Uani 1 1 d . . . H47A H 0.1892 -0.1816 0.3386 0.284 Uiso 1 1 calc R . . C54 C 0.1388(10) -0.087(3) 0.254(2) 0.219(15) Uani 1 1 d . . . C55 C 0.1301(6) -0.169(2) 0.1784(13) 0.241(10) Uani 1 1 d . . . H13A H 0.1503 -0.2500 0.1876 0.361 Uiso 1 1 calc R . . H13B H 0.1358 -0.1092 0.1390 0.361 Uiso 1 1 calc R . . H13C H 0.0986 -0.2010 0.1603 0.361 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 Co1 0.0972(19) 0.076(2) 0.116(2) 0.000 0.0349(17) 0.000 Zr1 0.1023(12) 0.0884(12) 0.1299(13) 0.0149(13) 0.0358(9) 0.0022(11) O1 0.097(6) 0.110(9) 0.130(8) 0.000(7) 0.037(6) 0.002(6) O2 0.106(7) 0.085(8) 0.111(8) 0.012(6) 0.036(6) 0.015(6) O3 0.088(7) 0.134(9) 0.213(9) 0.029(8) 0.049(7) 0.009(7) O5 0.108(9) 0.170(14) 0.170(10) 0.067(10) 0.029(8) 0.016(8) O4 0.176(9) 0.122(11) 0.113(7) -0.025(8) 0.039(7) -0.016(7) O6 0.144(11) 0.131(12) 0.169(10) -0.024(9) 0.059(8) 0.002(8) C1 0.23(2) 0.46(7) 0.13(2) 0.00(3) 0.03(2) 0.15(3) C11 0.84(9) 0.39(6) 0.56(7) 0.32(5) 0.57(7) 0.34(6) C12 0.53(5) 0.13(3) 0.24(3) 0.08(2) 0.16(3) -0.03(3) C2 0.17(2) 0.31(4) 0.115(19) 0.01(2) 0.036(18) -0.11(2) C21 0.33(3) 0.20(3) 0.24(2) 0.08(2) 0.10(2) -0.11(2) C22 0.33(3) 0.29(3) 0.23(2) 0.12(2) -0.03(2) -0.16(3) C3 0.063(17) 0.47(6) 0.39(4) 0.09(4) 0.05(2) 0.01(3) C31 0.33(4) 0.50(7) 0.38(4) -0.08(4) 0.19(3) 0.01(4) C32 0.119(19) 0.92(11) 0.55(5) -0.22(6) 0.12(3) -0.21(4) C4 0.32(4) 0.19(3) 0.26(4) -0.09(3) -0.12(3) -0.05(3) C41 0.35(4) 0.51(7) 0.24(3) -0.01(3) -0.14(3) -0.15(4) C42 0.68(7) 0.15(3) 0.28(3) -0.06(3) 0.03(3) -0.07(4) C51 0.22(3) 0.44(5) 0.39(4) 0.27(4) -0.06(2) 0.10(3) C52 0.20(4) 0.26(6) 0.35(6) -0.05(4) 0.01(4) 0.00(3) C53 0.14(2) 0.18(3) 0.33(5) 0.08(3) 0.00(3) 0.03(2) C54 0.18(3) 0.24(4) 0.30(4) -0.14(4) 0.15(3) -0.06(3) C55 0.25(2) 0.23(3) 0.28(2) -0.07(2) 0.129(17) 0.057(18) _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 Co1 O1 1.928(9) 2 ? Co1 O1 1.928(9) . ? Co1 O2 1.937(8) 2 ? Co1 O2 1.937(8) . ? Co1 Zr1 3.1511(18) . ? Co1 Zr1 3.1511(18) 2 ? Zr1 O3 1.923(10) . ? Zr1 O4 1.944(11) . ? Zr1 O1 2.068(10) . ? Zr1 O5 2.106(11) . ? Zr1 O2 2.154(10) . ? Zr1 O6 2.164(13) . ? O1 C1 1.58(4) . ? O2 C2 1.40(2) . ? O3 C3 1.36(2) . ? O5 C52 1.30(5) . ? O4 C4 1.45(3) . ? O6 C54 1.34(3) . ? C1 C11 1.13(4) . ? C1 C12 1.32(3) . ? C2 C22 1.29(2) . ? C2 C21 1.44(2) . ? C3 C32 1.29(3) . ? C3 C31 1.61(4) . ? C4 C41 1.33(3) . ? C4 C42 1.44(3) . ? C51 C52 1.32(4) . ? C52 C53 1.35(4) . ? C53 C54 1.48(3) . ? C54 C55 1.51(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 O1 Co1 O1 123.9(6) 2 . ? O1 Co1 O2 81.6(5) 2 2 ? O1 Co1 O2 124.4(4) . 2 ? O1 Co1 O2 124.4(4) 2 . ? O1 Co1 O2 81.6(4) . . ? O2 Co1 O2 127.1(6) 2 . ? O1 Co1 Zr1 134.9(3) 2 . ? O1 Co1 Zr1 39.6(3) . . ? O2 Co1 Zr1 143.4(3) 2 . ? O2 Co1 Zr1 42.2(3) . . ? O1 Co1 Zr1 39.6(3) 2 2 ? O1 Co1 Zr1 134.9(3) . 2 ? O2 Co1 Zr1 42.2(3) 2 2 ? O2 Co1 Zr1 143.4(3) . 2 ? Zr1 Co1 Zr1 171.99(12) . 2 ? O3 Zr1 O4 98.2(4) . . ? O3 Zr1 O1 97.0(4) . . ? O4 Zr1 O1 100.0(4) . . ? O3 Zr1 O5 96.8(4) . . ? O4 Zr1 O5 90.7(5) . . ? O1 Zr1 O5 161.1(5) . . ? O3 Zr1 O2 164.9(4) . . ? O4 Zr1 O2 95.1(4) . . ? O1 Zr1 O2 73.4(4) . . ? O5 Zr1 O2 90.2(4) . . ? O3 Zr1 O6 86.8(5) . . ? O4 Zr1 O6 168.5(4) . . ? O1 Zr1 O6 89.5(4) . . ? O5 Zr1 O6 78.4(5) . . ? O2 Zr1 O6 81.6(4) . . ? O3 Zr1 Co1 133.0(3) . . ? O4 Zr1 Co1 96.9(3) . . ? O1 Zr1 Co1 36.4(3) . . ? O5 Zr1 Co1 127.2(3) . . ? O2 Zr1 Co1 37.2(2) . . ? O6 Zr1 Co1 87.1(3) . . ? C1 O1 Co1 131.6(12) . . ? C1 O1 Zr1 123.7(12) . . ? Co1 O1 Zr1 104.0(5) . . ? C2 O2 Co1 126.2(11) . . ? C2 O2 Zr1 133.2(11) . . ? Co1 O2 Zr1 100.6(5) . . ? C3 O3 Zr1 175.0(12) . . ? C52 O5 Zr1 149(2) . . ? C4 O4 Zr1 161.5(16) . . ? C54 O6 Zr1 129.2(19) . . ? C11 C1 C12 132(4) . . ? C11 C1 O1 111(3) . . ? C12 C1 O1 102(3) . . ? C22 C2 O2 118(2) . . ? C22 C2 C21 108(2) . . ? O2 C2 C21 110(2) . . ? C32 C3 O3 121(3) . . ? C32 C3 C31 107(3) . . ? O3 C3 C31 103(3) . . ? C41 C4 O4 113(3) . . ? C41 C4 C42 124(3) . . ? O4 C4 C42 106(3) . . ? O5 C52 C51 131(4) . . ? O5 C52 C53 102(5) . . ? C51 C52 C53 127(5) . . ? C52 C53 C54 141(5) . . ? O6 C54 C53 117(3) . . ? O6 C54 C55 108(3) . . ? C53 C54 C55 135(4) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 17.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.296 _refine_diff_density_min -0.179 _refine_diff_density_rms 0.051 data_cozr322 _database_code_depnum_ccdc_archive 'CCDC 234689' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H84 Co O17 Zr3' _chemical_formula_weight 1217.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 '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 12.123(7) _cell_length_b 12.823(7) _cell_length_c 21.622(14) _cell_angle_alpha 81.457(15) _cell_angle_beta 76.054(9) _cell_angle_gamma 64.937(10) _cell_volume 2951(3) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 994(I>10sigma(I)) _cell_measurement_theta_min 1.76 _cell_measurement_theta_max 19.00 _exptl_crystal_description block _exptl_crystal_colour 'pinkish purple' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.29 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6523 _exptl_absorpt_correction_T_max 0.7908 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7874 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1430 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 19.00 _reflns_number_total 4689 _reflns_number_gt 2292 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1292P)^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 4689 _refine_ls_number_parameters 571 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1725 _refine_ls_R_factor_gt 0.0784 _refine_ls_wR_factor_ref 0.2126 _refine_ls_wR_factor_gt 0.1810 _refine_ls_goodness_of_fit_ref 0.895 _refine_ls_restrained_S_all 0.896 _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 Co1 Co 0.9044(2) 0.33406(18) 0.28301(11) 0.0727(9) Uani 1 1 d . . . Zr1 Zr 0.77304(17) 0.30805(13) 0.17227(8) 0.0639(7) Uani 1 1 d . . . Zr2 Zr 1.02942(17) 0.07921(13) 0.22788(8) 0.0656(7) Uani 1 1 d . . . Zr3 Zr 0.73203(17) 0.17877(14) 0.32834(8) 0.0678(7) Uani 1 1 d . . . O1 O 0.8523(9) 0.2142(8) 0.2499(4) 0.056(3) Uani 1 1 d . . . O2 O 0.8244(10) 0.4248(9) 0.2126(5) 0.077(4) Uani 1 1 d . . . O3 O 1.0671(11) 0.2077(8) 0.2626(5) 0.070(4) Uani 1 1 d . . . O4 O 0.7829(12) 0.3163(10) 0.3610(5) 0.092(5) Uani 1 1 d . . . O5 O 0.6330(12) 0.3050(9) 0.2595(5) 0.076(4) Uani 1 1 d . . . O6 O 0.9220(11) 0.0477(9) 0.3218(5) 0.078(4) Uani 1 1 d . . . O7 O 0.9681(11) 0.1919(9) 0.1442(5) 0.070(4) Uani 1 1 d . . . O8 O 0.7223(11) 0.2185(10) 0.1308(6) 0.082(4) Uani 1 1 d . . . O9 O 0.9430(14) 0.4485(12) 0.3198(7) 0.097(5) Uani 1 1 d . . . O10 O 1.0175(11) -0.0465(9) 0.1950(5) 0.086(4) Uani 1 1 d . . . O11 O 0.6812(11) 0.0670(9) 0.3090(5) 0.083(4) Uani 1 1 d . . . O12 O 0.6046(12) 0.4641(11) 0.1570(7) 0.100(4) Uani 1 1 d . . . O13 O 0.5454(13) 0.2662(11) 0.3835(7) 0.110(5) Uani 1 1 d . . . O14 O 0.7400(15) 0.1028(12) 0.4266(7) 0.112(5) Uani 1 1 d . . . O15 O 1.2071(14) 0.0436(12) 0.1596(6) 0.098(5) Uani 1 1 d . . . O16 O 0.8298(15) 0.3835(11) 0.0800(7) 0.104(6) Uani 1 1 d . . . O17 O 1.1747(15) -0.0456(11) 0.2794(7) 0.097(5) Uani 1 1 d . . . C1 C 0.5003(17) 0.3594(16) 0.2627(8) 0.066(5) Uani 1 1 d . . . H1A H 0.4636 0.3081 0.2871 0.080 Uiso 1 1 calc R . . H1B H 0.4847 0.3693 0.2198 0.080 Uiso 1 1 calc R . . C2 C 0.4381(18) 0.4712(15) 0.2914(10) 0.103(8) Uani 1 1 d . . . H2A H 0.4679 0.5260 0.2653 0.123 Uiso 1 1 calc R . . H2B H 0.4561 0.4640 0.3335 0.123 Uiso 1 1 calc R . . C3 C 0.2946(18) 0.5148(16) 0.2963(13) 0.178(13) Uani 1 1 d . . . H3A H 0.2528 0.5880 0.3155 0.267 Uiso 1 1 calc R . . H3B H 0.2658 0.4601 0.3220 0.267 Uiso 1 1 calc R . . H3C H 0.2773 0.5232 0.2543 0.267 Uiso 1 1 calc R . . C4 C 0.9612(19) -0.0641(14) 0.3608(10) 0.095(7) Uani 1 1 d . . . H4A H 0.8895 -0.0828 0.3770 0.114 Uiso 1 1 calc R . . H4B H 1.0220 -0.1245 0.3332 0.114 Uiso 1 1 calc R . . C5 C 1.013(2) -0.0633(19) 0.4130(11) 0.143(11) Uani 1 1 d . . . H5A H 0.9538 -0.0034 0.4413 0.171 Uiso 1 1 calc R . . H5B H 1.0875 -0.0488 0.3978 0.171 Uiso 1 1 calc R . . C6 C 1.043(3) -0.180(2) 0.4476(13) 0.234(16) Uani 1 1 d . . . H6A H 1.0778 -0.1818 0.4836 0.351 Uiso 1 1 calc R . . H6B H 1.1027 -0.2379 0.4192 0.351 Uiso 1 1 calc R . . H6C H 0.9690 -0.1932 0.4620 0.351 Uiso 1 1 calc R . . C7 C 1.0314(19) 0.1717(15) 0.0824(9) 0.090(6) Uani 1 1 d . . . H7A H 0.9719 0.1920 0.0550 0.108 Uiso 1 1 calc R . . H7B H 1.0832 0.0899 0.0793 0.108 Uiso 1 1 calc R . . C8 C 1.111(2) 0.2372(16) 0.0585(9) 0.103(7) Uani 1 1 d . . . H8A H 1.1674 0.2195 0.0876 0.123 Uiso 1 1 calc R . . H8B H 1.0582 0.3189 0.0605 0.123 Uiso 1 1 calc R . . C9 C 1.190(2) 0.215(2) -0.0095(11) 0.182(13) Uani 1 1 d . . . H9A H 1.2373 0.2613 -0.0195 0.273 Uiso 1 1 calc R . . H9B H 1.1357 0.2355 -0.0394 0.273 Uiso 1 1 calc R . . H9C H 1.2447 0.1352 -0.0122 0.273 Uiso 1 1 calc R . . C11 C 1.182(2) 0.2033(16) 0.2659(10) 0.091(6) Uani 1 1 d . . . H11A H 1.2460 0.1303 0.2489 0.110 Uiso 1 1 calc R . . C12 C 1.190(2) 0.2037(16) 0.3342(11) 0.142(10) Uani 1 1 d . . . H12A H 1.1735 0.1410 0.3584 0.213 Uiso 1 1 calc R . . H12B H 1.1299 0.2753 0.3517 0.213 Uiso 1 1 calc R . . H12C H 1.2719 0.1950 0.3361 0.213 Uiso 1 1 calc R . . C13 C 1.208(2) 0.2990(19) 0.2255(12) 0.153(10) Uani 1 1 d . . . H13A H 1.2038 0.2948 0.1822 0.229 Uiso 1 1 calc R . . H13B H 1.2893 0.2919 0.2270 0.229 Uiso 1 1 calc R . . H13C H 1.1471 0.3718 0.2413 0.229 Uiso 1 1 calc R . . C21 C 0.804(3) 0.542(2) 0.1895(12) 0.133(9) Uani 1 1 d . . . H21A H 0.7772 0.5564 0.1487 0.160 Uiso 1 1 calc R . . C22 C 0.708(3) 0.6223(17) 0.234(2) 0.30(3) Uani 1 1 d . . . H22A H 0.6315 0.6146 0.2370 0.453 Uiso 1 1 calc R . . H22B H 0.6981 0.6995 0.2188 0.453 Uiso 1 1 calc R . . H22C H 0.7305 0.6061 0.2748 0.453 Uiso 1 1 calc R . . C23 C 0.914(3) 0.552(3) 0.179(2) 0.36(3) Uani 1 1 d . . . H23A H 0.9691 0.5068 0.1435 0.541 Uiso 1 1 calc R . . H23B H 0.9495 0.5243 0.2162 0.541 Uiso 1 1 calc R . . H23C H 0.9007 0.6312 0.1690 0.541 Uiso 1 1 calc R . . C31 C 0.683(3) 0.179(3) 0.0873(15) 0.172(13) Uani 1 1 d . . . H31A H 0.6810 0.1080 0.1107 0.207 Uiso 1 1 calc R . . C32 C 0.544(3) 0.244(2) 0.0846(13) 0.184(13) Uani 1 1 d . . . H32A H 0.4959 0.2580 0.1271 0.277 Uiso 1 1 calc R . . H32B H 0.5190 0.1987 0.0641 0.277 Uiso 1 1 calc R . . H32C H 0.5311 0.3164 0.0608 0.277 Uiso 1 1 calc R . . C33 C 0.762(5) 0.138(5) 0.041(2) 0.52(6) Uani 1 1 d . . . H33A H 0.8411 0.0990 0.0532 0.783 Uiso 1 1 calc R . . H33B H 0.7637 0.1980 0.0093 0.783 Uiso 1 1 calc R . . H33C H 0.7426 0.0837 0.0242 0.783 Uiso 1 1 calc R . . C41 C 0.638(4) -0.007(3) 0.2984(16) 0.23(2) Uani 1 1 d . . . H41A H 0.7175 -0.0547 0.2721 0.275 Uiso 1 1 calc R . . C42 C 0.639(3) -0.097(2) 0.3430(13) 0.202(15) Uani 1 1 d . . . H42A H 0.7037 -0.1151 0.3665 0.304 Uiso 1 1 calc R . . H42B H 0.6548 -0.1640 0.3216 0.304 Uiso 1 1 calc R . . H42C H 0.5604 -0.0751 0.3719 0.304 Uiso 1 1 calc R . . C43 C 0.580(4) 0.015(3) 0.2535(16) 0.28(2) Uani 1 1 d . . . H43A H 0.6027 0.0679 0.2224 0.419 Uiso 1 1 calc R . . H43B H 0.4921 0.0490 0.2703 0.419 Uiso 1 1 calc R . . H43C H 0.6005 -0.0549 0.2337 0.419 Uiso 1 1 calc R . . C51 C 1.019(3) -0.144(2) 0.1599(15) 0.188(12) Uiso 1 1 d D . . H51A H 0.9357 -0.1268 0.1531 0.226 Uiso 1 1 calc R . . C52 C 1.103(4) -0.152(3) 0.1011(15) 0.40(3) Uiso 1 1 d D . . H52A H 1.0970 -0.2027 0.0747 0.594 Uiso 1 1 calc R . . H52B H 1.1865 -0.1828 0.1088 0.594 Uiso 1 1 calc R . . H52C H 1.0843 -0.0773 0.0799 0.594 Uiso 1 1 calc R . . C53 C 1.053(4) -0.234(2) 0.2084(13) 0.32(3) Uani 1 1 d D . . H53A H 1.0549 -0.3034 0.1953 0.479 Uiso 1 1 calc R . . H53B H 0.9940 -0.2120 0.2476 0.479 Uiso 1 1 calc R . . H53C H 1.1343 -0.2485 0.2148 0.479 Uiso 1 1 calc R . . C101 C 0.942(2) 0.5797(19) 0.3819(12) 0.213(15) Uani 1 1 d . . . H10A H 1.0015 0.5875 0.3455 0.320 Uiso 1 1 calc R . . H10B H 0.9787 0.5556 0.4189 0.320 Uiso 1 1 calc R . . H10C H 0.8716 0.6525 0.3887 0.320 Uiso 1 1 calc R . . C102 C 0.894(3) 0.481(2) 0.3691(16) 0.140(11) Uani 1 1 d . . . C103 C 0.800(3) 0.453(3) 0.4165(15) 0.24(2) Uani 1 1 d . . . H10D H 0.7671 0.4937 0.4535 0.286 Uiso 1 1 calc R . . C104 C 0.754(3) 0.371(3) 0.4116(14) 0.170(13) Uani 1 1 d . . . C105 C 0.659(3) 0.378(3) 0.4623(12) 0.229(18) Uani 1 1 d . . . H10E H 0.6260 0.3235 0.4587 0.343 Uiso 1 1 calc R . . H10F H 0.5949 0.4544 0.4626 0.343 Uiso 1 1 calc R . . H10G H 0.6897 0.3607 0.5013 0.343 Uiso 1 1 calc R . . C201 C 0.346(2) 0.3075(19) 0.4504(10) 0.149(10) Uani 1 1 d . . . H20A H 0.3172 0.3648 0.4173 0.224 Uiso 1 1 calc R . . H20B H 0.3269 0.3444 0.4894 0.224 Uiso 1 1 calc R . . H20C H 0.3052 0.2557 0.4565 0.224 Uiso 1 1 calc R . . C202 C 0.478(3) 0.244(2) 0.4326(15) 0.116(9) Uiso 1 1 d . . . C203 C 0.534(3) 0.159(2) 0.4752(12) 0.128(10) Uani 1 1 d . . . H20D H 0.4795 0.1439 0.5099 0.154 Uiso 1 1 calc R . . C204 C 0.659(3) 0.091(2) 0.4758(12) 0.104(8) Uani 1 1 d . . . C205 C 0.715(3) 0.000(2) 0.5260(12) 0.192(14) Uani 1 1 d . . . H20E H 0.8035 -0.0323 0.5132 0.288 Uiso 1 1 calc R . . H20F H 0.6846 -0.0592 0.5307 0.288 Uiso 1 1 calc R . . H20G H 0.6912 0.0357 0.5660 0.288 Uiso 1 1 calc R . . C301 C 0.847(3) 0.4593(19) -0.0267(11) 0.163(13) Uani 1 1 d . . . H30A H 0.9332 0.4111 -0.0287 0.244 Uiso 1 1 calc R . . H30B H 0.8360 0.5380 -0.0368 0.244 Uiso 1 1 calc R . . H30C H 0.8163 0.4355 -0.0568 0.244 Uiso 1 1 calc R . . C302 C 0.780(3) 0.449(2) 0.0355(15) 0.103(10) Uani 1 1 d . . . C303 C 0.648(4) 0.515(2) 0.0485(13) 0.116(11) Uani 1 1 d . . . H30D H 0.6153 0.5563 0.0134 0.139 Uiso 1 1 calc R . . C304 C 0.564(4) 0.525(2) 0.1039(15) 0.115(11) Uani 1 1 d . . . C305 C 0.433(3) 0.603(2) 0.1187(15) 0.197(16) Uani 1 1 d . . . H30E H 0.4071 0.6454 0.0806 0.295 Uiso 1 1 calc R . . H30F H 0.4198 0.6549 0.1498 0.295 Uiso 1 1 calc R . . H30G H 0.3842 0.5580 0.1356 0.295 Uiso 1 1 calc R . . C401 C 1.345(2) -0.1934(19) 0.3179(14) 0.175(12) Uani 1 1 d . . . H40A H 1.2797 -0.1798 0.3551 0.262 Uiso 1 1 calc R . . H40B H 1.4102 -0.1772 0.3263 0.262 Uiso 1 1 calc R . . H40C H 1.3774 -0.2725 0.3075 0.262 Uiso 1 1 calc R . . C402 C 1.293(3) -0.113(2) 0.2607(17) 0.101(8) Uani 1 1 d . . . C403 C 1.357(2) -0.108(2) 0.2017(18) 0.109(10) Uani 1 1 d . . . H40D H 1.4364 -0.1660 0.1930 0.131 Uiso 1 1 calc R . . C404 C 1.321(3) -0.027(3) 0.1500(18) 0.120(10) Uani 1 1 d . . . C405 C 1.408(2) -0.025(2) 0.0920(13) 0.211(16) Uani 1 1 d . . . H40E H 1.3670 0.0347 0.0629 0.317 Uiso 1 1 calc R . . H40F H 1.4428 -0.0982 0.0731 0.317 Uiso 1 1 calc R . . H40G H 1.4740 -0.0107 0.1015 0.317 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 Co1 0.085(2) 0.0577(16) 0.088(2) -0.0149(15) -0.0041(17) -0.0439(16) Zr1 0.0742(16) 0.0533(11) 0.0714(14) -0.0001(9) -0.0055(11) -0.0382(11) Zr2 0.0747(16) 0.0494(11) 0.0779(14) -0.0090(10) -0.0018(11) -0.0355(10) Zr3 0.0752(16) 0.0700(13) 0.0685(14) -0.0082(10) 0.0060(12) -0.0483(12) O1 0.048(8) 0.069(7) 0.067(8) -0.025(6) 0.019(6) -0.048(6) O2 0.096(11) 0.057(7) 0.114(10) 0.003(7) -0.036(8) -0.059(7) O3 0.043(9) 0.067(7) 0.114(10) -0.020(7) -0.020(8) -0.028(7) O4 0.126(13) 0.101(9) 0.054(8) -0.053(7) 0.023(8) -0.056(9) O5 0.065(11) 0.078(8) 0.103(10) -0.031(7) -0.017(8) -0.037(8) O6 0.087(10) 0.073(8) 0.088(9) 0.002(7) 0.000(8) -0.056(8) O7 0.091(10) 0.090(8) 0.042(8) -0.024(7) 0.026(7) -0.063(8) O8 0.076(10) 0.103(9) 0.085(9) 0.014(7) -0.046(8) -0.044(8) O9 0.082(12) 0.129(12) 0.099(11) -0.068(9) 0.023(9) -0.062(10) O10 0.084(10) 0.080(8) 0.108(10) -0.026(7) -0.014(8) -0.041(8) O11 0.086(10) 0.076(8) 0.106(10) -0.010(7) -0.012(8) -0.053(8) O12 0.084(11) 0.088(10) 0.128(13) -0.017(9) -0.012(10) -0.035(9) O13 0.113(13) 0.127(11) 0.097(11) -0.016(9) 0.011(10) -0.068(10) O14 0.126(15) 0.146(12) 0.074(11) -0.019(9) 0.012(10) -0.077(12) O15 0.053(11) 0.124(11) 0.112(11) -0.044(9) 0.031(10) -0.043(9) O16 0.149(16) 0.074(10) 0.088(12) 0.032(8) -0.020(10) -0.056(11) O17 0.091(13) 0.074(9) 0.139(13) -0.002(9) -0.031(12) -0.043(9) C1 0.045(16) 0.110(16) 0.071(14) 0.021(12) -0.027(12) -0.057(13) C2 0.060(18) 0.056(13) 0.20(2) -0.025(14) -0.021(16) -0.023(12) C3 0.035(18) 0.087(15) 0.37(4) -0.06(2) 0.02(2) -0.006(13) C4 0.12(2) 0.065(14) 0.101(18) 0.046(13) -0.008(16) -0.067(14) C5 0.20(3) 0.12(2) 0.11(2) 0.073(17) -0.10(2) -0.06(2) C6 0.27(4) 0.19(3) 0.20(3) 0.12(3) -0.10(3) -0.07(3) C7 0.11(2) 0.085(14) 0.076(17) 0.016(13) -0.021(15) -0.046(15) C8 0.14(2) 0.093(15) 0.070(16) -0.015(12) 0.022(15) -0.059(16) C9 0.23(3) 0.19(3) 0.13(2) -0.069(19) 0.09(2) -0.13(3) C11 0.09(2) 0.087(15) 0.096(18) 0.003(13) -0.037(16) -0.029(14) C12 0.16(3) 0.118(19) 0.21(3) 0.038(18) -0.13(2) -0.075(18) C13 0.12(2) 0.16(2) 0.20(3) -0.040(19) 0.046(19) -0.10(2) C21 0.12(2) 0.10(2) 0.21(3) -0.039(19) -0.01(2) -0.085(19) C22 0.14(3) 0.038(15) 0.70(8) -0.10(3) -0.04(4) -0.010(16) C23 0.28(5) 0.21(4) 0.70(9) 0.18(5) -0.20(6) -0.20(4) C31 0.11(3) 0.29(4) 0.15(3) -0.05(3) 0.00(3) -0.11(3) C32 0.22(4) 0.21(3) 0.18(3) -0.01(2) -0.04(3) -0.15(3) C33 0.40(9) 0.86(13) 0.43(8) -0.49(9) 0.20(6) -0.38(9) C41 0.42(6) 0.24(4) 0.22(4) 0.08(3) -0.22(4) -0.26(4) C42 0.31(4) 0.15(2) 0.20(3) 0.03(2) 0.00(3) -0.18(3) C43 0.45(7) 0.25(4) 0.31(5) 0.06(3) -0.25(5) -0.23(4) C53 0.61(8) 0.16(3) 0.25(4) 0.01(3) -0.17(5) -0.17(4) C101 0.15(3) 0.22(3) 0.35(4) -0.20(3) 0.05(2) -0.14(2) C102 0.09(2) 0.13(2) 0.19(3) -0.09(2) 0.01(2) -0.035(18) C103 0.26(4) 0.25(4) 0.23(4) -0.14(3) 0.15(3) -0.20(4) C104 0.18(3) 0.21(3) 0.15(3) -0.09(2) 0.10(2) -0.15(3) C105 0.21(4) 0.37(5) 0.17(3) -0.20(3) 0.12(3) -0.20(4) C201 0.08(2) 0.19(2) 0.14(2) -0.064(19) 0.035(17) -0.029(19) C203 0.08(2) 0.19(3) 0.11(2) -0.06(2) 0.048(19) -0.06(2) C204 0.09(2) 0.16(2) 0.062(19) -0.021(18) 0.012(19) -0.06(2) C205 0.20(3) 0.27(3) 0.12(2) 0.10(2) -0.06(2) -0.13(3) C301 0.30(4) 0.15(2) 0.085(19) 0.055(17) -0.05(2) -0.14(3) C302 0.13(3) 0.058(18) 0.14(3) -0.013(19) -0.01(3) -0.064(19) C303 0.21(4) 0.11(2) 0.051(18) 0.029(17) -0.04(2) -0.09(2) C304 0.21(4) 0.076(18) 0.09(2) 0.024(18) -0.08(3) -0.07(2) C305 0.16(3) 0.15(3) 0.25(4) 0.04(2) -0.12(3) -0.01(2) C401 0.16(3) 0.11(2) 0.28(4) 0.03(2) -0.08(3) -0.07(2) C402 0.08(3) 0.076(18) 0.16(3) -0.03(2) -0.03(2) -0.034(18) C403 0.05(2) 0.10(2) 0.17(3) -0.07(2) 0.00(2) -0.018(18) C404 0.06(2) 0.13(2) 0.19(4) -0.06(2) -0.01(3) -0.05(2) C405 0.08(2) 0.28(4) 0.20(3) -0.11(3) 0.12(2) -0.04(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 Co1 O3 1.948(11) . ? Co1 O2 1.959(11) . ? Co1 O4 2.010(12) . ? Co1 O9 2.028(12) . ? Co1 O1 2.155(8) . ? Co1 Zr2 3.238(3) . ? Co1 Zr1 3.302(3) . ? Zr1 O8 1.916(12) . ? Zr1 O1 2.095(10) . ? Zr1 O16 2.172(14) . ? Zr1 O7 2.184(12) . ? Zr1 O2 2.197(9) . ? Zr1 O5 2.220(12) . ? Zr1 O12 2.224(14) . ? Zr1 Zr3 3.551(3) . ? Zr1 Zr2 3.570(3) . ? Zr2 O10 1.926(10) . ? Zr2 O1 2.106(10) . ? Zr2 O3 2.157(10) . ? Zr2 O15 2.204(14) . ? Zr2 O7 2.209(12) . ? Zr2 O6 2.216(11) . ? Zr2 O17 2.222(15) . ? Zr2 Zr3 3.535(3) . ? Zr3 O11 1.912(11) . ? Zr3 O1 2.085(9) . ? Zr3 O13 2.178(15) . ? Zr3 O5 2.186(12) . ? Zr3 O6 2.187(12) . ? Zr3 O14 2.209(14) . ? Zr3 O4 2.344(11) . ? O2 C21 1.45(2) . ? O3 C11 1.39(2) . ? O4 C104 1.28(3) . ? O5 C1 1.446(17) . ? O6 C4 1.498(18) . ? O7 C7 1.372(18) . ? O8 C31 1.39(3) . ? O9 C102 1.13(3) . ? O10 C51 1.55(3) . ? O11 C41 1.33(2) . ? O12 C304 1.36(2) . ? O13 C202 1.25(3) . ? O14 C204 1.30(2) . ? O15 C404 1.27(3) . ? O16 C302 1.27(3) . ? O17 C402 1.32(3) . ? C1 C2 1.46(2) . ? C2 C3 1.57(2) . ? C4 C5 1.42(2) . ? C5 C6 1.50(3) . ? C7 C8 1.49(2) . ? C8 C9 1.54(2) . ? C11 C13 1.50(2) . ? C11 C12 1.50(2) . ? C21 C23 1.34(3) . ? C21 C22 1.44(3) . ? C31 C33 1.21(4) . ? C31 C32 1.54(3) . ? C41 C43 1.27(3) . ? C41 C42 1.39(3) . ? C51 C52 1.413(19) . ? C51 C53 1.437(18) . ? C101 C102 1.67(3) . ? C102 C103 1.47(3) . ? C103 C104 1.41(3) . ? C104 C105 1.37(3) . ? C201 C202 1.44(3) . ? C202 C203 1.37(3) . ? C203 C204 1.39(3) . ? C204 C205 1.52(3) . ? C301 C302 1.41(3) . ? C302 C303 1.43(3) . ? C303 C304 1.36(3) . ? C304 C305 1.46(3) . ? C401 C402 1.56(3) . ? C402 C403 1.33(3) . ? C403 C404 1.42(3) . ? C404 C405 1.44(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 O3 Co1 O2 118.5(5) . . ? O3 Co1 O4 118.9(5) . . ? O2 Co1 O4 113.1(5) . . ? O3 Co1 O9 102.6(5) . . ? O2 Co1 O9 102.8(5) . . ? O4 Co1 O9 95.5(5) . . ? O3 Co1 O1 80.2(4) . . ? O2 Co1 O1 78.3(4) . . ? O4 Co1 O1 80.3(4) . . ? O9 Co1 O1 175.8(5) . . ? O3 Co1 Zr2 40.3(3) . . ? O2 Co1 Zr2 100.1(3) . . ? O4 Co1 Zr2 101.9(3) . . ? O9 Co1 Zr2 142.8(4) . . ? O1 Co1 Zr2 40.0(3) . . ? O3 Co1 Zr1 99.8(3) . . ? O2 Co1 Zr1 40.0(3) . . ? O4 Co1 Zr1 99.2(4) . . ? O9 Co1 Zr1 142.8(4) . . ? O1 Co1 Zr1 38.4(3) . . ? Zr2 Co1 Zr1 66.14(6) . . ? O8 Zr1 O1 111.2(4) . . ? O8 Zr1 O16 89.7(5) . . ? O1 Zr1 O16 138.2(5) . . ? O8 Zr1 O7 91.1(4) . . ? O1 Zr1 O7 67.0(4) . . ? O16 Zr1 O7 77.2(5) . . ? O8 Zr1 O2 174.3(4) . . ? O1 Zr1 O2 74.6(4) . . ? O16 Zr1 O2 85.7(5) . . ? O7 Zr1 O2 91.2(4) . . ? O8 Zr1 O5 89.9(4) . . ? O1 Zr1 O5 66.8(4) . . ? O16 Zr1 O5 152.1(5) . . ? O7 Zr1 O5 130.7(4) . . ? O2 Zr1 O5 92.6(4) . . ? O8 Zr1 O12 89.9(5) . . ? O1 Zr1 O12 137.1(5) . . ? O16 Zr1 O12 75.4(6) . . ? O7 Zr1 O12 152.5(5) . . ? O2 Zr1 O12 85.6(4) . . ? O5 Zr1 O12 76.8(5) . . ? O8 Zr1 Co1 150.8(3) . . ? O1 Zr1 Co1 39.7(2) . . ? O16 Zr1 Co1 112.4(4) . . ? O7 Zr1 Co1 76.2(3) . . ? O2 Zr1 Co1 35.0(3) . . ? O5 Zr1 Co1 79.4(3) . . ? O12 Zr1 Co1 113.4(3) . . ? O8 Zr1 Zr3 97.5(3) . . ? O1 Zr1 Zr3 31.8(2) . . ? O16 Zr1 Zr3 169.7(4) . . ? O7 Zr1 Zr3 95.2(3) . . ? O2 Zr1 Zr3 87.5(3) . . ? O5 Zr1 Zr3 36.0(3) . . ? O12 Zr1 Zr3 111.8(4) . . ? Co1 Zr1 Zr3 58.47(6) . . ? O8 Zr1 Zr2 98.7(3) . . ? O1 Zr1 Zr2 31.9(3) . . ? O16 Zr1 Zr2 112.2(4) . . ? O7 Zr1 Zr2 35.9(3) . . ? O2 Zr1 Zr2 86.3(3) . . ? O5 Zr1 Zr2 95.4(3) . . ? O12 Zr1 Zr2 168.4(4) . . ? Co1 Zr1 Zr2 56.07(6) . . ? Zr3 Zr1 Zr2 59.53(5) . . ? O10 Zr2 O1 110.2(4) . . ? O10 Zr2 O3 173.0(5) . . ? O1 Zr2 O3 76.8(4) . . ? O10 Zr2 O15 88.5(5) . . ? O1 Zr2 O15 139.4(5) . . ? O3 Zr2 O15 85.7(4) . . ? O10 Zr2 O7 90.6(4) . . ? O1 Zr2 O7 66.4(4) . . ? O3 Zr2 O7 92.1(4) . . ? O15 Zr2 O7 78.1(5) . . ? O10 Zr2 O6 89.7(4) . . ? O1 Zr2 O6 67.7(4) . . ? O3 Zr2 O6 93.4(4) . . ? O15 Zr2 O6 150.8(5) . . ? O7 Zr2 O6 131.0(4) . . ? O10 Zr2 O17 90.1(4) . . ? O1 Zr2 O17 138.0(5) . . ? O3 Zr2 O17 84.5(4) . . ? O15 Zr2 O17 74.5(6) . . ? O7 Zr2 O17 152.6(5) . . ? O6 Zr2 O17 76.4(5) . . ? O10 Zr2 Co1 151.3(3) . . ? O1 Zr2 Co1 41.1(2) . . ? O3 Zr2 Co1 35.7(3) . . ? O15 Zr2 Co1 113.8(3) . . ? O7 Zr2 Co1 77.4(3) . . ? O6 Zr2 Co1 79.3(3) . . ? O17 Zr2 Co1 112.4(3) . . ? O10 Zr2 Zr3 96.8(3) . . ? O1 Zr2 Zr3 32.3(2) . . ? O3 Zr2 Zr3 89.4(3) . . ? O15 Zr2 Zr3 171.6(4) . . ? O7 Zr2 Zr3 95.2(3) . . ? O6 Zr2 Zr3 36.3(3) . . ? O17 Zr2 Zr3 111.9(4) . . ? Co1 Zr2 Zr3 59.18(6) . . ? O10 Zr2 Zr1 97.8(3) . . ? O1 Zr2 Zr1 31.7(3) . . ? O3 Zr2 Zr1 88.1(3) . . ? O15 Zr2 Zr1 112.9(4) . . ? O7 Zr2 Zr1 35.4(3) . . ? O6 Zr2 Zr1 96.2(3) . . ? O17 Zr2 Zr1 169.1(4) . . ? Co1 Zr2 Zr1 57.79(6) . . ? Zr3 Zr2 Zr1 59.97(6) . . ? O11 Zr3 O1 110.6(4) . . ? O11 Zr3 O13 88.7(5) . . ? O1 Zr3 O13 138.7(5) . . ? O11 Zr3 O5 91.3(4) . . ? O1 Zr3 O5 67.6(4) . . ? O13 Zr3 O5 76.2(5) . . ? O11 Zr3 O6 89.8(4) . . ? O1 Zr3 O6 68.6(4) . . ? O13 Zr3 O6 150.4(5) . . ? O5 Zr3 O6 133.5(5) . . ? O11 Zr3 O14 91.0(5) . . ? O1 Zr3 O14 137.4(5) . . ? O13 Zr3 O14 74.9(6) . . ? O5 Zr3 O14 150.9(5) . . ? O6 Zr3 O14 75.5(5) . . ? O11 Zr3 O4 174.9(4) . . ? O1 Zr3 O4 74.5(4) . . ? O13 Zr3 O4 87.2(4) . . ? O5 Zr3 O4 90.7(4) . . ? O6 Zr3 O4 92.3(4) . . ? O14 Zr3 O4 85.0(4) . . ? O11 Zr3 Zr2 97.1(3) . . ? O1 Zr3 Zr2 32.7(3) . . ? O13 Zr3 Zr2 171.2(4) . . ? O5 Zr3 Zr2 97.0(3) . . ? O6 Zr3 Zr2 36.9(3) . . ? O14 Zr3 Zr2 111.5(4) . . ? O4 Zr3 Zr2 87.3(3) . . ? O11 Zr3 Zr1 98.0(3) . . ? O1 Zr3 Zr1 31.9(3) . . ? O13 Zr3 Zr1 112.2(4) . . ? O5 Zr3 Zr1 36.6(3) . . ? O6 Zr3 Zr1 97.3(3) . . ? O14 Zr3 Zr1 168.6(4) . . ? O4 Zr3 Zr1 86.4(3) . . ? Zr2 Zr3 Zr1 60.50(5) . . ? Zr3 O1 Zr1 116.3(5) . . ? Zr3 O1 Zr2 115.0(4) . . ? Zr1 O1 Zr2 116.4(4) . . ? Zr3 O1 Co1 104.6(4) . . ? Zr1 O1 Co1 102.0(4) . . ? Zr2 O1 Co1 98.9(4) . . ? C21 O2 Co1 129.0(11) . . ? C21 O2 Zr1 125.9(12) . . ? Co1 O2 Zr1 105.1(4) . . ? C11 O3 Co1 128.2(11) . . ? C11 O3 Zr2 127.6(11) . . ? Co1 O3 Zr2 104.0(5) . . ? C104 O4 Co1 123.2(14) . . ? C104 O4 Zr3 136.3(15) . . ? Co1 O4 Zr3 100.5(4) . . ? C1 O5 Zr3 127.4(10) . . ? C1 O5 Zr1 124.1(10) . . ? Zr3 O5 Zr1 107.4(5) . . ? C4 O6 Zr3 125.8(10) . . ? C4 O6 Zr2 124.2(10) . . ? Zr3 O6 Zr2 106.8(5) . . ? C7 O7 Zr1 124.9(11) . . ? C7 O7 Zr2 124.4(11) . . ? Zr1 O7 Zr2 108.7(5) . . ? C31 O8 Zr1 163.4(17) . . ? C102 O9 Co1 121.2(19) . . ? C51 O10 Zr2 172.1(14) . . ? C41 O11 Zr3 176(2) . . ? C304 O12 Zr1 133.5(18) . . ? C202 O13 Zr3 136.9(19) . . ? C204 O14 Zr3 134.8(17) . . ? C404 O15 Zr2 142(2) . . ? C302 O16 Zr1 138.2(19) . . ? C402 O17 Zr2 133.2(19) . . ? O5 C1 C2 114.8(14) . . ? C1 C2 C3 108.9(15) . . ? C5 C4 O6 114.2(16) . . ? C4 C5 C6 107(2) . . ? O7 C7 C8 113.8(15) . . ? C7 C8 C9 116.9(17) . . ? O3 C11 C13 111.2(17) . . ? O3 C11 C12 110.2(18) . . ? C13 C11 C12 112.1(19) . . ? C23 C21 C22 114(3) . . ? C23 C21 O2 108(2) . . ? C22 C21 O2 110(2) . . ? C33 C31 O8 115(4) . . ? C33 C31 C32 123(4) . . ? O8 C31 C32 115(3) . . ? C43 C41 O11 119(3) . . ? C43 C41 C42 120(3) . . ? O11 C41 C42 119(2) . . ? C52 C51 C53 118(2) . . ? C52 C51 O10 107(3) . . ? C53 C51 O10 98(2) . . ? O9 C102 C103 130(3) . . ? O9 C102 C101 108(3) . . ? C103 C102 C101 121(2) . . ? C104 C103 C102 127(3) . . ? O4 C104 C105 127(2) . . ? O4 C104 C103 123(2) . . ? C105 C104 C103 109(2) . . ? O13 C202 C203 118(3) . . ? O13 C202 C201 125(3) . . ? C203 C202 C201 117(3) . . ? C202 C203 C204 131(3) . . ? O14 C204 C203 117(3) . . ? O14 C204 C205 114(3) . . ? C203 C204 C205 129(3) . . ? O16 C302 C301 123(3) . . ? O16 C302 C303 118(3) . . ? C301 C302 C303 118(3) . . ? C304 C303 C302 130(3) . . ? C303 C304 O12 118(3) . . ? C303 C304 C305 130(3) . . ? O12 C304 C305 112(3) . . ? O17 C402 C403 124(3) . . ? O17 C402 C401 110(3) . . ? C403 C402 C401 126(3) . . ? C402 C403 C404 129(3) . . ? O15 C404 C403 115(3) . . ? O15 C404 C405 123(3) . . ? C403 C404 C405 122(3) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 19.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.634 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.110 data_bazr1m _database_code_depnum_ccdc_archive 'CCDC 234690' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H140 Ba2 O22 Zr4' _chemical_formula_weight 1901.32 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.443(4) _cell_length_b 12.546(3) _cell_length_c 19.772(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.494(6) _cell_angle_gamma 90.00 _cell_volume 4535.7(16) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 968(I>10sigma(I)) _cell_measurement_theta_min 1.93 _cell_measurement_theta_max 23.00 _exptl_crystal_description 'rectangular prism' _exptl_crystal_colour colorless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1944 _exptl_absorpt_coefficient_mu 1.355 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4104 _exptl_absorpt_correction_T_max 0.8226 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7071 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 4 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 21.00 _reflns_number_total 4276 _reflns_number_gt 2671 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0937P)^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 SHELXL _refine_ls_extinction_coef 0.00062(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4276 _refine_ls_number_parameters 423 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1110 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1708 _refine_ls_wR_factor_gt 0.1540 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.079 _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 Ba1 Ba 0.09933(4) 0.97204(7) 0.04290(4) 0.0798(4) Uani 1 1 d . . . Zr2 Zr 0.28551(7) 1.05486(10) 0.12952(7) 0.0728(5) Uani 1 1 d . . . Zr3 Zr 0.26495(7) 0.79905(10) 0.09734(7) 0.0777(5) Uani 1 1 d . . . O1 O 0.2507(4) 0.9519(6) 0.0374(4) 0.067(2) Uani 1 1 d . . . O2 O 0.2078(4) 0.9267(6) 0.1524(4) 0.063(2) Uani 1 1 d . . . O3 O 0.3549(5) 1.1418(8) 0.0905(5) 0.107(3) Uani 1 1 d . . . O4 O 0.3493(4) 0.9095(7) 0.1416(5) 0.089(3) Uani 1 1 d . . . O5 O 0.1921(4) 1.1340(7) 0.0979(5) 0.090(3) Uani 1 1 d . . . O6 O 0.3216(5) 0.7280(8) 0.0386(5) 0.112(3) Uani 1 1 d . . . O7 O 0.1612(5) 0.7703(7) 0.0524(5) 0.100(3) Uani 1 1 d . . . O8 O 0.2746(6) 0.6965(7) 0.1702(5) 0.109(3) Uani 1 1 d . . . O9 O -0.0194(8) 1.0891(13) 0.0791(7) 0.128(5) Uani 1 1 d . . . O10 O 0.3045(5) 1.1073(8) 0.2211(5) 0.103(3) Uani 1 1 d . . . O11 O -0.0362(5) 0.8700(10) 0.0545(7) 0.124(4) Uani 1 1 d . . . C112 C -0.0567(9) 0.871(2) 0.1160(13) 0.128(7) Uani 1 1 d . . . C111 C -0.0552(12) 0.964(3) 0.1543(12) 0.168(13) Uani 1 1 d . . . H11A H -0.0654 0.9576 0.1990 0.202 Uiso 1 1 calc R . . C113 C -0.0795(11) 0.762(2) 0.1419(12) 0.238(15) Uani 1 1 d . . . H11B H -0.0940 0.7697 0.1865 0.357 Uiso 1 1 calc R . . H11C H -0.0389 0.7132 0.1442 0.357 Uiso 1 1 calc R . . H11D H -0.1197 0.7339 0.1112 0.357 Uiso 1 1 calc R . . C1 C 0.2688(8) 0.9655(13) -0.0285(8) 0.095(5) Uani 1 1 d D . . C11 C 0.2312(15) 0.8840(18) -0.0758(12) 0.172(13) Uani 0.67 1 d PD . . H11E H 0.1797 0.8852 -0.0728 0.259 Uiso 0.67 1 calc PR . . H11F H 0.2505 0.8147 -0.0633 0.259 Uiso 0.67 1 calc PR . . H11G H 0.2393 0.8999 -0.1218 0.259 Uiso 0.67 1 calc PR . . C12 C 0.2504(16) 1.0702(15) -0.0590(12) 0.148(11) Uani 0.67 1 d PD . . H12A H 0.2729 1.1250 -0.0296 0.223 Uiso 0.67 1 calc PR . . H12B H 0.1983 1.0795 -0.0649 0.223 Uiso 0.67 1 calc PR . . H12C H 0.2679 1.0746 -0.1026 0.223 Uiso 0.67 1 calc PR . . C13 C 0.3472(10) 0.965(2) -0.0335(12) 0.119(9) Uani 0.67 1 d PD . . H13A H 0.3711 1.0184 -0.0039 0.178 Uiso 0.67 1 calc PR . . H13B H 0.3550 0.9791 -0.0797 0.178 Uiso 0.67 1 calc PR . . H13C H 0.3671 0.8961 -0.0200 0.178 Uiso 0.67 1 calc PR . . C2 C 0.1761(10) 0.9096(15) 0.2147(8) 0.122(7) Uani 1 1 d D . . C21 C 0.1356(11) 1.0027(16) 0.2356(11) 0.119(10) Uani 0.67 1 d PD . . H21A H 0.1652 1.0655 0.2345 0.179 Uiso 0.67 1 calc PR . . H21B H 0.1241 0.9919 0.2811 0.179 Uiso 0.67 1 calc PR . . H21C H 0.0912 1.0113 0.2049 0.179 Uiso 0.67 1 calc PR . . C22 C 0.2270(13) 0.8731(19) 0.2739(13) 0.179(14) Uani 0.67 1 d PD . . H22A H 0.2674 0.9216 0.2818 0.269 Uiso 0.67 1 calc PR . . H22B H 0.2447 0.8032 0.2648 0.269 Uiso 0.67 1 calc PR . . H22C H 0.2020 0.8705 0.3135 0.269 Uiso 0.67 1 calc PR . . C23 C 0.134(2) 0.8124(18) 0.221(2) 0.27(3) Uani 0.67 1 d PD . . H23A H 0.0917 0.8121 0.1871 0.411 Uiso 0.67 1 calc PR . . H23B H 0.1184 0.8099 0.2657 0.411 Uiso 0.67 1 calc PR . . H23C H 0.1637 0.7514 0.2151 0.411 Uiso 0.67 1 calc PR . . C3 C 0.4084(13) 1.220(2) 0.0749(14) 0.204(12) Uani 1 1 d . . . H3 H 0.4411 1.1678 0.0579 0.245 Uiso 1 1 calc R . . C31 C 0.3921(16) 1.273(3) 0.0125(15) 0.30(2) Uani 1 1 d D . . H31A H 0.4328 1.3163 0.0043 0.457 Uiso 1 1 calc R . . H31B H 0.3497 1.3166 0.0136 0.457 Uiso 1 1 calc R . . H31C H 0.3825 1.2210 -0.0234 0.457 Uiso 1 1 calc R . . C32 C 0.454(2) 1.247(3) 0.1266(14) 0.515(13) Uani 1 1 d D . . H32A H 0.4898 1.2939 0.1124 0.772 Uiso 1 1 calc R . . H32B H 0.4772 1.1841 0.1468 0.772 Uiso 1 1 calc R . . H32C H 0.4280 1.2822 0.1594 0.772 Uiso 1 1 calc R . . C4 C 0.4261(12) 0.891(2) 0.1602(9) 0.159(8) Uani 1 1 d . . . H4A H 0.4245 0.8136 0.1566 0.190 Uiso 1 1 calc R . . C41 C 0.4702(11) 0.909(2) 0.1092(13) 0.235(14) Uani 1 1 d D . . H41A H 0.5198 0.8900 0.1259 0.352 Uiso 1 1 calc R . . H41B H 0.4680 0.9827 0.0964 0.352 Uiso 1 1 calc R . . H41C H 0.4532 0.8657 0.0703 0.352 Uiso 1 1 calc R . . C42 C 0.4390(16) 0.896(2) 0.2229(13) 0.269(15) Uiso 1 1 d D . . H42A H 0.4002 0.8620 0.2427 0.404 Uiso 1 1 calc R . . H42B H 0.4426 0.9693 0.2371 0.404 Uiso 1 1 calc R . . H42C H 0.4843 0.8603 0.2379 0.404 Uiso 1 1 calc R . . C5 C 0.1720(14) 1.2454(14) 0.0967(12) 0.165(9) Uani 1 1 d . . . H5 H 0.2178 1.2721 0.1216 0.198 Uiso 1 1 calc R . . C51 C 0.1768(14) 1.3003(14) 0.0349(11) 0.196(11) Uani 1 1 d . . . H51A H 0.1633 1.3736 0.0397 0.294 Uiso 1 1 calc R . . H51B H 0.1444 1.2680 -0.0013 0.294 Uiso 1 1 calc R . . H51C H 0.2261 1.2967 0.0243 0.294 Uiso 1 1 calc R . . C52 C 0.1268(12) 1.2720(17) 0.1461(13) 0.196(10) Uani 1 1 d . . . H52A H 0.1339 1.2214 0.1828 0.293 Uiso 1 1 calc R . . H52B H 0.0766 1.2706 0.1259 0.293 Uiso 1 1 calc R . . H52C H 0.1390 1.3421 0.1635 0.293 Uiso 1 1 calc R . . C6 C 0.362(2) 0.668(2) -0.008(2) 0.261(19) Uani 1 1 d . . . H6A H 0.3908 0.7169 -0.0325 0.313 Uiso 1 1 calc R . . C61 C 0.331(3) 0.599(4) -0.047(3) 0.56(6) Uani 1 1 d . . . H61A H 0.3673 0.5605 -0.0678 0.834 Uiso 1 1 calc R . . H61B H 0.2979 0.6334 -0.0816 0.834 Uiso 1 1 calc R . . H61C H 0.3048 0.5511 -0.0215 0.834 Uiso 1 1 calc R . . C62 C 0.4136(16) 0.603(3) 0.0459(19) 0.31(2) Uani 1 1 d . . . H62A H 0.4457 0.5594 0.0228 0.472 Uiso 1 1 calc R . . H62B H 0.3847 0.5574 0.0710 0.472 Uiso 1 1 calc R . . H62C H 0.4421 0.6502 0.0767 0.472 Uiso 1 1 calc R . . C7 C 0.1228(14) 0.6706(18) 0.0313(15) 0.197(11) Uani 1 1 d . . . H7A H 0.1651 0.6234 0.0419 0.236 Uiso 1 1 calc R . . C71 C 0.1146(16) 0.656(2) -0.0388(13) 0.290(19) Uani 1 1 d . . . H71A H 0.0930 0.5875 -0.0498 0.435 Uiso 1 1 calc R . . H71B H 0.1617 0.6595 -0.0546 0.435 Uiso 1 1 calc R . . H71C H 0.0836 0.7108 -0.0605 0.435 Uiso 1 1 calc R . . C72 C 0.0815(12) 0.6290(17) 0.0814(14) 0.207(12) Uani 1 1 d . . . H72A H 0.0629 0.5599 0.0674 0.310 Uiso 1 1 calc R . . H72B H 0.0415 0.6760 0.0863 0.310 Uiso 1 1 calc R . . H72C H 0.1123 0.6232 0.1243 0.310 Uiso 1 1 calc R . . C8 C 0.2912(17) 0.615(2) 0.2142(19) 0.242(17) Uani 1 1 d . . . H8 H 0.2781 0.6520 0.2546 0.290 Uiso 1 1 calc R . . C81 C 0.2422(19) 0.544(2) 0.2119(18) 0.30(2) Uani 1 1 d . . . H81A H 0.1951 0.5754 0.1985 0.452 Uiso 1 1 calc R . . H81B H 0.2432 0.5118 0.2561 0.452 Uiso 1 1 calc R . . H81C H 0.2512 0.4903 0.1794 0.452 Uiso 1 1 calc R . . C82 C 0.3602(16) 0.590(3) 0.2411(17) 0.30(2) Uani 1 1 d . . . H82A H 0.3911 0.6509 0.2405 0.446 Uiso 1 1 calc R . . H82B H 0.3781 0.5335 0.2147 0.446 Uiso 1 1 calc R . . H82C H 0.3603 0.5659 0.2873 0.446 Uiso 1 1 calc R . . C9 C -0.0392(12) 1.068(3) 0.1309(15) 0.149(11) Uani 1 1 d . . . C91 C -0.0499(10) 1.160(2) 0.1856(11) 0.226(14) Uani 1 1 d . . . H91A H -0.0364 1.2274 0.1685 0.339 Uiso 1 1 calc R . . H91B H -0.0196 1.1445 0.2277 0.339 Uiso 1 1 calc R . . H91C H -0.1002 1.1617 0.1933 0.339 Uiso 1 1 calc R . . C10 C 0.3312(16) 1.148(2) 0.2913(14) 0.201(10) Uiso 1 1 d . . . C101 C 0.2789(18) 1.240(3) 0.298(2) 0.191(17) Uiso 0.66(3) 1 d PD . . C102 C 0.4031(19) 1.175(3) 0.303(2) 0.23(2) Uiso 0.66(3) 1 d PD . . C10A C 0.338(3) 1.273(4) 0.277(2) 0.11(2) Uiso 0.34(3) 1 d PD . . C10B C 0.267(3) 1.150(5) 0.341(3) 0.20(3) Uiso 0.34(3) 1 d PD . . 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 Ba1 0.0564(6) 0.0980(7) 0.0790(7) 0.0033(5) -0.0134(5) 0.0038(5) Zr2 0.0652(9) 0.0714(10) 0.0764(11) -0.0042(7) -0.0114(8) -0.0037(7) Zr3 0.0766(10) 0.0656(9) 0.0881(11) 0.0004(7) -0.0005(8) 0.0066(7) O1 0.071(6) 0.077(6) 0.048(6) 0.002(4) -0.009(5) 0.000(4) O2 0.059(5) 0.071(5) 0.051(5) 0.003(4) -0.020(4) -0.010(4) O3 0.093(7) 0.093(7) 0.130(9) -0.002(6) -0.005(6) -0.016(6) O4 0.048(5) 0.093(7) 0.117(8) 0.013(6) -0.029(6) 0.004(5) O5 0.084(6) 0.065(6) 0.112(7) -0.005(5) -0.023(6) 0.008(5) O6 0.111(8) 0.093(8) 0.135(9) -0.015(7) 0.020(7) 0.019(6) O7 0.102(7) 0.074(7) 0.117(8) -0.010(6) -0.006(6) -0.013(5) O8 0.146(9) 0.069(7) 0.113(8) 0.022(6) 0.015(7) 0.003(6) O9 0.132(11) 0.169(12) 0.084(9) -0.018(10) 0.018(8) 0.010(8) O10 0.109(7) 0.100(8) 0.093(7) -0.019(6) -0.015(6) -0.006(6) O11 0.095(8) 0.147(10) 0.133(10) 0.021(9) 0.020(8) -0.003(7) C112 0.063(11) 0.21(3) 0.106(18) 0.056(18) -0.001(13) 0.012(13) C111 0.127(19) 0.31(4) 0.070(16) -0.04(2) 0.015(13) 0.01(2) C113 0.18(2) 0.25(3) 0.28(3) 0.20(3) -0.016(19) -0.046(19) C1 0.096(13) 0.111(14) 0.076(13) 0.014(11) 0.006(10) -0.007(10) C11 0.15(3) 0.27(4) 0.09(2) -0.01(3) 0.02(2) -0.03(3) C12 0.20(3) 0.16(3) 0.087(19) 0.04(2) 0.022(19) 0.01(2) C13 0.11(2) 0.14(2) 0.11(2) -0.007(16) 0.035(16) 0.012(16) C2 0.133(16) 0.162(19) 0.064(12) 0.040(12) -0.016(12) 0.014(14) C21 0.103(18) 0.17(3) 0.097(18) 0.010(17) 0.041(15) 0.075(18) C22 0.21(3) 0.11(2) 0.23(4) -0.05(3) 0.09(3) -0.04(2) C23 0.29(5) 0.34(6) 0.19(4) 0.00(4) 0.02(3) -0.18(5) C3 0.20(2) 0.24(3) 0.17(2) 0.05(2) 0.01(2) -0.14(2) C31 0.33(4) 0.36(5) 0.22(3) 0.08(3) 0.00(3) -0.20(3) C32 0.59(3) 0.70(4) 0.24(4) -0.14(4) 0.04(4) -0.602 C4 0.17(2) 0.23(3) 0.074(14) 0.008(15) -0.001(15) 0.001(19) C41 0.124(18) 0.32(4) 0.27(3) 0.14(3) 0.06(2) 0.02(2) C5 0.27(3) 0.063(13) 0.17(2) -0.004(14) 0.08(2) 0.043(15) C51 0.35(3) 0.078(14) 0.17(2) 0.035(14) 0.06(2) 0.035(17) C52 0.20(2) 0.130(19) 0.27(3) -0.03(2) 0.07(2) 0.005(16) C6 0.24(4) 0.16(3) 0.40(5) -0.03(3) 0.12(4) 0.10(3) C61 0.42(7) 0.58(9) 0.64(9) -0.53(8) -0.05(6) 0.17(6) C62 0.25(4) 0.21(3) 0.50(6) -0.15(4) 0.11(4) 0.06(3) C7 0.24(3) 0.125(19) 0.22(3) -0.066(19) 0.01(2) -0.102(18) C71 0.37(4) 0.28(4) 0.19(3) -0.12(3) -0.11(3) -0.07(3) C72 0.20(2) 0.098(17) 0.32(3) 0.00(2) 0.05(2) -0.070(16) C8 0.23(3) 0.17(3) 0.31(4) 0.16(3) -0.02(3) -0.04(2) C81 0.41(5) 0.13(2) 0.32(4) 0.10(3) -0.13(4) -0.05(3) C82 0.25(3) 0.26(4) 0.35(4) 0.17(3) -0.08(3) 0.01(3) C9 0.080(16) 0.22(3) 0.13(3) -0.05(2) -0.055(18) 0.040(18) C91 0.149(19) 0.37(4) 0.15(2) -0.14(2) -0.006(15) 0.01(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 Ba1 O7 2.772(9) . ? Ba1 O5 2.784(8) . ? Ba1 O9 2.766(14) 3_575 ? Ba1 O9 2.806(13) . ? Ba1 O2 2.808(7) . ? Ba1 O1 2.820(8) . ? Ba1 O11 2.844(11) . ? Ba1 O11 2.900(12) 3_575 ? Ba1 Zr2 3.7773(16) . ? Ba1 Zr3 3.7870(16) . ? Ba1 Ba1 3.8951(17) 3_575 ? Zr2 O10 1.915(9) . ? Zr2 O3 1.919(10) . ? Zr2 O5 2.016(8) . ? Zr2 O4 2.167(9) . ? Zr2 O2 2.239(7) . ? Zr2 O1 2.257(8) . ? Zr2 Zr3 3.2843(19) . ? Zr3 O6 1.885(10) . ? Zr3 O8 1.922(10) . ? Zr3 O7 2.035(9) . ? Zr3 O4 2.179(9) . ? Zr3 O1 2.252(8) . ? Zr3 O2 2.272(8) . ? O1 C1 1.397(16) . ? O2 C2 1.446(17) . ? O3 C3 1.454(19) . ? O4 C4 1.44(2) . ? O5 C5 1.446(18) . ? O6 C6 1.46(3) . ? O7 C7 1.471(19) . ? O8 C8 1.35(2) . ? O9 C9 1.16(3) . ? O9 Ba1 2.766(14) 3_575 ? O10 C10 1.50(3) . ? O11 C112 1.32(2) . ? O11 Ba1 2.900(12) 3_575 ? C112 C111 1.39(3) . ? C112 C113 1.54(3) . ? C111 C9 1.44(4) . ? C1 C13 1.461(15) . ? C1 C12 1.467(14) . ? C1 C11 1.494(15) . ? C2 C23 1.462(15) . ? C2 C22 1.474(15) . ? C2 C21 1.474(14) . ? C22 C23 2.04(4) . ? C3 C32 1.28(3) . ? C3 C31 1.40(3) . ? C4 C42 1.23(2) . ? C4 C41 1.39(2) . ? C5 C52 1.40(2) . ? C5 C51 1.42(2) . ? C6 C61 1.25(5) . ? C6 C62 1.56(4) . ? C7 C71 1.39(3) . ? C7 C72 1.42(3) . ? C8 C81 1.27(3) . ? C8 C82 1.35(3) . ? C9 C91 1.60(3) . ? C10 C102 1.36(4) . ? C10 C101 1.52(4) . ? C10 C10A 1.60(5) . ? C10 C10B 1.63(6) . ? C101 C10A 1.29(4) . ? C101 C10B 1.45(5) . ? C102 C10A 1.75(5) . ? 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 O7 Ba1 O5 114.4(3) . . ? O7 Ba1 O9 88.5(4) . 3_575 ? O5 Ba1 O9 140.7(4) . 3_575 ? O7 Ba1 O9 142.0(4) . . ? O5 Ba1 O9 88.8(4) . . ? O9 Ba1 O9 91.3(4) 3_575 . ? O7 Ba1 O2 61.1(2) . . ? O5 Ba1 O2 60.5(2) . . ? O9 Ba1 O2 149.5(4) 3_575 . ? O9 Ba1 O2 114.2(3) . . ? O7 Ba1 O1 61.3(2) . . ? O5 Ba1 O1 61.3(2) . . ? O9 Ba1 O1 111.0(3) 3_575 . ? O9 Ba1 O1 150.1(3) . . ? O2 Ba1 O1 53.3(2) . . ? O7 Ba1 O11 86.6(3) . . ? O5 Ba1 O11 143.0(3) . . ? O9 Ba1 O11 64.7(4) 3_575 . ? O9 Ba1 O11 59.5(4) . . ? O2 Ba1 O11 113.0(3) . . ? O1 Ba1 O11 148.0(3) . . ? O7 Ba1 O11 142.7(3) . 3_575 ? O5 Ba1 O11 86.2(3) . 3_575 ? O9 Ba1 O11 59.2(4) 3_575 3_575 ? O9 Ba1 O11 63.4(4) . 3_575 ? O2 Ba1 O11 146.6(3) . 3_575 ? O1 Ba1 O11 110.4(3) . 3_575 ? O11 Ba1 O11 94.6(3) . 3_575 ? O7 Ba1 Zr2 83.04(18) . . ? O5 Ba1 Zr2 31.39(17) . . ? O9 Ba1 Zr2 145.2(3) 3_575 . ? O9 Ba1 Zr2 115.7(3) . . ? O2 Ba1 Zr2 36.11(15) . . ? O1 Ba1 Zr2 36.50(16) . . ? O11 Ba1 Zr2 147.5(3) . . ? O11 Ba1 Zr2 112.1(2) 3_575 . ? O7 Ba1 Zr3 31.58(18) . . ? O5 Ba1 Zr3 82.86(17) . . ? O9 Ba1 Zr3 114.0(3) 3_575 . ? O9 Ba1 Zr3 148.7(3) . . ? O2 Ba1 Zr3 36.64(16) . . ? O1 Ba1 Zr3 36.26(16) . . ? O11 Ba1 Zr3 113.8(2) . . ? O11 Ba1 Zr3 145.0(2) 3_575 . ? Zr2 Ba1 Zr3 51.47(3) . . ? O7 Ba1 Ba1 123.31(19) . 3_575 ? O5 Ba1 Ba1 122.26(17) . 3_575 ? O9 Ba1 Ba1 46.1(3) 3_575 3_575 ? O9 Ba1 Ba1 45.2(3) . 3_575 ? O2 Ba1 Ba1 155.14(17) . 3_575 ? O1 Ba1 Ba1 151.54(17) . 3_575 ? O11 Ba1 Ba1 47.9(2) . 3_575 ? O11 Ba1 Ba1 46.7(2) 3_575 3_575 ? Zr2 Ba1 Ba1 153.60(5) . 3_575 ? Zr3 Ba1 Ba1 154.82(5) . 3_575 ? O10 Zr2 O3 97.8(4) . . ? O10 Zr2 O5 99.7(4) . . ? O3 Zr2 O5 100.6(4) . . ? O10 Zr2 O4 98.9(4) . . ? O3 Zr2 O4 98.2(4) . . ? O5 Zr2 O4 151.4(3) . . ? O10 Zr2 O2 95.7(4) . . ? O3 Zr2 O2 165.4(4) . . ? O5 Zr2 O2 82.7(3) . . ? O4 Zr2 O2 74.1(3) . . ? O10 Zr2 O1 163.2(4) . . ? O3 Zr2 O1 97.8(4) . . ? O5 Zr2 O1 83.7(3) . . ? O4 Zr2 O1 72.6(3) . . ? O2 Zr2 O1 68.3(3) . . ? O10 Zr2 Zr3 121.4(3) . . ? O3 Zr2 Zr3 122.9(3) . . ? O5 Zr2 Zr3 110.4(2) . . ? O4 Zr2 Zr3 41.1(2) . . ? O2 Zr2 Zr3 43.7(2) . . ? O1 Zr2 Zr3 43.2(2) . . ? O10 Zr2 Ba1 124.5(3) . . ? O3 Zr2 Ba1 126.1(3) . . ? O5 Zr2 Ba1 46.0(2) . . ? O4 Zr2 Ba1 105.5(2) . . ? O2 Zr2 Ba1 47.64(19) . . ? O1 Zr2 Ba1 48.0(2) . . ? Zr3 Zr2 Ba1 64.42(3) . . ? O6 Zr3 O8 98.1(4) . . ? O6 Zr3 O7 102.3(4) . . ? O8 Zr3 O7 101.5(4) . . ? O6 Zr3 O4 97.1(4) . . ? O8 Zr3 O4 97.6(4) . . ? O7 Zr3 O4 150.4(3) . . ? O6 Zr3 O1 96.5(4) . . ? O8 Zr3 O1 163.3(4) . . ? O7 Zr3 O1 83.2(3) . . ? O4 Zr3 O1 72.4(3) . . ? O6 Zr3 O2 163.3(4) . . ? O8 Zr3 O2 96.7(4) . . ? O7 Zr3 O2 82.2(3) . . ? O4 Zr3 O2 73.2(3) . . ? O1 Zr3 O2 67.8(3) . . ? O6 Zr3 Zr2 121.5(3) . . ? O8 Zr3 Zr2 120.8(3) . . ? O7 Zr3 Zr2 109.6(3) . . ? O4 Zr3 Zr2 40.8(2) . . ? O1 Zr3 Zr2 43.3(2) . . ? O2 Zr3 Zr2 42.89(19) . . ? O6 Zr3 Ba1 126.0(3) . . ? O8 Zr3 Ba1 126.1(3) . . ? O7 Zr3 Ba1 45.5(3) . . ? O4 Zr3 Ba1 104.9(2) . . ? O1 Zr3 Ba1 47.8(2) . . ? O2 Zr3 Ba1 47.53(18) . . ? Zr2 Zr3 Ba1 64.11(3) . . ? C1 O1 Zr3 124.7(8) . . ? C1 O1 Zr2 127.3(8) . . ? Zr3 O1 Zr2 93.5(3) . . ? C1 O1 Ba1 112.6(7) . . ? Zr3 O1 Ba1 96.0(3) . . ? Zr2 O1 Ba1 95.5(3) . . ? C2 O2 Zr2 128.3(9) . . ? C2 O2 Zr3 124.6(8) . . ? Zr2 O2 Zr3 93.4(3) . . ? C2 O2 Ba1 111.1(8) . . ? Zr2 O2 Ba1 96.2(3) . . ? Zr3 O2 Ba1 95.8(3) . . ? C3 O3 Zr2 167.5(14) . . ? C4 O4 Zr2 131.6(12) . . ? C4 O4 Zr3 129.2(12) . . ? Zr2 O4 Zr3 98.2(3) . . ? C5 O5 Zr2 133.5(12) . . ? C5 O5 Ba1 123.8(11) . . ? Zr2 O5 Ba1 102.6(3) . . ? C6 O6 Zr3 176.7(17) . . ? C7 O7 Zr3 131.6(13) . . ? C7 O7 Ba1 125.4(13) . . ? Zr3 O7 Ba1 102.9(3) . . ? C8 O8 Zr3 168.5(18) . . ? C9 O9 Ba1 121.0(17) . 3_575 ? C9 O9 Ba1 117.0(16) . . ? Ba1 O9 Ba1 88.7(4) 3_575 . ? C10 O10 Zr2 171.5(14) . . ? C112 O11 Ba1 115.6(11) . . ? C112 O11 Ba1 118.0(11) . 3_575 ? Ba1 O11 Ba1 85.4(3) . 3_575 ? O11 C112 C111 121(2) . . ? O11 C112 C113 115(3) . . ? C111 C112 C113 124(3) . . ? C112 C111 C9 126(3) . . ? O1 C1 C13 114.8(14) . . ? O1 C1 C12 115.0(15) . . ? C13 C1 C12 99.0(18) . . ? O1 C1 C11 110.6(14) . . ? C13 C1 C11 109.7(19) . . ? C12 C1 C11 107.0(13) . . ? O2 C2 C23 119(2) . . ? O2 C2 C22 115.8(18) . . ? C23 C2 C22 88(2) . . ? O2 C2 C21 113.4(14) . . ? C23 C2 C21 109.9(14) . . ? C22 C2 C21 108.5(14) . . ? C2 C22 C23 45.8(11) . . ? C2 C23 C22 46.3(12) . . ? C32 C3 C31 129(2) . . ? C32 C3 O3 113(2) . . ? C31 C3 O3 116(2) . . ? C42 C4 C41 132(2) . . ? C42 C4 O4 108(2) . . ? C41 C4 O4 116.1(16) . . ? C52 C5 O5 113.1(19) . . ? C52 C5 C51 127(2) . . ? O5 C5 C51 116.1(17) . . ? C61 C6 O6 121(4) . . ? C61 C6 C62 104(4) . . ? O6 C6 C62 99(3) . . ? C71 C7 C72 130(2) . . ? C71 C7 O7 112(2) . . ? C72 C7 O7 113(2) . . ? C81 C8 O8 114(3) . . ? C81 C8 C82 118(3) . . ? O8 C8 C82 124(3) . . ? O9 C9 C111 126(3) . . ? O9 C9 C91 121(3) . . ? C111 C9 C91 113(3) . . ? C102 C10 C101 114(3) . . ? C102 C10 O10 116(3) . . ? C101 C10 O10 101(2) . . ? C102 C10 C10A 72(2) . . ? C101 C10 C10A 48.7(19) . . ? O10 C10 C10A 101(2) . . ? C102 C10 C10B 132(4) . . ? C101 C10 C10B 55(2) . . ? O10 C10 C10B 112(3) . . ? C10A C10 C10B 100(3) . . ? C10A C101 C10B 130(4) . . ? C10A C101 C10 69(2) . . ? C10B C101 C10 67(3) . . ? C10 C102 C10A 60.6(19) . . ? C101 C10A C10 62(2) . . ? C101 C10A C102 105(3) . . ? C10 C10A C102 47.6(18) . . ? C101 C10B C10 59(2) . . ? _diffrn_measured_fraction_theta_max 0.876 _diffrn_reflns_theta_full 21.00 _diffrn_measured_fraction_theta_full 0.876 _refine_diff_density_max 0.631 _refine_diff_density_min -0.719 _refine_diff_density_rms 0.094 data_bazr22m _database_code_depnum_ccdc_archive 'CCDC 234691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C74 H148 Ba2 O18 Zr2' _chemical_formula_weight 1783.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Ba Ba -0.3244 2.2819 '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 10.820(7) _cell_length_b 14.977(9) _cell_length_c 16.885(9) _cell_angle_alpha 104.801(19) _cell_angle_beta 104.294(11) _cell_angle_gamma 107.671(13) _cell_volume 2359(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3031(I>6sigma(I)) _cell_measurement_theta_min 1.33 _cell_measurement_theta_max 28.17 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.255 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.092 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5602 _exptl_absorpt_correction_T_max 0.7353 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5672 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_sigmaI/netI 0.1322 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 17.99 _reflns_number_total 3201 _reflns_number_gt 1939 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1543P)^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 3201 _refine_ls_number_parameters 433 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1439 _refine_ls_R_factor_gt 0.0861 _refine_ls_wR_factor_ref 0.2268 _refine_ls_wR_factor_gt 0.2012 _refine_ls_goodness_of_fit_ref 0.931 _refine_ls_restrained_S_all 0.931 _refine_ls_shift/su_max 0.004 _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 Ba1 Ba 0.55277(15) 0.66419(10) 0.10173(8) 0.0673(7) Uani 1 1 d . . . Zr1 Zr 0.5852(2) 0.43240(15) 0.15429(12) 0.0612(8) Uani 1 1 d . . . O1 O 0.4854(15) 0.5275(11) 0.1773(10) 0.076(5) Uani 1 1 d . . . O2 O 0.4207(16) 0.3196(12) 0.0544(8) 0.076(4) Uani 1 1 d . . . O3 O 0.6426(12) 0.5021(10) 0.0736(8) 0.068(4) Uani 1 1 d . . . O4 O 0.5613(19) 0.7955(14) 0.2429(11) 0.096(5) Uani 1 1 d . . . O5 O 0.7468(16) 0.5367(12) 0.2731(12) 0.081(5) Uani 1 1 d . . . O6 O 0.3563(19) 0.7257(15) 0.0276(11) 0.116(7) Uani 1 1 d . . . O7 O 0.7861(19) 0.8092(13) 0.1839(13) 0.106(6) Uani 1 1 d . . . O8 O 0.7127(17) 0.3579(12) 0.1447(10) 0.093(5) Uani 1 1 d . . . O9 O 0.5317(15) 0.3693(10) 0.2495(11) 0.071(4) Uani 1 1 d . . . C3 C 0.761(3) 0.5275(19) 0.0437(17) 0.091(8) Uani 1 1 d . . . H1A H 0.7777 0.4676 0.0202 0.109 Uiso 1 1 calc R . . H1B H 0.7417 0.5544 -0.0023 0.109 Uiso 1 1 calc R . . C31 C 0.883(3) 0.601(2) 0.117(2) 0.128(10) Uani 1 1 d . . . H2A H 0.9037 0.5740 0.1627 0.154 Uiso 1 1 calc R . . H2B H 0.8668 0.6608 0.1408 0.154 Uiso 1 1 calc R . . C32 C 1.012(3) 0.629(2) 0.083(2) 0.143(12) Uani 1 1 d . . . H3A H 1.0930 0.6788 0.1305 0.214 Uiso 1 1 calc R . . H3B H 0.9901 0.6547 0.0370 0.214 Uiso 1 1 calc R . . H3C H 1.0290 0.5698 0.0609 0.214 Uiso 1 1 calc R . . C5 C 0.768(3) 0.5468(18) 0.354(2) 0.087(8) Uani 1 1 d . . . C51 C 0.891(3) 0.642(2) 0.4167(17) 0.091(8) Uani 1 1 d . . . C59 C 0.696(3) 0.479(3) 0.3840(15) 0.089(8) Uani 1 1 d . . . H6A H 0.7265 0.4918 0.4439 0.107 Uiso 1 1 calc R . . C2 C 0.322(5) 0.227(3) 0.048(2) 0.143(13) Uani 1 1 d . . . H7A H 0.2921 0.1785 -0.0101 0.172 Uiso 1 1 calc R . . H7B H 0.3665 0.2020 0.0896 0.172 Uiso 1 1 calc R . . C91 C 0.499(4) 0.316(2) 0.3668(19) 0.121(11) Uani 1 1 d . . . C9 C 0.580(3) 0.392(2) 0.330(2) 0.080(8) Uani 1 1 d . . . C1 C 0.435(3) 0.5553(19) 0.2439(19) 0.107(10) Uani 1 1 d . . . H10A H 0.4356 0.5098 0.2758 0.128 Uiso 1 1 calc R . . H10B H 0.4996 0.6219 0.2842 0.128 Uiso 1 1 calc R . . C12 C 0.242(4) 0.580(3) 0.291(2) 0.208(18) Uani 1 1 d . . . H11A H 0.1509 0.5773 0.2642 0.312 Uiso 1 1 calc R . . H11B H 0.2991 0.6462 0.3337 0.312 Uiso 1 1 calc R . . H11C H 0.2356 0.5318 0.3195 0.312 Uiso 1 1 calc R . . C47 C 0.781(4) 0.9285(19) 0.3048(18) 0.097(10) Uani 1 1 d . . . H12A H 0.8355 0.9907 0.3489 0.117 Uiso 1 1 calc R . . C71 C 0.993(3) 0.952(2) 0.265(2) 0.111(10) Uani 1 1 d . . . C7 C 0.839(3) 0.886(2) 0.246(2) 0.093(9) Uani 1 1 d . . . C4 C 0.645(4) 0.879(2) 0.2985(17) 0.093(10) Uani 1 1 d . . . C6 C 0.337(4) 0.806(3) 0.0606(19) 0.154(15) Uani 1 1 d D . . H16A H 0.2404 0.7928 0.0318 0.185 Uiso 1 1 calc R . . H16B H 0.3506 0.8161 0.1217 0.185 Uiso 1 1 calc R . . C41 C 0.585(4) 0.923(3) 0.369(2) 0.129(12) Uani 1 1 d . . . C52 C 0.917(5) 0.659(3) 0.513(2) 0.25(3) Uani 1 1 d . . . H18A H 0.9937 0.7211 0.5480 0.377 Uiso 1 1 calc R . . H18B H 0.9377 0.6047 0.5256 0.377 Uiso 1 1 calc R . . H18C H 0.8357 0.6600 0.5255 0.377 Uiso 1 1 calc R . . C42 C 0.591(5) 0.868(3) 0.433(2) 0.21(2) Uani 1 1 d . . . H19A H 0.5534 0.8928 0.4753 0.311 Uiso 1 1 calc R . . H19B H 0.6854 0.8789 0.4614 0.311 Uiso 1 1 calc R . . H19C H 0.5375 0.7975 0.4014 0.311 Uiso 1 1 calc R . . C8 C 0.852(4) 0.362(2) 0.193(2) 0.166(15) Uani 1 1 d D . . H20A H 0.9092 0.3703 0.1573 0.199 Uiso 1 1 calc R . . H20B H 0.8960 0.4213 0.2461 0.199 Uiso 1 1 calc R . . C92 C 0.476(6) 0.214(3) 0.318(3) 0.27(3) Uani 1 1 d . . . H21A H 0.4285 0.1691 0.3425 0.407 Uiso 1 1 calc R . . H21B H 0.5634 0.2094 0.3213 0.407 Uiso 1 1 calc R . . H21C H 0.4206 0.1960 0.2581 0.407 Uiso 1 1 calc R . . C53 C 0.862(4) 0.729(2) 0.408(2) 0.22(2) Uani 1 1 d . . . H22A H 0.8416 0.7253 0.3488 0.334 Uiso 1 1 calc R . . H22B H 0.9408 0.7893 0.4458 0.334 Uiso 1 1 calc R . . H22C H 0.7832 0.7290 0.4253 0.334 Uiso 1 1 calc R . . C21 C 0.207(5) 0.239(4) 0.066(3) 0.22(2) Uani 1 1 d . . . H23A H 0.1569 0.2591 0.0219 0.263 Uiso 1 1 calc R . . H23B H 0.2357 0.2901 0.1228 0.263 Uiso 1 1 calc R . . C43 C 0.445(4) 0.909(4) 0.327(2) 0.29(4) Uani 1 1 d . . . H24A H 0.4097 0.9356 0.3706 0.439 Uiso 1 1 calc R . . H24B H 0.3893 0.8388 0.2965 0.439 Uiso 1 1 calc R . . H24C H 0.4415 0.9436 0.2865 0.439 Uiso 1 1 calc R . . C54 C 1.010(4) 0.658(3) 0.395(3) 0.24(3) Uani 1 1 d . . . H25A H 0.9877 0.6498 0.3347 0.362 Uiso 1 1 calc R . . H25B H 1.0476 0.6097 0.4062 0.362 Uiso 1 1 calc R . . H25C H 1.0775 0.7243 0.4308 0.362 Uiso 1 1 calc R . . C72 C 1.079(5) 1.010(4) 0.352(2) 0.35(4) Uani 1 1 d . . . H26A H 1.1692 1.0488 0.3536 0.523 Uiso 1 1 calc R . . H26B H 1.0861 0.9670 0.3842 0.523 Uiso 1 1 calc R . . H26C H 1.0397 1.0550 0.3767 0.523 Uiso 1 1 calc R . . C73 C 0.999(5) 1.032(4) 0.219(4) 0.34(4) Uani 1 1 d D . . H27A H 1.0940 1.0695 0.2281 0.507 Uiso 1 1 calc R . . H27B H 0.9602 1.0765 0.2445 0.507 Uiso 1 1 calc R . . H27C H 0.9474 0.9982 0.1578 0.507 Uiso 1 1 calc R . . C93 C 0.367(5) 0.329(3) 0.361(4) 0.26(3) Uani 1 1 d . . . H28A H 0.3131 0.2831 0.3825 0.394 Uiso 1 1 calc R . . H28B H 0.3154 0.3157 0.3015 0.394 Uiso 1 1 calc R . . H28C H 0.3866 0.3965 0.3963 0.394 Uiso 1 1 calc R . . C44 C 0.679(5) 1.030(3) 0.424(3) 0.27(3) Uani 1 1 d . . . H29A H 0.6412 1.0555 0.4662 0.404 Uiso 1 1 calc R . . H29B H 0.6884 1.0693 0.3880 0.404 Uiso 1 1 calc R . . H29C H 0.7688 1.0323 0.4546 0.404 Uiso 1 1 calc R . . C94 C 0.576(5) 0.335(4) 0.462(3) 0.40(5) Uani 1 1 d . . . H30A H 0.5245 0.2848 0.4802 0.600 Uiso 1 1 calc R . . H30B H 0.5874 0.4002 0.4981 0.600 Uiso 1 1 calc R . . H30C H 0.6658 0.3330 0.4681 0.600 Uiso 1 1 calc R . . C22 C 0.114(6) 0.137(4) 0.063(3) 0.39(6) Uani 1 1 d . . . H31A H 0.0336 0.1420 0.0745 0.586 Uiso 1 1 calc R . . H31B H 0.1649 0.1187 0.1069 0.586 Uiso 1 1 calc R . . H31C H 0.0871 0.0876 0.0064 0.586 Uiso 1 1 calc R . . C11 C 0.307(4) 0.556(3) 0.220(2) 0.187(17) Uani 1 1 d . . . H32A H 0.2440 0.4911 0.1768 0.224 Uiso 1 1 calc R . . H32B H 0.3086 0.6050 0.1917 0.224 Uiso 1 1 calc R . . C62 C 0.369(6) 0.984(3) 0.093(3) 0.30(3) Uani 1 1 d D . . H42A H 0.4328 1.0433 0.0918 0.445 Uiso 1 1 calc R . . H42B H 0.3724 0.9932 0.1523 0.445 Uiso 1 1 calc R . . H42C H 0.2767 0.9699 0.0569 0.445 Uiso 1 1 calc R . . C61 C 0.411(8) 0.890(4) 0.057(3) 0.38(5) Uani 1 1 d . . . H41A H 0.4035 0.8793 -0.0033 0.452 Uiso 1 1 calc R . . H41B H 0.5070 0.9072 0.0907 0.452 Uiso 1 1 calc R . . C74 C 1.073(4) 0.894(3) 0.239(4) 0.40(5) Uani 1 1 d D . . H40A H 1.1635 0.9387 0.2465 0.597 Uiso 1 1 calc R . . H40B H 1.0260 0.8513 0.1781 0.597 Uiso 1 1 calc R . . H40C H 1.0806 0.8537 0.2740 0.597 Uiso 1 1 calc R . . C82 C 0.772(11) 0.198(4) 0.212(5) 0.55(9) Uani 1 1 d D . . H44A H 0.8297 0.1643 0.2319 0.825 Uiso 1 1 calc R . . H44B H 0.7102 0.1577 0.1531 0.825 Uiso 1 1 calc R . . H44C H 0.7198 0.2073 0.2494 0.825 Uiso 1 1 calc R . . C81 C 0.855(9) 0.290(4) 0.214(4) 0.37(5) Uani 1 1 d . . . H43A H 0.9086 0.3233 0.2766 0.446 Uiso 1 1 calc R . . H43B H 0.9188 0.2723 0.1886 0.446 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 Ba1 0.0516(10) 0.0730(12) 0.0654(11) 0.0188(8) 0.0153(8) 0.0179(8) Zr1 0.0472(16) 0.0671(17) 0.0571(15) 0.0177(12) 0.0124(13) 0.0149(13) O1 0.058(11) 0.090(12) 0.089(11) 0.026(9) 0.037(10) 0.038(9) O2 0.082(12) 0.096(13) 0.078(11) 0.053(9) 0.046(9) 0.039(11) O3 0.005(8) 0.106(12) 0.075(10) 0.027(9) 0.004(8) 0.009(8) O4 0.107(15) 0.086(13) 0.068(12) 0.004(11) 0.038(11) 0.018(12) O5 0.075(12) 0.090(13) 0.084(12) 0.034(11) 0.040(11) 0.029(10) O6 0.118(15) 0.109(15) 0.122(15) 0.016(12) 0.011(12) 0.090(13) O7 0.102(15) 0.066(13) 0.108(14) -0.007(11) 0.043(13) 0.007(12) O8 0.074(12) 0.107(13) 0.082(11) 0.023(10) 0.011(10) 0.036(11) O9 0.043(10) 0.065(11) 0.070(12) 0.016(9) -0.006(10) 0.002(8) C3 0.06(2) 0.08(2) 0.12(2) 0.049(18) 0.02(2) 0.023(17) C31 0.09(2) 0.14(3) 0.17(3) 0.08(3) 0.07(3) 0.03(2) C32 0.06(2) 0.12(2) 0.24(4) 0.07(2) 0.06(2) 0.018(18) C5 0.08(2) 0.029(17) 0.13(3) 0.02(2) 0.04(2) -0.010(16) C51 0.10(2) 0.08(2) 0.08(2) 0.023(18) 0.021(19) 0.02(2) C59 0.08(2) 0.13(3) 0.034(16) 0.03(2) -0.001(17) 0.03(2) C2 0.18(4) 0.12(3) 0.09(2) 0.05(2) 0.04(3) 0.00(3) C91 0.17(3) 0.09(3) 0.12(3) 0.06(2) 0.06(3) 0.03(2) C9 0.06(2) 0.07(2) 0.052(19) -0.003(18) -0.028(18) 0.018(18) C1 0.09(3) 0.07(2) 0.15(3) 0.037(19) 0.02(2) 0.038(18) C12 0.17(4) 0.27(5) 0.19(4) 0.04(3) 0.10(4) 0.10(4) C47 0.08(2) 0.06(2) 0.08(2) -0.004(16) -0.02(2) -0.015(19) C71 0.05(2) 0.10(2) 0.12(3) 0.004(19) 0.011(19) -0.003(19) C7 0.11(3) 0.07(2) 0.10(2) 0.026(19) 0.05(3) 0.04(3) C4 0.11(3) 0.06(2) 0.06(2) -0.015(17) -0.01(2) 0.04(2) C6 0.23(4) 0.12(3) 0.11(3) 0.06(3) 0.01(3) 0.08(3) C41 0.13(3) 0.11(3) 0.08(2) -0.04(2) 0.02(2) 0.03(2) C52 0.31(6) 0.13(3) 0.12(3) 0.01(2) 0.01(3) -0.08(3) C42 0.42(7) 0.19(4) 0.20(4) 0.13(3) 0.22(5) 0.21(5) C8 0.20(4) 0.11(3) 0.16(3) 0.03(2) 0.00(3) 0.07(3) C92 0.54(10) 0.12(3) 0.34(6) 0.16(4) 0.32(7) 0.16(5) C53 0.17(4) 0.07(2) 0.25(4) -0.04(3) -0.10(3) 0.02(2) C21 0.12(4) 0.34(7) 0.15(4) 0.06(4) -0.01(3) 0.09(4) C43 0.18(4) 0.62(10) 0.08(2) 0.01(4) 0.03(3) 0.27(6) C54 0.10(3) 0.24(5) 0.20(4) -0.09(3) 0.04(3) -0.03(3) C72 0.18(5) 0.51(9) 0.06(3) -0.05(4) -0.01(3) -0.08(5) C73 0.14(4) 0.43(10) 0.43(9) 0.28(8) 0.10(5) 0.00(5) C93 0.26(6) 0.24(5) 0.46(8) 0.22(6) 0.27(6) 0.12(5) C44 0.32(7) 0.20(4) 0.24(5) -0.04(4) 0.17(5) 0.08(5) C94 0.25(6) 0.48(9) 0.21(5) 0.26(6) -0.13(4) -0.15(6) C22 0.33(8) 0.26(6) 0.35(7) -0.02(5) 0.23(7) -0.17(6) C11 0.11(3) 0.24(5) 0.19(4) 0.04(3) 0.08(3) 0.05(3) C62 0.39(9) 0.17(5) 0.30(6) 0.12(4) 0.12(6) 0.05(5) C61 0.80(15) 0.13(4) 0.13(3) 0.08(3) 0.01(5) 0.19(7) C74 0.11(4) 0.18(4) 0.72(14) -0.05(7) 0.19(6) -0.05(3) C82 0.9(2) 0.17(6) 0.39(10) 0.12(7) 0.22(12) 0.03(10) C81 0.64(16) 0.17(6) 0.33(7) 0.12(6) 0.12(9) 0.23(9) _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 Ba1 O7 2.533(18) . ? Ba1 O4 2.635(17) . ? Ba1 O1 2.691(15) . ? Ba1 O6 2.721(16) . ? Ba1 O2 2.783(13) 2_665 ? Ba1 O3 2.853(13) . ? Ba1 O3 3.063(13) 2_665 ? Ba1 Zr1 3.889(3) . ? Ba1 Zr1 3.914(3) 2_665 ? Ba1 Ba1 4.829(4) 2_665 ? Zr1 O3 2.021(14) . ? Zr1 O2 2.026(16) . ? Zr1 O8 2.032(16) . ? Zr1 O1 2.050(15) . ? Zr1 O5 2.128(17) . ? Zr1 O9 2.172(16) . ? Zr1 Ba1 3.914(3) 2_665 ? O1 C1 1.39(3) . ? O2 C2 1.42(3) . ? O2 Ba1 2.783(13) 2_665 ? O3 C3 1.47(3) . ? O3 Ba1 3.063(13) 2_665 ? O4 C4 1.25(3) . ? O5 C5 1.29(3) . ? O6 C6 1.29(3) . ? O7 C7 1.20(3) . ? O8 C8 1.51(4) . ? O9 C9 1.25(2) . ? C3 C31 1.45(3) . ? C31 C32 1.62(3) . ? C5 C59 1.37(3) . ? C5 C51 1.52(3) . ? C51 C54 1.39(4) . ? C51 C53 1.46(3) . ? C51 C52 1.52(4) . ? C59 C9 1.39(3) . ? C2 C21 1.40(5) . ? C91 C92 1.44(4) . ? C91 C93 1.48(5) . ? C91 C94 1.52(4) . ? C91 C9 1.57(4) . ? C1 C11 1.35(4) . ? C12 C11 1.55(4) . ? C47 C4 1.40(4) . ? C47 C7 1.42(4) . ? C71 C72 1.40(4) . ? C71 C74 1.46(5) . ? C71 C73 1.56(5) . ? C71 C7 1.57(4) . ? C4 C41 1.58(4) . ? C6 C61 1.29(6) . ? C41 C43 1.43(4) . ? C41 C44 1.50(5) . ? C41 C42 1.51(4) . ? C8 C81 1.22(4) . ? C21 C22 1.53(6) . ? C62 C61 1.63(6) . ? C82 C81 1.39(8) . ? 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 O7 Ba1 O4 66.1(6) . . ? O7 Ba1 O1 116.1(5) . . ? O4 Ba1 O1 86.4(5) . . ? O7 Ba1 O6 111.5(6) . . ? O4 Ba1 O6 80.2(5) . . ? O1 Ba1 O6 119.1(6) . . ? O7 Ba1 O2 88.9(5) . 2_665 ? O4 Ba1 O2 131.8(5) . 2_665 ? O1 Ba1 O2 141.5(5) . 2_665 ? O6 Ba1 O2 71.6(5) . 2_665 ? O7 Ba1 O3 99.3(5) . . ? O4 Ba1 O3 133.5(4) . . ? O1 Ba1 O3 59.7(4) . . ? O6 Ba1 O3 142.6(4) . . ? O2 Ba1 O3 88.9(4) 2_665 . ? O7 Ba1 O3 146.3(5) . 2_665 ? O4 Ba1 O3 143.6(5) . 2_665 ? O1 Ba1 O3 87.2(4) . 2_665 ? O6 Ba1 O3 71.9(4) . 2_665 ? O2 Ba1 O3 59.7(4) 2_665 2_665 ? O3 Ba1 O3 70.6(4) . 2_665 ? O7 Ba1 Zr1 107.3(4) . . ? O4 Ba1 Zr1 109.1(4) . . ? O1 Ba1 Zr1 29.8(3) . . ? O6 Ba1 Zr1 140.3(4) . . ? O2 Ba1 Zr1 117.7(3) 2_665 . ? O3 Ba1 Zr1 30.2(3) . . ? O3 Ba1 Zr1 80.5(3) 2_665 . ? O7 Ba1 Zr1 118.3(4) . 2_665 ? O4 Ba1 Zr1 143.8(4) . 2_665 ? O1 Ba1 Zr1 117.2(3) . 2_665 ? O6 Ba1 Zr1 64.6(4) . 2_665 ? O2 Ba1 Zr1 29.5(4) 2_665 2_665 ? O3 Ba1 Zr1 82.5(3) . 2_665 ? O3 Ba1 Zr1 30.7(3) 2_665 2_665 ? Zr1 Ba1 Zr1 103.53(5) . 2_665 ? O7 Ba1 Ba1 128.6(4) . 2_665 ? O4 Ba1 Ba1 156.6(4) . 2_665 ? O1 Ba1 Ba1 70.8(3) . 2_665 ? O6 Ba1 Ba1 105.8(4) . 2_665 ? O2 Ba1 Ba1 70.7(3) 2_665 2_665 ? O3 Ba1 Ba1 36.8(2) . 2_665 ? O3 Ba1 Ba1 33.9(2) 2_665 2_665 ? Zr1 Ba1 Ba1 52.00(5) . 2_665 ? Zr1 Ba1 Ba1 51.53(4) 2_665 2_665 ? O3 Zr1 O2 92.3(5) . . ? O3 Zr1 O8 92.3(6) . . ? O2 Zr1 O8 93.4(6) . . ? O3 Zr1 O1 85.5(6) . . ? O2 Zr1 O1 95.8(6) . . ? O8 Zr1 O1 170.6(6) . . ? O3 Zr1 O5 97.7(6) . . ? O2 Zr1 O5 170.0(6) . . ? O8 Zr1 O5 85.9(6) . . ? O1 Zr1 O5 85.4(6) . . ? O3 Zr1 O9 175.4(6) . . ? O2 Zr1 O9 91.9(6) . . ? O8 Zr1 O9 89.4(6) . . ? O1 Zr1 O9 92.1(6) . . ? O5 Zr1 O9 78.2(6) . . ? O3 Zr1 Ba1 45.2(4) . . ? O2 Zr1 Ba1 100.7(4) . . ? O8 Zr1 Ba1 135.2(5) . . ? O1 Zr1 Ba1 40.7(4) . . ? O5 Zr1 Ba1 86.7(4) . . ? O9 Zr1 Ba1 131.7(4) . . ? O3 Zr1 Ba1 50.7(4) . 2_665 ? O2 Zr1 Ba1 42.6(4) . 2_665 ? O8 Zr1 Ba1 86.6(4) . 2_665 ? O1 Zr1 Ba1 99.0(4) . 2_665 ? O5 Zr1 Ba1 147.1(5) . 2_665 ? O9 Zr1 Ba1 133.7(4) . 2_665 ? Ba1 Zr1 Ba1 76.47(5) . 2_665 ? C1 O1 Zr1 131.5(14) . . ? C1 O1 Ba1 114.6(13) . . ? Zr1 O1 Ba1 109.5(7) . . ? C2 O2 Zr1 133.3(15) . . ? C2 O2 Ba1 116.6(14) . 2_665 ? Zr1 O2 Ba1 107.9(7) . 2_665 ? C3 O3 Zr1 137.1(12) . . ? C3 O3 Ba1 109.6(12) . . ? Zr1 O3 Ba1 104.6(5) . . ? C3 O3 Ba1 94.0(12) . 2_665 ? Zr1 O3 Ba1 98.6(5) . 2_665 ? Ba1 O3 Ba1 109.4(4) . 2_665 ? C4 O4 Ba1 137.2(19) . . ? C5 O5 Zr1 132.7(16) . . ? C6 O6 Ba1 128.2(17) . . ? C7 O7 Ba1 139.2(19) . . ? C8 O8 Zr1 141.4(16) . . ? C9 O9 Zr1 136.4(16) . . ? C31 C3 O3 109(2) . . ? C3 C31 C32 108(3) . . ? O5 C5 C59 126(2) . . ? O5 C5 C51 113(3) . . ? C59 C5 C51 121(3) . . ? C54 C51 C53 101(3) . . ? C54 C51 C52 114(3) . . ? C53 C51 C52 103(3) . . ? C54 C51 C5 114(3) . . ? C53 C51 C5 109(2) . . ? C52 C51 C5 114(3) . . ? C5 C59 C9 124(2) . . ? C21 C2 O2 112(4) . . ? C92 C91 C93 112(4) . . ? C92 C91 C94 106(4) . . ? C93 C91 C94 108(4) . . ? C92 C91 C9 111(3) . . ? C93 C91 C9 106(3) . . ? C94 C91 C9 113(3) . . ? O9 C9 C59 122(3) . . ? O9 C9 C91 115(2) . . ? C59 C9 C91 123(3) . . ? C11 C1 O1 117(3) . . ? C4 C47 C7 122(3) . . ? C72 C71 C74 101(4) . . ? C72 C71 C73 103(4) . . ? C74 C71 C73 111(3) . . ? C72 C71 C7 118(3) . . ? C74 C71 C7 113(3) . . ? C73 C71 C7 110(3) . . ? O7 C7 C47 130(3) . . ? O7 C7 C71 117(3) . . ? C47 C7 C71 114(3) . . ? O4 C4 C47 126(3) . . ? O4 C4 C41 113(3) . . ? C47 C4 C41 121(3) . . ? C61 C6 O6 119(5) . . ? C43 C41 C44 114(4) . . ? C43 C41 C42 110(4) . . ? C44 C41 C42 104(3) . . ? C43 C41 C4 110(3) . . ? C44 C41 C4 110(3) . . ? C42 C41 C4 108(3) . . ? C81 C8 O8 117(5) . . ? C2 C21 C22 107(5) . . ? C1 C11 C12 120(4) . . ? C6 C61 C62 115(6) . . ? C8 C81 C82 144(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 17.99 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.177 _refine_diff_density_min -1.368 _refine_diff_density_rms 0.140 data_bazr32m _database_code_depnum_ccdc_archive 'CCDC 234692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H132 Ba2 O16 Zr2' _chemical_formula_weight 1662.86 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' Ba Ba -0.3244 2.2819 '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 10.452(7) _cell_length_b 14.373(9) _cell_length_c 16.179(9) _cell_angle_alpha 67.072(11) _cell_angle_beta 76.53(2) _cell_angle_gamma 89.253(15) _cell_volume 2169(2) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 1653(I>6sigma(I)) _cell_measurement_theta_min 1.41 _cell_measurement_theta_max 27.84 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 860 _exptl_absorpt_coefficient_mu 1.182 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5375 _exptl_absorpt_correction_T_max 0.7182 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6520 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1225 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 20.00 _reflns_number_total 3960 _reflns_number_gt 2058 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1401P)^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 SHELXL _refine_ls_extinction_coef 0.0006(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 3960 _refine_ls_number_parameters 391 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1412 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2083 _refine_ls_wR_factor_gt 0.1845 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.866 _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 Ba1 Ba 0.51188(12) 0.55780(8) 0.10418(6) 0.0825(6) Uani 1 1 d D . . Zr1 Zr 0.43671(16) 0.26734(11) 0.16048(10) 0.0720(6) Uani 1 1 d . . . O1 O 0.3661(10) 0.4067(7) 0.0818(6) 0.067(3) Uani 1 1 d . . . O2 O 0.6654(10) 0.6309(9) 0.1674(8) 0.099(4) Uani 1 1 d . . . O3 O 0.5358(10) 0.2756(8) 0.0331(7) 0.084(3) Uani 1 1 d . . . O4 O 0.4930(11) 0.1396(8) 0.2369(8) 0.102(4) Uani 1 1 d D . . O5 O 0.2752(11) 0.1854(8) 0.1528(8) 0.076(3) Uani 1 1 d . . . O6 O 0.3957(10) 0.5900(9) 0.2453(7) 0.089(3) Uani 1 1 d . . . O7 O 0.2812(15) 0.2593(8) 0.2801(8) 0.094(4) Uani 1 1 d . . . O8 O 0.5595(10) 0.3602(8) 0.1800(7) 0.087(3) Uani 1 1 d . . . C26 C 0.548(2) 0.6593(12) 0.3027(11) 0.077(5) Uani 1 1 d . . . H1A H 0.5542 0.6842 0.3468 0.092 Uiso 1 1 calc R . . C21 C 0.810(2) 0.695(2) 0.2367(18) 0.133(8) Uani 1 1 d . . . C6 C 0.306(2) 0.6347(19) 0.3716(14) 0.117(7) Uani 1 1 d . . . C2 C 0.659(2) 0.6573(13) 0.2389(14) 0.099(6) Uani 1 1 d . . . C61 C 0.430(2) 0.6253(12) 0.3016(10) 0.079(5) Uani 1 1 d . . . C72 C 0.209(3) 0.204(4) 0.4685(19) 0.35(3) Uani 1 1 d . . . H6A H 0.2267 0.1340 0.4850 0.526 Uiso 1 1 calc R . . H6B H 0.1751 0.2156 0.5237 0.526 Uiso 1 1 calc R . . H6C H 0.2898 0.2463 0.4336 0.526 Uiso 1 1 calc R . . C22 C 0.791(2) 0.719(2) 0.3254(15) 0.178(11) Uani 1 1 d . . . H7A H 0.8750 0.7431 0.3280 0.266 Uiso 1 1 calc R . . H7B H 0.7575 0.6584 0.3798 0.266 Uiso 1 1 calc R . . H7C H 0.7305 0.7699 0.3226 0.266 Uiso 1 1 calc R . . C51 C 0.094(2) 0.0707(17) 0.1824(14) 0.111(6) Uani 1 1 d . . . C5 C 0.174(2) 0.1396(13) 0.2081(14) 0.084(5) Uani 1 1 d . . . C52 C 0.034(5) 0.129(2) 0.108(2) 0.35(3) Uani 1 1 d . . . H10A H 0.1013 0.1712 0.0552 0.521 Uiso 1 1 calc R . . H10B H -0.0280 0.1698 0.1280 0.521 Uiso 1 1 calc R . . H10C H -0.0106 0.0831 0.0914 0.521 Uiso 1 1 calc R . . C7 C 0.170(2) 0.2090(14) 0.3229(13) 0.093(6) Uani 1 1 d . . . C73 C -0.027(3) 0.166(2) 0.4613(17) 0.196(12) Uani 1 1 d . . . H12A H -0.0138 0.0953 0.4898 0.295 Uiso 1 1 calc R . . H12B H -0.0789 0.1751 0.4174 0.295 Uiso 1 1 calc R . . H12C H -0.0725 0.1885 0.5080 0.295 Uiso 1 1 calc R . . C57 C 0.114(2) 0.1498(15) 0.2910(13) 0.110(7) Uani 1 1 d . . . H13A H 0.0323 0.1143 0.3253 0.132 Uiso 1 1 calc R . . C74 C 0.055(3) 0.3376(19) 0.3721(19) 0.240(17) Uani 1 1 d . . . H14A H 0.1279 0.3885 0.3397 0.361 Uiso 1 1 calc R . . H14B H 0.0023 0.3507 0.4229 0.361 Uiso 1 1 calc R . . H14C H 0.0019 0.3391 0.3306 0.361 Uiso 1 1 calc R . . C53 C -0.029(5) 0.003(3) 0.263(2) 0.42(4) Uani 1 1 d . . . H15A H -0.0726 -0.0378 0.2416 0.624 Uiso 1 1 calc R . . H15B H -0.0897 0.0468 0.2809 0.624 Uiso 1 1 calc R . . H15C H 0.0017 -0.0399 0.3159 0.624 Uiso 1 1 calc R . . C54 C 0.192(3) 0.005(3) 0.154(4) 0.40(4) Uani 1 1 d . . . H17A H 0.2650 0.0470 0.1059 0.597 Uiso 1 1 calc R . . H17B H 0.1507 -0.0369 0.1327 0.597 Uiso 1 1 calc R . . H17C H 0.2242 -0.0370 0.2068 0.597 Uiso 1 1 calc R . . C1 C 0.221(3) 0.4162(17) 0.0962(14) 0.142(9) Uani 1 1 d . . . H18A H 0.1777 0.3589 0.1535 0.171 Uiso 1 1 calc R . . C62 C 0.328(3) 0.668(4) 0.437(3) 0.38(4) Uani 1 1 d . . . H19A H 0.2455 0.6721 0.4754 0.573 Uiso 1 1 calc R . . H19B H 0.3758 0.7343 0.4056 0.573 Uiso 1 1 calc R . . H19C H 0.3796 0.6219 0.4738 0.573 Uiso 1 1 calc R . . C23 C 0.845(4) 0.793(3) 0.1575(18) 0.36(3) Uani 1 1 d . . . H20A H 0.9321 0.8187 0.1527 0.536 Uiso 1 1 calc R . . H20B H 0.7827 0.8397 0.1664 0.536 Uiso 1 1 calc R . . H20C H 0.8439 0.7844 0.1017 0.536 Uiso 1 1 calc R . . C63 C 0.240(5) 0.537(4) 0.430(4) 0.51(6) Uani 1 1 d . . . H21A H 0.1627 0.5443 0.4723 0.759 Uiso 1 1 calc R . . H21B H 0.2984 0.4964 0.4649 0.759 Uiso 1 1 calc R . . H21C H 0.2152 0.5056 0.3934 0.759 Uiso 1 1 calc R . . C41 C 0.414(6) 0.012(2) 0.381(3) 0.45(4) Uani 1 1 d . . . H22A H 0.4136 -0.0552 0.4267 0.677 Uiso 1 1 calc R . . H22B H 0.3285 0.0201 0.3669 0.677 Uiso 1 1 calc R . . H22C H 0.4323 0.0611 0.4035 0.677 Uiso 1 1 calc R . . C71 C 0.109(3) 0.2286(19) 0.4106(16) 0.151(10) Uani 1 1 d . . . C64 C 0.218(3) 0.706(3) 0.327(2) 0.28(3) Uani 1 1 d . . . H24A H 0.1428 0.7083 0.3734 0.421 Uiso 1 1 calc R . . H24B H 0.1886 0.6844 0.2849 0.421 Uiso 1 1 calc R . . H24C H 0.2641 0.7723 0.2938 0.421 Uiso 1 1 calc R . . C24 C 0.891(3) 0.600(4) 0.255(4) 0.45(5) Uani 1 1 d . . . H25A H 0.9801 0.6188 0.2525 0.681 Uiso 1 1 calc R . . H25B H 0.8920 0.5741 0.2081 0.681 Uiso 1 1 calc R . . H25C H 0.8512 0.5486 0.3147 0.681 Uiso 1 1 calc R . . C42 C 0.641(11) 0.010(7) 0.308(9) 1.00(14) Uiso 1 1 d D . . H26A H 0.7041 0.0229 0.2500 1.507 Uiso 1 1 calc R . . H26B H 0.6411 -0.0598 0.3490 1.507 Uiso 1 1 calc R . . H26C H 0.6632 0.0536 0.3348 1.507 Uiso 1 1 calc R . . C4 C 0.520(5) 0.026(3) 0.292(2) 0.32(3) Uani 1 1 d . . . H27A H 0.4958 -0.0178 0.2635 0.379 Uiso 1 1 calc R . . C11 C 0.162(3) 0.413(2) 0.023(2) 0.223(14) Uani 1 1 d . . . H28A H 0.1852 0.3542 0.0107 0.334 Uiso 1 1 calc R . . H28B H 0.1939 0.4730 -0.0330 0.334 Uiso 1 1 calc R . . H28C H 0.0672 0.4113 0.0422 0.334 Uiso 1 1 calc R . . C32A C 0.453(3) 0.163(2) -0.0545(18) 0.063(8) Uiso 0.50 1 d P . . H31A H 0.4157 0.0966 -0.0419 0.094 Uiso 0.50 1 calc PR . . H31B H 0.4843 0.1997 -0.1202 0.094 Uiso 0.50 1 calc PR . . H31C H 0.3858 0.1986 -0.0304 0.094 Uiso 0.50 1 calc PR . . C12 C 0.1728(18) 0.516(2) 0.108(2) 0.251(17) Uani 1 1 d D . . H32A H 0.2070 0.5249 0.1546 0.376 Uiso 1 1 calc R . . H32B H 0.0780 0.5109 0.1255 0.376 Uiso 1 1 calc R . . H32C H 0.2039 0.5734 0.0500 0.376 Uiso 1 1 calc R . . C82A C 0.465(3) 0.371(2) 0.3675(19) 0.071(9) Uiso 0.50 1 d P . . H33A H 0.4440 0.3419 0.4340 0.107 Uiso 0.50 1 calc PR . . H33B H 0.3931 0.3553 0.3465 0.107 Uiso 0.50 1 calc PR . . H33C H 0.4811 0.4434 0.3455 0.107 Uiso 0.50 1 calc PR . . C3 C 0.636(4) 0.195(2) 0.009(2) 0.27(3) Uani 1 1 d D . . C32 C 0.766(4) 0.205(5) 0.010(5) 0.22(3) Uiso 0.50 1 d PD . . H35A H 0.8121 0.1553 -0.0094 0.323 Uiso 0.50 1 calc PR . . H35B H 0.7725 0.1934 0.0709 0.323 Uiso 0.50 1 calc PR . . H35C H 0.8042 0.2714 -0.0325 0.323 Uiso 0.50 1 calc PR . . C31 C 0.554(2) 0.154(2) -0.014(3) 0.24(2) Uani 1 1 d D . . C82 C 0.769(4) 0.303(3) 0.207(3) 0.109(13) Uiso 0.50 1 d P . . H37A H 0.8307 0.3020 0.2433 0.163 Uiso 0.50 1 calc PR . . H37B H 0.8111 0.3384 0.1426 0.163 Uiso 0.50 1 calc PR . . H37C H 0.7424 0.2341 0.2188 0.163 Uiso 0.50 1 calc PR . . C8 C 0.658(4) 0.351(2) 0.2320(19) 0.211(15) Uani 1 1 d . . . C81 C 0.596(3) 0.326(2) 0.328(2) 0.178(11) Uani 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 Ba1 0.1166(11) 0.0710(8) 0.0685(8) -0.0353(6) -0.0249(6) 0.0005(7) Zr1 0.0920(14) 0.0540(11) 0.0713(11) -0.0218(9) -0.0282(10) 0.0048(9) O1 0.063(7) 0.078(7) 0.071(7) -0.033(6) -0.030(6) 0.011(6) O2 0.084(9) 0.115(10) 0.113(9) -0.072(8) -0.006(7) -0.013(7) O3 0.084(8) 0.072(7) 0.103(8) -0.043(6) -0.023(6) 0.015(6) O4 0.114(10) 0.067(8) 0.112(9) -0.011(7) -0.047(8) 0.015(7) O5 0.061(8) 0.088(8) 0.077(8) -0.029(7) -0.020(6) -0.011(7) O6 0.077(8) 0.126(10) 0.083(7) -0.062(8) -0.018(6) -0.008(7) O7 0.147(12) 0.050(7) 0.089(9) -0.032(6) -0.031(9) 0.003(8) O8 0.093(9) 0.096(8) 0.087(8) -0.032(6) -0.058(7) 0.018(7) C26 0.083(15) 0.074(12) 0.069(12) -0.042(10) 0.014(11) -0.021(11) C21 0.123(19) 0.15(2) 0.19(2) -0.115(19) -0.072(17) -0.014(16) C6 0.13(2) 0.123(18) 0.092(15) -0.056(14) 0.001(15) -0.016(16) C2 0.16(2) 0.070(12) 0.101(15) -0.046(12) -0.066(16) 0.015(13) C61 0.117(18) 0.065(11) 0.044(10) -0.018(9) -0.007(12) 0.000(12) C72 0.25(4) 0.76(10) 0.14(2) -0.27(4) -0.08(3) 0.14(5) C22 0.15(2) 0.26(3) 0.17(2) -0.13(2) -0.057(18) -0.08(2) C51 0.124(18) 0.118(17) 0.088(14) -0.034(13) -0.032(13) -0.011(15) C5 0.104(17) 0.069(13) 0.093(16) -0.041(12) -0.033(13) 0.008(12) C52 0.66(9) 0.16(3) 0.31(4) -0.06(3) -0.35(6) -0.06(4) C7 0.107(18) 0.058(12) 0.083(15) -0.007(11) -0.001(13) -0.016(12) C73 0.23(3) 0.20(3) 0.16(2) -0.11(2) 0.02(2) -0.03(3) C57 0.118(17) 0.111(16) 0.087(14) -0.039(13) 0.006(12) -0.052(13) C74 0.34(4) 0.10(2) 0.22(3) -0.06(2) 0.04(3) 0.05(2) C53 0.65(9) 0.34(5) 0.21(4) -0.14(4) 0.06(5) -0.37(6) C54 0.21(3) 0.38(6) 0.90(12) -0.56(8) -0.15(5) 0.09(4) C1 0.23(3) 0.120(18) 0.105(16) -0.049(14) -0.09(2) 0.05(2) C62 0.12(2) 0.83(11) 0.41(5) -0.53(7) 0.05(3) -0.06(4) C23 0.39(6) 0.45(6) 0.12(2) 0.00(3) -0.03(3) -0.38(5) C63 0.51(8) 0.38(7) 0.53(8) -0.37(7) 0.40(7) -0.24(7) C41 0.86(13) 0.13(3) 0.24(4) 0.06(3) -0.15(6) 0.15(5) C71 0.17(3) 0.12(2) 0.097(18) -0.029(15) 0.055(18) -0.031(19) C64 0.21(3) 0.48(7) 0.18(3) -0.17(4) -0.05(3) 0.21(4) C24 0.25(4) 0.67(9) 0.95(13) -0.74(10) -0.36(6) 0.26(6) C4 0.36(6) 0.22(4) 0.17(3) 0.14(3) -0.06(3) -0.13(4) C11 0.19(3) 0.21(3) 0.22(3) -0.03(3) -0.06(3) -0.04(2) C12 0.31(4) 0.17(3) 0.27(4) -0.13(3) 0.00(3) 0.03(3) C3 0.50(8) 0.18(3) 0.17(3) -0.13(2) -0.03(4) -0.11(4) C31 0.043(16) 0.21(3) 0.50(6) -0.20(4) -0.02(2) 0.016(18) C8 0.34(5) 0.20(3) 0.12(2) -0.09(2) -0.09(3) -0.02(3) C81 0.17(3) 0.22(3) 0.21(3) -0.12(3) -0.11(2) 0.04(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 Ba1 O2 2.524(11) . ? Ba1 O6 2.534(10) . ? Ba1 O3 2.694(10) 2_665 ? Ba1 O8 2.711(10) . ? Ba1 O1 2.824(9) 2_665 ? Ba1 O1 2.850(10) . ? Ba1 Zr1 3.939(3) 2_665 ? Ba1 Zr1 3.958(3) . ? Ba1 Ba1 4.353(3) 2_665 ? Zr1 O4 1.947(10) . ? Zr1 O8 2.023(11) . ? Zr1 O3 2.038(11) . ? Zr1 O5 2.125(11) . ? Zr1 O1 2.142(10) . ? Zr1 O7 2.183(13) . ? Zr1 Ba1 3.939(3) 2_665 ? O1 C1 1.49(3) . ? O1 Ba1 2.824(9) 2_665 ? O2 C2 1.339(18) . ? O3 C3 1.64(3) . ? O3 Ba1 2.694(10) 2_665 ? O4 C4 1.58(4) . ? O5 C5 1.212(19) . ? O6 C61 1.313(19) . ? O7 C7 1.271(19) . ? O8 C8 1.45(3) . ? C26 C61 1.34(2) . ? C26 C2 1.37(2) . ? C21 C23 1.47(3) . ? C21 C24 1.56(4) . ? C21 C22 1.57(3) . ? C21 C2 1.66(3) . ? C6 C62 1.38(3) . ? C6 C63 1.42(4) . ? C6 C64 1.46(3) . ? C6 C61 1.55(2) . ? C72 C71 1.51(3) . ? C51 C52 1.45(3) . ? C51 C54 1.49(3) . ? C51 C5 1.53(2) . ? C51 C53 1.60(4) . ? C5 C57 1.40(2) . ? C7 C57 1.35(2) . ? C7 C71 1.54(3) . ? C73 C71 1.56(3) . ? C74 C71 1.60(3) . ? C1 C11 1.48(3) . ? C1 C12 1.58(3) . ? C41 C4 1.53(6) . ? C42 C4 1.35(9) . ? C32A C31 1.36(4) . ? C82A C81 1.61(3) . ? C3 C31 1.24(3) . ? C3 C32 1.37(2) . ? C82 C8 1.41(4) . ? C8 C81 1.44(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Ba1 O6 66.5(3) . . ? O2 Ba1 O3 102.0(4) . 2_665 ? O6 Ba1 O3 101.0(3) . 2_665 ? O2 Ba1 O8 98.7(4) . . ? O6 Ba1 O8 102.3(3) . . ? O3 Ba1 O8 153.5(3) 2_665 . ? O2 Ba1 O1 109.0(3) . 2_665 ? O6 Ba1 O1 160.4(3) . 2_665 ? O3 Ba1 O1 60.5(3) 2_665 2_665 ? O8 Ba1 O1 97.2(3) . 2_665 ? O2 Ba1 O1 158.1(3) . . ? O6 Ba1 O1 111.6(3) . . ? O3 Ba1 O1 99.8(3) 2_665 . ? O8 Ba1 O1 59.7(3) . . ? O1 Ba1 O1 79.8(3) 2_665 . ? O2 Ba1 Zr1 107.8(3) . 2_665 ? O6 Ba1 Zr1 129.4(3) . 2_665 ? O3 Ba1 Zr1 28.7(2) 2_665 2_665 ? O8 Ba1 Zr1 127.7(2) . 2_665 ? O1 Ba1 Zr1 31.8(2) 2_665 2_665 ? O1 Ba1 Zr1 90.27(19) . 2_665 ? O2 Ba1 Zr1 126.6(3) . . ? O6 Ba1 Zr1 107.8(3) . . ? O3 Ba1 Zr1 130.1(2) 2_665 . ? O8 Ba1 Zr1 28.1(2) . . ? O1 Ba1 Zr1 90.3(2) 2_665 . ? O1 Ba1 Zr1 31.67(19) . . ? Zr1 Ba1 Zr1 113.10(4) 2_665 . ? O2 Ba1 Ba1 144.9(2) . 2_665 ? O6 Ba1 Ba1 148.5(2) . 2_665 ? O3 Ba1 Ba1 78.0(2) 2_665 2_665 ? O8 Ba1 Ba1 75.6(2) . 2_665 ? O1 Ba1 Ba1 40.1(2) 2_665 2_665 ? O1 Ba1 Ba1 39.68(18) . 2_665 ? Zr1 Ba1 Ba1 56.75(5) 2_665 2_665 ? Zr1 Ba1 Ba1 56.34(4) . 2_665 ? O4 Zr1 O8 97.2(4) . . ? O4 Zr1 O3 99.2(5) . . ? O8 Zr1 O3 100.3(4) . . ? O4 Zr1 O5 89.1(4) . . ? O8 Zr1 O5 167.6(4) . . ? O3 Zr1 O5 89.1(4) . . ? O4 Zr1 O1 177.1(4) . . ? O8 Zr1 O1 83.4(4) . . ? O3 Zr1 O1 83.4(4) . . ? O5 Zr1 O1 89.8(4) . . ? O4 Zr1 O7 89.4(4) . . ? O8 Zr1 O7 92.7(5) . . ? O3 Zr1 O7 163.3(4) . . ? O5 Zr1 O7 76.7(5) . . ? O1 Zr1 O7 87.8(4) . . ? O4 Zr1 Ba1 138.5(3) . 2_665 ? O8 Zr1 Ba1 93.0(3) . 2_665 ? O3 Zr1 Ba1 39.4(3) . 2_665 ? O5 Zr1 Ba1 89.3(3) . 2_665 ? O1 Zr1 Ba1 44.0(2) . 2_665 ? O7 Zr1 Ba1 130.2(3) . 2_665 ? O4 Zr1 Ba1 136.1(3) . . ? O8 Zr1 Ba1 39.2(3) . . ? O3 Zr1 Ba1 95.3(3) . . ? O5 Zr1 Ba1 132.5(3) . . ? O1 Zr1 Ba1 44.3(3) . . ? O7 Zr1 Ba1 88.2(3) . . ? Ba1 Zr1 Ba1 66.90(4) 2_665 . ? C1 O1 Zr1 119.6(11) . . ? C1 O1 Ba1 111.6(9) . 2_665 ? Zr1 O1 Ba1 104.1(4) . 2_665 ? C1 O1 Ba1 115.0(10) . . ? Zr1 O1 Ba1 104.0(3) . . ? Ba1 O1 Ba1 100.2(3) 2_665 . ? C2 O2 Ba1 138.3(12) . . ? C3 O3 Zr1 127.5(13) . . ? C3 O3 Ba1 120.5(13) . 2_665 ? Zr1 O3 Ba1 112.0(4) . 2_665 ? C4 O4 Zr1 168.8(18) . . ? C5 O5 Zr1 133.7(11) . . ? C61 O6 Ba1 136.7(11) . . ? C7 O7 Zr1 135.2(12) . . ? C8 O8 Zr1 137.9(14) . . ? C8 O8 Ba1 109.0(14) . . ? Zr1 O8 Ba1 112.6(4) . . ? C61 C26 C2 120.1(17) . . ? C23 C21 C24 127(3) . . ? C23 C21 C22 106(2) . . ? C24 C21 C22 106(2) . . ? C23 C21 C2 105(2) . . ? C24 C21 C2 107(2) . . ? C22 C21 C2 104.5(18) . . ? C62 C6 C63 101(3) . . ? C62 C6 C64 103(3) . . ? C63 C6 C64 113(3) . . ? C62 C6 C61 117(2) . . ? C63 C6 C61 110(2) . . ? C64 C6 C61 113.0(19) . . ? O2 C2 C26 127.3(18) . . ? O2 C2 C21 109.0(18) . . ? C26 C2 C21 123.6(17) . . ? O6 C61 C26 130.9(16) . . ? O6 C61 C6 110.9(18) . . ? C26 C61 C6 118.0(17) . . ? C52 C51 C54 111(3) . . ? C52 C51 C5 111.8(19) . . ? C54 C51 C5 104.7(18) . . ? C52 C51 C53 103(3) . . ? C54 C51 C53 111(3) . . ? C5 C51 C53 115.0(19) . . ? O5 C5 C57 126.8(18) . . ? O5 C5 C51 117.9(17) . . ? C57 C5 C51 115(2) . . ? O7 C7 C57 122.3(18) . . ? O7 C7 C71 111(2) . . ? C57 C7 C71 127(2) . . ? C7 C57 C5 122.6(18) . . ? C11 C1 O1 116(2) . . ? C11 C1 C12 103(2) . . ? O1 C1 C12 115.7(19) . . ? C72 C71 C7 107(2) . . ? C72 C71 C73 114(2) . . ? C7 C71 C73 110(2) . . ? C72 C71 C74 123(3) . . ? C7 C71 C74 104.1(19) . . ? C73 C71 C74 97(2) . . ? C42 C4 C41 113(7) . . ? C42 C4 O4 117(5) . . ? C41 C4 O4 95(3) . . ? C31 C3 C32 145(4) . . ? C31 C3 O3 95(3) . . ? C32 C3 O3 119(3) . . ? C3 C31 C32A 149(3) . . ? C82 C8 C81 120(3) . . ? C82 C8 O8 115(2) . . ? C81 C8 O8 110(3) . . ? C8 C81 C82A 126(3) . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.638 _refine_diff_density_min -1.079 _refine_diff_density_rms 0.122 data_bazroh1m _database_code_depnum_ccdc_archive 'CCDC 239960' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H120 Ba2 O18 Zr2' _chemical_formula_weight 1442.56 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' Ba Ba -0.3244 2.2819 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.050(3) _cell_length_b 15.636(5) _cell_length_c 21.543(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.920(5) _cell_angle_gamma 90.00 _cell_volume 3676.9(18) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 8037(I>2sigma(I)) _cell_measurement_theta_min 1.62 _cell_measurement_theta_max 26.14 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 1.384 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7235 _exptl_absorpt_correction_T_max 0.9340 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17937 _diffrn_reflns_av_R_equivalents 0.0813 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6437 _reflns_number_gt 3630 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.0551P)^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 6437 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1043 _refine_ls_R_factor_gt 0.0569 _refine_ls_wR_factor_ref 0.1218 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 0.898 _refine_ls_restrained_S_all 0.898 _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 Ba1 Ba 0.51416(4) 0.47868(3) 0.09952(2) 0.05349(16) Uani 1 1 d . . . Zr2 Zr 0.39201(6) 0.69016(4) 0.01662(3) 0.0509(2) Uani 1 1 d . . . O1 O 0.5414(4) 0.6002(3) 0.01413(19) 0.0482(11) Uani 1 1 d . . . O2 O 0.6805(4) 0.3654(3) 0.0698(2) 0.0579(12) Uani 1 1 d . . . O3 O 0.3281(4) 0.5851(3) 0.0637(2) 0.0606(13) Uani 1 1 d . . . O4 O 0.4915(4) 0.7708(3) -0.0337(2) 0.0620(13) Uani 1 1 d . . . O5 O 0.2538(5) 0.7657(3) 0.0206(3) 0.0774(16) Uani 1 1 d . . . O6 O 0.4919(5) 0.7332(3) 0.1020(2) 0.0698(14) Uani 1 1 d . . . O7 O 0.4077(5) 0.3206(3) 0.1162(3) 0.0796(16) Uani 1 1 d . . . O8 O 0.5279(8) 0.5128(5) 0.2290(3) 0.132(3) Uani 1 1 d . . . O9 O 0.6435(6) 0.6240(4) 0.1593(3) 0.0844(17) Uani 1 1 d . . . C1 C 0.4604(12) 0.7972(7) 0.1428(5) 0.118(4) Uani 1 1 d . . . H1A H 0.3938 0.8303 0.1187 0.141 Uiso 1 1 calc R . . C11 C 0.5569(15) 0.8576(7) 0.1643(5) 0.169(6) Uani 1 1 d . . . H11A H 0.5270 0.8998 0.1905 0.254 Uiso 1 1 calc R . . H11B H 0.5827 0.8852 0.1287 0.254 Uiso 1 1 calc R . . H11C H 0.6251 0.8280 0.1879 0.254 Uiso 1 1 calc R . . C12 C 0.4109(16) 0.7605(9) 0.1960(7) 0.207(9) Uani 1 1 d . . . H12A H 0.3419 0.7249 0.1808 0.310 Uiso 1 1 calc R . . H12B H 0.3855 0.8057 0.2213 0.310 Uiso 1 1 calc R . . H12C H 0.4729 0.7267 0.2209 0.310 Uiso 1 1 calc R . . C2 C 0.7656(8) 0.3318(7) 0.1166(5) 0.105(4) Uani 1 1 d . . . C21 C 0.8870(10) 0.3675(8) 0.1193(5) 0.133(5) Uani 1 1 d . . . H21A H 0.9017 0.3801 0.0775 0.200 Uiso 1 1 calc R . . H21B H 0.9467 0.3271 0.1384 0.200 Uiso 1 1 calc R . . H21C H 0.8931 0.4192 0.1436 0.200 Uiso 1 1 calc R . . C22 C 0.7369(12) 0.3030(13) 0.1675(7) 0.283(14) Uani 1 1 d . . . H22A H 0.6556 0.2797 0.1596 0.425 Uiso 1 1 calc R . . H22B H 0.7397 0.3485 0.1976 0.425 Uiso 1 1 calc R . . H22C H 0.7937 0.2590 0.1838 0.425 Uiso 1 1 calc R . . C3 C 0.2020(8) 0.5633(6) 0.0626(5) 0.089(3) Uani 1 1 d . . . H3A H 0.1502 0.6075 0.0398 0.107 Uiso 1 1 calc R . . C31 C 0.1744(9) 0.4761(7) 0.0294(5) 0.118(4) Uani 1 1 d . . . H31A H 0.1892 0.4801 -0.0132 0.178 Uiso 1 1 calc R . . H31B H 0.0903 0.4611 0.0298 0.178 Uiso 1 1 calc R . . H31C H 0.2267 0.4330 0.0511 0.178 Uiso 1 1 calc R . . C32 C 0.1782(11) 0.5591(8) 0.1277(6) 0.166(6) Uani 1 1 d . . . H32A H 0.1948 0.6138 0.1475 0.250 Uiso 1 1 calc R . . H32B H 0.2302 0.5166 0.1503 0.250 Uiso 1 1 calc R . . H32C H 0.0940 0.5442 0.1280 0.250 Uiso 1 1 calc R . . C4 C 0.5139(10) 0.8584(6) -0.0231(4) 0.091(3) Uani 1 1 d . . . H4A H 0.4714 0.8769 0.0112 0.109 Uiso 1 1 calc R . . C41 C 0.4674(14) 0.9101(6) -0.0804(5) 0.158(6) Uani 1 1 d . . . H41A H 0.3807 0.9019 -0.0914 0.238 Uiso 1 1 calc R . . H41B H 0.5076 0.8920 -0.1146 0.238 Uiso 1 1 calc R . . H41C H 0.4843 0.9695 -0.0718 0.238 Uiso 1 1 calc R . . C42 C 0.6515(12) 0.8701(8) -0.0026(6) 0.157(6) Uani 1 1 d . . . H42A H 0.6772 0.8382 0.0352 0.236 Uiso 1 1 calc R . . H42B H 0.6692 0.9296 0.0049 0.236 Uiso 1 1 calc R . . H42C H 0.6945 0.8498 -0.0352 0.236 Uiso 1 1 calc R . . C5 C 0.1509(12) 0.8201(8) 0.0204(8) 0.165(6) Uani 1 1 d . . . C51 C 0.1700(13) 0.9014(8) 0.0115(9) 0.241(11) Uani 1 1 d . . . H51A H 0.0969 0.9330 0.0149 0.362 Uiso 1 1 calc R . . H51B H 0.1914 0.9095 -0.0296 0.362 Uiso 1 1 calc R . . H51C H 0.2356 0.9212 0.0426 0.362 Uiso 1 1 calc R . . C52 C 0.0536(16) 0.7910(10) 0.0378(12) 0.317(16) Uani 1 1 d . . . H52A H -0.0028 0.8371 0.0403 0.476 Uiso 1 1 calc R . . H52B H 0.0737 0.7645 0.0783 0.476 Uiso 1 1 calc R . . H52C H 0.0167 0.7496 0.0078 0.476 Uiso 1 1 calc R . . C7 C 0.3418(12) 0.2768(9) 0.1559(6) 0.139(5) Uani 1 1 d . . . C71 C 0.2137(13) 0.2699(10) 0.1319(8) 0.200(8) Uani 1 1 d . . . H71A H 0.1733 0.2394 0.1615 0.300 Uiso 1 1 calc R . . H71B H 0.2032 0.2396 0.0927 0.300 Uiso 1 1 calc R . . H71C H 0.1790 0.3260 0.1255 0.300 Uiso 1 1 calc R . . C72 C 0.3898(16) 0.2683(13) 0.2123(8) 0.266(12) Uani 1 1 d . . . H72A H 0.4766 0.2772 0.2160 0.399 Uiso 1 1 calc R . . H72B H 0.3742 0.2116 0.2263 0.399 Uiso 1 1 calc R . . H72C H 0.3554 0.3095 0.2376 0.399 Uiso 1 1 calc R . . C8 C 0.505(3) 0.5029(14) 0.2928(6) 0.238(11) Uani 1 1 d . . . H8A H 0.4588 0.4490 0.2893 0.286 Uiso 1 1 calc R . . C81 C 0.619(2) 0.4756(18) 0.3304(9) 0.336(18) Uani 1 1 d . . . H81A H 0.6066 0.4657 0.3729 0.504 Uiso 1 1 calc R . . H81B H 0.6800 0.5193 0.3298 0.504 Uiso 1 1 calc R . . H81C H 0.6467 0.4237 0.3132 0.504 Uiso 1 1 calc R . . C82 C 0.426(3) 0.5530(17) 0.3122(10) 0.43(3) Uani 1 1 d . . . H82A H 0.3548 0.5572 0.2807 0.643 Uiso 1 1 calc R . . H82B H 0.4618 0.6087 0.3202 0.643 Uiso 1 1 calc R . . H82C H 0.4034 0.5305 0.3502 0.643 Uiso 1 1 calc R . . C9 C 0.7671(12) 0.6512(9) 0.1716(7) 0.141(5) Uani 1 1 d . . . H9A H 0.7610 0.7027 0.1968 0.169 Uiso 1 1 calc R . . C91 C 0.8201(13) 0.6819(12) 0.1243(7) 0.214(10) Uani 1 1 d . . . H91A H 0.7646 0.7201 0.0992 0.321 Uiso 1 1 calc R . . H91B H 0.8403 0.6354 0.0986 0.321 Uiso 1 1 calc R . . H91C H 0.8935 0.7122 0.1411 0.321 Uiso 1 1 calc R . . C92 C 0.8417(12) 0.5922(9) 0.2190(6) 0.168(6) Uani 1 1 d . . . H92A H 0.9244 0.6128 0.2281 0.252 Uiso 1 1 calc R . . H92B H 0.8416 0.5355 0.2019 0.252 Uiso 1 1 calc R . . H92C H 0.8062 0.5910 0.2569 0.252 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 Ba1 0.0570(3) 0.0570(3) 0.0486(3) 0.0022(2) 0.01508(19) 0.0048(2) Zr2 0.0507(4) 0.0481(4) 0.0573(4) 0.0030(3) 0.0192(3) 0.0042(3) O1 0.043(3) 0.057(3) 0.045(3) -0.001(2) 0.009(2) 0.000(2) O2 0.047(3) 0.070(3) 0.056(3) 0.004(2) 0.008(2) 0.004(2) O3 0.052(3) 0.064(3) 0.073(3) 0.011(2) 0.029(3) 0.000(2) O4 0.069(4) 0.050(3) 0.072(3) 0.004(2) 0.028(3) -0.001(3) O5 0.077(4) 0.066(3) 0.095(4) 0.002(3) 0.029(3) 0.024(3) O6 0.082(4) 0.067(3) 0.063(3) -0.014(3) 0.019(3) 0.003(3) O7 0.086(4) 0.074(4) 0.091(4) 0.014(3) 0.053(3) -0.007(3) O8 0.187(8) 0.149(6) 0.065(4) 0.001(4) 0.032(5) -0.002(6) O9 0.076(4) 0.087(4) 0.083(4) -0.015(3) -0.009(3) -0.012(3) C1 0.137(11) 0.129(10) 0.085(8) -0.035(7) 0.012(7) 0.018(8) C11 0.30(2) 0.098(9) 0.108(9) -0.045(7) 0.022(11) -0.034(11) C12 0.32(2) 0.176(14) 0.166(13) -0.092(11) 0.165(15) -0.096(14) C2 0.049(6) 0.157(10) 0.100(8) 0.051(7) -0.019(5) -0.002(6) C21 0.083(8) 0.185(12) 0.123(10) 0.060(9) -0.009(7) -0.003(8) C22 0.093(10) 0.56(4) 0.176(15) 0.24(2) -0.042(10) -0.071(16) C3 0.057(6) 0.087(6) 0.135(9) 0.019(6) 0.051(6) 0.010(5) C31 0.075(7) 0.106(8) 0.174(11) 0.011(8) 0.019(7) -0.024(6) C32 0.145(12) 0.194(14) 0.196(14) -0.006(11) 0.139(11) -0.029(10) C4 0.124(9) 0.064(6) 0.094(7) -0.007(5) 0.045(6) -0.004(6) C41 0.290(19) 0.074(7) 0.134(10) 0.026(7) 0.101(11) 0.040(9) C42 0.142(12) 0.142(11) 0.199(14) -0.051(10) 0.062(11) -0.077(10) C5 0.115(10) 0.087(9) 0.32(2) 0.035(10) 0.118(12) 0.056(8) C51 0.176(15) 0.104(11) 0.48(3) 0.110(15) 0.177(18) 0.079(10) C52 0.177(16) 0.145(14) 0.69(5) 0.07(2) 0.27(2) 0.080(13) C7 0.112(10) 0.199(13) 0.108(9) 0.071(9) 0.020(8) -0.050(9) C71 0.128(13) 0.204(17) 0.29(2) 0.045(15) 0.106(13) -0.045(12) C72 0.180(18) 0.43(3) 0.190(18) 0.19(2) 0.042(14) -0.067(19) C8 0.37(3) 0.28(2) 0.059(9) 0.022(12) 0.013(14) 0.03(2) C81 0.29(3) 0.60(5) 0.117(14) 0.12(2) 0.017(17) -0.03(3) C82 0.68(6) 0.49(4) 0.16(2) 0.01(2) 0.19(3) 0.38(5) C9 0.112(11) 0.140(11) 0.156(13) -0.001(9) -0.019(10) -0.003(9) C91 0.125(13) 0.33(3) 0.184(17) 0.102(16) 0.016(12) -0.050(14) C92 0.107(10) 0.200(15) 0.178(13) 0.035(11) -0.041(10) -0.015(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 Ba1 O3 2.665(5) . ? Ba1 O1 2.694(4) . ? Ba1 O2 2.700(5) . ? Ba1 O1 2.725(4) 3_665 ? Ba1 O7 2.784(5) . ? Ba1 O8 2.820(6) . ? Ba1 O9 2.879(5) . ? Ba1 Zr2 3.8870(11) 3_665 ? Ba1 Zr2 3.8984(11) . ? Ba1 Ba1 4.3024(15) 3_665 ? Zr2 O5 1.943(5) . ? Zr2 O4 2.084(5) . ? Zr2 O2 2.098(5) 3_665 ? Zr2 O6 2.104(5) . ? Zr2 O3 2.109(4) . ? Zr2 O1 2.176(4) . ? Zr2 Ba1 3.8870(11) 3_665 ? O1 Ba1 2.725(4) 3_665 ? O2 C2 1.372(9) . ? O2 Zr2 2.098(5) 3_665 ? O3 C3 1.431(9) . ? O4 C4 1.405(9) . ? O5 C5 1.419(11) . ? O6 C1 1.411(11) . ? O7 C7 1.388(11) . ? O8 C8 1.446(16) . ? O9 C9 1.416(13) . ? C1 C11 1.445(15) . ? C1 C12 1.462(15) . ? C2 C22 1.270(14) . ? C2 C21 1.446(13) . ? C3 C32 1.470(14) . ? C3 C31 1.547(13) . ? C4 C41 1.498(14) . ? C4 C42 1.527(14) . ? C5 C52 1.275(17) . ? C5 C51 1.307(15) . ? C7 C72 1.255(16) . ? C7 C71 1.433(17) . ? C8 C82 1.28(3) . ? C8 C81 1.46(3) . ? C9 C91 1.341(16) . ? C9 C92 1.521(16) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Ba1 O1 61.61(13) . . ? O3 Ba1 O2 149.78(14) . . ? O1 Ba1 O2 98.56(13) . . ? O3 Ba1 O1 88.05(14) . 3_665 ? O1 Ba1 O1 74.88(14) . 3_665 ? O2 Ba1 O1 63.71(13) . 3_665 ? O3 Ba1 O7 105.61(15) . . ? O1 Ba1 O7 143.93(15) . . ? O2 Ba1 O7 76.40(15) . . ? O1 Ba1 O7 70.92(14) 3_665 . ? O3 Ba1 O8 95.1(2) . . ? O1 Ba1 O8 123.17(18) . . ? O2 Ba1 O8 115.1(2) . . ? O1 Ba1 O8 160.76(18) 3_665 . ? O7 Ba1 O8 89.98(19) . . ? O3 Ba1 O9 86.79(16) . . ? O1 Ba1 O9 69.43(15) . . ? O2 Ba1 O9 108.35(16) . . ? O1 Ba1 O9 141.81(15) 3_665 . ? O7 Ba1 O9 146.41(16) . . ? O8 Ba1 O9 57.42(19) . . ? O3 Ba1 Zr2 120.56(11) . 3_665 ? O1 Ba1 Zr2 88.30(9) . 3_665 ? O2 Ba1 Zr2 30.97(10) . 3_665 ? O1 Ba1 Zr2 32.84(9) 3_665 3_665 ? O7 Ba1 Zr2 68.92(11) . 3_665 ? O8 Ba1 Zr2 141.84(16) . 3_665 ? O9 Ba1 Zr2 131.33(13) . 3_665 ? O3 Ba1 Zr2 30.77(9) . . ? O1 Ba1 Zr2 32.47(9) . . ? O2 Ba1 Zr2 130.40(10) . . ? O1 Ba1 Zr2 87.62(9) 3_665 . ? O7 Ba1 Zr2 133.52(12) . . ? O8 Ba1 Zr2 104.72(16) . . ? O9 Ba1 Zr2 69.41(12) . . ? Zr2 Ba1 Zr2 112.90(2) 3_665 . ? O3 Ba1 Ba1 71.38(10) . 3_665 ? O1 Ba1 Ba1 37.70(9) . 3_665 ? O2 Ba1 Ba1 79.20(9) . 3_665 ? O1 Ba1 Ba1 37.18(9) 3_665 3_665 ? O7 Ba1 Ba1 107.40(12) . 3_665 ? O8 Ba1 Ba1 160.15(15) . 3_665 ? O9 Ba1 Ba1 106.14(12) . 3_665 ? Zr2 Ba1 Ba1 56.58(2) 3_665 3_665 ? Zr2 Ba1 Ba1 56.326(15) . 3_665 ? O5 Zr2 O4 97.9(2) . . ? O5 Zr2 O2 95.5(2) . 3_665 ? O4 Zr2 O2 87.00(18) . 3_665 ? O5 Zr2 O6 94.4(2) . . ? O4 Zr2 O6 90.8(2) . . ? O2 Zr2 O6 170.05(19) 3_665 . ? O5 Zr2 O3 97.4(2) . . ? O4 Zr2 O3 164.64(18) . . ? O2 Zr2 O3 89.66(19) 3_665 . ? O6 Zr2 O3 89.9(2) . . ? O5 Zr2 O1 177.0(2) . . ? O4 Zr2 O1 85.11(17) . . ? O2 Zr2 O1 84.10(17) 3_665 . ? O6 Zr2 O1 86.04(18) . . ? O3 Zr2 O1 79.64(17) . . ? O5 Zr2 Ba1 136.98(17) . 3_665 ? O4 Zr2 Ba1 82.00(13) . 3_665 ? O2 Zr2 Ba1 41.47(12) 3_665 3_665 ? O6 Zr2 Ba1 128.60(14) . 3_665 ? O3 Zr2 Ba1 85.58(13) . 3_665 ? O1 Zr2 Ba1 42.77(11) . 3_665 ? O5 Zr2 Ba1 135.56(16) . . ? O4 Zr2 Ba1 125.33(14) . . ? O2 Zr2 Ba1 96.49(13) 3_665 . ? O6 Zr2 Ba1 76.88(14) . . ? O3 Zr2 Ba1 40.27(13) . . ? O1 Zr2 Ba1 41.65(11) . . ? Ba1 Zr2 Ba1 67.10(2) 3_665 . ? Zr2 O1 Ba1 105.88(16) . . ? Zr2 O1 Ba1 104.39(16) . 3_665 ? Ba1 O1 Ba1 105.12(14) . 3_665 ? C2 O2 Zr2 128.2(6) . 3_665 ? C2 O2 Ba1 119.4(6) . . ? Zr2 O2 Ba1 107.56(18) 3_665 . ? C3 O3 Zr2 125.1(5) . . ? C3 O3 Ba1 124.2(4) . . ? Zr2 O3 Ba1 108.96(18) . . ? C4 O4 Zr2 126.8(5) . . ? C5 O5 Zr2 177.3(8) . . ? C1 O6 Zr2 128.7(6) . . ? C7 O7 Ba1 142.2(7) . . ? C8 O8 Ba1 158.4(11) . . ? C9 O9 Ba1 135.9(7) . . ? O6 C1 C11 115.0(10) . . ? O6 C1 C12 111.5(10) . . ? C11 C1 C12 110.7(10) . . ? C22 C2 O2 122.4(10) . . ? C22 C2 C21 117.2(10) . . ? O2 C2 C21 114.0(9) . . ? O3 C3 C32 108.3(9) . . ? O3 C3 C31 109.8(7) . . ? C32 C3 C31 110.5(9) . . ? O4 C4 C41 111.3(8) . . ? O4 C4 C42 107.9(8) . . ? C41 C4 C42 111.8(10) . . ? C52 C5 C51 123.5(12) . . ? C52 C5 O5 119.8(12) . . ? C51 C5 O5 115.8(12) . . ? C72 C7 O7 117.8(12) . . ? C72 C7 C71 126.0(13) . . ? O7 C7 C71 113.4(11) . . ? C82 C8 O8 118(2) . . ? C82 C8 C81 125(2) . . ? O8 C8 C81 107(2) . . ? C91 C9 O9 119.2(12) . . ? C91 C9 C92 118.2(14) . . ? O9 C9 C92 110.5(12) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.834 _refine_diff_density_min -0.829 _refine_diff_density_rms 0.093 data_srzroh1m _database_code_depnum_ccdc_archive 'CCDC 239961' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H104 O16 Sr2 Zr2' _chemical_formula_weight 1222.93 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' Sr Sr -1.5307 3.2498 '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 10.901(5) _cell_length_b 12.732(7) _cell_length_c 13.026(7) _cell_angle_alpha 109.052(19) _cell_angle_beta 100.230(17) _cell_angle_gamma 99.51(2) _cell_volume 1632.6(14) _cell_formula_units_Z 1 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 2953 _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 27.15 _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 'not measured' _exptl_crystal_density_diffrn 1.244 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.985 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5433 _exptl_absorpt_correction_T_max 0.8262 _exptl_absorpt_process_details 'Bruker SADABS' _diffrn_special_details ; Warning! It should be mentioned that the placement of hydrogen atoms in this structure can not be considered as definite in the view of unresolved disorder in carbon atoms they are attached to. Their introduction, however, serves to reduce the residual electron density in the structure and improves considerably the quality of the resolved model and decreases the observed R-factor ; _diffrn_ambient_temperature 295(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 'Bruker SMART CCD 1k' _diffrn_measurement_method 'Bruker SMART' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6552 _diffrn_reflns_av_R_equivalents 0.0315 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4230 _reflns_number_gt 2507 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINTPLUS' _computing_data_reduction 'Bruker SAINTPLUS' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL-NT' _computing_publication_material 'Bruker SHELXTL-NT' _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^)+(0.1200P)^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 SHELXL _refine_ls_extinction_coef 0.0014(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4230 _refine_ls_number_parameters 265 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1122 _refine_ls_R_factor_gt 0.0636 _refine_ls_wR_factor_ref 0.1834 _refine_ls_wR_factor_gt 0.1672 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.917 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.66837(8) 0.69568(7) 0.22468(6) 0.0559(3) Uani 1 1 d . . . Sr1 Sr 0.47243(9) 0.39748(7) 0.08178(7) 0.0746(4) Uani 1 1 d . . . O1 O 0.5037(6) 0.5881(5) 0.2317(5) 0.0672(16) Uani 1 1 d . . . O2 O 0.5463(6) 0.7403(5) 0.1091(5) 0.0700(16) Uani 1 1 d . . . O3 O 0.6440(6) 0.5467(5) 0.0712(5) 0.0618(15) Uani 1 1 d D . . O4 O 0.7797(6) 0.6163(6) 0.3065(5) 0.085(2) Uani 1 1 d . . . O5 O 0.8176(6) 0.7732(6) 0.1768(6) 0.097(2) Uani 1 1 d . . . O6 O 0.6774(6) 0.8260(6) 0.3584(5) 0.089(2) Uani 1 1 d . . . O7 O 0.2653(8) 0.2526(8) 0.0459(7) 0.130(3) Uani 1 1 d D . . O8 O 0.6590(8) 0.3921(6) 0.2273(6) 0.112(3) Uani 1 1 d . . . C1 C 0.4446(14) 0.6031(14) 0.3221(16) 0.144(6) Uani 1 1 d . . . H1A H 0.5109 0.6606 0.3856 0.173 Uiso 1 1 calc R . . C11 C 0.412(2) 0.5219(19) 0.3602(17) 0.233(12) Uani 1 1 d . . . H11A H 0.3745 0.5506 0.4220 0.349 Uiso 1 1 calc R . . H11B H 0.4866 0.4974 0.3847 0.349 Uiso 1 1 calc R . . H11C H 0.3504 0.4584 0.3016 0.349 Uiso 1 1 calc R . . C12 C 0.352(3) 0.651(2) 0.317(2) 0.314(16) Uiso 1 1 d . . . H12A H 0.3202 0.6596 0.3833 0.472 Uiso 1 1 calc R . . H12B H 0.2846 0.6041 0.2520 0.472 Uiso 1 1 calc R . . H12C H 0.3807 0.7245 0.3137 0.472 Uiso 1 1 calc R . . C2 C 0.4952(17) 0.8344(18) 0.1323(14) 0.167(7) Uani 1 1 d . . . H2A H 0.5148 0.8728 0.2139 0.200 Uiso 1 1 calc R . . C21 C 0.536(2) 0.9115(17) 0.089(3) 0.290(17) Uani 1 1 d . . . H21A H 0.6279 0.9322 0.1080 0.435 Uiso 1 1 calc R . . H21B H 0.5042 0.9783 0.1183 0.435 Uiso 1 1 calc R . . H21C H 0.5042 0.8792 0.0086 0.435 Uiso 1 1 calc R . . C22 C 0.347(3) 0.784(2) 0.088(2) 0.313(14) Uiso 1 1 d . . . H22A H 0.3044 0.8454 0.1018 0.469 Uiso 1 1 calc R . . H22B H 0.3197 0.7348 0.1257 0.469 Uiso 1 1 calc R . . H22C H 0.3271 0.7411 0.0087 0.469 Uiso 1 1 calc R . . C4 C 0.8805(10) 0.6657(11) 0.4075(9) 0.100(4) Uani 1 1 d . . . H4A H 0.9086 0.7482 0.4250 0.120 Uiso 1 1 calc R . . C41 C 0.8346(15) 0.6472(14) 0.5001(10) 0.155(6) Uani 1 1 d . . . H41A H 0.7659 0.6845 0.5124 0.232 Uiso 1 1 calc R . . H41B H 0.9036 0.6783 0.5667 0.232 Uiso 1 1 calc R . . H41C H 0.8039 0.5666 0.4821 0.232 Uiso 1 1 calc R . . C42 C 0.9924(12) 0.6121(16) 0.3919(13) 0.176(8) Uani 1 1 d . . . H42A H 1.0243 0.6261 0.3323 0.264 Uiso 1 1 calc R . . H42B H 0.9649 0.5311 0.3735 0.264 Uiso 1 1 calc R . . H42C H 1.0592 0.6449 0.4601 0.264 Uiso 1 1 calc R . . C5 C 0.9332(12) 0.8510(14) 0.2461(12) 0.124(5) Uani 1 1 d . . . H5A H 0.9428 0.8597 0.3249 0.149 Uiso 1 1 calc R . . C51 C 0.9387(18) 0.9646(15) 0.2301(16) 0.201(9) Uani 1 1 d . . . H51A H 0.8741 0.9986 0.2596 0.301 Uiso 1 1 calc R . . H51B H 0.9238 0.9519 0.1517 0.301 Uiso 1 1 calc R . . H51C H 1.0219 1.0149 0.2690 0.301 Uiso 1 1 calc R . . C52 C 1.0417(15) 0.8182(18) 0.2051(15) 0.204(9) Uani 1 1 d . . . H52A H 1.0491 0.7462 0.2111 0.306 Uiso 1 1 calc R . . H52B H 1.1188 0.8756 0.2490 0.306 Uiso 1 1 calc R . . H52C H 1.0290 0.8110 0.1281 0.306 Uiso 1 1 calc R . . C6 C 0.690(3) 0.9240(17) 0.4515(14) 0.224(12) Uani 1 1 d . . . C61 C 0.6610(17) 0.9039(16) 0.5429(14) 0.201(9) Uani 1 1 d . . . H61A H 0.6765 0.9754 0.6042 0.302 Uiso 1 1 calc R . . H61B H 0.7141 0.8576 0.5643 0.302 Uiso 1 1 calc R . . H61C H 0.5723 0.8646 0.5242 0.302 Uiso 1 1 calc R . . C62 C 0.742(3) 1.0237(14) 0.4552(15) 0.260(15) Uani 1 1 d . . . H62A H 0.7469 1.0799 0.5270 0.391 Uiso 1 1 calc R . . H62B H 0.6913 1.0408 0.3973 0.391 Uiso 1 1 calc R . . H62C H 0.8270 1.0250 0.4442 0.391 Uiso 1 1 calc R . . C7 C 0.206(2) 0.1801(15) 0.102(2) 0.316(18) Uani 1 1 d D . . H7A H 0.2865 0.1989 0.1591 0.379 Uiso 1 1 calc R . . C71 C 0.146(3) 0.232(2) 0.180(2) 0.322(15) Uiso 1 1 d D . . H71A H 0.0985 0.1754 0.2017 0.482 Uiso 1 1 calc R . . H71B H 0.0879 0.2691 0.1491 0.482 Uiso 1 1 calc R . . H71C H 0.2084 0.2873 0.2446 0.482 Uiso 1 1 calc R . . C72 C 0.211(3) 0.067(2) 0.057(3) 0.363(18) Uiso 1 1 d D . . H72A H 0.1556 0.0219 0.0848 0.545 Uiso 1 1 calc R . . H72B H 0.2975 0.0608 0.0788 0.545 Uiso 1 1 calc R . . H72C H 0.1832 0.0404 -0.0230 0.545 Uiso 1 1 calc R . . C8 C 0.698(2) 0.3191(16) 0.2894(16) 0.172(7) Uani 1 1 d . . . H8A H 0.7427 0.3690 0.3667 0.206 Uiso 1 1 calc R . . C81 C 0.784(2) 0.2599(18) 0.2421(19) 0.221(10) Uani 1 1 d . . . H81A H 0.8150 0.2188 0.2872 0.331 Uiso 1 1 calc R . . H81B H 0.8553 0.3133 0.2388 0.331 Uiso 1 1 calc R . . H81C H 0.7411 0.2069 0.1677 0.331 Uiso 1 1 calc R . . C82 C 0.583(3) 0.246(2) 0.292(2) 0.297(16) Uani 1 1 d . . . H82A H 0.6054 0.2026 0.3367 0.445 Uiso 1 1 calc R . . H82B H 0.5392 0.1954 0.2167 0.445 Uiso 1 1 calc R . . H82C H 0.5281 0.2927 0.3230 0.445 Uiso 1 1 calc R . . H3 H 0.713(5) 0.521(7) 0.051(7) 0.07(3) Uiso 1 1 d 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 Zr1 0.0506(5) 0.0576(6) 0.0538(6) 0.0198(4) 0.0040(4) 0.0086(4) Sr1 0.1022(8) 0.0580(6) 0.0560(6) 0.0318(5) 0.0013(5) -0.0037(5) O1 0.069(4) 0.076(4) 0.061(4) 0.033(3) 0.020(3) 0.010(3) O2 0.073(4) 0.072(4) 0.074(4) 0.037(3) 0.008(3) 0.030(3) O3 0.066(4) 0.059(4) 0.057(4) 0.021(3) 0.009(3) 0.013(3) O4 0.077(4) 0.101(5) 0.067(4) 0.030(4) -0.013(3) 0.032(4) O5 0.066(4) 0.108(6) 0.096(5) 0.034(5) 0.016(4) -0.017(4) O6 0.103(5) 0.075(5) 0.064(4) 0.010(4) 0.007(4) 0.004(4) O7 0.106(6) 0.141(8) 0.133(7) 0.056(6) 0.043(5) -0.020(5) O8 0.141(7) 0.104(6) 0.099(5) 0.056(5) -0.006(5) 0.058(5) C1 0.105(11) 0.142(14) 0.201(17) 0.051(12) 0.090(12) 0.039(10) C11 0.30(3) 0.29(3) 0.28(3) 0.24(2) 0.19(2) 0.14(2) C2 0.149(15) 0.187(18) 0.141(13) 0.036(13) -0.024(11) 0.096(14) C21 0.31(3) 0.18(2) 0.55(5) 0.25(3) 0.23(3) 0.17(2) C4 0.084(8) 0.118(9) 0.083(8) 0.043(7) -0.020(6) 0.011(7) C41 0.179(15) 0.179(16) 0.077(9) 0.040(10) -0.011(9) 0.025(12) C42 0.079(9) 0.31(2) 0.148(13) 0.099(15) 0.001(9) 0.072(12) C5 0.069(9) 0.162(14) 0.123(10) 0.050(10) 0.022(8) -0.013(9) C51 0.21(2) 0.141(16) 0.204(19) 0.076(15) -0.009(15) -0.037(14) C52 0.105(13) 0.30(3) 0.187(17) 0.073(18) 0.025(12) 0.036(14) C6 0.43(3) 0.116(15) 0.094(11) -0.008(11) 0.127(17) -0.004(17) C61 0.213(19) 0.20(2) 0.124(13) -0.023(13) 0.053(13) 0.035(15) C62 0.50(4) 0.077(12) 0.138(15) 0.024(12) 0.00(2) 0.019(18) C7 0.33(3) 0.099(14) 0.55(4) 0.06(2) 0.36(3) 0.007(15) C8 0.198(19) 0.160(16) 0.180(16) 0.098(14) 0.001(14) 0.075(15) C81 0.21(2) 0.24(2) 0.27(2) 0.13(2) 0.031(17) 0.144(18) C82 0.35(3) 0.23(3) 0.45(4) 0.27(3) 0.17(3) 0.08(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 O6 1.948(7) . ? Zr1 O5 2.059(6) . ? Zr1 O4 2.068(6) . ? Zr1 O1 2.106(6) . ? Zr1 O2 2.111(6) . ? Zr1 O3 2.199(6) . ? Zr1 Sr1 3.706(2) . ? Zr1 Sr1 3.719(2) 2_665 ? Sr1 O2 2.481(6) 2_665 ? Sr1 O1 2.492(6) . ? Sr1 O3 2.493(6) . ? Sr1 O7 2.530(7) . ? Sr1 O3 2.532(6) 2_665 ? Sr1 O8 2.548(7) . ? Sr1 Zr1 3.719(2) 2_665 ? Sr1 Sr1 3.909(2) 2_665 ? O1 C1 1.416(15) . ? O2 C2 1.371(16) . ? O2 Sr1 2.481(6) 2_665 ? O3 Sr1 2.532(6) 2_665 ? O3 H3 0.92(2) . ? O4 C4 1.432(11) . ? O5 C5 1.409(13) . ? O6 C6 1.395(17) . ? O7 C7 1.491(14) . ? O8 C8 1.484(16) . ? C1 C12 1.26(3) . ? C1 C11 1.309(19) . ? C1 H1A 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C2 C21 1.34(2) . ? C2 C22 1.56(3) . ? C2 H2A 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C4 C41 1.457(16) . ? C4 C42 1.506(17) . ? C4 H4A 0.9800 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C5 C52 1.449(19) . ? C5 C51 1.519(19) . ? C5 H5A 0.9800 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C6 C62 1.28(2) . ? C6 C61 1.37(2) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? C7 C71 1.355(16) . ? C7 C72 1.377(16) . ? C7 H7A 0.9800 . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? C8 C81 1.40(2) . ? C8 C82 1.44(3) . ? C8 H8A 0.9800 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? 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 O6 Zr1 O5 96.7(3) . . ? O6 Zr1 O4 95.9(3) . . ? O5 Zr1 O4 94.6(3) . . ? O6 Zr1 O1 96.9(3) . . ? O5 Zr1 O1 165.7(2) . . ? O4 Zr1 O1 88.6(3) . . ? O6 Zr1 O2 97.3(3) . . ? O5 Zr1 O2 86.2(3) . . ? O4 Zr1 O2 166.6(2) . . ? O1 Zr1 O2 87.5(2) . . ? O6 Zr1 O3 176.1(3) . . ? O5 Zr1 O3 86.2(3) . . ? O4 Zr1 O3 86.5(2) . . ? O1 Zr1 O3 80.0(2) . . ? O2 Zr1 O3 80.2(2) . . ? O6 Zr1 Sr1 136.6(2) . . ? O5 Zr1 Sr1 126.7(2) . . ? O4 Zr1 Sr1 81.16(19) . . ? O1 Zr1 Sr1 40.00(17) . . ? O2 Zr1 Sr1 87.66(17) . . ? O3 Zr1 Sr1 40.70(16) . . ? O6 Zr1 Sr1 136.5(2) . 2_665 ? O5 Zr1 Sr1 79.31(19) . 2_665 ? O4 Zr1 Sr1 127.58(18) . 2_665 ? O1 Zr1 Sr1 87.66(16) . 2_665 ? O2 Zr1 Sr1 39.42(17) . 2_665 ? O3 Zr1 Sr1 41.48(15) . 2_665 ? Sr1 Zr1 Sr1 63.54(3) . 2_665 ? O2 Sr1 O1 156.98(19) 2_665 . ? O2 Sr1 O3 94.5(2) 2_665 . ? O1 Sr1 O3 67.48(19) . . ? O2 Sr1 O7 77.5(2) 2_665 . ? O1 Sr1 O7 116.3(3) . . ? O3 Sr1 O7 164.4(2) . . ? O2 Sr1 O3 67.28(19) 2_665 2_665 ? O1 Sr1 O3 94.03(19) . 2_665 ? O3 Sr1 O3 77.9(2) . 2_665 ? O7 Sr1 O3 86.7(2) . 2_665 ? O2 Sr1 O8 112.6(2) 2_665 . ? O1 Sr1 O8 79.7(2) . . ? O3 Sr1 O8 80.6(2) . . ? O7 Sr1 O8 114.7(3) . . ? O3 Sr1 O8 158.3(2) 2_665 . ? O2 Sr1 Zr1 129.27(14) 2_665 . ? O1 Sr1 Zr1 32.89(13) . . ? O3 Sr1 Zr1 35.11(14) . . ? O7 Sr1 Zr1 148.6(2) . . ? O3 Sr1 Zr1 89.77(14) 2_665 . ? O8 Sr1 Zr1 73.63(18) . . ? O2 Sr1 Zr1 32.70(13) 2_665 2_665 ? O1 Sr1 Zr1 128.90(13) . 2_665 ? O3 Sr1 Zr1 90.09(13) . 2_665 ? O7 Sr1 Zr1 75.89(19) . 2_665 ? O3 Sr1 Zr1 35.11(14) 2_665 2_665 ? O8 Sr1 Zr1 143.55(19) . 2_665 ? Zr1 Sr1 Zr1 116.46(3) . 2_665 ? O2 Sr1 Sr1 78.44(14) 2_665 2_665 ? O1 Sr1 Sr1 78.54(14) . 2_665 ? O3 Sr1 Sr1 39.29(13) . 2_665 ? O7 Sr1 Sr1 125.2(2) . 2_665 ? O3 Sr1 Sr1 38.56(13) 2_665 2_665 ? O8 Sr1 Sr1 119.87(19) . 2_665 ? Zr1 Sr1 Sr1 58.39(4) . 2_665 ? Zr1 Sr1 Sr1 58.07(4) 2_665 2_665 ? C1 O1 Zr1 127.6(8) . . ? C1 O1 Sr1 122.4(7) . . ? Zr1 O1 Sr1 107.1(2) . . ? C2 O2 Zr1 126.9(8) . . ? C2 O2 Sr1 125.0(8) . 2_665 ? Zr1 O2 Sr1 107.9(2) . 2_665 ? Zr1 O3 Sr1 104.2(2) . . ? Zr1 O3 Sr1 103.4(2) . 2_665 ? Sr1 O3 Sr1 102.1(2) . 2_665 ? Zr1 O3 H3 121(5) . . ? Sr1 O3 H3 115(5) . . ? Sr1 O3 H3 109(5) 2_665 . ? C4 O4 Zr1 129.4(7) . . ? C5 O5 Zr1 127.9(7) . . ? C6 O6 Zr1 175.9(10) . . ? C7 O7 Sr1 138.4(12) . . ? C8 O8 Sr1 141.1(10) . . ? C12 C1 C11 106.4(18) . . ? C12 C1 O1 115(2) . . ? C11 C1 O1 123.2(15) . . ? C12 C1 H1A 103.0 . . ? C11 C1 H1A 103.0 . . ? O1 C1 H1A 103.0 . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 109.5 . . ? C1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C21 C2 O2 116.1(18) . . ? C21 C2 C22 111.2(19) . . ? O2 C2 C22 104.5(18) . . ? C21 C2 H2A 108.3 . . ? O2 C2 H2A 108.3 . . ? C22 C2 H2A 108.3 . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O4 C4 C41 110.1(10) . . ? O4 C4 C42 109.8(11) . . ? C41 C4 C42 109.4(12) . . ? O4 C4 H4A 109.2 . . ? C41 C4 H4A 109.2 . . ? C42 C4 H4A 109.2 . . ? C4 C41 H41A 109.5 . . ? C4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C4 C42 H42A 109.5 . . ? C4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O5 C5 C52 110.4(13) . . ? O5 C5 C51 108.8(13) . . ? C52 C5 C51 101.2(13) . . ? O5 C5 H5A 112.0 . . ? C52 C5 H5A 112.0 . . ? C51 C5 H5A 112.0 . . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C62 C6 C61 123.1(17) . . ? C62 C6 O6 121.2(17) . . ? C61 C6 O6 114.9(17) . . ? C6 C61 H61A 109.5 . . ? C6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C6 C62 H62A 109.5 . . ? C6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C71 C7 C72 130.5(18) . . ? C71 C7 O7 115.8(17) . . ? C72 C7 O7 113.3(18) . . ? C71 C7 H7A 92.0 . . ? C72 C7 H7A 92.0 . . ? O7 C7 H7A 92.0 . . ? C7 C71 H71A 109.5 . . ? C7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C7 C72 H72A 109.5 . . ? C7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C81 C8 C82 114(2) . . ? C81 C8 O8 110.5(17) . . ? C82 C8 O8 107.6(16) . . ? C81 C8 H8A 108.1 . . ? C82 C8 H8A 108.1 . . ? O8 C8 H8A 108.1 . . ? C8 C81 H81A 109.5 . . ? C8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C8 C82 H82A 109.5 . . ? C8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.655 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.092