# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Anjana Devi' _publ_contact_author_email ANJANA.DEVI@RUB.DE _publ_section_title ; Monomeric malonate precursors for the MOCVD of HfO2 and ZrO2 thin films ; loop_ _publ_author_name 'Anjana Devi' 'Roland Fischer' 'Andrian Milanov' 'Harish Parala' 'Ramasamy Pothiraja' 'Manuela Winter' # Attachment 'DaltonTrans1.cif' data_cvd112 _database_code_depnum_ccdc_archive 'CCDC 692629' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H112 O20 Zr2' _chemical_formula_weight 1335.94 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' Zr Zr -2.9673 0.5597 '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' H H 0.0000 0.0000 '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 13.8318(5) _cell_length_b 16.0899(5) _cell_length_c 16.8531(5) _cell_angle_alpha 84.441(3) _cell_angle_beta 89.034(3) _cell_angle_gamma 84.501(3) _cell_volume 3715.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 9657 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 36.73 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.870 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '1109 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 59810 _diffrn_reflns_av_R_equivalents 0.0675 _diffrn_reflns_av_sigmaI/netI 0.0507 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13039 _reflns_number_gt 9651 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0616P)^2^+7.4490P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13039 _refine_ls_number_parameters 737 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0778 _refine_ls_R_factor_gt 0.0492 _refine_ls_wR_factor_ref 0.1368 _refine_ls_wR_factor_gt 0.1204 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.77827(3) 0.22609(2) 0.49853(2) 0.02437(11) Uani 1 1 d . . . Zr2 Zr 0.77523(2) 0.73969(2) -0.01903(2) 0.02086(10) Uani 1 1 d . . . O11 O 0.80819(18) 0.19002(15) 0.62125(14) 0.0271(6) Uani 1 1 d . . . O12 O 0.83274(18) 0.18655(15) 0.75382(15) 0.0263(6) Uani 1 1 d . . . C12 C 0.8112(2) 0.2292(2) 0.6832(2) 0.0235(8) Uani 1 1 d . . . C13 C 0.7946(3) 0.3156(2) 0.6850(2) 0.0250(8) Uani 1 1 d . . . H13A H 0.8003 0.3388 0.7343 0.030 Uiso 1 1 calc R . . O14 O 0.75606(19) 0.45081(15) 0.62960(15) 0.0287(6) Uani 1 1 d . . . C14 C 0.7697(3) 0.3692(2) 0.6171(2) 0.0255(8) Uani 1 1 d . . . O15 O 0.7594(2) 0.34747(15) 0.54800(15) 0.0308(6) Uani 1 1 d . . . O16 O 0.62448(18) 0.22840(16) 0.53507(15) 0.0299(6) Uani 1 1 d . . . O17 O 0.46125(19) 0.25721(18) 0.53971(15) 0.0353(7) Uani 1 1 d . . . C17 C 0.5478(3) 0.2618(2) 0.5015(2) 0.0283(9) Uani 1 1 d . . . C18 C 0.5413(3) 0.3045(3) 0.4264(2) 0.0326(9) Uani 1 1 d . . . H18A H 0.4790 0.3261 0.4069 0.039 Uiso 1 1 calc R . . O19 O 0.60128(18) 0.36235(16) 0.30852(14) 0.0282(6) Uani 1 1 d . . . C19 C 0.6215(3) 0.3173(2) 0.3784(2) 0.0251(8) Uani 1 1 d . . . O21 O 0.81341(16) 0.69785(15) 0.10044(14) 0.0237(5) Uani 1 1 d . . . O22 O 0.81790(17) 0.63147(16) 0.22436(14) 0.0272(6) Uani 1 1 d . . . C22 C 0.7683(3) 0.6638(2) 0.1592(2) 0.0212(7) Uani 1 1 d . . . C23 C 0.6687(3) 0.6583(2) 0.1638(2) 0.0237(8) Uani 1 1 d . . . H23A H 0.6425 0.6287 0.2094 0.028 Uiso 1 1 calc R . . O210 O 0.63015(16) 0.73130(14) 0.03765(14) 0.0223(5) Uani 1 1 d . . . O24 O 0.51181(17) 0.68784(15) 0.12133(14) 0.0236(5) Uani 1 1 d . . . C24 C 0.6059(2) 0.6949(2) 0.1034(2) 0.0206(7) Uani 1 1 d . . . O25 O 0.74873(17) 0.86542(14) 0.02029(14) 0.0240(5) Uani 1 1 d . . . O26 O 0.6844(2) 0.99699(15) 0.03526(15) 0.0316(6) Uani 1 1 d . . . C26 C 0.6947(3) 0.9295(2) -0.0066(2) 0.0238(8) Uani 1 1 d . . . C27 C 0.6446(3) 0.9396(2) -0.0780(2) 0.0268(8) Uani 1 1 d . . . H27A H 0.6045 0.9902 -0.0915 0.032 Uiso 1 1 calc R . . O28 O 0.60508(19) 0.89767(15) -0.19903(14) 0.0280(6) Uani 1 1 d . . . C28 C 0.6519(3) 0.8775(2) -0.1300(2) 0.0230(8) Uani 1 1 d . . . O29 O 0.69919(17) 0.80582(14) -0.11768(14) 0.0230(5) Uani 1 1 d . . . O31 O 0.90626(18) 0.24862(16) 0.46168(15) 0.0301(6) Uani 1 1 d . A . C31 C 0.9990(3) 0.2616(3) 0.4323(3) 0.074(2) Uani 1 1 d D . . C32 C 1.0580(13) 0.2483(17) 0.5084(8) 0.0734(14) Uiso 0.364(6) 1 d PD A 1 H32A H 1.0231 0.2778 0.5501 0.110 Uiso 0.364(6) 1 calc PR A 1 H32B H 1.1212 0.2703 0.4984 0.110 Uiso 0.364(6) 1 calc PR A 1 H32C H 1.0678 0.1882 0.5258 0.110 Uiso 0.364(6) 1 calc PR A 1 C33 C 1.0357(12) 0.2415(11) 0.3526(6) 0.0734(14) Uiso 0.364(6) 1 d PD A 1 H33A H 1.0371 0.1809 0.3490 0.110 Uiso 0.364(6) 1 calc PR A 1 H33B H 1.1015 0.2588 0.3446 0.110 Uiso 0.364(6) 1 calc PR A 1 H33C H 0.9929 0.2715 0.3114 0.110 Uiso 0.364(6) 1 calc PR A 1 C34 C 0.9882(13) 0.3576(5) 0.4343(11) 0.0734(14) Uiso 0.364(6) 1 d PD A 1 H34A H 0.9451 0.3832 0.3913 0.110 Uiso 0.364(6) 1 calc PR A 1 H34B H 1.0521 0.3789 0.4270 0.110 Uiso 0.364(6) 1 calc PR A 1 H34C H 0.9606 0.3716 0.4857 0.110 Uiso 0.364(6) 1 calc PR A 1 C321 C 1.0769(7) 0.2516(10) 0.4942(6) 0.0734(14) Uiso 0.636(6) 1 d PD A 2 H32D H 1.0663 0.2037 0.5328 0.110 Uiso 0.636(6) 1 calc PR A 2 H32E H 1.0748 0.3027 0.5217 0.110 Uiso 0.636(6) 1 calc PR A 2 H32F H 1.1405 0.2419 0.4685 0.110 Uiso 0.636(6) 1 calc PR A 2 C331 C 1.0237(7) 0.1835(5) 0.3852(6) 0.0734(14) Uiso 0.636(6) 1 d PD A 2 H33D H 1.0182 0.1323 0.4209 0.110 Uiso 0.636(6) 1 calc PR A 2 H33E H 1.0902 0.1837 0.3643 0.110 Uiso 0.636(6) 1 calc PR A 2 H33F H 0.9783 0.1854 0.3409 0.110 Uiso 0.636(6) 1 calc PR A 2 C341 C 0.9974(7) 0.3299(5) 0.3650(5) 0.0734(14) Uiso 0.636(6) 1 d PD A 2 H34D H 0.9476 0.3216 0.3266 0.110 Uiso 0.636(6) 1 calc PR A 2 H34E H 1.0611 0.3283 0.3384 0.110 Uiso 0.636(6) 1 calc PR A 2 H34F H 0.9825 0.3845 0.3859 0.110 Uiso 0.636(6) 1 calc PR A 2 O41 O 0.77606(19) 0.11295(15) 0.47187(15) 0.0319(6) Uani 1 1 d . B . C41 C 0.7795(4) 0.0323(3) 0.4522(3) 0.0695(18) Uani 1 1 d D . . C42 C 0.7469(8) -0.0289(5) 0.5158(5) 0.0727(14) Uiso 0.621(5) 1 d PD B 1 H42A H 0.7800 -0.0229 0.5656 0.109 Uiso 0.621(5) 1 calc PR B 1 H42B H 0.7624 -0.0859 0.5004 0.109 Uiso 0.621(5) 1 calc PR B 1 H42C H 0.6765 -0.0184 0.5235 0.109 Uiso 0.621(5) 1 calc PR B 1 C43 C 0.8921(5) 0.0130(6) 0.4524(6) 0.0727(14) Uiso 0.621(5) 1 d PD B 1 H43A H 0.9212 0.0536 0.4144 0.109 Uiso 0.621(5) 1 calc PR B 1 H43B H 0.9092 -0.0438 0.4371 0.109 Uiso 0.621(5) 1 calc PR B 1 H43C H 0.9167 0.0170 0.5060 0.109 Uiso 0.621(5) 1 calc PR B 1 C44 C 0.7608(8) 0.0233(6) 0.3668(4) 0.0727(14) Uiso 0.621(5) 1 d PD B 1 H44A H 0.6953 0.0486 0.3528 0.109 Uiso 0.621(5) 1 calc PR B 1 H44B H 0.7662 -0.0364 0.3582 0.109 Uiso 0.621(5) 1 calc PR B 1 H44C H 0.8086 0.0517 0.3332 0.109 Uiso 0.621(5) 1 calc PR B 1 C421 C 0.8115(13) -0.0310(8) 0.5208(7) 0.0727(14) Uiso 0.379(5) 1 d PD B 2 H42D H 0.8793 -0.0254 0.5336 0.109 Uiso 0.379(5) 1 calc PR B 2 H42E H 0.8057 -0.0877 0.5060 0.109 Uiso 0.379(5) 1 calc PR B 2 H42F H 0.7704 -0.0211 0.5675 0.109 Uiso 0.379(5) 1 calc PR B 2 C431 C 0.8439(11) 0.0018(10) 0.3860(8) 0.0727(14) Uiso 0.379(5) 1 d PD B 2 H43D H 0.8287 0.0373 0.3364 0.109 Uiso 0.379(5) 1 calc PR B 2 H43E H 0.8328 -0.0563 0.3790 0.109 Uiso 0.379(5) 1 calc PR B 2 H43F H 0.9120 0.0044 0.3997 0.109 Uiso 0.379(5) 1 calc PR B 2 C441 C 0.6864(8) 0.0428(10) 0.4043(9) 0.0727(14) Uiso 0.379(5) 1 d PD B 2 H44D H 0.6305 0.0413 0.4408 0.109 Uiso 0.379(5) 1 calc PR B 2 H44E H 0.6864 -0.0029 0.3698 0.109 Uiso 0.379(5) 1 calc PR B 2 H44F H 0.6821 0.0967 0.3715 0.109 Uiso 0.379(5) 1 calc PR B 2 O51 O 0.76550(17) 0.63177(14) -0.05589(14) 0.0251(5) Uani 1 1 d . . . C51 C 0.7429(3) 0.5525(2) -0.0757(2) 0.0268(8) Uani 1 1 d . . . C52 C 0.6365(3) 0.5438(2) -0.0562(3) 0.0372(10) Uani 1 1 d . . . H52A H 0.5960 0.5869 -0.0890 0.056 Uiso 1 1 calc R . . H52B H 0.6243 0.5508 0.0003 0.056 Uiso 1 1 calc R . . H52C H 0.6205 0.4881 -0.0675 0.056 Uiso 1 1 calc R . . C53 C 0.8086(3) 0.4861(2) -0.0261(3) 0.0419(10) Uani 1 1 d . . . H53A H 0.8767 0.4928 -0.0401 0.063 Uiso 1 1 calc R . . H53B H 0.7933 0.4301 -0.0369 0.063 Uiso 1 1 calc R . . H53C H 0.7981 0.4929 0.0307 0.063 Uiso 1 1 calc R . . C54 C 0.7628(3) 0.5480(3) -0.1647(3) 0.0420(11) Uani 1 1 d . . . H54A H 0.8318 0.5535 -0.1759 0.063 Uiso 1 1 calc R . . H54B H 0.7234 0.5936 -0.1952 0.063 Uiso 1 1 calc R . . H54C H 0.7460 0.4940 -0.1800 0.063 Uiso 1 1 calc R . . O61 O 0.90619(17) 0.75906(15) -0.05137(14) 0.0255(5) Uani 1 1 d . . . C61 C 0.9998(3) 0.7514(2) -0.0864(2) 0.0295(8) Uani 1 1 d . . . C62 C 1.0742(3) 0.7590(3) -0.0229(3) 0.0494(12) Uani 1 1 d . . . H62A H 1.0638 0.8147 -0.0035 0.074 Uiso 1 1 calc R . . H62B H 1.1397 0.7514 -0.0458 0.074 Uiso 1 1 calc R . . H62C H 1.0673 0.7159 0.0215 0.074 Uiso 1 1 calc R . . C63 C 1.0141(3) 0.6658(3) -0.1185(4) 0.0612(15) Uani 1 1 d . . . H63A H 1.0109 0.6218 -0.0744 0.092 Uiso 1 1 calc R . . H63B H 1.0777 0.6593 -0.1449 0.092 Uiso 1 1 calc R . . H63C H 0.9630 0.6613 -0.1570 0.092 Uiso 1 1 calc R . . C64 C 1.0040(3) 0.8221(3) -0.1529(3) 0.0486(12) Uani 1 1 d . . . H64A H 0.9946 0.8762 -0.1303 0.073 Uiso 1 1 calc R . . H64B H 0.9527 0.8188 -0.1915 0.073 Uiso 1 1 calc R . . H64C H 1.0675 0.8167 -0.1796 0.073 Uiso 1 1 calc R . . O110 O 0.70903(17) 0.29130(15) 0.39534(14) 0.0256(5) Uani 1 1 d . . . C121 C 0.8479(3) 0.0938(2) 0.7652(2) 0.0313(9) Uani 1 1 d . . . C122 C 0.8663(3) 0.0782(3) 0.8544(2) 0.0402(10) Uani 1 1 d . . . H12A H 0.8082 0.0984 0.8835 0.060 Uiso 1 1 calc R . . H12B H 0.9212 0.1082 0.8680 0.060 Uiso 1 1 calc R . . H12C H 0.8814 0.0179 0.8690 0.060 Uiso 1 1 calc R . . C123 C 0.9367(3) 0.0630(3) 0.7183(3) 0.0438(11) Uani 1 1 d . . . H12D H 0.9236 0.0742 0.6611 0.066 Uiso 1 1 calc R . . H12E H 0.9516 0.0025 0.7317 0.066 Uiso 1 1 calc R . . H12F H 0.9922 0.0924 0.7317 0.066 Uiso 1 1 calc R . . C124 C 0.7563(3) 0.0565(3) 0.7435(3) 0.0437(11) Uani 1 1 d . . . H12G H 0.7455 0.0676 0.6860 0.065 Uiso 1 1 calc R . . H12H H 0.7008 0.0821 0.7723 0.065 Uiso 1 1 calc R . . H12I H 0.7635 -0.0042 0.7583 0.065 Uiso 1 1 calc R . . C141 C 0.7225(3) 0.5163(2) 0.5669(2) 0.0352(9) Uani 1 1 d . . . C142 C 0.7183(3) 0.5951(2) 0.6099(2) 0.0325(9) Uani 1 1 d . . . H14A H 0.6697 0.5919 0.6529 0.049 Uiso 1 1 calc R . . H14B H 0.7003 0.6442 0.5722 0.049 Uiso 1 1 calc R . . H14C H 0.7820 0.6000 0.6325 0.049 Uiso 1 1 calc R . . C143 C 0.6233(4) 0.5017(3) 0.5389(3) 0.0629(16) Uani 1 1 d . . . H14D H 0.5783 0.4994 0.5845 0.094 Uiso 1 1 calc R . . H14E H 0.6269 0.4486 0.5146 0.094 Uiso 1 1 calc R . . H14F H 0.6000 0.5477 0.4994 0.094 Uiso 1 1 calc R . . C144 C 0.7966(5) 0.5207(3) 0.4987(3) 0.082(2) Uani 1 1 d . . . H14G H 0.7984 0.4696 0.4712 0.123 Uiso 1 1 calc R . . H14H H 0.8610 0.5257 0.5201 0.123 Uiso 1 1 calc R . . H14I H 0.7779 0.5697 0.4610 0.123 Uiso 1 1 calc R . . C171 C 0.4537(3) 0.2261(3) 0.6239(3) 0.0408(10) Uani 1 1 d . . . C172 C 0.3446(3) 0.2392(3) 0.6386(3) 0.0449(11) Uani 1 1 d . . . H17A H 0.3234 0.2993 0.6320 0.067 Uiso 1 1 calc R . . H17B H 0.3296 0.2163 0.6929 0.067 Uiso 1 1 calc R . . H17C H 0.3108 0.2104 0.6003 0.067 Uiso 1 1 calc R . . C173 C 0.5074(3) 0.2781(4) 0.6739(3) 0.0629(16) Uani 1 1 d . . . H17D H 0.4814 0.3370 0.6644 0.094 Uiso 1 1 calc R . . H17E H 0.5765 0.2726 0.6597 0.094 Uiso 1 1 calc R . . H17F H 0.4993 0.2587 0.7304 0.094 Uiso 1 1 calc R . . C174 C 0.4888(5) 0.1335(4) 0.6358(5) 0.103(3) Uani 1 1 d . . . H17G H 0.5590 0.1261 0.6261 0.154 Uiso 1 1 calc R . . H17H H 0.4555 0.1032 0.5983 0.154 Uiso 1 1 calc R . . H17I H 0.4744 0.1115 0.6905 0.154 Uiso 1 1 calc R . . C191 C 0.6753(3) 0.3804(2) 0.2472(2) 0.0326(9) Uani 1 1 d . . . C192 C 0.6139(3) 0.4271(3) 0.1805(3) 0.0433(11) Uani 1 1 d . . . H19A H 0.5827 0.4794 0.1984 0.065 Uiso 1 1 calc R . . H19B H 0.5640 0.3922 0.1659 0.065 Uiso 1 1 calc R . . H19C H 0.6553 0.4401 0.1341 0.065 Uiso 1 1 calc R . . C193 C 0.7245(3) 0.2992(3) 0.2205(2) 0.0397(10) Uani 1 1 d . . . H19D H 0.6754 0.2661 0.2012 0.060 Uiso 1 1 calc R . . H19E H 0.7589 0.2670 0.2656 0.060 Uiso 1 1 calc R . . H19F H 0.7709 0.3120 0.1775 0.060 Uiso 1 1 calc R . . C194 C 0.7466(4) 0.4361(3) 0.2779(3) 0.0525(13) Uani 1 1 d . . . H19G H 0.7110 0.4875 0.2940 0.079 Uiso 1 1 calc R . . H19H H 0.7933 0.4506 0.2356 0.079 Uiso 1 1 calc R . . H19I H 0.7814 0.4061 0.3239 0.079 Uiso 1 1 calc R . . C221 C 0.9228(3) 0.6385(2) 0.2327(2) 0.0271(8) Uani 1 1 d . . . C222 C 0.9421(3) 0.5956(3) 0.3157(3) 0.0456(11) Uani 1 1 d . . . H22A H 0.9037 0.6265 0.3546 0.068 Uiso 1 1 calc R . . H22B H 1.0113 0.5944 0.3277 0.068 Uiso 1 1 calc R . . H22C H 0.9236 0.5381 0.3184 0.068 Uiso 1 1 calc R . . C223 C 0.9801(3) 0.5917(3) 0.1708(3) 0.0423(10) Uani 1 1 d . . . H22D H 0.9654 0.5330 0.1761 0.063 Uiso 1 1 calc R . . H22E H 1.0497 0.5942 0.1789 0.063 Uiso 1 1 calc R . . H22F H 0.9622 0.6176 0.1174 0.063 Uiso 1 1 calc R . . C224 C 0.9410(3) 0.7302(3) 0.2290(3) 0.0418(10) Uani 1 1 d . . . H22G H 0.9020 0.7573 0.2700 0.063 Uiso 1 1 calc R . . H22H H 0.9229 0.7581 0.1763 0.063 Uiso 1 1 calc R . . H22I H 1.0100 0.7347 0.2382 0.063 Uiso 1 1 calc R . . C241 C 0.4325(2) 0.7360(2) 0.0741(2) 0.0230(7) Uani 1 1 d . . . C242 C 0.3433(3) 0.7123(2) 0.1217(2) 0.0312(9) Uani 1 1 d . . . H24A H 0.3459 0.7314 0.1751 0.047 Uiso 1 1 calc R . . H24B H 0.3419 0.6513 0.1263 0.047 Uiso 1 1 calc R . . H24C H 0.2847 0.7391 0.0946 0.047 Uiso 1 1 calc R . . C243 C 0.4419(3) 0.8289(2) 0.0728(2) 0.0294(8) Uani 1 1 d . . . H24D H 0.4429 0.8444 0.1276 0.044 Uiso 1 1 calc R . . H24E H 0.3865 0.8604 0.0446 0.044 Uiso 1 1 calc R . . H24F H 0.5023 0.8423 0.0454 0.044 Uiso 1 1 calc R . . C244 C 0.4301(3) 0.7071(2) -0.0090(2) 0.0281(8) Uani 1 1 d . . . H24G H 0.4879 0.7228 -0.0390 0.042 Uiso 1 1 calc R . . H24H H 0.3717 0.7338 -0.0367 0.042 Uiso 1 1 calc R . . H24I H 0.4290 0.6460 -0.0050 0.042 Uiso 1 1 calc R . . C261 C 0.7258(3) 0.9957(2) 0.1154(2) 0.0330(9) Uani 1 1 d . . . C262 C 0.6918(4) 1.0838(3) 0.1366(3) 0.0543(14) Uani 1 1 d . . . H26A H 0.7217 1.1251 0.0998 0.081 Uiso 1 1 calc R . . H26B H 0.7110 1.0899 0.1913 0.081 Uiso 1 1 calc R . . H26C H 0.6210 1.0932 0.1323 0.081 Uiso 1 1 calc R . . C263 C 0.6811(4) 0.9306(3) 0.1720(3) 0.0523(13) Uani 1 1 d . . . H26D H 0.7036 0.8744 0.1575 0.078 Uiso 1 1 calc R . . H26E H 0.6102 0.9392 0.1682 0.078 Uiso 1 1 calc R . . H26F H 0.7007 0.9361 0.2267 0.078 Uiso 1 1 calc R . . C264 C 0.8352(4) 0.9836(3) 0.1126(3) 0.0516(12) Uani 1 1 d . . . H26G H 0.8562 0.9267 0.0991 0.077 Uiso 1 1 calc R . . H26H H 0.8612 0.9916 0.1648 0.077 Uiso 1 1 calc R . . H26I H 0.8595 1.0245 0.0721 0.077 Uiso 1 1 calc R . . C281 C 0.6012(3) 0.8379(2) -0.2598(2) 0.0298(8) Uani 1 1 d . . . C282 C 0.5369(4) 0.8886(3) -0.3228(3) 0.0525(13) Uani 1 1 d . . . H28A H 0.4724 0.9025 -0.3000 0.079 Uiso 1 1 calc R . . H28B H 0.5309 0.8557 -0.3681 0.079 Uiso 1 1 calc R . . H28C H 0.5659 0.9405 -0.3409 0.079 Uiso 1 1 calc R . . C283 C 0.5531(3) 0.7615(2) -0.2250(2) 0.0343(9) Uani 1 1 d . . . H28D H 0.4883 0.7792 -0.2048 0.052 Uiso 1 1 calc R . . H28E H 0.5926 0.7322 -0.1813 0.052 Uiso 1 1 calc R . . H28F H 0.5474 0.7237 -0.2666 0.052 Uiso 1 1 calc R . . C284 C 0.7019(3) 0.8147(3) -0.2930(2) 0.0402(10) Uani 1 1 d . . . H28G H 0.7419 0.7821 -0.2513 0.060 Uiso 1 1 calc R . . H28H H 0.7321 0.8660 -0.3111 0.060 Uiso 1 1 calc R . . H28I H 0.6968 0.7812 -0.3380 0.060 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 0.0263(2) 0.02216(19) 0.0245(2) -0.00534(15) 0.00438(14) 0.00078(14) Zr2 0.02026(19) 0.02004(18) 0.02176(19) -0.00347(14) 0.00184(13) 0.00181(13) O11 0.0327(15) 0.0228(13) 0.0258(14) -0.0043(11) 0.0026(11) -0.0003(11) O12 0.0264(14) 0.0238(13) 0.0279(14) -0.0032(11) -0.0012(11) 0.0026(10) C12 0.0141(17) 0.0299(19) 0.027(2) -0.0045(16) 0.0023(14) -0.0018(14) C13 0.0237(19) 0.0264(19) 0.0253(19) -0.0067(15) 0.0011(15) 0.0000(15) O14 0.0332(15) 0.0215(13) 0.0313(14) -0.0054(11) 0.0013(11) 0.0004(11) C14 0.0207(19) 0.0231(18) 0.033(2) -0.0053(16) 0.0038(15) -0.0001(14) O15 0.0480(17) 0.0186(13) 0.0256(14) -0.0034(11) 0.0027(12) -0.0010(11) O16 0.0253(14) 0.0308(14) 0.0324(15) 0.0030(12) 0.0072(11) -0.0032(11) O17 0.0241(14) 0.0556(18) 0.0283(15) -0.0104(13) 0.0077(11) -0.0092(12) C17 0.026(2) 0.034(2) 0.028(2) -0.0161(17) 0.0074(16) -0.0079(16) C18 0.026(2) 0.051(3) 0.021(2) -0.0107(18) 0.0006(15) -0.0026(18) O19 0.0241(14) 0.0376(15) 0.0226(14) -0.0051(11) -0.0002(10) 0.0019(11) C19 0.026(2) 0.0268(19) 0.0241(19) -0.0079(16) 0.0009(15) -0.0027(15) O21 0.0176(12) 0.0270(13) 0.0254(13) 0.0001(11) 0.0009(10) 0.0010(10) O22 0.0237(13) 0.0314(14) 0.0255(14) 0.0040(11) -0.0044(11) -0.0039(11) C22 0.0281(19) 0.0151(16) 0.0202(18) -0.0023(14) -0.0024(15) -0.0001(14) C23 0.0236(19) 0.0227(18) 0.0237(19) 0.0015(15) 0.0008(14) -0.0004(14) O210 0.0191(12) 0.0256(13) 0.0214(13) -0.0001(10) 0.0010(10) 0.0005(10) O24 0.0185(13) 0.0276(13) 0.0237(13) -0.0001(10) 0.0004(10) 0.0008(10) C24 0.0189(18) 0.0174(17) 0.0258(19) -0.0069(15) 0.0016(14) 0.0017(13) O25 0.0290(14) 0.0198(12) 0.0224(13) -0.0023(10) -0.0040(10) 0.0030(10) O26 0.0501(17) 0.0200(13) 0.0238(14) -0.0062(11) -0.0066(12) 0.0064(11) C26 0.0275(19) 0.0196(18) 0.0248(19) -0.0042(15) 0.0065(15) -0.0042(15) C27 0.035(2) 0.0196(18) 0.0242(19) -0.0018(15) -0.0029(16) 0.0038(15) O28 0.0380(15) 0.0221(13) 0.0230(14) -0.0016(10) -0.0070(11) 0.0029(11) C28 0.0240(19) 0.0237(19) 0.0209(18) -0.0005(15) 0.0017(14) -0.0022(14) O29 0.0260(13) 0.0206(12) 0.0221(13) -0.0039(10) 0.0009(10) 0.0016(10) O31 0.0251(14) 0.0370(15) 0.0276(14) -0.0016(12) -0.0009(11) -0.0013(11) C31 0.023(2) 0.096(4) 0.094(4) 0.054(4) -0.017(3) -0.016(3) O41 0.0404(16) 0.0232(13) 0.0318(15) -0.0050(11) -0.0036(12) 0.0012(11) C41 0.124(5) 0.025(2) 0.059(3) -0.010(2) -0.044(3) 0.008(3) O51 0.0260(14) 0.0212(13) 0.0273(14) -0.0017(10) 0.0017(10) 0.0008(10) C51 0.031(2) 0.0165(17) 0.033(2) -0.0075(15) 0.0003(16) 0.0027(15) C52 0.037(2) 0.022(2) 0.054(3) -0.0075(19) 0.001(2) -0.0013(17) C53 0.041(3) 0.027(2) 0.055(3) 0.001(2) -0.005(2) 0.0070(18) C54 0.052(3) 0.036(2) 0.040(2) -0.017(2) 0.000(2) 0.003(2) O61 0.0215(13) 0.0275(13) 0.0270(13) -0.0012(11) 0.0035(10) -0.0011(10) C61 0.0217(19) 0.034(2) 0.033(2) -0.0042(17) 0.0057(16) -0.0038(16) C62 0.029(2) 0.069(3) 0.050(3) -0.001(2) -0.005(2) -0.007(2) C63 0.034(3) 0.054(3) 0.100(4) -0.036(3) 0.026(3) -0.005(2) C64 0.042(3) 0.059(3) 0.044(3) 0.009(2) 0.005(2) -0.013(2) O110 0.0236(14) 0.0263(13) 0.0265(14) -0.0033(11) 0.0042(10) -0.0002(10) C121 0.039(2) 0.0205(19) 0.033(2) -0.0024(16) 0.0020(17) -0.0007(16) C122 0.053(3) 0.030(2) 0.035(2) -0.0016(18) -0.002(2) 0.0051(19) C123 0.051(3) 0.027(2) 0.049(3) -0.0008(19) 0.004(2) 0.0149(19) C124 0.053(3) 0.042(3) 0.038(2) -0.001(2) 0.002(2) -0.017(2) C141 0.055(3) 0.0202(19) 0.030(2) -0.0025(16) 0.0010(19) -0.0011(17) C142 0.038(2) 0.0221(19) 0.038(2) -0.0069(17) -0.0007(18) 0.0003(16) C143 0.093(4) 0.025(2) 0.072(4) -0.009(2) -0.049(3) 0.002(2) C144 0.159(6) 0.028(3) 0.059(3) -0.006(2) 0.060(4) -0.012(3) C171 0.036(2) 0.044(3) 0.039(2) 0.005(2) 0.0140(19) 0.0011(19) C172 0.034(2) 0.061(3) 0.039(3) -0.001(2) 0.0126(19) -0.009(2) C173 0.037(3) 0.129(5) 0.025(2) -0.012(3) 0.0075(19) -0.016(3) C174 0.075(4) 0.061(4) 0.155(7) 0.044(4) 0.070(5) 0.015(3) C191 0.033(2) 0.033(2) 0.032(2) 0.0025(17) -0.0009(17) -0.0121(17) C192 0.046(3) 0.051(3) 0.033(2) 0.007(2) -0.0083(19) -0.017(2) C193 0.034(2) 0.054(3) 0.031(2) -0.006(2) 0.0131(18) -0.006(2) C194 0.056(3) 0.051(3) 0.052(3) 0.015(2) -0.021(2) -0.024(2) C221 0.0198(19) 0.030(2) 0.030(2) 0.0002(16) -0.0038(15) 0.0005(15) C222 0.030(2) 0.064(3) 0.040(3) 0.015(2) -0.0123(19) -0.008(2) C223 0.032(2) 0.049(3) 0.043(3) -0.002(2) -0.0040(19) 0.0104(19) C224 0.034(2) 0.037(2) 0.056(3) -0.003(2) -0.013(2) -0.0079(18) C241 0.0181(18) 0.0227(18) 0.0270(19) -0.0011(15) -0.0046(14) 0.0037(14) C242 0.0210(19) 0.036(2) 0.036(2) -0.0048(18) 0.0018(16) 0.0016(16) C243 0.025(2) 0.0260(19) 0.037(2) -0.0073(17) -0.0021(16) 0.0038(15) C244 0.024(2) 0.032(2) 0.028(2) -0.0067(16) -0.0031(15) 0.0027(15) C261 0.052(3) 0.024(2) 0.023(2) -0.0044(16) -0.0075(18) 0.0004(17) C262 0.096(4) 0.032(2) 0.035(3) -0.017(2) -0.017(2) 0.011(2) C263 0.087(4) 0.045(3) 0.026(2) -0.005(2) 0.005(2) -0.012(3) C264 0.055(3) 0.045(3) 0.057(3) -0.013(2) -0.018(2) -0.007(2) C281 0.042(2) 0.0245(19) 0.0234(19) -0.0049(16) -0.0050(16) -0.0021(16) C282 0.087(4) 0.036(2) 0.033(2) -0.004(2) -0.026(2) 0.007(2) C283 0.038(2) 0.034(2) 0.032(2) -0.0039(18) -0.0035(17) -0.0095(18) C284 0.053(3) 0.045(3) 0.026(2) -0.0143(19) 0.0132(19) -0.014(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 O41 1.920(2) . ? Zr1 O31 1.922(3) . ? Zr1 O11 2.130(2) . ? Zr1 O110 2.134(2) . ? Zr1 O15 2.188(2) . ? Zr1 O16 2.202(2) . ? Zr2 O51 1.917(2) . ? Zr2 O61 1.928(2) . ? Zr2 O21 2.119(2) . ? Zr2 O29 2.122(2) . ? Zr2 O25 2.185(2) . ? Zr2 O210 2.218(2) . ? O11 C12 1.274(4) . ? O12 C12 1.338(4) . ? O12 C121 1.482(4) . ? C12 C13 1.391(5) . ? C13 C14 1.392(5) . ? C13 H13A 0.9500 . ? O14 C14 1.345(4) . ? O14 C141 1.466(5) . ? C14 O15 1.262(4) . ? O16 C17 1.259(5) . ? O17 C17 1.354(4) . ? O17 C171 1.464(5) . ? C17 C18 1.381(5) . ? C18 C19 1.381(5) . ? C18 H18A 0.9500 . ? O19 C19 1.341(4) . ? O19 C191 1.471(5) . ? C19 O110 1.270(4) . ? O21 C22 1.269(4) . ? O22 C22 1.339(4) . ? O22 C221 1.476(4) . ? C22 C23 1.388(5) . ? C23 C24 1.398(5) . ? C23 H23A 0.9500 . ? O210 C24 1.258(4) . ? O24 C24 1.344(4) . ? O24 C241 1.478(4) . ? O25 C26 1.264(4) . ? O26 C26 1.346(4) . ? O26 C261 1.474(4) . ? C26 C27 1.386(5) . ? C27 C28 1.388(5) . ? C27 H27A 0.9500 . ? O28 C28 1.337(4) . ? O28 C281 1.476(4) . ? C28 O29 1.271(4) . ? O31 C31 1.395(5) . ? C31 C33 1.483(5) . ? C31 C321 1.499(5) . ? C31 C341 1.500(5) . ? C31 C32 1.518(5) . ? C31 C34 1.541(5) . ? C31 C331 1.557(5) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C321 H32D 0.9800 . ? C321 H32E 0.9800 . ? C321 H32F 0.9800 . ? C331 H33D 0.9800 . ? C331 H33E 0.9800 . ? C331 H33F 0.9800 . ? C341 H34D 0.9800 . ? C341 H34E 0.9800 . ? C341 H34F 0.9800 . ? O41 C41 1.366(5) . ? C41 C42 1.479(5) . ? C41 C44 1.489(5) . ? C41 C431 1.505(5) . ? C41 C421 1.509(5) . ? C41 C441 1.518(5) . ? C41 C43 1.559(5) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C421 H42D 0.9800 . ? C421 H42E 0.9800 . ? C421 H42F 0.9800 . ? C431 H43D 0.9800 . ? C431 H43E 0.9800 . ? C431 H43F 0.9800 . ? C441 H44D 0.9800 . ? C441 H44E 0.9800 . ? C441 H44F 0.9800 . ? O51 C51 1.413(4) . ? C51 C52 1.519(5) . ? C51 C54 1.527(5) . ? C51 C53 1.528(5) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? O61 C61 1.413(4) . ? C61 C62 1.519(6) . ? C61 C64 1.521(6) . ? C61 C63 1.523(6) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C121 C124 1.517(6) . ? C121 C123 1.519(6) . ? C121 C122 1.520(6) . ? C122 H12A 0.9800 . ? C122 H12B 0.9800 . ? C122 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C123 H12F 0.9800 . ? C124 H12G 0.9800 . ? C124 H12H 0.9800 . ? C124 H12I 0.9800 . ? C141 C143 1.505(7) . ? C141 C142 1.516(5) . ? C141 C144 1.528(6) . ? C142 H14A 0.9800 . ? C142 H14B 0.9800 . ? C142 H14C 0.9800 . ? C143 H14D 0.9800 . ? C143 H14E 0.9800 . ? C143 H14F 0.9800 . ? C144 H14G 0.9800 . ? C144 H14H 0.9800 . ? C144 H14I 0.9800 . ? C171 C173 1.496(7) . ? C171 C174 1.516(7) . ? C171 C172 1.523(6) . ? C172 H17A 0.9800 . ? C172 H17B 0.9800 . ? C172 H17C 0.9800 . ? C173 H17D 0.9800 . ? C173 H17E 0.9800 . ? C173 H17F 0.9800 . ? C174 H17G 0.9800 . ? C174 H17H 0.9800 . ? C174 H17I 0.9800 . ? C191 C192 1.515(6) . ? C191 C193 1.518(6) . ? C191 C194 1.524(6) . ? C192 H19A 0.9800 . ? C192 H19B 0.9800 . ? C192 H19C 0.9800 . ? C193 H19D 0.9800 . ? C193 H19E 0.9800 . ? C193 H19F 0.9800 . ? C194 H19G 0.9800 . ? C194 H19H 0.9800 . ? C194 H19I 0.9800 . ? C221 C223 1.514(5) . ? C221 C222 1.515(5) . ? C221 C224 1.516(5) . ? C222 H22A 0.9800 . ? C222 H22B 0.9800 . ? C222 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C223 H22F 0.9800 . ? C224 H22G 0.9800 . ? C224 H22H 0.9800 . ? C224 H22I 0.9800 . ? C241 C243 1.511(5) . ? C241 C242 1.519(5) . ? C241 C244 1.521(5) . ? C242 H24A 0.9800 . ? C242 H24B 0.9800 . ? C242 H24C 0.9800 . ? C243 H24D 0.9800 . ? C243 H24E 0.9800 . ? C243 H24F 0.9800 . ? C244 H24G 0.9800 . ? C244 H24H 0.9800 . ? C244 H24I 0.9800 . ? C261 C264 1.508(6) . ? C261 C263 1.516(6) . ? C261 C262 1.524(5) . ? C262 H26A 0.9800 . ? C262 H26B 0.9800 . ? C262 H26C 0.9800 . ? C263 H26D 0.9800 . ? C263 H26E 0.9800 . ? C263 H26F 0.9800 . ? C264 H26G 0.9800 . ? C264 H26H 0.9800 . ? C264 H26I 0.9800 . ? C281 C283 1.516(5) . ? C281 C284 1.519(6) . ? C281 C282 1.520(6) . ? C282 H28A 0.9800 . ? C282 H28B 0.9800 . ? C282 H28C 0.9800 . ? C283 H28D 0.9800 . ? C283 H28E 0.9800 . ? C283 H28F 0.9800 . ? C284 H28G 0.9800 . ? C284 H28H 0.9800 . ? C284 H28I 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O41 Zr1 O31 100.37(11) . . ? O41 Zr1 O11 94.20(10) . . ? O31 Zr1 O11 99.58(10) . . ? O41 Zr1 O110 99.36(10) . . ? O31 Zr1 O110 93.59(10) . . ? O11 Zr1 O110 159.08(9) . . ? O41 Zr1 O15 168.23(11) . . ? O31 Zr1 O15 90.12(11) . . ? O11 Zr1 O15 78.66(9) . . ? O110 Zr1 O15 85.17(9) . . ? O41 Zr1 O16 90.04(11) . . ? O31 Zr1 O16 168.14(10) . . ? O11 Zr1 O16 85.17(10) . . ? O110 Zr1 O16 79.00(9) . . ? O15 Zr1 O16 80.11(10) . . ? O51 Zr2 O61 100.86(10) . . ? O51 Zr2 O21 97.65(10) . . ? O61 Zr2 O21 94.20(10) . . ? O51 Zr2 O29 93.96(10) . . ? O61 Zr2 O29 99.30(10) . . ? O21 Zr2 O29 160.21(9) . . ? O51 Zr2 O25 166.33(10) . . ? O61 Zr2 O25 91.60(10) . . ? O21 Zr2 O25 86.91(9) . . ? O29 Zr2 O25 78.35(9) . . ? O51 Zr2 O210 88.48(9) . . ? O61 Zr2 O210 168.96(9) . . ? O21 Zr2 O210 78.60(9) . . ? O29 Zr2 O210 85.77(9) . . ? O25 Zr2 O210 79.76(9) . . ? C12 O11 Zr1 134.8(2) . . ? C12 O12 C121 123.0(3) . . ? O11 C12 O12 119.8(3) . . ? O11 C12 C13 125.5(3) . . ? O12 C12 C13 114.7(3) . . ? C12 C13 C14 122.2(3) . . ? C12 C13 H13A 118.9 . . ? C14 C13 H13A 118.9 . . ? C14 O14 C141 122.5(3) . . ? O15 C14 O14 119.7(3) . . ? O15 C14 C13 125.9(3) . . ? O14 C14 C13 114.3(3) . . ? C14 O15 Zr1 132.9(2) . . ? C17 O16 Zr1 132.0(2) . . ? C17 O17 C171 122.4(3) . . ? O16 C17 O17 119.9(3) . . ? O16 C17 C18 126.1(3) . . ? O17 C17 C18 114.0(3) . . ? C17 C18 C19 122.9(4) . . ? C17 C18 H18A 118.5 . . ? C19 C18 H18A 118.5 . . ? C19 O19 C191 123.3(3) . . ? O110 C19 O19 119.6(3) . . ? O110 C19 C18 126.0(4) . . ? O19 C19 C18 114.4(3) . . ? C22 O21 Zr2 133.8(2) . . ? C22 O22 C221 122.4(3) . . ? O21 C22 O22 119.3(3) . . ? O21 C22 C23 125.6(3) . . ? O22 C22 C23 115.1(3) . . ? C22 C23 C24 122.1(3) . . ? C22 C23 H23A 119.0 . . ? C24 C23 H23A 119.0 . . ? C24 O210 Zr2 130.6(2) . . ? C24 O24 C241 122.2(3) . . ? O210 C24 O24 120.6(3) . . ? O210 C24 C23 126.3(3) . . ? O24 C24 C23 113.2(3) . . ? C26 O25 Zr2 132.0(2) . . ? C26 O26 C261 122.1(3) . . ? O25 C26 O26 119.2(3) . . ? O25 C26 C27 126.5(3) . . ? O26 C26 C27 114.3(3) . . ? C26 C27 C28 121.4(3) . . ? C26 C27 H27A 119.3 . . ? C28 C27 H27A 119.3 . . ? C28 O28 C281 122.5(3) . . ? O29 C28 O28 119.1(3) . . ? O29 C28 C27 125.7(3) . . ? O28 C28 C27 115.2(3) . . ? C28 O29 Zr2 134.6(2) . . ? C31 O31 Zr1 177.0(3) . . ? O31 C31 C33 124.6(8) . . ? O31 C31 C321 114.8(6) . . ? C33 C31 C321 113.1(9) . . ? O31 C31 C341 112.4(5) . . ? C33 C31 C341 60.5(8) . . ? C321 C31 C341 121.1(7) . . ? O31 C31 C32 101.3(8) . . ? C33 C31 C32 125.2(12) . . ? C321 C31 C32 13.5(11) . . ? C341 C31 C32 130.5(11) . . ? O31 C31 C34 96.1(7) . . ? C33 C31 C34 108.8(10) . . ? C321 C31 C34 91.5(9) . . ? C341 C31 C34 50.1(7) . . ? C32 C31 C34 92.4(13) . . ? O31 C31 C331 101.9(5) . . ? C33 C31 C331 40.8(7) . . ? C321 C31 C331 102.8(8) . . ? C341 C31 C331 99.9(6) . . ? C32 C31 C331 107.7(11) . . ? C34 C31 C331 149.6(8) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? C31 C321 H32D 109.5 . . ? C31 C321 H32E 109.5 . . ? H32D C321 H32E 109.5 . . ? C31 C321 H32F 109.5 . . ? H32D C321 H32F 109.5 . . ? H32E C321 H32F 109.5 . . ? C31 C331 H33D 109.5 . . ? C31 C331 H33E 109.5 . . ? H33D C331 H33E 109.5 . . ? C31 C331 H33F 109.5 . . ? H33D C331 H33F 109.5 . . ? H33E C331 H33F 109.5 . . ? C31 C341 H34D 109.5 . . ? C31 C341 H34E 109.5 . . ? H34D C341 H34E 109.5 . . ? C31 C341 H34F 109.5 . . ? H34D C341 H34F 109.5 . . ? H34E C341 H34F 109.5 . . ? C41 O41 Zr1 177.1(3) . . ? O41 C41 C42 114.9(5) . . ? O41 C41 C44 115.4(5) . . ? C42 C41 C44 120.6(7) . . ? O41 C41 C431 121.9(8) . . ? C42 C41 C431 119.5(8) . . ? C44 C41 C431 47.6(7) . . ? O41 C41 C421 112.4(7) . . ? C42 C41 C421 34.9(7) . . ? C44 C41 C421 131.9(8) . . ? C431 C41 C421 101.1(10) . . ? O41 C41 C441 97.0(7) . . ? C42 C41 C441 96.6(8) . . ? C44 C41 C441 48.3(7) . . ? C431 C41 C441 95.6(9) . . ? C421 C41 C441 130.1(10) . . ? O41 C41 C43 97.6(5) . . ? C42 C41 C43 103.3(6) . . ? C44 C41 C43 99.2(6) . . ? C431 C41 C43 52.2(7) . . ? C421 C41 C43 69.0(8) . . ? C441 C41 C43 147.5(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? C41 C421 H42D 109.5 . . ? C41 C421 H42E 109.5 . . ? H42D C421 H42E 109.5 . . ? C41 C421 H42F 109.5 . . ? H42D C421 H42F 109.5 . . ? H42E C421 H42F 109.5 . . ? C41 C431 H43D 109.5 . . ? C41 C431 H43E 109.5 . . ? H43D C431 H43E 109.5 . . ? C41 C431 H43F 109.5 . . ? H43D C431 H43F 109.5 . . ? H43E C431 H43F 109.5 . . ? C41 C441 H44D 109.5 . . ? C41 C441 H44E 109.5 . . ? H44D C441 H44E 109.5 . . ? C41 C441 H44F 109.5 . . ? H44D C441 H44F 109.5 . . ? H44E C441 H44F 109.5 . . ? C51 O51 Zr2 170.0(2) . . ? O51 C51 C52 108.6(3) . . ? O51 C51 C54 108.1(3) . . ? C52 C51 C54 110.8(3) . . ? O51 C51 C53 107.2(3) . . ? C52 C51 C53 111.1(3) . . ? C54 C51 C53 110.8(3) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C51 C53 H53A 109.5 . . ? C51 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C51 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C51 C54 H54A 109.5 . . ? C51 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C51 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C61 O61 Zr2 162.9(2) . . ? O61 C61 C62 108.6(3) . . ? O61 C61 C64 107.9(3) . . ? C62 C61 C64 110.3(4) . . ? O61 C61 C63 107.4(3) . . ? C62 C61 C63 111.1(4) . . ? C64 C61 C63 111.4(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C19 O110 Zr1 133.8(2) . . ? O12 C121 C124 109.9(3) . . ? O12 C121 C123 109.9(3) . . ? C124 C121 C123 113.2(3) . . ? O12 C121 C122 101.8(3) . . ? C124 C121 C122 110.7(3) . . ? C123 C121 C122 110.8(3) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C121 C123 H12D 109.5 . . ? C121 C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C121 C123 H12F 109.5 . . ? H12D C123 H12F 109.5 . . ? H12E C123 H12F 109.5 . . ? C121 C124 H12G 109.5 . . ? C121 C124 H12H 109.5 . . ? H12G C124 H12H 109.5 . . ? C121 C124 H12I 109.5 . . ? H12G C124 H12I 109.5 . . ? H12H C124 H12I 109.5 . . ? O14 C141 C143 110.3(3) . . ? O14 C141 C142 102.3(3) . . ? C143 C141 C142 110.9(4) . . ? O14 C141 C144 110.4(4) . . ? C143 C141 C144 112.3(5) . . ? C142 C141 C144 110.3(4) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C141 C143 H14D 109.5 . . ? C141 C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C141 C143 H14F 109.5 . . ? H14D C143 H14F 109.5 . . ? H14E C143 H14F 109.5 . . ? C141 C144 H14G 109.5 . . ? C141 C144 H14H 109.5 . . ? H14G C144 H14H 109.5 . . ? C141 C144 H14I 109.5 . . ? H14G C144 H14I 109.5 . . ? H14H C144 H14I 109.5 . . ? O17 C171 C173 109.9(4) . . ? O17 C171 C174 110.2(4) . . ? C173 C171 C174 112.9(5) . . ? O17 C171 C172 101.7(3) . . ? C173 C171 C172 111.1(4) . . ? C174 C171 C172 110.4(4) . . ? C171 C172 H17A 109.5 . . ? C171 C172 H17B 109.5 . . ? H17A C172 H17B 109.5 . . ? C171 C172 H17C 109.5 . . ? H17A C172 H17C 109.5 . . ? H17B C172 H17C 109.5 . . ? C171 C173 H17D 109.5 . . ? C171 C173 H17E 109.5 . . ? H17D C173 H17E 109.5 . . ? C171 C173 H17F 109.5 . . ? H17D C173 H17F 109.5 . . ? H17E C173 H17F 109.5 . . ? C171 C174 H17G 109.5 . . ? C171 C174 H17H 109.5 . . ? H17G C174 H17H 109.5 . . ? C171 C174 H17I 109.5 . . ? H17G C174 H17I 109.5 . . ? H17H C174 H17I 109.5 . . ? O19 C191 C192 101.7(3) . . ? O19 C191 C193 110.2(3) . . ? C192 C191 C193 110.3(4) . . ? O19 C191 C194 110.0(3) . . ? C192 C191 C194 111.1(3) . . ? C193 C191 C194 113.0(4) . . ? C191 C192 H19A 109.5 . . ? C191 C192 H19B 109.5 . . ? H19A C192 H19B 109.5 . . ? C191 C192 H19C 109.5 . . ? H19A C192 H19C 109.5 . . ? H19B C192 H19C 109.5 . . ? C191 C193 H19D 109.5 . . ? C191 C193 H19E 109.5 . . ? H19D C193 H19E 109.5 . . ? C191 C193 H19F 109.5 . . ? H19D C193 H19F 109.5 . . ? H19E C193 H19F 109.5 . . ? C191 C194 H19G 109.5 . . ? C191 C194 H19H 109.5 . . ? H19G C194 H19H 109.5 . . ? C191 C194 H19I 109.5 . . ? H19G C194 H19I 109.5 . . ? H19H C194 H19I 109.5 . . ? O22 C221 C223 110.3(3) . . ? O22 C221 C222 101.7(3) . . ? C223 C221 C222 110.9(3) . . ? O22 C221 C224 109.6(3) . . ? C223 C221 C224 113.1(4) . . ? C222 C221 C224 110.6(3) . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C221 C223 H22D 109.5 . . ? C221 C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C221 C223 H22F 109.5 . . ? H22D C223 H22F 109.5 . . ? H22E C223 H22F 109.5 . . ? C221 C224 H22G 109.5 . . ? C221 C224 H22H 109.5 . . ? H22G C224 H22H 109.5 . . ? C221 C224 H22I 109.5 . . ? H22G C224 H22I 109.5 . . ? H22H C224 H22I 109.5 . . ? O24 C241 C243 110.1(3) . . ? O24 C241 C242 101.8(3) . . ? C243 C241 C242 110.7(3) . . ? O24 C241 C244 110.7(3) . . ? C243 C241 C244 112.7(3) . . ? C242 C241 C244 110.4(3) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C241 C243 H24D 109.5 . . ? C241 C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C241 C243 H24F 109.5 . . ? H24D C243 H24F 109.5 . . ? H24E C243 H24F 109.5 . . ? C241 C244 H24G 109.5 . . ? C241 C244 H24H 109.5 . . ? H24G C244 H24H 109.5 . . ? C241 C244 H24I 109.5 . . ? H24G C244 H24I 109.5 . . ? H24H C244 H24I 109.5 . . ? O26 C261 C264 111.1(3) . . ? O26 C261 C263 109.7(3) . . ? C264 C261 C263 113.3(4) . . ? O26 C261 C262 101.3(3) . . ? C264 C261 C262 110.2(4) . . ? C263 C261 C262 110.5(4) . . ? C261 C262 H26A 109.5 . . ? C261 C262 H26B 109.5 . . ? H26A C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26A C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C263 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? H26D C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26D C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C264 H26G 109.5 . . ? C261 C264 H26H 109.5 . . ? H26G C264 H26H 109.5 . . ? C261 C264 H26I 109.5 . . ? H26G C264 H26I 109.5 . . ? H26H C264 H26I 109.5 . . ? O28 C281 C283 110.0(3) . . ? O28 C281 C284 110.8(3) . . ? C283 C281 C284 112.2(3) . . ? O28 C281 C282 101.8(3) . . ? C283 C281 C282 110.5(4) . . ? C284 C281 C282 111.1(4) . . ? C281 C282 H28A 109.5 . . ? C281 C282 H28B 109.5 . . ? H28A C282 H28B 109.5 . . ? C281 C282 H28C 109.5 . . ? H28A C282 H28C 109.5 . . ? H28B C282 H28C 109.5 . . ? C281 C283 H28D 109.5 . . ? C281 C283 H28E 109.5 . . ? H28D C283 H28E 109.5 . . ? C281 C283 H28F 109.5 . . ? H28D C283 H28F 109.5 . . ? H28E C283 H28F 109.5 . . ? C281 C284 H28G 109.5 . . ? C281 C284 H28H 109.5 . . ? H28G C284 H28H 109.5 . . ? C281 C284 H28I 109.5 . . ? H28G C284 H28I 109.5 . . ? H28H C284 H28I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O41 Zr1 O11 C12 -171.3(3) . . . . ? O31 Zr1 O11 C12 87.4(3) . . . . ? O110 Zr1 O11 C12 -40.9(5) . . . . ? O15 Zr1 O11 C12 -0.8(3) . . . . ? O16 Zr1 O11 C12 -81.6(3) . . . . ? Zr1 O11 C12 O12 179.8(2) . . . . ? Zr1 O11 C12 C13 -0.9(5) . . . . ? C121 O12 C12 O11 -3.9(5) . . . . ? C121 O12 C12 C13 176.8(3) . . . . ? O11 C12 C13 C14 1.8(6) . . . . ? O12 C12 C13 C14 -178.9(3) . . . . ? C141 O14 C14 O15 4.5(5) . . . . ? C141 O14 C14 C13 -175.3(3) . . . . ? C12 C13 C14 O15 0.0(6) . . . . ? C12 C13 C14 O14 179.8(3) . . . . ? O14 C14 O15 Zr1 177.6(2) . . . . ? C13 C14 O15 Zr1 -2.6(6) . . . . ? O41 Zr1 O15 C14 56.0(7) . . . . ? O31 Zr1 O15 C14 -97.2(3) . . . . ? O11 Zr1 O15 C14 2.5(3) . . . . ? O110 Zr1 O15 C14 169.2(3) . . . . ? O16 Zr1 O15 C14 89.5(3) . . . . ? O41 Zr1 O16 C17 -103.6(3) . . . . ? O31 Zr1 O16 C17 47.9(7) . . . . ? O11 Zr1 O16 C17 162.2(3) . . . . ? O110 Zr1 O16 C17 -4.1(3) . . . . ? O15 Zr1 O16 C17 82.9(3) . . . . ? Zr1 O16 C17 O17 -176.4(2) . . . . ? Zr1 O16 C17 C18 3.8(6) . . . . ? C171 O17 C17 O16 9.7(5) . . . . ? C171 O17 C17 C18 -170.5(3) . . . . ? O16 C17 C18 C19 -1.3(6) . . . . ? O17 C17 C18 C19 178.9(3) . . . . ? C191 O19 C19 O110 3.1(5) . . . . ? C191 O19 C19 C18 -177.5(3) . . . . ? C17 C18 C19 O110 1.3(6) . . . . ? C17 C18 C19 O19 -178.1(3) . . . . ? O51 Zr2 O21 C22 -68.9(3) . . . . ? O61 Zr2 O21 C22 -170.5(3) . . . . ? O29 Zr2 O21 C22 56.5(4) . . . . ? O25 Zr2 O21 C22 98.1(3) . . . . ? O210 Zr2 O21 C22 17.9(3) . . . . ? Zr2 O21 C22 O22 168.7(2) . . . . ? Zr2 O21 C22 C23 -13.0(5) . . . . ? C221 O22 C22 O21 4.0(5) . . . . ? C221 O22 C22 C23 -174.5(3) . . . . ? O21 C22 C23 C24 -3.5(5) . . . . ? O22 C22 C23 C24 174.9(3) . . . . ? O51 Zr2 O210 C24 82.3(3) . . . . ? O61 Zr2 O210 C24 -65.7(6) . . . . ? O21 Zr2 O210 C24 -15.8(3) . . . . ? O29 Zr2 O210 C24 176.4(3) . . . . ? O25 Zr2 O210 C24 -104.7(3) . . . . ? Zr2 O210 C24 O24 -170.5(2) . . . . ? Zr2 O210 C24 C23 9.2(5) . . . . ? C241 O24 C24 O210 -12.8(4) . . . . ? C241 O24 C24 C23 167.5(3) . . . . ? C22 C23 C24 O210 4.8(5) . . . . ? C22 C23 C24 O24 -175.5(3) . . . . ? O51 Zr2 O25 C26 -44.5(6) . . . . ? O61 Zr2 O25 C26 111.4(3) . . . . ? O21 Zr2 O25 C26 -154.5(3) . . . . ? O29 Zr2 O25 C26 12.2(3) . . . . ? O210 Zr2 O25 C26 -75.6(3) . . . . ? Zr2 O25 C26 O26 172.7(2) . . . . ? Zr2 O25 C26 C27 -9.2(5) . . . . ? C261 O26 C26 O25 -6.6(5) . . . . ? C261 O26 C26 C27 175.1(3) . . . . ? O25 C26 C27 C28 -1.7(6) . . . . ? O26 C26 C27 C28 176.5(3) . . . . ? C281 O28 C28 O29 3.7(5) . . . . ? C281 O28 C28 C27 -177.0(3) . . . . ? C26 C27 C28 O29 3.4(6) . . . . ? C26 C27 C28 O28 -175.7(3) . . . . ? O28 C28 O29 Zr2 -174.5(2) . . . . ? C27 C28 O29 Zr2 6.3(6) . . . . ? O51 Zr2 O29 C28 157.6(3) . . . . ? O61 Zr2 O29 C28 -100.7(3) . . . . ? O21 Zr2 O29 C28 31.7(5) . . . . ? O25 Zr2 O29 C28 -11.0(3) . . . . ? O210 Zr2 O29 C28 69.4(3) . . . . ? O41 Zr1 O31 C31 22(5) . . . . ? O11 Zr1 O31 C31 118(5) . . . . ? O110 Zr1 O31 C31 -78(5) . . . . ? O15 Zr1 O31 C31 -164(5) . . . . ? O16 Zr1 O31 C31 -129(5) . . . . ? Zr1 O31 C31 C33 26(5) . . . . ? Zr1 O31 C31 C321 -121(5) . . . . ? Zr1 O31 C31 C341 95(5) . . . . ? Zr1 O31 C31 C32 -122(5) . . . . ? Zr1 O31 C31 C34 144(5) . . . . ? Zr1 O31 C31 C331 -11(5) . . . . ? O31 Zr1 O41 C41 12(5) . . . . ? O11 Zr1 O41 C41 -89(5) . . . . ? O110 Zr1 O41 C41 107(5) . . . . ? O15 Zr1 O41 C41 -141(5) . . . . ? O16 Zr1 O41 C41 -174(5) . . . . ? Zr1 O41 C41 C42 121(5) . . . . ? Zr1 O41 C41 C44 -92(5) . . . . ? Zr1 O41 C41 C431 -38(5) . . . . ? Zr1 O41 C41 C421 82(5) . . . . ? Zr1 O41 C41 C441 -139(5) . . . . ? Zr1 O41 C41 C43 12(5) . . . . ? O61 Zr2 O51 C51 171.3(13) . . . . ? O21 Zr2 O51 C51 75.5(13) . . . . ? O29 Zr2 O51 C51 -88.4(13) . . . . ? O25 Zr2 O51 C51 -33.3(16) . . . . ? O210 Zr2 O51 C51 -2.8(13) . . . . ? Zr2 O51 C51 C52 14.4(15) . . . . ? Zr2 O51 C51 C54 134.7(12) . . . . ? Zr2 O51 C51 C53 -105.7(13) . . . . ? O51 Zr2 O61 C61 7.9(8) . . . . ? O21 Zr2 O61 C61 106.5(8) . . . . ? O29 Zr2 O61 C61 -88.0(8) . . . . ? O25 Zr2 O61 C61 -166.5(8) . . . . ? O210 Zr2 O61 C61 155.3(7) . . . . ? Zr2 O61 C61 C62 -130.6(7) . . . . ? Zr2 O61 C61 C64 109.9(8) . . . . ? Zr2 O61 C61 C63 -10.4(10) . . . . ? O19 C19 O110 Zr1 175.4(2) . . . . ? C18 C19 O110 Zr1 -3.9(5) . . . . ? O41 Zr1 O110 C19 92.4(3) . . . . ? O31 Zr1 O110 C19 -166.5(3) . . . . ? O11 Zr1 O110 C19 -37.4(5) . . . . ? O15 Zr1 O110 C19 -76.7(3) . . . . ? O16 Zr1 O110 C19 4.2(3) . . . . ? C12 O12 C121 C124 -60.7(4) . . . . ? C12 O12 C121 C123 64.5(4) . . . . ? C12 O12 C121 C122 -178.1(3) . . . . ? C14 O14 C141 C143 61.7(5) . . . . ? C14 O14 C141 C142 179.7(3) . . . . ? C14 O14 C141 C144 -63.0(5) . . . . ? C17 O17 C171 C173 58.5(5) . . . . ? C17 O17 C171 C174 -66.6(5) . . . . ? C17 O17 C171 C172 176.3(3) . . . . ? C19 O19 C191 C192 176.6(3) . . . . ? C19 O19 C191 C193 59.7(4) . . . . ? C19 O19 C191 C194 -65.5(4) . . . . ? C22 O22 C221 C223 -64.1(4) . . . . ? C22 O22 C221 C222 178.2(3) . . . . ? C22 O22 C221 C224 61.1(4) . . . . ? C24 O24 C241 C243 -57.8(4) . . . . ? C24 O24 C241 C242 -175.2(3) . . . . ? C24 O24 C241 C244 67.5(4) . . . . ? C26 O26 C261 C264 64.6(4) . . . . ? C26 O26 C261 C263 -61.5(5) . . . . ? C26 O26 C261 C262 -178.3(4) . . . . ? C28 O28 C281 C283 60.1(4) . . . . ? C28 O28 C281 C284 -64.5(4) . . . . ? C28 O28 C281 C282 177.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.909 _refine_diff_density_min -1.356 _refine_diff_density_rms 0.091 #=================================END data_cvd176 _database_code_depnum_ccdc_archive 'CCDC 692630' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H76 Hf O16 Si8' _chemical_formula_weight 1168.18 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M I4(1)/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 20.2381(6) _cell_length_b 20.2381(6) _cell_length_c 14.2483(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5835.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 115(2) _cell_measurement_reflns_used 2800 _cell_measurement_theta_min 2.660 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.330 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 2.006 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.753 _exptl_absorpt_correction_T_max 0.835 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 115(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '407 images at 1.0 deg. in \w and 25 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13188 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0368 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2553 _reflns_number_gt 2230 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0264P)^2^+12.5344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2553 _refine_ls_number_parameters 144 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0361 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0622 _refine_ls_wR_factor_gt 0.0586 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Hf1 Hf 1.0000 0.2500 0.1250 0.01770(9) Uani 1 4 d S . . O1 O 1.07301(10) 0.31756(10) 0.08197(15) 0.0201(5) Uani 1 1 d . . . O2 O 1.14911(10) 0.37006(11) -0.00283(16) 0.0258(5) Uani 1 1 d . . . C2 C 1.08739(15) 0.34567(14) 0.0040(2) 0.0215(7) Uani 1 1 d . . . Si2 Si 1.20584(5) 0.36668(5) 0.08509(7) 0.0285(2) Uani 1 1 d . . . C21 C 1.1750(2) 0.4140(2) 0.1861(3) 0.0540(12) Uani 1 1 d . . . H21A H 1.1597 0.4575 0.1649 0.081 Uiso 1 1 calc R . . H21B H 1.2106 0.4196 0.2320 0.081 Uiso 1 1 calc R . . H21C H 1.1382 0.3901 0.2152 0.081 Uiso 1 1 calc R . . C22 C 1.27786(17) 0.4083(2) 0.0303(3) 0.0406(10) Uani 1 1 d . . . H22A H 1.2952 0.3806 -0.0204 0.061 Uiso 1 1 calc R . . H22B H 1.3123 0.4151 0.0777 0.061 Uiso 1 1 calc R . . H22C H 1.2641 0.4511 0.0049 0.061 Uiso 1 1 calc R . . C23 C 1.22463(18) 0.28026(18) 0.1186(3) 0.0393(9) Uani 1 1 d . . . H23A H 1.1834 0.2569 0.1327 0.059 Uiso 1 1 calc R . . H23B H 1.2531 0.2800 0.1742 0.059 Uiso 1 1 calc R . . H23C H 1.2473 0.2581 0.0666 0.059 Uiso 1 1 calc R . . C3 C 1.04564(15) 0.35325(15) -0.0714(2) 0.0232(7) Uani 1 1 d . . . H3 H 1.0612 0.3747 -0.1265 0.028 Uiso 1 1 calc R . . C4 C 0.98056(15) 0.32991(15) -0.0686(2) 0.0221(7) Uani 1 1 d . . . O4 O 0.94426(11) 0.34641(12) -0.14347(16) 0.0335(6) Uani 1 1 d . . . O5 O 0.95470(10) 0.29753(10) -0.00347(15) 0.0212(5) Uani 1 1 d . . . Si4 Si 0.87552(4) 0.31832(5) -0.19591(7) 0.0273(2) Uani 1 1 d . . . C41 C 0.9008(2) 0.2535(2) -0.2792(3) 0.0462(10) Uani 1 1 d . . . H41A H 0.9316 0.2721 -0.3252 0.069 Uiso 1 1 calc R . . H41B H 0.8617 0.2363 -0.3117 0.069 Uiso 1 1 calc R . . H41C H 0.9225 0.2175 -0.2450 0.069 Uiso 1 1 calc R . . C42 C 0.8448(2) 0.3919(2) -0.2585(3) 0.0547(12) Uani 1 1 d . . . H42A H 0.8338 0.4265 -0.2130 0.082 Uiso 1 1 calc R . . H42B H 0.8052 0.3801 -0.2945 0.082 Uiso 1 1 calc R . . H42C H 0.8790 0.4081 -0.3013 0.082 Uiso 1 1 calc R . . C43 C 0.81226(18) 0.2859(2) -0.1144(3) 0.0410(9) Uani 1 1 d . . . H43A H 0.8313 0.2502 -0.0767 0.061 Uiso 1 1 calc R . . H43B H 0.7747 0.2690 -0.1504 0.061 Uiso 1 1 calc R . . H43C H 0.7973 0.3215 -0.0729 0.061 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 Hf1 0.01679(11) 0.01679(11) 0.01951(15) 0.000 0.000 0.000 O1 0.0191(11) 0.0215(11) 0.0198(12) 0.0018(9) -0.0017(9) -0.0038(9) O2 0.0214(11) 0.0286(12) 0.0276(13) 0.0069(10) -0.0008(10) -0.0064(9) C2 0.0200(16) 0.0157(15) 0.0289(19) -0.0005(13) 0.0013(14) -0.0008(12) Si2 0.0251(5) 0.0325(5) 0.0279(5) 0.0053(4) -0.0022(4) -0.0107(4) C21 0.057(3) 0.058(3) 0.047(3) -0.017(2) 0.005(2) -0.023(2) C22 0.0256(19) 0.048(2) 0.048(2) 0.0188(19) -0.0058(17) -0.0128(16) C23 0.0305(19) 0.044(2) 0.044(2) 0.0150(19) -0.0089(18) -0.0080(16) C3 0.0255(17) 0.0217(16) 0.0223(18) 0.0048(13) -0.0006(14) -0.0037(13) C4 0.0257(17) 0.0181(16) 0.0227(18) 0.0000(14) -0.0019(14) 0.0044(13) O4 0.0296(13) 0.0398(14) 0.0309(15) 0.0136(11) -0.0115(10) -0.0046(10) O5 0.0215(11) 0.0202(11) 0.0217(12) -0.0006(9) -0.0007(9) 0.0023(9) Si4 0.0249(5) 0.0320(5) 0.0249(5) 0.0008(4) -0.0049(4) 0.0028(4) C41 0.050(2) 0.047(2) 0.042(2) -0.0083(19) 0.005(2) -0.0012(19) C42 0.053(3) 0.051(3) 0.061(3) 0.011(2) -0.023(2) 0.010(2) C43 0.0272(19) 0.056(2) 0.040(2) 0.001(2) 0.0019(17) -0.0023(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 O1 2.104(2) . ? Hf1 O1 2.1045(19) 6_654 ? Hf1 O1 2.1045(19) 15_665 ? Hf1 O1 2.1045(19) 12_756 ? Hf1 O5 2.262(2) 15_665 ? Hf1 O5 2.262(2) 6_654 ? Hf1 O5 2.262(2) . ? Hf1 O5 2.262(2) 12_756 ? O1 C2 1.282(4) . ? O2 C2 1.347(4) . ? O2 Si2 1.701(2) . ? C2 C3 1.376(4) . ? Si2 C21 1.838(4) . ? Si2 C23 1.852(4) . ? Si2 C22 1.855(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C3 C4 1.400(4) . ? C3 H3 0.9500 . ? C4 O5 1.250(4) . ? C4 O4 1.338(4) . ? O4 Si4 1.678(2) . ? Si4 C41 1.842(4) . ? Si4 C42 1.843(4) . ? Si4 C43 1.848(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? 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 Hf1 O1 146.13(11) . 6_654 ? O1 Hf1 O1 94.87(3) . 15_665 ? O1 Hf1 O1 94.87(3) 6_654 15_665 ? O1 Hf1 O1 94.87(3) . 12_756 ? O1 Hf1 O1 94.87(3) 6_654 12_756 ? O1 Hf1 O1 146.13(11) 15_665 12_756 ? O1 Hf1 O5 70.96(8) . 15_665 ? O1 Hf1 O5 142.91(8) 6_654 15_665 ? O1 Hf1 O5 76.85(8) 15_665 15_665 ? O1 Hf1 O5 75.88(8) 12_756 15_665 ? O1 Hf1 O5 75.88(8) . 6_654 ? O1 Hf1 O5 76.85(8) 6_654 6_654 ? O1 Hf1 O5 70.96(8) 15_665 6_654 ? O1 Hf1 O5 142.91(8) 12_756 6_654 ? O5 Hf1 O5 130.91(6) 15_665 6_654 ? O1 Hf1 O5 76.85(8) . . ? O1 Hf1 O5 75.88(8) 6_654 . ? O1 Hf1 O5 142.91(8) 15_665 . ? O1 Hf1 O5 70.96(8) 12_756 . ? O5 Hf1 O5 130.91(6) 15_665 . ? O5 Hf1 O5 71.95(10) 6_654 . ? O1 Hf1 O5 142.91(8) . 12_756 ? O1 Hf1 O5 70.96(8) 6_654 12_756 ? O1 Hf1 O5 75.88(8) 15_665 12_756 ? O1 Hf1 O5 76.85(8) 12_756 12_756 ? O5 Hf1 O5 71.95(10) 15_665 12_756 ? O5 Hf1 O5 130.91(6) 6_654 12_756 ? O5 Hf1 O5 130.91(6) . 12_756 ? C2 O1 Hf1 134.44(19) . . ? C2 O2 Si2 124.0(2) . . ? O1 C2 O2 115.8(3) . . ? O1 C2 C3 126.0(3) . . ? O2 C2 C3 118.2(3) . . ? O2 Si2 C21 109.04(18) . . ? O2 Si2 C23 111.49(15) . . ? C21 Si2 C23 111.1(2) . . ? O2 Si2 C22 101.69(15) . . ? C21 Si2 C22 111.10(19) . . ? C23 Si2 C22 112.05(18) . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C2 C3 C4 121.1(3) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O5 C4 O4 119.5(3) . . ? O5 C4 C3 126.3(3) . . ? O4 C4 C3 114.1(3) . . ? C4 O4 Si4 136.5(2) . . ? C4 O5 Hf1 130.80(19) . . ? O4 Si4 C41 107.34(17) . . ? O4 Si4 C42 102.80(17) . . ? C41 Si4 C42 110.9(2) . . ? O4 Si4 C43 114.49(16) . . ? C41 Si4 C43 110.14(19) . . ? C42 Si4 C43 110.9(2) . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Hf1 O1 C2 13.9(2) 6_654 . . . ? O1 Hf1 O1 C2 120.1(3) 15_665 . . . ? O1 Hf1 O1 C2 -92.3(2) 12_756 . . . ? O5 Hf1 O1 C2 -165.6(3) 15_665 . . . ? O5 Hf1 O1 C2 51.2(3) 6_654 . . . ? O5 Hf1 O1 C2 -23.2(3) . . . . ? O5 Hf1 O1 C2 -166.9(2) 12_756 . . . ? Hf1 O1 C2 O2 -160.41(19) . . . . ? Hf1 O1 C2 C3 20.1(5) . . . . ? Si2 O2 C2 O1 -1.3(4) . . . . ? Si2 O2 C2 C3 178.2(2) . . . . ? C2 O2 Si2 C21 -62.4(3) . . . . ? C2 O2 Si2 C23 60.6(3) . . . . ? C2 O2 Si2 C22 -179.8(3) . . . . ? O1 C2 C3 C4 0.4(5) . . . . ? O2 C2 C3 C4 -179.1(3) . . . . ? C2 C3 C4 O5 -4.5(5) . . . . ? C2 C3 C4 O4 174.0(3) . . . . ? O5 C4 O4 Si4 -22.8(5) . . . . ? C3 C4 O4 Si4 158.6(3) . . . . ? O4 C4 O5 Hf1 171.95(19) . . . . ? C3 C4 O5 Hf1 -9.6(5) . . . . ? O1 Hf1 O5 C4 17.8(2) . . . . ? O1 Hf1 O5 C4 -141.9(3) 6_654 . . . ? O1 Hf1 O5 C4 -62.7(3) 15_665 . . . ? O1 Hf1 O5 C4 117.7(3) 12_756 . . . ? O5 Hf1 O5 C4 67.6(2) 15_665 . . . ? O5 Hf1 O5 C4 -61.4(2) 6_654 . . . ? O5 Hf1 O5 C4 169.6(2) 12_756 . . . ? C4 O4 Si4 C41 -87.1(4) . . . . ? C4 O4 Si4 C42 155.8(3) . . . . ? C4 O4 Si4 C43 35.4(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.361 _refine_diff_density_min -0.293 _refine_diff_density_rms 0.078 #=================================END data_cvd182 _database_code_depnum_ccdc_archive 'CCDC 692631' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H36 Hf O16' _chemical_formula_weight 795.05 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' Hf Hf -0.5830 6.1852 '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 10.9049(3) _cell_length_b 13.6935(5) _cell_length_c 21.4560(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.425(3) _cell_angle_gamma 90.00 _cell_volume 3177.08(19) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 20359 _cell_measurement_theta_min 2.578 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1592 _exptl_absorpt_coefficient_mu 3.356 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.210 _exptl_absorpt_correction_T_max 0.340 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '586 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18215 _diffrn_reflns_av_R_equivalents 0.0176 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.85 _diffrn_reflns_theta_max 27.58 _reflns_number_total 7258 _reflns_number_gt 5843 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0222P)^2^+3.5839P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7258 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0555 _refine_ls_wR_factor_gt 0.0505 _refine_ls_goodness_of_fit_ref 1.121 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.751668(10) 0.777512(8) 0.084575(5) 0.01544(4) Uani 1 1 d . . . O41 O 0.76883(18) 0.71203(15) 0.17760(9) 0.0196(4) Uani 1 1 d . . . O35 O 0.62671(18) 0.86508(15) 0.13426(10) 0.0208(4) Uani 1 1 d . . . O45 O 0.59260(18) 0.68355(16) 0.08242(10) 0.0211(4) Uani 1 1 d . . . O31 O 0.87183(19) 0.87678(16) 0.14181(10) 0.0213(4) Uani 1 1 d . . . O15 O 0.73977(18) 0.68608(15) 0.00025(10) 0.0212(4) Uani 1 1 d . . . O11 O 0.91786(18) 0.69195(16) 0.09751(10) 0.0221(5) Uani 1 1 d . . . O25 O 0.62472(18) 0.85467(15) 0.01662(9) 0.0197(4) Uani 1 1 d . . . O21 O 0.87076(17) 0.85280(15) 0.02553(9) 0.0187(4) Uani 1 1 d . . . O22 O 0.95172(19) 0.90424(16) -0.05928(10) 0.0237(5) Uani 1 1 d . . . O42 O 0.7313(2) 0.65920(18) 0.27191(10) 0.0287(5) Uani 1 1 d . . . O34 O 0.5408(2) 0.93797(17) 0.21111(11) 0.0284(5) Uani 1 1 d . . . O44 O 0.4245(2) 0.60492(19) 0.10510(11) 0.0332(6) Uani 1 1 d . . . O12 O 1.0956(2) 0.62052(19) 0.08261(12) 0.0356(6) Uani 1 1 d . . . O24 O 0.52597(19) 0.91105(17) -0.07397(10) 0.0260(5) Uani 1 1 d . . . C14 C 0.8211(3) 0.6454(2) -0.02773(15) 0.0237(7) Uani 1 1 d . . . O32 O 0.9658(2) 0.95950(18) 0.22471(11) 0.0295(5) Uani 1 1 d . . . O14 O 0.7889(2) 0.61498(18) -0.08692(11) 0.0322(5) Uani 1 1 d . . . C43 C 0.5761(3) 0.6390(2) 0.18794(15) 0.0249(7) Uani 1 1 d . . . H42 H 0.5245 0.6123 0.2160 0.030 Uiso 1 1 calc R . . C20 C 0.6940(3) 0.6724(2) 0.20986(14) 0.0212(6) Uani 1 1 d . . . C12 C 0.9806(3) 0.6491(2) 0.06000(15) 0.0245(7) Uani 1 1 d . . . C13 C 0.9420(3) 0.6263(2) -0.00201(16) 0.0285(7) Uani 1 1 d . . . H22A H 0.9980 0.5976 -0.0271 0.034 Uiso 1 1 calc R . . C94 C 0.6156(3) 0.2794(3) 0.19071(17) 0.0336(8) Uani 1 1 d . . . H23A H 0.5355 0.2768 0.2036 0.040 Uiso 1 1 calc R . . C44 C 0.5354(3) 0.6454(2) 0.12410(15) 0.0227(7) Uani 1 1 d . . . C97 C 0.8465(3) 0.2873(3) 0.15183(17) 0.0344(8) Uani 1 1 d . . . H25A H 0.9261 0.2890 0.1384 0.041 Uiso 1 1 calc R . . C24 C 0.6308(3) 0.8865(2) -0.03778(14) 0.0191(6) Uani 1 1 d . . . C22 C 0.8524(3) 0.8841(2) -0.02998(14) 0.0186(6) Uani 1 1 d . . . C431 C 0.4238(3) 0.9108(3) 0.17702(16) 0.0328(8) Uani 1 1 d . . . H30A H 0.3569 0.9333 0.1999 0.049 Uiso 1 1 calc R . . H30B H 0.4197 0.8396 0.1726 0.049 Uiso 1 1 calc R . . H30C H 0.4149 0.9409 0.1352 0.049 Uiso 1 1 calc R . . C93 C 0.6570(3) 0.3653(3) 0.16585(16) 0.0321(8) Uani 1 1 d . . . H31A H 0.6051 0.4213 0.1626 0.038 Uiso 1 1 calc R . . C34 C 0.6419(3) 0.9112(2) 0.18514(15) 0.0229(7) Uani 1 1 d . . . C221 C 1.0714(3) 0.8838(3) -0.02455(16) 0.0280(7) Uani 1 1 d . . . H34A H 1.1363 0.9012 -0.0502 0.042 Uiso 1 1 calc R . . H34B H 1.0772 0.8141 -0.0142 0.042 Uiso 1 1 calc R . . H34C H 1.0819 0.9223 0.0143 0.042 Uiso 1 1 calc R . . C241 C 0.4115(3) 0.8948(3) -0.04798(16) 0.0304(8) Uani 1 1 d . . . H36A H 0.3416 0.9152 -0.0785 0.046 Uiso 1 1 calc R . . H36B H 0.4120 0.9329 -0.0093 0.046 Uiso 1 1 calc R . . H36C H 0.4036 0.8252 -0.0385 0.046 Uiso 1 1 calc R . . C92 C 0.7727(3) 0.3708(3) 0.14574(16) 0.0310(8) Uani 1 1 d . . . C95 C 0.6904(4) 0.1982(3) 0.19658(17) 0.0347(8) Uani 1 1 d . . . H41A H 0.6627 0.1397 0.2140 0.042 Uiso 1 1 calc R . . C421 C 0.8516(3) 0.6993(3) 0.29455(16) 0.0349(9) Uani 1 1 d . . . H42A H 0.8710 0.6864 0.3397 0.052 Uiso 1 1 calc R . . H42B H 0.8509 0.7700 0.2872 0.052 Uiso 1 1 calc R . . H42C H 0.9144 0.6688 0.2721 0.052 Uiso 1 1 calc R . . C32 C 0.8622(3) 0.9227(2) 0.19221(15) 0.0236(7) Uani 1 1 d . . . C23 C 0.7388(3) 0.9014(2) -0.06525(14) 0.0221(6) Uani 1 1 d . . . H47A H 0.7344 0.9231 -0.1075 0.027 Uiso 1 1 calc R . . C441 C 0.3791(3) 0.6109(3) 0.03938(18) 0.0410(9) Uani 1 1 d . . . H48A H 0.2981 0.5791 0.0315 0.062 Uiso 1 1 calc R . . H48B H 0.4371 0.5780 0.0150 0.062 Uiso 1 1 calc R . . H48C H 0.3712 0.6796 0.0267 0.062 Uiso 1 1 calc R . . C141 C 0.6651(3) 0.6370(3) -0.11480(17) 0.0354(8) Uani 1 1 d . . . H50A H 0.6519 0.6115 -0.1578 0.053 Uiso 1 1 calc R . . H50B H 0.6529 0.7079 -0.1156 0.053 Uiso 1 1 calc R . . H50C H 0.6060 0.6065 -0.0900 0.053 Uiso 1 1 calc R . . C91 C 0.8180(4) 0.4639(3) 0.1201(2) 0.0450(10) Uani 1 1 d . . . H53A H 0.7538 0.5141 0.1195 0.068 Uiso 1 1 calc R . . H53B H 0.8370 0.4529 0.0773 0.068 Uiso 1 1 calc R . . H53C H 0.8927 0.4856 0.1468 0.068 Uiso 1 1 calc R . . C33 C 0.7544(3) 0.9404(2) 0.21781(15) 0.0266(7) Uani 1 1 d . . . H54A H 0.7571 0.9722 0.2573 0.032 Uiso 1 1 calc R . . C96 C 0.8063(3) 0.2025(3) 0.17690(18) 0.0362(8) Uani 1 1 d . . . H55A H 0.8583 0.1465 0.1807 0.043 Uiso 1 1 calc R . . C321 C 1.0807(3) 0.9385(3) 0.20024(17) 0.0332(8) Uani 1 1 d . . . H16A H 1.1496 0.9685 0.2274 0.050 Uiso 1 1 calc R . . H16B H 1.0772 0.9650 0.1576 0.050 Uiso 1 1 calc R . . H16C H 1.0930 0.8676 0.1991 0.050 Uiso 1 1 calc R . . C121 C 1.1369(3) 0.6401(3) 0.14783(18) 0.0433(10) Uani 1 1 d . . . H81A H 1.2211 0.6150 0.1588 0.065 Uiso 1 1 calc R . . H81B H 1.0814 0.6080 0.1739 0.065 Uiso 1 1 calc R . . H81C H 1.1363 0.7107 0.1552 0.065 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 Hf1 0.01472(6) 0.01766(6) 0.01445(6) 0.00131(5) 0.00379(4) 0.00108(5) O41 0.0189(9) 0.0225(11) 0.0180(10) 0.0056(9) 0.0044(8) 0.0017(8) O35 0.0212(10) 0.0247(11) 0.0169(11) 0.0005(9) 0.0044(8) 0.0045(9) O45 0.0190(10) 0.0235(11) 0.0218(11) 0.0004(9) 0.0059(8) -0.0038(9) O31 0.0222(10) 0.0248(11) 0.0178(11) -0.0015(9) 0.0062(8) -0.0040(9) O15 0.0221(10) 0.0218(11) 0.0209(11) -0.0037(9) 0.0065(8) -0.0012(9) O11 0.0189(10) 0.0276(12) 0.0210(11) 0.0056(9) 0.0070(8) 0.0073(9) O25 0.0179(10) 0.0252(11) 0.0169(10) 0.0029(9) 0.0052(8) 0.0033(8) O21 0.0180(10) 0.0231(11) 0.0151(10) 0.0026(9) 0.0030(8) 0.0002(8) O22 0.0218(10) 0.0316(12) 0.0188(11) 0.0029(9) 0.0072(8) -0.0018(9) O42 0.0291(12) 0.0386(14) 0.0187(11) 0.0124(10) 0.0049(9) -0.0042(11) O34 0.0285(12) 0.0338(13) 0.0252(12) -0.0008(10) 0.0125(9) 0.0076(10) O44 0.0250(12) 0.0444(15) 0.0311(13) -0.0007(12) 0.0076(10) -0.0129(11) O12 0.0274(12) 0.0485(15) 0.0322(14) 0.0079(12) 0.0086(10) 0.0201(11) O24 0.0207(11) 0.0370(13) 0.0202(11) 0.0060(10) 0.0014(9) 0.0045(10) C14 0.0336(17) 0.0185(15) 0.0211(16) -0.0004(13) 0.0109(13) 0.0020(13) O32 0.0291(12) 0.0349(13) 0.0239(12) -0.0071(10) 0.0012(9) -0.0069(10) O14 0.0427(14) 0.0327(13) 0.0221(12) -0.0073(11) 0.0070(10) 0.0063(11) C43 0.0231(15) 0.0277(17) 0.0261(17) 0.0058(14) 0.0116(13) -0.0007(13) C20 0.0262(15) 0.0211(15) 0.0176(15) 0.0041(13) 0.0085(12) 0.0040(13) C12 0.0228(15) 0.0238(16) 0.0293(17) 0.0065(14) 0.0125(13) 0.0068(13) C13 0.0306(17) 0.0292(18) 0.0283(18) -0.0015(15) 0.0135(14) 0.0083(14) C94 0.0328(17) 0.038(2) 0.0307(18) -0.0062(17) 0.0060(14) 0.0014(16) C44 0.0196(14) 0.0199(15) 0.0305(17) -0.0024(13) 0.0103(12) -0.0007(12) C97 0.0314(17) 0.037(2) 0.0349(19) -0.0082(17) 0.0041(15) 0.0021(16) C24 0.0219(14) 0.0180(14) 0.0168(14) -0.0017(12) 0.0005(11) 0.0024(12) C22 0.0237(14) 0.0166(14) 0.0168(14) -0.0026(12) 0.0073(11) -0.0030(12) C431 0.0280(17) 0.043(2) 0.0295(19) 0.0063(16) 0.0112(14) 0.0119(15) C93 0.0382(19) 0.0299(19) 0.0288(19) -0.0003(15) 0.0073(15) 0.0096(15) C34 0.0297(16) 0.0217(16) 0.0194(15) 0.0041(13) 0.0113(13) 0.0051(13) C221 0.0189(15) 0.0346(18) 0.0314(18) -0.0009(15) 0.0068(13) -0.0017(13) C241 0.0198(15) 0.043(2) 0.0278(18) 0.0046(16) 0.0021(13) 0.0038(14) C92 0.0420(19) 0.0293(18) 0.0219(17) -0.0040(14) 0.0054(14) -0.0011(15) C95 0.046(2) 0.0266(19) 0.0303(19) 0.0000(15) 0.0010(16) -0.0030(15) C421 0.0289(17) 0.051(2) 0.0247(18) 0.0115(16) 0.0030(14) -0.0038(16) C32 0.0308(16) 0.0202(15) 0.0199(16) 0.0043(13) 0.0034(13) -0.0036(13) C23 0.0249(15) 0.0264(16) 0.0152(14) 0.0043(13) 0.0030(12) 0.0024(13) C441 0.0277(18) 0.062(3) 0.034(2) -0.0053(19) 0.0034(15) -0.0141(18) C141 0.039(2) 0.039(2) 0.0271(19) -0.0086(16) -0.0008(15) -0.0019(16) C91 0.060(3) 0.035(2) 0.043(2) 0.0004(18) 0.020(2) -0.0011(19) C33 0.0348(17) 0.0245(17) 0.0213(16) -0.0052(13) 0.0064(13) -0.0011(14) C96 0.0363(19) 0.030(2) 0.040(2) -0.0011(16) -0.0010(16) 0.0070(15) C321 0.0271(17) 0.042(2) 0.0305(19) -0.0028(16) 0.0022(14) -0.0084(15) C121 0.0257(18) 0.068(3) 0.036(2) 0.010(2) 0.0019(15) 0.0195(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 Hf1 O11 2.146(2) . ? Hf1 O25 2.153(2) . ? Hf1 O45 2.155(2) . ? Hf1 O31 2.158(2) . ? Hf1 O41 2.174(2) . ? Hf1 O21 2.1862(19) . ? Hf1 O15 2.190(2) . ? Hf1 O35 2.192(2) . ? O41 C20 1.259(3) . ? O35 C34 1.254(4) . ? O45 C44 1.267(4) . ? O31 C32 1.267(4) . ? O15 C14 1.263(4) . ? O11 C12 1.266(4) . ? O25 C24 1.256(4) . ? O21 C22 1.257(3) . ? O22 C22 1.349(3) . ? O22 C221 1.444(4) . ? O42 C20 1.353(4) . ? O42 C421 1.447(4) . ? O34 C34 1.349(3) . ? O34 C431 1.435(4) . ? O44 C44 1.345(4) . ? O44 C441 1.435(4) . ? O12 C12 1.344(4) . ? O12 C121 1.439(4) . ? O24 C24 1.339(4) . ? O24 C241 1.448(4) . ? C14 O14 1.340(4) . ? C14 C13 1.387(5) . ? O32 C32 1.346(4) . ? O32 C321 1.448(4) . ? O14 C141 1.436(4) . ? C43 C44 1.387(5) . ? C43 C20 1.388(4) . ? C43 H42 0.9500 . ? C12 C13 1.379(5) . ? C13 H22A 0.9500 . ? C94 C95 1.375(5) . ? C94 C93 1.392(5) . ? C94 H23A 0.9500 . ? C97 C96 1.375(5) . ? C97 C92 1.394(5) . ? C97 H25A 0.9500 . ? C24 C23 1.398(4) . ? C22 C23 1.386(4) . ? C431 H30A 0.9800 . ? C431 H30B 0.9800 . ? C431 H30C 0.9800 . ? C93 C92 1.387(5) . ? C93 H31A 0.9500 . ? C34 C33 1.391(5) . ? C221 H34A 0.9800 . ? C221 H34B 0.9800 . ? C221 H34C 0.9800 . ? C241 H36A 0.9800 . ? C241 H36B 0.9800 . ? C241 H36C 0.9800 . ? C92 C91 1.497(5) . ? C95 C96 1.385(5) . ? C95 H41A 0.9500 . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C32 C33 1.382(4) . ? C23 H47A 0.9500 . ? C441 H48A 0.9800 . ? C441 H48B 0.9800 . ? C441 H48C 0.9800 . ? C141 H50A 0.9800 . ? C141 H50B 0.9800 . ? C141 H50C 0.9800 . ? C91 H53A 0.9800 . ? C91 H53B 0.9800 . ? C91 H53C 0.9800 . ? C33 H54A 0.9500 . ? C96 H55A 0.9500 . ? C321 H16A 0.9800 . ? C321 H16B 0.9800 . ? C321 H16C 0.9800 . ? C121 H81A 0.9800 . ? C121 H81B 0.9800 . ? C121 H81C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Hf1 O25 144.47(8) . . ? O11 Hf1 O45 109.92(8) . . ? O25 Hf1 O45 80.40(8) . . ? O11 Hf1 O31 80.20(8) . . ? O25 Hf1 O31 111.48(8) . . ? O45 Hf1 O31 144.69(8) . . ? O11 Hf1 O41 71.64(7) . . ? O25 Hf1 O41 142.71(7) . . ? O45 Hf1 O41 75.35(8) . . ? O31 Hf1 O41 76.32(8) . . ? O11 Hf1 O21 77.14(8) . . ? O25 Hf1 O21 75.78(7) . . ? O45 Hf1 O21 143.68(8) . . ? O31 Hf1 O21 70.74(7) . . ? O41 Hf1 O21 137.68(7) . . ? O11 Hf1 O15 75.74(8) . . ? O25 Hf1 O15 75.93(8) . . ? O45 Hf1 O15 71.30(8) . . ? O31 Hf1 O15 142.84(7) . . ? O41 Hf1 O15 120.76(8) . . ? O21 Hf1 O15 76.54(8) . . ? O11 Hf1 O35 143.45(8) . . ? O25 Hf1 O35 71.06(7) . . ? O45 Hf1 O35 77.76(8) . . ? O31 Hf1 O35 75.44(8) . . ? O41 Hf1 O35 76.37(7) . . ? O21 Hf1 O35 118.49(8) . . ? O15 Hf1 O35 137.74(8) . . ? C20 O41 Hf1 134.2(2) . . ? C34 O35 Hf1 132.8(2) . . ? C44 O45 Hf1 134.3(2) . . ? C32 O31 Hf1 133.43(19) . . ? C14 O15 Hf1 132.4(2) . . ? C12 O11 Hf1 133.4(2) . . ? C24 O25 Hf1 133.87(18) . . ? C22 O21 Hf1 132.53(18) . . ? C22 O22 C221 116.5(2) . . ? C20 O42 C421 115.1(2) . . ? C34 O34 C431 116.1(3) . . ? C44 O44 C441 117.2(3) . . ? C12 O12 C121 117.2(3) . . ? C24 O24 C241 116.8(2) . . ? O15 C14 O14 118.3(3) . . ? O15 C14 C13 125.7(3) . . ? O14 C14 C13 115.9(3) . . ? C32 O32 C321 116.4(3) . . ? C14 O14 C141 116.5(3) . . ? C44 C43 C20 118.5(3) . . ? C44 C43 H42 120.7 . . ? C20 C43 H42 120.7 . . ? O41 C20 O42 117.7(3) . . ? O41 C20 C43 126.4(3) . . ? O42 C20 C43 115.9(3) . . ? O11 C12 O12 117.5(3) . . ? O11 C12 C13 126.6(3) . . ? O12 C12 C13 115.9(3) . . ? C12 C13 C14 119.8(3) . . ? C12 C13 H22A 120.1 . . ? C14 C13 H22A 120.1 . . ? C95 C94 C93 120.0(3) . . ? C95 C94 H23A 120.0 . . ? C93 C94 H23A 120.0 . . ? O45 C44 O44 117.5(3) . . ? O45 C44 C43 126.8(3) . . ? O44 C44 C43 115.7(3) . . ? C96 C97 C92 121.4(3) . . ? C96 C97 H25A 119.3 . . ? C92 C97 H25A 119.3 . . ? O25 C24 O24 118.8(3) . . ? O25 C24 C23 126.2(3) . . ? O24 C24 C23 114.9(3) . . ? O21 C22 O22 118.2(3) . . ? O21 C22 C23 126.7(3) . . ? O22 C22 C23 115.2(3) . . ? O34 C431 H30A 109.5 . . ? O34 C431 H30B 109.5 . . ? H30A C431 H30B 109.5 . . ? O34 C431 H30C 109.5 . . ? H30A C431 H30C 109.5 . . ? H30B C431 H30C 109.5 . . ? C92 C93 C94 121.2(3) . . ? C92 C93 H31A 119.4 . . ? C94 C93 H31A 119.4 . . ? O35 C34 O34 118.3(3) . . ? O35 C34 C33 126.3(3) . . ? O34 C34 C33 115.4(3) . . ? O22 C221 H34A 109.5 . . ? O22 C221 H34B 109.5 . . ? H34A C221 H34B 109.5 . . ? O22 C221 H34C 109.5 . . ? H34A C221 H34C 109.5 . . ? H34B C221 H34C 109.5 . . ? O24 C241 H36A 109.5 . . ? O24 C241 H36B 109.5 . . ? H36A C241 H36B 109.5 . . ? O24 C241 H36C 109.5 . . ? H36A C241 H36C 109.5 . . ? H36B C241 H36C 109.5 . . ? C93 C92 C97 117.6(3) . . ? C93 C92 C91 121.1(3) . . ? C97 C92 C91 121.3(3) . . ? C94 C95 C96 119.5(3) . . ? C94 C95 H41A 120.2 . . ? C96 C95 H41A 120.2 . . ? O42 C421 H42A 109.5 . . ? O42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? O42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? O31 C32 O32 118.1(3) . . ? O31 C32 C33 126.5(3) . . ? O32 C32 C33 115.4(3) . . ? C22 C23 C24 119.1(3) . . ? C22 C23 H47A 120.4 . . ? C24 C23 H47A 120.4 . . ? O44 C441 H48A 109.5 . . ? O44 C441 H48B 109.5 . . ? H48A C441 H48B 109.5 . . ? O44 C441 H48C 109.5 . . ? H48A C441 H48C 109.5 . . ? H48B C441 H48C 109.5 . . ? O14 C141 H50A 109.5 . . ? O14 C141 H50B 109.5 . . ? H50A C141 H50B 109.5 . . ? O14 C141 H50C 109.5 . . ? H50A C141 H50C 109.5 . . ? H50B C141 H50C 109.5 . . ? C92 C91 H53A 109.5 . . ? C92 C91 H53B 109.5 . . ? H53A C91 H53B 109.5 . . ? C92 C91 H53C 109.5 . . ? H53A C91 H53C 109.5 . . ? H53B C91 H53C 109.5 . . ? C32 C33 C34 119.3(3) . . ? C32 C33 H54A 120.3 . . ? C34 C33 H54A 120.3 . . ? C97 C96 C95 120.2(3) . . ? C97 C96 H55A 119.9 . . ? C95 C96 H55A 119.9 . . ? O32 C321 H16A 109.5 . . ? O32 C321 H16B 109.5 . . ? H16A C321 H16B 109.5 . . ? O32 C321 H16C 109.5 . . ? H16A C321 H16C 109.5 . . ? H16B C321 H16C 109.5 . . ? O12 C121 H81A 109.5 . . ? O12 C121 H81B 109.5 . . ? H81A C121 H81B 109.5 . . ? O12 C121 H81C 109.5 . . ? H81A C121 H81C 109.5 . . ? H81B C121 H81C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O11 Hf1 O41 C20 -138.5(3) . . . . ? O25 Hf1 O41 C20 29.8(3) . . . . ? O45 Hf1 O41 C20 -21.3(3) . . . . ? O31 Hf1 O41 C20 137.4(3) . . . . ? O21 Hf1 O41 C20 176.9(3) . . . . ? O15 Hf1 O41 C20 -78.5(3) . . . . ? O35 Hf1 O41 C20 59.4(3) . . . . ? O11 Hf1 O35 C34 24.8(3) . . . . ? O25 Hf1 O35 C34 -144.2(3) . . . . ? O45 Hf1 O35 C34 131.8(3) . . . . ? O31 Hf1 O35 C34 -25.0(3) . . . . ? O41 Hf1 O35 C34 54.2(3) . . . . ? O21 Hf1 O35 C34 -83.0(3) . . . . ? O15 Hf1 O35 C34 175.2(2) . . . . ? O11 Hf1 O45 C44 84.0(3) . . . . ? O25 Hf1 O45 C44 -131.2(3) . . . . ? O31 Hf1 O45 C44 -17.4(3) . . . . ? O41 Hf1 O45 C44 20.2(3) . . . . ? O21 Hf1 O45 C44 179.4(2) . . . . ? O15 Hf1 O45 C44 150.5(3) . . . . ? O35 Hf1 O45 C44 -58.7(3) . . . . ? O11 Hf1 O31 C32 -127.9(3) . . . . ? O25 Hf1 O31 C32 87.1(3) . . . . ? O45 Hf1 O31 C32 -17.1(4) . . . . ? O41 Hf1 O31 C32 -54.5(3) . . . . ? O21 Hf1 O31 C32 152.4(3) . . . . ? O15 Hf1 O31 C32 -177.9(2) . . . . ? O35 Hf1 O31 C32 24.7(3) . . . . ? O11 Hf1 O15 C14 -25.4(3) . . . . ? O25 Hf1 O15 C14 132.9(3) . . . . ? O45 Hf1 O15 C14 -142.6(3) . . . . ? O31 Hf1 O15 C14 25.8(3) . . . . ? O41 Hf1 O15 C14 -83.4(3) . . . . ? O21 Hf1 O15 C14 54.5(3) . . . . ? O35 Hf1 O15 C14 172.3(2) . . . . ? O25 Hf1 O11 C12 -13.7(4) . . . . ? O45 Hf1 O11 C12 87.9(3) . . . . ? O31 Hf1 O11 C12 -127.2(3) . . . . ? O41 Hf1 O11 C12 154.1(3) . . . . ? O21 Hf1 O11 C12 -54.9(3) . . . . ? O15 Hf1 O11 C12 24.3(3) . . . . ? O35 Hf1 O11 C12 -175.8(2) . . . . ? O11 Hf1 O25 C24 -17.5(3) . . . . ? O45 Hf1 O25 C24 -128.5(3) . . . . ? O31 Hf1 O25 C24 86.2(3) . . . . ? O41 Hf1 O25 C24 -178.3(2) . . . . ? O21 Hf1 O25 C24 23.9(3) . . . . ? O15 Hf1 O25 C24 -55.5(3) . . . . ? O35 Hf1 O25 C24 151.3(3) . . . . ? O11 Hf1 O21 C22 132.7(3) . . . . ? O25 Hf1 O21 C22 -24.0(3) . . . . ? O45 Hf1 O21 C22 26.5(3) . . . . ? O31 Hf1 O21 C22 -143.3(3) . . . . ? O41 Hf1 O21 C22 175.8(2) . . . . ? O15 Hf1 O21 C22 54.6(3) . . . . ? O35 Hf1 O21 C22 -82.8(3) . . . . ? Hf1 O15 C14 O14 -163.0(2) . . . . ? Hf1 O15 C14 C13 19.0(5) . . . . ? O15 C14 O14 C141 3.7(4) . . . . ? C13 C14 O14 C141 -178.1(3) . . . . ? Hf1 O41 C20 O42 -165.25(19) . . . . ? Hf1 O41 C20 C43 15.8(5) . . . . ? C421 O42 C20 O41 4.2(4) . . . . ? C421 O42 C20 C43 -176.7(3) . . . . ? C44 C43 C20 O41 2.6(5) . . . . ? C44 C43 C20 O42 -176.4(3) . . . . ? Hf1 O11 C12 O12 165.0(2) . . . . ? Hf1 O11 C12 C13 -16.7(5) . . . . ? C121 O12 C12 O11 0.7(5) . . . . ? C121 O12 C12 C13 -177.8(3) . . . . ? O11 C12 C13 C14 -3.9(5) . . . . ? O12 C12 C13 C14 174.4(3) . . . . ? O15 C14 C13 C12 2.4(5) . . . . ? O14 C14 C13 C12 -175.6(3) . . . . ? Hf1 O45 C44 O44 167.6(2) . . . . ? Hf1 O45 C44 C43 -13.7(5) . . . . ? C441 O44 C44 O45 -1.7(4) . . . . ? C441 O44 C44 C43 179.6(3) . . . . ? C20 C43 C44 O45 -3.7(5) . . . . ? C20 C43 C44 O44 175.0(3) . . . . ? Hf1 O25 C24 O24 164.13(19) . . . . ? Hf1 O25 C24 C23 -17.2(5) . . . . ? C241 O24 C24 O25 -2.6(4) . . . . ? C241 O24 C24 C23 178.6(3) . . . . ? Hf1 O21 C22 O22 -162.62(18) . . . . ? Hf1 O21 C22 C23 17.9(5) . . . . ? C221 O22 C22 O21 2.5(4) . . . . ? C221 O22 C22 C23 -177.9(3) . . . . ? C95 C94 C93 C92 1.0(6) . . . . ? Hf1 O35 C34 O34 -163.64(19) . . . . ? Hf1 O35 C34 C33 17.9(5) . . . . ? C431 O34 C34 O35 -0.3(4) . . . . ? C431 O34 C34 C33 178.3(3) . . . . ? C94 C93 C92 C97 -0.6(5) . . . . ? C94 C93 C92 C91 -178.9(4) . . . . ? C96 C97 C92 C93 0.0(5) . . . . ? C96 C97 C92 C91 178.3(4) . . . . ? C93 C94 C95 C96 -0.8(5) . . . . ? Hf1 O31 C32 O32 163.3(2) . . . . ? Hf1 O31 C32 C33 -17.3(5) . . . . ? C321 O32 C32 O31 -3.0(4) . . . . ? C321 O32 C32 C33 177.5(3) . . . . ? O21 C22 C23 C24 2.2(5) . . . . ? O22 C22 C23 C24 -177.4(3) . . . . ? O25 C24 C23 C22 -2.8(5) . . . . ? O24 C24 C23 C22 175.9(3) . . . . ? O31 C32 C33 C34 -3.9(5) . . . . ? O32 C32 C33 C34 175.5(3) . . . . ? O35 C34 C33 C32 3.4(5) . . . . ? O34 C34 C33 C32 -175.1(3) . . . . ? C92 C97 C96 C95 0.2(6) . . . . ? C94 C95 C96 C97 0.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 2.731 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.108 #=================================END data_cvd185 _database_code_depnum_ccdc_archive 'CCDC 692632' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H52 Hf O16' _chemical_formula_weight 907.26 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' Hf Hf -0.5830 6.1852 '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 15.3042(7) _cell_length_b 18.4262(8) _cell_length_c 15.8807(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.421(4) _cell_angle_gamma 90.00 _cell_volume 3975.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2100 _cell_measurement_theta_min 2.565 _cell_measurement_theta_max 27.499 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.516 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1848 _exptl_absorpt_coefficient_mu 2.692 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.350 _exptl_absorpt_correction_T_max 0.430 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32128 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_sigmaI/netI 0.0258 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6982 _reflns_number_gt 5379 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0203P)^2^+13.2862P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6982 _refine_ls_number_parameters 469 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0510 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0723 _refine_ls_wR_factor_gt 0.0620 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _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 Hf1 Hf 0.254718(13) 0.890089(9) 0.746876(13) 0.02340(6) Uani 1 1 d . . . O31 O 0.2310(2) 0.98481(16) 0.8160(2) 0.0272(7) Uani 1 1 d . . . O15 O 0.2615(2) 0.98077(16) 0.6624(2) 0.0267(7) Uani 1 1 d . . . O25 O 0.1798(2) 0.79342(16) 0.6683(2) 0.0267(7) Uani 1 1 d . . . O41 O 0.3438(2) 0.80048(16) 0.8367(2) 0.0285(7) Uani 1 1 d . . . O11 O 0.3418(2) 0.85008(15) 0.6802(2) 0.0262(7) Uani 1 1 d . . . O35 O 0.1837(2) 0.84823(16) 0.8259(2) 0.0281(7) Uani 1 1 d . . . O45 O 0.3955(2) 0.93846(16) 0.8368(2) 0.0260(7) Uani 1 1 d . . . O44 O 0.5550(2) 0.96378(17) 0.9216(2) 0.0323(7) Uani 1 1 d . . . O14 O 0.3203(2) 1.06692(16) 0.6020(2) 0.0340(8) Uani 1 1 d . . . C14 C 0.3203(3) 0.9980(2) 0.6301(3) 0.0272(10) Uani 1 1 d . . . O21 O 0.1058(2) 0.92596(16) 0.6542(2) 0.0291(7) Uani 1 1 d . . . O32 O 0.1621(3) 1.06777(18) 0.8696(3) 0.0419(9) Uani 1 1 d . . . O12 O 0.4601(2) 0.84065(17) 0.6340(2) 0.0337(7) Uani 1 1 d . . . O42 O 0.4692(2) 0.72373(17) 0.9166(2) 0.0359(8) Uani 1 1 d . . . C32 C 0.1754(3) 0.9981(2) 0.8526(3) 0.0295(10) Uani 1 1 d . . . O34 O 0.0991(2) 0.82811(19) 0.9070(3) 0.0419(9) Uani 1 1 d . . . C22 C 0.0243(3) 0.8944(3) 0.6112(3) 0.0331(11) Uani 1 1 d . . . C13 C 0.3865(3) 0.9527(2) 0.6191(3) 0.0323(11) Uani 1 1 d . . . H2A H 0.4272 0.9707 0.5932 0.039 Uiso 1 1 calc R . . C44 C 0.4814(3) 0.9153(2) 0.8872(3) 0.0267(10) Uani 1 1 d . . . C34 C 0.1383(3) 0.8745(3) 0.8680(3) 0.0313(11) Uani 1 1 d . . . C33 C 0.1256(3) 0.9476(3) 0.8799(3) 0.0340(11) Uani 1 1 d . . . H8A H 0.0840 0.9628 0.9061 0.041 Uiso 1 1 calc R . . C12 C 0.3925(3) 0.8808(2) 0.6462(3) 0.0270(10) Uani 1 1 d . . . C43 C 0.5070(3) 0.8435(2) 0.9119(3) 0.0306(10) Uani 1 1 d . . . H5A H 0.5743 0.8305 0.9475 0.037 Uiso 1 1 calc R . . C42 C 0.4348(3) 0.7906(2) 0.8849(3) 0.0271(10) Uani 1 1 d . . . O24 O 0.0687(2) 0.70400(17) 0.6090(2) 0.0377(8) Uani 1 1 d . . . O22 O -0.0579(2) 0.93535(19) 0.5737(3) 0.0531(10) Uani 1 1 d . . . C141 C 0.2603(3) 1.1187(2) 0.6204(3) 0.0323(10) Uani 1 1 d . . . H31A H 0.2823 1.1227 0.6894 0.039 Uiso 1 1 calc R . . H31B H 0.1904 1.1036 0.5887 0.039 Uiso 1 1 calc R . . C441 C 0.5300(3) 1.0391(3) 0.8934(4) 0.0344(11) Uani 1 1 d . . . H71A H 0.4808 1.0569 0.9127 0.041 Uiso 1 1 calc R . . H71B H 0.5023 1.0441 0.8237 0.041 Uiso 1 1 calc R . . C23 C 0.0100(3) 0.8201(3) 0.5972(4) 0.0380(12) Uani 1 1 d . . . H11A H -0.0548 0.8006 0.5670 0.046 Uiso 1 1 calc R . . C24 C 0.0905(3) 0.7748(2) 0.6273(3) 0.0300(10) Uani 1 1 d . . . C421 C 0.4016(4) 0.6634(3) 0.8865(4) 0.0369(11) Uani 1 1 d . . . H81A H 0.3335 0.6813 0.8639 0.044 Uiso 1 1 calc R . . H81B H 0.4172 0.6303 0.9407 0.044 Uiso 1 1 calc R . . C121 C 0.4804(4) 0.7689(3) 0.6760(4) 0.0373(12) Uani 1 1 d . . . H41A H 0.4213 0.7377 0.6451 0.045 Uiso 1 1 calc R . . H41B H 0.4995 0.7719 0.7446 0.045 Uiso 1 1 calc R . . C122 C 0.5630(4) 0.7379(3) 0.6616(4) 0.0415(12) Uani 1 1 d . . . H42A H 0.5792 0.6893 0.6897 0.062 Uiso 1 1 calc R . . H42B H 0.6209 0.7693 0.6922 0.062 Uiso 1 1 calc R . . H42C H 0.5429 0.7347 0.5936 0.062 Uiso 1 1 calc R . . C241 C 0.1483(4) 0.6525(3) 0.6454(4) 0.0400(12) Uani 1 1 d . . . H15A H 0.1880 0.6582 0.7149 0.048 Uiso 1 1 calc R . . H15B H 0.1918 0.6599 0.6154 0.048 Uiso 1 1 calc R . . C341 C 0.1106(4) 0.7509(3) 0.8954(4) 0.0430(13) Uani 1 1 d . . . H12A H 0.1004 0.7415 0.8302 0.052 Uiso 1 1 calc R . . H12B H 0.0600 0.7235 0.9047 0.052 Uiso 1 1 calc R . . C442 C 0.6239(4) 1.0812(3) 0.9426(4) 0.0402(12) Uani 1 1 d . . . H72A H 0.6109 1.1326 0.9259 0.060 Uiso 1 1 calc R . . H72B H 0.6717 1.0629 0.9229 0.060 Uiso 1 1 calc R . . H72C H 0.6504 1.0755 1.0114 0.060 Uiso 1 1 calc R . . C321 C 0.2096(5) 1.1222(3) 0.8393(5) 0.0547(16) Uani 1 1 d . . . H11B H 0.1917 1.1152 0.7715 0.066 Uiso 1 1 calc R . . H11C H 0.2820 1.1182 0.8768 0.066 Uiso 1 1 calc R . . C342 C 0.2111(4) 0.7249(3) 0.9653(4) 0.0474(14) Uani 1 1 d . . . H12C H 0.2169 0.6729 0.9560 0.071 Uiso 1 1 calc R . . H12D H 0.2208 0.7334 1.0300 0.071 Uiso 1 1 calc R . . H12E H 0.2612 0.7515 0.9556 0.071 Uiso 1 1 calc R . . C221 C -0.0489(4) 1.0139(3) 0.5856(5) 0.0607(18) Uani 1 1 d . . . H16A H 0.0208 1.0285 0.6101 0.073 Uiso 1 1 calc R . . H16B H -0.0879 1.0382 0.5238 0.073 Uiso 1 1 calc R . . C142 C 0.2730(4) 1.1901(3) 0.5811(4) 0.0463(13) Uani 1 1 d . . . H32A H 0.2333 1.2274 0.5916 0.069 Uiso 1 1 calc R . . H32B H 0.2514 1.1852 0.5129 0.069 Uiso 1 1 calc R . . H32C H 0.3425 1.2043 0.6132 0.069 Uiso 1 1 calc R . . C242 C 0.1025(4) 0.5782(3) 0.6222(4) 0.0475(14) Uani 1 1 d . . . H15C H 0.1544 0.5413 0.6460 0.071 Uiso 1 1 calc R . . H15D H 0.0637 0.5732 0.5533 0.071 Uiso 1 1 calc R . . H15E H 0.0596 0.5717 0.6521 0.071 Uiso 1 1 calc R . . C422 C 0.4093(4) 0.6234(3) 0.8087(4) 0.0566(16) Uani 1 1 d . . . H82A H 0.3637 0.5822 0.7888 0.085 Uiso 1 1 calc R . . H82B H 0.4768 0.6056 0.8314 0.085 Uiso 1 1 calc R . . H82C H 0.3926 0.6561 0.7548 0.085 Uiso 1 1 calc R . . C222 C -0.0842(7) 1.0346(4) 0.6507(6) 0.091(3) Uani 1 1 d . . . H16C H -0.0790 1.0874 0.6593 0.136 Uiso 1 1 calc R . . H16D H -0.0448 1.0108 0.7119 0.136 Uiso 1 1 calc R . . H16E H -0.1532 1.0200 0.6259 0.136 Uiso 1 1 calc R . . C93 C 0.6814(4) 0.9225(3) 0.7812(4) 0.0414(12) Uani 1 1 d . . . H99A H 0.6164 0.9402 0.7603 0.050 Uiso 1 1 calc R . . C94 C 0.7379(4) 0.9083(3) 0.8756(4) 0.0449(13) Uani 1 1 d . . . H99B H 0.7120 0.9162 0.9188 0.054 Uiso 1 1 calc R . . C92 C 0.7152(4) 0.9122(3) 0.7150(5) 0.0510(15) Uani 1 1 d . . . C91 C 0.6503(5) 0.9275(4) 0.6111(5) 0.074(2) Uani 1 1 d . . . H99C H 0.5867 0.9463 0.6022 0.111 Uiso 1 1 calc R . . H99D H 0.6401 0.8827 0.5747 0.111 Uiso 1 1 calc R . . H99E H 0.6821 0.9637 0.5891 0.111 Uiso 1 1 calc R . . C95 C 0.8324(4) 0.8824(3) 0.9080(5) 0.0544(15) Uani 1 1 d . . . H99F H 0.8723 0.8730 0.9736 0.065 Uiso 1 1 calc R . . C97 C 0.8104(5) 0.8851(3) 0.7488(6) 0.0639(19) Uani 1 1 d . . . H99G H 0.8363 0.8766 0.7056 0.077 Uiso 1 1 calc R . . C96 C 0.8678(4) 0.8704(3) 0.8442(6) 0.069(2) Uani 1 1 d . . . H99H H 0.9325 0.8518 0.8656 0.083 Uiso 1 1 calc R . . C322 C 0.1769(7) 1.1929(4) 0.8535(8) 0.114(4) Uani 1 1 d . . . H11D H 0.2093 1.2308 0.8345 0.172 Uiso 1 1 calc R . . H11E H 0.1941 1.1990 0.9206 0.172 Uiso 1 1 calc R . . H11F H 0.1054 1.1967 0.8150 0.172 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 Hf1 0.02158(10) 0.01862(9) 0.02632(10) 0.00054(9) 0.00788(7) -0.00055(8) O31 0.0280(16) 0.0230(16) 0.0320(17) -0.0036(13) 0.0150(15) -0.0015(13) O15 0.0254(16) 0.0242(17) 0.0305(17) 0.0030(13) 0.0129(14) 0.0029(13) O25 0.0255(16) 0.0234(16) 0.0293(17) -0.0018(13) 0.0110(14) -0.0019(13) O41 0.0261(17) 0.0232(16) 0.0344(18) 0.0040(14) 0.0125(15) -0.0001(13) O11 0.0293(16) 0.0211(16) 0.0299(17) -0.0020(13) 0.0151(14) -0.0019(13) O35 0.0285(16) 0.0249(17) 0.0321(18) 0.0019(13) 0.0151(15) 0.0018(13) O45 0.0217(15) 0.0236(16) 0.0280(17) -0.0001(13) 0.0076(14) 0.0011(12) O44 0.0241(16) 0.0281(18) 0.0382(19) -0.0013(15) 0.0088(15) -0.0029(13) O14 0.0389(18) 0.0239(18) 0.047(2) 0.0082(15) 0.0261(17) 0.0051(14) C14 0.026(2) 0.027(2) 0.026(2) 0.0021(19) 0.010(2) -0.0024(19) O21 0.0197(15) 0.0261(17) 0.0334(18) 0.0022(14) 0.0052(14) -0.0021(13) O32 0.050(2) 0.0260(19) 0.063(2) 0.0008(16) 0.038(2) 0.0053(16) O12 0.0370(18) 0.0255(17) 0.047(2) 0.0043(15) 0.0263(16) 0.0053(14) O42 0.0318(18) 0.0233(18) 0.045(2) 0.0061(15) 0.0117(16) 0.0053(14) C32 0.027(2) 0.029(3) 0.029(3) 0.002(2) 0.011(2) 0.0061(19) O34 0.0412(19) 0.037(2) 0.060(2) 0.0143(18) 0.0347(19) 0.0085(16) C22 0.022(2) 0.036(3) 0.035(3) 0.003(2) 0.008(2) 0.001(2) C13 0.034(3) 0.029(3) 0.041(3) 0.009(2) 0.024(2) 0.002(2) C44 0.025(2) 0.030(2) 0.027(2) -0.0020(19) 0.013(2) -0.0016(19) C34 0.021(2) 0.037(3) 0.034(3) 0.009(2) 0.011(2) 0.0042(19) C33 0.031(3) 0.034(3) 0.044(3) 0.006(2) 0.023(2) 0.008(2) C12 0.024(2) 0.030(3) 0.028(2) -0.002(2) 0.012(2) 0.0015(19) C43 0.023(2) 0.029(3) 0.035(3) 0.002(2) 0.009(2) 0.0025(19) C42 0.031(2) 0.026(2) 0.028(2) 0.0056(19) 0.016(2) 0.0069(19) O24 0.0308(18) 0.0240(18) 0.054(2) -0.0060(16) 0.0154(17) -0.0060(14) O22 0.0245(18) 0.033(2) 0.082(3) -0.003(2) 0.0082(19) 0.0023(15) C141 0.032(2) 0.027(3) 0.040(3) -0.001(2) 0.017(2) 0.001(2) C441 0.031(2) 0.029(3) 0.039(3) 0.001(2) 0.012(2) -0.003(2) C23 0.022(2) 0.029(3) 0.053(3) -0.007(2) 0.008(2) -0.008(2) C24 0.030(3) 0.026(3) 0.036(3) -0.005(2) 0.017(2) -0.008(2) C421 0.040(3) 0.025(3) 0.047(3) 0.006(2) 0.021(3) 0.001(2) C121 0.039(3) 0.025(3) 0.051(3) 0.001(2) 0.023(3) 0.004(2) C122 0.039(3) 0.041(3) 0.044(3) 0.000(2) 0.018(3) 0.009(2) C241 0.038(3) 0.025(3) 0.056(3) -0.001(2) 0.022(3) 0.002(2) C341 0.044(3) 0.032(3) 0.062(4) 0.009(3) 0.032(3) 0.000(2) C442 0.034(3) 0.030(3) 0.049(3) 0.004(2) 0.013(2) -0.005(2) C321 0.066(4) 0.030(3) 0.090(5) 0.001(3) 0.054(4) 0.000(3) C342 0.057(3) 0.045(3) 0.050(3) 0.015(3) 0.033(3) 0.016(3) C221 0.037(3) 0.039(3) 0.097(5) 0.008(3) 0.022(3) 0.010(3) C142 0.051(3) 0.027(3) 0.061(4) 0.008(2) 0.027(3) 0.004(2) C242 0.055(3) 0.026(3) 0.061(4) 0.000(3) 0.027(3) -0.001(2) C422 0.058(4) 0.048(4) 0.070(4) -0.019(3) 0.036(3) -0.010(3) C222 0.148(8) 0.046(4) 0.110(6) -0.002(4) 0.088(6) -0.005(5) C93 0.034(3) 0.036(3) 0.053(3) 0.000(2) 0.019(3) 0.002(2) C94 0.040(3) 0.034(3) 0.062(4) 0.000(3) 0.024(3) -0.004(2) C92 0.054(3) 0.040(3) 0.074(4) -0.019(3) 0.042(3) -0.017(3) C91 0.080(5) 0.087(5) 0.072(5) -0.015(4) 0.049(4) -0.023(4) C95 0.035(3) 0.037(3) 0.085(5) 0.010(3) 0.022(3) 0.000(2) C97 0.064(4) 0.040(3) 0.118(6) -0.022(4) 0.067(5) -0.013(3) C96 0.032(3) 0.039(4) 0.136(7) 0.000(4) 0.038(4) 0.002(3) C322 0.158(9) 0.039(4) 0.208(11) 0.003(5) 0.137(9) 0.004(5) _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 Hf1 O35 2.146(3) . ? Hf1 O45 2.154(3) . ? Hf1 O21 2.170(3) . ? Hf1 O25 2.174(3) . ? Hf1 O15 2.176(3) . ? Hf1 O11 2.178(3) . ? Hf1 O31 2.180(3) . ? Hf1 O41 2.197(3) . ? O31 C32 1.256(5) . ? O15 C14 1.264(5) . ? O25 C24 1.260(5) . ? O41 C42 1.256(5) . ? O11 C12 1.265(5) . ? O35 C34 1.262(5) . ? O45 C44 1.258(5) . ? O44 C44 1.342(5) . ? O44 C441 1.455(5) . ? O14 C14 1.346(5) . ? O14 C141 1.444(5) . ? C14 C13 1.386(6) . ? O21 C22 1.255(5) . ? O32 C32 1.346(5) . ? O32 C321 1.445(6) . ? O12 C12 1.356(5) . ? O12 C121 1.450(5) . ? O42 C42 1.343(5) . ? O42 C421 1.443(6) . ? C32 C33 1.393(6) . ? O34 C34 1.347(5) . ? O34 C341 1.456(6) . ? C22 O22 1.348(5) . ? C22 C23 1.388(7) . ? C13 C12 1.382(6) . ? C13 H2A 0.9500 . ? C44 C43 1.384(6) . ? C34 C33 1.386(7) . ? C33 H8A 0.9500 . ? C43 C42 1.386(6) . ? C43 H5A 0.9500 . ? O24 C24 1.345(5) . ? O24 C241 1.440(6) . ? O22 C221 1.458(7) . ? C141 C142 1.507(6) . ? C141 H31A 0.9900 . ? C141 H31B 0.9900 . ? C441 C442 1.497(6) . ? C441 H71A 0.9900 . ? C441 H71B 0.9900 . ? C23 C24 1.379(7) . ? C23 H11A 0.9500 . ? C421 C422 1.488(7) . ? C421 H81A 0.9900 . ? C421 H81B 0.9900 . ? C121 C122 1.497(6) . ? C121 H41A 0.9900 . ? C121 H41B 0.9900 . ? C122 H42A 0.9800 . ? C122 H42B 0.9800 . ? C122 H42C 0.9800 . ? C241 C242 1.504(7) . ? C241 H15A 0.9900 . ? C241 H15B 0.9900 . ? C341 C342 1.501(7) . ? C341 H12A 0.9900 . ? C341 H12B 0.9900 . ? C442 H72A 0.9800 . ? C442 H72B 0.9800 . ? C442 H72C 0.9800 . ? C321 C322 1.449(8) . ? C321 H11B 0.9900 . ? C321 H11C 0.9900 . ? C342 H12C 0.9800 . ? C342 H12D 0.9800 . ? C342 H12E 0.9800 . ? C221 C222 1.423(9) . ? C221 H16A 0.9900 . ? C221 H16B 0.9900 . ? C142 H32A 0.9800 . ? C142 H32B 0.9800 . ? C142 H32C 0.9800 . ? C242 H15C 0.9800 . ? C242 H15D 0.9800 . ? C242 H15E 0.9800 . ? C422 H82A 0.9800 . ? C422 H82B 0.9800 . ? C422 H82C 0.9800 . ? C222 H16C 0.9800 . ? C222 H16D 0.9800 . ? C222 H16E 0.9800 . ? C93 C94 1.368(8) . ? C93 C92 1.380(7) . ? C93 H99A 0.9500 . ? C94 C95 1.377(7) . ? C94 H99B 0.9500 . ? C92 C97 1.393(9) . ? C92 C91 1.510(9) . ? C91 H99C 0.9800 . ? C91 H99D 0.9800 . ? C91 H99E 0.9800 . ? C95 C96 1.370(9) . ? C95 H99F 0.9500 . ? C97 C96 1.384(10) . ? C97 H99G 0.9500 . ? C96 H99H 0.9500 . ? C322 H11D 0.9800 . ? C322 H11E 0.9800 . ? C322 H11F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O35 Hf1 O45 112.44(11) . . ? O35 Hf1 O21 81.34(11) . . ? O45 Hf1 O21 137.81(11) . . ? O35 Hf1 O25 76.47(11) . . ? O45 Hf1 O25 145.26(11) . . ? O21 Hf1 O25 75.44(11) . . ? O35 Hf1 O15 144.86(11) . . ? O45 Hf1 O15 76.93(11) . . ? O21 Hf1 O15 71.44(11) . . ? O25 Hf1 O15 115.94(11) . . ? O35 Hf1 O11 138.67(10) . . ? O45 Hf1 O11 79.25(11) . . ? O21 Hf1 O11 117.42(11) . . ? O25 Hf1 O11 73.90(11) . . ? O15 Hf1 O11 75.28(11) . . ? O35 Hf1 O31 75.31(11) . . ? O45 Hf1 O31 71.48(11) . . ? O21 Hf1 O31 74.38(11) . . ? O25 Hf1 O31 141.15(11) . . ? O15 Hf1 O31 76.25(11) . . ? O11 Hf1 O31 142.88(11) . . ? O35 Hf1 O41 71.33(11) . . ? O45 Hf1 O41 75.44(11) . . ? O21 Hf1 O41 144.38(11) . . ? O25 Hf1 O41 76.27(11) . . ? O15 Hf1 O41 141.82(11) . . ? O11 Hf1 O41 74.09(11) . . ? O31 Hf1 O41 118.17(11) . . ? C32 O31 Hf1 134.0(3) . . ? C14 O15 Hf1 133.5(3) . . ? C24 O25 Hf1 132.8(3) . . ? C42 O41 Hf1 133.4(3) . . ? C12 O11 Hf1 133.5(3) . . ? C34 O35 Hf1 136.3(3) . . ? C44 O45 Hf1 135.6(3) . . ? C44 O44 C441 117.2(3) . . ? C14 O14 C141 117.3(3) . . ? O15 C14 O14 118.8(4) . . ? O15 C14 C13 126.7(4) . . ? O14 C14 C13 114.5(4) . . ? C22 O21 Hf1 134.3(3) . . ? C32 O32 C321 116.7(4) . . ? C12 O12 C121 116.7(3) . . ? C42 O42 C421 119.0(4) . . ? O31 C32 O32 118.4(4) . . ? O31 C32 C33 126.7(4) . . ? O32 C32 C33 114.9(4) . . ? C34 O34 C341 117.2(4) . . ? O21 C22 O22 118.2(4) . . ? O21 C22 C23 126.0(4) . . ? O22 C22 C23 115.7(4) . . ? C12 C13 C14 119.1(4) . . ? C12 C13 H2A 120.5 . . ? C14 C13 H2A 120.5 . . ? O45 C44 O44 118.0(4) . . ? O45 C44 C43 125.5(4) . . ? O44 C44 C43 116.5(4) . . ? O35 C34 O34 118.1(4) . . ? O35 C34 C33 126.2(4) . . ? O34 C34 C33 115.7(4) . . ? C34 C33 C32 118.5(4) . . ? C34 C33 H8A 120.8 . . ? C32 C33 H8A 120.8 . . ? O11 C12 O12 118.3(4) . . ? O11 C12 C13 126.6(4) . . ? O12 C12 C13 115.1(4) . . ? C44 C43 C42 120.2(4) . . ? C44 C43 H5A 119.9 . . ? C42 C43 H5A 119.9 . . ? O41 C42 O42 119.7(4) . . ? O41 C42 C43 126.1(4) . . ? O42 C42 C43 114.2(4) . . ? C24 O24 C241 118.2(4) . . ? C22 O22 C221 119.0(4) . . ? O14 C141 C142 106.2(4) . . ? O14 C141 H31A 110.5 . . ? C142 C141 H31A 110.5 . . ? O14 C141 H31B 110.5 . . ? C142 C141 H31B 110.5 . . ? H31A C141 H31B 108.7 . . ? O44 C441 C442 106.3(4) . . ? O44 C441 H71A 110.5 . . ? C442 C441 H71A 110.5 . . ? O44 C441 H71B 110.5 . . ? C442 C441 H71B 110.5 . . ? H71A C441 H71B 108.7 . . ? C24 C23 C22 119.4(4) . . ? C24 C23 H11A 120.3 . . ? C22 C23 H11A 120.3 . . ? O25 C24 O24 118.6(4) . . ? O25 C24 C23 126.7(4) . . ? O24 C24 C23 114.8(4) . . ? O42 C421 C422 109.7(4) . . ? O42 C421 H81A 109.7 . . ? C422 C421 H81A 109.7 . . ? O42 C421 H81B 109.7 . . ? C422 C421 H81B 109.7 . . ? H81A C421 H81B 108.2 . . ? O12 C121 C122 107.2(4) . . ? O12 C121 H41A 110.3 . . ? C122 C121 H41A 110.3 . . ? O12 C121 H41B 110.3 . . ? C122 C121 H41B 110.3 . . ? H41A C121 H41B 108.5 . . ? C121 C122 H42A 109.5 . . ? C121 C122 H42B 109.5 . . ? H42A C122 H42B 109.5 . . ? C121 C122 H42C 109.5 . . ? H42A C122 H42C 109.5 . . ? H42B C122 H42C 109.5 . . ? O24 C241 C242 106.8(4) . . ? O24 C241 H15A 110.4 . . ? C242 C241 H15A 110.4 . . ? O24 C241 H15B 110.4 . . ? C242 C241 H15B 110.4 . . ? H15A C241 H15B 108.6 . . ? O34 C341 C342 111.1(4) . . ? O34 C341 H12A 109.4 . . ? C342 C341 H12A 109.4 . . ? O34 C341 H12B 109.4 . . ? C342 C341 H12B 109.4 . . ? H12A C341 H12B 108.0 . . ? C441 C442 H72A 109.5 . . ? C441 C442 H72B 109.5 . . ? H72A C442 H72B 109.5 . . ? C441 C442 H72C 109.5 . . ? H72A C442 H72C 109.5 . . ? H72B C442 H72C 109.5 . . ? O32 C321 C322 108.1(5) . . ? O32 C321 H11B 110.1 . . ? C322 C321 H11B 110.1 . . ? O32 C321 H11C 110.1 . . ? C322 C321 H11C 110.1 . . ? H11B C321 H11C 108.4 . . ? C341 C342 H12C 109.5 . . ? C341 C342 H12D 109.5 . . ? H12C C342 H12D 109.5 . . ? C341 C342 H12E 109.5 . . ? H12C C342 H12E 109.5 . . ? H12D C342 H12E 109.5 . . ? C222 C221 O22 108.4(5) . . ? C222 C221 H16A 110.0 . . ? O22 C221 H16A 110.0 . . ? C222 C221 H16B 110.0 . . ? O22 C221 H16B 110.0 . . ? H16A C221 H16B 108.4 . . ? C141 C142 H32A 109.5 . . ? C141 C142 H32B 109.5 . . ? H32A C142 H32B 109.5 . . ? C141 C142 H32C 109.5 . . ? H32A C142 H32C 109.5 . . ? H32B C142 H32C 109.5 . . ? C241 C242 H15C 109.5 . . ? C241 C242 H15D 109.5 . . ? H15C C242 H15D 109.5 . . ? C241 C242 H15E 109.5 . . ? H15C C242 H15E 109.5 . . ? H15D C242 H15E 109.5 . . ? C421 C422 H82A 109.5 . . ? C421 C422 H82B 109.5 . . ? H82A C422 H82B 109.5 . . ? C421 C422 H82C 109.5 . . ? H82A C422 H82C 109.5 . . ? H82B C422 H82C 109.5 . . ? C221 C222 H16C 109.5 . . ? C221 C222 H16D 109.5 . . ? H16C C222 H16D 109.5 . . ? C221 C222 H16E 109.5 . . ? H16C C222 H16E 109.5 . . ? H16D C222 H16E 109.5 . . ? C94 C93 C92 122.6(5) . . ? C94 C93 H99A 118.7 . . ? C92 C93 H99A 118.7 . . ? C93 C94 C95 120.1(6) . . ? C93 C94 H99B 120.0 . . ? C95 C94 H99B 120.0 . . ? C93 C92 C97 116.6(6) . . ? C93 C92 C91 121.2(5) . . ? C97 C92 C91 122.2(6) . . ? C92 C91 H99C 109.5 . . ? C92 C91 H99D 109.5 . . ? H99C C91 H99D 109.5 . . ? C92 C91 H99E 109.5 . . ? H99C C91 H99E 109.5 . . ? H99D C91 H99E 109.5 . . ? C96 C95 C94 118.9(6) . . ? C96 C95 H99F 120.5 . . ? C94 C95 H99F 120.5 . . ? C96 C97 C92 121.0(6) . . ? C96 C97 H99G 119.5 . . ? C92 C97 H99G 119.5 . . ? C95 C96 C97 120.7(5) . . ? C95 C96 H99H 119.6 . . ? C97 C96 H99H 119.6 . . ? C321 C322 H11D 109.5 . . ? C321 C322 H11E 109.5 . . ? H11D C322 H11E 109.5 . . ? C321 C322 H11F 109.5 . . ? H11D C322 H11F 109.5 . . ? H11E C322 H11F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O35 Hf1 O31 C32 -19.0(4) . . . . ? O45 Hf1 O31 C32 -139.3(4) . . . . ? O21 Hf1 O31 C32 65.9(4) . . . . ? O25 Hf1 O31 C32 25.7(5) . . . . ? O15 Hf1 O31 C32 140.1(4) . . . . ? O11 Hf1 O31 C32 -179.1(4) . . . . ? O41 Hf1 O31 C32 -78.0(4) . . . . ? O35 Hf1 O15 C14 169.9(3) . . . . ? O45 Hf1 O15 C14 59.3(4) . . . . ? O21 Hf1 O15 C14 -149.0(4) . . . . ? O25 Hf1 O15 C14 -86.3(4) . . . . ? O11 Hf1 O15 C14 -22.8(4) . . . . ? O31 Hf1 O15 C14 133.1(4) . . . . ? O41 Hf1 O15 C14 14.8(5) . . . . ? O35 Hf1 O25 C24 59.9(4) . . . . ? O45 Hf1 O25 C24 169.9(4) . . . . ? O21 Hf1 O25 C24 -24.5(4) . . . . ? O15 Hf1 O25 C24 -85.0(4) . . . . ? O11 Hf1 O25 C24 -149.2(4) . . . . ? O31 Hf1 O25 C24 15.5(5) . . . . ? O41 Hf1 O25 C24 133.7(4) . . . . ? O35 Hf1 O41 C42 -140.3(4) . . . . ? O45 Hf1 O41 C42 -20.0(4) . . . . ? O21 Hf1 O41 C42 177.9(3) . . . . ? O25 Hf1 O41 C42 139.6(4) . . . . ? O15 Hf1 O41 C42 24.9(5) . . . . ? O11 Hf1 O41 C42 62.7(4) . . . . ? O31 Hf1 O41 C42 -79.2(4) . . . . ? O35 Hf1 O11 C12 -168.1(3) . . . . ? O45 Hf1 O11 C12 -56.2(4) . . . . ? O21 Hf1 O11 C12 82.5(4) . . . . ? O25 Hf1 O11 C12 146.1(4) . . . . ? O15 Hf1 O11 C12 23.0(4) . . . . ? O31 Hf1 O11 C12 -18.1(5) . . . . ? O41 Hf1 O11 C12 -134.0(4) . . . . ? O45 Hf1 O35 C34 75.6(4) . . . . ? O21 Hf1 O35 C34 -62.9(4) . . . . ? O25 Hf1 O35 C34 -139.9(4) . . . . ? O15 Hf1 O35 C34 -23.8(5) . . . . ? O11 Hf1 O35 C34 175.0(4) . . . . ? O31 Hf1 O35 C34 13.2(4) . . . . ? O41 Hf1 O35 C34 140.3(4) . . . . ? O35 Hf1 O45 C44 80.7(4) . . . . ? O21 Hf1 O45 C44 -177.0(4) . . . . ? O25 Hf1 O45 C44 -18.0(5) . . . . ? O15 Hf1 O45 C44 -134.9(4) . . . . ? O11 Hf1 O45 C44 -57.7(4) . . . . ? O31 Hf1 O45 C44 145.4(4) . . . . ? O41 Hf1 O45 C44 18.4(4) . . . . ? Hf1 O15 C14 O14 -162.3(3) . . . . ? Hf1 O15 C14 C13 18.3(7) . . . . ? C141 O14 C14 O15 6.6(6) . . . . ? C141 O14 C14 C13 -173.9(4) . . . . ? O35 Hf1 O21 C22 -56.9(4) . . . . ? O45 Hf1 O21 C22 -170.9(4) . . . . ? O25 Hf1 O21 C22 21.3(4) . . . . ? O15 Hf1 O21 C22 145.6(4) . . . . ? O11 Hf1 O21 C22 84.0(4) . . . . ? O31 Hf1 O21 C22 -134.0(4) . . . . ? O41 Hf1 O21 C22 -17.1(5) . . . . ? Hf1 O31 C32 O32 -164.5(3) . . . . ? Hf1 O31 C32 C33 16.7(7) . . . . ? C321 O32 C32 O31 3.2(7) . . . . ? C321 O32 C32 C33 -177.9(5) . . . . ? Hf1 O21 C22 O22 167.4(3) . . . . ? Hf1 O21 C22 C23 -13.4(8) . . . . ? O15 C14 C13 C12 -0.8(8) . . . . ? O14 C14 C13 C12 179.8(4) . . . . ? Hf1 O45 C44 O44 168.9(3) . . . . ? Hf1 O45 C44 C43 -12.1(7) . . . . ? C441 O44 C44 O45 -3.3(6) . . . . ? C441 O44 C44 C43 177.6(4) . . . . ? Hf1 O35 C34 O34 176.8(3) . . . . ? Hf1 O35 C34 C33 -4.4(7) . . . . ? C341 O34 C34 O35 -1.4(6) . . . . ? C341 O34 C34 C33 179.7(4) . . . . ? O35 C34 C33 C32 -7.3(8) . . . . ? O34 C34 C33 C32 171.5(4) . . . . ? O31 C32 C33 C34 1.2(8) . . . . ? O32 C32 C33 C34 -177.7(4) . . . . ? Hf1 O11 C12 O12 161.5(3) . . . . ? Hf1 O11 C12 C13 -18.6(7) . . . . ? C121 O12 C12 O11 -10.3(6) . . . . ? C121 O12 C12 C13 169.9(4) . . . . ? C14 C13 C12 O11 1.0(7) . . . . ? C14 C13 C12 O12 -179.2(4) . . . . ? O45 C44 C43 C42 -3.4(7) . . . . ? O44 C44 C43 C42 175.6(4) . . . . ? Hf1 O41 C42 O42 -165.6(3) . . . . ? Hf1 O41 C42 C43 15.9(7) . . . . ? C421 O42 C42 O41 6.3(6) . . . . ? C421 O42 C42 C43 -175.0(4) . . . . ? C44 C43 C42 O41 1.2(7) . . . . ? C44 C43 C42 O42 -177.4(4) . . . . ? O21 C22 O22 C221 -0.8(7) . . . . ? C23 C22 O22 C221 179.9(5) . . . . ? C14 O14 C141 C142 -179.3(4) . . . . ? C44 O44 C441 C442 178.8(4) . . . . ? O21 C22 C23 C24 -3.9(8) . . . . ? O22 C22 C23 C24 175.3(5) . . . . ? Hf1 O25 C24 O24 -160.3(3) . . . . ? Hf1 O25 C24 C23 20.5(7) . . . . ? C241 O24 C24 O25 6.0(6) . . . . ? C241 O24 C24 C23 -174.7(4) . . . . ? C22 C23 C24 O25 0.3(8) . . . . ? C22 C23 C24 O24 -179.0(4) . . . . ? C42 O42 C421 C422 100.2(5) . . . . ? C12 O12 C121 C122 -174.7(4) . . . . ? C24 O24 C241 C242 175.0(4) . . . . ? C34 O34 C341 C342 80.0(5) . . . . ? C32 O32 C321 C322 173.3(6) . . . . ? C22 O22 C221 C222 -108.6(6) . . . . ? C92 C93 C94 C95 -0.2(8) . . . . ? C94 C93 C92 C97 1.0(8) . . . . ? C94 C93 C92 C91 179.2(5) . . . . ? C93 C94 C95 C96 -0.8(8) . . . . ? C93 C92 C97 C96 -0.8(8) . . . . ? C91 C92 C97 C96 -179.0(6) . . . . ? C94 C95 C96 C97 1.0(9) . . . . ? C92 C97 C96 C95 -0.2(9) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 3.003 _refine_diff_density_min -1.128 _refine_diff_density_rms 0.099 #=================================END data_cvd192 _database_code_depnum_ccdc_archive 'CCDC 692633' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H36 O16 Zr' _chemical_formula_weight 707.78 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 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 10.9113(3) _cell_length_b 13.6640(6) _cell_length_c 21.4648(8) _cell_angle_alpha 90.00 _cell_angle_beta 97.516(3) _cell_angle_gamma 90.00 _cell_volume 3172.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 3000 _cell_measurement_theta_min 2.669 _cell_measurement_theta_max 31.095 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.880 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '406 images at 1.0 deg. in \w and 20 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18409 _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5561 _reflns_number_gt 4368 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0397P)^2^+0.7590P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5561 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0440 _refine_ls_R_factor_gt 0.0303 _refine_ls_wR_factor_ref 0.0786 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_restrained_S_all 1.043 _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 1.74835(2) 1.722236(17) 0.915449(11) 0.01745(8) Uani 1 1 d . . . O12 O 2.07560(16) 1.89557(15) 0.89425(9) 0.0338(5) Uani 1 1 d . . . C121 C 2.1209(3) 1.8899(3) 0.96004(14) 0.0427(8) Uani 1 1 d . . . H12A H 2.2017 1.9220 0.9680 0.064 Uiso 1 1 calc R . . H12B H 2.1292 1.8211 0.9728 0.064 Uiso 1 1 calc R . . H12C H 2.0627 1.9227 0.9842 0.064 Uiso 1 1 calc R . . O11 O 1.90791(15) 1.81691(13) 0.91709(8) 0.0235(4) Uani 1 1 d . . . C12 C 1.9649(2) 1.85456(18) 0.87567(13) 0.0241(6) Uani 1 1 d . . . C13 C 1.9238(2) 1.86117(19) 0.81195(13) 0.0262(6) Uani 1 1 d . . . H13A H 1.9753 1.8883 0.7839 0.031 Uiso 1 1 calc R . . O14 O 1.76936(16) 1.83994(14) 0.72810(8) 0.0309(5) Uani 1 1 d . . . C14 C 1.8062(2) 1.82752(19) 0.78979(12) 0.0225(6) Uani 1 1 d . . . C141 C 1.6485(2) 1.8007(2) 0.70528(13) 0.0344(7) Uani 1 1 d . . . H14A H 1.6297 1.8131 0.6601 0.052 Uiso 1 1 calc R . . H14B H 1.5860 1.8323 0.7273 0.052 Uiso 1 1 calc R . . H14C H 1.6479 1.7300 0.7130 0.052 Uiso 1 1 calc R . . O15 O 1.73134(14) 1.78794(13) 0.82207(8) 0.0217(4) Uani 1 1 d . . . O21 O 1.76022(15) 1.81409(12) 1.00003(8) 0.0226(4) Uani 1 1 d . . . C221 C 1.8348(3) 1.8629(2) 1.11495(14) 0.0367(7) Uani 1 1 d . . . H22A H 1.8481 1.8879 1.1581 0.055 Uiso 1 1 calc R . . H22B H 1.8936 1.8938 1.0903 0.055 Uiso 1 1 calc R . . H22C H 1.8473 1.7918 1.1154 0.055 Uiso 1 1 calc R . . O22 O 1.71073(18) 1.88488(14) 1.08724(9) 0.0335(5) Uani 1 1 d . . . C22 C 1.6788(2) 1.85481(18) 1.02762(13) 0.0256(6) Uani 1 1 d . . . C23 C 1.5578(2) 1.8740(2) 1.00219(13) 0.0296(6) Uani 1 1 d . . . H23A H 1.5019 1.9028 1.0273 0.036 Uiso 1 1 calc R . . O24 O 1.40387(17) 1.87970(16) 0.91757(9) 0.0381(5) Uani 1 1 d . . . C24 C 1.5193(2) 1.85095(19) 0.94008(13) 0.0271(6) Uani 1 1 d . . . O25 O 1.58202(15) 1.80805(13) 0.90274(8) 0.0235(4) Uani 1 1 d . . . O34 O 1.53361(16) 1.54019(14) 0.77502(9) 0.0314(5) Uani 1 1 d . . . C321 C 2.0753(2) 1.5887(2) 0.82236(14) 0.0354(7) Uani 1 1 d . . . H32A H 2.1420 1.5660 0.7995 0.053 Uiso 1 1 calc R . . H32B H 2.0844 1.5587 0.8642 0.053 Uiso 1 1 calc R . . H32C H 2.0794 1.6601 0.8266 0.053 Uiso 1 1 calc R . . O32 O 1.95829(17) 1.56137(14) 0.78844(9) 0.0302(4) Uani 1 1 d . . . C32 C 1.8577(2) 1.58786(19) 0.81448(12) 0.0247(6) Uani 1 1 d . . . O31 O 1.87305(15) 1.63398(12) 0.86568(8) 0.0223(4) Uani 1 1 d . . . C341 C 1.4196(2) 1.5609(2) 0.79889(13) 0.0342(7) Uani 1 1 d . . . H34A H 1.3510 1.5307 0.7715 0.051 Uiso 1 1 calc R . . H34B H 1.4071 1.6318 0.8000 0.051 Uiso 1 1 calc R . . H34C H 1.4228 1.5342 0.8415 0.051 Uiso 1 1 calc R . . O35 O 1.62753(15) 1.62204(13) 0.85782(8) 0.0235(4) Uani 1 1 d . . . C33 C 1.7450(2) 1.5592(2) 0.78190(12) 0.0279(6) Uani 1 1 d . . . H33A H 1.7420 1.5277 0.7423 0.033 Uiso 1 1 calc R . . C34 C 1.6370(2) 1.57705(19) 0.80754(12) 0.0243(6) Uani 1 1 d . . . O42 O 1.54907(15) 1.59562(13) 1.05976(8) 0.0253(4) Uani 1 1 d . . . C42 C 1.6481(2) 1.61592(17) 1.03033(12) 0.0199(5) Uani 1 1 d . . . O41 O 1.62943(14) 1.64644(12) 0.97478(8) 0.0201(4) Uani 1 1 d . . . C43 C 1.7623(2) 1.59835(19) 1.06553(12) 0.0225(6) Uani 1 1 d . . . H43A H 1.7669 1.5763 1.1077 0.027 Uiso 1 1 calc R . . O44 O 1.97451(15) 1.58907(14) 1.07448(8) 0.0267(4) Uani 1 1 d . . . C44 C 1.8694(2) 1.61338(18) 1.03838(12) 0.0214(6) Uani 1 1 d . . . C441 C 2.0884(2) 1.6054(2) 1.04861(13) 0.0299(6) Uani 1 1 d . . . H44A H 2.1584 1.5849 1.0791 0.045 Uiso 1 1 calc R . . H44B H 2.0963 1.6751 1.0392 0.045 Uiso 1 1 calc R . . H44C H 2.0877 1.5672 1.0099 0.045 Uiso 1 1 calc R . . C421 C 1.4290(2) 1.6158(2) 1.02577(14) 0.0301(6) Uani 1 1 d . . . H42A H 1.3650 1.5982 1.0518 0.045 Uiso 1 1 calc R . . H42B H 1.4177 1.5773 0.9869 0.045 Uiso 1 1 calc R . . H42C H 1.4227 1.6857 1.0155 0.045 Uiso 1 1 calc R . . O45 O 1.87579(14) 1.64470(12) 0.98368(8) 0.0212(4) Uani 1 1 d . . . C94 C 1.8430(3) 1.1349(2) 0.83469(13) 0.0347(7) Uani 1 1 d . . . H94A H 1.8954 1.0791 0.8386 0.042 Uiso 1 1 calc R . . C95 C 1.8839(3) 1.2207(2) 0.80935(14) 0.0366(7) Uani 1 1 d . . . H95A H 1.9636 1.2232 0.7962 0.044 Uiso 1 1 calc R . . C96 C 1.8095(3) 1.3014(2) 0.80340(14) 0.0362(7) Uani 1 1 d . . . H96A H 1.8372 1.3602 0.7861 0.043 Uiso 1 1 calc R . . C97 C 1.6933(3) 1.2971(2) 0.82283(15) 0.0378(7) Uani 1 1 d . . . H97A H 1.6411 1.3530 0.8188 0.045 Uiso 1 1 calc R . . C98 C 1.6534(3) 1.2123(2) 0.84789(14) 0.0378(7) Uani 1 1 d . . . H98A H 1.5738 1.2102 0.8612 0.045 Uiso 1 1 calc R . . C99 C 1.7279(3) 1.1294(2) 0.85413(13) 0.0339(7) Uani 1 1 d . . . C93 C 1.6822(3) 1.0359(2) 0.88014(16) 0.0486(8) Uani 1 1 d . . . H93A H 1.7464 0.9856 0.8812 0.073 Uiso 1 1 calc R . . H93B H 1.6077 1.0139 0.8534 0.073 Uiso 1 1 calc R . . H93C H 1.6627 1.0475 0.9228 0.073 Uiso 1 1 calc R . . C241 C 1.3633(3) 1.8598(3) 0.85250(15) 0.0451(8) Uani 1 1 d . . . H24A H 1.2786 1.8839 0.8414 0.068 Uiso 1 1 calc R . . H24B H 1.3654 1.7891 0.8451 0.068 Uiso 1 1 calc R . . H24C H 1.4181 1.8929 0.8265 0.068 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 0.01770(13) 0.01771(13) 0.01769(13) 0.00121(11) 0.00513(9) 0.00117(10) O12 0.0256(10) 0.0421(12) 0.0349(11) 0.0002(10) 0.0082(8) -0.0111(9) C121 0.0319(17) 0.060(2) 0.0363(17) -0.0023(16) 0.0036(13) -0.0156(15) O11 0.0232(9) 0.0232(10) 0.0251(10) -0.0001(8) 0.0065(7) -0.0046(7) C12 0.0230(14) 0.0170(13) 0.0343(16) -0.0013(12) 0.0107(12) -0.0005(11) C13 0.0272(15) 0.0255(15) 0.0286(15) 0.0047(12) 0.0142(12) -0.0006(11) O14 0.0296(10) 0.0410(12) 0.0227(10) 0.0103(9) 0.0064(8) -0.0019(9) C14 0.0258(14) 0.0187(14) 0.0244(14) 0.0048(12) 0.0086(11) 0.0061(11) C141 0.0317(16) 0.0467(19) 0.0236(15) 0.0121(13) -0.0009(12) -0.0033(13) O15 0.0219(9) 0.0237(10) 0.0206(9) 0.0047(8) 0.0067(7) 0.0016(7) O21 0.0253(9) 0.0201(9) 0.0238(9) -0.0038(8) 0.0080(7) -0.0012(7) C221 0.0432(18) 0.0367(18) 0.0293(16) -0.0104(14) 0.0018(13) -0.0016(13) O22 0.0443(12) 0.0334(11) 0.0240(10) -0.0069(9) 0.0091(9) 0.0050(9) C22 0.0362(16) 0.0157(13) 0.0270(15) 0.0010(12) 0.0119(12) -0.0003(11) C23 0.0355(16) 0.0278(15) 0.0280(15) -0.0003(13) 0.0134(12) 0.0099(12) O24 0.0311(11) 0.0484(13) 0.0357(12) 0.0062(10) 0.0081(9) 0.0197(9) C24 0.0261(14) 0.0214(14) 0.0364(16) 0.0102(12) 0.0143(12) 0.0086(11) O25 0.0230(9) 0.0241(10) 0.0246(10) 0.0038(8) 0.0071(8) 0.0072(7) O34 0.0322(11) 0.0335(11) 0.0278(10) -0.0051(9) 0.0012(8) -0.0070(8) C321 0.0301(16) 0.0437(19) 0.0345(17) 0.0065(14) 0.0125(13) 0.0120(13) O32 0.0343(11) 0.0312(11) 0.0277(10) -0.0008(9) 0.0140(8) 0.0087(8) C32 0.0344(15) 0.0179(14) 0.0245(14) 0.0066(12) 0.0132(12) 0.0054(11) O31 0.0254(10) 0.0230(10) 0.0192(9) 0.0002(8) 0.0059(7) 0.0043(7) C341 0.0289(16) 0.0392(18) 0.0340(16) -0.0021(14) 0.0022(12) -0.0085(13) O35 0.0263(10) 0.0237(10) 0.0213(10) -0.0008(8) 0.0062(7) -0.0038(7) C33 0.0367(16) 0.0255(15) 0.0225(14) -0.0045(12) 0.0074(12) -0.0016(12) C34 0.0350(15) 0.0174(14) 0.0203(14) 0.0021(11) 0.0029(11) -0.0036(11) O42 0.0230(10) 0.0305(10) 0.0235(10) 0.0027(8) 0.0077(8) -0.0034(8) C42 0.0272(14) 0.0143(13) 0.0198(13) -0.0027(11) 0.0091(11) -0.0038(10) O41 0.0200(9) 0.0219(10) 0.0189(9) 0.0010(7) 0.0041(7) -0.0012(7) C43 0.0246(14) 0.0259(14) 0.0178(13) 0.0057(11) 0.0060(11) 0.0025(11) O44 0.0217(10) 0.0367(11) 0.0214(9) 0.0054(8) 0.0022(7) 0.0041(8) C44 0.0259(14) 0.0158(13) 0.0218(14) -0.0020(11) 0.0008(11) 0.0032(10) C441 0.0214(14) 0.0369(17) 0.0310(15) 0.0016(13) 0.0025(11) 0.0051(12) C421 0.0214(14) 0.0348(16) 0.0354(16) 0.0000(13) 0.0082(12) -0.0041(12) O45 0.0212(9) 0.0249(10) 0.0183(9) 0.0033(8) 0.0053(7) 0.0035(7) C94 0.0442(18) 0.0296(17) 0.0309(16) -0.0017(13) 0.0078(13) 0.0100(13) C95 0.0403(17) 0.0374(18) 0.0327(16) -0.0065(15) 0.0067(13) -0.0007(14) C96 0.0470(19) 0.0270(17) 0.0332(17) 0.0003(13) 0.0001(14) -0.0037(13) C97 0.0392(17) 0.0278(17) 0.0449(19) -0.0009(14) -0.0003(14) 0.0067(13) C98 0.0356(17) 0.0368(18) 0.0404(17) -0.0088(15) 0.0030(13) 0.0049(14) C99 0.0476(18) 0.0290(16) 0.0253(15) -0.0037(13) 0.0051(13) 0.0004(13) C93 0.061(2) 0.040(2) 0.048(2) 0.0027(16) 0.0206(17) -0.0024(16) C241 0.0284(17) 0.066(2) 0.0409(19) 0.0071(17) 0.0028(14) 0.0155(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O25 2.1479(16) . ? Zr1 O45 2.1606(16) . ? Zr1 O11 2.1656(17) . ? Zr1 O35 2.1716(17) . ? Zr1 O15 2.1819(17) . ? Zr1 O41 2.1933(16) . ? Zr1 O21 2.1970(17) . ? Zr1 O31 2.1970(17) . ? O12 C12 1.344(3) . ? O12 C121 1.436(3) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? O11 C12 1.260(3) . ? C12 C13 1.385(4) . ? C13 C14 1.388(4) . ? C13 H13A 0.9500 . ? O14 C14 1.343(3) . ? O14 C141 1.449(3) . ? C14 O15 1.260(3) . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? O21 C22 1.260(3) . ? C221 O22 1.438(3) . ? C221 H22A 0.9800 . ? C221 H22B 0.9800 . ? C221 H22C 0.9800 . ? O22 C22 1.346(3) . ? C22 C23 1.386(4) . ? C23 C24 1.381(4) . ? C23 H23A 0.9500 . ? O24 C24 1.347(3) . ? O24 C241 1.435(4) . ? C24 O25 1.264(3) . ? O34 C34 1.345(3) . ? O34 C341 1.434(3) . ? C321 O32 1.434(3) . ? C321 H32A 0.9800 . ? C321 H32B 0.9800 . ? C321 H32C 0.9800 . ? O32 C32 1.345(3) . ? C32 O31 1.259(3) . ? C32 C33 1.389(4) . ? C341 H34A 0.9800 . ? C341 H34B 0.9800 . ? C341 H34C 0.9800 . ? O35 C34 1.258(3) . ? C33 C34 1.386(4) . ? C33 H33A 0.9500 . ? O42 C42 1.350(3) . ? O42 C421 1.440(3) . ? C42 O41 1.254(3) . ? C42 C43 1.391(3) . ? C43 C44 1.388(3) . ? C43 H43A 0.9500 . ? O44 C44 1.339(3) . ? O44 C441 1.443(3) . ? C44 O45 1.260(3) . ? C441 H44A 0.9800 . ? C441 H44B 0.9800 . ? C441 H44C 0.9800 . ? C421 H42A 0.9800 . ? C421 H42B 0.9800 . ? C421 H42C 0.9800 . ? C94 C99 1.376(4) . ? C94 C95 1.391(4) . ? C94 H94A 0.9500 . ? C95 C96 1.365(4) . ? C95 H95A 0.9500 . ? C96 C97 1.387(4) . ? C96 H96A 0.9500 . ? C97 C98 1.372(4) . ? C97 H97A 0.9500 . ? C98 C99 1.391(4) . ? C98 H98A 0.9500 . ? C99 C93 1.504(4) . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C241 H24A 0.9800 . ? C241 H24B 0.9800 . ? C241 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O25 Zr1 O45 144.29(6) . . ? O25 Zr1 O11 109.89(7) . . ? O45 Zr1 O11 80.63(6) . . ? O25 Zr1 O35 80.32(7) . . ? O45 Zr1 O35 111.46(7) . . ? O11 Zr1 O35 144.36(6) . . ? O25 Zr1 O15 71.93(6) . . ? O45 Zr1 O15 142.59(6) . . ? O11 Zr1 O15 74.98(6) . . ? O35 Zr1 O15 76.33(6) . . ? O25 Zr1 O41 77.13(6) . . ? O45 Zr1 O41 75.64(6) . . ? O11 Zr1 O41 143.90(6) . . ? O35 Zr1 O41 70.84(6) . . ? O15 Zr1 O41 137.90(6) . . ? O25 Zr1 O21 75.56(6) . . ? O45 Zr1 O21 75.92(6) . . ? O11 Zr1 O21 71.63(6) . . ? O35 Zr1 O21 142.81(6) . . ? O15 Zr1 O21 120.85(7) . . ? O41 Zr1 O21 76.43(6) . . ? O25 Zr1 O31 143.57(6) . . ? O45 Zr1 O31 71.09(6) . . ? O11 Zr1 O31 77.76(6) . . ? O35 Zr1 O31 75.25(6) . . ? O15 Zr1 O31 76.28(6) . . ? O41 Zr1 O31 118.31(6) . . ? O21 Zr1 O31 137.90(6) . . ? C12 O12 C121 116.7(2) . . ? O12 C121 H12A 109.5 . . ? O12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? O12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C12 O11 Zr1 134.63(17) . . ? O11 C12 O12 117.9(2) . . ? O11 C12 C13 126.7(2) . . ? O12 C12 C13 115.3(2) . . ? C12 C13 C14 118.8(2) . . ? C12 C13 H13A 120.6 . . ? C14 C13 H13A 120.6 . . ? C14 O14 C141 115.3(2) . . ? O15 C14 O14 117.7(2) . . ? O15 C14 C13 126.2(2) . . ? O14 C14 C13 116.1(2) . . ? O14 C141 H14A 109.5 . . ? O14 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? O14 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C14 O15 Zr1 134.30(16) . . ? C22 O21 Zr1 132.21(17) . . ? O22 C221 H22A 109.5 . . ? O22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? O22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C22 O22 C221 116.2(2) . . ? O21 C22 O22 118.1(2) . . ? O21 C22 C23 126.3(3) . . ? O22 C22 C23 115.6(2) . . ? C24 C23 C22 119.4(2) . . ? C24 C23 H23A 120.3 . . ? C22 C23 H23A 120.3 . . ? C24 O24 C241 116.7(2) . . ? O25 C24 O24 117.8(3) . . ? O25 C24 C23 126.6(2) . . ? O24 C24 C23 115.6(2) . . ? C24 O25 Zr1 133.72(17) . . ? C34 O34 C341 116.7(2) . . ? O32 C321 H32A 109.5 . . ? O32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? O32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? C32 O32 C321 116.1(2) . . ? O31 C32 O32 118.3(2) . . ? O31 C32 C33 126.1(2) . . ? O32 C32 C33 115.6(2) . . ? C32 O31 Zr1 132.75(16) . . ? O34 C341 H34A 109.5 . . ? O34 C341 H34B 109.5 . . ? H34A C341 H34B 109.5 . . ? O34 C341 H34C 109.5 . . ? H34A C341 H34C 109.5 . . ? H34B C341 H34C 109.5 . . ? C34 O35 Zr1 133.22(16) . . ? C34 C33 C32 119.5(2) . . ? C34 C33 H33A 120.2 . . ? C32 C33 H33A 120.2 . . ? O35 C34 O34 118.1(2) . . ? O35 C34 C33 126.6(2) . . ? O34 C34 C33 115.3(2) . . ? C42 O42 C421 117.0(2) . . ? O41 C42 O42 118.2(2) . . ? O41 C42 C43 126.6(2) . . ? O42 C42 C43 115.1(2) . . ? C42 O41 Zr1 132.39(15) . . ? C44 C43 C42 119.3(2) . . ? C44 C43 H43A 120.3 . . ? C42 C43 H43A 120.3 . . ? C44 O44 C441 117.0(2) . . ? O45 C44 O44 118.4(2) . . ? O45 C44 C43 126.4(2) . . ? O44 C44 C43 115.1(2) . . ? O44 C441 H44A 109.5 . . ? O44 C441 H44B 109.5 . . ? H44A C441 H44B 109.5 . . ? O44 C441 H44C 109.5 . . ? H44A C441 H44C 109.5 . . ? H44B C441 H44C 109.5 . . ? O42 C421 H42A 109.5 . . ? O42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? O42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C44 O45 Zr1 133.54(16) . . ? C99 C94 C95 121.1(3) . . ? C99 C94 H94A 119.5 . . ? C95 C94 H94A 119.5 . . ? C96 C95 C94 120.1(3) . . ? C96 C95 H95A 120.0 . . ? C94 C95 H95A 120.0 . . ? C95 C96 C97 119.5(3) . . ? C95 C96 H96A 120.2 . . ? C97 C96 H96A 120.2 . . ? C98 C97 C96 120.2(3) . . ? C98 C97 H97A 119.9 . . ? C96 C97 H97A 119.9 . . ? C97 C98 C99 121.0(3) . . ? C97 C98 H98A 119.5 . . ? C99 C98 H98A 119.5 . . ? C94 C99 C98 118.1(3) . . ? C94 C99 C93 121.2(3) . . ? C98 C99 C93 120.6(3) . . ? C99 C93 H93A 109.5 . . ? C99 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C99 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? O24 C241 H24A 109.5 . . ? O24 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? O24 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O25 Zr1 O11 C12 -84.5(2) . . . . ? O45 Zr1 O11 C12 130.9(2) . . . . ? O35 Zr1 O11 C12 16.9(3) . . . . ? O15 Zr1 O11 C12 -20.5(2) . . . . ? O41 Zr1 O11 C12 -179.9(2) . . . . ? O21 Zr1 O11 C12 -150.9(2) . . . . ? O31 Zr1 O11 C12 58.4(2) . . . . ? Zr1 O11 C12 O12 -167.71(16) . . . . ? Zr1 O11 C12 C13 14.4(4) . . . . ? C121 O12 C12 O11 1.9(4) . . . . ? C121 O12 C12 C13 -180.0(2) . . . . ? O11 C12 C13 C14 3.0(4) . . . . ? O12 C12 C13 C14 -175.0(2) . . . . ? C141 O14 C14 O15 -3.3(3) . . . . ? C141 O14 C14 C13 177.5(2) . . . . ? C12 C13 C14 O15 -2.1(4) . . . . ? C12 C13 C14 O14 177.1(2) . . . . ? O14 C14 O15 Zr1 164.82(16) . . . . ? C13 C14 O15 Zr1 -16.1(4) . . . . ? O25 Zr1 O15 C14 138.6(2) . . . . ? O45 Zr1 O15 C14 -29.7(3) . . . . ? O11 Zr1 O15 C14 21.3(2) . . . . ? O35 Zr1 O15 C14 -137.3(2) . . . . ? O41 Zr1 O15 C14 -176.7(2) . . . . ? O21 Zr1 O15 C14 78.6(2) . . . . ? O31 Zr1 O15 C14 -59.5(2) . . . . ? O25 Zr1 O21 C22 25.0(2) . . . . ? O45 Zr1 O21 C22 -133.2(2) . . . . ? O11 Zr1 O21 C22 142.1(2) . . . . ? O35 Zr1 O21 C22 -26.2(3) . . . . ? O15 Zr1 O21 C22 83.2(2) . . . . ? O41 Zr1 O21 C22 -54.9(2) . . . . ? O31 Zr1 O21 C22 -172.3(2) . . . . ? Zr1 O21 C22 O22 162.65(16) . . . . ? Zr1 O21 C22 C23 -18.7(4) . . . . ? C221 O22 C22 O21 -3.0(3) . . . . ? C221 O22 C22 C23 178.2(2) . . . . ? O21 C22 C23 C24 -2.6(4) . . . . ? O22 C22 C23 C24 176.2(2) . . . . ? C241 O24 C24 O25 -0.8(4) . . . . ? C241 O24 C24 C23 177.8(3) . . . . ? C22 C23 C24 O25 4.0(4) . . . . ? C22 C23 C24 O24 -174.4(2) . . . . ? O24 C24 O25 Zr1 -164.92(17) . . . . ? C23 C24 O25 Zr1 16.7(4) . . . . ? O45 Zr1 O25 C24 13.7(3) . . . . ? O11 Zr1 O25 C24 -88.2(2) . . . . ? O35 Zr1 O25 C24 127.2(2) . . . . ? O15 Zr1 O25 C24 -154.1(2) . . . . ? O41 Zr1 O25 C24 54.8(2) . . . . ? O21 Zr1 O25 C24 -24.2(2) . . . . ? O31 Zr1 O25 C24 175.5(2) . . . . ? C321 O32 C32 O31 0.1(3) . . . . ? C321 O32 C32 C33 -178.7(2) . . . . ? O32 C32 O31 Zr1 163.17(15) . . . . ? C33 C32 O31 Zr1 -18.1(4) . . . . ? O25 Zr1 O31 C32 -24.2(3) . . . . ? O45 Zr1 O31 C32 144.7(2) . . . . ? O11 Zr1 O31 C32 -131.2(2) . . . . ? O35 Zr1 O31 C32 25.3(2) . . . . ? O15 Zr1 O31 C32 -53.9(2) . . . . ? O41 Zr1 O31 C32 83.5(2) . . . . ? O21 Zr1 O31 C32 -175.0(2) . . . . ? O25 Zr1 O35 C34 127.4(2) . . . . ? O45 Zr1 O35 C34 -87.8(2) . . . . ? O11 Zr1 O35 C34 16.6(3) . . . . ? O15 Zr1 O35 C34 53.8(2) . . . . ? O41 Zr1 O35 C34 -153.0(2) . . . . ? O21 Zr1 O35 C34 177.3(2) . . . . ? O31 Zr1 O35 C34 -25.4(2) . . . . ? O31 C32 C33 C34 -3.4(4) . . . . ? O32 C32 C33 C34 175.3(2) . . . . ? Zr1 O35 C34 O34 -163.10(16) . . . . ? Zr1 O35 C34 C33 18.2(4) . . . . ? C341 O34 C34 O35 3.7(3) . . . . ? C341 O34 C34 C33 -177.5(2) . . . . ? C32 C33 C34 O35 3.6(4) . . . . ? C32 C33 C34 O34 -175.1(2) . . . . ? C421 O42 C42 O41 -3.2(3) . . . . ? C421 O42 C42 C43 178.0(2) . . . . ? O42 C42 O41 Zr1 162.47(15) . . . . ? C43 C42 O41 Zr1 -18.9(4) . . . . ? O25 Zr1 O41 C42 -132.0(2) . . . . ? O45 Zr1 O41 C42 24.7(2) . . . . ? O11 Zr1 O41 C42 -25.8(3) . . . . ? O35 Zr1 O41 C42 143.9(2) . . . . ? O15 Zr1 O41 C42 -175.31(19) . . . . ? O21 Zr1 O41 C42 -54.0(2) . . . . ? O31 Zr1 O41 C42 83.5(2) . . . . ? O41 C42 C43 C44 -1.2(4) . . . . ? O42 C42 C43 C44 177.5(2) . . . . ? C441 O44 C44 O45 2.9(3) . . . . ? C441 O44 C44 C43 -178.8(2) . . . . ? C42 C43 C44 O45 1.9(4) . . . . ? C42 C43 C44 O44 -176.2(2) . . . . ? O44 C44 O45 Zr1 -163.91(16) . . . . ? C43 C44 O45 Zr1 18.0(4) . . . . ? O25 Zr1 O45 C44 17.1(3) . . . . ? O11 Zr1 O45 C44 128.2(2) . . . . ? O35 Zr1 O45 C44 -86.7(2) . . . . ? O15 Zr1 O45 C44 177.8(2) . . . . ? O41 Zr1 O45 C44 -24.4(2) . . . . ? O21 Zr1 O45 C44 54.9(2) . . . . ? O31 Zr1 O45 C44 -151.6(2) . . . . ? C99 C94 C95 C96 0.0(4) . . . . ? C94 C95 C96 C97 0.1(4) . . . . ? C95 C96 C97 C98 0.0(4) . . . . ? C96 C97 C98 C99 -0.2(5) . . . . ? C95 C94 C99 C98 -0.1(4) . . . . ? C95 C94 C99 C93 178.5(3) . . . . ? C97 C98 C99 C94 0.3(4) . . . . ? C97 C98 C99 C93 -178.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.373 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.063 #=================================END data_cvd215 _database_code_depnum_ccdc_archive 'CCDC 692634' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24 H56 O10 Si6 Zr' _chemical_formula_weight 764.45 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' Si Si 0.0817 0.0704 '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 20.1977(11) _cell_length_b 12.1970(11) _cell_length_c 20.2323(10) _cell_angle_alpha 90.00 _cell_angle_beta 106.847(7) _cell_angle_gamma 90.00 _cell_volume 4770.3(6) _cell_formula_units_Z 4 _cell_measurement_temperature 104(2) _cell_measurement_reflns_used 520 _cell_measurement_theta_min 2.602 _cell_measurement_theta_max 27.498 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.416 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.920 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 104(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '560 images at 1.0 deg. in \w and 30 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19257 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.1790 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4168 _reflns_number_gt 2055 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171.32.11, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171.32.11, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171.32.11, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4168 _refine_ls_number_parameters 195 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0971 _refine_ls_R_factor_gt 0.0473 _refine_ls_wR_factor_ref 0.0974 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 0.745 _refine_ls_restrained_S_all 0.745 _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 0.0000 0.22841(5) 0.2500 0.0261(2) Uani 1 2 d S . . O1 O 0.10686(14) 0.2059(2) 0.26142(13) 0.0275(7) Uani 1 1 d . . . C2 C 0.1415(2) 0.1524(4) 0.2288(2) 0.0325(11) Uani 1 1 d . . . O2 O 0.21014(16) 0.1697(2) 0.24706(17) 0.0452(9) Uani 1 1 d . . . Si2 Si 0.25302(7) 0.25647(12) 0.30949(6) 0.0433(4) Uani 1 1 d . . . C21 C 0.2187(3) 0.3963(4) 0.2862(4) 0.105(3) Uani 1 1 d . . . H21A H 0.2282 0.4193 0.2434 0.157 Uiso 1 1 calc R . . H21B H 0.2410 0.4473 0.3234 0.157 Uiso 1 1 calc R . . H21C H 0.1686 0.3965 0.2793 0.157 Uiso 1 1 calc R . . C22 C 0.2433(3) 0.2081(7) 0.3921(3) 0.121(3) Uani 1 1 d . . . H22A H 0.1953 0.2183 0.3926 0.181 Uiso 1 1 calc R . . H22B H 0.2742 0.2500 0.4300 0.181 Uiso 1 1 calc R . . H22C H 0.2553 0.1301 0.3979 0.181 Uiso 1 1 calc R . . C23 C 0.3431(2) 0.2445(4) 0.3062(3) 0.0623(16) Uani 1 1 d . . . H23A H 0.3571 0.1673 0.3107 0.093 Uiso 1 1 calc R . . H23B H 0.3736 0.2867 0.3442 0.093 Uiso 1 1 calc R . . H23C H 0.3464 0.2732 0.2621 0.093 Uiso 1 1 calc R . . C3 C 0.1154(2) 0.0749(4) 0.1787(2) 0.0351(12) Uani 1 1 d . . . H3 H 0.1459 0.0376 0.1584 0.042 Uiso 1 1 calc R . . C4 C 0.0450(2) 0.0500(3) 0.1572(2) 0.0298(11) Uani 1 1 d . . . O4 O 0.02497(15) -0.0289(2) 0.10921(14) 0.0349(8) Uani 1 1 d . . . Si4 Si -0.05742(7) -0.07473(10) 0.07948(7) 0.0344(4) Uani 1 1 d . . . C41 C -0.0861(3) -0.1212(4) 0.1529(2) 0.0484(14) Uani 1 1 d . . . H41A H -0.0495 -0.1648 0.1841 0.073 Uiso 1 1 calc R . . H41B H -0.1279 -0.1661 0.1361 0.073 Uiso 1 1 calc R . . H41C H -0.0964 -0.0574 0.1777 0.073 Uiso 1 1 calc R . . C42 C -0.1116(2) 0.0355(3) 0.0292(2) 0.0435(13) Uani 1 1 d . . . H42A H -0.1119 0.0980 0.0595 0.065 Uiso 1 1 calc R . . H42B H -0.1589 0.0086 0.0094 0.065 Uiso 1 1 calc R . . H42C H -0.0926 0.0586 -0.0080 0.065 Uiso 1 1 calc R . . C43 C -0.0475(3) -0.1894(3) 0.0230(2) 0.0452(14) Uani 1 1 d . . . H43A H -0.0320 -0.1606 -0.0152 0.068 Uiso 1 1 calc R . . H43B H -0.0920 -0.2267 0.0046 0.068 Uiso 1 1 calc R . . H43C H -0.0131 -0.2414 0.0499 0.068 Uiso 1 1 calc R . . O5 O -0.00067(15) 0.0940(2) 0.17920(14) 0.0291(7) Uani 1 1 d . . . O6 O 0.02216(17) 0.3329(2) 0.32618(16) 0.0423(9) Uani 1 1 d . . . Si6 Si 0.03481(8) 0.42959(11) 0.38191(7) 0.0467(4) Uani 1 1 d . . . C61 C -0.0454(3) 0.4556(5) 0.4027(3) 0.085(2) Uani 1 1 d . . . H61A H -0.0815 0.4765 0.3606 0.127 Uiso 1 1 calc R . . H61B H -0.0384 0.5153 0.4364 0.127 Uiso 1 1 calc R . . H61C H -0.0596 0.3892 0.4221 0.127 Uiso 1 1 calc R . . C62 C 0.1024(3) 0.3859(5) 0.4605(3) 0.082(2) Uani 1 1 d . . . H62A H 0.0861 0.3219 0.4806 0.124 Uiso 1 1 calc R . . H62B H 0.1124 0.4459 0.4941 0.124 Uiso 1 1 calc R . . H62C H 0.1446 0.3666 0.4484 0.124 Uiso 1 1 calc R . . C63 C 0.0629(4) 0.5548(4) 0.3466(3) 0.086(2) Uani 1 1 d . . . H63A H 0.1049 0.5392 0.3333 0.130 Uiso 1 1 calc R . . H63B H 0.0726 0.6126 0.3818 0.130 Uiso 1 1 calc R . . H63C H 0.0262 0.5792 0.3060 0.130 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 0.0249(4) 0.0224(4) 0.0294(4) 0.000 0.0053(3) 0.000 O1 0.0204(17) 0.0281(18) 0.0341(17) -0.0043(14) 0.0080(14) -0.0022(13) C2 0.026(3) 0.029(3) 0.040(3) 0.001(2) 0.005(2) -0.004(2) O2 0.022(2) 0.045(2) 0.068(2) -0.0210(17) 0.0120(18) -0.0068(16) Si2 0.0250(8) 0.0526(10) 0.0472(8) -0.0037(8) 0.0027(7) -0.0051(7) C21 0.044(4) 0.040(4) 0.214(8) -0.016(4) 0.011(5) -0.012(3) C22 0.052(4) 0.253(10) 0.051(4) 0.032(5) 0.004(3) -0.015(5) C23 0.027(3) 0.069(4) 0.086(4) 0.002(3) 0.008(3) -0.006(3) C3 0.023(3) 0.037(3) 0.047(3) -0.012(3) 0.014(2) 0.001(2) C4 0.039(3) 0.023(3) 0.027(3) 0.000(2) 0.008(2) 0.004(2) O4 0.034(2) 0.0306(18) 0.0406(19) -0.0128(16) 0.0115(15) -0.0050(15) Si4 0.0359(9) 0.0284(8) 0.0394(8) -0.0088(7) 0.0115(7) -0.0079(6) C41 0.055(4) 0.042(3) 0.050(3) -0.010(3) 0.018(3) -0.020(3) C42 0.038(3) 0.041(3) 0.047(3) -0.005(3) 0.005(3) -0.006(2) C43 0.048(3) 0.040(3) 0.049(3) -0.015(3) 0.015(3) -0.008(2) O5 0.0222(18) 0.0307(18) 0.0341(18) -0.0120(15) 0.0076(15) -0.0045(14) O6 0.040(2) 0.0373(19) 0.049(2) -0.0144(16) 0.0125(17) -0.0029(16) Si6 0.0525(10) 0.0404(9) 0.0433(9) -0.0157(8) 0.0077(8) 0.0011(8) C61 0.085(5) 0.091(5) 0.083(5) -0.023(4) 0.030(4) 0.029(4) C62 0.096(6) 0.087(5) 0.051(4) -0.016(4) 0.001(4) 0.005(4) C63 0.119(6) 0.050(4) 0.081(4) -0.001(4) 0.015(4) -0.018(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 O6 1.949(3) . ? Zr1 O6 1.949(3) 2 ? Zr1 O1 2.121(3) . ? Zr1 O1 2.121(3) 2 ? Zr1 O5 2.175(3) . ? Zr1 O5 2.175(3) 2 ? O1 C2 1.272(5) . ? C2 O2 1.344(5) . ? C2 C3 1.374(6) . ? O2 Si2 1.683(3) . ? Si2 C22 1.836(5) . ? Si2 C23 1.845(5) . ? Si2 C21 1.850(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C3 C4 1.394(6) . ? C3 H3 0.9500 . ? C4 O5 1.255(5) . ? C4 O4 1.344(4) . ? O4 Si4 1.692(3) . ? Si4 C41 1.834(4) . ? Si4 C42 1.842(4) . ? Si4 C43 1.853(4) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? O6 Si6 1.601(3) . ? Si6 C61 1.815(6) . ? Si6 C63 1.844(5) . ? Si6 C62 1.849(6) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Zr1 O6 98.37(18) . 2 ? O6 Zr1 O1 90.29(12) . . ? O6 Zr1 O1 99.43(12) 2 . ? O6 Zr1 O1 99.43(12) . 2 ? O6 Zr1 O1 90.29(12) 2 2 ? O1 Zr1 O1 165.15(14) . 2 ? O6 Zr1 O5 165.89(12) . . ? O6 Zr1 O5 90.91(11) 2 . ? O1 Zr1 O5 77.65(10) . . ? O1 Zr1 O5 91.08(10) 2 . ? O6 Zr1 O5 90.91(11) . 2 ? O6 Zr1 O5 165.89(12) 2 2 ? O1 Zr1 O5 91.08(10) . 2 ? O1 Zr1 O5 77.65(10) 2 2 ? O5 Zr1 O5 82.12(14) . 2 ? C2 O1 Zr1 134.8(3) . . ? O1 C2 O2 117.1(4) . . ? O1 C2 C3 125.7(4) . . ? O2 C2 C3 117.1(4) . . ? C2 O2 Si2 124.8(3) . . ? O2 Si2 C22 108.3(3) . . ? O2 Si2 C23 102.8(2) . . ? C22 Si2 C23 111.9(3) . . ? O2 Si2 C21 108.4(2) . . ? C22 Si2 C21 113.4(4) . . ? C23 Si2 C21 111.4(3) . . ? Si2 C21 H21A 109.5 . . ? Si2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si2 C22 H22A 109.5 . . ? Si2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si2 C23 H23A 109.5 . . ? Si2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C2 C3 C4 121.3(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O5 C4 O4 117.6(4) . . ? O5 C4 C3 125.7(4) . . ? O4 C4 C3 116.7(4) . . ? C4 O4 Si4 123.6(3) . . ? O4 Si4 C41 108.9(2) . . ? O4 Si4 C42 108.68(18) . . ? C41 Si4 C42 113.4(2) . . ? O4 Si4 C43 101.4(2) . . ? C41 Si4 C43 112.5(2) . . ? C42 Si4 C43 111.3(2) . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si4 C43 H43A 109.5 . . ? Si4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C4 O5 Zr1 133.7(3) . . ? Si6 O6 Zr1 172.8(2) . . ? O6 Si6 C61 108.7(2) . . ? O6 Si6 C63 110.0(2) . . ? C61 Si6 C63 109.9(3) . . ? O6 Si6 C62 108.7(2) . . ? C61 Si6 C62 109.8(3) . . ? C63 Si6 C62 109.8(3) . . ? Si6 C61 H61A 109.5 . . ? Si6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si6 C62 H62A 109.5 . . ? Si6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si6 C63 H63A 109.5 . . ? Si6 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? Si6 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Zr1 O1 C2 -175.7(4) . . . . ? O6 Zr1 O1 C2 -77.2(4) 2 . . . ? O1 Zr1 O1 C2 53.1(4) 2 . . . ? O5 Zr1 O1 C2 11.7(4) . . . . ? O5 Zr1 O1 C2 93.4(4) 2 . . . ? Zr1 O1 C2 O2 171.7(3) . . . . ? Zr1 O1 C2 C3 -11.3(7) . . . . ? O1 C2 O2 Si2 0.0(6) . . . . ? C3 C2 O2 Si2 -177.2(3) . . . . ? C2 O2 Si2 C22 63.1(4) . . . . ? C2 O2 Si2 C23 -178.3(4) . . . . ? C2 O2 Si2 C21 -60.4(4) . . . . ? O1 C2 C3 C4 2.0(7) . . . . ? O2 C2 C3 C4 179.0(4) . . . . ? C2 C3 C4 O5 0.8(7) . . . . ? C2 C3 C4 O4 -178.3(4) . . . . ? O5 C4 O4 Si4 -2.3(5) . . . . ? C3 C4 O4 Si4 176.9(3) . . . . ? C4 O4 Si4 C41 -55.9(3) . . . . ? C4 O4 Si4 C42 68.0(3) . . . . ? C4 O4 Si4 C43 -174.6(3) . . . . ? O4 C4 O5 Zr1 -175.8(2) . . . . ? C3 C4 O5 Zr1 5.1(6) . . . . ? O6 Zr1 O5 C4 -40.4(7) . . . . ? O6 Zr1 O5 C4 90.9(4) 2 . . . ? O1 Zr1 O5 C4 -8.6(3) . . . . ? O1 Zr1 O5 C4 -178.8(4) 2 . . . ? O5 Zr1 O5 C4 -101.4(4) 2 . . . ? O6 Zr1 O6 Si6 20.9(16) 2 . . . ? O1 Zr1 O6 Si6 120.5(17) . . . . ? O1 Zr1 O6 Si6 -70.8(17) 2 . . . ? O5 Zr1 O6 Si6 151.6(14) . . . . ? O5 Zr1 O6 Si6 -148.4(17) 2 . . . ? Zr1 O6 Si6 C61 71.9(17) . . . . ? Zr1 O6 Si6 C63 -48.4(18) . . . . ? Zr1 O6 Si6 C62 -168.6(17) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.389 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.079 #=================================END data_cvd218 _database_code_depnum_ccdc_archive 'CCDC 692635' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H76 Hf O16' _chemical_formula_weight 1039.54 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' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P4/ncc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-y+1/2, x, z' 'y, -x+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y, -x, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'y-1/2, -x, -z' '-y, x-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' '-y-1/2, -x-1/2, z-1/2' 'y, x, z-1/2' _cell_length_a 14.7752(3) _cell_length_b 14.7752(3) _cell_length_c 23.5966(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5151.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 2300 _cell_measurement_theta_min 2.598 _cell_measurement_theta_max 27.500 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 2.087 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.770 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '383 images at 1.0 deg. in \w and 20 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11329 _diffrn_reflns_av_R_equivalents 0.0931 _diffrn_reflns_av_sigmaI/netI 0.1095 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.45 _diffrn_reflns_theta_max 25.07 _reflns_number_total 2188 _reflns_number_gt 1190 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 1.171.13, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 1.171.13, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2188 _refine_ls_number_parameters 139 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0248 _refine_ls_wR_factor_ref 0.0380 _refine_ls_wR_factor_gt 0.0338 _refine_ls_goodness_of_fit_ref 0.675 _refine_ls_restrained_S_all 0.675 _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 Hf1 Hf 0.2500 0.2500 0.307071(13) 0.01244(8) Uani 1 4 d S . . O4 O 0.09895(17) 0.02697(17) 0.38640(10) 0.0174(7) Uani 1 1 d . . . O1 O 0.22209(15) 0.37035(16) 0.25740(10) 0.0145(7) Uani 1 1 d . . . O5 O 0.18729(16) 0.14321(16) 0.35756(10) 0.0147(7) Uani 1 1 d . . . O2 O 0.14796(18) 0.48675(19) 0.21628(11) 0.0243(8) Uani 1 1 d . . . C2 C 0.1583(3) 0.4272(3) 0.25963(18) 0.0159(10) Uani 1 1 d . . . C41 C 0.1574(3) 0.0037(2) 0.43478(18) 0.0192(10) Uani 1 1 d . . . C3 C 0.0930(2) 0.4358(2) 0.30109(16) 0.0166(12) Uani 1 1 d . . . H3A H 0.0482 0.4815 0.2975 0.020 Uiso 1 1 calc R . . C24 C 0.2517(6) 0.4324(2) 0.14086(13) 0.0394(10) Uani 1 1 d . . . H24A H 0.2002 0.4075 0.1199 0.059 Uiso 1 1 calc R . . H24B H 0.2774 0.3854 0.1654 0.059 Uiso 1 1 calc R . . H24C H 0.2979 0.4532 0.1141 0.059 Uiso 1 1 calc R . . C42 C 0.2483(4) -0.0296(2) 0.41371(14) 0.0297(9) Uani 1 1 d . . . H42A H 0.2392 -0.0803 0.3876 0.044 Uiso 1 1 calc R . . H42B H 0.2849 -0.0496 0.4460 0.044 Uiso 1 1 calc R . . H42C H 0.2795 0.0197 0.3940 0.044 Uiso 1 1 calc R . . C21 C 0.2202(3) 0.5112(3) 0.17681(18) 0.0225(13) Uani 1 1 d . . . C43 C 0.1645(3) 0.0833(3) 0.47526(15) 0.0284(12) Uani 1 1 d . . . H43A H 0.1038 0.1012 0.4876 0.043 Uiso 1 1 calc R . . H43B H 0.1937 0.1342 0.4560 0.043 Uiso 1 1 calc R . . H43C H 0.2006 0.0657 0.5083 0.043 Uiso 1 1 calc R . . C4 C 0.1207(3) 0.0914(3) 0.34768(16) 0.0139(12) Uani 1 1 d . . . C44 C 0.1047(3) -0.0734(3) 0.46188(15) 0.0243(11) Uani 1 1 d . . . H44A H 0.0465 -0.0506 0.4758 0.036 Uiso 1 1 calc R . . H44B H 0.1395 -0.0982 0.4936 0.036 Uiso 1 1 calc R . . H44C H 0.0941 -0.1209 0.4337 0.036 Uiso 1 1 calc R . . C23 C 0.1740(3) 0.5830(3) 0.14034(18) 0.0422(14) Uani 1 1 d . . . H23A H 0.1241 0.5553 0.1191 0.063 Uiso 1 1 calc R . . H23B H 0.2179 0.6087 0.1137 0.063 Uiso 1 1 calc R . . H23C H 0.1502 0.6311 0.1647 0.063 Uiso 1 1 calc R . . C22 C 0.2967(3) 0.5525(3) 0.20999(19) 0.0403(14) Uani 1 1 d . . . H22A H 0.2738 0.6032 0.2326 0.060 Uiso 1 1 calc R . . H22B H 0.3433 0.5744 0.1838 0.060 Uiso 1 1 calc R . . H22C H 0.3229 0.5067 0.2352 0.060 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 Hf1 0.01144(9) 0.01144(9) 0.01444(16) 0.000 0.000 0.000 O4 0.0198(16) 0.0158(15) 0.0167(17) 0.0048(13) 0.0004(13) -0.0043(13) O1 0.0165(19) 0.0118(14) 0.0151(15) 0.0012(11) -0.0001(11) 0.0006(11) O5 0.0127(15) 0.0176(15) 0.0136(14) -0.0012(12) 0.0009(11) -0.0042(12) O2 0.0183(17) 0.0268(18) 0.028(2) 0.0139(14) 0.0052(14) 0.0088(14) C2 0.023(3) 0.007(2) 0.018(3) -0.0030(19) -0.008(2) -0.0041(19) C41 0.019(2) 0.018(2) 0.021(3) 0.005(2) 0.001(2) 0.0023(18) C3 0.015(2) 0.020(3) 0.014(2) 0.002(2) -0.001(2) 0.009(2) C24 0.051(3) 0.042(3) 0.025(2) 0.013(2) 0.010(5) 0.006(6) C42 0.024(2) 0.032(2) 0.033(2) 0.0105(17) 0.001(5) -0.002(5) C21 0.027(3) 0.019(2) 0.021(3) 0.013(2) 0.002(2) 0.0035(19) C43 0.040(3) 0.027(3) 0.019(3) 0.008(2) 0.002(2) -0.010(2) C4 0.015(3) 0.012(2) 0.015(3) 0.0007(18) 0.0075(18) 0.004(2) C44 0.032(3) 0.021(2) 0.019(3) 0.0073(19) 0.007(2) -0.001(2) C23 0.030(3) 0.050(3) 0.047(4) 0.028(3) 0.006(3) 0.007(3) C22 0.034(3) 0.039(3) 0.049(4) 0.021(3) -0.005(3) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 O1 2.169(2) 4 ? Hf1 O1 2.169(2) 3 ? Hf1 O1 2.169(2) 2 ? Hf1 O1 2.169(2) . ? Hf1 O5 2.183(2) 2 ? Hf1 O5 2.183(2) 3 ? Hf1 O5 2.183(2) . ? Hf1 O5 2.183(2) 4 ? O4 C4 1.358(4) . ? O4 C41 1.472(4) . ? O1 C2 1.264(4) . ? O5 C4 1.268(4) . ? O2 C2 1.358(4) . ? O2 C21 1.462(4) . ? C2 C3 1.379(5) . ? C41 C42 1.513(6) . ? C41 C43 1.519(5) . ? C41 C44 1.520(5) . ? C3 C4 1.380(5) 4 ? C3 H3A 0.9500 . ? C24 C21 1.514(5) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C21 C22 1.504(5) . ? C21 C23 1.528(5) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C4 C3 1.380(5) 3 ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Hf1 O1 114.59(12) 4 3 ? O1 Hf1 O1 73.03(6) 4 2 ? O1 Hf1 O1 73.03(6) 3 2 ? O1 Hf1 O1 73.03(6) 4 . ? O1 Hf1 O1 73.03(6) 3 . ? O1 Hf1 O1 114.59(12) 2 . ? O1 Hf1 O5 79.02(8) 4 2 ? O1 Hf1 O5 141.26(8) 3 2 ? O1 Hf1 O5 143.76(8) 2 2 ? O1 Hf1 O5 77.47(8) . 2 ? O1 Hf1 O5 77.47(8) 4 3 ? O1 Hf1 O5 143.76(8) 3 3 ? O1 Hf1 O5 79.02(8) 2 3 ? O1 Hf1 O5 141.26(8) . 3 ? O5 Hf1 O5 72.68(6) 2 3 ? O1 Hf1 O5 141.26(8) 4 . ? O1 Hf1 O5 79.02(8) 3 . ? O1 Hf1 O5 77.47(8) 2 . ? O1 Hf1 O5 143.76(8) . . ? O5 Hf1 O5 113.86(12) 2 . ? O5 Hf1 O5 72.68(6) 3 . ? O1 Hf1 O5 143.76(8) 4 4 ? O1 Hf1 O5 77.47(8) 3 4 ? O1 Hf1 O5 141.26(8) 2 4 ? O1 Hf1 O5 79.02(8) . 4 ? O5 Hf1 O5 72.68(6) 2 4 ? O5 Hf1 O5 113.86(12) 3 4 ? O5 Hf1 O5 72.68(6) . 4 ? C4 O4 C41 123.2(3) . . ? C2 O1 Hf1 131.6(3) . . ? C4 O5 Hf1 131.7(2) . . ? C2 O2 C21 123.9(3) . . ? O1 C2 O2 118.9(4) . . ? O1 C2 C3 127.8(4) . . ? O2 C2 C3 113.3(4) . . ? O4 C41 C42 110.0(3) . . ? O4 C41 C43 110.3(3) . . ? C42 C41 C43 113.3(3) . . ? O4 C41 C44 101.6(3) . . ? C42 C41 C44 110.5(3) . . ? C43 C41 C44 110.5(3) . . ? C2 C3 C4 121.4(3) . 4 ? C2 C3 H3A 119.3 . . ? C4 C3 H3A 119.3 4 . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O2 C21 C22 108.5(3) . . ? O2 C21 C24 113.0(4) . . ? C22 C21 C24 111.9(4) . . ? O2 C21 C23 101.8(3) . . ? C22 C21 C23 110.4(4) . . ? C24 C21 C23 110.9(3) . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? O5 C4 O4 118.9(3) . . ? O5 C4 C3 127.2(4) . 3 ? O4 C4 C3 113.9(3) . 3 ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Hf1 O1 C2 -168.9(3) 4 . . . ? O1 Hf1 O1 C2 67.9(3) 3 . . . ? O1 Hf1 O1 C2 129.5(3) 2 . . . ? O5 Hf1 O1 C2 -86.7(3) 2 . . . ? O5 Hf1 O1 C2 -126.8(3) 3 . . . ? O5 Hf1 O1 C2 26.7(4) . . . . ? O5 Hf1 O1 C2 -12.2(3) 4 . . . ? O1 Hf1 O5 C4 -106.5(3) 4 . . . ? O1 Hf1 O5 C4 9.3(3) 3 . . . ? O1 Hf1 O5 C4 -65.5(3) 2 . . . ? O1 Hf1 O5 C4 49.2(4) . . . . ? O5 Hf1 O5 C4 150.9(3) 2 . . . ? O5 Hf1 O5 C4 -147.8(3) 3 . . . ? O5 Hf1 O5 C4 89.5(3) 4 . . . ? Hf1 O1 C2 O2 -167.4(2) . . . . ? Hf1 O1 C2 C3 10.5(6) . . . . ? C21 O2 C2 O1 -21.3(5) . . . . ? C21 O2 C2 C3 160.5(4) . . . . ? C4 O4 C41 C42 -60.3(4) . . . . ? C4 O4 C41 C43 65.5(4) . . . . ? C4 O4 C41 C44 -177.3(3) . . . . ? O1 C2 C3 C4 0.4(6) . . . 4 ? O2 C2 C3 C4 178.4(3) . . . 4 ? C2 O2 C21 C22 -60.2(5) . . . . ? C2 O2 C21 C24 64.5(5) . . . . ? C2 O2 C21 C23 -176.6(3) . . . . ? Hf1 O5 C4 O4 176.7(2) . . . . ? Hf1 O5 C4 C3 -4.3(5) . . . 3 ? C41 O4 C4 O5 -10.6(5) . . . . ? C41 O4 C4 C3 170.3(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.520 _refine_diff_density_min -0.584 _refine_diff_density_rms 0.083 #=================================END data_cvd220 _database_code_depnum_ccdc_archive 'CCDC 692636' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H52 O16 Zr' _chemical_formula_weight 819.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 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 15.2848(7) _cell_length_b 18.3600(7) _cell_length_c 15.8340(8) _cell_angle_alpha 90.00 _cell_angle_beta 117.278(6) _cell_angle_gamma 90.00 _cell_volume 3949.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 105(2) _cell_measurement_reflns_used 4500 _cell_measurement_theta_min 2.577 _cell_measurement_theta_max 27.498 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 0.347 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.930 _exptl_absorpt_correction_T_max 0.958 _exptl_absorpt_process_details 'Gaussian face-indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 105(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Sapphire2-CCD, Oxford Diffraction' _diffrn_measurement_method '369 images at 1.0 deg. in \w and 15 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19872 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6934 _reflns_number_gt 4147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD 171.32.11, Oxford Diffraction' _computing_cell_refinement 'CrysAlis RED 171.32.11, Oxford Diffraction' _computing_data_reduction 'CrysAlis RED 171.32.11, Oxford Diffraction' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXL-97 _computing_publication_material SHELXL-97 _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^)+(0.0289P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6934 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0716 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0738 _refine_ls_wR_factor_gt 0.0686 _refine_ls_goodness_of_fit_ref 0.793 _refine_ls_restrained_S_all 0.793 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.74536(2) 0.890419(16) 0.25411(2) 0.02081(9) Uani 1 1 d . . . O11 O 0.65539(14) 0.79999(11) 0.16330(13) 0.0234(5) Uani 1 1 d . . . C12 C 0.5638(2) 0.79073(18) 0.1149(2) 0.0239(8) Uani 1 1 d . . . O121 O 0.52966(14) 0.72363(11) 0.08297(14) 0.0290(5) Uani 1 1 d . . . C122 C 0.5969(2) 0.66269(18) 0.1139(2) 0.0313(8) Uani 1 1 d . . . H12A H 0.6648 0.6801 0.1332 0.038 Uiso 1 1 calc R . . H12B H 0.5792 0.6279 0.0607 0.038 Uiso 1 1 calc R . . C123 C 0.5927(3) 0.62529(19) 0.1954(2) 0.0448(10) Uani 1 1 d . . . H12C H 0.6171 0.6582 0.2502 0.067 Uiso 1 1 calc R . . H12D H 0.6338 0.5814 0.2119 0.067 Uiso 1 1 calc R . . H12E H 0.5245 0.6116 0.1777 0.067 Uiso 1 1 calc R . . C13 C 0.4923(2) 0.84411(18) 0.0881(2) 0.0251(8) Uani 1 1 d . . . H13 H 0.4249 0.8313 0.0524 0.030 Uiso 1 1 calc R . . C14 C 0.5180(2) 0.91524(18) 0.1128(2) 0.0219(7) Uani 1 1 d . . . O141 O 0.44446(14) 0.96420(11) 0.07778(13) 0.0258(5) Uani 1 1 d . . . C142 C 0.4694(2) 1.03956(17) 0.1056(2) 0.0275(8) Uani 1 1 d . . . H14A H 0.5187 1.0572 0.0861 0.033 Uiso 1 1 calc R . . H14B H 0.4971 1.0448 0.1753 0.033 Uiso 1 1 calc R . . C143 C 0.3757(2) 1.08209(17) 0.0562(2) 0.0328(8) Uani 1 1 d . . . H14C H 0.3478 1.0749 -0.0126 0.049 Uiso 1 1 calc R . . H14D H 0.3893 1.1340 0.0710 0.049 Uiso 1 1 calc R . . H14E H 0.3285 1.0652 0.0779 0.049 Uiso 1 1 calc R . . O15 O 0.60437(14) 0.93906(11) 0.16293(13) 0.0225(5) Uani 1 1 d . . . O21 O 0.65694(14) 0.85052(11) 0.32083(13) 0.0231(5) Uani 1 1 d . . . C22 C 0.6057(2) 0.88146(18) 0.35400(19) 0.0223(7) Uani 1 1 d . . . O221 O 0.53799(14) 0.84191(11) 0.36583(14) 0.0276(5) Uani 1 1 d . . . C222 C 0.5187(2) 0.76971(17) 0.3252(2) 0.0316(8) Uani 1 1 d . . . H22A H 0.5778 0.7387 0.3577 0.038 Uiso 1 1 calc R . . H22B H 0.5011 0.7720 0.2568 0.038 Uiso 1 1 calc R . . C223 C 0.4348(2) 0.73885(18) 0.3382(2) 0.0343(8) Uani 1 1 d . . . H22C H 0.4530 0.7370 0.4061 0.051 Uiso 1 1 calc R . . H22D H 0.4199 0.6896 0.3116 0.051 Uiso 1 1 calc R . . H22E H 0.3766 0.7698 0.3055 0.051 Uiso 1 1 calc R . . C23 C 0.6115(2) 0.95378(17) 0.3805(2) 0.0269(8) Uani 1 1 d . . . H23 H 0.5697 0.9721 0.4052 0.032 Uiso 1 1 calc R . . C24 C 0.6786(2) 0.99939(18) 0.3707(2) 0.0237(8) Uani 1 1 d . . . O241 O 0.67784(15) 1.06844(12) 0.39771(14) 0.0295(5) Uani 1 1 d . . . C242 C 0.7383(2) 1.12009(17) 0.3801(2) 0.0282(8) Uani 1 1 d . . . H24A H 0.7170 1.1242 0.3110 0.034 Uiso 1 1 calc R . . H24B H 0.8081 1.1046 0.4120 0.034 Uiso 1 1 calc R . . C243 C 0.7262(2) 1.19175(18) 0.4192(2) 0.0401(9) Uani 1 1 d . . . H24C H 0.6569 1.2065 0.3866 0.060 Uiso 1 1 calc R . . H24D H 0.7667 1.2287 0.4092 0.060 Uiso 1 1 calc R . . H24E H 0.7470 1.1867 0.4874 0.060 Uiso 1 1 calc R . . O25 O 0.73814(14) 0.98185(11) 0.33929(13) 0.0217(5) Uani 1 1 d . . . O31 O 0.89517(14) 0.92635(11) 0.34758(13) 0.0254(5) Uani 1 1 d . . . C32 C 0.9772(2) 0.89459(19) 0.3902(2) 0.0285(8) Uani 1 1 d . . . O321 O 1.05918(15) 0.93568(13) 0.42856(17) 0.0436(7) Uani 1 1 d . . . C322 C 1.0505(3) 1.0139(2) 0.4168(3) 0.0482(11) Uani 1 1 d . . . H32A H 0.9814 1.0290 0.3955 0.058 Uiso 1 1 calc R . . H32B H 1.0921 1.0382 0.4781 0.058 Uiso 1 1 calc R . . C323 C 1.0816(4) 1.0350(2) 0.3474(3) 0.0746(14) Uani 1 1 d . . . H32C H 1.1524 1.0261 0.3727 0.112 Uiso 1 1 calc R . . H32D H 1.0681 1.0869 0.3328 0.112 Uiso 1 1 calc R . . H32E H 1.0457 1.0063 0.2893 0.112 Uiso 1 1 calc R . . C33 C 0.9913(2) 0.82039(18) 0.4038(2) 0.0321(8) Uani 1 1 d . . . H33 H 1.0560 0.8009 0.4340 0.039 Uiso 1 1 calc R . . C34 C 0.9111(2) 0.77466(18) 0.3735(2) 0.0252(8) Uani 1 1 d . . . O341 O 0.93273(14) 0.70411(12) 0.39113(14) 0.0308(5) Uani 1 1 d . . . C342 C 0.8532(2) 0.65232(17) 0.3556(2) 0.0327(8) Uani 1 1 d . . . H34A H 0.8130 0.6581 0.2861 0.039 Uiso 1 1 calc R . . H34B H 0.8103 0.6599 0.3863 0.039 Uiso 1 1 calc R . . C343 C 0.8987(3) 0.57752(17) 0.3784(2) 0.0385(9) Uani 1 1 d . . . H34C H 0.9420 0.5711 0.3487 0.058 Uiso 1 1 calc R . . H34D H 0.8465 0.5406 0.3539 0.058 Uiso 1 1 calc R . . H34E H 0.9370 0.5721 0.4474 0.058 Uiso 1 1 calc R . . O35 O 0.82098(14) 0.79311(11) 0.33316(13) 0.0228(5) Uani 1 1 d . . . O41 O 0.76965(14) 0.98566(11) 0.18478(13) 0.0228(5) Uani 1 1 d . . . C42 C 0.8255(2) 0.99874(18) 0.1482(2) 0.0245(8) Uani 1 1 d . . . O421 O 0.83933(16) 1.06809(12) 0.13084(16) 0.0356(6) Uani 1 1 d . . . C422 C 0.7931(3) 1.1227(2) 0.1625(3) 0.0517(11) Uani 1 1 d . . . H42A H 0.7206 1.1200 0.1244 0.062 Uiso 1 1 calc R . . H42B H 0.8100 1.1145 0.2300 0.062 Uiso 1 1 calc R . . C423 C 0.8274(4) 1.1928(3) 0.1513(5) 0.120(2) Uani 1 1 d . . . H42C H 0.8996 1.1931 0.1826 0.180 Uiso 1 1 calc R . . H42D H 0.8036 1.2300 0.1801 0.180 Uiso 1 1 calc R . . H42E H 0.8027 1.2033 0.0835 0.180 Uiso 1 1 calc R . . C43 C 0.8741(2) 0.94759(18) 0.1199(2) 0.0292(8) Uani 1 1 d . . . H43 H 0.9153 0.9627 0.0929 0.035 Uiso 1 1 calc R . . C44 C 0.8615(2) 0.87499(18) 0.1317(2) 0.0270(8) Uani 1 1 d . . . O441 O 0.90020(15) 0.82812(12) 0.09245(15) 0.0340(6) Uani 1 1 d . . . C442 C 0.8891(2) 0.75081(17) 0.1037(2) 0.0353(9) Uani 1 1 d . . . H44A H 0.9008 0.7410 0.1695 0.042 Uiso 1 1 calc R . . H44B H 0.9389 0.7235 0.0928 0.042 Uiso 1 1 calc R . . C443 C 0.7874(2) 0.72477(18) 0.0347(2) 0.0387(9) Uani 1 1 d . . . H44C H 0.7383 0.7495 0.0480 0.058 Uiso 1 1 calc R . . H44D H 0.7828 0.6721 0.0416 0.058 Uiso 1 1 calc R . . H44E H 0.7750 0.7358 -0.0304 0.058 Uiso 1 1 calc R . . O45 O 0.81658(14) 0.84823(11) 0.17396(13) 0.0239(5) Uani 1 1 d . . . C90 C 0.6525(3) 1.0703(2) -0.3876(3) 0.0593(12) Uani 1 1 d . . . H90A H 0.6283 1.0201 -0.3946 0.089 Uiso 1 1 calc R . . H90B H 0.6914 1.0762 -0.4220 0.089 Uiso 1 1 calc R . . H90C H 0.5965 1.1039 -0.4135 0.089 Uiso 1 1 calc R . . C91 C 0.7158(3) 1.08669(18) -0.2841(3) 0.0390(9) Uani 1 1 d . . . C92 C 0.6822(2) 1.07567(18) -0.2176(2) 0.0340(8) Uani 1 1 d . . . H92 H 0.6177 1.0569 -0.2381 0.041 Uiso 1 1 calc R . . C93 C 0.7391(2) 1.09104(17) -0.1227(2) 0.0352(9) Uani 1 1 d . . . H93 H 0.7137 1.0830 -0.0787 0.042 Uiso 1 1 calc R . . C94 C 0.8332(2) 1.11814(19) -0.0915(3) 0.0442(10) Uani 1 1 d . . . H94 H 0.8733 1.1287 -0.0262 0.053 Uiso 1 1 calc R . . C95 C 0.8678(3) 1.12952(19) -0.1565(4) 0.0566(12) Uani 1 1 d . . . H95 H 0.9322 1.1484 -0.1357 0.068 Uiso 1 1 calc R . . C96 C 0.8106(3) 1.1141(2) -0.2514(3) 0.0486(10) Uani 1 1 d . . . H96 H 0.8363 1.1223 -0.2950 0.058 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 0.01672(14) 0.01908(15) 0.02403(15) -0.00028(16) 0.00709(11) 0.00069(16) O11 0.0166(11) 0.0228(13) 0.0273(12) -0.0041(10) 0.0071(10) -0.0003(10) C12 0.0269(19) 0.024(2) 0.0213(17) -0.0015(15) 0.0115(16) -0.0069(16) O121 0.0246(12) 0.0187(13) 0.0368(13) -0.0038(10) 0.0080(11) -0.0029(10) C122 0.0313(19) 0.026(2) 0.0338(19) -0.0053(16) 0.0123(17) 0.0012(16) C123 0.038(2) 0.037(2) 0.063(2) 0.0142(19) 0.026(2) 0.0072(18) C13 0.0161(16) 0.022(2) 0.0322(19) -0.0011(15) 0.0070(15) 0.0002(15) C14 0.0160(17) 0.030(2) 0.0184(16) 0.0037(14) 0.0069(15) 0.0030(15) O141 0.0178(11) 0.0228(14) 0.0310(12) 0.0011(10) 0.0063(10) 0.0026(10) C142 0.0220(17) 0.024(2) 0.0310(18) -0.0039(15) 0.0070(15) 0.0003(15) C143 0.0276(18) 0.026(2) 0.0361(19) -0.0046(15) 0.0067(16) 0.0055(15) O15 0.0180(11) 0.0214(13) 0.0242(12) 0.0011(9) 0.0062(10) -0.0002(10) O21 0.0221(11) 0.0229(13) 0.0261(12) 0.0011(9) 0.0125(10) 0.0029(10) C22 0.0174(15) 0.027(2) 0.0204(15) 0.0014(15) 0.0068(14) -0.0005(15) O221 0.0286(12) 0.0239(13) 0.0344(12) -0.0038(10) 0.0181(11) -0.0045(10) C222 0.0288(18) 0.0212(19) 0.042(2) 0.0005(15) 0.0143(17) -0.0041(15) C223 0.0307(19) 0.036(2) 0.0319(19) 0.0013(16) 0.0108(16) -0.0071(16) C23 0.0240(17) 0.024(2) 0.038(2) -0.0070(16) 0.0184(16) -0.0011(15) C24 0.0172(16) 0.026(2) 0.0220(17) -0.0046(14) 0.0039(15) 0.0031(15) O241 0.0314(12) 0.0226(14) 0.0406(13) -0.0089(10) 0.0218(11) -0.0062(11) C242 0.0221(16) 0.026(2) 0.0361(18) -0.0003(15) 0.0129(15) -0.0024(15) C243 0.038(2) 0.025(2) 0.055(2) -0.0041(17) 0.0190(19) -0.0019(17) O25 0.0179(11) 0.0217(13) 0.0261(11) -0.0027(9) 0.0107(10) -0.0015(9) O31 0.0168(11) 0.0244(13) 0.0287(12) -0.0023(10) 0.0052(10) 0.0016(10) C32 0.0173(16) 0.033(2) 0.0329(18) -0.0037(18) 0.0092(15) -0.0055(18) O321 0.0195(12) 0.0257(15) 0.0697(17) 0.0033(13) 0.0068(13) -0.0011(11) C322 0.026(2) 0.035(3) 0.072(3) -0.003(2) 0.013(2) -0.0033(18) C323 0.128(4) 0.040(3) 0.079(3) -0.001(2) 0.068(3) 0.002(3) C33 0.0182(17) 0.024(2) 0.047(2) 0.0042(16) 0.0089(17) 0.0051(15) C34 0.0241(19) 0.024(2) 0.0276(18) 0.0000(15) 0.0118(16) 0.0052(16) O341 0.0212(11) 0.0214(13) 0.0453(13) 0.0037(11) 0.0114(11) 0.0035(10) C342 0.0288(18) 0.026(2) 0.041(2) 0.0022(16) 0.0134(17) -0.0014(16) C343 0.042(2) 0.024(2) 0.052(2) -0.0028(17) 0.0235(19) 0.0001(17) O35 0.0169(11) 0.0216(12) 0.0257(11) 0.0045(10) 0.0062(10) 0.0027(10) O41 0.0180(11) 0.0249(13) 0.0260(11) 0.0031(9) 0.0107(10) 0.0019(10) C42 0.0230(17) 0.025(2) 0.0201(17) -0.0026(14) 0.0053(15) -0.0043(15) O421 0.0417(14) 0.0228(14) 0.0551(15) -0.0014(11) 0.0332(13) -0.0063(11) C422 0.063(3) 0.029(2) 0.083(3) 0.005(2) 0.051(2) 0.006(2) C423 0.127(5) 0.045(3) 0.250(7) -0.031(4) 0.138(5) -0.012(3) C43 0.0226(17) 0.033(2) 0.038(2) -0.0077(17) 0.0189(16) -0.0077(16) C44 0.0172(16) 0.035(2) 0.0254(17) -0.0103(16) 0.0068(15) -0.0012(15) O441 0.0302(12) 0.0319(15) 0.0486(14) -0.0117(11) 0.0255(12) -0.0065(11) C442 0.035(2) 0.026(2) 0.048(2) -0.0091(17) 0.0223(18) 0.0001(16) C443 0.045(2) 0.033(2) 0.044(2) -0.0109(17) 0.0259(18) -0.0116(18) O45 0.0232(11) 0.0249(13) 0.0245(12) -0.0015(10) 0.0118(10) 0.0009(10) C90 0.059(3) 0.070(3) 0.059(3) 0.007(2) 0.036(2) 0.012(2) C91 0.036(2) 0.030(2) 0.058(2) 0.0108(17) 0.0275(19) 0.0094(16) C92 0.0259(18) 0.031(2) 0.048(2) 0.0021(17) 0.0193(18) 0.0003(16) C93 0.0281(18) 0.028(2) 0.050(2) -0.0002(16) 0.0191(18) 0.0028(15) C94 0.0269(19) 0.030(2) 0.067(2) -0.010(2) 0.0135(19) -0.0002(17) C95 0.024(2) 0.032(3) 0.114(4) -0.001(2) 0.032(3) -0.0012(17) C96 0.048(2) 0.031(2) 0.088(3) 0.021(2) 0.049(2) 0.011(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 O45 2.159(2) . ? Zr1 O15 2.1620(19) . ? Zr1 O31 2.182(2) . ? Zr1 O35 2.184(2) . ? Zr1 O41 2.185(2) . ? Zr1 O25 2.188(2) . ? Zr1 O21 2.188(2) . ? Zr1 O11 2.214(2) . ? O11 C12 1.262(3) . ? C12 O121 1.343(3) . ? C12 C13 1.383(4) . ? O121 C122 1.445(4) . ? C122 C123 1.489(4) . ? C122 H12A 0.9900 . ? C122 H12B 0.9900 . ? C123 H12C 0.9800 . ? C123 H12D 0.9800 . ? C123 H12E 0.9800 . ? C13 C14 1.368(4) . ? C13 H13 0.9500 . ? C14 O15 1.267(3) . ? C14 O141 1.344(3) . ? O141 C142 1.449(3) . ? C142 C143 1.499(4) . ? C142 H14A 0.9900 . ? C142 H14B 0.9900 . ? C143 H14C 0.9800 . ? C143 H14D 0.9800 . ? C143 H14E 0.9800 . ? O21 C22 1.260(3) . ? C22 O221 1.346(3) . ? C22 C23 1.383(4) . ? O221 C222 1.444(3) . ? C222 C223 1.500(4) . ? C222 H22A 0.9900 . ? C222 H22B 0.9900 . ? C223 H22C 0.9800 . ? C223 H22D 0.9800 . ? C223 H22E 0.9800 . ? C23 C24 1.386(4) . ? C23 H23 0.9500 . ? C24 O25 1.264(3) . ? C24 O241 1.339(3) . ? O241 C242 1.438(3) . ? C242 C243 1.502(4) . ? C242 H24A 0.9900 . ? C242 H24B 0.9900 . ? C243 H24C 0.9800 . ? C243 H24D 0.9800 . ? C243 H24E 0.9800 . ? O31 C32 1.262(3) . ? C32 O321 1.346(4) . ? C32 C33 1.380(4) . ? O321 C322 1.447(4) . ? C322 C323 1.436(5) . ? C322 H32A 0.9900 . ? C322 H32B 0.9900 . ? C323 H32C 0.9800 . ? C323 H32D 0.9800 . ? C323 H32E 0.9800 . ? C33 C34 1.377(4) . ? C33 H33 0.9500 . ? C34 O35 1.271(3) . ? C34 O341 1.334(4) . ? O341 C342 1.439(4) . ? C342 C343 1.506(4) . ? C342 H34A 0.9900 . ? C342 H34B 0.9900 . ? C343 H34C 0.9800 . ? C343 H34D 0.9800 . ? C343 H34E 0.9800 . ? O41 C42 1.255(3) . ? C42 O421 1.340(4) . ? C42 C43 1.393(4) . ? O421 C422 1.443(4) . ? C422 C423 1.431(5) . ? C422 H42A 0.9900 . ? C422 H42B 0.9900 . ? C423 H42C 0.9800 . ? C423 H42D 0.9800 . ? C423 H42E 0.9800 . ? C43 C44 1.372(4) . ? C43 H43 0.9500 . ? C44 O45 1.259(3) . ? C44 O441 1.346(3) . ? O441 C442 1.450(4) . ? C442 C443 1.511(4) . ? C442 H44A 0.9900 . ? C442 H44B 0.9900 . ? C443 H44C 0.9800 . ? C443 H44D 0.9800 . ? C443 H44E 0.9800 . ? C90 C91 1.503(5) . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 C92 1.382(4) . ? C91 C96 1.391(5) . ? C92 C93 1.378(4) . ? C92 H92 0.9500 . ? C93 C94 1.382(5) . ? C93 H93 0.9500 . ? C94 C95 1.371(5) . ? C94 H94 0.9500 . ? C95 C96 1.377(5) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? 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 O45 Zr1 O15 111.87(7) . . ? O45 Zr1 O31 81.50(7) . . ? O15 Zr1 O31 137.98(7) . . ? O45 Zr1 O35 76.49(7) . . ? O15 Zr1 O35 145.53(8) . . ? O31 Zr1 O35 75.13(8) . . ? O45 Zr1 O41 75.18(8) . . ? O15 Zr1 O41 71.39(7) . . ? O31 Zr1 O41 74.44(7) . . ? O35 Zr1 O41 140.86(8) . . ? O45 Zr1 O25 145.00(8) . . ? O15 Zr1 O25 77.19(7) . . ? O31 Zr1 O25 71.55(7) . . ? O35 Zr1 O25 115.94(7) . . ? O41 Zr1 O25 76.34(7) . . ? O45 Zr1 O21 138.86(7) . . ? O15 Zr1 O21 79.25(7) . . ? O31 Zr1 O21 117.52(7) . . ? O35 Zr1 O21 74.40(7) . . ? O41 Zr1 O21 142.68(8) . . ? O25 Zr1 O21 75.07(8) . . ? O45 Zr1 O11 71.32(7) . . ? O15 Zr1 O11 75.15(7) . . ? O31 Zr1 O11 144.43(8) . . ? O35 Zr1 O11 76.51(7) . . ? O41 Zr1 O11 118.15(7) . . ? O25 Zr1 O11 141.63(7) . . ? O21 Zr1 O11 74.06(7) . . ? C12 O11 Zr1 132.9(2) . . ? O11 C12 O121 118.9(3) . . ? O11 C12 C13 126.3(3) . . ? O121 C12 C13 114.7(3) . . ? C12 O121 C122 119.3(2) . . ? O121 C122 C123 110.1(3) . . ? O121 C122 H12A 109.6 . . ? C123 C122 H12A 109.6 . . ? O121 C122 H12B 109.6 . . ? C123 C122 H12B 109.6 . . ? H12A C122 H12B 108.2 . . ? C122 C123 H12C 109.5 . . ? C122 C123 H12D 109.5 . . ? H12C C123 H12D 109.5 . . ? C122 C123 H12E 109.5 . . ? H12C C123 H12E 109.5 . . ? H12D C123 H12E 109.5 . . ? C14 C13 C12 120.4(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? O15 C14 O141 117.5(3) . . ? O15 C14 C13 126.1(3) . . ? O141 C14 C13 116.4(3) . . ? C14 O141 C142 117.4(2) . . ? O141 C142 C143 106.5(2) . . ? O141 C142 H14A 110.4 . . ? C143 C142 H14A 110.4 . . ? O141 C142 H14B 110.4 . . ? C143 C142 H14B 110.4 . . ? H14A C142 H14B 108.6 . . ? C142 C143 H14C 109.5 . . ? C142 C143 H14D 109.5 . . ? H14C C143 H14D 109.5 . . ? C142 C143 H14E 109.5 . . ? H14C C143 H14E 109.5 . . ? H14D C143 H14E 109.5 . . ? C14 O15 Zr1 135.2(2) . . ? C22 O21 Zr1 133.6(2) . . ? O21 C22 O221 118.6(3) . . ? O21 C22 C23 126.4(3) . . ? O221 C22 C23 114.9(3) . . ? C22 O221 C222 116.5(2) . . ? O221 C222 C223 107.4(3) . . ? O221 C222 H22A 110.2 . . ? C223 C222 H22A 110.2 . . ? O221 C222 H22B 110.2 . . ? C223 C222 H22B 110.2 . . ? H22A C222 H22B 108.5 . . ? C222 C223 H22C 109.5 . . ? C222 C223 H22D 109.5 . . ? H22C C223 H22D 109.5 . . ? C222 C223 H22E 109.5 . . ? H22C C223 H22E 109.5 . . ? H22D C223 H22E 109.5 . . ? C22 C23 C24 119.6(3) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? O25 C24 O241 118.7(3) . . ? O25 C24 C23 126.4(3) . . ? O241 C24 C23 114.9(3) . . ? C24 O241 C242 117.5(2) . . ? O241 C242 C243 106.6(3) . . ? O241 C242 H24A 110.4 . . ? C243 C242 H24A 110.4 . . ? O241 C242 H24B 110.4 . . ? C243 C242 H24B 110.4 . . ? H24A C242 H24B 108.6 . . ? C242 C243 H24C 109.5 . . ? C242 C243 H24D 109.5 . . ? H24C C243 H24D 109.5 . . ? C242 C243 H24E 109.5 . . ? H24C C243 H24E 109.5 . . ? H24D C243 H24E 109.5 . . ? C24 O25 Zr1 133.44(19) . . ? C32 O31 Zr1 134.4(2) . . ? O31 C32 O321 118.3(3) . . ? O31 C32 C33 125.8(3) . . ? O321 C32 C33 115.9(3) . . ? C32 O321 C322 119.2(3) . . ? C323 C322 O321 108.8(3) . . ? C323 C322 H32A 109.9 . . ? O321 C322 H32A 109.9 . . ? C323 C322 H32B 109.9 . . ? O321 C322 H32B 109.9 . . ? H32A C322 H32B 108.3 . . ? C322 C323 H32C 109.5 . . ? C322 C323 H32D 109.5 . . ? H32C C323 H32D 109.5 . . ? C322 C323 H32E 109.5 . . ? H32C C323 H32E 109.5 . . ? H32D C323 H32E 109.5 . . ? C34 C33 C32 119.8(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? O35 C34 O341 118.1(3) . . ? O35 C34 C33 126.8(3) . . ? O341 C34 C33 115.1(3) . . ? C34 O341 C342 118.4(2) . . ? O341 C342 C343 107.1(2) . . ? O341 C342 H34A 110.3 . . ? C343 C342 H34A 110.3 . . ? O341 C342 H34B 110.3 . . ? C343 C342 H34B 110.3 . . ? H34A C342 H34B 108.5 . . ? C342 C343 H34C 109.5 . . ? C342 C343 H34D 109.5 . . ? H34C C343 H34D 109.5 . . ? C342 C343 H34E 109.5 . . ? H34C C343 H34E 109.5 . . ? H34D C343 H34E 109.5 . . ? C34 O35 Zr1 132.3(2) . . ? C42 O41 Zr1 133.9(2) . . ? O41 C42 O421 118.8(3) . . ? O41 C42 C43 126.6(3) . . ? O421 C42 C43 114.6(3) . . ? C42 O421 C422 116.2(3) . . ? C423 C422 O421 108.4(3) . . ? C423 C422 H42A 110.0 . . ? O421 C422 H42A 110.0 . . ? C423 C422 H42B 110.0 . . ? O421 C422 H42B 110.0 . . ? H42A C422 H42B 108.4 . . ? C422 C423 H42C 109.5 . . ? C422 C423 H42D 109.5 . . ? H42C C423 H42D 109.5 . . ? C422 C423 H42E 109.5 . . ? H42C C423 H42E 109.5 . . ? H42D C423 H42E 109.5 . . ? C44 C43 C42 118.8(3) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? O45 C44 O441 117.3(3) . . ? O45 C44 C43 126.6(3) . . ? O441 C44 C43 116.1(3) . . ? C44 O441 C442 118.0(3) . . ? O441 C442 C443 111.1(3) . . ? O441 C442 H44A 109.4 . . ? C443 C442 H44A 109.4 . . ? O441 C442 H44B 109.4 . . ? C443 C442 H44B 109.4 . . ? H44A C442 H44B 108.0 . . ? C442 C443 H44C 109.5 . . ? C442 C443 H44D 109.5 . . ? H44C C443 H44D 109.5 . . ? C442 C443 H44E 109.5 . . ? H44C C443 H44E 109.5 . . ? H44D C443 H44E 109.5 . . ? C44 O45 Zr1 135.9(2) . . ? C91 C90 H90A 109.5 . . ? C91 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C91 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C92 C91 C96 117.2(4) . . ? C92 C91 C90 121.5(3) . . ? C96 C91 C90 121.3(4) . . ? C93 C92 C91 122.2(3) . . ? C93 C92 H92 118.9 . . ? C91 C92 H92 118.9 . . ? C92 C93 C94 119.7(4) . . ? C92 C93 H93 120.1 . . ? C94 C93 H93 120.1 . . ? C95 C94 C93 118.9(3) . . ? C95 C94 H94 120.5 . . ? C93 C94 H94 120.5 . . ? C94 C95 C96 121.2(3) . . ? C94 C95 H95 119.4 . . ? C96 C95 H95 119.4 . . ? C95 C96 C91 120.8(4) . . ? C95 C96 H96 119.6 . . ? C91 C96 H96 119.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O45 Zr1 O11 C12 -140.0(3) . . . . ? O15 Zr1 O11 C12 -20.2(3) . . . . ? O31 Zr1 O11 C12 177.9(2) . . . . ? O35 Zr1 O11 C12 140.0(3) . . . . ? O41 Zr1 O11 C12 -79.1(3) . . . . ? O25 Zr1 O11 C12 25.0(3) . . . . ? O21 Zr1 O11 C12 62.6(3) . . . . ? Zr1 O11 C12 O121 -165.88(18) . . . . ? Zr1 O11 C12 C13 16.0(5) . . . . ? O11 C12 O121 C122 7.2(4) . . . . ? C13 C12 O121 C122 -174.4(3) . . . . ? C12 O121 C122 C123 96.4(3) . . . . ? O11 C12 C13 C14 1.0(5) . . . . ? O121 C12 C13 C14 -177.2(3) . . . . ? C12 C13 C14 O15 -2.8(5) . . . . ? C12 C13 C14 O141 175.2(3) . . . . ? O15 C14 O141 C142 -4.0(4) . . . . ? C13 C14 O141 C142 177.9(3) . . . . ? C14 O141 C142 C143 179.2(3) . . . . ? O141 C14 O15 Zr1 168.72(17) . . . . ? C13 C14 O15 Zr1 -13.4(5) . . . . ? O45 Zr1 O15 C14 81.6(3) . . . . ? O31 Zr1 O15 C14 -176.4(2) . . . . ? O35 Zr1 O15 C14 -16.4(3) . . . . ? O41 Zr1 O15 C14 146.4(3) . . . . ? O25 Zr1 O15 C14 -133.9(3) . . . . ? O21 Zr1 O15 C14 -56.9(3) . . . . ? O11 Zr1 O15 C14 19.2(3) . . . . ? O45 Zr1 O21 C22 -166.9(2) . . . . ? O15 Zr1 O21 C22 -55.9(2) . . . . ? O31 Zr1 O21 C22 83.0(2) . . . . ? O35 Zr1 O21 C22 146.5(2) . . . . ? O41 Zr1 O21 C22 -17.6(3) . . . . ? O25 Zr1 O21 C22 23.5(2) . . . . ? O11 Zr1 O21 C22 -133.4(2) . . . . ? Zr1 O21 C22 O221 161.25(17) . . . . ? Zr1 O21 C22 C23 -18.8(4) . . . . ? O21 C22 O221 C222 -9.6(4) . . . . ? C23 C22 O221 C222 170.4(2) . . . . ? C22 O221 C222 C223 -174.5(2) . . . . ? O21 C22 C23 C24 0.3(5) . . . . ? O221 C22 C23 C24 -179.7(3) . . . . ? C22 C23 C24 O25 -0.2(5) . . . . ? C22 C23 C24 O241 179.5(3) . . . . ? O25 C24 O241 C242 6.2(4) . . . . ? C23 C24 O241 C242 -173.6(2) . . . . ? C24 O241 C242 C243 -178.4(2) . . . . ? O241 C24 O25 Zr1 -161.22(18) . . . . ? C23 C24 O25 Zr1 18.6(4) . . . . ? O45 Zr1 O25 C24 168.7(2) . . . . ? O15 Zr1 O25 C24 58.7(2) . . . . ? O31 Zr1 O25 C24 -149.8(3) . . . . ? O35 Zr1 O25 C24 -87.3(3) . . . . ? O41 Zr1 O25 C24 132.4(3) . . . . ? O21 Zr1 O25 C24 -23.4(2) . . . . ? O11 Zr1 O25 C24 14.0(3) . . . . ? O45 Zr1 O31 C32 -56.2(3) . . . . ? O15 Zr1 O31 C32 -169.6(2) . . . . ? O35 Zr1 O31 C32 22.0(3) . . . . ? O41 Zr1 O31 C32 -133.1(3) . . . . ? O25 Zr1 O31 C32 146.4(3) . . . . ? O21 Zr1 O31 C32 85.1(3) . . . . ? O11 Zr1 O31 C32 -16.2(3) . . . . ? Zr1 O31 C32 O321 167.67(19) . . . . ? Zr1 O31 C32 C33 -14.2(5) . . . . ? O31 C32 O321 C322 -2.1(5) . . . . ? C33 C32 O321 C322 179.6(3) . . . . ? C32 O321 C322 C323 -105.0(4) . . . . ? O31 C32 C33 C34 -3.2(5) . . . . ? O321 C32 C33 C34 175.0(3) . . . . ? C32 C33 C34 O35 -0.8(5) . . . . ? C32 C33 C34 O341 -179.2(3) . . . . ? O35 C34 O341 C342 5.9(4) . . . . ? C33 C34 O341 C342 -175.6(3) . . . . ? C34 O341 C342 C343 175.4(3) . . . . ? O341 C34 O35 Zr1 -159.84(19) . . . . ? C33 C34 O35 Zr1 21.8(5) . . . . ? O45 Zr1 O35 C34 59.4(3) . . . . ? O15 Zr1 O35 C34 168.5(2) . . . . ? O31 Zr1 O35 C34 -25.2(3) . . . . ? O41 Zr1 O35 C34 14.8(3) . . . . ? O25 Zr1 O35 C34 -85.7(3) . . . . ? O21 Zr1 O35 C34 -150.0(3) . . . . ? O11 Zr1 O35 C34 133.1(3) . . . . ? O45 Zr1 O41 C42 -19.2(2) . . . . ? O15 Zr1 O41 C42 -138.9(3) . . . . ? O31 Zr1 O41 C42 65.9(2) . . . . ? O35 Zr1 O41 C42 25.8(3) . . . . ? O25 Zr1 O41 C42 140.3(2) . . . . ? O21 Zr1 O41 C42 -178.9(2) . . . . ? O11 Zr1 O41 C42 -78.0(3) . . . . ? Zr1 O41 C42 O421 -164.63(19) . . . . ? Zr1 O41 C42 C43 17.5(4) . . . . ? O41 C42 O421 C422 4.2(4) . . . . ? C43 C42 O421 C422 -177.7(3) . . . . ? C42 O421 C422 C423 171.4(4) . . . . ? O41 C42 C43 C44 0.2(5) . . . . ? O421 C42 C43 C44 -177.7(3) . . . . ? C42 C43 C44 O45 -6.9(5) . . . . ? C42 C43 C44 O441 172.0(3) . . . . ? O45 C44 O441 C442 -1.3(4) . . . . ? C43 C44 O441 C442 179.6(3) . . . . ? C44 O441 C442 C443 79.0(3) . . . . ? O441 C44 O45 Zr1 176.95(16) . . . . ? C43 C44 O45 Zr1 -4.2(5) . . . . ? O15 Zr1 O45 C44 75.3(3) . . . . ? O31 Zr1 O45 C44 -63.2(3) . . . . ? O35 Zr1 O45 C44 -139.9(3) . . . . ? O41 Zr1 O45 C44 12.8(2) . . . . ? O25 Zr1 O45 C44 -23.7(3) . . . . ? O21 Zr1 O45 C44 174.2(2) . . . . ? O11 Zr1 O45 C44 140.0(3) . . . . ? C96 C91 C92 C93 0.1(5) . . . . ? C90 C91 C92 C93 -179.4(3) . . . . ? C91 C92 C93 C94 -0.3(5) . . . . ? C92 C93 C94 C95 0.3(5) . . . . ? C93 C94 C95 C96 -0.3(5) . . . . ? C94 C95 C96 C91 0.2(6) . . . . ? C92 C91 C96 C95 -0.1(5) . . . . ? C90 C91 C96 C95 179.5(3) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.812 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.064 #=================================END