# 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 'Zofia Janas' _publ_contact_author_email ZJ@WCHUWR.PL _publ_section_title ; Zirconium and hafnium complexes of the thio(bisphenolato) ligand: synthesis, structural characterization and testing as 1-hexene polymerization ; loop_ _publ_author_name 'Zofia Janas' 'Dorota Godbole' 'Tomasz Nerkowski' 'Krzysztof Szczegot' # Attachment '68rev.CIF' data_dor1 _database_code_depnum_ccdc_archive 'CCDC 721082' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C58.60 H86.80 Al2 Cl6.40 Hf O4 S2' _chemical_formula_sum 'C58.60 H86.80 Al2 Cl6.40 Hf O4 S2' _chemical_formula_weight 1378.73 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.802(4) _cell_length_b 15.571(4) _cell_length_c 16.625(4) _cell_angle_alpha 73.88(3) _cell_angle_beta 86.93(3) _cell_angle_gamma 62.71(3) _cell_volume 3259.2(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5321 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description BLOCK _exptl_crystal_colour YELLOW _exptl_crystal_size_max 0.324 _exptl_crystal_size_mid 0.215 _exptl_crystal_size_min 0.112 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1418 _exptl_absorpt_coefficient_mu 1.996 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.604 _exptl_absorpt_correction_T_max 0.821 _exptl_absorpt_process_details ; CrysAlis RED V1.171.13, Oxford Diffraction Ltd., Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD kappa-axis diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37547 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 27.00 _reflns_number_total 14204 _reflns_number_gt 10791 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis RED V1.171.30,Oxford Diffraction Ltd.,2006' _computing_data_reduction ' CrysAlis RED V1.171.30,Oxford Diffraction Ltd.,2006' _computing_structure_solution 'SHELXTL V6.14, Bruker AXS 2003' _computing_structure_refinement 'SHELXTL V6.14, Bruker AXS 2003' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXTL V6.14, Bruker AXS 2003' _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^)+(0.0181P)^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 14204 _refine_ls_number_parameters 742 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0572 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0568 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.007 _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 Hf Hf 0.615413(11) 0.168541(11) 0.730512(9) 0.01226(4) Uani 1 1 d . A . Al1 Al 0.69517(7) -0.00184(7) 0.63185(6) 0.0159(2) Uani 1 1 d . . . Al2 Al 0.84740(7) 0.11504(7) 0.78321(6) 0.0175(2) Uani 1 1 d . . . S1 S 0.56009(6) 0.34185(6) 0.59664(5) 0.01225(16) Uani 1 1 d . . . S2 S 0.56757(6) 0.07062(6) 0.88006(5) 0.01202(16) Uani 1 1 d . . . Cl5 Cl 0.44569(6) 0.19877(6) 0.69586(5) 0.01724(17) Uani 1 1 d . . . Cl6 Cl 0.55223(6) 0.29969(6) 0.79955(5) 0.01737(17) Uani 1 1 d . . . Cl1 Cl 0.8438(3) -0.0641(3) 0.5957(3) 0.0235(5) Uani 0.60 1 d P A 1 Cl2 Cl 0.6067(5) -0.0678(5) 0.6140(4) 0.0222(4) Uani 0.60 1 d P A 1 Cl3 Cl 0.8896(5) 0.2136(4) 0.8089(4) 0.0321(6) Uani 0.60 1 d P A 1 Cl4 Cl 0.9675(3) -0.0261(3) 0.7857(3) 0.0182(5) Uani 0.60 1 d P A 1 C1 C 0.831(2) -0.053(2) 0.597(2) 0.0235(5) Uani 0.40 1 d P A 2 H1A H 0.8286 -0.0209 0.5372 0.035 Uiso 0.40 1 calc PR A 2 H1B H 0.8601 -0.1260 0.6077 0.035 Uiso 0.40 1 calc PR A 2 H1C H 0.8724 -0.0378 0.6293 0.035 Uiso 0.40 1 calc PR A 2 C2 C 0.607(3) -0.065(3) 0.619(2) 0.0222(4) Uani 0.40 1 d P A 2 H2A H 0.5350 -0.0168 0.6169 0.033 Uiso 0.40 1 calc PR A 2 H2B H 0.6234 -0.1252 0.6664 0.033 Uiso 0.40 1 calc PR A 2 H2C H 0.6196 -0.0849 0.5664 0.033 Uiso 0.40 1 calc PR A 2 C3 C 0.882(3) 0.223(3) 0.802(2) 0.0321(6) Uani 0.40 1 d P A 2 H3A H 0.8896 0.2637 0.7475 0.048 Uiso 0.40 1 calc PR A 2 H3B H 0.9464 0.1900 0.8376 0.048 Uiso 0.40 1 calc PR A 2 H3C H 0.8274 0.2671 0.8293 0.048 Uiso 0.40 1 calc PR A 2 C4 C 0.957(2) -0.014(2) 0.783(2) 0.0182(5) Uani 0.40 1 d P A 2 H4A H 1.0113 -0.0349 0.8261 0.027 Uiso 0.40 1 calc PR A 2 H4B H 0.9836 -0.0103 0.7279 0.027 Uiso 0.40 1 calc PR A 2 H4C H 0.9312 -0.0643 0.7957 0.027 Uiso 0.40 1 calc PR A 2 O1 O 0.63400(15) 0.13350(15) 0.60270(12) 0.0151(5) Uani 1 1 d . A . O2 O 0.75546(15) 0.17646(15) 0.69072(12) 0.0147(5) Uani 1 1 d . A . O3 O 0.68858(15) 0.00940(15) 0.73915(12) 0.0152(5) Uani 1 1 d . A . O4 O 0.74415(15) 0.10084(16) 0.83686(12) 0.0153(5) Uani 1 1 d . A . C10 C 0.5769(2) 0.1969(2) 0.52779(19) 0.0145(7) Uani 1 1 d . . . C11 C 0.5330(2) 0.3005(2) 0.51530(18) 0.0125(7) Uani 1 1 d . A . C12 C 0.4741(2) 0.3681(2) 0.44140(18) 0.0129(7) Uani 1 1 d . . . H12 H 0.4449 0.4385 0.4344 0.015 Uiso 1 1 calc R A . C13 C 0.4573(2) 0.3338(2) 0.37741(18) 0.0141(7) Uani 1 1 d . A . C14 C 0.5043(2) 0.2297(2) 0.39016(19) 0.0172(7) Uani 1 1 d . . . H14 H 0.4959 0.2042 0.3470 0.021 Uiso 1 1 calc R A . C15 C 0.5631(2) 0.1623(2) 0.46380(19) 0.0182(7) Uani 1 1 d . A . H15 H 0.5940 0.0919 0.4703 0.022 Uiso 1 1 calc R . . C16 C 0.3877(2) 0.4051(2) 0.29708(19) 0.0180(7) Uani 1 1 d . . . C17 C 0.4477(3) 0.3843(3) 0.2204(2) 0.0289(9) Uani 1 1 d . A . H17A H 0.5077 0.3950 0.2227 0.043 Uiso 1 1 calc R . . H17B H 0.4039 0.4303 0.1688 0.043 Uiso 1 1 calc R . . H17C H 0.4696 0.3145 0.2208 0.043 Uiso 1 1 calc R . . C18 C 0.3515(3) 0.5164(3) 0.2912(2) 0.0286(9) Uani 1 1 d . A . H18A H 0.3168 0.5313 0.3412 0.043 Uiso 1 1 calc R . . H18B H 0.3041 0.5594 0.2409 0.043 Uiso 1 1 calc R . . H18C H 0.4104 0.5297 0.2877 0.043 Uiso 1 1 calc R . . C19 C 0.2956(3) 0.3838(3) 0.2886(2) 0.0216(8) Uani 1 1 d . A . H19A H 0.2602 0.4258 0.2322 0.026 Uiso 1 1 calc R . . H19B H 0.3254 0.3128 0.2876 0.026 Uiso 1 1 calc R . . C110 C 0.2116(2) 0.3982(3) 0.3502(2) 0.0229(8) Uani 1 1 d . . . C111 C 0.2531(3) 0.3408(3) 0.4422(2) 0.0277(8) Uani 1 1 d . A . H11A H 0.1967 0.3416 0.4762 0.042 Uiso 1 1 calc R . . H11B H 0.2863 0.3732 0.4631 0.042 Uiso 1 1 calc R . . H11C H 0.3027 0.2709 0.4462 0.042 Uiso 1 1 calc R . . C112 C 0.1474(3) 0.3548(3) 0.3240(3) 0.0392(10) Uani 1 1 d . A . H11D H 0.1902 0.2829 0.3298 0.059 Uiso 1 1 calc R . . H11E H 0.1198 0.3904 0.2653 0.059 Uiso 1 1 calc R . . H11F H 0.0910 0.3635 0.3600 0.059 Uiso 1 1 calc R . . C113 C 0.1406(3) 0.5092(3) 0.3452(2) 0.0318(9) Uani 1 1 d . A . H11G H 0.1173 0.5482 0.2863 0.048 Uiso 1 1 calc R . . H11H H 0.1777 0.5361 0.3691 0.048 Uiso 1 1 calc R . . H11I H 0.0816 0.5141 0.3769 0.048 Uiso 1 1 calc R . . C20 C 0.7686(2) 0.2378(2) 0.61727(18) 0.0144(7) Uani 1 1 d . . . C21 C 0.6858(2) 0.3220(2) 0.56983(18) 0.0126(7) Uani 1 1 d . A . C22 C 0.6987(2) 0.3856(2) 0.49829(18) 0.0136(7) Uani 1 1 d . . . H22 H 0.6405 0.4434 0.4667 0.016 Uiso 1 1 calc R A . C23 C 0.7950(2) 0.3667(2) 0.47183(19) 0.0162(7) Uani 1 1 d . A . C24 C 0.8775(2) 0.2796(2) 0.5203(2) 0.0204(8) Uani 1 1 d . . . H24 H 0.9443 0.2640 0.5035 0.025 Uiso 1 1 calc R A . C25 C 0.8659(2) 0.2155(2) 0.5913(2) 0.0203(8) Uani 1 1 d . A . H25 H 0.9237 0.1567 0.6223 0.024 Uiso 1 1 calc R . . C26 C 0.8129(2) 0.4358(2) 0.39392(19) 0.0167(7) Uani 1 1 d . . . C27 C 0.7142(3) 0.5329(2) 0.3561(2) 0.0230(8) Uani 1 1 d . A . H27A H 0.6638 0.5158 0.3387 0.035 Uiso 1 1 calc R . . H27B H 0.7289 0.5755 0.3073 0.035 Uiso 1 1 calc R . . H27C H 0.6870 0.5695 0.3984 0.035 Uiso 1 1 calc R . . C28 C 0.8862(3) 0.4693(3) 0.4217(2) 0.0244(8) Uani 1 1 d . A . H28A H 0.8555 0.5060 0.4634 0.037 Uiso 1 1 calc R . . H28B H 0.8989 0.5135 0.3728 0.037 Uiso 1 1 calc R . . H28C H 0.9508 0.4099 0.4466 0.037 Uiso 1 1 calc R . . C29 C 0.8660(2) 0.3800(2) 0.3271(2) 0.0185(7) Uani 1 1 d . A . H29A H 0.8751 0.4300 0.2802 0.022 Uiso 1 1 calc R . . H29B H 0.9353 0.3286 0.3529 0.022 Uiso 1 1 calc R . . C210 C 0.8237(3) 0.3260(3) 0.2863(2) 0.0249(8) Uani 1 1 d . . . C211 C 0.8936(3) 0.2939(3) 0.2176(3) 0.0462(12) Uani 1 1 d . A . H21A H 0.8705 0.2587 0.1897 0.069 Uiso 1 1 calc R . . H21B H 0.9637 0.2486 0.2428 0.069 Uiso 1 1 calc R . . H21C H 0.8914 0.3537 0.1762 0.069 Uiso 1 1 calc R . . C212 C 0.8303(4) 0.2299(3) 0.3487(3) 0.0541(13) Uani 1 1 d . A . H21D H 0.7775 0.2478 0.3879 0.081 Uiso 1 1 calc R . . H21E H 0.8977 0.1910 0.3800 0.081 Uiso 1 1 calc R . . H21F H 0.8199 0.1892 0.3180 0.081 Uiso 1 1 calc R . . C213 C 0.7155(3) 0.3922(4) 0.2455(3) 0.0602(14) Uani 1 1 d . A . H21G H 0.6995 0.3588 0.2105 0.090 Uiso 1 1 calc R . . H21H H 0.7092 0.4571 0.2105 0.090 Uiso 1 1 calc R . . H21I H 0.6677 0.4036 0.2893 0.090 Uiso 1 1 calc R . . C30 C 0.7019(2) -0.0722(2) 0.80831(18) 0.0153(7) Uani 1 1 d . . . C31 C 0.6466(2) -0.0562(2) 0.87668(18) 0.0131(7) Uani 1 1 d . A . C32 C 0.6583(2) -0.1369(2) 0.94564(19) 0.0149(7) Uani 1 1 d . . . H32 H 0.6191 -0.1246 0.9921 0.018 Uiso 1 1 calc R A . C33 C 0.7270(2) -0.2355(2) 0.94682(19) 0.0155(7) Uani 1 1 d . A . C34 C 0.7815(2) -0.2497(2) 0.87578(19) 0.0193(7) Uani 1 1 d . . . H34 H 0.8272 -0.3164 0.8744 0.023 Uiso 1 1 calc R A . C35 C 0.7703(2) -0.1694(2) 0.80779(19) 0.0198(8) Uani 1 1 d . A . H35 H 0.8092 -0.1808 0.7611 0.024 Uiso 1 1 calc R . . C36 C 0.7475(3) -0.3266(2) 1.0225(2) 0.0203(8) Uani 1 1 d . . . C37 C 0.6786(3) -0.2962(3) 1.0932(2) 0.0256(8) Uani 1 1 d . A . H37A H 0.6869 -0.2438 1.1088 0.038 Uiso 1 1 calc R . . H37B H 0.6980 -0.3553 1.1423 0.038 Uiso 1 1 calc R . . H37C H 0.6072 -0.2702 1.0735 0.038 Uiso 1 1 calc R . . C38 C 0.7213(3) -0.3992(3) 0.9932(2) 0.0311(9) Uani 1 1 d . A . H38A H 0.6500 -0.3638 0.9699 0.047 Uiso 1 1 calc R . . H38B H 0.7315 -0.4571 1.0411 0.047 Uiso 1 1 calc R . . H38C H 0.7659 -0.4228 0.9499 0.047 Uiso 1 1 calc R . . C39 C 0.8628(2) -0.3851(2) 1.0538(2) 0.0221(8) Uani 1 1 d . A . H39A H 0.8732 -0.4488 1.0956 0.027 Uiso 1 1 calc R . . H39B H 0.9003 -0.4040 1.0052 0.027 Uiso 1 1 calc R . . C310 C 0.9183(3) -0.3413(3) 1.0931(2) 0.0258(8) Uani 1 1 d . . . C311 C 1.0328(3) -0.4079(3) 1.0914(3) 0.0401(11) Uani 1 1 d . A . H31A H 1.0500 -0.4011 1.0330 0.060 Uiso 1 1 calc R . . H31B H 1.0501 -0.4784 1.1196 0.060 Uiso 1 1 calc R . . H31C H 1.0715 -0.3868 1.1206 0.060 Uiso 1 1 calc R . . C312 C 0.8982(3) -0.3485(3) 1.1862(2) 0.0415(11) Uani 1 1 d . A . H31D H 0.9139 -0.4180 1.2167 0.062 Uiso 1 1 calc R . . H31E H 0.8263 -0.3034 1.1899 0.062 Uiso 1 1 calc R . . H31F H 0.9416 -0.3285 1.2110 0.062 Uiso 1 1 calc R . . C313 C 0.8937(3) -0.2320(3) 1.0470(3) 0.0477(12) Uani 1 1 d . A . H31G H 0.9374 -0.2130 1.0726 0.072 Uiso 1 1 calc R . . H31H H 0.8220 -0.1873 1.0514 0.072 Uiso 1 1 calc R . . H31I H 0.9062 -0.2260 0.9877 0.072 Uiso 1 1 calc R . . C40 C 0.7342(2) 0.0828(2) 0.92269(18) 0.0155(7) Uani 1 1 d . . . C41 C 0.6497(2) 0.0735(2) 0.95264(18) 0.0114(7) Uani 1 1 d . A . C42 C 0.6335(2) 0.0597(2) 1.03799(18) 0.0131(7) Uani 1 1 d . . . H42 H 0.5744 0.0538 1.0573 0.016 Uiso 1 1 calc R A . C43 C 0.7021(2) 0.0546(2) 1.09484(18) 0.0146(7) Uani 1 1 d . A . C44 C 0.7896(2) 0.0600(2) 1.06358(19) 0.0199(8) Uani 1 1 d . . . H44 H 0.8394 0.0539 1.1015 0.024 Uiso 1 1 calc R A . C45 C 0.8058(2) 0.0742(3) 0.97855(19) 0.0198(7) Uani 1 1 d . A . H45 H 0.8658 0.0779 0.9591 0.024 Uiso 1 1 calc R . . C46 C 0.6860(2) 0.0424(2) 1.18917(18) 0.0153(7) Uani 1 1 d . . . C47 C 0.5760(2) 0.0609(3) 1.2043(2) 0.0223(8) Uani 1 1 d . A . H47A H 0.5283 0.1239 1.1640 0.033 Uiso 1 1 calc R . . H47B H 0.5623 0.0658 1.2616 0.033 Uiso 1 1 calc R . . H47C H 0.5672 0.0048 1.1969 0.033 Uiso 1 1 calc R . . C48 C 0.7004(3) 0.1245(2) 1.2137(2) 0.0218(8) Uani 1 1 d . A . H48A H 0.6576 0.1906 1.1744 0.033 Uiso 1 1 calc R . . H48B H 0.7722 0.1100 1.2114 0.033 Uiso 1 1 calc R . . H48C H 0.6807 0.1250 1.2708 0.033 Uiso 1 1 calc R . . C49 C 0.7639(2) -0.0671(2) 1.23742(19) 0.0188(7) Uani 1 1 d . A . H49A H 0.8287 -0.0813 1.2107 0.023 Uiso 1 1 calc R . . H49B H 0.7393 -0.1119 1.2252 0.023 Uiso 1 1 calc R . . C410 C 0.7920(2) -0.1035(2) 1.33404(19) 0.0201(8) Uani 1 1 d . . . C411 C 0.8592(3) -0.2188(3) 1.3555(2) 0.0385(11) Uani 1 1 d . A . H41A H 0.9181 -0.2338 1.3218 0.058 Uiso 1 1 calc R . . H41B H 0.8192 -0.2498 1.3429 0.058 Uiso 1 1 calc R . . H41C H 0.8831 -0.2460 1.4153 0.058 Uiso 1 1 calc R . . C412 C 0.6996(3) -0.0837(3) 1.3864(2) 0.0245(8) Uani 1 1 d . A . H41D H 0.7232 -0.1150 1.4462 0.037 Uiso 1 1 calc R . . H41E H 0.6593 -0.1127 1.3702 0.037 Uiso 1 1 calc R . . H41F H 0.6572 -0.0109 1.3761 0.037 Uiso 1 1 calc R . . C413 C 0.8551(3) -0.0594(3) 1.3600(2) 0.0319(9) Uani 1 1 d . A . H41G H 0.8114 0.0122 1.3550 0.048 Uiso 1 1 calc R . . H41H H 0.9106 -0.0665 1.3233 0.048 Uiso 1 1 calc R . . H41I H 0.8837 -0.0954 1.4183 0.048 Uiso 1 1 calc R . . C5A C 0.6465(16) 0.361(3) 0.9556(11) 0.080(13) Uiso 0.25 1 d PD B 3 H5A1 H 0.6650 0.3250 0.9121 0.096 Uiso 0.25 1 calc PR B 3 H5A2 H 0.6156 0.4345 0.9264 0.096 Uiso 0.25 1 calc PR B 3 Cl71 Cl 0.7572(10) 0.3264(17) 1.0162(13) 0.060(3) Uani 0.25 1 d PD B 3 Cl81 Cl 0.5565(7) 0.3355(6) 1.0147(5) 0.0461(19) Uani 0.25 1 d PD B 3 C5B C 0.6748(11) 0.3207(14) 0.9664(11) 0.039(5) Uiso 0.25 1 d PD C 4 H5B1 H 0.6759 0.3505 0.9056 0.046 Uiso 0.25 1 calc PR C 4 H5B2 H 0.6817 0.2525 0.9743 0.046 Uiso 0.25 1 calc PR C 4 Cl72 Cl 0.7779(11) 0.311(2) 1.0219(19) 0.150(11) Uani 0.25 1 d PD C 4 Cl82 Cl 0.5579(10) 0.3954(12) 0.9999(9) 0.177(7) Uani 0.25 1 d PD C 4 C5C C 0.6366(7) 0.3453(10) 0.9625(5) 0.029(3) Uiso 0.50 1 d PD D 5 H5C4 H 0.6017 0.3921 0.9071 0.035 Uiso 0.50 1 calc PR D 5 H5C5 H 0.6593 0.2757 0.9597 0.035 Uiso 0.50 1 calc PR D 5 Cl73 Cl 0.7433(4) 0.3588(5) 0.9826(4) 0.0714(15) Uani 0.50 1 d PD D 5 Cl83 Cl 0.5510(4) 0.3691(5) 1.0381(3) 0.0813(15) Uani 0.50 1 d PD D 5 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 Hf 0.01364(7) 0.01281(7) 0.01042(7) -0.00256(5) 0.00052(5) -0.00657(5) Al1 0.0192(5) 0.0144(5) 0.0109(5) -0.0033(4) 0.0016(4) -0.0053(4) Al2 0.0144(5) 0.0231(5) 0.0129(5) -0.0002(4) 0.0005(4) -0.0096(4) S1 0.0120(4) 0.0135(4) 0.0110(4) -0.0026(3) 0.0006(3) -0.0062(3) S2 0.0123(4) 0.0119(4) 0.0117(4) -0.0032(3) 0.0003(3) -0.0055(3) Cl5 0.0162(4) 0.0183(4) 0.0167(4) -0.0016(3) -0.0021(3) -0.0091(3) Cl6 0.0245(4) 0.0166(4) 0.0145(4) -0.0057(3) 0.0033(3) -0.0118(3) Cl1 0.0157(13) 0.0276(15) 0.0211(7) -0.0090(7) 0.0069(9) -0.0044(11) Cl2 0.0293(7) 0.0228(7) 0.0188(10) -0.0065(6) 0.0025(6) -0.0154(6) Cl3 0.0384(13) 0.0384(14) 0.0271(13) -0.0023(11) -0.0046(10) -0.0271(11) Cl4 0.0104(12) 0.0124(12) 0.0188(7) 0.0017(8) -0.0003(9) 0.0022(9) C1 0.0157(13) 0.0276(15) 0.0211(7) -0.0090(7) 0.0069(9) -0.0044(11) C2 0.0293(7) 0.0228(7) 0.0188(10) -0.0065(6) 0.0025(6) -0.0154(6) C3 0.0384(13) 0.0384(14) 0.0271(13) -0.0023(11) -0.0046(10) -0.0271(11) C4 0.0104(12) 0.0124(12) 0.0188(7) 0.0017(8) -0.0003(9) 0.0022(9) O1 0.0176(11) 0.0157(12) 0.0098(11) -0.0026(9) 0.0009(9) -0.0064(10) O2 0.0138(11) 0.0172(12) 0.0095(11) 0.0011(9) 0.0010(9) -0.0069(9) O3 0.0195(12) 0.0113(11) 0.0104(11) -0.0002(9) 0.0003(9) -0.0051(9) O4 0.0164(11) 0.0243(12) 0.0085(11) -0.0040(9) 0.0018(9) -0.0127(10) C10 0.0134(16) 0.0154(17) 0.0130(16) -0.0023(13) 0.0008(13) -0.0061(14) C11 0.0124(16) 0.0141(16) 0.0150(16) -0.0063(13) 0.0019(13) -0.0081(14) C12 0.0108(16) 0.0139(16) 0.0156(16) -0.0026(13) 0.0036(13) -0.0081(13) C13 0.0158(17) 0.0184(17) 0.0099(16) -0.0020(13) 0.0016(13) -0.0106(14) C14 0.0226(18) 0.0206(18) 0.0105(16) -0.0061(14) 0.0005(14) -0.0107(15) C15 0.0241(18) 0.0144(17) 0.0149(17) -0.0038(14) 0.0016(14) -0.0080(15) C16 0.0211(18) 0.0196(18) 0.0145(17) -0.0015(14) -0.0019(14) -0.0119(15) C17 0.031(2) 0.035(2) 0.0155(18) 0.0021(16) -0.0042(16) -0.0153(18) C18 0.037(2) 0.0210(19) 0.025(2) 0.0026(15) -0.0091(17) -0.0150(17) C19 0.0277(19) 0.0189(18) 0.0160(17) -0.0036(14) -0.0050(15) -0.0090(15) C110 0.0173(18) 0.0240(19) 0.0253(19) -0.0071(15) -0.0010(15) -0.0073(15) C111 0.027(2) 0.030(2) 0.0242(19) -0.0052(16) 0.0098(16) -0.0141(17) C112 0.028(2) 0.050(3) 0.053(3) -0.032(2) 0.0097(19) -0.019(2) C113 0.032(2) 0.032(2) 0.028(2) -0.0079(17) 0.0028(17) -0.0120(18) C20 0.0192(17) 0.0147(17) 0.0108(16) -0.0037(13) 0.0024(13) -0.0092(14) C21 0.0125(16) 0.0167(17) 0.0123(16) -0.0076(13) 0.0030(13) -0.0080(14) C22 0.0147(16) 0.0107(16) 0.0123(16) -0.0018(13) -0.0017(13) -0.0039(13) C23 0.0184(17) 0.0188(17) 0.0140(16) -0.0039(14) 0.0023(14) -0.0114(14) C24 0.0130(17) 0.0233(19) 0.0213(18) -0.0008(15) 0.0019(14) -0.0085(15) C25 0.0153(17) 0.0215(18) 0.0181(18) -0.0002(14) 0.0001(14) -0.0064(15) C26 0.0173(17) 0.0208(18) 0.0123(16) -0.0016(14) 0.0016(13) -0.0107(15) C27 0.0280(19) 0.0153(18) 0.0218(19) -0.0009(14) 0.0074(15) -0.0096(15) C28 0.031(2) 0.027(2) 0.0231(19) -0.0102(16) 0.0113(16) -0.0194(17) C29 0.0160(17) 0.0184(18) 0.0198(18) -0.0042(15) 0.0017(14) -0.0077(15) C210 0.028(2) 0.0239(19) 0.026(2) -0.0093(16) 0.0030(16) -0.0136(16) C211 0.059(3) 0.045(3) 0.041(3) -0.029(2) 0.017(2) -0.022(2) C212 0.097(4) 0.049(3) 0.043(3) -0.017(2) 0.009(3) -0.053(3) C213 0.045(3) 0.064(3) 0.078(4) -0.042(3) -0.016(3) -0.017(3) C30 0.0173(17) 0.0151(17) 0.0101(16) -0.0009(13) -0.0032(13) -0.0058(14) C31 0.0098(15) 0.0123(16) 0.0144(16) -0.0031(13) -0.0041(13) -0.0027(13) C32 0.0159(16) 0.0180(17) 0.0129(16) -0.0055(13) 0.0008(13) -0.0087(14) C33 0.0193(17) 0.0135(17) 0.0131(16) -0.0024(13) -0.0032(13) -0.0074(14) C34 0.0243(18) 0.0095(16) 0.0181(18) -0.0042(14) -0.0001(14) -0.0025(14) C35 0.0221(18) 0.0179(18) 0.0118(16) -0.0037(14) 0.0023(14) -0.0033(15) C36 0.0263(19) 0.0143(17) 0.0175(17) -0.0015(14) 0.0040(15) -0.0092(15) C37 0.030(2) 0.0178(18) 0.0205(19) 0.0025(15) 0.0048(16) -0.0090(16) C38 0.037(2) 0.024(2) 0.031(2) -0.0014(17) 0.0005(18) -0.0165(18) C39 0.0274(19) 0.0137(17) 0.0158(17) -0.0008(14) 0.0009(15) -0.0036(15) C310 0.0254(19) 0.0198(19) 0.0214(19) -0.0022(15) -0.0033(15) -0.0030(16) C311 0.030(2) 0.043(3) 0.038(2) -0.015(2) -0.0016(19) -0.007(2) C312 0.038(2) 0.050(3) 0.029(2) -0.019(2) 0.0008(19) -0.009(2) C313 0.052(3) 0.035(2) 0.057(3) -0.001(2) -0.020(2) -0.025(2) C40 0.0182(17) 0.0170(17) 0.0088(16) -0.0007(13) 0.0015(13) -0.0077(14) C41 0.0118(16) 0.0096(16) 0.0116(16) -0.0012(12) -0.0024(13) -0.0046(13) C42 0.0123(16) 0.0099(16) 0.0155(16) -0.0032(13) 0.0025(13) -0.0041(13) C43 0.0157(17) 0.0140(17) 0.0130(16) -0.0024(13) -0.0002(13) -0.0066(14) C44 0.0176(18) 0.029(2) 0.0147(17) -0.0025(15) -0.0050(14) -0.0137(16) C45 0.0163(17) 0.032(2) 0.0160(17) -0.0053(15) 0.0014(14) -0.0166(15) C46 0.0182(17) 0.0182(17) 0.0098(15) -0.0039(13) 0.0015(13) -0.0088(14) C47 0.0194(18) 0.034(2) 0.0125(17) -0.0070(15) 0.0036(14) -0.0114(16) C48 0.0277(19) 0.0185(18) 0.0197(18) -0.0053(14) -0.0004(15) -0.0109(16) C49 0.0181(17) 0.0213(18) 0.0145(17) -0.0062(14) 0.0057(14) -0.0070(15) C410 0.0197(18) 0.0244(19) 0.0140(17) -0.0048(14) 0.0039(14) -0.0090(15) C411 0.045(2) 0.028(2) 0.018(2) -0.0001(16) -0.0003(18) 0.0002(19) C412 0.028(2) 0.033(2) 0.0162(18) -0.0059(16) 0.0061(15) -0.0180(17) C413 0.024(2) 0.048(2) 0.0189(19) 0.0034(17) -0.0056(16) -0.0187(18) Cl71 0.094(7) 0.088(9) 0.040(7) -0.018(6) -0.011(5) -0.075(7) Cl81 0.060(4) 0.050(4) 0.031(3) -0.012(3) 0.009(3) -0.028(4) Cl72 0.26(2) 0.21(3) 0.090(15) -0.050(16) 0.024(16) -0.20(2) Cl82 0.242(14) 0.171(15) 0.116(10) -0.041(9) 0.096(9) -0.101(11) Cl73 0.061(3) 0.086(4) 0.090(4) -0.027(3) 0.003(3) -0.050(2) Cl83 0.053(2) 0.073(3) 0.072(3) 0.003(3) 0.031(2) -0.008(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 Hf O3 2.166(2) . ? Hf O2 2.189(2) . ? Hf O1 2.309(2) . ? Hf O4 2.313(2) . ? Hf Cl5 2.405(2) . ? Hf Cl6 2.408(2) . ? Hf S2 2.776(2) . ? Hf S1 2.782(2) . ? Hf Al1 3.234(2) . ? Hf Al2 3.248(2) . ? Al1 O1 1.796(2) . ? Al1 O3 1.833(2) . ? Al1 C1 1.91(3) . ? Al1 C2 2.02(4) . ? Al1 Cl2 2.073(6) . ? Al1 Cl1 2.090(4) . ? Al2 O4 1.799(2) . ? Al2 O2 1.829(2) . ? Al2 C4 1.92(3) . ? Al2 Cl3 2.049(6) . ? Al2 Cl4 2.090(4) . ? Al2 C3 2.07(4) . ? S1 C11 1.784(3) . ? S1 C21 1.794(3) . ? S2 C41 1.781(3) . ? S2 C31 1.791(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? O1 C10 1.380(3) . ? O2 C20 1.392(4) . ? O3 C30 1.399(4) . ? O4 C40 1.389(3) . ? C10 C15 1.380(4) . ? C10 C11 1.390(4) . ? C11 C12 1.391(4) . ? C12 C13 1.395(4) . ? C12 H12 0.9500 . ? C13 C14 1.395(4) . ? C13 C16 1.534(4) . ? C14 C15 1.385(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 C17 1.537(5) . ? C16 C18 1.537(5) . ? C16 C19 1.563(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C110 1.543(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C110 C111 1.534(5) . ? C110 C112 1.533(5) . ? C110 C113 1.537(5) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C20 C21 1.378(4) . ? C20 C25 1.392(4) . ? C21 C22 1.388(4) . ? C22 C23 1.389(4) . ? C22 H22 0.9500 . ? C23 C24 1.400(4) . ? C23 C26 1.535(4) . ? C24 C25 1.379(4) . ? C24 H24 0.9500 . ? C25 H25 0.9500 . ? C26 C27 1.537(4) . ? C26 C28 1.540(5) . ? C26 C29 1.556(4) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C210 1.551(5) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C210 C213 1.518(5) . ? C210 C212 1.530(5) . ? C210 C211 1.530(5) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C213 H21G 0.9800 . ? C213 H21H 0.9800 . ? C213 H21I 0.9800 . ? C30 C31 1.377(4) . ? C30 C35 1.384(4) . ? C31 C32 1.395(4) . ? C32 C33 1.395(4) . ? C32 H32 0.9500 . ? C33 C34 1.405(4) . ? C33 C36 1.530(4) . ? C34 C35 1.384(4) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.544(4) . ? C36 C38 1.548(5) . ? C36 C39 1.556(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C310 1.545(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C310 C313 1.533(5) . ? C310 C311 1.532(5) . ? C310 C312 1.543(5) . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C313 H31G 0.9800 . ? C313 H31H 0.9800 . ? C313 H31I 0.9800 . ? C40 C41 1.377(4) . ? C40 C45 1.382(4) . ? C41 C42 1.400(4) . ? C42 C43 1.385(4) . ? C42 H42 0.9500 . ? C43 C44 1.399(4) . ? C43 C46 1.546(4) . ? C44 C45 1.394(4) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.537(4) . ? C46 C48 1.548(4) . ? C46 C49 1.555(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C410 1.557(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C410 C413 1.525(5) . ? C410 C412 1.536(4) . ? C410 C411 1.544(5) . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C412 H41D 0.9800 . ? C412 H41E 0.9800 . ? C412 H41F 0.9800 . ? C413 H41G 0.9800 . ? C413 H41H 0.9800 . ? C413 H41I 0.9800 . ? C5A Cl71 1.747(10) . ? C5A Cl81 1.743(10) . ? C5A H5A1 0.9900 . ? C5A H5A2 0.9900 . ? C5B Cl82 1.751(9) . ? C5B Cl72 1.751(9) . ? C5B H5B1 0.9900 . ? C5B H5B2 0.9900 . ? C5C Cl83 1.726(7) . ? C5C Cl73 1.747(8) . ? C5C H5C4 0.9900 . ? C5C H5C5 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Hf O2 90.14(8) . . ? O3 Hf O1 65.42(8) . . ? O2 Hf O1 76.41(8) . . ? O3 Hf O4 77.32(8) . . ? O2 Hf O4 65.01(7) . . ? O1 Hf O4 125.52(7) . . ? O3 Hf Cl5 95.72(7) . . ? O2 Hf Cl5 149.67(6) . . ? O1 Hf Cl5 79.09(6) . . ? O4 Hf Cl5 145.28(6) . . ? O3 Hf Cl6 149.22(6) . . ? O2 Hf Cl6 98.00(6) . . ? O1 Hf Cl6 145.36(6) . . ? O4 Hf Cl6 79.39(6) . . ? Cl5 Hf Cl6 92.05(4) . . ? O3 Hf S2 72.75(6) . . ? O2 Hf S2 132.74(6) . . ? O1 Hf S2 128.85(6) . . ? O4 Hf S2 68.30(6) . . ? Cl5 Hf S2 77.12(4) . . ? Cl6 Hf S2 80.11(4) . . ? O3 Hf S1 133.13(6) . . ? O2 Hf S1 72.45(6) . . ? O1 Hf S1 68.23(6) . . ? O4 Hf S1 127.47(6) . . ? Cl5 Hf S1 82.04(5) . . ? Cl6 Hf S1 77.43(3) . . ? S2 Hf S1 148.61(3) . . ? O3 Hf Al1 32.70(6) . . ? O2 Hf Al1 82.23(6) . . ? O1 Hf Al1 32.72(6) . . ? O4 Hf Al1 102.50(6) . . ? Cl5 Hf Al1 86.79(4) . . ? Cl6 Hf Al1 177.97(3) . . ? S2 Hf Al1 101.24(3) . . ? S1 Hf Al1 100.74(3) . . ? O3 Hf Al2 81.54(7) . . ? O2 Hf Al2 32.48(5) . . ? O1 Hf Al2 101.11(6) . . ? O4 Hf Al2 32.56(5) . . ? Cl5 Hf Al2 176.82(3) . . ? Cl6 Hf Al2 89.53(4) . . ? S2 Hf Al2 100.45(4) . . ? S1 Hf Al2 101.00(4) . . ? Al1 Hf Al2 91.71(4) . . ? O1 Al1 O3 83.69(10) . . ? O1 Al1 C1 110.4(11) . . ? O3 Al1 C1 113.4(11) . . ? O1 Al1 C2 116.2(12) . . ? O3 Al1 C2 107.6(11) . . ? C1 Al1 C2 119.8(16) . . ? O1 Al1 Cl2 116.5(2) . . ? O3 Al1 Cl2 109.77(19) . . ? C1 Al1 Cl2 118.1(11) . . ? C2 Al1 Cl2 2.2(13) . . ? O1 Al1 Cl1 112.99(17) . . ? O3 Al1 Cl1 113.58(17) . . ? C1 Al1 Cl1 2.6(12) . . ? C2 Al1 Cl1 117.7(12) . . ? Cl2 Al1 Cl1 116.0(2) . . ? O1 Al1 Hf 44.03(7) . . ? O3 Al1 Hf 39.66(7) . . ? C1 Al1 Hf 120.3(11) . . ? C2 Al1 Hf 119.4(12) . . ? Cl2 Al1 Hf 121.29(18) . . ? Cl1 Al1 Hf 122.27(16) . . ? O4 Al2 O2 83.76(10) . . ? O4 Al2 C4 110.3(11) . . ? O2 Al2 C4 114.1(11) . . ? O4 Al2 Cl3 117.5(2) . . ? O2 Al2 Cl3 111.08(17) . . ? C4 Al2 Cl3 116.0(11) . . ? O4 Al2 Cl4 110.24(17) . . ? O2 Al2 Cl4 115.34(17) . . ? C4 Al2 Cl4 1.2(12) . . ? Cl3 Al2 Cl4 115.2(2) . . ? O4 Al2 C3 117.5(12) . . ? O2 Al2 C3 106.8(10) . . ? C4 Al2 C3 119.0(16) . . ? Cl3 Al2 C3 4.3(12) . . ? Cl4 Al2 C3 118.3(11) . . ? O4 Al2 Hf 43.81(7) . . ? O2 Al2 Hf 40.00(7) . . ? C4 Al2 Hf 119.0(11) . . ? Cl3 Al2 Hf 124.84(17) . . ? Cl4 Al2 Hf 119.89(16) . . ? C3 Al2 Hf 121.5(11) . . ? C11 S1 C21 96.58(14) . . ? C11 S1 Hf 99.71(10) . . ? C21 S1 Hf 98.16(11) . . ? C41 S2 C31 97.21(14) . . ? C41 S2 Hf 99.83(10) . . ? C31 S2 Hf 97.92(11) . . ? Al1 C1 H1A 109.5 . . ? Al1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Al1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Al1 C2 H2A 109.5 . . ? Al1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Al1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Al2 C3 H3A 109.5 . . ? Al2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Al2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Al2 C4 H4A 109.5 . . ? Al2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Al2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C10 O1 Al1 125.63(19) . . ? C10 O1 Hf 126.47(17) . . ? Al1 O1 Hf 103.25(10) . . ? C20 O2 Al2 122.21(19) . . ? C20 O2 Hf 128.25(18) . . ? Al2 O2 Hf 107.52(10) . . ? C30 O3 Al1 121.00(19) . . ? C30 O3 Hf 128.78(18) . . ? Al1 O3 Hf 107.64(10) . . ? C40 O4 Al2 126.60(19) . . ? C40 O4 Hf 127.16(18) . . ? Al2 O4 Hf 103.63(9) . . ? O1 C10 C15 123.0(3) . . ? O1 C10 C11 118.6(3) . . ? C15 C10 C11 118.4(3) . . ? C10 C11 C12 121.3(3) . . ? C10 C11 S1 116.8(2) . . ? C12 C11 S1 121.9(2) . . ? C11 C12 C13 120.7(3) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C14 117.1(3) . . ? C12 C13 C16 122.7(3) . . ? C14 C13 C16 120.1(3) . . ? C15 C14 C13 122.1(3) . . ? C15 C14 H14 119.0 . . ? C13 C14 H14 119.0 . . ? C14 C15 C10 120.4(3) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? C13 C16 C17 109.0(3) . . ? C13 C16 C18 112.1(3) . . ? C17 C16 C18 107.2(3) . . ? C13 C16 C19 111.3(3) . . ? C17 C16 C19 105.5(3) . . ? C18 C16 C19 111.4(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C110 C19 C16 124.2(3) . . ? C110 C19 H19A 106.3 . . ? C16 C19 H19A 106.3 . . ? C110 C19 H19B 106.3 . . ? C16 C19 H19B 106.3 . . ? H19A C19 H19B 106.4 . . ? C111 C110 C112 107.8(3) . . ? C111 C110 C113 108.2(3) . . ? C112 C110 C113 107.9(3) . . ? C111 C110 C19 113.6(3) . . ? C112 C110 C19 105.4(3) . . ? C113 C110 C19 113.6(3) . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C110 C112 H11D 109.5 . . ? C110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C110 C113 H11G 109.5 . . ? C110 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C110 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C21 C20 C25 119.0(3) . . ? C21 C20 O2 120.6(3) . . ? C25 C20 O2 120.3(3) . . ? C20 C21 C22 120.9(3) . . ? C20 C21 S1 118.6(2) . . ? C22 C21 S1 120.3(2) . . ? C23 C22 C21 121.5(3) . . ? C23 C22 H22 119.3 . . ? C21 C22 H22 119.3 . . ? C22 C23 C24 116.5(3) . . ? C22 C23 C26 123.2(3) . . ? C24 C23 C26 120.4(3) . . ? C25 C24 C23 122.8(3) . . ? C25 C24 H24 118.6 . . ? C23 C24 H24 118.6 . . ? C24 C25 C20 119.4(3) . . ? C24 C25 H25 120.3 . . ? C20 C25 H25 120.3 . . ? C27 C26 C23 111.8(3) . . ? C27 C26 C28 106.0(3) . . ? C23 C26 C28 108.0(3) . . ? C27 C26 C29 111.9(3) . . ? C23 C26 C29 112.3(3) . . ? C28 C26 C29 106.4(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C210 C29 C26 124.6(3) . . ? C210 C29 H29A 106.2 . . ? C26 C29 H29A 106.2 . . ? C210 C29 H29B 106.2 . . ? C26 C29 H29B 106.2 . . ? H29A C29 H29B 106.4 . . ? C213 C210 C212 109.4(4) . . ? C213 C210 C211 108.0(3) . . ? C212 C210 C211 107.0(3) . . ? C213 C210 C29 114.1(3) . . ? C212 C210 C29 112.0(3) . . ? C211 C210 C29 106.0(3) . . ? C210 C211 H21A 109.5 . . ? C210 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C210 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C210 C212 H21D 109.5 . . ? C210 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C210 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C210 C213 H21G 109.5 . . ? C210 C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C210 C213 H21I 109.5 . . ? H21G C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? C31 C30 C35 119.8(3) . . ? C31 C30 O3 120.2(3) . . ? C35 C30 O3 120.0(3) . . ? C30 C31 C32 120.8(3) . . ? C30 C31 S2 118.9(2) . . ? C32 C31 S2 120.0(2) . . ? C33 C32 C31 120.5(3) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 117.5(3) . . ? C32 C33 C36 122.9(3) . . ? C34 C33 C36 119.5(3) . . ? C35 C34 C33 121.8(3) . . ? C35 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? C30 C35 C34 119.6(3) . . ? C30 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C33 C36 C37 111.9(3) . . ? C33 C36 C38 108.0(3) . . ? C37 C36 C38 107.0(3) . . ? C33 C36 C39 110.3(3) . . ? C37 C36 C39 112.3(3) . . ? C38 C36 C39 107.0(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C310 C39 C36 123.5(3) . . ? C310 C39 H39A 106.5 . . ? C36 C39 H39A 106.5 . . ? C310 C39 H39B 106.5 . . ? C36 C39 H39B 106.5 . . ? H39A C39 H39B 106.5 . . ? C313 C310 C311 108.0(3) . . ? C313 C310 C312 108.3(3) . . ? C311 C310 C312 106.7(3) . . ? C313 C310 C39 115.1(3) . . ? C311 C310 C39 106.5(3) . . ? C312 C310 C39 111.8(3) . . ? C310 C311 H31A 109.5 . . ? C310 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C310 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C310 C312 H31D 109.5 . . ? C310 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C310 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? C310 C313 H31G 109.5 . . ? C310 C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? C310 C313 H31I 109.5 . . ? H31G C313 H31I 109.5 . . ? H31H C313 H31I 109.5 . . ? C41 C40 C45 119.2(3) . . ? C41 C40 O4 118.4(3) . . ? C45 C40 O4 122.4(3) . . ? C40 C41 C42 120.8(3) . . ? C40 C41 S2 117.3(2) . . ? C42 C41 S2 121.7(2) . . ? C43 C42 C41 121.1(3) . . ? C43 C42 H42 119.5 . . ? C41 C42 H42 119.5 . . ? C42 C43 C44 117.0(3) . . ? C42 C43 C46 123.0(3) . . ? C44 C43 C46 120.0(3) . . ? C45 C44 C43 122.1(3) . . ? C45 C44 H44 119.0 . . ? C43 C44 H44 119.0 . . ? C40 C45 C44 119.7(3) . . ? C40 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C47 C46 C43 109.9(2) . . ? C47 C46 C48 107.5(3) . . ? C43 C46 C48 107.9(2) . . ? C47 C46 C49 110.9(3) . . ? C43 C46 C49 106.8(2) . . ? C48 C46 C49 113.8(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C46 C49 C410 123.6(3) . . ? C46 C49 H49A 106.4 . . ? C410 C49 H49A 106.4 . . ? C46 C49 H49B 106.4 . . ? C410 C49 H49B 106.4 . . ? H49A C49 H49B 106.5 . . ? C413 C410 C412 109.3(3) . . ? C413 C410 C411 107.6(3) . . ? C412 C410 C411 107.7(3) . . ? C413 C410 C49 112.5(3) . . ? C412 C410 C49 113.9(3) . . ? C411 C410 C49 105.5(3) . . ? C410 C411 H41A 109.5 . . ? C410 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C410 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C410 C412 H41D 109.5 . . ? C410 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C410 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? C410 C413 H41G 109.5 . . ? C410 C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? C410 C413 H41I 109.5 . . ? H41G C413 H41I 109.5 . . ? H41H C413 H41I 109.5 . . ? Cl71 C5A Cl81 113.0(8) . . ? Cl71 C5A H5A1 109.0 . . ? Cl81 C5A H5A1 109.0 . . ? Cl71 C5A H5A2 109.0 . . ? Cl81 C5A H5A2 109.0 . . ? H5A1 C5A H5A2 107.8 . . ? Cl82 C5B Cl72 111.7(8) . . ? Cl82 C5B H5B1 109.3 . . ? Cl72 C5B H5B1 109.3 . . ? Cl82 C5B H5B2 109.3 . . ? Cl72 C5B H5B2 109.3 . . ? H5B1 C5B H5B2 107.9 . . ? Cl83 C5C Cl73 112.7(5) . . ? Cl83 C5C H5C4 109.0 . . ? Cl73 C5C H5C4 109.0 . . ? Cl83 C5C H5C5 109.0 . . ? Cl73 C5C H5C5 109.0 . . ? H5C4 C5C H5C5 107.8 . . ? 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 O3 Hf Al1 O1 -179.48(15) . . . . ? O2 Hf Al1 O1 -76.93(12) . . . . ? O4 Hf Al1 O1 -139.09(11) . . . . ? Cl5 Hf Al1 O1 74.73(11) . . . . ? Cl6 Hf Al1 O1 19.5(8) . . . . ? S2 Hf Al1 O1 150.91(10) . . . . ? S1 Hf Al1 O1 -6.54(10) . . . . ? Al2 Hf Al1 O1 -108.08(11) . . . . ? O2 Hf Al1 O3 102.55(12) . . . . ? O1 Hf Al1 O3 179.48(15) . . . . ? O4 Hf Al1 O3 40.39(12) . . . . ? Cl5 Hf Al1 O3 -105.79(11) . . . . ? Cl6 Hf Al1 O3 -161.0(7) . . . . ? S2 Hf Al1 O3 -29.61(11) . . . . ? S1 Hf Al1 O3 172.94(11) . . . . ? Al2 Hf Al1 O3 71.40(11) . . . . ? O3 Hf Al1 C1 -90.8(12) . . . . ? O2 Hf Al1 C1 11.7(12) . . . . ? O1 Hf Al1 C1 88.6(12) . . . . ? O4 Hf Al1 C1 -50.5(12) . . . . ? Cl5 Hf Al1 C1 163.4(12) . . . . ? Cl6 Hf Al1 C1 108.1(14) . . . . ? S2 Hf Al1 C1 -120.5(12) . . . . ? S1 Hf Al1 C1 82.1(12) . . . . ? Al2 Hf Al1 C1 -19.4(12) . . . . ? O3 Hf Al1 C2 82.2(13) . . . . ? O2 Hf Al1 C2 -175.2(13) . . . . ? O1 Hf Al1 C2 -98.3(13) . . . . ? O4 Hf Al1 C2 122.6(13) . . . . ? Cl5 Hf Al1 C2 -23.6(13) . . . . ? Cl6 Hf Al1 C2 -78.8(15) . . . . ? S2 Hf Al1 C2 52.6(13) . . . . ? S1 Hf Al1 C2 -104.9(13) . . . . ? Al2 Hf Al1 C2 153.6(13) . . . . ? O3 Hf Al1 Cl2 83.5(2) . . . . ? O2 Hf Al1 Cl2 -173.9(2) . . . . ? O1 Hf Al1 Cl2 -97.0(2) . . . . ? O4 Hf Al1 Cl2 123.9(2) . . . . ? Cl5 Hf Al1 Cl2 -22.3(2) . . . . ? Cl6 Hf Al1 Cl2 -77.5(8) . . . . ? S2 Hf Al1 Cl2 53.9(2) . . . . ? S1 Hf Al1 Cl2 -103.5(2) . . . . ? Al2 Hf Al1 Cl2 154.9(2) . . . . ? O3 Hf Al1 Cl1 -88.8(2) . . . . ? O2 Hf Al1 Cl1 13.72(18) . . . . ? O1 Hf Al1 Cl1 90.7(2) . . . . ? O4 Hf Al1 Cl1 -48.44(18) . . . . ? Cl5 Hf Al1 Cl1 165.38(17) . . . . ? Cl6 Hf Al1 Cl1 110.1(8) . . . . ? S2 Hf Al1 Cl1 -118.44(18) . . . . ? S1 Hf Al1 Cl1 84.11(18) . . . . ? Al2 Hf Al1 Cl1 -17.43(18) . . . . ? O3 Hf Al2 O4 -79.66(12) . . . . ? O2 Hf Al2 O4 176.55(15) . . . . ? O1 Hf Al2 O4 -142.42(11) . . . . ? Cl5 Hf Al2 O4 -49.0(5) . . . . ? Cl6 Hf Al2 O4 70.77(11) . . . . ? S2 Hf Al2 O4 -9.08(10) . . . . ? S1 Hf Al2 O4 147.87(10) . . . . ? Al1 Hf Al2 O4 -110.84(11) . . . . ? O3 Hf Al2 O2 103.79(12) . . . . ? O1 Hf Al2 O2 41.03(12) . . . . ? O4 Hf Al2 O2 -176.55(15) . . . . ? Cl5 Hf Al2 O2 134.4(5) . . . . ? Cl6 Hf Al2 O2 -105.78(11) . . . . ? S2 Hf Al2 O2 174.37(11) . . . . ? S1 Hf Al2 O2 -28.68(11) . . . . ? Al1 Hf Al2 O2 72.61(11) . . . . ? O3 Hf Al2 C4 10.0(12) . . . . ? O2 Hf Al2 C4 -93.7(12) . . . . ? O1 Hf Al2 C4 -52.7(12) . . . . ? O4 Hf Al2 C4 89.7(12) . . . . ? Cl5 Hf Al2 C4 40.7(13) . . . . ? Cl6 Hf Al2 C4 160.5(12) . . . . ? S2 Hf Al2 C4 80.6(12) . . . . ? S1 Hf Al2 C4 -122.4(12) . . . . ? Al1 Hf Al2 C4 -21.1(12) . . . . ? O3 Hf Al2 Cl3 -174.7(2) . . . . ? O2 Hf Al2 Cl3 81.5(2) . . . . ? O1 Hf Al2 Cl3 122.5(2) . . . . ? O4 Hf Al2 Cl3 -95.1(2) . . . . ? Cl5 Hf Al2 Cl3 -144.1(5) . . . . ? Cl6 Hf Al2 Cl3 -24.3(2) . . . . ? S2 Hf Al2 Cl3 -104.1(2) . . . . ? S1 Hf Al2 Cl3 52.8(2) . . . . ? Al1 Hf Al2 Cl3 154.1(2) . . . . ? O3 Hf Al2 Cl4 9.03(18) . . . . ? O2 Hf Al2 Cl4 -94.8(2) . . . . ? O1 Hf Al2 Cl4 -53.72(18) . . . . ? O4 Hf Al2 Cl4 88.7(2) . . . . ? Cl5 Hf Al2 Cl4 39.7(5) . . . . ? Cl6 Hf Al2 Cl4 159.47(17) . . . . ? S2 Hf Al2 Cl4 79.62(17) . . . . ? S1 Hf Al2 Cl4 -123.43(17) . . . . ? Al1 Hf Al2 Cl4 -22.14(17) . . . . ? O3 Hf Al2 C3 -177.9(13) . . . . ? O2 Hf Al2 C3 78.3(13) . . . . ? O1 Hf Al2 C3 119.4(13) . . . . ? O4 Hf Al2 C3 -98.2(13) . . . . ? Cl5 Hf Al2 C3 -147.2(14) . . . . ? Cl6 Hf Al2 C3 -27.5(13) . . . . ? S2 Hf Al2 C3 -107.3(13) . . . . ? S1 Hf Al2 C3 49.6(13) . . . . ? Al1 Hf Al2 C3 150.9(13) . . . . ? O3 Hf S1 C11 31.42(13) . . . . ? O2 Hf S1 C11 104.41(12) . . . . ? O1 Hf S1 C11 22.40(11) . . . . ? O4 Hf S1 C11 141.23(12) . . . . ? Cl5 Hf S1 C11 -58.98(10) . . . . ? Cl6 Hf S1 C11 -152.88(10) . . . . ? S2 Hf S1 C11 -107.57(11) . . . . ? Al1 Hf S1 C11 26.20(10) . . . . ? Al2 Hf S1 C11 120.09(10) . . . . ? O3 Hf S1 C21 -66.74(13) . . . . ? O2 Hf S1 C21 6.24(11) . . . . ? O1 Hf S1 C21 -75.77(12) . . . . ? O4 Hf S1 C21 43.06(12) . . . . ? Cl5 Hf S1 C21 -157.14(10) . . . . ? Cl6 Hf S1 C21 108.95(10) . . . . ? S2 Hf S1 C21 154.26(10) . . . . ? Al1 Hf S1 C21 -71.96(10) . . . . ? Al2 Hf S1 C21 21.92(10) . . . . ? O3 Hf S2 C41 104.75(12) . . . . ? O2 Hf S2 C41 31.21(13) . . . . ? O1 Hf S2 C41 140.70(12) . . . . ? O4 Hf S2 C41 21.86(11) . . . . ? Cl5 Hf S2 C41 -154.99(10) . . . . ? Cl6 Hf S2 C41 -60.57(10) . . . . ? S1 Hf S2 C41 -105.35(11) . . . . ? Al1 Hf S2 C41 120.98(10) . . . . ? Al2 Hf S2 C41 27.10(10) . . . . ? O3 Hf S2 C31 5.96(12) . . . . ? O2 Hf S2 C31 -67.57(13) . . . . ? O1 Hf S2 C31 41.92(12) . . . . ? O4 Hf S2 C31 -76.92(12) . . . . ? Cl5 Hf S2 C31 106.23(11) . . . . ? Cl6 Hf S2 C31 -159.35(10) . . . . ? S1 Hf S2 C31 155.87(10) . . . . ? Al1 Hf S2 C31 22.19(10) . . . . ? Al2 Hf S2 C31 -71.68(11) . . . . ? O3 Al1 O1 C10 -157.3(2) . . . . ? C1 Al1 O1 C10 90.1(12) . . . . ? C2 Al1 O1 C10 -50.7(13) . . . . ? Cl2 Al1 O1 C10 -48.3(3) . . . . ? Cl1 Al1 O1 C10 89.8(3) . . . . ? Hf Al1 O1 C10 -156.9(3) . . . . ? O3 Al1 O1 Hf -0.33(10) . . . . ? C1 Al1 O1 Hf -113.0(12) . . . . ? C2 Al1 O1 Hf 106.2(13) . . . . ? Cl2 Al1 O1 Hf 108.6(2) . . . . ? Cl1 Al1 O1 Hf -113.30(18) . . . . ? O3 Hf O1 C10 157.0(2) . . . . ? O2 Hf O1 C10 -106.5(2) . . . . ? O4 Hf O1 C10 -151.6(2) . . . . ? Cl5 Hf O1 C10 55.5(2) . . . . ? Cl6 Hf O1 C10 -22.1(3) . . . . ? S2 Hf O1 C10 118.9(2) . . . . ? S1 Hf O1 C10 -30.2(2) . . . . ? Al1 Hf O1 C10 156.7(3) . . . . ? Al2 Hf O1 C10 -127.8(2) . . . . ? O3 Hf O1 Al1 0.31(9) . . . . ? O2 Hf O1 Al1 96.82(11) . . . . ? O4 Hf O1 Al1 51.76(13) . . . . ? Cl5 Hf O1 Al1 -101.22(10) . . . . ? Cl6 Hf O1 Al1 -178.81(5) . . . . ? S2 Hf O1 Al1 -37.76(12) . . . . ? S1 Hf O1 Al1 173.08(11) . . . . ? Al2 Hf O1 Al1 75.55(10) . . . . ? O4 Al2 O2 C20 162.7(2) . . . . ? C4 Al2 O2 C20 -87.8(12) . . . . ? Cl3 Al2 O2 C20 45.5(3) . . . . ? Cl4 Al2 O2 C20 -87.9(3) . . . . ? C3 Al2 O2 C20 45.8(13) . . . . ? Hf Al2 O2 C20 165.1(3) . . . . ? O4 Al2 O2 Hf -2.40(11) . . . . ? C4 Al2 O2 Hf 107.1(12) . . . . ? Cl3 Al2 O2 Hf -119.6(2) . . . . ? Cl4 Al2 O2 Hf 107.07(18) . . . . ? C3 Al2 O2 Hf -119.2(12) . . . . ? O3 Hf O2 C20 122.3(2) . . . . ? O1 Hf O2 C20 57.6(2) . . . . ? O4 Hf O2 C20 -161.8(2) . . . . ? Cl5 Hf O2 C20 20.6(3) . . . . ? Cl6 Hf O2 C20 -87.5(2) . . . . ? S2 Hf O2 C20 -171.41(19) . . . . ? S1 Hf O2 C20 -13.5(2) . . . . ? Al1 Hf O2 C20 90.4(2) . . . . ? Al2 Hf O2 C20 -163.9(3) . . . . ? O3 Hf O2 Al2 -73.87(11) . . . . ? O1 Hf O2 Al2 -138.49(11) . . . . ? O4 Hf O2 Al2 2.05(9) . . . . ? Cl5 Hf O2 Al2 -175.50(5) . . . . ? Cl6 Hf O2 Al2 76.35(10) . . . . ? S2 Hf O2 Al2 -7.54(14) . . . . ? S1 Hf O2 Al2 150.39(11) . . . . ? Al1 Hf O2 Al2 -105.69(10) . . . . ? O1 Al1 O3 C30 163.7(2) . . . . ? C1 Al1 O3 C30 -86.8(12) . . . . ? C2 Al1 O3 C30 48.2(12) . . . . ? Cl2 Al1 O3 C30 47.8(3) . . . . ? Cl1 Al1 O3 C30 -84.0(3) . . . . ? Hf Al1 O3 C30 163.3(3) . . . . ? O1 Al1 O3 Hf 0.36(11) . . . . ? C1 Al1 O3 Hf 109.9(12) . . . . ? C2 Al1 O3 Hf -115.1(12) . . . . ? Cl2 Al1 O3 Hf -115.5(2) . . . . ? Cl1 Al1 O3 Hf 112.72(18) . . . . ? O2 Hf O3 C30 123.1(2) . . . . ? O1 Hf O3 C30 -161.9(3) . . . . ? O4 Hf O3 C30 58.8(2) . . . . ? Cl5 Hf O3 C30 -86.7(2) . . . . ? Cl6 Hf O3 C30 17.1(3) . . . . ? S2 Hf O3 C30 -12.1(2) . . . . ? S1 Hf O3 C30 -171.1(2) . . . . ? Al1 Hf O3 C30 -161.6(3) . . . . ? Al2 Hf O3 C30 91.7(2) . . . . ? O2 Hf O3 Al1 -75.27(11) . . . . ? O1 Hf O3 Al1 -0.31(9) . . . . ? O4 Hf O3 Al1 -139.58(11) . . . . ? Cl5 Hf O3 Al1 74.92(10) . . . . ? Cl6 Hf O3 Al1 178.71(5) . . . . ? S2 Hf O3 Al1 149.51(11) . . . . ? S1 Hf O3 Al1 -9.52(14) . . . . ? Al2 Hf O3 Al1 -106.71(10) . . . . ? O2 Al2 O4 C40 -160.4(2) . . . . ? C4 Al2 O4 C40 86.2(12) . . . . ? Cl3 Al2 O4 C40 -49.8(3) . . . . ? Cl4 Al2 O4 C40 84.9(3) . . . . ? C3 Al2 O4 C40 -54.7(12) . . . . ? Hf Al2 O4 C40 -162.6(3) . . . . ? O2 Al2 O4 Hf 2.23(10) . . . . ? C4 Al2 O4 Hf -111.2(12) . . . . ? Cl3 Al2 O4 Hf 112.78(18) . . . . ? Cl4 Al2 O4 Hf -112.51(18) . . . . ? C3 Al2 O4 Hf 107.9(12) . . . . ? O3 Hf O4 C40 -103.4(2) . . . . ? O2 Hf O4 C40 160.4(2) . . . . ? O1 Hf O4 C40 -150.2(2) . . . . ? Cl5 Hf O4 C40 -21.8(3) . . . . ? Cl6 Hf O4 C40 56.3(2) . . . . ? S2 Hf O4 C40 -27.1(2) . . . . ? S1 Hf O4 C40 121.3(2) . . . . ? Al1 Hf O4 C40 -124.4(2) . . . . ? Al2 Hf O4 C40 162.5(3) . . . . ? O3 Hf O4 Al2 94.14(11) . . . . ? O2 Hf O4 Al2 -2.04(9) . . . . ? O1 Hf O4 Al2 47.33(14) . . . . ? Cl5 Hf O4 Al2 175.78(5) . . . . ? Cl6 Hf O4 Al2 -106.13(10) . . . . ? S2 Hf O4 Al2 170.39(11) . . . . ? S1 Hf O4 Al2 -41.13(12) . . . . ? Al1 Hf O4 Al2 73.11(10) . . . . ? Al1 O1 C10 C15 -2.5(4) . . . . ? Hf O1 C10 C15 -154.2(2) . . . . ? Al1 O1 C10 C11 179.0(2) . . . . ? Hf O1 C10 C11 27.3(4) . . . . ? O1 C10 C11 C12 -179.5(3) . . . . ? C15 C10 C11 C12 1.9(5) . . . . ? O1 C10 C11 S1 2.8(4) . . . . ? C15 C10 C11 S1 -175.8(2) . . . . ? C21 S1 C11 C10 78.0(3) . . . . ? Hf S1 C11 C10 -21.5(2) . . . . ? C21 S1 C11 C12 -99.7(3) . . . . ? Hf S1 C11 C12 160.8(2) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? S1 C11 C12 C13 177.5(2) . . . . ? C11 C12 C13 C14 -1.8(4) . . . . ? C11 C12 C13 C16 176.2(3) . . . . ? C12 C13 C14 C15 1.8(5) . . . . ? C16 C13 C14 C15 -176.2(3) . . . . ? C13 C14 C15 C10 0.0(5) . . . . ? O1 C10 C15 C14 179.6(3) . . . . ? C11 C10 C15 C14 -1.9(5) . . . . ? C12 C13 C16 C17 125.9(3) . . . . ? C14 C13 C16 C17 -56.1(4) . . . . ? C12 C13 C16 C18 7.4(4) . . . . ? C14 C13 C16 C18 -174.7(3) . . . . ? C12 C13 C16 C19 -118.1(3) . . . . ? C14 C13 C16 C19 59.8(4) . . . . ? C13 C16 C19 C110 64.1(4) . . . . ? C17 C16 C19 C110 -177.8(3) . . . . ? C18 C16 C19 C110 -61.8(4) . . . . ? C16 C19 C110 C111 -54.6(4) . . . . ? C16 C19 C110 C112 -172.5(3) . . . . ? C16 C19 C110 C113 69.6(4) . . . . ? Al2 O2 C20 C21 -143.9(2) . . . . ? Hf O2 C20 C21 17.8(4) . . . . ? Al2 O2 C20 C25 35.2(4) . . . . ? Hf O2 C20 C25 -163.1(2) . . . . ? C25 C20 C21 C22 -1.6(5) . . . . ? O2 C20 C21 C22 177.5(3) . . . . ? C25 C20 C21 S1 172.7(2) . . . . ? O2 C20 C21 S1 -8.2(4) . . . . ? C11 S1 C21 C20 -102.2(3) . . . . ? Hf S1 C21 C20 -1.3(2) . . . . ? C11 S1 C21 C22 72.2(3) . . . . ? Hf S1 C21 C22 173.0(2) . . . . ? C20 C21 C22 C23 0.2(5) . . . . ? S1 C21 C22 C23 -174.0(2) . . . . ? C21 C22 C23 C24 1.0(5) . . . . ? C21 C22 C23 C26 -179.1(3) . . . . ? C22 C23 C24 C25 -0.8(5) . . . . ? C26 C23 C24 C25 179.3(3) . . . . ? C23 C24 C25 C20 -0.6(5) . . . . ? C21 C20 C25 C24 1.8(5) . . . . ? O2 C20 C25 C24 -177.3(3) . . . . ? C22 C23 C26 C27 6.8(4) . . . . ? C24 C23 C26 C27 -173.3(3) . . . . ? C22 C23 C26 C28 123.1(3) . . . . ? C24 C23 C26 C28 -57.0(4) . . . . ? C22 C23 C26 C29 -120.0(3) . . . . ? C24 C23 C26 C29 59.9(4) . . . . ? C27 C26 C29 C210 -69.5(4) . . . . ? C23 C26 C29 C210 57.3(4) . . . . ? C28 C26 C29 C210 175.2(3) . . . . ? C26 C29 C210 C213 54.5(5) . . . . ? C26 C29 C210 C212 -70.4(4) . . . . ? C26 C29 C210 C211 173.2(3) . . . . ? Al1 O3 C30 C31 -144.1(2) . . . . ? Hf O3 C30 C31 15.3(4) . . . . ? Al1 O3 C30 C35 35.3(4) . . . . ? Hf O3 C30 C35 -165.2(2) . . . . ? C35 C30 C31 C32 -0.2(5) . . . . ? O3 C30 C31 C32 179.3(3) . . . . ? C35 C30 C31 S2 174.3(2) . . . . ? O3 C30 C31 S2 -6.2(4) . . . . ? C41 S2 C31 C30 -103.0(3) . . . . ? Hf S2 C31 C30 -2.0(3) . . . . ? C41 S2 C31 C32 71.5(3) . . . . ? Hf S2 C31 C32 172.6(2) . . . . ? C30 C31 C32 C33 0.5(5) . . . . ? S2 C31 C32 C33 -173.9(2) . . . . ? C31 C32 C33 C34 -1.4(5) . . . . ? C31 C32 C33 C36 176.6(3) . . . . ? C32 C33 C34 C35 1.9(5) . . . . ? C36 C33 C34 C35 -176.1(3) . . . . ? C31 C30 C35 C34 0.7(5) . . . . ? O3 C30 C35 C34 -178.7(3) . . . . ? C33 C34 C35 C30 -1.6(5) . . . . ? C32 C33 C36 C37 3.5(5) . . . . ? C34 C33 C36 C37 -178.6(3) . . . . ? C32 C33 C36 C38 121.1(3) . . . . ? C34 C33 C36 C38 -61.0(4) . . . . ? C32 C33 C36 C39 -122.3(3) . . . . ? C34 C33 C36 C39 55.6(4) . . . . ? C33 C36 C39 C310 66.3(4) . . . . ? C37 C36 C39 C310 -59.3(4) . . . . ? C38 C36 C39 C310 -176.5(3) . . . . ? C36 C39 C310 C313 -44.4(5) . . . . ? C36 C39 C310 C311 -164.1(3) . . . . ? C36 C39 C310 C312 79.7(4) . . . . ? Al2 O4 C40 C41 -179.6(2) . . . . ? Hf O4 C40 C41 21.8(4) . . . . ? Al2 O4 C40 C45 0.5(4) . . . . ? Hf O4 C40 C45 -158.1(2) . . . . ? C45 C40 C41 C42 2.7(5) . . . . ? O4 C40 C41 C42 -177.2(3) . . . . ? C45 C40 C41 S2 -172.9(2) . . . . ? O4 C40 C41 S2 7.2(4) . . . . ? C31 S2 C41 C40 76.0(3) . . . . ? Hf S2 C41 C40 -23.4(2) . . . . ? C31 S2 C41 C42 -99.6(3) . . . . ? Hf S2 C41 C42 161.0(2) . . . . ? C40 C41 C42 C43 -0.3(4) . . . . ? S2 C41 C42 C43 175.1(2) . . . . ? C41 C42 C43 C44 -2.3(4) . . . . ? C41 C42 C43 C46 178.2(3) . . . . ? C42 C43 C44 C45 2.6(5) . . . . ? C46 C43 C44 C45 -177.9(3) . . . . ? C41 C40 C45 C44 -2.4(5) . . . . ? O4 C40 C45 C44 177.5(3) . . . . ? C43 C44 C45 C40 -0.3(5) . . . . ? C42 C43 C46 C47 -12.5(4) . . . . ? C44 C43 C46 C47 168.0(3) . . . . ? C42 C43 C46 C48 -129.5(3) . . . . ? C44 C43 C46 C48 51.0(4) . . . . ? C42 C43 C46 C49 107.8(3) . . . . ? C44 C43 C46 C49 -71.7(4) . . . . ? C47 C46 C49 C410 -75.5(4) . . . . ? C43 C46 C49 C410 164.8(3) . . . . ? C48 C46 C49 C410 45.8(4) . . . . ? C46 C49 C410 C413 -70.7(4) . . . . ? C46 C49 C410 C412 54.4(4) . . . . ? C46 C49 C410 C411 172.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.662 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.101 # Attachment '5rev.cif' data_zj72 _database_code_depnum_ccdc_archive 'CCDC 721083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H80 Al2 Cl6 O4 S2 Zr, 0.5(C6 H14)' _chemical_formula_sum 'C59 H87 Al2 Cl6 O4 S2 Zr' _chemical_formula_weight 1282.29 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' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.737(5) _cell_length_b 15.552(5) _cell_length_c 16.690(5) _cell_angle_alpha 73.73(2) _cell_angle_beta 86.36(2) _cell_angle_gamma 62.22(2) _cell_volume 3239(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7418 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 0.551 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.8230 _exptl_absorpt_correction_T_max 0.9124 _exptl_absorpt_process_details ; CrysAlis RED V1.171.13, Oxford Diffraction Ltd., Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD kappa-axis diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26815 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.1212 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.89 _diffrn_reflns_theta_max 27.00 _reflns_number_total 13944 _reflns_number_gt 8625 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD V1.171.3,Oxford Diffraction Ltd.,2006' _computing_cell_refinement 'CrysAlis RED V1.171.3,Oxford Diffraction Ltd.,2006' _computing_data_reduction ' CrysAlis RED V1.171.3,Oxford Diffraction Ltd.,2006' _computing_structure_solution 'SHELXTL V6.14, Bruker AXS 2003' _computing_structure_refinement 'SHELXTL V6.14, Bruker AXS 2003' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXTL V6.14, Bruker AXS 2003' _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^)+(0.0333P)^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 13944 _refine_ls_number_parameters 688 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1025 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.0916 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 Zr Zr 0.38512(2) 0.33026(2) 0.267279(19) 0.01344(9) Uani 1 1 d . . . S1 S 0.43176(6) 0.42853(6) 0.11798(5) 0.01402(18) Uani 1 1 d . . . S2 S 0.43845(6) 0.15890(6) 0.40273(5) 0.01450(19) Uani 1 1 d . . . Al1 Al 0.30242(8) 0.50314(7) 0.36351(6) 0.0165(2) Uani 1 1 d . . . Al2 Al 0.15174(8) 0.38556(8) 0.21685(6) 0.0177(2) Uani 1 1 d . . . Cl1 Cl 0.55530(6) 0.30001(6) 0.30100(5) 0.01967(19) Uani 1 1 d . . . Cl2 Cl 0.44771(6) 0.19864(6) 0.19919(5) 0.02011(19) Uani 1 1 d . . . Cl3 Cl 0.38945(7) 0.57177(7) 0.38187(5) 0.0268(2) Uani 1 1 d . . . Cl4 Cl 0.15292(7) 0.56575(7) 0.40086(6) 0.0317(2) Uani 1 1 d . . . Cl5 Cl 0.10854(7) 0.28373(7) 0.19362(6) 0.0316(2) Uani 1 1 d . . . Cl6 Cl 0.02881(7) 0.52716(7) 0.21297(6) 0.0323(2) Uani 1 1 d . . . O1 O 0.30971(16) 0.49265(15) 0.25820(12) 0.0151(5) Uani 1 1 d . . . O2 O 0.25314(16) 0.39942(16) 0.16183(12) 0.0162(5) Uani 1 1 d . . . O3 O 0.36501(16) 0.36863(15) 0.39483(12) 0.0162(5) Uani 1 1 d . . . O4 O 0.24131(15) 0.32552(16) 0.30861(12) 0.0155(5) Uani 1 1 d . . . C10 C 0.2951(2) 0.5741(2) 0.18846(19) 0.0149(7) Uani 1 1 d . . . C11 C 0.3511(2) 0.5565(2) 0.12061(19) 0.0143(7) Uani 1 1 d . . . C12 C 0.3391(2) 0.6364(2) 0.05159(19) 0.0160(7) Uani 1 1 d . . . H12A H 0.3785 0.6231 0.0051 0.019 Uiso 1 1 calc R . . C13 C 0.2708(3) 0.7349(2) 0.0496(2) 0.0185(8) Uani 1 1 d . . . C14 C 0.2158(3) 0.7513(3) 0.1198(2) 0.0225(8) Uani 1 1 d . . . H14A H 0.1698 0.8188 0.1203 0.027 Uiso 1 1 calc R . . C15 C 0.2264(3) 0.6721(3) 0.1884(2) 0.0212(8) Uani 1 1 d . . . H15A H 0.1870 0.6849 0.2350 0.025 Uiso 1 1 calc R . . C16 C 0.2505(3) 0.8248(2) -0.0273(2) 0.0233(8) Uani 1 1 d . . . C17 C 0.2719(4) 0.8998(3) -0.0014(3) 0.0498(12) Uani 1 1 d . . . H17A H 0.3430 0.8662 0.0228 0.075 Uiso 1 1 calc R . . H17B H 0.2248 0.9253 0.0403 0.075 Uiso 1 1 calc R . . H17C H 0.2617 0.9566 -0.0505 0.075 Uiso 1 1 calc R . . C18 C 0.3165(3) 0.7922(3) -0.0981(2) 0.0455(12) Uani 1 1 d . . . H18A H 0.3887 0.7689 -0.0817 0.068 Uiso 1 1 calc R . . H18B H 0.2937 0.8498 -0.1487 0.068 Uiso 1 1 calc R . . H18C H 0.3095 0.7369 -0.1093 0.068 Uiso 1 1 calc R . . C19 C 0.1324(3) 0.8831(3) -0.0592(2) 0.0376(10) Uani 1 1 d . . . H19A H 0.0937 0.9028 -0.0111 0.045 Uiso 1 1 calc R . . H19B H 0.1212 0.9468 -0.1016 0.045 Uiso 1 1 calc R . . C110 C 0.0793(3) 0.8382(3) -0.0966(2) 0.0362(10) Uani 1 1 d . . . C111 C -0.0360(3) 0.9042(4) -0.0922(3) 0.0613(14) Uani 1 1 d . . . H11A H -0.0544 0.9755 -0.1188 0.092 Uiso 1 1 calc R . . H11B H -0.0521 0.8951 -0.0335 0.092 Uiso 1 1 calc R . . H11C H -0.0753 0.8842 -0.1215 0.092 Uiso 1 1 calc R . . C112 C 0.0968(3) 0.8443(3) -0.1893(2) 0.0484(12) Uani 1 1 d . . . H11D H 0.1698 0.8020 -0.1949 0.073 Uiso 1 1 calc R . . H11E H 0.0761 0.9147 -0.2213 0.073 Uiso 1 1 calc R . . H11F H 0.0556 0.8199 -0.2109 0.073 Uiso 1 1 calc R . . C113 C 0.1070(3) 0.7277(3) -0.0502(3) 0.0509(13) Uani 1 1 d . . . H11G H 0.1798 0.6837 -0.0550 0.076 Uiso 1 1 calc R . . H11H H 0.0644 0.7072 -0.0749 0.076 Uiso 1 1 calc R . . H11I H 0.0946 0.7216 0.0090 0.076 Uiso 1 1 calc R . . C20 C 0.2643(3) 0.4158(2) 0.07683(19) 0.0179(8) Uani 1 1 d . . . C21 C 0.3498(2) 0.4250(2) 0.04641(19) 0.0133(7) Uani 1 1 d . . . C22 C 0.3680(2) 0.4366(2) -0.03761(19) 0.0163(8) Uani 1 1 d . . . H22A H 0.4280 0.4415 -0.0568 0.020 Uiso 1 1 calc R . . C23 C 0.2994(3) 0.4412(2) -0.09373(19) 0.0176(8) Uani 1 1 d . . . C24 C 0.2118(3) 0.4369(3) -0.0630(2) 0.0209(8) Uani 1 1 d . . . H24A H 0.1621 0.4432 -0.1009 0.025 Uiso 1 1 calc R . . C25 C 0.1939(2) 0.4238(3) 0.0206(2) 0.0203(8) Uani 1 1 d . . . H25A H 0.1333 0.4203 0.0395 0.024 Uiso 1 1 calc R . . C26 C 0.3184(2) 0.4495(3) -0.18760(19) 0.0186(8) Uani 1 1 d . . . C27 C 0.4295(2) 0.4310(3) -0.2021(2) 0.0266(9) Uani 1 1 d . . . H27A H 0.4444 0.4259 -0.2592 0.040 Uiso 1 1 calc R . . H27B H 0.4774 0.3679 -0.1618 0.040 Uiso 1 1 calc R . . H27C H 0.4373 0.4876 -0.1947 0.040 Uiso 1 1 calc R . . C28 C 0.3062(3) 0.3658(3) -0.2088(2) 0.0270(9) Uani 1 1 d . . . H28A H 0.3269 0.3634 -0.2655 0.041 Uiso 1 1 calc R . . H28B H 0.2342 0.3799 -0.2061 0.041 Uiso 1 1 calc R . . H28C H 0.3498 0.3004 -0.1686 0.041 Uiso 1 1 calc R . . C29 C 0.2389(3) 0.5577(3) -0.2376(2) 0.0219(8) Uani 1 1 d . . . H29A H 0.2597 0.6046 -0.2244 0.026 Uiso 1 1 calc R . . H29B H 0.1726 0.5704 -0.2128 0.026 Uiso 1 1 calc R . . C210 C 0.2148(3) 0.5936(3) -0.3339(2) 0.0219(8) Uani 1 1 d . . . C211 C 0.1426(3) 0.7080(3) -0.3561(2) 0.0382(10) Uani 1 1 d . . . H21A H 0.1785 0.7421 -0.3422 0.057 Uiso 1 1 calc R . . H21B H 0.0817 0.7210 -0.3243 0.057 Uiso 1 1 calc R . . H21C H 0.1214 0.7342 -0.4162 0.057 Uiso 1 1 calc R . . C212 C 0.3097(3) 0.5760(3) -0.3830(2) 0.0291(9) Uani 1 1 d . . . H21D H 0.3476 0.6055 -0.3644 0.044 Uiso 1 1 calc R . . H21E H 0.2883 0.6082 -0.4428 0.044 Uiso 1 1 calc R . . H21F H 0.3540 0.5030 -0.3733 0.044 Uiso 1 1 calc R . . C213 C 0.1585(3) 0.5439(3) -0.3617(2) 0.0345(10) Uani 1 1 d . . . H21G H 0.1272 0.5820 -0.4190 0.052 Uiso 1 1 calc R . . H21H H 0.1048 0.5441 -0.3240 0.052 Uiso 1 1 calc R . . H21I H 0.2077 0.4740 -0.3601 0.052 Uiso 1 1 calc R . . C30 C 0.4219(2) 0.3048(2) 0.46955(19) 0.0161(7) Uani 1 1 d . . . C31 C 0.4658(2) 0.2010(3) 0.48220(19) 0.0154(7) Uani 1 1 d . . . C32 C 0.5247(2) 0.1333(2) 0.55562(19) 0.0162(7) Uani 1 1 d . . . H32A H 0.5539 0.0625 0.5630 0.019 Uiso 1 1 calc R . . C33 C 0.5415(2) 0.1684(3) 0.6190(2) 0.0175(8) Uani 1 1 d . . . C34 C 0.4948(3) 0.2724(3) 0.6056(2) 0.0203(8) Uani 1 1 d . . . H34A H 0.5033 0.2982 0.6483 0.024 Uiso 1 1 calc R . . C35 C 0.4362(3) 0.3401(3) 0.5324(2) 0.0197(8) Uani 1 1 d . . . H35A H 0.4058 0.4110 0.5253 0.024 Uiso 1 1 calc R . . C36 C 0.6094(3) 0.0960(3) 0.6998(2) 0.0206(8) Uani 1 1 d . . . C37 C 0.5454(3) 0.1184(3) 0.7741(2) 0.0429(11) Uani 1 1 d . . . H37A H 0.4825 0.1134 0.7680 0.064 Uiso 1 1 calc R . . H37B H 0.5272 0.1870 0.7759 0.064 Uiso 1 1 calc R . . H37C H 0.5855 0.0692 0.8262 0.064 Uiso 1 1 calc R . . C38 C 0.6442(3) -0.0150(3) 0.7057(2) 0.0385(11) Uani 1 1 d . . . H38A H 0.5846 -0.0276 0.7122 0.058 Uiso 1 1 calc R . . H38B H 0.6943 -0.0589 0.7542 0.058 Uiso 1 1 calc R . . H38C H 0.6762 -0.0297 0.6545 0.058 Uiso 1 1 calc R . . C39 C 0.7004(3) 0.1158(3) 0.7101(2) 0.0278(9) Uani 1 1 d . . . H39A H 0.7342 0.0739 0.7669 0.033 Uiso 1 1 calc R . . H39B H 0.6702 0.1874 0.7107 0.033 Uiso 1 1 calc R . . C310 C 0.7881(3) 0.0993(3) 0.6499(2) 0.0283(9) Uani 1 1 d . . . C311 C 0.8584(3) -0.0119(3) 0.6543(2) 0.0386(10) Uani 1 1 d . . . H31A H 0.9189 -0.0178 0.6234 0.058 Uiso 1 1 calc R . . H31B H 0.8210 -0.0374 0.6293 0.058 Uiso 1 1 calc R . . H31C H 0.8805 -0.0518 0.7129 0.058 Uiso 1 1 calc R . . C312 C 0.7492(3) 0.1599(3) 0.5590(2) 0.0310(9) Uani 1 1 d . . . H31D H 0.8075 0.1571 0.5261 0.047 Uiso 1 1 calc R . . H31E H 0.7012 0.2305 0.5561 0.047 Uiso 1 1 calc R . . H31F H 0.7137 0.1309 0.5362 0.047 Uiso 1 1 calc R . . C313 C 0.8520(3) 0.1399(3) 0.6802(3) 0.0460(12) Uani 1 1 d . . . H31G H 0.9130 0.1268 0.6484 0.069 Uiso 1 1 calc R . . H31H H 0.8735 0.1058 0.7399 0.069 Uiso 1 1 calc R . . H31I H 0.8106 0.2130 0.6718 0.069 Uiso 1 1 calc R . . C40 C 0.2277(2) 0.2648(2) 0.38244(19) 0.0157(7) Uani 1 1 d . . . C41 C 0.3115(2) 0.1805(2) 0.42901(19) 0.0156(7) Uani 1 1 d . . . C42 C 0.2980(2) 0.1164(2) 0.50057(19) 0.0152(7) Uani 1 1 d . . . H42A H 0.3566 0.0580 0.5317 0.018 Uiso 1 1 calc R . . C43 C 0.2014(3) 0.1360(3) 0.5273(2) 0.0185(8) Uani 1 1 d . . . C44 C 0.1183(3) 0.2234(3) 0.4791(2) 0.0215(8) Uani 1 1 d . . . H44A H 0.0508 0.2393 0.4959 0.026 Uiso 1 1 calc R . . C45 C 0.1303(3) 0.2876(3) 0.4079(2) 0.0205(8) Uani 1 1 d . . . H45A H 0.0721 0.3467 0.3769 0.025 Uiso 1 1 calc R . . C46 C 0.1834(3) 0.0665(3) 0.6038(2) 0.0199(8) Uani 1 1 d . . . C47 C 0.1094(3) 0.0342(3) 0.5758(2) 0.0287(9) Uani 1 1 d . . . H47A H 0.0436 0.0943 0.5531 0.043 Uiso 1 1 calc R . . H47B H 0.0980 -0.0120 0.6239 0.043 Uiso 1 1 calc R . . H47C H 0.1394 -0.0003 0.5325 0.043 Uiso 1 1 calc R . . C48 C 0.2834(3) -0.0319(2) 0.6410(2) 0.0273(9) Uani 1 1 d . . . H48A H 0.3112 -0.0683 0.5987 0.041 Uiso 1 1 calc R . . H48B H 0.2686 -0.0748 0.6896 0.041 Uiso 1 1 calc R . . H48C H 0.3339 -0.0150 0.6585 0.041 Uiso 1 1 calc R . . C49 C 0.1297(3) 0.1221(3) 0.6709(2) 0.0222(8) Uani 1 1 d . . . H49A H 0.0600 0.1746 0.6455 0.027 Uiso 1 1 calc R . . H49B H 0.1199 0.0719 0.7173 0.027 Uiso 1 1 calc R . . C410 C 0.1722(3) 0.1743(3) 0.7120(2) 0.0259(9) Uani 1 1 d . . . C411 C 0.2808(3) 0.1071(4) 0.7522(3) 0.0565(14) Uani 1 1 d . . . H41A H 0.3291 0.0949 0.7084 0.085 Uiso 1 1 calc R . . H41B H 0.2867 0.0424 0.7874 0.085 Uiso 1 1 calc R . . H41C H 0.2970 0.1406 0.7866 0.085 Uiso 1 1 calc R . . C412 C 0.1005(3) 0.2070(3) 0.7809(3) 0.0462(12) Uani 1 1 d . . . H41D H 0.1267 0.2368 0.8119 0.069 Uiso 1 1 calc R . . H41E H 0.0978 0.1478 0.8193 0.069 Uiso 1 1 calc R . . H41F H 0.0312 0.2573 0.7552 0.069 Uiso 1 1 calc R . . C413 C 0.1663(4) 0.2714(3) 0.6511(3) 0.0505(13) Uani 1 1 d . . . H41G H 0.2158 0.2538 0.6089 0.076 Uiso 1 1 calc R . . H41H H 0.1827 0.3081 0.6820 0.076 Uiso 1 1 calc R . . H41I H 0.0967 0.3143 0.6234 0.076 Uiso 1 1 calc R . . C51 C 0.4433(3) 0.0213(4) -0.0065(3) 0.0608(16) Uani 1 1 d . . . H51A H 0.4235 -0.0308 0.0251 0.091 Uiso 1 1 calc R . . H51B H 0.4248 0.0362 -0.0666 0.091 Uiso 1 1 calc R . . C52 C 0.3812(5) 0.1169(4) 0.0202(3) 0.0705(17) Uani 1 1 d . . . H52A H 0.4032 0.1036 0.0791 0.106 Uiso 1 1 calc R . . H52B H 0.3968 0.1708 -0.0145 0.106 Uiso 1 1 calc R . . C53 C 0.2676(5) 0.1546(4) 0.0126(3) 0.0834(19) Uani 1 1 d . . . H53A H 0.2326 0.2150 0.0326 0.125 Uiso 1 1 calc R . . H53B H 0.2513 0.1017 0.0464 0.125 Uiso 1 1 calc R . . H53C H 0.2444 0.1719 -0.0462 0.125 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 Zr 0.01584(18) 0.01403(18) 0.01052(17) -0.00163(14) -0.00029(13) -0.00792(15) S1 0.0155(4) 0.0145(4) 0.0118(4) -0.0027(4) -0.0001(3) -0.0072(4) S2 0.0150(4) 0.0161(5) 0.0127(4) -0.0027(4) 0.0006(3) -0.0081(4) Al1 0.0204(6) 0.0149(6) 0.0119(5) -0.0035(4) 0.0005(4) -0.0066(5) Al2 0.0164(6) 0.0234(6) 0.0128(5) -0.0017(5) 0.0001(4) -0.0106(5) Cl1 0.0193(5) 0.0208(5) 0.0186(4) -0.0020(4) -0.0023(4) -0.0108(4) Cl2 0.0271(5) 0.0190(5) 0.0172(4) -0.0061(4) 0.0032(4) -0.0128(4) Cl3 0.0369(6) 0.0261(5) 0.0230(5) -0.0059(4) 0.0009(4) -0.0197(5) Cl4 0.0240(5) 0.0382(6) 0.0233(5) -0.0094(4) 0.0061(4) -0.0071(5) Cl5 0.0414(6) 0.0391(6) 0.0261(5) -0.0046(5) -0.0006(4) -0.0305(5) Cl6 0.0233(5) 0.0276(5) 0.0307(6) -0.0006(4) 0.0006(4) -0.0036(4) O1 0.0210(13) 0.0130(12) 0.0073(11) -0.0004(10) 0.0016(10) -0.0062(11) O2 0.0193(13) 0.0242(13) 0.0086(12) -0.0031(10) 0.0003(10) -0.0137(11) O3 0.0220(13) 0.0127(12) 0.0109(12) -0.0003(10) -0.0026(10) -0.0069(11) O4 0.0140(12) 0.0159(12) 0.0116(12) 0.0040(10) -0.0006(9) -0.0073(11) C10 0.0164(18) 0.0141(18) 0.0112(17) 0.0015(15) -0.0041(14) -0.0071(16) C11 0.0149(18) 0.0150(18) 0.0146(18) -0.0062(15) 0.0019(14) -0.0073(15) C12 0.0173(18) 0.0190(19) 0.0121(18) -0.0039(15) -0.0011(14) -0.0089(16) C13 0.021(2) 0.0163(19) 0.0200(19) -0.0042(16) -0.0001(15) -0.0108(17) C14 0.029(2) 0.0130(18) 0.019(2) -0.0050(16) 0.0011(16) -0.0039(17) C15 0.025(2) 0.024(2) 0.0119(18) -0.0043(16) 0.0012(15) -0.0092(18) C16 0.029(2) 0.0132(19) 0.020(2) 0.0011(16) 0.0038(17) -0.0074(17) C17 0.082(4) 0.038(3) 0.042(3) 0.001(2) -0.003(2) -0.044(3) C18 0.055(3) 0.030(2) 0.037(3) 0.005(2) 0.010(2) -0.017(2) C19 0.049(3) 0.030(2) 0.024(2) 0.0014(19) 0.003(2) -0.015(2) C110 0.047(3) 0.034(2) 0.025(2) 0.0049(19) -0.0143(19) -0.022(2) C111 0.052(3) 0.068(4) 0.048(3) -0.017(3) 0.002(2) -0.015(3) C112 0.047(3) 0.059(3) 0.031(3) -0.017(2) -0.005(2) -0.015(3) C113 0.061(3) 0.043(3) 0.052(3) 0.004(2) -0.026(2) -0.033(3) C20 0.025(2) 0.0203(19) 0.0095(17) -0.0036(15) 0.0013(15) -0.0123(17) C21 0.0156(18) 0.0121(17) 0.0112(17) -0.0026(14) -0.0013(14) -0.0059(15) C22 0.0162(18) 0.0160(18) 0.0160(18) -0.0038(15) 0.0016(14) -0.0074(16) C23 0.023(2) 0.0173(19) 0.0114(18) -0.0037(15) 0.0017(15) -0.0087(17) C24 0.020(2) 0.027(2) 0.0155(19) -0.0064(16) -0.0033(15) -0.0106(17) C25 0.0153(19) 0.029(2) 0.020(2) -0.0056(17) 0.0019(15) -0.0143(17) C26 0.0182(19) 0.028(2) 0.0100(17) -0.0081(16) 0.0015(14) -0.0101(17) C27 0.023(2) 0.042(2) 0.0129(19) -0.0101(18) 0.0043(16) -0.0123(19) C28 0.034(2) 0.029(2) 0.018(2) -0.0096(17) -0.0004(17) -0.0133(19) C29 0.020(2) 0.028(2) 0.0175(19) -0.0066(17) 0.0031(15) -0.0121(18) C210 0.026(2) 0.026(2) 0.0138(19) -0.0043(16) 0.0038(16) -0.0129(18) C211 0.049(3) 0.035(2) 0.019(2) -0.0035(19) -0.0031(19) -0.012(2) C212 0.040(2) 0.035(2) 0.016(2) -0.0058(17) 0.0026(17) -0.021(2) C213 0.038(2) 0.049(3) 0.019(2) -0.0003(19) -0.0036(18) -0.026(2) C30 0.0149(18) 0.0190(19) 0.0107(17) 0.0001(15) -0.0003(14) -0.0072(16) C31 0.0183(18) 0.0211(19) 0.0102(17) -0.0060(15) 0.0066(14) -0.0116(16) C32 0.0153(18) 0.0138(18) 0.0167(18) -0.0015(15) -0.0006(15) -0.0059(15) C33 0.0203(19) 0.023(2) 0.0128(18) -0.0039(16) 0.0020(15) -0.0138(17) C34 0.027(2) 0.027(2) 0.0119(18) -0.0054(16) -0.0002(15) -0.0165(18) C35 0.028(2) 0.0159(19) 0.0165(19) -0.0044(16) 0.0003(16) -0.0109(17) C36 0.026(2) 0.023(2) 0.0145(18) 0.0018(16) -0.0030(15) -0.0161(18) C37 0.046(3) 0.047(3) 0.023(2) 0.001(2) 0.001(2) -0.017(2) C38 0.052(3) 0.028(2) 0.032(2) 0.0077(19) -0.019(2) -0.022(2) C39 0.028(2) 0.028(2) 0.020(2) -0.0001(17) -0.0070(16) -0.0101(19) C310 0.022(2) 0.030(2) 0.032(2) -0.0091(19) 0.0030(17) -0.0109(19) C311 0.044(3) 0.036(3) 0.035(2) -0.005(2) -0.005(2) -0.019(2) C312 0.029(2) 0.033(2) 0.030(2) -0.0062(19) 0.0080(18) -0.016(2) C313 0.036(3) 0.055(3) 0.060(3) -0.034(3) 0.008(2) -0.022(2) C40 0.024(2) 0.0190(19) 0.0089(17) -0.0025(15) 0.0021(14) -0.0145(17) C41 0.0179(19) 0.0163(18) 0.0143(18) -0.0050(15) 0.0011(14) -0.0091(16) C42 0.0152(18) 0.0099(17) 0.0165(18) -0.0006(14) -0.0049(14) -0.0036(15) C43 0.0198(19) 0.021(2) 0.0160(19) -0.0028(16) 0.0034(15) -0.0125(17) C44 0.0162(19) 0.029(2) 0.0183(19) -0.0051(17) 0.0045(15) -0.0115(17) C45 0.0154(19) 0.021(2) 0.0165(19) 0.0003(16) -0.0009(15) -0.0046(16) C46 0.021(2) 0.0190(19) 0.0184(19) -0.0008(16) 0.0017(15) -0.0113(17) C47 0.038(2) 0.036(2) 0.025(2) -0.0111(18) 0.0109(18) -0.028(2) C48 0.035(2) 0.0162(19) 0.023(2) 0.0041(16) 0.0071(17) -0.0114(18) C49 0.023(2) 0.023(2) 0.0171(19) -0.0042(16) 0.0035(15) -0.0091(17) C410 0.030(2) 0.022(2) 0.023(2) -0.0049(17) 0.0001(17) -0.0109(18) C411 0.042(3) 0.065(3) 0.069(3) -0.039(3) -0.010(2) -0.017(3) C412 0.054(3) 0.043(3) 0.040(3) -0.020(2) 0.009(2) -0.018(2) C413 0.086(4) 0.046(3) 0.040(3) -0.011(2) 0.000(3) -0.048(3) C51 0.116(5) 0.084(4) 0.023(2) -0.013(3) 0.005(3) -0.080(4) C52 0.143(6) 0.071(4) 0.035(3) -0.005(3) -0.002(3) -0.085(4) C53 0.130(6) 0.086(5) 0.070(4) -0.028(3) 0.015(4) -0.078(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr O1 2.197(2) . ? Zr O4 2.215(2) . ? Zr O3 2.333(2) . ? Zr O2 2.337(2) . ? Zr Cl2 2.3965(10) . ? Zr Cl1 2.3997(12) . ? Zr S1 2.7649(10) . ? Zr S2 2.7797(11) . ? Zr Al1 3.2266(13) . ? Zr Al2 3.2374(15) . ? S1 C21 1.780(3) . ? S1 C11 1.792(3) . ? S2 C31 1.775(3) . ? S2 C41 1.788(3) . ? Al1 O3 1.775(2) . ? Al1 O1 1.802(2) . ? Al1 Cl4 2.0873(14) . ? Al1 Cl3 2.0945(14) . ? Al2 O2 1.771(2) . ? Al2 O4 1.807(2) . ? Al2 Cl6 2.0860(15) . ? Al2 Cl5 2.0926(14) . ? O1 C10 1.399(4) . ? O2 C20 1.383(3) . ? O3 C30 1.381(4) . ? O4 C40 1.394(3) . ? C10 C11 1.373(4) . ? C10 C15 1.382(4) . ? C11 C12 1.386(4) . ? C12 C13 1.378(4) . ? C12 H12A 0.9500 . ? C13 C14 1.396(4) . ? C13 C16 1.532(4) . ? C14 C15 1.380(4) . ? C14 H14A 0.9500 . ? C15 H15A 0.9500 . ? C16 C17 1.514(5) . ? C16 C18 1.526(5) . ? C16 C19 1.585(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C110 1.518(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C110 C111 1.532(5) . ? C110 C113 1.536(5) . ? C110 C112 1.536(5) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? C112 H11D 0.9800 . ? C112 H11E 0.9800 . ? C112 H11F 0.9800 . ? C113 H11G 0.9800 . ? C113 H11H 0.9800 . ? C113 H11I 0.9800 . ? C20 C21 1.383(4) . ? C20 C25 1.382(4) . ? C21 C22 1.388(4) . ? C22 C23 1.385(4) . ? C22 H22A 0.9500 . ? C23 C24 1.383(4) . ? C23 C26 1.553(4) . ? C24 C25 1.379(4) . ? C24 H24A 0.9500 . ? C25 H25A 0.9500 . ? C26 C28 1.529(4) . ? C26 C27 1.540(4) . ? C26 C29 1.549(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C210 1.550(4) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C210 C212 1.525(4) . ? C210 C213 1.532(5) . ? C210 C211 1.533(5) . ? C211 H21A 0.9800 . ? C211 H21B 0.9800 . ? C211 H21C 0.9800 . ? C212 H21D 0.9800 . ? C212 H21E 0.9800 . ? C212 H21F 0.9800 . ? C213 H21G 0.9800 . ? C213 H21H 0.9800 . ? C213 H21I 0.9800 . ? C30 C35 1.380(4) . ? C30 C31 1.386(4) . ? C31 C32 1.387(4) . ? C32 C33 1.401(4) . ? C32 H32A 0.9500 . ? C33 C34 1.386(4) . ? C33 C36 1.535(4) . ? C34 C35 1.383(4) . ? C34 H34A 0.9500 . ? C35 H35A 0.9500 . ? C36 C37 1.529(5) . ? C36 C38 1.529(5) . ? C36 C39 1.539(5) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C310 1.554(5) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C310 C312 1.525(5) . ? C310 C313 1.529(5) . ? C310 C311 1.529(5) . ? C311 H31A 0.9800 . ? C311 H31B 0.9800 . ? C311 H31C 0.9800 . ? C312 H31D 0.9800 . ? C312 H31E 0.9800 . ? C312 H31F 0.9800 . ? C313 H31G 0.9800 . ? C313 H31H 0.9800 . ? C313 H31I 0.9800 . ? C40 C41 1.375(4) . ? C40 C45 1.378(4) . ? C41 C42 1.395(4) . ? C42 C43 1.383(4) . ? C42 H42A 0.9500 . ? C43 C44 1.398(4) . ? C43 C46 1.523(4) . ? C44 C45 1.383(4) . ? C44 H44A 0.9500 . ? C45 H45A 0.9500 . ? C46 C47 1.539(4) . ? C46 C48 1.542(5) . ? C46 C49 1.556(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C410 1.537(5) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C410 C411 1.512(5) . ? C410 C413 1.533(5) . ? C410 C412 1.540(5) . ? C411 H41A 0.9800 . ? C411 H41B 0.9800 . ? C411 H41C 0.9800 . ? C412 H41D 0.9800 . ? C412 H41E 0.9800 . ? C412 H41F 0.9800 . ? C413 H41G 0.9800 . ? C413 H41H 0.9800 . ? C413 H41I 0.9800 . ? C51 C51 1.488(9) 2_655 ? C51 C52 1.515(6) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 C53 1.495(7) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 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 Zr O4 89.17(8) . . ? O1 Zr O3 64.71(7) . . ? O4 Zr O3 76.05(8) . . ? O1 Zr O2 77.06(8) . . ? O4 Zr O2 64.49(8) . . ? O3 Zr O2 124.66(7) . . ? O1 Zr Cl2 149.20(6) . . ? O4 Zr Cl2 98.41(6) . . ? O3 Zr Cl2 146.09(6) . . ? O2 Zr Cl2 79.44(6) . . ? O1 Zr Cl1 95.55(6) . . ? O4 Zr Cl1 149.57(6) . . ? O3 Zr Cl1 78.90(6) . . ? O2 Zr Cl1 145.81(6) . . ? Cl2 Zr Cl1 92.78(3) . . ? O1 Zr S1 72.45(6) . . ? O4 Zr S1 132.16(6) . . ? O3 Zr S1 128.12(6) . . ? O2 Zr S1 68.41(6) . . ? Cl2 Zr S1 80.56(4) . . ? Cl1 Zr S1 77.50(3) . . ? O1 Zr S2 132.10(6) . . ? O4 Zr S2 72.37(6) . . ? O3 Zr S2 68.01(6) . . ? O2 Zr S2 127.28(6) . . ? Cl2 Zr S2 78.37(4) . . ? Cl1 Zr S2 82.43(3) . . ? S1 Zr S2 150.00(3) . . ? O1 Zr Al1 32.25(5) . . ? O4 Zr Al1 81.18(6) . . ? O3 Zr Al1 32.45(5) . . ? O2 Zr Al1 101.61(6) . . ? Cl2 Zr Al1 178.54(3) . . ? Cl1 Zr Al1 86.91(3) . . ? S1 Zr Al1 100.76(4) . . ? S2 Zr Al1 100.17(4) . . ? O1 Zr Al2 81.20(6) . . ? O4 Zr Al2 32.31(6) . . ? O3 Zr Al2 100.77(6) . . ? O2 Zr Al2 32.20(5) . . ? Cl2 Zr Al2 89.39(3) . . ? Cl1 Zr Al2 176.50(3) . . ? S1 Zr Al2 100.17(3) . . ? S2 Zr Al2 100.71(3) . . ? Al1 Zr Al2 90.98(3) . . ? C21 S1 C11 97.14(14) . . ? C21 S1 Zr 99.96(11) . . ? C11 S1 Zr 98.42(10) . . ? C31 S2 C41 97.25(15) . . ? C31 S2 Zr 100.02(11) . . ? C41 S2 Zr 98.23(11) . . ? O3 Al1 O1 85.44(10) . . ? O3 Al1 Cl4 112.81(9) . . ? O1 Al1 Cl4 114.05(9) . . ? O3 Al1 Cl3 116.25(9) . . ? O1 Al1 Cl3 110.14(9) . . ? Cl4 Al1 Cl3 114.77(6) . . ? O3 Al1 Zr 44.86(7) . . ? O1 Al1 Zr 40.58(7) . . ? Cl4 Al1 Zr 122.57(5) . . ? Cl3 Al1 Zr 122.36(5) . . ? O2 Al2 O4 85.55(10) . . ? O2 Al2 Cl6 110.47(9) . . ? O4 Al2 Cl6 115.50(9) . . ? O2 Al2 Cl5 117.63(9) . . ? O4 Al2 Cl5 110.51(9) . . ? Cl6 Al2 Cl5 114.19(7) . . ? O2 Al2 Zr 44.66(7) . . ? O4 Al2 Zr 40.92(7) . . ? Cl6 Al2 Zr 121.20(5) . . ? Cl5 Al2 Zr 124.49(5) . . ? C10 O1 Al1 122.12(19) . . ? C10 O1 Zr 128.48(18) . . ? Al1 O1 Zr 107.16(10) . . ? C20 O2 Al2 127.85(19) . . ? C20 O2 Zr 126.13(18) . . ? Al2 O2 Zr 103.15(10) . . ? C30 O3 Al1 127.21(19) . . ? C30 O3 Zr 125.92(19) . . ? Al1 O3 Zr 102.69(10) . . ? C40 O4 Al2 122.86(19) . . ? C40 O4 Zr 128.03(18) . . ? Al2 O4 Zr 106.78(10) . . ? C11 C10 C15 120.0(3) . . ? C11 C10 O1 119.6(3) . . ? C15 C10 O1 120.4(3) . . ? C10 C11 C12 120.5(3) . . ? C10 C11 S1 119.4(2) . . ? C12 C11 S1 119.9(2) . . ? C13 C12 C11 120.8(3) . . ? C13 C12 H12A 119.6 . . ? C11 C12 H12A 119.6 . . ? C12 C13 C14 117.8(3) . . ? C12 C13 C16 122.5(3) . . ? C14 C13 C16 119.6(3) . . ? C15 C14 C13 121.8(3) . . ? C15 C14 H14A 119.1 . . ? C13 C14 H14A 119.1 . . ? C10 C15 C14 119.1(3) . . ? C10 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C17 C16 C18 109.9(3) . . ? C17 C16 C13 108.6(3) . . ? C18 C16 C13 112.2(3) . . ? C17 C16 C19 105.9(3) . . ? C18 C16 C19 110.1(3) . . ? C13 C16 C19 109.9(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C110 C19 C16 123.8(3) . . ? C110 C19 H19A 106.4 . . ? C16 C19 H19A 106.4 . . ? C110 C19 H19B 106.4 . . ? C16 C19 H19B 106.4 . . ? H19A C19 H19B 106.5 . . ? C19 C110 C111 105.3(4) . . ? C19 C110 C113 115.0(3) . . ? C111 C110 C113 108.3(4) . . ? C19 C110 C112 113.6(3) . . ? C111 C110 C112 106.8(3) . . ? C113 C110 C112 107.4(4) . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C110 C112 H11D 109.5 . . ? C110 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? C110 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? C110 C113 H11G 109.5 . . ? C110 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C110 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C21 C20 O2 118.5(3) . . ? C21 C20 C25 118.3(3) . . ? O2 C20 C25 123.2(3) . . ? C20 C21 C22 121.3(3) . . ? C20 C21 S1 117.4(2) . . ? C22 C21 S1 121.3(2) . . ? C23 C22 C21 120.6(3) . . ? C23 C22 H22A 119.7 . . ? C21 C22 H22A 119.7 . . ? C24 C23 C22 117.3(3) . . ? C24 C23 C26 120.0(3) . . ? C22 C23 C26 122.6(3) . . ? C25 C24 C23 122.4(3) . . ? C25 C24 H24A 118.8 . . ? C23 C24 H24A 118.8 . . ? C24 C25 C20 120.0(3) . . ? C24 C25 H25A 120.0 . . ? C20 C25 H25A 120.0 . . ? C28 C26 C27 107.8(3) . . ? C28 C26 C29 113.4(3) . . ? C27 C26 C29 111.5(3) . . ? C28 C26 C23 107.8(3) . . ? C27 C26 C23 109.9(3) . . ? C29 C26 C23 106.4(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 C210 124.6(3) . . ? C26 C29 H29A 106.2 . . ? C210 C29 H29A 106.2 . . ? C26 C29 H29B 106.2 . . ? C210 C29 H29B 106.2 . . ? H29A C29 H29B 106.4 . . ? C212 C210 C213 108.7(3) . . ? C212 C210 C211 108.3(3) . . ? C213 C210 C211 108.0(3) . . ? C212 C210 C29 113.6(3) . . ? C213 C210 C29 112.1(3) . . ? C211 C210 C29 106.0(3) . . ? C210 C211 H21A 109.5 . . ? C210 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? C210 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? C210 C212 H21D 109.5 . . ? C210 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? C210 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? C210 C213 H21G 109.5 . . ? C210 C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C210 C213 H21I 109.5 . . ? H21G C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? O3 C30 C35 122.7(3) . . ? O3 C30 C31 118.6(3) . . ? C35 C30 C31 118.7(3) . . ? C32 C31 C30 121.1(3) . . ? C32 C31 S2 121.6(3) . . ? C30 C31 S2 117.2(2) . . ? C31 C32 C33 120.6(3) . . ? C31 C32 H32A 119.7 . . ? C33 C32 H32A 119.7 . . ? C34 C33 C32 117.0(3) . . ? C34 C33 C36 120.8(3) . . ? C32 C33 C36 122.2(3) . . ? C35 C34 C33 122.5(3) . . ? C35 C34 H34A 118.8 . . ? C33 C34 H34A 118.8 . . ? C30 C35 C34 120.0(3) . . ? C30 C35 H35A 120.0 . . ? C34 C35 H35A 120.0 . . ? C37 C36 C38 106.9(3) . . ? C37 C36 C33 108.2(3) . . ? C38 C36 C33 112.1(3) . . ? C37 C36 C39 105.8(3) . . ? C38 C36 C39 112.3(3) . . ? C33 C36 C39 111.2(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 C310 123.9(3) . . ? C36 C39 H39A 106.4 . . ? C310 C39 H39A 106.4 . . ? C36 C39 H39B 106.4 . . ? C310 C39 H39B 106.4 . . ? H39A C39 H39B 106.4 . . ? C312 C310 C313 107.8(3) . . ? C312 C310 C311 109.2(3) . . ? C313 C310 C311 108.1(3) . . ? C312 C310 C39 113.2(3) . . ? C313 C310 C39 104.1(3) . . ? C311 C310 C39 114.0(3) . . ? C310 C311 H31A 109.5 . . ? C310 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? C310 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? C310 C312 H31D 109.5 . . ? C310 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? C310 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? C310 C313 H31G 109.5 . . ? C310 C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? C310 C313 H31I 109.5 . . ? H31G C313 H31I 109.5 . . ? H31H C313 H31I 109.5 . . ? C41 C40 C45 119.8(3) . . ? C41 C40 O4 119.9(3) . . ? C45 C40 O4 120.3(3) . . ? C40 C41 C42 120.2(3) . . ? C40 C41 S2 119.7(2) . . ? C42 C41 S2 119.8(2) . . ? C43 C42 C41 121.6(3) . . ? C43 C42 H42A 119.2 . . ? C41 C42 H42A 119.2 . . ? C42 C43 C44 116.5(3) . . ? C42 C43 C46 123.1(3) . . ? C44 C43 C46 120.5(3) . . ? C45 C44 C43 122.7(3) . . ? C45 C44 H44A 118.7 . . ? C43 C44 H44A 118.7 . . ? C40 C45 C44 119.2(3) . . ? C40 C45 H45A 120.4 . . ? C44 C45 H45A 120.4 . . ? C43 C46 C47 108.1(3) . . ? C43 C46 C48 111.9(3) . . ? C47 C46 C48 106.4(3) . . ? C43 C46 C49 111.9(3) . . ? C47 C46 C49 106.3(3) . . ? C48 C46 C49 111.8(3) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C410 C49 C46 124.6(3) . . ? C410 C49 H49A 106.2 . . ? C46 C49 H49A 106.2 . . ? C410 C49 H49B 106.2 . . ? C46 C49 H49B 106.2 . . ? H49A C49 H49B 106.4 . . ? C411 C410 C413 109.0(3) . . ? C411 C410 C49 114.5(3) . . ? C413 C410 C49 112.4(3) . . ? C411 C410 C412 108.2(3) . . ? C413 C410 C412 106.5(3) . . ? C49 C410 C412 105.8(3) . . ? C410 C411 H41A 109.5 . . ? C410 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? C410 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? C410 C412 H41D 109.5 . . ? C410 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? C410 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? C410 C413 H41G 109.5 . . ? C410 C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? C410 C413 H41I 109.5 . . ? H41G C413 H41I 109.5 . . ? H41H C413 H41I 109.5 . . ? C51 C51 C52 114.5(5) 2_655 . ? C51 C51 H51A 108.6 2_655 . ? C52 C51 H51A 108.6 . . ? C51 C51 H51B 108.6 2_655 . ? C52 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? C53 C52 C51 113.9(4) . . ? C53 C52 H52A 108.8 . . ? C51 C52 H52A 108.8 . . ? C53 C52 H52B 108.8 . . ? C51 C52 H52B 108.8 . . ? H52A C52 H52B 107.7 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 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 Zr S1 C21 -105.15(12) . . . . ? O4 Zr S1 C21 -33.02(13) . . . . ? O3 Zr S1 C21 -140.30(12) . . . . ? O2 Zr S1 C21 -22.47(12) . . . . ? Cl2 Zr S1 C21 59.82(11) . . . . ? Cl1 Zr S1 C21 154.83(11) . . . . ? S2 Zr S1 C21 105.66(12) . . . . ? Al1 Zr S1 C21 -120.81(11) . . . . ? Al2 Zr S1 C21 -27.84(11) . . . . ? O1 Zr S1 C11 -6.31(12) . . . . ? O4 Zr S1 C11 65.82(13) . . . . ? O3 Zr S1 C11 -41.46(13) . . . . ? O2 Zr S1 C11 76.37(12) . . . . ? Cl2 Zr S1 C11 158.66(11) . . . . ? Cl1 Zr S1 C11 -106.34(11) . . . . ? S2 Zr S1 C11 -155.50(11) . . . . ? Al1 Zr S1 C11 -21.97(11) . . . . ? Al2 Zr S1 C11 71.00(11) . . . . ? O1 Zr S2 C31 -32.31(13) . . . . ? O4 Zr S2 C31 -104.38(12) . . . . ? O3 Zr S2 C31 -22.68(12) . . . . ? O2 Zr S2 C31 -140.29(12) . . . . ? Cl2 Zr S2 C31 152.79(11) . . . . ? Cl1 Zr S2 C31 58.35(11) . . . . ? S1 Zr S2 C31 106.52(12) . . . . ? Al1 Zr S2 C31 -27.12(11) . . . . ? Al2 Zr S2 C31 -120.08(11) . . . . ? O1 Zr S2 C41 66.61(13) . . . . ? O4 Zr S2 C41 -5.46(12) . . . . ? O3 Zr S2 C41 76.24(12) . . . . ? O2 Zr S2 C41 -41.37(13) . . . . ? Cl2 Zr S2 C41 -108.29(11) . . . . ? Cl1 Zr S2 C41 157.27(11) . . . . ? S1 Zr S2 C41 -154.56(11) . . . . ? Al1 Zr S2 C41 71.80(11) . . . . ? Al2 Zr S2 C41 -21.16(11) . . . . ? O1 Zr Al1 O3 -179.55(15) . . . . ? O4 Zr Al1 O3 77.84(11) . . . . ? O2 Zr Al1 O3 139.37(11) . . . . ? Cl2 Zr Al1 O3 3.9(12) . . . . ? Cl1 Zr Al1 O3 -74.06(10) . . . . ? S1 Zr Al1 O3 -150.71(10) . . . . ? S2 Zr Al1 O3 7.68(10) . . . . ? Al2 Zr Al1 O3 108.74(10) . . . . ? O4 Zr Al1 O1 -102.61(12) . . . . ? O3 Zr Al1 O1 179.55(15) . . . . ? O2 Zr Al1 O1 -41.09(12) . . . . ? Cl2 Zr Al1 O1 -177(36) . . . . ? Cl1 Zr Al1 O1 105.49(11) . . . . ? S1 Zr Al1 O1 28.83(11) . . . . ? S2 Zr Al1 O1 -172.78(11) . . . . ? Al2 Zr Al1 O1 -71.71(11) . . . . ? O1 Zr Al1 Cl4 89.87(12) . . . . ? O4 Zr Al1 Cl4 -12.74(7) . . . . ? O3 Zr Al1 Cl4 -90.58(11) . . . . ? O2 Zr Al1 Cl4 48.78(8) . . . . ? Cl2 Zr Al1 Cl4 -86.7(12) . . . . ? Cl1 Zr Al1 Cl4 -164.64(6) . . . . ? S1 Zr Al1 Cl4 118.70(5) . . . . ? S2 Zr Al1 Cl4 -82.91(6) . . . . ? Al2 Zr Al1 Cl4 18.16(6) . . . . ? O1 Zr Al1 Cl3 -83.49(12) . . . . ? O4 Zr Al1 Cl3 173.90(7) . . . . ? O3 Zr Al1 Cl3 96.05(11) . . . . ? O2 Zr Al1 Cl3 -124.58(7) . . . . ? Cl2 Zr Al1 Cl3 100.0(12) . . . . ? Cl1 Zr Al1 Cl3 21.99(5) . . . . ? S1 Zr Al1 Cl3 -54.66(6) . . . . ? S2 Zr Al1 Cl3 103.73(5) . . . . ? Al2 Zr Al1 Cl3 -155.21(5) . . . . ? O1 Zr Al2 O2 79.67(11) . . . . ? O4 Zr Al2 O2 -177.79(16) . . . . ? O3 Zr Al2 O2 141.66(12) . . . . ? Cl2 Zr Al2 O2 -70.90(11) . . . . ? Cl1 Zr Al2 O2 57.5(5) . . . . ? S1 Zr Al2 O2 9.40(10) . . . . ? S2 Zr Al2 O2 -148.94(10) . . . . ? Al1 Zr Al2 O2 110.51(11) . . . . ? O1 Zr Al2 O4 -102.54(12) . . . . ? O3 Zr Al2 O4 -40.55(12) . . . . ? O2 Zr Al2 O4 177.79(16) . . . . ? Cl2 Zr Al2 O4 106.89(11) . . . . ? Cl1 Zr Al2 O4 -124.7(5) . . . . ? S1 Zr Al2 O4 -172.81(11) . . . . ? S2 Zr Al2 O4 28.85(11) . . . . ? Al1 Zr Al2 O4 -71.70(11) . . . . ? O1 Zr Al2 Cl6 -8.55(7) . . . . ? O4 Zr Al2 Cl6 94.00(12) . . . . ? O3 Zr Al2 Cl6 53.45(7) . . . . ? O2 Zr Al2 Cl6 -88.21(11) . . . . ? Cl2 Zr Al2 Cl6 -159.11(5) . . . . ? Cl1 Zr Al2 Cl6 -30.7(5) . . . . ? S1 Zr Al2 Cl6 -78.81(6) . . . . ? S2 Zr Al2 Cl6 122.85(6) . . . . ? Al1 Zr Al2 Cl6 22.30(5) . . . . ? O1 Zr Al2 Cl5 175.71(8) . . . . ? O4 Zr Al2 Cl5 -81.74(12) . . . . ? O3 Zr Al2 Cl5 -122.29(7) . . . . ? O2 Zr Al2 Cl5 96.05(12) . . . . ? Cl2 Zr Al2 Cl5 25.15(6) . . . . ? Cl1 Zr Al2 Cl5 153.5(4) . . . . ? S1 Zr Al2 Cl5 105.45(6) . . . . ? S2 Zr Al2 Cl5 -52.89(6) . . . . ? Al1 Zr Al2 Cl5 -153.44(6) . . . . ? O3 Al1 O1 C10 -164.0(2) . . . . ? Cl4 Al1 O1 C10 83.0(2) . . . . ? Cl3 Al1 O1 C10 -47.7(2) . . . . ? Zr Al1 O1 C10 -164.3(3) . . . . ? O3 Al1 O1 Zr 0.32(11) . . . . ? Cl4 Al1 O1 Zr -112.65(9) . . . . ? Cl3 Al1 O1 Zr 116.64(9) . . . . ? O4 Zr O1 C10 -122.3(2) . . . . ? O3 Zr O1 C10 162.7(2) . . . . ? O2 Zr O1 C10 -58.3(2) . . . . ? Cl2 Zr O1 C10 -17.2(3) . . . . ? Cl1 Zr O1 C10 87.8(2) . . . . ? S1 Zr O1 C10 12.8(2) . . . . ? S2 Zr O1 C10 172.62(19) . . . . ? Al1 Zr O1 C10 163.0(3) . . . . ? Al2 Zr O1 C10 -90.9(2) . . . . ? O4 Zr O1 Al1 74.68(11) . . . . ? O3 Zr O1 Al1 -0.27(9) . . . . ? O2 Zr O1 Al1 138.66(11) . . . . ? Cl2 Zr O1 Al1 179.83(6) . . . . ? Cl1 Zr O1 Al1 -75.20(10) . . . . ? S1 Zr O1 Al1 -150.20(11) . . . . ? S2 Zr O1 Al1 9.60(14) . . . . ? Al2 Zr O1 Al1 106.12(10) . . . . ? O4 Al2 O2 C20 160.0(2) . . . . ? Cl6 Al2 O2 C20 -84.4(2) . . . . ? Cl5 Al2 O2 C20 49.2(3) . . . . ? Zr Al2 O2 C20 161.5(3) . . . . ? O4 Al2 O2 Zr -1.45(10) . . . . ? Cl6 Al2 O2 Zr 114.14(8) . . . . ? Cl5 Al2 O2 Zr -112.30(8) . . . . ? O1 Zr O2 C20 104.0(2) . . . . ? O4 Zr O2 C20 -160.6(2) . . . . ? O3 Zr O2 C20 150.3(2) . . . . ? Cl2 Zr O2 C20 -55.9(2) . . . . ? Cl1 Zr O2 C20 23.3(3) . . . . ? S1 Zr O2 C20 28.0(2) . . . . ? S2 Zr O2 C20 -122.3(2) . . . . ? Al1 Zr O2 C20 125.1(2) . . . . ? Al2 Zr O2 C20 -161.9(3) . . . . ? O1 Zr O2 Al2 -94.03(10) . . . . ? O4 Zr O2 Al2 1.31(9) . . . . ? O3 Zr O2 Al2 -47.80(13) . . . . ? Cl2 Zr O2 Al2 106.02(10) . . . . ? Cl1 Zr O2 Al2 -174.74(5) . . . . ? S1 Zr O2 Al2 -170.04(11) . . . . ? S2 Zr O2 Al2 39.58(12) . . . . ? Al1 Zr O2 Al2 -72.94(10) . . . . ? O1 Al1 O3 C30 157.5(2) . . . . ? Cl4 Al1 O3 C30 -88.3(2) . . . . ? Cl3 Al1 O3 C30 47.3(3) . . . . ? Zr Al1 O3 C30 157.8(3) . . . . ? O1 Al1 O3 Zr -0.30(10) . . . . ? Cl4 Al1 O3 Zr 113.91(8) . . . . ? Cl3 Al1 O3 Zr -110.53(8) . . . . ? O1 Zr O3 C30 -157.9(2) . . . . ? O4 Zr O3 C30 106.3(2) . . . . ? O2 Zr O3 C30 150.9(2) . . . . ? Cl2 Zr O3 C30 22.0(3) . . . . ? Cl1 Zr O3 C30 -56.3(2) . . . . ? S1 Zr O3 C30 -120.6(2) . . . . ? S2 Zr O3 C30 29.9(2) . . . . ? Al1 Zr O3 C30 -158.2(3) . . . . ? Al2 Zr O3 C30 127.3(2) . . . . ? O1 Zr O3 Al1 0.27(9) . . . . ? O4 Zr O3 Al1 -95.52(11) . . . . ? O2 Zr O3 Al1 -50.85(13) . . . . ? Cl2 Zr O3 Al1 -179.82(5) . . . . ? Cl1 Zr O3 Al1 101.91(9) . . . . ? S1 Zr O3 Al1 37.65(12) . . . . ? S2 Zr O3 Al1 -171.85(11) . . . . ? Al2 Zr O3 Al1 -74.54(9) . . . . ? O2 Al2 O4 C40 -162.3(2) . . . . ? Cl6 Al2 O4 C40 87.1(2) . . . . ? Cl5 Al2 O4 C40 -44.5(2) . . . . ? Zr Al2 O4 C40 -163.9(3) . . . . ? O2 Al2 O4 Zr 1.56(11) . . . . ? Cl6 Al2 O4 Zr -109.03(9) . . . . ? Cl5 Al2 O4 Zr 119.44(8) . . . . ? O1 Zr O4 C40 -122.5(2) . . . . ? O3 Zr O4 C40 -58.4(2) . . . . ? O2 Zr O4 C40 161.5(2) . . . . ? Cl2 Zr O4 C40 87.5(2) . . . . ? Cl1 Zr O4 C40 -22.9(3) . . . . ? S1 Zr O4 C40 172.4(2) . . . . ? S2 Zr O4 C40 12.6(2) . . . . ? Al1 Zr O4 C40 -91.1(2) . . . . ? Al2 Zr O4 C40 162.8(3) . . . . ? O1 Zr O4 Al2 74.74(11) . . . . ? O3 Zr O4 Al2 138.85(12) . . . . ? O2 Zr O4 Al2 -1.30(9) . . . . ? Cl2 Zr O4 Al2 -75.29(10) . . . . ? Cl1 Zr O4 Al2 174.31(6) . . . . ? S1 Zr O4 Al2 9.57(14) . . . . ? S2 Zr O4 Al2 -150.17(11) . . . . ? Al1 Zr O4 Al2 106.13(10) . . . . ? Al1 O1 C10 C11 144.6(2) . . . . ? Zr O1 C10 C11 -16.2(4) . . . . ? Al1 O1 C10 C15 -33.9(4) . . . . ? Zr O1 C10 C15 165.3(2) . . . . ? C15 C10 C11 C12 -0.2(5) . . . . ? O1 C10 C11 C12 -178.8(3) . . . . ? C15 C10 C11 S1 -174.8(2) . . . . ? O1 C10 C11 S1 6.6(4) . . . . ? C21 S1 C11 C10 103.4(3) . . . . ? Zr S1 C11 C10 2.2(3) . . . . ? C21 S1 C11 C12 -71.2(3) . . . . ? Zr S1 C11 C12 -172.5(2) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? S1 C11 C12 C13 174.4(2) . . . . ? C11 C12 C13 C14 1.2(5) . . . . ? C11 C12 C13 C16 -176.3(3) . . . . ? C12 C13 C14 C15 -1.9(5) . . . . ? C16 C13 C14 C15 175.7(3) . . . . ? C11 C10 C15 C14 -0.5(5) . . . . ? O1 C10 C15 C14 178.1(3) . . . . ? C13 C14 C15 C10 1.5(5) . . . . ? C12 C13 C16 C17 -123.5(4) . . . . ? C14 C13 C16 C17 59.0(4) . . . . ? C12 C13 C16 C18 -1.8(5) . . . . ? C14 C13 C16 C18 -179.2(3) . . . . ? C12 C13 C16 C19 121.0(3) . . . . ? C14 C13 C16 C19 -56.4(4) . . . . ? C17 C16 C19 C110 175.9(3) . . . . ? C18 C16 C19 C110 57.2(4) . . . . ? C13 C16 C19 C110 -66.9(4) . . . . ? C16 C19 C110 C111 162.6(3) . . . . ? C16 C19 C110 C113 43.4(5) . . . . ? C16 C19 C110 C112 -80.9(4) . . . . ? Al2 O2 C20 C21 179.7(2) . . . . ? Zr O2 C20 C21 -22.8(4) . . . . ? Al2 O2 C20 C25 -0.1(5) . . . . ? Zr O2 C20 C25 157.4(3) . . . . ? O2 C20 C21 C22 176.9(3) . . . . ? C25 C20 C21 C22 -3.4(5) . . . . ? O2 C20 C21 S1 -6.6(4) . . . . ? C25 C20 C21 S1 173.2(2) . . . . ? C11 S1 C21 C20 -76.0(3) . . . . ? Zr S1 C21 C20 23.8(3) . . . . ? C11 S1 C21 C22 100.5(3) . . . . ? Zr S1 C21 C22 -159.6(2) . . . . ? C20 C21 C22 C23 1.2(5) . . . . ? S1 C21 C22 C23 -175.2(3) . . . . ? C21 C22 C23 C24 2.0(5) . . . . ? C21 C22 C23 C26 -177.4(3) . . . . ? C22 C23 C24 C25 -3.0(5) . . . . ? C26 C23 C24 C25 176.3(3) . . . . ? C23 C24 C25 C20 0.9(5) . . . . ? C21 C20 C25 C24 2.3(5) . . . . ? O2 C20 C25 C24 -177.9(3) . . . . ? C24 C23 C26 C28 -51.2(4) . . . . ? C22 C23 C26 C28 128.1(3) . . . . ? C24 C23 C26 C27 -168.4(3) . . . . ? C22 C23 C26 C27 10.9(4) . . . . ? C24 C23 C26 C29 70.8(4) . . . . ? C22 C23 C26 C29 -109.9(3) . . . . ? C28 C26 C29 C210 -49.3(4) . . . . ? C27 C26 C29 C210 72.6(4) . . . . ? C23 C26 C29 C210 -167.6(3) . . . . ? C26 C29 C210 C212 -54.3(4) . . . . ? C26 C29 C210 C213 69.4(4) . . . . ? C26 C29 C210 C211 -173.0(3) . . . . ? Al1 O3 C30 C35 1.1(4) . . . . ? Zr O3 C30 C35 154.0(2) . . . . ? Al1 O3 C30 C31 -179.5(2) . . . . ? Zr O3 C30 C31 -26.6(4) . . . . ? O3 C30 C31 C32 179.3(3) . . . . ? C35 C30 C31 C32 -1.3(5) . . . . ? O3 C30 C31 S2 -3.5(4) . . . . ? C35 C30 C31 S2 175.9(2) . . . . ? C41 S2 C31 C32 99.8(3) . . . . ? Zr S2 C31 C32 -160.5(2) . . . . ? C41 S2 C31 C30 -77.4(3) . . . . ? Zr S2 C31 C30 22.4(3) . . . . ? C30 C31 C32 C33 -0.1(5) . . . . ? S2 C31 C32 C33 -177.2(2) . . . . ? C31 C32 C33 C34 1.6(5) . . . . ? C31 C32 C33 C36 -177.7(3) . . . . ? C32 C33 C34 C35 -1.8(5) . . . . ? C36 C33 C34 C35 177.5(3) . . . . ? O3 C30 C35 C34 -179.5(3) . . . . ? C31 C30 C35 C34 1.1(5) . . . . ? C33 C34 C35 C30 0.4(5) . . . . ? C34 C33 C36 C37 56.7(4) . . . . ? C32 C33 C36 C37 -124.0(3) . . . . ? C34 C33 C36 C38 174.2(3) . . . . ? C32 C33 C36 C38 -6.5(5) . . . . ? C34 C33 C36 C39 -59.1(4) . . . . ? C32 C33 C36 C39 120.2(3) . . . . ? C37 C36 C39 C310 178.0(3) . . . . ? C38 C36 C39 C310 61.7(4) . . . . ? C33 C36 C39 C310 -64.8(4) . . . . ? C36 C39 C310 C312 57.2(5) . . . . ? C36 C39 C310 C313 174.0(3) . . . . ? C36 C39 C310 C311 -68.4(4) . . . . ? Al2 O4 C40 C41 143.1(2) . . . . ? Zr O4 C40 C41 -17.2(4) . . . . ? Al2 O4 C40 C45 -35.2(4) . . . . ? Zr O4 C40 C45 164.5(2) . . . . ? C45 C40 C41 C42 1.8(5) . . . . ? O4 C40 C41 C42 -176.6(3) . . . . ? C45 C40 C41 S2 -172.9(2) . . . . ? O4 C40 C41 S2 8.7(4) . . . . ? C31 S2 C41 C40 101.7(3) . . . . ? Zr S2 C41 C40 0.4(3) . . . . ? C31 S2 C41 C42 -73.0(3) . . . . ? Zr S2 C41 C42 -174.3(2) . . . . ? C40 C41 C42 C43 -0.8(5) . . . . ? S2 C41 C42 C43 173.9(2) . . . . ? C41 C42 C43 C44 -0.3(5) . . . . ? C41 C42 C43 C46 178.4(3) . . . . ? C42 C43 C44 C45 0.4(5) . . . . ? C46 C43 C44 C45 -178.4(3) . . . . ? C41 C40 C45 C44 -1.7(5) . . . . ? O4 C40 C45 C44 176.7(3) . . . . ? C43 C44 C45 C40 0.6(5) . . . . ? C42 C43 C46 C47 -122.8(3) . . . . ? C44 C43 C46 C47 55.8(4) . . . . ? C42 C43 C46 C48 -6.0(5) . . . . ? C44 C43 C46 C48 172.7(3) . . . . ? C42 C43 C46 C49 120.4(3) . . . . ? C44 C43 C46 C49 -60.9(4) . . . . ? C43 C46 C49 C410 -57.6(4) . . . . ? C47 C46 C49 C410 -175.4(3) . . . . ? C48 C46 C49 C410 68.8(4) . . . . ? C46 C49 C410 C411 -54.3(5) . . . . ? C46 C49 C410 C413 70.8(4) . . . . ? C46 C49 C410 C412 -173.4(3) . . . . ? C51 C51 C52 C53 -175.8(5) 2_655 . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.789 _refine_diff_density_min -0.434 _refine_diff_density_rms 0.080 # Attachment '3NEW.CIF' data_CCDC721085 _database_code_depnum_ccdc_archive 'CCDC 721085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C104 H148 O8 S2 Zr2' _chemical_formula_sum 'C104 H148 O8 S2 Zr2' _chemical_formula_weight 1772.78 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' S S 0.1246 0.1234 '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_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 21/c' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.830(5) _cell_length_b 19.186(5) _cell_length_c 28.187(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.15(2) _cell_angle_gamma 90.00 _cell_volume 9933(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9501 _cell_measurement_theta_min 3 _cell_measurement_theta_max 28 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.332 _exptl_crystal_size_mid 0.231 _exptl_crystal_size_min 0.121 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 0.304 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.797 _exptl_absorpt_correction_T_max 0.810 _exptl_absorpt_process_details ; CrysAlis RED V1.171.13, Oxford Diffraction Ltd., Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kuma KM-4 CCD kappa-axis diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 112927 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.0535 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.82 _diffrn_reflns_theta_max 27.00 _reflns_number_total 21660 _reflns_number_gt 17416 _reflns_threshold_expression >2sigma(I) _computing_cell_refinement 'CrysAlis RED V1.171.30,Oxford Diffraction Ltd.,2006' _computing_data_reduction ' CrysAlis RED V1.171.30,Oxford Diffraction Ltd.,2006' _computing_structure_solution 'SHELXTL V6.14, Bruker AXS 2003' _computing_structure_refinement 'SHELXTL V6.14, Bruker AXS 2003' _computing_molecular_graphics 'DIAMOND (Brandenburg & Putz, 2005)' _computing_publication_material 'SHELXTL V6.14, Bruker AXS 2003' _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^)+(0.0352P)^2^+6.1707P] 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 21660 _refine_ls_number_parameters 1072 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0924 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1140 _refine_ls_wR_factor_gt 0.1063 _refine_ls_goodness_of_fit_ref 1.245 _refine_ls_restrained_S_all 1.248 _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 0.657736(14) 0.456200(14) 0.238154(11) 0.01178(7) Uani 1 1 d . . . Zr2 Zr 0.837353(14) 0.507530(14) 0.257141(11) 0.01291(7) Uani 1 1 d . . . S1 S 0.65023(4) 0.60373(4) 0.24630(3) 0.01322(15) Uani 1 1 d . . . S2 S 0.84501(4) 0.36023(4) 0.24740(3) 0.01335(15) Uani 1 1 d . . . O1 O 0.57396(10) 0.45425(10) 0.17356(7) 0.0164(4) Uani 1 1 d . . . O2 O 0.60685(10) 0.47019(10) 0.28464(7) 0.0158(4) Uani 1 1 d . . . O3 O 0.91788(10) 0.50770(10) 0.32317(8) 0.0191(5) Uani 1 1 d . . . O4 O 0.89236(10) 0.49280(10) 0.21355(8) 0.0170(4) Uani 1 1 d . . . O5 O 0.76052(10) 0.49539(10) 0.29597(7) 0.0138(4) Uani 1 1 d . . . O6 O 0.80454(10) 0.60429(10) 0.24149(7) 0.0154(4) Uani 1 1 d . . . O7 O 0.73434(10) 0.46938(10) 0.19882(7) 0.0140(4) Uani 1 1 d . . . O8 O 0.69230(10) 0.36026(10) 0.25343(8) 0.0164(4) Uani 1 1 d . . . C10 C 0.51851(15) 0.44041(17) 0.12750(11) 0.0191(7) Uani 1 1 d . . . C11 C 0.48327(17) 0.49662(17) 0.09606(12) 0.0247(7) Uani 1 1 d . . . C12 C 0.50450(18) 0.57100(18) 0.11293(13) 0.0282(8) Uani 1 1 d . . . H12 H 0.5191 0.5723 0.1510 0.034 Uiso 1 1 calc R . . C13 C 0.5708(2) 0.59415(19) 0.10155(14) 0.0372(9) Uani 1 1 d . . . H13A H 0.5831 0.6424 0.1129 0.056 Uiso 1 1 calc R . . H13B H 0.5595 0.5910 0.0646 0.056 Uiso 1 1 calc R . . H13C H 0.6122 0.5638 0.1199 0.056 Uiso 1 1 calc R . . C14 C 0.4420(2) 0.6232(2) 0.09019(16) 0.0489(11) Uani 1 1 d . . . H14A H 0.4566 0.6685 0.1069 0.073 Uiso 1 1 calc R . . H14B H 0.3990 0.6063 0.0957 0.073 Uiso 1 1 calc R . . H14C H 0.4306 0.6280 0.0534 0.073 Uiso 1 1 calc R . . C15 C 0.42900(19) 0.4803(2) 0.04851(13) 0.0371(9) Uani 1 1 d . . . H15 H 0.4039 0.5168 0.0260 0.044 Uiso 1 1 calc R . . C16 C 0.41150(19) 0.4116(2) 0.03386(14) 0.0396(10) Uani 1 1 d . . . H16 H 0.3754 0.4016 0.0011 0.048 Uiso 1 1 calc R . . C17 C 0.44573(18) 0.3579(2) 0.06611(14) 0.0359(9) Uani 1 1 d . . . H17 H 0.4321 0.3112 0.0557 0.043 Uiso 1 1 calc R . . C18 C 0.50024(16) 0.37074(17) 0.11391(13) 0.0253(7) Uani 1 1 d . . . C19 C 0.53585(18) 0.31331(17) 0.15183(14) 0.0315(8) Uani 1 1 d . . . H19 H 0.5889 0.3244 0.1680 0.038 Uiso 1 1 calc R . . C110 C 0.5290(2) 0.2411(2) 0.12732(19) 0.0579(13) Uani 1 1 d . . . H11A H 0.5589 0.2077 0.1529 0.087 Uiso 1 1 calc R . . H11B H 0.5458 0.2432 0.0988 0.087 Uiso 1 1 calc R . . H11C H 0.4780 0.2261 0.1146 0.087 Uiso 1 1 calc R . . C111 C 0.50586(19) 0.3128(2) 0.19441(15) 0.0402(10) Uani 1 1 d . . . H11D H 0.5328 0.2788 0.2206 0.060 Uiso 1 1 calc R . . H11E H 0.4542 0.3001 0.1801 0.060 Uiso 1 1 calc R . . H11F H 0.5113 0.3593 0.2098 0.060 Uiso 1 1 calc R . . C20 C 0.57679(15) 0.49162(15) 0.31850(11) 0.0161(6) Uani 1 1 d . . . C21 C 0.60953(16) 0.47057(16) 0.36987(12) 0.0204(7) Uani 1 1 d . . . C22 C 0.67417(16) 0.42112(18) 0.38566(12) 0.0251(7) Uani 1 1 d . . . H22 H 0.7033 0.4326 0.3644 0.030 Uiso 1 1 calc R . . C23 C 0.72466(19) 0.4278(2) 0.44186(13) 0.0378(9) Uani 1 1 d . . . H23A H 0.7670 0.3973 0.4488 0.057 Uiso 1 1 calc R . . H23B H 0.6984 0.4142 0.4637 0.057 Uiso 1 1 calc R . . H23C H 0.7410 0.4762 0.4492 0.057 Uiso 1 1 calc R . . C24 C 0.64749(18) 0.34562(18) 0.37344(13) 0.0308(8) Uani 1 1 d . . . H24A H 0.6895 0.3144 0.3817 0.046 Uiso 1 1 calc R . . H24B H 0.6170 0.3416 0.3370 0.046 Uiso 1 1 calc R . . H24C H 0.6190 0.3327 0.3939 0.046 Uiso 1 1 calc R . . C25 C 0.57850(18) 0.49322(18) 0.40393(12) 0.0275(8) Uani 1 1 d . . . H25 H 0.6001 0.4802 0.4390 0.033 Uiso 1 1 calc R . . C26 C 0.51669(19) 0.53447(18) 0.38752(13) 0.0299(8) Uani 1 1 d . . . H26 H 0.4962 0.5495 0.4113 0.036 Uiso 1 1 calc R . . C27 C 0.48461(18) 0.55389(16) 0.33664(13) 0.0262(8) Uani 1 1 d . . . H27 H 0.4419 0.5818 0.3258 0.031 Uiso 1 1 calc R . . C28 C 0.51392(16) 0.53329(15) 0.30094(12) 0.0184(6) Uani 1 1 d . . . C29 C 0.47814(15) 0.55358(15) 0.24467(12) 0.0186(7) Uani 1 1 d . . . H29 H 0.5136 0.5430 0.2281 0.022 Uiso 1 1 calc R . . C210 C 0.40959(18) 0.51059(18) 0.21716(13) 0.0321(8) Uani 1 1 d . . . H21A H 0.3913 0.5207 0.1804 0.048 Uiso 1 1 calc R . . H21B H 0.3723 0.5226 0.2307 0.048 Uiso 1 1 calc R . . H21C H 0.4212 0.4609 0.2227 0.048 Uiso 1 1 calc R . . C211 C 0.46133(19) 0.63153(17) 0.23806(14) 0.0334(9) Uani 1 1 d . . . H21D H 0.4422 0.6433 0.2015 0.050 Uiso 1 1 calc R . . H21E H 0.5060 0.6581 0.2558 0.050 Uiso 1 1 calc R . . H21F H 0.4250 0.6432 0.2526 0.050 Uiso 1 1 calc R . . C30 C 0.97095(16) 0.51380(17) 0.37100(12) 0.0228(7) Uani 1 1 d . . . C31 C 0.99639(18) 0.45410(18) 0.40114(13) 0.0301(8) Uani 1 1 d . . . C32 C 0.96486(19) 0.38266(17) 0.38148(13) 0.0333(9) Uani 1 1 d . . . H32 H 0.9511 0.3827 0.3435 0.040 Uiso 1 1 calc R . . C33 C 0.8956(2) 0.36991(19) 0.39154(14) 0.0429(10) Uani 1 1 d . . . H33A H 0.8775 0.3228 0.3803 0.064 Uiso 1 1 calc R . . H33B H 0.8585 0.4041 0.3725 0.064 Uiso 1 1 calc R . . H33C H 0.9061 0.3746 0.4283 0.064 Uiso 1 1 calc R . . C34 C 1.0187(2) 0.3231(2) 0.40323(16) 0.0600(14) Uani 1 1 d . . . H34A H 0.9983 0.2800 0.3848 0.090 Uiso 1 1 calc R . . H34B H 1.0278 0.3171 0.4397 0.090 Uiso 1 1 calc R . . H34C H 1.0646 0.3340 0.3993 0.090 Uiso 1 1 calc R . . C35 C 1.0490(2) 0.4628(2) 0.44972(14) 0.0466(11) Uani 1 1 d . . . H35 H 1.0671 0.4232 0.4709 0.056 Uiso 1 1 calc R . . C36 C 1.0757(2) 0.5282(2) 0.46790(15) 0.0523(12) Uani 1 1 d . . . H36 H 1.1119 0.5330 0.5014 0.063 Uiso 1 1 calc R . . C37 C 1.0503(2) 0.5866(2) 0.43789(15) 0.0440(10) Uani 1 1 d . . . H37 H 1.0692 0.6312 0.4508 0.053 Uiso 1 1 calc R . . C38 C 0.99692(17) 0.58070(18) 0.38841(14) 0.0299(8) Uani 1 1 d . . . C39 C 0.96725(19) 0.64338(17) 0.35402(15) 0.0367(9) Uani 1 1 d . . . H39 H 0.9135 0.6364 0.3365 0.044 Uiso 1 1 calc R . . C310 C 0.9990(2) 0.6469(2) 0.31194(17) 0.0537(12) Uani 1 1 d . . . H31A H 0.9766 0.6856 0.2887 0.081 Uiso 1 1 calc R . . H31B H 0.9889 0.6031 0.2926 0.081 Uiso 1 1 calc R . . H31C H 1.0518 0.6542 0.3277 0.081 Uiso 1 1 calc R . . C311 C 0.9785(2) 0.7126(2) 0.38313(19) 0.0665(15) Uani 1 1 d . . . H31D H 0.9536 0.7500 0.3593 0.100 Uiso 1 1 calc R . . H31E H 1.0307 0.7230 0.3988 0.100 Uiso 1 1 calc R . . H31F H 0.9585 0.7091 0.4100 0.100 Uiso 1 1 calc R . . C40 C 0.92720(16) 0.47022(16) 0.18284(12) 0.0197(7) Uani 1 1 d . . . C41 C 0.89886(17) 0.49019(17) 0.13097(12) 0.0244(7) Uani 1 1 d . . . C42 C 0.83328(18) 0.53778(19) 0.11098(13) 0.0309(8) Uani 1 1 d . . . H42 H 0.8019 0.5270 0.1307 0.037 Uiso 1 1 calc R . . C43 C 0.7867(2) 0.5265(3) 0.05412(14) 0.0563(12) Uani 1 1 d . . . H43A H 0.7421 0.5543 0.0447 0.084 Uiso 1 1 calc R . . H43B H 0.7741 0.4771 0.0480 0.084 Uiso 1 1 calc R . . H43C H 0.8142 0.5411 0.0333 0.084 Uiso 1 1 calc R . . C44 C 0.8572(2) 0.6132(2) 0.12190(16) 0.0488(11) Uani 1 1 d . . . H44A H 0.8143 0.6433 0.1126 0.073 Uiso 1 1 calc R . . H44B H 0.8861 0.6263 0.1017 0.073 Uiso 1 1 calc R . . H44C H 0.8869 0.6187 0.1584 0.073 Uiso 1 1 calc R . . C45 C 0.93462(19) 0.46643(19) 0.10005(14) 0.0336(9) Uani 1 1 d . . . H45 H 0.9166 0.4789 0.0648 0.040 Uiso 1 1 calc R . . C46 C 0.9964(2) 0.42474(19) 0.11994(16) 0.0384(10) Uani 1 1 d . . . H46 H 1.0198 0.4086 0.0982 0.046 Uiso 1 1 calc R . . C47 C 1.02372(18) 0.40691(18) 0.17083(15) 0.0333(9) Uani 1 1 d . . . H47 H 1.0664 0.3791 0.1839 0.040 Uiso 1 1 calc R . . C48 C 0.99006(16) 0.42875(16) 0.20382(13) 0.0242(7) Uani 1 1 d . . . C49 C 1.02152(16) 0.40950(16) 0.26016(13) 0.0263(8) Uani 1 1 d . . . H49 H 0.9838 0.4205 0.2746 0.032 Uiso 1 1 calc R . . C410 C 1.0383(2) 0.33142(19) 0.26824(17) 0.0452(11) Uani 1 1 d . . . H41A H 1.0544 0.3204 0.3048 0.068 Uiso 1 1 calc R . . H41B H 1.0769 0.3193 0.2559 0.068 Uiso 1 1 calc R . . H41C H 0.9943 0.3046 0.2492 0.068 Uiso 1 1 calc R . . C411 C 1.08924(18) 0.4533(2) 0.28964(15) 0.0383(9) Uani 1 1 d . . . H41D H 1.1062 0.4422 0.3262 0.057 Uiso 1 1 calc R . . H41E H 1.0769 0.5029 0.2845 0.057 Uiso 1 1 calc R . . H41F H 1.1278 0.4427 0.2770 0.057 Uiso 1 1 calc R . . C50 C 0.76039(15) 0.54840(14) 0.32912(11) 0.0138(6) Uani 1 1 d . . . C51 C 0.70940(15) 0.60225(15) 0.31197(11) 0.0141(6) Uani 1 1 d . . . C52 C 0.70611(15) 0.65445(15) 0.34521(11) 0.0165(6) Uani 1 1 d . . . H52 H 0.6690 0.6888 0.3334 0.020 Uiso 1 1 calc R . . C53 C 0.75623(16) 0.65731(15) 0.39566(11) 0.0178(6) Uani 1 1 d . . . C54 C 0.80850(16) 0.60440(16) 0.41161(12) 0.0201(7) Uani 1 1 d . . . H54 H 0.8437 0.6053 0.4457 0.024 Uiso 1 1 calc R . . C55 C 0.81057(15) 0.55058(15) 0.37914(11) 0.0165(6) Uani 1 1 d . . . H55 H 0.8465 0.5152 0.3913 0.020 Uiso 1 1 calc R . . C56 C 0.74780(18) 0.71133(17) 0.43337(12) 0.0245(7) Uani 1 1 d . . . C57 C 0.8157(2) 0.71430(19) 0.48289(13) 0.0409(10) Uani 1 1 d . . . H57A H 0.8116 0.7535 0.5039 0.061 Uiso 1 1 calc R . . H57B H 0.8590 0.7205 0.4745 0.061 Uiso 1 1 calc R . . H57C H 0.8201 0.6707 0.5020 0.061 Uiso 1 1 calc R . . C58 C 0.6845(2) 0.68357(19) 0.44765(15) 0.0403(10) Uani 1 1 d . . . H58A H 0.6771 0.7149 0.4727 0.060 Uiso 1 1 calc R . . H58B H 0.6965 0.6368 0.4624 0.060 Uiso 1 1 calc R . . H58C H 0.6398 0.6815 0.4168 0.060 Uiso 1 1 calc R . . C59 C 0.72456(16) 0.78492(16) 0.41004(12) 0.0222(7) Uani 1 1 d . . . H59A H 0.6780 0.7786 0.3806 0.027 Uiso 1 1 calc R . . H59B H 0.7131 0.8120 0.4359 0.027 Uiso 1 1 calc R . . C510 C 0.77187(18) 0.83307(17) 0.39114(13) 0.0282(8) Uani 1 1 d . . . C511 C 0.8420(2) 0.8572(2) 0.43435(16) 0.0485(11) Uani 1 1 d . . . H51A H 0.8308 0.8722 0.4638 0.073 Uiso 1 1 calc R . . H51B H 0.8632 0.8962 0.4223 0.073 Uiso 1 1 calc R . . H51C H 0.8769 0.8186 0.4446 0.073 Uiso 1 1 calc R . . C512 C 0.7250(2) 0.89807(19) 0.36957(17) 0.0517(11) Uani 1 1 d . . . H51D H 0.7135 0.9207 0.3968 0.078 Uiso 1 1 calc R . . H51E H 0.6797 0.8843 0.3417 0.078 Uiso 1 1 calc R . . H51F H 0.7519 0.9307 0.3564 0.078 Uiso 1 1 calc R . . C513 C 0.7920(2) 0.80067(19) 0.34853(15) 0.0407(10) Uani 1 1 d . . . H51G H 0.7476 0.7871 0.3199 0.061 Uiso 1 1 calc R . . H51H H 0.8225 0.7594 0.3618 0.061 Uiso 1 1 calc R . . H51I H 0.8190 0.8348 0.3367 0.061 Uiso 1 1 calc R . . C60 C 0.76475(15) 0.66274(14) 0.22462(11) 0.0135(6) Uani 1 1 d . . . C61 C 0.69371(15) 0.66962(14) 0.22313(11) 0.0134(6) Uani 1 1 d . . . C62 C 0.65489(15) 0.73166(14) 0.20654(10) 0.0134(6) Uani 1 1 d . . . H62 H 0.6067 0.7350 0.2058 0.016 Uiso 1 1 calc R . . C63 C 0.68497(15) 0.78896(14) 0.19096(11) 0.0146(6) Uani 1 1 d . . . C64 C 0.75634(16) 0.78076(15) 0.19298(11) 0.0180(6) Uani 1 1 d . . . H64 H 0.7787 0.8186 0.1827 0.022 Uiso 1 1 calc R . . C65 C 0.79525(16) 0.71987(15) 0.20928(12) 0.0182(7) Uani 1 1 d . . . H65 H 0.8435 0.7168 0.2101 0.022 Uiso 1 1 calc R . . C66 C 0.64426(15) 0.85825(15) 0.17498(11) 0.0167(6) Uani 1 1 d . . . C67 C 0.57137(16) 0.85822(16) 0.18270(12) 0.0211(7) Uani 1 1 d . . . H67A H 0.5471 0.9032 0.1719 0.032 Uiso 1 1 calc R . . H67B H 0.5805 0.8505 0.2190 0.032 Uiso 1 1 calc R . . H67C H 0.5402 0.8209 0.1621 0.032 Uiso 1 1 calc R . . C68 C 0.69161(16) 0.91569(16) 0.21062(12) 0.0228(7) Uani 1 1 d . . . H68A H 0.6667 0.9607 0.2013 0.034 Uiso 1 1 calc R . . H68B H 0.7387 0.9181 0.2068 0.034 Uiso 1 1 calc R . . H68C H 0.6994 0.9046 0.2462 0.034 Uiso 1 1 calc R . . C69 C 0.63395(17) 0.88095(16) 0.11950(12) 0.0218(7) Uani 1 1 d . . . H69A H 0.6065 0.9254 0.1131 0.026 Uiso 1 1 calc R . . H69B H 0.6831 0.8924 0.1204 0.026 Uiso 1 1 calc R . . C610 C 0.59740(18) 0.83575(18) 0.07133(12) 0.0273(8) Uani 1 1 d . . . C611 C 0.52288(19) 0.8064(2) 0.06631(14) 0.0454(11) Uani 1 1 d . . . H61A H 0.4912 0.8447 0.0680 0.068 Uiso 1 1 calc R . . H61B H 0.5293 0.7736 0.0943 0.068 Uiso 1 1 calc R . . H61C H 0.5007 0.7823 0.0334 0.068 Uiso 1 1 calc R . . C612 C 0.5865(2) 0.8839(2) 0.02543(14) 0.0522(12) Uani 1 1 d . . . H61D H 0.6330 0.9055 0.0292 0.078 Uiso 1 1 calc R . . H61E H 0.5512 0.9204 0.0241 0.078 Uiso 1 1 calc R . . H61F H 0.5682 0.8567 -0.0063 0.078 Uiso 1 1 calc R . . C613 C 0.64589(19) 0.77492(17) 0.06880(13) 0.0303(8) Uani 1 1 d . . . H61G H 0.6936 0.7928 0.0717 0.045 Uiso 1 1 calc R . . H61H H 0.6231 0.7505 0.0361 0.045 Uiso 1 1 calc R . . H61I H 0.6520 0.7425 0.0970 0.045 Uiso 1 1 calc R . . C70 C 0.73383(15) 0.41671(14) 0.16524(11) 0.0136(6) Uani 1 1 d . . . C71 C 0.78526(14) 0.36311(15) 0.18194(11) 0.0142(6) Uani 1 1 d . . . C72 C 0.78883(16) 0.31134(15) 0.14821(11) 0.0174(6) Uani 1 1 d . . . H72 H 0.8262 0.2772 0.1598 0.021 Uiso 1 1 calc R . . C73 C 0.73861(16) 0.30858(15) 0.09777(11) 0.0183(7) Uani 1 1 d . . . C74 C 0.68605(16) 0.36113(16) 0.08275(12) 0.0197(7) Uani 1 1 d . . . H74 H 0.6503 0.3602 0.0489 0.024 Uiso 1 1 calc R . . C75 C 0.68376(16) 0.41483(16) 0.11523(11) 0.0189(7) Uani 1 1 d . . . H75 H 0.6478 0.4502 0.1031 0.023 Uiso 1 1 calc R . . C76 C 0.74681(19) 0.25437(17) 0.06045(12) 0.0277(8) Uani 1 1 d . . . C77 C 0.6790(3) 0.2523(2) 0.01061(15) 0.0716(17) Uani 1 1 d . . . H77A H 0.6832 0.2136 -0.0108 0.107 Uiso 1 1 calc R . . H77B H 0.6750 0.2963 -0.0080 0.107 Uiso 1 1 calc R . . H77C H 0.6355 0.2458 0.0187 0.107 Uiso 1 1 calc R . . C78 C 0.8107(3) 0.2794(2) 0.04639(17) 0.0595(14) Uani 1 1 d . . . H78A H 0.8178 0.2469 0.0219 0.089 Uiso 1 1 calc R . . H78B H 0.8551 0.2815 0.0774 0.089 Uiso 1 1 calc R . . H78C H 0.7998 0.3259 0.0309 0.089 Uiso 1 1 calc R . . C79 C 0.76818(17) 0.18022(16) 0.08329(12) 0.0227(7) Uani 1 1 d . . . H79A H 0.7770 0.1525 0.0566 0.027 Uiso 1 1 calc R . . H79B H 0.8160 0.1852 0.1118 0.027 Uiso 1 1 calc R . . C710 C 0.72154(19) 0.13351(19) 0.10390(14) 0.0338(9) Uani 1 1 d . . . C711 C 0.6461(2) 0.1168(3) 0.06400(17) 0.0815(19) Uani 1 1 d . . . H71A H 0.6230 0.0809 0.0775 0.122 Uiso 1 1 calc R . . H71B H 0.6508 0.0998 0.0326 0.122 Uiso 1 1 calc R . . H71C H 0.6161 0.1590 0.0563 0.122 Uiso 1 1 calc R . . C712 C 0.7648(3) 0.0651(3) 0.12006(19) 0.0696(14) Uiso 1 1 d . . . H71D H 0.7378 0.0325 0.1331 0.104 Uiso 1 1 calc R . . H71E H 0.8124 0.0748 0.1470 0.104 Uiso 1 1 calc R . . H71F H 0.7717 0.0444 0.0904 0.104 Uiso 1 1 calc R . . C713 C 0.7120(2) 0.16369(19) 0.15111(13) 0.0362(9) Uani 1 1 d . . . H71G H 0.6858 0.1302 0.1640 0.054 Uiso 1 1 calc R . . H71H H 0.6842 0.2072 0.1419 0.054 Uiso 1 1 calc R . . H71I H 0.7599 0.1730 0.1777 0.054 Uiso 1 1 calc R . . C80 C 0.73125(15) 0.30102(14) 0.26957(11) 0.0145(6) Uani 1 1 d . . . C81 C 0.80225(15) 0.29414(15) 0.27080(10) 0.0139(6) Uani 1 1 d . . . C82 C 0.84135(15) 0.23253(15) 0.28811(10) 0.0145(6) Uani 1 1 d . . . H82 H 0.8894 0.2291 0.2887 0.017 Uiso 1 1 calc R . . C83 C 0.81173(15) 0.17584(15) 0.30461(11) 0.0158(6) Uani 1 1 d . . . C84 C 0.74003(16) 0.18331(15) 0.30177(11) 0.0187(7) Uani 1 1 d . . . H84A H 0.7175 0.1453 0.3117 0.022 Uiso 1 1 calc R . . C85 C 0.70109(16) 0.24393(15) 0.28508(11) 0.0173(6) Uani 1 1 d . . . H85 H 0.6528 0.2469 0.2841 0.021 Uiso 1 1 calc R . . C86 C 0.85267(16) 0.10640(15) 0.32158(12) 0.0194(7) Uani 1 1 d . . . C87 C 0.81203(18) 0.05189(16) 0.28052(13) 0.0285(8) Uani 1 1 d . . . H87A H 0.7616 0.0479 0.2782 0.043 Uiso 1 1 calc R . . H87B H 0.8363 0.0066 0.2900 0.043 Uiso 1 1 calc R . . H87C H 0.8124 0.0665 0.2473 0.043 Uiso 1 1 calc R . . C88 C 0.93044(18) 0.10980(18) 0.32349(15) 0.0365(9) Uani 1 1 d . . . H88A H 0.9547 0.0651 0.3355 0.055 Uiso 1 1 calc R . . H88B H 0.9570 0.1469 0.3470 0.055 Uiso 1 1 calc R . . H88C H 0.9296 0.1196 0.2891 0.055 Uiso 1 1 calc R . . C89 C 0.8486(2) 0.07756(17) 0.37195(12) 0.0299(8) Uani 1 1 d . A . H89A H 0.7962 0.0723 0.3655 0.036 Uiso 1 1 calc R . . H89B H 0.8691 0.0298 0.3762 0.036 Uiso 1 1 calc R . . C810 C 0.8835(2) 0.1133(2) 0.42484(14) 0.0441(10) Uani 1 1 d D . . C811 C 0.8637(2) 0.1872(2) 0.42554(17) 0.0522(11) Uiso 1 1 d . A . H81A H 0.8106 0.1916 0.4129 0.078 Uiso 1 1 calc R . . H81B H 0.8822 0.2141 0.4035 0.078 Uiso 1 1 calc R . . H81C H 0.8852 0.2050 0.4607 0.078 Uiso 1 1 calc R . . C812 C 0.9609(4) 0.0883(4) 0.4523(3) 0.0373(18) Uiso 0.50 1 d P A 1 H81D H 0.9776 0.1010 0.4886 0.056 Uiso 0.50 1 calc PR A 1 H81E H 0.9925 0.1102 0.4369 0.056 Uiso 0.50 1 calc PR A 1 H81F H 0.9627 0.0375 0.4491 0.056 Uiso 0.50 1 calc PR A 1 C814 C 0.8400(4) 0.0775(4) 0.4554(3) 0.0303(16) Uiso 0.50 1 d PD A 1 H81G H 0.8480 0.0270 0.4566 0.045 Uiso 0.50 1 calc PR A 1 H81H H 0.7879 0.0874 0.4381 0.045 Uiso 0.50 1 calc PR A 1 H81I H 0.8573 0.0960 0.4904 0.045 Uiso 0.50 1 calc PR A 1 C813 C 0.9652(4) 0.1352(8) 0.4378(6) 0.125(5) Uiso 0.50 1 d PD A 2 H81J H 0.9886 0.1453 0.4744 0.187 Uiso 0.50 1 calc PR A 2 H81K H 0.9666 0.1769 0.4181 0.187 Uiso 0.50 1 calc PR A 2 H81L H 0.9910 0.0971 0.4288 0.187 Uiso 0.50 1 calc PR A 2 C815 C 0.8848(7) 0.0712(6) 0.4706(3) 0.091(4) Uiso 0.50 1 d PD A 2 H81M H 0.9061 0.0993 0.5017 0.136 Uiso 0.50 1 calc PR A 2 H81N H 0.9141 0.0291 0.4736 0.136 Uiso 0.50 1 calc PR A 2 H81O H 0.8350 0.0580 0.4659 0.136 Uiso 0.50 1 calc PR A 2 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 0.00976(13) 0.01055(14) 0.01414(15) 0.00122(11) 0.00351(11) 0.00075(11) Zr2 0.00956(13) 0.01203(15) 0.01638(15) 0.00170(12) 0.00400(11) 0.00107(11) S1 0.0116(3) 0.0129(3) 0.0144(4) 0.0015(3) 0.0041(3) 0.0000(3) S2 0.0112(3) 0.0122(3) 0.0150(4) 0.0017(3) 0.0031(3) 0.0001(3) O1 0.0122(10) 0.0169(11) 0.0172(11) -0.0004(9) 0.0021(8) 0.0007(8) O2 0.0133(10) 0.0159(10) 0.0187(11) 0.0025(9) 0.0067(8) 0.0002(8) O3 0.0155(10) 0.0156(11) 0.0221(12) 0.0001(9) 0.0024(9) 0.0018(8) O4 0.0136(10) 0.0159(11) 0.0239(11) 0.0027(9) 0.0098(9) 0.0023(8) O5 0.0134(10) 0.0118(10) 0.0155(10) 0.0012(8) 0.0046(8) 0.0014(8) O6 0.0115(10) 0.0109(10) 0.0229(11) 0.0044(9) 0.0054(9) 0.0034(8) O7 0.0136(10) 0.0142(10) 0.0133(10) -0.0014(8) 0.0039(8) 0.0010(8) O8 0.0142(10) 0.0133(11) 0.0213(11) 0.0008(9) 0.0065(9) -0.0001(8) C10 0.0125(14) 0.0265(18) 0.0163(16) -0.0008(13) 0.0033(12) 0.0016(13) C11 0.0214(16) 0.0296(19) 0.0204(17) 0.0030(14) 0.0048(14) 0.0034(14) C12 0.0323(19) 0.0267(19) 0.0222(18) 0.0076(15) 0.0066(15) 0.0080(15) C13 0.046(2) 0.029(2) 0.037(2) 0.0020(17) 0.0153(19) -0.0031(17) C14 0.047(2) 0.038(2) 0.052(3) 0.015(2) 0.006(2) 0.0187(19) C15 0.0289(19) 0.046(2) 0.026(2) 0.0094(17) -0.0016(16) 0.0067(17) C16 0.031(2) 0.052(3) 0.026(2) -0.0087(18) 0.0001(16) -0.0089(18) C17 0.0257(19) 0.039(2) 0.035(2) -0.0140(18) 0.0024(16) -0.0068(16) C18 0.0167(16) 0.0263(18) 0.0309(19) -0.0071(15) 0.0067(14) -0.0032(14) C19 0.0189(17) 0.0198(18) 0.045(2) -0.0028(16) 0.0005(16) -0.0021(14) C110 0.043(2) 0.025(2) 0.086(4) -0.019(2) 0.003(2) -0.0034(18) C111 0.0236(19) 0.037(2) 0.051(3) 0.0132(19) 0.0033(18) -0.0039(16) C20 0.0179(14) 0.0136(15) 0.0218(16) -0.0043(13) 0.0132(13) -0.0050(12) C21 0.0196(15) 0.0223(17) 0.0192(16) -0.0011(13) 0.0072(13) -0.0072(13) C22 0.0198(16) 0.0330(19) 0.0217(18) 0.0093(15) 0.0068(14) -0.0009(15) C23 0.0303(19) 0.047(2) 0.028(2) 0.0130(17) 0.0012(16) -0.0086(17) C24 0.0315(19) 0.032(2) 0.029(2) 0.0055(16) 0.0116(16) 0.0067(16) C25 0.0331(18) 0.034(2) 0.0170(17) -0.0050(15) 0.0114(15) -0.0123(16) C26 0.037(2) 0.031(2) 0.032(2) -0.0115(16) 0.0248(17) -0.0093(16) C27 0.0280(18) 0.0182(17) 0.040(2) -0.0062(15) 0.0214(16) -0.0038(14) C28 0.0188(15) 0.0131(15) 0.0257(17) -0.0030(13) 0.0111(13) -0.0042(12) C29 0.0148(14) 0.0128(15) 0.0300(18) 0.0026(13) 0.0107(13) 0.0024(12) C210 0.0252(18) 0.034(2) 0.033(2) 0.0056(16) 0.0065(15) -0.0081(15) C211 0.0309(19) 0.0226(19) 0.049(2) 0.0043(17) 0.0175(18) 0.0088(15) C30 0.0140(15) 0.0230(17) 0.0247(18) -0.0028(14) -0.0004(13) -0.0016(13) C31 0.0280(18) 0.0268(19) 0.0248(19) -0.0003(15) -0.0023(15) 0.0029(15) C32 0.041(2) 0.0196(18) 0.0230(19) 0.0004(14) -0.0061(16) 0.0057(16) C33 0.061(3) 0.025(2) 0.035(2) -0.0026(17) 0.010(2) -0.0077(19) C34 0.068(3) 0.036(2) 0.045(3) -0.006(2) -0.014(2) 0.020(2) C35 0.048(2) 0.036(2) 0.032(2) -0.0015(18) -0.0115(18) 0.0031(19) C36 0.045(2) 0.045(3) 0.037(2) -0.007(2) -0.0178(19) -0.001(2) C37 0.032(2) 0.033(2) 0.050(3) -0.0164(19) -0.0040(19) -0.0070(17) C38 0.0200(17) 0.0226(18) 0.038(2) -0.0022(16) 0.0004(15) -0.0004(14) C39 0.0220(18) 0.0199(18) 0.057(3) -0.0047(17) 0.0027(18) -0.0057(15) C310 0.030(2) 0.039(2) 0.082(3) 0.024(2) 0.009(2) -0.0066(18) C311 0.047(3) 0.025(2) 0.095(4) -0.006(2) -0.011(3) -0.0007(19) C40 0.0166(15) 0.0180(16) 0.0281(18) -0.0050(14) 0.0124(14) -0.0054(13) C41 0.0202(16) 0.0294(18) 0.0267(18) -0.0052(15) 0.0122(14) -0.0079(14) C42 0.0243(17) 0.045(2) 0.0268(19) 0.0043(17) 0.0132(15) -0.0005(16) C43 0.042(2) 0.091(4) 0.030(2) 0.012(2) 0.0069(19) 0.005(2) C44 0.046(2) 0.046(3) 0.059(3) 0.011(2) 0.025(2) 0.020(2) C45 0.034(2) 0.041(2) 0.030(2) -0.0141(17) 0.0173(17) -0.0149(17) C46 0.039(2) 0.037(2) 0.052(3) -0.0219(19) 0.033(2) -0.0073(18) C47 0.0241(18) 0.027(2) 0.054(3) -0.0083(17) 0.0204(18) 0.0019(15) C48 0.0169(15) 0.0153(16) 0.045(2) -0.0048(15) 0.0171(15) -0.0034(13) C49 0.0153(15) 0.0184(17) 0.047(2) 0.0062(15) 0.0135(16) 0.0028(13) C410 0.031(2) 0.026(2) 0.080(3) 0.016(2) 0.023(2) 0.0139(17) C411 0.0228(18) 0.043(2) 0.046(2) 0.0117(19) 0.0089(17) -0.0043(16) C50 0.0132(14) 0.0137(14) 0.0166(15) 0.0006(12) 0.0081(12) -0.0031(12) C51 0.0126(14) 0.0161(15) 0.0136(15) 0.0010(12) 0.0048(12) -0.0026(12) C52 0.0156(14) 0.0142(15) 0.0204(16) 0.0033(12) 0.0077(13) -0.0004(12) C53 0.0203(15) 0.0190(16) 0.0156(16) -0.0014(13) 0.0085(13) -0.0027(13) C54 0.0203(16) 0.0215(17) 0.0149(16) 0.0012(13) 0.0026(13) -0.0012(13) C55 0.0159(14) 0.0146(15) 0.0178(16) 0.0027(12) 0.0049(12) 0.0000(12) C56 0.0301(18) 0.0257(18) 0.0191(17) -0.0011(14) 0.0108(15) 0.0040(14) C57 0.059(3) 0.032(2) 0.0198(19) -0.0098(16) 0.0011(18) 0.0149(19) C58 0.059(3) 0.037(2) 0.041(2) -0.0030(18) 0.038(2) 0.0012(19) C59 0.0215(16) 0.0246(18) 0.0181(17) -0.0049(13) 0.0046(14) 0.0050(14) C510 0.0286(18) 0.0217(18) 0.031(2) -0.0030(15) 0.0069(16) -0.0015(14) C511 0.042(2) 0.047(3) 0.051(3) -0.013(2) 0.011(2) -0.017(2) C512 0.058(3) 0.023(2) 0.075(3) 0.013(2) 0.026(2) 0.0080(19) C513 0.054(2) 0.032(2) 0.047(2) -0.0044(18) 0.032(2) -0.0134(19) C60 0.0125(14) 0.0109(14) 0.0160(15) -0.0003(12) 0.0040(12) 0.0015(11) C61 0.0148(14) 0.0114(14) 0.0132(15) -0.0006(12) 0.0045(12) -0.0020(11) C62 0.0131(14) 0.0146(15) 0.0133(15) -0.0011(12) 0.0059(12) 0.0007(12) C63 0.0160(14) 0.0135(15) 0.0133(15) -0.0008(12) 0.0042(12) 0.0011(12) C64 0.0196(15) 0.0132(15) 0.0233(17) 0.0028(13) 0.0104(13) -0.0027(12) C65 0.0137(14) 0.0171(16) 0.0258(18) 0.0023(13) 0.0098(13) 0.0014(12) C66 0.0178(15) 0.0131(15) 0.0213(16) 0.0017(12) 0.0099(13) 0.0027(12) C67 0.0224(16) 0.0167(16) 0.0274(18) 0.0048(13) 0.0131(14) 0.0066(13) C68 0.0246(17) 0.0171(16) 0.0255(18) -0.0006(13) 0.0081(14) 0.0017(13) C69 0.0236(16) 0.0193(16) 0.0254(18) 0.0101(14) 0.0126(14) 0.0054(13) C610 0.0278(18) 0.034(2) 0.0205(18) 0.0055(15) 0.0090(15) 0.0064(15) C611 0.028(2) 0.072(3) 0.030(2) -0.013(2) 0.0039(17) -0.005(2) C612 0.074(3) 0.057(3) 0.029(2) 0.019(2) 0.022(2) 0.030(2) C613 0.040(2) 0.031(2) 0.0197(18) -0.0024(15) 0.0120(16) 0.0011(16) C70 0.0135(14) 0.0131(14) 0.0157(15) 0.0002(12) 0.0073(12) -0.0016(12) C71 0.0101(13) 0.0155(15) 0.0160(15) 0.0029(12) 0.0036(12) 0.0005(11) C72 0.0178(15) 0.0158(15) 0.0196(16) 0.0017(13) 0.0081(13) 0.0045(12) C73 0.0220(16) 0.0166(15) 0.0167(16) 0.0002(12) 0.0077(13) 0.0013(13) C74 0.0197(16) 0.0240(17) 0.0144(16) 0.0006(13) 0.0055(13) 0.0013(13) C75 0.0177(15) 0.0211(16) 0.0180(16) 0.0047(13) 0.0068(13) 0.0065(13) C76 0.039(2) 0.0252(18) 0.0173(17) -0.0015(14) 0.0085(15) 0.0107(15) C77 0.106(4) 0.052(3) 0.021(2) -0.0168(19) -0.017(2) 0.050(3) C78 0.115(4) 0.030(2) 0.073(3) 0.010(2) 0.081(3) 0.014(2) C79 0.0245(17) 0.0222(17) 0.0195(17) -0.0053(13) 0.0061(14) 0.0035(14) C710 0.034(2) 0.036(2) 0.032(2) -0.0082(17) 0.0131(17) -0.0080(17) C711 0.057(3) 0.147(5) 0.048(3) -0.043(3) 0.029(3) -0.061(3) C713 0.046(2) 0.034(2) 0.033(2) 0.0010(17) 0.0206(18) -0.0098(18) C80 0.0143(14) 0.0123(14) 0.0145(15) 0.0010(12) 0.0026(12) 0.0020(12) C81 0.0145(14) 0.0143(15) 0.0114(15) 0.0008(12) 0.0032(12) -0.0013(12) C82 0.0125(14) 0.0171(15) 0.0123(15) -0.0015(12) 0.0028(12) 0.0003(12) C83 0.0170(15) 0.0130(15) 0.0160(16) 0.0015(12) 0.0047(12) 0.0018(12) C84 0.0207(16) 0.0136(15) 0.0231(17) 0.0015(13) 0.0097(14) -0.0006(12) C85 0.0149(14) 0.0163(15) 0.0206(17) -0.0011(13) 0.0065(13) -0.0016(12) C86 0.0193(15) 0.0157(15) 0.0218(17) 0.0031(13) 0.0060(13) 0.0037(13) C87 0.0325(19) 0.0187(17) 0.032(2) -0.0017(15) 0.0100(16) 0.0054(14) C88 0.0250(18) 0.0216(18) 0.064(3) 0.0141(18) 0.0184(19) 0.0080(15) C89 0.046(2) 0.0174(17) 0.0263(19) 0.0051(14) 0.0143(17) 0.0111(16) C810 0.054(3) 0.047(3) 0.027(2) -0.0002(18) 0.0113(19) 0.021(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 O1 1.948(2) . ? Zr1 O2 1.950(2) . ? Zr1 O8 1.955(2) . ? Zr1 O7 2.2069(19) . ? Zr1 O5 2.2069(19) . ? Zr1 S1 2.8482(10) . ? Zr1 Zr2 3.5363(9) . ? Zr2 O3 1.942(2) . ? Zr2 O4 1.947(2) . ? Zr2 O6 1.9616(19) . ? Zr2 O5 2.1979(19) . ? Zr2 O7 2.2087(19) . ? Zr2 S2 2.8489(10) . ? S1 C51 1.780(3) . ? S1 C61 1.787(3) . ? S2 C71 1.778(3) . ? S2 C81 1.784(3) . ? O1 C10 1.374(3) . ? O2 C20 1.366(3) . ? O3 C30 1.367(3) . ? O4 C40 1.366(3) . ? O5 C50 1.382(3) . ? O6 C60 1.350(3) . ? O7 C70 1.382(3) . ? O8 C80 1.353(3) . ? C10 C18 1.400(4) . ? C10 C11 1.403(4) . ? C11 C15 1.402(4) . ? C11 C12 1.513(5) . ? C12 C14 1.532(5) . ? C12 C13 1.532(5) . ? C12 H12 1.0000 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.386(5) . ? C15 H15 0.9500 . ? C16 C17 1.372(5) . ? C16 H16 0.9500 . ? C17 C18 1.395(4) . ? C17 H17 0.9500 . ? C18 C19 1.512(5) . ? C19 C111 1.527(5) . ? C19 C110 1.532(5) . ? C19 H19 1.0000 . ? C110 H11A 0.9800 . ? C110 H11B 0.9800 . ? C110 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C20 C21 1.404(4) . ? C20 C28 1.405(4) . ? C21 C25 1.391(4) . ? C21 C22 1.520(4) . ? C22 C23 1.527(4) . ? C22 C24 1.536(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.384(5) . ? C25 H25 0.9500 . ? C26 C27 1.383(5) . ? C26 H26 0.9500 . ? C27 C28 1.395(4) . ? C27 H27 0.9500 . ? C28 C29 1.524(4) . ? C29 C210 1.528(4) . ? C29 C211 1.528(4) . ? C29 H29 1.0000 . ? C210 H21A 0.9800 . ? C210 H21B 0.9800 . ? C210 H21C 0.9800 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C211 H21F 0.9800 . ? C30 C38 1.401(4) . ? C30 C31 1.402(4) . ? C31 C35 1.383(5) . ? C31 C32 1.522(5) . ? C32 C33 1.524(5) . ? C32 C34 1.526(5) . ? C32 H32 1.0000 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.383(5) . ? C35 H35 0.9500 . ? C36 C37 1.378(5) . ? C36 H36 0.9500 . ? C37 C38 1.402(5) . ? C37 H37 0.9500 . ? C38 C39 1.517(5) . ? C39 C311 1.533(5) . ? C39 C310 1.540(6) . ? C39 H39 1.0000 . ? C310 H31A 0.9800 . ? C310 H31B 0.9800 . ? C310 H31C 0.9800 . ? C311 H31D 0.9800 . ? C311 H31E 0.9800 . ? C311 H31F 0.9800 . ? C40 C41 1.407(4) . ? C40 C48 1.407(4) . ? C41 C45 1.391(4) . ? C41 C42 1.513(5) . ? C42 C44 1.518(5) . ? C42 C43 1.534(5) . ? C42 H42 1.0000 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.392(5) . ? C45 H45 0.9500 . ? C46 C47 1.372(5) . ? C46 H46 0.9500 . ? C47 C48 1.398(4) . ? C47 H47 0.9500 . ? C48 C49 1.517(5) . ? C49 C410 1.533(4) . ? C49 C411 1.536(4) . ? C49 H49 1.0000 . ? C410 H41A 0.9800 . ? C410 H41B 0.9800 . ? C410 H41C 0.9800 . ? C411 H41D 0.9800 . ? C411 H41E 0.9800 . ? C411 H41F 0.9800 . ? C50 C55 1.386(4) . ? C50 C51 1.398(4) . ? C51 C52 1.390(4) . ? C52 C53 1.396(4) . ? C52 H52 0.9500 . ? C53 C54 1.398(4) . ? C53 C56 1.538(4) . ? C54 C55 1.391(4) . ? C54 H54 0.9500 . ? C55 H55 0.9500 . ? C56 C57 1.532(5) . ? C56 C58 1.551(5) . ? C56 C59 1.552(4) . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C510 1.547(4) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C510 C513 1.533(5) . ? C510 C511 1.535(5) . ? C510 C512 1.537(5) . ? C511 H51A 0.9800 . ? C511 H51B 0.9800 . ? C511 H51C 0.9800 . ? C512 H51D 0.9800 . ? C512 H51E 0.9800 . ? C512 H51F 0.9800 . ? C513 H51G 0.9800 . ? C513 H51H 0.9800 . ? C513 H51I 0.9800 . ? C60 C65 1.397(4) . ? C60 C61 1.400(4) . ? C61 C62 1.399(4) . ? C62 C63 1.398(4) . ? C62 H62 0.9500 . ? C63 C64 1.404(4) . ? C63 C66 1.532(4) . ? C64 C65 1.380(4) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 C67 1.541(4) . ? C66 C68 1.547(4) . ? C66 C69 1.561(4) . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C610 1.542(4) . ? C69 H69A 0.9900 . ? C69 H69B 0.9900 . ? C610 C613 1.531(4) . ? C610 C611 1.537(5) . ? C610 C612 1.538(5) . ? C611 H61A 0.9800 . ? C611 H61B 0.9800 . ? C611 H61C 0.9800 . ? C612 H61D 0.9800 . ? C612 H61E 0.9800 . ? C612 H61F 0.9800 . ? C613 H61G 0.9800 . ? C613 H61H 0.9800 . ? C613 H61I 0.9800 . ? C70 C75 1.385(4) . ? C70 C71 1.399(4) . ? C71 C72 1.395(4) . ? C72 C73 1.396(4) . ? C72 H72 0.9500 . ? C73 C74 1.396(4) . ? C73 C76 1.531(4) . ? C74 C75 1.390(4) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.536(5) . ? C76 C78 1.540(5) . ? C76 C79 1.553(4) . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C710 1.550(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C710 C713 1.527(5) . ? C710 C711 1.529(5) . ? C710 C712 1.540(6) . ? C711 H71A 0.9800 . ? C711 H71B 0.9800 . ? C711 H71C 0.9800 . ? C712 H71D 0.9800 . ? C712 H71E 0.9800 . ? C712 H71F 0.9800 . ? C713 H71G 0.9800 . ? C713 H71H 0.9800 . ? C713 H71I 0.9800 . ? C80 C85 1.395(4) . ? C80 C81 1.401(4) . ? C81 C82 1.397(4) . ? C82 C83 1.397(4) . ? C82 H82 0.9500 . ? C83 C84 1.401(4) . ? C83 C86 1.539(4) . ? C84 C85 1.377(4) . ? C84 H84A 0.9500 . ? C85 H85 0.9500 . ? C86 C88 1.524(4) . ? C86 C87 1.543(4) . ? C86 C89 1.554(4) . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 C810 1.547(5) . ? C89 H89A 0.9900 . ? C89 H89B 0.9900 . ? C810 C811 1.472(5) . ? C810 C812 1.513(8) . ? C810 C815 1.513(5) . ? C810 C813 1.577(5) . ? C810 C814 1.587(4) . ? C811 H81A 0.9800 . ? C811 H81B 0.9800 . ? C811 H81C 0.9800 . ? C812 H81D 0.9800 . ? C812 H81E 0.9800 . ? C812 H81F 0.9800 . ? C814 H81G 0.9800 . ? C814 H81H 0.9800 . ? C814 H81I 0.9800 . ? C813 H81J 0.9800 . ? C813 H81K 0.9800 . ? C813 H81L 0.9800 . ? C815 H81M 0.9800 . ? C815 H81N 0.9800 . ? C815 H81O 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 Zr1 O2 98.95(8) . . ? O1 Zr1 O8 107.00(8) . . ? O2 Zr1 O8 102.06(8) . . ? O1 Zr1 O7 92.22(8) . . ? O2 Zr1 O7 161.83(8) . . ? O8 Zr1 O7 88.16(8) . . ? O1 Zr1 O5 157.13(8) . . ? O2 Zr1 O5 91.42(8) . . ? O8 Zr1 O5 90.49(8) . . ? O7 Zr1 O5 73.32(7) . . ? O1 Zr1 S1 92.43(6) . . ? O2 Zr1 S1 75.70(6) . . ? O8 Zr1 S1 160.51(6) . . ? O7 Zr1 S1 89.62(5) . . ? O5 Zr1 S1 70.35(5) . . ? O1 Zr1 Zr2 127.03(6) . . ? O2 Zr1 Zr2 127.35(6) . . ? O8 Zr1 Zr2 88.82(6) . . ? O7 Zr1 Zr2 36.81(5) . . ? O5 Zr1 Zr2 36.51(5) . . ? S1 Zr1 Zr2 77.956(17) . . ? O3 Zr2 O4 98.69(8) . . ? O3 Zr2 O6 107.28(8) . . ? O4 Zr2 O6 102.28(8) . . ? O3 Zr2 O5 89.82(8) . . ? O4 Zr2 O5 163.22(8) . . ? O6 Zr2 O5 88.79(7) . . ? O3 Zr2 O7 155.39(8) . . ? O4 Zr2 O7 93.62(8) . . ? O6 Zr2 O7 90.63(8) . . ? O5 Zr2 O7 73.46(7) . . ? O3 Zr2 S2 92.27(6) . . ? O4 Zr2 S2 74.47(6) . . ? O6 Zr2 S2 160.45(6) . . ? O5 Zr2 S2 90.86(5) . . ? O7 Zr2 S2 70.58(5) . . ? O3 Zr2 Zr1 124.25(6) . . ? O4 Zr2 Zr1 129.50(6) . . ? O6 Zr2 Zr1 89.99(6) . . ? O5 Zr2 Zr1 36.69(5) . . ? O7 Zr2 Zr1 36.77(5) . . ? S2 Zr2 Zr1 78.251(17) . . ? C51 S1 C61 99.89(13) . . ? C51 S1 Zr1 91.95(9) . . ? C61 S1 Zr1 128.80(10) . . ? C71 S2 C81 100.49(13) . . ? C71 S2 Zr2 91.74(9) . . ? C81 S2 Zr2 128.27(10) . . ? C10 O1 Zr1 169.49(19) . . ? C20 O2 Zr1 169.69(18) . . ? C30 O3 Zr2 173.8(2) . . ? C40 O4 Zr2 169.67(19) . . ? C50 O5 Zr2 115.92(16) . . ? C50 O5 Zr1 120.89(16) . . ? Zr2 O5 Zr1 106.80(8) . . ? C60 O6 Zr2 164.88(18) . . ? C70 O7 Zr1 115.57(16) . . ? C70 O7 Zr2 121.19(16) . . ? Zr1 O7 Zr2 106.42(8) . . ? C80 O8 Zr1 166.78(18) . . ? O1 C10 C18 118.4(3) . . ? O1 C10 C11 118.6(3) . . ? C18 C10 C11 123.0(3) . . ? C15 C11 C10 116.9(3) . . ? C15 C11 C12 122.2(3) . . ? C10 C11 C12 120.9(3) . . ? C11 C12 C14 113.5(3) . . ? C11 C12 C13 111.5(3) . . ? C14 C12 C13 110.2(3) . . ? C11 C12 H12 107.1 . . ? C14 C12 H12 107.1 . . ? C13 C12 H12 107.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C11 120.9(3) . . ? C16 C15 H15 119.6 . . ? C11 C15 H15 119.6 . . ? C17 C16 C15 120.7(3) . . ? C17 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C16 C17 C18 121.2(3) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C17 C18 C10 117.3(3) . . ? C17 C18 C19 122.7(3) . . ? C10 C18 C19 119.9(3) . . ? C18 C19 C111 110.1(3) . . ? C18 C19 C110 113.7(3) . . ? C111 C19 C110 110.8(3) . . ? C18 C19 H19 107.3 . . ? C111 C19 H19 107.3 . . ? C110 C19 H19 107.3 . . ? C19 C110 H11A 109.5 . . ? C19 C110 H11B 109.5 . . ? H11A C110 H11B 109.5 . . ? C19 C110 H11C 109.5 . . ? H11A C110 H11C 109.5 . . ? H11B C110 H11C 109.5 . . ? C19 C111 H11D 109.5 . . ? C19 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C19 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? O2 C20 C21 118.7(3) . . ? O2 C20 C28 119.2(3) . . ? C21 C20 C28 122.1(3) . . ? C25 C21 C20 118.0(3) . . ? C25 C21 C22 122.4(3) . . ? C20 C21 C22 119.5(3) . . ? C21 C22 C23 113.7(3) . . ? C21 C22 C24 110.0(3) . . ? C23 C22 C24 110.3(3) . . ? C21 C22 H22 107.5 . . ? C23 C22 H22 107.5 . . ? C24 C22 H22 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C21 121.0(3) . . ? C26 C25 H25 119.5 . . ? C21 C25 H25 119.5 . . ? C27 C26 C25 120.2(3) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 121.2(3) . . ? C26 C27 H27 119.4 . . ? C28 C27 H27 119.4 . . ? C27 C28 C20 117.6(3) . . ? C27 C28 C29 121.4(3) . . ? C20 C28 C29 121.0(3) . . ? C28 C29 C210 111.5(2) . . ? C28 C29 C211 111.8(3) . . ? C210 C29 C211 110.8(3) . . ? C28 C29 H29 107.5 . . ? C210 C29 H29 107.5 . . ? C211 C29 H29 107.5 . . ? C29 C210 H21A 109.5 . . ? C29 C210 H21B 109.5 . . ? H21A C210 H21B 109.5 . . ? C29 C210 H21C 109.5 . . ? H21A C210 H21C 109.5 . . ? H21B C210 H21C 109.5 . . ? C29 C211 H21D 109.5 . . ? C29 C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? C29 C211 H21F 109.5 . . ? H21D C211 H21F 109.5 . . ? H21E C211 H21F 109.5 . . ? O3 C30 C38 117.9(3) . . ? O3 C30 C31 119.7(3) . . ? C38 C30 C31 122.4(3) . . ? C35 C31 C30 117.7(3) . . ? C35 C31 C32 121.5(3) . . ? C30 C31 C32 120.7(3) . . ? C31 C32 C33 110.6(3) . . ? C31 C32 C34 113.5(3) . . ? C33 C32 C34 110.4(3) . . ? C31 C32 H32 107.3 . . ? C33 C32 H32 107.3 . . ? C34 C32 H32 107.3 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C31 C35 C36 121.1(4) . . ? C31 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 120.6(4) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 120.6(3) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C30 C38 C37 117.5(3) . . ? C30 C38 C39 120.0(3) . . ? C37 C38 C39 122.5(3) . . ? C38 C39 C311 113.7(3) . . ? C38 C39 C310 110.7(3) . . ? C311 C39 C310 110.8(3) . . ? C38 C39 H39 107.1 . . ? C311 C39 H39 107.1 . . ? C310 C39 H39 107.1 . . ? C39 C310 H31A 109.5 . . ? C39 C310 H31B 109.5 . . ? H31A C310 H31B 109.5 . . ? C39 C310 H31C 109.5 . . ? H31A C310 H31C 109.5 . . ? H31B C310 H31C 109.5 . . ? C39 C311 H31D 109.5 . . ? C39 C311 H31E 109.5 . . ? H31D C311 H31E 109.5 . . ? C39 C311 H31F 109.5 . . ? H31D C311 H31F 109.5 . . ? H31E C311 H31F 109.5 . . ? O4 C40 C41 118.2(3) . . ? O4 C40 C48 119.5(3) . . ? C41 C40 C48 122.3(3) . . ? C45 C41 C40 117.6(3) . . ? C45 C41 C42 122.3(3) . . ? C40 C41 C42 120.1(3) . . ? C41 C42 C44 109.9(3) . . ? C41 C42 C43 113.5(3) . . ? C44 C42 C43 111.4(3) . . ? C41 C42 H42 107.2 . . ? C44 C42 H42 107.2 . . ? C43 C42 H42 107.2 . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C42 C44 H44A 109.5 . . ? C42 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C42 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C41 C45 C46 121.0(3) . . ? C41 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C47 C46 C45 120.3(3) . . ? C47 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C46 C47 C48 121.5(3) . . ? C46 C47 H47 119.3 . . ? C48 C47 H47 119.3 . . ? C47 C48 C40 117.3(3) . . ? C47 C48 C49 120.8(3) . . ? C40 C48 C49 121.8(3) . . ? C48 C49 C410 112.0(3) . . ? C48 C49 C411 111.3(3) . . ? C410 C49 C411 111.0(3) . . ? C48 C49 H49 107.4 . . ? C410 C49 H49 107.4 . . ? C411 C49 H49 107.4 . . ? C49 C410 H41A 109.5 . . ? C49 C410 H41B 109.5 . . ? H41A C410 H41B 109.5 . . ? C49 C410 H41C 109.5 . . ? H41A C410 H41C 109.5 . . ? H41B C410 H41C 109.5 . . ? C49 C411 H41D 109.5 . . ? C49 C411 H41E 109.5 . . ? H41D C411 H41E 109.5 . . ? C49 C411 H41F 109.5 . . ? H41D C411 H41F 109.5 . . ? H41E C411 H41F 109.5 . . ? O5 C50 C55 121.8(2) . . ? O5 C50 C51 119.7(2) . . ? C55 C50 C51 118.5(3) . . ? C52 C51 C50 120.7(3) . . ? C52 C51 S1 120.6(2) . . ? C50 C51 S1 118.6(2) . . ? C51 C52 C53 121.3(3) . . ? C51 C52 H52 119.4 . . ? C53 C52 H52 119.4 . . ? C52 C53 C54 117.1(3) . . ? C52 C53 C56 120.6(3) . . ? C54 C53 C56 121.8(3) . . ? C55 C54 C53 122.0(3) . . ? C55 C54 H54 119.0 . . ? C53 C54 H54 119.0 . . ? C50 C55 C54 120.2(3) . . ? C50 C55 H55 119.9 . . ? C54 C55 H55 119.9 . . ? C57 C56 C53 111.5(3) . . ? C57 C56 C58 107.2(3) . . ? C53 C56 C58 104.9(3) . . ? C57 C56 C59 111.8(3) . . ? C53 C56 C59 114.4(3) . . ? C58 C56 C59 106.4(3) . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C510 C59 C56 124.5(3) . . ? C510 C59 H59A 106.2 . . ? C56 C59 H59A 106.2 . . ? C510 C59 H59B 106.2 . . ? C56 C59 H59B 106.2 . . ? H59A C59 H59B 106.4 . . ? C513 C510 C511 108.5(3) . . ? C513 C510 C512 108.5(3) . . ? C511 C510 C512 107.5(3) . . ? C513 C510 C59 113.5(3) . . ? C511 C510 C59 113.1(3) . . ? C512 C510 C59 105.4(3) . . ? C510 C511 H51A 109.5 . . ? C510 C511 H51B 109.5 . . ? H51A C511 H51B 109.5 . . ? C510 C511 H51C 109.5 . . ? H51A C511 H51C 109.5 . . ? H51B C511 H51C 109.5 . . ? C510 C512 H51D 109.5 . . ? C510 C512 H51E 109.5 . . ? H51D C512 H51E 109.5 . . ? C510 C512 H51F 109.5 . . ? H51D C512 H51F 109.5 . . ? H51E C512 H51F 109.5 . . ? C510 C513 H51G 109.5 . . ? C510 C513 H51H 109.5 . . ? H51G C513 H51H 109.5 . . ? C510 C513 H51I 109.5 . . ? H51G C513 H51I 109.5 . . ? H51H C513 H51I 109.5 . . ? O6 C60 C65 119.8(2) . . ? O6 C60 C61 122.5(2) . . ? C65 C60 C61 117.7(3) . . ? C62 C61 C60 120.7(3) . . ? C62 C61 S1 116.3(2) . . ? C60 C61 S1 122.8(2) . . ? C63 C62 C61 121.9(3) . . ? C63 C62 H62 119.1 . . ? C61 C62 H62 119.1 . . ? C62 C63 C64 116.2(3) . . ? C62 C63 C66 122.3(3) . . ? C64 C63 C66 121.4(3) . . ? C65 C64 C63 122.5(3) . . ? C65 C64 H64 118.8 . . ? C63 C64 H64 118.8 . . ? C64 C65 C60 120.9(3) . . ? C64 C65 H65 119.5 . . ? C60 C65 H65 119.5 . . ? C63 C66 C67 112.1(2) . . ? C63 C66 C68 107.7(2) . . ? C67 C66 C68 106.3(2) . . ? C63 C66 C69 113.1(2) . . ? C67 C66 C69 111.5(2) . . ? C68 C66 C69 105.7(2) . . ? C66 C67 H67A 109.5 . . ? C66 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C66 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? C66 C68 H68A 109.5 . . ? C66 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C66 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C610 C69 C66 124.5(3) . . ? C610 C69 H69A 106.2 . . ? C66 C69 H69A 106.2 . . ? C610 C69 H69B 106.2 . . ? C66 C69 H69B 106.2 . . ? H69A C69 H69B 106.4 . . ? C613 C610 C611 108.4(3) . . ? C613 C610 C612 108.1(3) . . ? C611 C610 C612 108.5(3) . . ? C613 C610 C69 112.0(3) . . ? C611 C610 C69 113.8(3) . . ? C612 C610 C69 105.8(3) . . ? C610 C611 H61A 109.5 . . ? C610 C611 H61B 109.5 . . ? H61A C611 H61B 109.5 . . ? C610 C611 H61C 109.5 . . ? H61A C611 H61C 109.5 . . ? H61B C611 H61C 109.5 . . ? C610 C612 H61D 109.5 . . ? C610 C612 H61E 109.5 . . ? H61D C612 H61E 109.5 . . ? C610 C612 H61F 109.5 . . ? H61D C612 H61F 109.5 . . ? H61E C612 H61F 109.5 . . ? C610 C613 H61G 109.5 . . ? C610 C613 H61H 109.5 . . ? H61G C613 H61H 109.5 . . ? C610 C613 H61I 109.5 . . ? H61G C613 H61I 109.5 . . ? H61H C613 H61I 109.5 . . ? O7 C70 C75 122.2(2) . . ? O7 C70 C71 119.4(2) . . ? C75 C70 C71 118.4(3) . . ? C72 C71 C70 120.8(3) . . ? C72 C71 S2 120.0(2) . . ? C70 C71 S2 119.2(2) . . ? C71 C72 C73 121.4(3) . . ? C71 C72 H72 119.3 . . ? C73 C72 H72 119.3 . . ? C72 C73 C74 116.5(3) . . ? C72 C73 C76 120.4(3) . . ? C74 C73 C76 122.9(3) . . ? C75 C74 C73 122.8(3) . . ? C75 C74 H74 118.6 . . ? C73 C74 H74 118.6 . . ? C70 C75 C74 120.0(3) . . ? C70 C75 H75 120.0 . . ? C74 C75 H75 120.0 . . ? C73 C76 C77 111.3(3) . . ? C73 C76 C78 106.0(3) . . ? C77 C76 C78 107.1(3) . . ? C73 C76 C79 114.9(3) . . ? C77 C76 C79 111.3(3) . . ? C78 C76 C79 105.7(3) . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C710 C79 C76 125.2(3) . . ? C710 C79 H79A 106.0 . . ? C76 C79 H79A 106.0 . . ? C710 C79 H79B 106.0 . . ? C76 C79 H79B 106.0 . . ? H79A C79 H79B 106.3 . . ? C713 C710 C711 108.2(3) . . ? C713 C710 C712 107.7(3) . . ? C711 C710 C712 108.7(4) . . ? C713 C710 C79 113.3(3) . . ? C711 C710 C79 113.7(3) . . ? C712 C710 C79 105.0(3) . . ? C710 C711 H71A 109.5 . . ? C710 C711 H71B 109.5 . . ? H71A C711 H71B 109.5 . . ? C710 C711 H71C 109.5 . . ? H71A C711 H71C 109.5 . . ? H71B C711 H71C 109.5 . . ? C710 C712 H71D 109.5 . . ? C710 C712 H71E 109.5 . . ? H71D C712 H71E 109.5 . . ? C710 C712 H71F 109.5 . . ? H71D C712 H71F 109.5 . . ? H71E C712 H71F 109.5 . . ? C710 C713 H71G 109.5 . . ? C710 C713 H71H 109.5 . . ? H71G C713 H71H 109.5 . . ? C710 C713 H71I 109.5 . . ? H71G C713 H71I 109.5 . . ? H71H C713 H71I 109.5 . . ? O8 C80 C85 120.5(3) . . ? O8 C80 C81 121.9(3) . . ? C85 C80 C81 117.6(3) . . ? C82 C81 C80 120.6(3) . . ? C82 C81 S2 116.9(2) . . ? C80 C81 S2 122.5(2) . . ? C83 C82 C81 121.9(3) . . ? C83 C82 H82 119.1 . . ? C81 C82 H82 119.1 . . ? C82 C83 C84 116.5(3) . . ? C82 C83 C86 122.6(3) . . ? C84 C83 C86 120.8(3) . . ? C85 C84 C83 122.2(3) . . ? C85 C84 H84A 118.9 . . ? C83 C84 H84A 118.9 . . ? C84 C85 C80 121.2(3) . . ? C84 C85 H85 119.4 . . ? C80 C85 H85 119.4 . . ? C88 C86 C83 112.5(2) . . ? C88 C86 C87 106.9(3) . . ? C83 C86 C87 106.8(2) . . ? C88 C86 C89 112.5(3) . . ? C83 C86 C89 112.9(2) . . ? C87 C86 C89 104.6(3) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C86 C88 H88A 109.5 . . ? C86 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C86 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C810 C89 C86 124.3(3) . . ? C810 C89 H89A 106.2 . . ? C86 C89 H89A 106.2 . . ? C810 C89 H89B 106.2 . . ? C86 C89 H89B 106.2 . . ? H89A C89 H89B 106.4 . . ? C811 C810 C812 121.5(5) . . ? C811 C810 C815 114.9(6) . . ? C812 C810 C815 73.0(6) . . ? C811 C810 C89 114.5(3) . . ? C812 C810 C89 110.5(4) . . ? C815 C810 C89 116.2(6) . . ? C811 C810 C813 89.8(6) . . ? C812 C810 C813 37.9(6) . . ? C815 C810 C813 105.1(8) . . ? C89 C810 C813 112.8(6) . . ? C811 C810 C814 102.0(4) . . ? C812 C810 C814 103.8(5) . . ? C815 C810 C814 31.2(5) . . ? C89 C810 C814 101.2(4) . . ? C813 C810 C814 135.3(7) . . ? C810 C811 H81A 109.5 . . ? C810 C811 H81B 109.5 . . ? H81A C811 H81B 109.5 . . ? C810 C811 H81C 109.5 . . ? H81A C811 H81C 109.5 . . ? H81B C811 H81C 109.5 . . ? C810 C812 H81D 109.5 . . ? C810 C812 H81E 109.5 . . ? C810 C812 H81F 109.5 . . ? C810 C814 H81G 109.5 . . ? C810 C814 H81H 109.5 . . ? C810 C814 H81I 109.5 . . ? C810 C813 H81J 109.5 . . ? C810 C813 H81K 109.5 . . ? H81J C813 H81K 109.5 . . ? C810 C813 H81L 109.5 . . ? H81J C813 H81L 109.5 . . ? H81K C813 H81L 109.5 . . ? C810 C815 H81M 109.5 . . ? C810 C815 H81N 109.5 . . ? H81M C815 H81N 109.5 . . ? C810 C815 H81O 109.5 . . ? H81M C815 H81O 109.5 . . ? H81N C815 H81O 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 Zr1 Zr2 O3 -179.90(10) . . . . ? O2 Zr1 Zr2 O3 34.94(10) . . . . ? O8 Zr1 Zr2 O3 -69.37(9) . . . . ? O7 Zr1 Zr2 O3 -157.88(11) . . . . ? O5 Zr1 Zr2 O3 23.06(11) . . . . ? S1 Zr1 Zr2 O3 96.23(7) . . . . ? O1 Zr1 Zr2 O4 -36.95(10) . . . . ? O2 Zr1 Zr2 O4 177.90(11) . . . . ? O8 Zr1 Zr2 O4 73.58(9) . . . . ? O7 Zr1 Zr2 O4 -14.92(11) . . . . ? O5 Zr1 Zr2 O4 166.01(11) . . . . ? S1 Zr1 Zr2 O4 -120.82(8) . . . . ? O1 Zr1 Zr2 O6 69.04(9) . . . . ? O2 Zr1 Zr2 O6 -76.11(9) . . . . ? O8 Zr1 Zr2 O6 179.58(8) . . . . ? O7 Zr1 Zr2 O6 91.07(10) . . . . ? O5 Zr1 Zr2 O6 -87.99(10) . . . . ? S1 Zr1 Zr2 O6 -14.83(6) . . . . ? O1 Zr1 Zr2 O5 157.04(11) . . . . ? O2 Zr1 Zr2 O5 11.88(11) . . . . ? O8 Zr1 Zr2 O5 -92.43(10) . . . . ? O7 Zr1 Zr2 O5 179.06(12) . . . . ? S1 Zr1 Zr2 O5 73.16(8) . . . . ? O1 Zr1 Zr2 O7 -22.03(11) . . . . ? O2 Zr1 Zr2 O7 -167.18(11) . . . . ? O8 Zr1 Zr2 O7 88.51(10) . . . . ? O5 Zr1 Zr2 O7 -179.06(12) . . . . ? S1 Zr1 Zr2 O7 -105.90(8) . . . . ? O1 Zr1 Zr2 S2 -95.22(7) . . . . ? O2 Zr1 Zr2 S2 119.62(7) . . . . ? O8 Zr1 Zr2 S2 15.31(6) . . . . ? O7 Zr1 Zr2 S2 -73.20(8) . . . . ? O5 Zr1 Zr2 S2 107.74(8) . . . . ? S1 Zr1 Zr2 S2 -179.10(2) . . . . ? O1 Zr1 S1 C51 165.32(11) . . . . ? O2 Zr1 S1 C51 66.71(11) . . . . ? O8 Zr1 S1 C51 -19.1(2) . . . . ? O7 Zr1 S1 C51 -102.47(10) . . . . ? O5 Zr1 S1 C51 -30.08(10) . . . . ? Zr2 Zr1 S1 C51 -67.29(9) . . . . ? O1 Zr1 S1 C61 -90.33(13) . . . . ? O2 Zr1 S1 C61 171.05(13) . . . . ? O8 Zr1 S1 C61 85.3(2) . . . . ? O7 Zr1 S1 C61 1.88(13) . . . . ? O5 Zr1 S1 C61 74.27(13) . . . . ? Zr2 Zr1 S1 C61 37.06(12) . . . . ? O3 Zr2 S2 C71 -168.38(11) . . . . ? O4 Zr2 S2 C71 -69.99(11) . . . . ? O6 Zr2 S2 C71 13.0(2) . . . . ? O5 Zr2 S2 C71 101.76(10) . . . . ? O7 Zr2 S2 C71 29.66(10) . . . . ? Zr1 Zr2 S2 C71 67.07(9) . . . . ? O3 Zr2 S2 C81 86.79(13) . . . . ? O4 Zr2 S2 C81 -174.81(13) . . . . ? O6 Zr2 S2 C81 -91.9(2) . . . . ? O5 Zr2 S2 C81 -3.06(13) . . . . ? O7 Zr2 S2 C81 -75.17(13) . . . . ? Zr1 Zr2 S2 C81 -37.75(12) . . . . ? O2 Zr1 O1 C10 -115.0(10) . . . . ? O8 Zr1 O1 C10 -9.4(10) . . . . ? O7 Zr1 O1 C10 79.4(10) . . . . ? O5 Zr1 O1 C10 129.1(10) . . . . ? S1 Zr1 O1 C10 169.1(10) . . . . ? Zr2 Zr1 O1 C10 92.4(10) . . . . ? O1 Zr1 O2 C20 -110.8(10) . . . . ? O8 Zr1 O2 C20 139.5(10) . . . . ? O7 Zr1 O2 C20 16.4(12) . . . . ? O5 Zr1 O2 C20 48.7(10) . . . . ? S1 Zr1 O2 C20 -20.6(10) . . . . ? Zr2 Zr1 O2 C20 41.7(10) . . . . ? O4 Zr2 O3 C30 137.3(19) . . . . ? O6 Zr2 O3 C30 31.5(19) . . . . ? O5 Zr2 O3 C30 -57.2(19) . . . . ? O7 Zr2 O3 C30 -103.5(19) . . . . ? S2 Zr2 O3 C30 -148.1(19) . . . . ? Zr1 Zr2 O3 C30 -70.8(19) . . . . ? O3 Zr2 O4 C40 99.6(11) . . . . ? O6 Zr2 O4 C40 -150.5(10) . . . . ? O5 Zr2 O4 C40 -20.1(12) . . . . ? O7 Zr2 O4 C40 -59.0(11) . . . . ? S2 Zr2 O4 C40 9.7(10) . . . . ? Zr1 Zr2 O4 C40 -50.1(11) . . . . ? O3 Zr2 O5 C50 60.91(18) . . . . ? O4 Zr2 O5 C50 -178.2(2) . . . . ? O6 Zr2 O5 C50 -46.38(18) . . . . ? O7 Zr2 O5 C50 -137.40(18) . . . . ? S2 Zr2 O5 C50 153.17(17) . . . . ? Zr1 Zr2 O5 C50 -138.0(2) . . . . ? O3 Zr2 O5 Zr1 -161.11(9) . . . . ? O4 Zr2 O5 Zr1 -40.2(3) . . . . ? O6 Zr2 O5 Zr1 91.60(9) . . . . ? O7 Zr2 O5 Zr1 0.59(8) . . . . ? S2 Zr2 O5 Zr1 -68.84(7) . . . . ? O1 Zr1 O5 C50 82.2(3) . . . . ? O2 Zr1 O5 C50 -35.13(19) . . . . ? O8 Zr1 O5 C50 -137.21(19) . . . . ? O7 Zr1 O5 C50 134.86(19) . . . . ? S1 Zr1 O5 C50 39.14(17) . . . . ? Zr2 Zr1 O5 C50 135.4(2) . . . . ? O1 Zr1 O5 Zr2 -53.3(2) . . . . ? O2 Zr1 O5 Zr2 -170.58(8) . . . . ? O8 Zr1 O5 Zr2 87.34(9) . . . . ? O7 Zr1 O5 Zr2 -0.59(8) . . . . ? S1 Zr1 O5 Zr2 -96.31(7) . . . . ? O3 Zr2 O6 C60 -147.2(7) . . . . ? O4 Zr2 O6 C60 109.5(7) . . . . ? O5 Zr2 O6 C60 -57.8(7) . . . . ? O7 Zr2 O6 C60 15.6(7) . . . . ? S2 Zr2 O6 C60 31.4(8) . . . . ? Zr1 Zr2 O6 C60 -21.1(7) . . . . ? O1 Zr1 O7 C70 -59.74(18) . . . . ? O2 Zr1 O7 C70 172.1(2) . . . . ? O8 Zr1 O7 C70 47.21(18) . . . . ? O5 Zr1 O7 C70 138.28(18) . . . . ? S1 Zr1 O7 C70 -152.15(17) . . . . ? Zr2 Zr1 O7 C70 137.7(2) . . . . ? O1 Zr1 O7 Zr2 162.56(8) . . . . ? O2 Zr1 O7 Zr2 34.5(3) . . . . ? O8 Zr1 O7 Zr2 -90.49(9) . . . . ? O5 Zr1 O7 Zr2 0.58(8) . . . . ? S1 Zr1 O7 Zr2 70.15(7) . . . . ? O3 Zr2 O7 C70 -86.4(3) . . . . ? O4 Zr2 O7 C70 33.73(19) . . . . ? O6 Zr2 O7 C70 136.08(19) . . . . ? O5 Zr2 O7 C70 -135.37(19) . . . . ? S2 Zr2 O7 C70 -38.41(18) . . . . ? Zr1 Zr2 O7 C70 -134.8(2) . . . . ? O3 Zr2 O7 Zr1 48.4(2) . . . . ? O4 Zr2 O7 Zr1 168.51(8) . . . . ? O6 Zr2 O7 Zr1 -89.14(9) . . . . ? O5 Zr2 O7 Zr1 -0.58(8) . . . . ? S2 Zr2 O7 Zr1 96.38(7) . . . . ? O1 Zr1 O8 C80 150.9(8) . . . . ? O2 Zr1 O8 C80 -105.7(8) . . . . ? O7 Zr1 O8 C80 59.1(8) . . . . ? O5 Zr1 O8 C80 -14.2(8) . . . . ? S1 Zr1 O8 C80 -24.6(9) . . . . ? Zr2 Zr1 O8 C80 22.3(8) . . . . ? Zr1 O1 C10 C18 19.1(12) . . . . ? Zr1 O1 C10 C11 -160.4(9) . . . . ? O1 C10 C11 C15 177.5(3) . . . . ? C18 C10 C11 C15 -1.9(5) . . . . ? O1 C10 C11 C12 -1.4(4) . . . . ? C18 C10 C11 C12 179.2(3) . . . . ? C15 C11 C12 C14 29.4(5) . . . . ? C10 C11 C12 C14 -151.7(3) . . . . ? C15 C11 C12 C13 -95.8(4) . . . . ? C10 C11 C12 C13 83.1(4) . . . . ? C10 C11 C15 C16 0.1(5) . . . . ? C12 C11 C15 C16 179.1(3) . . . . ? C11 C15 C16 C17 1.6(6) . . . . ? C15 C16 C17 C18 -1.6(6) . . . . ? C16 C17 C18 C10 -0.1(5) . . . . ? C16 C17 C18 C19 176.0(3) . . . . ? O1 C10 C18 C17 -177.6(3) . . . . ? C11 C10 C18 C17 1.9(5) . . . . ? O1 C10 C18 C19 6.2(4) . . . . ? C11 C10 C18 C19 -174.4(3) . . . . ? C17 C18 C19 C111 -103.4(4) . . . . ? C10 C18 C19 C111 72.6(4) . . . . ? C17 C18 C19 C110 21.6(5) . . . . ? C10 C18 C19 C110 -162.4(3) . . . . ? Zr1 O2 C20 C21 -99.3(10) . . . . ? Zr1 O2 C20 C28 81.3(11) . . . . ? O2 C20 C21 C25 179.6(3) . . . . ? C28 C20 C21 C25 -1.0(4) . . . . ? O2 C20 C21 C22 -3.9(4) . . . . ? C28 C20 C21 C22 175.5(3) . . . . ? C25 C21 C22 C23 -29.9(4) . . . . ? C20 C21 C22 C23 153.8(3) . . . . ? C25 C21 C22 C24 94.4(4) . . . . ? C20 C21 C22 C24 -81.9(3) . . . . ? C20 C21 C25 C26 0.9(5) . . . . ? C22 C21 C25 C26 -175.6(3) . . . . ? C21 C25 C26 C27 0.0(5) . . . . ? C25 C26 C27 C28 -0.7(5) . . . . ? C26 C27 C28 C20 0.5(4) . . . . ? C26 C27 C28 C29 179.0(3) . . . . ? O2 C20 C28 C27 179.7(3) . . . . ? C21 C20 C28 C27 0.4(4) . . . . ? O2 C20 C28 C29 1.2(4) . . . . ? C21 C20 C28 C29 -178.1(3) . . . . ? C27 C28 C29 C210 -75.1(4) . . . . ? C20 C28 C29 C210 103.4(3) . . . . ? C27 C28 C29 C211 49.6(4) . . . . ? C20 C28 C29 C211 -132.0(3) . . . . ? Zr2 O3 C30 C38 -45(2) . . . . ? Zr2 O3 C30 C31 134.1(18) . . . . ? O3 C30 C31 C35 -178.6(3) . . . . ? C38 C30 C31 C35 0.0(5) . . . . ? O3 C30 C31 C32 -0.8(5) . . . . ? C38 C30 C31 C32 177.9(3) . . . . ? C35 C31 C32 C33 93.4(4) . . . . ? C30 C31 C32 C33 -84.3(4) . . . . ? C35 C31 C32 C34 -31.3(5) . . . . ? C30 C31 C32 C34 151.0(4) . . . . ? C30 C31 C35 C36 -0.1(6) . . . . ? C32 C31 C35 C36 -177.9(4) . . . . ? C31 C35 C36 C37 0.1(7) . . . . ? C35 C36 C37 C38 0.1(7) . . . . ? O3 C30 C38 C37 178.8(3) . . . . ? C31 C30 C38 C37 0.1(5) . . . . ? O3 C30 C38 C39 -1.3(5) . . . . ? C31 C30 C38 C39 -180.0(3) . . . . ? C36 C37 C38 C30 -0.1(6) . . . . ? C36 C37 C38 C39 179.9(4) . . . . ? C30 C38 C39 C311 159.1(3) . . . . ? C37 C38 C39 C311 -21.0(5) . . . . ? C30 C38 C39 C310 -75.5(4) . . . . ? C37 C38 C39 C310 104.5(4) . . . . ? Zr2 O4 C40 C41 109.1(10) . . . . ? Zr2 O4 C40 C48 -71.6(11) . . . . ? O4 C40 C41 C45 -179.6(3) . . . . ? C48 C40 C41 C45 1.1(5) . . . . ? O4 C40 C41 C42 2.4(4) . . . . ? C48 C40 C41 C42 -177.0(3) . . . . ? C45 C41 C42 C44 -94.6(4) . . . . ? C40 C41 C42 C44 83.4(4) . . . . ? C45 C41 C42 C43 30.9(5) . . . . ? C40 C41 C42 C43 -151.1(3) . . . . ? C40 C41 C45 C46 -0.4(5) . . . . ? C42 C41 C45 C46 177.6(3) . . . . ? C41 C45 C46 C47 -0.7(5) . . . . ? C45 C46 C47 C48 1.1(5) . . . . ? C46 C47 C48 C40 -0.4(5) . . . . ? C46 C47 C48 C49 -179.1(3) . . . . ? O4 C40 C48 C47 180.0(3) . . . . ? C41 C40 C48 C47 -0.7(5) . . . . ? O4 C40 C48 C49 -1.4(4) . . . . ? C41 C40 C48 C49 178.0(3) . . . . ? C47 C48 C49 C410 -49.5(4) . . . . ? C40 C48 C49 C410 131.9(3) . . . . ? C47 C48 C49 C411 75.4(4) . . . . ? C40 C48 C49 C411 -103.3(3) . . . . ? Zr2 O5 C50 C55 -83.0(3) . . . . ? Zr1 O5 C50 C55 145.3(2) . . . . ? Zr2 O5 C50 C51 95.9(3) . . . . ? Zr1 O5 C50 C51 -35.8(3) . . . . ? O5 C50 C51 C52 177.1(2) . . . . ? C55 C50 C51 C52 -4.0(4) . . . . ? O5 C50 C51 S1 -4.4(4) . . . . ? C55 C50 C51 S1 174.5(2) . . . . ? C61 S1 C51 C52 76.4(2) . . . . ? Zr1 S1 C51 C52 -153.6(2) . . . . ? C61 S1 C51 C50 -102.1(2) . . . . ? Zr1 S1 C51 C50 27.9(2) . . . . ? C50 C51 C52 C53 4.1(4) . . . . ? S1 C51 C52 C53 -174.4(2) . . . . ? C51 C52 C53 C54 -1.7(4) . . . . ? C51 C52 C53 C56 -174.4(3) . . . . ? C52 C53 C54 C55 -0.7(4) . . . . ? C56 C53 C54 C55 172.0(3) . . . . ? O5 C50 C55 C54 -179.5(3) . . . . ? C51 C50 C55 C54 1.7(4) . . . . ? C53 C54 C55 C50 0.6(5) . . . . ? C52 C53 C56 C57 -169.2(3) . . . . ? C54 C53 C56 C57 18.3(4) . . . . ? C52 C53 C56 C58 75.0(4) . . . . ? C54 C53 C56 C58 -97.4(3) . . . . ? C52 C53 C56 C59 -41.2(4) . . . . ? C54 C53 C56 C59 146.4(3) . . . . ? C57 C56 C59 C510 62.1(4) . . . . ? C53 C56 C59 C510 -65.8(4) . . . . ? C58 C56 C59 C510 178.9(3) . . . . ? C56 C59 C510 C513 59.2(4) . . . . ? C56 C59 C510 C511 -65.0(4) . . . . ? C56 C59 C510 C512 177.8(3) . . . . ? Zr2 O6 C60 C65 -145.7(6) . . . . ? Zr2 O6 C60 C61 36.2(9) . . . . ? O6 C60 C61 C62 178.5(3) . . . . ? C65 C60 C61 C62 0.3(4) . . . . ? O6 C60 C61 S1 3.2(4) . . . . ? C65 C60 C61 S1 -174.9(2) . . . . ? C51 S1 C61 C62 -113.3(2) . . . . ? Zr1 S1 C61 C62 146.09(18) . . . . ? C51 S1 C61 C60 62.1(3) . . . . ? Zr1 S1 C61 C60 -38.5(3) . . . . ? C60 C61 C62 C63 -0.1(4) . . . . ? S1 C61 C62 C63 175.4(2) . . . . ? C61 C62 C63 C64 -0.1(4) . . . . ? C61 C62 C63 C66 -177.2(3) . . . . ? C62 C63 C64 C65 0.1(4) . . . . ? C66 C63 C64 C65 177.2(3) . . . . ? C63 C64 C65 C60 0.2(5) . . . . ? O6 C60 C65 C64 -178.5(3) . . . . ? C61 C60 C65 C64 -0.3(4) . . . . ? C62 C63 C66 C67 4.9(4) . . . . ? C64 C63 C66 C67 -172.1(3) . . . . ? C62 C63 C66 C68 121.5(3) . . . . ? C64 C63 C66 C68 -55.6(4) . . . . ? C62 C63 C66 C69 -122.2(3) . . . . ? C64 C63 C66 C69 60.8(4) . . . . ? C63 C66 C69 C610 55.4(4) . . . . ? C67 C66 C69 C610 -72.0(4) . . . . ? C68 C66 C69 C610 173.0(3) . . . . ? C66 C69 C610 C613 -72.8(4) . . . . ? C66 C69 C610 C611 50.5(4) . . . . ? C66 C69 C610 C612 169.5(3) . . . . ? Zr1 O7 C70 C75 83.4(3) . . . . ? Zr2 O7 C70 C75 -145.6(2) . . . . ? Zr1 O7 C70 C71 -96.4(3) . . . . ? Zr2 O7 C70 C71 34.6(3) . . . . ? O7 C70 C71 C72 -176.4(2) . . . . ? C75 C70 C71 C72 3.8(4) . . . . ? O7 C70 C71 S2 5.2(4) . . . . ? C75 C70 C71 S2 -174.6(2) . . . . ? C81 S2 C71 C72 -77.0(3) . . . . ? Zr2 S2 C71 C72 153.5(2) . . . . ? C81 S2 C71 C70 101.4(2) . . . . ? Zr2 S2 C71 C70 -28.0(2) . . . . ? C70 C71 C72 C73 -4.1(4) . . . . ? S2 C71 C72 C73 174.3(2) . . . . ? C71 C72 C73 C74 1.5(4) . . . . ? C71 C72 C73 C76 175.7(3) . . . . ? C72 C73 C74 C75 1.5(4) . . . . ? C76 C73 C74 C75 -172.6(3) . . . . ? O7 C70 C75 C74 179.2(3) . . . . ? C71 C70 C75 C74 -0.9(4) . . . . ? C73 C74 C75 C70 -1.7(5) . . . . ? C72 C73 C76 C77 170.0(3) . . . . ? C74 C73 C76 C77 -16.1(5) . . . . ? C72 C73 C76 C78 -73.9(4) . . . . ? C74 C73 C76 C78 100.0(4) . . . . ? C72 C73 C76 C79 42.3(4) . . . . ? C74 C73 C76 C79 -143.8(3) . . . . ? C73 C76 C79 C710 62.7(4) . . . . ? C77 C76 C79 C710 -64.9(4) . . . . ? C78 C76 C79 C710 179.1(3) . . . . ? C76 C79 C710 C713 -64.9(4) . . . . ? C76 C79 C710 C711 59.2(5) . . . . ? C76 C79 C710 C712 177.8(3) . . . . ? Zr1 O8 C80 C85 143.5(7) . . . . ? Zr1 O8 C80 C81 -37.3(10) . . . . ? O8 C80 C81 C82 179.4(3) . . . . ? C85 C80 C81 C82 -1.4(4) . . . . ? O8 C80 C81 S2 -4.2(4) . . . . ? C85 C80 C81 S2 175.0(2) . . . . ? C71 S2 C81 C82 115.1(2) . . . . ? Zr2 S2 C81 C82 -144.27(18) . . . . ? C71 S2 C81 C80 -61.4(3) . . . . ? Zr2 S2 C81 C80 39.2(3) . . . . ? C80 C81 C82 C83 0.1(4) . . . . ? S2 C81 C82 C83 -176.4(2) . . . . ? C81 C82 C83 C84 1.5(4) . . . . ? C81 C82 C83 C86 177.2(3) . . . . ? C82 C83 C84 C85 -1.9(4) . . . . ? C86 C83 C84 C85 -177.8(3) . . . . ? C83 C84 C85 C80 0.7(5) . . . . ? O8 C80 C85 C84 -179.8(3) . . . . ? C81 C80 C85 C84 1.0(4) . . . . ? C82 C83 C86 C88 5.9(4) . . . . ? C84 C83 C86 C88 -178.4(3) . . . . ? C82 C83 C86 C87 -111.0(3) . . . . ? C84 C83 C86 C87 64.6(4) . . . . ? C82 C83 C86 C89 134.6(3) . . . . ? C84 C83 C86 C89 -49.8(4) . . . . ? C88 C86 C89 C810 62.9(4) . . . . ? C83 C86 C89 C810 -65.8(4) . . . . ? C87 C86 C89 C810 178.5(3) . . . . ? C86 C89 C810 C811 52.4(5) . . . . ? C86 C89 C810 C812 -89.3(5) . . . . ? C86 C89 C810 C815 -169.9(6) . . . . ? C86 C89 C810 C813 -48.4(8) . . . . ? C86 C89 C810 C814 161.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.940 _refine_diff_density_min -0.684 _refine_diff_density_rms 0.061