# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Sciences' _journal_coden_Cambridge 1475 _publ_contact_author_name 'McInnes, Eric' _publ_contact_author_email eric.mcinnes@manchester.ac.uk _publ_section_title ; Low-valent vanadium catecholate clusters ; _publ_author_name E.McInnes # Attachment 'complex-1new.cif.txt' data_test2pb1a _database_code_depnum_ccdc_archive 'CCDC 762899' #TrackingRef 'complex-1new.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H128 O23 V6' _chemical_formula_weight 1643.36 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.232(2) _cell_length_b 13.693(3) _cell_length_c 14.106(3) _cell_angle_alpha 96.27(3) _cell_angle_beta 91.40(3) _cell_angle_gamma 90.45(3) _cell_volume 2155.9(7) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 10272 _cell_measurement_theta_min 7.660 _cell_measurement_theta_max 65.999 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 870 _exptl_absorpt_coefficient_mu 0.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8202 _exptl_absorpt_correction_T_max 0.9344 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.79770 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SMX station 16.2' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method 'w/ rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27728 _diffrn_reflns_av_R_equivalents 0.0717 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.83 _diffrn_reflns_theta_max 27.98 _reflns_number_total 7070 _reflns_number_gt 6648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SAINT' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; The structure was solved by direct methods.Data processing was carried out to 0.85 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions except for the alcohol protons of the methanol group O6, and O1S and C1S of solvent methanol molecules. All non-hydrogen atomswere resolved anisotropically. The methyls of the tert-butyl group C12 > C14 were split over two sites. Displacement and geometric restraints have been applied to the split atoms anisotropic thermal parameters. C14X has high maximum to minimum displacement parameter ratios (although this is below 10:1). The parameter ratios for C12Y and C13Y are also a little high (although these are also below 10:1). As no further chemical information would be obtained by splitting these further it was decided to leave them as they are (displacement and geometrical restraints applied). 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^)+(0.1057P)^2^+2.2814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7070 _refine_ls_number_parameters 506 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0550 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.041 _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 V1 V 0.32999(4) 0.54475(3) 0.44509(3) 0.01474(15) Uani 1 1 d . . . V2 V 0.41886(4) 0.36249(3) 0.53577(3) 0.01383(15) Uani 1 1 d . . . V3 V 0.45910(4) 0.57131(3) 0.64348(3) 0.01415(15) Uani 1 1 d . . . O1 O 0.5000 0.5000 0.5000 0.0143(5) Uani 1 2 d S . . O2 O 0.27029(15) 0.42161(13) 0.48814(12) 0.0181(4) Uani 1 1 d . . . O3 O 0.31374(16) 0.61022(13) 0.57501(13) 0.0183(4) Uani 1 1 d . . . O4 O 0.41866(16) 0.66058(13) 0.41178(12) 0.0172(4) Uani 1 1 d . . . O5 O 0.37835(16) 0.47273(13) 0.32523(12) 0.0170(4) Uani 1 1 d . . . O6 O 0.16376(18) 0.57726(15) 0.39462(15) 0.0279(5) Uani 1 1 d . . . O7 O 0.46039(16) 0.30981(13) 0.40432(12) 0.0173(4) Uani 1 1 d . . . O8 O 0.35578(16) 0.23367(13) 0.54082(13) 0.0201(4) Uani 1 1 d . . . O9 O 0.38818(16) 0.44242(12) 0.66296(12) 0.0163(4) Uani 1 1 d . . . O10 O 0.40944(17) 0.60601(13) 0.77128(12) 0.0205(4) Uani 1 1 d . . . C1 C 0.4130(2) 0.21772(18) 0.37986(18) 0.0176(5) Uani 1 1 d . . . C2 C 0.3571(2) 0.17707(18) 0.45578(18) 0.0187(5) Uani 1 1 d . . . C3 C 0.3079(2) 0.0816(2) 0.4395(2) 0.0234(6) Uani 1 1 d . . . C4 C 0.3148(3) 0.0339(2) 0.3468(2) 0.0287(6) Uani 1 1 d . . . H4 H 0.2824 -0.0291 0.3349 0.034 Uiso 1 1 calc R . . C5 C 0.3671(3) 0.0747(2) 0.2712(2) 0.0302(7) Uani 1 1 d . A . C6 C 0.4181(3) 0.1686(2) 0.2898(2) 0.0247(6) Uani 1 1 d . . . H6 H 0.4552 0.1976 0.2415 0.030 Uiso 1 1 calc R . . C7 C 0.2514(3) 0.0334(2) 0.5211(2) 0.0288(6) Uani 1 1 d . . . C8 C 0.1490(3) 0.0957(2) 0.5635(3) 0.0379(8) Uani 1 1 d . . . H8B H 0.1795 0.1584 0.5911 0.057 Uiso 1 1 calc R . . H8C H 0.1120 0.0626 0.6119 0.057 Uiso 1 1 calc R . . H8A H 0.0912 0.1050 0.5141 0.057 Uiso 1 1 calc R . . C9 C 0.3475(3) 0.0221(3) 0.5982(2) 0.0388(8) Uani 1 1 d . . . H9A H 0.4107 -0.0179 0.5712 0.058 Uiso 1 1 calc R . . H9C H 0.3133 -0.0087 0.6493 0.058 Uiso 1 1 calc R . . H9B H 0.3787 0.0856 0.6224 0.058 Uiso 1 1 calc R . . C10 C 0.2009(3) -0.0696(2) 0.4861(3) 0.0432(8) Uani 1 1 d . . . H10A H 0.1421 -0.0645 0.4364 0.065 Uiso 1 1 calc R . . H10C H 0.1649 -0.0973 0.5383 0.065 Uiso 1 1 calc R . . H10B H 0.2642 -0.1111 0.4619 0.065 Uiso 1 1 calc R . . C11 C 0.3700(4) 0.0173(2) 0.1716(2) 0.0419(8) Uani 1 1 d . . . C12X C 0.4152(10) 0.0811(5) 0.0940(4) 0.068(2) Uani 0.655(6) 1 d PU A 1 H12A H 0.3990 0.0472 0.0317 0.101 Uiso 0.655(6) 1 calc PR A 1 H12C H 0.4994 0.0924 0.1028 0.101 Uiso 0.655(6) 1 calc PR A 1 H12B H 0.3748 0.1430 0.0997 0.101 Uiso 0.655(6) 1 calc PR A 1 C13X C 0.2382(8) -0.0065(7) 0.1328(5) 0.081(2) Uani 0.655(6) 1 d PU A 1 H13A H 0.1961 0.0538 0.1290 0.122 Uiso 0.655(6) 1 calc PR A 1 H13C H 0.1981 -0.0452 0.1754 0.122 Uiso 0.655(6) 1 calc PR A 1 H13B H 0.2404 -0.0425 0.0706 0.122 Uiso 0.655(6) 1 calc PR A 1 C14X C 0.4392(8) -0.0714(5) 0.1702(4) 0.066(2) Uani 0.655(6) 1 d PU A 1 H14A H 0.4455 -0.1009 0.1056 0.099 Uiso 0.655(6) 1 calc PR A 1 H14B H 0.4006 -0.1166 0.2072 0.099 Uiso 0.655(6) 1 calc PR A 1 H14C H 0.5173 -0.0556 0.1968 0.099 Uiso 0.655(6) 1 calc PR A 1 C12Y C 0.3276(17) 0.0740(10) 0.1041(8) 0.059(3) Uani 0.345(6) 1 d PU A 2 H12E H 0.3333 0.0384 0.0419 0.088 Uiso 0.345(6) 1 calc PR A 2 H12F H 0.3740 0.1335 0.1070 0.088 Uiso 0.345(6) 1 calc PR A 2 H12D H 0.2458 0.0899 0.1162 0.088 Uiso 0.345(6) 1 calc PR A 2 C13Y C 0.2850(18) -0.0755(12) 0.1695(10) 0.084(4) Uani 0.345(6) 1 d PU A 2 H13D H 0.2118 -0.0565 0.1998 0.126 Uiso 0.345(6) 1 calc PR A 2 H13F H 0.3231 -0.1246 0.2029 0.126 Uiso 0.345(6) 1 calc PR A 2 H13E H 0.2685 -0.1016 0.1045 0.126 Uiso 0.345(6) 1 calc PR A 2 C14Y C 0.5183(17) 0.0068(13) 0.1524(9) 0.089(4) Uani 0.345(6) 1 d PU A 2 H14D H 0.5310 -0.0078 0.0853 0.134 Uiso 0.345(6) 1 calc PR A 2 H14E H 0.5498 -0.0452 0.1857 0.134 Uiso 0.345(6) 1 calc PR A 2 H14F H 0.5580 0.0675 0.1754 0.134 Uiso 0.345(6) 1 calc PR A 2 C15 C 0.3401(2) 0.44177(19) 0.75146(16) 0.0159(5) Uani 1 1 d . . . C16 C 0.3532(2) 0.53182(18) 0.80988(17) 0.0164(5) Uani 1 1 d . . . C17 C 0.3084(2) 0.53962(19) 0.90256(18) 0.0195(5) Uani 1 1 d . . . C18 C 0.2504(2) 0.4568(2) 0.93014(18) 0.0216(6) Uani 1 1 d . . . H18 H 0.2198 0.4611 0.9911 0.026 Uiso 1 1 calc R . . C19 C 0.2354(2) 0.3681(2) 0.87175(18) 0.0206(6) Uani 1 1 d . . . C20 C 0.2830(2) 0.36181(19) 0.78047(18) 0.0192(5) Uani 1 1 d . . . H20 H 0.2759 0.3038 0.7398 0.023 Uiso 1 1 calc R . . C21 C 0.3245(3) 0.6357(2) 0.96964(19) 0.0250(6) Uani 1 1 d . . . C24 C 0.4575(3) 0.6577(2) 0.9871(2) 0.0350(7) Uani 1 1 d . . . H24B H 0.4941 0.6045 1.0155 0.053 Uiso 1 1 calc R . . H24C H 0.4677 0.7174 1.0292 0.053 Uiso 1 1 calc R . . H24A H 0.4941 0.6652 0.9275 0.053 Uiso 1 1 calc R . . C23 C 0.2645(3) 0.7212(2) 0.9252(2) 0.0361(7) Uani 1 1 d . . . H23A H 0.2973 0.7271 0.8639 0.054 Uiso 1 1 calc R . . H23C H 0.2784 0.7812 0.9661 0.054 Uiso 1 1 calc R . . H23B H 0.1804 0.7087 0.9180 0.054 Uiso 1 1 calc R . . C22 C 0.2690(4) 0.6278(3) 1.0668(2) 0.0429(8) Uani 1 1 d . . . H22A H 0.1858 0.6119 1.0578 0.064 Uiso 1 1 calc R . . H22C H 0.2783 0.6894 1.1059 0.064 Uiso 1 1 calc R . . H22B H 0.3081 0.5772 1.0974 0.064 Uiso 1 1 calc R . . C25 C 0.1707(3) 0.2783(2) 0.9037(2) 0.0273(6) Uani 1 1 d . . . C26 C 0.1370(4) 0.2933(3) 1.0087(2) 0.0528(10) Uani 1 1 d . . . H26C H 0.2074 0.3081 1.0478 0.079 Uiso 1 1 calc R . . H26A H 0.1003 0.2343 1.0259 0.079 Uiso 1 1 calc R . . H26B H 0.0822 0.3467 1.0184 0.079 Uiso 1 1 calc R . . C27 C 0.0573(3) 0.2563(3) 0.8418(3) 0.0423(8) Uani 1 1 d . . . H27B H 0.0181 0.1991 0.8604 0.063 Uiso 1 1 calc R . . H27A H 0.0780 0.2448 0.7760 0.063 Uiso 1 1 calc R . . H27C H 0.0048 0.3114 0.8504 0.063 Uiso 1 1 calc R . . C28 C 0.2512(3) 0.1878(2) 0.8895(3) 0.0407(8) Uani 1 1 d . . . H28C H 0.3219 0.1991 0.9289 0.061 Uiso 1 1 calc R . . H28A H 0.2726 0.1765 0.8238 0.061 Uiso 1 1 calc R . . H28B H 0.2092 0.1314 0.9070 0.061 Uiso 1 1 calc R . . C29 C 0.1620(2) 0.4116(2) 0.5376(2) 0.0254(6) Uani 1 1 d . . . H29C H 0.1653 0.4536 0.5968 0.038 Uiso 1 1 calc R . . H29B H 0.1520 0.3446 0.5503 0.038 Uiso 1 1 calc R . . H29A H 0.0960 0.4300 0.4991 0.038 Uiso 1 1 calc R . . C30 C 0.2590(3) 0.7023(2) 0.6019(2) 0.0334(7) Uani 1 1 d . . . H30B H 0.2966 0.7523 0.5701 0.050 Uiso 1 1 calc R . . H30C H 0.2676 0.7185 0.6697 0.050 Uiso 1 1 calc R . . H30A H 0.1759 0.6980 0.5840 0.050 Uiso 1 1 calc R . . C33 C 0.4102(3) 0.7052(2) 0.3247(2) 0.0265(6) Uani 1 1 d . . . H33A H 0.4140 0.6554 0.2715 0.040 Uiso 1 1 calc R . . H33C H 0.4750 0.7510 0.3225 0.040 Uiso 1 1 calc R . . H33B H 0.3361 0.7392 0.3218 0.040 Uiso 1 1 calc R . . C31 C 0.3077(3) 0.4224(2) 0.2496(2) 0.0284(6) Uani 1 1 d . . . H31A H 0.2733 0.3644 0.2706 0.043 Uiso 1 1 calc R . . H31B H 0.3569 0.4043 0.1959 0.043 Uiso 1 1 calc R . . H31C H 0.2454 0.4647 0.2313 0.043 Uiso 1 1 calc R . . C32 C 0.1152(3) 0.6660(3) 0.3683(4) 0.0571(11) Uani 1 1 d . . . H32C H 0.1556 0.7209 0.4036 0.086 Uiso 1 1 calc R . . H32B H 0.0319 0.6683 0.3821 0.086 Uiso 1 1 calc R . . H32A H 0.1251 0.6690 0.3012 0.086 Uiso 1 1 calc R . . O1S O 0.0962(3) 0.2397(3) 0.3388(4) 0.1021(15) Uani 1 1 d . B 1 H1S H 0.1679 0.2307 0.3331 0.153 Uiso 1 1 calc R B 1 C1S C 0.0357(5) 0.1648(4) 0.2904(5) 0.0889(17) Uani 1 1 d . . . H1SC H 0.0249 0.1135 0.3307 0.133 Uiso 1 1 calc R B 1 H1SA H 0.0795 0.1400 0.2355 0.133 Uiso 1 1 calc R B 1 H1SB H -0.0406 0.1873 0.2703 0.133 Uiso 1 1 calc R B 1 O2S O 1.0255(2) 0.43215(19) 0.32719(17) 0.0409(6) Uani 1 1 d D . . C2S C 0.9633(4) 0.4335(4) 0.2390(3) 0.0588(11) Uani 1 1 d . . . H2SC H 0.9489 0.5003 0.2276 0.088 Uiso 1 1 calc R . . H2SA H 0.8886 0.3992 0.2409 0.088 Uiso 1 1 calc R . . H2SB H 1.0100 0.4019 0.1887 0.088 Uiso 1 1 calc R . . H2S H 1.061(4) 0.370(2) 0.323(4) 0.073(15) Uiso 1 1 d D . . H6W H 0.121(4) 0.525(4) 0.367(3) 0.066(14) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0196(3) 0.0140(2) 0.0105(2) 0.00000(17) 0.00271(17) -0.00106(17) V2 0.0201(3) 0.0115(2) 0.0093(2) -0.00165(17) 0.00307(17) -0.00185(17) V3 0.0201(3) 0.0135(2) 0.0086(2) -0.00032(17) 0.00395(17) -0.00202(17) O1 0.0174(12) 0.0147(12) 0.0104(12) -0.0010(9) 0.0027(9) -0.0027(10) O2 0.0198(9) 0.0204(9) 0.0140(9) 0.0010(7) 0.0035(7) -0.0044(7) O3 0.0220(9) 0.0164(9) 0.0157(9) -0.0023(7) 0.0058(7) 0.0022(7) O4 0.0232(9) 0.0161(9) 0.0131(9) 0.0044(7) 0.0033(7) -0.0002(7) O5 0.0236(9) 0.0173(9) 0.0094(8) -0.0012(7) -0.0011(7) -0.0022(7) O6 0.0272(10) 0.0251(11) 0.0307(11) 0.0011(9) -0.0084(8) 0.0048(8) O7 0.0265(9) 0.0132(9) 0.0114(9) -0.0026(7) 0.0048(7) -0.0034(7) O8 0.0291(10) 0.0155(9) 0.0150(9) -0.0016(7) 0.0054(7) -0.0054(7) O9 0.0244(9) 0.0146(9) 0.0096(8) -0.0006(7) 0.0064(7) -0.0033(7) O10 0.0306(10) 0.0177(9) 0.0124(9) -0.0023(7) 0.0064(7) -0.0037(8) C1 0.0249(13) 0.0117(12) 0.0158(13) -0.0011(10) 0.0009(10) -0.0019(10) C2 0.0245(13) 0.0159(12) 0.0149(13) -0.0015(10) 0.0002(10) 0.0013(10) C3 0.0255(14) 0.0186(13) 0.0258(15) 0.0013(11) 0.0007(11) -0.0030(11) C4 0.0407(17) 0.0138(13) 0.0300(16) -0.0046(11) -0.0001(13) -0.0064(12) C5 0.0463(18) 0.0202(14) 0.0226(15) -0.0049(12) 0.0002(13) -0.0004(12) C6 0.0357(15) 0.0198(14) 0.0188(14) 0.0012(11) 0.0059(11) -0.0009(11) C7 0.0332(15) 0.0221(14) 0.0316(16) 0.0046(12) 0.0043(12) -0.0060(12) C8 0.0388(18) 0.0337(17) 0.0424(19) 0.0062(14) 0.0155(14) -0.0067(14) C9 0.0448(18) 0.0375(18) 0.0374(18) 0.0191(14) 0.0011(14) -0.0076(14) C10 0.054(2) 0.0272(17) 0.049(2) 0.0080(15) 0.0085(16) -0.0152(15) C11 0.075(2) 0.0268(16) 0.0217(16) -0.0076(13) 0.0032(15) 0.0010(16) C12X 0.135(7) 0.045(3) 0.021(3) -0.007(2) 0.003(4) 0.005(4) C13X 0.105(5) 0.089(5) 0.040(3) -0.033(3) -0.013(3) 0.001(4) C14X 0.136(7) 0.046(3) 0.013(2) -0.011(2) 0.004(3) 0.057(4) C12Y 0.103(7) 0.055(5) 0.014(4) -0.011(4) -0.009(5) 0.007(6) C13Y 0.139(8) 0.070(7) 0.035(6) -0.025(5) -0.006(6) -0.025(7) C14Y 0.144(9) 0.081(7) 0.035(5) -0.028(5) -0.003(6) 0.060(7) C15 0.0198(12) 0.0214(13) 0.0062(11) 0.0004(9) 0.0040(9) 0.0010(10) C16 0.0187(12) 0.0174(12) 0.0133(12) 0.0021(10) 0.0018(9) -0.0017(10) C17 0.0225(13) 0.0228(14) 0.0126(12) -0.0010(10) 0.0010(10) 0.0024(10) C18 0.0257(14) 0.0290(14) 0.0104(12) 0.0029(10) 0.0053(10) 0.0001(11) C19 0.0214(13) 0.0258(14) 0.0156(13) 0.0058(11) 0.0031(10) -0.0003(11) C20 0.0241(13) 0.0200(13) 0.0132(12) 0.0009(10) 0.0008(10) -0.0010(10) C21 0.0326(15) 0.0273(15) 0.0138(13) -0.0052(11) 0.0041(11) 0.0003(12) C24 0.0355(17) 0.0382(17) 0.0275(16) -0.0133(13) -0.0029(13) -0.0024(13) C23 0.0493(19) 0.0299(16) 0.0261(16) -0.0108(13) 0.0008(13) 0.0091(14) C22 0.065(2) 0.0442(19) 0.0168(15) -0.0124(13) 0.0127(14) -0.0067(17) C25 0.0319(15) 0.0319(15) 0.0189(14) 0.0069(12) 0.0048(11) -0.0064(12) C26 0.076(3) 0.055(2) 0.0285(19) 0.0087(16) 0.0183(18) -0.024(2) C27 0.0336(17) 0.049(2) 0.046(2) 0.0142(16) 0.0007(15) -0.0135(15) C28 0.048(2) 0.0348(17) 0.043(2) 0.0198(15) 0.0050(15) -0.0035(15) C29 0.0179(13) 0.0350(16) 0.0245(14) 0.0077(12) 0.0053(11) -0.0035(11) C30 0.0427(18) 0.0264(15) 0.0298(16) -0.0047(12) 0.0037(13) 0.0173(13) C33 0.0285(14) 0.0325(15) 0.0208(14) 0.0137(12) 0.0001(11) 0.0003(12) C31 0.0283(15) 0.0352(16) 0.0184(14) -0.0101(12) -0.0038(11) -0.0005(12) C32 0.0314(18) 0.046(2) 0.100(3) 0.037(2) -0.0037(19) 0.0048(16) O1S 0.062(2) 0.072(2) 0.174(4) 0.031(3) -0.043(2) -0.0054(18) C1S 0.091(4) 0.076(4) 0.095(4) -0.009(3) -0.005(3) 0.019(3) O2S 0.0295(11) 0.0478(14) 0.0419(14) -0.0087(11) -0.0065(10) -0.0018(10) C2S 0.049(2) 0.078(3) 0.043(2) -0.019(2) -0.0157(18) 0.012(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 V1 O5 1.9533(18) . ? V1 O3 1.9637(19) . ? V1 O2 1.9716(19) . ? V1 O4 1.9720(19) . ? V1 O6 2.051(2) . ? V1 O1 2.1614(7) . ? V1 V3 3.0770(11) 2_666 ? V1 V2 3.0782(10) 2_666 ? V2 O8 1.9050(18) . ? V2 O7 1.9829(18) . ? V2 O4 1.9929(19) 2_666 ? V2 O2 1.9942(19) . ? V2 O9 2.0355(18) . ? V2 O1 2.1985(7) . ? V2 V1 3.0783(10) 2_666 ? V3 O10 1.9113(18) . ? V3 O9 1.9797(18) . ? V3 O5 1.9819(19) 2_666 ? V3 O3 1.9829(19) . ? V3 O7 2.0418(19) 2_666 ? V3 O1 2.2095(7) . ? V3 V1 3.0771(11) 2_666 ? O1 V1 2.1615(7) 2_666 ? O1 V2 2.1985(7) 2_666 ? O1 V3 2.2094(7) 2_666 ? O2 C29 1.430(3) . ? O3 C30 1.425(3) . ? O4 C33 1.432(3) . ? O4 V2 1.9930(19) 2_666 ? O5 C31 1.425(3) . ? O5 V3 1.9819(19) 2_666 ? O6 C32 1.419(4) . ? O6 H6W 0.91(5) . ? O7 C1 1.370(3) . ? O7 V3 2.0417(19) 2_666 ? O8 C2 1.356(3) . ? O9 C15 1.373(3) . ? O10 C16 1.362(3) . ? C1 C6 1.374(4) . ? C1 C2 1.417(4) . ? C2 C3 1.408(4) . ? C3 C4 1.400(4) . ? C3 C7 1.536(4) . ? C4 C5 1.396(4) . ? C4 H4 0.9300 . ? C5 C6 1.400(4) . ? C5 C11 1.534(4) . ? C6 H6 0.9300 . ? C7 C8 1.532(4) . ? C7 C9 1.535(4) . ? C7 C10 1.542(4) . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C8 H8A 0.9600 . ? C9 H9A 0.9600 . ? C9 H9C 0.9600 . ? C9 H9B 0.9600 . ? C10 H10A 0.9600 . ? C10 H10C 0.9600 . ? C10 H10B 0.9600 . ? C11 C12Y 1.372(13) . ? C11 C14X 1.445(6) . ? C11 C12X 1.566(8) . ? C11 C13Y 1.580(16) . ? C11 C13X 1.585(9) . ? C11 C14Y 1.699(19) . ? C12X H12A 0.9600 . ? C12X H12C 0.9600 . ? C12X H12B 0.9600 . ? C13X H13A 0.9600 . ? C13X H13C 0.9600 . ? C13X H13B 0.9600 . ? C14X H14A 0.9600 . ? C14X H14B 0.9600 . ? C14X H14C 0.9600 . ? C12Y H12E 0.9600 . ? C12Y H12F 0.9600 . ? C12Y H12D 0.9600 . ? C13Y H13D 0.9600 . ? C13Y H13F 0.9600 . ? C13Y H13E 0.9600 . ? C14Y H14D 0.9600 . ? C14Y H14E 0.9600 . ? C14Y H14F 0.9600 . ? C15 C20 1.370(4) . ? C15 C16 1.411(4) . ? C16 C17 1.406(4) . ? C17 C18 1.399(4) . ? C17 C21 1.541(4) . ? C18 C19 1.399(4) . ? C18 H18 0.9300 . ? C19 C20 1.400(4) . ? C19 C25 1.538(4) . ? C20 H20 0.9300 . ? C21 C24 1.531(4) . ? C21 C22 1.533(4) . ? C21 C23 1.540(4) . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24 H24A 0.9600 . ? C23 H23A 0.9600 . ? C23 H23C 0.9600 . ? C23 H23B 0.9600 . ? C22 H22A 0.9600 . ? C22 H22C 0.9600 . ? C22 H22B 0.9600 . ? C25 C26 1.530(4) . ? C25 C27 1.536(4) . ? C25 C28 1.538(5) . ? C26 H26C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C27 H27B 0.9600 . ? C27 H27A 0.9600 . ? C27 H27C 0.9600 . ? C28 H28C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C29 H29C 0.9600 . ? C29 H29B 0.9600 . ? C29 H29A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C30 H30A 0.9600 . ? C33 H33A 0.9600 . ? C33 H33C 0.9600 . ? C33 H33B 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32C 0.9600 . ? C32 H32B 0.9600 . ? C32 H32A 0.9600 . ? O1S C1S 1.339(7) . ? O1S H1S 0.8200 . ? C1S H1SC 0.9600 . ? C1S H1SA 0.9600 . ? C1S H1SB 0.9600 . ? O2S C2S 1.414(4) . ? O2S H2S 0.941(19) . ? C2S H2SC 0.9600 . ? C2S H2SA 0.9600 . ? C2S H2SB 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 V1 O3 168.32(8) . . ? O5 V1 O2 90.11(8) . . ? O3 V1 O2 89.46(8) . . ? O5 V1 O4 89.08(8) . . ? O3 V1 O4 89.17(8) . . ? O2 V1 O4 169.26(8) . . ? O5 V1 O6 94.69(8) . . ? O3 V1 O6 96.99(9) . . ? O2 V1 O6 91.38(9) . . ? O4 V1 O6 99.35(9) . . ? O5 V1 O1 84.73(6) . . ? O3 V1 O1 83.61(6) . . ? O2 V1 O1 84.44(6) . . ? O4 V1 O1 84.82(6) . . ? O6 V1 O1 175.78(6) . . ? O5 V1 V3 38.90(6) . 2_666 ? O3 V1 V3 129.42(6) . 2_666 ? O2 V1 V3 88.34(6) . 2_666 ? O4 V1 V3 84.31(6) . 2_666 ? O6 V1 V3 133.57(6) . 2_666 ? O1 V1 V3 45.892(19) . 2_666 ? O5 V1 V2 87.94(6) . 2_666 ? O3 V1 V2 83.40(6) . 2_666 ? O2 V1 V2 129.95(6) . 2_666 ? O4 V1 V2 39.32(6) . 2_666 ? O6 V1 V2 138.62(6) . 2_666 ? O1 V1 V2 45.579(17) . 2_666 ? V3 V1 V2 60.75(2) 2_666 2_666 ? O8 V2 O7 83.49(8) . . ? O8 V2 O4 97.64(8) . 2_666 ? O7 V2 O4 93.09(8) . 2_666 ? O8 V2 O2 96.90(8) . . ? O7 V2 O2 91.24(8) . . ? O4 V2 O2 165.20(8) 2_666 . ? O8 V2 O9 107.85(8) . . ? O7 V2 O9 168.59(7) . . ? O4 V2 O9 86.66(8) 2_666 . ? O2 V2 O9 86.31(8) . . ? O8 V2 O1 168.36(6) . . ? O7 V2 O1 84.88(6) . . ? O4 V2 O1 83.36(6) 2_666 . ? O2 V2 O1 82.95(6) . . ? O9 V2 O1 83.77(6) . . ? O8 V2 V1 134.80(6) . 2_666 ? O7 V2 V1 87.06(6) . 2_666 ? O4 V2 V1 38.83(5) 2_666 2_666 ? O2 V2 V1 127.48(5) . 2_666 ? O9 V2 V1 85.61(6) . 2_666 ? O1 V2 V1 44.60(2) . 2_666 ? O10 V3 O9 82.89(8) . . ? O10 V3 O5 97.54(8) . 2_666 ? O9 V3 O5 92.16(8) . 2_666 ? O10 V3 O3 98.57(8) . . ? O9 V3 O3 91.96(8) . . ? O5 V3 O3 163.74(8) 2_666 . ? O10 V3 O7 109.10(8) . 2_666 ? O9 V3 O7 168.01(7) . 2_666 ? O5 V3 O7 86.46(8) 2_666 2_666 ? O3 V3 O7 86.25(8) . 2_666 ? O10 V3 O1 167.67(6) . . ? O9 V3 O1 84.78(6) . . ? O5 V3 O1 82.79(6) 2_666 . ? O3 V3 O1 81.93(6) . . ? O7 V3 O1 83.23(6) 2_666 . ? O10 V3 V1 134.04(6) . 2_666 ? O9 V3 V1 86.58(6) . 2_666 ? O5 V3 V1 38.23(5) 2_666 2_666 ? O3 V3 V1 126.47(6) . 2_666 ? O7 V3 V1 84.98(6) 2_666 2_666 ? O1 V3 V1 44.62(2) . 2_666 ? V1 O1 V1 180.0 . 2_666 ? V1 O1 V2 89.82(3) . 2_666 ? V1 O1 V2 90.18(3) 2_666 2_666 ? V1 O1 V2 90.18(3) . . ? V1 O1 V2 89.82(3) 2_666 . ? V2 O1 V2 180.0 2_666 . ? V1 O1 V3 89.49(3) . 2_666 ? V1 O1 V3 90.51(3) 2_666 2_666 ? V2 O1 V3 89.83(3) 2_666 2_666 ? V2 O1 V3 90.17(3) . 2_666 ? V1 O1 V3 90.51(3) . . ? V1 O1 V3 89.49(3) 2_666 . ? V2 O1 V3 90.17(3) 2_666 . ? V2 O1 V3 89.83(3) . . ? V3 O1 V3 180.00(2) 2_666 . ? C29 O2 V1 125.07(17) . . ? C29 O2 V2 119.23(16) . . ? V1 O2 V2 102.27(8) . . ? C30 O3 V1 126.98(17) . . ? C30 O3 V3 120.64(17) . . ? V1 O3 V3 103.75(8) . . ? C33 O4 V1 127.57(17) . . ? C33 O4 V2 117.52(16) . 2_666 ? V1 O4 V2 101.85(8) . 2_666 ? C31 O5 V1 129.97(17) . . ? C31 O5 V3 121.56(16) . 2_666 ? V1 O5 V3 102.87(8) . 2_666 ? C32 O6 V1 131.6(2) . . ? C32 O6 H6W 110(3) . . ? V1 O6 H6W 115(3) . . ? C1 O7 V2 111.60(15) . . ? C1 O7 V3 145.95(16) . 2_666 ? V2 O7 V3 101.71(8) . 2_666 ? C2 O8 V2 113.29(16) . . ? C15 O9 V3 112.73(15) . . ? C15 O9 V2 145.65(16) . . ? V3 O9 V2 101.62(8) . . ? C16 O10 V3 113.94(15) . . ? O7 C1 C6 123.4(2) . . ? O7 C1 C2 114.1(2) . . ? C6 C1 C2 122.5(2) . . ? O8 C2 C3 124.1(2) . . ? O8 C2 C1 116.8(2) . . ? C3 C2 C1 119.0(2) . . ? C4 C3 C2 116.8(3) . . ? C4 C3 C7 122.6(2) . . ? C2 C3 C7 120.5(2) . . ? C5 C4 C3 124.3(3) . . ? C5 C4 H4 117.8 . . ? C3 C4 H4 117.8 . . ? C4 C5 C6 117.8(3) . . ? C4 C5 C11 120.8(3) . . ? C6 C5 C11 121.4(3) . . ? C1 C6 C5 119.5(3) . . ? C1 C6 H6 120.2 . . ? C5 C6 H6 120.2 . . ? C8 C7 C9 110.1(3) . . ? C8 C7 C3 110.7(2) . . ? C9 C7 C3 108.8(2) . . ? C8 C7 C10 107.8(3) . . ? C9 C7 C10 108.0(3) . . ? C3 C7 C10 111.4(3) . . ? C7 C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C12Y C11 C14X 135.3(6) . . ? C12Y C11 C5 110.3(6) . . ? C14X C11 C5 112.6(3) . . ? C12Y C11 C12X 39.2(7) . . ? C14X C11 C12X 109.9(5) . . ? C5 C11 C12X 112.8(3) . . ? C12Y C11 C13Y 107.6(10) . . ? C14X C11 C13Y 69.7(8) . . ? C5 C11 C13Y 108.6(5) . . ? C12X C11 C13Y 134.2(6) . . ? C12Y C11 C13X 64.0(8) . . ? C14X C11 C13X 111.0(5) . . ? C5 C11 C13X 109.7(4) . . ? C12X C11 C13X 100.3(5) . . ? C13Y C11 C13X 46.1(7) . . ? C12Y C11 C14Y 105.3(10) . . ? C14X C11 C14Y 53.5(7) . . ? C5 C11 C14Y 102.6(5) . . ? C12X C11 C14Y 66.5(7) . . ? C13Y C11 C14Y 122.1(9) . . ? C13X C11 C14Y 147.6(5) . . ? C11 C12X H12A 109.5 . . ? C11 C12X H12C 109.5 . . ? C11 C12X H12B 109.5 . . ? C11 C13X H13A 109.5 . . ? C11 C13X H13C 109.5 . . ? C11 C13X H13B 109.5 . . ? C11 C14X H14A 109.5 . . ? C11 C14X H14B 109.5 . . ? C11 C14X H14C 109.5 . . ? C11 C12Y H12E 109.5 . . ? C11 C12Y H12F 109.5 . . ? H12E C12Y H12F 109.5 . . ? C11 C12Y H12D 109.5 . . ? H12E C12Y H12D 109.5 . . ? H12F C12Y H12D 109.5 . . ? C11 C13Y H13D 109.5 . . ? C11 C13Y H13F 109.5 . . ? H13D C13Y H13F 109.5 . . ? C11 C13Y H13E 109.5 . . ? H13D C13Y H13E 109.5 . . ? H13F C13Y H13E 109.5 . . ? C11 C14Y H14D 109.5 . . ? C11 C14Y H14E 109.5 . . ? H14D C14Y H14E 109.5 . . ? C11 C14Y H14F 109.5 . . ? H14D C14Y H14F 109.5 . . ? H14E C14Y H14F 109.5 . . ? C20 C15 O9 123.4(2) . . ? C20 C15 C16 122.7(2) . . ? O9 C15 C16 113.8(2) . . ? O10 C16 C17 124.5(2) . . ? O10 C16 C15 116.6(2) . . ? C17 C16 C15 118.9(2) . . ? C18 C17 C16 117.1(2) . . ? C18 C17 C21 122.5(2) . . ? C16 C17 C21 120.5(2) . . ? C19 C18 C17 124.1(2) . . ? C19 C18 H18 117.9 . . ? C17 C18 H18 117.9 . . ? C18 C19 C20 117.6(2) . . ? C18 C19 C25 123.0(2) . . ? C20 C19 C25 119.4(2) . . ? C15 C20 C19 119.6(2) . . ? C15 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C24 C21 C22 107.7(3) . . ? C24 C21 C23 109.9(3) . . ? C22 C21 C23 108.0(3) . . ? C24 C21 C17 109.4(2) . . ? C22 C21 C17 111.7(2) . . ? C23 C21 C17 110.2(2) . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C26 C25 C27 109.0(3) . . ? C26 C25 C28 108.0(3) . . ? C27 C25 C28 107.9(3) . . ? C26 C25 C19 112.7(3) . . ? C27 C25 C19 109.4(2) . . ? C28 C25 C19 109.7(2) . . ? C25 C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26C C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? C25 C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? C25 C28 H28C 109.5 . . ? C25 C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O2 C29 H29C 109.5 . . ? O2 C29 H29B 109.5 . . ? H29C C29 H29B 109.5 . . ? O2 C29 H29A 109.5 . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? O3 C30 H30B 109.5 . . ? O3 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? H30C C30 H30A 109.5 . . ? O4 C33 H33A 109.5 . . ? O4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? O4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? H33C C33 H33B 109.5 . . ? O5 C31 H31A 109.5 . . ? O5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O6 C32 H32C 109.5 . . ? O6 C32 H32B 109.5 . . ? H32C C32 H32B 109.5 . . ? O6 C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 104(3) . . ? O2S C2S H2SC 109.5 . . ? O2S C2S H2SA 109.5 . . ? H2SC C2S H2SA 109.5 . . ? O2S C2S H2SB 109.5 . . ? H2SC C2S H2SB 109.5 . . ? H2SA C2S H2SB 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 O5 V1 O1 V1 60(16) . . . 2_666 ? O3 V1 O1 V1 -119(16) . . . 2_666 ? O2 V1 O1 V1 151(16) . . . 2_666 ? O4 V1 O1 V1 -29(16) . . . 2_666 ? O6 V1 O1 V1 142(16) . . . 2_666 ? V3 V1 O1 V1 58(16) 2_666 . . 2_666 ? V2 V1 O1 V1 -32(16) 2_666 . . 2_666 ? O5 V1 O1 V2 92.29(6) . . . 2_666 ? O3 V1 O1 V2 -87.00(6) . . . 2_666 ? O2 V1 O1 V2 -177.08(5) . . . 2_666 ? O4 V1 O1 V2 2.74(5) . . . 2_666 ? O6 V1 O1 V2 174.6(9) . . . 2_666 ? V3 V1 O1 V2 89.83(3) 2_666 . . 2_666 ? O5 V1 O1 V2 -87.71(6) . . . . ? O3 V1 O1 V2 93.00(6) . . . . ? O2 V1 O1 V2 2.92(5) . . . . ? O4 V1 O1 V2 -177.26(5) . . . . ? O6 V1 O1 V2 -5.4(9) . . . . ? V3 V1 O1 V2 -90.17(3) 2_666 . . . ? V2 V1 O1 V2 180.0 2_666 . . . ? O5 V1 O1 V3 2.46(5) . . . 2_666 ? O3 V1 O1 V3 -176.83(5) . . . 2_666 ? O2 V1 O1 V3 93.09(6) . . . 2_666 ? O4 V1 O1 V3 -87.09(6) . . . 2_666 ? O6 V1 O1 V3 84.7(9) . . . 2_666 ? V2 V1 O1 V3 -89.83(3) 2_666 . . 2_666 ? O5 V1 O1 V3 -177.54(5) . . . . ? O3 V1 O1 V3 3.17(5) . . . . ? O2 V1 O1 V3 -86.91(6) . . . . ? O4 V1 O1 V3 92.91(6) . . . . ? O6 V1 O1 V3 -95.3(9) . . . . ? V3 V1 O1 V3 179.999(2) 2_666 . . . ? V2 V1 O1 V3 90.17(3) 2_666 . . . ? O8 V2 O1 V1 87.1(3) . . . . ? O7 V2 O1 V1 89.00(6) . . . . ? O4 V2 O1 V1 -177.28(5) 2_666 . . . ? O2 V2 O1 V1 -2.90(5) . . . . ? O9 V2 O1 V1 -89.93(6) . . . . ? V1 V2 O1 V1 180.0 2_666 . . . ? O8 V2 O1 V1 -92.9(3) . . . 2_666 ? O7 V2 O1 V1 -91.00(6) . . . 2_666 ? O4 V2 O1 V1 2.72(5) 2_666 . . 2_666 ? O2 V2 O1 V1 177.10(5) . . . 2_666 ? O9 V2 O1 V1 90.07(6) . . . 2_666 ? O8 V2 O1 V2 18(22) . . . 2_666 ? O7 V2 O1 V2 20(22) . . . 2_666 ? O4 V2 O1 V2 114(22) 2_666 . . 2_666 ? O2 V2 O1 V2 -72(22) . . . 2_666 ? O9 V2 O1 V2 -159(22) . . . 2_666 ? V1 V2 O1 V2 111(22) 2_666 . . 2_666 ? O8 V2 O1 V3 -2.4(3) . . . 2_666 ? O7 V2 O1 V3 -0.49(5) . . . 2_666 ? O4 V2 O1 V3 93.23(6) 2_666 . . 2_666 ? O2 V2 O1 V3 -92.38(6) . . . 2_666 ? O9 V2 O1 V3 -179.42(5) . . . 2_666 ? V1 V2 O1 V3 90.51(3) 2_666 . . 2_666 ? O8 V2 O1 V3 177.6(3) . . . . ? O7 V2 O1 V3 179.51(5) . . . . ? O4 V2 O1 V3 -86.77(6) 2_666 . . . ? O2 V2 O1 V3 87.62(6) . . . . ? O9 V2 O1 V3 0.58(5) . . . . ? V1 V2 O1 V3 -89.49(3) 2_666 . . . ? O10 V3 O1 V1 90.1(3) . . . . ? O9 V3 O1 V1 89.59(6) . . . . ? O5 V3 O1 V1 -177.56(5) 2_666 . . . ? O3 V3 O1 V1 -3.15(5) . . . . ? O7 V3 O1 V1 -90.30(6) 2_666 . . . ? V1 V3 O1 V1 180.0 2_666 . . . ? O10 V3 O1 V1 -89.9(3) . . . 2_666 ? O9 V3 O1 V1 -90.42(6) . . . 2_666 ? O5 V3 O1 V1 2.43(5) 2_666 . . 2_666 ? O3 V3 O1 V1 176.85(5) . . . 2_666 ? O7 V3 O1 V1 89.70(6) 2_666 . . 2_666 ? O10 V3 O1 V2 179.9(3) . . . 2_666 ? O9 V3 O1 V2 179.41(5) . . . 2_666 ? O5 V3 O1 V2 -87.74(6) 2_666 . . 2_666 ? O3 V3 O1 V2 86.67(6) . . . 2_666 ? O7 V3 O1 V2 -0.48(5) 2_666 . . 2_666 ? V1 V3 O1 V2 -90.18(3) 2_666 . . 2_666 ? O10 V3 O1 V2 -0.1(3) . . . . ? O9 V3 O1 V2 -0.59(5) . . . . ? O5 V3 O1 V2 92.26(6) 2_666 . . . ? O3 V3 O1 V2 -93.33(6) . . . . ? O7 V3 O1 V2 179.52(5) 2_666 . . . ? V1 V3 O1 V2 89.82(3) 2_666 . . . ? O10 V3 O1 V3 125(43) . . . 2_666 ? O9 V3 O1 V3 125(43) . . . 2_666 ? O5 V3 O1 V3 -142(43) 2_666 . . 2_666 ? O3 V3 O1 V3 32(43) . . . 2_666 ? O7 V3 O1 V3 -55(43) 2_666 . . 2_666 ? V1 V3 O1 V3 -145(43) 2_666 . . 2_666 ? O5 V1 O2 C29 -138.85(19) . . . . ? O3 V1 O2 C29 52.8(2) . . . . ? O4 V1 O2 C29 135.5(4) . . . . ? O6 V1 O2 C29 -44.2(2) . . . . ? O1 V1 O2 C29 136.45(19) . . . . ? V3 V1 O2 C29 -177.71(19) 2_666 . . . ? V2 V1 O2 C29 133.73(18) 2_666 . . . ? O5 V1 O2 V2 81.40(9) . . . . ? O3 V1 O2 V2 -86.93(9) . . . . ? O4 V1 O2 V2 -4.3(4) . . . . ? O6 V1 O2 V2 176.09(8) . . . . ? O1 V1 O2 V2 -3.30(6) . . . . ? V3 V1 O2 V2 42.53(6) 2_666 . . . ? V2 V1 O2 V2 -6.02(11) 2_666 . . . ? O8 V2 O2 C29 52.27(19) . . . . ? O7 V2 O2 C29 135.86(18) . . . . ? O4 V2 O2 C29 -117.1(3) 2_666 . . . ? O9 V2 O2 C29 -55.29(19) . . . . ? O1 V2 O2 C29 -139.45(18) . . . . ? V1 V2 O2 C29 -136.89(17) 2_666 . . . ? O8 V2 O2 V1 -165.03(8) . . . . ? O7 V2 O2 V1 -81.43(9) . . . . ? O4 V2 O2 V1 25.6(3) 2_666 . . . ? O9 V2 O2 V1 87.41(8) . . . . ? O1 V2 O2 V1 3.25(6) . . . . ? V1 V2 O2 V1 5.81(10) 2_666 . . . ? O5 V1 O3 C30 140.2(4) . . . . ? O2 V1 O3 C30 -131.9(2) . . . . ? O4 V1 O3 C30 58.7(2) . . . . ? O6 V1 O3 C30 -40.6(2) . . . . ? O1 V1 O3 C30 143.6(2) . . . . ? V3 V1 O3 C30 140.7(2) 2_666 . . . ? V2 V1 O3 C30 97.7(2) 2_666 . . . ? O5 V1 O3 V3 -7.1(4) . . . . ? O2 V1 O3 V3 80.83(9) . . . . ? O4 V1 O3 V3 -88.52(9) . . . . ? O6 V1 O3 V3 172.16(9) . . . . ? O1 V1 O3 V3 -3.63(6) . . . . ? V3 V1 O3 V3 -6.58(11) 2_666 . . . ? V2 V1 O3 V3 -49.52(7) 2_666 . . . ? O10 V3 O3 C30 46.2(2) . . . . ? O9 V3 O3 C30 129.3(2) . . . . ? O5 V3 O3 C30 -126.1(3) 2_666 . . . ? O7 V3 O3 C30 -62.6(2) 2_666 . . . ? O1 V3 O3 C30 -146.3(2) . . . . ? V1 V3 O3 C30 -143.54(18) 2_666 . . . ? O10 V3 O3 V1 -163.98(8) . . . . ? O9 V3 O3 V1 -80.87(9) . . . . ? O5 V3 O3 V1 23.7(3) 2_666 . . . ? O7 V3 O3 V1 87.25(9) 2_666 . . . ? O1 V3 O3 V1 3.57(6) . . . . ? V1 V3 O3 V1 6.32(11) 2_666 . . . ? O5 V1 O4 C33 51.3(2) . . . . ? O3 V1 O4 C33 -140.2(2) . . . . ? O2 V1 O4 C33 137.1(4) . . . . ? O6 V1 O4 C33 -43.3(2) . . . . ? O1 V1 O4 C33 136.1(2) . . . . ? V3 V1 O4 C33 90.0(2) 2_666 . . . ? V2 V1 O4 C33 139.2(2) 2_666 . . . ? O5 V1 O4 V2 -87.87(9) . . . 2_666 ? O3 V1 O4 V2 80.57(9) . . . 2_666 ? O2 V1 O4 V2 -2.1(4) . . . 2_666 ? O6 V1 O4 V2 177.52(8) . . . 2_666 ? O1 V1 O4 V2 -3.09(6) . . . 2_666 ? V3 V1 O4 V2 -49.19(6) 2_666 . . 2_666 ? O3 V1 O5 C31 153.8(4) . . . . ? O2 V1 O5 C31 65.9(2) . . . . ? O4 V1 O5 C31 -124.8(2) . . . . ? O6 V1 O5 C31 -25.5(2) . . . . ? O1 V1 O5 C31 150.3(2) . . . . ? V3 V1 O5 C31 153.2(3) 2_666 . . . ? V2 V1 O5 C31 -164.1(2) 2_666 . . . ? O3 V1 O5 V3 0.6(4) . . . 2_666 ? O2 V1 O5 V3 -87.22(9) . . . 2_666 ? O4 V1 O5 V3 82.07(9) . . . 2_666 ? O6 V1 O5 V3 -178.62(8) . . . 2_666 ? O1 V1 O5 V3 -2.82(6) . . . 2_666 ? V2 V1 O5 V3 42.75(7) 2_666 . . 2_666 ? O5 V1 O6 C32 -105.7(3) . . . . ? O3 V1 O6 C32 74.4(3) . . . . ? O2 V1 O6 C32 164.1(3) . . . . ? O4 V1 O6 C32 -15.9(3) . . . . ? O1 V1 O6 C32 172.4(8) . . . . ? V3 V1 O6 C32 -106.9(3) 2_666 . . . ? V2 V1 O6 C32 -13.5(4) 2_666 . . . ? O8 V2 O7 C1 7.32(16) . . . . ? O4 V2 O7 C1 104.67(16) 2_666 . . . ? O2 V2 O7 C1 -89.49(16) . . . . ? O9 V2 O7 C1 -166.9(3) . . . . ? O1 V2 O7 C1 -172.29(16) . . . . ? V1 V2 O7 C1 143.04(16) 2_666 . . . ? O8 V2 O7 V3 -179.85(9) . . . 2_666 ? O4 V2 O7 V3 -82.50(9) 2_666 . . 2_666 ? O2 V2 O7 V3 83.35(9) . . . 2_666 ? O9 V2 O7 V3 5.9(4) . . . 2_666 ? O1 V2 O7 V3 0.54(6) . . . 2_666 ? V1 V2 O7 V3 -44.12(7) 2_666 . . 2_666 ? O7 V2 O8 C2 -6.81(17) . . . . ? O4 V2 O8 C2 -99.07(17) 2_666 . . . ? O2 V2 O8 C2 83.66(17) . . . . ? O9 V2 O8 C2 171.99(16) . . . . ? O1 V2 O8 C2 -4.9(4) . . . . ? V1 V2 O8 C2 -86.09(18) 2_666 . . . ? O10 V3 O9 C15 0.93(16) . . . . ? O5 V3 O9 C15 98.26(16) 2_666 . . . ? O3 V3 O9 C15 -97.47(16) . . . . ? O7 V3 O9 C15 -178.6(3) 2_666 . . . ? O1 V3 O9 C15 -179.18(15) . . . . ? V1 V3 O9 C15 136.10(15) 2_666 . . . ? O10 V3 O9 V2 -179.24(9) . . . . ? O5 V3 O9 V2 -81.91(9) 2_666 . . . ? O3 V3 O9 V2 82.36(9) . . . . ? O7 V3 O9 V2 1.2(4) 2_666 . . . ? O1 V3 O9 V2 0.65(6) . . . . ? V1 V3 O9 V2 -44.07(7) 2_666 . . . ? O8 V2 O9 C15 -0.3(3) . . . . ? O7 V2 O9 C15 173.7(3) . . . . ? O4 V2 O9 C15 -97.3(3) 2_666 . . . ? O2 V2 O9 C15 95.8(3) . . . . ? O1 V2 O9 C15 179.1(3) . . . . ? V1 V2 O9 C15 -136.2(3) 2_666 . . . ? O8 V2 O9 V3 179.98(7) . . . . ? O7 V2 O9 V3 -6.1(4) . . . . ? O4 V2 O9 V3 83.01(9) 2_666 . . . ? O2 V2 O9 V3 -83.95(8) . . . . ? O1 V2 O9 V3 -0.66(6) . . . . ? V1 V2 O9 V3 44.11(7) 2_666 . . . ? O9 V3 O10 C16 -0.55(16) . . . . ? O5 V3 O10 C16 -91.80(17) 2_666 . . . ? O3 V3 O10 C16 90.37(17) . . . . ? O7 V3 O10 C16 179.35(15) 2_666 . . . ? O1 V3 O10 C16 -1.1(4) . . . . ? V1 V3 O10 C16 -78.76(18) 2_666 . . . ? V2 O7 C1 C6 173.2(2) . . . . ? V3 O7 C1 C6 5.8(5) 2_666 . . . ? V2 O7 C1 C2 -6.4(3) . . . . ? V3 O7 C1 C2 -173.8(2) 2_666 . . . ? V2 O8 C2 C3 -175.4(2) . . . . ? V2 O8 C2 C1 5.2(3) . . . . ? O7 C1 C2 O8 1.0(3) . . . . ? C6 C1 C2 O8 -178.6(2) . . . . ? O7 C1 C2 C3 -178.4(2) . . . . ? C6 C1 C2 C3 2.0(4) . . . . ? O8 C2 C3 C4 178.8(2) . . . . ? C1 C2 C3 C4 -1.8(4) . . . . ? O8 C2 C3 C7 -2.0(4) . . . . ? C1 C2 C3 C7 177.4(2) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C7 C3 C4 C5 -178.9(3) . . . . ? C3 C4 C5 C6 1.4(5) . . . . ? C3 C4 C5 C11 -179.6(3) . . . . ? O7 C1 C6 C5 -179.9(3) . . . . ? C2 C1 C6 C5 -0.3(4) . . . . ? C4 C5 C6 C1 -1.3(4) . . . . ? C11 C5 C6 C1 179.7(3) . . . . ? C4 C3 C7 C8 -122.2(3) . . . . ? C2 C3 C7 C8 58.7(4) . . . . ? C4 C3 C7 C9 116.7(3) . . . . ? C2 C3 C7 C9 -62.4(3) . . . . ? C4 C3 C7 C10 -2.2(4) . . . . ? C2 C3 C7 C10 178.6(3) . . . . ? C4 C5 C11 C12Y 129.3(9) . . . . ? C6 C5 C11 C12Y -51.7(9) . . . . ? C4 C5 C11 C14X -63.5(6) . . . . ? C6 C5 C11 C14X 115.5(5) . . . . ? C4 C5 C11 C12X 171.5(5) . . . . ? C6 C5 C11 C12X -9.5(6) . . . . ? C4 C5 C11 C13Y 11.6(9) . . . . ? C6 C5 C11 C13Y -169.4(9) . . . . ? C4 C5 C11 C13X 60.6(5) . . . . ? C6 C5 C11 C13X -120.4(5) . . . . ? C4 C5 C11 C14Y -118.9(7) . . . . ? C6 C5 C11 C14Y 60.0(7) . . . . ? V3 O9 C15 C20 178.1(2) . . . . ? V2 O9 C15 C20 -1.6(4) . . . . ? V3 O9 C15 C16 -1.1(3) . . . . ? V2 O9 C15 C16 179.2(2) . . . . ? V3 O10 C16 C17 -179.8(2) . . . . ? V3 O10 C16 C15 0.1(3) . . . . ? C20 C15 C16 O10 -178.5(2) . . . . ? O9 C15 C16 O10 0.7(3) . . . . ? C20 C15 C16 C17 1.4(4) . . . . ? O9 C15 C16 C17 -179.4(2) . . . . ? O10 C16 C17 C18 178.5(2) . . . . ? C15 C16 C17 C18 -1.4(4) . . . . ? O10 C16 C17 C21 -2.0(4) . . . . ? C15 C16 C17 C21 178.1(2) . . . . ? C16 C17 C18 C19 0.4(4) . . . . ? C21 C17 C18 C19 -179.1(3) . . . . ? C17 C18 C19 C20 0.8(4) . . . . ? C17 C18 C19 C25 -179.7(2) . . . . ? O9 C15 C20 C19 -179.3(2) . . . . ? C16 C15 C20 C19 -0.2(4) . . . . ? C18 C19 C20 C15 -0.9(4) . . . . ? C25 C19 C20 C15 179.6(2) . . . . ? C18 C17 C21 C24 118.6(3) . . . . ? C16 C17 C21 C24 -60.9(3) . . . . ? C18 C17 C21 C22 -0.5(4) . . . . ? C16 C17 C21 C22 -179.9(3) . . . . ? C18 C17 C21 C23 -120.5(3) . . . . ? C16 C17 C21 C23 60.1(3) . . . . ? C18 C19 C25 C26 -6.2(4) . . . . ? C20 C19 C25 C26 173.3(3) . . . . ? C18 C19 C25 C27 115.3(3) . . . . ? C20 C19 C25 C27 -65.2(3) . . . . ? C18 C19 C25 C28 -126.6(3) . . . . ? C20 C19 C25 C28 53.0(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2S H2S O1S 0.941(19) 1.86(2) 2.780(5) 164(4) 1_655 O6 H6W O2S 0.91(5) 1.69(5) 2.595(3) 171(4) 1_455 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 27.98 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.744 _refine_diff_density_min -0.591 _refine_diff_density_rms 0.090 # Attachment 'complex-2new.cif.txt' data_test2 _database_code_depnum_ccdc_archive 'CCDC 762900' #TrackingRef 'complex-2new.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C98 H124 O24 V6' _chemical_formula_weight 1991.61 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.486(4) _cell_length_b 28.417(11) _cell_length_c 14.966(5) _cell_angle_alpha 90.00 _cell_angle_beta 100.286(9) _cell_angle_gamma 90.00 _cell_volume 4806(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9960 _cell_measurement_theta_min 4.918 _cell_measurement_theta_max 46.520 _exptl_crystal_description blue/black _exptl_crystal_colour needle _exptl_crystal_size_max 0.57 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2042 _exptl_absorpt_coefficient_mu 0.632 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7148 _exptl_absorpt_correction_T_max 0.9571 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10297 _diffrn_reflns_av_R_equivalents 0.1527 _diffrn_reflns_av_sigmaI/netI 0.2416 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 23.33 _reflns_number_total 5527 _reflns_number_gt 2521 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data processing was carried out to 1.1 angstroms as the data was only complete to this resolution. All non hydrogen atoms were refined anisotropically with the exception of O4 which always remained NPD when refined anisotropically. The ratio of unique:expected reflections is low, because the resolution was low and the data was only complete to 1.1 angstroms. Thermal restraints were applied to all carbons and oxygen atoms to prevent as many NPD as possible. This is a consequnce of the limited data range and poor data to parameter ratio. Hydrogen atoms were included in calculated positions. 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^)+(0.0681P)^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 0.0020(4) _refine_ls_number_reflns 5527 _refine_ls_number_parameters 573 _refine_ls_number_restraints 459 _refine_ls_R_factor_all 0.1574 _refine_ls_R_factor_gt 0.0778 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1614 _refine_ls_goodness_of_fit_ref 0.836 _refine_ls_restrained_S_all 0.809 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.47607(13) 1.04736(5) 0.45542(12) 0.0275(5) Uani 1 1 d . . . V2 V 0.42111(13) 0.95890(5) 0.33543(12) 0.0284(5) Uani 1 1 d . . . V3 V 0.30720(13) 1.02245(5) 0.62863(12) 0.0291(5) Uani 1 1 d . . . O1 O 0.4496(4) 1.01332(18) 0.5712(4) 0.0256(17) Uani 1 1 d . . . O2 O 0.3907(5) 1.10651(19) 0.4784(5) 0.0341(10) Uani 1 1 d U . . O9 O 0.2519(5) 1.0820(2) 0.5593(4) 0.0338(10) Uani 1 1 d U . . O3 O 0.3403(5) 1.0177(2) 0.3734(4) 0.0326(9) Uani 1 1 d U . . O4 O 0.5213(5) 1.07784(19) 0.3461(4) 0.0271(16) Uiso 1 1 d . . . O5 O 0.6051(4) 1.07193(19) 0.5471(4) 0.0259(14) Uani 1 1 d U . . O6 O 0.3322(5) 0.9055(2) 0.2892(4) 0.0349(10) Uani 1 1 d U . . O7 O 0.5647(5) 0.9391(2) 0.2942(5) 0.0343(15) Uani 1 1 d U . . O8 O 0.3716(5) 0.9864(2) 0.2220(4) 0.0334(9) Uani 1 1 d U . . O10 O 0.2066(5) 0.9808(2) 0.5461(4) 0.0323(11) Uani 1 1 d U . . O11 O 0.1753(5) 1.0339(2) 0.6948(4) 0.0331(11) Uani 1 1 d U . . O12 O 0.3547(5) 0.96822(19) 0.7151(4) 0.0295(11) Uani 1 1 d U . . C1 C 0.6568(7) 1.1160(3) 0.5596(7) 0.0260(15) Uani 1 1 d U . . C2 C 0.3088(8) 0.8721(3) 0.3518(7) 0.0354(9) Uani 1 1 d U . . C3 C 0.2515(8) 0.8292(3) 0.3248(7) 0.0363(9) Uani 1 1 d U . . C4 C 0.2348(8) 0.8008(3) 0.3987(7) 0.0367(9) Uani 1 1 d U . . H4 H 0.1946 0.7718 0.3846 0.055 Uiso 1 1 calc R . . C5 C 0.2708(8) 0.8111(3) 0.4885(7) 0.0371(9) Uani 1 1 d U . . C6 C 0.3278(8) 0.8548(3) 0.5107(7) 0.0368(10) Uani 1 1 d U . . H6 H 0.3546 0.8638 0.5721 0.055 Uiso 1 1 calc R . . C7 C 0.2106(8) 0.8165(3) 0.2260(7) 0.0374(9) Uani 1 1 d U . . C8 C 0.3185(8) 0.8124(3) 0.1789(7) 0.0383(12) Uani 1 1 d U . . H8A H 0.3587 0.8429 0.1808 0.057 Uiso 1 1 calc R . . H8B H 0.2925 0.8029 0.1155 0.057 Uiso 1 1 calc R . . H8C H 0.3732 0.7888 0.2103 0.057 Uiso 1 1 calc R . . C9 C 0.1246(8) 0.8528(3) 0.1775(7) 0.0391(12) Uani 1 1 d U . . H9A H 0.0558 0.8551 0.2076 0.059 Uiso 1 1 calc R . . H9B H 0.0987 0.8433 0.1141 0.059 Uiso 1 1 calc R . . H9C H 0.1639 0.8835 0.1794 0.059 Uiso 1 1 calc R . . C10 C 0.1463(8) 0.7684(3) 0.2163(7) 0.0387(12) Uani 1 1 d U . . H10A H 0.1982 0.7443 0.2489 0.058 Uiso 1 1 calc R . . H10B H 0.1262 0.7600 0.1519 0.058 Uiso 1 1 calc R . . H10C H 0.0737 0.7706 0.2419 0.058 Uiso 1 1 calc R . . C11 C 0.2484(8) 0.7758(3) 0.5650(7) 0.0381(9) Uani 1 1 d U . . C12 C 0.3221(8) 0.7316(3) 0.5579(7) 0.0400(12) Uani 1 1 d U . . H12A H 0.3100 0.7091 0.6051 0.060 Uiso 1 1 calc R . . H12B H 0.4060 0.7401 0.5661 0.060 Uiso 1 1 calc R . . H12C H 0.2975 0.7172 0.4980 0.060 Uiso 1 1 calc R . . C13 C 0.2912(8) 0.7963(3) 0.6598(6) 0.0391(12) Uani 1 1 d U . . H13A H 0.2573 0.8278 0.6633 0.059 Uiso 1 1 calc R . . H13B H 0.3777 0.7985 0.6712 0.059 Uiso 1 1 calc R . . H13C H 0.2658 0.7759 0.7054 0.059 Uiso 1 1 calc R . . C14 C 0.1213(8) 0.7646(3) 0.5542(7) 0.0389(12) Uani 1 1 d U . . H14A H 0.0947 0.7499 0.4948 0.058 Uiso 1 1 calc R . . H14B H 0.0765 0.7937 0.5583 0.058 Uiso 1 1 calc R . . H14C H 0.1082 0.7429 0.6023 0.058 Uiso 1 1 calc R . . C15 C 0.2759(8) 1.0405(3) 0.2994(7) 0.0337(8) Uani 1 1 d U . . C16 C 0.2924(8) 1.0227(3) 0.2143(7) 0.0339(8) Uani 1 1 d U . . C17 C 0.2340(8) 1.0412(3) 0.1325(7) 0.0350(8) Uani 1 1 d U . . C18 C 0.1580(8) 1.0796(3) 0.1409(7) 0.0353(8) Uani 1 1 d U . . H18 H 0.1135 1.0927 0.0870 0.053 Uiso 1 1 calc R . . C19 C 0.1450(8) 1.0994(3) 0.2243(7) 0.0356(8) Uani 1 1 d U . . C20 C 0.2046(7) 1.0785(3) 0.3031(7) 0.0346(8) Uani 1 1 d U . . H20 H 0.1955 1.0908 0.3604 0.052 Uiso 1 1 calc R . . C21 C 0.2481(8) 1.0207(3) 0.0406(7) 0.0359(9) Uani 1 1 d U . . C22 C 0.3731(7) 1.0188(3) 0.0303(7) 0.0361(11) Uani 1 1 d U . . H22A H 0.4061 1.0507 0.0344 0.054 Uiso 1 1 calc R . . H22B H 0.3789 1.0052 -0.0289 0.054 Uiso 1 1 calc R . . H22C H 0.4176 0.9993 0.0787 0.054 Uiso 1 1 calc R . . C23 C 0.1913(8) 0.9708(3) 0.0363(7) 0.0369(12) Uani 1 1 d U . . H23A H 0.1717 0.9605 -0.0272 0.055 Uiso 1 1 calc R . . H23B H 0.1192 0.9718 0.0626 0.055 Uiso 1 1 calc R . . H23C H 0.2475 0.9486 0.0706 0.055 Uiso 1 1 calc R . . C24 C 0.1780(8) 1.0494(3) -0.0389(6) 0.0385(12) Uani 1 1 d U . . H24A H 0.2042 1.0822 -0.0340 0.058 Uiso 1 1 calc R . . H24B H 0.0933 1.0478 -0.0366 0.058 Uiso 1 1 calc R . . H24C H 0.1919 1.0362 -0.0966 0.058 Uiso 1 1 calc R . . C25 C 0.0602(8) 1.1416(3) 0.2251(7) 0.0367(9) Uani 1 1 d U . . C26 C 0.0745(8) 1.1645(3) 0.3178(7) 0.0380(12) Uani 1 1 d U . . H26A H 0.0304 1.1942 0.3130 0.057 Uiso 1 1 calc R . . H26B H 0.1585 1.1707 0.3405 0.057 Uiso 1 1 calc R . . H26C H 0.0437 1.1434 0.3599 0.057 Uiso 1 1 calc R . . C27 C 0.0925(8) 1.1790(3) 0.1590(7) 0.0381(12) Uani 1 1 d U . . H27A H 0.0796 1.1661 0.0973 0.057 Uiso 1 1 calc R . . H27B H 0.1759 1.1878 0.1772 0.057 Uiso 1 1 calc R . . H27C H 0.0427 1.2069 0.1606 0.057 Uiso 1 1 calc R . . C28 C -0.0636(7) 1.1269(3) 0.1931(7) 0.0379(12) Uani 1 1 d U . . H28A H -0.0703 1.1116 0.1337 0.057 Uiso 1 1 calc R . . H28B H -0.1153 1.1546 0.1877 0.057 Uiso 1 1 calc R . . H28C H -0.0875 1.1048 0.2367 0.057 Uiso 1 1 calc R . . C29 C 0.3146(8) 1.1134(3) 0.5242(7) 0.0344(9) Uani 1 1 d U . . C30 C 0.2820(8) 1.1642(3) 0.5462(7) 0.0354(9) Uani 1 1 d U . . C31 C 0.1891(8) 1.1739(3) 0.5876(7) 0.0359(10) Uani 1 1 d U . . H31 H 0.1402 1.1491 0.6020 0.054 Uiso 1 1 calc R . . C32 C 0.1652(8) 1.2202(3) 0.6090(7) 0.0367(10) Uani 1 1 d U . . H32 H 0.0992 1.2277 0.6367 0.055 Uiso 1 1 calc R . . C33 C 0.2409(8) 1.2551(3) 0.5886(7) 0.0370(10) Uani 1 1 d U . . H33 H 0.2265 1.2868 0.6036 0.056 Uiso 1 1 calc R . . C34 C 0.3322(8) 1.2458(3) 0.5489(7) 0.0368(10) Uani 1 1 d U . . H34 H 0.3816 1.2710 0.5367 0.055 Uiso 1 1 calc R . . C35 C 0.3581(8) 1.1999(3) 0.5245(7) 0.0362(10) Uani 1 1 d U . . H35 H 0.4229 1.1931 0.4950 0.054 Uiso 1 1 calc R . . C36 C 0.4239(8) 0.9341(3) 0.7176(7) 0.0294(10) Uani 1 1 d U . . C37 C 0.4423(8) 0.9035(3) 0.8008(7) 0.0298(10) Uani 1 1 d U . . C38 C 0.5338(8) 0.8711(3) 0.8141(7) 0.0303(10) Uani 1 1 d U . . H38 H 0.5838 0.8672 0.7705 0.045 Uiso 1 1 calc R . . C39 C 0.5503(8) 0.8442(3) 0.8933(7) 0.0306(10) Uani 1 1 d U . . H39 H 0.6133 0.8221 0.9036 0.046 Uiso 1 1 calc R . . C40 C 0.4789(8) 0.8487(3) 0.9564(7) 0.0306(10) Uani 1 1 d U . . H40 H 0.4924 0.8299 1.0098 0.046 Uiso 1 1 calc R . . C41 C 0.3876(8) 0.8804(3) 0.9424(7) 0.0304(10) Uani 1 1 d U . . H41 H 0.3374 0.8836 0.9862 0.046 Uiso 1 1 calc R . . C42 C 0.3683(8) 0.9077(3) 0.8650(7) 0.0301(10) Uani 1 1 d U . . H42 H 0.3045 0.9294 0.8553 0.045 Uiso 1 1 calc R . . C43 C 0.1105(8) 0.9612(3) 0.5559(7) 0.0328(10) Uani 1 1 d U . . C44 C 0.0454(8) 0.9747(3) 0.6228(7) 0.0333(10) Uani 1 1 d U . . H44 H -0.0255 0.9580 0.6256 0.050 Uiso 1 1 calc R . . C45 C 0.0775(8) 1.0111(3) 0.6854(7) 0.0335(10) Uani 1 1 d U . . C46 C 0.0669(7) 0.9228(3) 0.4916(7) 0.0338(13) Uani 1 1 d U . . H46A H 0.0900 0.9291 0.4328 0.051 Uiso 1 1 calc R . . H46B H -0.0195 0.9210 0.4838 0.051 Uiso 1 1 calc R . . H46C H 0.1014 0.8928 0.5158 0.051 Uiso 1 1 calc R . . C47 C -0.0056(7) 1.0250(3) 0.7479(7) 0.0351(13) Uani 1 1 d U . . H47A H 0.0137 1.0568 0.7711 0.053 Uiso 1 1 calc R . . H47B H 0.0024 1.0028 0.7988 0.053 Uiso 1 1 calc R . . H47C H -0.0872 1.0243 0.7145 0.053 Uiso 1 1 calc R . . C48 C 0.5647(8) 0.9229(3) 0.2024(7) 0.0349(15) Uani 1 1 d U . . H48A H 0.5975 0.9476 0.1674 0.052 Uiso 1 1 calc R . . H48B H 0.4827 0.9161 0.1718 0.052 Uiso 1 1 calc R . . C49 C 0.6398(8) 0.8785(3) 0.2060(7) 0.0365(16) Uani 1 1 d U . . H49A H 0.7184 0.8846 0.2418 0.055 Uiso 1 1 calc R . . H49B H 0.6475 0.8693 0.1442 0.055 Uiso 1 1 calc R . . H49C H 0.6017 0.8530 0.2343 0.055 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 V1 0.0247(9) 0.0271(9) 0.0341(14) -0.0019(9) 0.0146(9) -0.0015(8) V2 0.0252(9) 0.0262(9) 0.0368(14) -0.0006(9) 0.0140(9) -0.0007(8) V3 0.0242(9) 0.0303(9) 0.0349(14) 0.0001(9) 0.0114(9) -0.0009(8) O1 0.013(3) 0.029(4) 0.041(5) -0.002(3) 0.021(3) -0.002(3) O2 0.0281(19) 0.0326(18) 0.044(3) -0.0021(18) 0.0144(18) 0.0044(16) O9 0.0277(19) 0.0333(18) 0.044(3) -0.0025(18) 0.0145(18) 0.0052(16) O3 0.0289(18) 0.0344(18) 0.037(2) -0.0021(16) 0.0130(17) -0.0009(14) O5 0.020(3) 0.030(3) 0.033(4) -0.001(3) 0.021(3) -0.007(2) O6 0.036(2) 0.0345(19) 0.037(3) -0.0044(17) 0.0141(19) -0.0051(16) O7 0.030(3) 0.033(3) 0.044(4) -0.007(3) 0.016(3) 0.000(2) O8 0.0297(17) 0.0351(17) 0.038(2) -0.0017(15) 0.0127(16) -0.0014(13) O10 0.0281(19) 0.035(2) 0.038(3) 0.0020(19) 0.018(2) -0.0008(18) O11 0.029(2) 0.037(2) 0.038(3) 0.0014(19) 0.018(2) -0.0013(17) O12 0.029(2) 0.031(2) 0.031(3) 0.0012(19) 0.013(2) 0.0002(17) C1 0.020(3) 0.030(3) 0.033(4) -0.001(3) 0.021(3) -0.007(2) C2 0.0367(19) 0.0347(18) 0.038(2) -0.0040(16) 0.0139(18) -0.0050(15) C3 0.0385(17) 0.0347(17) 0.038(2) -0.0038(15) 0.0134(17) -0.0054(14) C4 0.0393(18) 0.0347(17) 0.039(2) -0.0034(16) 0.0142(17) -0.0052(15) C5 0.0404(18) 0.0348(17) 0.039(2) -0.0030(16) 0.0145(18) -0.0052(15) C6 0.040(2) 0.0349(19) 0.039(2) -0.0033(17) 0.015(2) -0.0052(17) C7 0.0402(18) 0.0353(18) 0.039(2) -0.0039(16) 0.0122(17) -0.0059(15) C8 0.043(2) 0.037(2) 0.038(3) -0.005(2) 0.014(2) -0.0061(19) C9 0.042(2) 0.036(2) 0.041(3) -0.004(2) 0.010(2) -0.0062(19) C10 0.042(2) 0.036(2) 0.040(3) -0.004(2) 0.011(2) -0.0064(19) C11 0.0421(19) 0.0353(18) 0.040(2) -0.0024(17) 0.0148(19) -0.0056(16) C12 0.045(2) 0.036(2) 0.042(3) -0.0015(19) 0.014(2) -0.004(2) C13 0.045(2) 0.036(2) 0.040(2) -0.0015(19) 0.015(2) -0.008(2) C14 0.043(2) 0.035(2) 0.041(3) -0.002(2) 0.015(2) -0.0069(19) C15 0.0301(16) 0.0354(16) 0.038(2) -0.0017(14) 0.0124(15) -0.0007(13) C16 0.0303(16) 0.0358(16) 0.038(2) -0.0015(14) 0.0125(15) -0.0009(12) C17 0.0317(16) 0.0373(16) 0.038(2) -0.0010(14) 0.0124(15) -0.0005(12) C18 0.0321(16) 0.0373(16) 0.038(2) -0.0006(14) 0.0121(16) 0.0000(13) C19 0.0327(16) 0.0372(16) 0.039(2) -0.0007(14) 0.0120(15) 0.0007(13) C20 0.0313(16) 0.0362(16) 0.038(2) -0.0013(15) 0.0121(16) 0.0002(13) C21 0.0327(17) 0.0390(17) 0.038(2) -0.0014(15) 0.0126(16) -0.0005(14) C22 0.0330(19) 0.039(2) 0.039(3) -0.001(2) 0.0136(19) -0.0014(18) C23 0.033(2) 0.040(2) 0.039(3) -0.0034(17) 0.013(2) -0.0024(19) C24 0.036(2) 0.043(2) 0.039(2) -0.001(2) 0.012(2) 0.001(2) C25 0.0342(17) 0.0381(17) 0.040(2) -0.0004(15) 0.0122(17) 0.0019(13) C26 0.037(2) 0.039(2) 0.040(3) -0.0009(18) 0.013(2) 0.003(2) C27 0.037(2) 0.039(2) 0.041(3) 0.001(2) 0.012(2) 0.0024(19) C28 0.0341(18) 0.039(2) 0.042(3) 0.000(2) 0.012(2) 0.0029(16) C29 0.0288(18) 0.0333(17) 0.044(3) -0.0025(17) 0.0143(17) 0.0047(15) C30 0.0308(18) 0.0336(17) 0.045(3) -0.0032(17) 0.0141(17) 0.0049(15) C31 0.0313(19) 0.0341(18) 0.045(3) -0.0039(18) 0.0141(18) 0.0053(16) C32 0.0325(19) 0.0345(18) 0.046(3) -0.0041(18) 0.0139(18) 0.0055(16) C33 0.033(2) 0.0342(18) 0.046(3) -0.0036(19) 0.0137(19) 0.0052(16) C34 0.0333(19) 0.0339(17) 0.046(3) -0.0032(19) 0.0138(19) 0.0046(16) C35 0.0323(19) 0.0337(17) 0.045(3) -0.0031(18) 0.0141(18) 0.0043(15) C36 0.029(2) 0.031(2) 0.031(3) 0.0010(18) 0.0132(19) -0.0001(16) C37 0.030(2) 0.031(2) 0.031(3) 0.0012(18) 0.0133(19) 0.0002(16) C38 0.030(2) 0.032(2) 0.032(3) 0.0013(18) 0.0134(19) 0.0007(16) C39 0.031(2) 0.032(2) 0.032(3) 0.0014(18) 0.013(2) 0.0009(17) C40 0.031(2) 0.032(2) 0.032(3) 0.0015(19) 0.014(2) 0.0006(17) C41 0.031(2) 0.032(2) 0.032(3) 0.0014(19) 0.0138(19) 0.0004(17) C42 0.030(2) 0.031(2) 0.032(3) 0.0012(18) 0.0136(19) 0.0003(16) C43 0.0285(19) 0.036(2) 0.038(3) 0.0018(18) 0.018(2) -0.0013(17) C44 0.0289(19) 0.037(2) 0.039(3) 0.0018(18) 0.019(2) -0.0018(17) C45 0.0293(19) 0.037(2) 0.038(3) 0.0015(18) 0.018(2) -0.0016(17) C46 0.030(2) 0.037(3) 0.040(3) 0.001(2) 0.018(2) -0.002(2) C47 0.030(2) 0.041(3) 0.039(3) 0.000(2) 0.019(2) -0.003(2) C48 0.030(3) 0.034(3) 0.044(4) -0.007(3) 0.015(3) 0.001(2) C49 0.031(3) 0.036(3) 0.046(4) -0.008(3) 0.016(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O5 1.960(6) . ? V1 O3 1.991(6) . ? V1 O1 1.995(5) 3_676 ? V1 O4 2.000(6) . ? V1 O2 2.006(6) . ? V1 O1 2.054(6) . ? V1 V1 3.011(3) 3_676 ? V1 V2 3.088(2) . ? V2 O8 1.863(6) . ? V2 O6 1.891(6) . ? V2 O7 1.944(6) . ? V2 O1 2.010(6) 3_676 ? V2 O5 2.035(6) 3_676 ? V2 O3 2.041(6) . ? V2 V3 3.116(2) 3_676 ? V3 O10 1.937(6) . ? V3 O11 1.980(6) . ? V3 O1 1.996(5) . ? V3 O7 2.021(6) 3_676 ? V3 O12 2.024(6) . ? V3 O9 2.026(6) . ? V3 V2 3.116(2) 3_676 ? O1 V1 1.995(5) 3_676 ? O1 V2 2.010(6) 3_676 ? O2 C29 1.219(10) . ? O9 C29 1.314(11) . ? O3 C15 1.378(10) . ? O4 C36 1.278(10) 3_676 ? O5 C1 1.385(9) . ? O5 V2 2.035(6) 3_676 ? O6 C2 1.391(11) . ? O7 C48 1.449(10) . ? O7 V3 2.021(6) 3_676 ? O8 C16 1.366(10) . ? O10 C43 1.267(10) . ? O11 C45 1.283(10) . ? O12 C36 1.251(10) . ? C1 C2 1.357(13) 3_676 ? C1 C6 1.374(12) 3_676 ? C2 C1 1.357(13) 3_676 ? C2 C3 1.409(12) . ? C3 C4 1.410(12) . ? C3 C7 1.514(13) . ? C4 C5 1.366(13) . ? C4 H4 0.9500 . ? C5 C6 1.417(12) . ? C5 C11 1.577(13) . ? C6 C1 1.374(12) 3_676 ? C6 H6 0.9500 . ? C7 C9 1.521(11) . ? C7 C8 1.536(12) . ? C7 C10 1.548(11) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C14 1.474(11) . ? C11 C12 1.530(12) . ? C11 C13 1.531(12) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? 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 C20 1.361(12) . ? C15 C16 1.415(13) . ? C16 C17 1.390(13) . ? C17 C18 1.417(12) . ? C17 C21 1.528(13) . ? C18 C19 1.401(13) . ? C18 H18 0.9500 . ? C19 C20 1.387(12) . ? C19 C25 1.546(12) . ? C20 H20 0.9500 . ? C21 C22 1.473(11) . ? C21 C24 1.545(12) . ? C21 C23 1.559(11) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? 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 C28 1.478(11) . ? C25 C26 1.516(12) . ? C25 C27 1.541(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 C30 1.542(12) . ? C30 C31 1.354(12) . ? C30 C35 1.415(12) . ? C31 C32 1.394(11) . ? C31 H31 0.9500 . ? C32 C33 1.388(12) . ? C32 H32 0.9500 . ? C33 C34 1.320(11) . ? C33 H33 0.9500 . ? C34 C35 1.403(11) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 O4 1.278(10) 3_676 ? C36 C37 1.502(13) . ? C37 C38 1.385(11) . ? C37 C42 1.397(12) . ? C38 C39 1.394(12) . ? C38 H38 0.9500 . ? C39 C40 1.363(11) . ? C39 H39 0.9500 . ? C40 C41 1.371(11) . ? C40 H40 0.9500 . ? C41 C42 1.379(12) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.405(12) . ? C43 C46 1.483(12) . ? C44 C45 1.399(12) . ? C44 H44 0.9500 . ? C45 C47 1.504(12) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.524(11) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 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 O5 V1 O3 173.5(3) . . ? O5 V1 O1 98.7(2) . 3_676 ? O3 V1 O1 80.1(2) . 3_676 ? O5 V1 O4 98.3(2) . . ? O3 V1 O4 88.2(2) . . ? O1 V1 O4 91.6(2) 3_676 . ? O5 V1 O2 85.0(2) . . ? O3 V1 O2 96.1(2) . . ? O1 V1 O2 176.1(2) 3_676 . ? O4 V1 O2 89.1(3) . . ? O5 V1 O1 77.6(2) . . ? O3 V1 O1 95.9(2) . . ? O1 V1 O1 83.9(2) 3_676 . ? O4 V1 O1 173.3(2) . . ? O2 V1 O1 95.7(2) . . ? O5 V1 V1 87.30(18) . 3_676 ? O3 V1 V1 87.49(18) . 3_676 ? O1 V1 V1 42.70(17) 3_676 3_676 ? O4 V1 V1 134.12(19) . 3_676 ? O2 V1 V1 136.8(2) . 3_676 ? O1 V1 V1 41.22(15) . 3_676 ? O5 V1 V2 138.38(17) . . ? O3 V1 V2 40.61(17) . . ? O1 V1 V2 39.73(16) 3_676 . ? O4 V1 V2 86.15(18) . . ? O2 V1 V2 136.56(19) . . ? O1 V1 V2 93.52(16) . . ? V1 V1 V2 62.11(7) 3_676 . ? O8 V2 O6 87.0(3) . . ? O8 V2 O7 88.3(3) . . ? O6 V2 O7 94.9(3) . . ? O8 V2 O1 122.4(2) . 3_676 ? O6 V2 O1 148.6(3) . 3_676 ? O7 V2 O1 76.8(2) . 3_676 ? O8 V2 O5 154.1(2) . 3_676 ? O6 V2 O5 79.4(3) . 3_676 ? O7 V2 O5 114.5(3) . 3_676 ? O1 V2 O5 76.9(2) 3_676 3_676 ? O8 V2 O3 80.2(3) . . ? O6 V2 O3 121.1(2) . . ? O7 V2 O3 141.1(2) . . ? O1 V2 O3 78.5(2) 3_676 . ? O5 V2 O3 88.1(2) 3_676 . ? O8 V2 V1 100.69(19) . . ? O6 V2 V1 155.1(2) . . ? O7 V2 V1 108.85(19) . . ? O1 V2 V1 39.39(15) 3_676 . ? O5 V2 V1 83.95(17) 3_676 . ? O3 V2 V1 39.42(17) . . ? O8 V2 V3 102.66(19) . 3_676 ? O6 V2 V3 131.21(19) . 3_676 ? O7 V2 V3 39.09(18) . 3_676 ? O1 V2 V3 38.78(15) 3_676 3_676 ? O5 V2 V3 102.85(16) 3_676 3_676 ? O3 V2 V3 107.68(17) . 3_676 ? V1 V2 V3 70.53(5) . 3_676 ? O10 V3 O11 89.8(3) . . ? O10 V3 O1 95.0(2) . . ? O11 V3 O1 175.0(3) . . ? O10 V3 O7 170.1(2) . 3_676 ? O11 V3 O7 99.7(2) . 3_676 ? O1 V3 O7 75.4(2) . 3_676 ? O10 V3 O12 90.3(2) . . ? O11 V3 O12 87.0(2) . . ? O1 V3 O12 91.6(2) . . ? O7 V3 O12 87.7(2) 3_676 . ? O10 V3 O9 95.0(3) . . ? O11 V3 O9 85.4(2) . . ? O1 V3 O9 95.4(2) . . ? O7 V3 O9 88.4(2) 3_676 . ? O12 V3 O9 170.8(3) . . ? O10 V3 V2 132.77(18) . 3_676 ? O11 V3 V2 135.89(19) . 3_676 ? O1 V3 V2 39.10(17) . 3_676 ? O7 V3 V2 37.33(17) 3_676 3_676 ? O12 V3 V2 82.63(17) . 3_676 ? O9 V3 V2 99.18(17) . 3_676 ? V1 O1 V3 127.6(3) 3_676 . ? V1 O1 V2 100.9(2) 3_676 3_676 ? V3 O1 V2 102.1(3) . 3_676 ? V1 O1 V1 96.1(2) 3_676 . ? V3 O1 V1 123.9(3) . . ? V2 O1 V1 101.5(2) 3_676 . ? C29 O2 V1 130.6(6) . . ? C29 O9 V3 128.8(6) . . ? C15 O3 V1 123.1(5) . . ? C15 O3 V2 111.6(6) . . ? V1 O3 V2 100.0(3) . . ? C36 O4 V1 136.9(6) 3_676 . ? C1 O5 V1 132.0(6) . . ? C1 O5 V2 113.5(5) . 3_676 ? V1 O5 V2 104.0(2) . 3_676 ? C2 O6 V2 117.2(6) . . ? C48 O7 V2 122.5(5) . . ? C48 O7 V3 126.2(5) . 3_676 ? V2 O7 V3 103.6(3) . 3_676 ? C16 O8 V2 118.9(6) . . ? C43 O10 V3 128.8(7) . . ? C45 O11 V3 126.5(6) . . ? C36 O12 V3 135.0(7) . . ? C2 C1 C6 122.9(9) 3_676 3_676 ? C2 C1 O5 113.6(9) 3_676 . ? C6 C1 O5 123.5(9) 3_676 . ? C1 C2 O6 115.5(8) 3_676 . ? C1 C2 C3 122.3(10) 3_676 . ? O6 C2 C3 122.2(9) . . ? C2 C3 C4 113.1(9) . . ? C2 C3 C7 122.3(9) . . ? C4 C3 C7 124.6(9) . . ? C5 C4 C3 126.2(9) . . ? C5 C4 H4 116.9 . . ? C3 C4 H4 116.9 . . ? C4 C5 C6 117.6(10) . . ? C4 C5 C11 121.3(9) . . ? C6 C5 C11 121.1(9) . . ? C1 C6 C5 117.9(10) 3_676 . ? C1 C6 H6 121.1 3_676 . ? C5 C6 H6 121.1 . . ? C3 C7 C9 111.5(8) . . ? C3 C7 C8 109.4(8) . . ? C9 C7 C8 110.0(8) . . ? C3 C7 C10 111.2(8) . . ? C9 C7 C10 107.2(7) . . ? C8 C7 C10 107.5(7) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C14 C11 C12 111.4(8) . . ? C14 C11 C13 109.4(9) . . ? C12 C11 C13 106.7(8) . . ? C14 C11 C5 110.1(8) . . ? C12 C11 C5 107.9(8) . . ? C13 C11 C5 111.3(8) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 O3 125.5(10) . . ? C20 C15 C16 119.9(10) . . ? O3 C15 C16 114.5(8) . . ? O8 C16 C17 124.7(10) . . ? O8 C16 C15 112.9(9) . . ? C17 C16 C15 122.5(9) . . ? C16 C17 C18 114.9(10) . . ? C16 C17 C21 122.5(9) . . ? C18 C17 C21 122.6(9) . . ? C19 C18 C17 123.6(10) . . ? C19 C18 H18 118.2 . . ? C17 C18 H18 118.2 . . ? C20 C19 C18 118.1(9) . . ? C20 C19 C25 122.8(10) . . ? C18 C19 C25 119.1(9) . . ? C15 C20 C19 120.9(10) . . ? C15 C20 H20 119.5 . . ? C19 C20 H20 119.5 . . ? C22 C21 C17 111.7(8) . . ? C22 C21 C24 108.8(8) . . ? C17 C21 C24 111.7(8) . . ? C22 C21 C23 111.7(8) . . ? C17 C21 C23 105.9(8) . . ? C24 C21 C23 106.9(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C28 C25 C26 111.0(8) . . ? C28 C25 C27 108.4(8) . . ? C26 C25 C27 106.9(8) . . ? C28 C25 C19 110.5(8) . . ? C26 C25 C19 112.0(8) . . ? C27 C25 C19 107.8(8) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O2 C29 O9 128.1(9) . . ? O2 C29 C30 119.7(9) . . ? O9 C29 C30 112.2(9) . . ? C31 C30 C35 121.9(9) . . ? C31 C30 C29 122.1(9) . . ? C35 C30 C29 116.0(9) . . ? C30 C31 C32 120.2(9) . . ? C30 C31 H31 119.9 . . ? C32 C31 H31 119.9 . . ? C33 C32 C31 117.7(9) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C34 C33 C32 122.4(9) . . ? C34 C33 H33 118.8 . . ? C32 C33 H33 118.8 . . ? C33 C34 C35 121.7(9) . . ? C33 C34 H34 119.2 . . ? C35 C34 H34 119.2 . . ? C34 C35 C30 116.1(9) . . ? C34 C35 H35 122.0 . . ? C30 C35 H35 122.0 . . ? O12 C36 O4 125.4(9) . 3_676 ? O12 C36 C37 117.8(9) . . ? O4 C36 C37 116.8(8) 3_676 . ? C38 C37 C42 119.8(9) . . ? C38 C37 C36 119.6(10) . . ? C42 C37 C36 120.6(9) . . ? C37 C38 C39 118.1(10) . . ? C37 C38 H38 120.9 . . ? C39 C38 H38 120.9 . . ? C40 C39 C38 122.0(9) . . ? C40 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? C39 C40 C41 119.6(9) . . ? C39 C40 H40 120.2 . . ? C41 C40 H40 120.2 . . ? C40 C41 C42 120.1(10) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C41 C42 C37 120.3(9) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? O10 C43 C44 123.2(9) . . ? O10 C43 C46 116.6(9) . . ? C44 C43 C46 120.1(8) . . ? C45 C44 C43 124.6(9) . . ? C45 C44 H44 117.7 . . ? C43 C44 H44 117.7 . . ? O11 C45 C44 124.6(9) . . ? O11 C45 C47 116.1(8) . . ? C44 C45 C47 119.3(8) . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? O7 C48 C49 109.0(8) . . ? O7 C48 H48A 109.9 . . ? C49 C48 H48A 109.9 . . ? O7 C48 H48B 109.9 . . ? C49 C48 H48B 109.9 . . ? H48A C48 H48B 108.3 . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 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 O5 V1 V2 O8 -130.0(3) . . . . ? O3 V1 V2 O8 59.8(3) . . . . ? O1 V1 V2 O8 -129.0(3) 3_676 . . . ? O4 V1 V2 O8 -31.8(2) . . . . ? O2 V1 V2 O8 52.7(4) . . . . ? O1 V1 V2 O8 154.9(2) . . . . ? V1 V1 V2 O8 -177.4(2) 3_676 . . . ? O5 V1 V2 O6 123.9(5) . . . . ? O3 V1 V2 O6 -46.4(5) . . . . ? O1 V1 V2 O6 124.8(5) 3_676 . . . ? O4 V1 V2 O6 -138.0(5) . . . . ? O2 V1 V2 O6 -53.5(6) . . . . ? O1 V1 V2 O6 48.7(5) . . . . ? V1 V1 V2 O6 76.4(5) 3_676 . . . ? O5 V1 V2 O7 -38.1(3) . . . . ? O3 V1 V2 O7 151.7(4) . . . . ? O1 V1 V2 O7 -37.2(3) 3_676 . . . ? O4 V1 V2 O7 60.0(3) . . . . ? O2 V1 V2 O7 144.6(4) . . . . ? O1 V1 V2 O7 -113.3(3) . . . . ? V1 V1 V2 O7 -85.6(2) 3_676 . . . ? O5 V1 V2 O1 -0.9(4) . . . 3_676 ? O3 V1 V2 O1 -171.1(4) . . . 3_676 ? O4 V1 V2 O1 97.2(3) . . . 3_676 ? O2 V1 V2 O1 -178.3(4) . . . 3_676 ? O1 V1 V2 O1 -76.1(3) . . . 3_676 ? V1 V1 V2 O1 -48.4(3) 3_676 . . 3_676 ? O5 V1 V2 O5 75.8(3) . . . 3_676 ? O3 V1 V2 O5 -94.5(3) . . . 3_676 ? O1 V1 V2 O5 76.7(3) 3_676 . . 3_676 ? O4 V1 V2 O5 173.9(2) . . . 3_676 ? O2 V1 V2 O5 -101.6(3) . . . 3_676 ? O1 V1 V2 O5 0.6(2) . . . 3_676 ? V1 V1 V2 O5 28.30(16) 3_676 . . 3_676 ? O5 V1 V2 O3 170.2(4) . . . . ? O1 V1 V2 O3 171.1(4) 3_676 . . . ? O4 V1 V2 O3 -91.7(3) . . . . ? O2 V1 V2 O3 -7.1(4) . . . . ? O1 V1 V2 O3 95.0(3) . . . . ? V1 V1 V2 O3 122.8(3) 3_676 . . . ? O5 V1 V2 V3 -30.2(3) . . . 3_676 ? O3 V1 V2 V3 159.6(3) . . . 3_676 ? O1 V1 V2 V3 -29.3(3) 3_676 . . 3_676 ? O4 V1 V2 V3 67.94(16) . . . 3_676 ? O2 V1 V2 V3 152.5(3) . . . 3_676 ? O1 V1 V2 V3 -105.37(15) . . . 3_676 ? V1 V1 V2 V3 -77.64(6) 3_676 . . 3_676 ? O10 V3 O1 V1 -52.4(4) . . . 3_676 ? O11 V3 O1 V1 113(3) . . . 3_676 ? O7 V3 O1 V1 125.2(4) 3_676 . . 3_676 ? O12 V3 O1 V1 38.0(4) . . . 3_676 ? O9 V3 O1 V1 -147.9(4) . . . 3_676 ? V2 V3 O1 V1 114.2(5) 3_676 . . 3_676 ? O10 V3 O1 V2 -166.6(3) . . . 3_676 ? O11 V3 O1 V2 -2(3) . . . 3_676 ? O7 V3 O1 V2 11.0(2) 3_676 . . 3_676 ? O12 V3 O1 V2 -76.2(3) . . . 3_676 ? O9 V3 O1 V2 97.9(3) . . . 3_676 ? O10 V3 O1 V1 80.4(3) . . . . ? O11 V3 O1 V1 -115(3) . . . . ? O7 V3 O1 V1 -102.0(3) 3_676 . . . ? O12 V3 O1 V1 170.8(3) . . . . ? O9 V3 O1 V1 -15.1(4) . . . . ? V2 V3 O1 V1 -113.0(4) 3_676 . . . ? O5 V1 O1 V1 -100.3(2) . . . 3_676 ? O3 V1 O1 V1 79.3(2) . . . 3_676 ? O1 V1 O1 V1 0.0 3_676 . . 3_676 ? O4 V1 O1 V1 -48(2) . . . 3_676 ? O2 V1 O1 V1 176.1(2) . . . 3_676 ? V2 V1 O1 V1 38.61(18) . . . 3_676 ? O5 V1 O1 V3 115.4(3) . . . . ? O3 V1 O1 V3 -65.0(3) . . . . ? O1 V1 O1 V3 -144.3(4) 3_676 . . . ? O4 V1 O1 V3 167.3(19) . . . . ? O2 V1 O1 V3 31.8(4) . . . . ? V1 V1 O1 V3 -144.3(4) 3_676 . . . ? V2 V1 O1 V3 -105.7(3) . . . . ? O5 V1 O1 V2 2.2(2) . . . 3_676 ? O3 V1 O1 V2 -178.3(2) . . . 3_676 ? O1 V1 O1 V2 102.4(3) 3_676 . . 3_676 ? O4 V1 O1 V2 54(2) . . . 3_676 ? O2 V1 O1 V2 -81.4(2) . . . 3_676 ? V1 V1 O1 V2 102.4(3) 3_676 . . 3_676 ? V2 V1 O1 V2 141.05(17) . . . 3_676 ? O5 V1 O2 C29 -100.3(9) . . . . ? O3 V1 O2 C29 73.3(9) . . . . ? O1 V1 O2 C29 61(5) 3_676 . . . ? O4 V1 O2 C29 161.4(9) . . . . ? O1 V1 O2 C29 -23.3(9) . . . . ? V1 V1 O2 C29 -19.6(10) 3_676 . . . ? V2 V1 O2 C29 78.0(9) . . . . ? O10 V3 O9 C29 -122.1(8) . . . . ? O11 V3 O9 C29 148.5(9) . . . . ? O1 V3 O9 C29 -26.6(9) . . . . ? O7 V3 O9 C29 48.5(9) 3_676 . . . ? O12 V3 O9 C29 113.4(16) . . . . ? V2 V3 O9 C29 12.7(9) 3_676 . . . ? O5 V1 O3 C15 151(2) . . . . ? O1 V1 O3 C15 -129.8(7) 3_676 . . . ? O4 V1 O3 C15 -37.8(7) . . . . ? O2 V1 O3 C15 51.1(7) . . . . ? O1 V1 O3 C15 147.5(7) . . . . ? V1 V1 O3 C15 -172.1(7) 3_676 . . . ? V2 V1 O3 C15 -124.0(8) . . . . ? O5 V1 O3 V2 -85(2) . . . . ? O1 V1 O3 V2 -5.7(3) 3_676 . . . ? O4 V1 O3 V2 86.2(3) . . . . ? O2 V1 O3 V2 175.1(3) . . . . ? O1 V1 O3 V2 -88.5(3) . . . . ? V1 V1 O3 V2 -48.1(2) 3_676 . . . ? O8 V2 O3 C15 11.2(5) . . . . ? O6 V2 O3 C15 -69.1(6) . . . . ? O7 V2 O3 C15 86.0(7) . . . . ? O1 V2 O3 C15 137.4(5) 3_676 . . . ? O5 V2 O3 C15 -145.6(5) 3_676 . . . ? V1 V2 O3 C15 131.7(6) . . . . ? V3 V2 O3 C15 111.5(5) 3_676 . . . ? O8 V2 O3 V1 -120.4(3) . . . . ? O6 V2 O3 V1 159.2(3) . . . . ? O7 V2 O3 V1 -45.7(5) . . . . ? O1 V2 O3 V1 5.7(3) 3_676 . . . ? O5 V2 O3 V1 82.7(3) 3_676 . . . ? V3 V2 O3 V1 -20.2(3) 3_676 . . . ? O5 V1 O4 C36 98.5(8) . . . 3_676 ? O3 V1 O4 C36 -80.5(8) . . . 3_676 ? O1 V1 O4 C36 -0.5(8) 3_676 . . 3_676 ? O2 V1 O4 C36 -176.7(8) . . . 3_676 ? O1 V1 O4 C36 48(2) . . . 3_676 ? V1 V1 O4 C36 4.2(9) 3_676 . . 3_676 ? V2 V1 O4 C36 -39.9(8) . . . 3_676 ? O3 V1 O5 C1 -147(2) . . . . ? O1 V1 O5 C1 135.1(7) 3_676 . . . ? O4 V1 O5 C1 42.2(7) . . . . ? O2 V1 O5 C1 -46.2(7) . . . . ? O1 V1 O5 C1 -143.2(7) . . . . ? V1 V1 O5 C1 176.4(7) 3_676 . . . ? V2 V1 O5 C1 135.7(6) . . . . ? O3 V1 O5 V2 -6(2) . . . 3_676 ? O1 V1 O5 V2 -83.9(3) 3_676 . . 3_676 ? O4 V1 O5 V2 -176.8(2) . . . 3_676 ? O2 V1 O5 V2 94.8(3) . . . 3_676 ? O1 V1 O5 V2 -2.2(2) . . . 3_676 ? V1 V1 O5 V2 -42.6(2) 3_676 . . 3_676 ? V2 V1 O5 V2 -83.3(3) . . . 3_676 ? O8 V2 O6 C2 -165.3(6) . . . . ? O7 V2 O6 C2 106.7(6) . . . . ? O1 V2 O6 C2 34.2(9) 3_676 . . . ? O5 V2 O6 C2 -7.4(6) 3_676 . . . ? O3 V2 O6 C2 -88.7(7) . . . . ? V1 V2 O6 C2 -56.2(9) . . . . ? V3 V2 O6 C2 90.5(6) 3_676 . . . ? O8 V2 O7 C48 -38.2(6) . . . . ? O6 V2 O7 C48 48.6(6) . . . . ? O1 V2 O7 C48 -162.1(6) 3_676 . . . ? O5 V2 O7 C48 129.2(6) 3_676 . . . ? O3 V2 O7 C48 -110.3(7) . . . . ? V1 V2 O7 C48 -138.9(6) . . . . ? V3 V2 O7 C48 -150.8(8) 3_676 . . . ? O8 V2 O7 V3 112.6(3) . . . 3_676 ? O6 V2 O7 V3 -160.6(3) . . . 3_676 ? O1 V2 O7 V3 -11.3(3) 3_676 . . 3_676 ? O5 V2 O7 V3 -80.0(3) 3_676 . . 3_676 ? O3 V2 O7 V3 40.5(6) . . . 3_676 ? V1 V2 O7 V3 11.9(3) . . . 3_676 ? O6 V2 O8 C16 109.6(6) . . . . ? O7 V2 O8 C16 -155.4(6) . . . . ? O1 V2 O8 C16 -82.3(6) 3_676 . . . ? O5 V2 O8 C16 51.7(9) 3_676 . . . ? O3 V2 O8 C16 -12.7(6) . . . . ? V1 V2 O8 C16 -46.6(6) . . . . ? V3 V2 O8 C16 -118.8(5) 3_676 . . . ? O11 V3 O10 C43 -17.4(7) . . . . ? O1 V3 O10 C43 161.3(7) . . . . ? O7 V3 O10 C43 147.9(14) 3_676 . . . ? O12 V3 O10 C43 69.7(7) . . . . ? O9 V3 O10 C43 -102.8(7) . . . . ? V2 V3 O10 C43 149.9(6) 3_676 . . . ? O10 V3 O11 C45 11.3(7) . . . . ? O1 V3 O11 C45 -154(3) . . . . ? O7 V3 O11 C45 -166.1(7) 3_676 . . . ? O12 V3 O11 C45 -79.0(7) . . . . ? O9 V3 O11 C45 106.3(7) . . . . ? V2 V3 O11 C45 -155.2(6) 3_676 . . . ? O10 V3 O12 C36 77.3(8) . . . . ? O11 V3 O12 C36 167.1(8) . . . . ? O1 V3 O12 C36 -17.7(8) . . . . ? O7 V3 O12 C36 -93.0(8) 3_676 . . . ? O9 V3 O12 C36 -157.8(14) . . . . ? V2 V3 O12 C36 -55.8(8) 3_676 . . . ? V1 O5 C1 C2 144.9(7) . . . 3_676 ? V2 O5 C1 C2 6.6(9) 3_676 . . 3_676 ? V1 O5 C1 C6 -35.2(12) . . . 3_676 ? V2 O5 C1 C6 -173.5(7) 3_676 . . 3_676 ? V2 O6 C2 C1 6.0(11) . . . 3_676 ? V2 O6 C2 C3 -174.9(7) . . . . ? C1 C2 C3 C4 -0.1(13) 3_676 . . . ? O6 C2 C3 C4 -179.1(8) . . . . ? C1 C2 C3 C7 178.6(9) 3_676 . . . ? O6 C2 C3 C7 -0.4(14) . . . . ? C2 C3 C4 C5 -1.6(15) . . . . ? C7 C3 C4 C5 179.7(9) . . . . ? C3 C4 C5 C6 1.7(15) . . . . ? C3 C4 C5 C11 -179.0(9) . . . . ? C4 C5 C6 C1 -0.1(13) . . . 3_676 ? C11 C5 C6 C1 -179.4(9) . . . 3_676 ? C2 C3 C7 C9 -58.1(12) . . . . ? C4 C3 C7 C9 120.4(10) . . . . ? C2 C3 C7 C8 63.7(11) . . . . ? C4 C3 C7 C8 -117.8(10) . . . . ? C2 C3 C7 C10 -177.7(8) . . . . ? C4 C3 C7 C10 0.8(13) . . . . ? C4 C5 C11 C14 -55.7(12) . . . . ? C6 C5 C11 C14 123.6(9) . . . . ? C4 C5 C11 C12 66.1(11) . . . . ? C6 C5 C11 C12 -114.6(10) . . . . ? C4 C5 C11 C13 -177.1(9) . . . . ? C6 C5 C11 C13 2.2(12) . . . . ? V1 O3 C15 C20 -67.0(11) . . . . ? V2 O3 C15 C20 174.3(7) . . . . ? V1 O3 C15 C16 110.3(8) . . . . ? V2 O3 C15 C16 -8.4(9) . . . . ? V2 O8 C16 C17 -169.1(7) . . . . ? V2 O8 C16 C15 11.6(10) . . . . ? C20 C15 C16 O8 176.4(8) . . . . ? O3 C15 C16 O8 -1.1(11) . . . . ? C20 C15 C16 C17 -3.0(14) . . . . ? O3 C15 C16 C17 179.6(8) . . . . ? O8 C16 C17 C18 -178.4(8) . . . . ? C15 C16 C17 C18 0.8(13) . . . . ? O8 C16 C17 C21 3.2(14) . . . . ? C15 C16 C17 C21 -177.6(8) . . . . ? C16 C17 C18 C19 2.6(14) . . . . ? C21 C17 C18 C19 -179.0(9) . . . . ? C17 C18 C19 C20 -3.9(14) . . . . ? C17 C18 C19 C25 179.5(8) . . . . ? O3 C15 C20 C19 178.8(8) . . . . ? C16 C15 C20 C19 1.7(14) . . . . ? C18 C19 C20 C15 1.6(14) . . . . ? C25 C19 C20 C15 178.1(8) . . . . ? C16 C17 C21 C22 -55.2(12) . . . . ? C18 C17 C21 C22 126.5(9) . . . . ? C16 C17 C21 C24 -177.4(8) . . . . ? C18 C17 C21 C24 4.3(12) . . . . ? C16 C17 C21 C23 66.6(11) . . . . ? C18 C17 C21 C23 -111.6(9) . . . . ? C20 C19 C25 C28 -109.6(10) . . . . ? C18 C19 C25 C28 66.8(11) . . . . ? C20 C19 C25 C26 14.7(13) . . . . ? C18 C19 C25 C26 -168.9(8) . . . . ? C20 C19 C25 C27 132.1(9) . . . . ? C18 C19 C25 C27 -51.5(11) . . . . ? V1 O2 C29 O9 -13.1(16) . . . . ? V1 O2 C29 C30 167.4(6) . . . . ? V3 O9 C29 O2 46.4(15) . . . . ? V3 O9 C29 C30 -134.0(7) . . . . ? O2 C29 C30 C31 172.1(9) . . . . ? O9 C29 C30 C31 -7.5(15) . . . . ? O2 C29 C30 C35 -10.6(15) . . . . ? O9 C29 C30 C35 169.7(9) . . . . ? C35 C30 C31 C32 0.8(16) . . . . ? C29 C30 C31 C32 177.8(9) . . . . ? C30 C31 C32 C33 -1.5(16) . . . . ? C31 C32 C33 C34 1.0(16) . . . . ? C32 C33 C34 C35 0.3(17) . . . . ? C33 C34 C35 C30 -1.1(16) . . . . ? C31 C30 C35 C34 0.5(16) . . . . ? C29 C30 C35 C34 -176.7(9) . . . . ? V3 O12 C36 O4 -7.5(14) . . . 3_676 ? V3 O12 C36 C37 174.2(5) . . . . ? O12 C36 C37 C38 -167.9(8) . . . . ? O4 C36 C37 C38 13.7(12) 3_676 . . . ? O12 C36 C37 C42 11.9(12) . . . . ? O4 C36 C37 C42 -166.5(8) 3_676 . . . ? C42 C37 C38 C39 -1.5(13) . . . . ? C36 C37 C38 C39 178.3(8) . . . . ? C37 C38 C39 C40 0.7(13) . . . . ? C38 C39 C40 C41 0.1(13) . . . . ? C39 C40 C41 C42 -0.2(13) . . . . ? C40 C41 C42 C37 -0.6(13) . . . . ? C38 C37 C42 C41 1.5(13) . . . . ? C36 C37 C42 C41 -178.3(8) . . . . ? V3 O10 C43 C44 14.4(13) . . . . ? V3 O10 C43 C46 -166.4(6) . . . . ? O10 C43 C44 C45 0.4(15) . . . . ? C46 C43 C44 C45 -178.7(9) . . . . ? V3 O11 C45 C44 -2.8(13) . . . . ? V3 O11 C45 C47 176.6(6) . . . . ? C43 C44 C45 O11 -6.3(15) . . . . ? C43 C44 C45 C47 174.4(9) . . . . ? V2 O7 C48 C49 -134.6(6) . . . . ? V3 O7 C48 C49 81.3(8) 3_676 . . . ? _diffrn_measured_fraction_theta_max 0.794 _diffrn_reflns_theta_full 23.33 _diffrn_measured_fraction_theta_full 0.794 _refine_diff_density_max 0.639 _refine_diff_density_min -0.713 _refine_diff_density_rms 0.093 # Attachment 'complex-3new.CIF.txt' data_testpb1 _database_code_depnum_ccdc_archive 'CCDC 762901' #TrackingRef 'complex-3new.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H98 O11 V2' _chemical_formula_weight 1121.28 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.2421(8) _cell_length_b 14.0373(10) _cell_length_c 21.6847(16) _cell_angle_alpha 105.9570(10) _cell_angle_beta 93.7700(10) _cell_angle_gamma 95.8850(10) _cell_volume 3257.0(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 15525 _cell_measurement_theta_min 7.269 _cell_measurement_theta_max 62.953 _exptl_crystal_description plate _exptl_crystal_colour blue/black _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1208 _exptl_absorpt_coefficient_mu 0.340 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9414 _exptl_absorpt_correction_T_max 0.9832 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.78480 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SMX station 16.2' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 57516 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0496 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.63 _diffrn_reflns_theta_max 31.53 _reflns_number_total 15525 _reflns_number_gt 13200 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SAINT' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; The structure was solved by direct methods. Data processing was carried out to 0.85 angstroms. All non hydrogen atoms were resolved anisotropically. H9 and H10 of O9 and O10 coordinated ethanols were found as electron density and labelled, not calculated. The methyls of tertiary butyl group C40, C41 and C42 are disordered over two sites. Structural and geometrical constraints have been applied to these. The Ueq(max)/Ueq(min) ratio is slightly high for C41X of the split tert-butyl group and its associated hydrogens. However, it was not split further as the ratio was <10:1 and no further chemical information would be gained from doing so. 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^)+(0.0960P)^2^+0.9810P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15525 _refine_ls_number_parameters 716 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0624 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1591 _refine_ls_wR_factor_gt 0.1512 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.083 _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 V1 V 0.79315(2) 1.03343(2) 0.291800(13) 0.01284(9) Uani 1 1 d . . . V2 V 0.72464(3) 0.81133(2) 0.191274(13) 0.01334(9) Uani 1 1 d . . . O1 O 0.64921(11) 0.92607(9) 0.24659(6) 0.0149(2) Uani 1 1 d . . . O2 O 0.67489(11) 1.07860(9) 0.34215(6) 0.0167(2) Uani 1 1 d . . . O3 O 0.79260(11) 1.11497(9) 0.23424(6) 0.0174(3) Uani 1 1 d . . . O4 O 0.91483(11) 1.13218(9) 0.33824(6) 0.0151(2) Uani 1 1 d . . . O5 O 0.85684(11) 0.92912(9) 0.22523(6) 0.0162(2) Uani 1 1 d . . . O6 O 0.84829(11) 0.76721(9) 0.14222(6) 0.0177(3) Uani 1 1 d . . . O7 O 0.74159(11) 0.76828(9) 0.26843(6) 0.0174(3) Uani 1 1 d . . . O8 O 0.61733(11) 0.69441(9) 0.16331(6) 0.0160(2) Uani 1 1 d . . . O9 O 0.83972(12) 0.94206(10) 0.34821(6) 0.0192(3) Uani 1 1 d . . . H9 H 0.815(2) 0.885(2) 0.3312(13) 0.035(7) Uiso 1 1 d . . . O10 O 0.64349(13) 0.85554(10) 0.11842(6) 0.0218(3) Uani 1 1 d . . . H10 H 0.652(3) 0.916(2) 0.1222(14) 0.047(8) Uiso 1 1 d . . . C1 C 0.55877(15) 0.92871(12) 0.28610(8) 0.0145(3) Uani 1 1 d . . . C2 C 0.57277(15) 1.01527(12) 0.33882(8) 0.0145(3) Uani 1 1 d . . . C3 C 0.48682(15) 1.03299(12) 0.38318(8) 0.0146(3) Uani 1 1 d . . . C4 C 0.38793(16) 0.95867(13) 0.37204(8) 0.0168(3) Uani 1 1 d . . . H4A H 0.3294 0.9677 0.4008 0.020 Uiso 1 1 calc R . . C5 C 0.37231(15) 0.87173(13) 0.32021(8) 0.0158(3) Uani 1 1 d . . . C6 C 0.46016(15) 0.85677(13) 0.27635(8) 0.0167(3) Uani 1 1 d . . . H6A H 0.4521 0.7997 0.2415 0.020 Uiso 1 1 calc R . . C7 C 0.49928(17) 1.13039(13) 0.43827(9) 0.0186(3) Uani 1 1 d . . . C8 C 0.4006(2) 1.12920(15) 0.48399(10) 0.0290(4) Uani 1 1 d . . . H8A H 0.3232 1.1173 0.4599 0.043 Uiso 1 1 calc R . . H8B H 0.4084 1.1924 0.5163 0.043 Uiso 1 1 calc R . . H8C H 0.4088 1.0771 0.5043 0.043 Uiso 1 1 calc R . . C9 C 0.48834(19) 1.21724(14) 0.40846(10) 0.0256(4) Uani 1 1 d . . . H9A H 0.4125 1.2060 0.3828 0.038 Uiso 1 1 calc R . . H9B H 0.5524 1.2211 0.3818 0.038 Uiso 1 1 calc R . . H9C H 0.4932 1.2787 0.4422 0.038 Uiso 1 1 calc R . . C10 C 0.62130(19) 1.14982(15) 0.47933(9) 0.0256(4) Uani 1 1 d . . . H10A H 0.6290 1.0962 0.4983 0.038 Uiso 1 1 calc R . . H10B H 0.6258 1.2116 0.5128 0.038 Uiso 1 1 calc R . . H10C H 0.6851 1.1538 0.4525 0.038 Uiso 1 1 calc R . . C11 C 0.26401(16) 0.79101(13) 0.31006(9) 0.0188(4) Uani 1 1 d . . . C12 C 0.17071(18) 0.82230(16) 0.35793(11) 0.0299(5) Uani 1 1 d . . . H12A H 0.2075 0.8354 0.4011 0.045 Uiso 1 1 calc R . . H12B H 0.1053 0.7695 0.3500 0.045 Uiso 1 1 calc R . . H12C H 0.1410 0.8816 0.3526 0.045 Uiso 1 1 calc R . . C13 C 0.20200(18) 0.77038(17) 0.24169(10) 0.0295(4) Uani 1 1 d . . . H13A H 0.1739 0.8303 0.2365 0.044 Uiso 1 1 calc R . . H13B H 0.1351 0.7191 0.2349 0.044 Uiso 1 1 calc R . . H13C H 0.2582 0.7488 0.2108 0.044 Uiso 1 1 calc R . . C14 C 0.30920(19) 0.69557(15) 0.31882(11) 0.0292(4) Uani 1 1 d . . . H14A H 0.3477 0.7089 0.3617 0.044 Uiso 1 1 calc R . . H14B H 0.3656 0.6739 0.2881 0.044 Uiso 1 1 calc R . . H14C H 0.2425 0.6442 0.3121 0.044 Uiso 1 1 calc R . . C15 C 0.85856(15) 1.20538(12) 0.25922(8) 0.0156(3) Uani 1 1 d . . . C16 C 0.92571(15) 1.21616(12) 0.31820(8) 0.0146(3) Uani 1 1 d . . . C17 C 0.99638(15) 1.30675(13) 0.35117(8) 0.0168(3) Uani 1 1 d . . . C18 C 0.99986(16) 1.38140(13) 0.31973(9) 0.0206(4) Uani 1 1 d . . . H18A H 1.0474 1.4417 0.3398 0.025 Uiso 1 1 calc R . . C19 C 0.93603(16) 1.37129(13) 0.25960(9) 0.0198(4) Uani 1 1 d . . . C20 C 0.86348(16) 1.28143(13) 0.22943(9) 0.0190(3) Uani 1 1 d . . . H20A H 0.8192 1.2726 0.1901 0.023 Uiso 1 1 calc R . . C21 C 1.06143(17) 1.32211(14) 0.41801(9) 0.0220(4) Uani 1 1 d . . . C22 C 0.9699(2) 1.30325(17) 0.46436(10) 0.0331(5) Uani 1 1 d . . . H22A H 0.9112 1.3490 0.4671 0.050 Uiso 1 1 calc R . . H22B H 1.0108 1.3131 0.5063 0.050 Uiso 1 1 calc R . . H22C H 0.9306 1.2359 0.4486 0.050 Uiso 1 1 calc R . . C23 C 1.1259(2) 1.42910(16) 0.44607(11) 0.0369(5) Uani 1 1 d . . . H23A H 1.0683 1.4758 0.4495 0.055 Uiso 1 1 calc R . . H23B H 1.1845 1.4422 0.4182 0.055 Uiso 1 1 calc R . . H23C H 1.1653 1.4360 0.4880 0.055 Uiso 1 1 calc R . . C24 C 1.1558(2) 1.24941(17) 0.41339(12) 0.0365(5) Uani 1 1 d . . . H24A H 1.2126 1.2616 0.3844 0.055 Uiso 1 1 calc R . . H24B H 1.1168 1.1820 0.3975 0.055 Uiso 1 1 calc R . . H24C H 1.1968 1.2591 0.4553 0.055 Uiso 1 1 calc R . . C25 C 0.95107(18) 1.45607(15) 0.22750(10) 0.0265(4) Uani 1 1 d . . . C26 C 0.9538(2) 1.55822(15) 0.27667(12) 0.0337(5) Uani 1 1 d . . . H26A H 1.0183 1.5672 0.3098 0.051 Uiso 1 1 calc R . . H26B H 0.8789 1.5619 0.2955 0.051 Uiso 1 1 calc R . . H26C H 0.9659 1.6097 0.2555 0.051 Uiso 1 1 calc R . . C27 C 0.8464(3) 1.4462(2) 0.17581(14) 0.0484(7) Uani 1 1 d . . . H27A H 0.8420 1.3828 0.1439 0.073 Uiso 1 1 calc R . . H27B H 0.8594 1.4989 0.1557 0.073 Uiso 1 1 calc R . . H27C H 0.7724 1.4507 0.1956 0.073 Uiso 1 1 calc R . . C28 C 1.0704(2) 1.45087(18) 0.19645(13) 0.0419(6) Uani 1 1 d . . . H28A H 1.1353 1.4569 0.2289 0.063 Uiso 1 1 calc R . . H28B H 1.0832 1.5044 0.1771 0.063 Uiso 1 1 calc R . . H28C H 1.0672 1.3881 0.1640 0.063 Uiso 1 1 calc R . . C29 C 0.95374(15) 0.92382(12) 0.19078(8) 0.0143(3) Uani 1 1 d . . . C30 C 0.94787(15) 0.83181(13) 0.14354(8) 0.0150(3) Uani 1 1 d . . . C31 C 1.04083(16) 0.81278(13) 0.10308(8) 0.0160(3) Uani 1 1 d . . . C32 C 1.13547(16) 0.89014(14) 0.11327(8) 0.0192(4) Uani 1 1 d . . . H32A H 1.1974 0.8801 0.0867 0.023 Uiso 1 1 calc R . . C33 C 1.14302(16) 0.98196(13) 0.16102(9) 0.0184(3) Uani 1 1 d . A . C34 C 1.04931(15) 0.99879(13) 0.20054(8) 0.0167(3) Uani 1 1 d . . . H34A H 1.0511 1.0588 0.2326 0.020 Uiso 1 1 calc R . . C35 C 1.03600(17) 0.71188(13) 0.05135(8) 0.0194(4) Uani 1 1 d . . . C36 C 0.9269(2) 0.69741(17) 0.00178(10) 0.0334(5) Uani 1 1 d . . . H36A H 0.9331 0.7505 -0.0183 0.050 Uiso 1 1 calc R . . H36B H 0.8546 0.6981 0.0231 0.050 Uiso 1 1 calc R . . H36C H 0.9247 0.6346 -0.0305 0.050 Uiso 1 1 calc R . . C37 C 1.0267(2) 0.62686(14) 0.08347(10) 0.0261(4) Uani 1 1 d . . . H37A H 1.0237 0.5640 0.0512 0.039 Uiso 1 1 calc R . . H37B H 0.9550 0.6278 0.1053 0.039 Uiso 1 1 calc R . . H37C H 1.0956 0.6357 0.1140 0.039 Uiso 1 1 calc R . . C38 C 1.1500(2) 0.70457(16) 0.01546(11) 0.0340(5) Uani 1 1 d . . . H38A H 1.1586 0.7566 -0.0054 0.051 Uiso 1 1 calc R . . H38B H 1.1435 0.6408 -0.0163 0.051 Uiso 1 1 calc R . . H38C H 1.2190 0.7117 0.0457 0.051 Uiso 1 1 calc R . . C39 C 1.24979(18) 1.06454(15) 0.17058(10) 0.0254(4) Uani 1 1 d . . . C40X C 1.2369(9) 1.1610(7) 0.2231(5) 0.052(2) Uani 0.290(5) 1 d PU A 1 H40A H 1.3068 1.2086 0.2271 0.078 Uiso 0.290(5) 1 calc PR A 1 H40B H 1.2291 1.1464 0.2634 0.078 Uiso 0.290(5) 1 calc PR A 1 H40C H 1.1668 1.1884 0.2114 0.078 Uiso 0.290(5) 1 calc PR A 1 C41X C 1.2183(9) 1.1310(7) 0.1317(5) 0.124(3) Uani 0.710(5) 1 d PU A 1 H41A H 1.2600 1.1968 0.1512 0.186 Uiso 0.710(5) 1 calc PR A 1 H41B H 1.1333 1.1338 0.1297 0.186 Uiso 0.710(5) 1 calc PR A 1 H41C H 1.2412 1.1058 0.0890 0.186 Uiso 0.710(5) 1 calc PR A 1 C42X C 1.3627(9) 1.0289(9) 0.1933(6) 0.066(3) Uani 0.290(5) 1 d PU A 1 H42A H 1.3757 0.9677 0.1629 0.099 Uiso 0.290(5) 1 calc PR A 1 H42B H 1.3540 1.0178 0.2347 0.099 Uiso 0.290(5) 1 calc PR A 1 H42C H 1.4302 1.0786 0.1969 0.099 Uiso 0.290(5) 1 calc PR A 1 C40Y C 1.2993(3) 1.0992(3) 0.24164(17) 0.0482(11) Uani 0.710(5) 1 d PU A 2 H40D H 1.3680 1.1485 0.2474 0.072 Uiso 0.710(5) 1 calc PR A 2 H40E H 1.3224 1.0432 0.2547 0.072 Uiso 0.710(5) 1 calc PR A 2 H40F H 1.2385 1.1277 0.2674 0.072 Uiso 0.710(5) 1 calc PR A 2 C41Y C 1.2021(16) 1.1636(11) 0.1662(9) 0.064(3) Uani 0.290(5) 1 d PU A 2 H41D H 1.2663 1.2177 0.1800 0.095 Uiso 0.290(5) 1 calc PR A 2 H41E H 1.1383 1.1771 0.1934 0.095 Uiso 0.290(5) 1 calc PR A 2 H41F H 1.1725 1.1567 0.1224 0.095 Uiso 0.290(5) 1 calc PR A 2 C42Y C 1.3539(4) 1.0271(4) 0.1334(2) 0.0680(16) Uani 0.710(5) 1 d PU A 2 H42D H 1.3305 1.0110 0.0880 0.102 Uiso 0.710(5) 1 calc PR A 2 H42E H 1.3752 0.9685 0.1439 0.102 Uiso 0.710(5) 1 calc PR A 2 H42F H 1.4217 1.0782 0.1449 0.102 Uiso 0.710(5) 1 calc PR A 2 C43 C 0.67166(15) 0.68220(12) 0.26514(8) 0.0155(3) Uani 1 1 d . . . C44 C 0.60410(15) 0.63848(12) 0.20528(8) 0.0153(3) Uani 1 1 d . . . C45 C 0.53029(16) 0.54696(13) 0.19295(8) 0.0170(3) Uani 1 1 d . . . C46 C 0.52364(16) 0.50610(13) 0.24478(9) 0.0193(4) Uani 1 1 d . . . H46A H 0.4751 0.4457 0.2383 0.023 Uiso 1 1 calc R . . C47 C 0.58571(16) 0.55058(13) 0.30610(9) 0.0180(3) Uani 1 1 d . . . C48 C 0.66197(16) 0.63984(13) 0.31576(8) 0.0185(3) Uani 1 1 d . . . H48A H 0.7055 0.6704 0.3555 0.022 Uiso 1 1 calc R . . C49 C 0.46325(16) 0.49529(13) 0.12616(9) 0.0200(4) Uani 1 1 d . . . C50 C 0.3895(2) 0.39571(15) 0.12422(10) 0.0307(5) Uani 1 1 d . . . H50A H 0.3306 0.4078 0.1546 0.046 Uiso 1 1 calc R . . H50B H 0.4421 0.3518 0.1351 0.046 Uiso 1 1 calc R . . H50C H 0.3498 0.3654 0.0817 0.046 Uiso 1 1 calc R . . C51 C 0.55638(18) 0.47288(15) 0.07657(9) 0.0246(4) Uani 1 1 d . . . H51A H 0.6035 0.5341 0.0769 0.037 Uiso 1 1 calc R . . H51B H 0.5155 0.4421 0.0344 0.037 Uiso 1 1 calc R . . H51C H 0.6081 0.4285 0.0876 0.037 Uiso 1 1 calc R . . C52 C 0.37605(18) 0.56291(16) 0.10748(11) 0.0294(4) Uani 1 1 d . . . H52A H 0.3186 0.5764 0.1386 0.044 Uiso 1 1 calc R . . H52B H 0.3348 0.5298 0.0657 0.044 Uiso 1 1 calc R . . H52C H 0.4204 0.6246 0.1065 0.044 Uiso 1 1 calc R . . C53 C 0.57288(18) 0.50049(14) 0.36051(9) 0.0229(4) Uani 1 1 d . . . C54 C 0.4511(2) 0.4373(3) 0.35272(14) 0.0551(8) Uani 1 1 d . . . H54A H 0.4419 0.3861 0.3123 0.083 Uiso 1 1 calc R . . H54B H 0.3883 0.4790 0.3536 0.083 Uiso 1 1 calc R . . H54C H 0.4463 0.4071 0.3873 0.083 Uiso 1 1 calc R . . C55 C 0.6726(3) 0.4356(3) 0.36153(18) 0.0680(11) Uani 1 1 d . . . H55A H 0.6686 0.3861 0.3206 0.102 Uiso 1 1 calc R . . H55B H 0.6633 0.4032 0.3949 0.102 Uiso 1 1 calc R . . H55C H 0.7490 0.4764 0.3698 0.102 Uiso 1 1 calc R . . C56 C 0.5793(4) 0.5794(2) 0.42604(12) 0.0703(11) Uani 1 1 d . . . H56A H 0.5713 0.5468 0.4594 0.106 Uiso 1 1 calc R . . H56B H 0.5155 0.6198 0.4257 0.106 Uiso 1 1 calc R . . H56C H 0.6552 0.6209 0.4340 0.106 Uiso 1 1 calc R . . C57 C 0.8386(2) 0.96664(16) 0.41739(9) 0.0308(5) Uani 1 1 d . . . H57A H 0.7563 0.9683 0.4282 0.037 Uiso 1 1 calc R . . H57B H 0.8822 1.0326 0.4370 0.037 Uiso 1 1 calc R . . C58 C 0.8944(2) 0.89237(17) 0.44432(10) 0.0315(5) Uani 1 1 d . . . H58A H 0.8917 0.9106 0.4902 0.047 Uiso 1 1 calc R . . H58B H 0.9764 0.8917 0.4346 0.047 Uiso 1 1 calc R . . H58C H 0.8507 0.8272 0.4254 0.047 Uiso 1 1 calc R . . C59 C 0.61744(19) 0.79502(15) 0.05247(9) 0.0255(4) Uani 1 1 d . . . H59A H 0.6112 0.7250 0.0510 0.031 Uiso 1 1 calc R . . H59B H 0.6828 0.8087 0.0278 0.031 Uiso 1 1 calc R . . C60 C 0.50235(11) 0.81598(8) 0.02276(5) 0.0481(7) Uani 1 1 d . . . H60A H 0.4871 0.7749 -0.0211 0.072 Uiso 1 1 calc R . . H60B H 0.5089 0.8851 0.0236 0.072 Uiso 1 1 calc R . . H60C H 0.4374 0.8014 0.0467 0.072 Uiso 1 1 calc R . . O1S O 0.67355(11) 0.04089(8) 0.11770(5) 0.0316(3) Uani 1 1 d R . . H1S H 0.7100 0.0712 0.1528 0.047 Uiso 1 1 calc R . . C1S C 0.73272(11) 0.06875(8) 0.06765(5) 0.0389(5) Uani 1 1 d R . . H20B H 0.7319 0.1398 0.0738 0.047 Uiso 1 1 calc R . . H20C H 0.6878 0.0338 0.0265 0.047 Uiso 1 1 calc R . . C2S C 0.8595(3) 0.0463(3) 0.06536(15) 0.0548(7) Uani 1 1 d . . . H20D H 0.8938 0.0666 0.0309 0.082 Uiso 1 1 calc R . . H20E H 0.8611 -0.0242 0.0582 0.082 Uiso 1 1 calc R . . H20F H 0.9053 0.0819 0.1055 0.082 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 V1 0.01599(15) 0.00988(14) 0.01146(14) 0.00179(11) 0.00330(11) -0.00173(10) V2 0.01654(15) 0.01062(14) 0.01160(14) 0.00194(11) 0.00355(11) -0.00214(10) O1 0.0160(6) 0.0144(6) 0.0127(5) 0.0019(5) 0.0043(4) -0.0017(4) O2 0.0190(6) 0.0125(6) 0.0167(6) 0.0016(5) 0.0041(5) -0.0017(5) O3 0.0231(6) 0.0139(6) 0.0138(6) 0.0043(5) 0.0002(5) -0.0046(5) O4 0.0193(6) 0.0109(5) 0.0142(6) 0.0029(5) 0.0020(5) -0.0003(4) O5 0.0176(6) 0.0125(6) 0.0168(6) 0.0014(5) 0.0070(5) -0.0019(4) O6 0.0202(6) 0.0132(6) 0.0172(6) 0.0007(5) 0.0057(5) -0.0024(5) O7 0.0228(6) 0.0131(6) 0.0149(6) 0.0042(5) 0.0011(5) -0.0039(5) O8 0.0212(6) 0.0128(6) 0.0131(6) 0.0037(5) 0.0015(5) -0.0027(5) O9 0.0299(7) 0.0122(6) 0.0136(6) 0.0024(5) 0.0005(5) -0.0011(5) O10 0.0353(8) 0.0149(6) 0.0141(6) 0.0030(5) 0.0003(5) 0.0018(5) C1 0.0163(8) 0.0145(8) 0.0130(7) 0.0038(6) 0.0042(6) 0.0017(6) C2 0.0167(8) 0.0115(7) 0.0153(8) 0.0045(6) 0.0025(6) -0.0004(6) C3 0.0192(8) 0.0121(7) 0.0133(7) 0.0038(6) 0.0034(6) 0.0027(6) C4 0.0181(8) 0.0173(8) 0.0165(8) 0.0063(7) 0.0057(6) 0.0024(6) C5 0.0149(8) 0.0159(8) 0.0165(8) 0.0049(7) 0.0022(6) -0.0005(6) C6 0.0176(8) 0.0150(8) 0.0149(8) 0.0011(6) 0.0017(6) -0.0008(6) C7 0.0259(9) 0.0112(8) 0.0185(8) 0.0027(7) 0.0076(7) 0.0023(7) C8 0.0398(12) 0.0178(9) 0.0287(10) 0.0024(8) 0.0189(9) 0.0024(8) C9 0.0362(11) 0.0146(8) 0.0293(10) 0.0078(8) 0.0126(8) 0.0076(8) C10 0.0360(11) 0.0208(9) 0.0161(8) 0.0001(7) 0.0004(8) 0.0014(8) C11 0.0165(8) 0.0176(8) 0.0198(8) 0.0032(7) 0.0033(7) -0.0039(6) C12 0.0213(9) 0.0284(10) 0.0350(11) 0.0023(9) 0.0096(8) -0.0057(8) C13 0.0222(9) 0.0367(11) 0.0257(10) 0.0078(9) -0.0025(8) -0.0078(8) C14 0.0259(10) 0.0227(10) 0.0399(12) 0.0123(9) 0.0031(9) -0.0023(8) C15 0.0174(8) 0.0127(8) 0.0153(8) 0.0025(6) 0.0034(6) -0.0020(6) C16 0.0166(8) 0.0114(7) 0.0161(8) 0.0038(6) 0.0044(6) 0.0012(6) C17 0.0168(8) 0.0122(8) 0.0187(8) 0.0001(6) 0.0011(6) 0.0012(6) C18 0.0212(9) 0.0122(8) 0.0257(9) 0.0028(7) 0.0014(7) -0.0024(6) C19 0.0217(9) 0.0155(8) 0.0240(9) 0.0086(7) 0.0047(7) 0.0011(7) C20 0.0217(9) 0.0175(8) 0.0176(8) 0.0060(7) 0.0006(7) -0.0010(7) C21 0.0242(9) 0.0160(8) 0.0209(9) 0.0001(7) -0.0043(7) -0.0020(7) C22 0.0472(13) 0.0283(11) 0.0188(9) 0.0013(8) 0.0022(9) -0.0029(9) C23 0.0463(13) 0.0249(11) 0.0300(11) 0.0014(9) -0.0124(10) -0.0109(9) C24 0.0328(11) 0.0333(12) 0.0386(12) 0.0045(10) -0.0114(10) 0.0078(9) C25 0.0283(10) 0.0212(9) 0.0343(11) 0.0159(8) 0.0038(8) -0.0006(8) C26 0.0314(11) 0.0188(10) 0.0564(15) 0.0183(10) 0.0105(10) 0.0031(8) C27 0.0567(16) 0.0380(13) 0.0578(16) 0.0359(13) -0.0144(13) -0.0090(12) C28 0.0516(15) 0.0339(12) 0.0532(15) 0.0276(11) 0.0276(12) 0.0091(11) C29 0.0166(8) 0.0141(8) 0.0129(7) 0.0044(6) 0.0041(6) 0.0011(6) C30 0.0176(8) 0.0141(8) 0.0140(8) 0.0057(6) 0.0020(6) 0.0002(6) C31 0.0195(8) 0.0161(8) 0.0133(7) 0.0050(6) 0.0035(6) 0.0031(6) C32 0.0202(8) 0.0224(9) 0.0163(8) 0.0065(7) 0.0069(7) 0.0025(7) C33 0.0189(8) 0.0183(8) 0.0180(8) 0.0066(7) 0.0031(7) -0.0020(7) C34 0.0180(8) 0.0135(8) 0.0172(8) 0.0033(6) 0.0019(6) -0.0011(6) C35 0.0254(9) 0.0175(8) 0.0144(8) 0.0015(7) 0.0059(7) 0.0035(7) C36 0.0426(12) 0.0329(11) 0.0195(9) -0.0021(8) -0.0026(9) 0.0106(10) C37 0.0374(11) 0.0161(9) 0.0237(9) 0.0032(7) 0.0058(8) 0.0037(8) C38 0.0385(12) 0.0269(11) 0.0343(11) 0.0008(9) 0.0205(10) 0.0042(9) C39 0.0241(9) 0.0227(9) 0.0271(10) 0.0060(8) 0.0057(8) -0.0074(7) C40X 0.040(4) 0.043(4) 0.061(5) 0.005(4) 0.014(4) -0.030(3) C41X 0.105(5) 0.101(6) 0.178(8) 0.102(6) -0.057(6) -0.066(5) C42X 0.041(4) 0.059(4) 0.079(5) -0.002(4) 0.003(4) -0.022(4) C40Y 0.0396(19) 0.056(2) 0.0333(17) -0.0013(16) 0.0025(14) -0.0281(17) C41Y 0.051(4) 0.042(5) 0.108(7) 0.056(5) -0.023(6) -0.025(4) C42Y 0.038(2) 0.066(3) 0.067(3) -0.028(2) 0.0343(19) -0.0310(19) C43 0.0192(8) 0.0097(7) 0.0164(8) 0.0025(6) 0.0030(6) -0.0009(6) C44 0.0192(8) 0.0134(8) 0.0136(7) 0.0045(6) 0.0047(6) 0.0004(6) C45 0.0191(8) 0.0134(8) 0.0169(8) 0.0019(6) 0.0024(6) 0.0004(6) C46 0.0241(9) 0.0114(8) 0.0210(9) 0.0039(7) 0.0040(7) -0.0025(6) C47 0.0228(9) 0.0143(8) 0.0191(8) 0.0078(7) 0.0061(7) 0.0015(7) C48 0.0242(9) 0.0161(8) 0.0148(8) 0.0048(7) 0.0009(7) 0.0009(7) C49 0.0225(9) 0.0159(8) 0.0180(8) 0.0016(7) -0.0007(7) -0.0038(7) C50 0.0364(11) 0.0222(10) 0.0267(10) 0.0020(8) 0.0001(9) -0.0116(8) C51 0.0306(10) 0.0233(9) 0.0162(8) 0.0011(7) 0.0023(7) -0.0019(8) C52 0.0255(10) 0.0278(10) 0.0309(11) 0.0049(9) -0.0053(8) 0.0000(8) C53 0.0328(10) 0.0174(9) 0.0219(9) 0.0114(7) 0.0049(8) 0.0018(7) C54 0.0441(14) 0.082(2) 0.0533(16) 0.0528(16) 0.0005(12) -0.0171(14) C55 0.066(2) 0.090(2) 0.092(2) 0.078(2) 0.0448(18) 0.0469(18) C56 0.148(3) 0.0376(15) 0.0246(12) 0.0142(11) 0.0160(16) -0.0111(18) C57 0.0457(13) 0.0296(11) 0.0177(9) 0.0069(8) 0.0026(8) 0.0075(9) C58 0.0390(12) 0.0348(11) 0.0253(10) 0.0146(9) 0.0032(9) 0.0087(9) C59 0.0355(11) 0.0238(9) 0.0145(8) 0.0007(7) -0.0009(8) 0.0069(8) C60 0.0429(14) 0.0435(14) 0.0453(15) -0.0049(12) -0.0192(12) 0.0106(11) O1S 0.0447(9) 0.0247(7) 0.0222(7) 0.0085(6) -0.0092(6) -0.0075(6) C1S 0.0553(15) 0.0378(13) 0.0271(11) 0.0181(10) -0.0051(10) 0.0030(11) C2S 0.0536(17) 0.070(2) 0.0518(17) 0.0347(15) 0.0062(13) 0.0101(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O2 1.8288(12) . ? V1 O4 1.8627(12) . ? V1 O3 1.9115(12) . ? V1 O5 1.9823(12) . ? V1 O1 2.0808(12) . ? V1 O9 2.0814(13) . ? V2 O6 1.8591(13) . ? V2 O8 1.8621(12) . ? V2 O7 1.9336(12) . ? V2 O1 2.0257(12) . ? V2 O5 2.0415(12) . ? V2 O10 2.0442(13) . ? O1 C1 1.3690(19) . ? O2 C2 1.363(2) . ? O3 C15 1.353(2) . ? O4 C16 1.361(2) . ? O5 C29 1.358(2) . ? O6 C30 1.360(2) . ? O7 C43 1.354(2) . ? O8 C44 1.361(2) . ? O9 C57 1.445(2) . ? O9 H9 0.79(3) . ? O10 C59 1.442(2) . ? O10 H10 0.83(3) . ? C1 C6 1.384(2) . ? C1 C2 1.408(2) . ? C2 C3 1.400(2) . ? C3 C4 1.404(2) . ? C3 C7 1.535(2) . ? C4 C5 1.400(2) . ? C4 H4A 0.9300 . ? C5 C6 1.407(2) . ? C5 C11 1.536(2) . ? C6 H6A 0.9300 . ? C7 C8 1.537(3) . ? C7 C9 1.540(2) . ? C7 C10 1.542(3) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C13 1.534(3) . ? C11 C14 1.535(3) . ? C11 C12 1.535(3) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.390(2) . ? C15 C16 1.404(2) . ? C16 C17 1.406(2) . ? C17 C18 1.397(3) . ? C17 C21 1.529(3) . ? C18 C19 1.411(3) . ? C18 H18A 0.9300 . ? C19 C20 1.396(3) . ? C19 C25 1.536(2) . ? C20 H20A 0.9300 . ? C21 C24 1.535(3) . ? C21 C22 1.538(3) . ? C21 C23 1.539(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.530(3) . ? C25 C27 1.539(3) . ? C25 C28 1.539(3) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.387(2) . ? C29 C30 1.403(2) . ? C30 C31 1.408(2) . ? C31 C32 1.400(2) . ? C31 C35 1.539(2) . ? C32 C33 1.405(3) . ? C32 H32A 0.9300 . ? C33 C34 1.400(2) . ? C33 C39 1.542(2) . ? C34 H34A 0.9300 . ? C35 C36 1.535(3) . ? C35 C37 1.537(3) . ? C35 C38 1.541(3) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C41X 1.472(9) . ? C39 C42X 1.513(12) . ? C39 C42Y 1.521(4) . ? C39 C40Y 1.530(4) . ? C39 C40X 1.538(10) . ? C39 C41Y 1.565(15) . ? C40X H40A 0.9600 . ? C40X H40B 0.9600 . ? C40X H40C 0.9600 . ? C41X H41A 0.9600 . ? C41X H41B 0.9600 . ? C41X H41C 0.9600 . ? C42X H42A 0.9600 . ? C42X H42B 0.9600 . ? C42X H42C 0.9600 . ? C40Y H40D 0.9600 . ? C40Y H40E 0.9600 . ? C40Y H40F 0.9600 . ? C41Y H41D 0.9600 . ? C41Y H41E 0.9600 . ? C41Y H41F 0.9600 . ? C42Y H42D 0.9600 . ? C42Y H42E 0.9600 . ? C42Y H42F 0.9600 . ? C43 C48 1.390(2) . ? C43 C44 1.405(2) . ? C44 C45 1.405(2) . ? C45 C46 1.398(2) . ? C45 C49 1.536(2) . ? C46 C47 1.406(3) . ? C46 H46A 0.9300 . ? C47 C48 1.400(2) . ? C47 C53 1.538(2) . ? C48 H48A 0.9300 . ? C49 C50 1.539(3) . ? C49 C52 1.541(3) . ? C49 C51 1.543(3) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C55 1.518(3) . ? C53 C54 1.526(3) . ? C53 C56 1.535(3) . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 H55A 0.9600 . ? C55 H55B 0.9600 . ? C55 H55C 0.9600 . ? C56 H56A 0.9600 . ? C56 H56B 0.9600 . ? C56 H56C 0.9600 . ? C57 C58 1.497(3) . ? C57 H57A 0.9700 . ? C57 H57B 0.9700 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.500(2) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? O1S C1S 1.4313 . ? O1S H1S 0.8200 . ? C1S C2S 1.493(3) . ? C1S H20B 0.9700 . ? C1S H20C 0.9700 . ? C2S H20D 0.9600 . ? C2S H20E 0.9600 . ? C2S H20F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 V1 O4 95.77(5) . . ? O2 V1 O3 101.67(6) . . ? O4 V1 O3 83.02(5) . . ? O2 V1 O5 151.60(5) . . ? O4 V1 O5 111.65(5) . . ? O3 V1 O5 89.30(5) . . ? O2 V1 O1 79.72(5) . . ? O4 V1 O1 175.24(5) . . ? O3 V1 O1 99.32(5) . . ? O5 V1 O1 72.64(5) . . ? O2 V1 O9 92.13(5) . . ? O4 V1 O9 89.70(5) . . ? O3 V1 O9 164.94(6) . . ? O5 V1 O9 81.14(5) . . ? O1 V1 O9 88.95(5) . . ? O6 V2 O8 97.81(5) . . ? O6 V2 O7 107.38(6) . . ? O8 V2 O7 82.03(5) . . ? O6 V2 O1 149.04(5) . . ? O8 V2 O1 112.12(5) . . ? O7 V2 O1 85.25(5) . . ? O6 V2 O5 78.40(5) . . ? O8 V2 O5 172.99(5) . . ? O7 V2 O5 93.42(5) . . ? O1 V2 O5 72.60(5) . . ? O6 V2 O10 91.89(6) . . ? O8 V2 O10 87.11(5) . . ? O7 V2 O10 158.94(6) . . ? O1 V2 O10 82.21(5) . . ? O5 V2 O10 98.85(5) . . ? C1 O1 V2 132.04(10) . . ? C1 O1 V1 110.31(10) . . ? V2 O1 V1 105.00(5) . . ? C2 O2 V1 118.59(10) . . ? C15 O3 V1 113.03(10) . . ? C16 O4 V1 114.49(10) . . ? C29 O5 V1 136.27(10) . . ? C29 O5 V2 114.46(10) . . ? V1 O5 V2 108.13(5) . . ? C30 O6 V2 119.67(11) . . ? C43 O7 V2 114.06(10) . . ? C44 O8 V2 116.73(10) . . ? C57 O9 V1 125.06(12) . . ? C57 O9 H9 111.9(19) . . ? V1 O9 H9 111.5(19) . . ? C59 O10 V2 125.16(12) . . ? C59 O10 H10 113(2) . . ? V2 O10 H10 117(2) . . ? O1 C1 C6 125.33(15) . . ? O1 C1 C2 113.24(14) . . ? C6 C1 C2 121.41(15) . . ? O2 C2 C3 124.03(15) . . ? O2 C2 C1 114.49(14) . . ? C3 C2 C1 121.48(15) . . ? C2 C3 C4 115.77(15) . . ? C2 C3 C7 121.07(15) . . ? C4 C3 C7 123.10(15) . . ? C5 C4 C3 123.82(16) . . ? C5 C4 H4A 118.1 . . ? C3 C4 H4A 118.1 . . ? C4 C5 C6 118.82(15) . . ? C4 C5 C11 122.49(15) . . ? C6 C5 C11 118.68(15) . . ? C1 C6 C5 118.69(15) . . ? C1 C6 H6A 120.7 . . ? C5 C6 H6A 120.7 . . ? C3 C7 C8 111.70(15) . . ? C3 C7 C9 108.12(15) . . ? C8 C7 C9 108.74(15) . . ? C3 C7 C10 112.14(15) . . ? C8 C7 C10 107.29(16) . . ? C9 C7 C10 108.77(16) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C14 109.89(16) . . ? C13 C11 C12 107.99(16) . . ? C14 C11 C12 108.64(16) . . ? C13 C11 C5 109.28(15) . . ? C14 C11 C5 108.55(15) . . ? C12 C11 C5 112.48(15) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O3 C15 C20 124.07(16) . . ? O3 C15 C16 114.14(15) . . ? C20 C15 C16 121.77(15) . . ? O4 C16 C15 113.54(14) . . ? O4 C16 C17 125.47(15) . . ? C15 C16 C17 120.98(15) . . ? C18 C17 C16 115.70(16) . . ? C18 C17 C21 122.92(16) . . ? C16 C17 C21 121.36(16) . . ? C17 C18 C19 124.28(16) . . ? C17 C18 H18A 117.9 . . ? C19 C18 H18A 117.9 . . ? C20 C19 C18 118.31(16) . . ? C20 C19 C25 121.47(17) . . ? C18 C19 C25 120.16(17) . . ? C15 C20 C19 118.87(16) . . ? C15 C20 H20A 120.6 . . ? C19 C20 H20A 120.6 . . ? C17 C21 C24 109.40(16) . . ? C17 C21 C22 109.51(16) . . ? C24 C21 C22 109.87(18) . . ? C17 C21 C23 111.82(16) . . ? C24 C21 C23 108.20(18) . . ? C22 C21 C23 108.01(17) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C19 111.36(17) . . ? C26 C25 C27 107.04(19) . . ? C19 C25 C27 111.35(17) . . ? C26 C25 C28 109.45(18) . . ? C19 C25 C28 107.76(16) . . ? C27 C25 C28 109.9(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O5 C29 C34 125.11(15) . . ? O5 C29 C30 112.12(14) . . ? C34 C29 C30 122.77(15) . . ? O6 C30 C29 114.10(15) . . ? O6 C30 C31 125.78(15) . . ? C29 C30 C31 120.13(15) . . ? C32 C31 C30 116.03(16) . . ? C32 C31 C35 123.29(15) . . ? C30 C31 C35 120.68(15) . . ? C31 C32 C33 124.28(16) . . ? C31 C32 H32A 117.9 . . ? C33 C32 H32A 117.9 . . ? C34 C33 C32 118.43(16) . . ? C34 C33 C39 119.32(16) . . ? C32 C33 C39 122.25(16) . . ? C29 C34 C33 118.36(16) . . ? C29 C34 H34A 120.8 . . ? C33 C34 H34A 120.8 . . ? C36 C35 C37 109.70(17) . . ? C36 C35 C31 109.92(15) . . ? C37 C35 C31 109.54(14) . . ? C36 C35 C38 108.40(17) . . ? C37 C35 C38 107.14(16) . . ? C31 C35 C38 112.08(16) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C41X C39 C42X 137.1(7) . . ? C41X C39 C42Y 95.8(6) . . ? C42X C39 C42Y 50.3(5) . . ? C41X C39 C40Y 125.0(5) . . ? C42X C39 C40Y 59.1(5) . . ? C42Y C39 C40Y 105.8(3) . . ? C41X C39 C40X 78.3(6) . . ? C42X C39 C40X 105.0(6) . . ? C42Y C39 C40X 133.1(4) . . ? C40Y C39 C40X 50.1(5) . . ? C41X C39 C33 107.9(4) . . ? C42X C39 C33 109.3(4) . . ? C42Y C39 C33 112.3(2) . . ? C40Y C39 C33 109.25(19) . . ? C40X C39 C33 113.7(3) . . ? C41X C39 C41Y 30.6(7) . . ? C42X C39 C41Y 139.8(7) . . ? C42Y C39 C41Y 120.4(7) . . ? C40Y C39 C41Y 98.1(7) . . ? C40X C39 C41Y 48.7(8) . . ? C33 C39 C41Y 109.5(6) . . ? C39 C40X H40A 109.5 . . ? C39 C40X H40B 109.5 . . ? C39 C40X H40C 109.5 . . ? C39 C41X H41A 109.5 . . ? C39 C41X H41B 109.5 . . ? C39 C41X H41C 109.5 . . ? C39 C42X H42A 109.5 . . ? C39 C42X H42B 109.5 . . ? C39 C42X H42C 109.5 . . ? C39 C40Y H40D 109.5 . . ? C39 C40Y H40E 109.5 . . ? H40D C40Y H40E 109.5 . . ? C39 C40Y H40F 109.5 . . ? H40D C40Y H40F 109.5 . . ? H40E C40Y H40F 109.5 . . ? C39 C41Y H41D 109.5 . . ? C39 C41Y H41E 109.5 . . ? H41D C41Y H41E 109.5 . . ? C39 C41Y H41F 109.5 . . ? H41D C41Y H41F 109.5 . . ? H41E C41Y H41F 109.5 . . ? C39 C42Y H42D 109.5 . . ? C39 C42Y H42E 109.5 . . ? H42D C42Y H42E 109.5 . . ? C39 C42Y H42F 109.5 . . ? H42D C42Y H42F 109.5 . . ? H42E C42Y H42F 109.5 . . ? O7 C43 C48 124.78(16) . . ? O7 C43 C44 113.99(15) . . ? C48 C43 C44 121.20(15) . . ? O8 C44 C45 125.59(16) . . ? O8 C44 C43 113.11(14) . . ? C45 C44 C43 121.29(15) . . ? C46 C45 C44 115.79(16) . . ? C46 C45 C49 122.73(15) . . ? C44 C45 C49 121.47(15) . . ? C45 C46 C47 124.09(16) . . ? C45 C46 H46A 118.0 . . ? C47 C46 H46A 118.0 . . ? C48 C47 C46 118.38(16) . . ? C48 C47 C53 120.96(16) . . ? C46 C47 C53 120.64(16) . . ? C43 C48 C47 119.10(16) . . ? C43 C48 H48A 120.4 . . ? C47 C48 H48A 120.4 . . ? C45 C49 C50 111.96(16) . . ? C45 C49 C52 110.30(15) . . ? C50 C49 C52 107.83(16) . . ? C45 C49 C51 108.63(15) . . ? C50 C49 C51 107.96(16) . . ? C52 C49 C51 110.13(16) . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C55 C53 C54 109.7(2) . . ? C55 C53 C56 109.4(3) . . ? C54 C53 C56 105.7(2) . . ? C55 C53 C47 109.65(17) . . ? C54 C53 C47 111.74(17) . . ? C56 C53 C47 110.65(16) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56A 109.5 . . ? C53 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C53 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? O9 C57 C58 111.63(17) . . ? O9 C57 H57A 109.3 . . ? C58 C57 H57A 109.3 . . ? O9 C57 H57B 109.3 . . ? C58 C57 H57B 109.3 . . ? H57A C57 H57B 108.0 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? O10 C59 C60 111.08(15) . . ? O10 C59 H59A 109.4 . . ? C60 C59 H59A 109.4 . . ? O10 C59 H59B 109.4 . . ? C60 C59 H59B 109.4 . . ? H59A C59 H59B 108.0 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C1S O1S H1S 109.5 . . ? O1S C1S C2S 113.69(12) . . ? O1S C1S H20B 108.8 . . ? C2S C1S H20B 108.8 . . ? O1S C1S H20C 108.8 . . ? C2S C1S H20C 108.8 . . ? H20B C1S H20C 107.7 . . ? C1S C2S H20D 109.5 . . ? C1S C2S H20E 109.5 . . ? H20D C2S H20E 109.5 . . ? C1S C2S H20F 109.5 . . ? H20D C2S H20F 109.5 . . ? H20E C2S H20F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 V2 O1 C1 -167.34(13) . . . . ? O8 V2 O1 C1 28.41(15) . . . . ? O7 V2 O1 C1 -50.98(14) . . . . ? O5 V2 O1 C1 -146.07(15) . . . . ? O10 V2 O1 C1 112.06(14) . . . . ? O6 V2 O1 V1 -30.83(13) . . . . ? O8 V2 O1 V1 164.93(5) . . . . ? O7 V2 O1 V1 85.53(6) . . . . ? O5 V2 O1 V1 -9.56(5) . . . . ? O10 V2 O1 V1 -111.42(6) . . . . ? O2 V1 O1 C1 -16.58(10) . . . . ? O4 V1 O1 C1 2.2(7) . . . . ? O3 V1 O1 C1 -116.87(11) . . . . ? O5 V1 O1 C1 156.82(11) . . . . ? O9 V1 O1 C1 75.78(11) . . . . ? O2 V1 O1 V2 -163.55(6) . . . . ? O4 V1 O1 V2 -144.7(6) . . . . ? O3 V1 O1 V2 96.16(6) . . . . ? O5 V1 O1 V2 9.85(5) . . . . ? O9 V1 O1 V2 -71.20(6) . . . . ? O4 V1 O2 C2 -161.98(12) . . . . ? O3 V1 O2 C2 113.98(12) . . . . ? O5 V1 O2 C2 3.15(19) . . . . ? O1 V1 O2 C2 16.48(12) . . . . ? O9 V1 O2 C2 -72.07(12) . . . . ? O2 V1 O3 C15 83.57(12) . . . . ? O4 V1 O3 C15 -10.91(11) . . . . ? O5 V1 O3 C15 -122.82(11) . . . . ? O1 V1 O3 C15 164.90(11) . . . . ? O9 V1 O3 C15 -72.5(2) . . . . ? O2 V1 O4 C16 -88.93(11) . . . . ? O3 V1 O4 C16 12.17(11) . . . . ? O5 V1 O4 C16 98.61(11) . . . . ? O1 V1 O4 C16 -107.5(6) . . . . ? O9 V1 O4 C16 178.95(11) . . . . ? O2 V1 O5 C29 170.32(14) . . . . ? O4 V1 O5 C29 -25.63(17) . . . . ? O3 V1 O5 C29 56.57(16) . . . . ? O1 V1 O5 C29 156.57(17) . . . . ? O9 V1 O5 C29 -111.76(16) . . . . ? O2 V1 O5 V2 3.82(15) . . . . ? O4 V1 O5 V2 167.87(5) . . . . ? O3 V1 O5 V2 -109.93(6) . . . . ? O1 V1 O5 V2 -9.93(5) . . . . ? O9 V1 O5 V2 81.74(6) . . . . ? O6 V2 O5 C29 9.44(11) . . . . ? O8 V2 O5 C29 67.2(4) . . . . ? O7 V2 O5 C29 116.49(11) . . . . ? O1 V2 O5 C29 -159.58(12) . . . . ? O10 V2 O5 C29 -80.68(11) . . . . ? O6 V2 O5 V1 179.23(7) . . . . ? O8 V2 O5 V1 -123.0(4) . . . . ? O7 V2 O5 V1 -73.72(6) . . . . ? O1 V2 O5 V1 10.21(5) . . . . ? O10 V2 O5 V1 89.10(6) . . . . ? O8 V2 O6 C30 175.86(12) . . . . ? O7 V2 O6 C30 -100.10(12) . . . . ? O1 V2 O6 C30 10.57(19) . . . . ? O5 V2 O6 C30 -10.12(12) . . . . ? O10 V2 O6 C30 88.52(12) . . . . ? O6 V2 O7 C43 -96.64(12) . . . . ? O8 V2 O7 C43 -0.91(11) . . . . ? O1 V2 O7 C43 112.25(12) . . . . ? O5 V2 O7 C43 -175.55(11) . . . . ? O10 V2 O7 C43 58.7(2) . . . . ? O6 V2 O8 C44 105.53(12) . . . . ? O7 V2 O8 C44 -1.04(11) . . . . ? O1 V2 O8 C44 -82.57(12) . . . . ? O5 V2 O8 C44 48.8(5) . . . . ? O10 V2 O8 C44 -162.96(12) . . . . ? O2 V1 O9 C57 -36.18(16) . . . . ? O4 V1 O9 C57 59.58(16) . . . . ? O3 V1 O9 C57 120.4(2) . . . . ? O5 V1 O9 C57 171.56(16) . . . . ? O1 V1 O9 C57 -115.85(16) . . . . ? O6 V2 O10 C59 49.86(15) . . . . ? O8 V2 O10 C59 -47.87(15) . . . . ? O7 V2 O10 C59 -106.69(19) . . . . ? O1 V2 O10 C59 -160.67(15) . . . . ? O5 V2 O10 C59 128.41(15) . . . . ? V2 O1 C1 C6 -32.8(2) . . . . ? V1 O1 C1 C6 -167.63(14) . . . . ? V2 O1 C1 C2 148.86(12) . . . . ? V1 O1 C1 C2 14.00(17) . . . . ? V1 O2 C2 C3 166.84(13) . . . . ? V1 O2 C2 C1 -13.53(19) . . . . ? O1 C1 C2 O2 -2.1(2) . . . . ? C6 C1 C2 O2 179.50(15) . . . . ? O1 C1 C2 C3 177.58(15) . . . . ? C6 C1 C2 C3 -0.9(3) . . . . ? O2 C2 C3 C4 -179.53(15) . . . . ? C1 C2 C3 C4 0.9(2) . . . . ? O2 C2 C3 C7 3.2(3) . . . . ? C1 C2 C3 C7 -176.44(15) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C7 C3 C4 C5 176.74(16) . . . . ? C3 C4 C5 C6 0.1(3) . . . . ? C3 C4 C5 C11 178.95(16) . . . . ? O1 C1 C6 C5 -177.83(16) . . . . ? C2 C1 C6 C5 0.4(3) . . . . ? C4 C5 C6 C1 0.0(3) . . . . ? C11 C5 C6 C1 -178.93(16) . . . . ? C2 C3 C7 C8 -175.09(16) . . . . ? C4 C3 C7 C8 7.8(2) . . . . ? C2 C3 C7 C9 65.3(2) . . . . ? C4 C3 C7 C9 -111.79(19) . . . . ? C2 C3 C7 C10 -54.6(2) . . . . ? C4 C3 C7 C10 128.30(18) . . . . ? C4 C5 C11 C13 126.33(19) . . . . ? C6 C5 C11 C13 -54.8(2) . . . . ? C4 C5 C11 C14 -113.84(19) . . . . ? C6 C5 C11 C14 65.0(2) . . . . ? C4 C5 C11 C12 6.4(2) . . . . ? C6 C5 C11 C12 -174.74(17) . . . . ? V1 O3 C15 C20 -173.83(14) . . . . ? V1 O3 C15 C16 7.69(18) . . . . ? V1 O4 C16 C15 -11.15(18) . . . . ? V1 O4 C16 C17 169.15(14) . . . . ? O3 C15 C16 O4 2.0(2) . . . . ? C20 C15 C16 O4 -176.50(15) . . . . ? O3 C15 C16 C17 -178.28(15) . . . . ? C20 C15 C16 C17 3.2(3) . . . . ? O4 C16 C17 C18 176.28(16) . . . . ? C15 C16 C17 C18 -3.4(2) . . . . ? O4 C16 C17 C21 -5.5(3) . . . . ? C15 C16 C17 C21 174.82(16) . . . . ? C16 C17 C18 C19 1.5(3) . . . . ? C21 C17 C18 C19 -176.65(17) . . . . ? C17 C18 C19 C20 0.6(3) . . . . ? C17 C18 C19 C25 -176.87(17) . . . . ? O3 C15 C20 C19 -179.24(16) . . . . ? C16 C15 C20 C19 -0.9(3) . . . . ? C18 C19 C20 C15 -1.0(3) . . . . ? C25 C19 C20 C15 176.49(17) . . . . ? C18 C17 C21 C24 -118.0(2) . . . . ? C16 C17 C21 C24 63.9(2) . . . . ? C18 C17 C21 C22 121.53(19) . . . . ? C16 C17 C21 C22 -56.5(2) . . . . ? C18 C17 C21 C23 1.8(3) . . . . ? C16 C17 C21 C23 -176.23(17) . . . . ? C20 C19 C25 C26 140.83(19) . . . . ? C18 C19 C25 C26 -41.7(2) . . . . ? C20 C19 C25 C27 21.4(3) . . . . ? C18 C19 C25 C27 -161.1(2) . . . . ? C20 C19 C25 C28 -99.1(2) . . . . ? C18 C19 C25 C28 78.3(2) . . . . ? V1 O5 C29 C34 7.6(3) . . . . ? V2 O5 C29 C34 173.52(14) . . . . ? V1 O5 C29 C30 -173.12(12) . . . . ? V2 O5 C29 C30 -7.23(17) . . . . ? V2 O6 C30 C29 9.25(19) . . . . ? V2 O6 C30 C31 -171.37(13) . . . . ? O5 C29 C30 O6 -0.5(2) . . . . ? C34 C29 C30 O6 178.74(15) . . . . ? O5 C29 C30 C31 -179.96(15) . . . . ? C34 C29 C30 C31 -0.7(3) . . . . ? O6 C30 C31 C32 -179.58(16) . . . . ? C29 C30 C31 C32 -0.2(2) . . . . ? O6 C30 C31 C35 0.2(3) . . . . ? C29 C30 C31 C35 179.57(16) . . . . ? C30 C31 C32 C33 1.2(3) . . . . ? C35 C31 C32 C33 -178.60(17) . . . . ? C31 C32 C33 C34 -1.2(3) . . . . ? C31 C32 C33 C39 179.54(17) . . . . ? O5 C29 C34 C33 179.86(16) . . . . ? C30 C29 C34 C33 0.7(3) . . . . ? C32 C33 C34 C29 0.2(3) . . . . ? C39 C33 C34 C29 179.50(16) . . . . ? C32 C31 C35 C36 -117.3(2) . . . . ? C30 C31 C35 C36 62.9(2) . . . . ? C32 C31 C35 C37 122.05(19) . . . . ? C30 C31 C35 C37 -57.7(2) . . . . ? C32 C31 C35 C38 3.3(3) . . . . ? C30 C31 C35 C38 -176.51(17) . . . . ? C34 C33 C39 C41X -87.1(6) . . . . ? C32 C33 C39 C41X 92.1(6) . . . . ? C34 C33 C39 C42X 114.6(6) . . . . ? C32 C33 C39 C42X -66.1(6) . . . . ? C34 C33 C39 C42Y 168.6(3) . . . . ? C32 C33 C39 C42Y -12.1(4) . . . . ? C34 C33 C39 C40Y 51.6(3) . . . . ? C32 C33 C39 C40Y -129.2(3) . . . . ? C34 C33 C39 C40X -2.3(6) . . . . ? C32 C33 C39 C40X 176.9(6) . . . . ? C34 C33 C39 C41Y -54.9(8) . . . . ? C32 C33 C39 C41Y 124.4(7) . . . . ? V2 O7 C43 C48 -175.49(14) . . . . ? V2 O7 C43 C44 2.60(18) . . . . ? V2 O8 C44 C45 -178.32(13) . . . . ? V2 O8 C44 C43 2.71(19) . . . . ? O7 C43 C44 O8 -3.4(2) . . . . ? C48 C43 C44 O8 174.77(15) . . . . ? O7 C43 C44 C45 177.58(15) . . . . ? C48 C43 C44 C45 -4.3(3) . . . . ? O8 C44 C45 C46 -175.41(16) . . . . ? C43 C44 C45 C46 3.5(2) . . . . ? O8 C44 C45 C49 5.5(3) . . . . ? C43 C44 C45 C49 -175.64(16) . . . . ? C44 C45 C46 C47 -0.4(3) . . . . ? C49 C45 C46 C47 178.72(17) . . . . ? C45 C46 C47 C48 -2.0(3) . . . . ? C45 C46 C47 C53 179.82(17) . . . . ? O7 C43 C48 C47 179.65(16) . . . . ? C44 C43 C48 C47 1.7(3) . . . . ? C46 C47 C48 C43 1.3(3) . . . . ? C53 C47 C48 C43 179.49(16) . . . . ? C46 C45 C49 C50 0.3(3) . . . . ? C44 C45 C49 C50 179.34(17) . . . . ? C46 C45 C49 C52 120.36(19) . . . . ? C44 C45 C49 C52 -60.6(2) . . . . ? C46 C45 C49 C51 -118.85(19) . . . . ? C44 C45 C49 C51 60.2(2) . . . . ? C48 C47 C53 C55 -84.8(3) . . . . ? C46 C47 C53 C55 93.3(3) . . . . ? C48 C47 C53 C54 153.4(2) . . . . ? C46 C47 C53 C54 -28.5(3) . . . . ? C48 C47 C53 C56 36.0(3) . . . . ? C46 C47 C53 C56 -145.9(2) . . . . ? V1 O9 C57 C58 -171.37(14) . . . . ? V2 O10 C59 C60 145.22(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9 O7 0.79(3) 1.89(3) 2.6528(18) 161(3) . O10 H10 O1S 0.83(3) 1.77(3) 2.5936(18) 171(3) 1_565 O1S H1S O3 0.82 1.85 2.6615(16) 168.8 1_545 _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 31.53 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 1.083 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.089 # Attachment 'complex-4new.cif.txt' data_testp-1 _database_code_depnum_ccdc_archive 'CCDC 762902' #TrackingRef 'complex-4new.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67 H120 O24 V6' _chemical_formula_weight 1615.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.520(3) _cell_length_b 18.220(4) _cell_length_c 19.290(4) _cell_angle_alpha 89.59(3) _cell_angle_beta 74.53(3) _cell_angle_gamma 82.69(3) _cell_volume 4540.6(16) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 18496 _cell_measurement_theta_min 4.517 _cell_measurement_theta_max 50.226 _exptl_crystal_description rod _exptl_crystal_colour blue/black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.181 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1626 _exptl_absorpt_coefficient_mu 0.648 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8293 _exptl_absorpt_correction_T_max 0.9808 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.69420 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS STATION 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX II CCD diffractometer' _diffrn_measurement_method 'w\ rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33491 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0851 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 24.10 _reflns_number_total 15418 _reflns_number_gt 9869 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The structure was solved by direct methods. Data processing was carried out to 0.85 angstroms as the data was only complete to this resolution. All non-hydrogen atoms were refined anisotropically except methanol and water solvent molecules which were left isotropic. Hydrogen atoms were included in calculated positions whereever possible. The methyls of the tert-butyl group C44 > C46 are disordered over two sites. In order to aid in the modelling of this disorder geometric and displacenent restraints were applied to the disordered atoms anisotropic thermal parameters. The residual electron denisty in the strutcure refinement is due to the presence of a small amount of solvate. However, it was not possible to find a suitable model for this. A level alerts are present due to short contacts for the modelled disorder of the solvent methanol. 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^)+(0.1629P)^2^+2.2778P] 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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15418 _refine_ls_number_parameters 924 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0724 _refine_ls_wR_factor_ref 0.2421 _refine_ls_wR_factor_gt 0.2100 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.48155(5) 1.03365(4) 0.37965(4) 0.03095(17) Uani 1 1 d . . . V2 V 0.58438(5) 0.89895(3) 0.45782(3) 0.02792(17) Uani 1 1 d . . . V3 V 0.64184(5) 1.04599(3) 0.47834(3) 0.02830(17) Uani 1 1 d . . . V4 V 0.52222(5) 0.62274(4) 0.04204(3) 0.03322(18) Uani 1 1 d . . . V5 V 0.52031(5) 0.45475(4) 0.09534(3) 0.02969(17) Uani 1 1 d . . . V6 V 0.33760(5) 0.52121(4) 0.04847(3) 0.03176(18) Uani 1 1 d . . . O1 O 0.5000 1.0000 0.5000 0.0311(10) Uani 1 2 d S . . O2 O 0.5652(2) 0.93539(14) 0.36435(14) 0.0326(7) Uani 1 1 d . . . O3 O 0.6100(2) 1.07130(13) 0.38619(14) 0.0297(7) Uani 1 1 d . . . O4 O 0.59531(19) 0.88129(14) 0.55673(14) 0.0295(7) Uani 1 1 d . . . O5 O 0.63985(19) 1.01829(14) 0.57846(14) 0.0308(7) Uani 1 1 d . . . O6 O 0.4704(2) 1.05582(16) 0.30134(14) 0.0386(8) Uani 1 1 d . . . O7 O 0.44924(19) 0.85985(13) 0.47986(13) 0.0286(7) Uani 1 1 d . . . O8 O 0.63284(19) 0.80200(14) 0.42461(14) 0.0308(7) Uani 1 1 d . . . O9 O 0.71242(18) 0.94671(14) 0.43968(14) 0.0302(7) Uani 1 1 d . . . O10 O 0.7786(2) 1.07036(14) 0.45003(14) 0.0324(7) Uani 1 1 d . . . O11 O 0.5000 0.5000 0.0000 0.0329(10) Uani 1 2 d S . . O12 O 0.54312(19) 0.55548(15) 0.11894(13) 0.0306(7) Uani 1 1 d . . . O13 O 0.3723(2) 0.61511(15) 0.08108(13) 0.0337(7) Uani 1 1 d . . . O14 O 0.6636(2) 0.58050(15) -0.01320(13) 0.0335(7) Uani 1 1 d . . . O15 O 0.5061(2) 0.35957(15) 0.05222(14) 0.0338(7) Uani 1 1 d . . . O16 O 0.5364(2) 0.70281(16) 0.06905(15) 0.0419(8) Uani 1 1 d . . . O17 O 0.36768(19) 0.47571(15) 0.13697(13) 0.0322(7) Uani 1 1 d . . . O18 O 0.51489(19) 0.41886(15) 0.18660(13) 0.0303(7) Uani 1 1 d . . . O19 O 0.6692(2) 0.43680(15) 0.04531(13) 0.0337(7) Uani 1 1 d . . . O20 O 0.1940(2) 0.54976(16) 0.07118(13) 0.0343(7) Uani 1 1 d . . . C1 C 0.4577(3) 0.78810(19) 0.45749(19) 0.0250(9) Uani 1 1 d . . . C2 C 0.5602(3) 0.7573(2) 0.42678(19) 0.0266(9) Uani 1 1 d . . . C3 C 0.5820(3) 0.6832(2) 0.40165(19) 0.0272(9) Uani 1 1 d . . . C4 C 0.4967(3) 0.6453(2) 0.40834(19) 0.0290(10) Uani 1 1 d . . . H4 H 0.5095 0.5953 0.3913 0.035 Uiso 1 1 calc R . . C5 C 0.3927(3) 0.6759(2) 0.4386(2) 0.0281(10) Uani 1 1 d . . . C6 C 0.3750(3) 0.7494(2) 0.46403(19) 0.0290(10) Uani 1 1 d . . . H6 H 0.3066 0.7723 0.4856 0.035 Uiso 1 1 calc R . . C7 C 0.6940(3) 0.6499(2) 0.3661(2) 0.0317(10) Uani 1 1 d . . . C8 C 0.6998(3) 0.5687(2) 0.3403(2) 0.0394(11) Uani 1 1 d . . . H8C H 0.7716 0.5497 0.3157 0.059 Uiso 1 1 calc R . . H8A H 0.6565 0.5668 0.3070 0.059 Uiso 1 1 calc R . . H8B H 0.6748 0.5384 0.3819 0.059 Uiso 1 1 calc R . . C9 C 0.7367(3) 0.6945(2) 0.2997(2) 0.0421(12) Uani 1 1 d . . . H9C H 0.7423 0.7447 0.3148 0.063 Uiso 1 1 calc R . . H9A H 0.6899 0.6970 0.2684 0.063 Uiso 1 1 calc R . . H9B H 0.8053 0.6704 0.2732 0.063 Uiso 1 1 calc R . . C10 C 0.7615(3) 0.6508(2) 0.4178(2) 0.0394(12) Uani 1 1 d . . . H10C H 0.7552 0.7011 0.4374 0.059 Uiso 1 1 calc R . . H10B H 0.8338 0.6345 0.3920 0.059 Uiso 1 1 calc R . . H10A H 0.7389 0.6173 0.4572 0.059 Uiso 1 1 calc R . . C11 C 0.3063(3) 0.6292(2) 0.4422(2) 0.0354(11) Uani 1 1 d . . . C12 C 0.1998(3) 0.6723(2) 0.4764(3) 0.0440(12) Uani 1 1 d . . . H12C H 0.1936 0.6838 0.5271 0.066 Uiso 1 1 calc R . . H12A H 0.1459 0.6422 0.4732 0.066 Uiso 1 1 calc R . . H12B H 0.1916 0.7184 0.4509 0.066 Uiso 1 1 calc R . . C13 C 0.3086(3) 0.6062(2) 0.3648(2) 0.0423(12) Uani 1 1 d . . . H13C H 0.3003 0.6506 0.3369 0.063 Uiso 1 1 calc R . . H13A H 0.2520 0.5770 0.3663 0.063 Uiso 1 1 calc R . . H13B H 0.3750 0.5764 0.3422 0.063 Uiso 1 1 calc R . . C14 C 0.3193(3) 0.5609(2) 0.4855(2) 0.0434(12) Uani 1 1 d . . . H14B H 0.3871 0.5324 0.4643 0.065 Uiso 1 1 calc R . . H14A H 0.2647 0.5303 0.4852 0.065 Uiso 1 1 calc R . . H14C H 0.3144 0.5756 0.5352 0.065 Uiso 1 1 calc R . . C15 C 0.8161(3) 0.9475(2) 0.4089(2) 0.0280(10) Uani 1 1 d . . . C16 C 0.8508(3) 1.0151(2) 0.4145(2) 0.0285(10) Uani 1 1 d . . . C17 C 0.9562(3) 1.0227(2) 0.3846(2) 0.0288(10) Uani 1 1 d . . . C18 C 1.0192(3) 0.9597(2) 0.3498(2) 0.0328(10) Uani 1 1 d . . . H18 H 1.0901 0.9638 0.3283 0.039 Uiso 1 1 calc R . . C19 C 0.9854(3) 0.8912(2) 0.3444(2) 0.0337(11) Uani 1 1 d . . . C20 C 0.8802(3) 0.8850(2) 0.3750(2) 0.0301(10) Uani 1 1 d . . . H20 H 0.8538 0.8395 0.3725 0.036 Uiso 1 1 calc R . . C21 C 0.9976(3) 1.0958(2) 0.3894(2) 0.0336(10) Uani 1 1 d . . . C22 C 0.9371(3) 1.1571(2) 0.3562(2) 0.0415(12) Uani 1 1 d . . . H22A H 0.9439 1.1438 0.3059 0.062 Uiso 1 1 calc R . . H22C H 0.9649 1.2038 0.3586 0.062 Uiso 1 1 calc R . . H22B H 0.8638 1.1627 0.3831 0.062 Uiso 1 1 calc R . . C23 C 0.9843(3) 1.1163(2) 0.4684(2) 0.0399(11) Uani 1 1 d . . . H23A H 0.9110 1.1199 0.4947 0.060 Uiso 1 1 calc R . . H23C H 1.0092 1.1641 0.4716 0.060 Uiso 1 1 calc R . . H23B H 1.0244 1.0782 0.4895 0.060 Uiso 1 1 calc R . . C24 C 1.1119(3) 1.0923(3) 0.3495(2) 0.0443(12) Uani 1 1 d . . . H24B H 1.1527 1.0553 0.3714 0.066 Uiso 1 1 calc R . . H24C H 1.1346 1.1408 0.3527 0.066 Uiso 1 1 calc R . . H24A H 1.1220 1.0784 0.2989 0.066 Uiso 1 1 calc R . . C25 C 1.0587(3) 0.8246(2) 0.3036(2) 0.0402(12) Uani 1 1 d . . . C26 C 1.0639(5) 0.8323(3) 0.2243(3) 0.0688(18) Uani 1 1 d . . . H26B H 1.1094 0.7902 0.1969 0.103 Uiso 1 1 calc R . . H26C H 1.0913 0.8784 0.2072 0.103 Uiso 1 1 calc R . . H26A H 0.9943 0.8334 0.2177 0.103 Uiso 1 1 calc R . . C27 C 1.0228(4) 0.7525(2) 0.3291(3) 0.0643(17) Uani 1 1 d . . . H27C H 1.0157 0.7491 0.3809 0.096 Uiso 1 1 calc R . . H27B H 1.0734 0.7117 0.3035 0.096 Uiso 1 1 calc R . . H27A H 0.9557 0.7493 0.3197 0.096 Uiso 1 1 calc R . . C28 C 1.1678(3) 0.8241(3) 0.3130(3) 0.0559(15) Uani 1 1 d . . . H28B H 1.1643 0.8251 0.3644 0.084 Uiso 1 1 calc R . . H28C H 1.1972 0.8677 0.2907 0.084 Uiso 1 1 calc R . . H28A H 1.2117 0.7792 0.2900 0.084 Uiso 1 1 calc R . . C29 C 0.6519(3) 0.9244(2) 0.3014(2) 0.0406(12) Uani 1 1 d . . . H29B H 0.6273 0.9329 0.2583 0.061 Uiso 1 1 calc R . . H29A H 0.6865 0.8736 0.2998 0.061 Uiso 1 1 calc R . . H29C H 0.7007 0.9592 0.3034 0.061 Uiso 1 1 calc R . . C30 C 0.6292(3) 1.1420(2) 0.3584(2) 0.0377(11) Uani 1 1 d . . . H30B H 0.5689 1.1785 0.3793 0.057 Uiso 1 1 calc R . . H30A H 0.6418 1.1400 0.3059 0.057 Uiso 1 1 calc R . . H30C H 0.6900 1.1562 0.3707 0.057 Uiso 1 1 calc R . . C31 C 0.6932(3) 0.8484(2) 0.5660(2) 0.0371(11) Uani 1 1 d . . . H31A H 0.7214 0.8068 0.5315 0.056 Uiso 1 1 calc R . . H31B H 0.6836 0.8306 0.6151 0.056 Uiso 1 1 calc R . . H31C H 0.7414 0.8855 0.5576 0.056 Uiso 1 1 calc R . . C32 C 0.6720(3) 1.0689(2) 0.6218(2) 0.0397(11) Uani 1 1 d . . . H32B H 0.6177 1.1111 0.6370 0.060 Uiso 1 1 calc R . . H32C H 0.7359 1.0865 0.5939 0.060 Uiso 1 1 calc R . . H32A H 0.6844 1.0437 0.6644 0.060 Uiso 1 1 calc R . . C33 C 0.3359(3) 0.4504(2) 0.20474(19) 0.0319(10) Uani 1 1 d . . . C34 C 0.4180(3) 0.4199(2) 0.2325(2) 0.0296(10) Uani 1 1 d . . . C35 C 0.3989(3) 0.3923(2) 0.30155(19) 0.0292(10) Uani 1 1 d . . . C36 C 0.2951(3) 0.3965(2) 0.3402(2) 0.0343(11) Uani 1 1 d . . . H36 H 0.2796 0.3781 0.3876 0.041 Uiso 1 1 calc R . . C37 C 0.2123(3) 0.4262(2) 0.3134(2) 0.0315(10) Uani 1 1 d . A . C38 C 0.2342(3) 0.4547(2) 0.2448(2) 0.0319(10) Uani 1 1 d . . . H38 H 0.1799 0.4767 0.2258 0.038 Uiso 1 1 calc R . . C39 C 0.4896(3) 0.3611(2) 0.3322(2) 0.0327(10) Uani 1 1 d . . . C40 C 0.4519(3) 0.3343(2) 0.4087(2) 0.0395(12) Uani 1 1 d . . . H40C H 0.5117 0.3163 0.4266 0.059 Uiso 1 1 calc R . . H40A H 0.4102 0.2941 0.4087 0.059 Uiso 1 1 calc R . . H40B H 0.4097 0.3754 0.4398 0.059 Uiso 1 1 calc R . . C41 C 0.5588(3) 0.4203(2) 0.3328(2) 0.0381(11) Uani 1 1 d . . . H41B H 0.5189 0.4623 0.3636 0.057 Uiso 1 1 calc R . . H41A H 0.5854 0.4370 0.2837 0.057 Uiso 1 1 calc R . . H41C H 0.6169 0.3998 0.3515 0.057 Uiso 1 1 calc R . . C42 C 0.5537(3) 0.2957(2) 0.2833(2) 0.0362(11) Uani 1 1 d . . . H42B H 0.5723 0.3113 0.2332 0.054 Uiso 1 1 calc R . . H42A H 0.5128 0.2544 0.2874 0.054 Uiso 1 1 calc R . . H42C H 0.6169 0.2799 0.2981 0.054 Uiso 1 1 calc R . . C43 C 0.1007(3) 0.4253(3) 0.3584(2) 0.0411(12) Uani 1 1 d . . . C44X C 0.0808(9) 0.4572(9) 0.4336(6) 0.066(3) Uani 0.436(6) 1 d PU A 2 H44B H 0.0061 0.4698 0.4546 0.099 Uiso 0.436(6) 1 calc PR A 2 H44C H 0.1146 0.5020 0.4318 0.099 Uiso 0.436(6) 1 calc PR A 2 H44A H 0.1088 0.4207 0.4633 0.099 Uiso 0.436(6) 1 calc PR A 2 C45X C 0.0731(7) 0.3430(6) 0.3585(5) 0.072(2) Uani 0.564(6) 1 d PU A 2 H45B H -0.0013 0.3431 0.3800 0.108 Uiso 0.564(6) 1 calc PR A 2 H45C H 0.1119 0.3119 0.3865 0.108 Uiso 0.564(6) 1 calc PR A 2 H45A H 0.0916 0.3233 0.3089 0.108 Uiso 0.564(6) 1 calc PR A 2 C46X C 0.0196(6) 0.4740(6) 0.3268(5) 0.063(2) Uani 0.564(6) 1 d PU A 2 H46A H 0.0187 0.4522 0.2807 0.095 Uiso 0.564(6) 1 calc PR A 2 H46C H 0.0386 0.5242 0.3194 0.095 Uiso 0.564(6) 1 calc PR A 2 H46B H -0.0493 0.4762 0.3606 0.095 Uiso 0.564(6) 1 calc PR A 2 C44Y C 0.0932(7) 0.4128(7) 0.4385(4) 0.067(3) Uani 0.564(6) 1 d PU A 1 H44E H 0.0219 0.4277 0.4672 0.101 Uiso 0.564(6) 1 calc PR A 1 H44F H 0.1397 0.4424 0.4539 0.101 Uiso 0.564(6) 1 calc PR A 1 H44D H 0.1134 0.3602 0.4455 0.101 Uiso 0.564(6) 1 calc PR A 1 C45Y C 0.0516(10) 0.3717(8) 0.3254(7) 0.077(3) Uani 0.436(6) 1 d PU A 1 H45D H 0.0923 0.3227 0.3215 0.115 Uiso 0.436(6) 1 calc PR A 1 H45E H 0.0487 0.3879 0.2773 0.115 Uiso 0.436(6) 1 calc PR A 1 H45F H -0.0188 0.3691 0.3555 0.115 Uiso 0.436(6) 1 calc PR A 1 C46Y C 0.0405(8) 0.5060(7) 0.3634(6) 0.058(3) Uani 0.436(6) 1 d PU A 1 H46D H 0.0386 0.5219 0.3151 0.086 Uiso 0.436(6) 1 calc PR A 1 H46F H 0.0758 0.5400 0.3845 0.086 Uiso 0.436(6) 1 calc PR A 1 H46E H -0.0304 0.5061 0.3938 0.086 Uiso 0.436(6) 1 calc PR A 1 C47 C 0.7674(3) 0.4048(2) 0.0445(2) 0.0314(10) Uani 1 1 d . . . C48 C 0.1585(3) 0.5868(2) 0.0198(2) 0.0328(10) Uani 1 1 d . . . C49 C 0.0560(3) 0.6179(2) 0.0271(2) 0.0352(11) Uani 1 1 d . . . C50 C 0.0350(3) 0.6542(3) -0.0315(2) 0.0416(12) Uani 1 1 d . . . H50 H -0.0344 0.6752 -0.0273 0.050 Uiso 1 1 calc R . . C51 C 0.1093(3) 0.6622(2) -0.0973(2) 0.0374(11) Uani 1 1 d . . . C52 C 0.7894(3) 0.3689(2) 0.1023(2) 0.0372(11) Uani 1 1 d . . . H52 H 0.7361 0.3653 0.1452 0.045 Uiso 1 1 calc R . . C53 C -0.0268(3) 0.6105(3) 0.0976(2) 0.0448(13) Uani 1 1 d . . . C54 C -0.0385(4) 0.5285(3) 0.1118(3) 0.0536(14) Uani 1 1 d . . . H54B H 0.0267 0.5024 0.1176 0.080 Uiso 1 1 calc R . . H54A H -0.0557 0.5063 0.0710 0.080 Uiso 1 1 calc R . . H54C H -0.0940 0.5246 0.1557 0.080 Uiso 1 1 calc R . . C55 C 0.0046(4) 0.6447(4) 0.1590(3) 0.0713(18) Uani 1 1 d . . . H55A H 0.0760 0.6245 0.1574 0.107 Uiso 1 1 calc R . . H55B H -0.0417 0.6330 0.2051 0.107 Uiso 1 1 calc R . . H55C H -0.0002 0.6985 0.1542 0.107 Uiso 1 1 calc R . . C56 C -0.1328(3) 0.6505(3) 0.0949(3) 0.0593(16) Uani 1 1 d . . . H56B H -0.1839 0.6450 0.1407 0.089 Uiso 1 1 calc R . . H56A H -0.1543 0.6287 0.0558 0.089 Uiso 1 1 calc R . . H56C H -0.1278 0.7031 0.0863 0.089 Uiso 1 1 calc R . . C57 C 0.0861(4) 0.7050(3) -0.1603(3) 0.0563(15) Uani 1 1 d . . . C58 C 0.1378(5) 0.7748(3) -0.1681(4) 0.083(2) Uani 1 1 d . . . H58B H 0.1049 0.8080 -0.1263 0.124 Uiso 1 1 calc R . . H58C H 0.1306 0.7996 -0.2120 0.124 Uiso 1 1 calc R . . H58A H 0.2114 0.7619 -0.1709 0.124 Uiso 1 1 calc R . . C59 C 0.1290(4) 0.6586(4) -0.2298(3) 0.0737(19) Uani 1 1 d . . . H59B H 0.2047 0.6498 -0.2409 0.110 Uiso 1 1 calc R . . H59C H 0.1086 0.6851 -0.2692 0.110 Uiso 1 1 calc R . . H59A H 0.1014 0.6111 -0.2239 0.110 Uiso 1 1 calc R . . C60 C -0.0296(4) 0.7268(4) -0.1509(3) 0.080(2) Uani 1 1 d . . . H60A H -0.0630 0.6821 -0.1508 0.120 Uiso 1 1 calc R . . H60C H -0.0400 0.7578 -0.1908 0.120 Uiso 1 1 calc R . . H60B H -0.0600 0.7545 -0.1053 0.120 Uiso 1 1 calc R . . C61 C 0.6241(3) 0.5636(3) 0.1514(2) 0.0396(11) Uani 1 1 d . . . H61B H 0.6906 0.5570 0.1145 0.059 Uiso 1 1 calc R . . H61A H 0.6248 0.5262 0.1881 0.059 Uiso 1 1 calc R . . H61C H 0.6127 0.6131 0.1738 0.059 Uiso 1 1 calc R . . C62 C 0.3221(3) 0.6416(3) 0.1536(2) 0.0407(12) Uani 1 1 d . . . H62A H 0.2490 0.6341 0.1655 0.061 Uiso 1 1 calc R . . H62C H 0.3273 0.6944 0.1577 0.061 Uiso 1 1 calc R . . H62B H 0.3556 0.6142 0.1869 0.061 Uiso 1 1 calc R . . C63 C 0.7290(3) 0.6272(2) -0.0599(2) 0.0411(12) Uani 1 1 d . . . H63A H 0.6953 0.6472 -0.0964 0.062 Uiso 1 1 calc R . . H63B H 0.7954 0.5980 -0.0837 0.062 Uiso 1 1 calc R . . H63C H 0.7408 0.6680 -0.0316 0.062 Uiso 1 1 calc R . . C64 C 0.5748(3) 0.2948(2) 0.0584(2) 0.0406(12) Uani 1 1 d . . . H64A H 0.5439 0.2506 0.0511 0.061 Uiso 1 1 calc R . . H64B H 0.5864 0.2943 0.1064 0.061 Uiso 1 1 calc R . . H64C H 0.6409 0.2950 0.0219 0.061 Uiso 1 1 calc R . . O1S O 0.6917(8) 0.7674(5) 0.7860(5) 0.119(3) Uiso 0.562(5) 1 d PD B 1 H1S H 0.6432 0.7420 0.7890 0.143 Uiso 0.562(5) 1 calc PR B 1 C1S C 0.6681(10) 0.8150(6) 0.8458(6) 0.088(4) Uiso 0.562(5) 1 d PD B 1 H1SB H 0.6231 0.8592 0.8382 0.106 Uiso 0.562(5) 1 calc PR B 1 H1SC H 0.7321 0.8296 0.8529 0.106 Uiso 0.562(5) 1 calc PR B 1 H1SA H 0.6323 0.7899 0.8885 0.106 Uiso 0.562(5) 1 calc PR B 1 O2S O 0.4789(12) 0.8912(9) 0.8323(8) 0.149(6) Uiso 0.438(5) 1 d P B 2 H2S H 0.5024 0.8543 0.8042 0.179 Uiso 0.438(5) 1 calc PR B 2 C2S C 0.3546(16) 0.8947(13) 0.8621(12) 0.137(8) Uiso 0.438(5) 1 d P B 2 H2SA H 0.3349 0.8453 0.8582 0.165 Uiso 0.438(5) 1 calc PR B 2 H2SB H 0.3211 0.9291 0.8335 0.165 Uiso 0.438(5) 1 calc PR B 2 H2SC H 0.3327 0.9117 0.9126 0.165 Uiso 0.438(5) 1 calc PR B 2 O3S O 0.4447(12) 0.0587(8) 0.9840(8) 0.073(4) Uiso 0.2680(10) 1 d P C 1 H3S H 0.3805 0.0721 0.9951 0.087 Uiso 0.2680(10) 1 calc PR C 1 C3S C 0.474(2) -0.0241(17) 0.9316(16) 0.115(10) Uiso 0.2680(10) 1 d P C 1 H3SB H 0.4208 -0.0566 0.9509 0.138 Uiso 0.2680(10) 1 calc PR C 1 H3SC H 0.5416 -0.0490 0.9330 0.138 Uiso 0.2680(10) 1 calc PR C 1 H3SA H 0.4743 -0.0126 0.8817 0.138 Uiso 0.2680(10) 1 calc PR C 1 O4S O 0.5219(15) 0.0549(11) 0.8314(10) 0.115(6) Uiso 0.2861(13) 1 d P D 2 H4S H 0.5596 0.0315 0.7944 0.138 Uiso 0.2861(13) 1 calc PR D 2 C4S C 0.589(2) 0.0713(19) 0.8824(17) 0.130(11) Uiso 0.2861(13) 1 d P D 2 H4SB H 0.5801 0.1246 0.8930 0.156 Uiso 0.2861(13) 1 calc PR D 2 H4SA H 0.6624 0.0545 0.8589 0.156 Uiso 0.2861(13) 1 calc PR D 2 H4SC H 0.5678 0.0450 0.9273 0.156 Uiso 0.2861(13) 1 calc PR D 2 O5S O 0.772(3) 0.8552(19) 0.1237(17) 0.107(10) Uiso 0.1579(19) 1 d P E 4 H5S H 0.7078 0.8549 0.1389 0.128 Uiso 0.1579(19) 1 calc PR E 4 C5S C 0.794(2) 0.8633(15) 0.0625(14) 0.038(6) Uiso 0.1579(19) 1 d P E 4 H5SB H 0.8692 0.8540 0.0433 0.046 Uiso 0.1579(19) 1 calc PR E 4 H5SC H 0.7692 0.9142 0.0526 0.046 Uiso 0.1579(19) 1 calc PR E 4 H5SA H 0.7615 0.8287 0.0396 0.046 Uiso 0.1579(19) 1 calc PR E 4 O6S O 0.5188(7) 0.2289(5) 0.7490(4) 0.188(3) Uiso 1 1 d . . . H6S H 0.5537 0.2645 0.7443 0.226 Uiso 1 1 calc R . . C6S C 0.5169(9) 0.1956(6) 0.8152(6) 0.166(4) Uiso 1 1 d . . . H6SC H 0.5651 0.2165 0.8371 0.200 Uiso 1 1 calc R . . H6SA H 0.5374 0.1421 0.8073 0.200 Uiso 1 1 calc R . . H6SB H 0.4467 0.2049 0.8474 0.200 Uiso 1 1 calc R . . O7S O 0.7011(17) 0.1307(12) 0.9279(12) 0.133(7) Uiso 0.2883(17) 1 d P F 3 H7S H 0.6683 0.1485 0.8990 0.160 Uiso 0.2883(17) 1 calc PR F 3 C7S C 0.6384(15) 0.0384(10) 0.9742(10) 0.062(5) Uiso 0.2883(17) 1 d P F 3 H7SC H 0.6764 0.0178 1.0082 0.074 Uiso 0.2883(17) 1 calc PR F 3 H7SA H 0.6436 0.0011 0.9366 0.074 Uiso 0.2883(17) 1 calc PR F 3 H7SB H 0.5654 0.0526 0.9999 0.074 Uiso 0.2883(17) 1 calc PR F 3 O1SW O 0.6354(8) 0.8207(6) -0.0090(5) 0.233(4) Uiso 1 1 d . . . O2SW O 0.8840(16) 0.0220(12) 0.2098(11) 0.458(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0272(3) 0.0297(3) 0.0316(3) -0.0053(3) -0.0012(3) -0.0014(3) V2 0.0228(3) 0.0244(3) 0.0318(3) -0.0066(3) 0.0003(3) -0.0013(3) V3 0.0225(3) 0.0252(3) 0.0314(3) -0.0065(3) 0.0014(3) 0.0003(3) V4 0.0299(3) 0.0398(4) 0.0254(3) -0.0044(3) 0.0001(3) -0.0033(3) V5 0.0228(3) 0.0390(4) 0.0213(3) -0.0038(3) 0.0031(2) -0.0010(3) V6 0.0254(3) 0.0409(4) 0.0240(3) -0.0032(3) 0.0006(3) -0.0012(3) O1 0.0250(18) 0.033(2) 0.0309(19) -0.0052(16) 0.0004(15) -0.0049(16) O2 0.0279(13) 0.0325(14) 0.0315(14) -0.0055(11) 0.0013(11) -0.0015(12) O3 0.0296(13) 0.0215(12) 0.0324(14) -0.0048(11) 0.0005(11) -0.0005(11) O4 0.0241(13) 0.0260(13) 0.0335(14) -0.0059(11) -0.0013(11) 0.0011(11) O5 0.0259(13) 0.0289(13) 0.0345(14) -0.0095(11) -0.0048(11) 0.0009(11) O6 0.0365(15) 0.0423(16) 0.0337(15) -0.0004(12) -0.0041(12) -0.0040(13) O7 0.0229(12) 0.0249(13) 0.0327(13) -0.0083(11) 0.0011(10) -0.0018(11) O8 0.0232(13) 0.0267(13) 0.0358(14) -0.0057(11) 0.0034(11) -0.0018(11) O9 0.0184(12) 0.0291(13) 0.0378(14) -0.0081(11) 0.0012(11) -0.0023(11) O10 0.0257(13) 0.0275(13) 0.0383(15) -0.0070(12) -0.0004(11) 0.0011(11) O11 0.0295(19) 0.041(2) 0.0266(18) -0.0043(16) -0.0064(15) 0.0003(17) O12 0.0243(12) 0.0437(15) 0.0213(12) -0.0031(11) -0.0030(10) -0.0012(12) O13 0.0322(14) 0.0407(15) 0.0208(13) -0.0050(11) 0.0020(11) 0.0037(12) O14 0.0301(13) 0.0414(15) 0.0259(13) 0.0007(12) -0.0006(11) -0.0073(12) O15 0.0300(14) 0.0353(14) 0.0326(14) -0.0005(12) -0.0036(11) -0.0012(12) O16 0.0443(16) 0.0448(16) 0.0326(15) -0.0080(13) -0.0027(13) -0.0071(14) O17 0.0256(13) 0.0428(15) 0.0235(13) -0.0018(11) 0.0006(10) -0.0021(12) O18 0.0238(12) 0.0399(15) 0.0207(12) -0.0029(11) 0.0035(10) -0.0003(12) O19 0.0270(13) 0.0456(16) 0.0240(13) -0.0012(12) -0.0015(11) 0.0003(12) O20 0.0272(13) 0.0468(16) 0.0227(13) -0.0047(12) 0.0028(11) -0.0019(12) C1 0.0272(18) 0.0185(17) 0.0248(18) -0.0071(14) -0.0004(15) 0.0003(15) C2 0.0271(18) 0.0233(18) 0.0246(18) -0.0043(15) 0.0014(15) -0.0030(16) C3 0.0231(18) 0.0271(19) 0.0258(18) -0.0082(15) 0.0004(15) 0.0029(16) C4 0.0312(19) 0.0248(18) 0.0252(18) -0.0082(15) 0.0018(15) -0.0021(16) C5 0.0243(18) 0.0259(19) 0.0288(19) -0.0066(15) 0.0004(15) 0.0006(16) C6 0.0222(18) 0.032(2) 0.0262(19) -0.0061(16) 0.0026(15) 0.0002(16) C7 0.0226(18) 0.035(2) 0.031(2) -0.0106(17) 0.0031(16) 0.0012(17) C8 0.035(2) 0.035(2) 0.040(2) -0.0149(18) -0.0009(18) 0.0056(18) C9 0.033(2) 0.046(2) 0.035(2) -0.0106(19) 0.0114(18) -0.002(2) C10 0.028(2) 0.035(2) 0.048(2) -0.0122(19) -0.0013(18) 0.0041(18) C11 0.030(2) 0.030(2) 0.040(2) -0.0105(17) 0.0013(17) -0.0041(17) C12 0.032(2) 0.035(2) 0.057(3) -0.012(2) 0.003(2) -0.0072(19) C13 0.039(2) 0.041(2) 0.045(2) -0.010(2) -0.0061(19) -0.006(2) C14 0.043(2) 0.036(2) 0.048(3) -0.002(2) -0.006(2) -0.009(2) C15 0.0193(17) 0.032(2) 0.0286(19) -0.0040(16) -0.0008(15) -0.0006(16) C16 0.0241(18) 0.0270(19) 0.0288(19) -0.0026(16) 0.0013(15) -0.0007(16) C17 0.0234(18) 0.035(2) 0.0265(18) -0.0045(16) -0.0024(15) -0.0057(16) C18 0.0200(18) 0.037(2) 0.035(2) -0.0088(17) 0.0032(16) -0.0004(17) C19 0.0227(18) 0.041(2) 0.033(2) -0.0082(18) -0.0006(16) 0.0010(17) C20 0.0245(18) 0.0267(19) 0.034(2) -0.0081(16) 0.0005(16) -0.0007(16) C21 0.0268(19) 0.036(2) 0.035(2) -0.0023(17) -0.0012(16) -0.0057(17) C22 0.042(2) 0.031(2) 0.049(2) 0.0054(19) -0.006(2) -0.0080(19) C23 0.039(2) 0.039(2) 0.040(2) -0.0050(19) -0.0061(18) -0.0104(19) C24 0.033(2) 0.044(2) 0.051(3) -0.010(2) 0.0022(19) -0.012(2) C25 0.025(2) 0.037(2) 0.049(2) -0.0234(19) 0.0038(18) 0.0032(18) C26 0.073(4) 0.067(3) 0.051(3) -0.030(3) 0.001(3) 0.010(3) C27 0.031(2) 0.036(2) 0.110(4) -0.027(3) 0.004(3) 0.005(2) C28 0.031(2) 0.045(3) 0.084(3) -0.032(2) -0.008(2) 0.010(2) C29 0.033(2) 0.042(2) 0.034(2) -0.0087(19) 0.0094(18) 0.0035(19) C30 0.041(2) 0.029(2) 0.037(2) 0.0021(17) -0.0002(18) -0.0053(18) C31 0.028(2) 0.036(2) 0.046(2) -0.0047(19) -0.0097(17) 0.0009(18) C32 0.039(2) 0.041(2) 0.037(2) -0.0137(19) -0.0073(18) -0.0014(19) C33 0.034(2) 0.040(2) 0.0187(18) -0.0041(16) 0.0005(15) -0.0084(18) C34 0.0227(18) 0.032(2) 0.0275(19) -0.0051(16) 0.0042(15) -0.0019(16) C35 0.0273(19) 0.032(2) 0.0241(18) -0.0050(16) 0.0009(15) -0.0038(16) C36 0.040(2) 0.035(2) 0.0226(19) -0.0029(16) 0.0035(16) -0.0101(18) C37 0.0271(19) 0.034(2) 0.028(2) -0.0075(16) 0.0030(16) -0.0060(17) C38 0.0262(19) 0.037(2) 0.0270(19) -0.0091(17) 0.0019(16) -0.0036(17) C39 0.037(2) 0.030(2) 0.0247(19) -0.0041(16) 0.0005(16) -0.0014(17) C40 0.041(2) 0.047(2) 0.027(2) -0.0003(18) -0.0041(17) -0.005(2) C41 0.039(2) 0.041(2) 0.029(2) -0.0048(18) -0.0016(17) 0.0007(19) C42 0.038(2) 0.035(2) 0.031(2) -0.0034(17) -0.0026(17) 0.0012(19) C43 0.029(2) 0.054(3) 0.033(2) -0.006(2) 0.0075(17) -0.011(2) C44X 0.032(4) 0.131(6) 0.026(4) -0.001(5) 0.007(4) -0.011(5) C45X 0.051(4) 0.096(5) 0.056(4) -0.021(4) 0.025(4) -0.043(4) C46X 0.031(4) 0.083(5) 0.057(4) 0.013(4) 0.013(3) 0.004(4) C44Y 0.030(4) 0.138(6) 0.023(3) 0.005(4) 0.007(3) -0.006(5) C45Y 0.050(4) 0.103(6) 0.060(5) -0.026(5) 0.031(4) -0.046(4) C46Y 0.028(4) 0.080(5) 0.049(5) 0.012(4) 0.008(4) 0.011(4) C47 0.0216(18) 0.041(2) 0.0270(19) -0.0050(17) -0.0005(15) 0.0023(17) C48 0.0261(19) 0.040(2) 0.028(2) -0.0089(17) -0.0006(16) -0.0012(17) C49 0.0249(19) 0.043(2) 0.031(2) -0.0099(18) 0.0031(16) -0.0019(18) C50 0.026(2) 0.048(3) 0.046(2) -0.005(2) -0.0054(18) 0.0047(19) C51 0.029(2) 0.041(2) 0.038(2) -0.0025(19) -0.0040(17) -0.0019(18) C52 0.027(2) 0.049(2) 0.029(2) 0.0002(18) 0.0028(16) -0.0019(19) C53 0.022(2) 0.074(3) 0.031(2) -0.016(2) 0.0040(17) -0.004(2) C54 0.040(2) 0.076(3) 0.038(2) 0.001(2) 0.005(2) -0.015(2) C55 0.027(2) 0.130(5) 0.048(3) -0.052(3) 0.002(2) -0.002(3) C56 0.023(2) 0.092(4) 0.051(3) -0.028(3) 0.004(2) 0.006(2) C57 0.037(2) 0.072(3) 0.059(3) 0.014(3) -0.012(2) -0.005(2) C58 0.082(4) 0.072(4) 0.105(4) 0.042(3) -0.043(3) -0.016(3) C59 0.054(3) 0.123(5) 0.041(3) 0.013(3) -0.017(2) 0.007(3) C60 0.039(3) 0.116(5) 0.079(4) 0.032(3) -0.015(3) 0.011(3) C61 0.037(2) 0.049(2) 0.033(2) -0.0026(19) -0.0082(18) -0.011(2) C62 0.033(2) 0.050(3) 0.031(2) -0.0131(19) 0.0023(17) 0.004(2) C63 0.037(2) 0.048(2) 0.038(2) 0.0001(19) -0.0040(18) -0.014(2) C64 0.040(2) 0.037(2) 0.039(2) -0.0055(19) -0.0050(19) 0.0058(19) _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 V1 O6 1.601(3) . ? V1 O2 1.971(3) . ? V1 O5 1.980(3) 2_676 ? V1 O3 1.980(3) . ? V1 O4 1.981(3) 2_676 ? V1 O1 2.4653(9) . ? V2 O8 1.859(3) . ? V2 O4 1.974(3) . ? V2 O9 1.983(3) . ? V2 O7 1.985(3) . ? V2 O2 1.987(3) . ? V2 O1 2.0844(10) . ? V2 V3 3.0174(13) 2_676 ? V3 O10 1.892(3) . ? V3 O3 1.976(3) . ? V3 O9 1.985(3) . ? V3 O5 1.987(3) . ? V3 O7 2.015(2) 2_676 ? V3 O1 2.1286(9) . ? V3 V2 3.0174(13) 2_676 ? V4 O16 1.604(3) . ? V4 O15 1.972(3) 2_665 ? V4 O12 1.973(3) . ? V4 O14 1.983(3) . ? V4 O13 1.987(3) . ? V4 O11 2.4649(9) . ? V5 O18 1.860(3) . ? V5 O19 1.973(3) . ? V5 O12 1.975(3) . ? V5 O15 1.981(3) . ? V5 O17 1.992(3) . ? V5 O11 2.0804(9) . ? V5 V6 2.9886(13) 2_665 ? V6 O20 1.878(3) . ? V6 O19 1.979(3) 2_665 ? V6 O13 1.980(3) . ? V6 O14 1.982(3) 2_665 ? V6 O17 2.008(3) . ? V6 O11 2.1304(9) . ? V6 V5 2.9886(13) 2_665 ? O1 V2 2.0845(10) 2_676 ? O1 V3 2.1285(9) 2_676 ? O1 V1 2.4652(9) 2_676 ? O2 C29 1.439(4) . ? O3 C30 1.420(5) . ? O4 C31 1.437(5) . ? O4 V1 1.981(3) 2_676 ? O5 C32 1.430(5) . ? O5 V1 1.980(3) 2_676 ? O7 C1 1.361(4) . ? O7 V3 2.015(2) 2_676 ? O8 C2 1.346(5) . ? O9 C15 1.370(4) . ? O10 C16 1.357(4) . ? O11 V5 2.0803(8) 2_665 ? O11 V6 2.1304(9) 2_665 ? O11 V4 2.4649(9) 2_665 ? O12 C61 1.421(5) . ? O13 C62 1.438(4) . ? O14 C63 1.440(5) . ? O14 V6 1.982(3) 2_665 ? O15 C64 1.431(5) . ? O15 V4 1.972(3) 2_665 ? O17 C33 1.359(4) . ? O18 C34 1.369(4) . ? O19 C47 1.377(5) . ? O19 V6 1.979(3) 2_665 ? O20 C48 1.353(5) . ? C1 C6 1.374(5) . ? C1 C2 1.398(5) . ? C2 C3 1.405(5) . ? C3 C4 1.394(6) . ? C3 C7 1.534(5) . ? C4 C5 1.414(5) . ? C4 H4 0.9500 . ? C5 C6 1.398(5) . ? C5 C11 1.517(6) . ? C6 H6 0.9500 . ? C7 C10 1.522(6) . ? C7 C9 1.531(6) . ? C7 C8 1.549(6) . ? C8 H8C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C9 H9C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C10 H10C 0.9800 . ? C10 H10B 0.9800 . ? C10 H10A 0.9800 . ? C11 C14 1.512(6) . ? C11 C12 1.529(5) . ? C11 C13 1.544(6) . ? C12 H12C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C13 H13C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C14 H14B 0.9800 . ? C14 H14A 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.387(6) . ? C15 C20 1.391(5) . ? C16 C17 1.412(5) . ? C17 C18 1.395(5) . ? C17 C21 1.521(6) . ? C18 C19 1.396(6) . ? C18 H18 0.9500 . ? C19 C20 1.406(5) . ? C19 C25 1.538(5) . ? C20 H20 0.9500 . ? C21 C24 1.526(5) . ? C21 C23 1.531(6) . ? C21 C22 1.537(6) . ? C22 H22A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C23 H23A 0.9800 . ? C23 H23C 0.9800 . ? C23 H23B 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 H24A 0.9800 . ? C25 C27 1.494(7) . ? C25 C26 1.518(7) . ? C25 C28 1.532(6) . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26A 0.9800 . ? C27 H27C 0.9800 . ? C27 H27B 0.9800 . ? C27 H27A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C28 H28A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29A 0.9800 . ? C29 H29C 0.9800 . ? C30 H30B 0.9800 . ? C30 H30A 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C32 H32A 0.9800 . ? C33 C38 1.379(5) . ? C33 C34 1.408(6) . ? C34 C35 1.391(5) . ? C35 C36 1.395(5) . ? C35 C39 1.543(6) . ? C36 C37 1.402(6) . ? C36 H36 0.9500 . ? C37 C38 1.388(5) . ? C37 C43 1.529(5) . ? C38 H38 0.9500 . ? C39 C41 1.518(6) . ? C39 C40 1.524(5) . ? C39 C42 1.543(5) . ? C40 H40C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C41 H41B 0.9800 . ? C41 H41A 0.9800 . ? C41 H41C 0.9800 . ? C42 H42B 0.9800 . ? C42 H42A 0.9800 . ? C42 H42C 0.9800 . ? C43 C45Y 1.483(15) . ? C43 C44X 1.510(12) . ? C43 C44Y 1.538(10) . ? C43 C46X 1.570(11) . ? C43 C46Y 1.577(13) . ? C43 C45X 1.590(11) . ? C44X H44B 0.9800 . ? C44X H44C 0.9800 . ? C44X H44A 0.9800 . ? C45X H45B 0.9800 . ? C45X H45C 0.9800 . ? C45X H45A 0.9800 . ? C46X H46A 0.9800 . ? C46X H46C 0.9800 . ? C46X H46B 0.9800 . ? C44Y H44E 0.9800 . ? C44Y H44F 0.9800 . ? C44Y H44D 0.9800 . ? C45Y H45D 0.9800 . ? C45Y H45E 0.9800 . ? C45Y H45F 0.9800 . ? C46Y H46D 0.9800 . ? C46Y H46F 0.9800 . ? C46Y H46E 0.9800 . ? C47 C52 1.369(6) . ? C47 C48 1.393(5) 2_665 ? C48 C47 1.393(5) 2_665 ? C48 C49 1.399(6) . ? C49 C50 1.381(6) . ? C49 C53 1.532(5) . ? C50 C51 1.413(6) . ? C50 H50 0.9500 . ? C51 C52 1.393(6) 2_665 ? C51 C57 1.521(7) . ? C52 C51 1.393(6) 2_665 ? C52 H52 0.9500 . ? C53 C55 1.523(7) . ? C53 C56 1.536(6) . ? C53 C54 1.537(7) . ? C54 H54B 0.9800 . ? C54 H54A 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56B 0.9800 . ? C56 H56A 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.515(8) . ? C57 C59 1.524(8) . ? C57 C60 1.526(7) . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C58 H58A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C59 H59A 0.9800 . ? C60 H60A 0.9800 . ? C60 H60C 0.9800 . ? C60 H60B 0.9800 . ? C61 H61B 0.9800 . ? C61 H61A 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62C 0.9800 . ? C62 H62B 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? O1S C1S 1.391(12) . ? O1S H1S 0.8400 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C1S H1SA 0.9800 . ? O2S C2S 1.62(2) . ? O2S H2S 0.8400 . ? C2S H2SA 0.9800 . ? C2S H2SB 0.9800 . ? C2S H2SC 0.9800 . ? O3S C3S 1.76(3) . ? O3S H3S 0.8400 . ? C3S H3SB 0.9800 . ? C3S H3SC 0.9800 . ? C3S H3SA 0.9800 . ? O4S C4S 1.56(4) . ? O4S H4S 0.8400 . ? C4S H4SB 0.9800 . ? C4S H4SA 0.9800 . ? C4S H4SC 0.9800 . ? O5S C5S 1.15(4) . ? O5S H5S 0.8400 . ? C5S H5SB 0.9800 . ? C5S H5SC 0.9800 . ? C5S H5SA 0.9800 . ? O6S C6S 1.405(13) . ? O6S H6S 0.8400 . ? C6S H6SC 0.9800 . ? C6S H6SA 0.9800 . ? C6S H6SB 0.9800 . ? O7S C7S 2.07(3) . ? O7S H7S 0.8400 . ? C7S H7SC 0.9800 . ? C7S H7SA 0.9800 . ? C7S H7SB 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 V1 O2 104.31(13) . . ? O6 V1 O5 104.26(14) . 2_676 ? O2 V1 O5 87.04(11) . 2_676 ? O6 V1 O3 104.80(14) . . ? O2 V1 O3 85.58(11) . . ? O5 V1 O3 150.94(12) 2_676 . ? O6 V1 O4 104.58(13) . 2_676 ? O2 V1 O4 151.11(12) . 2_676 ? O5 V1 O4 86.03(11) 2_676 2_676 ? O3 V1 O4 86.99(11) . 2_676 ? O6 V1 O1 179.52(12) . . ? O2 V1 O1 75.67(9) . . ? O5 V1 O1 76.21(9) 2_676 . ? O3 V1 O1 74.73(8) . . ? O4 V1 O1 75.43(8) 2_676 . ? O8 V2 O4 95.18(12) . . ? O8 V2 O9 103.35(11) . . ? O4 V2 O9 88.04(12) . . ? O8 V2 O7 81.83(11) . . ? O4 V2 O7 91.35(11) . . ? O9 V2 O7 174.81(10) . . ? O8 V2 O2 95.05(12) . . ? O4 V2 O2 169.76(11) . . ? O9 V2 O2 89.17(12) . . ? O7 V2 O2 90.54(12) . . ? O8 V2 O1 168.09(9) . . ? O4 V2 O1 85.15(8) . . ? O9 V2 O1 88.55(8) . . ? O7 V2 O1 86.26(7) . . ? O2 V2 O1 84.93(8) . . ? O8 V2 V3 123.25(9) . 2_676 ? O4 V2 V3 87.86(8) . 2_676 ? O9 V2 V3 133.40(8) . 2_676 ? O7 V2 V3 41.42(7) . 2_676 ? O2 V2 V3 86.90(8) . 2_676 ? O1 V2 V3 44.85(3) . 2_676 ? O10 V3 O3 95.51(12) . . ? O10 V3 O9 82.43(11) . . ? O3 V3 O9 91.62(11) . . ? O10 V3 O5 97.40(12) . . ? O3 V3 O5 166.96(11) . . ? O9 V3 O5 91.94(11) . . ? O10 V3 O7 105.96(11) . 2_676 ? O3 V3 O7 87.21(11) . 2_676 ? O9 V3 O7 171.60(11) . 2_676 ? O5 V3 O7 87.44(11) . 2_676 ? O10 V3 O1 169.58(8) . . ? O3 V3 O1 83.12(8) . . ? O9 V3 O1 87.28(8) . . ? O5 V3 O1 84.52(8) . . ? O7 V3 O1 84.33(8) 2_676 . ? O10 V3 V2 146.59(8) . 2_676 ? O3 V3 V2 83.68(8) . 2_676 ? O9 V3 V2 130.95(8) . 2_676 ? O5 V3 V2 84.52(8) . 2_676 ? O7 V3 V2 40.65(8) 2_676 2_676 ? O1 V3 V2 43.68(2) . 2_676 ? O16 V4 O15 104.24(14) . 2_665 ? O16 V4 O12 104.89(14) . . ? O15 V4 O12 150.87(12) 2_665 . ? O16 V4 O14 104.19(14) . . ? O15 V4 O14 86.15(11) 2_665 . ? O12 V4 O14 86.28(11) . . ? O16 V4 O13 104.79(14) . . ? O15 V4 O13 87.13(11) 2_665 . ? O12 V4 O13 86.01(11) . . ? O14 V4 O13 151.02(12) . . ? O16 V4 O11 179.66(13) . . ? O15 V4 O11 75.44(9) 2_665 . ? O12 V4 O11 75.44(8) . . ? O14 V4 O11 75.90(9) . . ? O13 V4 O11 75.12(9) . . ? O18 V5 O19 103.12(12) . . ? O18 V5 O12 94.80(12) . . ? O19 V5 O12 87.21(12) . . ? O18 V5 O15 95.86(12) . . ? O19 V5 O15 87.58(12) . . ? O12 V5 O15 168.97(11) . . ? O18 V5 O17 82.25(11) . . ? O19 V5 O17 174.59(12) . . ? O12 V5 O17 93.05(11) . . ? O15 V5 O17 91.23(12) . . ? O18 V5 O11 170.46(8) . . ? O19 V5 O11 86.41(9) . . ? O12 V5 O11 85.07(8) . . ? O15 V5 O11 84.90(9) . . ? O17 V5 O11 88.23(8) . . ? O18 V5 V6 144.06(8) . 2_665 ? O19 V5 V6 40.95(8) . 2_665 ? O12 V5 V6 84.47(8) . 2_665 ? O15 V5 V6 85.23(8) . 2_665 ? O17 V5 V6 133.69(8) . 2_665 ? O11 V5 V6 45.46(2) . 2_665 ? O20 V6 O19 82.09(11) . 2_665 ? O20 V6 O13 96.20(12) . . ? O19 V6 O13 91.57(12) 2_665 . ? O20 V6 O14 96.68(12) . 2_665 ? O19 V6 O14 91.77(12) 2_665 2_665 ? O13 V6 O14 167.03(11) . 2_665 ? O20 V6 O17 106.56(11) . . ? O19 V6 O17 171.35(11) 2_665 . ? O13 V6 O17 87.33(12) . . ? O14 V6 O17 87.49(12) 2_665 . ? O20 V6 O11 166.98(9) . . ? O19 V6 O11 84.90(8) 2_665 . ? O13 V6 O11 83.53(8) . . ? O14 V6 O11 84.29(8) 2_665 . ? O17 V6 O11 86.45(8) . . ? O20 V6 V5 122.88(9) . 2_665 ? O19 V6 V5 40.79(8) 2_665 2_665 ? O13 V6 V5 87.15(8) . 2_665 ? O14 V6 V5 87.20(8) 2_665 2_665 ? O17 V6 V5 130.56(8) . 2_665 ? O11 V6 V5 44.11(3) . 2_665 ? V2 O1 V2 179.999(1) . 2_676 ? V2 O1 V3 91.48(3) . 2_676 ? V2 O1 V3 88.52(3) 2_676 2_676 ? V2 O1 V3 88.52(3) . . ? V2 O1 V3 91.48(3) 2_676 . ? V3 O1 V3 180.000(2) 2_676 . ? V2 O1 V1 89.97(4) . 2_676 ? V2 O1 V1 90.03(4) 2_676 2_676 ? V3 O1 V1 90.51(4) 2_676 2_676 ? V3 O1 V1 89.49(4) . 2_676 ? V2 O1 V1 90.02(4) . . ? V2 O1 V1 89.98(4) 2_676 . ? V3 O1 V1 89.49(4) 2_676 . ? V3 O1 V1 90.51(4) . . ? V1 O1 V1 180.00(3) 2_676 . ? C29 O2 V1 117.4(2) . . ? C29 O2 V2 118.7(2) . . ? V1 O2 V2 109.34(12) . . ? C30 O3 V3 117.6(3) . . ? C30 O3 V1 118.3(3) . . ? V3 O3 V1 111.56(12) . . ? C31 O4 V2 118.1(2) . . ? C31 O4 V1 118.6(2) . 2_676 ? V2 O4 V1 109.40(12) . 2_676 ? C32 O5 V1 120.3(2) . 2_676 ? C32 O5 V3 118.0(2) . . ? V1 O5 V3 109.67(14) 2_676 . ? C1 O7 V2 113.0(2) . . ? C1 O7 V3 148.9(2) . 2_676 ? V2 O7 V3 97.93(11) . 2_676 ? C2 O8 V2 116.1(2) . . ? C15 O9 V2 151.9(2) . . ? C15 O9 V3 111.8(2) . . ? V2 O9 V3 95.65(10) . . ? C16 O10 V3 114.7(2) . . ? V5 O11 V5 180.0 2_665 . ? V5 O11 V6 89.58(4) 2_665 2_665 ? V5 O11 V6 90.42(4) . 2_665 ? V5 O11 V6 90.42(4) 2_665 . ? V5 O11 V6 89.58(4) . . ? V6 O11 V6 180.0 2_665 . ? V5 O11 V4 90.09(3) 2_665 . ? V5 O11 V4 89.91(3) . . ? V6 O11 V4 89.67(4) 2_665 . ? V6 O11 V4 90.33(4) . . ? V5 O11 V4 89.91(3) 2_665 2_665 ? V5 O11 V4 90.09(3) . 2_665 ? V6 O11 V4 90.33(4) 2_665 2_665 ? V6 O11 V4 89.67(4) . 2_665 ? V4 O11 V4 180.0 . 2_665 ? C61 O12 V4 119.2(2) . . ? C61 O12 V5 118.7(2) . . ? V4 O12 V5 109.44(13) . . ? C62 O13 V6 118.2(2) . . ? C62 O13 V4 118.4(3) . . ? V6 O13 V4 110.88(12) . . ? C63 O14 V6 117.9(2) . 2_665 ? C63 O14 V4 119.5(2) . . ? V6 O14 V4 110.05(14) 2_665 . ? C64 O15 V4 117.5(2) . 2_665 ? C64 O15 V5 119.3(3) . . ? V4 O15 V5 109.47(13) 2_665 . ? C33 O17 V5 112.8(2) . . ? C33 O17 V6 151.3(2) . . ? V5 O17 V6 95.74(11) . . ? C34 O18 V5 115.9(2) . . ? C47 O19 V5 149.0(2) . . ? C47 O19 V6 112.4(2) . 2_665 ? V5 O19 V6 98.27(12) . 2_665 ? C48 O20 V6 115.8(2) . . ? O7 C1 C6 124.1(3) . . ? O7 C1 C2 112.8(3) . . ? C6 C1 C2 123.1(3) . . ? O8 C2 C1 116.1(3) . . ? O8 C2 C3 124.1(3) . . ? C1 C2 C3 119.8(3) . . ? C4 C3 C2 116.1(3) . . ? C4 C3 C7 123.9(3) . . ? C2 C3 C7 119.9(3) . . ? C3 C4 C5 124.7(3) . . ? C3 C4 H4 117.6 . . ? C5 C4 H4 117.6 . . ? C6 C5 C4 117.0(4) . . ? C6 C5 C11 123.1(3) . . ? C4 C5 C11 119.8(3) . . ? C1 C6 C5 119.3(3) . . ? C1 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C10 C7 C9 109.9(4) . . ? C10 C7 C3 111.4(3) . . ? C9 C7 C3 108.6(3) . . ? C10 C7 C8 108.0(3) . . ? C9 C7 C8 107.5(3) . . ? C3 C7 C8 111.3(3) . . ? C7 C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C9 H9C 109.5 . . ? C7 C9 H9A 109.5 . . ? H9C C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9C C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C10 H10C 109.5 . . ? C7 C10 H10B 109.5 . . ? H10C C10 H10B 109.5 . . ? C7 C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? C14 C11 C5 110.8(4) . . ? C14 C11 C12 108.3(3) . . ? C5 C11 C12 111.8(3) . . ? C14 C11 C13 109.7(3) . . ? C5 C11 C13 108.6(3) . . ? C12 C11 C13 107.5(4) . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C13 H13C 109.5 . . ? C11 C13 H13A 109.5 . . ? H13C C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13C C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C14 H14B 109.5 . . ? C11 C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C11 C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? O9 C15 C16 114.7(3) . . ? O9 C15 C20 121.9(3) . . ? C16 C15 C20 123.4(3) . . ? O10 C16 C15 116.1(3) . . ? O10 C16 C17 124.2(3) . . ? C15 C16 C17 119.8(3) . . ? C18 C17 C16 116.1(4) . . ? C18 C17 C21 122.4(3) . . ? C16 C17 C21 121.5(3) . . ? C17 C18 C19 124.7(3) . . ? C17 C18 H18 117.6 . . ? C19 C18 H18 117.6 . . ? C18 C19 C20 118.1(3) . . ? C18 C19 C25 121.8(3) . . ? C20 C19 C25 120.0(4) . . ? C15 C20 C19 117.9(4) . . ? C15 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C17 C21 C24 112.3(3) . . ? C17 C21 C23 109.4(3) . . ? C24 C21 C23 108.3(4) . . ? C17 C21 C22 109.8(4) . . ? C24 C21 C22 107.9(3) . . ? C23 C21 C22 109.0(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? H23C C23 H23B 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? H24C C24 H24A 109.5 . . ? C27 C25 C26 109.8(4) . . ? C27 C25 C28 107.6(4) . . ? C26 C25 C28 108.8(4) . . ? C27 C25 C19 112.2(3) . . ? C26 C25 C19 107.5(4) . . ? C28 C25 C19 110.8(4) . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C25 C27 H27C 109.5 . . ? C25 C27 H27B 109.5 . . ? H27C C27 H27B 109.5 . . ? C25 C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? C25 C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? H28C C28 H28A 109.5 . . ? O2 C29 H29B 109.5 . . ? O2 C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? O2 C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? O3 C30 H30B 109.5 . . ? O3 C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? O3 C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O5 C32 H32B 109.5 . . ? O5 C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? O5 C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? H32C C32 H32A 109.5 . . ? O17 C33 C38 124.9(4) . . ? O17 C33 C34 113.5(3) . . ? C38 C33 C34 121.6(3) . . ? O18 C34 C35 123.9(4) . . ? O18 C34 C33 115.3(3) . . ? C35 C34 C33 120.8(3) . . ? C34 C35 C36 116.1(4) . . ? C34 C35 C39 120.3(3) . . ? C36 C35 C39 123.5(3) . . ? C35 C36 C37 123.9(4) . . ? C35 C36 H36 118.0 . . ? C37 C36 H36 118.0 . . ? C38 C37 C36 118.4(3) . . ? C38 C37 C43 121.3(4) . . ? C36 C37 C43 120.3(4) . . ? C33 C38 C37 119.1(4) . . ? C33 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? C41 C39 C40 108.5(3) . . ? C41 C39 C42 108.6(3) . . ? C40 C39 C42 109.1(3) . . ? C41 C39 C35 109.9(3) . . ? C40 C39 C35 112.0(3) . . ? C42 C39 C35 108.6(3) . . ? C39 C40 H40C 109.5 . . ? C39 C40 H40A 109.5 . . ? H40C C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40C C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C41 H41B 109.5 . . ? C39 C41 H41A 109.5 . . ? H41B C41 H41A 109.5 . . ? C39 C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? C39 C42 H42B 109.5 . . ? C39 C42 H42A 109.5 . . ? H42B C42 H42A 109.5 . . ? C39 C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? C45Y C43 C44X 134.0(8) . . ? C45Y C43 C37 109.3(5) . . ? C44X C43 C37 113.0(6) . . ? C45Y C43 C44Y 114.1(8) . . ? C44X C43 C44Y 31.0(7) . . ? C37 C43 C44Y 112.4(5) . . ? C45Y C43 C46X 74.9(8) . . ? C44X C43 C46X 103.6(7) . . ? C37 C43 C46X 113.0(4) . . ? C44Y C43 C46X 126.6(6) . . ? C45Y C43 C46Y 111.7(8) . . ? C44X C43 C46Y 70.4(8) . . ? C37 C43 C46Y 109.0(5) . . ? C44Y C43 C46Y 100.0(7) . . ? C46X C43 C46Y 38.4(6) . . ? C45Y C43 C45X 34.1(7) . . ? C44X C43 C45X 112.2(8) . . ? C37 C43 C45X 108.8(4) . . ? C44Y C43 C45X 84.4(7) . . ? C46X C43 C45X 106.0(6) . . ? C46Y C43 C45X 136.7(7) . . ? C43 C44X H44B 109.5 . . ? C43 C44X H44C 109.5 . . ? H44B C44X H44C 109.5 . . ? C43 C44X H44A 109.5 . . ? H44B C44X H44A 109.5 . . ? H44C C44X H44A 109.5 . . ? C43 C45X H45B 109.5 . . ? C43 C45X H45C 109.5 . . ? H45B C45X H45C 109.5 . . ? C43 C45X H45A 109.5 . . ? H45B C45X H45A 109.5 . . ? H45C C45X H45A 109.5 . . ? C43 C46X H46A 109.5 . . ? C43 C46X H46C 109.5 . . ? H46A C46X H46C 109.5 . . ? C43 C46X H46B 109.5 . . ? H46A C46X H46B 109.5 . . ? H46C C46X H46B 109.5 . . ? C43 C44Y H44E 109.5 . . ? C43 C44Y H44F 109.5 . . ? C43 C44Y H44D 109.5 . . ? C43 C45Y H45D 109.5 . . ? C43 C45Y H45E 109.5 . . ? C43 C45Y H45F 109.5 . . ? C43 C46Y H46D 109.5 . . ? C43 C46Y H46F 109.5 . . ? C43 C46Y H46E 109.5 . . ? C52 C47 O19 122.6(3) . . ? C52 C47 C48 123.6(4) . 2_665 ? O19 C47 C48 113.8(3) . 2_665 ? O20 C48 C47 115.7(3) . 2_665 ? O20 C48 C49 125.5(3) . . ? C47 C48 C49 118.8(4) 2_665 . ? C50 C49 C48 116.9(3) . . ? C50 C49 C53 123.1(4) . . ? C48 C49 C53 120.0(4) . . ? C49 C50 C51 124.7(4) . . ? C49 C50 H50 117.6 . . ? C51 C50 H50 117.6 . . ? C52 C51 C50 116.7(4) 2_665 . ? C52 C51 C57 119.0(4) 2_665 . ? C50 C51 C57 124.3(4) . . ? C47 C52 C51 119.2(4) . 2_665 ? C47 C52 H52 120.4 . . ? C51 C52 H52 120.4 2_665 . ? C55 C53 C49 109.1(4) . . ? C55 C53 C56 108.6(4) . . ? C49 C53 C56 111.4(4) . . ? C55 C53 C54 109.9(4) . . ? C49 C53 C54 110.1(4) . . ? C56 C53 C54 107.7(4) . . ? C53 C54 H54B 109.5 . . ? C53 C54 H54A 109.5 . . ? H54B C54 H54A 109.5 . . ? C53 C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? C53 C55 H55A 109.5 . . ? C53 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C53 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? C53 C56 H56B 109.5 . . ? C53 C56 H56A 109.5 . . ? H56B C56 H56A 109.5 . . ? C53 C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? C58 C57 C51 108.9(5) . . ? C58 C57 C59 108.6(5) . . ? C51 C57 C59 110.3(4) . . ? C58 C57 C60 108.6(5) . . ? C51 C57 C60 112.8(4) . . ? C59 C57 C60 107.7(5) . . ? C57 C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C58 H58A 109.5 . . ? H58B C58 H58A 109.5 . . ? H58C C58 H58A 109.5 . . ? C57 C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C59 H59A 109.5 . . ? H59B C59 H59A 109.5 . . ? H59C C59 H59A 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? H60C C60 H60B 109.5 . . ? O12 C61 H61B 109.5 . . ? O12 C61 H61A 109.5 . . ? H61B C61 H61A 109.5 . . ? O12 C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? O13 C62 H62A 109.5 . . ? O13 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? O13 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? H62C C62 H62B 109.5 . . ? O14 C63 H63A 109.5 . . ? O14 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? O14 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? O15 C64 H64A 109.5 . . ? O15 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? O15 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O1S C1S H1SB 109.5 . . ? O1S C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? O1S C1S H1SA 109.5 . . ? H1SB C1S H1SA 109.5 . . ? H1SC C1S H1SA 109.5 . . ? C2S O2S H2S 109.5 . . ? O2S C2S H2SA 109.5 . . ? O2S C2S H2SB 109.5 . . ? H2SA C2S H2SB 109.5 . . ? O2S C2S H2SC 109.5 . . ? H2SA C2S H2SC 109.5 . . ? H2SB C2S H2SC 109.5 . . ? O3S C3S H3SB 109.5 . . ? O3S C3S H3SC 109.5 . . ? H3SB C3S H3SC 109.5 . . ? O3S C3S H3SA 109.5 . . ? H3SB C3S H3SA 109.5 . . ? H3SC C3S H3SA 109.5 . . ? C4S O4S H4S 109.5 . . ? O4S C4S H4SB 109.5 . . ? O4S C4S H4SA 109.5 . . ? H4SB C4S H4SA 109.5 . . ? O4S C4S H4SC 109.5 . . ? H4SB C4S H4SC 109.5 . . ? H4SA C4S H4SC 109.5 . . ? O5S C5S H5SB 109.5 . . ? O5S C5S H5SC 109.5 . . ? H5SB C5S H5SC 109.5 . . ? O5S C5S H5SA 109.5 . . ? H5SB C5S H5SA 109.5 . . ? H5SC C5S H5SA 109.5 . . ? C6S O6S H6S 109.5 . . ? O6S C6S H6SC 109.5 . . ? O6S C6S H6SA 109.5 . . ? H6SC C6S H6SA 109.5 . . ? O6S C6S H6SB 109.5 . . ? H6SC C6S H6SB 109.5 . . ? H6SA C6S H6SB 109.5 . . ? O7S C7S H7SC 109.5 . . ? O7S C7S H7SA 109.5 . . ? H7SC C7S H7SA 109.5 . . ? O7S C7S H7SB 109.5 . . ? H7SC C7S H7SB 109.5 . . ? H7SA C7S H7SB 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 O8 V2 O1 V2 97(25) . . . 2_676 ? O4 V2 O1 V2 5(25) . . . 2_676 ? O9 V2 O1 V2 -83(25) . . . 2_676 ? O7 V2 O1 V2 97(25) . . . 2_676 ? O2 V2 O1 V2 -172(25) . . . 2_676 ? V3 V2 O1 V2 97(25) 2_676 . . 2_676 ? O8 V2 O1 V3 0.3(4) . . . 2_676 ? O4 V2 O1 V3 -91.85(8) . . . 2_676 ? O9 V2 O1 V3 180.00(8) . . . 2_676 ? O7 V2 O1 V3 -0.17(8) . . . 2_676 ? O2 V2 O1 V3 90.70(9) . . . 2_676 ? O8 V2 O1 V3 -180(50) . . . . ? O4 V2 O1 V3 88.15(8) . . . . ? O9 V2 O1 V3 0.00(8) . . . . ? O7 V2 O1 V3 179.82(8) . . . . ? O2 V2 O1 V3 -89.30(9) . . . . ? V3 V2 O1 V3 180.0 2_676 . . . ? O8 V2 O1 V1 90.8(4) . . . 2_676 ? O4 V2 O1 V1 -1.34(8) . . . 2_676 ? O9 V2 O1 V1 -89.49(9) . . . 2_676 ? O7 V2 O1 V1 90.34(8) . . . 2_676 ? O2 V2 O1 V1 -178.79(8) . . . 2_676 ? V3 V2 O1 V1 90.51(4) 2_676 . . 2_676 ? O8 V2 O1 V1 -89.2(4) . . . . ? O4 V2 O1 V1 178.66(8) . . . . ? O9 V2 O1 V1 90.51(9) . . . . ? O7 V2 O1 V1 -89.66(8) . . . . ? O2 V2 O1 V1 1.21(8) . . . . ? V3 V2 O1 V1 -89.49(4) 2_676 . . . ? O10 V3 O1 V2 9.0(5) . . . . ? O3 V3 O1 V2 91.96(8) . . . . ? O9 V3 O1 V2 0.00(8) . . . . ? O5 V3 O1 V2 -92.21(8) . . . . ? O7 V3 O1 V2 179.83(8) 2_676 . . . ? V2 V3 O1 V2 180.0 2_676 . . . ? O10 V3 O1 V2 -171.0(5) . . . 2_676 ? O3 V3 O1 V2 -88.04(8) . . . 2_676 ? O9 V3 O1 V2 180.00(8) . . . 2_676 ? O5 V3 O1 V2 87.79(8) . . . 2_676 ? O7 V3 O1 V2 -0.17(8) 2_676 . . 2_676 ? O10 V3 O1 V3 51(100) . . . 2_676 ? O3 V3 O1 V3 134(100) . . . 2_676 ? O9 V3 O1 V3 42(100) . . . 2_676 ? O5 V3 O1 V3 -50(100) . . . 2_676 ? O7 V3 O1 V3 -138(100) 2_676 . . 2_676 ? V2 V3 O1 V3 -138(100) 2_676 . . 2_676 ? O10 V3 O1 V1 98.9(5) . . . 2_676 ? O3 V3 O1 V1 -178.05(7) . . . 2_676 ? O9 V3 O1 V1 89.99(9) . . . 2_676 ? O5 V3 O1 V1 -2.22(7) . . . 2_676 ? O7 V3 O1 V1 -90.19(8) 2_676 . . 2_676 ? V2 V3 O1 V1 -90.01(4) 2_676 . . 2_676 ? O10 V3 O1 V1 -81.1(5) . . . . ? O3 V3 O1 V1 1.95(7) . . . . ? O9 V3 O1 V1 -90.01(9) . . . . ? O5 V3 O1 V1 177.78(7) . . . . ? O7 V3 O1 V1 89.82(8) 2_676 . . . ? V2 V3 O1 V1 89.99(4) 2_676 . . . ? O6 V1 O1 V2 -89(15) . . . . ? O2 V1 O1 V2 -1.25(8) . . . . ? O5 V1 O1 V2 89.19(8) 2_676 . . . ? O3 V1 O1 V2 -90.53(8) . . . . ? O4 V1 O1 V2 178.63(8) 2_676 . . . ? O6 V1 O1 V2 91(15) . . . 2_676 ? O2 V1 O1 V2 178.75(8) . . . 2_676 ? O5 V1 O1 V2 -90.81(8) 2_676 . . 2_676 ? O3 V1 O1 V2 89.47(8) . . . 2_676 ? O4 V1 O1 V2 -1.37(8) 2_676 . . 2_676 ? O6 V1 O1 V3 179(100) . . . 2_676 ? O2 V1 O1 V3 -92.73(9) . . . 2_676 ? O5 V1 O1 V3 -2.28(7) 2_676 . . 2_676 ? O3 V1 O1 V3 178.00(7) . . . 2_676 ? O4 V1 O1 V3 87.15(8) 2_676 . . 2_676 ? O6 V1 O1 V3 -1(15) . . . . ? O2 V1 O1 V3 87.27(9) . . . . ? O5 V1 O1 V3 177.72(7) 2_676 . . . ? O3 V1 O1 V3 -2.00(7) . . . . ? O4 V1 O1 V3 -92.85(8) 2_676 . . . ? O6 V1 O1 V1 -134(29) . . . 2_676 ? O2 V1 O1 V1 -46(25) . . . 2_676 ? O5 V1 O1 V1 44(25) 2_676 . . 2_676 ? O3 V1 O1 V1 -135(25) . . . 2_676 ? O4 V1 O1 V1 134(25) 2_676 . . 2_676 ? O6 V1 O2 C29 41.8(3) . . . . ? O5 V1 O2 C29 145.8(3) 2_676 . . . ? O3 V1 O2 C29 -62.3(3) . . . . ? O4 V1 O2 C29 -137.9(3) 2_676 . . . ? O1 V1 O2 C29 -137.7(3) . . . . ? O6 V1 O2 V2 -179.10(14) . . . . ? O5 V1 O2 V2 -75.13(14) 2_676 . . . ? O3 V1 O2 V2 76.74(14) . . . . ? O4 V1 O2 V2 1.2(3) 2_676 . . . ? O1 V1 O2 V2 1.39(9) . . . . ? O8 V2 O2 C29 -55.1(3) . . . . ? O4 V2 O2 C29 122.4(6) . . . . ? O9 V2 O2 C29 48.2(3) . . . . ? O7 V2 O2 C29 -137.0(3) . . . . ? O1 V2 O2 C29 136.8(3) . . . . ? V3 V2 O2 C29 -178.2(3) 2_676 . . . ? O8 V2 O2 V1 166.45(13) . . . . ? O4 V2 O2 V1 -16.0(7) . . . . ? O9 V2 O2 V1 -90.22(14) . . . . ? O7 V2 O2 V1 84.60(13) . . . . ? O1 V2 O2 V1 -1.60(11) . . . . ? V3 V2 O2 V1 43.32(11) 2_676 . . . ? O10 V3 O3 C30 -51.6(3) . . . . ? O9 V3 O3 C30 -134.1(2) . . . . ? O5 V3 O3 C30 120.1(5) . . . . ? O7 V3 O3 C30 54.2(2) 2_676 . . . ? O1 V3 O3 C30 138.8(2) . . . . ? V2 V3 O3 C30 94.9(2) 2_676 . . . ? O10 V3 O3 V1 166.99(12) . . . . ? O9 V3 O3 V1 84.45(13) . . . . ? O5 V3 O3 V1 -21.3(5) . . . . ? O7 V3 O3 V1 -87.23(13) 2_676 . . . ? O1 V3 O3 V1 -2.61(9) . . . . ? V2 V3 O3 V1 -46.59(10) 2_676 . . . ? O6 V1 O3 C30 41.2(3) . . . . ? O2 V1 O3 C30 144.8(2) . . . . ? O5 V1 O3 C30 -139.4(3) 2_676 . . . ? O4 V1 O3 C30 -63.1(2) 2_676 . . . ? O1 V1 O3 C30 -138.9(2) . . . . ? O6 V1 O3 V3 -177.67(13) . . . . ? O2 V1 O3 V3 -74.02(13) . . . . ? O5 V1 O3 V3 1.8(3) 2_676 . . . ? O4 V1 O3 V3 78.04(13) 2_676 . . . ? O1 V1 O3 V3 2.32(8) . . . . ? O8 V2 O4 C31 53.9(3) . . . . ? O9 V2 O4 C31 -49.3(3) . . . . ? O7 V2 O4 C31 135.8(3) . . . . ? O2 V2 O4 C31 -123.6(6) . . . . ? O1 V2 O4 C31 -138.0(3) . . . . ? V3 V2 O4 C31 177.1(3) 2_676 . . . ? O8 V2 O4 V1 -166.29(13) . . . 2_676 ? O9 V2 O4 V1 90.48(13) . . . 2_676 ? O7 V2 O4 V1 -84.37(13) . . . 2_676 ? O2 V2 O4 V1 16.2(7) . . . 2_676 ? O1 V2 O4 V1 1.76(10) . . . 2_676 ? V3 V2 O4 V1 -43.09(11) 2_676 . . 2_676 ? O10 V3 O5 C32 50.4(3) . . . . ? O3 V3 O5 C32 -121.2(5) . . . . ? O9 V3 O5 C32 133.0(2) . . . . ? O7 V3 O5 C32 -55.3(2) 2_676 . . . ? O1 V3 O5 C32 -139.9(2) . . . . ? V2 V3 O5 C32 -96.0(2) 2_676 . . . ? O10 V3 O5 V1 -166.75(12) . . . 2_676 ? O3 V3 O5 V1 21.6(5) . . . 2_676 ? O9 V3 O5 V1 -84.14(13) . . . 2_676 ? O7 V3 O5 V1 87.48(13) 2_676 . . 2_676 ? O1 V3 O5 V1 2.94(9) . . . 2_676 ? V2 V3 O5 V1 46.83(10) 2_676 . . 2_676 ? O8 V2 O7 C1 -3.5(2) . . . . ? O4 V2 O7 C1 -98.5(2) . . . . ? O9 V2 O7 C1 178(50) . . . . ? O2 V2 O7 C1 91.6(2) . . . . ? O1 V2 O7 C1 176.4(2) . . . . ? V3 V2 O7 C1 176.2(3) 2_676 . . . ? O8 V2 O7 V3 -179.72(13) . . . 2_676 ? O4 V2 O7 V3 85.24(12) . . . 2_676 ? O9 V2 O7 V3 2.1(14) . . . 2_676 ? O2 V2 O7 V3 -84.70(12) . . . 2_676 ? O1 V2 O7 V3 0.19(9) . . . 2_676 ? O4 V2 O8 C2 94.4(3) . . . . ? O9 V2 O8 C2 -176.4(2) . . . . ? O7 V2 O8 C2 3.8(3) . . . . ? O2 V2 O8 C2 -86.0(3) . . . . ? O1 V2 O8 C2 3.3(6) . . . . ? V3 V2 O8 C2 3.6(3) 2_676 . . . ? O8 V2 O9 C15 12.3(5) . . . . ? O4 V2 O9 C15 107.2(5) . . . . ? O7 V2 O9 C15 -169.5(11) . . . . ? O2 V2 O9 C15 -82.7(5) . . . . ? O1 V2 O9 C15 -167.6(5) . . . . ? V3 V2 O9 C15 -167.6(5) 2_676 . . . ? O8 V2 O9 V3 179.94(11) . . . . ? O4 V2 O9 V3 -85.19(12) . . . . ? O7 V2 O9 V3 -1.9(14) . . . . ? O2 V2 O9 V3 84.95(12) . . . . ? O1 V2 O9 V3 0.00(9) . . . . ? V3 V2 O9 V3 0.01(17) 2_676 . . . ? O10 V3 O9 C15 -4.6(2) . . . . ? O3 V3 O9 C15 90.7(2) . . . . ? O5 V3 O9 C15 -101.8(2) . . . . ? O7 V3 O9 C15 172.5(7) 2_676 . . . ? O1 V3 O9 C15 173.8(2) . . . . ? V2 V3 O9 C15 173.7(2) 2_676 . . . ? O10 V3 O9 V2 -178.38(13) . . . . ? O3 V3 O9 V2 -83.04(12) . . . . ? O5 V3 O9 V2 84.42(12) . . . . ? O7 V3 O9 V2 -1.2(8) 2_676 . . . ? O1 V3 O9 V2 0.00(9) . . . . ? V2 V3 O9 V2 -0.01(16) 2_676 . . . ? O3 V3 O10 C16 -85.8(3) . . . . ? O9 V3 O10 C16 5.1(3) . . . . ? O5 V3 O10 C16 96.1(3) . . . . ? O7 V3 O10 C16 -174.4(2) 2_676 . . . ? O1 V3 O10 C16 -3.9(7) . . . . ? V2 V3 O10 C16 -172.63(19) 2_676 . . . ? O18 V5 O11 V5 79(24) . . . 2_665 ? O19 V5 O11 V5 -98(24) . . . 2_665 ? O12 V5 O11 V5 -11(24) . . . 2_665 ? O15 V5 O11 V5 174(24) . . . 2_665 ? O17 V5 O11 V5 82(24) . . . 2_665 ? V6 V5 O11 V5 -98(24) 2_665 . . 2_665 ? O18 V5 O11 V6 176.7(6) . . . 2_665 ? O19 V5 O11 V6 -0.42(9) . . . 2_665 ? O12 V5 O11 V6 87.09(8) . . . 2_665 ? O15 V5 O11 V6 -88.31(8) . . . 2_665 ? O17 V5 O11 V6 -179.70(8) . . . 2_665 ? O18 V5 O11 V6 -3.3(6) . . . . ? O19 V5 O11 V6 179.58(9) . . . . ? O12 V5 O11 V6 -92.91(8) . . . . ? O15 V5 O11 V6 91.69(8) . . . . ? O17 V5 O11 V6 0.30(8) . . . . ? V6 V5 O11 V6 180.000(2) 2_665 . . . ? O18 V5 O11 V4 87.0(6) . . . . ? O19 V5 O11 V4 -90.09(9) . . . . ? O12 V5 O11 V4 -2.59(7) . . . . ? O15 V5 O11 V4 -177.98(8) . . . . ? O17 V5 O11 V4 90.63(9) . . . . ? V6 V5 O11 V4 -89.67(4) 2_665 . . . ? O18 V5 O11 V4 -93.0(6) . . . 2_665 ? O19 V5 O11 V4 89.91(9) . . . 2_665 ? O12 V5 O11 V4 177.41(7) . . . 2_665 ? O15 V5 O11 V4 2.02(8) . . . 2_665 ? O17 V5 O11 V4 -89.37(9) . . . 2_665 ? V6 V5 O11 V4 90.33(4) 2_665 . . 2_665 ? O20 V6 O11 V5 -3.0(4) . . . 2_665 ? O19 V6 O11 V5 -0.42(9) 2_665 . . 2_665 ? O13 V6 O11 V5 -92.59(8) . . . 2_665 ? O14 V6 O11 V5 91.88(9) 2_665 . . 2_665 ? O17 V6 O11 V5 179.70(8) . . . 2_665 ? O20 V6 O11 V5 177.0(4) . . . . ? O19 V6 O11 V5 179.58(9) 2_665 . . . ? O13 V6 O11 V5 87.41(8) . . . . ? O14 V6 O11 V5 -88.12(9) 2_665 . . . ? O17 V6 O11 V5 -0.30(8) . . . . ? V5 V6 O11 V5 180.0 2_665 . . . ? O20 V6 O11 V6 163(100) . . . 2_665 ? O19 V6 O11 V6 165(100) 2_665 . . 2_665 ? O13 V6 O11 V6 73(100) . . . 2_665 ? O14 V6 O11 V6 -102(100) 2_665 . . 2_665 ? O17 V6 O11 V6 -15(100) . . . 2_665 ? V5 V6 O11 V6 166(100) 2_665 . . 2_665 ? O20 V6 O11 V4 87.1(4) . . . . ? O19 V6 O11 V4 89.68(9) 2_665 . . . ? O13 V6 O11 V4 -2.49(8) . . . . ? O14 V6 O11 V4 -178.03(8) 2_665 . . . ? O17 V6 O11 V4 -90.20(9) . . . . ? V5 V6 O11 V4 90.10(3) 2_665 . . . ? O20 V6 O11 V4 -92.9(4) . . . 2_665 ? O19 V6 O11 V4 -90.33(9) 2_665 . . 2_665 ? O13 V6 O11 V4 177.51(8) . . . 2_665 ? O14 V6 O11 V4 1.97(8) 2_665 . . 2_665 ? O17 V6 O11 V4 89.80(9) . . . 2_665 ? V5 V6 O11 V4 -89.91(3) 2_665 . . 2_665 ? O16 V4 O11 V5 19(24) . . . 2_665 ? O15 V4 O11 V5 2.09(8) 2_665 . . 2_665 ? O12 V4 O11 V5 -177.33(7) . . . 2_665 ? O14 V4 O11 V5 -87.55(9) . . . 2_665 ? O13 V4 O11 V5 92.97(9) . . . 2_665 ? O16 V4 O11 V5 -161(73) . . . . ? O15 V4 O11 V5 -177.91(8) 2_665 . . . ? O12 V4 O11 V5 2.67(7) . . . . ? O14 V4 O11 V5 92.45(9) . . . . ? O13 V4 O11 V5 -87.03(9) . . . . ? O16 V4 O11 V6 108(24) . . . 2_665 ? O15 V4 O11 V6 91.66(8) 2_665 . . 2_665 ? O12 V4 O11 V6 -87.76(8) . . . 2_665 ? O14 V4 O11 V6 2.02(8) . . . 2_665 ? O13 V4 O11 V6 -177.45(8) . . . 2_665 ? O16 V4 O11 V6 -72(24) . . . . ? O15 V4 O11 V6 -88.34(8) 2_665 . . . ? O12 V4 O11 V6 92.24(8) . . . . ? O14 V4 O11 V6 -177.98(8) . . . . ? O13 V4 O11 V6 2.55(8) . . . . ? O16 V4 O11 V4 168(100) . . . 2_665 ? O15 V4 O11 V4 151(5) 2_665 . . 2_665 ? O12 V4 O11 V4 -28(5) . . . 2_665 ? O14 V4 O11 V4 62(5) . . . 2_665 ? O13 V4 O11 V4 -118(5) . . . 2_665 ? O16 V4 O12 C61 -41.8(3) . . . . ? O15 V4 O12 C61 137.2(3) 2_665 . . . ? O14 V4 O12 C61 61.9(3) . . . . ? O13 V4 O12 C61 -146.0(3) . . . . ? O11 V4 O12 C61 138.3(2) . . . . ? O16 V4 O12 V5 176.93(13) . . . . ? O15 V4 O12 V5 -4.1(3) 2_665 . . . ? O14 V4 O12 V5 -79.37(13) . . . . ? O13 V4 O12 V5 72.68(13) . . . . ? O11 V4 O12 V5 -2.98(8) . . . . ? O18 V5 O12 C61 51.5(2) . . . . ? O19 V5 O12 C61 -51.4(2) . . . . ? O15 V5 O12 C61 -113.4(6) . . . . ? O17 V5 O12 C61 134.0(2) . . . . ? O11 V5 O12 C61 -138.1(2) . . . . ? V6 V5 O12 C61 -92.4(2) 2_665 . . . ? O18 V5 O12 V4 -166.99(12) . . . . ? O19 V5 O12 V4 90.06(13) . . . . ? O15 V5 O12 V4 28.1(6) . . . . ? O17 V5 O12 V4 -84.53(13) . . . . ? O11 V5 O12 V4 3.43(10) . . . . ? V6 V5 O12 V4 49.09(10) 2_665 . . . ? O20 V6 O13 C62 54.9(3) . . . . ? O19 V6 O13 C62 137.1(3) 2_665 . . . ? O14 V6 O13 C62 -118.0(5) 2_665 . . . ? O17 V6 O13 C62 -51.5(3) . . . . ? O11 V6 O13 C62 -138.2(3) . . . . ? V5 V6 O13 C62 177.7(3) 2_665 . . . ? O20 V6 O13 V4 -163.59(13) . . . . ? O19 V6 O13 V4 -81.38(14) 2_665 . . . ? O14 V6 O13 V4 23.5(6) 2_665 . . . ? O17 V6 O13 V4 90.04(14) . . . . ? O11 V6 O13 V4 3.31(11) . . . . ? V5 V6 O13 V4 -40.82(11) 2_665 . . . ? O16 V4 O13 C62 -41.9(3) . . . . ? O15 V4 O13 C62 -145.8(3) 2_665 . . . ? O12 V4 O13 C62 62.5(3) . . . . ? O14 V4 O13 C62 137.4(3) . . . . ? O11 V4 O13 C62 138.5(3) . . . . ? O16 V4 O13 V6 176.73(15) . . . . ? O15 V4 O13 V6 72.76(14) 2_665 . . . ? O12 V4 O13 V6 -78.92(14) . . . . ? O14 V4 O13 V6 -4.0(3) . . . . ? O11 V4 O13 V6 -2.94(10) . . . . ? O16 V4 O14 C63 -40.8(3) . . . . ? O15 V4 O14 C63 62.9(3) 2_665 . . . ? O12 V4 O14 C63 -145.3(3) . . . . ? O13 V4 O14 C63 139.9(3) . . . . ? O11 V4 O14 C63 138.8(3) . . . . ? O16 V4 O14 V6 178.02(15) . . . 2_665 ? O15 V4 O14 V6 -78.26(14) 2_665 . . 2_665 ? O12 V4 O14 V6 73.59(14) . . . 2_665 ? O13 V4 O14 V6 -1.3(3) . . . 2_665 ? O11 V4 O14 V6 -2.32(10) . . . 2_665 ? O18 V5 O15 C64 -52.7(3) . . . . ? O19 V5 O15 C64 50.2(3) . . . . ? O12 V5 O15 C64 112.2(6) . . . . ? O17 V5 O15 C64 -135.0(3) . . . . ? O11 V5 O15 C64 136.9(3) . . . . ? V6 V5 O15 C64 91.2(2) 2_665 . . . ? O18 V5 O15 V4 167.77(13) . . . 2_665 ? O19 V5 O15 V4 -89.28(14) . . . 2_665 ? O12 V5 O15 V4 -27.4(6) . . . 2_665 ? O17 V5 O15 V4 85.44(13) . . . 2_665 ? O11 V5 O15 V4 -2.67(10) . . . 2_665 ? V6 V5 O15 V4 -48.32(10) 2_665 . . 2_665 ? O18 V5 O17 C33 -4.3(3) . . . . ? O19 V5 O17 C33 168.7(12) . . . . ? O12 V5 O17 C33 -98.7(3) . . . . ? O15 V5 O17 C33 91.5(3) . . . . ? O11 V5 O17 C33 176.3(2) . . . . ? V6 V5 O17 C33 176.0(2) 2_665 . . . ? O18 V5 O17 V6 179.07(13) . . . . ? O19 V5 O17 V6 -8.0(14) . . . . ? O12 V5 O17 V6 84.64(12) . . . . ? O15 V5 O17 V6 -85.18(12) . . . . ? O11 V5 O17 V6 -0.32(9) . . . . ? V6 V5 O17 V6 -0.62(17) 2_665 . . . ? O20 V6 O17 C33 7.4(5) . . . . ? O19 V6 O17 C33 -174.0(7) 2_665 . . . ? O13 V6 O17 C33 103.1(5) . . . . ? O14 V6 O17 C33 -88.8(5) 2_665 . . . ? O11 V6 O17 C33 -173.2(5) . . . . ? V5 V6 O17 C33 -173.0(5) 2_665 . . . ? O20 V6 O17 V5 -179.04(12) . . . . ? O19 V6 O17 V5 -0.5(9) 2_665 . . . ? O13 V6 O17 V5 -83.37(12) . . . . ? O14 V6 O17 V5 84.74(12) 2_665 . . . ? O11 V6 O17 V5 0.31(9) . . . . ? V5 V6 O17 V5 0.59(16) 2_665 . . . ? O19 V5 O18 C34 -175.9(2) . . . . ? O12 V5 O18 C34 95.8(3) . . . . ? O15 V5 O18 C34 -87.0(3) . . . . ? O17 V5 O18 C34 3.4(3) . . . . ? O11 V5 O18 C34 7.1(7) . . . . ? V6 V5 O18 C34 -176.98(19) 2_665 . . . ? O18 V5 O19 C47 9.6(5) . . . . ? O12 V5 O19 C47 103.9(5) . . . . ? O15 V5 O19 C47 -85.9(5) . . . . ? O17 V5 O19 C47 -163.3(11) . . . . ? O11 V5 O19 C47 -170.9(5) . . . . ? V6 V5 O19 C47 -171.4(6) 2_665 . . . ? O18 V5 O19 V6 -179.05(12) . . . 2_665 ? O12 V5 O19 V6 -84.77(13) . . . 2_665 ? O15 V5 O19 V6 85.50(13) . . . 2_665 ? O17 V5 O19 V6 8.1(14) . . . 2_665 ? O11 V5 O19 V6 0.46(9) . . . 2_665 ? O19 V6 O20 C48 -4.4(3) 2_665 . . . ? O13 V6 O20 C48 86.3(3) . . . . ? O14 V6 O20 C48 -95.3(3) 2_665 . . . ? O17 V6 O20 C48 175.4(3) . . . . ? O11 V6 O20 C48 -1.8(6) . . . . ? V5 V6 O20 C48 -4.3(3) 2_665 . . . ? V2 O7 C1 C6 -177.5(3) . . . . ? V3 O7 C1 C6 -4.7(7) 2_676 . . . ? V2 O7 C1 C2 2.5(4) . . . . ? V3 O7 C1 C2 175.3(3) 2_676 . . . ? V2 O8 C2 C1 -3.5(4) . . . . ? V2 O8 C2 C3 177.6(3) . . . . ? O7 C1 C2 O8 0.5(5) . . . . ? C6 C1 C2 O8 -179.6(3) . . . . ? O7 C1 C2 C3 179.4(3) . . . . ? C6 C1 C2 C3 -0.7(6) . . . . ? O8 C2 C3 C4 179.9(3) . . . . ? C1 C2 C3 C4 1.1(5) . . . . ? O8 C2 C3 C7 -2.9(6) . . . . ? C1 C2 C3 C7 178.3(3) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C7 C3 C4 C5 -177.6(4) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C3 C4 C5 C11 179.4(4) . . . . ? O7 C1 C6 C5 179.5(3) . . . . ? C2 C1 C6 C5 -0.5(6) . . . . ? C4 C5 C6 C1 1.1(6) . . . . ? C11 C5 C6 C1 -178.9(4) . . . . ? C4 C3 C7 C10 -121.8(4) . . . . ? C2 C3 C7 C10 61.2(5) . . . . ? C4 C3 C7 C9 117.0(4) . . . . ? C2 C3 C7 C9 -60.0(5) . . . . ? C4 C3 C7 C8 -1.2(5) . . . . ? C2 C3 C7 C8 -178.2(4) . . . . ? C6 C5 C11 C14 -120.8(4) . . . . ? C4 C5 C11 C14 59.3(5) . . . . ? C6 C5 C11 C12 0.1(6) . . . . ? C4 C5 C11 C12 -179.8(4) . . . . ? C6 C5 C11 C13 118.7(4) . . . . ? C4 C5 C11 C13 -61.3(5) . . . . ? V2 O9 C15 C16 170.1(4) . . . . ? V3 O9 C15 C16 3.3(4) . . . . ? V2 O9 C15 C20 -9.9(8) . . . . ? V3 O9 C15 C20 -176.6(3) . . . . ? V3 O10 C16 C15 -4.8(4) . . . . ? V3 O10 C16 C17 175.8(3) . . . . ? O9 C15 C16 O10 0.8(5) . . . . ? C20 C15 C16 O10 -179.3(4) . . . . ? O9 C15 C16 C17 -179.8(3) . . . . ? C20 C15 C16 C17 0.2(6) . . . . ? O10 C16 C17 C18 -179.9(4) . . . . ? C15 C16 C17 C18 0.7(6) . . . . ? O10 C16 C17 C21 -0.7(6) . . . . ? C15 C16 C17 C21 179.9(4) . . . . ? C16 C17 C18 C19 -1.4(6) . . . . ? C21 C17 C18 C19 179.4(4) . . . . ? C17 C18 C19 C20 1.1(6) . . . . ? C17 C18 C19 C25 178.4(4) . . . . ? O9 C15 C20 C19 179.5(4) . . . . ? C16 C15 C20 C19 -0.5(6) . . . . ? C18 C19 C20 C15 -0.1(6) . . . . ? C25 C19 C20 C15 -177.5(4) . . . . ? C18 C17 C21 C24 2.6(6) . . . . ? C16 C17 C21 C24 -176.6(4) . . . . ? C18 C17 C21 C23 -117.8(4) . . . . ? C16 C17 C21 C23 63.1(5) . . . . ? C18 C17 C21 C22 122.6(4) . . . . ? C16 C17 C21 C22 -56.5(5) . . . . ? C18 C19 C25 C27 156.0(5) . . . . ? C20 C19 C25 C27 -26.7(6) . . . . ? C18 C19 C25 C26 -83.1(5) . . . . ? C20 C19 C25 C26 94.2(5) . . . . ? C18 C19 C25 C28 35.7(6) . . . . ? C20 C19 C25 C28 -147.1(4) . . . . ? V5 O17 C33 C38 -177.0(3) . . . . ? V6 O17 C33 C38 -4.0(8) . . . . ? V5 O17 C33 C34 4.3(4) . . . . ? V6 O17 C33 C34 177.3(4) . . . . ? V5 O18 C34 C35 177.0(3) . . . . ? V5 O18 C34 C33 -2.0(4) . . . . ? O17 C33 C34 O18 -1.7(5) . . . . ? C38 C33 C34 O18 179.6(4) . . . . ? O17 C33 C34 C35 179.2(3) . . . . ? C38 C33 C34 C35 0.5(6) . . . . ? O18 C34 C35 C36 -178.6(4) . . . . ? C33 C34 C35 C36 0.4(6) . . . . ? O18 C34 C35 C39 2.8(6) . . . . ? C33 C34 C35 C39 -178.2(4) . . . . ? C34 C35 C36 C37 0.0(6) . . . . ? C39 C35 C36 C37 178.5(4) . . . . ? C35 C36 C37 C38 -1.3(6) . . . . ? C35 C36 C37 C43 177.2(4) . . . . ? O17 C33 C38 C37 179.6(4) . . . . ? C34 C33 C38 C37 -1.8(6) . . . . ? C36 C37 C38 C33 2.1(6) . . . . ? C43 C37 C38 C33 -176.3(4) . . . . ? C34 C35 C39 C41 58.8(5) . . . . ? C36 C35 C39 C41 -119.6(4) . . . . ? C34 C35 C39 C40 179.5(4) . . . . ? C36 C35 C39 C40 1.1(5) . . . . ? C34 C35 C39 C42 -59.9(5) . . . . ? C36 C35 C39 C42 121.7(4) . . . . ? C38 C37 C43 C45Y 68.6(8) . . . . ? C36 C37 C43 C45Y -109.8(8) . . . . ? C38 C37 C43 C44X -130.0(8) . . . . ? C36 C37 C43 C44X 51.6(8) . . . . ? C38 C37 C43 C44Y -163.7(6) . . . . ? C36 C37 C43 C44Y 17.9(7) . . . . ? C38 C37 C43 C46X -12.7(7) . . . . ? C36 C37 C43 C46X 168.9(6) . . . . ? C38 C37 C43 C46Y -53.8(7) . . . . ? C36 C37 C43 C46Y 127.8(6) . . . . ? C38 C37 C43 C45X 104.7(6) . . . . ? C36 C37 C43 C45X -73.7(6) . . . . ? V5 O19 C47 C52 -5.8(8) . . . . ? V6 O19 C47 C52 -176.5(3) 2_665 . . . ? V5 O19 C47 C48 174.9(4) . . . 2_665 ? V6 O19 C47 C48 4.1(4) 2_665 . . 2_665 ? V6 O20 C48 C47 3.4(5) . . . 2_665 ? V6 O20 C48 C49 -175.1(3) . . . . ? O20 C48 C49 C50 179.5(4) . . . . ? C47 C48 C49 C50 1.1(6) 2_665 . . . ? O20 C48 C49 C53 -0.7(7) . . . . ? C47 C48 C49 C53 -179.1(4) 2_665 . . . ? C48 C49 C50 C51 -0.4(7) . . . . ? C53 C49 C50 C51 179.8(4) . . . . ? C49 C50 C51 C52 -0.1(7) . . . 2_665 ? C49 C50 C51 C57 -177.4(5) . . . . ? O19 C47 C52 C51 179.8(4) . . . 2_665 ? C48 C47 C52 C51 -0.9(7) 2_665 . . 2_665 ? C50 C49 C53 C55 -121.8(5) . . . . ? C48 C49 C53 C55 58.4(6) . . . . ? C50 C49 C53 C56 -1.9(6) . . . . ? C48 C49 C53 C56 178.3(4) . . . . ? C50 C49 C53 C54 117.5(5) . . . . ? C48 C49 C53 C54 -62.2(5) . . . . ? C52 C51 C57 C58 -67.1(6) 2_665 . . . ? C50 C51 C57 C58 110.1(5) . . . . ? C52 C51 C57 C59 52.0(6) 2_665 . . . ? C50 C51 C57 C59 -130.9(5) . . . . ? C52 C51 C57 C60 172.4(5) 2_665 . . . ? C50 C51 C57 C60 -10.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.10 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.356 _refine_diff_density_min -0.852 _refine_diff_density_rms 0.111 # Attachment 'complex-5new.CIF.txt' data_sadtest _database_code_depnum_ccdc_archive 'CCDC 762903' #TrackingRef 'complex-5new.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H98 O13 V2' _chemical_formula_weight 1153.28 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.7603(12) _cell_length_b 11.8807(10) _cell_length_c 20.3294(18) _cell_angle_alpha 90.00 _cell_angle_beta 95.249(2) _cell_angle_gamma 90.00 _cell_volume 3309.6(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9454 _cell_measurement_theta_min 4.533 _cell_measurement_theta_max 45.248 _exptl_crystal_description block _exptl_crystal_colour blue/black _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.42 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7977 _exptl_absorpt_correction_T_max 0.8710 _exptl_absorpt_process_details SADABS _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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12901 _diffrn_reflns_av_R_equivalents 0.0572 _diffrn_reflns_av_sigmaI/netI 0.0814 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 21.98 _reflns_number_total 4046 _reflns_number_gt 2638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure was solved by direct methods. Data was processed to a resolution of 0.95 angstroms. All non-hydrogen atoms were refined anisotropically. The ethanol molecules have displacement restraints applied to their anisotropic thermal parameters and one has been split over two sites.. One ethanol is on a symmetry site and hydrogens could not be placed on this molecule, accounting for the discrepancy between the UnIT ans atom list. The resolution is slightly low because the data was only complete to 0.95 angstroms. Enough chemical information can be obtained from the current data set. 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^)+(0.1287P)^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 constrained _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4046 _refine_ls_number_parameters 405 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0907 _refine_ls_R_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1712 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 1.020 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.50689(6) 0.10112(7) 0.05116(4) 0.0226(3) Uani 1 1 d . . . O1 O 0.5597(2) 0.0436(3) -0.03087(16) 0.0226(9) Uani 1 1 d . . . O2 O 0.6195(2) 0.1895(3) 0.05045(17) 0.0250(9) Uani 1 1 d . . . O3 O 0.6247(2) -0.0283(3) 0.10145(16) 0.0244(9) Uani 1 1 d . . . O4 O 0.5031(2) 0.1177(3) 0.13990(17) 0.0221(9) Uani 1 1 d . . . O5 O 0.4187(2) 0.1831(3) 0.02780(18) 0.0281(9) Uani 1 1 d . . . C1 C 0.6543(4) 0.0759(4) -0.0364(3) 0.0218(13) Uani 1 1 d . . . C2 C 0.6859(4) 0.1581(4) 0.0090(3) 0.0212(13) Uani 1 1 d . . . C3 C 0.7808(4) 0.2020(4) 0.0095(3) 0.0248(14) Uani 1 1 d . . . C4 C 0.8379(4) 0.1572(4) -0.0373(3) 0.0280(14) Uani 1 1 d . . . H4 H 0.9010 0.1850 -0.0380 0.034 Uiso 1 1 calc R . . C5 C 0.8081(4) 0.0747(4) -0.0829(3) 0.0285(14) Uani 1 1 d . . . C6 C 0.7126(4) 0.0328(4) -0.0820(3) 0.0256(14) Uani 1 1 d . . . H6 H 0.6893 -0.0228 -0.1116 0.031 Uiso 1 1 calc R . . C7 C 0.8195(4) 0.2889(4) 0.0616(3) 0.0288(14) Uani 1 1 d . . . C8 C 0.7501(4) 0.3893(4) 0.0625(3) 0.0376(16) Uani 1 1 d . . . H8C H 0.7731 0.4399 0.0973 0.056 Uiso 1 1 calc R . . H8A H 0.6860 0.3633 0.0698 0.056 Uiso 1 1 calc R . . H8B H 0.7478 0.4279 0.0208 0.056 Uiso 1 1 calc R . . C9 C 0.8297(4) 0.2322(5) 0.1299(3) 0.0362(16) Uani 1 1 d . . . H9B H 0.8731 0.1690 0.1291 0.054 Uiso 1 1 calc R . . H9A H 0.7669 0.2069 0.1407 0.054 Uiso 1 1 calc R . . H9C H 0.8557 0.2852 0.1625 0.054 Uiso 1 1 calc R . . C10 C 0.9196(4) 0.3346(5) 0.0482(3) 0.0380(16) Uani 1 1 d . . . H10B H 0.9665 0.2745 0.0516 0.057 Uiso 1 1 calc R . . H10C H 0.9392 0.3919 0.0800 0.057 Uiso 1 1 calc R . . H10A H 0.9161 0.3660 0.0045 0.057 Uiso 1 1 calc R . . C11 C 0.8726(4) 0.0302(5) -0.1346(3) 0.0354(15) Uani 1 1 d . . . C12 C 0.9772(5) 0.0713(7) -0.1227(4) 0.079(3) Uani 1 1 d . . . H12C H 1.0135 0.0467 -0.1582 0.119 Uiso 1 1 calc R . . H12B H 1.0064 0.0412 -0.0818 0.119 Uiso 1 1 calc R . . H12A H 0.9779 0.1520 -0.1207 0.119 Uiso 1 1 calc R . . C13 C 0.8760(5) -0.0980(6) -0.1315(4) 0.076(3) Uani 1 1 d . . . H13A H 0.8108 -0.1271 -0.1332 0.114 Uiso 1 1 calc R . . H13B H 0.9119 -0.1211 -0.0910 0.114 Uiso 1 1 calc R . . H13C H 0.9075 -0.1264 -0.1683 0.114 Uiso 1 1 calc R . . C14 C 0.8305(5) 0.0650(7) -0.2027(3) 0.070(2) Uani 1 1 d . . . H14A H 0.7651 0.0370 -0.2107 0.104 Uiso 1 1 calc R . . H14C H 0.8698 0.0347 -0.2351 0.104 Uiso 1 1 calc R . . H14B H 0.8299 0.1457 -0.2058 0.104 Uiso 1 1 calc R . . C15 C 0.6434(4) 0.0075(4) 0.1655(2) 0.0211(13) Uani 1 1 d . . . C16 C 0.5767(4) 0.0868(4) 0.1851(3) 0.0221(13) Uani 1 1 d . . . C17 C 0.5871(4) 0.1334(4) 0.2492(3) 0.0265(14) Uani 1 1 d . . . C18 C 0.6645(4) 0.0937(5) 0.2905(3) 0.0304(14) Uani 1 1 d . . . H18 H 0.6733 0.1225 0.3331 0.036 Uiso 1 1 calc R . . C19 C 0.7309(4) 0.0128(5) 0.2722(3) 0.0284(14) Uani 1 1 d . . . C20 C 0.7193(4) -0.0280(4) 0.2084(3) 0.0252(13) Uani 1 1 d . . . H20 H 0.7635 -0.0802 0.1945 0.030 Uiso 1 1 calc R . . C21 C 0.5158(4) 0.2244(5) 0.2691(3) 0.0321(15) Uani 1 1 d . . . C22 C 0.5206(4) 0.3269(4) 0.2235(3) 0.0406(16) Uani 1 1 d . . . H22C H 0.5862 0.3553 0.2264 0.061 Uiso 1 1 calc R . . H22B H 0.4776 0.3845 0.2368 0.061 Uiso 1 1 calc R . . H22A H 0.5011 0.3051 0.1788 0.061 Uiso 1 1 calc R . . C23 C 0.4114(4) 0.1778(5) 0.2647(3) 0.0421(17) Uani 1 1 d . . . H23A H 0.3908 0.1590 0.2196 0.063 Uiso 1 1 calc R . . H23B H 0.3684 0.2338 0.2799 0.063 Uiso 1 1 calc R . . H23C H 0.4096 0.1117 0.2916 0.063 Uiso 1 1 calc R . . C24 C 0.5432(5) 0.2635(6) 0.3408(3) 0.055(2) Uani 1 1 d . . . H24B H 0.5392 0.2009 0.3703 0.082 Uiso 1 1 calc R . . H24A H 0.4989 0.3214 0.3520 0.082 Uiso 1 1 calc R . . H24C H 0.6086 0.2926 0.3448 0.082 Uiso 1 1 calc R . . C25 C 0.8149(4) -0.0258(5) 0.3224(3) 0.0415(17) Uani 1 1 d . . . C26 C 0.7710(6) -0.0770(7) 0.3821(3) 0.079(3) Uani 1 1 d . . . H26B H 0.7324 -0.0214 0.4019 0.119 Uiso 1 1 calc R . . H26C H 0.8225 -0.1020 0.4137 0.119 Uiso 1 1 calc R . . H26A H 0.7305 -0.1399 0.3679 0.119 Uiso 1 1 calc R . . C27 C 0.8807(5) 0.0764(6) 0.3425(4) 0.081(3) Uani 1 1 d . . . H27B H 0.9090 0.1048 0.3043 0.122 Uiso 1 1 calc R . . H27C H 0.9316 0.0536 0.3752 0.122 Uiso 1 1 calc R . . H27A H 0.8422 0.1344 0.3603 0.122 Uiso 1 1 calc R . . C28 C 0.8777(5) -0.1166(6) 0.2935(3) 0.053(2) Uani 1 1 d . . . H28A H 0.8370 -0.1784 0.2779 0.080 Uiso 1 1 calc R . . H28C H 0.9261 -0.1427 0.3270 0.080 Uiso 1 1 calc R . . H28B H 0.9093 -0.0855 0.2574 0.080 Uiso 1 1 calc R . . O1S O 0.7915(7) 0.7227(8) 0.0881(5) 0.0522(15) Uani 0.463(5) 1 d PDU A 1 H1S H 0.7459 0.6799 0.0776 0.078 Uiso 0.463(5) 1 calc PR A 1 C1S C 0.8096(13) 0.7922(12) 0.0322(7) 0.0416(15) Uani 0.463(5) 1 d PDU A 1 H1S1 H 0.7660 0.7728 -0.0063 0.050 Uiso 0.463(5) 1 calc PR A 1 H1S2 H 0.8765 0.7849 0.0215 0.050 Uiso 0.463(5) 1 calc PR A 1 C2S C 0.7899(8) 0.9062(8) 0.0556(6) 0.0268(17) Uani 0.463(5) 1 d PDU A 1 H2S1 H 0.7240 0.9103 0.0672 0.040 Uiso 0.463(5) 1 calc PR A 1 H2S2 H 0.7989 0.9595 0.0211 0.040 Uiso 0.463(5) 1 calc PR A 1 H2S3 H 0.8340 0.9232 0.0936 0.040 Uiso 0.463(5) 1 calc PR A 1 O1T O 0.7088(5) 0.7794(7) 0.0930(4) 0.0426(15) Uani 0.537(5) 1 d PDU A 2 H1T H 0.6703 0.7309 0.0785 0.064 Uiso 0.537(5) 1 calc PR A 2 C1T C 0.7880(10) 0.7911(13) 0.0488(7) 0.0416(14) Uani 0.537(5) 1 d PDU A 2 H1T1 H 0.8211 0.8627 0.0561 0.050 Uiso 0.537(5) 1 calc PR A 2 H1T2 H 0.7618 0.7869 0.0029 0.050 Uiso 0.537(5) 1 calc PR A 2 C2T C 0.8592(8) 0.6927(9) 0.0658(6) 0.0471(16) Uani 0.537(5) 1 d PDU A 2 H2T1 H 0.8764 0.6910 0.1127 0.071 Uiso 0.537(5) 1 calc PR A 2 H2T2 H 0.9170 0.7029 0.0434 0.071 Uiso 0.537(5) 1 calc PR A 2 H2T3 H 0.8284 0.6230 0.0521 0.071 Uiso 0.537(5) 1 calc PR A 2 O2S O 0.5886(7) 0.6088(8) 0.0402(6) 0.083(3) Uani 0.50 1 d PDU . . C3S C 0.5047(16) 0.5334(19) 0.0423(11) 0.083(3) Uani 0.50 1 d PDU . . C4S C 0.4826(17) 0.4576(19) -0.0142(12) 0.084(4) Uani 0.50 1 d PDU . . 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 V1 0.0190(6) 0.0258(6) 0.0225(6) -0.0018(4) -0.0005(4) -0.0023(4) O1 0.017(2) 0.027(2) 0.023(2) -0.0014(16) 0.0001(16) -0.0069(17) O2 0.018(2) 0.028(2) 0.029(2) -0.0037(17) 0.0011(17) -0.0023(17) O3 0.025(2) 0.031(2) 0.017(2) -0.0034(16) -0.0039(17) 0.0009(17) O4 0.017(2) 0.023(2) 0.026(2) -0.0026(16) 0.0009(17) -0.0007(16) O5 0.019(2) 0.032(2) 0.033(2) 0.0002(18) -0.0027(17) 0.0007(17) C1 0.018(3) 0.024(3) 0.022(3) 0.004(3) -0.004(3) -0.002(3) C2 0.018(3) 0.024(3) 0.021(3) 0.003(3) -0.003(3) 0.002(3) C3 0.020(3) 0.026(3) 0.028(3) 0.004(3) -0.002(3) 0.000(3) C4 0.017(3) 0.033(3) 0.033(4) 0.003(3) 0.000(3) -0.006(3) C5 0.021(3) 0.027(3) 0.037(4) 0.002(3) 0.001(3) -0.001(3) C6 0.026(3) 0.026(3) 0.024(3) -0.002(3) -0.001(3) -0.006(3) C7 0.022(3) 0.031(3) 0.033(4) -0.002(3) -0.001(3) -0.004(3) C8 0.037(4) 0.029(3) 0.045(4) -0.006(3) -0.005(3) -0.005(3) C9 0.034(4) 0.042(4) 0.030(4) -0.001(3) -0.012(3) -0.009(3) C10 0.028(4) 0.044(4) 0.040(4) -0.003(3) -0.004(3) -0.013(3) C11 0.027(3) 0.039(4) 0.042(4) -0.006(3) 0.010(3) -0.007(3) C12 0.032(4) 0.119(7) 0.090(6) -0.044(5) 0.025(4) -0.016(5) C13 0.065(5) 0.060(5) 0.110(7) -0.012(5) 0.046(5) 0.006(4) C14 0.065(5) 0.106(6) 0.040(5) -0.008(4) 0.023(4) 0.012(5) C15 0.024(3) 0.024(3) 0.015(3) 0.002(2) 0.001(3) -0.004(3) C16 0.020(3) 0.023(3) 0.024(3) 0.003(3) 0.001(3) -0.005(3) C17 0.032(3) 0.023(3) 0.024(4) -0.004(3) 0.003(3) -0.003(3) C18 0.042(4) 0.034(3) 0.014(3) -0.007(3) -0.003(3) 0.000(3) C19 0.035(4) 0.026(3) 0.023(4) 0.003(3) -0.005(3) -0.002(3) C20 0.027(3) 0.023(3) 0.026(3) 0.000(3) 0.003(3) 0.003(3) C21 0.038(4) 0.034(3) 0.024(4) -0.011(3) 0.000(3) 0.001(3) C22 0.046(4) 0.025(3) 0.051(4) -0.007(3) 0.005(3) 0.004(3) C23 0.043(4) 0.043(4) 0.042(4) -0.006(3) 0.013(3) 0.008(3) C24 0.063(5) 0.062(5) 0.038(4) -0.020(4) -0.002(4) 0.023(4) C25 0.052(4) 0.044(4) 0.026(4) 0.001(3) -0.011(3) 0.011(3) C26 0.102(7) 0.102(6) 0.033(4) 0.017(4) -0.001(4) 0.052(5) C27 0.075(6) 0.062(5) 0.094(7) -0.022(5) -0.063(5) 0.013(4) C28 0.052(4) 0.064(5) 0.040(4) -0.003(3) -0.018(3) 0.017(4) O1S 0.044(3) 0.055(3) 0.059(4) -0.003(3) 0.011(3) 0.006(3) C1S 0.029(3) 0.051(3) 0.046(4) -0.010(3) 0.008(3) 0.009(3) C2S 0.007(4) 0.048(3) 0.026(4) -0.009(3) 0.007(3) 0.007(3) O1T 0.032(3) 0.051(3) 0.046(4) -0.003(3) 0.009(3) 0.006(3) C1T 0.029(3) 0.052(3) 0.045(4) -0.007(3) 0.008(2) 0.007(3) C2T 0.035(3) 0.053(3) 0.054(4) -0.007(3) 0.010(3) 0.010(3) O2S 0.059(5) 0.046(5) 0.141(10) -0.021(6) 0.000(6) 0.001(4) C3S 0.059(5) 0.047(5) 0.142(10) -0.021(6) -0.001(6) 0.000(4) C4S 0.060(5) 0.047(5) 0.143(10) -0.021(6) -0.002(6) 0.000(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 V1 O5 1.594(3) . ? V1 O4 1.820(3) . ? V1 O2 1.873(3) . ? V1 O1 1.975(3) 3_655 ? V1 O1 1.999(3) . ? V1 O3 2.395(3) . ? O1 C1 1.371(6) . ? O1 V1 1.975(3) 3_655 ? O2 C2 1.352(6) . ? O3 C15 1.372(6) . ? O4 C16 1.354(6) . ? C1 C6 1.379(7) . ? C1 C2 1.386(7) . ? C2 C3 1.405(7) . ? C3 C4 1.394(7) . ? C3 C7 1.538(7) . ? C4 C5 1.386(7) . ? C4 H4 0.9300 . ? C5 C6 1.406(7) . ? C5 C11 1.530(8) . ? C6 H6 0.9300 . ? C7 C8 1.529(7) . ? C7 C10 1.529(7) . ? C7 C9 1.538(7) . ? C8 H8C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C9 H9B 0.9600 . ? C9 H9A 0.9600 . ? C9 H9C 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C10 H10A 0.9600 . ? C11 C14 1.509(9) . ? C11 C12 1.519(8) . ? C11 C13 1.524(9) . ? C12 H12C 0.9600 . ? C12 H12B 0.9600 . ? C12 H12A 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14C 0.9600 . ? C14 H14B 0.9600 . ? C15 C20 1.364(7) . ? C15 C16 1.398(7) . ? C16 C17 1.411(7) . ? C17 C18 1.378(7) . ? C17 C21 1.538(7) . ? C18 C19 1.399(7) . ? C18 H18 0.9300 . ? C19 C20 1.380(7) . ? C19 C25 1.541(7) . ? C20 H20 0.9300 . ? C21 C23 1.535(8) . ? C21 C22 1.536(8) . ? C21 C24 1.544(8) . ? C22 H22C 0.9600 . ? C22 H22B 0.9600 . ? C22 H22A 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24B 0.9600 . ? C24 H24A 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.530(9) . ? C25 C28 1.533(8) . ? C25 C27 1.547(9) . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26 H26A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 H27A 0.9600 . ? C28 H28A 0.9600 . ? C28 H28C 0.9600 . ? C28 H28B 0.9600 . ? O1S C1S 1.443(12) . ? O1S H1S 0.8200 . ? C1S C2S 1.468(16) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? O1T C1T 1.481(12) . ? O1T H1T 0.8200 . ? C1T C2T 1.544(16) . ? C1T H1T1 0.9700 . ? C1T H1T2 0.9700 . ? C2T H2T1 0.9600 . ? C2T H2T2 0.9600 . ? C2T H2T3 0.9600 . ? O2S C4S 1.33(2) 3_665 ? O2S C3S 1.464(16) . ? C3S C4S 0.62(4) 3_665 ? C3S C4S 1.471(15) . ? C3S C3S 1.89(4) 3_665 ? C4S C3S 0.62(4) 3_665 ? C4S C4S 1.24(4) 3_665 ? C4S O2S 1.33(2) 3_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 V1 O4 98.01(17) . . ? O5 V1 O2 105.24(16) . . ? O4 V1 O2 92.61(15) . . ? O5 V1 O1 98.27(16) . 3_655 ? O4 V1 O1 104.28(15) . 3_655 ? O2 V1 O1 148.78(15) . 3_655 ? O5 V1 O1 106.55(17) . . ? O4 V1 O1 155.39(15) . . ? O2 V1 O1 79.68(14) . . ? O1 V1 O1 74.07(15) 3_655 . ? O5 V1 O3 170.64(16) . . ? O4 V1 O3 74.10(13) . . ? O2 V1 O3 80.51(13) . . ? O1 V1 O3 79.22(12) 3_655 . ? O1 V1 O3 81.56(13) . . ? C1 O1 V1 130.7(3) . 3_655 ? C1 O1 V1 113.2(3) . . ? V1 O1 V1 105.94(15) 3_655 . ? C2 O2 V1 117.2(3) . . ? C15 O3 V1 105.4(3) . . ? C16 O4 V1 123.7(3) . . ? O1 C1 C6 124.5(5) . . ? O1 C1 C2 112.6(5) . . ? C6 C1 C2 122.9(5) . . ? O2 C2 C1 114.9(4) . . ? O2 C2 C3 125.0(5) . . ? C1 C2 C3 120.1(5) . . ? C4 C3 C2 115.7(5) . . ? C4 C3 C7 123.0(5) . . ? C2 C3 C7 121.1(5) . . ? C5 C4 C3 125.2(5) . . ? C5 C4 H4 117.4 . . ? C3 C4 H4 117.4 . . ? C4 C5 C6 117.4(5) . . ? C4 C5 C11 123.3(5) . . ? C6 C5 C11 119.2(5) . . ? C1 C6 C5 118.6(5) . . ? C1 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C8 C7 C10 107.4(4) . . ? C8 C7 C9 109.7(5) . . ? C10 C7 C9 107.9(4) . . ? C8 C7 C3 110.8(4) . . ? C10 C7 C3 112.1(5) . . ? C9 C7 C3 109.0(4) . . ? C7 C8 H8C 109.5 . . ? C7 C8 H8A 109.5 . . ? H8C C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8C C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C9 H9B 109.5 . . ? C7 C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? C7 C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? H10C C10 H10A 109.5 . . ? C14 C11 C12 109.6(6) . . ? C14 C11 C13 108.7(6) . . ? C12 C11 C13 106.8(6) . . ? C14 C11 C5 109.7(5) . . ? C12 C11 C5 112.4(5) . . ? C13 C11 C5 109.5(5) . . ? C11 C12 H12C 109.5 . . ? C11 C12 H12B 109.5 . . ? H12C C12 H12B 109.5 . . ? C11 C12 H12A 109.5 . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? H14C C14 H14B 109.5 . . ? C20 C15 O3 125.2(5) . . ? C20 C15 C16 120.7(5) . . ? O3 C15 C16 114.1(4) . . ? O4 C16 C15 117.3(4) . . ? O4 C16 C17 121.7(5) . . ? C15 C16 C17 120.9(5) . . ? C18 C17 C16 115.8(5) . . ? C18 C17 C21 123.8(5) . . ? C16 C17 C21 120.4(5) . . ? C17 C18 C19 124.1(5) . . ? C17 C18 H18 117.9 . . ? C19 C18 H18 117.9 . . ? C20 C19 C18 118.0(5) . . ? C20 C19 C25 122.2(5) . . ? C18 C19 C25 119.8(5) . . ? C15 C20 C19 120.5(5) . . ? C15 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C23 C21 C22 110.0(5) . . ? C23 C21 C17 110.3(4) . . ? C22 C21 C17 109.6(5) . . ? C23 C21 C24 108.1(5) . . ? C22 C21 C24 108.1(5) . . ? C17 C21 C24 110.7(5) . . ? C21 C22 H22C 109.5 . . ? C21 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? C21 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24B 109.5 . . ? C21 C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? C21 C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? C26 C25 C28 107.5(5) . . ? C26 C25 C19 108.4(5) . . ? C28 C25 C19 111.7(5) . . ? C26 C25 C27 111.6(6) . . ? C28 C25 C27 108.5(6) . . ? C19 C25 C27 109.1(5) . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? H26C C26 H26A 109.5 . . ? C25 C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? H27C C27 H27A 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? H28C C28 H28B 109.5 . . ? O1S C1S C2S 102.9(10) . . ? O1S C1S H1S1 111.2 . . ? C2S C1S H1S1 111.2 . . ? O1S C1S H1S2 111.2 . . ? C2S C1S H1S2 111.2 . . ? H1S1 C1S H1S2 109.1 . . ? C1T O1T H1T 109.5 . . ? O1T C1T C2T 106.2(10) . . ? O1T C1T H1T1 110.5 . . ? C2T C1T H1T1 110.5 . . ? O1T C1T H1T2 110.5 . . ? C2T C1T H1T2 110.5 . . ? H1T1 C1T H1T2 108.7 . . ? C1T C2T H2T1 109.5 . . ? C1T C2T H2T2 109.5 . . ? H2T1 C2T H2T2 109.5 . . ? C1T C2T H2T3 109.5 . . ? H2T1 C2T H2T3 109.5 . . ? H2T2 C2T H2T3 109.5 . . ? C4S O2S C3S 25.1(16) 3_665 . ? C4S C3S O2S 65(3) 3_665 . ? C4S C3S C4S 56(3) 3_665 . ? O2S C3S C4S 117.3(14) . . ? C4S C3S C3S 40(3) 3_665 3_665 ? O2S C3S C3S 102.7(15) . 3_665 ? C4S C3S C3S 15.9(10) . 3_665 ? C3S C4S C4S 99(4) 3_665 3_665 ? C3S C4S O2S 90(4) 3_665 3_665 ? C4S C4S O2S 155(3) 3_665 3_665 ? C3S C4S C3S 124(3) 3_665 . ? C4S C4S C3S 24.7(17) 3_665 . ? O2S C4S C3S 140.1(16) 3_665 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1S H1S O2S 0.82 2.38 3.175(13) 162.5 . O1T H1T O2S 0.82 1.95 2.771(12) 174.8 . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 21.98 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.435 _refine_diff_density_min -1.097 _refine_diff_density_rms 0.075