Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_s980bsq _database_code_depnum_ccdc_archive 'CCDC 278652' #------------------------------------------------------------------------------ _audit_creation_date 19101-10-02 _audit_creation_method 'by teXsan v1.7' _audit_update_record ; ? ; _publ_section_abstract ; ENTER ABSTRACT ; _publ_section_exptl_prep ; ENTER EXPERIMENTAL SECTION ; _publ_section_exptl_refinement ; The data were collected using the RAXIS in 44 x 1.5 degree phi oscillations of 30 minutes per exposure. The structure was solved by direct methods. In addition to the V cluster, a propanol and water molecules were found. SQUEEZE was used to indicate further solvent incorporation: 158.9e/cell ~ 4 x C3H8O + 2 x H2O, which was included in the formula. H atoms bonded to C were included in calculated positions. Other H atoms were not included. Refining the Flack parameter suggested that the crystal is a racemic twin. The thermal motion was very high in some parts of the molecule, and restraints were used on some bond lengths and angles and on the anisotropic thermal motion of the C atoms. In addition it was nescessary to constrain ring F to be a regular hexagon. Most non H atoms were refined anisotropically, except for some of the C atoms of the propanyl molecules where the thermal motion was particularly high. ; _publ_section_comment ; ENTER TEXT ; _publ_section_references ; ENTER OTHER REFERENCES Molecular Structure Corporation. (1995). teXsan. Single Crystal Structure Analysis Software. Version 1.7. MSC, 3200 Research Forest Drive, The Woodlands, TX 77381, USA. Sheldrick, G.M. (1985). In: "Crystallographic Computing 3" (Eds G.M. Sheldrick, C. Kruger and R. Goddard) Oxford University Press, pp. 175-189. ; _publ_section_acknowledgements ; ENTER ACKNOWLEDGEMENTS ; _publ_section_table_legends ; ENTER TABLE LEGENDS ; _publ_section_figure_captions ; ENTER FIGURE CAPTIONS ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C73.50 H122.50 O29.75 V6' _chemical_formula_weight 1787.85 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' 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' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'P -4 21 c ' _symmetry_Int_Tables_number 114 _symmetry_space_group_name_Hall ? 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' '-y, x, -z' 'y+1/2, x+1/2, z+1/2' 'y, -x, -z' '-y+1/2, -x+1/2, z+1/2' _cell_length_a 27.942(10) _cell_length_b 27.942 _cell_length_c 25.627(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 20008(8) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 88493 _cell_measurement_theta_min 1.63 _cell_measurement_theta_max 24.78 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.187 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7516 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rigaku rotating anode' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'image plate' _diffrn_measurement_device 'Rigaku RAXIS' _diffrn_measurement_method '44 x 1.5 degree phi scans' _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 88493 _diffrn_reflns_av_R_equivalents 0.06 _diffrn_reflns_av_sigmaI/netI 0.0781 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 24.78 _reflns_number_total 12419 _reflns_number_gt 8237 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'MSC RAXIS11 Control' _computing_cell_refinement 'DENZO (Otwinowski, Z. 1988)' _computing_data_reduction 'DENZO (Otwinowski, Z. 1988)' _computing_structure_solution ; SIR97 (Altomare, et. al. 1997) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'teXsan (MSC, 1995)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0912P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(3) _refine_ls_number_reflns 12419 _refine_ls_number_parameters 884 _refine_ls_number_restraints 550 _refine_ls_R_factor_all 0.0813 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1446 _refine_ls_wR_factor_gt 0.1328 _refine_ls_goodness_of_fit_ref 0.928 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.30623(4) 0.11801(4) 0.10804(5) 0.0554(3) Uani 1 1 d . . . V2 V 0.42005(4) 0.06255(4) 0.10427(5) 0.0496(3) Uani 1 1 d . . . V3 V 0.49211(4) 0.14600(4) 0.10459(5) 0.0461(3) Uani 1 1 d . . . V4 V 0.48623(4) 0.27242(4) 0.09862(5) 0.0540(3) Uani 1 1 d . . . V5 V 0.37739(4) 0.29008(4) 0.09833(5) 0.0576(3) Uani 1 1 d . . . V6 V 0.27024(4) 0.22271(4) 0.11056(5) 0.0581(3) Uani 1 1 d . . . O1A O 0.30164(18) 0.06916(19) 0.05011(18) 0.0592(14) Uani 1 1 d . . . O2A O 0.37726(19) 0.03979(18) 0.04523(19) 0.0565(13) Uani 1 1 d . . . O1B O 0.30377(18) 0.06850(18) 0.16482(18) 0.0561(13) Uani 1 1 d . . . O2B O 0.37799(18) 0.03808(18) 0.1618(2) 0.0568(14) Uani 1 1 d . . . O1C O 0.53506(17) 0.16838(18) 0.16251(16) 0.0504(12) Uani 1 1 d . . . O2C O 0.52796(16) 0.24913(17) 0.15858(17) 0.0485(12) Uani 1 1 d . . . O2D O 0.52828(17) 0.24413(18) 0.04235(18) 0.0538(13) Uani 1 1 d . . . O1D O 0.53853(16) 0.16556(18) 0.04923(16) 0.0476(12) Uani 1 1 d . . . O1E O 0.3359(2) 0.31447(19) 0.03868(19) 0.0650(15) Uani 1 1 d . . . O2E O 0.26905(19) 0.2701(2) 0.05221(19) 0.0623(14) Uani 1 1 d . . . O1F O 0.3387(2) 0.32222(19) 0.15352(19) 0.0659(15) Uani 1 1 d . . . O2F O 0.2771(2) 0.2727(2) 0.16803(18) 0.0661(15) Uani 1 1 d . . . O1G O 0.45503(16) 0.10538(16) 0.15117(16) 0.0455(12) Uani 1 1 d . . . O1I O 0.45677(16) 0.10372(16) 0.05565(16) 0.0446(12) Uani 1 1 d . . . O1J O 0.43251(18) 0.28457(17) 0.14645(16) 0.0549(13) Uani 1 1 d . . . O1K O 0.43099(18) 0.27847(18) 0.05127(17) 0.0576(13) Uani 1 1 d . . . O1L O 0.28966(18) 0.16987(18) 0.15628(17) 0.0584(14) Uani 1 1 d . . . O1M O 0.28282(18) 0.16938(18) 0.06259(17) 0.0581(14) Uani 1 1 d . . . O1N O 0.22743(18) 0.0980(2) 0.1090(2) 0.0780(15) Uani 1 1 d . . . O1O O 0.54518(14) 0.08534(15) 0.10774(19) 0.0542(11) Uani 1 1 d . . . O1P O 0.4017(2) 0.36815(19) 0.0946(2) 0.0876(17) Uani 1 1 d . . . O1 O 0.36421(13) 0.12078(14) 0.10541(17) 0.0486(10) Uani 1 1 d . . . O2 O 0.46263(14) 0.19559(14) 0.10226(17) 0.0470(10) Uani 1 1 d . . . O3 O 0.35001(15) 0.23902(15) 0.10327(19) 0.0546(11) Uani 1 1 d . . . O1W O 0.45207(15) 0.01435(15) 0.1036(2) 0.0580(12) Uani 1 1 d . . . O2W O 0.50997(17) 0.32519(15) 0.09706(18) 0.0613(13) Uani 1 1 d . . . O3W O 0.21289(16) 0.22044(18) 0.1139(2) 0.0676(14) Uani 1 1 d . . . C1A C 0.3359(3) 0.0457(3) 0.0289(3) 0.0570(19) Uani 1 1 d U . . C2A C 0.3238(3) 0.0230(3) -0.0228(3) 0.0593(18) Uani 1 1 d U . . C3A C 0.2810(3) 0.0306(3) -0.0475(3) 0.077(2) Uani 1 1 d U . . H3A H 0.2580 0.0491 -0.0308 0.092 Uiso 1 1 calc R . . C4A C 0.2708(4) 0.0121(3) -0.0958(3) 0.087(2) Uani 1 1 d U . . H4A H 0.2415 0.0184 -0.1114 0.104 Uiso 1 1 calc R . . C5A C 0.3036(4) -0.0156(3) -0.1207(3) 0.093(3) Uani 1 1 d U . . H5A H 0.2964 -0.0294 -0.1528 0.111 Uiso 1 1 calc R . . C6A C 0.3493(3) -0.0231(3) -0.0972(3) 0.079(2) Uani 1 1 d U . . H6A H 0.3726 -0.0409 -0.1144 0.094 Uiso 1 1 calc R . . C7A C 0.3583(3) -0.0042(3) -0.0499(3) 0.071(2) Uani 1 1 d U . . H7A H 0.3880 -0.0093 -0.0346 0.086 Uiso 1 1 calc R . . C1B C 0.3381(3) 0.0444(3) 0.1833(3) 0.0532(18) Uani 1 1 d U . . C2B C 0.3293(3) 0.0187(3) 0.2335(3) 0.0625(19) Uani 1 1 d U . . C3B C 0.2843(3) 0.0230(3) 0.2584(4) 0.094(3) Uani 1 1 d U . . H3B H 0.2599 0.0417 0.2444 0.113 Uiso 1 1 calc R . . C4B C 0.2785(4) -0.0025(4) 0.3053(4) 0.116(3) Uani 1 1 d U . . H4B H 0.2487 -0.0020 0.3217 0.140 Uiso 1 1 calc R . . C5B C 0.3137(4) -0.0271(4) 0.3271(4) 0.102(3) Uani 1 1 d U . . H5B H 0.3083 -0.0420 0.3590 0.123 Uiso 1 1 calc R . . C6B C 0.3575(4) -0.0314(3) 0.3045(3) 0.089(3) Uani 1 1 d U . . H6B H 0.3816 -0.0490 0.3206 0.107 Uiso 1 1 calc R . . C7B C 0.3659(3) -0.0088(3) 0.2566(3) 0.071(2) Uani 1 1 d U . . H7B H 0.3954 -0.0119 0.2402 0.085 Uiso 1 1 calc R . . C1C C 0.5431(3) 0.2109(3) 0.1789(3) 0.0474(16) Uani 1 1 d U . . C2C C 0.5741(3) 0.2143(3) 0.2270(2) 0.0497(16) Uani 1 1 d U . . C3C C 0.5931(3) 0.1749(3) 0.2493(3) 0.0540(18) Uani 1 1 d U . . H3C H 0.5859 0.1449 0.2357 0.065 Uiso 1 1 calc R . . C4C C 0.6224(3) 0.1784(3) 0.2911(3) 0.069(2) Uani 1 1 d U . . H4C H 0.6346 0.1509 0.3065 0.083 Uiso 1 1 calc R . . C5C C 0.6341(3) 0.2226(3) 0.3108(3) 0.069(2) Uani 1 1 d U . . H5C H 0.6554 0.2253 0.3385 0.083 Uiso 1 1 calc R . . C6C C 0.6134(3) 0.2637(3) 0.2886(3) 0.076(2) Uani 1 1 d U . . H6C H 0.6200 0.2937 0.3027 0.091 Uiso 1 1 calc R . . C7C C 0.5843(3) 0.2601(3) 0.2474(3) 0.0612(18) Uani 1 1 d U . . H7C H 0.5710 0.2874 0.2324 0.073 Uiso 1 1 calc R . . C1D C 0.5444(3) 0.2060(3) 0.0267(3) 0.0474(16) Uani 1 1 d U . . C2D C 0.5763(2) 0.2062(3) -0.0199(2) 0.0454(15) Uani 1 1 d U . . C3D C 0.5990(3) 0.1651(3) -0.0369(3) 0.0581(18) Uani 1 1 d U . . H3D H 0.5937 0.1361 -0.0200 0.070 Uiso 1 1 calc R . . C4D C 0.6298(3) 0.1673(3) -0.0795(3) 0.0627(19) Uani 1 1 d U . . H4D H 0.6461 0.1401 -0.0902 0.075 Uiso 1 1 calc R . . C5D C 0.6361(3) 0.2103(3) -0.1059(3) 0.0639(18) Uani 1 1 d U . . H5D H 0.6568 0.2117 -0.1344 0.077 Uiso 1 1 calc R . . C6D C 0.6120(3) 0.2508(3) -0.0904(3) 0.0606(18) Uani 1 1 d U . . H6D H 0.6152 0.2791 -0.1090 0.073 Uiso 1 1 calc R . . C7D C 0.5828(3) 0.2489(3) -0.0464(3) 0.0546(17) Uani 1 1 d U . . H7D H 0.5676 0.2765 -0.0348 0.066 Uiso 1 1 calc R . . C1E C 0.2946(3) 0.2984(3) 0.0262(3) 0.063(2) Uani 1 1 d U . . C2E C 0.2750(3) 0.3163(3) -0.0242(3) 0.069(2) Uani 1 1 d U . . C3E C 0.3010(3) 0.3462(3) -0.0548(3) 0.072(2) Uani 1 1 d U . . H3E H 0.3310 0.3567 -0.0441 0.087 Uiso 1 1 calc R . . C4E C 0.2813(3) 0.3619(3) -0.1049(4) 0.086(2) Uani 1 1 d U . . H4E H 0.2990 0.3813 -0.1271 0.103 Uiso 1 1 calc R . . C5E C 0.2359(4) 0.3470(3) -0.1181(4) 0.102(3) Uani 1 1 d U . . H5E H 0.2220 0.3573 -0.1491 0.123 Uiso 1 1 calc R . . C6E C 0.2106(4) 0.3160(4) -0.0844(4) 0.119(3) Uani 1 1 d U . . H6E H 0.1803 0.3055 -0.0938 0.143 Uiso 1 1 calc R . . C7E C 0.2297(3) 0.3014(4) -0.0385(3) 0.098(3) Uani 1 1 d U . . H7E H 0.2123 0.2813 -0.0166 0.118 Uiso 1 1 calc R . . C1F C 0.3028(4) 0.3086(4) 0.1792(3) 0.068(2) Uani 1 1 d U . . C2F C 0.2898(2) 0.3394(2) 0.2242(2) 0.091(3) Uani 1 1 d GU . . C3F C 0.2472(3) 0.3315(3) 0.2508(3) 0.140(4) Uani 1 1 d GU . . H3F H 0.2292 0.3042 0.2438 0.168 Uiso 1 1 calc R . . C4F C 0.2316(3) 0.3642(3) 0.2879(3) 0.194(5) Uani 1 1 d GU . . H4F H 0.2031 0.3589 0.3057 0.233 Uiso 1 1 calc R . . C5F C 0.2585(3) 0.4049(3) 0.2984(3) 0.206(6) Uani 1 1 d GU . . H5F H 0.2480 0.4268 0.3232 0.248 Uiso 1 1 calc R . . C6F C 0.3011(3) 0.4129(3) 0.2717(3) 0.176(5) Uani 1 1 d GU . . H6F H 0.3191 0.4401 0.2787 0.211 Uiso 1 1 calc R . . C7F C 0.3168(2) 0.3802(3) 0.2346(3) 0.126(4) Uani 1 1 d GU . . H7F H 0.3452 0.3855 0.2168 0.151 Uiso 1 1 calc R . . C1G C 0.4569(3) 0.1037(3) 0.2081(3) 0.081(3) Uani 1 1 d DU . . H1G1 H 0.4248 0.0982 0.2214 0.097 Uiso 1 1 calc R . . H1G2 H 0.4676 0.1345 0.2210 0.097 Uiso 1 1 calc R . . C2G C 0.4887(4) 0.0663(3) 0.2279(3) 0.098(3) Uani 1 1 d DU . . H2G1 H 0.5208 0.0712 0.2145 0.118 Uiso 1 1 calc R . . H2G2 H 0.4776 0.0352 0.2164 0.118 Uiso 1 1 calc R . . C3G C 0.4892(5) 0.0683(5) 0.2889(3) 0.166(6) Uani 1 1 d DU . . H3G1 H 0.5099 0.0437 0.3021 0.249 Uiso 1 1 calc R . . H3G2 H 0.4574 0.0635 0.3019 0.249 Uiso 1 1 calc R . . H3G3 H 0.5007 0.0990 0.3000 0.249 Uiso 1 1 calc R . . C1I C 0.4601(3) 0.1007(4) 0.0020(3) 0.091(3) Uani 1 1 d DU . . H1I1 H 0.4713 0.1312 -0.0113 0.110 Uiso 1 1 calc R . . H1I2 H 0.4284 0.0952 -0.0121 0.110 Uiso 1 1 calc R . . C2I C 0.4910(4) 0.0643(4) -0.0162(4) 0.126(4) Uani 1 1 d DU . . H2I1 H 0.4788 0.0333 -0.0055 0.151 Uiso 1 1 calc R . . H2I2 H 0.5225 0.0685 -0.0010 0.151 Uiso 1 1 calc R . . C3I C 0.4949(5) 0.0661(5) -0.0774(4) 0.189(7) Uani 1 1 d DU . . H3I1 H 0.5161 0.0413 -0.0891 0.284 Uiso 1 1 calc R . . H3I2 H 0.5071 0.0967 -0.0879 0.284 Uiso 1 1 calc R . . H3I3 H 0.4638 0.0612 -0.0924 0.284 Uiso 1 1 calc R . . C1J C 0.4306(3) 0.2857(4) 0.2017(3) 0.087(3) Uani 1 1 d DU . . H1J1 H 0.4088 0.3108 0.2128 0.104 Uiso 1 1 calc R . . H1J2 H 0.4621 0.2931 0.2155 0.104 Uiso 1 1 calc R . . C2J C 0.4143(5) 0.2396(5) 0.2226(4) 0.151(5) Uani 1 1 d DU . . H2J1 H 0.4360 0.2148 0.2107 0.181 Uiso 1 1 calc R . . H2J2 H 0.3829 0.2326 0.2084 0.181 Uiso 1 1 calc R . . C3J C 0.4115(6) 0.2374(6) 0.2804(4) 0.210(8) Uani 1 1 d DU . . H3J1 H 0.4008 0.2062 0.2909 0.314 Uiso 1 1 calc R . . H3J2 H 0.3893 0.2611 0.2927 0.314 Uiso 1 1 calc R . . H3J3 H 0.4425 0.2435 0.2950 0.314 Uiso 1 1 calc R . . C1K C 0.4245(5) 0.2615(6) -0.0029(5) 0.172(6) Uani 1 1 d DU . . H1K1 H 0.4420 0.2322 -0.0095 0.207 Uiso 1 1 calc R . . H1K2 H 0.3910 0.2568 -0.0113 0.207 Uiso 1 1 calc R . . C2K C 0.4437(8) 0.2997(7) -0.0296(8) 0.246(8) Uiso 1 1 d DU . . H2K1 H 0.4761 0.3070 -0.0185 0.296 Uiso 1 1 calc R . . H2K2 H 0.4239 0.3282 -0.0270 0.296 Uiso 1 1 calc R . . C3K C 0.4421(11) 0.2764(10) -0.0877(9) 0.405(16) Uiso 1 1 d DU . . H3K1 H 0.4546 0.2989 -0.1125 0.607 Uiso 1 1 calc R . . H3K2 H 0.4097 0.2686 -0.0965 0.607 Uiso 1 1 calc R . . H3K3 H 0.4613 0.2478 -0.0882 0.607 Uiso 1 1 calc R . . C1L C 0.2903(3) 0.1693(3) 0.2121(3) 0.075(2) Uani 1 1 d DU . . H1L1 H 0.3056 0.1983 0.2247 0.090 Uiso 1 1 calc R . . H1L2 H 0.3093 0.1423 0.2239 0.090 Uiso 1 1 calc R . . C2L C 0.2416(3) 0.1658(4) 0.2347(3) 0.105(3) Uani 1 1 d DU . . H2L1 H 0.2263 0.1368 0.2225 0.126 Uiso 1 1 calc R . . H2L2 H 0.2225 0.1928 0.2232 0.126 Uiso 1 1 calc R . . C3L C 0.2443(5) 0.1654(5) 0.2935(3) 0.157(5) Uani 1 1 d DU . . H3L1 H 0.2126 0.1631 0.3077 0.236 Uiso 1 1 calc R . . H3L2 H 0.2590 0.1945 0.3054 0.236 Uiso 1 1 calc R . . H3L3 H 0.2630 0.1385 0.3048 0.236 Uiso 1 1 calc R . . C1M C 0.2741(5) 0.1682(4) 0.0078(4) 0.143(5) Uani 1 1 d DU . . H1M1 H 0.2636 0.1364 -0.0023 0.172 Uiso 1 1 calc R . . H1M2 H 0.2489 0.1906 -0.0009 0.172 Uiso 1 1 calc R . . C2M C 0.3156(6) 0.1801(7) -0.0197(7) 0.225(7) Uiso 1 1 d DU . . H2M1 H 0.3413 0.1572 -0.0151 0.270 Uiso 1 1 calc R . . H2M2 H 0.3268 0.2123 -0.0127 0.270 Uiso 1 1 calc R . . C3M C 0.2873(9) 0.1747(10) -0.0779(7) 0.368(15) Uiso 1 1 d DU . . H3M1 H 0.3097 0.1802 -0.1057 0.552 Uiso 1 1 calc R . . H3M2 H 0.2619 0.1977 -0.0800 0.552 Uiso 1 1 calc R . . H3M3 H 0.2743 0.1430 -0.0811 0.552 Uiso 1 1 calc R . . C1N C 0.2078(5) 0.0507(5) 0.1153(6) 0.170(5) Uani 1 1 d DU . . H1N1 H 0.2339 0.0283 0.1207 0.204 Uiso 1 1 calc R . . H1N2 H 0.1879 0.0502 0.1463 0.204 Uiso 1 1 calc R . . C2N C 0.1805(7) 0.0356(7) 0.0724(7) 0.244(8) Uiso 1 1 d DU . . H2N1 H 0.2007 0.0303 0.0422 0.293 Uiso 1 1 calc R . . H2N2 H 0.1563 0.0591 0.0637 0.293 Uiso 1 1 calc R . . C3N C 0.1561(9) -0.0141(8) 0.0914(10) 0.343(13) Uiso 1 1 d DU . . H3N1 H 0.1360 -0.0263 0.0641 0.515 Uiso 1 1 calc R . . H3N2 H 0.1372 -0.0083 0.1220 0.515 Uiso 1 1 calc R . . H3N3 H 0.1806 -0.0370 0.0994 0.515 Uiso 1 1 calc R . . C1O C 0.5971(3) 0.0856(3) 0.1201(4) 0.094(3) Uani 1 1 d DU . . H1O1 H 0.6055 0.1162 0.1354 0.113 Uiso 1 1 calc R . . H1O2 H 0.6038 0.0609 0.1457 0.113 Uiso 1 1 calc R . . C2O C 0.6257(3) 0.0777(3) 0.0747(3) 0.087(2) Uani 1 1 d DU . . H2O1 H 0.6258 0.1059 0.0526 0.105 Uiso 1 1 calc R . . H2O2 H 0.6133 0.0509 0.0547 0.105 Uiso 1 1 calc R . . C3O C 0.6790(3) 0.0663(3) 0.0953(5) 0.120(4) Uani 1 1 d DU . . H3O1 H 0.6997 0.0605 0.0660 0.180 Uiso 1 1 calc R . . H3O2 H 0.6783 0.0384 0.1172 0.180 Uiso 1 1 calc R . . H3O3 H 0.6908 0.0931 0.1149 0.180 Uiso 1 1 calc R . . C1P C 0.4107(12) 0.3980(10) 0.0612(9) 0.338(13) Uiso 1 1 d DU . . H1P1 H 0.3958 0.3847 0.0302 0.406 Uiso 1 1 calc R . . H1P2 H 0.4448 0.3941 0.0557 0.406 Uiso 1 1 calc R . . C2P C 0.4039(11) 0.4487(9) 0.0545(9) 0.332(12) Uiso 1 1 d DU . . H2P1 H 0.4260 0.4674 0.0754 0.399 Uiso 1 1 calc R . . H2P2 H 0.3713 0.4586 0.0619 0.399 Uiso 1 1 calc R . . C3P C 0.4166(9) 0.4511(9) -0.0085(9) 0.316(13) Uiso 1 1 d DU . . H3P1 H 0.4134 0.4835 -0.0206 0.475 Uiso 1 1 calc R . . H3P2 H 0.3949 0.4308 -0.0274 0.475 Uiso 1 1 calc R . . H3P3 H 0.4489 0.4404 -0.0140 0.475 Uiso 1 1 calc R . . O1S O 0.1476(4) 0.1549(4) 0.0965(5) 0.187(4) Uiso 1 1 d . . . C1S C 0.1087(10) 0.1631(10) 0.0574(10) 0.297(12) Uiso 1 1 d U . . H1S1 H 0.1213 0.1504 0.0250 0.357 Uiso 1 1 calc R . . H1S2 H 0.0834 0.1413 0.0678 0.357 Uiso 1 1 calc R . . C2S C 0.0858(10) 0.2034(12) 0.0434(11) 0.315(12) Uiso 1 1 d U . . H2S1 H 0.0627 0.2109 0.0705 0.378 Uiso 1 1 calc R . . H2S2 H 0.0678 0.1967 0.0118 0.378 Uiso 1 1 calc R . . C3S C 0.1134(6) 0.2444(6) 0.0344(6) 0.171(6) Uiso 1 1 d U . . H3S1 H 0.0929 0.2702 0.0236 0.257 Uiso 1 1 calc R . . H3S2 H 0.1364 0.2380 0.0076 0.257 Uiso 1 1 calc R . . H3S3 H 0.1297 0.2532 0.0660 0.257 Uiso 1 1 calc R . . O4W O 0.0507(7) 0.1198(7) 0.3242(8) 0.368(10) 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 0.0496(7) 0.0582(8) 0.0584(7) 0.0061(7) 0.0038(7) 0.0108(6) V2 0.0452(7) 0.0449(7) 0.0588(7) 0.0047(7) 0.0008(7) 0.0052(5) V3 0.0484(7) 0.0434(6) 0.0465(6) 0.0003(6) 0.0013(6) 0.0025(5) V4 0.0601(8) 0.0485(7) 0.0534(7) 0.0036(6) -0.0009(6) 0.0067(6) V5 0.0630(8) 0.0555(7) 0.0542(7) 0.0019(7) -0.0036(7) 0.0156(6) V6 0.0601(8) 0.0605(8) 0.0538(7) 0.0011(6) 0.0013(7) 0.0190(6) O1A 0.046(3) 0.065(4) 0.066(3) -0.006(3) -0.009(3) 0.009(3) O2A 0.044(3) 0.062(3) 0.064(3) 0.000(3) -0.002(3) 0.006(3) O1B 0.044(3) 0.065(3) 0.059(3) 0.011(3) 0.005(2) 0.011(3) O2B 0.040(3) 0.052(3) 0.079(4) 0.019(3) 0.006(3) 0.002(3) O1C 0.052(3) 0.048(3) 0.050(3) -0.006(2) -0.004(2) -0.001(3) O2C 0.047(3) 0.046(3) 0.053(3) 0.000(2) -0.001(2) 0.008(3) O2D 0.057(3) 0.046(3) 0.058(3) 0.001(2) 0.001(2) 0.003(3) O1D 0.045(3) 0.048(3) 0.049(3) -0.006(2) -0.001(2) 0.005(3) O1E 0.074(4) 0.055(3) 0.066(3) 0.006(3) -0.005(3) 0.016(3) O2E 0.060(3) 0.064(3) 0.063(3) -0.001(3) -0.009(3) 0.013(3) O1F 0.075(4) 0.065(4) 0.058(3) -0.004(3) -0.008(3) 0.017(3) O2F 0.071(4) 0.074(4) 0.053(3) -0.003(3) 0.002(3) 0.029(4) O1G 0.047(3) 0.045(3) 0.044(3) 0.002(2) 0.003(2) 0.001(3) O1I 0.048(3) 0.051(3) 0.034(2) -0.003(2) 0.007(2) 0.004(3) O1J 0.071(3) 0.052(3) 0.041(3) -0.005(2) 0.006(2) 0.023(3) O1K 0.070(4) 0.059(3) 0.044(3) -0.001(2) -0.001(2) 0.002(3) O1L 0.058(3) 0.068(3) 0.049(3) 0.001(2) 0.006(2) 0.017(3) O1M 0.069(4) 0.064(3) 0.041(3) -0.006(2) -0.004(2) 0.024(3) O1N 0.061(3) 0.080(4) 0.093(4) 0.002(4) 0.002(3) 0.001(3) O1O 0.038(3) 0.058(3) 0.067(3) 0.002(3) 0.000(3) 0.001(2) O1P 0.120(5) 0.057(3) 0.086(4) 0.007(3) -0.005(4) 0.014(3) O1 0.041(2) 0.053(3) 0.052(3) 0.006(3) -0.002(2) 0.007(2) O2 0.050(3) 0.045(2) 0.047(2) -0.003(2) 0.005(2) 0.008(2) O3 0.061(3) 0.050(3) 0.053(3) 0.001(3) -0.001(3) 0.013(2) O1W 0.046(3) 0.044(3) 0.084(3) 0.010(3) -0.011(3) 0.010(2) O2W 0.075(3) 0.041(3) 0.068(3) 0.008(3) -0.002(3) -0.008(2) O3W 0.051(3) 0.072(3) 0.080(4) 0.003(3) 0.002(3) 0.020(3) C1A 0.067(6) 0.042(5) 0.062(4) 0.007(3) 0.004(4) -0.003(5) C2A 0.064(4) 0.054(5) 0.060(4) 0.005(3) 0.000(3) -0.006(4) C3A 0.083(5) 0.059(5) 0.088(5) -0.009(4) -0.020(4) 0.009(4) C4A 0.108(6) 0.071(6) 0.082(5) -0.003(4) -0.033(5) 0.007(4) C5A 0.132(7) 0.078(6) 0.068(5) 0.000(4) -0.010(4) -0.004(5) C6A 0.101(5) 0.067(5) 0.068(5) -0.005(4) 0.016(4) -0.004(4) C7A 0.081(5) 0.059(5) 0.074(4) -0.007(4) 0.002(4) 0.002(4) C1B 0.055(5) 0.047(5) 0.057(4) 0.002(3) -0.002(4) -0.007(4) C2B 0.071(5) 0.046(4) 0.071(4) 0.012(3) 0.017(3) 0.005(4) C3B 0.091(5) 0.090(6) 0.101(6) 0.031(5) 0.040(5) 0.011(5) C4B 0.102(6) 0.126(8) 0.120(7) 0.054(6) 0.054(5) 0.021(6) C5B 0.115(7) 0.089(7) 0.103(6) 0.044(5) 0.028(5) -0.003(6) C6B 0.105(6) 0.090(6) 0.073(5) 0.025(4) 0.006(4) 0.012(6) C7B 0.083(5) 0.059(5) 0.070(4) 0.014(4) 0.000(4) 0.001(4) C1C 0.053(5) 0.045(5) 0.044(4) 0.004(3) 0.000(3) 0.004(4) C2C 0.054(4) 0.055(4) 0.040(3) -0.001(3) 0.005(3) 0.003(3) C3C 0.051(5) 0.059(4) 0.052(4) -0.002(3) -0.010(3) -0.002(4) C4C 0.081(6) 0.068(4) 0.059(4) 0.003(4) -0.024(4) -0.003(4) C5C 0.072(5) 0.074(4) 0.062(5) -0.005(4) -0.013(4) -0.011(4) C6C 0.093(6) 0.063(4) 0.072(5) -0.002(4) -0.015(4) -0.013(5) C7C 0.062(5) 0.060(4) 0.062(4) 0.001(3) -0.004(3) -0.012(4) C1D 0.050(5) 0.043(5) 0.049(4) 0.004(3) -0.009(3) 0.001(4) C2D 0.040(4) 0.047(4) 0.049(3) 0.005(3) 0.000(3) -0.007(3) C3D 0.062(5) 0.054(4) 0.058(4) 0.003(3) 0.002(3) 0.002(4) C4D 0.065(5) 0.071(4) 0.053(4) -0.010(3) 0.000(3) 0.003(4) C5D 0.059(4) 0.079(4) 0.054(4) -0.003(4) 0.007(4) -0.016(4) C6D 0.066(5) 0.069(4) 0.047(4) -0.001(3) 0.006(3) -0.016(4) C7D 0.060(5) 0.054(4) 0.050(4) 0.002(3) -0.002(3) -0.005(4) C1E 0.058(5) 0.073(6) 0.060(4) 0.006(4) 0.003(4) 0.022(5) C2E 0.066(4) 0.068(5) 0.072(4) 0.018(4) -0.007(3) 0.019(4) C3E 0.074(5) 0.077(6) 0.066(4) 0.014(4) -0.007(4) 0.011(4) C4E 0.104(5) 0.074(5) 0.079(5) 0.020(4) -0.017(5) 0.015(4) C5E 0.125(7) 0.100(7) 0.082(6) 0.036(5) -0.044(5) -0.008(6) C6E 0.111(7) 0.129(8) 0.117(7) 0.057(6) -0.051(5) -0.019(6) C7E 0.072(5) 0.118(7) 0.105(6) 0.062(5) -0.022(4) 0.002(5) C1F 0.075(6) 0.065(5) 0.065(5) -0.009(4) -0.017(4) 0.030(5) C2F 0.083(6) 0.131(7) 0.059(5) -0.033(4) 0.006(4) -0.002(5) C3F 0.131(8) 0.187(9) 0.102(7) -0.063(6) 0.049(5) -0.039(7) C4F 0.195(10) 0.230(12) 0.158(9) -0.109(8) 0.113(8) -0.079(8) C5F 0.226(12) 0.246(12) 0.148(9) -0.125(9) 0.108(8) -0.091(9) C6F 0.173(10) 0.193(10) 0.161(9) -0.113(8) 0.071(7) -0.063(8) C7F 0.127(8) 0.152(9) 0.099(7) -0.073(6) 0.024(6) -0.027(6) C1G 0.084(6) 0.090(6) 0.068(5) 0.021(5) -0.013(5) -0.017(5) C2G 0.110(8) 0.104(7) 0.081(5) 0.030(5) -0.024(6) -0.009(6) C3G 0.214(14) 0.203(13) 0.081(5) 0.069(7) -0.061(8) -0.067(12) C1I 0.083(7) 0.113(8) 0.078(6) -0.025(5) 0.022(5) -0.069(6) C2I 0.130(9) 0.149(10) 0.099(6) -0.014(7) 0.004(7) -0.019(7) C3I 0.223(14) 0.250(16) 0.096(6) -0.079(8) 0.069(8) -0.115(13) C1J 0.077(6) 0.131(8) 0.052(5) -0.012(4) -0.004(4) 0.033(6) C2J 0.148(10) 0.214(11) 0.090(5) 0.071(8) 0.025(7) 0.015(9) C3J 0.256(17) 0.288(18) 0.085(6) 0.082(9) -0.013(9) 0.033(15) C1K 0.123(9) 0.258(15) 0.137(10) 0.034(10) 0.047(8) 0.106(10) C1L 0.089(6) 0.070(5) 0.066(5) 0.003(4) 0.012(4) 0.012(5) C2L 0.116(7) 0.119(7) 0.081(5) 0.026(6) 0.046(6) 0.041(7) C3L 0.216(14) 0.181(12) 0.075(5) 0.013(7) 0.062(7) 0.049(11) C1M 0.222(13) 0.067(7) 0.141(9) 0.015(6) 0.084(9) 0.058(8) C1N 0.127(10) 0.169(12) 0.214(13) -0.002(11) -0.049(10) 0.025(9) C1O 0.088(6) 0.058(5) 0.137(8) 0.001(5) 0.030(5) -0.008(5) C2O 0.091(6) 0.079(6) 0.092(6) 0.000(5) -0.009(4) -0.001(5) C3O 0.056(5) 0.088(7) 0.217(12) -0.014(9) -0.005(6) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.623(4) . ? V1 O1L 1.960(5) . ? V1 O1M 1.961(5) . ? V1 O1B 2.009(5) . ? V1 O1A 2.021(5) . ? V1 O1N 2.272(5) . ? V1 V6 3.0943(16) . ? V2 O1W 1.617(4) . ? V2 O1G 1.957(5) . ? V2 O1I 1.982(4) . ? V2 O2B 2.006(5) . ? V2 O2A 2.031(5) . ? V2 O1 2.254(4) . ? V2 V3 3.0806(16) . ? V3 O2 1.613(4) . ? V3 O1G 1.946(5) . ? V3 O1I 1.986(5) . ? V3 O1D 1.998(5) . ? V3 O1C 2.009(5) . ? V3 O1O 2.254(4) . ? V4 O2W 1.617(4) . ? V4 O1K 1.971(5) . ? V4 O1J 1.968(5) . ? V4 O2D 2.021(5) . ? V4 O2C 2.036(5) . ? V4 O2 2.248(4) . ? V4 V5 3.081(2) . ? V5 O3 1.624(4) . ? V5 O1K 1.950(5) . ? V5 O1J 1.979(5) . ? V5 O1F 1.994(6) . ? V5 O1E 2.036(5) . ? V5 O1P 2.287(6) . ? V6 O3W 1.606(5) . ? V6 O1L 1.961(5) . ? V6 O1M 1.964(5) . ? V6 O2E 1.998(5) . ? V6 O2F 2.040(6) . ? V6 O3 2.283(5) . ? O1A C1A 1.283(9) . ? O2A C1A 1.239(9) . ? O1B C1B 1.265(9) . ? O2B C1B 1.254(9) . ? O1C C1C 1.280(8) . ? O2C C1C 1.261(8) . ? O2D C1D 1.226(8) . ? O1D C1D 1.279(8) . ? O1E C1E 1.278(10) . ? O2E C1E 1.257(10) . ? O1F C1F 1.259(11) . ? O2F C1F 1.265(10) . ? O1G C1G 1.460(9) . ? O1I C1I 1.380(9) . ? O1J C1J 1.418(8) . ? O1K C1K 1.478(15) . ? O1L C1L 1.430(8) . ? O1M C1M 1.426(12) . ? O1N C1N 1.438(14) . ? O1O C1O 1.484(10) . ? O1P C1P 1.22(2) . ? C1A C2A 1.508(11) . ? C2A C3A 1.369(11) . ? C2A C7A 1.408(11) . ? C3A C4A 1.372(11) . ? C3A H3A 0.9300 . ? C4A C5A 1.357(12) . ? C4A H4A 0.9300 . ? C5A C6A 1.428(13) . ? C5A H5A 0.9300 . ? C6A C7A 1.346(11) . ? C6A H6A 0.9300 . ? C7A H7A 0.9300 . ? C1B C2B 1.495(10) . ? C2B C3B 1.414(11) . ? C2B C7B 1.409(11) . ? C3B C4B 1.408(12) . ? C3B H3B 0.9300 . ? C4B C5B 1.326(13) . ? C4B H4B 0.9300 . ? C5B C6B 1.359(13) . ? C5B H5B 0.9300 . ? C6B C7B 1.399(11) . ? C6B H6B 0.9300 . ? C7B H7B 0.9300 . ? C1C C2C 1.510(9) . ? C2C C3C 1.349(9) . ? C2C C7C 1.412(10) . ? C3C C4C 1.352(10) . ? C3C H3C 0.9300 . ? C4C C5C 1.374(10) . ? C4C H4C 0.9300 . ? C5C C6C 1.406(11) . ? C5C H5C 0.9300 . ? C6C C7C 1.337(10) . ? C6C H6C 0.9300 . ? C7C H7C 0.9300 . ? C1D C2D 1.489(9) . ? C2D C3D 1.382(10) . ? C2D C7D 1.386(9) . ? C3D C4D 1.390(10) . ? C3D H3D 0.9300 . ? C4D C5D 1.390(10) . ? C4D H4D 0.9300 . ? C5D C6D 1.377(10) . ? C5D H5D 0.9300 . ? C6D C7D 1.391(10) . ? C6D H6D 0.9300 . ? C7D H7D 0.9300 . ? C1E C2E 1.491(10) . ? C2E C3E 1.358(10) . ? C2E C7E 1.381(12) . ? C3E C4E 1.462(11) . ? C3E H3E 0.9300 . ? C4E C5E 1.377(12) . ? C4E H4E 0.9300 . ? C5E C6E 1.413(13) . ? C5E H5E 0.9300 . ? C6E C7E 1.354(11) . ? C6E H6E 0.9300 . ? C7E H7E 0.9300 . ? C1F C2F 1.484(9) . ? C2F C3F 1.3900 . ? C2F C7F 1.3900 . ? C3F C4F 1.3900 . ? C3F H3F 0.9300 . ? C4F C5F 1.3900 . ? C4F H4F 0.9300 . ? C5F C6F 1.3900 . ? C5F H5F 0.9300 . ? C6F C7F 1.3900 . ? C6F H6F 0.9300 . ? C7F H7F 0.9300 . ? C1G C2G 1.465(9) . ? C1G H1G1 0.9700 . ? C1G H1G2 0.9700 . ? C2G C3G 1.563(10) . ? C2G H2G1 0.9700 . ? C2G H2G2 0.9700 . ? C3G H3G1 0.9600 . ? C3G H3G2 0.9600 . ? C3G H3G3 0.9600 . ? C1I C2I 1.414(11) . ? C1I H1I1 0.9700 . ? C1I H1I2 0.9700 . ? C2I C3I 1.572(11) . ? C2I H2I1 0.9700 . ? C2I H2I2 0.9700 . ? C3I H3I1 0.9600 . ? C3I H3I2 0.9600 . ? C3I H3I3 0.9600 . ? C1J C2J 1.469(11) . ? C1J H1J1 0.9700 . ? C1J H1J2 0.9700 . ? C2J C3J 1.483(11) . ? C2J H2J1 0.9700 . ? C2J H2J2 0.9700 . ? C3J H3J1 0.9600 . ? C3J H3J2 0.9600 . ? C3J H3J3 0.9600 . ? C1K C2K 1.378(14) . ? C1K H1K1 0.9700 . ? C1K H1K2 0.9700 . ? C2K C3K 1.624(15) . ? C2K H2K1 0.9700 . ? C2K H2K2 0.9700 . ? C3K H3K1 0.9600 . ? C3K H3K2 0.9600 . ? C3K H3K3 0.9600 . ? C1L C2L 1.483(10) . ? C1L H1L1 0.9700 . ? C1L H1L2 0.9700 . ? C2L C3L 1.509(10) . ? C2L H2L1 0.9700 . ? C2L H2L2 0.9700 . ? C3L H3L1 0.9600 . ? C3L H3L2 0.9600 . ? C3L H3L3 0.9600 . ? C1M C2M 1.397(13) . ? C1M H1M1 0.9700 . ? C1M H1M2 0.9700 . ? C2M C3M 1.695(14) . ? C2M H2M1 0.9700 . ? C2M H2M2 0.9700 . ? C3M H3M1 0.9600 . ? C3M H3M2 0.9600 . ? C3M H3M3 0.9600 . ? C1N C2N 1.404(13) . ? C1N H1N1 0.9700 . ? C1N H1N2 0.9700 . ? C2N C3N 1.621(14) . ? C2N H2N1 0.9700 . ? C2N H2N2 0.9700 . ? C3N H3N1 0.9600 . ? C3N H3N2 0.9600 . ? C3N H3N3 0.9600 . ? C1O C2O 1.431(9) . ? C1O H1O1 0.9700 . ? C1O H1O2 0.9700 . ? C2O C3O 1.612(10) . ? C2O H2O1 0.9700 . ? C2O H2O2 0.9700 . ? C3O H3O1 0.9600 . ? C3O H3O2 0.9600 . ? C3O H3O3 0.9600 . ? C1P C2P 1.440(15) . ? C1P H1P1 0.9700 . ? C1P H1P2 0.9700 . ? C2P C3P 1.656(15) . ? C2P H2P1 0.9700 . ? C2P H2P2 0.9700 . ? C3P H3P1 0.9600 . ? C3P H3P2 0.9600 . ? C3P H3P3 0.9600 . ? O1S C1S 1.50(3) . ? C1S C2S 1.34(3) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S C3S 1.40(3) . ? C2S H2S1 0.9700 . ? C2S H2S2 0.9700 . ? C3S H3S1 0.9600 . ? C3S H3S2 0.9600 . ? C3S H3S3 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 O1 V1 O1L 103.1(2) . . ? O1 V1 O1M 105.9(2) . . ? O1L V1 O1M 75.80(18) . . ? O1 V1 O1B 95.6(2) . . ? O1L V1 O1B 92.5(2) . . ? O1M V1 O1B 157.4(2) . . ? O1 V1 O1A 93.7(2) . . ? O1L V1 O1A 161.4(2) . . ? O1M V1 O1A 92.1(2) . . ? O1B V1 O1A 93.72(18) . . ? O1 V1 O1N 168.3(2) . . ? O1L V1 O1N 86.9(2) . . ? O1M V1 O1N 82.2(2) . . ? O1B V1 O1N 77.8(2) . . ? O1A V1 O1N 77.3(2) . . ? O1 V1 V6 106.28(15) . . ? O1L V1 V6 37.92(14) . . ? O1M V1 V6 37.99(13) . . ? O1B V1 V6 128.66(15) . . ? O1A V1 V6 129.30(15) . . ? O1N V1 V6 85.29(15) . . ? O1W V2 O1G 103.8(2) . . ? O1W V2 O1I 101.0(2) . . ? O1G V2 O1I 76.87(16) . . ? O1W V2 O2B 92.7(2) . . ? O1G V2 O2B 92.8(2) . . ? O1I V2 O2B 164.4(2) . . ? O1W V2 O2A 93.3(2) . . ? O1G V2 O2A 160.6(2) . . ? O1I V2 O2A 91.0(2) . . ? O2B V2 O2A 95.51(18) . . ? O1W V2 O1 169.79(19) . . ? O1G V2 O1 84.06(18) . . ? O1I V2 O1 87.00(17) . . ? O2B V2 O1 80.27(18) . . ? O2A V2 O1 80.10(19) . . ? O1W V2 V3 105.59(16) . . ? O1G V2 V3 37.76(13) . . ? O1I V2 V3 39.11(13) . . ? O2B V2 V3 129.72(16) . . ? O2A V2 V3 128.59(15) . . ? O1 V2 V3 84.62(11) . . ? O2 V3 O1G 104.6(2) . . ? O2 V3 O1I 103.5(2) . . ? O1G V3 O1I 77.04(16) . . ? O2 V3 O1D 94.0(2) . . ? O1G V3 O1D 160.15(19) . . ? O1I V3 O1D 92.13(18) . . ? O2 V3 O1C 93.7(2) . . ? O1G V3 O1C 92.65(19) . . ? O1I V3 O1C 161.62(19) . . ? O1D V3 O1C 92.96(17) . . ? O2 V3 O1O 169.55(19) . . ? O1G V3 O1O 83.66(18) . . ? O1I V3 O1O 84.40(17) . . ? O1D V3 O1O 78.70(18) . . ? O1C V3 O1O 79.31(19) . . ? O2 V3 V2 108.45(15) . . ? O1G V3 V2 38.02(13) . . ? O1I V3 V2 39.03(13) . . ? O1D V3 V2 129.01(14) . . ? O1C V3 V2 128.90(14) . . ? O1O V3 V2 82.00(11) . . ? O2W V4 O1K 103.2(2) . . ? O2W V4 O1J 99.8(2) . . ? O1K V4 O1J 76.77(18) . . ? O2W V4 O2D 95.8(2) . . ? O1K V4 O2D 92.8(2) . . ? O1J V4 O2D 162.8(2) . . ? O2W V4 O2C 94.3(2) . . ? O1K V4 O2C 160.2(2) . . ? O1J V4 O2C 91.25(19) . . ? O2D V4 O2C 94.61(16) . . ? O2W V4 O2 172.8(2) . . ? O1K V4 O2 82.97(18) . . ? O1J V4 O2 85.12(18) . . ? O2D V4 O2 80.01(17) . . ? O2C V4 O2 80.29(17) . . ? O2W V4 V5 104.99(18) . . ? O1K V4 V5 37.97(14) . . ? O1J V4 V5 38.81(14) . . ? O2D V4 V5 129.41(15) . . ? O2C V4 V5 128.19(14) . . ? O2 V4 V5 82.15(11) . . ? O3 V5 O1K 105.3(2) . . ? O3 V5 O1J 104.5(2) . . ? O1K V5 O1J 76.98(17) . . ? O3 V5 O1F 94.9(2) . . ? O1K V5 O1F 158.4(2) . . ? O1J V5 O1F 90.9(2) . . ? O3 V5 O1E 94.8(2) . . ? O1K V5 O1E 91.6(2) . . ? O1J V5 O1E 159.6(2) . . ? O1F V5 O1E 94.18(19) . . ? O3 V5 O1P 168.9(2) . . ? O1K V5 O1P 84.5(2) . . ? O1J V5 O1P 82.4(2) . . ? O1F V5 O1P 76.2(2) . . ? O1E V5 O1P 79.6(2) . . ? O3 V5 V4 108.92(15) . . ? O1K V5 V4 38.44(14) . . ? O1J V5 V4 38.55(13) . . ? O1F V5 V4 127.29(17) . . ? O1E V5 V4 128.12(17) . . ? O1P V5 V4 81.90(16) . . ? O3W V6 O1L 102.4(2) . . ? O3W V6 O1M 100.5(2) . . ? O1L V6 O1M 75.71(18) . . ? O3W V6 O2E 92.9(2) . . ? O1L V6 O2E 161.9(2) . . ? O1M V6 O2E 92.1(2) . . ? O3W V6 O2F 94.7(2) . . ? O1L V6 O2F 93.4(2) . . ? O1M V6 O2F 162.8(2) . . ? O2E V6 O2F 95.0(2) . . ? O3W V6 O3 170.6(2) . . ? O1L V6 O3 85.92(19) . . ? O1M V6 O3 85.72(19) . . ? O2E V6 O3 79.8(2) . . ? O2F V6 O3 80.2(2) . . ? O3W V6 V1 106.75(19) . . ? O1L V6 V1 37.90(13) . . ? O1M V6 V1 37.92(14) . . ? O2E V6 V1 128.05(15) . . ? O2F V6 V1 129.24(15) . . ? O3 V6 V1 82.51(11) . . ? C1A O1A V1 127.6(5) . . ? C1A O2A V2 139.4(5) . . ? C1B O1B V1 127.7(5) . . ? C1B O2B V2 142.6(5) . . ? C1C O1C V3 129.5(4) . . ? C1C O2C V4 140.8(4) . . ? C1D O2D V4 142.0(5) . . ? C1D O1D V3 130.2(5) . . ? C1E O1E V5 125.7(5) . . ? C1E O2E V6 143.5(5) . . ? C1F O1F V5 131.8(6) . . ? C1F O2F V6 139.4(6) . . ? C1G O1G V3 127.8(5) . . ? C1G O1G V2 127.7(5) . . ? V3 O1G V2 104.2(2) . . ? C1I O1I V2 128.8(5) . . ? C1I O1I V3 129.1(5) . . ? V2 O1I V3 101.86(19) . . ? C1J O1J V4 131.0(5) . . ? C1J O1J V5 126.2(5) . . ? V4 O1J V5 102.64(19) . . ? C1K O1K V5 122.7(6) . . ? C1K O1K V4 130.3(6) . . ? V5 O1K V4 103.6(2) . . ? C1L O1L V6 127.6(5) . . ? C1L O1L V1 128.2(5) . . ? V6 O1L V1 104.2(2) . . ? C1M O1M V1 128.7(5) . . ? C1M O1M V6 127.2(5) . . ? V1 O1M V6 104.1(2) . . ? C1N O1N V1 126.6(6) . . ? C1O O1O V3 130.3(4) . . ? C1P O1P V5 137.8(15) . . ? V1 O1 V2 131.1(2) . . ? V3 O2 V4 132.2(2) . . ? V5 O3 V6 129.9(2) . . ? O2A C1A O1A 128.4(7) . . ? O2A C1A C2A 116.7(8) . . ? O1A C1A C2A 114.9(8) . . ? C3A C2A C7A 117.1(8) . . ? C3A C2A C1A 122.3(8) . . ? C7A C2A C1A 120.4(8) . . ? C2A C3A C4A 122.5(9) . . ? C2A C3A H3A 118.7 . . ? C4A C3A H3A 118.7 . . ? C5A C4A C3A 120.0(9) . . ? C5A C4A H4A 120.0 . . ? C3A C4A H4A 120.0 . . ? C4A C5A C6A 119.2(8) . . ? C4A C5A H5A 120.4 . . ? C6A C5A H5A 120.4 . . ? C7A C6A C5A 119.3(9) . . ? C7A C6A H6A 120.3 . . ? C5A C6A H6A 120.3 . . ? C6A C7A C2A 121.8(9) . . ? C6A C7A H7A 119.1 . . ? C2A C7A H7A 119.1 . . ? O2B C1B O1B 125.8(7) . . ? O2B C1B C2B 117.2(7) . . ? O1B C1B C2B 116.9(7) . . ? C3B C2B C7B 120.2(7) . . ? C3B C2B C1B 119.5(8) . . ? C7B C2B C1B 120.2(7) . . ? C4B C3B C2B 116.3(9) . . ? C4B C3B H3B 121.8 . . ? C2B C3B H3B 121.8 . . ? C5B C4B C3B 122.5(10) . . ? C5B C4B H4B 118.8 . . ? C3B C4B H4B 118.8 . . ? C4B C5B C6B 122.4(9) . . ? C4B C5B H5B 118.8 . . ? C6B C5B H5B 118.8 . . ? C5B C6B C7B 119.0(9) . . ? C5B C6B H6B 120.5 . . ? C7B C6B H6B 120.5 . . ? C6B C7B C2B 119.5(8) . . ? C6B C7B H7B 120.2 . . ? C2B C7B H7B 120.2 . . ? O2C C1C O1C 126.3(6) . . ? O2C C1C C2C 118.5(7) . . ? O1C C1C C2C 115.2(6) . . ? C3C C2C C7C 120.4(7) . . ? C3C C2C C1C 121.3(7) . . ? C7C C2C C1C 118.3(7) . . ? C4C C3C C2C 120.9(7) . . ? C4C C3C H3C 119.6 . . ? C2C C3C H3C 119.6 . . ? C3C C4C C5C 120.1(8) . . ? C3C C4C H4C 119.9 . . ? C5C C4C H4C 119.9 . . ? C4C C5C C6C 119.2(7) . . ? C4C C5C H5C 120.4 . . ? C6C C5C H5C 120.4 . . ? C7C C6C C5C 120.6(8) . . ? C7C C6C H6C 119.7 . . ? C5C C6C H6C 119.7 . . ? C6C C7C C2C 118.8(8) . . ? C6C C7C H7C 120.6 . . ? C2C C7C H7C 120.6 . . ? O2D C1D O1D 124.9(7) . . ? O2D C1D C2D 118.6(7) . . ? O1D C1D C2D 116.3(7) . . ? C3D C2D C7D 120.0(6) . . ? C3D C2D C1D 121.6(7) . . ? C7D C2D C1D 118.4(7) . . ? C4D C3D C2D 119.6(7) . . ? C4D C3D H3D 120.2 . . ? C2D C3D H3D 120.2 . . ? C3D C4D C5D 120.0(7) . . ? C3D C4D H4D 120.0 . . ? C5D C4D H4D 120.0 . . ? C6D C5D C4D 120.4(7) . . ? C6D C5D H5D 119.8 . . ? C4D C5D H5D 119.8 . . ? C5D C6D C7D 119.4(7) . . ? C5D C6D H6D 120.3 . . ? C7D C6D H6D 120.3 . . ? C6D C7D C2D 120.5(7) . . ? C6D C7D H7D 119.8 . . ? C2D C7D H7D 119.8 . . ? O2E C1E O1E 127.0(8) . . ? O2E C1E C2E 117.4(8) . . ? O1E C1E C2E 115.6(8) . . ? C3E C2E C7E 121.5(8) . . ? C3E C2E C1E 120.6(8) . . ? C7E C2E C1E 117.8(8) . . ? C2E C3E C4E 119.3(8) . . ? C2E C3E H3E 120.4 . . ? C4E C3E H3E 120.4 . . ? C5E C4E C3E 118.3(9) . . ? C5E C4E H4E 120.9 . . ? C3E C4E H4E 120.9 . . ? C4E C5E C6E 119.6(8) . . ? C4E C5E H5E 120.2 . . ? C6E C5E H5E 120.2 . . ? C7E C6E C5E 121.3(10) . . ? C7E C6E H6E 119.4 . . ? C5E C6E H6E 119.4 . . ? C6E C7E C2E 120.0(9) . . ? C6E C7E H7E 120.0 . . ? C2E C7E H7E 120.0 . . ? O2F C1F O1F 125.0(8) . . ? O2F C1F C2F 119.8(9) . . ? O1F C1F C2F 115.1(9) . . ? C3F C2F C7F 120.0 . . ? C3F C2F C1F 119.8(6) . . ? C7F C2F C1F 119.6(6) . . ? C4F C3F C2F 120.0 . . ? C4F C3F H3F 120.0 . . ? C2F C3F H3F 120.0 . . ? C3F C4F C5F 120.0 . . ? C3F C4F H4F 120.0 . . ? C5F C4F H4F 120.0 . . ? C6F C5F C4F 120.0 . . ? C6F C5F H5F 120.0 . . ? C4F C5F H5F 120.0 . . ? C5F C6F C7F 120.0 . . ? C5F C6F H6F 120.0 . . ? C7F C6F H6F 120.0 . . ? C6F C7F C2F 120.0 . . ? C6F C7F H7F 120.0 . . ? C2F C7F H7F 120.0 . . ? O1G C1G C2G 113.0(7) . . ? O1G C1G H1G1 109.0 . . ? C2G C1G H1G1 109.0 . . ? O1G C1G H1G2 109.0 . . ? C2G C1G H1G2 109.0 . . ? H1G1 C1G H1G2 107.8 . . ? C1G C2G C3G 109.1(9) . . ? C1G C2G H2G1 109.9 . . ? C3G C2G H2G1 109.9 . . ? C1G C2G H2G2 109.9 . . ? C3G C2G H2G2 109.9 . . ? H2G1 C2G H2G2 108.3 . . ? C2G C3G H3G1 109.5 . . ? C2G C3G H3G2 109.5 . . ? H3G1 C3G H3G2 109.5 . . ? C2G C3G H3G3 109.5 . . ? H3G1 C3G H3G3 109.5 . . ? H3G2 C3G H3G3 109.5 . . ? O1I C1I C2I 114.4(9) . . ? O1I C1I H1I1 108.7 . . ? C2I C1I H1I1 108.7 . . ? O1I C1I H1I2 108.7 . . ? C2I C1I H1I2 108.7 . . ? H1I1 C1I H1I2 107.6 . . ? C1I C2I C3I 110.4(10) . . ? C1I C2I H2I1 109.6 . . ? C3I C2I H2I1 109.6 . . ? C1I C2I H2I2 109.6 . . ? C3I C2I H2I2 109.6 . . ? H2I1 C2I H2I2 108.1 . . ? C2I C3I H3I1 109.5 . . ? C2I C3I H3I2 109.5 . . ? H3I1 C3I H3I2 109.5 . . ? C2I C3I H3I3 109.5 . . ? H3I1 C3I H3I3 109.5 . . ? H3I2 C3I H3I3 109.5 . . ? O1J C1J C2J 110.8(8) . . ? O1J C1J H1J1 109.5 . . ? C2J C1J H1J1 109.5 . . ? O1J C1J H1J2 109.5 . . ? C2J C1J H1J2 109.5 . . ? H1J1 C1J H1J2 108.1 . . ? C1J C2J C3J 114.6(11) . . ? C1J C2J H2J1 108.6 . . ? C3J C2J H2J1 108.6 . . ? C1J C2J H2J2 108.6 . . ? C3J C2J H2J2 108.6 . . ? H2J1 C2J H2J2 107.6 . . ? C2J C3J H3J1 109.5 . . ? C2J C3J H3J2 109.5 . . ? H3J1 C3J H3J2 109.5 . . ? C2J C3J H3J3 109.5 . . ? H3J1 C3J H3J3 109.5 . . ? H3J2 C3J H3J3 109.5 . . ? C2K C1K O1K 99.9(16) . . ? C2K C1K H1K1 111.8 . . ? O1K C1K H1K1 111.8 . . ? C2K C1K H1K2 111.8 . . ? O1K C1K H1K2 111.8 . . ? H1K1 C1K H1K2 109.5 . . ? C1K C2K C3K 97.7(14) . . ? C1K C2K H2K1 112.2 . . ? C3K C2K H2K1 112.2 . . ? C1K C2K H2K2 112.2 . . ? C3K C2K H2K2 112.2 . . ? H2K1 C2K H2K2 109.8 . . ? C2K C3K H3K1 109.5 . . ? C2K C3K H3K2 109.5 . . ? H3K1 C3K H3K2 109.5 . . ? C2K C3K H3K3 109.5 . . ? H3K1 C3K H3K3 109.5 . . ? H3K2 C3K H3K3 109.5 . . ? O1L C1L C2L 112.3(7) . . ? O1L C1L H1L1 109.2 . . ? C2L C1L H1L1 109.2 . . ? O1L C1L H1L2 109.2 . . ? C2L C1L H1L2 109.2 . . ? H1L1 C1L H1L2 107.9 . . ? C1L C2L C3L 110.1(9) . . ? C1L C2L H2L1 109.6 . . ? C3L C2L H2L1 109.6 . . ? C1L C2L H2L2 109.6 . . ? C3L C2L H2L2 109.6 . . ? H2L1 C2L H2L2 108.1 . . ? C2L C3L H3L1 109.5 . . ? C2L C3L H3L2 109.5 . . ? H3L1 C3L H3L2 109.5 . . ? C2L C3L H3L3 109.5 . . ? H3L1 C3L H3L3 109.5 . . ? H3L2 C3L H3L3 109.5 . . ? C2M C1M O1M 110.5(13) . . ? C2M C1M H1M1 109.6 . . ? O1M C1M H1M1 109.6 . . ? C2M C1M H1M2 109.6 . . ? O1M C1M H1M2 109.6 . . ? H1M1 C1M H1M2 108.1 . . ? C1M C2M C3M 92.0(12) . . ? C1M C2M H2M1 113.3 . . ? C3M C2M H2M1 113.3 . . ? C1M C2M H2M2 113.3 . . ? C3M C2M H2M2 113.3 . . ? H2M1 C2M H2M2 110.6 . . ? C2M C3M H3M1 109.5 . . ? C2M C3M H3M2 109.5 . . ? H3M1 C3M H3M2 109.5 . . ? C2M C3M H3M3 109.5 . . ? H3M1 C3M H3M3 109.5 . . ? H3M2 C3M H3M3 109.5 . . ? C2N C1N O1N 113.3(14) . . ? C2N C1N H1N1 108.9 . . ? O1N C1N H1N1 108.9 . . ? C2N C1N H1N2 108.9 . . ? O1N C1N H1N2 108.9 . . ? H1N1 C1N H1N2 107.7 . . ? C1N C2N C3N 104.6(14) . . ? C1N C2N H2N1 110.8 . . ? C3N C2N H2N1 110.8 . . ? C1N C2N H2N2 110.8 . . ? C3N C2N H2N2 110.8 . . ? H2N1 C2N H2N2 108.9 . . ? C2N C3N H3N1 109.5 . . ? C2N C3N H3N2 109.5 . . ? H3N1 C3N H3N2 109.5 . . ? C2N C3N H3N3 109.5 . . ? H3N1 C3N H3N3 109.5 . . ? H3N2 C3N H3N3 109.5 . . ? C2O C1O O1O 111.8(8) . . ? C2O C1O H1O1 109.3 . . ? O1O C1O H1O1 109.3 . . ? C2O C1O H1O2 109.3 . . ? O1O C1O H1O2 109.3 . . ? H1O1 C1O H1O2 107.9 . . ? C1O C2O C3O 106.3(8) . . ? C1O C2O H2O1 110.5 . . ? C3O C2O H2O1 110.5 . . ? C1O C2O H2O2 110.5 . . ? C3O C2O H2O2 110.5 . . ? H2O1 C2O H2O2 108.7 . . ? C2O C3O H3O1 109.5 . . ? C2O C3O H3O2 109.5 . . ? H3O1 C3O H3O2 109.5 . . ? C2O C3O H3O3 109.5 . . ? H3O1 C3O H3O3 109.5 . . ? H3O2 C3O H3O3 109.5 . . ? O1P C1P C2P 137(3) . . ? O1P C1P H1P1 103.0 . . ? C2P C1P H1P1 103.0 . . ? O1P C1P H1P2 103.0 . . ? C2P C1P H1P2 103.0 . . ? H1P1 C1P H1P2 105.1 . . ? C1P C2P C3P 97.3(16) . . ? C1P C2P H2P1 112.3 . . ? C3P C2P H2P1 112.3 . . ? C1P C2P H2P2 112.3 . . ? C3P C2P H2P2 112.3 . . ? H2P1 C2P H2P2 109.9 . . ? C2P C3P H3P1 109.5 . . ? C2P C3P H3P2 109.5 . . ? H3P1 C3P H3P2 109.5 . . ? C2P C3P H3P3 109.5 . . ? H3P1 C3P H3P3 109.5 . . ? H3P2 C3P H3P3 109.5 . . ? C2S C1S O1S 131(3) . . ? C2S C1S H1S1 104.6 . . ? O1S C1S H1S1 104.6 . . ? C2S C1S H1S2 104.6 . . ? O1S C1S H1S2 104.6 . . ? H1S1 C1S H1S2 105.7 . . ? C1S C2S C3S 118(3) . . ? C1S C2S H2S1 107.8 . . ? C3S C2S H2S1 107.8 . . ? C1S C2S H2S2 107.8 . . ? C3S C2S H2S2 107.8 . . ? H2S1 C2S H2S2 107.2 . . ? C2S C3S H3S1 109.5 . . ? C2S C3S H3S2 109.5 . . ? H3S1 C3S H3S2 109.5 . . ? C2S C3S H3S3 109.5 . . ? H3S1 C3S H3S3 109.5 . . ? H3S2 C3S H3S3 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 O1W V2 V3 O2 177.1(3) . . . . ? O1G V2 V3 O2 -90.3(3) . . . . ? O1I V2 V3 O2 88.9(3) . . . . ? O2B V2 V3 O2 -75.6(3) . . . . ? O2A V2 V3 O2 69.8(3) . . . . ? O1 V2 V3 O2 -3.0(2) . . . . ? O1W V2 V3 O1G -92.6(3) . . . . ? O1I V2 V3 O1G 179.1(3) . . . . ? O2B V2 V3 O1G 14.6(3) . . . . ? O2A V2 V3 O1G 160.0(3) . . . . ? O1 V2 V3 O1G 87.3(2) . . . . ? O1W V2 V3 O1I 88.3(3) . . . . ? O1G V2 V3 O1I -179.1(3) . . . . ? O2B V2 V3 O1I -164.5(3) . . . . ? O2A V2 V3 O1I -19.1(3) . . . . ? O1 V2 V3 O1I -91.9(2) . . . . ? O1W V2 V3 O1D 65.7(3) . . . . ? O1G V2 V3 O1D 158.3(3) . . . . ? O1I V2 V3 O1D -22.6(3) . . . . ? O2B V2 V3 O1D 173.0(3) . . . . ? O2A V2 V3 O1D -41.7(3) . . . . ? O1 V2 V3 O1D -114.4(2) . . . . ? O1W V2 V3 O1C -71.9(3) . . . . ? O1G V2 V3 O1C 20.7(3) . . . . ? O1I V2 V3 O1C -160.2(3) . . . . ? O2B V2 V3 O1C 35.3(3) . . . . ? O2A V2 V3 O1C -179.3(3) . . . . ? O1 V2 V3 O1C 107.9(2) . . . . ? O1W V2 V3 O1O -2.7(2) . . . . ? O1G V2 V3 O1O 89.9(2) . . . . ? O1I V2 V3 O1O -91.0(2) . . . . ? O2B V2 V3 O1O 104.6(2) . . . . ? O2A V2 V3 O1O -110.0(2) . . . . ? O1 V2 V3 O1O 177.18(18) . . . . ? O2W V4 V5 O3 -176.7(3) . . . . ? O1K V4 V5 O3 91.0(3) . . . . ? O1J V4 V5 O3 -89.6(3) . . . . ? O2D V4 V5 O3 72.5(3) . . . . ? O2C V4 V5 O3 -68.7(3) . . . . ? O2 V4 V5 O3 2.4(2) . . . . ? O2W V4 V5 O1K 92.3(3) . . . . ? O1J V4 V5 O1K 179.4(3) . . . . ? O2D V4 V5 O1K -18.5(3) . . . . ? O2C V4 V5 O1K -159.7(3) . . . . ? O2 V4 V5 O1K -88.6(3) . . . . ? O2W V4 V5 O1J -87.1(3) . . . . ? O1K V4 V5 O1J -179.4(3) . . . . ? O2D V4 V5 O1J 162.1(3) . . . . ? O2C V4 V5 O1J 21.0(3) . . . . ? O2 V4 V5 O1J 92.0(3) . . . . ? O2W V4 V5 O1F -64.8(3) . . . . ? O1K V4 V5 O1F -157.1(3) . . . . ? O1J V4 V5 O1F 22.3(3) . . . . ? O2D V4 V5 O1F -175.6(3) . . . . ? O2C V4 V5 O1F 43.3(3) . . . . ? O2 V4 V5 O1F 114.3(2) . . . . ? O2W V4 V5 O1E 70.8(3) . . . . ? O1K V4 V5 O1E -21.5(3) . . . . ? O1J V4 V5 O1E 157.9(3) . . . . ? O2D V4 V5 O1E -40.0(3) . . . . ? O2C V4 V5 O1E 178.8(3) . . . . ? O2 V4 V5 O1E -110.1(2) . . . . ? O2W V4 V5 O1P 0.9(2) . . . . ? O1K V4 V5 O1P -91.4(3) . . . . ? O1J V4 V5 O1P 88.0(3) . . . . ? O2D V4 V5 O1P -109.9(2) . . . . ? O2C V4 V5 O1P 109.0(2) . . . . ? O2 V4 V5 O1P 180.0(2) . . . . ? O1 V1 V6 O3W -179.3(3) . . . . ? O1L V1 V6 O3W -88.7(3) . . . . ? O1M V1 V6 O3W 85.6(3) . . . . ? O1B V1 V6 O3W -68.0(3) . . . . ? O1A V1 V6 O3W 71.7(3) . . . . ? O1N V1 V6 O3W 2.3(3) . . . . ? O1 V1 V6 O1L -90.5(3) . . . . ? O1M V1 V6 O1L 174.3(3) . . . . ? O1B V1 V6 O1L 20.7(3) . . . . ? O1A V1 V6 O1L 160.4(3) . . . . ? O1N V1 V6 O1L 91.0(3) . . . . ? O1 V1 V6 O1M 95.1(3) . . . . ? O1L V1 V6 O1M -174.3(3) . . . . ? O1B V1 V6 O1M -153.6(3) . . . . ? O1A V1 V6 O1M -13.9(3) . . . . ? O1N V1 V6 O1M -83.3(3) . . . . ? O1 V1 V6 O2E 73.2(3) . . . . ? O1L V1 V6 O2E 163.7(3) . . . . ? O1M V1 V6 O2E -21.9(3) . . . . ? O1B V1 V6 O2E -175.5(3) . . . . ? O1A V1 V6 O2E -35.9(3) . . . . ? O1N V1 V6 O2E -105.3(3) . . . . ? O1 V1 V6 O2F -68.4(3) . . . . ? O1L V1 V6 O2F 22.1(3) . . . . ? O1M V1 V6 O2F -163.5(3) . . . . ? O1B V1 V6 O2F 42.9(3) . . . . ? O1A V1 V6 O2F -177.5(3) . . . . ? O1N V1 V6 O2F 113.2(3) . . . . ? O1 V1 V6 O3 2.4(2) . . . . ? O1L V1 V6 O3 93.0(3) . . . . ? O1M V1 V6 O3 -92.7(3) . . . . ? O1B V1 V6 O3 113.7(2) . . . . ? O1A V1 V6 O3 -106.6(2) . . . . ? O1N V1 V6 O3 -176.0(2) . . . . ? O1 V1 O1A C1A 10.1(6) . . . . ? O1L V1 O1A C1A 164.9(6) . . . . ? O1M V1 O1A C1A 116.1(6) . . . . ? O1B V1 O1A C1A -85.8(6) . . . . ? O1N V1 O1A C1A -162.4(6) . . . . ? V6 V1 O1A C1A 124.7(5) . . . . ? O1W V2 O2A C1A 153.0(8) . . . . ? O1G V2 O2A C1A -55.1(11) . . . . ? O1I V2 O2A C1A -105.9(8) . . . . ? O2B V2 O2A C1A 60.0(8) . . . . ? O1 V2 O2A C1A -19.1(8) . . . . ? V3 V2 O2A C1A -94.0(8) . . . . ? O1 V1 O1B C1B -9.7(6) . . . . ? O1L V1 O1B C1B -113.1(6) . . . . ? O1M V1 O1B C1B -171.0(6) . . . . ? O1A V1 O1B C1B 84.4(6) . . . . ? O1N V1 O1B C1B 160.6(6) . . . . ? V6 V1 O1B C1B -125.7(6) . . . . ? O1W V2 O2B C1B -161.4(8) . . . . ? O1G V2 O2B C1B 94.6(8) . . . . ? O1I V2 O2B C1B 46.7(13) . . . . ? O2A V2 O2B C1B -67.8(8) . . . . ? O1 V2 O2B C1B 11.1(8) . . . . ? V3 V2 O2B C1B 85.7(8) . . . . ? O2 V3 O1C C1C -16.8(6) . . . . ? O1G V3 O1C C1C -121.7(6) . . . . ? O1I V3 O1C C1C -176.7(6) . . . . ? O1D V3 O1C C1C 77.4(6) . . . . ? O1O V3 O1C C1C 155.3(6) . . . . ? V2 V3 O1C C1C -134.2(5) . . . . ? O2W V4 O2C C1C -158.3(7) . . . . ? O1K V4 O2C C1C 49.6(10) . . . . ? O1J V4 O2C C1C 101.7(7) . . . . ? O2D V4 O2C C1C -62.2(7) . . . . ? O2 V4 O2C C1C 16.8(7) . . . . ? V5 V4 O2C C1C 88.7(7) . . . . ? O2W V4 O2D C1D 155.0(8) . . . . ? O1K V4 O2D C1D -101.5(8) . . . . ? O1J V4 O2D C1D -49.5(12) . . . . ? O2C V4 O2D C1D 60.1(8) . . . . ? O2 V4 O2D C1D -19.1(8) . . . . ? V5 V4 O2D C1D -90.2(8) . . . . ? O2 V3 O1D C1D 7.8(6) . . . . ? O1G V3 O1D C1D 167.6(6) . . . . ? O1I V3 O1D C1D 111.5(6) . . . . ? O1C V3 O1D C1D -86.1(6) . . . . ? O1O V3 O1D C1D -164.6(6) . . . . ? V2 V3 O1D C1D 125.5(5) . . . . ? O3 V5 O1E C1E 19.3(6) . . . . ? O1K V5 O1E C1E 124.8(6) . . . . ? O1J V5 O1E C1E -179.8(6) . . . . ? O1F V5 O1E C1E -75.9(6) . . . . ? O1P V5 O1E C1E -151.0(6) . . . . ? V4 V5 O1E C1E 138.0(5) . . . . ? O3W V6 O2E C1E 168.0(9) . . . . ? O1L V6 O2E C1E -44.4(13) . . . . ? O1M V6 O2E C1E -91.4(9) . . . . ? O2F V6 O2E C1E 73.0(9) . . . . ? O3 V6 O2E C1E -6.1(9) . . . . ? V1 V6 O2E C1E -78.1(9) . . . . ? O3 V5 O1F C1F -5.8(7) . . . . ? O1K V5 O1F C1F -165.4(6) . . . . ? O1J V5 O1F C1F -110.4(7) . . . . ? O1E V5 O1F C1F 89.4(7) . . . . ? O1P V5 O1F C1F 167.6(7) . . . . ? V4 V5 O1F C1F -124.1(6) . . . . ? O3W V6 O2F C1F -143.8(8) . . . . ? O1L V6 O2F C1F 113.5(8) . . . . ? O1M V6 O2F C1F 63.9(12) . . . . ? O2E V6 O2F C1F -50.5(8) . . . . ? O3 V6 O2F C1F 28.2(8) . . . . ? V1 V6 O2F C1F 100.1(8) . . . . ? O2 V3 O1G C1G -84.6(6) . . . . ? O1I V3 O1G C1G 174.6(6) . . . . ? O1D V3 O1G C1G 116.3(7) . . . . ? O1C V3 O1G C1G 10.0(6) . . . . ? O1O V3 O1G C1G 88.9(6) . . . . ? V2 V3 O1G C1G 174.0(7) . . . . ? O2 V3 O1G V2 101.4(2) . . . . ? O1I V3 O1G V2 0.57(17) . . . . ? O1D V3 O1G V2 -57.8(6) . . . . ? O1C V3 O1G V2 -164.0(2) . . . . ? O1O V3 O1G V2 -85.1(2) . . . . ? O1W V2 O1G C1G -76.3(6) . . . . ? O1I V2 O1G C1G -174.6(6) . . . . ? O2B V2 O1G C1G 17.2(6) . . . . ? O2A V2 O1G C1G 132.7(7) . . . . ? O1 V2 O1G C1G 97.1(6) . . . . ? V3 V2 O1G C1G -174.0(7) . . . . ? O1W V2 O1G V3 97.7(3) . . . . ? O1I V2 O1G V3 -0.57(17) . . . . ? O2B V2 O1G V3 -168.8(2) . . . . ? O2A V2 O1G V3 -53.3(7) . . . . ? O1 V2 O1G V3 -88.9(2) . . . . ? O1W V2 O1I C1I 73.5(7) . . . . ? O1G V2 O1I C1I 175.4(7) . . . . ? O2B V2 O1I C1I -135.0(9) . . . . ? O2A V2 O1I C1I -20.0(7) . . . . ? O1 V2 O1I C1I -100.0(7) . . . . ? V3 V2 O1I C1I 174.8(8) . . . . ? O1W V2 O1I V3 -101.3(2) . . . . ? O1G V2 O1I V3 0.56(17) . . . . ? O2B V2 O1I V3 50.2(8) . . . . ? O2A V2 O1I V3 165.2(2) . . . . ? O1 V2 O1I V3 85.2(2) . . . . ? O2 V3 O1I C1I 82.5(7) . . . . ? O1G V3 O1I C1I -175.3(8) . . . . ? O1D V3 O1I C1I -12.1(7) . . . . ? O1C V3 O1I C1I -118.2(8) . . . . ? O1O V3 O1I C1I -90.6(7) . . . . ? V2 V3 O1I C1I -174.8(8) . . . . ? O2 V3 O1I V2 -102.7(2) . . . . ? O1G V3 O1I V2 -0.56(17) . . . . ? O1D V3 O1I V2 162.6(2) . . . . ? O1C V3 O1I V2 56.6(7) . . . . ? O1O V3 O1I V2 84.2(2) . . . . ? O2W V4 O1J C1J -82.8(7) . . . . ? O1K V4 O1J C1J 175.8(7) . . . . ? O2D V4 O1J C1J 121.9(8) . . . . ? O2C V4 O1J C1J 11.8(7) . . . . ? O2 V4 O1J C1J 91.9(7) . . . . ? V5 V4 O1J C1J 175.4(8) . . . . ? O2W V4 O1J V5 101.7(2) . . . . ? O1K V4 O1J V5 0.38(19) . . . . ? O2D V4 O1J V5 -53.6(7) . . . . ? O2C V4 O1J V5 -163.7(2) . . . . ? O2 V4 O1J V5 -83.5(2) . . . . ? O3 V5 O1J C1J -73.4(6) . . . . ? O1K V5 O1J C1J -176.1(7) . . . . ? O1F V5 O1J C1J 21.9(6) . . . . ? O1E V5 O1J C1J 126.3(7) . . . . ? O1P V5 O1J C1J 97.8(6) . . . . ? V4 V5 O1J C1J -175.7(7) . . . . ? O3 V5 O1J V4 102.3(2) . . . . ? O1K V5 O1J V4 -0.39(19) . . . . ? O1F V5 O1J V4 -162.4(2) . . . . ? O1E V5 O1J V4 -58.0(6) . . . . ? O1P V5 O1J V4 -86.5(2) . . . . ? O3 V5 O1K C1K 59.8(9) . . . . ? O1J V5 O1K C1K 161.5(9) . . . . ? O1F V5 O1K C1K -141.4(9) . . . . ? O1E V5 O1K C1K -35.7(8) . . . . ? O1P V5 O1K C1K -115.0(8) . . . . ? V4 V5 O1K C1K 161.1(9) . . . . ? O3 V5 O1K V4 -101.3(2) . . . . ? O1J V5 O1K V4 0.39(19) . . . . ? O1F V5 O1K V4 57.5(6) . . . . ? O1E V5 O1K V4 163.2(2) . . . . ? O1P V5 O1K V4 83.9(2) . . . . ? O2W V4 O1K C1K 103.4(10) . . . . ? O1J V4 O1K C1K -159.4(10) . . . . ? O2D V4 O1K C1K 6.8(10) . . . . ? O2C V4 O1K C1K -105.3(11) . . . . ? O2 V4 O1K C1K -72.8(10) . . . . ? V5 V4 O1K C1K -159.0(11) . . . . ? O2W V4 O1K V5 -97.6(3) . . . . ? O1J V4 O1K V5 -0.39(19) . . . . ? O2D V4 O1K V5 165.8(2) . . . . ? O2C V4 O1K V5 53.7(7) . . . . ? O2 V4 O1K V5 86.2(2) . . . . ? O3W V6 O1L C1L -77.2(6) . . . . ? O1M V6 O1L C1L -175.1(7) . . . . ? O2E V6 O1L C1L 136.0(7) . . . . ? O2F V6 O1L C1L 18.4(6) . . . . ? O3 V6 O1L C1L 98.3(6) . . . . ? V1 V6 O1L C1L -178.6(7) . . . . ? O3W V6 O1L V1 101.4(3) . . . . ? O1M V6 O1L V1 3.6(2) . . . . ? O2E V6 O1L V1 -45.4(8) . . . . ? O2F V6 O1L V1 -163.0(2) . . . . ? O3 V6 O1L V1 -83.0(2) . . . . ? O1 V1 O1L C1L -81.6(6) . . . . ? O1M V1 O1L C1L 175.0(7) . . . . ? O1B V1 O1L C1L 14.7(6) . . . . ? O1A V1 O1L C1L 124.2(7) . . . . ? O1N V1 O1L C1L 92.3(6) . . . . ? V6 V1 O1L C1L 178.6(7) . . . . ? O1 V1 O1L V6 99.8(3) . . . . ? O1M V1 O1L V6 -3.6(2) . . . . ? O1B V1 O1L V6 -163.9(2) . . . . ? O1A V1 O1L V6 -54.4(8) . . . . ? O1N V1 O1L V6 -86.3(2) . . . . ? O1 V1 O1M C1M 86.9(9) . . . . ? O1L V1 O1M C1M -173.3(9) . . . . ? O1B V1 O1M C1M -112.5(9) . . . . ? O1A V1 O1M C1M -7.6(9) . . . . ? O1N V1 O1M C1M -84.5(9) . . . . ? V6 V1 O1M C1M -176.8(10) . . . . ? O1 V1 O1M V6 -96.3(3) . . . . ? O1L V1 O1M V6 3.6(2) . . . . ? O1B V1 O1M V6 64.3(6) . . . . ? O1A V1 O1M V6 169.2(2) . . . . ? O1N V1 O1M V6 92.4(3) . . . . ? O3W V6 O1M C1M 73.1(9) . . . . ? O1L V6 O1M C1M 173.3(9) . . . . ? O2E V6 O1M C1M -20.2(8) . . . . ? O2F V6 O1M C1M -135.0(10) . . . . ? O3 V6 O1M C1M -99.8(8) . . . . ? V1 V6 O1M C1M 176.9(9) . . . . ? O3W V6 O1M V1 -103.8(3) . . . . ? O1L V6 O1M V1 -3.6(2) . . . . ? O2E V6 O1M V1 162.9(3) . . . . ? O2F V6 O1M V1 48.1(9) . . . . ? O3 V6 O1M V1 83.3(2) . . . . ? O1 V1 O1N C1N 16.2(17) . . . . ? O1L V1 O1N C1N -133.3(10) . . . . ? O1M V1 O1N C1N 150.6(10) . . . . ? O1B V1 O1N C1N -40.0(9) . . . . ? O1A V1 O1N C1N 56.7(10) . . . . ? V6 V1 O1N C1N -171.3(10) . . . . ? O2 V3 O1O C1O 15.0(15) . . . . ? O1G V3 O1O C1O -127.7(6) . . . . ? O1I V3 O1O C1O 154.8(6) . . . . ? O1D V3 O1O C1O 61.5(6) . . . . ? O1C V3 O1O C1O -33.8(6) . . . . ? V2 V3 O1O C1O -166.0(6) . . . . ? O3 V5 O1P C1P -100(3) . . . . ? O1K V5 O1P C1P 53(2) . . . . ? O1J V5 O1P C1P 130(2) . . . . ? O1F V5 O1P C1P -137(2) . . . . ? O1E V5 O1P C1P -40(2) . . . . ? V4 V5 O1P C1P 91(2) . . . . ? O1L V1 O1 V2 139.2(3) . . . . ? O1M V1 O1 V2 -142.1(3) . . . . ? O1B V1 O1 V2 45.3(3) . . . . ? O1A V1 O1 V2 -48.8(3) . . . . ? O1N V1 O1 V2 -9.5(14) . . . . ? V6 V1 O1 V2 178.3(2) . . . . ? O1W V2 O1 V1 1.7(15) . . . . ? O1G V2 O1 V1 -139.5(4) . . . . ? O1I V2 O1 V1 143.4(3) . . . . ? O2B V2 O1 V1 -45.5(3) . . . . ? O2A V2 O1 V1 51.9(3) . . . . ? V3 V2 O1 V1 -177.4(3) . . . . ? O1G V3 O2 V4 142.6(3) . . . . ? O1I V3 O2 V4 -137.5(3) . . . . ? O1D V3 O2 V4 -44.3(3) . . . . ? O1C V3 O2 V4 48.9(3) . . . . ? O1O V3 O2 V4 1.1(14) . . . . ? V2 V3 O2 V4 -177.8(2) . . . . ? O2W V4 O2 V3 -6.9(19) . . . . ? O1K V4 O2 V3 141.9(4) . . . . ? O1J V4 O2 V3 -140.8(3) . . . . ? O2D V4 O2 V3 47.8(3) . . . . ? O2C V4 O2 V3 -48.7(3) . . . . ? V5 V4 O2 V3 -179.8(3) . . . . ? O1K V5 O3 V6 -143.9(3) . . . . ? O1J V5 O3 V6 135.9(3) . . . . ? O1F V5 O3 V6 43.7(4) . . . . ? O1E V5 O3 V6 -50.9(3) . . . . ? O1P V5 O3 V6 8.2(15) . . . . ? V4 V5 O3 V6 175.9(2) . . . . ? O3W V6 O3 V5 7.6(16) . . . . ? O1L V6 O3 V5 -144.6(4) . . . . ? O1M V6 O3 V5 139.5(4) . . . . ? O2E V6 O3 V5 46.5(3) . . . . ? O2F V6 O3 V5 -50.4(3) . . . . ? V1 V6 O3 V5 177.5(3) . . . . ? V2 O2A C1A O1A -6.5(13) . . . . ? V2 O2A C1A C2A 173.0(5) . . . . ? V1 O1A C1A O2A 16.4(11) . . . . ? V1 O1A C1A C2A -163.0(5) . . . . ? O2A C1A C2A C3A -173.6(8) . . . . ? O1A C1A C2A C3A 5.9(11) . . . . ? O2A C1A C2A C7A 1.2(11) . . . . ? O1A C1A C2A C7A -179.3(7) . . . . ? C7A C2A C3A C4A 1.5(13) . . . . ? C1A C2A C3A C4A 176.5(8) . . . . ? C2A C3A C4A C5A 0.8(14) . . . . ? C3A C4A C5A C6A -2.8(14) . . . . ? C4A C5A C6A C7A 2.5(13) . . . . ? C5A C6A C7A C2A -0.1(13) . . . . ? C3A C2A C7A C6A -1.8(12) . . . . ? C1A C2A C7A C6A -176.9(7) . . . . ? V2 O2B C1B O1B 14.7(13) . . . . ? V2 O2B C1B C2B -169.4(6) . . . . ? V1 O1B C1B O2B -18.4(11) . . . . ? V1 O1B C1B C2B 165.7(5) . . . . ? O2B C1B C2B C3B -177.5(8) . . . . ? O1B C1B C2B C3B -1.3(11) . . . . ? O2B C1B C2B C7B 3.9(11) . . . . ? O1B C1B C2B C7B -179.8(7) . . . . ? C7B C2B C3B C4B -1.9(14) . . . . ? C1B C2B C3B C4B 179.6(9) . . . . ? C2B C3B C4B C5B 3.8(17) . . . . ? C3B C4B C5B C6B -3(2) . . . . ? C4B C5B C6B C7B 0.3(17) . . . . ? C5B C6B C7B C2B 1.5(14) . . . . ? C3B C2B C7B C6B -0.6(13) . . . . ? C1B C2B C7B C6B 177.9(8) . . . . ? V4 O2C C1C O1C 2.1(12) . . . . ? V4 O2C C1C C2C -178.3(4) . . . . ? V3 O1C C1C O2C -6.1(11) . . . . ? V3 O1C C1C C2C 174.3(4) . . . . ? O2C C1C C2C C3C -177.2(7) . . . . ? O1C C1C C2C C3C 2.4(10) . . . . ? O2C C1C C2C C7C 0.7(10) . . . . ? O1C C1C C2C C7C -179.7(6) . . . . ? C7C C2C C3C C4C -0.6(11) . . . . ? C1C C2C C3C C4C 177.3(7) . . . . ? C2C C3C C4C C5C -1.3(12) . . . . ? C3C C4C C5C C6C 3.1(13) . . . . ? C4C C5C C6C C7C -2.9(13) . . . . ? C5C C6C C7C C2C 0.9(12) . . . . ? C3C C2C C7C C6C 0.8(11) . . . . ? C1C C2C C7C C6C -177.2(7) . . . . ? V4 O2D C1D O1D -4.1(13) . . . . ? V4 O2D C1D C2D -179.6(5) . . . . ? V3 O1D C1D O2D 15.4(10) . . . . ? V3 O1D C1D C2D -169.0(4) . . . . ? O2D C1D C2D C3D 174.3(7) . . . . ? O1D C1D C2D C3D -1.6(10) . . . . ? O2D C1D C2D C7D -5.7(10) . . . . ? O1D C1D C2D C7D 178.4(6) . . . . ? C7D C2D C3D C4D 2.4(11) . . . . ? C1D C2D C3D C4D -177.6(6) . . . . ? C2D C3D C4D C5D -2.5(11) . . . . ? C3D C4D C5D C6D -0.1(12) . . . . ? C4D C5D C6D C7D 2.8(11) . . . . ? C5D C6D C7D C2D -2.9(11) . . . . ? C3D C2D C7D C6D 0.3(11) . . . . ? C1D C2D C7D C6D -179.7(6) . . . . ? V6 O2E C1E O1E -17.2(15) . . . . ? V6 O2E C1E C2E 164.0(6) . . . . ? V5 O1E C1E O2E 11.2(11) . . . . ? V5 O1E C1E C2E -170.0(5) . . . . ? O2E C1E C2E C3E -178.6(8) . . . . ? O1E C1E C2E C3E 2.5(11) . . . . ? O2E C1E C2E C7E 1.2(12) . . . . ? O1E C1E C2E C7E -177.7(8) . . . . ? C7E C2E C3E C4E -1.9(13) . . . . ? C1E C2E C3E C4E 177.9(7) . . . . ? C2E C3E C4E C5E 2.6(13) . . . . ? C3E C4E C5E C6E -2.3(15) . . . . ? C4E C5E C6E C7E 1.5(17) . . . . ? C5E C6E C7E C2E -0.8(17) . . . . ? C3E C2E C7E C6E 1.0(15) . . . . ? C1E C2E C7E C6E -178.8(9) . . . . ? V6 O2F C1F O1F -5.3(13) . . . . ? V6 O2F C1F C2F 171.5(5) . . . . ? V5 O1F C1F O2F -14.4(12) . . . . ? V5 O1F C1F C2F 168.7(5) . . . . ? O2F C1F C2F C3F -5.9(10) . . . . ? O1F C1F C2F C3F 171.3(6) . . . . ? O2F C1F C2F C7F -176.7(6) . . . . ? O1F C1F C2F C7F 0.5(9) . . . . ? C7F C2F C3F C4F 0.0 . . . . ? C1F C2F C3F C4F -170.8(7) . . . . ? C2F C3F C4F C5F 0.0 . . . . ? C3F C4F C5F C6F 0.0 . . . . ? C4F C5F C6F C7F 0.0 . . . . ? C5F C6F C7F C2F 0.0 . . . . ? C3F C2F C7F C6F 0.0 . . . . ? C1F C2F C7F C6F 170.8(7) . . . . ? V3 O1G C1G C2G -95.2(8) . . . . ? V2 O1G C1G C2G 77.4(9) . . . . ? O1G C1G C2G C3G 178.5(8) . . . . ? V2 O1I C1I C2I -77.5(10) . . . . ? V3 O1I C1I C2I 95.9(9) . . . . ? O1I C1I C2I C3I -176.3(8) . . . . ? V4 O1J C1J C2J -96.4(10) . . . . ? V5 O1J C1J C2J 78.1(10) . . . . ? O1J C1J C2J C3J 179.6(11) . . . . ? V5 O1K C1K C2K 117.7(12) . . . . ? V4 O1K C1K C2K -86.7(14) . . . . ? O1K C1K C2K C3K 172.9(14) . . . . ? V6 O1L C1L C2L 73.9(9) . . . . ? V1 O1L C1L C2L -104.4(8) . . . . ? O1L C1L C2L C3L -179.9(8) . . . . ? V1 O1M C1M C2M -88.3(13) . . . . ? V6 O1M C1M C2M 95.6(13) . . . . ? O1M C1M C2M C3M -179.0(12) . . . . ? V1 O1N C1N C2N -118.9(13) . . . . ? O1N C1N C2N C3N -171.9(14) . . . . ? V3 O1O C1O C2O -107.7(8) . . . . ? O1O C1O C2O C3O -166.7(7) . . . . ? V5 O1P C1P C2P 142(3) . . . . ? O1P C1P C2P C3P -167(4) . . . . ? O1S C1S C2S C3S 45(5) . . . . ? _diffrn_measured_fraction_theta_max 0.783 _diffrn_reflns_theta_full 24.78 _diffrn_measured_fraction_theta_full 0.783 _refine_diff_density_max 0.421 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.056 data_cs2116 _database_code_depnum_ccdc_archive 'CCDC 278653' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H85 O30.25 V6' _chemical_formula_weight 1643.96 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 22.953(5) _cell_length_b 16.460(3) _cell_length_c 42.240(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.41(3) _cell_angle_gamma 90.00 _cell_volume 15384(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7207 _cell_measurement_theta_min 2.95 _cell_measurement_theta_max 28.76 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.125 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6792 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.84 _exptl_absorpt_correction_T_max 0.92 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6894 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART APEXII CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 76360 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0395 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -58 _diffrn_reflns_limit_l_max 60 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 30.54 _reflns_number_total 23207 _reflns_number_gt 17424 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All non-hydrogen were refined anisotropically. Hydrogens were placed geometrically and refined using a riding model. Most terminal and bridging ethanol groups were heavily disordered in two or more positions. In particular, the terminal ethanol O14-C5-C6 was free rotating and modelled split in two parts. The solvent ethanol molecules were disordered and had to be constrained. Further splitting of the disordered EtOH and ETO- groups did not significantly improve the R-factors. ; _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^)+(0.1036P)^2^+31.0630P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23207 _refine_ls_number_parameters 981 _refine_ls_number_restraints 174 _refine_ls_R_factor_all 0.0863 _refine_ls_R_factor_gt 0.0666 _refine_ls_wR_factor_ref 0.2029 _refine_ls_wR_factor_gt 0.1891 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.047 _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 0.29791(2) 0.55465(3) 0.070679(12) 0.03655(11) Uani 1 1 d . A . V2 V 0.42825(2) 0.49805(3) 0.083805(12) 0.03479(11) Uani 1 1 d . A . V3 V 0.42978(2) 0.31882(3) 0.128330(12) 0.03520(11) Uani 1 1 d . A . V4 V 0.33651(2) 0.21978(3) 0.151821(13) 0.04180(13) Uani 1 1 d . A . V5 V 0.20335(2) 0.33383(3) 0.126952(13) 0.04163(13) Uani 1 1 d . A . V6 V 0.16419(2) 0.49206(3) 0.089132(14) 0.04275(13) Uani 1 1 d . A . O1 O 0.26060(9) 0.49172(12) 0.08693(5) 0.0382(4) Uani 1 1 d . . . O2 O 0.45529(10) 0.57044(13) 0.06629(6) 0.0434(5) Uani 1 1 d . . . O3 O 0.39527(9) 0.39657(12) 0.10906(5) 0.0354(4) Uani 1 1 d . . . O4 O 0.37708(11) 0.14389(16) 0.16953(7) 0.0548(6) Uani 1 1 d . . . O5 O 0.27409(10) 0.31981(13) 0.12981(5) 0.0395(4) Uani 1 1 d . . . O6 O 0.09479(11) 0.50040(16) 0.08907(7) 0.0572(6) Uani 1 1 d . . . O7 O 0.37571(9) 0.56140(12) 0.10450(5) 0.0376(4) Uani 1 1 d . . . O8 O 0.34933(9) 0.48623(12) 0.05126(5) 0.0351(4) Uani 1 1 d . . . O9 O 0.36952(10) 0.23188(12) 0.11397(5) 0.0415(5) Uani 1 1 d . . . O10 O 0.39490(10) 0.30879(14) 0.16597(5) 0.0414(4) Uani 1 1 d . . . O11 O 0.17051(10) 0.37446(13) 0.08228(5) 0.0447(5) Uani 1 1 d . . . O12 O 0.19830(10) 0.45163(14) 0.13424(6) 0.0446(5) Uani 1 1 d . . . O13 O 0.34326(12) 0.65002(14) 0.04695(7) 0.0540(6) Uani 1 1 d D . . O14 O 0.48650(14) 0.21445(16) 0.15373(7) 0.0604(7) Uani 1 1 d D . . O15 O 0.26770(10) 0.65531(13) 0.08782(6) 0.0446(5) Uani 1 1 d . . . O16 O 0.18526(11) 0.60932(14) 0.10140(7) 0.0500(5) Uani 1 1 d . . . O17 O 0.23366(10) 0.56304(13) 0.02778(6) 0.0432(5) Uani 1 1 d . . . O18 O 0.15145(10) 0.51503(14) 0.04078(6) 0.0466(5) Uani 1 1 d . . . O19 O 0.49656(10) 0.49429(12) 0.12485(5) 0.0412(5) Uani 1 1 d . . . O20 O 0.50222(9) 0.38103(13) 0.15479(5) 0.0401(4) Uani 1 1 d . . . O21 O 0.46280(9) 0.40479(12) 0.06388(5) 0.0378(4) Uani 1 1 d . . . O22 O 0.47293(10) 0.29130(12) 0.09424(5) 0.0387(4) Uani 1 1 d . . . O23 O 0.26670(11) 0.15272(14) 0.12553(6) 0.0460(5) Uani 1 1 d . . . O24 O 0.17874(10) 0.21989(14) 0.11229(6) 0.0456(5) Uani 1 1 d . . . O25 O 0.29769(12) 0.23838(17) 0.18897(6) 0.0522(6) Uani 1 1 d . . . O26 O 0.20970(12) 0.30501(16) 0.17409(6) 0.0506(5) Uani 1 1 d . . . O27 O 0.10625(12) 0.3381(2) 0.12850(8) 0.0723(9) Uani 1 1 d D . . C1 C 0.3329(2) 0.7272(2) 0.03284(12) 0.0699(12) Uani 1 1 d D A . H1A H 0.3671 0.7620 0.0426 0.084 Uiso 1 1 calc R . . H1B H 0.2974 0.7505 0.0376 0.084 Uiso 1 1 calc R . . C2 C 0.3240(2) 0.7249(3) -0.00351(12) 0.0767(13) Uani 1 1 d D . . H2A H 0.3605 0.7067 -0.0083 0.115 Uiso 1 1 calc R A . H2B H 0.3140 0.7784 -0.0124 0.115 Uiso 1 1 calc R . . H2C H 0.2916 0.6882 -0.0132 0.115 Uiso 1 1 calc R . . C4 C 0.0122(3) 0.2670(5) 0.1031(2) 0.144(4) Uani 1 1 d D . . H4A H -0.0191 0.2348 0.1081 0.216 Uiso 1 1 calc R B . H4B H 0.0238 0.2431 0.0850 0.216 Uiso 1 1 calc R . . H4C H -0.0026 0.3211 0.0974 0.216 Uiso 1 1 calc R . . C7 C 0.34515(16) 0.4759(2) 0.01689(7) 0.0437(6) Uani 1 1 d . A . H7A H 0.3852 0.4800 0.0134 0.052 Uiso 1 1 calc R . . H7B H 0.3204 0.5189 0.0045 0.052 Uiso 1 1 calc R . . C8 C 0.3184(2) 0.3960(3) 0.00472(10) 0.0689(12) Uani 1 1 d . . . H8A H 0.3416 0.3534 0.0177 0.103 Uiso 1 1 calc R A . H8B H 0.3188 0.3894 -0.0178 0.103 Uiso 1 1 calc R . . H8C H 0.2775 0.3937 0.0064 0.103 Uiso 1 1 calc R . . C9 C 0.3797(4) 0.5757(7) 0.13863(19) 0.066(2) Uani 0.50 1 d P A 3 H9A H 0.3975 0.5291 0.1517 0.079 Uiso 0.50 1 calc PR A 3 H9B H 0.3397 0.5846 0.1416 0.079 Uiso 0.50 1 calc PR A 3 C10 C 0.4187(6) 0.6501(12) 0.1493(5) 0.148(8) Uani 0.50 1 d P A 3 H10A H 0.4276 0.6747 0.1305 0.222 Uiso 0.50 1 calc PR A 3 H10B H 0.4557 0.6345 0.1648 0.222 Uiso 0.50 1 calc PR A 3 H10C H 0.3976 0.6884 0.1594 0.222 Uiso 0.50 1 calc PR A 3 C15 C 0.3741(2) 0.1641(2) 0.09307(10) 0.0591(9) Uani 1 1 d . B 5 H15A H 0.3612 0.1148 0.1019 0.071 Uiso 1 1 calc R B 5 H15B H 0.4159 0.1571 0.0928 0.071 Uiso 1 1 calc R B 5 C16 C 0.3364(2) 0.1771(3) 0.05920(10) 0.0711(12) Uani 1 1 d . B 5 H16A H 0.3400 0.1311 0.0459 0.107 Uiso 1 1 calc R B 5 H16B H 0.3497 0.2251 0.0503 0.107 Uiso 1 1 calc R B 5 H16C H 0.2949 0.1835 0.0594 0.107 Uiso 1 1 calc R B 5 C17 C 0.3965(4) 0.3712(6) 0.1896(2) 0.075(3) Uani 0.638(13) 1 d PU B 1 H17A H 0.3559 0.3849 0.1905 0.090 Uiso 0.638(13) 1 calc PR B 1 H17B H 0.4156 0.4196 0.1839 0.090 Uiso 0.638(13) 1 calc PR B 1 C18 C 0.4331(7) 0.3378(14) 0.2226(3) 0.173(8) Uani 0.638(13) 1 d PU B 1 H18A H 0.4316 0.2795 0.2221 0.260 Uiso 0.638(13) 1 calc PR B 1 H18B H 0.4163 0.3574 0.2397 0.260 Uiso 0.638(13) 1 calc PR B 1 H18C H 0.4743 0.3554 0.2267 0.260 Uiso 0.638(13) 1 calc PR B 1 C19 C 0.22366(15) 0.66287(19) 0.10017(8) 0.0446(7) Uani 1 1 d . A . C20 C 0.21709(17) 0.74314(19) 0.11559(8) 0.0482(7) Uani 1 1 d . . . C21 C 0.26596(18) 0.7954(2) 0.12470(9) 0.0511(8) Uani 1 1 d . A . H21 H 0.3022 0.7828 0.1199 0.061 Uiso 1 1 calc R . . C22 C 0.2600(2) 0.8677(2) 0.14119(10) 0.0644(11) Uani 1 1 d . . . H22 H 0.2929 0.9024 0.1482 0.077 Uiso 1 1 calc R A . C23 C 0.2056(3) 0.8870(2) 0.14703(11) 0.0739(13) Uani 1 1 d . A . H23 H 0.2016 0.9352 0.1578 0.089 Uiso 1 1 calc R . . C24 C 0.1566(2) 0.8354(3) 0.13695(12) 0.0721(12) Uani 1 1 d . . . H24 H 0.1195 0.8496 0.1404 0.087 Uiso 1 1 calc R A . C25 C 0.1626(2) 0.7629(2) 0.12181(11) 0.0619(10) Uani 1 1 d . A . H25 H 0.1301 0.7273 0.1158 0.074 Uiso 1 1 calc R . . C26 C 0.17947(14) 0.53816(18) 0.02077(8) 0.0421(7) Uani 1 1 d . A . C27 C 0.14587(14) 0.53628(18) -0.01495(8) 0.0444(7) Uani 1 1 d . . . C28 C 0.17344(17) 0.5626(2) -0.03847(9) 0.0524(8) Uani 1 1 d . A . H28 H 0.2132 0.5808 -0.0322 0.063 Uiso 1 1 calc R . . C29 C 0.1419(2) 0.5619(2) -0.07137(10) 0.0605(10) Uani 1 1 d . . . H29 H 0.1603 0.5798 -0.0872 0.073 Uiso 1 1 calc R A . C30 C 0.08259(19) 0.5343(2) -0.08053(10) 0.0610(10) Uani 1 1 d . A . H30 H 0.0612 0.5344 -0.1026 0.073 Uiso 1 1 calc R . . C31 C 0.05515(17) 0.5068(2) -0.05735(11) 0.0590(10) Uani 1 1 d . . . H31 H 0.0156 0.4878 -0.0638 0.071 Uiso 1 1 calc R A . C32 C 0.08647(15) 0.5074(2) -0.02434(10) 0.0507(8) Uani 1 1 d . A . H32 H 0.0681 0.4887 -0.0086 0.061 Uiso 1 1 calc R . . C33 C 0.52020(13) 0.45077(18) 0.14910(7) 0.0378(6) Uani 1 1 d . A . C34 C 0.57471(14) 0.4844(2) 0.17307(8) 0.0441(7) Uani 1 1 d . . . C35 C 0.60252(19) 0.4419(3) 0.20120(9) 0.0613(10) Uani 1 1 d . A . H35 H 0.5874 0.3919 0.2055 0.074 Uiso 1 1 calc R . . C36 C 0.6539(2) 0.4752(4) 0.22329(11) 0.0841(16) Uani 1 1 d . . . H36 H 0.6728 0.4471 0.2424 0.101 Uiso 1 1 calc R A . C37 C 0.6761(2) 0.5475(4) 0.21698(11) 0.0869(17) Uani 1 1 d . A . H37 H 0.7096 0.5695 0.2320 0.104 Uiso 1 1 calc R . . C38 C 0.6495(2) 0.5894(3) 0.18833(12) 0.0783(14) Uani 1 1 d . . . H38 H 0.6656 0.6386 0.1839 0.094 Uiso 1 1 calc R A . C39 C 0.59872(18) 0.5575(2) 0.16633(10) 0.0570(9) Uani 1 1 d . A . H39 H 0.5808 0.5852 0.1470 0.068 Uiso 1 1 calc R . . C40 C 0.47618(12) 0.33128(16) 0.06922(7) 0.0345(5) Uani 1 1 d . A . C41 C 0.49643(13) 0.28697(17) 0.04330(7) 0.0371(6) Uani 1 1 d . . . C42 C 0.51739(14) 0.20707(19) 0.04867(8) 0.0433(6) Uani 1 1 d . A . H42 H 0.5194 0.1817 0.0686 0.052 Uiso 1 1 calc R . . C43 C 0.53519(17) 0.1657(2) 0.02417(9) 0.0515(8) Uani 1 1 d . . . H43 H 0.5501 0.1130 0.0279 0.062 Uiso 1 1 calc R A . C44 C 0.53068(19) 0.2030(2) -0.00577(10) 0.0568(9) Uani 1 1 d . A . H44 H 0.5415 0.1747 -0.0224 0.068 Uiso 1 1 calc R . . C45 C 0.5101(2) 0.2823(2) -0.01110(9) 0.0566(9) Uani 1 1 d . . . H45 H 0.5076 0.3073 -0.0312 0.068 Uiso 1 1 calc R A . C46 C 0.49333(16) 0.3242(2) 0.01344(8) 0.0451(7) Uani 1 1 d . A . H46 H 0.4799 0.3775 0.0099 0.054 Uiso 1 1 calc R . . C47 C 0.25116(17) 0.2684(2) 0.19455(8) 0.0483(8) Uani 1 1 d . B . C48 C 0.2448(2) 0.2591(2) 0.22859(9) 0.0596(10) Uani 1 1 d . . . C49 C 0.1912(3) 0.2801(3) 0.23505(13) 0.0866(17) Uani 1 1 d . B . H49 H 0.1595 0.3022 0.2189 0.104 Uiso 1 1 calc R . . C50 C 0.1860(4) 0.2665(4) 0.26786(18) 0.118(3) Uani 1 1 d . . . H50 H 0.1500 0.2799 0.2728 0.141 Uiso 1 1 calc R B . C51 C 0.2309(5) 0.2357(4) 0.29126(16) 0.129(3) Uani 1 1 d . B . H51 H 0.2263 0.2279 0.3123 0.155 Uiso 1 1 calc R . . C52 C 0.2833(4) 0.2155(4) 0.28436(12) 0.110(3) Uani 1 1 d . . . H52 H 0.3148 0.1940 0.3008 0.132 Uiso 1 1 calc R B . C53 C 0.2908(3) 0.2264(3) 0.25296(10) 0.0776(14) Uani 1 1 d . B . H53 H 0.3269 0.2116 0.2485 0.093 Uiso 1 1 calc R . . C54 C 0.21108(15) 0.15842(19) 0.11152(7) 0.0408(6) Uani 1 1 d . B . C55 C 0.18107(14) 0.08747(19) 0.09225(7) 0.0403(6) Uani 1 1 d . . . C56 C 0.11852(15) 0.0850(2) 0.07943(9) 0.0486(7) Uani 1 1 d . B . H56 H 0.0951 0.1286 0.0827 0.058 Uiso 1 1 calc R . . C57 C 0.09117(17) 0.0183(2) 0.06187(9) 0.0534(8) Uani 1 1 d . . . H57 H 0.0494 0.0168 0.0536 0.064 Uiso 1 1 calc R B . C58 C 0.12566(17) -0.0460(2) 0.05668(9) 0.0519(8) Uani 1 1 d . B . H58 H 0.1072 -0.0912 0.0450 0.062 Uiso 1 1 calc R . . C59 C 0.18769(18) -0.0435(2) 0.06885(10) 0.0555(9) Uani 1 1 d . . . H59 H 0.2109 -0.0868 0.0650 0.067 Uiso 1 1 calc R B . C60 C 0.21555(16) 0.0227(2) 0.08665(9) 0.0494(7) Uani 1 1 d . B . H60 H 0.2574 0.0238 0.0948 0.059 Uiso 1 1 calc R . . C9A C 0.3979(3) 0.6242(5) 0.12754(19) 0.0492(15) Uani 0.50 1 d P A 4 H9A1 H 0.3847 0.6761 0.1172 0.059 Uiso 0.50 1 calc PR A 4 H9A2 H 0.4417 0.6233 0.1334 0.059 Uiso 0.50 1 calc PR A 4 C10A C 0.3784(6) 0.6178(7) 0.1569(2) 0.081(3) Uani 0.50 1 d P A 4 H10D H 0.3815 0.6699 0.1674 0.121 Uiso 0.50 1 calc PR A 4 H10E H 0.4035 0.5794 0.1715 0.121 Uiso 0.50 1 calc PR A 4 H10F H 0.3372 0.5997 0.1515 0.121 Uiso 0.50 1 calc PR A 4 C11 C 0.1890(4) 0.3377(5) 0.05434(19) 0.0561(17) Uani 0.50 1 d PDU C 1 H11A H 0.2094 0.3782 0.0445 0.067 Uiso 0.50 1 calc PR C 1 H11B H 0.2171 0.2936 0.0623 0.067 Uiso 0.50 1 calc PR C 1 C12 C 0.1378(7) 0.3076(10) 0.0302(3) 0.088(4) Uani 0.50 1 d PDU C 1 H12A H 0.1171 0.2683 0.0401 0.132 Uiso 0.50 1 calc PR C 1 H12B H 0.1508 0.2824 0.0128 0.132 Uiso 0.50 1 calc PR C 1 H12C H 0.1109 0.3517 0.0216 0.132 Uiso 0.50 1 calc PR C 1 C11A C 0.1349(4) 0.3316(5) 0.05447(19) 0.068(2) Uani 0.50 1 d PDU C 2 H11C H 0.1026 0.3657 0.0418 0.081 Uiso 0.50 1 calc PR C 2 H11D H 0.1174 0.2831 0.0613 0.081 Uiso 0.50 1 calc PR C 2 C12A C 0.1769(11) 0.3103(13) 0.0353(5) 0.163(9) Uani 0.50 1 d PDU C 2 H12D H 0.1557 0.2813 0.0159 0.245 Uiso 0.50 1 calc PR C 2 H12E H 0.2085 0.2767 0.0482 0.245 Uiso 0.50 1 calc PR C 2 H12F H 0.1941 0.3590 0.0290 0.245 Uiso 0.50 1 calc PR C 2 C17A C 0.4236(6) 0.3247(9) 0.1994(2) 0.061(4) Uani 0.362(13) 1 d PDU B 2 H17C H 0.4658 0.3093 0.2037 0.073 Uiso 0.362(13) 1 calc PR B 2 H17D H 0.4054 0.2902 0.2128 0.073 Uiso 0.362(13) 1 calc PR B 2 C18A C 0.4206(7) 0.4076(10) 0.2097(3) 0.083(5) Uani 0.362(13) 1 d PDU B 2 H18D H 0.4464 0.4408 0.2005 0.124 Uiso 0.362(13) 1 calc PR B 2 H18E H 0.4337 0.4105 0.2332 0.124 Uiso 0.362(13) 1 calc PR B 2 H18F H 0.3798 0.4268 0.2023 0.124 Uiso 0.362(13) 1 calc PR B 2 C5 C 0.5296(8) 0.1655(8) 0.1487(5) 0.150(7) Uani 0.50 1 d PDU B 1 H5A H 0.5598 0.1679 0.1697 0.180 Uiso 0.50 1 calc PR B 1 H5B H 0.5463 0.1978 0.1340 0.180 Uiso 0.50 1 calc PR B 1 C6 C 0.5374(5) 0.0839(7) 0.1380(4) 0.102(4) Uani 0.50 1 d PDU B 1 H6A H 0.5790 0.0756 0.1383 0.153 Uiso 0.50 1 calc PR B 1 H6B H 0.5125 0.0762 0.1160 0.153 Uiso 0.50 1 calc PR B 1 H6C H 0.5260 0.0457 0.1524 0.153 Uiso 0.50 1 calc PR B 1 C5A C 0.5374(8) 0.2088(11) 0.1796(6) 0.221(12) Uani 0.50 1 d PDU B 2 H5A1 H 0.5302 0.2322 0.1993 0.265 Uiso 0.50 1 calc PR B 2 H5A2 H 0.5711 0.2370 0.1747 0.265 Uiso 0.50 1 calc PR B 2 C6A C 0.5499(9) 0.1212(13) 0.1840(9) 0.298(16) Uani 0.50 1 d PDU B 2 H6A1 H 0.5821 0.1125 0.2034 0.446 Uiso 0.50 1 calc PR B 2 H6A2 H 0.5615 0.1005 0.1653 0.446 Uiso 0.50 1 calc PR B 2 H6A3 H 0.5143 0.0935 0.1860 0.446 Uiso 0.50 1 calc PR B 2 C13 C 0.1944(3) 0.4943(3) 0.16245(12) 0.0897(18) Uani 1 1 d . C . H13A H 0.1763 0.5470 0.1558 0.108 Uiso 1 1 calc R . . H13B H 0.1676 0.4649 0.1727 0.108 Uiso 1 1 calc R . . C14 C 0.2500(4) 0.5062(4) 0.18590(18) 0.129(3) Uani 1 1 d . . . H14A H 0.2635 0.4557 0.1967 0.194 Uiso 1 1 calc R C . H14B H 0.2451 0.5455 0.2018 0.194 Uiso 1 1 calc R . . H14C H 0.2794 0.5255 0.1752 0.194 Uiso 1 1 calc R . . C1S C 0.3450(6) 0.0170(7) 0.2247(4) 0.241(7) Uani 1 1 d DU . . H1S1 H 0.3069 0.0457 0.2172 0.289 Uiso 1 1 calc R . . H1S2 H 0.3467 -0.0291 0.2107 0.289 Uiso 1 1 calc R . . C2S C 0.3603(13) -0.0020(16) 0.2583(5) 0.456(19) Uani 1 1 d DU . . H2S1 H 0.3308 -0.0385 0.2626 0.684 Uiso 1 1 calc R . . H2S2 H 0.3612 0.0469 0.2708 0.684 Uiso 1 1 calc R . . H2S3 H 0.3994 -0.0273 0.2644 0.684 Uiso 1 1 calc R . . O1S O 0.3990(5) 0.0709(6) 0.2307(2) 0.226(4) Uani 1 1 d DU . . O2S O 0.5000 0.0012(8) 0.2500 0.142(6) Uani 0.50 2 d SP . . O3S O 0.4392(10) 0.8685(18) 0.1737(6) 0.60(2) Uani 1 1 d DU . . C4S C 0.5292(11) 0.887(2) 0.1817(5) 0.63(3) Uani 1 1 d DU . . H4S1 H 0.5577 0.9280 0.1922 0.942 Uiso 1 1 calc R . . H4S2 H 0.5057 0.9072 0.1609 0.942 Uiso 1 1 calc R . . H4S3 H 0.5505 0.8392 0.1784 0.942 Uiso 1 1 calc R . . C3S C 0.4885(14) 0.867(3) 0.2028(6) 0.70(3) Uani 1 1 d DU . . H3S1 H 0.4960 0.8147 0.2134 0.842 Uiso 1 1 calc R . . H3S2 H 0.4864 0.9096 0.2185 0.842 Uiso 1 1 calc R . . O4S O 0.5229(7) 0.6609(19) 0.2359(4) 0.55(2) Uani 1 1 d . . . C3 C 0.0673(3) 0.2702(5) 0.1333(2) 0.54(3) Uani 1 1 d D B . H3A H 0.0542 0.2787 0.1531 0.652 Uiso 1 1 calc R . . H3B H 0.0894 0.2194 0.1355 0.652 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 0.0340(2) 0.0305(2) 0.0419(2) -0.00612(18) 0.00448(18) 0.00301(17) V2 0.0324(2) 0.0291(2) 0.0417(2) -0.00204(17) 0.00787(18) -0.00020(16) V3 0.0384(2) 0.0311(2) 0.0349(2) -0.00251(17) 0.00773(18) -0.00357(17) V4 0.0422(3) 0.0421(3) 0.0390(3) 0.0036(2) 0.0072(2) -0.0082(2) V5 0.0414(3) 0.0431(3) 0.0404(3) -0.0093(2) 0.0110(2) -0.0030(2) V6 0.0341(2) 0.0401(3) 0.0519(3) -0.0113(2) 0.0078(2) 0.00306(19) O1 0.0346(10) 0.0343(9) 0.0437(11) -0.0059(8) 0.0069(8) 0.0025(8) O2 0.0405(11) 0.0341(10) 0.0561(13) 0.0029(9) 0.0137(9) -0.0003(8) O3 0.0332(9) 0.0335(9) 0.0383(10) -0.0029(7) 0.0074(7) -0.0037(7) O4 0.0486(13) 0.0499(13) 0.0604(14) 0.0150(11) 0.0046(11) -0.0054(10) O5 0.0418(11) 0.0389(10) 0.0378(10) -0.0029(8) 0.0103(8) -0.0020(8) O6 0.0363(11) 0.0601(15) 0.0750(17) -0.0144(13) 0.0142(11) 0.0018(10) O7 0.0353(10) 0.0326(9) 0.0420(10) -0.0097(8) 0.0053(8) -0.0022(7) O8 0.0353(9) 0.0340(9) 0.0345(9) -0.0029(7) 0.0069(7) 0.0005(7) O9 0.0504(12) 0.0339(10) 0.0408(10) -0.0075(8) 0.0130(9) -0.0093(9) O10 0.0446(11) 0.0440(11) 0.0344(10) -0.0038(8) 0.0083(8) -0.0091(9) O11 0.0476(12) 0.0387(10) 0.0428(11) -0.0116(9) 0.0034(9) 0.0023(9) O12 0.0434(11) 0.0464(12) 0.0442(11) -0.0165(9) 0.0119(9) -0.0004(9) O13 0.0609(15) 0.0348(11) 0.0658(15) 0.0051(10) 0.0162(12) -0.0013(10) O14 0.0771(18) 0.0497(14) 0.0521(14) 0.0095(11) 0.0131(13) 0.0185(13) O15 0.0410(11) 0.0339(10) 0.0561(13) -0.0105(9) 0.0078(9) 0.0050(8) O16 0.0426(12) 0.0400(11) 0.0673(15) -0.0127(10) 0.0145(11) 0.0060(9) O17 0.0373(10) 0.0379(10) 0.0481(12) -0.0030(9) 0.0005(9) 0.0040(8) O18 0.0365(11) 0.0468(12) 0.0510(13) -0.0049(10) 0.0019(9) 0.0056(9) O19 0.0355(10) 0.0359(10) 0.0474(11) -0.0022(8) 0.0028(9) -0.0027(8) O20 0.0364(10) 0.0401(10) 0.0407(10) -0.0023(8) 0.0050(8) -0.0037(8) O21 0.0387(10) 0.0318(9) 0.0442(10) -0.0016(8) 0.0137(8) 0.0004(8) O22 0.0424(11) 0.0336(9) 0.0401(10) -0.0018(8) 0.0109(8) 0.0036(8) O23 0.0450(12) 0.0401(11) 0.0482(12) 0.0026(9) 0.0044(9) -0.0084(9) O24 0.0411(11) 0.0447(12) 0.0523(12) -0.0107(10) 0.0147(10) -0.0070(9) O25 0.0515(13) 0.0659(15) 0.0385(11) 0.0050(10) 0.0107(10) -0.0136(12) O26 0.0556(14) 0.0521(13) 0.0488(13) -0.0092(10) 0.0221(11) -0.0114(11) O27 0.0422(13) 0.100(2) 0.0779(19) -0.0338(17) 0.0221(13) -0.0099(14) C1 0.073(3) 0.0373(17) 0.097(3) 0.0072(19) 0.017(2) 0.0048(17) C2 0.077(3) 0.054(2) 0.087(3) 0.016(2) -0.001(2) -0.009(2) C4 0.101(5) 0.105(5) 0.187(8) -0.050(5) -0.032(5) 0.000(4) C7 0.0485(17) 0.0432(15) 0.0374(14) -0.0016(12) 0.0082(12) 0.0032(13) C8 0.098(3) 0.061(2) 0.0447(19) -0.0176(17) 0.013(2) -0.021(2) C9 0.053(4) 0.098(7) 0.040(4) -0.020(4) 0.002(3) 0.021(5) C10 0.073(7) 0.186(17) 0.163(14) -0.135(14) -0.005(8) -0.009(9) C15 0.072(2) 0.0428(17) 0.061(2) -0.0104(15) 0.0155(19) -0.0091(16) C16 0.092(3) 0.065(2) 0.050(2) -0.0132(18) 0.006(2) -0.005(2) C17 0.063(4) 0.079(5) 0.099(6) -0.051(5) 0.050(4) -0.028(4) C18 0.134(11) 0.32(2) 0.056(6) -0.039(8) 0.014(5) -0.111(12) C19 0.0424(15) 0.0375(14) 0.0490(16) -0.0105(12) 0.0035(13) 0.0077(12) C20 0.0577(19) 0.0364(14) 0.0462(16) -0.0072(12) 0.0065(14) 0.0118(13) C21 0.067(2) 0.0341(14) 0.0498(17) -0.0048(13) 0.0106(16) 0.0052(14) C22 0.093(3) 0.0394(17) 0.062(2) -0.0125(16) 0.022(2) -0.0008(18) C23 0.115(4) 0.0429(19) 0.069(3) -0.0157(18) 0.033(3) 0.009(2) C24 0.085(3) 0.054(2) 0.083(3) -0.018(2) 0.031(2) 0.017(2) C25 0.063(2) 0.051(2) 0.070(2) -0.0172(17) 0.0149(19) 0.0167(17) C26 0.0388(14) 0.0315(13) 0.0495(16) -0.0071(11) 0.0004(12) 0.0085(11) C27 0.0423(15) 0.0308(13) 0.0522(17) -0.0054(12) -0.0013(13) 0.0075(11) C28 0.0529(19) 0.0426(16) 0.0520(18) 0.0001(14) -0.0027(15) 0.0001(14) C29 0.066(2) 0.053(2) 0.054(2) 0.0027(16) -0.0005(17) -0.0003(17) C30 0.064(2) 0.0497(19) 0.054(2) -0.0040(16) -0.0116(17) 0.0071(17) C31 0.0426(17) 0.0513(19) 0.070(2) -0.0143(17) -0.0074(16) 0.0066(14) C32 0.0388(15) 0.0440(16) 0.062(2) -0.0116(14) -0.0003(14) 0.0081(13) C33 0.0327(13) 0.0395(14) 0.0405(14) -0.0107(11) 0.0085(11) -0.0006(10) C34 0.0393(15) 0.0520(17) 0.0389(14) -0.0123(13) 0.0065(12) -0.0062(13) C35 0.059(2) 0.079(3) 0.0399(16) 0.0004(17) 0.0019(15) -0.0206(19) C36 0.076(3) 0.115(4) 0.046(2) 0.005(2) -0.011(2) -0.034(3) C37 0.074(3) 0.114(4) 0.057(2) -0.014(3) -0.010(2) -0.045(3) C38 0.075(3) 0.075(3) 0.071(3) -0.009(2) -0.004(2) -0.037(2) C39 0.055(2) 0.055(2) 0.0532(19) -0.0095(16) 0.0015(16) -0.0162(16) C40 0.0307(12) 0.0324(12) 0.0394(13) -0.0037(10) 0.0077(10) -0.0027(9) C41 0.0327(12) 0.0358(13) 0.0426(14) -0.0060(11) 0.0097(11) -0.0017(10) C42 0.0425(15) 0.0393(14) 0.0486(16) -0.0013(12) 0.0130(13) 0.0052(12) C43 0.057(2) 0.0405(16) 0.062(2) -0.0047(14) 0.0237(16) 0.0075(14) C44 0.068(2) 0.0531(19) 0.059(2) -0.0066(16) 0.0332(18) 0.0049(17) C45 0.074(2) 0.0530(19) 0.0497(18) 0.0006(15) 0.0290(18) 0.0051(17) C46 0.0521(18) 0.0376(14) 0.0487(17) -0.0014(12) 0.0192(14) -0.0009(13) C47 0.060(2) 0.0474(17) 0.0383(15) -0.0075(13) 0.0153(14) -0.0197(15) C48 0.095(3) 0.0452(17) 0.0452(17) -0.0121(14) 0.0307(19) -0.0255(19) C49 0.137(5) 0.069(3) 0.075(3) -0.013(2) 0.066(3) -0.010(3) C50 0.203(8) 0.087(4) 0.100(5) -0.013(4) 0.104(6) -0.005(5) C51 0.269(11) 0.080(4) 0.064(3) -0.003(3) 0.089(6) -0.014(5) C52 0.196(8) 0.088(4) 0.044(2) 0.004(2) 0.028(4) -0.033(4) C53 0.113(4) 0.075(3) 0.0426(19) 0.0005(19) 0.017(2) -0.028(3) C54 0.0454(16) 0.0406(14) 0.0378(14) 0.0004(11) 0.0134(12) -0.0091(12) C55 0.0439(15) 0.0404(14) 0.0374(14) 0.0018(11) 0.0123(11) -0.0103(12) C56 0.0422(16) 0.0547(18) 0.0522(18) -0.0117(15) 0.0185(14) -0.0099(14) C57 0.0442(17) 0.062(2) 0.057(2) -0.0143(16) 0.0174(15) -0.0177(15) C58 0.056(2) 0.0477(17) 0.0485(17) -0.0035(14) 0.0087(15) -0.0165(15) C59 0.056(2) 0.0377(16) 0.067(2) -0.0047(15) 0.0065(17) -0.0016(14) C60 0.0465(17) 0.0379(15) 0.0580(19) 0.0005(14) 0.0036(14) -0.0027(13) C9A 0.043(3) 0.044(3) 0.055(4) -0.019(3) 0.004(3) 0.000(3) C10A 0.113(9) 0.076(6) 0.046(4) -0.017(4) 0.010(5) 0.010(6) C11 0.077(5) 0.044(3) 0.054(4) -0.010(3) 0.029(4) 0.002(3) C12 0.140(11) 0.057(6) 0.052(5) -0.022(4) 0.002(6) -0.020(7) C11A 0.094(6) 0.045(4) 0.046(4) -0.005(3) -0.014(4) -0.024(4) C12A 0.34(3) 0.087(11) 0.099(12) -0.022(10) 0.120(17) 0.039(18) C17A 0.055(7) 0.096(9) 0.033(5) -0.019(5) 0.012(4) -0.039(6) C18A 0.080(9) 0.120(11) 0.046(7) -0.035(7) 0.013(6) 0.017(9) C5 0.130(11) 0.122(9) 0.246(19) 0.114(10) 0.134(13) 0.075(9) C6 0.059(6) 0.100(8) 0.146(11) 0.030(8) 0.027(7) 0.033(6) C5A 0.087(10) 0.208(17) 0.33(3) 0.168(18) -0.006(15) 0.060(12) C6A 0.110(13) 0.234(18) 0.52(4) 0.28(2) 0.03(2) 0.051(14) C13 0.146(6) 0.067(3) 0.060(3) -0.020(2) 0.035(3) 0.002(3) C14 0.146(7) 0.102(5) 0.102(5) -0.041(4) -0.034(5) 0.008(4) C1S 0.270(14) 0.152(9) 0.38(2) 0.120(11) 0.234(14) 0.034(8) C2S 0.59(4) 0.44(4) 0.41(2) 0.17(3) 0.26(3) -0.08(3) O1S 0.270(11) 0.204(9) 0.223(9) 0.070(7) 0.096(8) -0.013(7) O2S 0.117(11) 0.085(9) 0.185(16) 0.000 -0.025(11) 0.000 O3S 0.55(3) 0.84(4) 0.56(3) -0.44(3) 0.40(3) -0.37(3) C4S 0.60(3) 1.08(6) 0.26(2) -0.30(3) 0.21(2) -0.66(4) C3S 0.66(4) 0.97(5) 0.59(4) -0.23(5) 0.36(3) -0.61(4) O4S 0.247(15) 1.13(6) 0.285(17) -0.32(3) 0.106(12) -0.04(2) C3 0.124(9) 0.71(4) 0.87(5) -0.65(4) 0.263(19) -0.223(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.609(2) . ? V1 O8 1.962(2) . ? V1 O7 1.971(2) . ? V1 O15 2.004(2) . ? V1 O17 2.014(2) . ? V1 O13 2.260(3) . ? V1 V2 3.0403(9) . ? V2 O2 1.611(2) . ? V2 O7 1.966(2) . ? V2 O8 1.971(2) . ? V2 O19 2.006(2) . ? V2 O21 2.012(2) . ? V2 O3 2.220(2) . ? V3 O3 1.608(2) . ? V3 O10 1.968(2) . ? V3 O9 1.971(2) . ? V3 O22 2.004(2) . ? V3 O20 2.018(2) . ? V3 O14 2.248(3) . ? V3 V4 3.0585(9) . ? V4 O4 1.618(3) . ? V4 O9 1.953(2) . ? V4 O10 1.968(2) . ? V4 O23 2.018(2) . ? V4 O25 2.023(3) . ? V4 O5 2.218(2) . ? V5 O5 1.612(2) . ? V5 O11 1.955(2) . ? V5 O12 1.971(2) . ? V5 O24 2.009(2) . ? V5 O26 2.014(3) . ? V5 O27 2.248(3) . ? V5 V6 3.0627(10) . ? V6 O6 1.598(3) . ? V6 O11 1.968(2) . ? V6 O12 1.973(3) . ? V6 O18 2.021(3) . ? V6 O16 2.023(2) . ? V6 O1 2.239(2) . ? O7 C9A 1.418(6) . ? O7 C9 1.439(8) . ? O8 C7 1.440(4) . ? O9 C15 1.444(4) . ? O10 C17A 1.415(9) . ? O10 C17 1.424(7) . ? O11 C11A 1.427(7) . ? O11 C11 1.485(8) . ? O12 C13 1.406(5) . ? O13 C1 1.396(4) . ? O14 C5 1.337(10) . ? O14 C5A 1.375(13) . ? O15 C19 1.261(4) . ? O16 C19 1.257(4) . ? O17 C26 1.268(4) . ? O18 C26 1.249(4) . ? O19 C33 1.250(4) . ? O20 C33 1.264(4) . ? O21 C40 1.254(3) . ? O22 C40 1.264(4) . ? O23 C54 1.260(4) . ? O24 C54 1.260(4) . ? O25 C47 1.254(5) . ? O26 C47 1.257(5) . ? O27 C3 1.4795(11) . ? C1 C2 1.495(7) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C4 C3 1.5394(12) . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C7 C8 1.483(5) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 C10 1.514(19) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C15 C16 1.478(6) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 C18 1.53(2) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.498(4) . ? C20 C25 1.384(5) . ? C20 C21 1.385(5) . ? C21 C22 1.403(5) . ? C21 H21 0.9300 . ? C22 C23 1.374(7) . ? C22 H22 0.9300 . ? C23 C24 1.384(7) . ? C23 H23 0.9300 . ? C24 C25 1.377(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.502(4) . ? C27 C28 1.381(6) . ? C27 C32 1.398(5) . ? C28 C29 1.386(5) . ? C28 H28 0.9300 . ? C29 C30 1.389(6) . ? C29 H29 0.9300 . ? C30 C31 1.374(7) . ? C30 H30 0.9300 . ? C31 C32 1.389(5) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.491(4) . ? C34 C35 1.380(5) . ? C34 C39 1.384(5) . ? C35 C36 1.406(5) . ? C35 H35 0.9300 . ? C36 C37 1.349(7) . ? C36 H36 0.9300 . ? C37 C38 1.385(7) . ? C37 H37 0.9300 . ? C38 C39 1.386(5) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.489(4) . ? C41 C46 1.387(4) . ? C41 C42 1.398(4) . ? C42 C43 1.388(5) . ? C42 H42 0.9300 . ? C43 C44 1.385(5) . ? C43 H43 0.9300 . ? C44 C45 1.385(5) . ? C44 H44 0.9300 . ? C45 C46 1.382(5) . ? C45 H45 0.9300 . ? C46 H46 0.9300 . ? C47 C48 1.491(5) . ? C48 C53 1.373(7) . ? C48 C49 1.375(7) . ? C49 C50 1.439(8) . ? C49 H49 0.9300 . ? C50 C51 1.325(12) . ? C50 H50 0.9300 . ? C51 C52 1.352(12) . ? C51 H51 0.9300 . ? C52 C53 1.394(7) . ? C52 H52 0.9300 . ? C53 H53 0.9300 . ? C54 C55 1.484(4) . ? C55 C60 1.385(5) . ? C55 C56 1.394(5) . ? C56 C57 1.379(5) . ? C56 H56 0.9300 . ? C57 C58 1.374(6) . ? C57 H57 0.9300 . ? C58 C59 1.380(5) . ? C58 H58 0.9300 . ? C59 C60 1.381(5) . ? C59 H59 0.9300 . ? C60 H60 0.9300 . ? C9A C10A 1.428(13) . ? C9A H9A1 0.9700 . ? C9A H9A2 0.9700 . ? C10A H10D 0.9600 . ? C10A H10E 0.9600 . ? C10A H10F 0.9600 . ? C11 C12 1.425(11) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C11A C12A 1.457(13) . ? C11A H11C 0.9700 . ? C11A H11D 0.9700 . ? C12A H12D 0.9600 . ? C12A H12E 0.9600 . ? C12A H12F 0.9600 . ? C17A C18A 1.439(15) . ? C17A H17C 0.9700 . ? C17A H17D 0.9700 . ? C18A H18D 0.9600 . ? C18A H18E 0.9600 . ? C18A H18F 0.9600 . ? C5 C6 1.442(13) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C5A C6A 1.472(15) . ? C5A H5A1 0.9700 . ? C5A H5A2 0.9700 . ? C6A H6A1 0.9600 . ? C6A H6A2 0.9600 . ? C6A H6A3 0.9600 . ? C13 C14 1.406(9) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C1S C2S 1.402(14) . ? C1S O1S 1.490(12) . ? C1S H1S1 0.9700 . ? C1S H1S2 0.9700 . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 0.9600 . ? O3S C3S 1.433(17) . ? C4S C3S 1.490(15) . ? C4S H4S1 0.9600 . ? C4S H4S2 0.9600 . ? C4S H4S3 0.9600 . ? C3S H3S1 0.9700 . ? C3S H3S2 0.9700 . ? O4S O4S 1.79(3) 2_655 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O8 104.84(10) . . ? O1 V1 O7 102.09(10) . . ? O8 V1 O7 78.79(8) . . ? O1 V1 O15 95.95(10) . . ? O8 V1 O15 158.42(10) . . ? O7 V1 O15 91.45(9) . . ? O1 V1 O17 94.73(10) . . ? O8 V1 O17 92.36(9) . . ? O7 V1 O17 162.50(10) . . ? O15 V1 O17 91.57(9) . . ? O1 V1 O13 175.09(10) . . ? O8 V1 O13 79.29(9) . . ? O7 V1 O13 81.20(10) . . ? O15 V1 O13 80.23(10) . . ? O17 V1 O13 82.34(10) . . ? O1 V1 V2 109.53(8) . . ? O8 V1 V2 39.48(6) . . ? O7 V1 V2 39.39(6) . . ? O15 V1 V2 127.27(7) . . ? O17 V1 V2 129.40(7) . . ? O13 V1 V2 75.34(7) . . ? O2 V2 O7 99.70(10) . . ? O2 V2 O8 98.49(10) . . ? O7 V2 O8 78.69(8) . . ? O2 V2 O19 96.41(11) . . ? O7 V2 O19 93.61(9) . . ? O8 V2 O19 164.19(9) . . ? O2 V2 O21 97.43(10) . . ? O7 V2 O21 161.28(9) . . ? O8 V2 O21 91.39(9) . . ? O19 V2 O21 91.92(9) . . ? O2 V2 O3 177.38(10) . . ? O7 V2 O3 81.82(8) . . ? O8 V2 O3 83.88(8) . . ? O19 V2 O3 81.34(8) . . ? O21 V2 O3 81.35(8) . . ? O2 V2 V1 99.79(8) . . ? O7 V2 V1 39.52(6) . . ? O8 V2 V1 39.26(6) . . ? O19 V2 V1 132.26(7) . . ? O21 V2 V1 129.47(6) . . ? O3 V2 V1 82.74(6) . . ? O3 V3 O10 102.96(10) . . ? O3 V3 O9 102.18(10) . . ? O10 V3 O9 77.58(9) . . ? O3 V3 O22 95.01(10) . . ? O10 V3 O22 161.12(9) . . ? O9 V3 O22 93.15(9) . . ? O3 V3 O20 95.69(10) . . ? O10 V3 O20 92.71(9) . . ? O9 V3 O20 161.15(9) . . ? O22 V3 O20 91.20(9) . . ? O3 V3 O14 174.09(11) . . ? O10 V3 O14 81.87(10) . . ? O9 V3 O14 82.07(11) . . ? O22 V3 O14 80.57(10) . . ? O20 V3 O14 80.56(10) . . ? O3 V3 V4 107.18(8) . . ? O10 V3 V4 39.02(6) . . ? O9 V3 V4 38.58(6) . . ? O22 V3 V4 129.39(7) . . ? O20 V3 V4 129.44(7) . . ? O14 V3 V4 78.72(8) . . ? O4 V4 O9 99.00(13) . . ? O4 V4 O10 99.93(12) . . ? O9 V4 O10 77.98(9) . . ? O4 V4 O23 96.16(12) . . ? O9 V4 O23 91.67(10) . . ? O10 V4 O23 162.02(10) . . ? O4 V4 O25 94.37(13) . . ? O9 V4 O25 165.07(11) . . ? O10 V4 O25 93.24(10) . . ? O23 V4 O25 93.48(10) . . ? O4 V4 O5 174.46(11) . . ? O9 V4 O5 85.94(9) . . ? O10 V4 O5 83.49(9) . . ? O23 V4 O5 81.11(9) . . ? O25 V4 O5 81.04(10) . . ? O4 V4 V3 101.25(10) . . ? O9 V4 V3 38.99(6) . . ? O10 V4 V3 39.01(6) . . ? O23 V4 V3 129.41(7) . . ? O25 V4 V3 131.41(8) . . ? O5 V4 V3 84.16(6) . . ? O5 V5 O11 104.11(11) . . ? O5 V5 O12 103.23(10) . . ? O11 V5 O12 77.92(9) . . ? O5 V5 O24 94.85(10) . . ? O11 V5 O24 90.97(10) . . ? O12 V5 O24 160.58(10) . . ? O5 V5 O26 94.89(11) . . ? O11 V5 O26 160.57(11) . . ? O12 V5 O26 93.97(10) . . ? O24 V5 O26 91.46(10) . . ? O5 V5 O27 171.35(13) . . ? O11 V5 O27 83.48(12) . . ? O12 V5 O27 82.23(11) . . ? O24 V5 O27 80.70(11) . . ? O26 V5 O27 77.90(12) . . ? O5 V5 V6 108.12(8) . . ? O11 V5 V6 38.84(6) . . ? O12 V5 V6 39.08(7) . . ? O24 V5 V6 127.86(8) . . ? O26 V5 V6 130.55(8) . . ? O27 V5 V6 80.38(10) . . ? O6 V6 O11 101.33(12) . . ? O6 V6 O12 99.79(14) . . ? O11 V6 O12 77.55(9) . . ? O6 V6 O18 96.08(13) . . ? O11 V6 O18 91.82(10) . . ? O12 V6 O18 162.34(9) . . ? O6 V6 O16 95.09(12) . . ? O11 V6 O16 162.52(10) . . ? O12 V6 O16 93.89(10) . . ? O18 V6 O16 92.35(11) . . ? O6 V6 O1 174.66(13) . . ? O11 V6 O1 83.06(9) . . ? O12 V6 O1 84.05(9) . . ? O18 V6 O1 80.66(9) . . ? O16 V6 O1 80.88(8) . . ? O6 V6 V5 103.18(11) . . ? O11 V6 V5 38.51(7) . . ? O12 V6 V5 39.04(6) . . ? O18 V6 V5 129.05(7) . . ? O16 V6 V5 131.33(8) . . ? O1 V6 V5 82.14(6) . . ? V1 O1 V6 131.28(11) . . ? V3 O3 V2 131.08(11) . . ? V5 O5 V4 131.54(12) . . ? C9A O7 C9 43.7(5) . . ? C9A O7 V2 122.8(3) . . ? C9 O7 V2 130.5(4) . . ? C9A O7 V1 129.0(3) . . ? C9 O7 V1 122.6(4) . . ? V2 O7 V1 101.09(9) . . ? C7 O8 V1 127.12(18) . . ? C7 O8 V2 121.17(19) . . ? V1 O8 V2 101.26(9) . . ? C15 O9 V4 121.9(2) . . ? C15 O9 V3 126.2(2) . . ? V4 O9 V3 102.43(9) . . ? C17A O10 C17 41.4(6) . . ? C17A O10 V3 127.6(5) . . ? C17 O10 V3 124.4(4) . . ? C17A O10 V4 122.6(5) . . ? C17 O10 V4 129.6(3) . . ? V3 O10 V4 101.97(10) . . ? C11A O11 C11 50.7(5) . . ? C11A O11 V5 128.0(4) . . ? C11 O11 V5 120.6(3) . . ? C11A O11 V6 124.0(4) . . ? C11 O11 V6 124.4(3) . . ? V5 O11 V6 102.65(10) . . ? C13 O12 V5 130.0(3) . . ? C13 O12 V6 123.5(3) . . ? V5 O12 V6 101.87(10) . . ? C1 O13 V1 140.8(3) . . ? C5 O14 C5A 65.1(12) . . ? C5 O14 V3 138.0(7) . . ? C5A O14 V3 133.8(8) . . ? C19 O15 V1 128.6(2) . . ? C19 O16 V6 141.3(2) . . ? C26 O17 V1 128.8(2) . . ? C26 O18 V6 141.1(2) . . ? C33 O19 V2 142.7(2) . . ? C33 O20 V3 128.15(19) . . ? C40 O21 V2 140.0(2) . . ? C40 O22 V3 129.29(19) . . ? C54 O23 V4 140.8(2) . . ? C54 O24 V5 129.7(2) . . ? C47 O25 V4 141.0(2) . . ? C47 O26 V5 129.5(2) . . ? C3 O27 V5 128.4(4) . . ? O13 C1 C2 112.2(4) . . ? O13 C1 H1A 109.2 . . ? C2 C1 H1A 109.2 . . ? O13 C1 H1B 109.2 . . ? C2 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O8 C7 C8 111.4(3) . . ? O8 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? O8 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? 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 . . ? O7 C9 C10 107.8(11) . . ? O7 C9 H9A 110.1 . . ? C10 C9 H9A 110.1 . . ? O7 C9 H9B 110.1 . . ? C10 C9 H9B 110.1 . . ? H9A C9 H9B 108.5 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O9 C15 C16 111.1(3) . . ? O9 C15 H15A 109.4 . . ? C16 C15 H15A 109.4 . . ? O9 C15 H15B 109.4 . . ? C16 C15 H15B 109.4 . . ? H15A C15 H15B 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O10 C17 C18 106.6(11) . . ? O10 C17 H17A 110.4 . . ? C18 C17 H17A 110.4 . . ? O10 C17 H17B 110.4 . . ? C18 C17 H17B 110.4 . . ? H17A C17 H17B 108.6 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? O16 C19 O15 126.6(3) . . ? O16 C19 C20 116.6(3) . . ? O15 C19 C20 116.8(3) . . ? C25 C20 C21 120.5(3) . . ? C25 C20 C19 119.4(3) . . ? C21 C20 C19 120.1(3) . . ? C20 C21 C22 119.1(4) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C23 C22 C21 119.9(4) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 120.4(4) . . ? C22 C23 H23 119.8 . . ? C24 C23 H23 119.8 . . ? C25 C24 C23 120.1(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C20 120.0(4) . . ? C24 C25 H25 120.0 . . ? C20 C25 H25 120.0 . . ? O18 C26 O17 126.2(3) . . ? O18 C26 C27 117.0(3) . . ? O17 C26 C27 116.8(3) . . ? C28 C27 C32 120.1(3) . . ? C28 C27 C26 120.3(3) . . ? C32 C27 C26 119.6(3) . . ? C27 C28 C29 120.1(4) . . ? C27 C28 H28 119.9 . . ? C29 C28 H28 119.9 . . ? C28 C29 C30 119.6(4) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C31 C30 C29 120.7(4) . . ? C31 C30 H30 119.7 . . ? C29 C30 H30 119.7 . . ? C30 C31 C32 120.0(4) . . ? C30 C31 H31 120.0 . . ? C32 C31 H31 120.0 . . ? C31 C32 C27 119.5(4) . . ? C31 C32 H32 120.2 . . ? C27 C32 H32 120.2 . . ? O19 C33 O20 125.7(3) . . ? O19 C33 C34 116.6(3) . . ? O20 C33 C34 117.7(3) . . ? C35 C34 C39 119.9(3) . . ? C35 C34 C33 120.6(3) . . ? C39 C34 C33 119.4(3) . . ? C34 C35 C36 119.3(4) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 120.4(4) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C36 C37 C38 120.7(4) . . ? C36 C37 H37 119.7 . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 119.6(4) . . ? C37 C38 H38 120.2 . . ? C39 C38 H38 120.2 . . ? C34 C39 C38 120.1(4) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? O21 C40 O22 125.9(3) . . ? O21 C40 C41 116.7(3) . . ? O22 C40 C41 117.3(2) . . ? C46 C41 C42 119.7(3) . . ? C46 C41 C40 120.1(3) . . ? C42 C41 C40 120.2(3) . . ? C43 C42 C41 119.8(3) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 119.8(3) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 120.4(3) . . ? C45 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? C46 C45 C44 119.9(3) . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.3(3) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? O25 C47 O26 125.9(3) . . ? O25 C47 C48 116.5(4) . . ? O26 C47 C48 117.5(4) . . ? C53 C48 C49 120.0(4) . . ? C53 C48 C47 120.7(4) . . ? C49 C48 C47 119.2(4) . . ? C48 C49 C50 117.4(7) . . ? C48 C49 H49 121.3 . . ? C50 C49 H49 121.3 . . ? C51 C50 C49 122.1(7) . . ? C51 C50 H50 118.9 . . ? C49 C50 H50 118.9 . . ? C50 C51 C52 119.5(5) . . ? C50 C51 H51 120.2 . . ? C52 C51 H51 120.2 . . ? C51 C52 C53 121.1(7) . . ? C51 C52 H52 119.5 . . ? C53 C52 H52 119.5 . . ? C48 C53 C52 119.9(6) . . ? C48 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? O23 C54 O24 125.3(3) . . ? O23 C54 C55 117.6(3) . . ? O24 C54 C55 117.1(3) . . ? C60 C55 C56 119.1(3) . . ? C60 C55 C54 119.8(3) . . ? C56 C55 C54 121.1(3) . . ? C57 C56 C55 120.5(3) . . ? C57 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C58 C57 C56 120.0(3) . . ? C58 C57 H57 120.0 . . ? C56 C57 H57 120.0 . . ? C57 C58 C59 119.9(3) . . ? C57 C58 H58 120.0 . . ? C59 C58 H58 120.0 . . ? C58 C59 C60 120.6(4) . . ? C58 C59 H59 119.7 . . ? C60 C59 H59 119.7 . . ? C59 C60 C55 119.8(3) . . ? C59 C60 H60 120.1 . . ? C55 C60 H60 120.1 . . ? O7 C9A C10A 113.8(8) . . ? O7 C9A H9A1 108.8 . . ? C10A C9A H9A1 108.8 . . ? O7 C9A H9A2 108.8 . . ? C10A C9A H9A2 108.8 . . ? H9A1 C9A H9A2 107.7 . . ? C9A C10A H10D 109.5 . . ? C9A C10A H10E 109.5 . . ? H10D C10A H10E 109.5 . . ? C9A C10A H10F 109.5 . . ? H10D C10A H10F 109.5 . . ? H10E C10A H10F 109.5 . . ? C12 C11 O11 110.8(9) . . ? C12 C11 H11A 109.5 . . ? O11 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? O11 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? 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 . . ? O11 C11A C12A 104.9(11) . . ? O11 C11A H11C 110.8 . . ? C12A C11A H11C 110.8 . . ? O11 C11A H11D 110.8 . . ? C12A C11A H11D 110.8 . . ? H11C C11A H11D 108.8 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? O10 C17A C18A 115.5(12) . . ? O10 C17A H17C 108.4 . . ? C18A C17A H17C 108.4 . . ? O10 C17A H17D 108.4 . . ? C18A C17A H17D 108.4 . . ? H17C C17A H17D 107.5 . . ? C17A C18A H18D 109.5 . . ? C17A C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? C17A C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? O14 C5 C6 140.4(15) . . ? O14 C5 H5A 101.9 . . ? C6 C5 H5A 101.9 . . ? O14 C5 H5B 101.9 . . ? C6 C5 H5B 101.9 . . ? H5A C5 H5B 104.7 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O14 C5A C6A 105.1(14) . . ? O14 C5A H5A1 110.7 . . ? C6A C5A H5A1 110.7 . . ? O14 C5A H5A2 110.7 . . ? C6A C5A H5A2 110.7 . . ? H5A1 C5A H5A2 108.8 . . ? C5A C6A H6A1 109.5 . . ? C5A C6A H6A2 109.5 . . ? H6A1 C6A H6A2 109.5 . . ? C5A C6A H6A3 109.5 . . ? H6A1 C6A H6A3 109.5 . . ? H6A2 C6A H6A3 109.5 . . ? C14 C13 O12 114.6(6) . . ? C14 C13 H13A 108.6 . . ? O12 C13 H13A 108.6 . . ? C14 C13 H13B 108.6 . . ? O12 C13 H13B 108.6 . . ? H13A C13 H13B 107.6 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C2S C1S O1S 89.2(13) . . ? C2S C1S H1S1 113.8 . . ? O1S C1S H1S1 113.8 . . ? C2S C1S H1S2 113.8 . . ? O1S C1S H1S2 113.8 . . ? H1S1 C1S H1S2 111.0 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 109.5 . . ? C3S C4S H4S1 109.5 . . ? C3S C4S H4S2 109.5 . . ? H4S1 C4S H4S2 109.5 . . ? C3S C4S H4S3 109.5 . . ? H4S1 C4S H4S3 109.5 . . ? H4S2 C4S H4S3 109.5 . . ? O3S C3S C4S 87.8(15) . . ? O3S C3S H3S1 114.0 . . ? C4S C3S H3S1 114.0 . . ? O3S C3S H3S2 114.0 . . ? C4S C3S H3S2 114.0 . . ? H3S1 C3S H3S2 111.2 . . ? O27 C3 C4 107.8(5) . . ? O27 C3 H3A 110.1 . . ? C4 C3 H3A 110.1 . . ? O27 C3 H3B 110.1 . . ? C4 C3 H3B 110.1 . . ? H3A C3 H3B 108.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 V1 V2 O2 -178.72(12) . . . . ? O8 V1 V2 O2 91.46(13) . . . . ? O7 V1 V2 O2 -93.41(13) . . . . ? O15 V1 V2 O2 -64.63(13) . . . . ? O17 V1 V2 O2 67.41(12) . . . . ? O13 V1 V2 O2 0.57(11) . . . . ? O1 V1 V2 O7 -85.31(13) . . . . ? O8 V1 V2 O7 -175.13(14) . . . . ? O15 V1 V2 O7 28.78(13) . . . . ? O17 V1 V2 O7 160.82(13) . . . . ? O13 V1 V2 O7 93.98(12) . . . . ? O1 V1 V2 O8 89.82(12) . . . . ? O7 V1 V2 O8 175.13(14) . . . . ? O15 V1 V2 O8 -156.09(14) . . . . ? O17 V1 V2 O8 -24.05(13) . . . . ? O13 V1 V2 O8 -90.89(12) . . . . ? O1 V1 V2 O19 -70.67(12) . . . . ? O8 V1 V2 O19 -160.49(13) . . . . ? O7 V1 V2 O19 14.64(13) . . . . ? O15 V1 V2 O19 43.42(13) . . . . ? O17 V1 V2 O19 175.46(12) . . . . ? O13 V1 V2 O19 108.62(11) . . . . ? O1 V1 V2 O21 73.09(12) . . . . ? O8 V1 V2 O21 -16.73(12) . . . . ? O7 V1 V2 O21 158.40(13) . . . . ? O15 V1 V2 O21 -172.82(12) . . . . ? O17 V1 V2 O21 -40.78(12) . . . . ? O13 V1 V2 O21 -107.62(11) . . . . ? O1 V1 V2 O3 0.62(9) . . . . ? O8 V1 V2 O3 -89.20(11) . . . . ? O7 V1 V2 O3 85.93(11) . . . . ? O15 V1 V2 O3 114.72(11) . . . . ? O17 V1 V2 O3 -113.25(10) . . . . ? O13 V1 V2 O3 179.91(9) . . . . ? O3 V3 V4 O4 178.54(13) . . . . ? O10 V3 V4 O4 -91.94(15) . . . . ? O9 V3 V4 O4 90.45(15) . . . . ? O22 V3 V4 O4 66.70(13) . . . . ? O20 V3 V4 O4 -68.59(14) . . . . ? O14 V3 V4 O4 -0.96(13) . . . . ? O3 V3 V4 O9 88.10(13) . . . . ? O10 V3 V4 O9 177.61(15) . . . . ? O22 V3 V4 O9 -23.75(13) . . . . ? O20 V3 V4 O9 -159.04(14) . . . . ? O14 V3 V4 O9 -91.41(13) . . . . ? O3 V3 V4 O10 -89.51(13) . . . . ? O9 V3 V4 O10 -177.61(15) . . . . ? O22 V3 V4 O10 158.64(14) . . . . ? O20 V3 V4 O10 23.35(14) . . . . ? O14 V3 V4 O10 90.98(13) . . . . ? O3 V3 V4 O23 70.79(12) . . . . ? O10 V3 V4 O23 160.30(15) . . . . ? O9 V3 V4 O23 -17.31(14) . . . . ? O22 V3 V4 O23 -41.06(13) . . . . ? O20 V3 V4 O23 -176.35(12) . . . . ? O14 V3 V4 O23 -108.72(12) . . . . ? O3 V3 V4 O25 -75.25(13) . . . . ? O10 V3 V4 O25 14.26(15) . . . . ? O9 V3 V4 O25 -163.35(15) . . . . ? O22 V3 V4 O25 172.90(13) . . . . ? O20 V3 V4 O25 37.61(14) . . . . ? O14 V3 V4 O25 105.24(13) . . . . ? O3 V3 V4 O5 -2.65(9) . . . . ? O10 V3 V4 O5 86.86(12) . . . . ? O9 V3 V4 O5 -90.75(12) . . . . ? O22 V3 V4 O5 -114.49(10) . . . . ? O20 V3 V4 O5 110.21(10) . . . . ? O14 V3 V4 O5 177.84(9) . . . . ? O5 V5 V6 O6 -178.14(13) . . . . ? O11 V5 V6 O6 91.71(16) . . . . ? O12 V5 V6 O6 -89.34(15) . . . . ? O24 V5 V6 O6 70.33(14) . . . . ? O26 V5 V6 O6 -64.69(14) . . . . ? O27 V5 V6 O6 0.17(13) . . . . ? O5 V5 V6 O11 90.14(14) . . . . ? O12 V5 V6 O11 178.95(16) . . . . ? O24 V5 V6 O11 -21.38(14) . . . . ? O26 V5 V6 O11 -156.41(15) . . . . ? O27 V5 V6 O11 -91.54(14) . . . . ? O5 V5 V6 O12 -88.81(14) . . . . ? O11 V5 V6 O12 -178.95(16) . . . . ? O24 V5 V6 O12 159.67(14) . . . . ? O26 V5 V6 O12 24.64(14) . . . . ? O27 V5 V6 O12 89.51(13) . . . . ? O5 V5 V6 O18 72.58(12) . . . . ? O11 V5 V6 O18 -17.56(14) . . . . ? O12 V5 V6 O18 161.39(14) . . . . ? O24 V5 V6 O18 -38.94(13) . . . . ? O26 V5 V6 O18 -173.97(13) . . . . ? O27 V5 V6 O18 -109.10(12) . . . . ? O5 V5 V6 O16 -69.03(13) . . . . ? O11 V5 V6 O16 -159.18(15) . . . . ? O12 V5 V6 O16 19.78(14) . . . . ? O24 V5 V6 O16 179.45(13) . . . . ? O26 V5 V6 O16 44.42(14) . . . . ? O27 V5 V6 O16 109.28(12) . . . . ? O5 V5 V6 O1 1.43(10) . . . . ? O11 V5 V6 O1 -88.72(13) . . . . ? O12 V5 V6 O1 90.24(12) . . . . ? O24 V5 V6 O1 -110.10(10) . . . . ? O26 V5 V6 O1 114.88(11) . . . . ? O27 V5 V6 O1 179.74(9) . . . . ? O8 V1 O1 V6 -140.53(13) . . . . ? O7 V1 O1 V6 138.04(14) . . . . ? O15 V1 O1 V6 45.27(16) . . . . ? O17 V1 O1 V6 -46.81(15) . . . . ? O13 V1 O1 V6 6.4(13) . . . . ? V2 V1 O1 V6 178.34(11) . . . . ? O6 V6 O1 V1 -4.4(14) . . . . ? O11 V6 O1 V1 141.24(16) . . . . ? O12 V6 O1 V1 -140.63(16) . . . . ? O18 V6 O1 V1 48.23(15) . . . . ? O16 V6 O1 V1 -45.70(16) . . . . ? V5 V6 O1 V1 -179.92(15) . . . . ? O10 V3 O3 V2 140.60(13) . . . . ? O9 V3 O3 V2 -139.54(13) . . . . ? O22 V3 O3 V2 -45.21(15) . . . . ? O20 V3 O3 V2 46.50(15) . . . . ? O14 V3 O3 V2 -3.9(11) . . . . ? V4 V3 O3 V2 -179.15(11) . . . . ? O2 V2 O3 V3 -14(2) . . . . ? O7 V2 O3 V3 -139.62(15) . . . . ? O8 V2 O3 V3 140.97(15) . . . . ? O19 V2 O3 V3 -44.67(15) . . . . ? O21 V2 O3 V3 48.62(15) . . . . ? V1 V2 O3 V3 -179.50(14) . . . . ? O11 V5 O5 V4 -137.76(14) . . . . ? O12 V5 O5 V4 141.60(14) . . . . ? O24 V5 O5 V4 -45.53(16) . . . . ? O26 V5 O5 V4 46.36(16) . . . . ? O27 V5 O5 V4 13.1(8) . . . . ? V6 V5 O5 V4 -178.04(11) . . . . ? O4 V4 O5 V5 -13.0(13) . . . . ? O9 V4 O5 V5 140.13(16) . . . . ? O10 V4 O5 V5 -141.53(16) . . . . ? O23 V4 O5 V5 47.79(16) . . . . ? O25 V4 O5 V5 -47.20(16) . . . . ? V3 V4 O5 V5 179.23(15) . . . . ? O2 V2 O7 C9A -59.0(5) . . . . ? O8 V2 O7 C9A -155.8(5) . . . . ? O19 V2 O7 C9A 38.1(5) . . . . ? O21 V2 O7 C9A 145.0(5) . . . . ? O3 V2 O7 C9A 118.8(5) . . . . ? V1 V2 O7 C9A -152.7(5) . . . . ? O2 V2 O7 C9 -113.6(7) . . . . ? O8 V2 O7 C9 149.6(7) . . . . ? O19 V2 O7 C9 -16.4(7) . . . . ? O21 V2 O7 C9 90.5(7) . . . . ? O3 V2 O7 C9 64.3(7) . . . . ? V1 V2 O7 C9 152.8(7) . . . . ? O2 V2 O7 V1 93.67(11) . . . . ? O8 V2 O7 V1 -3.14(9) . . . . ? O19 V2 O7 V1 -169.20(10) . . . . ? O21 V2 O7 V1 -62.3(3) . . . . ? O3 V2 O7 V1 -88.49(9) . . . . ? O1 V1 O7 C9A -103.6(5) . . . . ? O8 V1 O7 C9A 153.4(5) . . . . ? O15 V1 O7 C9A -7.2(5) . . . . ? O17 V1 O7 C9A 92.7(6) . . . . ? O13 V1 O7 C9A 72.7(5) . . . . ? V2 V1 O7 C9A 150.2(5) . . . . ? O1 V1 O7 C9 -49.5(6) . . . . ? O8 V1 O7 C9 -152.4(6) . . . . ? O15 V1 O7 C9 46.9(6) . . . . ? O17 V1 O7 C9 146.8(6) . . . . ? O13 V1 O7 C9 126.8(6) . . . . ? V2 V1 O7 C9 -155.6(6) . . . . ? O1 V1 O7 V2 106.13(11) . . . . ? O8 V1 O7 V2 3.15(9) . . . . ? O15 V1 O7 V2 -157.46(10) . . . . ? O17 V1 O7 V2 -57.6(3) . . . . ? O13 V1 O7 V2 -77.58(10) . . . . ? O1 V1 O8 C7 112.8(2) . . . . ? O7 V1 O8 C7 -147.5(2) . . . . ? O15 V1 O8 C7 -83.0(3) . . . . ? O17 V1 O8 C7 17.3(2) . . . . ? O13 V1 O8 C7 -64.5(2) . . . . ? V2 V1 O8 C7 -144.3(3) . . . . ? O1 V1 O8 V2 -102.84(11) . . . . ? O7 V1 O8 V2 -3.15(9) . . . . ? O15 V1 O8 V2 61.3(3) . . . . ? O17 V1 O8 V2 161.63(10) . . . . ? O13 V1 O8 V2 79.89(10) . . . . ? O2 V2 O8 C7 52.0(2) . . . . ? O7 V2 O8 C7 150.2(2) . . . . ? O19 V2 O8 C7 -147.8(3) . . . . ? O21 V2 O8 C7 -45.8(2) . . . . ? O3 V2 O8 C7 -126.9(2) . . . . ? V1 V2 O8 C7 147.1(2) . . . . ? O2 V2 O8 V1 -95.12(11) . . . . ? O7 V2 O8 V1 3.16(9) . . . . ? O19 V2 O8 V1 65.1(3) . . . . ? O21 V2 O8 V1 167.15(9) . . . . ? O3 V2 O8 V1 86.01(9) . . . . ? O4 V4 O9 C15 51.3(3) . . . . ? O10 V4 O9 C15 149.7(3) . . . . ? O23 V4 O9 C15 -45.2(3) . . . . ? O25 V4 O9 C15 -155.4(4) . . . . ? O5 V4 O9 C15 -126.1(3) . . . . ? V3 V4 O9 C15 148.1(3) . . . . ? O4 V4 O9 V3 -96.79(13) . . . . ? O10 V4 O9 V3 1.54(10) . . . . ? O23 V4 O9 V3 166.70(11) . . . . ? O25 V4 O9 V3 56.5(4) . . . . ? O5 V4 O9 V3 85.74(10) . . . . ? O3 V3 O9 C15 111.4(3) . . . . ? O10 V3 O9 C15 -147.8(3) . . . . ? O22 V3 O9 C15 15.6(3) . . . . ? O20 V3 O9 C15 -87.5(4) . . . . ? O14 V3 O9 C15 -64.5(3) . . . . ? V4 V3 O9 C15 -146.3(3) . . . . ? O3 V3 O9 V4 -102.34(11) . . . . ? O10 V3 O9 V4 -1.54(10) . . . . ? O22 V3 O9 V4 161.84(10) . . . . ? O20 V3 O9 V4 58.8(3) . . . . ? O14 V3 O9 V4 81.83(11) . . . . ? O3 V3 O10 C17A -109.5(8) . . . . ? O9 V3 O10 C17A 150.7(8) . . . . ? O22 V3 O10 C17A 88.7(9) . . . . ? O20 V3 O10 C17A -13.0(8) . . . . ? O14 V3 O10 C17A 67.1(8) . . . . ? V4 V3 O10 C17A 149.2(8) . . . . ? O3 V3 O10 C17 -57.8(6) . . . . ? O9 V3 O10 C17 -157.7(6) . . . . ? O22 V3 O10 C17 140.3(6) . . . . ? O20 V3 O10 C17 38.6(6) . . . . ? O14 V3 O10 C17 118.7(6) . . . . ? V4 V3 O10 C17 -159.2(6) . . . . ? O3 V3 O10 V4 101.38(11) . . . . ? O9 V3 O10 V4 1.53(10) . . . . ? O22 V3 O10 V4 -60.4(3) . . . . ? O20 V3 O10 V4 -162.16(10) . . . . ? O14 V3 O10 V4 -82.09(12) . . . . ? O4 V4 O10 C17A -55.5(8) . . . . ? O9 V4 O10 C17A -152.7(8) . . . . ? O23 V4 O10 C17A 151.3(8) . . . . ? O25 V4 O10 C17A 39.5(8) . . . . ? O5 V4 O10 C17A 120.1(8) . . . . ? V3 V4 O10 C17A -151.2(8) . . . . ? O4 V4 O10 C17 -106.7(7) . . . . ? O9 V4 O10 C17 156.1(7) . . . . ? O23 V4 O10 C17 100.1(7) . . . . ? O25 V4 O10 C17 -11.7(7) . . . . ? O5 V4 O10 C17 68.9(7) . . . . ? V3 V4 O10 C17 157.6(7) . . . . ? O4 V4 O10 V3 95.65(14) . . . . ? O9 V4 O10 V3 -1.54(10) . . . . ? O23 V4 O10 V3 -57.5(4) . . . . ? O25 V4 O10 V3 -169.34(11) . . . . ? O5 V4 O10 V3 -88.75(10) . . . . ? O5 V5 O11 C11A 104.1(6) . . . . ? O12 V5 O11 C11A -155.1(6) . . . . ? O24 V5 O11 C11A 8.8(6) . . . . ? O26 V5 O11 C11A -88.3(6) . . . . ? O27 V5 O11 C11A -71.7(6) . . . . ? V6 V5 O11 C11A -154.4(6) . . . . ? O5 V5 O11 C11 42.3(4) . . . . ? O12 V5 O11 C11 143.1(4) . . . . ? O24 V5 O11 C11 -53.0(4) . . . . ? O26 V5 O11 C11 -150.1(4) . . . . ? O27 V5 O11 C11 -133.5(4) . . . . ? V6 V5 O11 C11 143.8(4) . . . . ? O5 V5 O11 V6 -101.49(12) . . . . ? O12 V5 O11 V6 -0.68(10) . . . . ? O24 V5 O11 V6 163.27(11) . . . . ? O26 V5 O11 V6 66.1(3) . . . . ? O27 V5 O11 V6 82.74(12) . . . . ? O6 V6 O11 C11A 58.8(5) . . . . ? O12 V6 O11 C11A 156.4(5) . . . . ? O18 V6 O11 C11A -37.8(5) . . . . ? O16 V6 O11 C11A -141.6(6) . . . . ? O1 V6 O11 C11A -118.2(5) . . . . ? V5 V6 O11 C11A 155.8(6) . . . . ? O6 V6 O11 C11 121.1(4) . . . . ? O12 V6 O11 C11 -141.2(4) . . . . ? O18 V6 O11 C11 24.5(4) . . . . ? O16 V6 O11 C11 -79.2(6) . . . . ? O1 V6 O11 C11 -55.8(4) . . . . ? V5 V6 O11 C11 -141.9(5) . . . . ? O6 V6 O11 V5 -96.99(15) . . . . ? O12 V6 O11 V5 0.68(10) . . . . ? O18 V6 O11 V5 166.44(11) . . . . ? O16 V6 O11 V5 62.7(4) . . . . ? O1 V6 O11 V5 86.08(11) . . . . ? O5 V5 O12 C13 -101.6(4) . . . . ? O11 V5 O12 C13 156.5(4) . . . . ? O24 V5 O12 C13 100.2(5) . . . . ? O26 V5 O12 C13 -5.6(4) . . . . ? O27 V5 O12 C13 71.6(4) . . . . ? V6 V5 O12 C13 155.8(5) . . . . ? O5 V5 O12 V6 102.54(12) . . . . ? O11 V5 O12 V6 0.67(10) . . . . ? O24 V5 O12 V6 -55.6(3) . . . . ? O26 V5 O12 V6 -161.48(11) . . . . ? O27 V5 O12 V6 -84.28(12) . . . . ? O6 V6 O12 C13 -59.0(4) . . . . ? O11 V6 O12 C13 -158.6(4) . . . . ? O18 V6 O12 C13 147.3(4) . . . . ? O16 V6 O12 C13 36.8(4) . . . . ? O1 V6 O12 C13 117.2(4) . . . . ? V5 V6 O12 C13 -157.9(4) . . . . ? O6 V6 O12 V5 98.90(13) . . . . ? O11 V6 O12 V5 -0.67(10) . . . . ? O18 V6 O12 V5 -54.8(4) . . . . ? O16 V6 O12 V5 -165.25(10) . . . . ? O1 V6 O12 V5 -84.85(10) . . . . ? O1 V1 O13 C1 3.0(14) . . . . ? O8 V1 O13 C1 150.6(4) . . . . ? O7 V1 O13 C1 -129.2(4) . . . . ? O15 V1 O13 C1 -36.2(4) . . . . ? O17 V1 O13 C1 56.7(4) . . . . ? V2 V1 O13 C1 -169.1(4) . . . . ? O3 V3 O14 C5 -37.4(18) . . . . ? O10 V3 O14 C5 177.5(14) . . . . ? O9 V3 O14 C5 99.0(14) . . . . ? O22 V3 O14 C5 4.5(14) . . . . ? O20 V3 O14 C5 -88.3(14) . . . . ? V4 V3 O14 C5 138.0(14) . . . . ? O3 V3 O14 C5A 64(2) . . . . ? O10 V3 O14 C5A -81.2(17) . . . . ? O9 V3 O14 C5A -159.7(17) . . . . ? O22 V3 O14 C5A 105.7(17) . . . . ? O20 V3 O14 C5A 12.9(17) . . . . ? V4 V3 O14 C5A -120.7(17) . . . . ? O1 V1 O15 C19 -14.3(3) . . . . ? O8 V1 O15 C19 -178.9(3) . . . . ? O7 V1 O15 C19 -116.6(3) . . . . ? O17 V1 O15 C19 80.6(3) . . . . ? O13 V1 O15 C19 162.6(3) . . . . ? V2 V1 O15 C19 -134.4(2) . . . . ? O6 V6 O16 C19 -158.6(4) . . . . ? O11 V6 O16 C19 41.4(6) . . . . ? O12 V6 O16 C19 101.2(4) . . . . ? O18 V6 O16 C19 -62.3(4) . . . . ? O1 V6 O16 C19 17.8(4) . . . . ? V5 V6 O16 C19 88.8(4) . . . . ? O1 V1 O17 C26 11.8(3) . . . . ? O8 V1 O17 C26 117.0(2) . . . . ? O7 V1 O17 C26 175.9(3) . . . . ? O15 V1 O17 C26 -84.3(3) . . . . ? O13 V1 O17 C26 -164.2(3) . . . . ? V2 V1 O17 C26 132.0(2) . . . . ? O6 V6 O18 C26 158.8(3) . . . . ? O11 V6 O18 C26 -99.6(3) . . . . ? O12 V6 O18 C26 -47.2(5) . . . . ? O16 V6 O18 C26 63.5(3) . . . . ? O1 V6 O18 C26 -16.9(3) . . . . ? V5 V6 O18 C26 -88.7(3) . . . . ? O2 V2 O19 C33 -162.8(3) . . . . ? O7 V2 O19 C33 97.0(3) . . . . ? O8 V2 O19 C33 36.8(6) . . . . ? O21 V2 O19 C33 -65.1(3) . . . . ? O3 V2 O19 C33 15.8(3) . . . . ? V1 V2 O19 C33 87.7(3) . . . . ? O3 V3 O20 C33 -19.4(3) . . . . ? O10 V3 O20 C33 -122.7(3) . . . . ? O9 V3 O20 C33 179(17) . . . . ? O22 V3 O20 C33 75.8(3) . . . . ? O14 V3 O20 C33 156.0(3) . . . . ? V4 V3 O20 C33 -137.1(2) . . . . ? O2 V2 O21 C40 158.0(3) . . . . ? O7 V2 O21 C40 -45.9(5) . . . . ? O8 V2 O21 C40 -103.2(3) . . . . ? O19 V2 O21 C40 61.3(3) . . . . ? O3 V2 O21 C40 -19.6(3) . . . . ? V1 V2 O21 C40 -92.7(3) . . . . ? O3 V3 O22 C40 8.6(2) . . . . ? O10 V3 O22 C40 170.8(3) . . . . ? O9 V3 O22 C40 111.1(2) . . . . ? O20 V3 O22 C40 -87.2(2) . . . . ? O14 V3 O22 C40 -167.5(3) . . . . ? V4 V3 O22 C40 125.7(2) . . . . ? O4 V4 O23 C54 157.0(3) . . . . ? O9 V4 O23 C54 -103.8(3) . . . . ? O10 V4 O23 C54 -49.5(5) . . . . ? O25 V4 O23 C54 62.2(3) . . . . ? O5 V4 O23 C54 -18.1(3) . . . . ? V3 V4 O23 C54 -93.0(3) . . . . ? O5 V5 O24 C54 10.1(3) . . . . ? O11 V5 O24 C54 114.4(3) . . . . ? O12 V5 O24 C54 168.8(3) . . . . ? O26 V5 O24 C54 -84.9(3) . . . . ? O27 V5 O24 C54 -162.4(3) . . . . ? V6 V5 O24 C54 127.6(3) . . . . ? O4 V4 O25 C47 -155.8(4) . . . . ? O9 V4 O25 C47 50.6(6) . . . . ? O10 V4 O25 C47 103.9(4) . . . . ? O23 V4 O25 C47 -59.4(4) . . . . ? O5 V4 O25 C47 21.0(4) . . . . ? V3 V4 O25 C47 95.0(4) . . . . ? O5 V5 O26 C47 -16.4(3) . . . . ? O11 V5 O26 C47 175.7(3) . . . . ? O12 V5 O26 C47 -120.1(3) . . . . ? O24 V5 O26 C47 78.6(3) . . . . ? O27 V5 O26 C47 158.8(3) . . . . ? V6 V5 O26 C47 -135.3(3) . . . . ? O5 V5 O27 C3 -33.3(10) . . . . ? O11 V5 O27 C3 118.3(5) . . . . ? O12 V5 O27 C3 -163.1(5) . . . . ? O24 V5 O27 C3 26.2(5) . . . . ? O26 V5 O27 C3 -67.3(5) . . . . ? V6 V5 O27 C3 157.4(5) . . . . ? V1 O13 C1 C2 -109.2(5) . . . . ? V1 O8 C7 C8 -105.1(3) . . . . ? V2 O8 C7 C8 116.8(3) . . . . ? C9A O7 C9 C10 -9.6(8) . . . . ? V2 O7 C9 C10 88.3(9) . . . . ? V1 O7 C9 C10 -123.9(7) . . . . ? V4 O9 C15 C16 117.2(3) . . . . ? V3 O9 C15 C16 -102.5(4) . . . . ? C17A O10 C17 C18 -7.5(8) . . . . ? V3 O10 C17 C18 -117.4(7) . . . . ? V4 O10 C17 C18 89.4(7) . . . . ? V6 O16 C19 O15 1.4(6) . . . . ? V6 O16 C19 C20 -177.2(3) . . . . ? V1 O15 C19 O16 -7.6(5) . . . . ? V1 O15 C19 C20 171.0(2) . . . . ? O16 C19 C20 C25 -17.9(5) . . . . ? O15 C19 C20 C25 163.4(3) . . . . ? O16 C19 C20 C21 159.5(3) . . . . ? O15 C19 C20 C21 -19.2(5) . . . . ? C25 C20 C21 C22 1.9(6) . . . . ? C19 C20 C21 C22 -175.5(3) . . . . ? C20 C21 C22 C23 -2.4(6) . . . . ? C21 C22 C23 C24 0.5(7) . . . . ? C22 C23 C24 C25 1.9(8) . . . . ? C23 C24 C25 C20 -2.4(7) . . . . ? C21 C20 C25 C24 0.5(6) . . . . ? C19 C20 C25 C24 177.9(4) . . . . ? V6 O18 C26 O17 -5.9(5) . . . . ? V6 O18 C26 C27 174.0(2) . . . . ? V1 O17 C26 O18 13.0(4) . . . . ? V1 O17 C26 C27 -166.97(18) . . . . ? O18 C26 C27 C28 178.6(3) . . . . ? O17 C26 C27 C28 -1.5(4) . . . . ? O18 C26 C27 C32 -1.7(4) . . . . ? O17 C26 C27 C32 178.3(3) . . . . ? C32 C27 C28 C29 1.3(5) . . . . ? C26 C27 C28 C29 -179.0(3) . . . . ? C27 C28 C29 C30 -0.3(6) . . . . ? C28 C29 C30 C31 -0.7(6) . . . . ? C29 C30 C31 C32 0.8(6) . . . . ? C30 C31 C32 C27 0.2(5) . . . . ? C28 C27 C32 C31 -1.2(5) . . . . ? C26 C27 C32 C31 179.0(3) . . . . ? V2 O19 C33 O20 0.6(6) . . . . ? V2 O19 C33 C34 179.9(2) . . . . ? V3 O20 C33 O19 -2.0(4) . . . . ? V3 O20 C33 C34 178.6(2) . . . . ? O19 C33 C34 C35 177.6(3) . . . . ? O20 C33 C34 C35 -3.0(5) . . . . ? O19 C33 C34 C39 -4.7(5) . . . . ? O20 C33 C34 C39 174.7(3) . . . . ? C39 C34 C35 C36 2.2(7) . . . . ? C33 C34 C35 C36 179.9(4) . . . . ? C34 C35 C36 C37 -0.4(9) . . . . ? C35 C36 C37 C38 -1.5(10) . . . . ? C36 C37 C38 C39 1.5(9) . . . . ? C35 C34 C39 C38 -2.2(6) . . . . ? C33 C34 C39 C38 -179.8(4) . . . . ? C37 C38 C39 C34 0.3(8) . . . . ? V2 O21 C40 O22 -4.2(5) . . . . ? V2 O21 C40 C41 174.4(2) . . . . ? V3 O22 C40 O21 15.3(4) . . . . ? V3 O22 C40 C41 -163.31(19) . . . . ? O21 C40 C41 C46 -7.3(4) . . . . ? O22 C40 C41 C46 171.4(3) . . . . ? O21 C40 C41 C42 174.2(3) . . . . ? O22 C40 C41 C42 -7.1(4) . . . . ? C46 C41 C42 C43 0.3(5) . . . . ? C40 C41 C42 C43 178.9(3) . . . . ? C41 C42 C43 C44 -1.6(5) . . . . ? C42 C43 C44 C45 1.8(6) . . . . ? C43 C44 C45 C46 -0.7(6) . . . . ? C44 C45 C46 C41 -0.6(6) . . . . ? C42 C41 C46 C45 0.8(5) . . . . ? C40 C41 C46 C45 -177.7(3) . . . . ? V4 O25 C47 O26 -4.0(6) . . . . ? V4 O25 C47 C48 175.7(3) . . . . ? V5 O26 C47 O25 -3.2(5) . . . . ? V5 O26 C47 C48 177.1(2) . . . . ? O25 C47 C48 C53 6.2(5) . . . . ? O26 C47 C48 C53 -174.0(3) . . . . ? O25 C47 C48 C49 -170.7(4) . . . . ? O26 C47 C48 C49 9.0(5) . . . . ? C53 C48 C49 C50 0.1(7) . . . . ? C47 C48 C49 C50 177.1(4) . . . . ? C48 C49 C50 C51 0.5(9) . . . . ? C49 C50 C51 C52 -0.5(11) . . . . ? C50 C51 C52 C53 -0.2(10) . . . . ? C49 C48 C53 C52 -0.8(7) . . . . ? C47 C48 C53 C52 -177.7(4) . . . . ? C51 C52 C53 C48 0.8(9) . . . . ? V4 O23 C54 O24 -4.6(6) . . . . ? V4 O23 C54 C55 174.8(2) . . . . ? V5 O24 C54 O23 13.5(5) . . . . ? V5 O24 C54 C55 -165.9(2) . . . . ? O23 C54 C55 C60 -8.4(4) . . . . ? O24 C54 C55 C60 171.0(3) . . . . ? O23 C54 C55 C56 172.0(3) . . . . ? O24 C54 C55 C56 -8.5(4) . . . . ? C60 C55 C56 C57 1.1(5) . . . . ? C54 C55 C56 C57 -179.3(3) . . . . ? C55 C56 C57 C58 -0.6(6) . . . . ? C56 C57 C58 C59 -0.4(6) . . . . ? C57 C58 C59 C60 0.9(6) . . . . ? C58 C59 C60 C55 -0.3(6) . . . . ? C56 C55 C60 C59 -0.7(5) . . . . ? C54 C55 C60 C59 179.7(3) . . . . ? C9 O7 C9A C10A -14.0(7) . . . . ? V2 O7 C9A C10A -130.4(6) . . . . ? V1 O7 C9A C10A 85.0(8) . . . . ? C11A O11 C11 C12 5.8(9) . . . . ? V5 O11 C11 C12 121.8(9) . . . . ? V6 O11 C11 C12 -102.6(9) . . . . ? C11 O11 C11A C12A -0.3(11) . . . . ? V5 O11 C11A C12A -101.7(11) . . . . ? V6 O11 C11A C12A 108.9(11) . . . . ? C17 O10 C17A C18A -14.6(9) . . . . ? V3 O10 C17A C18A 87.2(13) . . . . ? V4 O10 C17A C18A -129.4(9) . . . . ? C5A O14 C5 C6 129(2) . . . . ? V3 O14 C5 C6 -102.6(18) . . . . ? C5 O14 C5A C6A -47.7(17) . . . . ? V3 O14 C5A C6A 178.6(13) . . . . ? V5 O12 C13 C14 81.7(7) . . . . ? V6 O12 C13 C14 -127.0(5) . . . . ? V5 O27 C3 C4 -121.3(6) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 30.54 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.279 _refine_diff_density_min -0.896 _refine_diff_density_rms 0.083 data_orepw112p1bfinal _database_code_depnum_ccdc_archive 'CCDC 278654' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C11 H18 O8 V2' _chemical_formula_weight 380.13 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 8.269(3) _cell_length_b 10.410(4) _cell_length_c 10.932(3) _cell_angle_alpha 71.69(3) _cell_angle_beta 69.23(3) _cell_angle_gamma 80.42(3) _cell_volume 833.7(5) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3550 _cell_measurement_theta_min 2.7772 _cell_measurement_theta_max 31.9431 _exptl_crystal_description BLOCK _exptl_crystal_colour blue _exptl_crystal_size_max 0.21015 _exptl_crystal_size_mid 0.14491 _exptl_crystal_size_min 0.04276 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.514 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 388 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_T_min 0.70008 _exptl_absorpt_correction_T_max 0.88538 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8848 _diffrn_reflns_av_R_equivalents 0.0481 _diffrn_reflns_av_sigmaI/netI 0.0800 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 31.96 _reflns_number_total 5201 _reflns_number_gt 3577 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.pre23_9 beta (release 18.06.2004 CrysAlis171 .NET) (compiled Jun 18 2004,12:34:04) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. All noh-hydrogen atoms were refined anisotropically. Hydrogen atoms were calculated and placed geometrically using the riding-model and refined isotropically. ; _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^)+(0.0756P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5201 _refine_ls_number_parameters 216 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0666 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1402 _refine_ls_wR_factor_gt 0.1220 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.008 _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 1.13406(5) 0.02867(5) 0.07333(4) 0.01166(12) Uani 1 1 d . . . V2 V 0.74590(5) -0.05145(5) 0.24529(4) 0.01194(12) Uani 1 1 d . . . O3 O 0.6540(2) -0.1576(2) 0.38561(19) 0.0177(4) Uani 1 1 d . . . O5 O 0.9900(2) -0.10301(19) 0.23411(18) 0.0128(4) Uani 1 1 d . . . O4 O 1.3148(2) -0.0166(2) 0.10412(19) 0.0179(4) Uani 1 1 d . . . O8 O 0.5207(2) 0.0510(2) 0.2131(2) 0.0166(4) Uani 1 1 d . . . O7 O 0.7760(2) -0.15365(19) 0.11015(18) 0.0140(4) Uani 1 1 d . . . O6 O 1.1298(2) -0.08467(18) -0.04146(18) 0.0117(4) Uani 1 1 d . . . O1 O 1.0395(2) 0.1696(2) 0.17717(18) 0.0146(4) Uani 1 1 d . . . O2 O 0.7707(2) 0.1074(2) 0.30627(19) 0.0147(4) Uani 1 1 d . . . C2 C 0.8682(3) 0.2959(3) 0.3273(3) 0.0136(5) Uani 1 1 d . . . C8 C 1.0341(4) -0.1452(3) 0.3565(3) 0.0181(6) Uani 1 1 d . . . H8A H 1.1540 -0.1768 0.3366 0.027 Uiso 1 1 calc R . . H8B H 0.9634 -0.2172 0.4209 0.027 Uiso 1 1 calc R . . H8C H 1.0146 -0.0701 0.3942 0.027 Uiso 1 1 calc R . . C5 C 0.8150(4) 0.5095(3) 0.4429(3) 0.0238(6) Uani 1 1 d . . . H5 H 0.7974 0.5812 0.4807 0.029 Uiso 1 1 calc R . . C7 C 0.9906(4) 0.3923(3) 0.2780(3) 0.0185(6) Uani 1 1 d . . . H7 H 1.0914 0.3854 0.2064 0.022 Uiso 1 1 calc R . . C6 C 0.9632(4) 0.4977(3) 0.3347(3) 0.0236(6) Uani 1 1 d . . . H6 H 1.0452 0.5623 0.3001 0.028 Uiso 1 1 calc R . . C1 C 0.8948(3) 0.1825(3) 0.2662(3) 0.0133(5) Uani 1 1 d . . . C3 C 0.7188(3) 0.3073(3) 0.4360(3) 0.0166(5) Uani 1 1 d . . . H3 H 0.6357 0.2438 0.4697 0.020 Uiso 1 1 calc R . . C11 C 0.3856(4) 0.0887(4) 0.3232(3) 0.0257(7) Uani 1 1 d . . . H11A H 0.3360 0.0086 0.3909 0.039 Uiso 1 1 calc R . . H11B H 0.2976 0.1453 0.2897 0.039 Uiso 1 1 calc R . . H11C H 0.4327 0.1374 0.3629 0.039 Uiso 1 1 calc R . . C10 C 0.6798(4) -0.2645(3) 0.1339(3) 0.0200(6) Uani 1 1 d . . . H10A H 0.5632 -0.2326 0.1363 0.030 Uiso 1 1 calc R . . H10B H 0.6784 -0.3285 0.2194 0.030 Uiso 1 1 calc R . . H10C H 0.7326 -0.3076 0.0621 0.030 Uiso 1 1 calc R . . C4 C 0.6940(4) 0.4126(3) 0.4935(3) 0.0201(6) Uani 1 1 d . . . H4 H 0.5951 0.4186 0.5669 0.024 Uiso 1 1 calc R . . C9 C 1.1817(4) -0.2259(3) 0.0044(3) 0.0168(5) Uani 1 1 d . . . H9A H 1.2580 -0.2356 0.0559 0.025 Uiso 1 1 calc R . . H9B H 1.2406 -0.2605 -0.0729 0.025 Uiso 1 1 calc R . . H9C H 1.0810 -0.2758 0.0607 0.025 Uiso 1 1 calc R . . C2S C 0.4205(11) 0.4023(16) 0.1063(9) 0.234(8) Uani 1 1 d DU . . H2S1 H 0.3529 0.3245 0.1558 0.352 Uiso 1 1 calc R . . H2S2 H 0.5266 0.3768 0.0433 0.352 Uiso 1 1 calc R . . H2S3 H 0.3561 0.4713 0.0571 0.352 Uiso 1 1 calc R . . O2S O 0.4595(15) 0.4535(14) 0.1999(13) 0.335(7) Uani 1 1 d DU . . H8 H 0.483(5) 0.030(4) 0.176(4) 0.023(10) 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 0.0068(2) 0.0191(2) 0.0099(2) -0.00477(18) -0.00205(16) -0.00319(16) V2 0.0081(2) 0.0180(2) 0.0099(2) -0.00417(18) -0.00134(16) -0.00430(17) O3 0.0154(9) 0.0217(10) 0.0145(9) -0.0047(8) -0.0011(7) -0.0058(8) O5 0.0106(8) 0.0180(9) 0.0104(8) -0.0023(7) -0.0051(7) -0.0016(7) O4 0.0105(9) 0.0304(11) 0.0152(9) -0.0084(9) -0.0039(7) -0.0035(8) O8 0.0089(9) 0.0308(12) 0.0141(10) -0.0114(9) -0.0030(7) -0.0034(8) O7 0.0116(9) 0.0185(10) 0.0126(9) -0.0054(8) -0.0015(7) -0.0062(7) O6 0.0086(8) 0.0148(9) 0.0116(9) -0.0032(7) -0.0036(7) -0.0009(7) O1 0.0095(8) 0.0219(10) 0.0131(9) -0.0063(8) -0.0018(7) -0.0040(7) O2 0.0104(9) 0.0211(10) 0.0138(9) -0.0074(8) -0.0022(7) -0.0035(7) C2 0.0130(12) 0.0166(13) 0.0122(12) -0.0032(10) -0.0055(10) -0.0016(10) C8 0.0182(13) 0.0234(14) 0.0137(13) -0.0003(11) -0.0089(10) -0.0044(11) C5 0.0309(16) 0.0184(14) 0.0250(16) -0.0082(12) -0.0114(13) 0.0006(12) C7 0.0169(13) 0.0196(14) 0.0168(13) -0.0037(11) -0.0017(11) -0.0062(11) C6 0.0249(15) 0.0205(15) 0.0239(15) -0.0031(12) -0.0054(12) -0.0089(12) C1 0.0132(12) 0.0181(13) 0.0098(11) -0.0030(10) -0.0059(9) -0.0010(10) C3 0.0107(12) 0.0205(14) 0.0174(13) -0.0038(11) -0.0044(10) -0.0007(10) C11 0.0141(14) 0.044(2) 0.0232(15) -0.0186(15) -0.0063(12) 0.0054(13) C10 0.0204(14) 0.0208(14) 0.0201(14) -0.0068(12) -0.0025(11) -0.0109(11) C4 0.0167(13) 0.0241(15) 0.0201(14) -0.0093(12) -0.0066(11) 0.0053(11) C9 0.0167(13) 0.0181(13) 0.0156(13) -0.0027(11) -0.0074(10) 0.0002(11) C2S 0.085(6) 0.51(3) 0.101(7) -0.084(11) 0.004(5) -0.089(11) O2S 0.346(15) 0.430(17) 0.339(15) -0.261(14) -0.082(11) -0.083(13) _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 O4 1.610(2) . ? V1 O7 1.973(2) 2_755 ? V1 O5 1.983(2) . ? V1 O6 1.986(2) . ? V1 O1 2.022(2) . ? V1 O6 2.2825(19) 2_755 ? V2 O3 1.593(2) . ? V2 O5 1.9701(19) . ? V2 O7 2.004(2) . ? V2 O2 2.030(2) . ? V2 O8 2.073(2) . ? V2 O6 2.215(2) 2_755 ? O5 C8 1.428(3) . ? O8 C11 1.431(3) . ? O8 H8 0.69(4) . ? O7 C10 1.415(3) . ? O7 V1 1.973(2) 2_755 ? O6 C9 1.441(3) . ? O6 V2 2.215(2) 2_755 ? O6 V1 2.2825(19) 2_755 ? O1 C1 1.265(3) . ? O2 C1 1.261(3) . ? C2 C7 1.391(4) . ? C2 C3 1.397(4) . ? C2 C1 1.481(4) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C5 C4 1.385(4) . ? C5 C6 1.388(4) . ? C5 H5 0.9300 . ? C7 C6 1.372(4) . ? C7 H7 0.9300 . ? C6 H6 0.9300 . ? C3 C4 1.380(4) . ? C3 H3 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C4 H4 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C2S O2S 1.438(8) . ? C2S H2S1 0.9600 . ? C2S H2S2 0.9600 . ? C2S H2S3 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 O4 V1 O7 98.16(9) . 2_755 ? O4 V1 O5 97.32(9) . . ? O7 V1 O5 162.39(8) 2_755 . ? O4 V1 O6 104.83(10) . . ? O7 V1 O6 79.31(8) 2_755 . ? O5 V1 O6 88.65(8) . . ? O4 V1 O1 99.82(9) . . ? O7 V1 O1 97.82(8) 2_755 . ? O5 V1 O1 87.75(8) . . ? O6 V1 O1 155.34(8) . . ? O4 V1 O6 176.73(8) . 2_755 ? O7 V1 O6 85.11(8) 2_755 2_755 ? O5 V1 O6 79.44(7) . 2_755 ? O6 V1 O6 75.62(8) . 2_755 ? O1 V1 O6 79.74(7) . 2_755 ? O3 V2 O5 99.47(10) . . ? O3 V2 O7 101.89(10) . . ? O5 V2 O7 88.61(8) . . ? O3 V2 O2 102.66(9) . . ? O5 V2 O2 86.06(8) . . ? O7 V2 O2 155.41(8) . . ? O3 V2 O8 96.57(10) . . ? O5 V2 O8 163.49(8) . . ? O7 V2 O8 91.89(9) . . ? O2 V2 O8 86.66(8) . . ? O3 V2 O6 175.21(9) . 2_755 ? O5 V2 O6 81.40(8) . 2_755 ? O7 V2 O6 73.39(8) . 2_755 ? O2 V2 O6 82.08(8) . 2_755 ? O8 V2 O6 82.93(8) . 2_755 ? C8 O5 V2 118.94(16) . . ? C8 O5 V1 118.84(16) . . ? V2 O5 V1 107.46(9) . . ? C11 O8 V2 119.45(18) . . ? C11 O8 H8 108(3) . . ? V2 O8 H8 119(3) . . ? C10 O7 V1 121.56(17) . 2_755 ? C10 O7 V2 125.04(16) . . ? V1 O7 V2 107.46(9) 2_755 . ? C9 O6 V1 115.06(16) . . ? C9 O6 V2 124.63(16) . 2_755 ? V1 O6 V2 99.37(8) . 2_755 ? C9 O6 V1 118.71(15) . 2_755 ? V1 O6 V1 104.38(8) . 2_755 ? V2 O6 V1 90.24(7) 2_755 2_755 ? C1 O1 V1 130.83(18) . . ? C1 O2 V2 130.64(18) . . ? C7 C2 C3 118.9(3) . . ? C7 C2 C1 120.9(2) . . ? C3 C2 C1 120.2(2) . . ? O5 C8 H8A 109.5 . . ? O5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C5 C6 118.9(3) . . ? C4 C5 H5 120.5 . . ? C6 C5 H5 120.5 . . ? C6 C7 C2 120.2(3) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C7 C6 C5 121.1(3) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? O2 C1 O1 125.3(3) . . ? O2 C1 C2 117.3(2) . . ? O1 C1 C2 117.4(2) . . ? C4 C3 C2 120.3(3) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? O8 C11 H11A 109.5 . . ? O8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? O8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O7 C10 H10A 109.5 . . ? O7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? O7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? O6 C9 H9A 109.5 . . ? O6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? O6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 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 O3 V2 O5 C8 -35.9(2) . . . . ? O7 V2 O5 C8 -137.67(19) . . . . ? O2 V2 O5 C8 66.35(19) . . . . ? O8 V2 O5 C8 130.4(3) . . . . ? O6 V2 O5 C8 148.92(19) 2_755 . . . ? O3 V2 O5 V1 -174.59(10) . . . . ? O7 V2 O5 V1 83.59(10) . . . . ? O2 V2 O5 V1 -72.39(10) . . . . ? O8 V2 O5 V1 -8.4(3) . . . . ? O6 V2 O5 V1 10.18(8) 2_755 . . . ? O4 V1 O5 C8 30.9(2) . . . . ? O7 V1 O5 C8 -177.8(2) 2_755 . . . ? O6 V1 O5 C8 135.66(19) . . . . ? O1 V1 O5 C8 -68.74(19) . . . . ? O6 V1 O5 C8 -148.72(19) 2_755 . . . ? O4 V1 O5 V2 169.67(10) . . . . ? O7 V1 O5 V2 -39.0(3) 2_755 . . . ? O6 V1 O5 V2 -85.55(10) . . . . ? O1 V1 O5 V2 70.05(10) . . . . ? O6 V1 O5 V2 -9.93(8) 2_755 . . . ? O3 V2 O8 C11 45.4(2) . . . . ? O5 V2 O8 C11 -121.0(3) . . . . ? O7 V2 O8 C11 147.6(2) . . . . ? O2 V2 O8 C11 -57.0(2) . . . . ? O6 V2 O8 C11 -139.4(2) 2_755 . . . ? O3 V2 O7 C10 20.9(2) . . . . ? O5 V2 O7 C10 120.3(2) . . . . ? O2 V2 O7 C10 -162.3(2) . . . . ? O8 V2 O7 C10 -76.2(2) . . . . ? O6 V2 O7 C10 -158.2(2) 2_755 . . . ? O3 V2 O7 V1 173.87(9) . . . 2_755 ? O5 V2 O7 V1 -86.74(10) . . . 2_755 ? O2 V2 O7 V1 -9.3(2) . . . 2_755 ? O8 V2 O7 V1 76.75(10) . . . 2_755 ? O6 V2 O7 V1 -5.29(7) 2_755 . . 2_755 ? O4 V1 O6 C9 44.80(18) . . . . ? O7 V1 O6 C9 140.50(17) 2_755 . . . ? O5 V1 O6 C9 -52.42(17) . . . . ? O1 V1 O6 C9 -134.1(2) . . . . ? O6 V1 O6 C9 -131.86(19) 2_755 . . . ? O4 V1 O6 V2 -90.67(10) . . . 2_755 ? O7 V1 O6 V2 5.03(7) 2_755 . . 2_755 ? O5 V1 O6 V2 172.11(8) . . . 2_755 ? O1 V1 O6 V2 90.48(19) . . . 2_755 ? O6 V1 O6 V2 92.67(9) 2_755 . . 2_755 ? O4 V1 O6 V1 176.66(9) . . . 2_755 ? O7 V1 O6 V1 -87.64(9) 2_755 . . 2_755 ? O5 V1 O6 V1 79.44(8) . . . 2_755 ? O1 V1 O6 V1 -2.2(2) . . . 2_755 ? O6 V1 O6 V1 0.0 2_755 . . 2_755 ? O4 V1 O1 C1 -127.6(2) . . . . ? O7 V1 O1 C1 132.6(2) 2_755 . . . ? O5 V1 O1 C1 -30.6(2) . . . . ? O6 V1 O1 C1 51.2(3) . . . . ? O6 V1 O1 C1 49.1(2) 2_755 . . . ? O3 V2 O2 C1 138.4(2) . . . . ? O5 V2 O2 C1 39.5(2) . . . . ? O7 V2 O2 C1 -38.4(3) . . . . ? O8 V2 O2 C1 -125.6(2) . . . . ? O6 V2 O2 C1 -42.3(2) 2_755 . . . ? C3 C2 C7 C6 -0.8(4) . . . . ? C1 C2 C7 C6 179.2(3) . . . . ? C2 C7 C6 C5 0.9(5) . . . . ? C4 C5 C6 C7 0.0(5) . . . . ? V2 O2 C1 O1 -2.5(4) . . . . ? V2 O2 C1 C2 176.81(16) . . . . ? V1 O1 C1 O2 -3.0(4) . . . . ? V1 O1 C1 C2 177.66(17) . . . . ? C7 C2 C1 O2 -172.7(3) . . . . ? C3 C2 C1 O2 7.3(4) . . . . ? C7 C2 C1 O1 6.7(4) . . . . ? C3 C2 C1 O1 -173.3(2) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C1 C2 C3 C4 179.8(2) . . . . ? C2 C3 C4 C5 1.2(4) . . . . ? C6 C5 C4 C3 -1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.900 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.138 _refine_diff_density_min -1.147 _refine_diff_density_rms 0.245