# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global #TrackingRef '- Compound 2.CIF' _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Wolfgang Schmitt' _publ_contact_author_email schmittw@tcd.ie _publ_author_name 'Wolfgang Schmitt' data_2 _database_code_depnum_ccdc_archive 'CCDC 820349' #TrackingRef '- Compound 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H106 As4 N6 Na9 O59 V5' _chemical_formula_weight 2448.65 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.026(4) _cell_length_b 23.202(5) _cell_length_c 26.312(9) _cell_angle_alpha 90.00 _cell_angle_beta 121.29(2) _cell_angle_gamma 90.00 _cell_volume 9404(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8736 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 27.47 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.730 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4968 _exptl_absorpt_coefficient_mu 2.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.622 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn 724' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 73662 _diffrn_reflns_av_R_equivalents 0.0505 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 25.00 _reflns_number_total 16358 _reflns_number_gt 13866 _reflns_threshold_expression >2sigma(I) _computing_data_collection Crystalclear _computing_cell_refinement Crystalclear _computing_data_reduction Crystalclear _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. The wR2 value of the dataset is relatively high due to a large number of disordered constitutional solvent molecules. ; _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^)+(0.3560P)^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 16358 _refine_ls_number_parameters 1163 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1268 _refine_ls_R_factor_gt 0.0929 _refine_ls_wR_factor_ref 0.3785 _refine_ls_wR_factor_gt 0.3066 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.021 _refine_ls_shift/su_mean 0.001 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 As1 As 0.78331(5) 0.35067(3) 0.03633(3) 0.0162(3) Uani 1 1 d . . . As3 As 1.07348(5) 0.36254(3) -0.13651(4) 0.0165(3) Uani 1 1 d . . . As4 As 0.69904(5) 0.35663(3) -0.21409(3) 0.0164(3) Uani 1 1 d . . . As2 As 1.15645(5) 0.37732(3) 0.11312(3) 0.0183(3) Uani 1 1 d . . . V3 V 0.89393(8) 0.30322(5) -0.16219(6) 0.0162(3) Uani 1 1 d . . . V5 V 0.93896(8) 0.25664(5) -0.04727(5) 0.0160(3) Uani 1 1 d . . . V1 V 0.97280(8) 0.30816(5) 0.06352(6) 0.0170(3) Uani 1 1 d . . . V4 V 0.76510(8) 0.29595(6) -0.08509(6) 0.0173(3) Uani 1 1 d . . . V2 V 1.10186(8) 0.31325(6) -0.01239(6) 0.0199(4) Uani 1 1 d . . . Na1 Na 1.1917(4) 0.4490(2) 0.0033(2) 0.0779(18) Uani 1 1 d . . . Na9 Na 0.6799(4) 0.4346(2) -0.1000(2) 0.0703(15) Uani 1 1 d . . . Na5 Na 0.85727(18) 0.06397(12) 0.26674(13) 0.0198(7) Uani 1 1 d . . . Na7 Na 0.6231(2) 0.03310(13) 0.16599(14) 0.0240(7) Uani 1 1 d . . . Na8 Na 0.4288(2) 0.00892(14) 0.02080(15) 0.0267(7) Uani 1 1 d . . . Na10 Na 0.9115(2) 0.07783(17) 0.16093(15) 0.0339(8) Uani 1 1 d . . . Na6 Na 0.9760(2) 0.44012(15) 0.12254(18) 0.0363(9) Uani 1 1 d . . . Na12 Na 0.4978(2) 0.02041(16) -0.28948(19) 0.0402(9) Uani 1 1 d . . . Na13 Na 0.4001(2) 0.01393(14) 0.13666(15) 0.0273(7) Uani 1 1 d . . . N1 N 0.2066(5) -0.0906(3) 0.0107(3) 0.0293(16) Uani 1 1 d . . . N2 N 0.3924(5) 0.1621(3) 0.0628(3) 0.0327(17) Uani 1 1 d . . . N3 N 0.5299(5) -0.1322(3) 0.1618(3) 0.0263(16) Uani 1 1 d . . . N10 N 0.1632(5) 0.1139(3) 0.1055(4) 0.0345(18) Uani 1 1 d . . . N15 N 0.7157(5) 0.1036(3) -0.1914(4) 0.0320(17) Uani 1 1 d . . . N47 N 0.9294(7) -0.0867(4) 0.0913(5) 0.065(3) Uani 1 1 d . . . O1 O 1.0333(3) 0.2886(2) 0.0217(2) 0.0171(11) Uani 1 1 d . . . O2 O 0.9962(3) 0.2855(2) -0.0841(2) 0.0182(11) Uani 1 1 d . . . O3 O 0.8391(3) 0.2787(2) -0.1173(2) 0.0158(11) Uani 1 1 d . . . O4 O 0.8760(3) 0.2796(2) -0.0126(2) 0.0167(11) Uani 1 1 d . . . O5 O 0.9973(3) 0.2589(2) 0.1128(3) 0.0220(12) Uani 1 1 d . . . O6 O 1.1770(4) 0.2657(3) 0.0065(3) 0.0275(13) Uani 1 1 d . . . O7 O 0.8797(4) 0.2503(2) -0.2068(3) 0.0240(12) Uani 1 1 d . . . O8 O 0.7020(3) 0.2413(2) -0.1008(3) 0.0238(12) Uani 1 1 d . . . O9 O 1.0544(3) 0.3734(2) 0.1007(3) 0.0226(12) Uani 1 1 d . . . O12 O 0.9628(3) 0.3616(2) -0.1737(2) 0.0143(10) Uani 1 1 d . . . O13 O 0.7993(3) 0.3595(2) -0.2050(3) 0.0248(13) Uani 1 1 d . . . O14 O 0.7043(3) 0.3545(2) -0.1483(2) 0.0198(12) Uani 1 1 d . . . O15 O 0.7353(3) 0.3486(2) -0.0392(2) 0.0179(11) Uani 1 1 d . . . O16 O 0.8917(3) 0.3604(2) 0.0686(2) 0.0150(11) Uani 1 1 d . . . O17 O 1.3337(7) 0.1461(6) 0.3001(8) 0.141(7) Uani 1 1 d . . . O18 O 1.4304(5) 0.1535(3) 0.2719(4) 0.054(2) Uani 1 1 d . . . O19 O 0.6468(4) 0.1118(3) 0.1215(2) 0.0243(12) Uani 1 1 d . . . O20 O 0.7881(4) 0.0927(3) 0.1636(3) 0.0339(15) Uani 1 1 d . . . O21 O 0.4756(4) 0.1059(3) -0.3445(3) 0.0412(17) Uani 1 1 d . . . O22 O 0.5675(5) 0.1065(4) -0.3770(4) 0.063(3) Uani 1 1 d . . . O23 O 1.1732(4) 0.1034(3) -0.2124(3) 0.0362(15) Uani 1 1 d . . . O24 O 1.3032(4) 0.1251(3) -0.1347(3) 0.0330(15) Uani 1 1 d . . . O25 O 0.9455(3) 0.1877(2) -0.0446(2) 0.0236(12) Uani 1 1 d . . . O26 O 0.3166(4) -0.0253(3) 0.0360(3) 0.0299(14) Uani 1 1 d . . . O27 O 0.4630(4) 0.0779(3) 0.0995(3) 0.0309(14) Uani 1 1 d . . . O28 O 1.2001(3) 0.4391(2) 0.1467(3) 0.0237(12) Uani 1 1 d . . . O29 O 0.5120(4) -0.0401(2) 0.1270(3) 0.0281(13) Uani 1 1 d . . . O30 O 1.1537(4) 0.3754(2) 0.0488(3) 0.0223(12) Uani 1 1 d . . . O31 O 1.1150(3) 0.3706(2) -0.0626(2) 0.0195(11) Uani 1 1 d . . . O33 O 1.1070(4) 0.4168(3) -0.1615(3) 0.0273(13) Uani 1 1 d . . . O34 O 0.6428(3) 0.4148(2) -0.2506(2) 0.0202(11) Uani 1 1 d . . . O35 O 0.7392(3) 0.4050(2) 0.0530(3) 0.0260(13) Uani 1 1 d . . . O75 O 0.7545(3) -0.0151(2) 0.2382(2) 0.0203(11) Uani 1 1 d . . . O76 O 0.9695(4) 0.0309(2) 0.2488(3) 0.0266(13) Uani 1 1 d . . . O77 O 0.9243(4) 0.0142(2) 0.3618(3) 0.0280(13) Uani 1 1 d . . . O78 O 0.6482(4) 0.5022(3) -0.1788(3) 0.0336(14) Uani 1 1 d . . . O79 O 0.5277(4) 0.0710(3) 0.0098(2) 0.0262(13) Uani 1 1 d . . . O95 O 0.5185(4) -0.0618(3) -0.2289(3) 0.0312(14) Uani 1 1 d . . . O96 O 0.5981(4) 0.0637(3) -0.1955(3) 0.0382(16) Uani 1 1 d . . . O97 O 0.5768(9) -0.0339(5) -0.3247(6) 0.100(4) Uani 1 1 d . . . O98 O 0.2790(4) 0.0584(3) 0.1244(4) 0.049(2) Uani 1 1 d . . . O99 O 0.6647(4) -0.0159(3) 0.0901(3) 0.0391(16) Uani 1 1 d . . . O100 O 1.0042(4) 0.1499(3) 0.1715(3) 0.0364(15) Uani 1 1 d . . . O101 O 1.0046(4) 0.4163(3) 0.2179(3) 0.0376(16) Uani 1 1 d . . . O102 O 1.1499(5) 0.5040(3) -0.0817(3) 0.0444(18) Uani 1 1 d . . . O130 O 0.4505(4) 0.1736(3) 0.9551(3) 0.0429(17) Uani 1 1 d . . . O200 O 0.8930(5) 0.1416(3) 0.7431(4) 0.049(2) Uani 1 1 d . . . O334 O 0.371(3) 0.0955(19) 0.4274(19) 0.353(19) Uiso 1 1 d . . . O400 O 0.7398(5) 0.0933(4) 0.6551(3) 0.0461(18) Uani 1 1 d . . . O500 O 0.1646(6) 0.3908(4) 0.7631(4) 0.064(3) Uani 1 1 d . . . O600 O 0.8940(9) 0.0040(5) 0.1022(5) 0.101(4) Uani 1 1 d U . . O601 O 0.9461(9) 0.4068(6) 0.9578(5) 0.113(5) Uani 1 1 d . . . O602 O 0.6301(13) 0.4708(9) -0.0358(6) 0.223(13) Uani 1 1 d . . . O603 O 0.5545(6) 0.3703(7) -0.1131(5) 0.129(6) Uani 1 1 d . . . H603 H 0.5276 0.3573 -0.1471 0.194 Uiso 1 1 d R . . O700 O 1.1860(9) 0.5225(6) 0.0553(6) 0.103(4) Uani 1 1 d . . . O703 O 0.2738(12) 0.0184(6) 0.3319(8) 0.146(6) Uani 1 1 d . . . O704 O 0.5588(12) 0.1188(8) 0.5152(8) 0.148(6) Uiso 1 1 d . . . O705 O 0.4510(9) 0.2924(6) 0.9387(7) 0.125(5) Uani 1 1 d . . . O750 O 1.3226(9) 0.4020(11) 0.0400(7) 0.206(11) Uani 1 1 d . . . C1 C 1.1173(5) 0.2923(4) -0.1489(4) 0.0235(17) Uani 1 1 d . . . C2 C 1.0699(5) 0.2603(3) -0.2006(3) 0.0203(17) Uani 1 1 d . . . H2 H 1.0147 0.2721 -0.2300 0.024 Uiso 1 1 calc R . . C3 C 1.1050(5) 0.2116(4) -0.2077(4) 0.0246(18) Uani 1 1 d . . . H3 H 1.0723 0.1897 -0.2420 0.030 Uiso 1 1 calc R . . C4 C 1.1879(5) 0.1933(3) -0.1658(4) 0.0210(16) Uani 1 1 d . . . C5 C 1.2366(5) 0.2278(4) -0.1151(4) 0.0290(19) Uani 1 1 d . . . H5 H 1.2933 0.2172 -0.0872 0.035 Uiso 1 1 calc R . . C6 C 1.2029(5) 0.2767(4) -0.1057(4) 0.0291(19) Uani 1 1 d . . . H6 H 1.2356 0.2990 -0.0718 0.035 Uiso 1 1 calc R . . C7 C 0.5788(5) 0.2615(4) -0.2530(4) 0.0232(17) Uani 1 1 d . . . H7 H 0.5586 0.2780 -0.2303 0.028 Uiso 1 1 calc R . . C8 C 0.6441(5) 0.2873(3) -0.2580(3) 0.0194(16) Uani 1 1 d . . . C9 C 0.6707(5) 0.2646(3) -0.2936(3) 0.0196(16) Uani 1 1 d . . . H9 H 0.7139 0.2829 -0.2969 0.023 Uiso 1 1 calc R . . C10 C 0.6332(5) 0.2137(4) -0.3254(4) 0.0282(18) Uani 1 1 d . . . H10 H 0.6501 0.1992 -0.3509 0.034 Uiso 1 1 calc R . . C11 C 0.5714(5) 0.1851(4) -0.3192(4) 0.0301(19) Uani 1 1 d . . . C12 C 0.5442(5) 0.2095(3) -0.2837(4) 0.0272(19) Uani 1 1 d . . . H12 H 0.5016 0.1908 -0.2799 0.033 Uiso 1 1 calc R . . C13 C 0.5332(6) 0.1285(4) -0.3501(4) 0.036(2) Uani 1 1 d . . . C14 C 1.2250(5) 0.1374(4) -0.1707(4) 0.0279(19) Uani 1 1 d . . . C15 C 1.2199(5) 0.3129(4) 0.1596(4) 0.0264(18) Uani 1 1 d . . . C16 C 1.2867(5) 0.2874(4) 0.1555(4) 0.0289(19) Uani 1 1 d . . . H16 H 1.3011 0.3017 0.1287 0.035 Uiso 1 1 calc R . . C17 C 1.3322(5) 0.2402(4) 0.1917(4) 0.029(2) Uani 1 1 d . . . H17 H 1.3768 0.2236 0.1888 0.035 Uiso 1 1 calc R . . C18 C 1.3117(5) 0.2180(4) 0.2314(4) 0.032(2) Uani 1 1 d . . . C19 C 1.3617(6) 0.1690(5) 0.2711(5) 0.049(3) Uani 1 1 d . . . C20 C 1.2441(6) 0.2443(5) 0.2357(5) 0.039(2) Uani 1 1 d . . . H20 H 1.2302 0.2296 0.2626 0.047 Uiso 1 1 calc R . . C21 C 1.1988(5) 0.2903(4) 0.2015(4) 0.0238(17) Uani 1 1 d . . . H21 H 1.1548 0.3068 0.2052 0.029 Uiso 1 1 calc R . . C22 C 0.7223(5) 0.1240(3) 0.1343(4) 0.0199(16) Uani 1 1 d . . . C23 C 0.7358(5) 0.1814(3) 0.1108(3) 0.0180(15) Uani 1 1 d . . . C24 C 0.8136(5) 0.2099(3) 0.1425(3) 0.0176(15) Uani 1 1 d . . . H24 H 0.8573 0.1953 0.1788 0.021 Uiso 1 1 calc R . . C25 C 0.8267(5) 0.2606(3) 0.1202(4) 0.0200(16) Uani 1 1 d . . . H25 H 0.8782 0.2810 0.1423 0.024 Uiso 1 1 calc R . . C26 C 0.7641(5) 0.2802(3) 0.0658(3) 0.0148(15) Uani 1 1 d . . . C27 C 0.6848(5) 0.2525(3) 0.0337(4) 0.0234(18) Uani 1 1 d . . . H27 H 0.6418 0.2666 -0.0031 0.028 Uiso 1 1 calc R . . C28 C 0.6705(5) 0.2031(4) 0.0573(4) 0.0261(18) Uani 1 1 d . . . H28 H 0.6168 0.1847 0.0370 0.031 Uiso 1 1 calc R . . C29 C 0.1703(7) -0.0610(5) 0.0404(5) 0.049(3) Uani 1 1 d . . . H29A H 0.2058 -0.0283 0.0612 0.073 Uiso 1 1 calc R . . H29B H 0.1680 -0.0865 0.0683 0.073 Uiso 1 1 calc R . . H29C H 0.1127 -0.0482 0.0117 0.073 Uiso 1 1 calc R . . C30 C 0.1624(6) -0.1407(4) -0.0237(5) 0.038(2) Uani 1 1 d . . . H30A H 0.1856 -0.1511 -0.0480 0.057 Uiso 1 1 calc R . . H30B H 0.1016 -0.1325 -0.0486 0.057 Uiso 1 1 calc R . . H30C H 0.1705 -0.1721 0.0026 0.057 Uiso 1 1 calc R . . C31 C 0.2727(6) -0.0687(4) 0.0089(4) 0.031(2) Uani 1 1 d . . . H31 H 0.2884 -0.0877 -0.0153 0.037 Uiso 1 1 calc R . . C32 C 0.3134(6) 0.1340(4) 0.0138(4) 0.038(2) Uani 1 1 d . . . H32A H 0.2995 0.1007 0.0289 0.057 Uiso 1 1 calc R . . H32B H 0.3239 0.1225 -0.0170 0.057 Uiso 1 1 calc R . . H32C H 0.2658 0.1607 -0.0022 0.057 Uiso 1 1 calc R . . C33 C 0.3954(7) 0.2257(4) 0.0622(5) 0.044(2) Uani 1 1 d . . . H33A H 0.3914 0.2385 0.0261 0.065 Uiso 1 1 calc R . . H33B H 0.4491 0.2389 0.0957 0.065 Uiso 1 1 calc R . . H33C H 0.3478 0.2411 0.0644 0.065 Uiso 1 1 calc R . . C34 C 0.4591(6) 0.1313(4) 0.0991(4) 0.031(2) Uani 1 1 d . . . H34 H 0.5084 0.1509 0.1274 0.037 Uiso 1 1 calc R . . C35 C 0.6007(6) -0.1178(5) 0.2222(5) 0.045(3) Uani 1 1 d . . . H35A H 0.6096 -0.0768 0.2255 0.068 Uiso 1 1 calc R . . H35B H 0.6530 -0.1367 0.2300 0.068 Uiso 1 1 calc R . . H35C H 0.5857 -0.1304 0.2505 0.068 Uiso 1 1 calc R . . C36 C 0.5054(6) -0.1932(4) 0.1510(5) 0.041(2) Uani 1 1 d . . . H36A H 0.4604 -0.1984 0.1102 0.062 Uiso 1 1 calc R . . H36B H 0.4847 -0.2052 0.1763 0.062 Uiso 1 1 calc R . . H36C H 0.5551 -0.2158 0.1594 0.062 Uiso 1 1 calc R . . C37 C 0.4953(5) -0.0929(4) 0.1207(4) 0.0269(19) Uani 1 1 d . . . H37 H 0.4538 -0.1053 0.0828 0.032 Uiso 1 1 calc R . . C70 C 0.1193(9) 0.0666(5) 0.1164(7) 0.063(3) Uani 1 1 d . . . H70A H 0.1194 0.0741 0.1524 0.094 Uiso 1 1 calc R . . H70B H 0.1492 0.0311 0.1205 0.094 Uiso 1 1 calc R . . H70C H 0.0605 0.0636 0.0837 0.094 Uiso 1 1 calc R . . C71 C 0.2397(6) 0.1044(5) 0.1116(5) 0.041(2) Uani 1 1 d . . . H71 H 0.2665 0.1358 0.1056 0.050 Uiso 1 1 calc R . . C80 C 0.6502(6) 0.1024(5) -0.1823(4) 0.038(2) Uani 1 1 d . . . H80 H 0.6434 0.1345 -0.1639 0.046 Uiso 1 1 calc R . . C81 C 0.7288(9) 0.0550(5) -0.2207(6) 0.059(3) Uani 1 1 d . . . H81A H 0.7113 0.0201 -0.2102 0.088 Uiso 1 1 calc R . . H81B H 0.7891 0.0524 -0.2082 0.088 Uiso 1 1 calc R . . H81C H 0.6948 0.0602 -0.2630 0.088 Uiso 1 1 calc R . . C82 C 0.1222(7) 0.1699(4) 0.0929(5) 0.047(3) Uani 1 1 d . . . H82A H 0.1597 0.1981 0.0910 0.070 Uiso 1 1 calc R . . H82B H 0.1114 0.1802 0.1239 0.070 Uiso 1 1 calc R . . H82C H 0.0682 0.1687 0.0555 0.070 Uiso 1 1 calc R . . C115 C 0.7699(6) 0.1527(4) -0.1787(5) 0.044(3) Uani 1 1 d . . . H11A H 0.7466 0.1845 -0.1681 0.066 Uiso 1 1 calc R . . H11B H 0.7725 0.1626 -0.2132 0.066 Uiso 1 1 calc R . . H11C H 0.8273 0.1441 -0.1462 0.066 Uiso 1 1 calc R . . C570 C 0.8875(14) -0.0519(7) 0.1044(7) 0.094(5) Uani 1 1 d U . . H570 H 0.8507 -0.0669 0.1161 0.113 Uiso 1 1 calc R . . C571 C 0.9344(8) -0.1469(5) 0.0983(6) 0.055(3) Uani 1 1 d . . . H57A H 0.8772 -0.1623 0.0829 0.083 Uiso 1 1 calc R . . H57B H 0.9701 -0.1562 0.1398 0.083 Uiso 1 1 calc R . . H57C H 0.9594 -0.1632 0.0770 0.083 Uiso 1 1 calc R . . C572 C 0.962(2) -0.0688(11) 0.0474(14) 0.166(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.0119(4) 0.0118(4) 0.0211(5) 0.0019(3) 0.0059(4) 0.0008(3) As3 0.0100(4) 0.0103(4) 0.0259(5) -0.0008(3) 0.0070(4) -0.0003(3) As4 0.0063(4) 0.0142(5) 0.0207(5) 0.0021(3) 0.0015(3) 0.0008(3) As2 0.0100(4) 0.0137(5) 0.0233(5) -0.0053(3) 0.0031(4) -0.0034(3) V3 0.0094(6) 0.0125(7) 0.0211(7) -0.0013(5) 0.0039(5) -0.0004(4) V5 0.0103(6) 0.0101(6) 0.0218(7) -0.0014(5) 0.0041(6) -0.0005(4) V1 0.0094(6) 0.0129(7) 0.0224(7) 0.0003(5) 0.0037(5) -0.0008(5) V4 0.0091(6) 0.0154(7) 0.0221(7) 0.0011(5) 0.0043(5) 0.0005(5) V2 0.0117(6) 0.0165(7) 0.0260(8) -0.0033(5) 0.0060(6) -0.0004(5) Na1 0.078(4) 0.060(3) 0.054(3) 0.015(3) 0.005(3) -0.019(3) Na9 0.087(4) 0.062(3) 0.060(3) 0.012(3) 0.037(3) 0.016(3) Na5 0.0133(14) 0.0148(15) 0.0259(16) 0.0028(12) 0.0064(13) 0.0002(11) Na7 0.0256(16) 0.0141(15) 0.0244(16) 0.0050(12) 0.0075(14) 0.0009(12) Na8 0.0206(16) 0.0249(17) 0.0312(17) 0.0006(14) 0.0111(14) -0.0017(13) Na10 0.0321(19) 0.038(2) 0.0314(19) -0.0003(15) 0.0162(16) -0.0037(15) Na6 0.0321(19) 0.0221(18) 0.055(2) -0.0168(16) 0.0227(18) -0.0091(15) Na12 0.0308(19) 0.029(2) 0.052(2) -0.0024(17) 0.0159(18) -0.0037(15) Na13 0.0186(15) 0.0245(17) 0.0330(18) -0.0002(14) 0.0092(14) -0.0012(13) N1 0.023(4) 0.025(4) 0.034(4) -0.005(3) 0.011(3) -0.006(3) N2 0.026(4) 0.031(4) 0.036(4) -0.001(3) 0.012(3) 0.000(3) N3 0.022(4) 0.021(4) 0.023(4) -0.005(3) 0.002(3) 0.000(3) N10 0.019(4) 0.028(4) 0.051(5) 0.000(4) 0.014(4) 0.008(3) N15 0.022(4) 0.034(4) 0.040(4) 0.003(3) 0.017(3) -0.003(3) N47 0.050(6) 0.035(5) 0.082(8) 0.016(5) 0.014(6) 0.017(5) O1 0.006(2) 0.016(3) 0.023(3) -0.003(2) 0.003(2) -0.0031(19) O2 0.008(2) 0.022(3) 0.018(3) -0.006(2) 0.003(2) 0.000(2) O3 0.010(2) 0.019(3) 0.019(3) -0.003(2) 0.008(2) -0.0013(19) O4 0.011(2) 0.018(3) 0.018(3) 0.004(2) 0.006(2) -0.0017(19) O5 0.020(3) 0.012(3) 0.029(3) 0.002(2) 0.010(2) 0.001(2) O6 0.016(3) 0.029(3) 0.036(3) 0.000(3) 0.012(3) 0.003(2) O7 0.019(3) 0.016(3) 0.027(3) -0.001(2) 0.005(2) -0.002(2) O8 0.018(3) 0.023(3) 0.031(3) 0.005(2) 0.013(3) -0.002(2) O9 0.008(2) 0.016(3) 0.032(3) -0.009(2) 0.002(2) 0.000(2) O12 0.012(2) 0.011(2) 0.024(3) 0.002(2) 0.012(2) -0.0010(19) O13 0.009(3) 0.009(3) 0.040(3) 0.001(2) 0.002(2) 0.002(2) O14 0.012(3) 0.020(3) 0.026(3) 0.006(2) 0.009(2) 0.006(2) O15 0.014(3) 0.025(3) 0.019(3) 0.004(2) 0.011(2) 0.004(2) O16 0.017(3) 0.015(3) 0.020(3) -0.001(2) 0.015(2) -0.002(2) O17 0.062(7) 0.143(12) 0.237(17) 0.147(12) 0.090(10) 0.071(7) O18 0.032(4) 0.049(5) 0.053(5) 0.002(4) 0.003(3) 0.020(3) O19 0.023(3) 0.022(3) 0.024(3) 0.001(2) 0.010(2) -0.009(2) O20 0.021(3) 0.036(4) 0.032(3) 0.017(3) 0.005(3) -0.001(3) O21 0.032(3) 0.039(4) 0.049(4) -0.013(3) 0.019(3) -0.020(3) O22 0.057(5) 0.066(6) 0.086(6) -0.051(5) 0.051(5) -0.037(4) O23 0.026(3) 0.021(3) 0.053(4) -0.010(3) 0.014(3) 0.002(3) O24 0.019(3) 0.024(3) 0.032(3) -0.002(3) -0.004(3) 0.009(2) O25 0.016(3) 0.018(3) 0.032(3) 0.004(2) 0.008(2) 0.000(2) O26 0.020(3) 0.032(3) 0.028(3) 0.000(3) 0.005(3) -0.007(3) O27 0.023(3) 0.027(3) 0.038(3) -0.003(3) 0.013(3) 0.000(2) O28 0.019(3) 0.014(3) 0.028(3) -0.009(2) 0.005(2) -0.005(2) O29 0.019(3) 0.018(3) 0.040(3) 0.003(3) 0.011(3) 0.000(2) O30 0.021(3) 0.017(3) 0.029(3) -0.008(2) 0.013(3) -0.008(2) O31 0.020(3) 0.023(3) 0.019(3) -0.008(2) 0.013(2) -0.006(2) O33 0.022(3) 0.022(3) 0.035(3) 0.006(3) 0.013(3) -0.005(2) O34 0.010(2) 0.016(3) 0.024(3) 0.005(2) 0.002(2) 0.001(2) O35 0.017(3) 0.021(3) 0.038(3) 0.002(2) 0.013(3) 0.007(2) O75 0.018(3) 0.014(3) 0.023(3) -0.001(2) 0.006(2) 0.003(2) O76 0.022(3) 0.022(3) 0.027(3) -0.002(2) 0.007(2) 0.004(2) O77 0.022(3) 0.015(3) 0.039(3) 0.007(2) 0.010(3) 0.001(2) O78 0.022(3) 0.029(3) 0.039(4) 0.000(3) 0.009(3) -0.004(3) O79 0.025(3) 0.025(3) 0.023(3) -0.004(2) 0.008(2) -0.004(2) O95 0.014(3) 0.024(3) 0.044(4) -0.007(3) 0.008(3) -0.005(2) O96 0.029(3) 0.031(4) 0.048(4) 0.000(3) 0.015(3) -0.009(3) O97 0.109(10) 0.076(8) 0.111(10) -0.019(7) 0.055(8) -0.013(7) O98 0.031(4) 0.035(4) 0.076(5) -0.020(4) 0.023(4) 0.006(3) O99 0.028(3) 0.026(3) 0.042(4) 0.001(3) 0.003(3) 0.006(3) O100 0.030(3) 0.034(4) 0.043(4) 0.013(3) 0.018(3) 0.006(3) O101 0.025(3) 0.025(3) 0.043(4) 0.001(3) 0.004(3) -0.003(3) O102 0.055(5) 0.019(3) 0.046(4) 0.000(3) 0.016(4) -0.006(3) O130 0.021(3) 0.044(4) 0.047(4) -0.001(3) 0.006(3) 0.009(3) O200 0.033(4) 0.051(5) 0.059(5) -0.022(4) 0.022(4) -0.001(3) O400 0.038(4) 0.063(5) 0.038(4) -0.001(4) 0.020(3) -0.009(4) O500 0.058(5) 0.056(5) 0.099(7) -0.037(5) 0.057(5) -0.022(4) O600 0.142(8) 0.061(6) 0.063(5) -0.006(5) 0.028(5) 0.016(6) O601 0.129(11) 0.117(11) 0.069(7) 0.046(7) 0.035(7) 0.032(9) O602 0.25(2) 0.219(18) 0.066(8) -0.012(10) -0.008(10) 0.200(18) O603 0.037(5) 0.225(16) 0.088(8) -0.082(10) 0.006(5) 0.005(7) O700 0.120(10) 0.100(9) 0.094(9) -0.004(7) 0.060(8) -0.007(8) O703 0.174(16) 0.082(10) 0.153(14) 0.010(10) 0.065(13) -0.023(10) O705 0.100(10) 0.096(10) 0.190(15) -0.062(10) 0.083(11) -0.047(8) O750 0.072(9) 0.31(3) 0.121(12) -0.039(15) -0.031(8) 0.099(14) C1 0.017(4) 0.024(4) 0.031(4) 0.006(3) 0.014(4) 0.000(3) C2 0.015(4) 0.015(4) 0.015(4) -0.003(3) -0.003(3) 0.002(3) C3 0.011(4) 0.027(4) 0.022(4) -0.002(3) -0.002(3) 0.000(3) C4 0.012(3) 0.014(4) 0.033(4) 0.000(3) 0.009(3) 0.003(3) C5 0.014(4) 0.027(5) 0.030(4) 0.001(4) 0.000(3) 0.002(3) C6 0.010(4) 0.023(4) 0.036(5) -0.004(4) 0.000(4) -0.004(3) C7 0.013(4) 0.023(4) 0.024(4) -0.004(3) 0.004(3) -0.002(3) C8 0.012(3) 0.014(4) 0.023(4) 0.003(3) 0.002(3) -0.002(3) C9 0.016(4) 0.023(4) 0.020(4) 0.000(3) 0.009(3) -0.004(3) C10 0.023(4) 0.023(4) 0.035(5) -0.002(4) 0.013(4) -0.001(3) C11 0.020(4) 0.031(5) 0.033(5) 0.000(4) 0.009(4) 0.004(4) C12 0.016(4) 0.017(4) 0.034(5) 0.001(3) 0.002(3) -0.006(3) C13 0.029(5) 0.035(5) 0.038(5) -0.018(4) 0.014(4) -0.019(4) C14 0.014(4) 0.021(4) 0.030(4) -0.005(3) -0.001(4) 0.002(3) C15 0.009(3) 0.026(4) 0.031(4) -0.009(4) 0.000(3) -0.006(3) C16 0.013(4) 0.027(5) 0.030(4) -0.006(4) 0.000(3) 0.000(3) C17 0.015(4) 0.028(5) 0.033(5) -0.010(4) 0.003(4) -0.001(3) C18 0.016(4) 0.022(5) 0.045(5) -0.006(4) 0.007(4) 0.001(3) C19 0.025(5) 0.052(7) 0.059(7) 0.019(6) 0.014(5) 0.014(5) C20 0.018(4) 0.041(6) 0.042(6) 0.012(4) 0.003(4) 0.008(4) C21 0.016(4) 0.030(5) 0.027(4) 0.009(4) 0.013(3) 0.000(3) C22 0.015(4) 0.018(4) 0.026(4) 0.001(3) 0.010(3) -0.001(3) C23 0.016(4) 0.013(4) 0.021(4) -0.002(3) 0.007(3) 0.001(3) C24 0.011(3) 0.018(4) 0.017(4) -0.001(3) 0.003(3) 0.000(3) C25 0.017(4) 0.012(4) 0.027(4) 0.001(3) 0.009(3) 0.000(3) C26 0.015(3) 0.015(4) 0.017(3) 0.003(3) 0.009(3) 0.002(3) C27 0.011(4) 0.021(4) 0.028(4) 0.011(3) 0.003(3) -0.002(3) C28 0.016(4) 0.022(4) 0.029(4) 0.005(3) 0.003(3) -0.005(3) C29 0.031(5) 0.058(7) 0.057(7) -0.030(6) 0.023(5) -0.014(5) C30 0.026(5) 0.029(5) 0.062(7) -0.014(5) 0.025(5) -0.015(4) C31 0.026(4) 0.040(5) 0.029(4) -0.012(4) 0.017(4) -0.011(4) C32 0.024(5) 0.038(5) 0.037(5) 0.001(4) 0.006(4) 0.001(4) C33 0.053(6) 0.029(5) 0.042(6) -0.009(4) 0.020(5) 0.006(5) C34 0.033(5) 0.021(4) 0.030(5) -0.003(4) 0.011(4) -0.004(4) C35 0.030(5) 0.036(6) 0.040(6) 0.006(4) -0.002(5) -0.010(4) C36 0.035(5) 0.020(5) 0.055(6) 0.003(4) 0.013(5) -0.006(4) C37 0.014(4) 0.033(5) 0.032(4) 0.002(4) 0.010(4) 0.006(3) C70 0.059(8) 0.044(7) 0.091(10) 0.003(7) 0.042(8) 0.005(6) C71 0.026(5) 0.041(6) 0.049(6) -0.025(5) 0.014(4) -0.008(4) C80 0.032(5) 0.036(6) 0.041(5) 0.003(4) 0.015(4) 0.002(4) C81 0.058(7) 0.044(7) 0.077(9) -0.020(6) 0.037(7) -0.003(6) C82 0.034(5) 0.022(5) 0.059(7) -0.006(5) 0.007(5) 0.004(4) C115 0.027(5) 0.037(6) 0.050(6) 0.004(5) 0.007(5) -0.011(4) C570 0.140(10) 0.068(8) 0.070(7) -0.015(6) 0.052(7) 0.016(7) C571 0.051(7) 0.042(7) 0.090(9) -0.002(6) 0.049(7) -0.002(5) C572 0.28(4) 0.114(19) 0.22(3) 0.054(19) 0.20(3) 0.02(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O35 1.667(5) . ? As1 O16 1.693(5) . ? As1 O15 1.707(5) . ? As1 C26 1.917(7) . ? As3 O33 1.672(6) . ? As3 O31 1.694(5) . ? As3 O12 1.706(5) . ? As3 C1 1.912(9) . ? As4 O34 1.661(5) . ? As4 O14 1.686(6) . ? As4 O13 1.696(6) . ? As4 C8 1.928(8) . ? As2 O28 1.653(5) . ? As2 O30 1.667(6) . ? As2 O9 1.695(5) . ? As2 C15 1.893(9) . ? V3 O7 1.624(6) . ? V3 O2 1.963(5) . ? V3 O12 1.964(5) . ? V3 O13 1.972(5) . ? V3 O3 1.978(5) . ? V3 V5 2.902(2) . ? V3 Na5 3.485(3) 4_565 ? V5 O25 1.602(6) . ? V5 O3 1.857(5) . ? V5 O4 1.866(5) . ? V5 O2 1.869(5) . ? V5 O1 1.879(5) . ? V5 V2 2.8967(19) . ? V5 V4 2.8992(18) . ? V5 V1 2.907(2) . ? V1 O5 1.609(6) . ? V1 O16 1.957(5) . ? V1 O1 1.964(5) . ? V1 O4 1.966(5) . ? V1 O9 1.979(5) . ? V1 Na6 3.420(4) . ? V4 O8 1.607(5) . ? V4 O4 1.954(5) . ? V4 O3 1.957(5) . ? V4 O15 1.977(5) . ? V4 O14 1.979(5) . ? V4 Na9 3.497(6) . ? V2 O6 1.612(6) . ? V2 O1 1.951(5) . ? V2 O2 1.967(5) . ? V2 O31 1.973(6) . ? V2 O30 1.997(5) . ? V2 Na1 3.467(5) . ? Na1 O700 2.223(14) . ? Na1 O750 2.306(15) . ? Na1 O102 2.334(9) . ? Na1 O30 2.381(8) . ? Na1 O31 2.394(8) . ? Na1 Na9 3.608(8) 3_765 ? Na1 Na6 4.040(7) 3_765 ? Na9 O700 2.296(15) 3_765 ? Na9 O14 2.416(8) . ? Na9 O78 2.420(8) . ? Na9 O15 2.425(7) . ? Na9 O602 2.437(19) . ? Na9 O603 2.577(16) . ? Na9 Na12 3.606(7) 2_654 ? Na9 Na1 3.608(8) 3_765 ? Na5 O13 2.367(6) 4_566 ? Na5 O20 2.418(7) . ? Na5 O76 2.428(6) . ? Na5 O77 2.430(7) . ? Na5 O75 2.431(6) . ? Na5 O12 2.442(6) 4_566 ? Na5 Na10 3.411(5) . ? Na5 V3 3.485(3) 4_566 ? Na5 Na7 3.705(4) . ? Na5 Na6 4.085(5) 2_745 ? Na7 O19 2.324(6) . ? Na7 O34 2.365(6) 4_566 ? Na7 O75 2.407(6) . ? Na7 O29 2.411(6) . ? Na7 O27 2.688(7) . ? Na7 O99 2.720(8) . ? Na7 Na8 3.644(5) . ? Na7 Na13 3.707(5) . ? Na8 O79 2.316(7) 3_655 ? Na8 O26 2.392(7) . ? Na8 O79 2.424(7) . ? Na8 O27 2.430(7) . ? Na8 O99 2.504(8) 3_655 ? Na8 O29 2.644(7) . ? Na8 Na8 3.298(6) 3_655 ? Na8 Na13 3.349(5) . ? Na10 O600 2.216(11) . ? Na10 O76 2.263(7) . ? Na10 O100 2.277(8) . ? Na10 O20 2.288(7) . ? Na6 O102 2.335(8) 3_765 ? Na6 O16 2.346(6) . ? Na6 O101 2.349(8) . ? Na6 O9 2.361(6) . ? Na6 O77 2.364(7) 2_755 ? Na6 Na1 4.040(7) 3_765 ? Na6 Na5 4.085(5) 2_755 ? Na12 O78 2.349(7) 2_644 ? Na12 O21 2.363(8) . ? Na12 O95 2.386(8) . ? Na12 O96 2.398(8) . ? Na12 O97 2.418(13) . ? Na12 Na13 3.536(6) 3_655 ? Na12 Na9 3.606(7) 2_644 ? Na13 O98 2.280(7) . ? Na13 O95 2.362(7) 3_655 ? Na13 O96 2.363(7) 3_655 ? Na13 O27 2.366(7) . ? Na13 O26 2.442(7) . ? Na13 O29 2.499(7) . ? Na13 Na12 3.536(6) 3_655 ? N1 C31 1.320(11) . ? N1 C29 1.429(13) . ? N1 C30 1.434(11) . ? N2 C34 1.294(12) . ? N2 C33 1.478(12) . ? N2 C32 1.486(12) . ? N3 C37 1.298(11) . ? N3 C36 1.466(11) . ? N3 C35 1.468(11) . ? N10 C71 1.320(12) . ? N10 C82 1.447(12) . ? N10 C70 1.466(15) . ? N15 C80 1.322(12) . ? N15 C115 1.422(12) . ? N15 C81 1.453(14) . ? N47 C570 1.270(19) . ? N47 C571 1.406(14) . ? N47 C572 1.60(2) . ? O12 Na5 2.442(6) 4_565 ? O13 Na5 2.367(6) 4_565 ? O17 C19 1.233(16) . ? O18 C19 1.279(13) . ? O19 C22 1.253(9) . ? O20 C22 1.256(10) . ? O21 C13 1.238(11) . ? O22 C13 1.265(12) . ? O23 C14 1.278(10) . ? O24 C14 1.257(10) . ? O26 C31 1.251(10) . ? O27 C34 1.241(11) . ? O29 C37 1.253(11) . ? O34 Na7 2.365(6) 4_565 ? O77 Na6 2.364(7) 2_745 ? O78 Na12 2.349(7) 2_654 ? O79 Na8 2.316(7) 3_655 ? O95 Na13 2.362(7) 3_655 ? O96 C80 1.214(12) . ? O96 Na13 2.363(7) 3_655 ? O98 C71 1.228(12) . ? O99 Na8 2.504(8) 3_655 ? O102 Na6 2.335(8) 3_765 ? O600 C570 1.308(19) . ? O603 H603 0.8199 . ? O700 Na9 2.296(15) 3_765 ? C1 C2 1.388(11) . ? C1 C6 1.407(11) . ? C2 C3 1.354(11) . ? C2 H2 0.9300 . ? C3 C4 1.385(11) . ? C3 H3 0.9300 . ? C4 C5 1.406(12) . ? C4 C14 1.495(11) . ? C5 C6 1.368(12) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.386(11) . ? C7 C12 1.405(11) . ? C7 H7 0.9300 . ? C8 C9 1.360(11) . ? C9 C10 1.401(12) . ? C9 H9 0.9300 . ? C10 C11 1.379(12) . ? C10 H10 0.9300 . ? C11 C12 1.382(13) . ? C11 C13 1.509(12) . ? C12 H12 0.9300 . ? C15 C16 1.396(12) . ? C15 C21 1.440(12) . ? C16 C17 1.403(12) . ? C16 H16 0.9300 . ? C17 C18 1.377(14) . ? C17 H17 0.9300 . ? C18 C20 1.419(13) . ? C18 C19 1.488(13) . ? C20 C21 1.361(12) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 C23 1.539(11) . ? C23 C24 1.373(10) . ? C23 C28 1.379(11) . ? C24 C25 1.388(11) . ? C24 H24 0.9300 . ? C25 C26 1.360(11) . ? C25 H25 0.9300 . ? C26 C27 1.385(10) . ? C27 C28 1.390(11) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31 0.9300 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37 0.9300 . ? C70 H70A 0.9600 . ? C70 H70B 0.9600 . ? C70 H70C 0.9600 . ? C71 H71 0.9300 . ? C80 H80 0.9300 . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? C115 H11A 0.9600 . ? C115 H11B 0.9600 . ? C115 H11C 0.9600 . ? C570 H570 0.9300 . ? C571 H57A 0.9600 . ? C571 H57B 0.9600 . ? C571 H57C 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 O35 As1 O16 110.5(3) . . ? O35 As1 O15 107.8(3) . . ? O16 As1 O15 110.0(2) . . ? O35 As1 C26 109.1(3) . . ? O16 As1 C26 108.4(3) . . ? O15 As1 C26 111.0(3) . . ? O33 As3 O31 109.5(3) . . ? O33 As3 O12 109.8(3) . . ? O31 As3 O12 110.3(2) . . ? O33 As3 C1 108.0(3) . . ? O31 As3 C1 108.3(3) . . ? O12 As3 C1 110.8(3) . . ? O34 As4 O14 108.1(3) . . ? O34 As4 O13 109.6(3) . . ? O14 As4 O13 111.6(3) . . ? O34 As4 C8 111.2(3) . . ? O14 As4 C8 109.2(3) . . ? O13 As4 C8 107.2(3) . . ? O28 As2 O30 108.7(3) . . ? O28 As2 O9 108.5(3) . . ? O30 As2 O9 110.2(3) . . ? O28 As2 C15 112.3(3) . . ? O30 As2 C15 108.9(3) . . ? O9 As2 C15 108.2(3) . . ? O7 V3 O2 108.0(3) . . ? O7 V3 O12 106.6(3) . . ? O2 V3 O12 88.9(2) . . ? O7 V3 O13 108.8(3) . . ? O2 V3 O13 143.1(2) . . ? O12 V3 O13 83.3(2) . . ? O7 V3 O3 105.9(3) . . ? O2 V3 O3 78.7(2) . . ? O12 V3 O3 147.4(2) . . ? O13 V3 O3 88.8(2) . . ? O7 V3 V5 109.0(2) . . ? O2 V3 V5 39.57(15) . . ? O12 V3 V5 124.06(16) . . ? O13 V3 V5 122.2(2) . . ? O3 V3 V5 39.31(14) . . ? O7 V3 Na5 111.4(2) . 4_565 ? O2 V3 Na5 124.05(17) . 4_565 ? O12 V3 Na5 42.83(16) . 4_565 ? O13 V3 Na5 40.64(17) . 4_565 ? O3 V3 Na5 124.12(16) . 4_565 ? V5 V3 Na5 139.55(7) . 4_565 ? O25 V5 O3 109.2(3) . . ? O25 V5 O4 108.2(3) . . ? O3 V5 O4 83.3(2) . . ? O25 V5 O2 109.5(3) . . ? O3 V5 O2 84.2(2) . . ? O4 V5 O2 142.3(2) . . ? O25 V5 O1 110.0(3) . . ? O3 V5 O1 140.7(2) . . ? O4 V5 O1 83.7(2) . . ? O2 V5 O1 83.8(2) . . ? O25 V5 V2 113.6(2) . . ? O3 V5 V2 119.37(16) . . ? O4 V5 V2 119.31(16) . . ? O2 V5 V2 42.25(15) . . ? O1 V5 V2 41.80(16) . . ? O25 V5 V4 111.7(2) . . ? O3 V5 V4 41.82(15) . . ? O4 V5 V4 41.78(16) . . ? O2 V5 V4 119.93(17) . . ? O1 V5 V4 118.84(16) . . ? V2 V5 V4 134.69(6) . . ? O25 V5 V3 113.1(2) . . ? O3 V5 V3 42.42(15) . . ? O4 V5 V3 119.43(16) . . ? O2 V5 V3 42.01(15) . . ? O1 V5 V3 118.83(17) . . ? V2 V5 V3 81.39(5) . . ? V4 V5 V3 81.82(5) . . ? O25 V5 V1 113.2(2) . . ? O3 V5 V1 118.14(16) . . ? O4 V5 V1 41.94(16) . . ? O2 V5 V1 119.20(16) . . ? O1 V5 V1 41.94(16) . . ? V2 V5 V1 81.12(5) . . ? V4 V5 V1 80.86(5) . . ? V3 V5 V1 133.72(6) . . ? O5 V1 O16 106.7(3) . . ? O5 V1 O1 106.7(3) . . ? O16 V1 O1 146.5(2) . . ? O5 V1 O4 107.9(2) . . ? O16 V1 O4 88.8(2) . . ? O1 V1 O4 79.0(2) . . ? O5 V1 O9 108.8(3) . . ? O16 V1 O9 83.3(2) . . ? O1 V1 O9 88.1(2) . . ? O4 V1 O9 143.1(2) . . ? O5 V1 V5 110.0(2) . . ? O16 V1 V5 123.24(16) . . ? O1 V1 V5 39.76(14) . . ? O4 V1 V5 39.39(15) . . ? O9 V1 V5 121.64(18) . . ? O5 V1 Na6 109.7(2) . . ? O16 V1 Na6 41.51(16) . . ? O1 V1 Na6 125.32(17) . . ? O4 V1 Na6 124.11(17) . . ? O9 V1 Na6 42.14(16) . . ? V5 V1 Na6 140.24(9) . . ? O8 V4 O4 109.0(3) . . ? O8 V4 O3 106.1(3) . . ? O4 V4 O3 78.5(2) . . ? O8 V4 O15 105.3(3) . . ? O4 V4 O15 89.3(2) . . ? O3 V4 O15 148.5(2) . . ? O8 V4 O14 108.5(3) . . ? O4 V4 O14 142.4(2) . . ? O3 V4 O14 89.0(2) . . ? O15 V4 O14 83.2(2) . . ? O8 V4 V5 109.5(2) . . ? O4 V4 V5 39.52(15) . . ? O3 V4 V5 39.27(15) . . ? O15 V4 V5 124.92(16) . . ? O14 V4 V5 122.18(16) . . ? O8 V4 Na9 119.1(2) . . ? O4 V4 Na9 117.07(19) . . ? O3 V4 Na9 119.89(19) . . ? O15 V4 Na9 42.10(18) . . ? O14 V4 Na9 41.86(18) . . ? V5 V4 Na9 131.41(12) . . ? O6 V2 O1 106.7(3) . . ? O6 V2 O2 108.2(3) . . ? O1 V2 O2 79.4(2) . . ? O6 V2 O31 107.1(3) . . ? O1 V2 O31 146.1(2) . . ? O2 V2 O31 88.4(2) . . ? O6 V2 O30 106.2(3) . . ? O1 V2 O30 89.1(2) . . ? O2 V2 O30 145.6(2) . . ? O31 V2 O30 83.3(2) . . ? O6 V2 V5 109.8(2) . . ? O1 V2 V5 39.94(15) . . ? O2 V2 V5 39.70(16) . . ? O31 V2 V5 123.23(17) . . ? O30 V2 V5 123.80(17) . . ? O6 V2 Na1 108.6(2) . . ? O1 V2 Na1 125.4(2) . . ? O2 V2 Na1 124.83(19) . . ? O31 V2 Na1 41.93(18) . . ? O30 V2 Na1 41.71(19) . . ? V5 V2 Na1 141.61(12) . . ? O700 Na1 O750 118.0(6) . . ? O700 Na1 O102 94.3(4) . . ? O750 Na1 O102 114.2(7) . . ? O700 Na1 O30 97.0(4) . . ? O750 Na1 O30 87.1(7) . . ? O102 Na1 O30 147.1(3) . . ? O700 Na1 O31 146.5(5) . . ? O750 Na1 O31 91.4(6) . . ? O102 Na1 O31 86.8(3) . . ? O30 Na1 O31 67.1(2) . . ? O700 Na1 V2 127.0(4) . . ? O750 Na1 V2 86.2(7) . . ? O102 Na1 V2 118.9(3) . . ? O30 Na1 V2 33.92(15) . . ? O31 Na1 V2 33.42(15) . . ? O700 Na1 Na9 37.7(4) . 3_765 ? O750 Na1 Na9 85.2(6) . 3_765 ? O102 Na1 Na9 92.1(2) . 3_765 ? O30 Na1 Na9 115.4(2) . 3_765 ? O31 Na1 Na9 175.7(3) . 3_765 ? V2 Na1 Na9 148.57(18) . 3_765 ? O700 Na1 Na6 76.2(4) . 3_765 ? O750 Na1 Na6 144.2(7) . 3_765 ? O102 Na1 Na6 30.1(2) . 3_765 ? O30 Na1 Na6 125.5(3) . 3_765 ? O31 Na1 Na6 89.2(2) . 3_765 ? V2 Na1 Na6 112.12(15) . 3_765 ? Na9 Na1 Na6 91.94(16) 3_765 3_765 ? O700 Na9 O14 99.9(4) 3_765 . ? O700 Na9 O78 82.8(4) 3_765 . ? O14 Na9 O78 94.3(3) . . ? O700 Na9 O15 93.2(4) 3_765 . ? O14 Na9 O15 65.7(2) . . ? O78 Na9 O15 158.8(3) . . ? O700 Na9 O602 99.5(7) 3_765 . ? O14 Na9 O602 149.6(7) . . ? O78 Na9 O602 111.2(5) . . ? O15 Na9 O602 90.0(5) . . ? O700 Na9 O603 159.6(5) 3_765 . ? O14 Na9 O603 82.6(3) . . ? O78 Na9 O603 117.4(4) . . ? O15 Na9 O603 69.2(4) . . ? O602 Na9 O603 71.3(7) . . ? O700 Na9 V4 93.3(4) 3_765 . ? O14 Na9 V4 33.13(15) . . ? O78 Na9 V4 126.0(3) . . ? O15 Na9 V4 33.15(14) . . ? O602 Na9 V4 122.6(5) . . ? O603 Na9 V4 77.7(3) . . ? O700 Na9 Na12 115.6(4) 3_765 2_654 ? O14 Na9 Na12 109.2(2) . 2_654 ? O78 Na9 Na12 40.13(18) . 2_654 ? O15 Na9 Na12 151.1(3) . 2_654 ? O602 Na9 Na12 82.9(3) . 2_654 ? O603 Na9 Na12 82.1(4) . 2_654 ? V4 Na9 Na12 138.83(19) . 2_654 ? O700 Na9 Na1 36.3(4) 3_765 3_765 ? O14 Na9 Na1 136.2(3) . 3_765 ? O78 Na9 Na1 84.1(2) . 3_765 ? O15 Na9 Na1 104.9(2) . 3_765 ? O602 Na9 Na1 65.5(6) . 3_765 ? O603 Na9 Na1 136.4(3) . 3_765 ? V4 Na9 Na1 121.74(19) . 3_765 ? Na12 Na9 Na1 97.51(17) 2_654 3_765 ? O13 Na5 O20 95.2(2) 4_566 . ? O13 Na5 O76 147.8(2) 4_566 . ? O20 Na5 O76 82.3(2) . . ? O13 Na5 O77 95.6(2) 4_566 . ? O20 Na5 O77 167.6(3) . . ? O76 Na5 O77 91.7(2) . . ? O13 Na5 O75 105.8(2) 4_566 . ? O20 Na5 O75 89.7(2) . . ? O76 Na5 O75 106.2(2) . . ? O77 Na5 O75 81.5(2) . . ? O13 Na5 O12 65.90(19) 4_566 4_566 ? O20 Na5 O12 107.5(2) . 4_566 ? O76 Na5 O12 84.2(2) . 4_566 ? O77 Na5 O12 82.5(2) . 4_566 ? O75 Na5 O12 161.1(2) . 4_566 ? O13 Na5 Na10 123.10(19) 4_566 . ? O20 Na5 Na10 42.06(17) . . ? O76 Na5 Na10 41.47(16) . . ? O77 Na5 Na10 133.19(19) . . ? O75 Na5 Na10 108.31(17) . . ? O12 Na5 Na10 89.97(16) 4_566 . ? O13 Na5 V3 32.86(13) 4_566 4_566 ? O20 Na5 V3 101.64(19) . 4_566 ? O76 Na5 V3 116.04(17) . 4_566 ? O77 Na5 V3 90.77(17) . 4_566 ? O75 Na5 V3 137.25(17) . 4_566 ? O12 Na5 V3 33.14(12) 4_566 4_566 ? Na10 Na5 V3 107.44(10) . 4_566 ? O13 Na5 Na7 81.09(16) 4_566 . ? O20 Na5 Na7 61.22(16) . . ? O76 Na5 Na7 123.66(18) . . ? O77 Na5 Na7 114.67(17) . . ? O75 Na5 Na7 39.78(14) . . ? O12 Na5 Na7 144.51(16) 4_566 . ? Na10 Na5 Na7 97.88(11) . . ? V3 Na5 Na7 112.51(9) 4_566 . ? O13 Na5 Na6 125.80(19) 4_566 2_745 ? O20 Na5 Na6 138.9(2) . 2_745 ? O76 Na5 Na6 62.42(16) . 2_745 ? O77 Na5 Na6 31.09(16) . 2_745 ? O75 Na5 Na6 81.38(15) . 2_745 ? O12 Na5 Na6 90.01(15) 4_566 2_745 ? Na10 Na5 Na6 103.40(11) . 2_745 ? V3 Na5 Na6 112.03(10) 4_566 2_745 ? Na7 Na5 Na6 121.14(10) . 2_745 ? O19 Na7 O34 95.0(2) . 4_566 ? O19 Na7 O75 113.6(2) . . ? O34 Na7 O75 83.9(2) 4_566 . ? O19 Na7 O29 131.9(2) . . ? O34 Na7 O29 116.5(2) 4_566 . ? O75 Na7 O29 105.6(2) . . ? O19 Na7 O27 77.5(2) . . ? O34 Na7 O27 89.9(2) 4_566 . ? O75 Na7 O27 167.7(2) . . ? O29 Na7 O27 67.8(2) . . ? O19 Na7 O99 76.5(2) . . ? O34 Na7 O99 158.3(2) 4_566 . ? O75 Na7 O99 81.5(2) . . ? O29 Na7 O99 82.9(2) . . ? O27 Na7 O99 107.2(2) . . ? O19 Na7 Na8 85.44(17) . . ? O34 Na7 Na8 130.56(18) 4_566 . ? O75 Na7 Na8 140.53(18) . . ? O29 Na7 Na8 46.48(16) . . ? O27 Na7 Na8 41.81(15) . . ? O99 Na7 Na8 69.34(16) . . ? O19 Na7 Na5 76.71(16) . . ? O34 Na7 Na5 70.83(15) 4_566 . ? O75 Na7 Na5 40.26(14) . . ? O29 Na7 Na5 145.73(18) . . ? O27 Na7 Na5 146.09(18) . . ? O99 Na7 Na5 87.74(16) . . ? Na8 Na7 Na5 153.81(12) . . ? O19 Na7 Na13 116.88(18) . . ? O34 Na7 Na13 82.99(16) 4_566 . ? O75 Na7 Na13 128.67(18) . . ? O29 Na7 Na13 41.88(16) . . ? O27 Na7 Na13 39.54(15) . . ? O99 Na7 Na13 118.65(18) . . ? Na8 Na7 Na13 54.19(9) . . ? Na5 Na7 Na13 151.82(12) . . ? O79 Na8 O26 105.1(2) 3_655 . ? O79 Na8 O79 91.8(2) 3_655 . ? O26 Na8 O79 162.8(3) . . ? O79 Na8 O27 147.4(2) 3_655 . ? O26 Na8 O27 86.5(2) . . ? O79 Na8 O27 80.4(2) . . ? O79 Na8 O99 77.9(2) 3_655 3_655 ? O26 Na8 O99 95.8(2) . 3_655 ? O79 Na8 O99 85.1(2) . 3_655 ? O27 Na8 O99 132.0(3) . 3_655 ? O79 Na8 O29 85.1(2) 3_655 . ? O26 Na8 O29 75.3(2) . . ? O79 Na8 O29 109.4(2) . . ? O27 Na8 O29 68.2(2) . . ? O99 Na8 O29 158.1(2) 3_655 . ? O79 Na8 Na8 47.26(16) 3_655 3_655 ? O26 Na8 Na8 152.3(2) . 3_655 ? O79 Na8 Na8 44.57(16) . 3_655 ? O27 Na8 Na8 117.9(2) . 3_655 ? O99 Na8 Na8 77.9(2) 3_655 3_655 ? O29 Na8 Na8 100.61(19) . 3_655 ? O79 Na8 Na13 125.8(2) 3_655 . ? O26 Na8 Na13 46.77(16) . . ? O79 Na8 Na13 123.97(19) . . ? O27 Na8 Na13 44.93(17) . . ? O99 Na8 Na13 136.9(2) 3_655 . ? O29 Na8 Na13 47.52(15) . . ? Na8 Na8 Na13 145.23(17) 3_655 . ? O79 Na8 Na7 99.99(18) 3_655 . ? O26 Na8 Na7 108.15(18) . . ? O79 Na8 Na7 70.55(16) . . ? O27 Na8 Na7 47.52(16) . . ? O99 Na8 Na7 155.5(2) 3_655 . ? O29 Na8 Na7 41.38(14) . . ? Na8 Na8 Na7 82.94(13) 3_655 . ? Na13 Na8 Na7 63.85(10) . . ? O600 Na10 O76 99.4(4) . . ? O600 Na10 O100 118.8(5) . . ? O76 Na10 O100 108.0(3) . . ? O600 Na10 O20 110.4(5) . . ? O76 Na10 O20 88.9(2) . . ? O100 Na10 O20 123.3(3) . . ? O600 Na10 Na5 119.9(4) . . ? O76 Na10 Na5 45.28(16) . . ? O100 Na10 Na5 118.2(2) . . ? O20 Na10 Na5 45.07(16) . . ? O102 Na6 O16 89.5(2) 3_765 . ? O102 Na6 O101 104.1(3) 3_765 . ? O16 Na6 O101 100.1(2) . . ? O102 Na6 O9 144.5(3) 3_765 . ? O16 Na6 O9 67.49(19) . . ? O101 Na6 O9 106.2(3) . . ? O102 Na6 O77 98.3(3) 3_765 2_755 ? O16 Na6 O77 150.9(3) . 2_755 ? O101 Na6 O77 105.0(3) . 2_755 ? O9 Na6 O77 91.3(2) . 2_755 ? O102 Na6 V1 120.4(2) 3_765 . ? O16 Na6 V1 33.56(13) . . ? O101 Na6 V1 102.5(2) . . ? O9 Na6 V1 34.21(14) . . ? O77 Na6 V1 124.2(2) 2_755 . ? O102 Na6 Na1 30.1(2) 3_765 3_765 ? O16 Na6 Na1 91.86(19) . 3_765 ? O101 Na6 Na1 132.9(2) . 3_765 ? O9 Na6 Na1 120.4(2) . 3_765 ? O77 Na6 Na1 81.79(19) 2_755 3_765 ? V1 Na6 Na1 111.66(14) . 3_765 ? O102 Na6 Na5 96.7(2) 3_765 2_755 ? O16 Na6 Na5 172.6(2) . 2_755 ? O101 Na6 Na5 74.44(18) . 2_755 ? O9 Na6 Na5 108.86(17) . 2_755 ? O77 Na6 Na5 32.05(16) 2_755 2_755 ? V1 Na6 Na5 141.83(12) . 2_755 ? Na1 Na6 Na5 95.55(12) 3_765 2_755 ? O78 Na12 O21 97.5(3) 2_644 . ? O78 Na12 O95 81.5(2) 2_644 . ? O21 Na12 O95 175.8(3) . . ? O78 Na12 O96 123.2(3) 2_644 . ? O21 Na12 O96 94.5(3) . . ? O95 Na12 O96 82.7(2) . . ? O78 Na12 O97 123.0(4) 2_644 . ? O21 Na12 O97 98.5(4) . . ? O95 Na12 O97 85.4(4) . . ? O96 Na12 O97 109.5(4) . . ? O78 Na12 Na13 100.9(2) 2_644 3_655 ? O21 Na12 Na13 135.1(2) . 3_655 ? O95 Na12 Na13 41.61(17) . 3_655 ? O96 Na12 Na13 41.66(18) . 3_655 ? O97 Na12 Na13 104.8(3) . 3_655 ? O78 Na12 Na9 41.62(19) 2_644 2_644 ? O21 Na12 Na9 99.9(2) . 2_644 ? O95 Na12 Na9 82.10(19) . 2_644 ? O96 Na12 Na9 160.2(2) . 2_644 ? O97 Na12 Na9 81.7(3) . 2_644 ? Na13 Na12 Na9 120.82(15) 3_655 2_644 ? O98 Na13 O95 88.3(3) . 3_655 ? O98 Na13 O96 97.1(3) . 3_655 ? O95 Na13 O96 84.0(2) 3_655 3_655 ? O98 Na13 O27 106.7(3) . . ? O95 Na13 O27 87.4(2) 3_655 . ? O96 Na13 O27 154.4(3) 3_655 . ? O98 Na13 O26 90.6(3) . . ? O95 Na13 O26 173.5(3) 3_655 . ? O96 Na13 O26 102.5(2) 3_655 . ? O27 Na13 O26 86.8(2) . . ? O98 Na13 O29 167.7(3) . . ? O95 Na13 O29 103.7(2) 3_655 . ? O96 Na13 O29 87.0(2) 3_655 . ? O27 Na13 O29 71.7(2) . . ? O26 Na13 O29 77.2(2) . . ? O98 Na13 Na8 118.4(3) . . ? O95 Na13 Na8 130.2(2) 3_655 . ? O96 Na13 Na8 127.8(2) 3_655 . ? O27 Na13 Na8 46.50(17) . . ? O26 Na13 Na8 45.54(16) . . ? O29 Na13 Na8 51.29(16) . . ? O98 Na13 Na12 99.1(3) . 3_655 ? O95 Na13 Na12 42.13(18) 3_655 3_655 ? O96 Na13 Na12 42.42(18) 3_655 3_655 ? O27 Na13 Na12 122.19(19) . 3_655 ? O26 Na13 Na12 144.4(2) . 3_655 ? O29 Na13 Na12 91.83(18) . 3_655 ? Na8 Na13 Na12 142.36(13) . 3_655 ? O98 Na13 Na7 146.1(2) . . ? O95 Na13 Na7 72.67(17) 3_655 . ? O96 Na13 Na7 108.1(2) 3_655 . ? O27 Na13 Na7 46.32(16) . . ? O26 Na13 Na7 105.15(19) . . ? O29 Na13 Na7 40.10(15) . . ? Na8 Na13 Na7 61.95(9) . . ? Na12 Na13 Na7 85.54(11) 3_655 . ? C31 N1 C29 120.9(8) . . ? C31 N1 C30 120.3(8) . . ? C29 N1 C30 118.2(8) . . ? C34 N2 C33 122.3(8) . . ? C34 N2 C32 120.2(8) . . ? C33 N2 C32 117.0(8) . . ? C37 N3 C36 123.3(8) . . ? C37 N3 C35 120.9(8) . . ? C36 N3 C35 115.7(8) . . ? C71 N10 C82 123.7(9) . . ? C71 N10 C70 119.2(9) . . ? C82 N10 C70 116.9(8) . . ? C80 N15 C115 122.9(9) . . ? C80 N15 C81 119.1(9) . . ? C115 N15 C81 117.8(9) . . ? C570 N47 C571 127.0(14) . . ? C570 N47 C572 121.8(15) . . ? C571 N47 C572 109.2(13) . . ? V5 O1 V2 98.3(2) . . ? V5 O1 V1 98.3(2) . . ? V2 O1 V1 149.2(3) . . ? V5 O2 V3 98.4(2) . . ? V5 O2 V2 98.1(2) . . ? V3 O2 V2 148.3(3) . . ? V5 O3 V4 98.9(2) . . ? V5 O3 V3 98.3(2) . . ? V4 O3 V3 149.8(3) . . ? V5 O4 V4 98.7(2) . . ? V5 O4 V1 98.7(2) . . ? V4 O4 V1 147.8(3) . . ? As2 O9 V1 126.2(3) . . ? As2 O9 Na6 130.1(3) . . ? V1 O9 Na6 103.7(2) . . ? As3 O12 V3 124.4(3) . . ? As3 O12 Na5 130.4(3) . 4_565 ? V3 O12 Na5 104.0(2) . 4_565 ? As4 O13 V3 126.6(3) . . ? As4 O13 Na5 126.6(3) . 4_565 ? V3 O13 Na5 106.5(2) . 4_565 ? As4 O14 V4 126.5(3) . . ? As4 O14 Na9 126.1(3) . . ? V4 O14 Na9 105.0(3) . . ? As1 O15 V4 126.5(3) . . ? As1 O15 Na9 122.1(3) . . ? V4 O15 Na9 104.7(3) . . ? As1 O16 V1 126.3(3) . . ? As1 O16 Na6 128.7(3) . . ? V1 O16 Na6 104.9(2) . . ? C22 O19 Na7 120.0(5) . . ? C22 O20 Na10 133.7(5) . . ? C22 O20 Na5 128.3(6) . . ? Na10 O20 Na5 92.9(2) . . ? C13 O21 Na12 122.8(7) . . ? C31 O26 Na8 120.7(6) . . ? C31 O26 Na13 140.4(6) . . ? Na8 O26 Na13 87.7(2) . . ? C34 O27 Na13 126.3(6) . . ? C34 O27 Na8 131.5(6) . . ? Na13 O27 Na8 88.6(2) . . ? C34 O27 Na7 115.4(6) . . ? Na13 O27 Na7 94.1(2) . . ? Na8 O27 Na7 90.7(2) . . ? C37 O29 Na7 146.7(5) . . ? C37 O29 Na13 110.6(5) . . ? Na7 O29 Na13 98.0(2) . . ? C37 O29 Na8 108.5(5) . . ? Na7 O29 Na8 92.1(2) . . ? Na13 O29 Na8 81.19(19) . . ? As2 O30 V2 126.3(3) . . ? As2 O30 Na1 128.9(3) . . ? V2 O30 Na1 104.4(3) . . ? As3 O31 V2 124.0(3) . . ? As3 O31 Na1 131.3(3) . . ? V2 O31 Na1 104.6(3) . . ? As4 O34 Na7 134.8(3) . 4_565 ? Na7 O75 Na5 100.0(2) . . ? Na10 O76 Na5 93.3(2) . . ? Na6 O77 Na5 116.9(3) 2_745 . ? Na12 O78 Na9 98.2(3) 2_654 . ? Na8 O79 Na8 88.2(2) 3_655 . ? Na13 O95 Na12 96.3(2) 3_655 . ? C80 O96 Na13 129.2(7) . 3_655 ? C80 O96 Na12 131.5(7) . . ? Na13 O96 Na12 95.9(3) 3_655 . ? C71 O98 Na13 143.7(7) . . ? Na8 O99 Na7 123.6(3) 3_655 . ? Na1 O102 Na6 119.8(4) . 3_765 ? C570 O600 Na10 136.1(11) . . ? Na9 O603 H603 109.8 . . ? Na1 O700 Na9 105.9(6) . 3_765 ? C2 C1 C6 120.8(8) . . ? C2 C1 As3 121.7(6) . . ? C6 C1 As3 117.3(6) . . ? C3 C2 C1 119.2(7) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 122.2(8) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 117.7(7) . . ? C3 C4 C14 122.9(7) . . ? C5 C4 C14 119.3(7) . . ? C6 C5 C4 121.7(7) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C1 118.1(8) . . ? C5 C6 H6 120.9 . . ? C1 C6 H6 120.9 . . ? C8 C7 C12 117.5(8) . . ? C8 C7 H7 121.2 . . ? C12 C7 H7 121.2 . . ? C9 C8 C7 121.2(7) . . ? C9 C8 As4 118.8(6) . . ? C7 C8 As4 120.0(6) . . ? C8 C9 C10 120.3(7) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C11 C10 C9 120.2(8) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 118.4(9) . . ? C10 C11 C13 121.7(8) . . ? C12 C11 C13 119.8(8) . . ? C11 C12 C7 122.1(8) . . ? C11 C12 H12 118.9 . . ? C7 C12 H12 118.9 . . ? O21 C13 O22 125.4(9) . . ? O21 C13 C11 118.8(9) . . ? O22 C13 C11 115.7(8) . . ? O24 C14 O23 122.6(8) . . ? O24 C14 C4 120.7(7) . . ? O23 C14 C4 116.7(7) . . ? C16 C15 C21 119.1(8) . . ? C16 C15 As2 122.7(7) . . ? C21 C15 As2 118.2(6) . . ? C15 C16 C17 120.2(9) . . ? C15 C16 H16 119.9 . . ? C17 C16 H16 119.9 . . ? C18 C17 C16 121.0(8) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C20 118.6(9) . . ? C17 C18 C19 121.0(9) . . ? C20 C18 C19 120.3(10) . . ? O17 C19 O18 124.8(10) . . ? O17 C19 C18 118.1(10) . . ? O18 C19 C18 117.1(10) . . ? C21 C20 C18 122.0(10) . . ? C21 C20 H20 119.0 . . ? C18 C20 H20 119.0 . . ? C20 C21 C15 119.1(8) . . ? C20 C21 H21 120.5 . . ? C15 C21 H21 120.5 . . ? O19 C22 O20 125.6(7) . . ? O19 C22 C23 117.6(7) . . ? O20 C22 C23 116.8(7) . . ? C24 C23 C28 120.3(7) . . ? C24 C23 C22 119.9(7) . . ? C28 C23 C22 119.8(7) . . ? C23 C24 C25 119.8(7) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 119.9(7) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 121.1(7) . . ? C25 C26 As1 119.1(6) . . ? C27 C26 As1 119.7(5) . . ? C26 C27 C28 118.8(7) . . ? C26 C27 H27 120.6 . . ? C28 C27 H27 120.6 . . ? C23 C28 C27 120.0(7) . . ? C23 C28 H28 120.0 . . ? C27 C28 H28 120.0 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O26 C31 N1 127.2(8) . . ? O26 C31 H31 116.4 . . ? N1 C31 H31 116.4 . . ? N2 C32 H32A 109.5 . . ? N2 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N2 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O27 C34 N2 125.8(9) . . ? O27 C34 H34 117.1 . . ? N2 C34 H34 117.1 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O29 C37 N3 126.8(8) . . ? O29 C37 H37 116.6 . . ? N3 C37 H37 116.6 . . ? N10 C70 H70A 109.5 . . ? N10 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? N10 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? O98 C71 N10 126.5(10) . . ? O98 C71 H71 116.7 . . ? N10 C71 H71 116.7 . . ? O96 C80 N15 126.5(10) . . ? O96 C80 H80 116.7 . . ? N15 C80 H80 116.7 . . ? N15 C81 H81A 109.5 . . ? N15 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N15 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N10 C82 H82A 109.5 . . ? N10 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N10 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N15 C115 H11A 109.5 . . ? N15 C115 H11B 109.5 . . ? H11A C115 H11B 109.5 . . ? N15 C115 H11C 109.5 . . ? H11A C115 H11C 109.5 . . ? H11B C115 H11C 109.5 . . ? N47 C570 O600 122.6(19) . . ? N47 C570 H570 118.7 . . ? O600 C570 H570 118.7 . . ? N47 C571 H57A 109.5 . . ? N47 C571 H57B 109.5 . . ? H57A C571 H57B 109.5 . . ? N47 C571 H57C 109.5 . . ? H57A C571 H57C 109.5 . . ? H57B C571 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 4.767 _refine_diff_density_min -4.386 _refine_diff_density_rms 0.442 # Attachment '- Compound 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 820350' #TrackingRef '- Compound 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H66 As8 Na8 O62 V10' _chemical_formula_weight 2927.69 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' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 orthorhombic _symmetry_space_group_name_H-M 'P n n 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.512(7) _cell_length_b 22.664(12) _cell_length_c 13.699(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4506(4) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6035 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 27.3 _exptl_crystal_description cube _exptl_crystal_colour green _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1432 _exptl_absorpt_coefficient_mu 2.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.497 _exptl_absorpt_correction_T_max 0.738 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator 'graphite Monochromator' _diffrn_measurement_device_type 'Rigaku Saturn 724' _diffrn_measurement_method 'omega and phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19143 _diffrn_reflns_av_R_equivalents 0.0548 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.23 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7704 _reflns_number_gt 6549 _reflns_threshold_expression >2sigma(I) _computing_data_collection Crystalclear _computing_cell_refinement Crystalclear _computing_data_reduction Crystalclear _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. The structure contains highly disordered solvent molecules and we applied the Platon routine SQUEEZE (A. L. Spek, J. Appl. Cryst., 2003, 36, 7). See end of cif file. ; _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^)+(0.1640P)^2^+12.4216P] 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 0.44(3) _refine_ls_number_reflns 7704 _refine_ls_number_parameters 302 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.2863 _refine_ls_wR_factor_gt 0.2742 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _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 As1 As 1.68125(8) 1.35813(5) 0.44584(11) 0.0544(3) Uani 1 1 d . . . As2 As 1.27519(8) 1.38417(5) 0.44119(11) 0.0559(4) Uani 1 1 d . . . V1 V 1.5000 1.5000 0.2533(2) 0.0435(6) Uani 1 2 d S . . V2 V 1.48051(14) 1.38380(9) 0.34017(18) 0.0524(5) Uani 1 1 d . . . V3 V 1.68397(13) 1.48810(9) 0.33559(17) 0.0518(5) Uani 1 1 d . . . Na2 Na 1.4675(4) 1.2876(3) 0.5265(6) 0.093(2) Uani 1 1 d . . . O1 O 1.5775(5) 1.4406(4) 0.2997(6) 0.055(2) Uani 1 1 d . . . O2 O 1.4035(5) 1.4515(4) 0.2983(6) 0.0515(19) Uani 1 1 d . . . O6 O 1.7185(6) 1.4300(4) 0.4363(8) 0.059(2) Uani 1 1 d . . . O7 O 1.5638(5) 1.3519(4) 0.4439(8) 0.062(2) Uani 1 1 d . . . O8 O 1.7557(6) 1.4809(5) 0.2466(7) 0.067(3) Uani 1 1 d . . . O9 O 1.4724(7) 1.3343(4) 0.2577(8) 0.067(2) Uani 1 1 d . . . O10 O 1.2587(5) 1.4575(4) 0.4312(7) 0.059(2) Uani 1 1 d . . . O11 O 1.3883(5) 1.3656(4) 0.4431(7) 0.0575(19) Uani 1 1 d . . . O17 O 1.0993(8) 1.2415(6) 0.1197(10) 0.095(4) Uani 1 1 d . . . O36 O 1.7095(7) 1.3326(5) 0.5563(8) 0.072(3) Uani 1 1 d . . . O45 O 1.8411(8) 1.2082(8) 0.1238(13) 0.141(7) Uani 1 1 d . . . O46 O 1.2313(7) 1.3612(5) 0.5495(7) 0.065(3) Uani 1 1 d . . . O6W O 1.4626(18) 1.2029(12) 0.439(2) 0.107(7) Uiso 0.50 1 d P . . O7W O 1.794(2) 1.4103(14) 0.674(2) 0.106(8) Uiso 0.50 1 d P . . O8W O 1.8833(18) 1.5544(13) 0.626(2) 0.105(8) Uiso 0.50 1 d P . . O5 O 1.5000 1.5000 0.1353(10) 0.059(3) Uani 1 2 d S . . C1 C 1.1018(10) 1.3331(6) 0.2096(13) 0.073(4) Uani 1 1 d . . . H1 H 1.0527 1.3485 0.1744 0.087 Uiso 1 1 calc R . . C2 C 1.1430(11) 1.3657(7) 0.2859(13) 0.073(4) Uani 1 1 d . . . H2 H 1.1181 1.4020 0.3030 0.088 Uiso 1 1 calc R . . C3 C 1.2199(8) 1.3447(6) 0.3364(12) 0.060(3) Uani 1 1 d . . . C4 C 1.2590(12) 1.2881(7) 0.3103(13) 0.082(5) Uani 1 1 d . . . H4 H 1.3120 1.2737 0.3402 0.098 Uiso 1 1 calc R . . C5 C 1.2120(11) 1.2554(7) 0.2361(15) 0.086(6) Uani 1 1 d . . . H5 H 1.2340 1.2180 0.2205 0.103 Uiso 1 1 calc R . . C7 C 1.7315(10) 1.3113(8) 0.3479(12) 0.072(4) Uani 1 1 d . . . C12 C 1.6801(8) 1.2677(7) 0.3049(11) 0.064(4) Uani 1 1 d . . . H12 H 1.6189 1.2629 0.3234 0.077 Uiso 1 1 calc R . . C15 C 1.8078(11) 1.2355(10) 0.2028(17) 0.099(6) Uani 1 1 d . . . C17 C 1.1374(11) 1.2757(7) 0.1875(14) 0.077(4) Uani 1 1 d . . . C45 C 1.7193(11) 1.2284(8) 0.2303(10) 0.077(4) Uani 1 1 d . . . H45A H 1.6834 1.1989 0.2023 0.092 Uiso 1 1 calc R . . C100 C 1.8203(19) 1.3211(14) 0.322(2) 0.137(9) Uiso 1 1 d . . . C101 C 1.865(2) 1.2820(15) 0.244(3) 0.160(11) Uani 1 1 d U . . O4W O 1.945(2) 1.4517(17) 0.471(2) 0.063(9) Uiso 0.25 1 d P . . O1W O 1.5000 1.5000 0.494(4) 0.133(17) Uiso 0.50 2 d SP . . O2W O 1.447(2) 1.0461(17) 0.763(3) 0.136(11) Uiso 0.50 1 d P . . O3W O 0.970(3) 1.302(2) 0.711(3) 0.074(11) Uiso 0.25 1 d P . . O5W O 1.149(3) 1.1219(17) 0.586(3) 0.063(9) Uiso 0.25 1 d P . . Na1 Na 1.8177(8) 1.4760(5) 0.5434(10) 0.148(4) 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 As1 0.0567(6) 0.0500(7) 0.0566(7) 0.0035(7) -0.0023(7) 0.0083(5) As2 0.0525(6) 0.0531(7) 0.0619(7) -0.0075(8) 0.0041(7) -0.0084(5) V1 0.0407(12) 0.0480(15) 0.0417(14) 0.000 0.000 0.0044(10) V2 0.0547(11) 0.0460(10) 0.0564(12) -0.0067(10) 0.0025(10) 0.0045(8) V3 0.0457(9) 0.0542(12) 0.0554(12) 0.0079(11) 0.0038(10) 0.0043(8) Na2 0.064(3) 0.092(5) 0.121(6) 0.037(4) 0.008(4) 0.013(3) O1 0.056(5) 0.048(5) 0.061(5) -0.012(4) 0.003(4) 0.009(4) O2 0.047(4) 0.050(5) 0.057(5) -0.007(4) -0.011(4) -0.003(4) O6 0.061(4) 0.053(5) 0.065(5) 0.004(5) -0.007(5) 0.003(3) O7 0.058(4) 0.064(5) 0.064(5) 0.001(5) 0.004(5) 0.011(4) O8 0.054(5) 0.085(7) 0.064(6) 0.020(5) 0.018(5) 0.008(5) O9 0.076(6) 0.049(5) 0.075(6) -0.009(5) -0.011(5) -0.003(4) O10 0.051(4) 0.067(5) 0.058(5) -0.011(5) -0.002(4) -0.001(4) O11 0.061(4) 0.059(5) 0.052(4) 0.010(5) -0.020(5) 0.001(4) O17 0.073(7) 0.094(9) 0.116(9) -0.039(8) -0.021(7) 0.004(6) O36 0.078(6) 0.060(6) 0.077(6) 0.017(5) -0.021(5) 0.002(5) O45 0.080(8) 0.164(14) 0.179(15) -0.112(13) 0.065(9) -0.020(9) O46 0.063(5) 0.072(7) 0.059(5) 0.015(5) 0.006(5) -0.014(4) O5 0.067(7) 0.059(8) 0.052(7) 0.000 0.000 0.012(6) C1 0.068(8) 0.049(7) 0.101(12) -0.017(8) -0.016(8) 0.007(6) C2 0.070(9) 0.053(8) 0.097(12) -0.005(8) -0.002(8) 0.004(7) C3 0.047(6) 0.060(8) 0.071(8) -0.006(7) -0.016(6) -0.011(5) C4 0.090(10) 0.062(9) 0.094(12) -0.002(8) -0.045(9) 0.003(8) C5 0.072(9) 0.052(8) 0.133(16) -0.039(10) -0.032(10) 0.006(7) C7 0.059(8) 0.089(11) 0.067(9) -0.005(9) 0.013(7) 0.019(7) C12 0.044(6) 0.078(10) 0.069(8) -0.020(7) 0.011(6) -0.006(6) C15 0.058(9) 0.106(14) 0.133(16) -0.034(14) 0.006(10) -0.002(9) C17 0.071(9) 0.056(8) 0.104(12) -0.017(8) -0.027(9) -0.009(7) C45 0.084(10) 0.100(12) 0.046(7) 0.008(8) 0.018(7) 0.014(9) C101 0.152(13) 0.163(14) 0.165(13) -0.021(9) 0.004(9) -0.001(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 O36 1.671(10) . ? As1 O7 1.710(8) . ? As1 O6 1.720(8) . ? As1 C7 1.859(15) . ? As2 O10 1.684(9) . ? As2 O11 1.695(8) . ? As2 O46 1.697(9) . ? As2 C3 1.872(14) . ? V1 O5 1.617(14) . ? V1 O1 1.867(8) 2_885 ? V1 O1 1.867(8) . ? V1 O2 1.884(8) 2_885 ? V1 O2 1.884(8) . ? V1 V2 2.904(3) 2_885 ? V1 V2 2.904(3) . ? V1 V3 2.911(3) 2_885 ? V1 V3 2.911(3) . ? V2 O9 1.597(10) . ? V2 O2 1.983(9) . ? V2 O1 1.986(9) . ? V2 O11 1.987(10) . ? V2 O7 2.002(10) . ? V3 O8 1.612(9) . ? V3 O2 1.936(9) 2_885 ? V3 O1 1.946(9) . ? V3 O6 1.973(10) . ? V3 O10 1.982(10) 2_885 ? O2 V3 1.936(9) 2_885 ? O10 V3 1.982(10) 2_885 ? O17 C17 1.331(18) . ? O45 C15 1.34(2) . ? C1 C2 1.41(2) . ? C1 C17 1.43(2) . ? C1 H1 0.9300 . ? C2 C3 1.40(2) . ? C2 H2 0.9300 . ? C3 C4 1.45(2) . ? C4 C5 1.43(2) . ? C4 H4 0.9300 . ? C5 C17 1.35(2) . ? C5 H5 0.9300 . ? C7 C100 1.36(3) . ? C7 C12 1.37(2) . ? C12 C45 1.47(2) . ? C12 H12 0.9300 . ? C15 C45 1.35(2) . ? C15 C101 1.45(4) . ? C45 H45A 0.9300 . ? C100 C101 1.53(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O36 As1 O7 103.3(5) . . ? O36 As1 O6 108.6(5) . . ? O7 As1 O6 113.0(4) . . ? O36 As1 C7 111.1(7) . . ? O7 As1 C7 109.4(6) . . ? O6 As1 C7 111.2(7) . . ? O10 As2 O11 112.6(4) . . ? O10 As2 O46 108.7(5) . . ? O11 As2 O46 105.9(5) . . ? O10 As2 C3 110.4(6) . . ? O11 As2 C3 107.9(5) . . ? O46 As2 C3 111.3(5) . . ? O5 V1 O1 109.9(3) . 2_885 ? O5 V1 O1 109.9(3) . . ? O1 V1 O1 140.1(5) 2_885 . ? O5 V1 O2 109.1(3) . 2_885 ? O1 V1 O2 85.1(4) 2_885 2_885 ? O1 V1 O2 82.0(4) . 2_885 ? O5 V1 O2 109.1(3) . . ? O1 V1 O2 82.0(4) 2_885 . ? O1 V1 O2 85.1(4) . . ? O2 V1 O2 141.8(5) 2_885 . ? O5 V1 V2 114.20(7) . 2_885 ? O1 V1 V2 42.7(3) 2_885 2_885 ? O1 V1 V2 117.1(3) . 2_885 ? O2 V1 V2 42.6(3) 2_885 2_885 ? O2 V1 V2 117.9(3) . 2_885 ? O5 V1 V2 114.20(7) . . ? O1 V1 V2 117.1(3) 2_885 . ? O1 V1 V2 42.7(3) . . ? O2 V1 V2 117.9(3) 2_885 . ? O2 V1 V2 42.6(3) . . ? V2 V1 V2 131.61(14) 2_885 . ? O5 V1 V3 112.79(7) . 2_885 ? O1 V1 V3 41.3(3) 2_885 2_885 ? O1 V1 V3 119.2(3) . 2_885 ? O2 V1 V3 120.0(3) 2_885 2_885 ? O2 V1 V3 41.0(3) . 2_885 ? V2 V1 V3 81.17(7) 2_885 2_885 ? V2 V1 V3 80.55(7) . 2_885 ? O5 V1 V3 112.79(7) . . ? O1 V1 V3 119.2(3) 2_885 . ? O1 V1 V3 41.3(3) . . ? O2 V1 V3 41.0(3) 2_885 . ? O2 V1 V3 120.0(3) . . ? V2 V1 V3 80.55(7) 2_885 . ? V2 V1 V3 81.17(7) . . ? V3 V1 V3 134.41(14) 2_885 . ? O9 V2 O2 107.3(4) . . ? O9 V2 O1 108.1(5) . . ? O2 V2 O1 79.5(4) . . ? O9 V2 O11 107.8(5) . . ? O2 V2 O11 89.2(3) . . ? O1 V2 O11 144.1(4) . . ? O9 V2 O7 107.0(5) . . ? O2 V2 O7 145.6(4) . . ? O1 V2 O7 90.2(4) . . ? O11 V2 O7 80.1(4) . . ? O9 V2 V1 110.8(4) . . ? O2 V2 V1 40.0(2) . . ? O1 V2 V1 39.6(2) . . ? O11 V2 V1 123.0(3) . . ? O7 V2 V1 124.1(3) . . ? O8 V3 O2 107.2(4) . 2_885 ? O8 V3 O1 105.4(5) . . ? O2 V3 O1 78.7(4) 2_885 . ? O8 V3 O6 107.3(5) . . ? O2 V3 O6 145.4(4) 2_885 . ? O1 V3 O6 90.5(4) . . ? O8 V3 O10 106.9(5) . 2_885 ? O2 V3 O10 90.6(4) 2_885 2_885 ? O1 V3 O10 147.6(4) . 2_885 ? O6 V3 O10 81.2(4) . 2_885 ? O8 V3 V1 108.0(4) . . ? O2 V3 V1 39.7(2) 2_885 . ? O1 V3 V1 39.2(3) . . ? O6 V3 V1 124.4(3) . . ? O10 V3 V1 125.7(3) 2_885 . ? V1 O1 V3 99.5(4) . . ? V1 O1 V2 97.8(4) . . ? V3 O1 V2 148.3(5) . . ? V1 O2 V3 99.3(4) . 2_885 ? V1 O2 V2 97.3(4) . . ? V3 O2 V2 147.2(5) 2_885 . ? As1 O6 V3 127.3(5) . . ? As1 O7 V2 125.6(6) . . ? As2 O10 V3 127.4(5) . 2_885 ? As2 O11 V2 126.1(5) . . ? C2 C1 C17 118.6(14) . . ? C2 C1 H1 120.7 . . ? C17 C1 H1 120.7 . . ? C3 C2 C1 121.8(14) . . ? C3 C2 H2 119.1 . . ? C1 C2 H2 119.1 . . ? C2 C3 C4 119.5(13) . . ? C2 C3 As2 124.0(12) . . ? C4 C3 As2 116.4(10) . . ? C5 C4 C3 116.6(13) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? C17 C5 C4 123.7(14) . . ? C17 C5 H5 118.1 . . ? C4 C5 H5 118.1 . . ? C100 C7 C12 121.5(18) . . ? C100 C7 As1 118.0(17) . . ? C12 C7 As1 120.5(10) . . ? C7 C12 C45 121.7(13) . . ? C7 C12 H12 119.2 . . ? C45 C12 H12 119.2 . . ? O45 C15 C45 121.0(18) . . ? O45 C15 C101 116(2) . . ? C45 C15 C101 121(2) . . ? O17 C17 C5 118.6(14) . . ? O17 C17 C1 121.8(14) . . ? C5 C17 C1 119.7(13) . . ? C15 C45 C12 119.3(17) . . ? C15 C45 H45A 120.3 . . ? C12 C45 H45A 120.3 . . ? C7 C100 C101 119(3) . . ? C15 C101 C100 117(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.050 _refine_diff_density_min -0.902 _refine_diff_density_rms 0.186 # SQUEEZE RESULTS (APPEND TO CIF) loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.051 0.000 0.078 437.3 5.0 2 0.132 0.500 0.578 437.3 5.8 _platon_squeeze_details ; ; # Attachment '- Compound 5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 820351' #TrackingRef '- Compound 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H127 N0 Na10 O93.50 P8 V10' _chemical_formula_weight 3091.48 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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' P P 0.1023 0.0942 '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 14.9555(15) _cell_length_b 15.1182(15) _cell_length_c 17.0608(17) _cell_angle_alpha 109.381(2) _cell_angle_beta 106.595(2) _cell_angle_gamma 107.314(2) _cell_volume 3141.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5495 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 25.015 _exptl_crystal_description cube _exptl_crystal_colour green _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1575 _exptl_absorpt_coefficient_mu 0.955 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5 _exptl_absorpt_correction_T_max 0.6 _exptl_absorpt_process_details 'SABAS Bruker 2001' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Smart Apex' _diffrn_measurement_method 'area detector, omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33332 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11020 _reflns_number_gt 8149 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker Smart' _computing_cell_refinement 'Bruker Smart' _computing_data_reduction 'Bruker Smart' _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. ; _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^)+(0.1725P)^2^+39.9486P] 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 11020 _refine_ls_number_parameters 671 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1327 _refine_ls_R_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.3064 _refine_ls_wR_factor_gt 0.2895 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.020 _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 V2 V -0.24238(10) 0.96459(11) 0.66692(10) 0.0182(3) Uani 1 1 d . . . V3 V -0.00525(10) 0.94679(11) 0.65925(10) 0.0188(3) Uani 1 1 d . . . V4 V 0.32998(10) 1.29047(10) 1.33672(10) 0.0171(3) Uani 1 1 d . . . V5 V 0.09459(11) 1.30794(11) 1.34531(10) 0.0190(4) Uani 1 1 d . . . V1 V -0.21614(10) 0.78157(10) 0.56585(9) 0.0163(3) Uani 1 1 d . . . P1 P -0.01341(17) 1.15684(18) 0.78412(16) 0.0231(5) Uani 1 1 d . . . P2 P -0.14505(17) 1.13118(18) 1.23027(16) 0.0232(5) Uani 1 1 d . . . P3 P 0.20384(17) 1.38689(18) 1.22669(16) 0.0223(5) Uani 1 1 d . . . P4 P -0.36051(17) 0.90386(17) 0.78752(16) 0.0227(5) Uani 1 1 d . . . Na1 Na -0.2788(3) 0.7890(3) 0.3383(2) 0.0282(8) Uani 1 1 d . . . Na2 Na -0.3913(3) 0.5502(3) 0.3322(2) 0.0254(8) Uani 1 1 d . . . Na3 Na -0.3086(5) 0.3782(5) 0.3445(5) 0.0813(18) Uani 1 1 d . . . Na5 Na -0.3418(7) 0.9776(6) 0.3726(6) 0.101(2) Uani 1 1 d U . . O1W O -0.3476(7) 0.3521(7) -0.2130(6) 0.054(2) Uani 1 1 d . . . O1 O -0.3077(4) 0.8118(4) 0.6167(4) 0.0189(12) Uani 1 1 d . . . O2 O -0.1493(4) 0.9284(4) 0.6150(4) 0.0191(12) Uani 1 1 d . . . O4 O 0.2361(4) 1.3192(4) 1.3901(4) 0.0186(12) Uani 1 1 d . . . O3 O -0.0775(4) 0.7971(5) 0.6082(4) 0.0220(13) Uani 1 1 d . . . O5 O -0.2730(4) 0.7283(4) 0.4557(4) 0.0204(13) Uani 1 1 d . . . O44 O -0.1060(5) 0.8082(5) 0.3683(5) 0.0305(15) Uani 1 1 d . . . O45 O -0.1959(5) 0.9677(5) 0.4642(5) 0.0310(15) Uani 1 1 d . . . O46 O -0.4384(6) 0.7981(7) 0.3469(6) 0.056(2) Uani 1 1 d . . . O47 O -0.3903(5) 0.6145(5) 0.2213(4) 0.0291(15) Uani 1 1 d . . . O43 O -0.5293(5) 0.5668(6) 0.3723(5) 0.0411(18) Uani 1 1 d . . . O40 O -0.4758(5) 0.3675(5) 0.2418(5) 0.0314(15) Uani 1 1 d . . . O41 O -0.3513(5) 0.4942(5) 0.4498(4) 0.0258(14) Uani 1 1 d . . . O42 O -0.2323(7) 0.5338(7) 0.3323(6) 0.052(2) Uani 1 1 d . . . O9 O 0.4418(4) 1.3842(4) 1.4114(4) 0.0226(13) Uani 1 1 d . . . O16 O -0.3583(5) 0.7977(5) 0.7594(4) 0.0244(13) Uani 1 1 d . . . O20 O 0.2649(5) 1.5032(5) 1.2663(5) 0.0354(16) Uani 1 1 d . . . O14 O 0.1161(5) 1.3598(5) 1.2560(4) 0.0250(14) Uani 1 1 d . . . O7 O 0.0292(5) 0.9691(5) 0.5841(4) 0.0274(14) Uani 1 1 d . . . O11 O 0.0322(5) 1.0788(5) 0.7611(5) 0.0315(15) Uani 1 1 d . . . O10 O -0.1290(5) 1.1035(5) 0.7580(4) 0.0266(14) Uani 1 1 d . . . O18 O 0.0108(5) 1.2307(5) 0.7429(5) 0.0318(15) Uani 1 1 d . . . O6 O -0.3164(5) 0.9856(5) 0.5928(5) 0.0317(15) Uani 1 1 d . . . O17 O -0.2893(6) 0.9739(5) 0.7622(5) 0.0347(16) Uani 1 1 d . . . O39 O -0.4685(5) 0.8945(6) 0.7507(5) 0.0369(17) Uani 1 1 d . . . O15 O 0.2736(5) 1.3337(6) 1.2471(5) 0.0326(16) Uani 1 1 d . . . O8 O 0.0984(5) 1.4058(5) 1.4243(5) 0.0295(15) Uani 1 1 d . . . O29 O -0.2821(5) 0.8846(6) 0.2550(5) 0.043(2) Uani 1 1 d . . . O34 O -0.2182(5) 1.1622(5) 1.2677(5) 0.0329(15) Uani 1 1 d . . . O12 O -0.1188(5) 1.0523(5) 1.2584(4) 0.0258(14) Uani 1 1 d . . . O13 O -0.0479(5) 1.2264(6) 1.2565(6) 0.048(2) Uani 1 1 d . . . O50 O -0.4441(6) 0.3699(6) -0.0995(6) 0.049(2) Uani 1 1 d . . . O56 O -0.2339(7) 0.4348(7) 0.4320(6) 0.057(2) Uani 1 1 d . . . O58 O -0.2142(10) 1.1523(10) 0.4229(9) 0.095(4) Uiso 1 1 d . . . O63 O -0.3772(10) 0.2606(10) 0.4033(9) 0.032(3) Uiso 0.50 1 d P . . O65 O -0.1278(17) 0.3782(17) 0.4010(14) 0.072(6) Uiso 0.50 1 d P . . O66 O -0.3726(10) 0.2088(10) 0.2090(9) 0.028(3) Uiso 0.50 1 d P . . O69 O -0.2850(12) 1.0731(12) 0.4972(10) 0.039(3) Uiso 0.50 1 d P . . O100 O -0.4165(13) 1.0088(13) 0.2264(11) 0.046(4) Uiso 0.50 1 d P . . O205 O -0.493(3) 0.961(3) 0.297(2) 0.056(9) Uiso 0.25 1 d P . . O59 O -0.5137(10) 0.2428(10) -0.4760(8) 0.089(3) Uiso 1 1 d . . . O61 O -0.2696(12) 0.2083(12) -0.2604(10) 0.040(3) Uiso 0.50 1 d P . . C1 C -0.3042(6) 0.9691(6) 0.9110(6) 0.0205(18) Uani 1 1 d . . . C2 C -0.2778(6) 1.0775(7) 0.9609(6) 0.0219(18) Uani 1 1 d . . . C3 C -0.2998(8) 1.1363(7) 0.9139(7) 0.027(2) Uani 1 1 d . . . H3 H -0.3325 1.1038 0.8500 0.032 Uiso 1 1 calc R . . C4 C -0.2735(8) 1.2400(8) 0.9616(7) 0.033(2) Uani 1 1 d . . . H4 H -0.2873 1.2775 0.9300 0.040 Uiso 1 1 calc R . . C5 C -0.2258(8) 1.2897(7) 1.0576(7) 0.031(2) Uani 1 1 d . . . H5 H -0.2084 1.3600 1.0900 0.037 Uiso 1 1 calc R . . C6 C -0.2046(7) 1.2335(7) 1.1044(6) 0.0235(19) Uani 1 1 d . . . H6A H -0.1729 1.2669 1.1682 0.028 Uiso 1 1 calc R . . C7 C -0.2296(6) 1.1281(7) 1.0580(6) 0.0209(18) Uani 1 1 d . . . C8 C -0.2818(8) 0.9152(7) 0.9601(7) 0.031(2) Uani 1 1 d . . . H8 H -0.2978 0.8451 0.9285 0.037 Uiso 1 1 calc R . . C9 C 0.0392(7) 1.2818(8) 1.0544(7) 0.031(2) Uani 1 1 d . . . H9 H -0.0021 1.2817 1.0861 0.038 Uiso 1 1 calc R . . C10 C 0.1451(6) 1.3300(7) 1.1029(6) 0.0216(18) Uani 1 1 d . . . C11 C 0.2091(6) 1.3325(7) 1.0540(6) 0.0217(18) Uani 1 1 d . . . C12 C 0.3191(7) 1.3816(7) 1.0996(6) 0.0212(18) Uani 1 1 d . . . H12 H 0.3517 1.4157 1.1635 0.025 Uiso 1 1 calc R . . C13 C 0.3781(7) 1.3793(7) 1.0506(7) 0.0242(19) Uani 1 1 d . . . H13 H 0.4500 1.4127 1.0819 0.029 Uiso 1 1 calc R . . C14 C 0.3320(7) 1.3281(7) 0.9555(7) 0.0252(19) Uani 1 1 d . . . H14 H 0.3728 1.3258 0.9234 0.030 Uiso 1 1 calc R . . C15 C 0.2240(6) 1.2798(7) 0.9077(6) 0.0228(19) Uani 1 1 d . . . H15 H 0.1935 1.2470 0.8438 0.027 Uiso 1 1 calc R . . C16 C 0.1610(6) 1.2801(6) 0.9553(6) 0.0200(18) Uani 1 1 d . . . C17 C -0.2080(6) 1.0682(7) 1.1061(7) 0.0233(19) Uani 1 1 d . . . C18 C -0.2347(7) 0.9653(7) 1.0577(7) 0.028(2) Uani 1 1 d . . . H18 H -0.2219 0.9272 1.0890 0.034 Uiso 1 1 calc R . . C19 C 0.0493(6) 1.2289(7) 0.9076(6) 0.0227(18) Uani 1 1 d . . . C20 C -0.0083(7) 1.2326(8) 0.9574(7) 0.031(2) Uani 1 1 d . . . H20 H -0.0802 1.2021 0.9267 0.037 Uiso 1 1 calc R . . Na6 Na -0.3428(7) 0.4751(7) 0.1014(6) 0.101(2) Uiso 1 1 d . . . O2W O -0.1343(7) 0.5637(7) 0.2052(6) 0.055(2) Uiso 1 1 d . . . O3W O 0.1040(7) 0.6626(7) 0.4445(6) 0.051(2) Uiso 1 1 d . . . O4W O 0.4653(8) 1.1791(8) 0.8942(7) 0.071(3) Uiso 1 1 d . . . O5W O 0.0408(8) 1.2971(8) 0.5437(7) 0.071(3) Uiso 1 1 d . . . O6W O -0.4467(10) 0.2761(10) 0.0860(8) 0.085(3) Uiso 1 1 d . . . O7W O 0.1523(11) 0.7658(11) 0.3691(9) 0.099(4) Uiso 1 1 d . . . O8W O -0.0031(12) 0.4932(12) 0.2967(10) 0.113(5) Uiso 1 1 d . . . O9W O 0.2490(13) 0.6149(13) 0.4330(11) 0.119(5) Uiso 1 1 d . . . O10W O 0.5054(15) 1.1142(14) 0.9888(13) 0.058(5) Uiso 0.50 1 d P . . 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 V2 0.0110(7) 0.0164(7) 0.0258(8) 0.0121(6) 0.0068(6) 0.0025(6) V3 0.0110(7) 0.0199(7) 0.0251(8) 0.0148(6) 0.0075(6) 0.0011(6) V4 0.0110(7) 0.0143(7) 0.0236(8) 0.0106(6) 0.0071(6) 0.0006(6) V5 0.0123(7) 0.0167(7) 0.0277(8) 0.0124(6) 0.0084(6) 0.0034(6) V1 0.0114(7) 0.0138(7) 0.0212(7) 0.0100(6) 0.0060(6) 0.0010(5) P1 0.0119(10) 0.0229(12) 0.0266(12) 0.0111(10) 0.0063(9) -0.0001(9) P2 0.0123(10) 0.0205(11) 0.0292(12) 0.0147(10) 0.0027(9) -0.0003(9) P3 0.0161(11) 0.0237(12) 0.0274(12) 0.0155(10) 0.0092(9) 0.0048(9) P4 0.0186(11) 0.0186(11) 0.0303(13) 0.0122(10) 0.0133(10) 0.0036(9) Na1 0.0209(18) 0.0269(19) 0.0295(19) 0.0158(16) 0.0082(15) 0.0005(15) Na2 0.0272(19) 0.0201(17) 0.0276(19) 0.0132(15) 0.0117(15) 0.0060(15) Na3 0.076(4) 0.077(4) 0.099(5) 0.044(4) 0.041(4) 0.036(4) Na5 0.101(2) 0.100(2) 0.103(2) 0.0476(14) 0.0424(14) 0.0440(14) O1W 0.062(6) 0.048(5) 0.075(6) 0.038(5) 0.039(5) 0.033(4) O1 0.014(3) 0.018(3) 0.022(3) 0.011(2) 0.007(2) 0.003(2) O2 0.012(3) 0.020(3) 0.022(3) 0.011(2) 0.007(2) 0.002(2) O4 0.011(3) 0.016(3) 0.024(3) 0.009(2) 0.006(2) 0.001(2) O3 0.016(3) 0.022(3) 0.028(3) 0.015(3) 0.011(3) 0.002(2) O5 0.015(3) 0.017(3) 0.035(3) 0.018(3) 0.015(3) 0.004(2) O44 0.026(3) 0.024(3) 0.043(4) 0.014(3) 0.020(3) 0.007(3) O45 0.027(3) 0.034(4) 0.036(4) 0.022(3) 0.016(3) 0.009(3) O46 0.040(5) 0.064(6) 0.059(5) 0.025(5) 0.017(4) 0.025(4) O47 0.028(4) 0.030(4) 0.029(3) 0.018(3) 0.012(3) 0.007(3) O43 0.028(4) 0.061(5) 0.055(5) 0.043(4) 0.022(4) 0.020(4) O40 0.032(4) 0.025(3) 0.035(4) 0.015(3) 0.016(3) 0.008(3) O41 0.019(3) 0.023(3) 0.030(3) 0.011(3) 0.010(3) 0.003(3) O42 0.051(5) 0.067(6) 0.069(6) 0.041(5) 0.041(5) 0.035(5) O9 0.011(3) 0.018(3) 0.033(3) 0.013(3) 0.009(3) -0.002(2) O16 0.020(3) 0.021(3) 0.028(3) 0.011(3) 0.013(3) 0.001(3) O20 0.021(3) 0.025(4) 0.052(4) 0.016(3) 0.015(3) 0.002(3) O14 0.018(3) 0.028(3) 0.038(4) 0.020(3) 0.014(3) 0.012(3) O7 0.020(3) 0.028(3) 0.032(4) 0.019(3) 0.011(3) 0.002(3) O11 0.017(3) 0.030(4) 0.032(4) 0.007(3) 0.006(3) 0.005(3) O10 0.017(3) 0.026(3) 0.033(4) 0.013(3) 0.011(3) 0.004(3) O18 0.024(3) 0.033(4) 0.035(4) 0.020(3) 0.013(3) 0.004(3) O6 0.021(3) 0.028(4) 0.042(4) 0.022(3) 0.006(3) 0.008(3) O17 0.045(4) 0.020(3) 0.042(4) 0.012(3) 0.030(4) 0.009(3) O39 0.028(4) 0.037(4) 0.042(4) 0.020(3) 0.012(3) 0.011(3) O15 0.029(4) 0.049(4) 0.033(4) 0.027(3) 0.018(3) 0.020(3) O8 0.023(3) 0.026(3) 0.040(4) 0.014(3) 0.013(3) 0.012(3) O29 0.028(4) 0.041(4) 0.041(4) 0.029(4) 0.002(3) -0.008(3) O34 0.035(4) 0.032(4) 0.030(4) 0.015(3) 0.011(3) 0.016(3) O12 0.017(3) 0.024(3) 0.032(3) 0.018(3) 0.006(3) 0.002(3) O13 0.020(4) 0.035(4) 0.061(5) 0.037(4) -0.010(3) -0.013(3) O50 0.040(4) 0.035(4) 0.069(6) 0.027(4) 0.018(4) 0.014(4) O56 0.046(5) 0.045(5) 0.066(6) 0.012(4) 0.018(5) 0.023(4) C1 0.019(4) 0.016(4) 0.028(5) 0.011(4) 0.012(4) 0.006(3) C2 0.017(4) 0.016(4) 0.038(5) 0.015(4) 0.014(4) 0.008(3) C3 0.035(5) 0.030(5) 0.031(5) 0.020(4) 0.020(4) 0.019(4) C4 0.045(6) 0.034(6) 0.041(6) 0.026(5) 0.024(5) 0.029(5) C5 0.040(6) 0.022(5) 0.038(6) 0.014(4) 0.020(5) 0.020(4) C6 0.020(4) 0.022(5) 0.028(5) 0.012(4) 0.009(4) 0.009(4) C7 0.014(4) 0.025(5) 0.031(5) 0.019(4) 0.012(4) 0.007(4) C8 0.034(5) 0.015(4) 0.055(7) 0.022(4) 0.026(5) 0.010(4) C9 0.019(5) 0.040(6) 0.038(6) 0.020(5) 0.017(4) 0.008(4) C10 0.014(4) 0.021(4) 0.035(5) 0.016(4) 0.012(4) 0.010(4) C11 0.014(4) 0.020(4) 0.037(5) 0.022(4) 0.010(4) 0.004(3) C12 0.018(4) 0.020(4) 0.023(4) 0.010(4) 0.008(4) 0.005(4) C13 0.014(4) 0.019(4) 0.040(5) 0.016(4) 0.011(4) 0.004(3) C14 0.017(4) 0.030(5) 0.035(5) 0.019(4) 0.013(4) 0.011(4) C15 0.012(4) 0.021(4) 0.028(5) 0.011(4) 0.008(4) -0.002(3) C16 0.016(4) 0.012(4) 0.032(5) 0.013(4) 0.009(4) 0.003(3) C17 0.014(4) 0.024(5) 0.042(5) 0.022(4) 0.017(4) 0.009(4) C18 0.026(5) 0.020(5) 0.034(5) 0.017(4) 0.010(4) 0.002(4) C19 0.015(4) 0.019(4) 0.030(5) 0.011(4) 0.009(4) 0.003(3) C20 0.011(4) 0.042(6) 0.037(5) 0.022(5) 0.011(4) 0.003(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V2 O6 1.613(6) . ? V2 O17 1.926(7) . ? V2 O2 1.964(6) . ? V2 O1 1.972(6) . ? V2 O10 1.977(6) . ? V2 V1 2.941(2) . ? V3 O7 1.607(6) . ? V3 O3 1.936(6) . ? V3 O11 1.948(7) . ? V3 O2 1.966(6) . ? V3 O12 1.974(6) 2_577 ? V3 V1 2.9196(19) . ? V4 O9 1.613(6) . ? V4 O15 1.932(7) . ? V4 O1 1.948(6) 2_577 ? V4 O4 1.953(6) . ? V4 O16 1.982(6) 2_577 ? V4 V1 2.9263(19) 2_577 ? V5 O8 1.609(7) . ? V5 O13 1.926(7) . ? V5 O4 1.967(6) . ? V5 O3 1.982(6) 2_577 ? V5 O14 1.991(6) . ? V5 V1 2.947(2) 2_577 ? V1 O5 1.606(6) . ? V1 O4 1.895(6) 2_577 ? V1 O2 1.897(6) . ? V1 O3 1.902(6) . ? V1 O1 1.904(6) . ? V1 V4 2.9263(19) 2_577 ? V1 V5 2.947(2) 2_577 ? P1 O18 1.516(7) . ? P1 O10 1.526(6) . ? P1 O11 1.528(7) . ? P1 C19 1.801(9) . ? P2 O34 1.527(7) . ? P2 O13 1.530(7) . ? P2 O12 1.535(6) . ? P2 C17 1.809(10) . ? P3 O20 1.512(7) . ? P3 O14 1.526(6) . ? P3 O15 1.527(7) . ? P3 C10 1.804(9) . ? P4 O39 1.500(7) . ? P4 O16 1.529(7) . ? P4 O17 1.529(7) . ? P4 C1 1.798(9) . ? Na1 O29 2.340(8) . ? Na1 O47 2.390(7) . ? Na1 O44 2.393(7) . ? Na1 O5 2.456(7) . ? Na1 O45 2.466(8) . ? Na1 O46 2.474(9) . ? Na1 Na5 3.189(9) . ? Na1 Na2 3.452(5) . ? Na2 O40 2.364(7) . ? Na2 O47 2.398(7) . ? Na2 O43 2.406(8) . ? Na2 O41 2.417(7) . ? Na2 O42 2.464(9) . ? Na2 O5 2.468(7) . ? Na2 Na3 3.235(7) . ? Na2 Na6 4.060(9) . ? Na3 O56 1.356(11) . ? Na3 O42 2.396(11) . ? Na3 O63 2.430(15) . ? Na3 O41 2.439(9) . ? Na3 O66 2.483(14) . ? Na3 O40 2.534(10) . ? Na3 O65 2.60(2) . ? Na5 O69 1.878(17) . ? Na5 O205 2.15(4) . ? Na5 O45 2.372(11) . ? Na5 O58 2.432(16) . ? Na5 O46 2.482(13) . ? Na5 O29 2.589(12) . ? Na5 O100 2.682(18) . ? O1 V4 1.948(6) 2_577 ? O4 V1 1.895(6) 2_577 ? O3 V5 1.982(6) 2_577 ? O47 Na6 2.826(11) . ? O16 V4 1.982(6) 2_577 ? O12 V3 1.974(6) 2_577 ? O50 Na6 2.924(12) . ? C1 C8 1.391(13) . ? C1 C2 1.436(12) . ? C2 C7 1.413(13) . ? C2 C3 1.428(12) . ? C3 C4 1.371(14) . ? C3 H3 0.9300 . ? C4 C5 1.397(14) . ? C4 H4 0.9300 . ? C5 C6 1.388(13) . ? C5 H5 0.9300 . ? C6 C7 1.394(13) . ? C6 H6A 0.9300 . ? C7 C17 1.453(12) . ? C8 C18 1.420(14) . ? C8 H8 0.9300 . ? C9 C10 1.374(13) . ? C9 C20 1.411(14) . ? C9 H9 0.9300 . ? C10 C11 1.440(12) . ? C11 C12 1.422(12) . ? C11 C16 1.436(13) . ? C12 C13 1.377(12) . ? C12 H12 0.9300 . ? C13 C14 1.386(14) . ? C13 H13 0.9300 . ? C14 C15 1.399(12) . ? C14 H14 0.9300 . ? C15 C16 1.409(12) . ? C15 H15 0.9300 . ? C16 C19 1.445(12) . ? C17 C18 1.362(13) . ? C18 H18 0.9300 . ? C19 C20 1.373(13) . ? C20 H20 0.9300 . ? Na6 O2W 2.728(12) . ? Na6 O6W 2.828(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 V2 O17 108.2(4) . . ? O6 V2 O2 105.0(3) . . ? O17 V2 O2 146.4(3) . . ? O6 V2 O1 103.4(3) . . ? O17 V2 O1 88.6(3) . . ? O2 V2 O1 79.3(2) . . ? O6 V2 O10 105.0(3) . . ? O17 V2 O10 85.2(3) . . ? O2 V2 O10 90.7(3) . . ? O1 V2 O10 151.5(3) . . ? O6 V2 V1 108.0(3) . . ? O17 V2 V1 122.2(2) . . ? O2 V2 V1 39.53(17) . . ? O1 V2 V1 39.80(17) . . ? O10 V2 V1 125.59(19) . . ? O7 V3 O3 106.4(3) . . ? O7 V3 O11 109.1(3) . . ? O3 V3 O11 144.2(3) . . ? O7 V3 O2 102.6(3) . . ? O3 V3 O2 80.1(2) . . ? O11 V3 O2 88.4(3) . . ? O7 V3 O12 102.9(3) . 2_577 ? O3 V3 O12 90.8(3) . 2_577 ? O11 V3 O12 85.3(3) . 2_577 ? O2 V3 O12 154.4(3) . 2_577 ? O7 V3 V1 109.0(2) . . ? O3 V3 V1 40.05(18) . . ? O11 V3 V1 120.8(2) . . ? O2 V3 V1 40.01(17) . . ? O12 V3 V1 126.75(18) 2_577 . ? O9 V4 O15 107.2(3) . . ? O9 V4 O1 104.8(3) . 2_577 ? O15 V4 O1 147.7(3) . 2_577 ? O9 V4 O4 103.4(3) . . ? O15 V4 O4 88.7(3) . . ? O1 V4 O4 79.8(2) 2_577 . ? O9 V4 O16 104.9(3) . 2_577 ? O15 V4 O16 85.0(3) . 2_577 ? O1 V4 O16 90.9(3) 2_577 2_577 ? O4 V4 O16 151.6(3) . 2_577 ? O9 V4 V1 108.6(2) . 2_577 ? O15 V4 V1 122.3(2) . 2_577 ? O1 V4 V1 40.01(17) 2_577 2_577 ? O4 V4 V1 39.78(17) . 2_577 ? O16 V4 V1 125.78(18) 2_577 2_577 ? O8 V5 O13 106.7(4) . . ? O8 V5 O4 104.9(3) . . ? O13 V5 O4 148.0(3) . . ? O8 V5 O3 103.6(3) . 2_577 ? O13 V5 O3 88.5(3) . 2_577 ? O4 V5 O3 79.0(2) . 2_577 ? O8 V5 O14 103.2(3) . . ? O13 V5 O14 86.2(3) . . ? O4 V5 O14 91.8(2) . . ? O3 V5 O14 153.1(3) 2_577 . ? O8 V5 V1 108.4(2) . 2_577 ? O13 V5 V1 122.4(2) . 2_577 ? O4 V5 V1 39.38(17) . 2_577 ? O3 V5 V1 39.65(17) 2_577 2_577 ? O14 V5 V1 126.73(18) . 2_577 ? O5 V1 O4 111.5(3) . 2_577 ? O5 V1 O2 110.4(3) . . ? O4 V1 O2 138.0(3) 2_577 . ? O5 V1 O3 111.6(3) . . ? O4 V1 O3 82.8(2) 2_577 . ? O2 V1 O3 82.7(3) . . ? O5 V1 O1 110.2(3) . . ? O4 V1 O1 82.4(2) 2_577 . ? O2 V1 O1 82.7(2) . . ? O3 V1 O1 138.2(3) . . ? O5 V1 V3 118.5(2) . . ? O4 V1 V3 114.07(18) 2_577 . ? O2 V1 V3 41.80(17) . . ? O3 V1 V3 40.90(18) . . ? O1 V1 V3 114.74(18) . . ? O5 V1 V4 118.3(2) . 2_577 ? O4 V1 V4 41.25(17) 2_577 2_577 ? O2 V1 V4 114.08(18) . 2_577 ? O3 V1 V4 114.36(18) . 2_577 ? O1 V1 V4 41.11(17) . 2_577 ? V3 V1 V4 123.20(6) . 2_577 ? O5 V1 V2 116.9(2) . . ? O4 V1 V2 114.57(19) 2_577 . ? O2 V1 V2 41.22(17) . . ? O3 V1 V2 114.69(19) . . ? O1 V1 V2 41.53(17) . . ? V3 V1 V2 77.56(5) . . ? V4 V1 V2 77.13(5) 2_577 . ? O5 V1 V5 119.2(2) . 2_577 ? O4 V1 V5 41.19(17) 2_577 2_577 ? O2 V1 V5 114.57(18) . 2_577 ? O3 V1 V5 41.66(18) . 2_577 ? O1 V1 V5 114.08(18) . 2_577 ? V3 V1 V5 76.88(5) . 2_577 ? V4 V1 V5 76.79(5) 2_577 2_577 ? V2 V1 V5 123.96(6) . 2_577 ? O18 P1 O10 112.3(4) . . ? O18 P1 O11 111.4(4) . . ? O10 P1 O11 112.2(4) . . ? O18 P1 C19 109.5(4) . . ? O10 P1 C19 106.2(4) . . ? O11 P1 C19 104.8(4) . . ? O34 P2 O13 111.7(5) . . ? O34 P2 O12 111.8(4) . . ? O13 P2 O12 112.1(4) . . ? O34 P2 C17 109.2(4) . . ? O13 P2 C17 105.1(4) . . ? O12 P2 C17 106.7(4) . . ? O20 P3 O14 111.9(4) . . ? O20 P3 O15 112.1(4) . . ? O14 P3 O15 112.5(4) . . ? O20 P3 C10 109.3(4) . . ? O14 P3 C10 106.9(4) . . ? O15 P3 C10 103.7(4) . . ? O39 P4 O16 112.2(4) . . ? O39 P4 O17 111.9(4) . . ? O16 P4 O17 111.9(4) . . ? O39 P4 C1 109.1(4) . . ? O16 P4 C1 106.9(4) . . ? O17 P4 C1 104.4(4) . . ? O29 Na1 O47 102.5(3) . . ? O29 Na1 O44 96.1(3) . . ? O47 Na1 O44 105.9(3) . . ? O29 Na1 O5 165.3(3) . . ? O47 Na1 O5 89.6(2) . . ? O44 Na1 O5 88.5(2) . . ? O29 Na1 O45 79.3(3) . . ? O47 Na1 O45 168.1(3) . . ? O44 Na1 O45 85.4(2) . . ? O5 Na1 O45 87.2(2) . . ? O29 Na1 O46 88.4(3) . . ? O47 Na1 O46 85.6(3) . . ? O44 Na1 O46 166.3(3) . . ? O5 Na1 O46 84.1(3) . . ? O45 Na1 O46 82.7(3) . . ? O29 Na1 Na5 53.2(3) . . ? O47 Na1 Na5 124.4(3) . . ? O44 Na1 Na5 123.9(3) . . ? O5 Na1 Na5 112.9(2) . . ? O45 Na1 Na5 47.5(2) . . ? O46 Na1 Na5 50.1(3) . . ? O29 Na1 Na2 145.5(2) . . ? O47 Na1 Na2 43.96(17) . . ? O44 Na1 Na2 101.0(2) . . ? O5 Na1 Na2 45.63(16) . . ? O45 Na1 Na2 131.5(2) . . ? O46 Na1 Na2 82.0(2) . . ? Na5 Na1 Na2 131.5(2) . . ? O40 Na2 O47 103.4(3) . . ? O40 Na2 O43 96.6(3) . . ? O47 Na2 O43 106.8(3) . . ? O40 Na2 O41 79.4(2) . . ? O47 Na2 O41 166.7(3) . . ? O43 Na2 O41 85.6(2) . . ? O40 Na2 O42 85.4(3) . . ? O47 Na2 O42 87.7(3) . . ? O43 Na2 O42 164.4(3) . . ? O41 Na2 O42 79.5(3) . . ? O40 Na2 O5 164.0(3) . . ? O47 Na2 O5 89.1(2) . . ? O43 Na2 O5 89.1(3) . . ? O41 Na2 O5 86.2(2) . . ? O42 Na2 O5 85.2(3) . . ? O40 Na2 Na3 50.9(2) . . ? O47 Na2 Na3 123.5(2) . . ? O43 Na2 Na3 123.5(2) . . ? O41 Na2 Na3 48.5(2) . . ? O42 Na2 Na3 47.4(2) . . ? O5 Na2 Na3 113.7(2) . . ? O40 Na2 Na1 146.4(2) . . ? O47 Na2 Na1 43.77(18) . . ? O43 Na2 Na1 100.4(2) . . ? O41 Na2 Na1 130.5(2) . . ? O42 Na2 Na1 85.9(2) . . ? O5 Na2 Na1 45.35(15) . . ? Na3 Na2 Na1 132.94(18) . . ? O40 Na2 Na6 70.7(2) . . ? O47 Na2 Na6 43.0(2) . . ? O43 Na2 Na6 136.6(2) . . ? O41 Na2 Na6 129.3(2) . . ? O42 Na2 Na6 58.6(2) . . ? O5 Na2 Na6 114.7(2) . . ? Na3 Na2 Na6 81.07(19) . . ? Na1 Na2 Na6 77.06(15) . . ? O56 Na3 O42 83.3(6) . . ? O56 Na3 O63 83.1(6) . . ? O42 Na3 O63 161.8(5) . . ? O56 Na3 O41 65.5(5) . . ? O42 Na3 O41 80.5(3) . . ? O63 Na3 O41 82.9(4) . . ? O56 Na3 O66 139.1(6) . . ? O42 Na3 O66 117.8(5) . . ? O63 Na3 O66 80.3(5) . . ? O41 Na3 O66 147.0(4) . . ? O56 Na3 O40 140.5(6) . . ? O42 Na3 O40 83.3(3) . . ? O63 Na3 O40 99.8(4) . . ? O41 Na3 O40 75.8(3) . . ? O66 Na3 O40 79.3(4) . . ? O56 Na3 O65 54.7(6) . . ? O42 Na3 O65 89.2(6) . . ? O63 Na3 O65 92.7(6) . . ? O41 Na3 O65 120.1(6) . . ? O66 Na3 O65 89.0(6) . . ? O40 Na3 O65 161.1(6) . . ? O56 Na3 Na2 98.5(5) . . ? O42 Na3 Na2 49.2(2) . . ? O63 Na3 Na2 121.6(4) . . ? O41 Na3 Na2 47.9(2) . . ? O66 Na3 Na2 122.0(4) . . ? O40 Na3 Na2 46.45(19) . . ? O65 Na3 Na2 135.3(5) . . ? O69 Na5 O205 111.7(11) . . ? O69 Na5 O45 67.4(5) . . ? O205 Na5 O45 167.1(11) . . ? O69 Na5 O58 62.2(6) . . ? O205 Na5 O58 108.9(11) . . ? O45 Na5 O58 82.4(4) . . ? O69 Na5 O46 110.9(6) . . ? O205 Na5 O46 84.0(10) . . ? O45 Na5 O46 84.4(4) . . ? O58 Na5 O46 166.7(5) . . ? O69 Na5 O29 139.0(6) . . ? O205 Na5 O29 108.0(10) . . ? O45 Na5 O29 76.2(3) . . ? O58 Na5 O29 95.4(5) . . ? O46 Na5 O29 82.9(4) . . ? O69 Na5 O100 127.5(7) . . ? O205 Na5 O100 48.5(11) . . ? O45 Na5 O100 142.9(5) . . ? O58 Na5 O100 78.8(5) . . ? O46 Na5 O100 113.2(5) . . ? O29 Na5 O100 74.1(4) . . ? O69 Na5 Na1 113.4(6) . . ? O205 Na5 Na1 124.0(10) . . ? O45 Na5 Na1 50.0(2) . . ? O58 Na5 Na1 120.5(4) . . ? O46 Na5 Na1 49.8(3) . . ? O29 Na5 Na1 46.4(2) . . ? O100 Na5 Na1 116.4(4) . . ? V1 O1 V4 98.9(3) . 2_577 ? V1 O1 V2 98.7(3) . . ? V4 O1 V2 137.8(3) 2_577 . ? V1 O2 V2 99.3(2) . . ? V1 O2 V3 98.2(3) . . ? V2 O2 V3 138.2(3) . . ? V1 O4 V4 99.0(3) 2_577 . ? V1 O4 V5 99.4(2) 2_577 . ? V4 O4 V5 137.0(3) . . ? V1 O3 V3 99.1(3) . . ? V1 O3 V5 98.7(3) . 2_577 ? V3 O3 V5 137.2(3) . 2_577 ? V1 O5 Na1 135.6(3) . . ? V1 O5 Na2 135.4(3) . . ? Na1 O5 Na2 89.0(2) . . ? Na5 O45 Na1 82.4(3) . . ? Na1 O46 Na5 80.1(3) . . ? Na1 O47 Na2 92.3(2) . . ? Na1 O47 Na6 128.6(3) . . ? Na2 O47 Na6 101.7(3) . . ? Na2 O40 Na3 82.6(3) . . ? Na2 O41 Na3 83.6(3) . . ? Na3 O42 Na2 83.5(3) . . ? P4 O16 V4 135.0(4) . 2_577 ? P3 O14 V5 134.0(4) . . ? P1 O11 V3 137.6(4) . . ? P1 O10 V2 134.6(4) . . ? P4 O17 V2 140.0(4) . . ? P3 O15 V4 140.8(4) . . ? Na1 O29 Na5 80.5(3) . . ? P2 O12 V3 136.1(4) . 2_577 ? P2 O13 V5 141.2(4) . . ? C8 C1 C2 118.7(8) . . ? C8 C1 P4 119.7(7) . . ? C2 C1 P4 121.5(7) . . ? C7 C2 C3 118.6(8) . . ? C7 C2 C1 120.4(8) . . ? C3 C2 C1 121.0(8) . . ? C4 C3 C2 120.9(9) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.3(9) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C6 C5 C4 119.5(9) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? C5 C6 C7 121.7(9) . . ? C5 C6 H6A 119.1 . . ? C7 C6 H6A 119.2 . . ? C6 C7 C2 119.0(8) . . ? C6 C7 C17 122.3(8) . . ? C2 C7 C17 118.7(8) . . ? C1 C8 C18 121.1(8) . . ? C1 C8 H8 119.5 . . ? C18 C8 H8 119.5 . . ? C10 C9 C20 121.5(8) . . ? C10 C9 H9 119.3 . . ? C20 C9 H9 119.3 . . ? C9 C10 C11 119.4(8) . . ? C9 C10 P3 120.6(7) . . ? C11 C10 P3 120.0(6) . . ? C12 C11 C16 118.2(8) . . ? C12 C11 C10 122.5(8) . . ? C16 C11 C10 119.3(8) . . ? C13 C12 C11 121.0(8) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C14 121.0(8) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C15 120.0(8) . . ? C13 C14 H14 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 C16 120.7(8) . . ? C14 C15 H15 119.6 . . ? C16 C15 H15 119.6 . . ? C15 C16 C11 119.1(8) . . ? C15 C16 C19 121.8(8) . . ? C11 C16 C19 119.1(8) . . ? C18 C17 C7 120.0(9) . . ? C18 C17 P2 120.2(7) . . ? C7 C17 P2 119.8(7) . . ? C17 C18 C8 121.0(8) . . ? C17 C18 H18 119.5 . . ? C8 C18 H18 119.5 . . ? C20 C19 C16 119.3(8) . . ? C20 C19 P1 120.4(7) . . ? C16 C19 P1 120.2(7) . . ? C19 C20 C9 121.4(8) . . ? C19 C20 H20 119.3 . . ? C9 C20 H20 119.3 . . ? O2W Na6 O47 97.9(3) . . ? O2W Na6 O6W 113.1(4) . . ? O47 Na6 O6W 107.1(4) . . ? O2W Na6 O50 124.9(4) . . ? O47 Na6 O50 127.3(4) . . ? O6W Na6 O50 84.8(4) . . ? O2W Na6 Na2 90.5(3) . . ? O47 Na6 Na2 35.34(17) . . ? O6W Na6 Na2 78.6(3) . . ? O50 Na6 Na2 144.6(3) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 3.269 _refine_diff_density_min -1.639 _refine_diff_density_rms 0.226