Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _publ_contact_author_email p.nichols@sci.monash.edu.au _publ_contact_author_name 'Peter Nichols' _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name P.J.Nichols C.L.Raston data_compound1 _database_code_CSD 202923 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H88 N2 Na2 O55 S8' _chemical_formula_weight 2043.80 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.8958(1) _cell_length_b 12.0330(1) _cell_length_c 15.7894(2) _cell_angle_alpha 99.42 _cell_angle_beta 108.451(1) _cell_angle_gamma 90.123(1) _cell_volume 2111.53(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.607 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1064 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9514 _exptl_absorpt_correction_T_max 0.9609 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38710 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 28.33 _reflns_number_total 19318 _reflns_number_gt 15874 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 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^)+(0.1008P)^2^+4.7202P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.03(7) _refine_ls_number_reflns 19318 _refine_ls_number_parameters 1162 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1860 _refine_ls_wR_factor_gt 0.1740 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.027 _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 S5 S 0.75584(11) 0.86466(10) 0.92046(8) 0.0149(2) Uani 1 1 d . . . S6 S 0.12605(11) 1.08700(12) 0.91395(9) 0.0211(3) Uani 1 1 d . . . S8 S 0.94351(15) 1.48436(13) 0.91751(11) 0.0298(3) Uani 1 1 d . . . S7 S 0.33498(12) 1.70844(11) 0.94166(10) 0.0261(3) Uani 1 1 d . . . C42 C 0.7388(4) 1.6146(4) 1.1624(3) 0.0117(9) Uani 1 1 d . . . H42A H 0.7637 1.6182 1.2276 0.014 Uiso 1 1 calc R . . H42B H 0.7600 1.6872 1.1509 0.014 Uiso 1 1 calc R . . C47 C 0.4215(4) 1.5030(4) 1.1254(3) 0.0108(9) Uani 1 1 d . . . C45 C 0.4180(5) 1.6282(4) 1.0206(3) 0.0159(10) Uani 1 1 d . . . O29 O 0.7375(3) 1.2051(3) 1.2286(2) 0.0163(7) Uani 1 1 d . . . C38 C 0.8946(4) 1.4572(4) 1.0073(3) 0.0159(10) Uani 1 1 d . . . O30 O 0.5308(3) 1.2768(3) 1.2350(2) 0.0150(7) Uani 1 1 d . . . C51 C 0.2537(5) 1.2561(4) 1.0478(3) 0.0176(10) Uani 1 1 d . . . H51 H 0.1912 1.3005 1.0247 0.021 Uiso 1 1 calc R . . O31 O 0.6100(3) 1.4828(3) 1.2368(2) 0.0160(7) Uani 1 1 d . . . C39 C 0.8343(4) 1.5385(4) 1.0450(3) 0.0154(10) Uani 1 1 d . . . H39 H 0.8127 1.6029 1.0196 0.018 Uiso 1 1 calc R . . O32 O 0.8213(3) 1.4123(3) 1.2382(2) 0.0167(7) Uani 1 1 d . . . C30 C 0.8364(4) 1.0583(4) 1.0450(3) 0.0123(9) Uani 1 1 d . . . H30 H 0.8981 1.0600 1.0208 0.015 Uiso 1 1 calc R . . C44 C 0.5409(4) 1.6474(4) 1.0541(3) 0.0133(9) Uani 1 1 d . . . H44 H 0.5793 1.6952 1.0300 0.016 Uiso 1 1 calc R . . C43 C 0.6050(4) 1.5934(4) 1.1244(3) 0.0135(9) Uani 1 1 d . . . O19 O 0.8759(3) 0.8753(3) 0.9164(3) 0.0251(9) Uani 1 1 d . . . O25 O 0.2363(6) 1.6426(7) 0.8859(6) 0.118(4) Uani 1 1 d . . . C34 C 0.6500(4) 0.9700(4) 1.0408(3) 0.0130(9) Uani 1 1 d . . . H34 H 0.5892 0.9143 1.0135 0.016 Uiso 1 1 calc R . . C29 C 0.7459(4) 0.9735(4) 1.0087(3) 0.0117(9) Uani 1 1 d . . . C54 C 0.4426(4) 1.1198(4) 1.1152(3) 0.0126(9) Uani 1 1 d . . . C37 C 0.9253(4) 1.3583(4) 1.0425(3) 0.0155(10) Uani 1 1 d . . . H37 H 0.9644 1.3042 1.0151 0.019 Uiso 1 1 calc R . . C36 C 0.8973(4) 1.3411(4) 1.1182(3) 0.0124(9) Uani 1 1 d . . . O17 O 0.6672(3) 0.8839(3) 0.8373(2) 0.0190(8) Uani 1 1 d . . . C56 C 0.5431(4) 1.0445(4) 1.1514(3) 0.0140(10) Uani 1 1 d . . . H56A H 0.5740 1.0658 1.2168 0.017 Uiso 1 1 calc R . . H56B H 0.5109 0.9671 1.1377 0.017 Uiso 1 1 calc R . . C40 C 0.8063(4) 1.5228(4) 1.1213(3) 0.0113(9) Uani 1 1 d . . . O18 O 0.7305(4) 0.7596(3) 0.9469(3) 0.0213(8) Uani 1 1 d . . . C35 C 0.9319(4) 1.2333(4) 1.1575(3) 0.0106(9) Uani 1 1 d . . . H35A H 1.0033 1.2073 1.1453 0.013 Uiso 1 1 calc R . . H35B H 0.9493 1.2499 1.2227 0.013 Uiso 1 1 calc R . . C49 C 0.3551(4) 1.4254(4) 1.1638(3) 0.0129(10) Uani 1 1 d . . . H49A H 0.3935 1.4335 1.2287 0.016 Uiso 1 1 calc R . . H49B H 0.2745 1.4486 1.1534 0.016 Uiso 1 1 calc R . . O23 O 0.4088(5) 1.7687(6) 0.9115(5) 0.080(2) Uani 1 1 d . . . C50 C 0.3515(4) 1.3030(4) 1.1215(3) 0.0124(9) Uani 1 1 d . . . C31 C 0.8343(4) 1.1406(4) 1.1176(3) 0.0115(9) Uani 1 1 d . . . C48 C 0.5453(4) 1.5253(4) 1.1613(3) 0.0095(9) Uani 1 1 d . . . C41 C 0.8398(4) 1.4258(4) 1.1586(3) 0.0133(9) Uani 1 1 d . . . C32 C 0.7383(4) 1.1336(4) 1.1517(3) 0.0128(9) Uani 1 1 d . . . C53 C 0.3427(4) 1.0752(4) 1.0416(3) 0.0156(10) Uani 1 1 d . . . H53 H 0.3385 0.9999 1.0146 0.019 Uiso 1 1 calc R . . C46 C 0.3594(4) 1.5570(4) 1.0552(3) 0.0161(10) Uani 1 1 d . . . H46 H 0.2773 1.5453 1.0311 0.019 Uiso 1 1 calc R . . C33 C 0.6452(4) 1.0496(4) 1.1135(3) 0.0092(9) Uani 1 1 d . . . C55 C 0.4429(5) 1.2319(4) 1.1557(3) 0.0140(10) Uani 1 1 d . . . S2 S 0.70044(10) 1.10243(10) 0.51753(8) 0.0163(3) Uani 1 1 d . . . S4 S -0.13368(10) 0.69160(10) 0.49371(8) 0.0153(2) Uani 1 1 d . . . S1 S 0.49581(10) 0.51432(10) 0.50803(8) 0.0145(2) Uani 1 1 d . . . S3 S 0.07286(10) 1.32368(10) 0.50457(8) 0.0145(2) Uani 1 1 d . . . C19 C -0.0022(4) 1.0465(4) 0.3070(3) 0.0118(9) Uani 1 1 d . . . C15 C 0.1832(4) 1.1394(4) 0.3119(3) 0.0145(10) Uani 1 1 d . . . C20 C 0.0919(4) 1.0563(4) 0.2737(3) 0.0118(9) Uani 1 1 d . . . C13 C 0.3883(4) 0.9602(4) 0.2726(3) 0.0129(9) Uani 1 1 d . . . O14 O 0.2996(3) 0.9188(3) 0.1935(2) 0.0178(7) Uani 1 1 d . . . O9 O 0.1183(3) 1.4271(3) 0.4860(3) 0.0225(8) Uani 1 1 d . . . O15 O 0.0895(3) 0.9832(3) 0.1953(2) 0.0164(7) Uani 1 1 d . . . C27 C -0.0058(4) 0.7604(4) 0.2659(3) 0.0100(9) Uani 1 1 d . . . C4 C 0.2916(4) 0.6676(4) 0.2652(3) 0.0128(9) Uani 1 1 d . . . C8 C 0.4801(4) 0.8912(4) 0.3060(3) 0.0103(9) Uani 1 1 d . . . O16 O 0.0182(3) 0.7752(3) 0.1887(2) 0.0171(7) Uani 1 1 d . . . O13 O 0.2288(3) 0.7063(3) 0.1876(2) 0.0157(7) Uani 1 1 d . . . O7 O 0.1494(4) 1.2944(3) 0.5895(3) 0.0240(8) Uani 1 1 d . . . C2 C 0.4750(4) 0.6415(4) 0.3754(3) 0.0108(9) Uani 1 1 d . . . H2 H 0.5570 0.6541 0.4001 0.013 Uiso 1 1 calc R . . C11 C 0.4820(4) 1.1169(4) 0.3894(3) 0.0136(10) Uani 1 1 d . . . H11 H 0.4824 1.1905 0.4188 0.016 Uiso 1 1 calc R . . C16 C 0.1758(4) 1.2198(4) 0.3838(3) 0.0142(10) Uani 1 1 d . . . H16 H 0.2351 1.2771 0.4103 0.017 Uiso 1 1 calc R . . C14 C 0.2868(4) 1.1485(4) 0.2757(3) 0.0118(9) Uani 1 1 d . . . H14A H 0.3179 1.2264 0.2908 0.014 Uiso 1 1 calc R . . H14B H 0.2578 1.1284 0.2101 0.014 Uiso 1 1 calc R . . C17 C 0.0797(4) 1.2151(4) 0.4167(3) 0.0157(10) Uani 1 1 d . . . O8 O -0.0510(3) 1.3241(3) 0.5007(3) 0.0226(8) Uani 1 1 d . . . C21 C -0.0980(5) 0.9513(4) 0.2673(3) 0.0153(10) Uani 1 1 d . . . H21A H -0.1700 0.9767 0.2789 0.018 Uiso 1 1 calc R . . H21B H -0.1150 0.9353 0.2021 0.018 Uiso 1 1 calc R . . C23 C -0.1023(4) 0.8215(4) 0.3763(3) 0.0122(9) Uani 1 1 d . . . H23 H -0.1428 0.8748 0.4032 0.015 Uiso 1 1 calc R . . C26 C 0.0256(4) 0.6597(4) 0.3001(3) 0.0109(9) Uani 1 1 d . . . C22 C -0.0668(4) 0.8434(4) 0.3041(3) 0.0120(9) Uani 1 1 d . . . O11 O -0.2505(3) 0.7347(3) 0.4719(2) 0.0181(7) Uani 1 1 d . . . C5 C 0.2285(4) 0.5990(4) 0.3014(3) 0.0105(9) Uani 1 1 d . . . C6 C 0.2936(4) 0.5545(4) 0.3771(3) 0.0136(9) Uani 1 1 d . . . H6 H 0.2547 0.5113 0.4042 0.016 Uiso 1 1 calc R . . O3 O 0.4474(3) 0.3989(3) 0.4903(2) 0.0203(8) Uani 1 1 d . . . C12 C 0.3880(4) 1.0734(4) 0.3129(3) 0.0125(9) Uani 1 1 d . . . C18 C -0.0071(4) 1.1286(4) 0.3796(3) 0.0133(9) Uani 1 1 d . . . H18 H -0.0694 1.1248 0.4030 0.016 Uiso 1 1 calc R . . C28 C 0.0946(4) 0.5733(4) 0.2612(3) 0.0142(10) Uani 1 1 d . . . H28A H 0.0709 0.5699 0.1961 0.017 Uiso 1 1 calc R . . H28B H 0.0754 0.4998 0.2724 0.017 Uiso 1 1 calc R . . C9 C 0.5744(4) 0.9378(4) 0.3813(3) 0.0105(9) Uani 1 1 d . . . H9 H 0.6372 0.8940 0.4049 0.013 Uiso 1 1 calc R . . C1 C 0.4156(4) 0.5740(4) 0.4125(3) 0.0129(9) Uani 1 1 d . . . C25 C -0.0106(4) 0.6417(4) 0.3733(3) 0.0133(9) Uani 1 1 d . . . H25 H 0.0101 0.5771 0.3986 0.016 Uiso 1 1 calc R . . C24 C -0.0772(4) 0.7201(4) 0.4080(3) 0.0147(10) Uani 1 1 d . . . C3 C 0.4132(4) 0.6908(4) 0.3012(3) 0.0112(9) Uani 1 1 d . . . O2 O 0.6212(3) 0.5212(3) 0.5134(3) 0.0231(8) Uani 1 1 d . . . O1 O 0.4763(3) 0.5809(3) 0.5870(2) 0.0190(7) Uani 1 1 d . . . O10 O -0.0543(3) 0.7511(4) 0.5785(3) 0.0299(9) Uani 1 1 d . . . O6 O 0.8037(3) 1.0584(3) 0.4967(3) 0.0243(8) Uani 1 1 d . . . O22 O 0.0238(4) 1.1367(5) 0.9288(4) 0.0465(14) Uani 1 1 d . . . O4 O 0.6829(4) 1.0613(4) 0.5955(3) 0.0283(9) Uani 1 1 d . . . C52 C 0.2499(4) 1.1432(4) 1.0088(3) 0.0164(10) Uani 1 1 d . . . C10 C 0.5756(4) 1.0502(4) 0.4220(3) 0.0141(9) Uani 1 1 d . . . O20 O 0.1539(5) 1.1073(6) 0.8370(3) 0.0616(18) Uani 1 1 d . . . O21 O 0.1200(5) 0.9663(4) 0.9165(4) 0.0598(17) Uani 1 1 d . . . O5 O 0.6997(4) 1.2256(3) 0.5323(3) 0.0311(10) Uani 1 1 d . . . Na1 Na 0.59515(18) 0.73665(17) 0.69912(13) 0.0201(4) Uani 1 1 d . . . Na2 Na 0.1301(2) 1.1757(3) 0.69599(18) 0.0482(8) Uani 1 1 d . . . O40 O 0.6353(3) 0.8310(3) 0.5855(3) 0.0240(8) Uani 1 1 d . . . O34 O 0.4051(4) 0.8463(3) 0.5097(3) 0.0259(9) Uani 1 1 d . . . O37 O 0.3956(4) 1.3073(4) 0.9110(3) 0.0438(12) Uani 1 1 d . . . O50 O 0.1987(4) 1.4018(5) 0.8419(4) 0.0540(15) Uani 1 1 d . . . O44 O 0.3890(3) 0.3285(3) 0.6258(3) 0.0257(8) Uani 1 1 d . . . O33 O 0.4182(3) 0.8309(3) 0.6524(2) 0.0216(8) Uani 1 1 d . . . O42 O -0.0015(4) 1.0112(5) 0.6410(4) 0.0468(12) Uani 1 1 d . . . O36 O 0.3409(3) 1.2037(3) 0.7711(3) 0.0239(8) Uani 1 1 d . . . O53 O 0.2538(5) 1.5982(4) 0.6182(4) 0.0466(12) Uani 1 1 d . . . C62 C 0.6304(6) 1.2361(5) 0.9127(4) 0.0302(13) Uani 1 1 d . . . H62A H 0.6281 1.2982 0.9597 0.036 Uiso 1 1 calc R . . H62B H 0.6985 1.1932 0.9372 0.036 Uiso 1 1 calc R . . O41 O 0.5515(4) 0.6376(4) 0.8113(3) 0.0335(10) Uani 1 1 d . . . O35 O 0.2368(4) 1.0454(4) 0.6075(3) 0.0330(9) Uani 1 1 d . . . O51 O 0.7996(6) 1.1464(7) 0.7945(4) 0.088(3) Uani 1 1 d . . . O54 O 0.7235(4) 1.3702(4) 0.4402(3) 0.0343(9) Uani 1 1 d . . . C59 C 0.1929(6) 0.9668(6) 0.5282(4) 0.0306(14) Uani 1 1 d . . . H59A H 0.2252 0.9859 0.4829 0.037 Uiso 1 1 calc R . . H59B H 0.1072 0.9690 0.5050 0.037 Uiso 1 1 calc R . . O38 O 0.6419(4) 1.2793(4) 0.8366(3) 0.0374(10) Uani 1 1 d . . . N2 N 0.5125(4) 1.0636(4) 0.8119(3) 0.0261(10) Uani 1 1 d . . . C58 C 0.2260(5) 0.8473(5) 0.5454(4) 0.0240(11) Uani 1 1 d . . . H58 H 0.1897 0.7929 0.4896 0.029 Uiso 1 1 calc R . . C57 C 0.3610(4) 0.8394(4) 0.5755(3) 0.0185(10) Uani 1 1 d . . . N1 N 0.1872(4) 0.8158(5) 0.6198(3) 0.0351(12) Uani 1 1 d . . . O39 O 0.7757(5) 0.6534(6) 0.7232(4) 0.073(2) Uani 1 1 d . . . O55 O 1.0602(4) 1.7757(4) 0.9984(4) 0.0461(12) Uani 1 1 d . . . C60 C 0.4072(5) 1.2271(5) 0.8487(4) 0.0258(12) Uani 1 1 d . . . C61 C 0.5169(5) 1.1605(5) 0.8839(4) 0.0265(12) Uani 1 1 d . . . H61 H 0.5116 1.1314 0.9371 0.032 Uiso 1 1 calc R . . O49 O 0.4753(4) 1.1173(3) 0.6382(3) 0.0294(9) Uani 1 1 d . . . O48 O 0.3103(4) 0.9334(3) 0.8023(3) 0.0307(9) Uani 1 1 d . . . O12 O -0.1347(4) 0.5693(3) 0.4877(3) 0.0340(10) Uani 1 1 d . . . O45 O -0.0394(6) 0.5186(4) 0.6595(4) 0.0546(14) Uani 1 1 d . . . O47 O -0.0460(8) 0.8465(6) 0.7579(4) 0.082(2) Uani 1 1 d . . . O52 O 0.5050(8) 1.4306(5) 0.7752(6) 0.109(4) Uani 1 1 d . . . O28 O 1.0439(7) 1.5685(7) 0.9606(6) 0.092(2) Uani 1 1 d . . . O46 O 0.0906(6) 0.6926(8) 0.7402(4) 0.084(2) Uani 1 1 d . . . O26 O 0.8550(10) 1.5454(8) 0.8651(6) 0.127(4) Uani 1 1 d . . . O43 O -0.0440(6) 1.2947(5) 0.6902(4) 0.0573(15) Uani 1 1 d . . . O24 O 0.2821(7) 1.7944(5) 0.9981(5) 0.0736(19) Uani 1 1 d . . . O27 O 0.9638(12) 1.3835(5) 0.8716(6) 0.139(5) Uani 1 1 d . . . C7 C 0.4782(4) 0.7681(4) 0.2640(3) 0.0124(9) Uani 1 1 d . . . H7A H 0.4404 0.7596 0.1990 0.015 Uiso 1 1 calc R . . H7B H 0.5592 0.7458 0.2750 0.015 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 S5 0.0157(6) 0.0119(5) 0.0169(6) 0.0001(4) 0.0059(5) 0.0029(4) S6 0.0114(6) 0.0283(7) 0.0185(6) -0.0079(5) 0.0035(5) -0.0008(5) S8 0.0411(9) 0.0306(8) 0.0309(7) 0.0183(6) 0.0237(7) 0.0133(6) S7 0.0192(6) 0.0200(7) 0.0342(8) 0.0162(6) -0.0042(6) -0.0015(5) C42 0.009(2) 0.008(2) 0.019(2) 0.0005(18) 0.0046(19) -0.0027(16) C47 0.013(2) 0.010(2) 0.010(2) -0.0001(17) 0.0049(18) 0.0010(17) C45 0.017(2) 0.012(2) 0.018(2) 0.0046(18) 0.003(2) 0.0079(18) O29 0.0177(17) 0.0148(17) 0.0145(17) -0.0029(13) 0.0052(15) 0.0007(14) C38 0.015(2) 0.017(2) 0.021(2) 0.0059(19) 0.011(2) 0.0065(18) O30 0.0161(17) 0.0169(17) 0.0105(16) 0.0027(13) 0.0022(14) -0.0008(13) C51 0.020(3) 0.016(2) 0.017(2) 0.0003(19) 0.007(2) 0.0028(19) O31 0.0171(17) 0.0132(17) 0.0152(17) 0.0047(13) 0.0005(14) 0.0041(13) C39 0.015(2) 0.011(2) 0.023(2) 0.0100(19) 0.007(2) 0.0036(18) O32 0.0185(17) 0.0171(17) 0.0165(17) 0.0050(14) 0.0075(15) 0.0016(13) C30 0.010(2) 0.010(2) 0.016(2) 0.0018(18) 0.0024(19) 0.0011(17) C44 0.015(2) 0.009(2) 0.017(2) 0.0029(17) 0.0056(19) -0.0001(17) C43 0.013(2) 0.017(2) 0.012(2) 0.0019(18) 0.0059(19) 0.0016(18) O19 0.0181(18) 0.029(2) 0.026(2) -0.0073(16) 0.0095(16) 0.0004(16) O25 0.049(4) 0.121(6) 0.157(8) 0.121(6) -0.053(4) -0.044(4) C34 0.009(2) 0.011(2) 0.018(2) 0.0045(18) 0.0019(19) 0.0016(17) C29 0.014(2) 0.013(2) 0.008(2) 0.0004(17) 0.0049(18) 0.0029(17) C54 0.018(2) 0.009(2) 0.014(2) 0.0020(17) 0.011(2) -0.0003(18) C37 0.016(2) 0.014(2) 0.017(2) 0.0032(19) 0.006(2) 0.0024(18) C36 0.004(2) 0.014(2) 0.017(2) 0.0026(18) 0.0000(18) -0.0012(16) O17 0.0230(19) 0.0182(18) 0.0137(17) 0.0006(13) 0.0042(15) 0.0057(14) C56 0.015(2) 0.007(2) 0.022(3) 0.0026(18) 0.009(2) -0.0061(17) C40 0.008(2) 0.007(2) 0.018(2) -0.0003(17) 0.0037(18) -0.0005(16) O18 0.031(2) 0.0091(16) 0.0223(19) 0.0015(14) 0.0062(17) 0.0031(14) C35 0.0030(19) 0.013(2) 0.015(2) 0.0034(18) 0.0015(18) 0.0013(16) C49 0.010(2) 0.008(2) 0.018(2) -0.0004(18) 0.002(2) 0.0011(17) O23 0.035(3) 0.105(5) 0.109(5) 0.091(5) -0.001(3) -0.014(3) C50 0.013(2) 0.013(2) 0.017(2) 0.0043(18) 0.011(2) 0.0018(17) C31 0.010(2) 0.014(2) 0.013(2) 0.0084(17) 0.0031(18) 0.0014(17) C48 0.008(2) 0.0053(19) 0.012(2) -0.0030(16) 0.0017(18) 0.0019(16) C41 0.011(2) 0.015(2) 0.013(2) -0.0013(18) 0.0059(19) -0.0040(18) C32 0.016(2) 0.014(2) 0.009(2) 0.0025(17) 0.0051(19) 0.0034(18) C53 0.014(2) 0.017(2) 0.016(2) 0.0003(19) 0.006(2) -0.0025(18) C46 0.014(2) 0.013(2) 0.020(3) 0.0001(19) 0.004(2) 0.0025(18) C33 0.008(2) 0.006(2) 0.015(2) 0.0057(17) 0.0031(18) 0.0022(16) C55 0.020(2) 0.013(2) 0.010(2) -0.0029(18) 0.009(2) -0.0055(19) S2 0.0149(6) 0.0160(6) 0.0175(6) -0.0003(5) 0.0061(5) -0.0007(4) S4 0.0116(5) 0.0172(6) 0.0219(6) 0.0087(5) 0.0096(5) 0.0038(4) S1 0.0128(5) 0.0141(5) 0.0164(6) 0.0051(4) 0.0032(5) 0.0002(4) S3 0.0138(6) 0.0126(6) 0.0198(6) 0.0036(5) 0.0088(5) 0.0026(4) C19 0.009(2) 0.011(2) 0.015(2) 0.0073(18) 0.0017(18) 0.0062(17) C15 0.015(2) 0.016(2) 0.017(2) 0.0092(19) 0.009(2) 0.0044(18) C20 0.015(2) 0.008(2) 0.016(2) 0.0090(17) 0.007(2) 0.0062(17) C13 0.005(2) 0.015(2) 0.019(2) 0.0079(19) 0.0037(19) -0.0002(17) O14 0.0162(17) 0.0195(18) 0.0151(17) 0.0019(14) 0.0021(15) 0.0000(14) O9 0.026(2) 0.0175(19) 0.028(2) 0.0077(15) 0.0113(17) 0.0008(15) O15 0.0205(18) 0.0152(17) 0.0148(16) 0.0038(13) 0.0067(15) -0.0003(14) C27 0.006(2) 0.010(2) 0.014(2) 0.0045(17) 0.0027(18) -0.0031(16) C4 0.017(2) 0.011(2) 0.015(2) 0.0056(18) 0.010(2) 0.0058(18) C8 0.011(2) 0.010(2) 0.014(2) 0.0029(17) 0.0093(19) 0.0018(17) O16 0.0180(17) 0.0221(18) 0.0127(16) 0.0046(14) 0.0064(14) -0.0012(14) O13 0.0174(17) 0.0216(18) 0.0090(15) 0.0055(13) 0.0041(14) 0.0024(14) O7 0.027(2) 0.026(2) 0.0212(19) 0.0051(15) 0.0108(17) 0.0016(16) C2 0.009(2) 0.011(2) 0.013(2) 0.0004(17) 0.0051(18) -0.0018(16) C11 0.017(2) 0.008(2) 0.020(2) 0.0024(18) 0.012(2) -0.0002(17) C16 0.015(2) 0.010(2) 0.018(2) 0.0055(18) 0.006(2) -0.0027(17) C14 0.009(2) 0.015(2) 0.014(2) 0.0079(18) 0.0061(19) 0.0039(17) C17 0.018(2) 0.011(2) 0.019(2) 0.0046(19) 0.005(2) 0.0017(18) O8 0.0203(19) 0.0170(18) 0.036(2) 0.0002(15) 0.0191(18) 0.0048(15) C21 0.018(2) 0.014(2) 0.017(2) 0.0058(19) 0.010(2) 0.0028(19) C23 0.008(2) 0.015(2) 0.017(2) 0.0045(18) 0.0060(18) 0.0032(17) C26 0.008(2) 0.011(2) 0.014(2) 0.0024(17) 0.0029(18) 0.0008(16) C22 0.012(2) 0.009(2) 0.015(2) 0.0034(17) 0.0029(18) 0.0029(16) O11 0.0100(15) 0.0267(19) 0.0238(18) 0.0113(14) 0.0106(14) 0.0067(13) C5 0.008(2) 0.005(2) 0.017(2) -0.0054(17) 0.0056(18) -0.0031(16) C6 0.014(2) 0.010(2) 0.019(2) 0.0001(18) 0.009(2) 0.0003(17) O3 0.0237(19) 0.0173(18) 0.0226(18) 0.0121(14) 0.0066(16) -0.0009(14) C12 0.008(2) 0.014(2) 0.019(2) 0.0070(18) 0.0066(19) 0.0022(17) C18 0.011(2) 0.016(2) 0.015(2) 0.0084(19) 0.0060(19) 0.0013(18) C28 0.016(2) 0.007(2) 0.018(2) 0.0013(18) 0.005(2) 0.0020(18) C9 0.010(2) 0.009(2) 0.015(2) 0.0072(17) 0.0050(18) 0.0008(16) C1 0.015(2) 0.013(2) 0.010(2) 0.0027(17) 0.0025(19) 0.0010(18) C25 0.007(2) 0.013(2) 0.021(2) 0.0039(18) 0.0039(19) 0.0033(16) C24 0.014(2) 0.014(2) 0.016(2) 0.0034(18) 0.0046(19) -0.0030(18) C3 0.012(2) 0.008(2) 0.017(2) 0.0021(17) 0.0089(19) 0.0023(17) O2 0.0080(16) 0.036(2) 0.030(2) 0.0170(17) 0.0068(15) 0.0079(14) O1 0.0188(17) 0.0240(18) 0.0089(15) -0.0004(13) -0.0017(14) 0.0002(14) O10 0.0186(19) 0.050(3) 0.0211(19) 0.0106(18) 0.0043(16) -0.0010(17) O6 0.0186(19) 0.029(2) 0.0244(19) -0.0028(16) 0.0095(17) -0.0014(16) O22 0.011(2) 0.062(3) 0.047(3) -0.027(2) 0.001(2) 0.007(2) O4 0.030(2) 0.040(2) 0.0139(18) 0.0004(16) 0.0079(16) -0.0091(18) C52 0.016(2) 0.019(3) 0.013(2) -0.0033(19) 0.007(2) -0.0025(19) C10 0.013(2) 0.013(2) 0.017(2) 0.0019(18) 0.007(2) -0.0024(17) O20 0.036(3) 0.123(5) 0.022(2) 0.015(3) 0.003(2) -0.030(3) O21 0.044(3) 0.026(2) 0.073(4) -0.014(2) -0.020(3) -0.005(2) O5 0.034(2) 0.0152(19) 0.034(2) -0.0077(16) 0.0031(19) 0.0003(16) Na1 0.0202(10) 0.0216(10) 0.0174(9) 0.0043(7) 0.0038(8) 0.0016(8) Na2 0.0279(13) 0.089(2) 0.0351(15) 0.0370(15) 0.0079(12) 0.0072(13) O40 0.0244(19) 0.030(2) 0.0256(19) 0.0103(16) 0.0165(17) 0.0068(15) O34 0.029(2) 0.031(2) 0.0218(19) 0.0035(16) 0.0146(17) 0.0045(17) O37 0.038(3) 0.043(3) 0.035(3) -0.019(2) 0.004(2) 0.006(2) O50 0.027(2) 0.066(4) 0.057(3) -0.009(3) 0.006(2) 0.013(2) O44 0.027(2) 0.025(2) 0.026(2) 0.0117(16) 0.0045(16) -0.0037(15) O33 0.0143(16) 0.029(2) 0.0245(19) 0.0090(15) 0.0086(15) 0.0051(14) O42 0.036(3) 0.057(3) 0.045(3) 0.020(2) 0.003(2) 0.011(2) O36 0.0231(18) 0.0251(19) 0.024(2) 0.0035(15) 0.0085(16) 0.0040(15) O53 0.059(3) 0.026(2) 0.049(3) -0.005(2) 0.013(3) -0.013(2) C62 0.030(3) 0.027(3) 0.029(3) 0.009(2) 0.003(3) 0.005(2) O41 0.046(3) 0.027(2) 0.025(2) 0.0002(17) 0.0103(19) -0.0177(19) O35 0.028(2) 0.034(2) 0.037(2) 0.0074(18) 0.0091(19) 0.0097(17) O51 0.074(4) 0.128(6) 0.037(3) -0.013(3) -0.001(3) 0.059(4) O54 0.029(2) 0.035(2) 0.034(2) 0.0050(18) 0.0051(19) -0.0006(18) C59 0.024(3) 0.049(4) 0.021(3) 0.015(3) 0.006(2) 0.015(3) O38 0.034(2) 0.037(2) 0.042(3) 0.017(2) 0.009(2) -0.0043(19) N2 0.038(3) 0.022(2) 0.022(2) 0.0086(18) 0.012(2) 0.0123(19) C58 0.015(2) 0.035(3) 0.020(3) 0.005(2) 0.004(2) -0.001(2) C57 0.022(2) 0.015(2) 0.017(2) -0.0029(18) 0.007(2) -0.0017(18) N1 0.021(2) 0.064(4) 0.027(3) 0.015(2) 0.013(2) 0.000(2) O39 0.052(3) 0.101(5) 0.066(4) 0.005(3) 0.022(3) 0.050(3) O55 0.041(3) 0.051(3) 0.050(3) 0.015(2) 0.017(2) 0.002(2) C60 0.025(3) 0.025(3) 0.035(3) 0.008(2) 0.018(3) 0.005(2) C61 0.033(3) 0.030(3) 0.026(3) 0.016(2) 0.017(2) 0.009(2) O49 0.034(2) 0.032(2) 0.032(2) 0.0132(17) 0.0192(18) 0.0065(17) O48 0.040(2) 0.030(2) 0.029(2) 0.0083(17) 0.0185(19) 0.0079(18) O12 0.045(2) 0.0193(19) 0.061(3) 0.0225(19) 0.042(2) 0.0145(17) O45 0.082(4) 0.032(3) 0.051(3) 0.006(2) 0.024(3) 0.002(3) O47 0.133(7) 0.067(4) 0.053(4) 0.003(3) 0.044(4) -0.018(4) O52 0.131(7) 0.029(3) 0.103(6) 0.013(3) -0.053(5) 0.003(4) O28 0.074(5) 0.087(5) 0.139(7) 0.045(5) 0.056(5) -0.005(4) O46 0.050(4) 0.149(7) 0.053(4) 0.048(4) 0.000(3) -0.008(4) O26 0.224(10) 0.137(7) 0.111(6) 0.108(6) 0.137(7) 0.145(8) O43 0.085(4) 0.048(3) 0.051(3) 0.003(2) 0.042(3) -0.008(3) O24 0.098(5) 0.053(4) 0.088(5) 0.030(3) 0.045(4) 0.035(3) O27 0.336(15) 0.037(4) 0.129(7) 0.014(4) 0.194(10) 0.021(6) C7 0.013(2) 0.013(2) 0.018(2) 0.0038(18) 0.012(2) 0.0065(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 S5 O17 1.454(4) . ? S5 O18 1.454(4) . ? S5 O19 1.456(4) . ? S5 C29 1.783(5) . ? S6 O20 1.414(5) . ? S6 O22 1.424(4) . ? S6 O21 1.461(6) . ? S6 C52 1.771(5) . ? S8 O27 1.372(6) . ? S8 O26 1.408(7) . ? S8 O28 1.472(8) . ? S8 C38 1.770(5) . ? S7 O25 1.377(7) . ? S7 O23 1.378(5) . ? S7 O24 1.522(7) . ? S7 C45 1.755(5) . ? C42 C43 1.517(7) . ? C42 C40 1.545(7) . ? C47 C46 1.384(7) . ? C47 C48 1.408(6) . ? C47 C49 1.533(7) . ? C45 C46 1.382(8) . ? C45 C44 1.393(7) . ? O29 C32 1.371(6) . ? C38 C39 1.382(7) . ? C38 C37 1.394(7) . ? O30 C55 1.379(6) . ? C51 C52 1.391(7) . ? C51 C50 1.396(7) . ? O31 C48 1.376(6) . ? C39 C40 1.388(7) . ? O32 C41 1.378(6) . ? C30 C29 1.394(7) . ? C30 C31 1.394(7) . ? C44 C43 1.392(7) . ? C43 C48 1.389(7) . ? C34 C33 1.386(7) . ? C34 C29 1.390(7) . ? C54 C55 1.395(6) . ? C54 C53 1.403(7) . ? C54 C56 1.522(7) . ? C37 C36 1.384(7) . ? C36 C41 1.408(7) . ? C36 C35 1.530(7) . ? O17 Na1 2.486(4) . ? C56 C33 1.520(6) . ? C40 C41 1.394(7) . ? C35 C31 1.514(6) . ? C49 C50 1.509(6) . ? C50 C55 1.410(7) . ? C31 C32 1.416(7) . ? C32 C33 1.408(7) . ? C53 C52 1.392(7) . ? S2 O6 1.450(4) . ? S2 O5 1.463(4) . ? S2 O4 1.471(4) . ? S2 C10 1.773(5) . ? S4 O11 1.442(3) . ? S4 O10 1.442(4) . ? S4 O12 1.459(4) . ? S4 C24 1.768(5) . ? S1 O3 1.452(4) . ? S1 O1 1.452(4) . ? S1 O2 1.469(4) . ? S1 C1 1.774(5) . ? S3 O8 1.455(4) . ? S3 O7 1.460(4) . ? S3 O9 1.464(4) . ? S3 C17 1.765(5) . ? C19 C20 1.392(7) . ? C19 C18 1.402(7) . ? C19 C21 1.521(7) . ? C15 C20 1.388(7) . ? C15 C16 1.392(7) . ? C15 C14 1.525(6) . ? C20 O15 1.388(6) . ? C13 O14 1.372(6) . ? C13 C8 1.394(6) . ? C13 C12 1.407(7) . ? C27 O16 1.376(6) . ? C27 C22 1.404(7) . ? C27 C26 1.410(6) . ? C4 O13 1.374(6) . ? C4 C3 1.385(7) . ? C4 C5 1.413(7) . ? C8 C9 1.385(7) . ? C8 C7 1.518(6) . ? O7 Na2 2.439(5) . ? C2 C1 1.385(7) . ? C2 C3 1.396(7) . ? C11 C12 1.385(7) . ? C11 C10 1.387(7) . ? C16 C17 1.402(7) . ? C14 C12 1.530(6) . ? C17 C18 1.380(7) . ? C21 C22 1.507(7) . ? C23 C24 1.392(7) . ? C23 C22 1.396(7) . ? C26 C25 1.401(7) . ? C26 C28 1.499(7) . ? C5 C6 1.392(7) . ? C5 C28 1.526(6) . ? C6 C1 1.384(7) . ? C9 C10 1.398(7) . ? C25 C24 1.389(7) . ? C3 C7 1.507(7) . ? O1 Na1 2.442(4) . ? O20 Na2 2.432(6) . ? Na1 O39 2.319(5) . ? Na1 O33 2.359(4) . ? Na1 O40 2.438(4) . ? Na1 O41 2.469(4) . ? Na2 O42 2.385(6) . ? Na2 O36 2.407(5) . ? Na2 O43 2.506(7) . ? Na2 O35 2.537(5) . ? O34 C57 1.318(6) . ? O37 C60 1.301(7) . ? O33 C57 1.210(6) . ? O36 C60 1.215(7) . ? C62 O38 1.428(8) . ? C62 C61 1.526(9) . ? O35 C59 1.390(8) . ? C59 C58 1.535(8) . ? N2 C61 1.478(7) . ? C58 N1 1.491(7) . ? C58 C57 1.532(7) . ? C60 C61 1.531(8) . ? 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 O17 S5 O18 112.2(2) . . ? O17 S5 O19 112.0(2) . . ? O18 S5 O19 113.1(2) . . ? O17 S5 C29 106.9(2) . . ? O18 S5 C29 105.5(2) . . ? O19 S5 C29 106.6(2) . . ? O20 S6 O22 117.4(4) . . ? O20 S6 O21 111.3(4) . . ? O22 S6 O21 109.7(4) . . ? O20 S6 C52 105.9(3) . . ? O22 S6 C52 107.1(3) . . ? O21 S6 C52 104.7(3) . . ? O27 S8 O26 114.6(7) . . ? O27 S8 O28 118.2(6) . . ? O26 S8 O28 103.4(6) . . ? O27 S8 C38 108.6(3) . . ? O26 S8 C38 106.2(3) . . ? O28 S8 C38 104.8(4) . . ? O25 S7 O23 124.4(5) . . ? O25 S7 O24 102.2(6) . . ? O23 S7 O24 106.5(5) . . ? O25 S7 C45 107.6(3) . . ? O23 S7 C45 110.5(3) . . ? O24 S7 C45 103.2(3) . . ? C43 C42 C40 113.1(4) . . ? C46 C47 C48 117.7(4) . . ? C46 C47 C49 120.1(4) . . ? C48 C47 C49 122.1(4) . . ? C46 C45 C44 121.6(4) . . ? C46 C45 S7 119.2(4) . . ? C44 C45 S7 118.8(4) . . ? C39 C38 C37 121.8(5) . . ? C39 C38 S8 118.8(4) . . ? C37 C38 S8 119.3(4) . . ? C52 C51 C50 120.1(5) . . ? C38 C39 C40 119.0(4) . . ? C29 C30 C31 119.8(4) . . ? C43 C44 C45 118.5(5) . . ? C48 C43 C44 119.7(4) . . ? C48 C43 C42 121.1(4) . . ? C44 C43 C42 119.2(4) . . ? C33 C34 C29 119.9(4) . . ? C34 C29 C30 122.0(4) . . ? C34 C29 S5 119.3(4) . . ? C30 C29 S5 118.8(4) . . ? C55 C54 C53 117.9(5) . . ? C55 C54 C56 122.1(4) . . ? C53 C54 C56 120.0(4) . . ? C36 C37 C38 119.8(5) . . ? C37 C36 C41 118.4(4) . . ? C37 C36 C35 120.0(4) . . ? C41 C36 C35 121.6(4) . . ? S5 O17 Na1 123.1(2) . . ? C33 C56 C54 114.8(4) . . ? C39 C40 C41 119.6(4) . . ? C39 C40 C42 118.3(4) . . ? C41 C40 C42 122.1(4) . . ? C31 C35 C36 112.0(4) . . ? C50 C49 C47 112.6(4) . . ? C51 C50 C55 118.1(4) . . ? C51 C50 C49 119.9(4) . . ? C55 C50 C49 122.0(4) . . ? C30 C31 C32 117.6(4) . . ? C30 C31 C35 120.4(4) . . ? C32 C31 C35 122.1(4) . . ? O31 C48 C43 118.2(4) . . ? O31 C48 C47 120.2(4) . . ? C43 C48 C47 121.6(4) . . ? O32 C41 C40 120.7(4) . . ? O32 C41 C36 118.0(4) . . ? C40 C41 C36 121.3(4) . . ? O29 C32 C33 117.2(4) . . ? O29 C32 C31 120.2(4) . . ? C33 C32 C31 122.5(4) . . ? C52 C53 C54 120.3(5) . . ? C45 C46 C47 120.7(5) . . ? C34 C33 C32 118.1(4) . . ? C34 C33 C56 120.6(4) . . ? C32 C33 C56 121.3(4) . . ? O30 C55 C54 120.8(5) . . ? O30 C55 C50 116.7(4) . . ? C54 C55 C50 122.5(4) . . ? O6 S2 O5 114.1(3) . . ? O6 S2 O4 112.6(3) . . ? O5 S2 O4 109.1(3) . . ? O6 S2 C10 106.5(2) . . ? O5 S2 C10 107.3(2) . . ? O4 S2 C10 106.8(2) . . ? O11 S4 O10 112.1(2) . . ? O11 S4 O12 113.4(2) . . ? O10 S4 O12 113.0(3) . . ? O11 S4 C24 105.4(2) . . ? O10 S4 C24 106.7(2) . . ? O12 S4 C24 105.5(2) . . ? O3 S1 O1 112.4(2) . . ? O3 S1 O2 112.7(2) . . ? O1 S1 O2 111.7(2) . . ? O3 S1 C1 105.7(2) . . ? O1 S1 C1 107.3(2) . . ? O2 S1 C1 106.7(2) . . ? O8 S3 O7 111.8(2) . . ? O8 S3 O9 114.4(2) . . ? O7 S3 O9 111.3(2) . . ? O8 S3 C17 105.9(2) . . ? O7 S3 C17 106.9(2) . . ? O9 S3 C17 105.9(2) . . ? C20 C19 C18 117.7(4) . . ? C20 C19 C21 122.3(4) . . ? C18 C19 C21 119.9(4) . . ? C20 C15 C16 117.7(4) . . ? C20 C15 C14 122.7(4) . . ? C16 C15 C14 119.5(4) . . ? C15 C20 O15 119.0(4) . . ? C15 C20 C19 123.1(4) . . ? O15 C20 C19 117.8(4) . . ? O14 C13 C8 118.6(4) . . ? O14 C13 C12 118.6(4) . . ? C8 C13 C12 122.5(4) . . ? O16 C27 C22 118.3(4) . . ? O16 C27 C26 118.7(4) . . ? C22 C27 C26 122.9(4) . . ? O13 C4 C3 119.7(4) . . ? O13 C4 C5 117.3(4) . . ? C3 C4 C5 123.0(4) . . ? C9 C8 C13 117.8(4) . . ? C9 C8 C7 119.9(4) . . ? C13 C8 C7 122.3(4) . . ? S3 O7 Na2 136.3(2) . . ? C1 C2 C3 120.7(4) . . ? C12 C11 C10 119.8(4) . . ? C15 C16 C17 120.6(4) . . ? C15 C14 C12 113.8(4) . . ? C18 C17 C16 120.2(5) . . ? C18 C17 S3 121.9(4) . . ? C16 C17 S3 118.0(4) . . ? C22 C21 C19 114.7(4) . . ? C24 C23 C22 120.1(4) . . ? C25 C26 C27 117.4(4) . . ? C25 C26 C28 119.9(4) . . ? C27 C26 C28 122.7(4) . . ? C23 C22 C27 117.8(4) . . ? C23 C22 C21 120.1(4) . . ? C27 C22 C21 122.1(4) . . ? C6 C5 C4 117.2(4) . . ? C6 C5 C28 120.1(4) . . ? C4 C5 C28 122.7(4) . . ? C1 C6 C5 120.8(4) . . ? C11 C12 C13 118.3(4) . . ? C11 C12 C14 119.6(4) . . ? C13 C12 C14 122.1(4) . . ? C17 C18 C19 120.6(5) . . ? C26 C28 C5 112.7(4) . . ? C8 C9 C10 120.4(4) . . ? C6 C1 C2 120.6(4) . . ? C6 C1 S1 119.5(4) . . ? C2 C1 S1 119.9(4) . . ? C24 C25 C26 120.1(4) . . ? C25 C24 C23 121.5(5) . . ? C25 C24 S4 120.1(4) . . ? C23 C24 S4 118.4(4) . . ? C4 C3 C2 117.7(4) . . ? C4 C3 C7 122.1(4) . . ? C2 C3 C7 120.2(4) . . ? S1 O1 Na1 131.2(2) . . ? C51 C52 C53 121.1(5) . . ? C51 C52 S6 119.0(4) . . ? C53 C52 S6 119.9(4) . . ? C11 C10 C9 121.0(4) . . ? C11 C10 S2 121.9(4) . . ? C9 C10 S2 117.1(4) . . ? S6 O20 Na2 158.1(4) . . ? O39 Na1 O33 169.8(2) . . ? O39 Na1 O40 90.0(2) . . ? O33 Na1 O40 80.00(14) . . ? O39 Na1 O1 96.4(2) . . ? O33 Na1 O1 82.57(14) . . ? O40 Na1 O1 93.65(14) . . ? O39 Na1 O41 90.2(2) . . ? O33 Na1 O41 99.74(16) . . ? O40 Na1 O41 178.63(17) . . ? O1 Na1 O41 84.98(14) . . ? O39 Na1 O17 94.5(2) . . ? O33 Na1 O17 89.38(14) . . ? O40 Na1 O17 101.67(15) . . ? O1 Na1 O17 161.21(15) . . ? O41 Na1 O17 79.66(14) . . ? O42 Na2 O36 132.8(2) . . ? O42 Na2 O20 79.7(2) . . ? O36 Na2 O20 77.72(17) . . ? O42 Na2 O7 119.15(19) . . ? O36 Na2 O7 88.86(16) . . ? O20 Na2 O7 161.1(2) . . ? O42 Na2 O43 89.6(2) . . ? O36 Na2 O43 134.8(2) . . ? O20 Na2 O43 99.8(2) . . ? O7 Na2 O43 80.14(17) . . ? O42 Na2 O35 77.45(19) . . ? O36 Na2 O35 70.67(15) . . ? O20 Na2 O35 107.3(2) . . ? O7 Na2 O35 80.04(15) . . ? O43 Na2 O35 147.0(2) . . ? C57 O33 Na1 127.0(3) . . ? C60 O36 Na2 136.9(4) . . ? O38 C62 C61 110.0(5) . . ? C59 O35 Na2 130.8(4) . . ? O35 C59 C58 110.9(5) . . ? N1 C58 C57 105.9(4) . . ? N1 C58 C59 112.3(5) . . ? C57 C58 C59 110.5(5) . . ? O33 C57 O34 125.5(5) . . ? O33 C57 C58 122.2(5) . . ? O34 C57 C58 112.3(4) . . ? O36 C60 O37 126.3(5) . . ? O36 C60 C61 121.6(5) . . ? O37 C60 C61 112.1(5) . . ? N2 C61 C62 113.4(5) . . ? N2 C61 C60 107.3(5) . . ? C62 C61 C60 111.0(5) . . ? C3 C7 C8 112.8(4) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 2.552 _refine_diff_density_min -0.860 _refine_diff_density_rms 0.115 #END #_________________________________________________ data_compound2 _database_code_CSD 202924 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H87 N2 Na5 O53 S8' _chemical_formula_weight 2079.77 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' O O 0.0106 0.0060 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.78340(10) _cell_length_b 12.3597(2) _cell_length_c 15.4799(2) _cell_angle_alpha 83.0760(10) _cell_angle_beta 67.8400(10) _cell_angle_gamma 89.7120(10) _cell_volume 2070.72(5) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.668 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.356 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9486 _exptl_absorpt_correction_T_max 0.9653 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35201 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0836 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 28.29 _reflns_number_total 18956 _reflns_number_gt 13634 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; 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^)+(0.0813P)^2^+3.7475P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(8) _refine_ls_number_reflns 18956 _refine_ls_number_parameters 1171 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0659 _refine_ls_wR_factor_ref 0.1761 _refine_ls_wR_factor_gt 0.1573 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.032 _refine_ls_shift/su_mean 0.003 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 S5 S 0.57422(15) 0.56859(12) 0.56453(11) 0.0210(3) Uani 1 1 d . . . S7 S 0.15090(13) 1.41958(13) 0.56645(11) 0.0194(3) Uani 1 1 d . . . S6 S -0.05882(16) 0.81872(15) 0.60597(15) 0.0377(5) Uani 1 1 d . . . C38 C 0.2356(5) 1.3373(5) 0.4798(4) 0.0161(13) Uani 1 1 d . . . O31 O 0.4427(4) 1.1763(3) 0.2572(3) 0.0184(9) Uani 1 1 d . . . Na1 Na 0.5841(2) 0.63159(18) 0.76204(17) 0.0236(5) Uani 1 1 d . . . O32 O 0.6597(4) 1.1098(4) 0.2531(3) 0.0210(10) Uani 1 1 d . . . C52 C 0.5705(6) 0.6786(5) 0.4818(4) 0.0158(13) Uani 1 1 d . . . O29 O 0.5756(4) 0.9096(3) 0.2656(3) 0.0212(10) Uani 1 1 d . . . O19 O 0.5298(5) 0.4730(4) 0.5399(3) 0.0273(11) Uani 1 1 d . . . O30 O 0.3635(4) 0.9770(4) 0.2594(3) 0.0218(10) Uani 1 1 d . . . O24 O 0.0234(4) 1.3834(4) 0.6000(3) 0.0325(12) Uani 1 1 d . . . O17 O 0.4883(6) 0.5933(4) 0.6570(3) 0.0423(14) Uani 1 1 d . . . O25 O 0.1762(4) 1.5333(4) 0.5224(3) 0.0314(11) Uani 1 1 d . . . C51 C 0.6617(5) 0.7623(5) 0.4489(4) 0.0128(12) Uani 1 1 d . . . H51 H 0.7232 0.7638 0.4745 0.015 Uiso 1 1 calc R . . C41 C 0.3742(5) 1.2260(5) 0.3348(4) 0.0148(12) Uani 1 1 d . . . C48 C 0.6707(5) 1.1244(5) 0.3366(4) 0.0126(12) Uani 1 1 d . . . C43 C 0.6373(5) 1.2247(5) 0.3721(4) 0.0119(12) Uani 1 1 d . . . C40 C 0.4344(5) 1.2934(5) 0.3698(4) 0.0138(12) Uani 1 1 d . . . O39 O 0.7884(4) 0.5562(4) 0.7250(3) 0.0236(10) Uani 1 1 d . . . O21 O -0.0213(5) 0.7352(5) 0.6586(4) 0.0442(14) Uani 1 1 d . . . C36 C 0.2454(6) 1.2083(5) 0.3730(4) 0.0152(12) Uani 1 1 d . . . C31 C 0.2702(6) 0.8347(5) 0.3851(5) 0.0184(13) Uani 1 1 d . . . C50 C 0.6617(5) 0.8448(4) 0.3773(4) 0.0143(12) Uani 1 1 d . . . O22 O -0.1431(7) 0.7885(8) 0.5716(5) 0.084(3) Uani 1 1 d . . . C47 C 0.7256(5) 1.0436(5) 0.3774(4) 0.0130(12) Uani 1 1 d . . . C42 C 0.5743(5) 1.3109(5) 0.3310(4) 0.0150(12) Uani 1 1 d . . . H42A H 0.6064 1.3116 0.2619 0.018 Uiso 1 1 calc R . . H42B H 0.5949 1.3831 0.3440 0.018 Uiso 1 1 calc R . . O18 O 0.6962(6) 0.5653(5) 0.5635(5) 0.061(2) Uani 1 1 d . . . C49 C 0.7618(5) 0.9362(5) 0.3385(4) 0.0146(12) Uani 1 1 d . . . H49A H 0.8340 0.9109 0.3520 0.018 Uiso 1 1 calc R . . H49B H 0.7872 0.9492 0.2693 0.018 Uiso 1 1 calc R . . C46 C 0.7505(5) 1.0663(5) 0.4541(4) 0.0155(12) Uani 1 1 d . . . H46 H 0.7894 1.0138 0.4824 0.019 Uiso 1 1 calc R . . O20 O -0.1020(6) 0.9106(5) 0.6665(5) 0.0563(17) Uani 1 1 d . . . C32 C 0.2710(6) 0.9414(5) 0.3436(5) 0.0180(13) Uani 1 1 d . . . C55 C 0.5689(5) 0.8405(5) 0.3422(4) 0.0122(12) Uani 1 1 d . . . C56 C 0.3700(6) 0.7571(5) 0.3423(4) 0.0164(13) Uani 1 1 d . . . H56A H 0.4051 0.7766 0.2731 0.020 Uiso 1 1 calc R . . H56B H 0.3333 0.6820 0.3561 0.020 Uiso 1 1 calc R . . C44 C 0.6606(5) 1.2426(5) 0.4523(4) 0.0138(12) Uani 1 1 d . . . H44 H 0.6362 1.3077 0.4800 0.017 Uiso 1 1 calc R . . C37 C 0.1788(6) 1.2666(5) 0.4442(5) 0.0177(13) Uani 1 1 d . . . H37 H 0.0919 1.2583 0.4696 0.021 Uiso 1 1 calc R . . C33 C 0.1773(6) 1.0126(5) 0.3818(4) 0.0179(13) Uani 1 1 d . . . C35 C 0.1804(6) 1.1276(5) 0.3365(5) 0.0174(13) Uani 1 1 d . . . H35A H 0.0953 1.1498 0.3492 0.021 Uiso 1 1 calc R . . H35B H 0.2234 1.1306 0.2675 0.021 Uiso 1 1 calc R . . C30 C 0.1686(6) 0.7993(5) 0.4683(5) 0.0231(15) Uani 1 1 d . . . H30 H 0.1651 0.7274 0.4990 0.028 Uiso 1 1 calc R . . C53 C 0.4752(5) 0.6801(5) 0.4483(4) 0.0142(12) Uani 1 1 d . . . H53 H 0.4112 0.6251 0.4740 0.017 Uiso 1 1 calc R . . O40 O 0.4935(5) 0.4740(4) 0.8778(3) 0.0303(11) Uani 1 1 d . . . C29 C 0.0760(6) 0.8662(6) 0.5049(6) 0.0334(18) Uani 1 1 d . . . C34 C 0.0778(6) 0.9735(5) 0.4632(5) 0.0267(16) Uani 1 1 d . . . H34 H 0.0119 1.0191 0.4902 0.032 Uiso 1 1 calc R . . C39 C 0.3646(5) 1.3502(5) 0.4437(4) 0.0138(12) Uani 1 1 d . . . H39 H 0.4038 1.3970 0.4694 0.017 Uiso 1 1 calc R . . O23 O 0.1981(4) 1.4008(4) 0.6427(3) 0.0296(10) Uani 1 1 d . . . S3 S -0.24000(13) 0.41093(11) 0.96298(10) 0.0135(3) Uani 1 1 d . . . S4 S -0.05624(14) 1.01912(12) 0.98826(12) 0.0230(4) Uani 1 1 d . . . S2 S 0.35606(13) 0.15670(12) 0.99537(11) 0.0177(3) Uani 1 1 d . . . O14 O 0.0665(4) 0.4135(3) 1.2932(3) 0.0188(9) Uani 1 1 d . . . O15 O -0.1499(4) 0.4832(3) 1.3015(3) 0.0162(9) Uani 1 1 d . . . O16 O -0.0573(4) 0.6794(3) 1.2906(3) 0.0187(9) Uani 1 1 d . . . O13 O 0.1558(4) 0.6075(3) 1.2974(3) 0.0171(9) Uani 1 1 d . . . C14 C -0.0628(5) 0.2819(5) 1.2232(4) 0.0124(12) Uani 1 1 d . . . H14A H -0.0912 0.2843 1.2918 0.015 Uiso 1 1 calc R . . H14B H -0.0883 0.2096 1.2137 0.015 Uiso 1 1 calc R . . C20 C -0.1637(5) 0.4656(5) 1.2197(4) 0.0117(11) Uani 1 1 d . . . O7 O -0.3694(4) 0.4314(4) 0.9868(3) 0.0211(9) Uani 1 1 d . . . C8 C 0.2646(5) 0.3801(5) 1.1784(4) 0.0133(12) Uani 1 1 d . . . C4 C 0.2442(5) 0.6463(4) 1.2123(4) 0.0106(11) Uani 1 1 d . . . C26 C 0.0401(5) 0.8305(5) 1.1772(4) 0.0149(13) Uani 1 1 d . . . C13 C 0.1372(5) 0.3643(5) 1.2170(4) 0.0121(12) Uani 1 1 d . . . C5 C 0.2452(5) 0.7545(5) 1.1703(4) 0.0143(12) Uani 1 1 d . . . O9 O -0.2111(4) 0.2992(3) 0.9454(3) 0.0212(10) Uani 1 1 d . . . C27 C -0.0560(5) 0.7517(5) 1.2153(4) 0.0138(12) Uani 1 1 d . . . O2 O 0.5360(4) 0.8697(3) 0.8998(3) 0.0208(9) Uani 1 1 d . . . C28 C 0.1425(5) 0.8314(5) 1.2136(4) 0.0150(13) Uani 1 1 d . . . H28A H 0.1073 0.8109 1.2826 0.018 Uiso 1 1 calc R . . H28B H 0.1784 0.9066 1.2009 0.018 Uiso 1 1 calc R . . C3 C 0.3377(5) 0.5761(5) 1.1702(4) 0.0132(12) Uani 1 1 d . . . C12 C 0.0763(5) 0.2943(5) 1.1806(4) 0.0120(12) Uani 1 1 d . . . O3 O 0.6596(4) 0.8048(3) 0.9891(3) 0.0196(9) Uani 1 1 d . . . C19 C -0.2180(5) 0.5496(5) 1.1794(4) 0.0131(12) Uani 1 1 d . . . C7 C 0.3321(6) 0.4570(5) 1.2135(4) 0.0135(12) Uani 1 1 d . . . H7A H 0.4168 0.4328 1.1990 0.016 Uiso 1 1 calc R . . H7B H 0.2910 0.4525 1.2827 0.016 Uiso 1 1 calc R . . O8 O -0.1595(4) 0.4886(4) 0.8861(3) 0.0230(10) Uani 1 1 d . . . C21 C -0.2516(5) 0.6577(4) 1.2185(4) 0.0128(12) Uani 1 1 d . . . H21A H -0.3229 0.6852 1.2048 0.015 Uiso 1 1 calc R . . H21B H -0.2771 0.6447 1.2878 0.015 Uiso 1 1 calc R . . C22 C -0.1487(5) 0.7451(5) 1.1792(4) 0.0135(12) Uani 1 1 d . . . C18 C -0.2419(5) 0.5291(4) 1.1008(4) 0.0104(11) Uani 1 1 d . . . H18 H -0.2817 0.5817 1.0735 0.012 Uiso 1 1 calc R . . C23 C -0.1482(6) 0.8274(5) 1.1103(4) 0.0176(13) Uani 1 1 d . . . H23 H -0.2121 0.8275 1.0870 0.021 Uiso 1 1 calc R . . C17 C -0.2075(5) 0.4316(5) 1.0621(4) 0.0125(12) Uani 1 1 d . . . C1 C 0.4379(5) 0.7220(5) 1.0465(4) 0.0126(12) Uani 1 1 d . . . C11 C 0.1445(6) 0.2365(5) 1.1100(4) 0.0152(12) Uani 1 1 d . . . H11 H 0.1047 0.1886 1.0857 0.018 Uiso 1 1 calc R . . C9 C 0.3317(5) 0.3195(4) 1.1052(4) 0.0113(11) Uani 1 1 d . . . H9 H 0.4186 0.3283 1.0775 0.014 Uiso 1 1 calc R . . C15 C -0.1258(5) 0.3712(5) 1.1806(4) 0.0137(12) Uani 1 1 d . . . O1 O 0.6132(4) 0.6872(3) 0.8918(3) 0.0198(9) Uani 1 1 d . . . C25 C 0.0375(6) 0.9107(5) 1.1069(4) 0.0174(13) Uani 1 1 d . . . H25 H 0.1007 0.9664 1.0810 0.021 Uiso 1 1 calc R . . C2 C 0.4335(5) 0.6156(5) 1.0883(4) 0.0132(12) Uani 1 1 d . . . H2 H 0.4977 0.5691 1.0599 0.016 Uiso 1 1 calc R . . C16 C -0.1508(5) 0.3527(5) 1.1014(4) 0.0139(12) Uani 1 1 d . . . H16 H -0.1290 0.2865 1.0750 0.017 Uiso 1 1 calc R . . C6 C 0.3427(6) 0.7920(5) 1.0866(4) 0.0163(13) Uani 1 1 d . . . H6 H 0.3448 0.8643 1.0569 0.020 Uiso 1 1 calc R . . O43 O -0.2880(5) 1.0461(4) 0.8338(3) 0.0279(11) Uani 1 1 d . . . O41 O 0.6050(4) 0.8236(4) 0.6992(4) 0.0338(12) Uani 1 1 d . . . S8 S 0.75650(15) 1.18890(13) 0.58733(11) 0.0205(3) Uani 1 1 d . . . S1 S 0.57062(13) 0.77332(11) 0.94984(10) 0.0153(3) Uani 1 1 d . . . O49 O -0.4392(4) 1.0079(4) 1.0840(3) 0.0332(12) Uani 1 1 d . . . O34 O 0.2828(4) 0.5561(4) 0.9585(3) 0.0273(10) Uani 1 1 d . . . O5 O 0.4824(4) 0.1994(4) 0.9518(4) 0.0283(11) Uani 1 1 d . . . O26 O 0.7221(4) 1.2992(4) 0.6078(3) 0.0248(10) Uani 1 1 d . . . O27 O 0.8857(4) 1.1736(4) 0.5609(4) 0.0344(12) Uani 1 1 d . . . O11 O -0.1761(4) 1.0169(4) 0.9830(4) 0.0302(11) Uani 1 1 d . . . C59 C 0.0462(6) 0.6162(6) 0.9673(5) 0.0321(16) Uani 1 1 d . . . H59A H 0.0429 0.5587 1.0188 0.039 Uiso 1 1 calc R . . H59B H -0.0317 0.6544 0.9876 0.039 Uiso 1 1 calc R . . O35 O 0.0625(4) 0.5687(4) 0.8847(3) 0.0366(12) Uani 1 1 d . . . O12 O -0.0288(6) 1.1174(4) 1.0181(5) 0.0461(16) Uani 1 1 d . . . O33 O 0.3602(3) 0.6879(3) 0.8384(3) 0.0251(9) Uani 1 1 d . . . C10 C 0.2714(5) 0.2474(4) 1.0737(4) 0.0123(12) Uani 1 1 d . . . C45 C 0.7195(5) 1.1646(5) 0.4906(4) 0.0147(12) Uani 1 1 d . . . N2 N 0.4415(7) 1.0678(6) 0.6875(5) 0.0509(18) Uani 1 1 d . . . O6 O 0.3457(5) 0.0516(4) 1.0550(4) 0.0337(12) Uani 1 1 d . . . C24 C -0.0578(6) 0.9092(5) 1.0744(4) 0.0164(13) Uani 1 1 d . . . N1 N 0.1518(5) 0.7897(4) 0.8721(4) 0.0298(12) Uani 1 1 d . . . C57 C 0.2784(5) 0.6465(4) 0.9075(4) 0.0203(11) Uani 1 1 d . . . C58 C 0.1540(5) 0.6967(5) 0.9457(4) 0.0248(12) Uani 1 1 d . . . H58 H 0.1455 0.7275 1.0046 0.030 Uiso 1 1 calc R . . O4 O 0.2946(4) 0.1461(4) 0.9316(3) 0.0312(11) Uani 1 1 d . . . O10 O 0.0407(5) 0.9979(5) 0.9011(4) 0.0523(17) Uani 1 1 d . . . O46 O 0.0069(5) 1.2629(5) 0.7999(4) 0.0509(16) Uani 1 1 d . . . O28 O 0.6817(5) 1.1072(4) 0.6645(3) 0.0320(12) Uani 1 1 d . . . O44 O -0.0980(5) 0.7895(7) 0.8611(4) 0.065(2) Uani 1 1 d . . . O42 O 0.9657(5) 0.5858(5) 0.4749(4) 0.0509(16) Uani 1 1 d . . . O50 O 0.3349(4) 0.9406(3) 0.8656(3) 0.0256(9) Uani 1 1 d . . . O51 O 0.1878(5) 0.7253(5) 0.6954(3) 0.0478(13) Uani 1 1 d . . . O53 O 0.5135(7) 0.3099(5) 0.7744(5) 0.0653(19) Uani 1 1 d . . . O52 O 0.2675(4) 0.5402(4) 0.7141(3) 0.0346(10) Uani 1 1 d . . . O38 O 0.3901(4) 0.8542(4) 0.6557(3) 0.0405(12) Uani 1 1 d . . . C62 C 0.4419(7) 0.9393(7) 0.5794(5) 0.0422(19) Uani 1 1 d . . . H62A H 0.4151 0.9274 0.5278 0.051 Uiso 1 1 calc R . . H62B H 0.5325 0.9376 0.5552 0.051 Uiso 1 1 calc R . . O45 O -0.0045(5) 1.1213(6) 0.6899(4) 0.0590(18) Uani 1 1 d . . . C61 C 0.4030(6) 1.0480(6) 0.6105(4) 0.0406(18) Uani 1 1 d . . . H61 H 0.4427 1.1058 0.5561 0.049 Uiso 1 1 calc R . . O37 O 0.2182(6) 1.0597(8) 0.5958(6) 0.097(3) Uani 1 1 d . . . C60 C 0.2676(8) 1.0610(10) 0.6474(6) 0.086(4) Uani 1 1 d . . . O36 O 0.2195(9) 1.0948(14) 0.7265(5) 0.206(8) Uani 1 1 d . . . Na5 Na -0.3262(2) 1.1410(2) 0.96492(19) 0.0271(6) Uani 1 1 d . . . Na4 Na 0.1461(2) 1.19492(19) 0.86796(17) 0.0270(5) Uani 1 1 d . . . C54 C 0.4728(5) 0.7593(5) 0.3792(4) 0.0150(13) Uani 1 1 d . . . Na2 Na 0.8387(2) 0.4547(2) 0.59337(18) 0.0263(6) Uani 1 1 d . . . Na3 Na -0.0899(4) 0.9787(5) 0.8035(3) 0.0970(19) Uani 1 1 d . . . O47 O 0.1890(15) 1.3669(5) 0.8871(11) 0.217(9) Uani 1 1 d . . . O48 O 0.3395(17) 1.2646(10) 0.7140(13) 0.219(9) 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 S5 0.0264(9) 0.0136(7) 0.0311(9) 0.0014(7) -0.0214(7) 0.0004(6) S7 0.0123(7) 0.0273(8) 0.0188(7) -0.0020(6) -0.0064(6) 0.0017(6) S6 0.0149(9) 0.0284(10) 0.0559(13) 0.0143(9) -0.0037(8) -0.0001(7) C38 0.010(3) 0.025(3) 0.012(3) 0.006(2) -0.004(2) -0.001(2) O31 0.020(2) 0.015(2) 0.017(2) -0.0005(17) -0.0041(18) 0.0041(18) Na1 0.0323(14) 0.0186(11) 0.0281(13) -0.0040(9) -0.0202(11) -0.0026(10) O32 0.018(2) 0.029(2) 0.019(2) -0.0039(19) -0.0090(18) 0.0003(19) C52 0.017(3) 0.019(3) 0.015(3) -0.007(2) -0.009(2) 0.001(3) O29 0.027(3) 0.022(2) 0.015(2) 0.0009(18) -0.0106(18) 0.0016(19) O19 0.036(3) 0.018(2) 0.034(3) -0.001(2) -0.022(2) -0.004(2) O30 0.027(3) 0.025(2) 0.017(2) -0.0014(18) -0.0131(19) 0.0005(19) O24 0.015(2) 0.050(3) 0.029(3) -0.014(2) -0.001(2) -0.002(2) O17 0.082(4) 0.030(3) 0.015(2) -0.005(2) -0.019(2) 0.017(3) O25 0.036(3) 0.019(2) 0.034(3) -0.0015(19) -0.007(2) 0.0064(19) C51 0.013(3) 0.014(3) 0.013(3) -0.003(2) -0.007(2) 0.000(2) C41 0.013(3) 0.009(3) 0.023(3) -0.001(2) -0.009(2) 0.005(2) C48 0.010(3) 0.013(3) 0.017(3) -0.002(2) -0.008(2) -0.004(2) C43 0.006(3) 0.013(3) 0.017(3) -0.003(2) -0.005(2) -0.002(2) C40 0.015(3) 0.012(3) 0.015(3) 0.003(2) -0.008(2) -0.001(2) O39 0.026(2) 0.022(2) 0.026(2) -0.0028(18) -0.0130(19) 0.0009(18) O21 0.021(3) 0.066(4) 0.032(3) 0.006(3) 0.001(2) 0.000(2) C36 0.019(3) 0.010(3) 0.021(3) 0.001(2) -0.014(3) -0.001(2) C31 0.013(3) 0.015(3) 0.033(4) 0.002(3) -0.017(3) -0.006(2) C50 0.013(3) 0.009(3) 0.026(3) -0.011(2) -0.012(2) 0.008(2) O22 0.052(4) 0.149(7) 0.041(4) 0.022(4) -0.017(3) -0.042(5) C47 0.009(3) 0.013(3) 0.015(3) -0.004(2) -0.002(2) 0.003(2) C42 0.013(3) 0.012(3) 0.018(3) 0.002(2) -0.004(2) -0.002(2) O18 0.042(4) 0.046(3) 0.114(6) 0.035(4) -0.063(4) -0.018(3) C49 0.013(3) 0.017(3) 0.016(3) -0.005(2) -0.007(2) 0.000(2) C46 0.008(3) 0.015(3) 0.020(3) 0.003(2) -0.003(2) 0.000(2) O20 0.061(4) 0.038(3) 0.058(4) -0.005(3) -0.010(3) 0.009(3) C32 0.015(3) 0.018(3) 0.026(3) 0.001(3) -0.015(3) -0.001(2) C55 0.014(3) 0.011(3) 0.016(3) -0.003(2) -0.011(2) 0.001(2) C56 0.013(3) 0.024(3) 0.017(3) -0.004(3) -0.010(2) -0.001(3) C44 0.011(3) 0.017(3) 0.018(3) -0.010(2) -0.008(2) 0.003(2) C37 0.010(3) 0.014(3) 0.029(3) 0.007(2) -0.011(3) -0.004(2) C33 0.016(3) 0.018(3) 0.025(3) 0.004(3) -0.015(3) -0.002(3) C35 0.010(3) 0.015(3) 0.033(4) 0.003(3) -0.016(3) -0.003(2) C30 0.012(3) 0.015(3) 0.042(4) 0.011(3) -0.014(3) 0.002(2) C53 0.013(3) 0.011(3) 0.020(3) -0.003(2) -0.008(2) -0.004(2) O40 0.030(3) 0.037(3) 0.034(3) -0.008(2) -0.022(2) 0.001(2) C29 0.013(3) 0.026(4) 0.053(5) 0.008(3) -0.006(3) 0.001(3) C34 0.017(3) 0.018(3) 0.039(4) 0.008(3) -0.008(3) -0.001(3) C39 0.007(3) 0.019(3) 0.015(3) 0.001(2) -0.005(2) -0.001(2) O23 0.033(2) 0.041(3) 0.020(2) -0.0069(19) -0.0150(18) 0.003(2) S3 0.0108(7) 0.0150(7) 0.0166(7) -0.0047(5) -0.0064(5) 0.0039(5) S4 0.0179(8) 0.0148(8) 0.0410(10) 0.0054(7) -0.0190(7) -0.0021(6) S2 0.0147(7) 0.0196(7) 0.0237(8) -0.0113(6) -0.0104(6) 0.0046(6) O14 0.018(2) 0.023(2) 0.019(2) -0.0079(18) -0.0096(18) 0.0049(18) O15 0.021(2) 0.018(2) 0.011(2) -0.0034(17) -0.0063(17) 0.0012(17) O16 0.021(2) 0.021(2) 0.020(2) -0.0007(18) -0.0144(18) 0.0060(18) O13 0.013(2) 0.023(2) 0.015(2) -0.0053(17) -0.0039(16) -0.0022(17) C14 0.010(3) 0.011(3) 0.014(3) 0.003(2) -0.003(2) 0.001(2) C20 0.007(3) 0.011(3) 0.013(3) -0.001(2) 0.000(2) -0.002(2) O7 0.016(2) 0.026(2) 0.026(2) -0.0067(18) -0.0128(18) 0.0061(17) C8 0.017(3) 0.012(3) 0.016(3) 0.003(2) -0.013(2) 0.000(2) C4 0.014(3) 0.013(3) 0.012(3) -0.009(2) -0.011(2) 0.004(2) C26 0.016(3) 0.012(3) 0.018(3) 0.002(2) -0.010(2) 0.003(2) C13 0.018(3) 0.014(3) 0.005(3) 0.003(2) -0.006(2) 0.002(2) C5 0.014(3) 0.016(3) 0.020(3) -0.010(2) -0.013(2) 0.009(2) O9 0.022(2) 0.017(2) 0.031(3) -0.0126(19) -0.014(2) 0.0097(18) C27 0.016(3) 0.013(3) 0.013(3) -0.008(2) -0.004(2) 0.009(2) O2 0.021(2) 0.0103(19) 0.033(2) 0.0014(17) -0.0141(19) 0.0020(16) C28 0.015(3) 0.009(3) 0.027(3) -0.007(3) -0.013(3) 0.003(2) C3 0.011(3) 0.016(3) 0.018(3) -0.008(2) -0.010(2) 0.001(2) C12 0.010(3) 0.014(3) 0.013(3) 0.003(2) -0.006(2) 0.000(2) O3 0.014(2) 0.019(2) 0.034(2) -0.0041(18) -0.0180(18) 0.0010(16) C19 0.008(3) 0.013(3) 0.016(3) 0.002(2) -0.003(2) -0.001(2) C7 0.016(3) 0.011(3) 0.015(3) -0.004(2) -0.008(2) 0.007(2) O8 0.021(2) 0.029(2) 0.020(2) 0.0065(19) -0.0123(18) -0.0073(19) C21 0.014(3) 0.007(3) 0.018(3) -0.004(2) -0.006(2) 0.005(2) C22 0.013(3) 0.016(3) 0.013(3) -0.007(2) -0.004(2) -0.001(2) C18 0.017(3) 0.004(2) 0.012(3) -0.001(2) -0.007(2) 0.000(2) C23 0.017(3) 0.012(3) 0.028(3) -0.008(3) -0.013(3) 0.011(2) C17 0.009(3) 0.018(3) 0.013(3) -0.001(2) -0.007(2) -0.002(2) C1 0.012(3) 0.013(3) 0.016(3) -0.002(2) -0.009(2) -0.002(2) C11 0.018(3) 0.008(3) 0.027(3) 0.000(2) -0.017(3) -0.003(2) C9 0.011(3) 0.015(3) 0.009(3) 0.001(2) -0.005(2) 0.004(2) C15 0.007(3) 0.016(3) 0.015(3) 0.005(2) -0.002(2) -0.004(2) O1 0.019(2) 0.023(2) 0.016(2) -0.0054(18) -0.0045(17) 0.0057(18) C25 0.016(3) 0.018(3) 0.021(3) -0.005(3) -0.010(3) 0.008(3) C2 0.010(3) 0.015(3) 0.020(3) -0.010(2) -0.010(2) 0.007(2) C16 0.008(3) 0.010(3) 0.018(3) 0.001(2) -0.001(2) -0.001(2) C6 0.019(3) 0.015(3) 0.020(3) -0.006(2) -0.012(2) -0.003(2) O43 0.037(3) 0.030(3) 0.020(2) -0.0037(19) -0.015(2) 0.012(2) O41 0.025(3) 0.035(3) 0.039(3) 0.012(2) -0.015(2) -0.0013(19) S8 0.0261(9) 0.0189(7) 0.0257(8) -0.0060(6) -0.0194(7) 0.0039(6) S1 0.0147(7) 0.0157(7) 0.0168(7) -0.0007(6) -0.0079(6) 0.0027(6) O49 0.020(2) 0.055(3) 0.023(2) 0.005(2) -0.0093(19) 0.007(2) O34 0.028(2) 0.024(2) 0.032(3) 0.0068(18) -0.017(2) -0.0059(18) O5 0.019(2) 0.025(2) 0.041(3) -0.018(2) -0.008(2) 0.0034(19) O26 0.037(3) 0.021(2) 0.025(2) -0.0061(19) -0.021(2) 0.003(2) O27 0.022(3) 0.046(3) 0.050(3) -0.026(2) -0.025(2) 0.014(2) O11 0.027(3) 0.019(2) 0.053(3) 0.011(2) -0.028(2) -0.0004(19) C59 0.012(3) 0.046(4) 0.030(3) 0.003(3) -0.002(2) -0.011(3) O35 0.028(2) 0.060(3) 0.020(2) -0.004(2) -0.0075(18) -0.012(2) O12 0.060(4) 0.015(2) 0.086(4) 0.002(3) -0.056(3) -0.002(2) O33 0.0182(19) 0.031(2) 0.022(2) -0.0027(17) -0.0023(16) 0.0007(17) C10 0.014(3) 0.008(3) 0.018(3) -0.003(2) -0.009(2) 0.006(2) C45 0.013(3) 0.015(3) 0.017(3) -0.001(2) -0.008(2) -0.003(2) N2 0.059(4) 0.056(4) 0.037(3) -0.013(3) -0.015(3) 0.023(3) O6 0.031(3) 0.030(3) 0.042(3) -0.006(2) -0.014(2) 0.008(2) C24 0.013(3) 0.014(3) 0.025(3) 0.003(2) -0.012(3) 0.002(2) N1 0.022(3) 0.036(3) 0.026(3) 0.009(2) -0.006(2) 0.001(2) C57 0.022(3) 0.020(3) 0.025(3) -0.007(2) -0.013(2) -0.003(2) C58 0.017(3) 0.032(3) 0.023(3) -0.007(2) -0.005(2) -0.005(2) O4 0.033(3) 0.040(3) 0.034(2) -0.022(2) -0.022(2) 0.013(2) O10 0.043(3) 0.052(4) 0.044(3) 0.025(3) -0.005(3) 0.020(3) O46 0.041(3) 0.077(4) 0.027(3) -0.004(3) -0.006(2) 0.036(3) O28 0.058(4) 0.024(3) 0.023(3) 0.001(2) -0.026(2) -0.003(2) O44 0.022(3) 0.140(6) 0.045(3) -0.038(4) -0.017(3) 0.019(3) O42 0.038(3) 0.061(4) 0.044(3) 0.022(3) -0.013(3) -0.008(3) O50 0.036(2) 0.023(2) 0.026(2) -0.0126(17) -0.0180(17) 0.0089(18) O51 0.043(3) 0.072(4) 0.027(2) -0.002(2) -0.013(2) -0.018(3) O53 0.073(5) 0.041(3) 0.062(4) -0.003(3) -0.005(3) -0.001(3) O52 0.038(3) 0.041(3) 0.036(2) -0.023(2) -0.022(2) 0.014(2) O38 0.033(3) 0.047(3) 0.039(3) -0.003(2) -0.012(2) -0.001(2) C62 0.024(4) 0.064(5) 0.029(4) -0.004(4) -0.001(3) 0.001(4) O45 0.032(3) 0.082(5) 0.051(4) 0.012(3) -0.009(3) 0.009(3) C61 0.028(3) 0.064(5) 0.019(3) 0.012(3) -0.002(2) 0.012(3) O37 0.032(4) 0.180(9) 0.070(5) 0.027(5) -0.021(3) 0.019(4) C60 0.040(5) 0.153(10) 0.033(5) 0.042(6) 0.008(4) 0.052(6) O36 0.114(7) 0.43(2) 0.032(4) 0.014(7) 0.001(4) 0.175(11) Na5 0.0217(14) 0.0257(14) 0.0344(15) -0.0055(11) -0.0104(11) 0.0003(11) Na4 0.0231(12) 0.0255(12) 0.0370(13) -0.0007(10) -0.0177(10) 0.0024(9) C54 0.013(3) 0.011(3) 0.027(3) -0.014(3) -0.012(3) 0.009(2) Na2 0.0215(14) 0.0376(15) 0.0218(13) -0.0041(11) -0.0105(11) 0.0008(12) Na3 0.087(3) 0.162(4) 0.0355(19) 0.005(2) -0.0224(19) 0.085(3) O47 0.43(2) 0.019(3) 0.410(19) -0.013(6) -0.393(19) 0.011(6) O48 0.34(2) 0.130(10) 0.35(2) -0.142(12) -0.289(18) 0.151(12) _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 S5 O18 1.432(6) . ? S5 O19 1.442(5) . ? S5 O17 1.476(5) . ? S5 C52 1.764(6) . ? S7 O24 1.445(5) . ? S7 O25 1.466(5) . ? S7 O23 1.478(4) . ? S7 C38 1.771(6) . ? S6 O22 1.363(7) . ? S6 O21 1.411(6) . ? S6 O20 1.523(7) . ? S6 C29 1.796(7) . ? C38 C37 1.385(9) . ? C38 C39 1.411(8) . ? O31 C41 1.384(7) . ? Na1 O1 2.341(5) . ? Na1 O17 2.391(6) . ? Na1 O40 2.425(5) . ? Na1 O41 2.431(5) . ? Na1 O39 2.461(5) . ? Na1 O33 2.583(5) . ? O32 C48 1.379(7) . ? C52 C51 1.398(8) . ? C52 C53 1.403(8) . ? O29 C55 1.352(7) . ? O30 C32 1.370(8) . ? O24 Na2 2.377(6) 1_465 ? O17 O1 4.668(7) . ? C51 C50 1.412(8) . ? C41 C40 1.377(8) . ? C41 C36 1.413(9) . ? C48 C47 1.402(8) . ? C48 C43 1.410(8) . ? C43 C44 1.410(8) . ? C43 C42 1.509(8) . ? C40 C39 1.399(8) . ? C40 C42 1.533(8) . ? O39 Na2 2.403(5) . ? O21 O8 4.181(7) . ? C36 C37 1.372(9) . ? C36 C35 1.540(8) . ? C31 C32 1.394(8) . ? C31 C30 1.410(9) . ? C31 C56 1.516(9) . ? C50 C55 1.397(8) . ? C50 C49 1.531(8) . ? C47 C46 1.386(9) . ? C47 C49 1.516(8) . ? O18 Na2 2.304(6) . ? C46 C45 1.391(8) . ? O20 Na3 2.426(9) . ? C32 C33 1.402(9) . ? C55 C54 1.415(8) . ? C56 C54 1.523(8) . ? C44 C45 1.388(8) . ? C33 C34 1.394(9) . ? C33 C35 1.501(8) . ? C30 C29 1.354(10) . ? C53 C54 1.369(9) . ? C29 C34 1.399(10) . ? S3 O9 1.454(4) . ? S3 O7 1.455(5) . ? S3 O8 1.456(5) . ? S3 C17 1.762(6) . ? S4 O12 1.430(5) . ? S4 O11 1.446(5) . ? S4 O10 1.454(6) . ? S4 C24 1.780(6) . ? S2 O4 1.446(4) . ? S2 O5 1.454(5) . ? S2 O6 1.478(5) . ? S2 C10 1.768(6) . ? O14 C13 1.373(7) . ? O15 C20 1.376(7) . ? O16 C27 1.375(7) . ? O13 C4 1.367(7) . ? C14 C12 1.519(8) . ? C14 C15 1.546(8) . ? C20 C15 1.374(8) . ? C20 C19 1.419(8) . ? C8 C13 1.395(8) . ? C8 C9 1.412(8) . ? C8 C7 1.513(8) . ? C4 C3 1.405(8) . ? C4 C5 1.413(8) . ? C26 C25 1.390(8) . ? C26 C27 1.396(9) . ? C26 C28 1.512(8) . ? C13 C12 1.418(8) . ? C5 C6 1.397(9) . ? C5 C28 1.532(8) . ? O9 Na5 2.309(5) 1_545 ? C27 C22 1.408(8) . ? O2 S1 1.482(4) . ? C3 C2 1.377(8) . ? C3 C7 1.533(8) . ? C12 C11 1.368(9) . ? O3 S1 1.471(4) . ? C19 C18 1.400(8) . ? C19 C21 1.522(8) . ? C21 C22 1.519(8) . ? C22 C23 1.382(8) . ? C18 C17 1.400(8) . ? C23 C24 1.377(9) . ? C17 C16 1.387(8) . ? C1 C2 1.386(8) . ? C1 C6 1.410(8) . ? C1 S1 1.762(6) . ? C11 C10 1.385(8) . ? C9 C10 1.382(8) . ? C15 C16 1.409(9) . ? O1 S1 1.441(4) . ? C25 C24 1.394(8) . ? O43 Na5 2.362(6) . ? O43 Na3 2.369(6) . ? S8 O27 1.437(5) . ? S8 O26 1.458(5) . ? S8 O28 1.465(5) . ? S8 C45 1.767(6) . ? O49 Na5 2.306(5) . ? O34 C57 1.301(7) . ? O5 Na5 2.438(6) 1_645 ? O26 Na2 2.307(5) 1_565 ? O11 Na5 2.408(5) . ? O11 Na3 2.675(7) . ? C59 O35 1.419(8) . ? C59 C58 1.526(8) . ? O12 Na4 2.538(7) . ? O33 C57 1.196(7) . ? N2 C61 1.473(10) . ? N1 C58 1.525(8) . ? C57 C58 1.519(8) . ? O4 Na4 2.354(5) 1_545 ? O10 Na3 2.560(8) . ? O10 Na4 2.642(7) . ? O46 Na4 2.363(6) . ? O44 Na3 2.389(10) . ? O42 Na2 2.338(6) . ? O38 C62 1.426(9) . ? C62 C61 1.494(11) . ? O45 Na3 2.269(8) . ? C61 C60 1.493(10) . ? O37 C60 1.154(12) . ? C60 O36 1.261(14) . ? O36 Na4 2.508(12) . ? Na5 O9 2.309(5) 1_565 ? Na5 O5 2.438(6) 1_465 ? Na4 O47 2.267(7) . ? Na4 O4 2.354(5) 1_565 ? Na4 O48 2.65(2) . ? Na2 O26 2.307(5) 1_545 ? Na2 O24 2.377(6) 1_645 ? 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 O18 S5 O19 116.0(4) . . ? O18 S5 O17 109.7(4) . . ? O19 S5 O17 110.0(3) . . ? O18 S5 C52 107.9(3) . . ? O19 S5 C52 106.4(3) . . ? O17 S5 C52 106.2(3) . . ? O24 S7 O25 114.3(3) . . ? O24 S7 O23 110.8(3) . . ? O25 S7 O23 110.3(3) . . ? O24 S7 C38 107.5(3) . . ? O25 S7 C38 107.1(3) . . ? O23 S7 C38 106.4(3) . . ? O22 S6 O21 116.1(5) . . ? O22 S6 O20 112.3(5) . . ? O21 S6 O20 107.2(4) . . ? O22 S6 C29 105.9(4) . . ? O21 S6 C29 106.2(3) . . ? O20 S6 C29 108.9(4) . . ? C37 C38 C39 120.2(6) . . ? C37 C38 S7 122.0(5) . . ? C39 C38 S7 117.7(5) . . ? O1 Na1 O17 161.2(2) . . ? O1 Na1 O40 80.00(17) . . ? O17 Na1 O40 95.95(18) . . ? O1 Na1 O41 86.73(18) . . ? O17 Na1 O41 89.82(19) . . ? O40 Na1 O41 155.0(2) . . ? O1 Na1 O39 84.87(17) . . ? O17 Na1 O39 113.7(2) . . ? O40 Na1 O39 90.10(17) . . ? O41 Na1 O39 109.78(18) . . ? O1 Na1 O33 86.59(16) . . ? O17 Na1 O33 74.57(18) . . ? O40 Na1 O33 78.83(17) . . ? O41 Na1 O33 79.38(17) . . ? O39 Na1 O33 167.05(17) . . ? C51 C52 C53 120.3(6) . . ? C51 C52 S5 120.9(5) . . ? C53 C52 S5 118.8(5) . . ? S7 O24 Na2 137.0(3) . 1_465 ? S5 O17 Na1 114.4(4) . . ? S5 O17 O1 123.6(3) . . ? Na1 O17 O1 9.32(10) . . ? C52 C51 C50 119.6(5) . . ? C40 C41 O31 118.4(5) . . ? C40 C41 C36 122.8(6) . . ? O31 C41 C36 118.7(5) . . ? O32 C48 C47 118.5(5) . . ? O32 C48 C43 118.4(5) . . ? C47 C48 C43 122.8(5) . . ? C48 C43 C44 117.7(5) . . ? C48 C43 C42 123.4(5) . . ? C44 C43 C42 118.9(5) . . ? C41 C40 C39 118.5(6) . . ? C41 C40 C42 123.4(5) . . ? C39 C40 C42 118.1(5) . . ? Na2 O39 Na1 110.6(2) . . ? S6 O21 O8 142.0(3) . . ? C37 C36 C41 117.5(5) . . ? C37 C36 C35 120.5(5) . . ? C41 C36 C35 122.0(5) . . ? C32 C31 C30 116.9(6) . . ? C32 C31 C56 122.6(6) . . ? C30 C31 C56 120.4(5) . . ? C55 C50 C51 118.4(5) . . ? C55 C50 C49 120.8(5) . . ? C51 C50 C49 120.7(5) . . ? C46 C47 C48 117.5(5) . . ? C46 C47 C49 120.0(5) . . ? C48 C47 C49 122.5(5) . . ? C43 C42 C40 113.5(5) . . ? S5 O18 Na2 144.7(4) . . ? C47 C49 C50 115.3(5) . . ? C47 C46 C45 121.2(6) . . ? S6 O20 Na3 141.7(4) . . ? O30 C32 C31 119.0(6) . . ? O30 C32 C33 118.1(5) . . ? C31 C32 C33 122.8(6) . . ? O29 C55 C50 119.6(5) . . ? O29 C55 C54 118.3(5) . . ? C50 C55 C54 121.9(5) . . ? C31 C56 C54 112.8(5) . . ? C45 C44 C43 119.7(5) . . ? C36 C37 C38 121.5(6) . . ? C34 C33 C32 118.2(6) . . ? C34 C33 C35 119.8(6) . . ? C32 C33 C35 122.0(6) . . ? C33 C35 C36 112.1(5) . . ? C29 C30 C31 121.1(6) . . ? C54 C53 C52 121.1(6) . . ? C30 C29 C34 121.7(6) . . ? C30 C29 S6 121.3(5) . . ? C34 C29 S6 116.9(5) . . ? C33 C34 C29 119.3(6) . . ? C40 C39 C38 119.4(6) . . ? O9 S3 O7 113.0(3) . . ? O9 S3 O8 111.3(3) . . ? O7 S3 O8 112.9(3) . . ? O9 S3 C17 107.0(3) . . ? O7 S3 C17 106.4(3) . . ? O8 S3 C17 105.8(3) . . ? O12 S4 O11 112.9(3) . . ? O12 S4 O10 111.0(4) . . ? O11 S4 O10 112.5(4) . . ? O12 S4 C24 107.4(3) . . ? O11 S4 C24 106.7(3) . . ? O10 S4 C24 105.9(3) . . ? O4 S2 O5 115.6(3) . . ? O4 S2 O6 109.5(3) . . ? O5 S2 O6 111.5(3) . . ? O4 S2 C10 106.8(3) . . ? O5 S2 C10 107.8(3) . . ? O6 S2 C10 105.0(3) . . ? C12 C14 C15 113.2(4) . . ? C15 C20 O15 120.7(5) . . ? C15 C20 C19 122.9(6) . . ? O15 C20 C19 116.4(5) . . ? C13 C8 C9 117.9(5) . . ? C13 C8 C7 122.6(5) . . ? C9 C8 C7 119.6(5) . . ? O13 C4 C3 117.5(5) . . ? O13 C4 C5 121.3(5) . . ? C3 C4 C5 121.1(5) . . ? C25 C26 C27 118.4(6) . . ? C25 C26 C28 120.6(5) . . ? C27 C26 C28 121.0(5) . . ? O14 C13 C8 121.2(5) . . ? O14 C13 C12 117.5(5) . . ? C8 C13 C12 121.2(5) . . ? C6 C5 C4 118.8(5) . . ? C6 C5 C28 119.2(5) . . ? C4 C5 C28 122.0(5) . . ? S3 O9 Na5 134.5(3) . 1_545 ? O16 C27 C26 117.3(5) . . ? O16 C27 C22 120.5(5) . . ? C26 C27 C22 122.2(6) . . ? C26 C28 C5 114.3(5) . . ? C2 C3 C4 118.8(5) . . ? C2 C3 C7 120.5(5) . . ? C4 C3 C7 120.7(5) . . ? C11 C12 C13 119.1(5) . . ? C11 C12 C14 121.5(5) . . ? C13 C12 C14 119.4(5) . . ? C18 C19 C20 117.0(5) . . ? C18 C19 C21 119.9(5) . . ? C20 C19 C21 123.1(5) . . ? C8 C7 C3 113.5(5) . . ? S3 O8 O21 163.9(3) . . ? C22 C21 C19 114.2(5) . . ? C23 C22 C27 117.0(6) . . ? C23 C22 C21 120.2(5) . . ? C27 C22 C21 122.6(5) . . ? C19 C18 C17 120.5(5) . . ? C24 C23 C22 121.8(6) . . ? C16 C17 C18 120.9(5) . . ? C16 C17 S3 120.8(5) . . ? C18 C17 S3 118.3(4) . . ? C2 C1 C6 120.4(5) . . ? C2 C1 S1 119.3(4) . . ? C6 C1 S1 120.0(4) . . ? C12 C11 C10 120.4(5) . . ? C10 C9 C8 120.2(5) . . ? C20 C15 C16 118.7(5) . . ? C20 C15 C14 122.5(5) . . ? C16 C15 C14 118.7(5) . . ? S1 O1 Na1 136.1(3) . . ? S1 O1 O17 128.3(2) . . ? Na1 O1 O17 9.52(11) . . ? C26 C25 C24 120.0(6) . . ? C3 C2 C1 121.2(5) . . ? C17 C16 C15 119.7(6) . . ? C5 C6 C1 119.6(5) . . ? Na5 O43 Na3 104.1(2) . . ? O27 S8 O26 113.2(3) . . ? O27 S8 O28 112.4(3) . . ? O26 S8 O28 111.3(3) . . ? O27 S8 C45 106.9(3) . . ? O26 S8 C45 107.8(3) . . ? O28 S8 C45 104.7(3) . . ? O1 S1 O3 112.2(3) . . ? O1 S1 O2 112.3(3) . . ? O3 S1 O2 110.9(2) . . ? O1 S1 C1 107.4(3) . . ? O3 S1 C1 106.3(3) . . ? O2 S1 C1 107.5(3) . . ? S2 O5 Na5 133.8(3) . 1_645 ? S8 O26 Na2 131.6(3) . 1_565 ? S4 O11 Na5 139.7(3) . . ? S4 O11 Na3 94.0(3) . . ? Na5 O11 Na3 94.31(18) . . ? O35 C59 C58 108.4(5) . . ? S4 O12 Na4 98.9(3) . . ? C57 O33 Na1 129.8(4) . . ? C9 C10 C11 121.0(5) . . ? C9 C10 S2 119.9(4) . . ? C11 C10 S2 118.7(4) . . ? C44 C45 C46 121.0(6) . . ? C44 C45 S8 120.3(5) . . ? C46 C45 S8 118.7(5) . . ? C23 C24 C25 120.3(6) . . ? C23 C24 S4 123.3(5) . . ? C25 C24 S4 116.3(5) . . ? O33 C57 O34 125.9(5) . . ? O33 C57 C58 122.1(5) . . ? O34 C57 C58 112.0(5) . . ? C57 C58 N1 107.3(4) . . ? C57 C58 C59 113.6(5) . . ? N1 C58 C59 109.4(5) . . ? S2 O4 Na4 152.7(3) . 1_545 ? S4 O10 Na3 98.6(3) . . ? S4 O10 Na4 93.8(3) . . ? Na3 O10 Na4 112.4(2) . . ? O38 C62 C61 110.7(5) . . ? N2 C61 C60 105.4(7) . . ? N2 C61 C62 110.7(6) . . ? C60 C61 C62 114.5(8) . . ? O37 C60 O36 123.2(9) . . ? O37 C60 C61 117.9(8) . . ? O36 C60 C61 117.3(11) . . ? C60 O36 Na4 169.2(13) . . ? O49 Na5 O9 139.0(2) . 1_565 ? O49 Na5 O43 99.8(2) . . ? O9 Na5 O43 118.5(2) 1_565 . ? O49 Na5 O11 75.71(18) . . ? O9 Na5 O11 96.34(18) 1_565 . ? O43 Na5 O11 79.45(19) . . ? O49 Na5 O5 88.05(19) . 1_465 ? O9 Na5 O5 105.72(18) 1_565 1_465 ? O43 Na5 O5 88.89(19) . 1_465 ? O11 Na5 O5 157.9(2) . 1_465 ? O47 Na4 O4 84.4(2) . 1_565 ? O47 Na4 O46 89.9(3) . . ? O4 Na4 O46 173.9(2) 1_565 . ? O47 Na4 O36 131.5(6) . . ? O4 Na4 O36 100.0(2) 1_565 . ? O46 Na4 O36 82.1(2) . . ? O47 Na4 O12 106.6(5) . . ? O4 Na4 O12 92.46(19) 1_565 . ? O46 Na4 O12 91.27(19) . . ? O36 Na4 O12 121.3(4) . . ? O47 Na4 O10 161.1(5) . . ? O4 Na4 O10 96.13(18) 1_565 . ? O46 Na4 O10 90.0(2) . . ? O36 Na4 O10 67.1(4) . . ? O12 Na4 O10 54.55(19) . . ? O47 Na4 O48 75.3(6) . . ? O4 Na4 O48 83.9(3) 1_565 . ? O46 Na4 O48 92.6(3) . . ? O36 Na4 O48 57.5(4) . . ? O12 Na4 O48 175.7(3) . . ? O10 Na4 O48 123.5(3) . . ? C53 C54 C55 118.4(5) . . ? C53 C54 C56 120.1(5) . . ? C55 C54 C56 121.5(5) . . ? O18 Na2 O26 91.9(2) . 1_545 ? O18 Na2 O42 78.7(2) . . ? O26 Na2 O42 138.8(2) 1_545 . ? O18 Na2 O24 163.8(2) . 1_645 ? O26 Na2 O24 102.7(2) 1_545 1_645 ? O42 Na2 O24 85.7(2) . 1_645 ? O18 Na2 O39 81.3(2) . . ? O26 Na2 O39 119.03(19) 1_545 . ? O42 Na2 O39 99.2(2) . . ? O24 Na2 O39 97.26(18) 1_645 . ? O45 Na3 O43 90.8(2) . . ? O45 Na3 O44 150.3(3) . . ? O43 Na3 O44 112.0(3) . . ? O45 Na3 O20 78.3(3) . . ? O43 Na3 O20 87.7(2) . . ? O44 Na3 O20 83.8(3) . . ? O45 Na3 O10 98.4(3) . . ? O43 Na3 O10 126.2(3) . . ? O44 Na3 O10 83.5(2) . . ? O20 Na3 O10 146.1(3) . . ? O45 Na3 O11 118.2(3) . . ? O43 Na3 O11 74.11(18) . . ? O44 Na3 O11 87.2(2) . . ? O20 Na3 O11 155.0(3) . . ? O10 Na3 O11 54.80(19) . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 1.567 _refine_diff_density_min -1.375 _refine_diff_density_rms 0.109 #END #________________________________________ data_compound3 _database_code_CSD 202925 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H81 Cl Cs2 N2 Na2 O49 S8' _chemical_formula_weight 2242.02 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cs Cs -0.3680 2.1192 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.60930(10) _cell_length_b 12.38640(10) _cell_length_c 15.6609(2) _cell_angle_alpha 69.58 _cell_angle_beta 73.75 _cell_angle_gamma 89.8430(10) _cell_volume 2014.82(4) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.848 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 1.267 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8041 _exptl_absorpt_correction_T_max 0.8426 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 36178 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0536 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 28.32 _reflns_number_total 18658 _reflns_number_gt 16560 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Two carbon atoms, C8 and C40, were left isotropic. The atoms are present in aromatic rings on the calixarene and the other similar carbons atoms have low thermal parameters. 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^)+(0.0955P)^2^+6.4719P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(12) _refine_ls_number_reflns 18658 _refine_ls_number_parameters 1125 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1596 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 S4 S 2.16423(13) 1.04405(12) 0.22082(11) 0.0135(3) Uani 1 1 d . . . S6 S 1.44220(14) 1.63289(13) 0.62644(12) 0.0179(3) Uani 1 1 d . . . S8 S 1.87089(15) 0.78876(15) 0.62662(12) 0.0214(3) Uani 1 1 d . . . S5 S 2.04694(13) 1.41624(12) 0.57091(11) 0.0139(3) Uani 1 1 d . . . S7 S 1.27430(13) 1.04784(12) 0.59712(10) 0.0116(3) Uani 1 1 d . . . S1 S 2.30066(14) 1.61557(13) 0.26046(11) 0.0148(3) Uani 1 1 d . . . S2 S 1.71736(13) 1.86958(13) 0.22689(11) 0.0151(3) Uani 1 1 d . . . S3 S 1.54032(13) 1.26620(12) 0.26600(11) 0.0155(3) Uani 1 1 d . . . C42 C 1.2798(5) 1.2073(5) 0.8651(4) 0.0106(11) Uani 1 1 d . . . H42A H 1.2643 1.1711 0.9350 0.013 Uiso 1 1 calc R . . H42B H 1.2038 1.2359 0.8534 0.013 Uiso 1 1 calc R . . O13 O 2.2120(4) 1.6679(4) -0.1034(3) 0.0137(8) Uani 1 1 d . . . O29 O 1.7056(4) 1.1395(3) 0.9452(3) 0.0110(8) Uani 1 1 d . . . C22 C 2.0355(5) 1.2784(5) 0.0253(4) 0.0101(11) Uani 1 1 d . . . O30 O 1.4869(4) 1.2124(3) 0.9371(3) 0.0112(8) Uani 1 1 d . . . C4 C 2.2257(5) 1.6556(5) -0.0164(4) 0.0091(10) Uani 1 1 d . . . C5 C 2.2843(5) 1.5609(5) 0.0258(4) 0.0098(11) Uani 1 1 d . . . C7 C 2.1217(5) 1.8401(5) -0.0155(4) 0.0120(11) Uani 1 1 d . . . H7A H 2.1462 1.8623 -0.0857 0.014 Uiso 1 1 calc R . . H7B H 2.1468 1.9067 -0.0014 0.014 Uiso 1 1 calc R . . C39 C 1.3681(5) 1.4110(5) 0.7534(4) 0.0088(11) Uani 1 1 d . . . H39 H 1.3030 1.4157 0.7270 0.011 Uiso 1 1 calc R . . O32 O 1.6132(4) 0.9500(4) 0.9332(3) 0.0122(8) Uani 1 1 d . . . C36 C 1.5647(5) 1.3984(5) 0.8248(4) 0.0101(11) Uani 1 1 d . . . O6 O 1.7434(4) 1.9959(4) 0.1921(4) 0.0228(10) Uani 1 1 d . . . O18 O 2.1023(4) 1.3372(4) 0.5252(3) 0.0160(9) Uani 1 1 d . . . C41 C 1.4758(5) 1.3059(5) 0.8620(4) 0.0077(10) Uani 1 1 d . . . C38 C 1.4546(5) 1.5050(5) 0.7190(4) 0.0107(11) Uani 1 1 d . . . C1 C 2.2690(5) 1.6290(5) 0.1542(4) 0.0108(11) Uani 1 1 d . . . C35 C 1.6753(5) 1.3885(5) 0.8623(4) 0.0106(11) Uani 1 1 d . . . H35A H 1.7113 1.4671 0.8493 0.013 Uiso 1 1 calc R . . H35B H 1.6490 1.3466 0.9323 0.013 Uiso 1 1 calc R . . C52 C 1.7953(5) 0.8472(5) 0.7118(4) 0.0116(11) Uani 1 1 d . . . C30 C 1.9469(5) 1.2139(5) 0.7192(4) 0.0092(10) Uani 1 1 d . . . H30 H 2.0063 1.1776 0.6865 0.011 Uiso 1 1 calc R . . C10 C 1.7970(5) 1.8266(5) 0.1317(4) 0.0107(10) Uani 1 1 d . . . O31 O 1.3895(4) 1.0106(4) 0.9490(3) 0.0112(8) Uani 1 1 d . . . C48 C 1.3730(5) 1.0206(5) 0.8630(4) 0.0082(10) Uani 1 1 d . . . C17 C 1.6550(5) 1.3492(5) 0.1623(4) 0.0133(11) Uani 1 1 d . . . C23 C 2.0479(5) 1.1791(5) 0.0966(5) 0.0130(11) Uani 1 1 d . . . H23 H 1.9879 1.1148 0.1228 0.016 Uiso 1 1 calc R . . C14 C 1.7265(5) 1.6584(5) -0.0141(5) 0.0132(11) Uani 1 1 d . . . H14A H 1.6412 1.6750 0.0000 0.016 Uiso 1 1 calc R . . H14B H 1.7605 1.6824 -0.0843 0.016 Uiso 1 1 calc R . . C44 C 1.2858(5) 1.1224(5) 0.7378(4) 0.0098(10) Uani 1 1 d . . . H44 H 1.2445 1.1843 0.7086 0.012 Uiso 1 1 calc R . . C45 C 1.3183(5) 1.0384(5) 0.6985(4) 0.0081(10) Uani 1 1 d . . . C43 C 1.3141(5) 1.1160(5) 0.8212(4) 0.0084(10) Uani 1 1 d . . . C3 C 2.1865(5) 1.7367(5) 0.0271(4) 0.0109(11) Uani 1 1 d . . . C20 C 1.8228(5) 1.4716(5) -0.0105(4) 0.0096(10) Uani 1 1 d . . . C31 C 1.8651(5) 1.1499(5) 0.8089(4) 0.0079(10) Uani 1 1 d . . . C47 C 1.4086(5) 0.9371(5) 0.8220(4) 0.0086(10) Uani 1 1 d . . . O11 O 2.2682(4) 1.0667(4) 0.2491(3) 0.0193(9) Uani 1 1 d . . . C32 C 1.7797(5) 1.2059(5) 0.8552(4) 0.0084(10) Uani 1 1 d . . . C53 C 1.8610(5) 0.9109(5) 0.7441(4) 0.0104(10) Uani 1 1 d . . . H53 H 1.9460 0.9273 0.7164 0.012 Uiso 1 1 calc R . . C6 C 2.3063(5) 1.5492(5) 0.1111(4) 0.0085(10) Uani 1 1 d . . . H6 H 2.3469 1.4865 0.1399 0.010 Uiso 1 1 calc R . . O12 O 2.1825(5) 0.9540(4) 0.1787(4) 0.0250(11) Uani 1 1 d . . . C2 C 2.2101(5) 1.7218(5) 0.1121(4) 0.0115(11) Uani 1 1 d . . . H2 H 2.1856 1.7759 0.1424 0.014 Uiso 1 1 calc R . . C29 C 1.9380(5) 1.3328(5) 0.6798(4) 0.0094(11) Uani 1 1 d . . . C56 C 1.8721(5) 1.0199(5) 0.8527(4) 0.0092(10) Uani 1 1 d . . . H56A H 1.9577 1.0044 0.8370 0.011 Uiso 1 1 calc R . . H56B H 1.8396 0.9943 0.9230 0.011 Uiso 1 1 calc R . . C15 C 1.7313(5) 1.5292(5) 0.0313(4) 0.0084(10) Uani 1 1 d . . . C51 C 1.6703(5) 0.8235(4) 0.7509(4) 0.0080(10) Uani 1 1 d . . . H51 H 1.6262 0.7810 0.7280 0.010 Uiso 1 1 calc R . . C33 C 1.7704(5) 1.3245(5) 0.8153(4) 0.0075(10) Uani 1 1 d . . . C26 C 2.2270(5) 1.3669(5) 0.0199(4) 0.0078(10) Uani 1 1 d . . . C16 C 1.6477(5) 1.4653(5) 0.1178(4) 0.0104(11) Uani 1 1 d . . . H16 H 1.5848 1.5021 0.1467 0.012 Uiso 1 1 calc R . . C34 C 1.8517(5) 1.3870(5) 0.7260(4) 0.0102(10) Uani 1 1 d . . . H34 H 1.8476 1.4676 0.6968 0.012 Uiso 1 1 calc R . . C46 C 1.3798(5) 0.9473(5) 0.7389(4) 0.0089(10) Uani 1 1 d . . . H46 H 1.4024 0.8917 0.7098 0.011 Uiso 1 1 calc R . . O5 O 1.5891(4) 1.8335(4) 0.2482(4) 0.0269(11) Uani 1 1 d . . . C55 C 1.6766(5) 0.9229(5) 0.8569(4) 0.0076(10) Uani 1 1 d . . . C11 C 1.7346(5) 1.7678(5) 0.0943(4) 0.0149(12) Uani 1 1 d . . . H11 H 1.6491 1.7533 0.1187 0.018 Uiso 1 1 calc R . . C28 C 2.3214(5) 1.4709(5) -0.0190(4) 0.0096(10) Uani 1 1 d . . . H28A H 2.3979 1.4437 -0.0075 0.011 Uiso 1 1 calc R . . H28B H 2.3364 1.5074 -0.0889 0.011 Uiso 1 1 calc R . . C18 C 1.7465(5) 1.2933(5) 0.1211(4) 0.0119(11) Uani 1 1 d . . . H18 H 1.7513 1.2134 0.1531 0.014 Uiso 1 1 calc R . . C21 C 1.9272(5) 1.2880(5) -0.0114(4) 0.0102(11) Uani 1 1 d . . . H21A H 1.8911 1.2092 0.0022 0.012 Uiso 1 1 calc R . . H21B H 1.9539 1.3289 -0.0815 0.012 Uiso 1 1 calc R . . C25 C 2.2367(5) 1.2661(5) 0.0928(4) 0.0099(10) Uani 1 1 d . . . H25 H 2.3039 1.2614 0.1168 0.012 Uiso 1 1 calc R . . O25 O 1.1469(5) 1.0670(6) 0.6202(4) 0.0310(13) Uani 1 1 d . . . C19 C 1.8303(5) 1.3534(5) 0.0340(4) 0.0088(10) Uani 1 1 d . . . C27 C 2.1274(5) 1.3706(5) -0.0139(4) 0.0101(11) Uani 1 1 d . . . C37 C 1.5540(5) 1.4993(5) 0.7543(4) 0.0118(11) Uani 1 1 d . . . H37 H 1.6131 1.5641 0.7301 0.014 Uiso 1 1 calc R . . C50 C 1.6111(5) 0.8616(5) 0.8223(4) 0.0095(10) Uani 1 1 d . . . C54 C 1.8021(5) 0.9505(4) 0.8171(4) 0.0065(10) Uani 1 1 d . . . C49 C 1.4734(5) 0.8364(5) 0.8655(4) 0.0099(10) Uani 1 1 d . . . H49A H 1.4460 0.7674 0.8555 0.012 Uiso 1 1 calc R . . H49B H 1.4521 0.8184 0.9352 0.012 Uiso 1 1 calc R . . C13 C 1.9206(5) 1.7561(5) -0.0133(4) 0.0114(11) Uani 1 1 d . . . O2 O 2.3141(7) 1.4968(5) 0.3064(4) 0.0408(16) Uani 1 1 d . . . O8 O 1.5110(4) 1.3344(4) 0.3277(3) 0.0180(9) Uani 1 1 d . . . O19 O 2.1327(5) 1.4763(5) 0.5957(4) 0.0269(11) Uani 1 1 d . . . C24 C 2.1478(5) 1.1724(5) 0.1304(4) 0.0094(10) Uani 1 1 d . . . O10 O 2.0519(4) 1.0172(4) 0.2988(4) 0.0261(11) Uani 1 1 d . . . O7 O 1.5872(5) 1.1586(4) 0.3079(4) 0.0359(14) Uani 1 1 d . . . C9 C 1.9218(5) 1.8487(5) 0.0969(4) 0.0113(11) Uani 1 1 d . . . H9 H 1.9640 1.8877 0.1235 0.014 Uiso 1 1 calc R . . C12 C 1.7960(5) 1.7299(5) 0.0211(4) 0.0120(11) Uani 1 1 d . . . O27 O 1.9884(7) 0.8393(7) 0.5851(7) 0.087(4) Uani 1 1 d . . . O22 O 1.3163(6) 1.6293(6) 0.6330(6) 0.065(3) Uani 1 1 d . . . O9 O 1.4400(5) 1.2470(5) 0.2328(4) 0.0311(13) Uani 1 1 d . . . O3 O 2.4109(6) 1.6890(5) 0.2331(4) 0.0420(16) Uani 1 1 d . . . O23 O 1.3507(5) 1.1416(5) 0.5175(3) 0.0312(12) Uani 1 1 d . . . O28 O 1.8453(10) 0.6733(7) 0.6642(8) 0.122(6) Uani 1 1 d . . . O26 O 1.8112(12) 0.8277(16) 0.5497(9) 0.141(7) Uani 1 1 d . . . O21 O 1.4822(11) 1.7269(5) 0.6457(6) 0.080(3) Uani 1 1 d . . . O15 O 1.8970(4) 1.5360(4) -0.0995(3) 0.0156(9) Uani 1 1 d . . . O14 O 1.9854(4) 1.7277(4) -0.0895(3) 0.0136(8) Uani 1 1 d . . . O16 O 2.1164(4) 1.4639(4) -0.0884(3) 0.0162(9) Uani 1 1 d . . . O17 O 1.9797(4) 1.4976(4) 0.5138(3) 0.0222(10) Uani 1 1 d . . . O36 O 1.6376(5) 1.4016(4) 0.4727(4) 0.0297(12) Uani 1 1 d . . . O37 O 1.6399(5) 1.3478(5) 0.6238(4) 0.0316(12) Uani 1 1 d . . . O33 O 1.8587(5) 1.5591(5) 0.3446(4) 0.0280(11) Uani 1 1 d . . . N2 N 1.6215(6) 1.1881(5) 0.4764(5) 0.0251(13) Uani 1 1 d . . . O20 O 1.5047(7) 1.6230(6) 0.5392(4) 0.0520(19) Uani 1 1 d . . . C61 C 1.6215(7) 1.1993(7) 0.5661(6) 0.0274(16) Uani 1 1 d . . . H61 H 1.5443 1.1607 0.6166 0.033 Uiso 1 1 calc R . . C60 C 1.6324(6) 1.3310(6) 0.5477(5) 0.0221(13) Uani 1 1 d . . . O4 O 1.7625(5) 1.8052(5) 0.3053(3) 0.0250(11) Uani 1 1 d . . . O1 O 2.1990(8) 1.6539(10) 0.3146(5) 0.085(4) Uani 1 1 d . . . O38 O 1.8370(5) 1.2085(5) 0.5276(4) 0.0288(11) Uani 1 1 d . . . O34 O 1.8177(5) 1.5308(5) 0.2229(4) 0.0295(12) Uani 1 1 d . . . O35 O 1.8471(5) 1.2763(5) 0.3131(4) 0.0299(11) Uani 1 1 d . . . C57 C 1.8781(6) 1.5150(6) 0.2854(5) 0.0198(13) Uani 1 1 d . . . N1 N 2.0109(6) 1.3967(6) 0.3634(4) 0.0253(13) Uani 1 1 d . . . C58 C 1.9793(6) 1.4396(7) 0.2725(5) 0.0248(15) Uani 1 1 d . . . H58 H 2.0509 1.4897 0.2214 0.030 Uiso 1 1 calc R . . C59 C 1.9505(7) 1.3429(6) 0.2441(5) 0.0249(14) Uani 1 1 d . . . H59A H 1.9363 1.3738 0.1809 0.030 Uiso 1 1 calc R . . H59B H 2.0187 1.2949 0.2399 0.030 Uiso 1 1 calc R . . C62 C 1.7263(7) 1.1456(6) 0.5965(5) 0.0260(15) Uani 1 1 d . . . H62A H 1.7222 1.1476 0.6599 0.031 Uiso 1 1 calc R . . H62B H 1.7233 1.0636 0.6016 0.031 Uiso 1 1 calc R . . Cs1 Cs 1.98212(3) 1.75868(3) 0.38619(3) 0.02226(10) Uani 1 1 d . . . Cs2 Cs 1.41734(5) 0.92949(4) 0.39375(4) 0.03718(14) Uani 1 1 d . . . O40 O 2.2375(8) 1.7276(6) 0.4613(6) 0.057(2) Uani 1 1 d . . . Na2 Na 1.6663(3) 1.6149(3) 0.4173(2) 0.0279(6) Uani 1 1 d . . . O42 O 2.2008(4) 1.2539(4) 0.3453(3) 0.0163(9) Uani 1 1 d . . . Na1 Na 2.3053(2) 1.3289(2) 0.43216(17) 0.0146(5) Uani 1 1 d . . . O49 O 2.4108(4) 0.9154(4) 0.1419(3) 0.0205(10) Uani 1 1 d . . . O48 O 1.5326(4) 2.0806(4) 0.1409(4) 0.0218(10) Uani 1 1 d . . . O46 O 1.1662(7) 0.7501(6) 0.7071(5) 0.0512(17) Uani 1 1 d . . . O39 O 1.7538(5) 1.5645(5) 0.5455(4) 0.0301(11) Uani 1 1 d . . . O45 O 1.8176(5) 1.0536(5) 0.3354(4) 0.0323(12) Uani 1 1 d . . . O44 O 2.0540(8) 1.5879(7) 0.7145(6) 0.061(2) Uani 1 1 d . . . O43 O 1.5948(5) 1.5706(5) 0.3040(4) 0.0299(12) Uani 1 1 d . . . O41 O 2.3684(6) 1.4171(6) 0.5248(5) 0.0408(14) Uani 1 1 d . . . O47 O 2.0271(4) 1.0894(4) 0.4894(4) 0.0228(10) Uani 1 1 d . . . Cl1 Cl 1.6182(2) 0.9283(2) 0.4705(2) 0.0633(9) Uani 1 1 d . . . O24 O 1.2905(6) 0.9360(5) 0.5875(4) 0.0371(14) Uani 1 1 d . . . C8 C 1.9844(5) 1.8140(5) 0.0236(4) 0.0082(10) Uiso 1 1 d . . . C40 C 1.3758(5) 1.3098(5) 0.8261(4) 0.0075(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 S4 0.0090(6) 0.0058(6) 0.0238(8) -0.0017(5) -0.0068(6) 0.0020(5) S6 0.0145(7) 0.0088(6) 0.0283(8) -0.0019(6) -0.0096(6) 0.0032(5) S8 0.0164(8) 0.0250(8) 0.0276(9) -0.0198(7) -0.0007(6) 0.0029(6) S5 0.0106(6) 0.0098(6) 0.0164(7) -0.0043(5) 0.0031(5) 0.0002(5) S7 0.0133(7) 0.0110(6) 0.0137(7) -0.0059(5) -0.0069(5) 0.0055(5) S1 0.0182(7) 0.0164(7) 0.0150(7) -0.0083(6) -0.0099(6) 0.0118(6) S2 0.0108(7) 0.0149(7) 0.0191(7) -0.0062(6) -0.0036(5) 0.0057(6) S3 0.0099(6) 0.0078(6) 0.0221(7) -0.0038(6) 0.0033(5) -0.0016(5) C42 0.007(3) 0.010(3) 0.013(3) -0.003(2) -0.002(2) 0.002(2) O13 0.019(2) 0.0105(19) 0.0103(19) -0.0008(16) -0.0058(16) 0.0004(16) O29 0.0133(19) 0.0103(19) 0.0084(18) -0.0023(15) -0.0030(15) 0.0010(16) C22 0.007(3) 0.015(3) 0.011(3) -0.007(2) -0.003(2) 0.004(2) O30 0.0114(19) 0.0086(18) 0.014(2) -0.0026(16) -0.0059(16) 0.0024(16) C4 0.003(2) 0.009(2) 0.013(3) 0.000(2) -0.0016(19) -0.001(2) C5 0.005(2) 0.006(2) 0.015(3) -0.002(2) 0.000(2) -0.002(2) C7 0.009(3) 0.007(2) 0.018(3) -0.002(2) -0.005(2) -0.002(2) C39 0.009(3) 0.004(2) 0.016(3) -0.008(2) -0.004(2) 0.003(2) O32 0.0122(19) 0.0135(19) 0.013(2) -0.0079(16) -0.0031(15) 0.0046(16) C36 0.006(2) 0.008(2) 0.019(3) -0.011(2) 0.000(2) 0.002(2) O6 0.021(2) 0.019(2) 0.031(3) -0.014(2) -0.005(2) 0.0038(19) O18 0.0108(19) 0.013(2) 0.019(2) -0.0084(17) 0.0059(16) 0.0029(16) C41 0.007(2) 0.010(2) 0.009(2) -0.008(2) -0.0017(19) 0.002(2) C38 0.008(3) 0.006(2) 0.016(3) -0.005(2) 0.000(2) 0.002(2) C1 0.004(2) 0.010(3) 0.013(3) -0.001(2) 0.000(2) 0.002(2) C35 0.008(3) 0.011(3) 0.017(3) -0.010(2) -0.003(2) 0.000(2) C52 0.011(3) 0.007(2) 0.015(3) -0.002(2) -0.002(2) 0.003(2) C30 0.001(2) 0.012(3) 0.016(3) -0.008(2) -0.001(2) 0.002(2) C10 0.010(3) 0.006(2) 0.014(3) -0.002(2) -0.002(2) 0.006(2) O31 0.0112(19) 0.0118(19) 0.0093(19) -0.0017(15) -0.0039(15) -0.0003(16) C48 0.007(2) 0.009(2) 0.009(2) -0.004(2) -0.0023(19) -0.004(2) C17 0.012(3) 0.009(3) 0.012(3) 0.001(2) 0.000(2) -0.002(2) C23 0.010(3) 0.006(2) 0.022(3) -0.004(2) -0.004(2) 0.002(2) C14 0.008(3) 0.006(2) 0.025(3) -0.001(2) -0.009(2) 0.002(2) C44 0.005(2) 0.008(2) 0.012(3) -0.002(2) 0.000(2) 0.004(2) C45 0.005(2) 0.005(2) 0.015(3) -0.001(2) -0.006(2) -0.0005(19) C43 0.002(2) 0.007(2) 0.015(3) -0.005(2) 0.0003(19) 0.0005(19) C3 0.008(2) 0.005(2) 0.017(3) 0.000(2) -0.004(2) 0.003(2) C20 0.007(2) 0.010(2) 0.017(3) -0.007(2) -0.009(2) 0.002(2) C31 0.008(2) 0.007(2) 0.009(2) -0.003(2) -0.003(2) 0.000(2) C47 0.005(2) 0.007(2) 0.011(3) 0.002(2) -0.003(2) -0.002(2) O11 0.022(2) 0.012(2) 0.026(2) -0.0018(18) -0.0168(19) 0.0035(18) C32 0.004(2) 0.010(2) 0.009(2) -0.001(2) -0.0010(19) 0.000(2) C53 0.006(2) 0.005(2) 0.015(3) -0.001(2) 0.001(2) -0.0011(19) C6 0.006(2) 0.005(2) 0.015(3) -0.003(2) -0.005(2) 0.0005(19) O12 0.028(3) 0.014(2) 0.044(3) -0.012(2) -0.024(2) 0.0031(19) C2 0.009(3) 0.008(2) 0.017(3) -0.007(2) -0.001(2) 0.000(2) C29 0.011(3) 0.009(3) 0.008(2) -0.005(2) 0.000(2) 0.001(2) C56 0.008(2) 0.009(2) 0.012(3) -0.002(2) -0.006(2) 0.002(2) C15 0.005(2) 0.005(2) 0.018(3) -0.005(2) -0.008(2) 0.0039(19) C51 0.007(2) 0.004(2) 0.014(3) -0.003(2) -0.005(2) 0.0027(19) C33 0.005(2) 0.009(2) 0.011(2) -0.006(2) -0.0040(19) 0.0029(19) C26 0.005(2) 0.007(2) 0.011(2) -0.005(2) -0.0012(19) 0.0005(19) C16 0.003(2) 0.009(2) 0.020(3) -0.005(2) -0.004(2) 0.000(2) C34 0.009(3) 0.007(2) 0.014(3) -0.003(2) -0.005(2) 0.001(2) C46 0.004(2) 0.006(2) 0.017(3) -0.005(2) -0.003(2) 0.0013(19) O5 0.009(2) 0.022(2) 0.042(3) -0.010(2) 0.002(2) 0.0001(19) C55 0.009(2) 0.006(2) 0.009(2) -0.0035(19) -0.003(2) 0.005(2) C11 0.009(3) 0.013(3) 0.020(3) -0.001(2) -0.006(2) 0.005(2) C28 0.006(2) 0.006(2) 0.014(3) -0.005(2) 0.001(2) -0.003(2) C18 0.005(2) 0.008(2) 0.020(3) -0.001(2) -0.006(2) 0.001(2) C21 0.007(2) 0.012(3) 0.015(3) -0.009(2) -0.005(2) 0.002(2) C25 0.008(3) 0.010(3) 0.012(3) -0.004(2) -0.005(2) 0.003(2) O25 0.018(2) 0.058(4) 0.028(3) -0.023(3) -0.013(2) 0.007(2) C19 0.004(2) 0.008(2) 0.017(3) -0.006(2) -0.006(2) 0.002(2) C27 0.007(2) 0.008(2) 0.012(3) -0.003(2) 0.002(2) 0.004(2) C37 0.010(3) 0.012(3) 0.013(3) -0.006(2) 0.000(2) 0.003(2) C50 0.013(3) 0.003(2) 0.009(2) 0.0028(19) -0.005(2) 0.002(2) C54 0.005(2) 0.006(2) 0.008(2) -0.0001(19) -0.0051(19) -0.0012(19) C49 0.009(3) 0.004(2) 0.015(3) -0.001(2) -0.003(2) 0.002(2) C13 0.011(3) 0.004(2) 0.016(3) 0.003(2) -0.007(2) 0.001(2) O2 0.077(5) 0.018(3) 0.029(3) 0.003(2) -0.035(3) -0.001(3) O8 0.024(2) 0.013(2) 0.016(2) -0.0066(17) -0.0028(18) -0.0023(17) O19 0.021(2) 0.030(3) 0.028(3) -0.016(2) 0.003(2) -0.007(2) C24 0.006(2) 0.007(2) 0.014(3) -0.002(2) -0.003(2) 0.000(2) O10 0.015(2) 0.018(2) 0.027(3) 0.0100(19) -0.0013(19) 0.0035(18) O7 0.037(3) 0.014(2) 0.036(3) 0.000(2) 0.010(2) 0.006(2) C9 0.012(3) 0.003(2) 0.018(3) 0.001(2) -0.010(2) 0.002(2) C12 0.013(3) 0.004(2) 0.018(3) 0.001(2) -0.008(2) 0.003(2) O27 0.054(5) 0.063(5) 0.128(8) -0.083(6) 0.060(5) -0.041(4) O22 0.032(3) 0.049(4) 0.082(5) 0.030(4) -0.040(4) 0.000(3) O9 0.019(2) 0.049(3) 0.026(3) -0.024(3) 0.006(2) -0.018(2) O3 0.058(4) 0.028(3) 0.038(3) 0.008(2) -0.037(3) -0.014(3) O23 0.033(3) 0.032(3) 0.015(2) 0.008(2) -0.006(2) -0.010(2) O28 0.139(9) 0.042(4) 0.123(8) -0.064(5) 0.101(7) -0.061(5) O26 0.134(10) 0.294(19) 0.123(9) -0.178(12) -0.107(8) 0.162(12) O21 0.192(11) 0.008(3) 0.069(5) -0.007(3) -0.093(6) 0.007(4) O15 0.015(2) 0.021(2) 0.0079(19) -0.0044(17) -0.0004(16) -0.0062(18) O14 0.0100(19) 0.014(2) 0.014(2) -0.0044(16) -0.0014(16) 0.0013(17) O16 0.019(2) 0.013(2) 0.012(2) 0.0020(17) -0.0074(18) 0.0017(18) O17 0.026(2) 0.0072(19) 0.018(2) 0.0069(17) 0.0028(19) 0.0057(18) O36 0.035(3) 0.020(2) 0.034(3) -0.004(2) -0.018(2) 0.006(2) O37 0.038(3) 0.029(3) 0.029(3) -0.015(2) -0.006(2) 0.005(2) O33 0.029(3) 0.027(3) 0.041(3) -0.018(2) -0.021(2) 0.011(2) N2 0.028(3) 0.016(3) 0.034(3) -0.008(2) -0.015(3) 0.003(2) O20 0.074(5) 0.046(4) 0.027(3) -0.007(3) -0.010(3) 0.036(4) C61 0.030(4) 0.024(4) 0.029(4) -0.010(3) -0.007(3) 0.006(3) C60 0.020(3) 0.021(3) 0.026(3) -0.007(3) -0.010(3) 0.005(3) O4 0.029(3) 0.029(3) 0.010(2) -0.0009(19) -0.0034(19) 0.002(2) O1 0.074(5) 0.181(10) 0.040(4) -0.073(5) -0.038(4) 0.106(6) O38 0.024(3) 0.026(3) 0.034(3) -0.007(2) -0.011(2) 0.007(2) O34 0.039(3) 0.031(3) 0.031(3) -0.015(2) -0.024(2) 0.014(2) O35 0.034(3) 0.023(2) 0.032(3) -0.013(2) -0.006(2) 0.003(2) C57 0.013(3) 0.030(3) 0.020(3) -0.011(3) -0.008(2) 0.005(3) N1 0.032(3) 0.029(3) 0.026(3) -0.016(3) -0.020(3) 0.017(3) C58 0.017(3) 0.037(4) 0.020(3) -0.012(3) -0.004(3) 0.015(3) C59 0.031(4) 0.026(3) 0.021(3) -0.012(3) -0.009(3) 0.010(3) C62 0.026(4) 0.022(3) 0.026(4) -0.003(3) -0.008(3) -0.004(3) Cs1 0.0251(2) 0.01193(17) 0.0262(2) -0.00521(15) -0.00427(16) 0.00367(15) Cs2 0.0383(3) 0.0410(3) 0.0326(3) -0.0166(2) -0.0068(2) 0.0032(2) O40 0.092(6) 0.032(3) 0.057(4) -0.021(3) -0.030(4) 0.012(4) Na2 0.0252(14) 0.0241(14) 0.0312(16) -0.0094(12) -0.0041(12) 0.0019(11) O42 0.016(2) 0.019(2) 0.022(2) -0.0129(18) -0.0112(17) 0.0073(17) Na1 0.0131(11) 0.0169(12) 0.0134(11) -0.0056(9) -0.0032(9) 0.0046(9) O49 0.020(2) 0.022(2) 0.021(2) -0.0052(19) -0.0111(18) 0.0096(19) O48 0.014(2) 0.020(2) 0.027(2) -0.0056(19) -0.0019(18) 0.0034(18) O46 0.062(5) 0.035(3) 0.047(4) -0.015(3) -0.001(3) 0.007(3) O39 0.029(3) 0.034(3) 0.026(3) -0.012(2) -0.006(2) 0.006(2) O45 0.034(3) 0.028(3) 0.042(3) -0.019(3) -0.015(3) 0.010(2) O44 0.075(5) 0.049(4) 0.064(5) -0.024(4) -0.024(4) 0.005(4) O43 0.019(2) 0.023(3) 0.042(3) -0.005(2) -0.010(2) 0.000(2) O41 0.044(3) 0.055(4) 0.043(3) -0.030(3) -0.028(3) 0.015(3) O47 0.019(2) 0.023(2) 0.027(3) -0.007(2) -0.012(2) 0.0035(19) Cl1 0.0365(12) 0.0318(12) 0.084(2) 0.0207(12) -0.0131(12) 0.0015(10) O24 0.066(4) 0.026(3) 0.035(3) -0.018(2) -0.031(3) 0.023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag S4 O11 1.456(5) . ? S4 O10 1.460(5) . ? S4 O12 1.469(5) . ? S4 C24 1.774(6) . ? S4 Cs1 3.7761(14) 1_545 ? S6 O20 1.403(7) . ? S6 O21 1.411(6) . ? S6 O22 1.436(6) . ? S6 C38 1.773(6) . ? S8 O28 1.341(8) . ? S8 O27 1.379(7) . ? S8 O26 1.491(9) . ? S8 C52 1.757(6) . ? S8 Cs1 3.7736(17) 1_545 ? S5 O18 1.453(4) . ? S5 O19 1.456(5) . ? S5 O17 1.477(5) . ? S5 C29 1.773(6) . ? S7 O23 1.438(5) . ? S7 O24 1.451(5) . ? S7 O25 1.460(5) . ? S7 C45 1.766(6) . ? S7 Cs2 3.9161(15) . ? S1 O2 1.424(6) . ? S1 O1 1.433(6) . ? S1 O3 1.440(6) . ? S1 C1 1.755(6) . ? S2 O4 1.447(5) . ? S2 O5 1.466(5) . ? S2 O6 1.467(5) . ? S2 C10 1.772(6) . ? S2 Cs2 3.9694(15) 1_565 ? S3 O7 1.445(6) . ? S3 O9 1.453(6) . ? S3 O8 1.465(5) . ? S3 C17 1.760(6) . ? S3 Cs2 4.0058(15) . ? C42 C43 1.516(8) . ? C42 C40 1.521(8) . ? O13 C4 1.373(7) . ? O29 C32 1.385(6) . ? C22 C23 1.382(8) . ? C22 C27 1.404(8) . ? C22 C21 1.511(8) . ? O30 C41 1.369(7) . ? C4 C3 1.407(8) . ? C4 C5 1.408(8) . ? C5 C6 1.388(8) . ? C5 C28 1.516(8) . ? C7 C3 1.526(8) . ? C7 C8 1.529(8) . ? C39 C38 1.386(8) . ? C39 C40 1.392(8) . ? O32 C55 1.367(7) . ? C36 C37 1.382(8) . ? C36 C41 1.387(8) . ? C36 C35 1.542(8) . ? O18 Na1 2.423(5) . ? C41 C40 1.418(7) . ? C38 C37 1.403(8) . ? C1 C6 1.385(8) . ? C1 C2 1.394(8) . ? C35 C33 1.529(8) . ? C52 C51 1.395(8) . ? C52 C53 1.399(9) . ? C30 C29 1.400(8) . ? C30 C31 1.408(8) . ? C10 C9 1.388(8) . ? C10 C11 1.391(9) . ? O31 C48 1.377(7) . ? C48 C47 1.402(8) . ? C48 C43 1.414(8) . ? C17 C16 1.376(8) . ? C17 C18 1.396(8) . ? C23 C24 1.395(8) . ? C14 C15 1.516(7) . ? C14 C12 1.527(8) . ? C44 C45 1.386(8) . ? C44 C43 1.409(8) . ? C45 C46 1.390(7) . ? C3 C2 1.384(8) . ? C20 O15 1.371(7) . ? C20 C19 1.399(8) . ? C20 C15 1.413(8) . ? C31 C32 1.391(8) . ? C31 C56 1.526(8) . ? C47 C46 1.397(8) . ? C47 C49 1.509(7) . ? O11 Cs2 3.242(4) 1_655 ? C32 C33 1.399(8) . ? C53 C54 1.403(8) . ? O12 Cs1 3.483(5) 1_545 ? C29 C34 1.381(8) . ? C56 C54 1.518(7) . ? C15 C16 1.387(8) . ? C51 C50 1.373(8) . ? C33 C34 1.399(8) . ? C26 C27 1.395(8) . ? C26 C25 1.397(8) . ? C26 C28 1.522(7) . ? O5 Cs2 3.149(5) 1_565 ? C55 C50 1.402(8) . ? C55 C54 1.405(7) . ? C11 C12 1.400(9) . ? C18 C19 1.383(8) . ? C21 C19 1.541(8) . ? C25 C24 1.396(8) . ? C27 O16 1.362(7) . ? C50 C49 1.536(8) . ? C13 O14 1.379(8) . ? C13 C8 1.390(8) . ? C13 C12 1.390(8) . ? O2 Na1 2.290(6) . ? O8 Na1 2.474(5) 1_455 ? O10 Cs1 3.020(5) 1_545 ? O7 Cs2 3.104(5) . ? C9 C8 1.381(8) . ? O27 Cs1 3.606(9) 1_545 ? O23 Na1 2.380(6) 1_455 ? O23 Cs2 3.737(6) . ? O26 Cs1 3.147(9) 1_545 ? O17 Cs1 3.149(4) . ? O36 C60 1.180(9) . ? O36 Na2 2.467(6) . ? O37 C60 1.304(9) . ? O33 C57 1.203(9) . ? O33 Na2 2.426(6) . ? O33 Cs1 3.202(5) . ? N2 C61 1.460(10) . ? O20 Na2 2.302(7) . ? C61 C62 1.500(11) . ? C61 C60 1.554(10) . ? O4 Na2 2.431(6) . ? O4 Cs1 3.119(5) . ? O1 Cs1 2.950(6) . ? O38 C62 1.437(9) . ? O34 C57 1.319(8) . ? O35 C59 1.396(9) . ? C57 C58 1.511(9) . ? N1 C58 1.486(9) . ? C58 C59 1.483(11) . ? Cs1 O10 3.020(5) 1_565 ? Cs1 O26 3.147(9) 1_565 ? Cs1 O39 3.343(6) . ? Cs1 O40 3.457(9) . ? Cs1 O12 3.483(5) 1_565 ? Cs1 O27 3.606(9) 1_565 ? Cs1 S8 3.7736(17) 1_565 ? Cs1 S4 3.7761(14) 1_565 ? Cs2 Cl1 2.905(3) . ? Cs2 O40 2.945(8) 1_445 ? Cs2 O24 3.009(6) . ? Cs2 O5 3.149(5) 1_545 ? Cs2 O11 3.242(4) 1_455 ? Cs2 O48 3.584(5) 1_545 ? Cs2 S2 3.9694(15) 1_545 ? Cs2 Na2 4.817(3) 1_545 ? O40 Cs2 2.945(8) 1_665 ? Na2 O43 2.377(7) . ? Na2 O39 2.391(6) . ? Na2 Cs2 4.817(3) 1_565 ? O42 Na1 2.449(5) . ? Na1 O41 2.355(6) . ? Na1 O23 2.380(6) 1_655 ? Na1 O8 2.474(5) 1_655 ? O48 Cs2 3.584(5) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 S4 O10 112.4(3) . . ? O11 S4 O12 111.6(3) . . ? O10 S4 O12 111.7(3) . . ? O11 S4 C24 108.0(3) . . ? O10 S4 C24 106.2(3) . . ? O12 S4 C24 106.6(3) . . ? O11 S4 Cs1 112.35(19) . 1_545 ? O10 S4 Cs1 48.7(2) . 1_545 ? O12 S4 Cs1 67.3(2) . 1_545 ? C24 S4 Cs1 138.40(19) . 1_545 ? O20 S6 O21 117.1(6) . . ? O20 S6 O22 107.3(5) . . ? O21 S6 O22 112.5(6) . . ? O20 S6 C38 107.6(3) . . ? O21 S6 C38 106.7(3) . . ? O22 S6 C38 104.9(3) . . ? O28 S8 O27 121.2(7) . . ? O28 S8 O26 104.6(10) . . ? O27 S8 O26 106.0(9) . . ? O28 S8 C52 108.8(4) . . ? O27 S8 C52 109.7(4) . . ? O26 S8 C52 105.3(4) . . ? O28 S8 Cs1 87.1(4) . 1_545 ? O27 S8 Cs1 72.5(4) . 1_545 ? O26 S8 Cs1 54.4(3) . 1_545 ? C52 S8 Cs1 157.8(2) . 1_545 ? O18 S5 O19 112.7(3) . . ? O18 S5 O17 111.7(3) . . ? O19 S5 O17 112.0(3) . . ? O18 S5 C29 107.7(3) . . ? O19 S5 C29 106.4(3) . . ? O17 S5 C29 105.8(3) . . ? O23 S7 O24 113.1(4) . . ? O23 S7 O25 113.6(4) . . ? O24 S7 O25 111.0(4) . . ? O23 S7 C45 107.2(3) . . ? O24 S7 C45 105.4(3) . . ? O25 S7 C45 105.7(3) . . ? O23 S7 Cs2 72.2(3) . . ? O24 S7 Cs2 42.4(3) . . ? O25 S7 Cs2 120.6(2) . . ? C45 S7 Cs2 129.92(19) . . ? O2 S1 O1 112.6(6) . . ? O2 S1 O3 111.8(4) . . ? O1 S1 O3 112.8(6) . . ? O2 S1 C1 107.4(3) . . ? O1 S1 C1 105.3(3) . . ? O3 S1 C1 106.3(3) . . ? O4 S2 O5 110.9(3) . . ? O4 S2 O6 115.4(3) . . ? O5 S2 O6 112.3(3) . . ? O4 S2 C10 104.4(3) . . ? O5 S2 C10 106.9(3) . . ? O6 S2 C10 106.1(3) . . ? O4 S2 Cs2 94.2(2) . 1_565 ? O5 S2 Cs2 46.7(2) . 1_565 ? O6 S2 Cs2 83.0(2) . 1_565 ? C10 S2 Cs2 152.6(2) . 1_565 ? O7 S3 O9 111.2(4) . . ? O7 S3 O8 113.6(3) . . ? O9 S3 O8 112.3(3) . . ? O7 S3 C17 106.6(3) . . ? O9 S3 C17 105.2(3) . . ? O8 S3 C17 107.4(3) . . ? O7 S3 Cs2 42.8(2) . . ? O9 S3 Cs2 72.2(3) . . ? O8 S3 Cs2 115.17(19) . . ? C17 S3 Cs2 134.9(2) . . ? C43 C42 C40 113.5(5) . . ? C23 C22 C27 118.4(5) . . ? C23 C22 C21 121.4(5) . . ? C27 C22 C21 120.2(5) . . ? O13 C4 C3 121.2(5) . . ? O13 C4 C5 117.1(5) . . ? C3 C4 C5 121.6(5) . . ? C6 C5 C4 119.0(5) . . ? C6 C5 C28 119.7(5) . . ? C4 C5 C28 121.4(5) . . ? C3 C7 C8 112.4(5) . . ? C38 C39 C40 120.6(5) . . ? C37 C36 C41 119.9(5) . . ? C37 C36 C35 120.2(5) . . ? C41 C36 C35 119.9(5) . . ? S5 O18 Na1 133.9(3) . . ? O30 C41 C36 116.8(5) . . ? O30 C41 C40 121.7(5) . . ? C36 C41 C40 121.5(5) . . ? C39 C38 C37 121.0(5) . . ? C39 C38 S6 119.5(5) . . ? C37 C38 S6 119.5(4) . . ? C6 C1 C2 120.4(6) . . ? C6 C1 S1 119.7(4) . . ? C2 C1 S1 119.9(5) . . ? C33 C35 C36 111.6(4) . . ? C51 C52 C53 120.5(5) . . ? C51 C52 S8 119.3(4) . . ? C53 C52 S8 120.0(4) . . ? C29 C30 C31 118.0(5) . . ? C9 C10 C11 120.4(5) . . ? C9 C10 S2 119.7(5) . . ? C11 C10 S2 119.9(4) . . ? O31 C48 C47 121.1(5) . . ? O31 C48 C43 116.4(5) . . ? C47 C48 C43 122.4(5) . . ? C16 C17 C18 120.6(5) . . ? C16 C17 S3 120.1(5) . . ? C18 C17 S3 119.0(4) . . ? C22 C23 C24 120.6(5) . . ? C15 C14 C12 113.0(5) . . ? C45 C44 C43 120.0(5) . . ? C44 C45 C46 121.5(5) . . ? C44 C45 S7 117.7(4) . . ? C46 C45 S7 120.8(4) . . ? C44 C43 C48 117.7(5) . . ? C44 C43 C42 120.8(5) . . ? C48 C43 C42 121.6(5) . . ? C2 C3 C4 117.6(5) . . ? C2 C3 C7 119.0(5) . . ? C4 C3 C7 123.4(5) . . ? O15 C20 C19 122.3(5) . . ? O15 C20 C15 116.1(5) . . ? C19 C20 C15 121.4(5) . . ? C32 C31 C30 119.6(5) . . ? C32 C31 C56 121.5(5) . . ? C30 C31 C56 118.9(5) . . ? C46 C47 C48 118.0(5) . . ? C46 C47 C49 119.5(5) . . ? C48 C47 C49 122.5(5) . . ? S4 O11 Cs2 138.8(2) . 1_655 ? O29 C32 C31 116.9(5) . . ? O29 C32 C33 120.7(5) . . ? C31 C32 C33 122.3(5) . . ? C52 C53 C54 120.4(5) . . ? C1 C6 C5 120.0(5) . . ? S4 O12 Cs1 89.8(2) . 1_545 ? C3 C2 C1 121.4(5) . . ? C34 C29 C30 121.8(5) . . ? C34 C29 S5 119.6(4) . . ? C30 C29 S5 118.4(4) . . ? C54 C56 C31 112.2(4) . . ? C16 C15 C20 118.3(5) . . ? C16 C15 C14 120.1(5) . . ? C20 C15 C14 121.5(5) . . ? C50 C51 C52 119.9(5) . . ? C32 C33 C34 117.5(5) . . ? C32 C33 C35 124.0(5) . . ? C34 C33 C35 118.5(5) . . ? C27 C26 C25 118.3(5) . . ? C27 C26 C28 121.3(5) . . ? C25 C26 C28 120.3(5) . . ? C17 C16 C15 120.7(5) . . ? C29 C34 C33 120.7(5) . . ? C45 C46 C47 120.4(5) . . ? S2 O5 Cs2 113.6(3) . 1_565 ? O32 C55 C50 116.8(5) . . ? O32 C55 C54 121.9(5) . . ? C50 C55 C54 121.2(5) . . ? C10 C11 C12 120.9(5) . . ? C5 C28 C26 113.1(5) . . ? C19 C18 C17 120.5(5) . . ? C22 C21 C19 112.6(5) . . ? C24 C25 C26 120.1(5) . . ? C18 C19 C20 118.5(5) . . ? C18 C19 C21 119.2(5) . . ? C20 C19 C21 122.3(5) . . ? O16 C27 C26 121.0(5) . . ? O16 C27 C22 116.9(5) . . ? C26 C27 C22 122.1(5) . . ? C36 C37 C38 119.2(5) . . ? C51 C50 C55 119.9(5) . . ? C51 C50 C49 120.3(5) . . ? C55 C50 C49 119.7(5) . . ? C53 C54 C55 118.0(5) . . ? C53 C54 C56 121.0(5) . . ? C55 C54 C56 121.1(5) . . ? C47 C49 C50 112.3(4) . . ? O14 C13 C8 117.3(5) . . ? O14 C13 C12 119.8(5) . . ? C8 C13 C12 122.9(6) . . ? S1 O2 Na1 156.5(4) . . ? S3 O8 Na1 123.3(3) . 1_455 ? C23 C24 C25 120.4(5) . . ? C23 C24 S4 120.3(4) . . ? C25 C24 S4 119.3(4) . . ? S4 O10 Cs1 110.0(3) . 1_545 ? S3 O7 Cs2 118.8(3) . . ? C8 C9 C10 119.9(5) . . ? C13 C12 C11 117.0(6) . . ? C13 C12 C14 123.1(6) . . ? C11 C12 C14 119.9(5) . . ? S8 O27 Cs1 86.2(4) . 1_545 ? S7 O23 Na1 130.0(4) . 1_455 ? S7 O23 Cs2 86.3(3) . . ? Na1 O23 Cs2 118.54(19) 1_455 . ? S8 O26 Cs1 103.0(4) . 1_545 ? S5 O17 Cs1 143.4(3) . . ? C60 O36 Na2 130.2(5) . . ? C57 O33 Na2 126.2(5) . . ? C57 O33 Cs1 138.6(5) . . ? Na2 O33 Cs1 86.85(16) . . ? S6 O20 Na2 158.4(5) . . ? N2 C61 C62 110.1(6) . . ? N2 C61 C60 106.9(6) . . ? C62 C61 C60 110.3(6) . . ? O36 C60 O37 127.8(7) . . ? O36 C60 C61 122.0(7) . . ? O37 C60 C61 110.2(6) . . ? S2 O4 Na2 121.2(3) . . ? S2 O4 Cs1 147.5(3) . . ? Na2 O4 Cs1 88.67(16) . . ? S1 O1 Cs1 167.8(4) . . ? O33 C57 O34 124.0(6) . . ? O33 C57 C58 122.7(6) . . ? O34 C57 C58 113.2(6) . . ? C59 C58 N1 111.6(6) . . ? C59 C58 C57 114.1(6) . . ? N1 C58 C57 107.1(5) . . ? O35 C59 C58 108.0(6) . . ? O38 C62 C61 109.4(6) . . ? O1 Cs1 O10 105.7(3) . 1_565 ? O1 Cs1 O4 126.55(17) . . ? O10 Cs1 O4 87.01(14) 1_565 . ? O1 Cs1 O26 149.9(2) . 1_565 ? O10 Cs1 O26 81.5(4) 1_565 1_565 ? O4 Cs1 O26 82.32(19) . 1_565 ? O1 Cs1 O17 66.9(2) . . ? O10 Cs1 O17 159.09(14) 1_565 . ? O4 Cs1 O17 113.29(14) . . ? O26 Cs1 O17 95.8(3) 1_565 . ? O1 Cs1 O33 80.4(2) . . ? O10 Cs1 O33 139.46(14) 1_565 . ? O4 Cs1 O33 59.92(14) . . ? O26 Cs1 O33 113.4(3) 1_565 . ? O17 Cs1 O33 60.51(14) . . ? O1 Cs1 O39 113.6(3) . . ? O10 Cs1 O39 140.36(14) 1_565 . ? O4 Cs1 O39 73.57(13) . . ? O26 Cs1 O39 62.2(4) 1_565 . ? O17 Cs1 O39 49.27(13) . . ? O33 Cs1 O39 55.77(14) . . ? O1 Cs1 O40 52.9(2) . . ? O10 Cs1 O40 88.83(15) 1_565 . ? O4 Cs1 O40 175.38(16) . . ? O26 Cs1 O40 99.1(2) 1_565 . ? O17 Cs1 O40 71.04(16) . . ? O33 Cs1 O40 122.95(14) . . ? O39 Cs1 O40 110.99(16) . . ? O1 Cs1 O12 67.8(2) . 1_565 ? O10 Cs1 O12 43.03(13) 1_565 1_565 ? O4 Cs1 O12 93.50(12) . 1_565 ? O26 Cs1 O12 124.5(4) 1_565 1_565 ? O17 Cs1 O12 134.76(12) . 1_565 ? O33 Cs1 O12 111.51(13) . 1_565 ? O39 Cs1 O12 165.09(12) . 1_565 ? O40 Cs1 O12 82.07(15) . 1_565 ? O1 Cs1 O27 113.4(2) . 1_565 ? O10 Cs1 O27 75.76(18) 1_565 1_565 ? O4 Cs1 O27 120.03(19) . 1_565 ? O26 Cs1 O27 39.0(2) 1_565 1_565 ? O17 Cs1 O27 89.05(19) . 1_565 ? O33 Cs1 O27 139.52(15) . 1_565 ? O39 Cs1 O27 84.46(14) . 1_565 ? O40 Cs1 O27 60.7(2) . 1_565 ? O12 Cs1 O27 108.90(14) 1_565 1_565 ? O1 Cs1 S8 127.28(12) . 1_565 ? O10 Cs1 S8 88.19(11) 1_565 1_565 ? O4 Cs1 S8 104.29(10) . 1_565 ? O26 Cs1 S8 22.65(16) 1_565 1_565 ? O17 Cs1 S8 82.14(10) . 1_565 ? O33 Cs1 S8 120.45(11) . 1_565 ? O39 Cs1 S8 64.68(10) . 1_565 ? O40 Cs1 S8 77.58(13) . 1_565 ? O12 Cs1 S8 127.28(8) 1_565 1_565 ? O27 Cs1 S8 21.38(11) 1_565 1_565 ? O1 Cs1 S4 85.1(2) . 1_565 ? O10 Cs1 S4 21.31(10) 1_565 1_565 ? O4 Cs1 S4 95.27(10) . 1_565 ? O26 Cs1 S4 102.0(4) 1_565 1_565 ? O17 Cs1 S4 148.13(9) . 1_565 ? O33 Cs1 S4 131.57(11) . 1_565 ? O39 Cs1 S4 161.28(10) . 1_565 ? O40 Cs1 S4 80.14(13) . 1_565 ? O12 Cs1 S4 22.89(8) 1_565 1_565 ? O27 Cs1 S4 88.51(12) 1_565 1_565 ? S8 Cs1 S4 105.07(4) 1_565 1_565 ? Cl1 Cs2 O40 122.85(16) . 1_445 ? Cl1 Cs2 O24 78.67(14) . . ? O40 Cs2 O24 81.79(19) 1_445 . ? Cl1 Cs2 O7 64.08(13) . . ? O40 Cs2 O7 173.0(2) 1_445 . ? O24 Cs2 O7 99.68(16) . . ? Cl1 Cs2 O5 86.15(13) . 1_545 ? O40 Cs2 O5 90.84(18) 1_445 1_545 ? O24 Cs2 O5 155.67(15) . 1_545 ? O7 Cs2 O5 90.44(14) . 1_545 ? Cl1 Cs2 O11 149.45(9) . 1_455 ? O40 Cs2 O11 87.69(17) 1_445 1_455 ? O24 Cs2 O11 107.89(14) . 1_455 ? O7 Cs2 O11 85.38(14) . 1_455 ? O5 Cs2 O11 94.86(14) 1_545 1_455 ? Cl1 Cs2 O48 106.65(9) . 1_545 ? O40 Cs2 O48 117.20(17) 1_445 1_545 ? O24 Cs2 O48 148.59(13) . 1_545 ? O7 Cs2 O48 58.54(14) . 1_545 ? O5 Cs2 O48 54.43(12) 1_545 1_545 ? O11 Cs2 O48 52.50(11) 1_455 1_545 ? Cl1 Cs2 O23 76.14(11) . . ? O40 Cs2 O23 117.00(17) 1_445 . ? O24 Cs2 O23 40.08(13) . . ? O7 Cs2 O23 62.36(13) . . ? O5 Cs2 O23 151.95(12) 1_545 . ? O11 Cs2 O23 89.89(12) 1_455 . ? O48 Cs2 O23 109.94(11) 1_545 . ? Cl1 Cs2 S7 79.54(8) . . ? O40 Cs2 S7 97.06(15) 1_445 . ? O24 Cs2 S7 18.99(11) . . ? O7 Cs2 S7 83.16(11) . . ? O5 Cs2 S7 165.69(11) 1_545 . ? O11 Cs2 S7 97.35(9) 1_455 . ? O48 Cs2 S7 129.91(8) 1_545 . ? O23 Cs2 S7 21.49(8) . . ? Cl1 Cs2 S2 68.89(8) . 1_545 ? O40 Cs2 S2 108.12(16) 1_445 1_545 ? O24 Cs2 S2 146.34(12) . 1_545 ? O7 Cs2 S2 74.43(10) . 1_545 ? O5 Cs2 S2 19.79(10) 1_545 1_545 ? O11 Cs2 S2 104.66(9) 1_455 1_545 ? O48 Cs2 S2 55.22(8) 1_545 1_545 ? O23 Cs2 S2 133.05(9) . 1_545 ? S7 Cs2 S2 146.89(3) . 1_545 ? Cl1 Cs2 S3 80.98(5) . . ? O40 Cs2 S3 154.88(16) 1_445 . ? O24 Cs2 S3 96.94(11) . . ? O7 Cs2 S3 18.43(11) . . ? O5 Cs2 S3 99.34(9) 1_545 . ? O11 Cs2 S3 68.71(8) 1_455 . ? O48 Cs2 S3 54.88(8) 1_545 . ? O23 Cs2 S3 56.91(8) . . ? S7 Cs2 S3 78.33(3) . . ? S2 Cs2 S3 86.88(3) 1_545 . ? Cl1 Cs2 Na2 60.97(7) . 1_545 ? O40 Cs2 Na2 77.86(17) 1_445 1_545 ? O24 Cs2 Na2 111.22(11) . 1_545 ? O7 Cs2 Na2 107.69(11) . 1_545 ? O5 Cs2 Na2 44.45(11) 1_545 1_545 ? O11 Cs2 Na2 135.52(9) 1_455 1_545 ? O48 Cs2 Na2 97.74(8) 1_545 1_545 ? O23 Cs2 Na2 134.16(9) . 1_545 ? S7 Cs2 Na2 125.83(4) . 1_545 ? S2 Cs2 Na2 44.43(4) 1_545 1_545 ? S3 Cs2 Na2 124.97(4) . 1_545 ? Cs2 O40 Cs1 119.3(2) 1_665 . ? O20 Na2 O43 109.5(3) . . ? O20 Na2 O39 79.5(2) . . ? O43 Na2 O39 152.3(2) . . ? O20 Na2 O33 157.0(3) . . ? O43 Na2 O33 86.5(2) . . ? O39 Na2 O33 79.0(2) . . ? O20 Na2 O4 113.1(2) . . ? O43 Na2 O4 93.8(2) . . ? O39 Na2 O4 106.9(2) . . ? O33 Na2 O4 81.1(2) . . ? O20 Na2 O36 93.4(2) . . ? O43 Na2 O36 73.87(19) . . ? O39 Na2 O36 79.6(2) . . ? O33 Na2 O36 74.8(2) . . ? O4 Na2 O36 153.4(2) . . ? O20 Na2 Cs1 118.2(2) . . ? O43 Na2 Cs1 129.28(16) . . ? O39 Na2 Cs1 58.31(15) . . ? O33 Na2 Cs1 54.87(13) . . ? O4 Na2 Cs1 52.89(13) . . ? O36 Na2 Cs1 117.49(16) . . ? O20 Na2 Cs2 55.27(16) . 1_565 ? O43 Na2 Cs2 89.55(15) . 1_565 ? O39 Na2 Cs2 115.82(16) . 1_565 ? O33 Na2 Cs2 144.14(16) . 1_565 ? O4 Na2 Cs2 63.60(14) . 1_565 ? O36 Na2 Cs2 137.65(16) . 1_565 ? Cs1 Na2 Cs2 103.30(6) . 1_565 ? O2 Na1 O41 96.0(2) . . ? O2 Na1 O23 158.9(3) . 1_655 ? O41 Na1 O23 94.0(2) . 1_655 ? O2 Na1 O18 96.0(2) . . ? O41 Na1 O18 85.5(2) . . ? O23 Na1 O18 103.20(19) 1_655 . ? O2 Na1 O42 80.80(19) . . ? O41 Na1 O42 168.2(2) . . ? O23 Na1 O42 92.79(19) 1_655 . ? O18 Na1 O42 83.56(17) . . ? O2 Na1 O8 79.6(2) . 1_655 ? O41 Na1 O8 94.9(2) . 1_655 ? O23 Na1 O8 81.15(18) 1_655 1_655 ? O18 Na1 O8 175.60(19) . 1_655 ? O42 Na1 O8 95.65(17) . 1_655 ? Na2 O39 Cs1 84.22(17) . . ? S7 O24 Cs2 118.6(3) . . ? C9 C8 C13 118.9(5) . . ? C9 C8 C7 119.8(5) . . ? C13 C8 C7 121.3(5) . . ? C39 C40 C41 117.8(5) . . ? C39 C40 C42 120.6(5) . . ? C41 C40 C42 121.6(5) . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 2.697 _refine_diff_density_min -2.047 _refine_diff_density_rms 0.171 #END #______________________________________________