# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_mm140 _database_code_depnum_ccdc_archive 'CCDC 284293' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H39 Na O26 S4 Yb, C24 H20 P, 5(H2 O)' _chemical_formula_sum 'C52 H69 Na O31 P S4 Yb' _chemical_formula_weight 1545.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.271(3) _cell_length_b 11.375(2) _cell_length_c 26.372(4) _cell_angle_alpha 90.0 _cell_angle_beta 104.908(2) _cell_angle_gamma 90.0 _cell_volume 6166.1(17) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6446 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 28.66 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.665 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3156 _exptl_absorpt_coefficient_mu 1.778 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.347 _exptl_absorpt_correction_T_max 0.645 _exptl_absorpt_process_details 'SADABS - Bruker area detector absorption corrections' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker AXS CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 58944 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 28.98 _reflns_number_total 15191 _reflns_number_gt 12980 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL, v. 5.1' _computing_structure_refinement 'Bruker SHELXTL, v. 5.1' _computing_molecular_graphics 'Bruker SHELXTL, v. 5.1' _computing_publication_material 'Bruker SHELXTL, v. 5.1' _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^)+(0.0270P)^2^+9.5437P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15191 _refine_ls_number_parameters 904 _refine_ls_number_restraints 135 _refine_ls_R_factor_all 0.0389 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0666 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.024 _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 Yb1 Yb 0.071198(5) 0.536041(9) -0.109230(4) 0.01170(3) Uani 1 1 d . . . Na1 Na 0.08720(5) 0.03630(9) -0.08719(4) 0.0170(2) Uani 1 1 d . . . O1W O 0.08058(10) 0.53065(16) -0.02003(7) 0.0212(4) Uani 1 1 d D . . H1WA H 0.08223 0.46314 -0.00592 0.032 Uiso 1 1 d D . . H1WB H 0.09819 0.57808 0.00441 0.032 Uiso 1 1 d D . . O2W O -0.01449(9) 0.64710(17) -0.10005(7) 0.0185(4) Uani 1 1 d D . . H2WA H -0.04281 0.67510 -0.12606 0.028 Uiso 1 1 d D . . H2WB H -0.03188 0.64667 -0.07441 0.028 Uiso 1 1 d D . . O3W O 0.03896(9) 0.66221(15) -0.18080(7) 0.0179(4) Uani 1 1 d D . . H3WA H 0.04812 0.64678 -0.20962 0.027 Uiso 1 1 d D . . H3WB H 0.03885 0.73669 -0.17819 0.027 Uiso 1 1 d D . . O4W O 0.16544(9) 0.54353(16) -0.13830(7) 0.0173(4) Uani 1 1 d D . . H4WA H 0.16670 0.51347 -0.16753 0.026 Uiso 1 1 d D . . H4WB H 0.18566 0.60858 -0.13595 0.026 Uiso 1 1 d D . . O5W O 0.13362(9) 0.37310(16) -0.07896(7) 0.0183(4) Uani 1 1 d D . . H5WA H 0.12733 0.31524 -0.06047 0.027 Uiso 1 1 d D . . H5WB H 0.15680 0.34736 -0.09842 0.027 Uiso 1 1 d D . . O6W O -0.00383(9) 0.39823(16) -0.09905(8) 0.0228(4) Uani 1 1 d D . . H6WA H -0.00106 0.32569 -0.10591 0.034 Uiso 1 1 d D . . H6WB H -0.04017 0.40678 -0.09166 0.034 Uiso 1 1 d D . . O7W O 0.04515(9) 0.42437(16) -0.18606(7) 0.0181(4) Uani 1 1 d D . . H7WA H 0.00524 0.40866 -0.19935 0.027 Uiso 1 1 d D . . H7WB H 0.06677 0.37659 -0.19975 0.027 Uiso 1 1 d D . . O8W O -0.00239(9) 0.16489(17) -0.11896(7) 0.0214(4) Uani 1 1 d D . . H8WA H -0.02292 0.15552 -0.15090 0.032 Uiso 1 1 d D . . H8WB H -0.02835 0.14462 -0.10083 0.032 Uiso 1 1 d D . . O9W O 0.02939(9) -0.10791(16) -0.04851(7) 0.0202(4) Uani 1 1 d D . . H9WA H -0.01177 -0.10883 -0.05398 0.030 Uiso 1 1 d D . . H9WB H 0.03940 -0.17087 -0.06193 0.030 Uiso 1 1 d D . . O10W O 0.03300(10) -0.09529(17) -0.16940(8) 0.0241(4) Uani 1 1 d D . . H101 H -0.00625 -0.07188 -0.17834 0.036 Uiso 1 1 d D . . H102 H 0.05140 -0.06557 -0.19145 0.036 Uiso 1 1 d D . . O11W O -0.08948(10) 0.11900(17) -0.05941(8) 0.0240(4) Uani 1 1 d D . . H111 H -0.10470 0.05088 -0.06846 0.036 Uiso 1 1 d D . . H112 H -0.06965 0.11442 -0.02708 0.036 Uiso 1 1 d D . . O12W O -0.10718(9) 0.73367(17) -0.17587(7) 0.0202(4) Uani 1 1 d D . . H121 H -0.10505 0.72696 -0.20748 0.030 Uiso 1 1 d D . . H122 H -0.11152 0.80665 -0.17073 0.030 Uiso 1 1 d D . . O13W O -0.08317(10) 0.38416(18) -0.23109(8) 0.0273(4) Uani 1 1 d D . . H131 H -0.08732 0.31024 -0.22851 0.041 Uiso 1 1 d D . . H132 H -0.10787 0.41506 -0.21406 0.041 Uiso 1 1 d D . . O14W O 0.16264(11) 0.5011(2) 0.16873(9) 0.0325(5) Uani 1 1 d D . . H141 H 0.20160 0.49978 0.18761 0.049 Uiso 1 1 d D . . H142 H 0.15006 0.43000 0.16501 0.049 Uiso 1 1 d D . . O15W O 0.12294(10) 0.64161(18) 0.07474(8) 0.0272(4) Uani 1 1 d D . . H151 H 0.14724 0.61040 0.10212 0.041 Uiso 1 1 d D . . H152 H 0.13298 0.71406 0.07576 0.041 Uiso 1 1 d D . . O1 O 0.36772(9) 0.47933(16) 0.23026(7) 0.0176(4) Uani 1 1 d . . . H1 H 0.3682 0.5531 0.2286 0.026 Uiso 1 1 calc R . . C11 C 0.31827(12) 0.4446(2) 0.25035(9) 0.0145(5) Uani 1 1 d . . . C12 C 0.29519(11) 0.3283(2) 0.24078(9) 0.0128(5) Uani 1 1 d . . . C13 C 0.24525(12) 0.2912(2) 0.26197(9) 0.0146(5) Uani 1 1 d . . . H13 H 0.2302 0.2124 0.2568 0.017 Uiso 1 1 calc R . . C14 C 0.21706(12) 0.3680(2) 0.29062(9) 0.0143(5) Uani 1 1 d . . . C15 C 0.23923(12) 0.4818(2) 0.29971(9) 0.0151(5) Uani 1 1 d . . . H15 H 0.2191 0.5338 0.3190 0.018 Uiso 1 1 calc R . . C16 C 0.29107(12) 0.5211(2) 0.28078(9) 0.0140(5) Uani 1 1 d . . . S1 S 0.15754(3) 0.31379(5) 0.32032(2) 0.01628(12) Uani 1 1 d . . . O11 O 0.13952(10) 0.41023(17) 0.34951(7) 0.0236(4) Uani 1 1 d . . . O12 O 0.10292(9) 0.27133(17) 0.27870(7) 0.0214(4) Uani 1 1 d . . . O13 O 0.19064(10) 0.21840(17) 0.35350(7) 0.0243(4) Uani 1 1 d . . . C1 C 0.32253(12) 0.2463(2) 0.20665(9) 0.0152(5) Uani 1 1 d . . . H1A H 0.3115 0.1642 0.2134 0.018 Uiso 1 1 calc R . . H1B H 0.3705 0.2532 0.2162 0.018 Uiso 1 1 calc R . . O2 O 0.39401(8) 0.37551(17) 0.14584(7) 0.0189(4) Uani 1 1 d . . . H2 H 0.3948 0.4083 0.1745 0.028 Uiso 1 1 calc R . . C21 C 0.33150(12) 0.3430(2) 0.12160(10) 0.0145(5) Uani 1 1 d . . . C22 C 0.30438(12) 0.3779(2) 0.06975(9) 0.0140(5) Uani 1 1 d . . . C23 C 0.24289(12) 0.3376(2) 0.04437(9) 0.0146(5) Uani 1 1 d . . . H23 H 0.2239 0.3604 0.0091 0.018 Uiso 1 1 calc R . . C24 C 0.20875(12) 0.2642(2) 0.06983(9) 0.0140(5) Uani 1 1 d . . . C25 C 0.23498(12) 0.2328(2) 0.12185(9) 0.0144(5) Uani 1 1 d . . . H25 H 0.2109 0.1838 0.1392 0.017 Uiso 1 1 calc R . . C26 C 0.29641(12) 0.2728(2) 0.14878(9) 0.0143(5) Uani 1 1 d . . . S2 S 0.12991(3) 0.21664(5) 0.03580(2) 0.01306(11) Uani 1 1 d . . . O21 O 0.11092(9) 0.12708(15) 0.06817(7) 0.0179(4) Uani 1 1 d . . . O22 O 0.08791(8) 0.32034(15) 0.03009(7) 0.0176(4) Uani 1 1 d . . . O23 O 0.13433(9) 0.17397(16) -0.01525(7) 0.0182(4) Uani 1 1 d . . . C2 C 0.33940(12) 0.4614(2) 0.04121(9) 0.0142(5) Uani 1 1 d . . . H2A H 0.3860 0.4660 0.0603 0.017 Uiso 1 1 calc R . . H2B H 0.3366 0.4309 0.0055 0.017 Uiso 1 1 calc R . . O3 O 0.37788(9) 0.62761(17) 0.12019(7) 0.0194(4) Uani 1 1 d . . . H3 H 0.3735 0.6587 0.1480 0.029 Uiso 1 1 calc R . . C31 C 0.32853(12) 0.6613(2) 0.07974(9) 0.0144(5) Uani 1 1 d . . . C32 C 0.29829(12) 0.7711(2) 0.07914(9) 0.0132(5) Uani 1 1 d . . . C33 C 0.25078(12) 0.8031(2) 0.03451(10) 0.0149(5) Uani 1 1 d . . . H33 H 0.2292 0.8765 0.0336 0.018 Uiso 1 1 calc R . . C34 C 0.23447(11) 0.7292(2) -0.00864(9) 0.0137(5) Uani 1 1 d . . . C35 C 0.26275(12) 0.6185(2) -0.00684(9) 0.0146(5) Uani 1 1 d . . . H35 H 0.2500 0.5672 -0.0361 0.018 Uiso 1 1 calc R . . C36 C 0.30946(12) 0.5828(2) 0.03741(9) 0.0143(5) Uani 1 1 d . . . S3 S 0.18102(3) 0.77973(5) -0.06665(2) 0.01321(11) Uani 1 1 d . . . O31 O 0.16787(8) 0.90124(15) -0.05810(7) 0.0179(4) Uani 1 1 d . . . O32 O 0.21298(8) 0.76004(16) -0.10869(7) 0.0178(4) Uani 1 1 d . . . O33 O 0.12156(8) 0.70759(15) -0.07457(7) 0.0152(3) Uani 1 1 d . . . C3 C 0.31849(12) 0.8556(2) 0.12472(9) 0.0152(5) Uani 1 1 d . . . H3A H 0.3072 0.9365 0.1117 0.018 Uiso 1 1 calc R . . H3B H 0.3663 0.8518 0.1386 0.018 Uiso 1 1 calc R . . O4 O 0.37003(8) 0.69356(16) 0.20889(7) 0.0167(4) Uani 1 1 d . . . C41 C 0.31545(12) 0.7503(2) 0.20903(9) 0.0144(5) Uani 1 1 d . . . C42 C 0.28564(12) 0.7314(2) 0.25048(9) 0.0141(5) Uani 1 1 d . . . C43 C 0.22950(12) 0.7905(2) 0.25143(9) 0.0151(5) Uani 1 1 d . . . H43 H 0.2098 0.7772 0.2794 0.018 Uiso 1 1 calc R . . C44 C 0.20142(12) 0.8695(2) 0.21189(9) 0.0148(5) Uani 1 1 d . . . C45 C 0.23060(12) 0.8901(2) 0.17133(9) 0.0149(5) Uani 1 1 d . . . H45 H 0.2115 0.9448 0.1446 0.018 Uiso 1 1 calc R . . C46 C 0.28730(12) 0.8319(2) 0.16924(9) 0.0151(5) Uani 1 1 d . . . S4 S 0.13470(3) 0.95246(5) 0.21887(2) 0.01445(12) Uani 1 1 d . . . O41 O 0.10960(9) 1.01820(16) 0.17049(7) 0.0210(4) Uani 1 1 d . . . O42 O 0.08628(9) 0.86792(16) 0.22788(7) 0.0192(4) Uani 1 1 d . . . O43 O 0.15964(9) 1.02833(15) 0.26395(7) 0.0190(4) Uani 1 1 d . . . C4 C 0.31581(12) 0.6450(2) 0.29339(9) 0.0148(5) Uani 1 1 d . . . H4A H 0.3062 0.6704 0.3265 0.018 Uiso 1 1 calc R . . H4B H 0.3636 0.6458 0.2989 0.018 Uiso 1 1 calc R . . P1 P 0.54734(3) 0.78953(6) 0.08191(3) 0.01703(13) Uani 1 1 d . . . C11A C 0.52693(13) 0.9024(3) 0.12254(10) 0.0218(6) Uani 1 1 d . . . C12A C 0.52896(15) 1.0202(3) 0.10765(12) 0.0301(7) Uani 1 1 d . . . H12A H 0.5447 1.0402 0.0782 0.036 Uiso 1 1 calc R . . C13A C 0.50802(16) 1.1074(3) 0.13590(14) 0.0408(8) Uani 1 1 d . . . H13A H 0.5095 1.1874 0.1260 0.049 Uiso 1 1 calc R . . C14A C 0.48487(16) 1.0776(3) 0.17865(14) 0.0438(9) Uani 1 1 d . . . H14A H 0.4701 1.1376 0.1978 0.053 Uiso 1 1 calc R . . C15A C 0.48305(16) 0.9626(4) 0.19366(13) 0.0412(9) Uani 1 1 d . . . H15A H 0.4673 0.9435 0.2232 0.049 Uiso 1 1 calc R . . C16A C 0.50411(14) 0.8736(3) 0.16583(11) 0.0305(7) Uani 1 1 d . . . H16A H 0.5029 0.7939 0.1763 0.037 Uiso 1 1 calc R . . C21A C 0.57520(12) 0.6596(2) 0.12000(10) 0.0187(5) Uani 1 1 d . . . C22A C 0.52890(13) 0.5882(3) 0.13350(11) 0.0233(6) Uani 1 1 d . . . H22A H 0.4840 0.6063 0.1211 0.028 Uiso 1 1 calc R . . C23A C 0.54850(15) 0.4910(3) 0.16504(12) 0.0280(6) Uani 1 1 d . . . H23A H 0.5170 0.4414 0.1739 0.034 Uiso 1 1 calc R . . C24A C 0.61420(15) 0.4662(3) 0.18370(11) 0.0296(6) Uani 1 1 d . . . H24A H 0.6277 0.4005 0.2061 0.036 Uiso 1 1 calc R . . C25A C 0.66017(14) 0.5364(3) 0.16984(11) 0.0276(6) Uani 1 1 d . . . H25A H 0.7051 0.5180 0.1824 0.033 Uiso 1 1 calc R . . C26A C 0.64128(13) 0.6333(3) 0.13783(11) 0.0235(6) Uani 1 1 d . . . H26A H 0.6729 0.6813 0.1281 0.028 Uiso 1 1 calc R . . C31A C 0.60833(13) 0.8428(2) 0.05216(11) 0.0199(5) Uani 1 1 d . . . C32A C 0.66587(14) 0.8872(2) 0.08455(11) 0.0240(6) Uani 1 1 d . . . H32A H 0.6707 0.8942 0.1213 0.029 Uiso 1 1 calc R . . C33A C 0.71616(14) 0.9210(3) 0.06290(12) 0.0270(6) Uani 1 1 d . . . H33A H 0.7558 0.9501 0.0849 0.032 Uiso 1 1 calc R . . C34A C 0.70847(14) 0.9125(2) 0.00969(12) 0.0267(6) Uani 1 1 d . . . H34A H 0.7431 0.9346 -0.0050 0.032 Uiso 1 1 calc R . . C35A C 0.65072(15) 0.8719(2) -0.02267(12) 0.0252(6) Uani 1 1 d . . . H35A H 0.6455 0.8685 -0.0595 0.030 Uiso 1 1 calc R . . C36A C 0.60048(14) 0.8362(2) -0.00168(11) 0.0218(6) Uani 1 1 d . . . H36A H 0.5610 0.8074 -0.0239 0.026 Uiso 1 1 calc R . . C41A C 0.47700(12) 0.7548(2) 0.03035(10) 0.0174(5) Uani 1 1 d . . . C42A C 0.42506(12) 0.8321(2) 0.01628(10) 0.0193(5) Uani 1 1 d . . . H42A H 0.4236 0.8997 0.0371 0.023 Uiso 1 1 calc R . . C43A C 0.37507(12) 0.8104(2) -0.02837(10) 0.0207(5) Uani 1 1 d . . . H43A H 0.3397 0.8638 -0.0383 0.025 Uiso 1 1 calc R . . C44A C 0.37670(13) 0.7111(2) -0.05834(11) 0.0228(6) Uani 1 1 d . . . H44A H 0.3424 0.6961 -0.0887 0.027 Uiso 1 1 calc R . . C45A C 0.42845(14) 0.6334(3) -0.04405(11) 0.0239(6) Uani 1 1 d . . . H45A H 0.4296 0.5654 -0.0647 0.029 Uiso 1 1 calc R . . C46A C 0.47860(13) 0.6548(2) 0.00029(11) 0.0222(6) Uani 1 1 d . . . H46A H 0.5140 0.6013 0.0101 0.027 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 Yb1 0.01315(5) 0.01137(5) 0.01113(5) -0.00032(4) 0.00411(3) 0.00014(4) Na1 0.0167(5) 0.0157(5) 0.0189(5) 0.0030(4) 0.0050(4) 0.0012(4) O1W 0.0390(11) 0.0116(9) 0.0132(8) 0.0003(7) 0.0070(8) -0.0025(8) O2W 0.0165(9) 0.0251(10) 0.0154(9) 0.0028(8) 0.0066(7) 0.0067(8) O3W 0.0272(10) 0.0147(9) 0.0128(8) 0.0011(7) 0.0071(7) 0.0047(8) O4W 0.0195(9) 0.0164(9) 0.0181(9) -0.0037(7) 0.0086(7) -0.0030(7) O5W 0.0252(10) 0.0167(9) 0.0159(9) 0.0044(7) 0.0103(7) 0.0064(8) O6W 0.0241(10) 0.0164(9) 0.0340(11) -0.0067(8) 0.0186(9) -0.0072(8) O7W 0.0158(9) 0.0188(9) 0.0198(9) -0.0055(7) 0.0045(7) 0.0013(7) O8W 0.0215(10) 0.0214(10) 0.0195(9) -0.0012(8) 0.0019(8) 0.0010(8) O9W 0.0175(9) 0.0192(9) 0.0254(10) -0.0018(8) 0.0080(8) -0.0012(8) O10W 0.0231(10) 0.0227(10) 0.0265(10) 0.0021(8) 0.0062(8) 0.0013(8) O11W 0.0323(11) 0.0171(9) 0.0217(10) -0.0020(8) 0.0051(8) -0.0019(8) O12W 0.0221(10) 0.0225(10) 0.0154(9) -0.0002(7) 0.0036(7) 0.0033(8) O13W 0.0246(11) 0.0226(10) 0.0338(12) -0.0028(9) 0.0057(9) -0.0021(9) O14W 0.0309(12) 0.0302(11) 0.0312(12) 0.0024(10) -0.0012(9) 0.0010(9) O15W 0.0324(12) 0.0237(10) 0.0242(10) -0.0023(8) 0.0049(9) -0.0007(9) O1 0.0161(9) 0.0173(9) 0.0202(9) 0.0012(7) 0.0064(7) -0.0008(7) C11 0.0131(11) 0.0176(12) 0.0108(11) 0.0044(9) -0.0003(9) 0.0003(9) C12 0.0132(11) 0.0146(12) 0.0089(10) 0.0013(9) -0.0003(9) 0.0023(9) C13 0.0188(12) 0.0133(11) 0.0095(11) 0.0011(9) -0.0002(9) -0.0022(10) C14 0.0166(12) 0.0157(12) 0.0107(11) 0.0016(9) 0.0037(9) -0.0016(10) C15 0.0181(12) 0.0174(12) 0.0093(11) 0.0010(9) 0.0025(9) 0.0016(10) C16 0.0166(12) 0.0135(12) 0.0100(11) 0.0014(9) -0.0003(9) -0.0011(9) S1 0.0210(3) 0.0150(3) 0.0152(3) -0.0017(2) 0.0091(2) -0.0036(2) O11 0.0302(11) 0.0200(10) 0.0263(10) -0.0084(8) 0.0177(8) -0.0065(8) O12 0.0202(10) 0.0233(10) 0.0219(9) -0.0032(8) 0.0074(8) -0.0065(8) O13 0.0302(11) 0.0244(10) 0.0204(10) 0.0070(8) 0.0102(8) -0.0016(8) C1 0.0163(12) 0.0160(12) 0.0129(11) 0.0026(9) 0.0031(9) 0.0022(10) O2 0.0128(9) 0.0249(10) 0.0179(9) 0.0008(8) 0.0021(7) 0.0004(7) C21 0.0131(11) 0.0136(11) 0.0173(12) 0.0001(9) 0.0050(9) 0.0023(9) C22 0.0151(12) 0.0119(11) 0.0160(12) 0.0001(9) 0.0060(9) 0.0024(9) C23 0.0181(12) 0.0132(12) 0.0135(11) 0.0002(9) 0.0059(9) 0.0002(9) C24 0.0144(12) 0.0132(11) 0.0146(11) -0.0008(9) 0.0043(9) 0.0013(9) C25 0.0165(12) 0.0128(11) 0.0153(12) -0.0008(9) 0.0066(9) 0.0010(9) C26 0.0183(12) 0.0120(11) 0.0130(11) -0.0007(9) 0.0051(9) 0.0029(9) S2 0.0141(3) 0.0133(3) 0.0123(3) 0.0005(2) 0.0042(2) -0.0011(2) O21 0.0203(9) 0.0149(9) 0.0182(9) 0.0037(7) 0.0043(7) -0.0038(7) O22 0.0172(9) 0.0164(9) 0.0207(9) 0.0044(7) 0.0075(7) 0.0034(7) O23 0.0195(9) 0.0219(9) 0.0133(8) -0.0047(7) 0.0045(7) -0.0013(7) C2 0.0137(11) 0.0149(11) 0.0150(11) 0.0010(9) 0.0056(9) 0.0005(10) O3 0.0178(9) 0.0247(10) 0.0143(9) -0.0004(7) 0.0017(7) 0.0051(8) C31 0.0116(11) 0.0183(12) 0.0143(11) 0.0027(9) 0.0051(9) -0.0010(9) C32 0.0157(12) 0.0137(11) 0.0113(11) 0.0002(9) 0.0054(9) -0.0032(9) C33 0.0132(11) 0.0136(12) 0.0190(12) 0.0007(9) 0.0063(9) -0.0007(9) C34 0.0112(11) 0.0153(12) 0.0138(11) 0.0026(9) 0.0016(9) -0.0003(9) C35 0.0152(12) 0.0152(12) 0.0141(11) -0.0002(9) 0.0050(9) -0.0013(9) C36 0.0139(12) 0.0141(11) 0.0168(12) 0.0017(9) 0.0078(9) -0.0001(9) S3 0.0127(3) 0.0125(3) 0.0137(3) 0.0011(2) 0.0020(2) -0.0010(2) O31 0.0169(9) 0.0132(9) 0.0209(9) 0.0006(7) -0.0003(7) -0.0004(7) O32 0.0172(9) 0.0218(9) 0.0150(8) 0.0018(7) 0.0056(7) -0.0016(7) O33 0.0137(8) 0.0152(9) 0.0166(8) -0.0017(7) 0.0038(7) -0.0020(7) C3 0.0163(12) 0.0152(12) 0.0137(11) 0.0001(9) 0.0029(9) -0.0014(10) O4 0.0131(8) 0.0199(9) 0.0167(9) 0.0016(7) 0.0032(7) -0.0004(7) C41 0.0139(12) 0.0133(11) 0.0142(11) -0.0030(9) 0.0005(9) -0.0040(9) C42 0.0176(12) 0.0107(11) 0.0128(11) -0.0015(9) 0.0018(9) -0.0033(9) C43 0.0185(12) 0.0133(11) 0.0141(11) -0.0017(9) 0.0053(9) -0.0046(10) C44 0.0164(12) 0.0137(12) 0.0145(11) -0.0008(9) 0.0045(9) -0.0007(9) C45 0.0198(12) 0.0129(11) 0.0103(11) -0.0001(9) 0.0010(9) -0.0019(10) C46 0.0172(12) 0.0147(12) 0.0131(11) -0.0031(9) 0.0033(9) -0.0054(10) S4 0.0187(3) 0.0131(3) 0.0121(3) 0.0003(2) 0.0049(2) 0.0010(2) O41 0.0273(10) 0.0208(10) 0.0149(9) 0.0041(7) 0.0055(7) 0.0070(8) O42 0.0204(9) 0.0185(9) 0.0203(9) 0.0001(7) 0.0081(7) -0.0006(7) O43 0.0292(10) 0.0148(9) 0.0144(8) -0.0029(7) 0.0080(7) -0.0010(8) C4 0.0166(12) 0.0150(12) 0.0111(11) -0.0002(9) 0.0007(9) -0.0019(10) P1 0.0137(3) 0.0193(3) 0.0171(3) -0.0014(3) 0.0022(2) 0.0008(3) C11A 0.0151(12) 0.0272(15) 0.0206(13) -0.0079(11) -0.0001(10) 0.0031(11) C12A 0.0287(16) 0.0278(16) 0.0320(16) -0.0079(13) 0.0049(12) 0.0018(13) C13A 0.0343(18) 0.0332(18) 0.048(2) -0.0174(16) -0.0018(15) 0.0062(15) C14A 0.0271(17) 0.054(2) 0.047(2) -0.0326(18) 0.0016(15) 0.0071(16) C15A 0.0289(17) 0.066(3) 0.0295(16) -0.0200(17) 0.0089(13) 0.0002(17) C16A 0.0236(15) 0.0435(19) 0.0240(15) -0.0084(13) 0.0057(12) -0.0003(13) C21A 0.0168(12) 0.0207(13) 0.0174(12) -0.0006(10) 0.0024(10) 0.0034(10) C22A 0.0173(13) 0.0317(15) 0.0210(13) 0.0026(12) 0.0049(10) 0.0043(12) C23A 0.0264(15) 0.0315(16) 0.0278(15) 0.0070(12) 0.0099(12) 0.0011(12) C24A 0.0332(16) 0.0301(16) 0.0228(14) 0.0074(12) 0.0023(12) 0.0079(13) C25A 0.0191(13) 0.0300(15) 0.0289(15) 0.0000(13) -0.0026(11) 0.0069(12) C26A 0.0149(13) 0.0282(15) 0.0255(14) -0.0021(12) 0.0019(11) -0.0006(11) C31A 0.0176(13) 0.0178(13) 0.0238(13) -0.0008(10) 0.0046(10) 0.0008(10) C32A 0.0234(14) 0.0226(14) 0.0226(14) 0.0012(11) 0.0000(11) -0.0037(11) C33A 0.0177(14) 0.0217(14) 0.0395(17) 0.0042(12) 0.0035(12) -0.0019(11) C34A 0.0239(15) 0.0173(13) 0.0428(17) 0.0025(12) 0.0157(13) 0.0047(11) C35A 0.0332(16) 0.0174(13) 0.0290(15) -0.0024(11) 0.0150(12) 0.0010(12) C36A 0.0224(14) 0.0185(13) 0.0242(14) -0.0017(11) 0.0057(11) 0.0010(11) C41A 0.0142(12) 0.0195(13) 0.0173(12) 0.0009(10) 0.0017(9) -0.0015(10) C42A 0.0176(13) 0.0183(13) 0.0224(13) 0.0006(10) 0.0059(10) 0.0015(10) C43A 0.0135(12) 0.0237(14) 0.0238(13) 0.0083(11) 0.0027(10) 0.0025(10) C44A 0.0190(13) 0.0273(15) 0.0195(13) 0.0054(11) 0.0001(10) -0.0024(11) C45A 0.0249(14) 0.0223(14) 0.0221(14) -0.0026(11) 0.0015(11) -0.0009(11) C46A 0.0180(13) 0.0204(13) 0.0252(14) -0.0013(11) 0.0001(11) 0.0038(11) _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 Yb1 O2W 2.281(2) . ? Yb1 O33 2.299(2) . ? Yb1 O5W 2.300(2) . ? Yb1 O6W 2.302(2) . ? Yb1 O1W 2.310(2) . ? Yb1 O4W 2.325(2) . ? Yb1 O3W 2.330(2) . ? Yb1 O7W 2.334(18) . ? Na1 O31 2.284(2) 1_545 ? Na1 O11 2.313(2) 4_565 ? Na1 O8W 2.377(2) . ? Na1 O9W 2.427(2) . ? Na1 O23 2.465(2) . ? Na1 O10W 2.643(2) . ? O1W H1WA 0.85 . ? O1W H1WB 0.85 . ? O2W H2WA 0.85 . ? O2W H2WB 0.85 . ? O3W H3WA 0.85 . ? O3W H3WB 0.85 . ? O4W H4WA 0.85 . ? O4W H4WB 0.85 . ? O5W H5WA 0.85 . ? O5W H5WB 0.85 . ? O6W H6WA 0.85 . ? O6W H6WB 0.85 . ? O7W H7WA 0.85 . ? O7W H7WB 0.85 . ? O8W H8WA 0.85 . ? O8W H8WB 0.85 . ? O9W H9WA 0.85 . ? O9W H9WB 0.85 . ? O10W H101 0.85 . ? O10W H102 0.85 . ? O11W H111 0.85 . ? O11W H112 0.85 . ? O12W H121 0.85 . ? O12W H122 0.85 . ? O13W H131 0.85 . ? O13W H132 0.85 . ? O14W H141 0.85 . ? O14W H142 0.85 . ? O15W H151 0.85 . ? O15W H152 0.85 . ? O1 C11 1.353(3) . ? O1 H1 0.84 . ? C11 C16 1.405(3) . ? C11 C12 1.411(3) . ? C12 C13 1.387(3) . ? C12 C1 1.513(3) . ? C13 C14 1.388(3) . ? C13 H13 0.95 . ? C14 C15 1.378(3) . ? C14 S1 1.762(2) . ? C15 C16 1.396(3) . ? C15 H15 0.95 . ? C16 C4 1.512(3) . ? S1 O11 1.447(2) . ? S1 O13 1.456(2) . ? S1 O12 1.460(2) . ? O11 Na1 2.313(2) 4_566 ? C1 C26 1.514(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? O2 C21 1.370(3) . ? O2 H2 0.84 . ? C21 C22 1.398(3) . ? C21 C26 1.408(3) . ? C22 C23 1.385(3) . ? C22 C2 1.520(3) . ? C23 C24 1.388(3) . ? C23 H23 0.95 . ? C24 C25 1.388(3) . ? C24 S2 1.771(3) . ? C25 C26 1.393(3) . ? C25 H25 0.95 . ? S2 O21 1.452(2) . ? S2 O23 1.457(2) . ? S2 O22 1.464(2) . ? C2 C36 1.513(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O3 C31 1.345(3) . ? O3 H3 0.84 . ? C31 C32 1.404(3) . ? C31 C36 1.405(3) . ? C32 C33 1.388(3) . ? C32 C3 1.512(3) . ? C33 C34 1.385(3) . ? C33 H33 0.95 . ? C34 C35 1.391(3) . ? C34 S3 1.752(2) . ? C35 C36 1.385(3) . ? C35 H35 0.95 . ? S3 O31 1.439(2) . ? S3 O32 1.459(2) . ? S3 O33 1.477(2) . ? O31 Na1 2.284(2) 1_565 ? C3 C46 1.514(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C41 1.329(3) . ? C41 C46 1.413(3) . ? C41 C42 1.414(3) . ? C42 C43 1.377(3) . ? C42 C4 1.511(3) . ? C43 C44 1.389(3) . ? C43 H43 0.95 . ? C44 C45 1.388(3) . ? C44 S4 1.753(3) . ? C45 C46 1.389(4) . ? C45 H45 0.95 . ? S4 O43 1.454(2) . ? S4 O41 1.457(2) . ? S4 O42 1.473(2) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? P1 C31A 1.786(3) . ? P1 C41A 1.788(3) . ? P1 C11A 1.796(3) . ? P1 C21A 1.800(3) . ? C11A C16A 1.390(4) . ? C11A C12A 1.400(4) . ? C12A C13A 1.381(4) . ? C12A H12A 0.95 . ? C13A C14A 1.384(5) . ? C13A H13A 0.95 . ? C14A C15A 1.370(6) . ? C14A H14A 0.95 . ? C15A C16A 1.390(4) . ? C15A H15A 0.95 . ? C16A H16A 0.95 . ? C21A C22A 1.391(4) . ? C21A C26A 1.395(4) . ? C22A C23A 1.382(4) . ? C22A H22A 0.95 . ? C23A C24A 1.386(4) . ? C23A H23A 0.95 . ? C24A C25A 1.383(4) . ? C24A H24A 0.95 . ? C25A C26A 1.384(4) . ? C25A H25A 0.95 . ? C26A H26A 0.95 . ? C31A C36A 1.389(4) . ? C31A C32A 1.394(4) . ? C32A C33A 1.390(4) . ? C32A H32A 0.95 . ? C33A C34A 1.374(4) . ? C33A H33A 0.95 . ? C34A C35A 1.382(4) . ? C34A H34A 0.95 . ? C35A C36A 1.385(4) . ? C35A H35A 0.95 . ? C36A H36A 0.95 . ? C41A C42A 1.386(4) . ? C41A C46A 1.392(4) . ? C42A C43A 1.391(4) . ? C42A H42A 0.95 . ? C43A C44A 1.384(4) . ? C43A H43A 0.95 . ? C44A C45A 1.386(4) . ? C44A H44A 0.95 . ? C45A C46A 1.386(4) . ? C45A H45A 0.95 . ? C46A H46A 0.95 . ? 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 O2W Yb1 O33 77.94(6) . . ? O2W Yb1 O5W 144.60(6) . . ? O33 Yb1 O5W 112.19(7) . . ? O2W Yb1 O6W 76.58(7) . . ? O33 Yb1 O6W 142.92(6) . . ? O5W Yb1 O6W 76.49(7) . . ? O2W Yb1 O1W 76.62(7) . . ? O33 Yb1 O1W 73.04(6) . . ? O5W Yb1 O1W 74.59(6) . . ? O6W Yb1 O1W 75.17(7) . . ? O2W Yb1 O4W 142.66(7) . . ? O33 Yb1 O4W 75.34(6) . . ? O5W Yb1 O4W 70.99(6) . . ? O6W Yb1 O4W 138.25(6) . . ? O1W Yb1 O4W 118.75(7) . . ? O2W Yb1 O3W 70.62(6) . . ? O33 Yb1 O3W 79.00(6) . . ? O5W Yb1 O3W 143.23(6) . . ? O6W Yb1 O3W 116.47(7) . . ? O1W Yb1 O3W 140.52(6) . . ? O4W Yb1 O3W 79.00(6) . . ? O2W Yb1 O7W 112.08(6) . . ? O33 Yb1 O7W 142.11(6) . . ? O5W Yb1 O7W 81.35(7) . . ? O6W Yb1 O7W 73.36(7) . . ? O1W Yb1 O7W 143.96(6) . . ? O4W Yb1 O7W 76.46(6) . . ? O3W Yb1 O7W 71.17(7) . . ? O31 Na1 O11 87.70(7) 1_545 4_565 ? O31 Na1 O8W 175.68(8) 1_545 . ? O11 Na1 O8W 94.29(8) 4_565 . ? O31 Na1 O9W 79.76(7) 1_545 . ? O11 Na1 O9W 150.57(8) 4_565 . ? O8W Na1 O9W 96.72(7) . . ? O31 Na1 O23 92.70(7) 1_545 . ? O11 Na1 O23 102.27(8) 4_565 . ? O8W Na1 O23 90.62(7) . . ? O9W Na1 O23 104.80(7) . . ? O31 Na1 O10W 91.49(7) 1_545 . ? O11 Na1 O10W 75.30(7) 4_565 . ? O8W Na1 O10W 85.32(7) . . ? O9W Na1 O10W 78.51(7) . . ? O23 Na1 O10W 175.07(7) . . ? Yb1 O1W H1WA 116.9 . . ? Yb1 O1W H1WB 131.4 . . ? H1WA O1W H1WB 106.3 . . ? Yb1 O2W H2WA 122.8 . . ? Yb1 O2W H2WB 127.2 . . ? H2WA O2W H2WB 106.3 . . ? Yb1 O3W H3WA 120.6 . . ? Yb1 O3W H3WB 123.7 . . ? H3WA O3W H3WB 106.5 . . ? Yb1 O4W H4WA 121.0 . . ? Yb1 O4W H4WB 118.1 . . ? H4WA O4W H4WB 106.4 . . ? Yb1 O5W H5WA 131.4 . . ? Yb1 O5W H5WB 116.2 . . ? H5WA O5W H5WB 106.3 . . ? Yb1 O6W H6WA 123.3 . . ? Yb1 O6W H6WB 130.4 . . ? H6WA O6W H6WB 106.1 . . ? Yb1 O7W H7WA 117.5 . . ? Yb1 O7W H7WB 133.1 . . ? H7WA O7W H7WB 106.4 . . ? Na1 O8W H8WA 115.7 . . ? Na1 O8W H8WB 102.3 . . ? H8WA O8W H8WB 106.3 . . ? Na1 O9W H9WA 123.2 . . ? Na1 O9W H9WB 100.7 . . ? H9WA O9W H9WB 106.0 . . ? Na1 O10W H101 103.9 . . ? Na1 O10W H102 98.9 . . ? H101 O10W H102 106.1 . . ? H111 O11W H112 106.3 . . ? H121 O12W H122 106.2 . . ? H131 O13W H132 106.0 . . ? H141 O14W H142 106.3 . . ? H151 O15W H152 106.6 . . ? C11 O1 H1 109.5 . . ? O1 C11 C16 121.3(2) . . ? O1 C11 C12 118.2(2) . . ? C16 C11 C12 120.5(2) . . ? C13 C12 C11 118.7(2) . . ? C13 C12 C1 120.2(2) . . ? C11 C12 C1 121.0(2) . . ? C14 C13 C12 120.7(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 120.6(2) . . ? C15 C14 S1 120.3(2) . . ? C13 C14 S1 118.9(2) . . ? C14 C15 C16 120.3(2) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C15 C16 C11 119.1(2) . . ? C15 C16 C4 118.8(2) . . ? C11 C16 C4 122.1(2) . . ? O11 S1 O13 113.5(1) . . ? O11 S1 O12 112.5(1) . . ? O13 S1 O12 111.9(1) . . ? O11 S1 C14 106.9(1) . . ? O13 S1 C14 103.7(1) . . ? O12 S1 C14 107.8(1) . . ? S1 O11 Na1 145.6(1) . 4_566 ? C12 C1 C26 112.3(2) . . ? C12 C1 H1A 109.2 . . ? C26 C1 H1A 109.2 . . ? C12 C1 H1B 109.2 . . ? C26 C1 H1B 109.2 . . ? H1A C1 H1B 107.9 . . ? C21 O2 H2 109.5 . . ? O2 C21 C22 119.1(2) . . ? O2 C21 C26 119.6(2) . . ? C22 C21 C26 121.3(2) . . ? C23 C22 C21 118.6(2) . . ? C23 C22 C2 119.3(2) . . ? C21 C22 C2 122.0(2) . . ? C22 C23 C24 120.8(2) . . ? C22 C23 H23 119.6 . . ? C24 C23 H23 119.6 . . ? C23 C24 C25 120.4(2) . . ? C23 C24 S2 118.9(2) . . ? C25 C24 S2 120.6(2) . . ? C24 C25 C26 120.4(2) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C25 C26 C21 118.4(2) . . ? C25 C26 C1 120.1(2) . . ? C21 C26 C1 121.4(2) . . ? O21 S2 O23 113.8(1) . . ? O21 S2 O22 111.8(1) . . ? O23 S2 O22 110.9(1) . . ? O21 S2 C24 106.7(1) . . ? O23 S2 C24 107.0(1) . . ? O22 S2 C24 106.2(1) . . ? S2 O23 Na1 144.4(1) . . ? C36 C2 C22 110.6(2) . . ? C36 C2 H2A 109.5 . . ? C22 C2 H2A 109.5 . . ? C36 C2 H2B 109.5 . . ? C22 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C31 O3 H3 109.5 . . ? O3 C31 C32 121.6(2) . . ? O3 C31 C36 117.1(2) . . ? C32 C31 C36 121.3(2) . . ? C33 C32 C31 118.3(2) . . ? C33 C32 C3 120.3(2) . . ? C31 C32 C3 121.4(2) . . ? C34 C33 C32 120.8(2) . . ? C34 C33 H33 119.6 . . ? C32 C33 H33 119.6 . . ? C33 C34 C35 120.4(2) . . ? C33 C34 S3 119.2(2) . . ? C35 C34 S3 120.3(2) . . ? C36 C35 C34 120.3(2) . . ? C36 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? C35 C36 C31 118.7(2) . . ? C35 C36 C2 121.5(2) . . ? C31 C36 C2 119.8(2) . . ? O31 S3 O32 114.4(1) . . ? O31 S3 O33 111.2(1) . . ? O32 S3 O33 110.9(1) . . ? O31 S3 C34 106.7(1) . . ? O32 S3 C34 106.8(1) . . ? O33 S3 C34 106.3(1) . . ? S3 O31 Na1 138.8(1) . 1_565 ? S3 O33 Yb1 145.3(10) . . ? C32 C3 C46 114.3(2) . . ? C32 C3 H3A 108.7 . . ? C46 C3 H3A 108.7 . . ? C32 C3 H3B 108.7 . . ? C46 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? O4 C41 C46 121.4(2) . . ? O4 C41 C42 119.6(2) . . ? C46 C41 C42 119.1(2) . . ? C43 C42 C41 120.2(2) . . ? C43 C42 C4 120.5(2) . . ? C41 C42 C4 119.3(2) . . ? C42 C43 C44 120.6(2) . . ? C42 C43 H43 119.7 . . ? C44 C43 H43 119.7 . . ? C45 C44 C43 119.8(2) . . ? C45 C44 S4 121.6(2) . . ? C43 C44 S4 118.2(2) . . ? C44 C45 C46 121.0(2) . . ? C44 C45 H45 119.5 . . ? C46 C45 H45 119.5 . . ? C45 C46 C41 119.3(2) . . ? C45 C46 C3 120.3(2) . . ? C41 C46 C3 120.4(2) . . ? O43 S4 O41 112.7(1) . . ? O43 S4 O42 112.3(1) . . ? O41 S4 O42 111.3(1) . . ? O43 S4 C44 105.7(1) . . ? O41 S4 C44 108.0(1) . . ? O42 S4 C44 106.5(1) . . ? C42 C4 C16 112.6(2) . . ? C42 C4 H4A 109.1 . . ? C16 C4 H4A 109.1 . . ? C42 C4 H4B 109.1 . . ? C16 C4 H4B 109.1 . . ? H4A C4 H4B 107.8 . . ? C31A P1 C41A 107.54(12) . . ? C31A P1 C11A 109.50(13) . . ? C41A P1 C11A 109.15(12) . . ? C31A P1 C21A 110.61(12) . . ? C41A P1 C21A 109.53(12) . . ? C11A P1 C21A 110.46(13) . . ? C16A C11A C12A 119.9(3) . . ? C16A C11A P1 120.7(2) . . ? C12A C11A P1 119.2(2) . . ? C13A C12A C11A 119.9(3) . . ? C13A C12A H12A 120.1 . . ? C11A C12A H12A 120.1 . . ? C12A C13A C14A 119.7(3) . . ? C12A C13A H13A 120.1 . . ? C14A C13A H13A 120.1 . . ? C15A C14A C13A 120.8(3) . . ? C15A C14A H14A 119.6 . . ? C13A C14A H14A 119.6 . . ? C14A C15A C16A 120.4(3) . . ? C14A C15A H15A 119.8 . . ? C16A C15A H15A 119.8 . . ? C11A C16A C15A 119.3(3) . . ? C11A C16A H16A 120.3 . . ? C15A C16A H16A 120.3 . . ? C22A C21A C26A 120.5(3) . . ? C22A C21A P1 118.0(2) . . ? C26A C21A P1 121.5(2) . . ? C23A C22A C21A 119.8(3) . . ? C23A C22A H22A 120.1 . . ? C21A C22A H22A 120.1 . . ? C22A C23A C24A 119.8(3) . . ? C22A C23A H23A 120.1 . . ? C24A C23A H23A 120.1 . . ? C25A C24A C23A 120.4(3) . . ? C25A C24A H24A 119.8 . . ? C23A C24A H24A 119.8 . . ? C24A C25A C26A 120.5(3) . . ? C24A C25A H25A 119.7 . . ? C26A C25A H25A 119.7 . . ? C25A C26A C21A 119.0(3) . . ? C25A C26A H26A 120.5 . . ? C21A C26A H26A 120.5 . . ? C36A C31A C32A 120.1(3) . . ? C36A C31A P1 121.4(2) . . ? C32A C31A P1 118.4(2) . . ? C33A C32A C31A 119.7(3) . . ? C33A C32A H32A 120.1 . . ? C31A C32A H32A 120.1 . . ? C34A C33A C32A 119.8(3) . . ? C34A C33A H33A 120.1 . . ? C32A C33A H33A 120.1 . . ? C33A C34A C35A 120.5(3) . . ? C33A C34A H34A 119.7 . . ? C35A C34A H34A 119.7 . . ? C34A C35A C36A 120.4(3) . . ? C34A C35A H35A 119.8 . . ? C36A C35A H35A 119.8 . . ? C35A C36A C31A 119.4(3) . . ? C35A C36A H36A 120.3 . . ? C31A C36A H36A 120.3 . . ? C42A C41A C46A 120.0(2) . . ? C42A C41A P1 121.2(2) . . ? C46A C41A P1 118.4(2) . . ? C41A C42A C43A 119.8(2) . . ? C41A C42A H42A 120.1 . . ? C43A C42A H42A 120.1 . . ? C44A C43A C42A 120.2(2) . . ? C44A C43A H43A 119.9 . . ? C42A C43A H43A 119.9 . . ? C43A C44A C45A 120.0(3) . . ? C43A C44A H44A 120.0 . . ? C45A C44A H44A 120.0 . . ? C44A C45A C46A 120.2(3) . . ? C44A C45A H45A 119.9 . . ? C46A C45A H45A 119.9 . . ? C45A C46A C41A 119.8(2) . . ? C45A C46A H46A 120.1 . . ? C41A C46A H46A 120.1 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O4 0.84 1.68 2.505(3) 164.8 . O2 H2 O1 0.84 1.89 2.703(3) 161.7 . O3 H3 O4 0.84 1.67 2.503(2) 168.1 . O1W H1WA O22 0.85 1.87 2.718(2) 176 . O1W H1WB O15W 0.85 1.93 2.737(3) 157 . O2W H2WA O12W 0.85 1.77 2.613(3) 174 . O2W H2WB O22 0.85 1.91 2.732(2) 163 3_565 O3W H3WA O42 0.85 2.02 2.859(2) 168 4_575 O3W H3WB O10W 0.85 1.93 2.781(3) 175 1_565 O4W H4WA O43 0.85 1.84 2.677(2) 169 4_575 O4W H4WB O32 0.85 1.90 2.700(3) 156 . O5W H5WA O23 0.85 1.98 2.818(3) 167 . O5W H5WB O13 0.85 1.78 2.615(2) 169 4_565 O6W H6WA O8W 0.85 1.86 2.707(3) 174 . O6W H6WB O15W 0.85 2.00 2.806(3) 157 3_565 O7W H7WA O13W 0.85 1.87 2.721(3) 176 . O7W H7WB O12 0.85 1.99 2.814(3) 162 4_565 O7W H7WB O43 0.85 2.64 3.100(3) 115 4_575 O8W H8WA O42 0.85 2.15 2.990(3) 172 3_565 O8W H8WB O11W 0.85 1.92 2.769(3) 173 . O9W H9WA O21 0.85 2.06 2.903(3) 175 3 O9W H9WB O33 0.85 2.32 3.068(3) 147 1_545 O9W H9WB O2W 0.85 2.45 3.136(3) 138 1_545 O10W H101 O41 0.85 2.34 3.151(3) 159 3_565 O10W H102 O13W 0.85 2.38 3.086(3) 141 2_544 O10W H102 O11 0.85 2.60 3.038(3) 113 4_565 O11W H111 O21 0.85 2.03 2.836(3) 158 3 O11W H112 O9W 0.85 1.96 2.807(3) 176 3 O12W H121 O12 0.85 1.89 2.737(3) 174 3_565 O12W H122 O41 0.85 1.99 2.827(3) 167 3_575 O13W H131 O42 0.85 2.03 2.870(3) 171 3_565 O13W H132 O14W 0.85 2.10 2.948(3) 176 3_565 O14W H142 O12W 0.85 2.13 2.945(3) 162 3_565 O15W H151 O14W 0.85 2.11 2.887(3) 152 . O15W H152 O11W 0.85 2.11 2.817(3) 141 3_565 _diffrn_measured_fraction_theta_max 0.93 _diffrn_reflns_theta_full 28.98 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.850 _refine_diff_density_min -0.820 _refine_diff_density_rms 0.094