# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2003 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Cameron Jones' 'Stephen Bruce' 'David E. Hibbs' 'Jon Steed' 'Ryan C. Thomas' 'Thomas C. WIlliams' _publ_contact_author_name 'Dr Cameron Jones' _publ_contact_author_address ; Department of Chemistry Cardiff University PO Box 912 Park Place Cardiff CF10 3TB UK ; _publ_contact_author_email 'JONESCA6@CARDIFF.AC.UK' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; The synthesis and structural characterisation of 2-arsa- and 2-stiba-1,3-dionato complexes of s- and p-block elements ; data_compound_15 _database_code_CSD 195258 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H40 As3 O7 P' _chemical_formula_weight 960.51 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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.075(3) _cell_length_b 14.159(3) _cell_length_c 15.026(3) _cell_angle_alpha 97.50(3) _cell_angle_beta 111.62(3) _cell_angle_gamma 117.04(3) _cell_volume 2149.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 972 _exptl_absorpt_coefficient_mu 2.406 _exptl_absorpt_correction_type 'Sortav (Blessing)' _exptl_absorpt_correction_T_min 0.63 _exptl_absorpt_correction_T_max 0.71 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _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 35408 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0407 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.47 _reflns_number_total 9793 _reflns_number_gt 8221 _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^)+(0.0245P)^2^+1.3753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9793 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0427 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0699 _refine_ls_wR_factor_gt 0.0654 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.45371(2) 0.844280(18) 0.265822(16) 0.02038(6) Uani 1 1 d . . . As2 As 0.57532(2) 0.761782(18) 0.484122(16) 0.01922(6) Uani 1 1 d . . . As3 As 0.41309(2) 0.560188(18) 0.222561(16) 0.02174(6) Uani 1 1 d . . . P1 P 0.40440(5) 0.69289(5) 0.32089(4) 0.01955(12) Uani 1 1 d . . . O1 O 0.27404(17) 0.71569(15) 0.05291(12) 0.0337(4) Uani 1 1 d . . . O2 O 0.56582(16) 0.75921(13) 0.17269(12) 0.0280(4) Uani 1 1 d . . . O3 O 0.58649(16) 0.95541(13) 0.57937(13) 0.0344(4) Uani 1 1 d . . . O4 O 0.71480(15) 0.92910(13) 0.41477(11) 0.0272(3) Uani 1 1 d . . . O5 O 0.68528(15) 0.68696(13) 0.37271(12) 0.0273(3) Uani 1 1 d . . . O6 O 0.46554(17) 0.44860(15) 0.36004(14) 0.0364(4) Uani 1 1 d . . . O7 O 0.81793(17) 0.83447(15) 0.87967(13) 0.0366(4) Uani 1 1 d . . . C1 C 0.2797(2) 0.74925(18) 0.13405(16) 0.0238(5) Uani 1 1 d . . . C2 C 0.5505(2) 0.83647(19) 0.18947(16) 0.0227(5) Uani 1 1 d . . . C3 C 0.1607(2) 0.72371(18) 0.14250(16) 0.0227(5) Uani 1 1 d . . . C4 C 0.1694(2) 0.7852(2) 0.22808(18) 0.0304(5) Uani 1 1 d . . . H4 H 0.2510 0.8433 0.2823 0.037 Uiso 1 1 calc R . . C5 C 0.0559(3) 0.7596(2) 0.2323(2) 0.0391(6) Uani 1 1 d . . . H5 H 0.0615 0.8017 0.2889 0.047 Uiso 1 1 calc R . . C6 C -0.0653(3) 0.6722(2) 0.1531(2) 0.0407(6) Uani 1 1 d . . . H6 H -0.1410 0.6552 0.1566 0.049 Uiso 1 1 calc R . . C7 C -0.0743(3) 0.6096(2) 0.0684(2) 0.0378(6) Uani 1 1 d . . . H7 H -0.1560 0.5497 0.0156 0.045 Uiso 1 1 calc R . . C8 C 0.0374(2) 0.6361(2) 0.06225(18) 0.0298(5) Uani 1 1 d . . . H8 H 0.0308 0.5954 0.0044 0.036 Uiso 1 1 calc R . . C9 C 0.5975(2) 0.93285(19) 0.15305(16) 0.0238(5) Uani 1 1 d . . . C10 C 0.6198(2) 1.0366(2) 0.20080(18) 0.0304(5) Uani 1 1 d . . . H10 H 0.6060 1.0467 0.2568 0.037 Uiso 1 1 calc R . . C11 C 0.6626(3) 1.1247(2) 0.1652(2) 0.0370(6) Uani 1 1 d . . . H11 H 0.6782 1.1942 0.1975 0.044 Uiso 1 1 calc R . . C12 C 0.6820(2) 1.1093(2) 0.0816(2) 0.0371(6) Uani 1 1 d . . . H12 H 0.7105 1.1685 0.0576 0.045 Uiso 1 1 calc R . . C13 C 0.6593(2) 1.0067(2) 0.0334(2) 0.0366(6) Uani 1 1 d . . . H13 H 0.6723 0.9969 -0.0231 0.044 Uiso 1 1 calc R . . C14 C 0.6170(2) 0.9179(2) 0.06858(18) 0.0286(5) Uani 1 1 d . . . H14 H 0.6017 0.8487 0.0359 0.034 Uiso 1 1 calc R . . C15 C 0.5154(2) 0.85303(18) 0.54000(16) 0.0216(4) Uani 1 1 d . . . C16 C 0.7275(2) 0.90103(18) 0.48863(16) 0.0209(4) Uani 1 1 d . . . C17 C 0.3824(2) 0.78744(18) 0.53033(15) 0.0218(4) Uani 1 1 d . . . C18 C 0.3158(2) 0.8420(2) 0.52866(18) 0.0303(5) Uani 1 1 d . . . H18 H 0.3553 0.9179 0.5347 0.036 Uiso 1 1 calc R . . C19 C 0.1913(3) 0.7831(2) 0.5180(2) 0.0388(6) Uani 1 1 d . . . H19 H 0.1473 0.8195 0.5173 0.047 Uiso 1 1 calc R . . C20 C 0.1324(3) 0.6704(2) 0.5086(2) 0.0411(6) Uani 1 1 d . . . H20 H 0.0483 0.6308 0.5009 0.049 Uiso 1 1 calc R . . C21 C 0.1978(3) 0.6163(2) 0.5105(2) 0.0418(7) Uani 1 1 d . . . H21 H 0.1579 0.5405 0.5047 0.050 Uiso 1 1 calc R . . C22 C 0.3220(2) 0.6740(2) 0.52098(18) 0.0308(5) Uani 1 1 d . . . H22 H 0.3653 0.6369 0.5218 0.037 Uiso 1 1 calc R . . C23 C 0.8542(2) 0.96191(18) 0.58519(16) 0.0223(4) Uani 1 1 d . . . C24 C 0.8655(2) 0.9359(2) 0.67318(18) 0.0309(5) Uani 1 1 d . . . H24 H 0.7917 0.8788 0.6724 0.037 Uiso 1 1 calc R . . C25 C 0.9857(3) 0.9946(2) 0.76179(19) 0.0385(6) Uani 1 1 d . . . H25 H 0.9924 0.9777 0.8207 0.046 Uiso 1 1 calc R . . C26 C 1.0958(3) 1.0784(2) 0.7626(2) 0.0376(6) Uani 1 1 d . . . H26 H 1.1767 1.1175 0.8220 0.045 Uiso 1 1 calc R . . C27 C 1.0863(2) 1.1044(2) 0.67548(19) 0.0344(6) Uani 1 1 d . . . H27 H 1.1609 1.1605 0.6764 0.041 Uiso 1 1 calc R . . C28 C 0.9667(2) 1.0474(2) 0.58732(18) 0.0270(5) Uani 1 1 d . . . H28 H 0.9606 1.0656 0.5291 0.032 Uiso 1 1 calc R . . C29 C 0.6043(2) 0.60949(18) 0.29106(16) 0.0218(4) Uani 1 1 d . . . C30 C 0.3815(2) 0.46392(18) 0.31080(17) 0.0249(5) Uani 1 1 d . . . C31 C 0.6364(2) 0.54014(19) 0.23735(17) 0.0253(5) Uani 1 1 d . . . C32 C 0.5635(2) 0.4820(2) 0.13148(18) 0.0299(5) Uani 1 1 d . . . H32 H 0.4925 0.4860 0.0924 0.036 Uiso 1 1 calc R . . C33 C 0.5968(3) 0.4181(2) 0.0842(2) 0.0370(6) Uani 1 1 d . . . H33 H 0.5494 0.3810 0.0134 0.044 Uiso 1 1 calc R . . C34 C 0.6995(3) 0.4097(2) 0.1419(2) 0.0440(7) Uani 1 1 d . . . H34 H 0.7207 0.3659 0.1102 0.053 Uiso 1 1 calc R . . C35 C 0.7711(3) 0.4657(3) 0.2466(2) 0.0552(9) Uani 1 1 d . . . H35 H 0.8405 0.4595 0.2855 0.066 Uiso 1 1 calc R . . C36 C 0.7401(3) 0.5314(3) 0.2943(2) 0.0437(7) Uani 1 1 d . . . H36 H 0.7893 0.5697 0.3650 0.052 Uiso 1 1 calc R . . C37 C 0.2540(2) 0.41408(18) 0.31212(17) 0.0262(5) Uani 1 1 d . . . C38 C 0.1465(2) 0.4078(2) 0.23835(19) 0.0343(6) Uani 1 1 d . . . H38 H 0.1537 0.4378 0.1879 0.041 Uiso 1 1 calc R . . C39 C 0.0282(3) 0.3566(2) 0.2398(2) 0.0451(7) Uani 1 1 d . . . H39 H -0.0440 0.3521 0.1902 0.054 Uiso 1 1 calc R . . C40 C 0.0182(3) 0.3125(2) 0.3150(2) 0.0456(7) Uani 1 1 d . . . H40 H -0.0615 0.2769 0.3152 0.055 Uiso 1 1 calc R . . C41 C 0.1255(3) 0.3206(2) 0.3900(2) 0.0405(6) Uani 1 1 d . . . H41 H 0.1183 0.2918 0.4410 0.049 Uiso 1 1 calc R . . C42 C 0.2435(3) 0.3716(2) 0.3892(2) 0.0320(5) Uani 1 1 d . . . H42 H 0.3160 0.3776 0.4400 0.038 Uiso 1 1 calc R . . C43 C 0.6152(3) 0.8161(3) 0.7815(2) 0.0593(9) Uani 1 1 d . . . H43A H 0.6627 0.8963 0.7955 0.089 Uiso 1 1 calc R . . H43B H 0.5306 0.7911 0.7758 0.089 Uiso 1 1 calc R . . H43C H 0.6042 0.7766 0.7184 0.089 Uiso 1 1 calc R . . C44 C 0.6898(3) 0.7914(3) 0.8668(2) 0.0464(7) Uani 1 1 d . . . H44A H 0.6956 0.8266 0.9299 0.056 Uiso 1 1 calc R . . H44B H 0.6445 0.7100 0.8514 0.056 Uiso 1 1 calc R . . C45 C 0.8916(3) 0.8095(2) 0.9578(2) 0.0433(7) Uani 1 1 d . . . H45A H 0.8527 0.7281 0.9370 0.052 Uiso 1 1 calc R . . H45B H 0.8904 0.8348 1.0204 0.052 Uiso 1 1 calc R . . C46 C 1.0301(3) 0.8687(3) 0.9767(2) 0.0529(8) Uani 1 1 d . . . H46A H 1.0307 0.8440 0.9143 0.079 Uiso 1 1 calc R . . H46B H 1.0796 0.8507 1.0285 0.079 Uiso 1 1 calc R . . H46C H 1.0689 0.9494 0.9993 0.079 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 As1 0.02113(12) 0.02036(11) 0.02032(11) 0.00737(9) 0.01028(9) 0.01160(10) As2 0.01938(12) 0.01880(11) 0.01828(11) 0.00587(9) 0.00892(9) 0.00991(10) As3 0.02127(12) 0.01965(12) 0.01954(11) 0.00385(9) 0.00833(9) 0.00980(10) P1 0.0186(3) 0.0194(3) 0.0193(3) 0.0062(2) 0.0093(2) 0.0096(2) O1 0.0337(10) 0.0415(10) 0.0224(8) 0.0079(7) 0.0141(8) 0.0186(9) O2 0.0317(9) 0.0301(9) 0.0293(8) 0.0121(7) 0.0178(8) 0.0193(8) O3 0.0288(9) 0.0194(9) 0.0459(10) 0.0017(7) 0.0204(8) 0.0075(8) O4 0.0240(9) 0.0298(9) 0.0247(8) 0.0118(7) 0.0120(7) 0.0119(7) O5 0.0222(9) 0.0266(9) 0.0263(8) 0.0031(7) 0.0102(7) 0.0113(7) O6 0.0342(10) 0.0403(10) 0.0464(11) 0.0249(9) 0.0224(9) 0.0241(9) O7 0.0357(10) 0.0356(10) 0.0364(10) 0.0160(8) 0.0181(8) 0.0168(9) C1 0.0281(13) 0.0213(11) 0.0214(11) 0.0083(9) 0.0101(10) 0.0142(10) C2 0.0191(11) 0.0251(11) 0.0185(10) 0.0053(9) 0.0067(9) 0.0107(10) C3 0.0224(12) 0.0195(11) 0.0248(11) 0.0092(9) 0.0090(10) 0.0120(10) C4 0.0242(13) 0.0299(13) 0.0287(12) 0.0027(10) 0.0078(10) 0.0146(11) C5 0.0337(15) 0.0434(16) 0.0410(15) 0.0060(12) 0.0187(13) 0.0235(13) C6 0.0276(14) 0.0418(16) 0.0507(16) 0.0137(13) 0.0187(13) 0.0186(13) C7 0.0223(13) 0.0317(14) 0.0389(14) 0.0062(12) 0.0061(11) 0.0085(11) C8 0.0294(13) 0.0284(13) 0.0241(12) 0.0070(10) 0.0090(10) 0.0142(11) C9 0.0157(11) 0.0279(12) 0.0220(11) 0.0089(9) 0.0066(9) 0.0098(10) C10 0.0288(13) 0.0294(13) 0.0275(12) 0.0112(10) 0.0127(11) 0.0123(11) C11 0.0305(14) 0.0269(13) 0.0429(15) 0.0139(12) 0.0136(12) 0.0110(12) C12 0.0233(13) 0.0360(15) 0.0417(15) 0.0239(12) 0.0128(12) 0.0086(12) C13 0.0281(14) 0.0479(16) 0.0351(14) 0.0224(12) 0.0189(12) 0.0170(13) C14 0.0233(12) 0.0338(13) 0.0293(12) 0.0135(10) 0.0140(10) 0.0145(11) C15 0.0227(12) 0.0202(11) 0.0203(10) 0.0061(9) 0.0108(9) 0.0107(10) C16 0.0206(11) 0.0193(10) 0.0242(11) 0.0057(9) 0.0127(9) 0.0110(9) C17 0.0232(12) 0.0211(11) 0.0177(10) 0.0043(9) 0.0115(9) 0.0091(10) C18 0.0300(13) 0.0291(13) 0.0339(13) 0.0100(10) 0.0185(11) 0.0158(11) C19 0.0331(15) 0.0458(16) 0.0468(16) 0.0158(13) 0.0231(13) 0.0254(13) C20 0.0279(14) 0.0433(16) 0.0461(16) 0.0113(13) 0.0235(13) 0.0121(13) C21 0.0414(16) 0.0270(13) 0.0562(17) 0.0145(13) 0.0337(15) 0.0104(12) C22 0.0368(14) 0.0260(12) 0.0388(13) 0.0138(11) 0.0264(12) 0.0168(11) C23 0.0198(11) 0.0223(11) 0.0233(11) 0.0046(9) 0.0101(9) 0.0116(10) C24 0.0253(13) 0.0291(13) 0.0280(12) 0.0098(10) 0.0102(11) 0.0098(11) C25 0.0342(15) 0.0426(15) 0.0246(12) 0.0109(11) 0.0057(11) 0.0178(13) C26 0.0226(13) 0.0421(15) 0.0311(13) 0.0036(12) 0.0028(11) 0.0161(12) C27 0.0212(13) 0.0342(14) 0.0409(14) 0.0056(11) 0.0161(11) 0.0113(11) C28 0.0240(12) 0.0292(12) 0.0298(12) 0.0073(10) 0.0160(10) 0.0144(11) C29 0.0216(12) 0.0207(11) 0.0245(11) 0.0101(9) 0.0135(10) 0.0104(10) C30 0.0244(12) 0.0193(11) 0.0274(11) 0.0065(9) 0.0116(10) 0.0106(10) C31 0.0295(13) 0.0221(11) 0.0283(12) 0.0101(9) 0.0182(11) 0.0134(10) C32 0.0335(14) 0.0254(12) 0.0293(12) 0.0079(10) 0.0176(11) 0.0138(11) C33 0.0480(17) 0.0260(13) 0.0355(14) 0.0067(11) 0.0278(13) 0.0143(13) C34 0.069(2) 0.0421(16) 0.0533(17) 0.0214(14) 0.0445(17) 0.0410(16) C35 0.074(2) 0.078(2) 0.0514(18) 0.0241(17) 0.0344(17) 0.064(2) C36 0.0543(18) 0.0571(18) 0.0361(14) 0.0128(13) 0.0226(14) 0.0426(16) C37 0.0255(12) 0.0176(11) 0.0306(12) 0.0046(9) 0.0139(10) 0.0090(10) C38 0.0253(13) 0.0325(14) 0.0301(13) 0.0073(11) 0.0093(11) 0.0093(11) C39 0.0184(13) 0.0525(18) 0.0409(15) 0.0080(14) 0.0083(12) 0.0095(13) C40 0.0286(15) 0.0433(16) 0.0499(17) 0.0084(14) 0.0229(14) 0.0080(13) C41 0.0451(17) 0.0330(14) 0.0474(16) 0.0161(12) 0.0311(14) 0.0169(13) C42 0.0339(14) 0.0267(12) 0.0411(14) 0.0145(11) 0.0210(12) 0.0178(12) C43 0.0443(19) 0.083(3) 0.0528(19) 0.0229(18) 0.0252(16) 0.0353(19) C44 0.0466(18) 0.0487(17) 0.0427(16) 0.0138(14) 0.0298(14) 0.0194(15) C45 0.0569(19) 0.0317(14) 0.0378(15) 0.0157(12) 0.0213(14) 0.0221(14) C46 0.0472(19) 0.0395(16) 0.0580(19) 0.0191(15) 0.0123(15) 0.0234(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C2 2.023(2) . ? As1 C1 2.027(3) . ? As1 P1 2.3010(9) . ? As2 C15 2.027(2) . ? As2 C16 2.037(2) . ? As2 P1 2.3057(15) . ? As3 C29 2.031(2) . ? As3 C30 2.037(2) . ? As3 P1 2.3063(9) . ? O1 C1 1.211(3) . ? O2 C2 1.210(3) . ? O3 C15 1.209(3) . ? O4 C16 1.207(3) . ? O5 C29 1.210(3) . ? O6 C30 1.209(3) . ? O7 C45 1.419(3) . ? O7 C44 1.420(3) . ? C1 C3 1.489(3) . ? C2 C9 1.490(3) . ? C3 C4 1.391(3) . ? C3 C8 1.396(3) . ? C4 C5 1.387(3) . ? C5 C6 1.379(4) . ? C6 C7 1.385(4) . ? C7 C8 1.377(3) . ? C9 C14 1.392(3) . ? C9 C10 1.392(3) . ? C10 C11 1.385(3) . ? C11 C12 1.379(4) . ? C12 C13 1.378(4) . ? C13 C14 1.386(3) . ? C15 C17 1.489(3) . ? C16 C23 1.482(3) . ? C17 C22 1.389(3) . ? C17 C18 1.399(3) . ? C18 C19 1.382(4) . ? C19 C20 1.379(4) . ? C20 C21 1.379(4) . ? C21 C22 1.379(4) . ? C23 C24 1.392(3) . ? C23 C28 1.402(3) . ? C24 C25 1.384(4) . ? C25 C26 1.383(4) . ? C26 C27 1.382(4) . ? C27 C28 1.378(3) . ? C29 C31 1.487(3) . ? C30 C37 1.495(3) . ? C31 C36 1.382(3) . ? C31 C32 1.394(3) . ? C32 C33 1.389(3) . ? C33 C34 1.372(4) . ? C34 C35 1.376(4) . ? C35 C36 1.389(4) . ? C37 C38 1.387(3) . ? C37 C42 1.394(3) . ? C38 C39 1.388(4) . ? C39 C40 1.380(4) . ? C40 C41 1.380(4) . ? C41 C42 1.380(4) . ? C43 C44 1.491(4) . ? C45 C46 1.498(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 As1 C1 90.94(9) . . ? C2 As1 P1 106.15(7) . . ? C1 As1 P1 91.04(7) . . ? C15 As2 C16 93.39(9) . . ? C15 As2 P1 91.23(7) . . ? C16 As2 P1 104.26(8) . . ? C29 As3 C30 89.18(9) . . ? C29 As3 P1 105.55(8) . . ? C30 As3 P1 90.67(6) . . ? As1 P1 As2 105.79(5) . . ? As1 P1 As3 108.63(3) . . ? As2 P1 As3 105.72(4) . . ? C45 O7 C44 111.8(2) . . ? O1 C1 C3 122.2(2) . . ? O1 C1 As1 121.22(18) . . ? C3 C1 As1 116.57(15) . . ? O2 C2 C9 123.1(2) . . ? O2 C2 As1 123.12(17) . . ? C9 C2 As1 113.71(15) . . ? C4 C3 C8 119.4(2) . . ? C4 C3 C1 121.6(2) . . ? C8 C3 C1 119.0(2) . . ? C5 C4 C3 119.8(2) . . ? C6 C5 C4 120.4(2) . . ? C5 C6 C7 120.0(2) . . ? C8 C7 C6 120.0(2) . . ? C7 C8 C3 120.3(2) . . ? C14 C9 C10 119.6(2) . . ? C14 C9 C2 119.3(2) . . ? C10 C9 C2 121.1(2) . . ? C11 C10 C9 120.2(2) . . ? C12 C11 C10 119.9(2) . . ? C13 C12 C11 120.4(2) . . ? C12 C13 C14 120.3(2) . . ? C13 C14 C9 119.7(2) . . ? O3 C15 C17 123.03(19) . . ? O3 C15 As2 120.33(17) . . ? C17 C15 As2 116.63(15) . . ? O4 C16 C23 122.5(2) . . ? O4 C16 As2 121.03(17) . . ? C23 C16 As2 116.42(15) . . ? C22 C17 C18 119.3(2) . . ? C22 C17 C15 122.2(2) . . ? C18 C17 C15 118.5(2) . . ? C19 C18 C17 120.0(2) . . ? C20 C19 C18 120.1(2) . . ? C19 C20 C21 120.1(2) . . ? C22 C21 C20 120.4(2) . . ? C21 C22 C17 120.1(2) . . ? C24 C23 C28 119.0(2) . . ? C24 C23 C16 122.2(2) . . ? C28 C23 C16 118.8(2) . . ? C25 C24 C23 120.4(2) . . ? C26 C25 C24 119.8(2) . . ? C27 C26 C25 120.3(2) . . ? C28 C27 C26 120.2(2) . . ? C27 C28 C23 120.1(2) . . ? O5 C29 C31 122.3(2) . . ? O5 C29 As3 122.00(16) . . ? C31 C29 As3 115.63(16) . . ? O6 C30 C37 122.1(2) . . ? O6 C30 As3 119.39(17) . . ? C37 C30 As3 118.50(16) . . ? C36 C31 C32 119.0(2) . . ? C36 C31 C29 119.0(2) . . ? C32 C31 C29 121.9(2) . . ? C33 C32 C31 120.1(2) . . ? C34 C33 C32 120.1(2) . . ? C33 C34 C35 120.3(2) . . ? C34 C35 C36 120.1(3) . . ? C31 C36 C35 120.4(3) . . ? C38 C37 C42 119.6(2) . . ? C38 C37 C30 121.8(2) . . ? C42 C37 C30 118.6(2) . . ? C37 C38 C39 120.0(2) . . ? C40 C39 C38 119.8(3) . . ? C41 C40 C39 120.5(3) . . ? C40 C41 C42 120.0(3) . . ? C41 C42 C37 120.0(2) . . ? O7 C44 C43 109.6(2) . . ? O7 C45 C46 109.4(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.372 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.078 data_compound_13 _database_code_CSD 195259 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H38 As Cl3 In Li O5' _chemical_formula_weight 637.51 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'In' 'In' -0.7276 1.3100 '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' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 17.155(3) _cell_length_b 18.028(4) _cell_length_c 18.480(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5715(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2576 _exptl_absorpt_coefficient_mu 2.279 _exptl_absorpt_correction_type 'Sortav (Blessing, 1995)' _exptl_absorpt_correction_T_min 0.553 _exptl_absorpt_correction_T_max 0.751 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Kappa CCD' _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 91098 _diffrn_reflns_av_R_equivalents 0.1246 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.49 _reflns_number_total 6540 _reflns_number_gt 4852 _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^)+(0.0532P)^2^+26.7221P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6540 _refine_ls_number_parameters 252 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0980 _refine_ls_R_factor_gt 0.0665 _refine_ls_wR_factor_ref 0.1521 _refine_ls_wR_factor_gt 0.1398 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.105 _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 In1 In 0.64307(3) 0.10287(2) 0.68112(2) 0.03521(14) Uani 1 1 d . . . As1 As 0.53260(4) 0.11841(3) 0.58525(3) 0.03425(17) Uani 1 1 d . . . Cl1 Cl 0.64856(13) 0.20358(10) 0.76376(11) 0.0604(5) Uani 1 1 d . . . Cl2 Cl 0.76816(10) 0.09363(11) 0.62682(11) 0.0544(5) Uani 1 1 d . . . Cl3 Cl 0.62527(13) -0.00576(10) 0.75123(11) 0.0591(5) Uani 1 1 d . . . O1 O 0.5206(3) 0.2735(2) 0.6202(2) 0.0433(11) Uani 1 1 d . . . O2 O 0.6260(3) 0.2273(3) 0.5128(2) 0.0440(11) Uani 1 1 d . . . O3 O 0.7261(4) 0.3218(4) 0.6018(3) 0.0792(18) Uani 1 1 d U . . O4 O 0.6166(5) 0.4114(4) 0.6400(4) 0.089(2) Uani 1 1 d . . . O5 O 0.5572(4) 0.3805(4) 0.4892(3) 0.086(2) Uani 1 1 d D . . C1 C 0.4942(4) 0.2128(4) 0.6331(3) 0.0360(14) Uani 1 1 d . . . C2 C 0.6045(3) 0.1640(3) 0.5107(3) 0.0331(13) Uani 1 1 d . . . C3 C 0.4245(4) 0.2026(4) 0.6830(4) 0.0515(18) Uani 1 1 d . . . C4 C 0.4162(6) 0.2690(5) 0.7317(5) 0.088(3) Uani 1 1 d . . . H4A H 0.4632 0.2756 0.7591 0.133 Uiso 1 1 calc R . . H4B H 0.3732 0.2615 0.7641 0.133 Uiso 1 1 calc R . . H4C H 0.4069 0.3125 0.7029 0.133 Uiso 1 1 calc R . . C5 C 0.3537(4) 0.1937(6) 0.6321(6) 0.081(3) Uani 1 1 d . . . H5A H 0.3444 0.2396 0.6072 0.121 Uiso 1 1 calc R . . H5B H 0.3085 0.1807 0.6600 0.121 Uiso 1 1 calc R . . H5C H 0.3642 0.1553 0.5975 0.121 Uiso 1 1 calc R . . C6 C 0.4331(5) 0.1324(5) 0.7291(4) 0.064(2) Uani 1 1 d . . . H6A H 0.4327 0.0896 0.6982 0.096 Uiso 1 1 calc R . . H6B H 0.3905 0.1293 0.7626 0.096 Uiso 1 1 calc R . . H6C H 0.4814 0.1342 0.7552 0.096 Uiso 1 1 calc R . . C7 C 0.6249(4) 0.1133(4) 0.4467(4) 0.0451(16) Uani 1 1 d . . . C8 C 0.5551(6) 0.1186(6) 0.3952(4) 0.073(3) Uani 1 1 d . . . H8A H 0.5626 0.0853 0.3553 0.110 Uiso 1 1 calc R . . H8B H 0.5507 0.1685 0.3774 0.110 Uiso 1 1 calc R . . H8C H 0.5083 0.1055 0.4206 0.110 Uiso 1 1 calc R . . C9 C 0.6995(5) 0.1429(5) 0.4099(4) 0.059(2) Uani 1 1 d . . . H9A H 0.7425 0.1396 0.4430 0.088 Uiso 1 1 calc R . . H9B H 0.6918 0.1937 0.3962 0.088 Uiso 1 1 calc R . . H9C H 0.7106 0.1138 0.3676 0.088 Uiso 1 1 calc R . . C10 C 0.6361(5) 0.0332(4) 0.4706(4) 0.056(2) Uani 1 1 d . . . H10A H 0.6771 0.0307 0.5058 0.083 Uiso 1 1 calc R . . H10B H 0.6496 0.0034 0.4294 0.083 Uiso 1 1 calc R . . H10C H 0.5886 0.0151 0.4915 0.083 Uiso 1 1 calc R . . C11 C 0.7910(7) 0.2915(7) 0.5661(7) 0.108(4) Uani 1 1 d U . . H11A H 0.8225 0.3309 0.5469 0.162 Uiso 1 1 calc R . . H11B H 0.7737 0.2602 0.5273 0.162 Uiso 1 1 calc R . . H11C H 0.8213 0.2629 0.5997 0.162 Uiso 1 1 calc R . . C12 C 0.7490(7) 0.3791(6) 0.6451(6) 0.091(3) Uani 1 1 d U . . H12A H 0.7674 0.4206 0.6163 0.109 Uiso 1 1 calc R . . H12B H 0.7902 0.3637 0.6777 0.109 Uiso 1 1 calc R . . C13 C 0.6755(6) 0.4004(4) 0.6873(4) 0.062(2) Uani 1 1 d . . . H13A H 0.6618 0.3610 0.7208 0.075 Uiso 1 1 calc R . . H13B H 0.6848 0.4453 0.7150 0.075 Uiso 1 1 calc R . . C14 C 0.5538(8) 0.4409(6) 0.6742(6) 0.107(4) Uani 1 1 d . . . H14A H 0.5349 0.4065 0.7097 0.160 Uiso 1 1 calc R . . H14B H 0.5134 0.4507 0.6394 0.160 Uiso 1 1 calc R . . H14C H 0.5685 0.4863 0.6975 0.160 Uiso 1 1 calc R . . Li1 Li 0.6071(8) 0.3221(6) 0.5679(6) 0.049(3) Uani 1 1 d . . . C15 C 0.6699(7) 0.4288(7) 0.4455(7) 0.110(4) Uiso 1 1 d D . . H15A H 0.6732 0.4606 0.4871 0.165 Uiso 1 1 calc R . . H15B H 0.6921 0.4535 0.4044 0.165 Uiso 1 1 calc R . . H15C H 0.6980 0.3837 0.4548 0.165 Uiso 1 1 calc R . . C16 C 0.5878(8) 0.4114(9) 0.4307(8) 0.152(6) Uiso 1 1 d D . . H16A H 0.5596 0.4563 0.4186 0.182 Uiso 1 1 calc R . . H16B H 0.5840 0.3775 0.3901 0.182 Uiso 1 1 calc R . . C17 C 0.4694(10) 0.3833(11) 0.4882(13) 0.213(10) Uiso 1 1 d D . . H17A H 0.4476 0.3824 0.5366 0.255 Uiso 1 1 calc R . . H17B H 0.4501 0.4264 0.4624 0.255 Uiso 1 1 calc R . . C18 C 0.4548(10) 0.3194(9) 0.4517(9) 0.155(6) Uiso 1 1 d D . . H18A H 0.4865 0.3176 0.4090 0.233 Uiso 1 1 calc R . . H18B H 0.4008 0.3177 0.4383 0.233 Uiso 1 1 calc R . . H18C H 0.4668 0.2778 0.4821 0.233 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 In1 0.0375(3) 0.0335(2) 0.0346(2) 0.00218(18) -0.00017(19) -0.00002(18) As1 0.0310(3) 0.0361(3) 0.0357(3) -0.0035(3) 0.0014(3) -0.0070(2) Cl1 0.0818(14) 0.0459(10) 0.0533(11) -0.0089(8) -0.0169(10) 0.0007(9) Cl2 0.0348(9) 0.0690(12) 0.0593(11) 0.0116(9) 0.0020(8) -0.0011(8) Cl3 0.0816(13) 0.0423(9) 0.0534(11) 0.0114(8) 0.0209(10) 0.0062(9) O1 0.051(3) 0.034(2) 0.045(3) -0.002(2) 0.007(2) 0.005(2) O2 0.052(3) 0.044(3) 0.037(3) -0.009(2) 0.011(2) -0.011(2) O3 0.100(4) 0.070(3) 0.067(3) -0.001(3) -0.007(3) -0.026(3) O4 0.097(5) 0.088(5) 0.081(5) -0.002(4) -0.010(4) -0.013(4) O5 0.101(5) 0.101(5) 0.057(4) 0.031(4) -0.008(4) -0.005(4) C1 0.034(3) 0.042(4) 0.032(3) -0.001(3) 0.000(3) 0.003(3) C2 0.029(3) 0.040(3) 0.031(3) -0.005(3) 0.000(2) -0.003(3) C3 0.044(4) 0.056(4) 0.054(4) 0.005(4) 0.018(4) 0.006(3) C4 0.105(8) 0.068(6) 0.092(8) -0.012(5) 0.058(6) 0.004(5) C5 0.035(4) 0.104(8) 0.102(8) 0.021(6) 0.011(5) 0.003(4) C6 0.061(5) 0.078(6) 0.053(5) 0.020(4) 0.031(4) 0.001(4) C7 0.052(4) 0.052(4) 0.031(3) -0.010(3) 0.001(3) 0.000(3) C8 0.085(6) 0.099(7) 0.037(4) -0.027(4) -0.017(4) 0.006(5) C9 0.073(5) 0.062(5) 0.042(4) -0.008(4) 0.025(4) -0.005(4) C10 0.063(5) 0.052(4) 0.051(5) -0.016(4) 0.011(4) -0.007(4) C11 0.104(5) 0.106(5) 0.113(5) -0.001(4) -0.004(4) 0.006(4) C12 0.093(5) 0.087(5) 0.091(5) -0.007(4) -0.011(4) -0.006(4) C13 0.100(7) 0.045(4) 0.042(4) -0.005(3) -0.022(4) -0.005(4) C14 0.148(11) 0.082(8) 0.091(8) -0.029(6) 0.016(8) 0.024(7) Li1 0.072(8) 0.039(6) 0.036(6) 0.004(5) 0.013(6) -0.002(6) _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 In1 Cl3 2.3680(18) . ? In1 Cl1 2.3744(19) . ? In1 Cl2 2.3748(18) . ? In1 As1 2.6094(9) . ? As1 C2 2.024(6) . ? As1 C1 2.028(6) . ? O1 C1 1.209(8) . ? O1 Li1 1.976(13) . ? O2 C2 1.200(7) . ? O2 Li1 2.015(12) . ? O3 C12 1.365(11) . ? O3 C11 1.405(12) . ? O3 Li1 2.135(15) . ? O4 C13 1.351(10) . ? O4 C14 1.356(12) . ? O4 Li1 2.097(14) . ? O5 C16 1.323(13) . ? O5 C17 1.507(15) . ? O5 Li1 1.990(14) . ? C1 C3 1.520(9) . ? C2 C7 1.535(9) . ? C3 C4 1.505(11) . ? C3 C6 1.532(10) . ? C3 C5 1.545(12) . ? C7 C10 1.520(10) . ? C7 C8 1.534(11) . ? C7 C9 1.544(10) . ? C12 C13 1.532(14) . ? C15 C16 1.469(14) . ? C17 C18 1.358(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl3 In1 Cl1 106.60(7) . . ? Cl3 In1 Cl2 106.84(7) . . ? Cl1 In1 Cl2 106.83(8) . . ? Cl3 In1 As1 111.51(6) . . ? Cl1 In1 As1 112.55(5) . . ? Cl2 In1 As1 112.14(5) . . ? C2 As1 C1 98.9(3) . . ? C2 As1 In1 93.60(17) . . ? C1 As1 In1 91.72(18) . . ? C1 O1 Li1 141.2(5) . . ? C2 O2 Li1 140.7(5) . . ? C12 O3 C11 110.0(8) . . ? C12 O3 Li1 116.4(7) . . ? C11 O3 Li1 128.4(7) . . ? C13 O4 C14 110.5(8) . . ? C13 O4 Li1 110.8(7) . . ? C14 O4 Li1 122.3(8) . . ? C16 O5 C17 111.9(12) . . ? C16 O5 Li1 130.4(9) . . ? C17 O5 Li1 117.2(11) . . ? O1 C1 C3 121.6(6) . . ? O1 C1 As1 123.5(5) . . ? C3 C1 As1 114.7(5) . . ? O2 C2 C7 121.5(6) . . ? O2 C2 As1 123.5(5) . . ? C7 C2 As1 114.9(4) . . ? C4 C3 C1 109.9(6) . . ? C4 C3 C6 109.6(7) . . ? C1 C3 C6 111.2(6) . . ? C4 C3 C5 111.8(7) . . ? C1 C3 C5 105.1(6) . . ? C6 C3 C5 109.1(7) . . ? C10 C7 C8 109.8(6) . . ? C10 C7 C2 111.8(6) . . ? C8 C7 C2 105.2(6) . . ? C10 C7 C9 110.6(6) . . ? C8 C7 C9 110.6(7) . . ? C2 C7 C9 108.8(6) . . ? O3 C12 C13 104.6(8) . . ? O4 C13 C12 108.8(8) . . ? O1 Li1 O5 105.6(7) . . ? O1 Li1 O2 89.5(5) . . ? O5 Li1 O2 98.6(6) . . ? O1 Li1 O4 95.0(5) . . ? O5 Li1 O4 95.2(6) . . ? O2 Li1 O4 163.8(8) . . ? O1 Li1 O3 125.0(6) . . ? O5 Li1 O3 128.9(6) . . ? O2 Li1 O3 89.6(5) . . ? O4 Li1 O3 75.0(5) . . ? O5 C16 C15 108.6(12) . . ? C18 C17 O5 99.3(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 2.140 _refine_diff_density_min -0.615 _refine_diff_density_rms 0.123 data_compound_12 _database_code_CSD 195260 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H30 As2 Mg O6' _chemical_formula_weight 684.71 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Mg' 'Mg' 0.0486 0.0363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 8.4986(6) _cell_length_b 22.694(2) _cell_length_c 16.2467(11) _cell_angle_alpha 90.00 _cell_angle_beta 105.137(4) _cell_angle_gamma 90.00 _cell_volume 3024.7(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.504 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.273 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.4634 _exptl_absorpt_correction_T_max 0.8948 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 34110 _diffrn_reflns_av_R_equivalents 0.060 _diffrn_reflns_av_sigmaI/netI 0.1112 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4962 _reflns_number_gt 4298 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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^)+(0.0000P)^2^+8.6048P] 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 SHELXL _refine_ls_extinction_coef 0.0011(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.024(17) _refine_ls_number_reflns 4962 _refine_ls_number_parameters 373 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0844 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1630 _refine_ls_wR_factor_gt 0.1546 _refine_ls_goodness_of_fit_ref 1.192 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.72548(10) 0.19648(6) 0.10157(7) 0.0645(4) Uani 1 1 d . . . Mg1 Mg 0.3543(3) 0.12486(17) -0.05929(18) 0.0446(8) Uani 1 1 d . . . O1 O 0.3984(6) 0.2061(3) -0.0061(4) 0.0514(18) Uani 1 1 d . . . C1 C 0.5275(9) 0.2318(5) 0.0320(5) 0.049(3) Uani 1 1 d . . . As2 As 0.56453(9) 0.05352(6) -0.22001(6) 0.0641(4) Uani 1 1 d . . . O2 O 0.5426(6) 0.0945(3) 0.0330(3) 0.0478(16) Uani 1 1 d . . . C2 C 0.5347(9) 0.2969(5) 0.0241(6) 0.057(3) Uani 1 1 d . . . O3 O 0.4505(6) 0.1552(3) -0.1510(3) 0.0503(17) Uani 1 1 d . . . C3 C 0.4206(13) 0.3244(6) -0.0431(7) 0.061(3) Uani 1 1 d . . . H3 H 0.3400 0.3013 -0.0810 0.074 Uiso 1 1 calc R . . O4 O 0.3454(6) 0.0436(3) -0.1124(4) 0.0495(17) Uani 1 1 d . . . C4 C 0.4237(13) 0.3833(7) -0.0546(7) 0.070(4) Uani 1 1 d . . . H4 H 0.3462 0.4009 -0.1011 0.084 Uiso 1 1 calc R . . O5 O 0.1190(6) 0.1526(3) -0.1311(4) 0.0556(18) Uani 1 1 d . . . C5 C 0.5389(15) 0.4191(6) 0.0007(7) 0.079(4) Uani 1 1 d . . . H5 H 0.5409 0.4604 -0.0085 0.095 Uiso 1 1 calc R . . O6 O 0.1908(7) 0.0973(3) 0.0126(4) 0.0579(19) Uani 1 1 d . . . C6 C 0.6514(14) 0.3929(6) 0.0699(7) 0.071(4) Uani 1 1 d . . . H6 H 0.7283 0.4163 0.1095 0.086 Uiso 1 1 calc R . . C7 C 0.6484(11) 0.3334(6) 0.0794(6) 0.060(3) Uani 1 1 d . . . H7 H 0.7267 0.3157 0.1254 0.072 Uiso 1 1 calc R . . C8 C 0.6649(9) 0.1151(5) 0.0855(5) 0.042(2) Uani 1 1 d . . . C9 C 0.7800(10) 0.0719(5) 0.1380(5) 0.048(3) Uani 1 1 d . . . C10 C 0.7764(11) 0.0139(5) 0.1112(5) 0.050(3) Uani 1 1 d . . . H10 H 0.6989 0.0021 0.0605 0.060 Uiso 1 1 calc R . . C11 C 0.8844(11) -0.0269(5) 0.1577(6) 0.059(3) Uani 1 1 d . . . H11 H 0.8803 -0.0668 0.1395 0.070 Uiso 1 1 calc R . . C12 C 0.9981(11) -0.0093(6) 0.2305(6) 0.064(3) Uani 1 1 d . . . H12 H 1.0751 -0.0372 0.2608 0.077 Uiso 1 1 calc R . . C13 C 1.0031(10) 0.0468(7) 0.2602(6) 0.072(4) Uani 1 1 d . . . H13 H 1.0798 0.0578 0.3117 0.087 Uiso 1 1 calc R . . C14 C 0.8941(10) 0.0880(6) 0.2140(6) 0.066(3) Uani 1 1 d . . . H14 H 0.8969 0.1275 0.2339 0.079 Uiso 1 1 calc R . . C15 C 0.5212(9) 0.1345(5) -0.2031(5) 0.046(2) Uani 1 1 d . . . C16 C 0.5828(9) 0.1780(5) -0.2560(5) 0.044(2) Uani 1 1 d . . . C17 C 0.6059(10) 0.2358(5) -0.2309(5) 0.050(3) Uani 1 1 d . . . H17 H 0.5792 0.2477 -0.1802 0.060 Uiso 1 1 calc R . . C18 C 0.6663(10) 0.2769(5) -0.2764(6) 0.055(2) Uani 1 1 d . . . H18 H 0.6787 0.3168 -0.2583 0.066 Uiso 1 1 calc R . . C19 C 0.7089(10) 0.2593(6) -0.3491(6) 0.059(3) Uani 1 1 d . . . H19 H 0.7568 0.2870 -0.3791 0.070 Uiso 1 1 calc R . . C20 C 0.6836(11) 0.2032(6) -0.3784(6) 0.064(3) Uani 1 1 d . . . H20 H 0.7090 0.1921 -0.4298 0.077 Uiso 1 1 calc R . . C21 C 0.6200(9) 0.1623(6) -0.3324(6) 0.060(3) Uani 1 1 d . . . H21 H 0.6014 0.1230 -0.3528 0.072 Uiso 1 1 calc R . . C22 C 0.4371(9) 0.0181(5) -0.1508(5) 0.050(3) Uani 1 1 d . . . C23 C 0.4502(9) -0.0469(5) -0.1425(5) 0.052(3) Uani 1 1 d . . . C24 C 0.4046(12) -0.0743(6) -0.0753(7) 0.061(3) Uani 1 1 d . . . H24 H 0.3629 -0.0511 -0.0371 0.073 Uiso 1 1 calc R . . C25 C 0.4193(13) -0.1350(6) -0.0633(7) 0.066(3) Uani 1 1 d . . . H25 H 0.3884 -0.1530 -0.0171 0.079 Uiso 1 1 calc R . . C26 C 0.4787(15) -0.1688(6) -0.1189(7) 0.077(3) Uani 1 1 d . . . H26 H 0.4905 -0.2102 -0.1104 0.093 Uiso 1 1 calc R . . C27 C 0.5215(14) -0.1427(6) -0.1874(8) 0.074(4) Uani 1 1 d . . . H27 H 0.5577 -0.1663 -0.2272 0.089 Uiso 1 1 calc R . . C28 C 0.5114(11) -0.0830(5) -0.1975(6) 0.059(3) Uani 1 1 d . . . H28 H 0.5466 -0.0654 -0.2426 0.071 Uiso 1 1 calc R . . C29 C 0.0815(14) 0.1824(6) -0.2105(8) 0.068(3) Uani 1 1 d . . . H29A H 0.0426 0.1540 -0.2568 0.102 Uiso 1 1 calc R . . H29B H 0.1796 0.2021 -0.2179 0.102 Uiso 1 1 calc R . . H29C H -0.0035 0.2119 -0.2118 0.102 Uiso 1 1 calc R . . C30 C -0.0111(12) 0.1379(7) -0.1008(9) 0.089(4) Uani 1 1 d . . . H30A H -0.0804 0.1098 -0.1409 0.107 Uiso 1 1 calc R . . H30B H -0.0767 0.1738 -0.0997 0.107 Uiso 1 1 calc R . . C31 C 0.0308(12) 0.1122(7) -0.0170(9) 0.091(4) Uani 1 1 d . . . H31A H 0.0025 0.1404 0.0233 0.109 Uiso 1 1 calc R . . H31B H -0.0363 0.0764 -0.0180 0.109 Uiso 1 1 calc R . . C32 C 0.2355(15) 0.0666(5) 0.0920(8) 0.068(3) Uani 1 1 d . . . H32A H 0.2234 0.0930 0.1377 0.102 Uiso 1 1 calc R . . H32B H 0.3492 0.0537 0.1034 0.102 Uiso 1 1 calc R . . H32C H 0.1646 0.0322 0.0894 0.102 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 As1 0.0194(4) 0.0820(8) 0.0829(8) -0.0366(6) -0.0030(4) -0.0023(5) Mg1 0.0168(12) 0.086(2) 0.0333(13) -0.0253(14) 0.0096(10) -0.0055(14) O1 0.019(3) 0.082(5) 0.052(4) -0.041(4) 0.009(2) 0.002(3) C1 0.023(4) 0.079(7) 0.047(5) -0.042(5) 0.015(4) -0.012(4) As2 0.0469(5) 0.0819(8) 0.0811(7) -0.0372(6) 0.0479(5) -0.0157(5) O2 0.028(3) 0.077(5) 0.036(3) -0.013(3) 0.004(2) -0.009(3) C2 0.019(4) 0.105(9) 0.048(5) -0.041(5) 0.011(4) 0.003(5) O3 0.033(3) 0.087(5) 0.032(3) -0.010(3) 0.012(2) 0.006(3) C3 0.043(6) 0.082(9) 0.067(7) -0.029(7) 0.028(5) -0.004(6) O4 0.025(3) 0.071(5) 0.058(4) -0.035(3) 0.021(3) -0.019(3) C4 0.056(6) 0.116(12) 0.042(5) -0.014(6) 0.019(5) 0.028(7) O5 0.023(3) 0.076(5) 0.065(5) -0.017(4) 0.006(3) 0.004(3) C5 0.085(8) 0.090(9) 0.060(7) -0.038(7) 0.013(6) 0.003(7) O6 0.038(3) 0.091(6) 0.054(4) -0.017(4) 0.030(3) -0.012(3) C6 0.063(7) 0.083(10) 0.064(7) -0.052(6) 0.009(5) -0.004(6) C7 0.040(5) 0.085(9) 0.055(6) -0.036(6) 0.012(4) 0.011(5) C8 0.026(4) 0.080(7) 0.026(4) -0.009(4) 0.019(3) -0.001(4) C9 0.023(4) 0.095(9) 0.029(4) -0.006(5) 0.014(3) 0.000(5) C10 0.041(5) 0.083(8) 0.031(5) -0.005(5) 0.017(4) -0.013(5) C11 0.041(5) 0.087(8) 0.054(6) 0.016(5) 0.023(5) -0.012(5) C12 0.032(5) 0.112(11) 0.056(6) 0.010(6) 0.024(4) 0.005(6) C13 0.022(4) 0.144(13) 0.047(6) -0.021(6) 0.002(4) 0.023(6) C14 0.027(4) 0.121(10) 0.051(5) -0.028(6) 0.012(4) 0.008(5) C15 0.012(3) 0.087(8) 0.039(5) -0.014(4) 0.007(3) 0.003(4) C16 0.017(4) 0.084(8) 0.030(4) -0.013(4) 0.002(3) -0.008(4) C17 0.027(4) 0.094(9) 0.025(4) -0.001(5) -0.001(3) 0.016(5) C18 0.036(5) 0.072(7) 0.053(6) 0.015(5) 0.004(4) 0.019(5) C19 0.031(4) 0.095(9) 0.048(6) 0.016(6) 0.006(4) 0.005(5) C20 0.035(5) 0.125(11) 0.040(5) -0.020(6) 0.022(4) -0.020(6) C21 0.027(4) 0.108(9) 0.049(5) -0.022(5) 0.017(4) -0.018(5) C22 0.024(4) 0.079(7) 0.048(5) -0.039(5) 0.012(4) -0.011(4) C23 0.022(4) 0.090(8) 0.047(5) -0.034(5) 0.014(3) -0.020(4) C24 0.041(5) 0.078(8) 0.061(7) -0.023(6) 0.007(5) -0.002(6) C25 0.059(6) 0.095(10) 0.045(6) -0.042(6) 0.015(5) -0.009(6) C26 0.080(8) 0.081(9) 0.064(7) -0.026(6) 0.005(6) -0.022(7) C27 0.067(7) 0.085(10) 0.073(8) -0.045(7) 0.026(6) -0.021(6) C28 0.044(5) 0.072(8) 0.062(6) -0.035(6) 0.016(4) -0.023(5) C29 0.045(6) 0.084(9) 0.071(7) -0.018(7) 0.008(5) 0.017(6) C30 0.030(5) 0.141(13) 0.103(10) 0.007(9) 0.029(5) 0.017(6) C31 0.022(5) 0.142(13) 0.114(10) 0.000(9) 0.029(6) -0.013(6) C32 0.062(6) 0.077(8) 0.072(8) -0.016(7) 0.030(5) -0.024(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C8 1.916(10) . ? As1 C1 1.938(9) . ? Mg1 O3 2.000(6) . ? Mg1 O2 2.007(6) . ? Mg1 O4 2.028(7) . ? Mg1 O1 2.029(7) . ? Mg1 O6 2.129(6) . ? Mg1 O5 2.131(6) . ? O1 C1 1.253(9) . ? C1 C2 1.486(15) . ? As2 C15 1.908(10) . ? As2 C22 1.928(9) . ? O2 C8 1.251(10) . ? C2 C7 1.405(13) . ? C2 C3 1.404(16) . ? O3 C15 1.250(9) . ? C3 C4 1.351(19) . ? O4 C22 1.261(9) . ? C4 C5 1.403(17) . ? O5 C30 1.364(12) . ? O5 C29 1.418(14) . ? C5 C6 1.404(18) . ? O6 C31 1.362(12) . ? O6 C32 1.427(14) . ? C6 C7 1.361(17) . ? C8 C9 1.486(13) . ? C9 C10 1.385(15) . ? C9 C14 1.404(13) . ? C10 C11 1.381(14) . ? C11 C12 1.376(14) . ? C12 C13 1.360(17) . ? C13 C14 1.390(16) . ? C15 C16 1.492(13) . ? C16 C17 1.372(15) . ? C16 C21 1.405(12) . ? C17 C18 1.370(14) . ? C18 C19 1.382(14) . ? C19 C20 1.356(16) . ? C20 C21 1.387(15) . ? C22 C23 1.482(15) . ? C23 C24 1.396(16) . ? C23 C28 1.408(13) . ? C24 C25 1.393(18) . ? C25 C26 1.377(15) . ? C26 C27 1.392(17) . ? C27 C28 1.363(17) . ? C30 C31 1.438(16) . ? 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 C8 As1 C1 99.1(4) . . ? O3 Mg1 O2 105.9(2) . . ? O3 Mg1 O4 88.5(3) . . ? O2 Mg1 O4 86.5(3) . . ? O3 Mg1 O1 86.5(3) . . ? O2 Mg1 O1 88.4(3) . . ? O4 Mg1 O1 171.6(2) . . ? O3 Mg1 O6 164.2(3) . . ? O2 Mg1 O6 89.8(3) . . ? O4 Mg1 O6 90.5(3) . . ? O1 Mg1 O6 96.2(3) . . ? O3 Mg1 O5 89.9(3) . . ? O2 Mg1 O5 164.1(3) . . ? O4 Mg1 O5 96.3(3) . . ? O1 Mg1 O5 90.4(3) . . ? O6 Mg1 O5 74.5(3) . . ? C1 O1 Mg1 132.3(6) . . ? O1 C1 C2 118.1(8) . . ? O1 C1 As1 127.6(8) . . ? C2 C1 As1 114.3(5) . . ? C15 As2 C22 99.2(4) . . ? C8 O2 Mg1 137.7(7) . . ? C7 C2 C3 117.1(11) . . ? C7 C2 C1 124.6(9) . . ? C3 C2 C1 118.3(8) . . ? C15 O3 Mg1 137.5(7) . . ? C4 C3 C2 120.9(11) . . ? C22 O4 Mg1 132.0(6) . . ? C3 C4 C5 121.3(12) . . ? C30 O5 C29 115.8(8) . . ? C30 O5 Mg1 117.6(7) . . ? C29 O5 Mg1 126.5(6) . . ? C4 C5 C6 118.9(13) . . ? C31 O6 C32 116.5(8) . . ? C31 O6 Mg1 117.9(7) . . ? C32 O6 Mg1 125.6(6) . . ? C7 C6 C5 118.8(10) . . ? C6 C7 C2 122.9(11) . . ? O2 C8 C9 116.7(9) . . ? O2 C8 As1 126.8(7) . . ? C9 C8 As1 116.4(6) . . ? C10 C9 C14 118.5(10) . . ? C10 C9 C8 119.3(8) . . ? C14 C9 C8 122.2(10) . . ? C11 C10 C9 120.6(9) . . ? C12 C11 C10 119.5(12) . . ? C13 C12 C11 121.7(11) . . ? C12 C13 C14 119.0(10) . . ? C13 C14 C9 120.6(12) . . ? O3 C15 C16 116.4(9) . . ? O3 C15 As2 127.2(8) . . ? C16 C15 As2 116.4(6) . . ? C17 C16 C21 117.3(9) . . ? C17 C16 C15 120.4(8) . . ? C21 C16 C15 122.3(10) . . ? C18 C17 C16 122.3(9) . . ? C17 C18 C19 118.9(11) . . ? C20 C19 C18 121.3(10) . . ? C19 C20 C21 119.1(9) . . ? C20 C21 C16 121.0(11) . . ? O4 C22 C23 117.0(8) . . ? O4 C22 As2 127.6(8) . . ? C23 C22 As2 115.4(5) . . ? C24 C23 C28 117.5(11) . . ? C24 C23 C22 119.0(8) . . ? C28 C23 C22 123.5(9) . . ? C25 C24 C23 121.1(10) . . ? C26 C25 C24 119.7(12) . . ? C25 C26 C27 120.2(13) . . ? C28 C27 C26 119.9(10) . . ? C27 C28 C23 121.6(11) . . ? O5 C30 C31 114.7(9) . . ? O6 C31 C30 114.4(9) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Mg1 O1 C1 -72.1(9) . . . . ? O2 Mg1 O1 C1 33.9(9) . . . . ? O4 Mg1 O1 C1 -19(3) . . . . ? O6 Mg1 O1 C1 123.5(8) . . . . ? O5 Mg1 O1 C1 -162.0(9) . . . . ? Mg1 O1 C1 C2 148.6(6) . . . . ? Mg1 O1 C1 As1 -31.0(11) . . . . ? C8 As1 C1 O1 3.9(7) . . . . ? C8 As1 C1 C2 -175.7(6) . . . . ? O3 Mg1 O2 C8 67.2(7) . . . . ? O4 Mg1 O2 C8 154.6(7) . . . . ? O1 Mg1 O2 C8 -18.7(7) . . . . ? O6 Mg1 O2 C8 -114.9(7) . . . . ? O5 Mg1 O2 C8 -104.5(13) . . . . ? O1 C1 C2 C7 161.7(7) . . . . ? As1 C1 C2 C7 -18.6(10) . . . . ? O1 C1 C2 C3 -18.2(11) . . . . ? As1 C1 C2 C3 161.5(6) . . . . ? O2 Mg1 O3 C15 66.8(8) . . . . ? O4 Mg1 O3 C15 -19.1(8) . . . . ? O1 Mg1 O3 C15 154.1(7) . . . . ? O6 Mg1 O3 C15 -105.4(14) . . . . ? O5 Mg1 O3 C15 -115.4(8) . . . . ? C7 C2 C3 C4 1.6(13) . . . . ? C1 C2 C3 C4 -178.5(8) . . . . ? O3 Mg1 O4 C22 33.5(9) . . . . ? O2 Mg1 O4 C22 -72.5(9) . . . . ? O1 Mg1 O4 C22 -20(3) . . . . ? O6 Mg1 O4 C22 -162.3(9) . . . . ? O5 Mg1 O4 C22 123.2(8) . . . . ? C2 C3 C4 C5 -1.0(15) . . . . ? O3 Mg1 O5 C30 174.3(9) . . . . ? O2 Mg1 O5 C30 -13.7(17) . . . . ? O4 Mg1 O5 C30 85.9(9) . . . . ? O1 Mg1 O5 C30 -99.2(9) . . . . ? O6 Mg1 O5 C30 -2.9(9) . . . . ? O3 Mg1 O5 C29 -2.1(8) . . . . ? O2 Mg1 O5 C29 169.9(11) . . . . ? O4 Mg1 O5 C29 -90.5(8) . . . . ? O1 Mg1 O5 C29 84.4(8) . . . . ? O6 Mg1 O5 C29 -179.2(8) . . . . ? C3 C4 C5 C6 -0.9(16) . . . . ? O3 Mg1 O6 C31 -13.7(17) . . . . ? O2 Mg1 O6 C31 173.8(9) . . . . ? O4 Mg1 O6 C31 -99.7(9) . . . . ? O1 Mg1 O6 C31 85.5(9) . . . . ? O5 Mg1 O6 C31 -3.3(9) . . . . ? O3 Mg1 O6 C32 169.5(11) . . . . ? O2 Mg1 O6 C32 -3.0(8) . . . . ? O4 Mg1 O6 C32 83.5(8) . . . . ? O1 Mg1 O6 C32 -91.3(8) . . . . ? O5 Mg1 O6 C32 180.0(8) . . . . ? C4 C5 C6 C7 2.2(16) . . . . ? C5 C6 C7 C2 -1.7(15) . . . . ? C3 C2 C7 C6 -0.2(13) . . . . ? C1 C2 C7 C6 179.9(8) . . . . ? Mg1 O2 C8 C9 -175.0(5) . . . . ? Mg1 O2 C8 As1 1.6(10) . . . . ? C1 As1 C8 O2 10.4(7) . . . . ? C1 As1 C8 C9 -173.0(5) . . . . ? O2 C8 C9 C10 18.9(10) . . . . ? As1 C8 C9 C10 -158.1(6) . . . . ? O2 C8 C9 C14 -161.7(7) . . . . ? As1 C8 C9 C14 21.4(10) . . . . ? C14 C9 C10 C11 -1.0(12) . . . . ? C8 C9 C10 C11 178.5(7) . . . . ? C9 C10 C11 C12 -1.0(12) . . . . ? C10 C11 C12 C13 2.7(13) . . . . ? C11 C12 C13 C14 -2.4(15) . . . . ? C12 C13 C14 C9 0.3(14) . . . . ? C10 C9 C14 C13 1.3(13) . . . . ? C8 C9 C14 C13 -178.2(8) . . . . ? Mg1 O3 C15 C16 -175.4(5) . . . . ? Mg1 O3 C15 As2 2.6(11) . . . . ? C22 As2 C15 O3 9.5(7) . . . . ? C22 As2 C15 C16 -172.5(6) . . . . ? O3 C15 C16 C17 19.5(11) . . . . ? As2 C15 C16 C17 -158.8(6) . . . . ? O3 C15 C16 C21 -160.8(8) . . . . ? As2 C15 C16 C21 21.0(10) . . . . ? C21 C16 C17 C18 -1.5(13) . . . . ? C15 C16 C17 C18 178.3(7) . . . . ? C16 C17 C18 C19 -1.5(12) . . . . ? C17 C18 C19 C20 3.7(13) . . . . ? C18 C19 C20 C21 -2.7(14) . . . . ? C19 C20 C21 C16 -0.4(14) . . . . ? C17 C16 C21 C20 2.5(13) . . . . ? C15 C16 C21 C20 -177.3(8) . . . . ? Mg1 O4 C22 C23 149.1(6) . . . . ? Mg1 O4 C22 As2 -30.8(12) . . . . ? C15 As2 C22 O4 4.4(8) . . . . ? C15 As2 C22 C23 -175.5(6) . . . . ? O4 C22 C23 C24 -19.1(11) . . . . ? As2 C22 C23 C24 160.8(7) . . . . ? O4 C22 C23 C28 163.0(7) . . . . ? As2 C22 C23 C28 -17.1(10) . . . . ? C28 C23 C24 C25 -0.1(14) . . . . ? C22 C23 C24 C25 -178.1(9) . . . . ? C23 C24 C25 C26 -0.4(16) . . . . ? C24 C25 C26 C27 -1.0(17) . . . . ? C25 C26 C27 C28 2.9(17) . . . . ? C26 C27 C28 C23 -3.4(16) . . . . ? C24 C23 C28 C27 2.0(14) . . . . ? C22 C23 C28 C27 179.9(9) . . . . ? C29 O5 C30 C31 -175.0(11) . . . . ? Mg1 O5 C30 C31 8.2(16) . . . . ? C32 O6 C31 C30 -174.4(11) . . . . ? Mg1 O6 C31 C30 8.5(16) . . . . ? O5 C30 C31 O6 -10.7(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.927 _refine_diff_density_min -1.188 _refine_diff_density_rms 0.104 data_compound_11 _database_code_CSD 195261 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H78 Na O6 Sb' _chemical_formula_weight 871.82 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' 'Sb' 'Sb' -0.5866 1.5461 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 27.506(3) _cell_length_b 10.440(2) _cell_length_c 19.595(3) _cell_angle_alpha 90.00 _cell_angle_beta 121.486(12) _cell_angle_gamma 90.00 _cell_volume 4798.5(13) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 0.626 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_T_min 0.70 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _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 4690 _diffrn_reflns_av_R_equivalents 0.0734 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.24 _reflns_number_total 4585 _reflns_number_gt 4483 _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^)+(0.0950P)^2^+67.7519P] 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 SHELXL _refine_ls_extinction_coef 0.00000(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(6) _refine_ls_number_reflns 4585 _refine_ls_number_parameters 512 _refine_ls_number_restraints 61 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.1943 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.092 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sb1 Sb 0.5000 0.43511(6) 0.5000 0.0206(3) Uani 1 2 d S . . Sb2 Sb 0.5000 0.49604(11) 0.0000 0.0577(5) Uani 1 2 d S . . Na1 Na 0.5000 0.0168(9) 0.5000 0.048(3) Uani 1 2 d S . . Na2 Na 0.5000 0.9174(8) 0.0000 0.028(2) Uani 1 2 d S . . O1 O 0.4418(3) 0.1805(9) 0.4905(4) 0.0170(16) Uani 1 1 d . . . O2 O 0.4277(5) -0.055(2) 0.3706(7) 0.074(3) Uani 1 1 d U . . O3 O 0.5589(4) -0.1325(14) 0.4752(7) 0.062(3) Uani 1 1 d U . . O4 O 0.5580(8) 0.7496(15) 0.0127(11) 0.090(6) Uani 1 1 d . . . O5 O 0.5761(3) 0.9936(18) 0.1299(4) 0.057(4) Uani 1 1 d . . . O6 O 0.4440(5) 1.0822(12) 0.0093(7) 0.068(4) Uani 1 1 d U . . C1 C 0.4401(4) 0.2969(12) 0.4956(5) 0.013(2) Uani 1 1 d U . . C2 C 0.3910(4) 0.3622(11) 0.5000(5) 0.015(2) Uani 1 1 d . . . C3 C 0.3952(4) 0.3712(14) 0.5753(6) 0.023(2) Uani 1 1 d . . . C4 C 0.3613(4) 0.4620(12) 0.5852(5) 0.020(4) Uani 1 1 d . . . H4 H 0.3640 0.4697 0.6344 0.024 Uiso 1 1 calc R . . C5 C 0.3232(4) 0.5416(12) 0.5203(6) 0.022(2) Uani 1 1 d . . . C6 C 0.3161(4) 0.5207(13) 0.4487(6) 0.021(3) Uani 1 1 d . . . H6 H 0.2882 0.5673 0.4055 0.026 Uiso 1 1 calc R . . C7 C 0.3484(3) 0.432(2) 0.4343(4) 0.0174(19) Uani 1 1 d . . . C8 C 0.4312(5) 0.2778(14) 0.6455(6) 0.026(3) Uani 1 1 d . . . C9 C 0.4211(6) 0.2998(17) 0.7154(6) 0.039(3) Uani 1 1 d . . . H9A H 0.4397 0.2334 0.7546 0.058 Uiso 1 1 calc R . . H9B H 0.3809 0.2980 0.6952 0.058 Uiso 1 1 calc R . . H9C H 0.4364 0.3815 0.7396 0.058 Uiso 1 1 calc R . . C10 C 0.4959(4) 0.2912(19) 0.6794(7) 0.040(4) Uani 1 1 d . . . H10A H 0.5061 0.3802 0.6867 0.060 Uiso 1 1 calc R . . H10B H 0.5050 0.2539 0.6426 0.060 Uiso 1 1 calc R . . H10C H 0.5167 0.2478 0.7299 0.060 Uiso 1 1 calc R . . C11 C 0.4134(6) 0.1389(14) 0.6190(8) 0.032(3) Uani 1 1 d . . . H11A H 0.4086 0.1260 0.5673 0.049 Uiso 1 1 calc R . . H11B H 0.3781 0.1216 0.6161 0.049 Uiso 1 1 calc R . . H11C H 0.4423 0.0821 0.6570 0.049 Uiso 1 1 calc R . . C12 C 0.2878(4) 0.6414(11) 0.5366(7) 0.021(2) Uani 1 1 d . . . C13 C 0.3286(5) 0.7342(16) 0.6014(8) 0.037(3) Uani 1 1 d . . . H13A H 0.3514 0.6886 0.6507 0.056 Uiso 1 1 calc R . . H13B H 0.3071 0.7996 0.6086 0.056 Uiso 1 1 calc R . . H13C H 0.3529 0.7730 0.5856 0.056 Uiso 1 1 calc R . . C14 C 0.2513(5) 0.5760(16) 0.5623(7) 0.028(3) Uani 1 1 d . . . H14A H 0.2752 0.5339 0.6126 0.041 Uiso 1 1 calc R . . H14B H 0.2273 0.5139 0.5227 0.041 Uiso 1 1 calc R . . H14C H 0.2280 0.6384 0.5679 0.041 Uiso 1 1 calc R . . C15 C 0.2498(5) 0.7214(16) 0.4601(7) 0.032(3) Uani 1 1 d . . . H15A H 0.2731 0.7606 0.4428 0.048 Uiso 1 1 calc R . . H15B H 0.2305 0.7867 0.4715 0.048 Uiso 1 1 calc R . . H15C H 0.2222 0.6664 0.4185 0.048 Uiso 1 1 calc R . . C16 C 0.3292(4) 0.4149(16) 0.3444(5) 0.023(4) Uani 1 1 d . . . C17 C 0.2646(4) 0.3876(16) 0.2973(6) 0.032(3) Uani 1 1 d . . . H17A H 0.2448 0.4594 0.3023 0.047 Uiso 1 1 calc R . . H17B H 0.2571 0.3124 0.3186 0.047 Uiso 1 1 calc R . . H17C H 0.2516 0.3742 0.2419 0.047 Uiso 1 1 calc R . . C18 C 0.3412(6) 0.5371(18) 0.3110(9) 0.033(4) Uani 1 1 d . . . H18A H 0.3276 0.6107 0.3254 0.050 Uiso 1 1 calc R . . H18B H 0.3220 0.5313 0.2537 0.050 Uiso 1 1 calc R . . H18C H 0.3815 0.5452 0.3330 0.050 Uiso 1 1 calc R . . C19 C 0.3562(6) 0.3019(19) 0.3265(8) 0.033(4) Uani 1 1 d . . . H19A H 0.3511 0.2252 0.3490 0.049 Uiso 1 1 calc R . . H19B H 0.3962 0.3177 0.3495 0.049 Uiso 1 1 calc R . . H19C H 0.3382 0.2919 0.2696 0.049 Uiso 1 1 calc R . . C20 C 0.4081(8) -0.008(3) 0.3003(15) 0.089(6) Uani 1 1 d U . . H20A H 0.4370 -0.0116 0.2869 0.133 Uiso 1 1 calc R . . H20B H 0.3971 0.0797 0.2994 0.133 Uiso 1 1 calc R . . H20C H 0.3755 -0.0566 0.2621 0.133 Uiso 1 1 calc R . . C21 C 0.3804(8) -0.113(2) 0.3834(14) 0.083(6) Uani 1 1 d U . . H21A H 0.3603 -0.0460 0.3929 0.100 Uiso 1 1 calc R . . H21B H 0.3530 -0.1618 0.3367 0.100 Uiso 1 1 calc R . . C22 C 0.4124(11) -0.202(3) 0.4579(13) 0.090(7) Uani 1 1 d U . . H22A H 0.3852 -0.2570 0.4611 0.108 Uiso 1 1 calc R . . H22B H 0.4388 -0.2566 0.4524 0.108 Uiso 1 1 calc R . . C23 C 0.5353(9) -0.219(3) 0.4171(15) 0.088(7) Uani 1 1 d U . . H23A H 0.5102 -0.1773 0.3671 0.132 Uiso 1 1 calc R . . H23B H 0.5139 -0.2792 0.4284 0.132 Uiso 1 1 calc R . . H23C H 0.5646 -0.2637 0.4139 0.132 Uiso 1 1 calc R . . C24 C 0.5616(9) 0.6341(18) 0.0083(12) 0.057(5) Uani 1 1 d . . . C25 C 0.6091(7) 0.5687(16) 0.0041(11) 0.056(5) Uani 1 1 d . . . C26 C 0.6047(6) 0.5656(16) -0.0747(9) 0.044(4) Uani 1 1 d . . . C27 C 0.6392(7) 0.4737(17) -0.0797(10) 0.049(5) Uani 1 1 d . . . H27 H 0.6357 0.4649 -0.1293 0.058 Uiso 1 1 calc R . . C28 C 0.6763(7) 0.3973(14) -0.0227(9) 0.043(4) Uani 1 1 d . . . C29 C 0.6845(7) 0.4144(16) 0.0544(9) 0.046(5) Uani 1 1 d . . . H29 H 0.7119 0.3659 0.0970 0.055 Uiso 1 1 calc R . . C30 C 0.6518(6) 0.504(2) 0.0681(10) 0.046(4) Uani 1 1 d . . . C31 C 0.5681(8) 0.657(2) -0.1454(12) 0.060(5) Uani 1 1 d . . . C32 C 0.5871(8) 0.797(2) -0.1199(11) 0.058(5) Uani 1 1 d . . . H32A H 0.6276 0.8031 -0.0965 0.087 Uiso 1 1 calc R . . H32B H 0.5775 0.8227 -0.0815 0.087 Uiso 1 1 calc R . . H32C H 0.5682 0.8516 -0.1660 0.087 Uiso 1 1 calc R . . C33 C 0.5049(8) 0.640(2) -0.1762(15) 0.087(7) Uani 1 1 d . . . H33A H 0.4948 0.5515 -0.1880 0.131 Uiso 1 1 calc R . . H33B H 0.4827 0.6902 -0.2238 0.131 Uiso 1 1 calc R . . H33C H 0.4972 0.6682 -0.1360 0.131 Uiso 1 1 calc R . . C34 C 0.5763(8) 0.635(2) -0.2142(11) 0.071(5) Uani 1 1 d . . . H34A H 0.6136 0.6632 -0.2001 0.106 Uiso 1 1 calc R . . H34B H 0.5480 0.6817 -0.2600 0.106 Uiso 1 1 calc R . . H34C H 0.5725 0.5450 -0.2266 0.106 Uiso 1 1 calc R . . C35 C 0.7114(9) 0.295(2) -0.0331(11) 0.062(5) Uani 1 1 d . . . C36 C 0.6699(8) 0.201(2) -0.1023(13) 0.079(6) Uani 1 1 d U . . H36A H 0.6552 0.1385 -0.0816 0.119 Uiso 1 1 calc R . . H36B H 0.6904 0.1578 -0.1231 0.119 Uiso 1 1 calc R . . H36C H 0.6389 0.2486 -0.1443 0.119 Uiso 1 1 calc R . . C37 C 0.7489(9) 0.365(2) -0.0625(13) 0.073(6) Uani 1 1 d . . . H37A H 0.7769 0.4183 -0.0203 0.109 Uiso 1 1 calc R . . H37B H 0.7246 0.4169 -0.1085 0.109 Uiso 1 1 calc R . . H37C H 0.7677 0.3021 -0.0765 0.109 Uiso 1 1 calc R . . C38 C 0.7523(10) 0.224(2) 0.0403(14) 0.081(7) Uani 1 1 d . . . H38A H 0.7784 0.2835 0.0800 0.122 Uiso 1 1 calc R . . H38B H 0.7732 0.1641 0.0281 0.122 Uiso 1 1 calc R . . H38C H 0.7320 0.1790 0.0604 0.122 Uiso 1 1 calc R . . C39 C 0.6695(7) 0.5222(17) 0.1535(11) 0.053(5) Uani 1 1 d . . . C40 C 0.7364(7) 0.543(2) 0.2049(10) 0.061(5) Uani 1 1 d . . . H40A H 0.7457 0.6232 0.1901 0.091 Uiso 1 1 calc R . . H40B H 0.7550 0.4745 0.1950 0.091 Uiso 1 1 calc R . . H40C H 0.7489 0.5451 0.2607 0.091 Uiso 1 1 calc R . . C41 C 0.6576(10) 0.402(2) 0.1847(12) 0.067(7) Uani 1 1 d . . . H41A H 0.6816 0.3342 0.1859 0.101 Uiso 1 1 calc R . . H41B H 0.6184 0.3783 0.1504 0.101 Uiso 1 1 calc R . . H41C H 0.6653 0.4169 0.2379 0.101 Uiso 1 1 calc R . . C42 C 0.6429(9) 0.636(2) 0.1711(13) 0.068(6) Uani 1 1 d . . . H42A H 0.6436 0.7098 0.1423 0.102 Uiso 1 1 calc R . . H42B H 0.6643 0.6538 0.2275 0.102 Uiso 1 1 calc R . . H42C H 0.6042 0.6162 0.1546 0.102 Uiso 1 1 calc R . . C43 C 0.5914(6) 0.931(2) 0.2068(6) 0.043(3) Uani 1 1 d . . . H43A H 0.6177 0.8623 0.2176 0.065 Uiso 1 1 calc R . . H43B H 0.5576 0.8975 0.2031 0.065 Uiso 1 1 calc R . . H43C H 0.6088 0.9927 0.2493 0.065 Uiso 1 1 calc R . . C44 C 0.6183(5) 1.0464(16) 0.1278(8) 0.047(4) Uani 1 1 d . . . H44A H 0.6463 0.9807 0.1382 0.056 Uiso 1 1 calc R . . H44B H 0.6364 1.1085 0.1709 0.056 Uiso 1 1 calc R . . C45 C 0.6032(6) 1.109(2) 0.0549(9) 0.062(4) Uani 1 1 d U . . H45A H 0.6034 1.2000 0.0639 0.075 Uiso 1 1 calc R . . H45B H 0.6335 1.0920 0.0446 0.075 Uiso 1 1 calc R . . C46 C 0.4614(6) 1.1539(15) 0.0823(8) 0.046(4) Uani 1 1 d . . . H46A H 0.4970 1.1963 0.0995 0.069 Uiso 1 1 calc R . . H46B H 0.4660 1.0962 0.1234 0.069 Uiso 1 1 calc R . . H46C H 0.4328 1.2165 0.0722 0.069 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 Sb1 0.0137(4) 0.0134(5) 0.0343(4) 0.000 0.0122(3) 0.000 Sb2 0.0633(9) 0.0260(8) 0.1192(14) 0.000 0.0721(10) 0.000 Na1 0.006(3) 0.030(6) 0.087(5) 0.000 0.010(3) 0.000 Na2 0.057(4) 0.013(5) 0.023(2) 0.000 0.026(2) 0.000 O1 0.012(3) 0.015(4) 0.027(3) 0.000(3) 0.013(3) -0.002(3) O2 0.067(5) 0.073(7) 0.097(6) -0.033(7) 0.052(5) -0.026(7) O3 0.046(5) 0.059(6) 0.079(6) 0.011(5) 0.032(5) -0.021(5) O4 0.151(15) 0.031(8) 0.167(16) -0.013(9) 0.138(14) 0.002(9) O5 0.029(4) 0.116(11) 0.017(3) 0.007(5) 0.006(3) 0.001(6) O6 0.066(6) 0.042(6) 0.059(6) -0.028(5) 0.007(4) 0.033(5) C1 0.007(3) 0.019(4) 0.017(3) -0.001(3) 0.010(3) -0.001(3) C2 0.010(4) 0.016(6) 0.023(4) 0.005(4) 0.012(3) 0.004(4) C3 0.014(5) 0.025(6) 0.017(4) 0.000(5) -0.001(4) 0.001(5) C4 0.019(4) 0.023(11) 0.016(4) 0.003(4) 0.009(3) -0.003(4) C5 0.011(4) 0.019(7) 0.033(5) -0.002(4) 0.009(4) -0.001(4) C6 0.008(4) 0.023(8) 0.023(5) 0.005(4) 0.001(4) -0.001(4) C7 0.013(3) 0.019(5) 0.017(4) 0.006(7) 0.005(3) -0.006(8) C8 0.023(5) 0.032(8) 0.022(5) 0.012(5) 0.010(4) 0.012(5) C9 0.048(7) 0.053(9) 0.019(5) 0.010(6) 0.020(5) 0.017(7) C10 0.018(5) 0.063(11) 0.028(5) 0.009(6) 0.004(4) 0.003(6) C11 0.036(7) 0.026(8) 0.038(6) 0.017(5) 0.022(6) 0.005(6) C12 0.021(5) 0.006(6) 0.041(6) 0.001(4) 0.020(4) 0.005(4) C13 0.046(6) 0.026(7) 0.059(7) -0.020(6) 0.040(6) -0.009(6) C14 0.024(5) 0.024(7) 0.043(6) -0.001(6) 0.023(5) 0.002(5) C15 0.031(6) 0.025(8) 0.050(7) 0.012(6) 0.028(5) 0.019(6) C16 0.014(4) 0.038(12) 0.016(4) 0.002(5) 0.007(3) 0.001(5) C17 0.023(5) 0.044(8) 0.017(4) -0.003(4) 0.003(4) -0.002(5) C18 0.026(7) 0.039(11) 0.033(7) 0.008(6) 0.014(6) 0.001(7) C19 0.030(7) 0.053(11) 0.016(5) -0.003(6) 0.013(5) 0.014(7) C20 0.059(8) 0.057(9) 0.130(11) -0.007(9) 0.034(7) 0.005(8) C21 0.058(8) 0.056(9) 0.121(10) -0.001(8) 0.036(7) 0.000(7) C22 0.109(11) 0.069(10) 0.091(10) 0.005(8) 0.052(8) 0.024(8) C23 0.078(9) 0.082(12) 0.145(11) 0.006(8) 0.086(8) 0.005(8) C24 0.067(11) 0.027(8) 0.088(12) -0.014(8) 0.049(10) -0.007(7) C25 0.075(10) 0.021(8) 0.101(12) -0.042(8) 0.066(10) -0.028(8) C26 0.060(8) 0.027(8) 0.077(9) -0.012(7) 0.060(8) -0.014(7) C27 0.067(9) 0.031(13) 0.081(10) -0.024(7) 0.062(9) -0.015(7) C28 0.081(10) 0.017(8) 0.064(8) -0.005(6) 0.060(8) -0.004(6) C29 0.072(8) 0.024(12) 0.077(8) -0.015(7) 0.063(7) -0.007(7) C30 0.051(8) 0.030(9) 0.085(10) -0.024(9) 0.054(8) -0.009(9) C31 0.064(11) 0.046(11) 0.089(12) -0.020(9) 0.054(10) -0.009(9) C32 0.062(10) 0.052(12) 0.080(11) -0.012(9) 0.051(9) 0.000(9) C33 0.084(14) 0.049(14) 0.117(17) -0.010(12) 0.045(13) -0.010(11) C34 0.079(12) 0.061(14) 0.073(11) -0.011(10) 0.040(10) -0.009(11) C35 0.097(13) 0.047(11) 0.080(11) -0.011(9) 0.073(10) -0.003(10) C36 0.090(9) 0.054(10) 0.122(10) -0.036(8) 0.075(8) -0.008(7) C37 0.108(14) 0.048(12) 0.120(15) -0.004(12) 0.100(13) 0.002(12) C38 0.136(18) 0.027(10) 0.15(2) -0.009(12) 0.127(17) -0.002(11) C39 0.078(10) 0.026(10) 0.089(11) -0.016(8) 0.068(10) -0.016(8) C40 0.076(10) 0.052(11) 0.086(11) -0.021(9) 0.065(9) -0.012(9) C41 0.108(15) 0.050(16) 0.077(11) -0.020(8) 0.072(11) -0.032(10) C42 0.086(13) 0.049(13) 0.105(14) -0.039(11) 0.074(12) -0.030(11) C43 0.071(7) 0.033(7) 0.023(4) -0.007(7) 0.023(5) 0.013(9) C44 0.025(6) 0.031(8) 0.047(7) 0.009(6) -0.007(5) -0.007(5) C45 0.041(6) 0.096(10) 0.055(7) 0.009(7) 0.029(5) -0.015(7) C46 0.058(8) 0.027(7) 0.046(7) -0.022(6) 0.023(6) 0.002(6) _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 Sb1 C1 2.156(11) . ? Sb1 C1 2.156(11) 2_656 ? Sb2 C24 2.17(2) . ? Sb2 C24 2.17(2) 2_655 ? Na1 O1 2.282(12) 2_656 ? Na1 O1 2.282(12) . ? Na1 O2 2.381(12) . ? Na1 O2 2.381(12) 2_656 ? Na1 O3 2.474(16) . ? Na1 O3 2.474(16) 2_656 ? Na1 C22 3.10(3) . ? Na1 C22 3.10(3) 2_656 ? Na2 O4 2.294(18) 2_655 ? Na2 O4 2.294(18) . ? Na2 O6 2.379(12) 2_655 ? Na2 O6 2.379(12) . ? Na2 O5 2.434(10) . ? Na2 O5 2.434(10) 2_655 ? O1 C1 1.222(16) . ? O2 C20 1.29(3) . ? O2 C21 1.57(3) . ? O3 C23 1.33(3) . ? O3 C22 1.34(3) 2_656 ? O4 C24 1.22(3) . ? O5 C44 1.305(18) . ? O5 C43 1.488(18) . ? O6 C45 1.280(19) 2_655 ? O6 C46 1.456(16) . ? C1 C2 1.557(13) . ? C2 C7 1.410(16) . ? C2 C3 1.422(14) . ? C3 C4 1.412(17) . ? C3 C8 1.550(15) . ? C4 C5 1.421(15) . ? C5 C6 1.329(15) . ? C5 C12 1.568(15) . ? C6 C7 1.41(2) . ? C7 C16 1.565(12) . ? C8 C11 1.53(2) . ? C8 C10 1.546(15) . ? C8 C9 1.550(15) . ? C12 C14 1.503(16) . ? C12 C13 1.524(17) . ? C12 C15 1.549(16) . ? C16 C19 1.53(2) . ? C16 C17 1.543(13) . ? C16 C18 1.55(2) . ? C21 C22 1.56(3) . ? C22 O3 1.34(3) 2_656 ? C24 C25 1.51(3) . ? C25 C30 1.37(3) . ? C25 C26 1.49(2) . ? C26 C27 1.39(2) . ? C26 C31 1.55(3) . ? C27 C28 1.32(2) . ? C28 C29 1.418(18) . ? C28 C35 1.53(2) . ? C29 C30 1.41(2) . ? C30 C39 1.49(2) . ? C31 C34 1.50(2) . ? C31 C33 1.52(3) . ? C31 C32 1.54(3) . ? C35 C38 1.48(3) . ? C35 C36 1.58(3) . ? C35 C37 1.60(2) . ? C39 C41 1.50(2) . ? C39 C42 1.53(3) . ? C39 C40 1.59(2) . ? C44 C45 1.42(2) . ? C45 O6 1.280(19) 2_655 ? 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 C1 Sb1 C1 96.0(6) . 2_656 ? C24 Sb2 C24 96.5(11) . 2_655 ? O1 Na1 O1 83.0(5) 2_656 . ? O1 Na1 O2 118.8(5) 2_656 . ? O1 Na1 O2 89.3(5) . . ? O1 Na1 O2 89.3(5) 2_656 2_656 ? O1 Na1 O2 118.8(5) . 2_656 ? O2 Na1 O2 143.5(12) . 2_656 ? O1 Na1 O3 89.1(3) 2_656 . ? O1 Na1 O3 163.7(4) . . ? O2 Na1 O3 82.0(5) . . ? O2 Na1 O3 75.2(5) 2_656 . ? O1 Na1 O3 163.7(4) 2_656 2_656 ? O1 Na1 O3 89.1(3) . 2_656 ? O2 Na1 O3 75.2(5) . 2_656 ? O2 Na1 O3 82.0(5) 2_656 2_656 ? O3 Na1 O3 101.9(6) . 2_656 ? O1 Na1 C22 170.9(4) 2_656 . ? O1 Na1 C22 96.7(5) . . ? O2 Na1 C22 52.1(6) . . ? O2 Na1 C22 98.8(7) 2_656 . ? O3 Na1 C22 88.9(6) . . ? O3 Na1 C22 24.6(5) 2_656 . ? O1 Na1 C22 96.7(5) 2_656 2_656 ? O1 Na1 C22 170.9(4) . 2_656 ? O2 Na1 C22 98.8(7) . 2_656 ? O2 Na1 C22 52.1(6) 2_656 2_656 ? O3 Na1 C22 24.6(5) . 2_656 ? O3 Na1 C22 88.9(6) 2_656 2_656 ? C22 Na1 C22 85.1(9) . 2_656 ? O4 Na2 O4 80.4(9) 2_655 . ? O4 Na2 O6 170.2(5) 2_655 2_655 ? O4 Na2 O6 96.8(5) . 2_655 ? O4 Na2 O6 96.8(5) 2_655 . ? O4 Na2 O6 170.2(5) . . ? O6 Na2 O6 87.4(8) 2_655 . ? O4 Na2 O5 122.2(6) 2_655 . ? O4 Na2 O5 88.1(6) . . ? O6 Na2 O5 66.8(4) 2_655 . ? O6 Na2 O5 85.5(5) . . ? O4 Na2 O5 88.1(6) 2_655 2_655 ? O4 Na2 O5 122.2(6) . 2_655 ? O6 Na2 O5 85.5(5) 2_655 2_655 ? O6 Na2 O5 66.8(4) . 2_655 ? O5 Na2 O5 141.9(9) . 2_655 ? C1 O1 Na1 142.4(8) . . ? C20 O2 C21 113.5(15) . . ? C20 O2 Na1 132.2(18) . . ? C21 O2 Na1 104.6(10) . . ? C23 O3 C22 104.0(19) . 2_656 ? C23 O3 Na1 121.3(11) . . ? C22 O3 Na1 105.1(14) 2_656 . ? C24 O4 Na2 145.8(18) . . ? C44 O5 C43 115.5(10) . . ? C44 O5 Na2 113.6(8) . . ? C43 O5 Na2 123.3(12) . . ? C45 O6 C46 120.0(13) 2_655 . ? C45 O6 Na2 116.4(10) 2_655 . ? C46 O6 Na2 123.6(9) . . ? O1 C1 C2 120.7(10) . . ? O1 C1 Sb1 127.5(8) . . ? C2 C1 Sb1 111.9(8) . . ? C7 C2 C3 119.4(10) . . ? C7 C2 C1 120.6(8) . . ? C3 C2 C1 118.9(8) . . ? C4 C3 C2 119.1(10) . . ? C4 C3 C8 117.5(9) . . ? C2 C3 C8 123.2(11) . . ? C3 C4 C5 120.1(9) . . ? C6 C5 C4 118.8(11) . . ? C6 C5 C12 124.1(10) . . ? C4 C5 C12 116.9(9) . . ? C5 C6 C7 124.0(10) . . ? C6 C7 C2 117.9(9) . . ? C6 C7 C16 115.1(10) . . ? C2 C7 C16 126.8(14) . . ? C11 C8 C10 108.9(12) . . ? C11 C8 C3 110.6(9) . . ? C10 C8 C3 112.6(11) . . ? C11 C8 C9 105.4(12) . . ? C10 C8 C9 107.7(10) . . ? C3 C8 C9 111.4(10) . . ? C14 C12 C13 109.9(10) . . ? C14 C12 C15 109.7(10) . . ? C13 C12 C15 107.1(11) . . ? C14 C12 C5 111.2(10) . . ? C13 C12 C5 109.1(9) . . ? C15 C12 C5 109.7(9) . . ? C19 C16 C17 105.5(12) . . ? C19 C16 C18 107.7(10) . . ? C17 C16 C18 109.5(10) . . ? C19 C16 C7 115.4(12) . . ? C17 C16 C7 107.4(8) . . ? C18 C16 C7 111.1(14) . . ? C22 C21 O2 105.7(16) . . ? O3 C22 C21 110(2) 2_656 . ? O3 C22 Na1 50.3(12) 2_656 . ? C21 C22 Na1 77.9(14) . . ? O4 C24 C25 124(2) . . ? O4 C24 Sb2 125.2(18) . . ? C25 C24 Sb2 111.0(11) . . ? C30 C25 C26 120.4(14) . . ? C30 C25 C24 121.7(15) . . ? C26 C25 C24 117.5(17) . . ? C27 C26 C25 113.6(15) . . ? C27 C26 C31 121.0(13) . . ? C25 C26 C31 125.3(15) . . ? C28 C27 C26 127.8(14) . . ? C27 C28 C29 116.7(14) . . ? C27 C28 C35 125.1(13) . . ? C29 C28 C35 118.2(15) . . ? C30 C29 C28 121.4(16) . . ? C25 C30 C29 118.7(14) . . ? C25 C30 C39 125.8(15) . . ? C29 C30 C39 115.5(16) . . ? C34 C31 C33 107.6(17) . . ? C34 C31 C32 104.7(18) . . ? C33 C31 C32 111.4(17) . . ? C34 C31 C26 112.0(16) . . ? C33 C31 C26 110.9(17) . . ? C32 C31 C26 110.1(15) . . ? C38 C35 C28 115.7(14) . . ? C38 C35 C36 111.5(19) . . ? C28 C35 C36 109.1(15) . . ? C38 C35 C37 105.9(17) . . ? C28 C35 C37 107.4(16) . . ? C36 C35 C37 106.8(15) . . ? C30 C39 C41 109.6(15) . . ? C30 C39 C42 116.1(18) . . ? C41 C39 C42 109.1(13) . . ? C30 C39 C40 108.7(12) . . ? C41 C39 C40 106.5(17) . . ? C42 C39 C40 106.4(14) . . ? O5 C44 C45 115.2(10) . . ? O6 C45 C44 120.3(15) 2_655 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 O1 C1 -7.2(10) 2_656 . . . ? O2 Na1 O1 C1 -126.3(13) . . . . ? O2 Na1 O1 C1 78.1(13) 2_656 . . . ? O3 Na1 O1 C1 -69(2) . . . . ? O3 Na1 O1 C1 158.5(12) 2_656 . . . ? C22 Na1 O1 C1 -178.0(13) . . . . ? C22 Na1 O1 C1 81(4) 2_656 . . . ? O1 Na1 O2 C20 -11(2) 2_656 . . . ? O1 Na1 O2 C20 70(2) . . . . ? O2 Na1 O2 C20 -147(2) 2_656 . . . ? O3 Na1 O2 C20 -96(2) . . . . ? O3 Na1 O2 C20 160(2) 2_656 . . . ? C22 Na1 O2 C20 169(2) . . . . ? C22 Na1 O2 C20 -114(2) 2_656 . . . ? O1 Na1 O2 C21 -153.8(12) 2_656 . . . ? O1 Na1 O2 C21 -72.1(13) . . . . ? O2 Na1 O2 C21 70.3(13) 2_656 . . . ? O3 Na1 O2 C21 121.7(14) . . . . ? O3 Na1 O2 C21 17.1(13) 2_656 . . . ? C22 Na1 O2 C21 26.9(13) . . . . ? C22 Na1 O2 C21 103.6(14) 2_656 . . . ? O1 Na1 O3 C23 -134.4(15) 2_656 . . . ? O1 Na1 O3 C23 -74(2) . . . . ? O2 Na1 O3 C23 -15.2(15) . . . . ? O2 Na1 O3 C23 136.1(16) 2_656 . . . ? O3 Na1 O3 C23 57.7(14) 2_656 . . . ? C22 Na1 O3 C23 36.7(15) . . . . ? C22 Na1 O3 C23 117(2) 2_656 . . . ? O1 Na1 O3 C22 108.3(12) 2_656 . . 2_656 ? O1 Na1 O3 C22 169.0(16) . . . 2_656 ? O2 Na1 O3 C22 -132.5(13) . . . 2_656 ? O2 Na1 O3 C22 18.8(12) 2_656 . . 2_656 ? O3 Na1 O3 C22 -59.5(11) 2_656 . . 2_656 ? C22 Na1 O3 C22 -80.6(14) . . . 2_656 ? O4 Na2 O4 C24 8(3) 2_655 . . . ? O6 Na2 O4 C24 -163(3) 2_655 . . . ? O6 Na2 O4 C24 82(6) . . . . ? O5 Na2 O4 C24 131(3) . . . . ? O5 Na2 O4 C24 -74(3) 2_655 . . . ? O4 Na2 O5 C44 152.2(12) 2_655 . . . ? O4 Na2 O5 C44 74.8(13) . . . . ? O6 Na2 O5 C44 -23.5(12) 2_655 . . . ? O6 Na2 O5 C44 -112.5(13) . . . . ? O5 Na2 O5 C44 -70.3(13) 2_655 . . . ? O4 Na2 O5 C43 4.1(14) 2_655 . . . ? O4 Na2 O5 C43 -73.3(12) . . . . ? O6 Na2 O5 C43 -171.6(13) 2_655 . . . ? O6 Na2 O5 C43 99.3(12) . . . . ? O5 Na2 O5 C43 141.6(11) 2_655 . . . ? O4 Na2 O6 C45 -71.2(17) 2_655 . . 2_655 ? O4 Na2 O6 C45 -144(4) . . . 2_655 ? O6 Na2 O6 C45 99.9(17) 2_655 . . 2_655 ? O5 Na2 O6 C45 166.8(16) . . . 2_655 ? O5 Na2 O6 C45 13.7(15) 2_655 . . 2_655 ? O4 Na2 O6 C46 110.3(14) 2_655 . . . ? O4 Na2 O6 C46 37(5) . . . . ? O6 Na2 O6 C46 -78.6(13) 2_655 . . . ? O5 Na2 O6 C46 -11.6(14) . . . . ? O5 Na2 O6 C46 -164.8(15) 2_655 . . . ? Na1 O1 C1 C2 -167.4(7) . . . . ? Na1 O1 C1 Sb1 12.3(17) . . . . ? C1 Sb1 C1 O1 -5.2(7) 2_656 . . . ? C1 Sb1 C1 C2 174.5(8) 2_656 . . . ? O1 C1 C2 C7 -108.2(15) . . . . ? Sb1 C1 C2 C7 72.0(13) . . . . ? O1 C1 C2 C3 83.6(14) . . . . ? Sb1 C1 C2 C3 -96.2(11) . . . . ? C7 C2 C3 C4 -7.8(18) . . . . ? C1 C2 C3 C4 160.5(11) . . . . ? C7 C2 C3 C8 166.5(13) . . . . ? C1 C2 C3 C8 -25.1(17) . . . . ? C2 C3 C4 C5 0.9(17) . . . . ? C8 C3 C4 C5 -173.8(10) . . . . ? C3 C4 C5 C6 6.2(17) . . . . ? C3 C4 C5 C12 -179.1(10) . . . . ? C4 C5 C6 C7 -6.6(19) . . . . ? C12 C5 C6 C7 179.1(12) . . . . ? C5 C6 C7 C2 0(2) . . . . ? C5 C6 C7 C16 174.9(12) . . . . ? C3 C2 C7 C6 8(2) . . . . ? C1 C2 C7 C6 -160.5(11) . . . . ? C3 C2 C7 C16 -167.1(12) . . . . ? C1 C2 C7 C16 25(2) . . . . ? C4 C3 C8 C11 119.0(13) . . . . ? C2 C3 C8 C11 -55.4(16) . . . . ? C4 C3 C8 C10 -118.9(13) . . . . ? C2 C3 C8 C10 66.6(16) . . . . ? C4 C3 C8 C9 2.1(16) . . . . ? C2 C3 C8 C9 -172.3(12) . . . . ? C6 C5 C12 C14 114.6(13) . . . . ? C4 C5 C12 C14 -59.7(13) . . . . ? C6 C5 C12 C13 -124.1(12) . . . . ? C4 C5 C12 C13 61.6(13) . . . . ? C6 C5 C12 C15 -6.9(16) . . . . ? C4 C5 C12 C15 178.7(10) . . . . ? C6 C7 C16 C19 -168.9(14) . . . . ? C2 C7 C16 C19 6(2) . . . . ? C6 C7 C16 C17 -51.6(19) . . . . ? C2 C7 C16 C17 123.3(14) . . . . ? C6 C7 C16 C18 68.2(14) . . . . ? C2 C7 C16 C18 -117.0(17) . . . . ? C20 O2 C21 C22 162(2) . . . . ? Na1 O2 C21 C22 -47.6(19) . . . . ? O2 C21 C22 O3 73(2) . . . 2_656 ? O2 C21 C22 Na1 34.1(13) . . . . ? O1 Na1 C22 O3 -160(3) 2_656 . . 2_656 ? O1 Na1 C22 O3 -72.9(11) . . . 2_656 ? O2 Na1 C22 O3 -156.8(15) . . . 2_656 ? O2 Na1 C22 O3 47.7(12) 2_656 . . 2_656 ? O3 Na1 C22 O3 122.5(11) . . . 2_656 ? C22 Na1 C22 O3 98.1(12) 2_656 . . 2_656 ? O1 Na1 C22 C21 -30(4) 2_656 . . . ? O1 Na1 C22 C21 57.0(12) . . . . ? O2 Na1 C22 C21 -26.8(12) . . . . ? O2 Na1 C22 C21 177.6(12) 2_656 . . . ? O3 Na1 C22 C21 -107.6(13) . . . . ? O3 Na1 C22 C21 129.9(19) 2_656 . . . ? C22 Na1 C22 C21 -132.0(15) 2_656 . . . ? Na2 O4 C24 C25 164.4(17) . . . . ? Na2 O4 C24 Sb2 -13(4) . . . . ? C24 Sb2 C24 O4 5.0(17) 2_655 . . . ? C24 Sb2 C24 C25 -172.5(17) 2_655 . . . ? O4 C24 C25 C30 106(3) . . . . ? Sb2 C24 C25 C30 -76.4(18) . . . . ? O4 C24 C25 C26 -80(3) . . . . ? Sb2 C24 C25 C26 97.4(15) . . . . ? C30 C25 C26 C27 12(2) . . . . ? C24 C25 C26 C27 -161.7(14) . . . . ? C30 C25 C26 C31 -165.2(17) . . . . ? C24 C25 C26 C31 21(2) . . . . ? C25 C26 C27 C28 -4(2) . . . . ? C31 C26 C27 C28 173.3(16) . . . . ? C26 C27 C28 C29 -3(2) . . . . ? C26 C27 C28 C35 177.7(16) . . . . ? C27 C28 C29 C30 4(2) . . . . ? C35 C28 C29 C30 -177.2(16) . . . . ? C26 C25 C30 C29 -12(3) . . . . ? C24 C25 C30 C29 161.4(15) . . . . ? C26 C25 C30 C39 164.8(15) . . . . ? C24 C25 C30 C39 -22(3) . . . . ? C28 C29 C30 C25 4(3) . . . . ? C28 C29 C30 C39 -173.2(15) . . . . ? C27 C26 C31 C34 -1(2) . . . . ? C25 C26 C31 C34 175.9(15) . . . . ? C27 C26 C31 C33 119.0(18) . . . . ? C25 C26 C31 C33 -64(2) . . . . ? C27 C26 C31 C32 -117.3(17) . . . . ? C25 C26 C31 C32 60(2) . . . . ? C27 C28 C35 C38 177.4(17) . . . . ? C29 C28 C35 C38 -1(2) . . . . ? C27 C28 C35 C36 -56(2) . . . . ? C29 C28 C35 C36 125.2(17) . . . . ? C27 C28 C35 C37 59(2) . . . . ? C29 C28 C35 C37 -119.4(17) . . . . ? C25 C30 C39 C41 115(2) . . . . ? C29 C30 C39 C41 -68(2) . . . . ? C25 C30 C39 C42 -9(3) . . . . ? C29 C30 C39 C42 168.2(16) . . . . ? C25 C30 C39 C40 -128.7(19) . . . . ? C29 C30 C39 C40 48(2) . . . . ? C43 O5 C44 C45 -178.6(18) . . . . ? Na2 O5 C44 C45 31(2) . . . . ? O5 C44 C45 O6 -19(3) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 2.678 (near Sb(2)) _refine_diff_density_min -3.499 _refine_diff_density_rms 0.150 data_compound_10 _database_code_CSD 195262 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H83 As Na O7' _chemical_formula_weight 870.05 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.440(3) _cell_length_b 19.134(4) _cell_length_c 19.562(4) _cell_angle_alpha 90.00 _cell_angle_beta 109.36(3) _cell_angle_gamma 90.00 _cell_volume 5099.1(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1884 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.7619 _exptl_absorpt_correction_T_max 0.8695 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '2o phi scans & omega to complete' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 58037 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 11668 _reflns_number_gt 9117 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _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^)+(0.0358P)^2^+3.3224P] 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 SHELXL _refine_ls_extinction_coef 0.0041(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 11668 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0686 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1045 _refine_ls_wR_factor_gt 0.0974 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.468037(15) 0.222603(11) 0.238464(11) 0.01982(7) Uani 1 1 d . . . Na1 Na 0.39599(6) 0.40799(4) 0.31701(4) 0.02323(19) Uani 1 1 d . . . O1 O 0.53495(10) 0.34823(8) 0.31806(8) 0.0235(3) Uani 1 1 d . . . O2 O 0.31857(10) 0.31607(8) 0.25263(8) 0.0233(3) Uani 1 1 d . . . O3 O 0.39860(12) 0.38091(9) 0.43725(8) 0.0316(4) Uani 1 1 d . . . O4 O 0.24501(12) 0.44401(9) 0.34182(9) 0.0320(4) Uani 1 1 d . . . O5 O 0.47488(12) 0.51716(9) 0.35512(8) 0.0302(4) Uani 1 1 d . . . O6 O 0.34109(12) 0.49577(9) 0.22332(8) 0.0304(4) Uani 1 1 d . . . C1 C 0.55293(15) 0.29792(11) 0.28425(11) 0.0197(4) Uani 1 1 d . . . C2 C 0.65446(15) 0.28530(11) 0.27663(11) 0.0193(4) Uani 1 1 d . . . C3 C 0.72751(15) 0.25293(12) 0.33277(11) 0.0211(4) Uani 1 1 d . . . C4 C 0.81089(15) 0.22982(12) 0.31749(12) 0.0241(5) Uani 1 1 d . . . H4 H 0.8613 0.2080 0.3558 0.029 Uiso 1 1 calc R . . C5 C 0.82625(15) 0.23621(12) 0.25033(12) 0.0243(5) Uani 1 1 d . . . C6 C 0.75696(15) 0.27157(12) 0.19912(11) 0.0228(4) Uani 1 1 d . . . H6 H 0.7652 0.2788 0.1534 0.027 Uiso 1 1 calc R . . C7 C 0.67212(15) 0.29856(11) 0.21049(11) 0.0204(4) Uani 1 1 d . . . C8 C 0.72151(15) 0.24426(12) 0.41054(11) 0.0243(5) Uani 1 1 d . . . C9 C 0.72437(18) 0.31651(14) 0.44482(12) 0.0337(6) Uani 1 1 d . . . H9A H 0.7186 0.3114 0.4931 0.040 Uiso 1 1 calc R . . H9B H 0.6697 0.3448 0.4143 0.040 Uiso 1 1 calc R . . H9C H 0.7866 0.3395 0.4490 0.040 Uiso 1 1 calc R . . C10 C 0.63073(17) 0.20424(13) 0.41453(12) 0.0277(5) Uani 1 1 d . . . H10A H 0.6243 0.1601 0.3879 0.033 Uiso 1 1 calc R . . H10B H 0.5718 0.2327 0.3930 0.033 Uiso 1 1 calc R . . H10C H 0.6384 0.1944 0.4653 0.033 Uiso 1 1 calc R . . C11 C 0.80738(17) 0.20262(15) 0.45717(12) 0.0350(6) Uani 1 1 d . . . H11A H 0.8685 0.2271 0.4609 0.042 Uiso 1 1 calc R . . H11B H 0.8074 0.1565 0.4354 0.042 Uiso 1 1 calc R . . H11C H 0.8023 0.1971 0.5056 0.042 Uiso 1 1 calc R . . C12 C 0.91969(17) 0.20790(13) 0.23767(13) 0.0296(5) Uani 1 1 d . . . C13 C 0.9381(2) 0.13299(16) 0.26549(18) 0.0531(8) Uani 1 1 d . . . H13A H 0.9950 0.1140 0.2550 0.064 Uiso 1 1 calc R . . H13B H 0.8801 0.1044 0.2414 0.064 Uiso 1 1 calc R . . H13C H 0.9510 0.1325 0.3179 0.064 Uiso 1 1 calc R . . C14 C 1.00441(18) 0.25462(18) 0.27743(16) 0.0480(7) Uani 1 1 d . . . H14A H 1.0642 0.2380 0.2695 0.058 Uiso 1 1 calc R . . H14B H 1.0137 0.2537 0.3294 0.058 Uiso 1 1 calc R . . H14C H 0.9904 0.3026 0.2593 0.058 Uiso 1 1 calc R . . C15 C 0.9152(2) 0.20769(17) 0.15826(14) 0.0445(7) Uani 1 1 d . . . H15A H 0.9073 0.2557 0.1397 0.053 Uiso 1 1 calc R . . H15B H 0.8594 0.1793 0.1295 0.053 Uiso 1 1 calc R . . H15C H 0.9762 0.1879 0.1548 0.053 Uiso 1 1 calc R . . C16 C 0.60689(15) 0.34136(12) 0.14712(11) 0.0219(4) Uani 1 1 d . . . C17 C 0.67090(16) 0.39037(12) 0.11681(12) 0.0260(5) Uani 1 1 d . . . H17A H 0.7147 0.3620 0.0991 0.031 Uiso 1 1 calc R . . H17B H 0.7101 0.4214 0.1555 0.031 Uiso 1 1 calc R . . H17C H 0.6280 0.4184 0.0769 0.031 Uiso 1 1 calc R . . C18 C 0.53222(16) 0.38941(12) 0.16562(12) 0.0253(5) Uani 1 1 d . . . H18A H 0.4999 0.4196 0.1241 0.030 Uiso 1 1 calc R . . H18B H 0.5667 0.4184 0.2077 0.030 Uiso 1 1 calc R . . H18C H 0.4829 0.3607 0.1768 0.030 Uiso 1 1 calc R . . C19 C 0.55431(16) 0.29048(12) 0.08791(11) 0.0266(5) Uani 1 1 d . . . H19A H 0.6027 0.2631 0.0741 0.032 Uiso 1 1 calc R . . H19B H 0.5125 0.3163 0.0457 0.032 Uiso 1 1 calc R . . H19C H 0.5137 0.2590 0.1056 0.032 Uiso 1 1 calc R . . C20 C 0.34166(14) 0.25670(11) 0.23932(10) 0.0189(4) Uani 1 1 d . . . C21 C 0.26920(14) 0.19734(11) 0.21574(11) 0.0196(4) Uani 1 1 d . . . C22 C 0.21174(14) 0.19214(11) 0.14339(11) 0.0200(4) Uani 1 1 d . . . C23 C 0.16879(15) 0.12821(12) 0.12002(11) 0.0227(4) Uani 1 1 d . . . H23 H 0.1292 0.1243 0.0705 0.027 Uiso 1 1 calc R . . C24 C 0.17882(14) 0.06925(12) 0.16304(11) 0.0211(4) Uani 1 1 d . . . C25 C 0.22719(15) 0.07808(12) 0.23483(11) 0.0219(4) Uani 1 1 d . . . H25 H 0.2315 0.0399 0.2668 0.026 Uiso 1 1 calc R . . C26 C 0.27056(14) 0.14101(11) 0.26306(11) 0.0203(4) Uani 1 1 d . . . C27 C 0.19164(15) 0.25460(12) 0.09017(11) 0.0235(4) Uani 1 1 d . . . C28 C 0.13981(16) 0.31306(13) 0.11909(12) 0.0288(5) Uani 1 1 d . . . H28A H 0.1220 0.3516 0.0841 0.035 Uiso 1 1 calc R . . H28B H 0.1843 0.3303 0.1655 0.035 Uiso 1 1 calc R . . H28C H 0.0804 0.2942 0.1259 0.035 Uiso 1 1 calc R . . C29 C 0.12447(18) 0.23411(13) 0.01662(12) 0.0334(6) Uani 1 1 d . . . H29A H 0.1544 0.1962 -0.0025 0.040 Uiso 1 1 calc R . . H29B H 0.1134 0.2745 -0.0160 0.040 Uiso 1 1 calc R . . H29C H 0.0617 0.2183 0.0201 0.040 Uiso 1 1 calc R . . C30 C 0.28429(17) 0.28326(13) 0.07656(12) 0.0290(5) Uani 1 1 d . . . H30A H 0.3183 0.2449 0.0616 0.035 Uiso 1 1 calc R . . H30B H 0.3283 0.3043 0.1212 0.035 Uiso 1 1 calc R . . H30C H 0.2650 0.3187 0.0383 0.035 Uiso 1 1 calc R . . C31 C 0.13191(16) -0.00052(12) 0.13341(12) 0.0262(5) Uani 1 1 d . . . C32 C 0.1422(2) -0.01383(13) 0.05905(13) 0.0354(6) Uani 1 1 d . . . H32A H 0.2119 -0.0163 0.0640 0.042 Uiso 1 1 calc R . . H32B H 0.1111 0.0244 0.0261 0.042 Uiso 1 1 calc R . . H32C H 0.1101 -0.0581 0.0394 0.042 Uiso 1 1 calc R . . C33 C 0.0246(2) 0.00366(18) 0.12829(18) 0.0542(9) Uani 1 1 d . . . H33A H -0.0085 -0.0402 0.1083 0.065 Uiso 1 1 calc R . . H33B H -0.0071 0.0426 0.0966 0.065 Uiso 1 1 calc R . . H33C H 0.0203 0.0113 0.1767 0.065 Uiso 1 1 calc R . . C34 C 0.1769(2) -0.06233(14) 0.18031(14) 0.0488(8) Uani 1 1 d . . . H34A H 0.2481 -0.0620 0.1908 0.059 Uiso 1 1 calc R . . H34B H 0.1493 -0.1056 0.1549 0.059 Uiso 1 1 calc R . . H34C H 0.1625 -0.0596 0.2258 0.059 Uiso 1 1 calc R . . C35 C 0.31389(16) 0.14157(12) 0.34557(11) 0.0223(4) Uani 1 1 d . . . C36 C 0.23735(18) 0.11194(14) 0.37937(12) 0.0314(5) Uani 1 1 d . . . H36A H 0.1766 0.1392 0.3618 0.038 Uiso 1 1 calc R . . H36B H 0.2643 0.1152 0.4323 0.038 Uiso 1 1 calc R . . H36C H 0.2233 0.0629 0.3651 0.038 Uiso 1 1 calc R . . C37 C 0.40374(16) 0.09503(12) 0.36698(12) 0.0271(5) Uani 1 1 d . . . H37A H 0.3853 0.0481 0.3469 0.033 Uiso 1 1 calc R . . H37B H 0.4311 0.0922 0.4199 0.033 Uiso 1 1 calc R . . H37C H 0.4530 0.1146 0.3479 0.033 Uiso 1 1 calc R . . C38 C 0.33977(17) 0.21418(12) 0.37907(11) 0.0266(5) Uani 1 1 d . . . H38A H 0.3950 0.2332 0.3664 0.032 Uiso 1 1 calc R . . H38B H 0.3581 0.2107 0.4319 0.032 Uiso 1 1 calc R . . H38C H 0.2828 0.2451 0.3604 0.032 Uiso 1 1 calc R . . C39 C 0.4889(2) 0.37891(17) 0.49010(14) 0.0465(7) Uani 1 1 d . . . H39A H 0.5102 0.4266 0.5060 0.056 Uiso 1 1 calc R . . H39B H 0.5364 0.3572 0.4707 0.056 Uiso 1 1 calc R . . H39C H 0.4848 0.3515 0.5313 0.056 Uiso 1 1 calc R . . C40 C 0.32656(19) 0.41523(15) 0.46120(13) 0.0376(6) Uani 1 1 d . . . H40A H 0.3443 0.4650 0.4721 0.045 Uiso 1 1 calc R . . H40B H 0.3225 0.3926 0.5056 0.045 Uiso 1 1 calc R . . C41 C 0.23370(19) 0.40960(15) 0.40326(14) 0.0382(6) Uani 1 1 d . . . H41A H 0.2163 0.3599 0.3920 0.046 Uiso 1 1 calc R . . H41B H 0.1810 0.4321 0.4174 0.046 Uiso 1 1 calc R . . C42 C 0.16228(18) 0.43539(16) 0.28200(14) 0.0405(6) Uani 1 1 d . . . H42A H 0.1504 0.3854 0.2718 0.049 Uiso 1 1 calc R . . H42B H 0.1719 0.4584 0.2401 0.049 Uiso 1 1 calc R . . H42C H 0.1057 0.4562 0.2915 0.049 Uiso 1 1 calc R . . C43 C 0.56656(18) 0.52921(15) 0.34283(14) 0.0370(6) Uani 1 1 d . . . H43A H 0.5565 0.5257 0.2909 0.044 Uiso 1 1 calc R . . H43B H 0.6146 0.4941 0.3691 0.044 Uiso 1 1 calc R . . H43C H 0.5909 0.5760 0.3601 0.044 Uiso 1 1 calc R . . C44 C 0.40443(17) 0.56896(13) 0.32360(13) 0.0301(5) Uani 1 1 d . . . H44A H 0.4328 0.6156 0.3398 0.036 Uiso 1 1 calc R . . H44B H 0.3470 0.5626 0.3400 0.036 Uiso 1 1 calc R . . C45 C 0.37211(18) 0.56537(12) 0.24344(13) 0.0306(5) Uani 1 1 d . . . H45A H 0.3173 0.5983 0.2220 0.037 Uiso 1 1 calc R . . H45B H 0.4270 0.5779 0.2260 0.037 Uiso 1 1 calc R . . C46 C 0.3068(2) 0.48835(15) 0.14802(13) 0.0394(6) Uani 1 1 d . . . H46A H 0.2477 0.5169 0.1274 0.047 Uiso 1 1 calc R . . H46B H 0.2910 0.4392 0.1355 0.047 Uiso 1 1 calc R . . H46C H 0.3576 0.5038 0.1284 0.047 Uiso 1 1 calc R . . C1S C -0.0618(3) 0.4459(2) 0.1367(2) 0.0749(11) Uani 1 1 d . . . O1S O -0.0710(4) 0.4535(3) 0.0591(3) 0.0792(16) Uani 0.50 1 d P A 1 C2S C 0.0055(7) 0.4992(5) 0.0403(4) 0.050(3) Uani 0.50 1 d P . 1 O1SA O -0.0105(9) 0.4955(10) 0.0885(9) 0.294(11) Uani 0.50 1 d P A 2 C2SA C -0.0275(9) 0.4787(7) 0.0160(6) 0.075(3) Uani 0.50 1 d P . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01850(11) 0.01935(12) 0.02163(11) -0.00155(9) 0.00667(8) 0.00055(9) Na1 0.0249(4) 0.0211(5) 0.0240(4) -0.0011(3) 0.0085(3) 0.0017(3) O1 0.0243(8) 0.0247(8) 0.0214(7) -0.0022(6) 0.0075(6) 0.0026(6) O2 0.0227(8) 0.0192(8) 0.0261(8) -0.0025(6) 0.0056(6) 0.0014(6) O3 0.0354(9) 0.0332(10) 0.0262(8) -0.0014(7) 0.0103(7) 0.0054(7) O4 0.0317(9) 0.0345(10) 0.0312(9) 0.0004(7) 0.0123(7) 0.0012(7) O5 0.0310(8) 0.0257(9) 0.0311(8) 0.0019(7) 0.0065(7) -0.0014(7) O6 0.0348(9) 0.0250(9) 0.0269(8) 0.0014(7) 0.0042(7) -0.0030(7) C1 0.0214(10) 0.0219(11) 0.0162(9) 0.0031(8) 0.0068(8) 0.0032(8) C2 0.0192(10) 0.0189(11) 0.0187(9) -0.0020(8) 0.0049(8) -0.0005(8) C3 0.0221(10) 0.0200(11) 0.0202(10) -0.0005(8) 0.0058(8) -0.0015(8) C4 0.0192(10) 0.0257(12) 0.0250(10) 0.0032(9) 0.0042(8) -0.0003(9) C5 0.0204(10) 0.0238(12) 0.0287(11) -0.0002(9) 0.0083(9) 0.0006(8) C6 0.0239(10) 0.0261(12) 0.0197(10) 0.0009(9) 0.0089(8) 0.0006(9) C7 0.0209(10) 0.0194(11) 0.0198(10) -0.0011(8) 0.0053(8) -0.0007(8) C8 0.0222(11) 0.0306(13) 0.0180(10) 0.0019(9) 0.0036(8) -0.0009(9) C9 0.0378(13) 0.0376(15) 0.0213(11) -0.0044(10) 0.0038(10) -0.0060(11) C10 0.0300(12) 0.0341(14) 0.0192(10) 0.0043(9) 0.0082(9) -0.0026(10) C11 0.0286(12) 0.0498(17) 0.0228(11) 0.0089(11) 0.0032(10) 0.0047(11) C12 0.0245(12) 0.0336(14) 0.0330(12) 0.0064(10) 0.0127(10) 0.0073(9) C13 0.0544(18) 0.0460(18) 0.072(2) 0.0159(16) 0.0379(16) 0.0256(15) C14 0.0216(12) 0.070(2) 0.0514(17) 0.0002(15) 0.0115(12) 0.0044(13) C15 0.0331(14) 0.068(2) 0.0390(14) 0.0037(13) 0.0201(12) 0.0173(13) C16 0.0211(10) 0.0258(12) 0.0178(9) 0.0010(8) 0.0052(8) 0.0006(9) C17 0.0257(11) 0.0279(13) 0.0240(11) 0.0041(9) 0.0077(9) 0.0005(9) C18 0.0268(11) 0.0253(12) 0.0242(11) 0.0061(9) 0.0091(9) 0.0051(9) C19 0.0265(11) 0.0322(13) 0.0199(10) -0.0020(9) 0.0061(9) -0.0008(9) C20 0.0185(10) 0.0222(11) 0.0152(9) 0.0008(8) 0.0043(8) -0.0023(8) C21 0.0175(10) 0.0211(11) 0.0207(10) -0.0015(8) 0.0068(8) 0.0000(8) C22 0.0171(10) 0.0234(11) 0.0191(10) 0.0019(8) 0.0056(8) 0.0006(8) C23 0.0181(10) 0.0292(12) 0.0179(10) -0.0002(9) 0.0020(8) -0.0010(8) C24 0.0172(10) 0.0246(11) 0.0199(10) -0.0011(8) 0.0039(8) -0.0030(8) C25 0.0215(10) 0.0230(11) 0.0193(10) 0.0031(8) 0.0045(8) -0.0010(8) C26 0.0173(10) 0.0248(12) 0.0176(9) 0.0000(8) 0.0041(8) -0.0004(8) C27 0.0232(11) 0.0247(12) 0.0208(10) 0.0030(9) 0.0048(8) 0.0030(9) C28 0.0268(12) 0.0281(13) 0.0292(12) 0.0031(10) 0.0062(9) 0.0071(10) C29 0.0350(13) 0.0353(15) 0.0231(11) 0.0056(10) 0.0003(10) 0.0017(10) C30 0.0305(12) 0.0319(13) 0.0251(11) 0.0073(10) 0.0100(9) 0.0005(10) C31 0.0256(11) 0.0269(12) 0.0218(10) -0.0029(9) 0.0020(9) -0.0086(9) C32 0.0482(15) 0.0282(13) 0.0288(12) -0.0050(10) 0.0115(11) -0.0051(11) C33 0.0341(15) 0.061(2) 0.071(2) -0.0342(17) 0.0219(14) -0.0243(14) C34 0.076(2) 0.0243(14) 0.0305(13) 0.0011(11) -0.0037(13) -0.0142(13) C35 0.0267(11) 0.0229(12) 0.0161(9) -0.0011(8) 0.0056(8) -0.0027(9) C36 0.0356(13) 0.0378(14) 0.0215(11) -0.0009(10) 0.0103(10) -0.0103(11) C37 0.0286(12) 0.0267(12) 0.0208(10) 0.0013(9) 0.0011(9) -0.0004(9) C38 0.0316(12) 0.0285(13) 0.0183(10) -0.0025(9) 0.0064(9) -0.0023(9) C39 0.0480(16) 0.0533(19) 0.0308(13) 0.0030(13) 0.0030(12) 0.0149(14) C40 0.0456(15) 0.0433(16) 0.0292(12) -0.0015(11) 0.0195(11) 0.0060(12) C41 0.0364(14) 0.0468(17) 0.0392(14) 0.0007(12) 0.0229(11) 0.0038(12) C42 0.0295(13) 0.0556(18) 0.0373(14) -0.0044(13) 0.0123(11) 0.0070(12) C43 0.0290(13) 0.0386(15) 0.0390(14) -0.0027(11) 0.0055(10) -0.0026(11) C44 0.0340(13) 0.0221(12) 0.0335(12) -0.0004(10) 0.0103(10) 0.0022(10) C45 0.0328(12) 0.0220(12) 0.0337(12) 0.0038(10) 0.0067(10) -0.0023(10) C46 0.0418(15) 0.0378(15) 0.0313(13) -0.0008(11) 0.0023(11) -0.0006(12) C1S 0.058(2) 0.083(3) 0.084(3) 0.005(2) 0.025(2) 0.012(2) O1S 0.055(3) 0.101(5) 0.070(3) -0.011(3) 0.005(3) -0.013(3) C2S 0.054(5) 0.051(5) 0.029(4) -0.028(3) -0.009(4) 0.006(3) O1SA 0.122(9) 0.41(2) 0.273(16) -0.263(17) -0.037(10) -0.012(11) C2SA 0.085(8) 0.083(8) 0.059(7) 0.004(6) 0.028(6) 0.026(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag As1 C1 1.911(2) . ? As1 C20 1.943(2) . ? Na1 O2 2.2351(17) . ? Na1 O1 2.3036(17) . ? Na1 O5 2.3777(19) . ? Na1 O3 2.3967(18) . ? Na1 O6 2.4177(18) . ? Na1 O4 2.4830(19) . ? Na1 C44 3.083(3) . ? O1 C1 1.243(3) . ? O2 C20 1.236(3) . ? O3 C39 1.370(3) . ? O3 C40 1.434(3) . ? O4 C42 1.377(3) . ? O4 C41 1.426(3) . ? O5 C44 1.408(3) . ? O5 C43 1.440(3) . ? O6 C46 1.397(3) . ? O6 C45 1.418(3) . ? C1 C2 1.541(3) . ? C2 C3 1.391(3) . ? C2 C7 1.422(3) . ? C3 C4 1.405(3) . ? C3 C8 1.561(3) . ? C4 C5 1.408(3) . ? C5 C6 1.341(3) . ? C5 C12 1.548(3) . ? C6 C7 1.413(3) . ? C7 C16 1.523(3) . ? C8 C11 1.501(3) . ? C8 C9 1.531(3) . ? C8 C10 1.542(3) . ? C12 C14 1.507(4) . ? C12 C13 1.525(4) . ? C12 C15 1.533(3) . ? C16 C19 1.511(3) . ? C16 C18 1.548(3) . ? C16 C17 1.565(3) . ? C20 C21 1.509(3) . ? C21 C22 1.387(3) . ? C21 C26 1.417(3) . ? C22 C23 1.379(3) . ? C22 C27 1.548(3) . ? C23 C24 1.386(3) . ? C24 C25 1.356(3) . ? C24 C31 1.522(3) . ? C25 C26 1.385(3) . ? C26 C35 1.525(3) . ? C27 C29 1.496(3) . ? C27 C30 1.548(3) . ? C27 C28 1.553(3) . ? C31 C34 1.506(3) . ? C31 C33 1.521(4) . ? C31 C32 1.532(3) . ? C35 C37 1.514(3) . ? C35 C38 1.529(3) . ? C35 C36 1.570(3) . ? C40 C41 1.444(4) . ? C44 C45 1.482(3) . ? C1S O1S 1.486(7) . ? C1S O1SA 1.67(2) . ? O1S C2S 1.546(12) . ? C2S C2S 1.531(17) 3_565 ? O1SA C2SA 1.395(16) . ? C2SA C2SA 1.42(3) 3_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 C1 As1 C20 101.60(9) . . ? O2 Na1 O1 83.45(6) . . ? O2 Na1 O5 165.04(7) . . ? O1 Na1 O5 96.19(6) . . ? O2 Na1 O3 103.00(7) . . ? O1 Na1 O3 98.84(7) . . ? O5 Na1 O3 91.85(6) . . ? O2 Na1 O6 98.19(7) . . ? O1 Na1 O6 114.66(7) . . ? O5 Na1 O6 68.28(6) . . ? O3 Na1 O6 142.07(7) . . ? O2 Na1 O4 91.20(6) . . ? O1 Na1 O4 162.68(7) . . ? O5 Na1 O4 93.17(6) . . ? O3 Na1 O4 66.25(6) . . ? O6 Na1 O4 82.35(6) . . ? O2 Na1 C44 144.59(7) . . ? O1 Na1 C44 118.24(7) . . ? O5 Na1 C44 26.00(6) . . ? O3 Na1 C44 100.80(7) . . ? O6 Na1 C44 48.41(6) . . ? O4 Na1 C44 74.91(6) . . ? C1 O1 Na1 135.61(14) . . ? C20 O2 Na1 136.27(13) . . ? C39 O3 C40 112.25(19) . . ? C39 O3 Na1 116.60(16) . . ? C40 O3 Na1 116.39(14) . . ? C42 O4 C41 110.6(2) . . ? C42 O4 Na1 111.78(14) . . ? C41 O4 Na1 112.94(14) . . ? C44 O5 C43 112.64(19) . . ? C44 O5 Na1 106.24(13) . . ? C43 O5 Na1 117.36(14) . . ? C46 O6 C45 110.92(18) . . ? C46 O6 Na1 129.88(15) . . ? C45 O6 Na1 116.60(13) . . ? O1 C1 C2 123.09(19) . . ? O1 C1 As1 128.20(16) . . ? C2 C1 As1 108.63(14) . . ? C3 C2 C7 118.68(19) . . ? C3 C2 C1 119.35(18) . . ? C7 C2 C1 121.57(17) . . ? C2 C3 C4 116.83(19) . . ? C2 C3 C8 122.97(19) . . ? C4 C3 C8 120.16(18) . . ? C3 C4 C5 125.6(2) . . ? C6 C5 C4 115.6(2) . . ? C6 C5 C12 122.1(2) . . ? C4 C5 C12 122.28(19) . . ? C5 C6 C7 122.5(2) . . ? C6 C7 C2 120.28(19) . . ? C6 C7 C16 113.76(18) . . ? C2 C7 C16 125.96(18) . . ? C11 C8 C9 108.43(19) . . ? C11 C8 C10 104.50(19) . . ? C9 C8 C10 109.03(19) . . ? C11 C8 C3 110.30(19) . . ? C9 C8 C3 109.19(19) . . ? C10 C8 C3 115.14(17) . . ? C14 C12 C13 111.0(2) . . ? C14 C12 C15 106.2(2) . . ? C13 C12 C15 107.6(2) . . ? C14 C12 C5 108.1(2) . . ? C13 C12 C5 109.3(2) . . ? C15 C12 C5 114.64(19) . . ? C19 C16 C7 107.18(18) . . ? C19 C16 C18 110.48(18) . . ? C7 C16 C18 114.82(17) . . ? C19 C16 C17 107.78(17) . . ? C7 C16 C17 110.30(17) . . ? C18 C16 C17 106.10(18) . . ? O2 C20 C21 123.23(18) . . ? O2 C20 As1 129.06(15) . . ? C21 C20 As1 107.62(14) . . ? C22 C21 C26 119.09(19) . . ? C22 C21 C20 119.05(19) . . ? C26 C21 C20 120.99(18) . . ? C23 C22 C21 116.95(19) . . ? C23 C22 C27 119.90(18) . . ? C21 C22 C27 123.12(19) . . ? C22 C23 C24 125.15(19) . . ? C25 C24 C23 116.2(2) . . ? C25 C24 C31 121.02(19) . . ? C23 C24 C31 122.61(18) . . ? C24 C25 C26 122.1(2) . . ? C25 C26 C21 119.64(18) . . ? C25 C26 C35 113.63(18) . . ? C21 C26 C35 126.72(19) . . ? C29 C27 C22 111.20(19) . . ? C29 C27 C30 104.42(18) . . ? C22 C27 C30 114.15(17) . . ? C29 C27 C28 107.58(18) . . ? C22 C27 C28 108.45(18) . . ? C30 C27 C28 110.84(19) . . ? C34 C31 C33 107.8(2) . . ? C34 C31 C24 114.16(18) . . ? C33 C31 C24 107.1(2) . . ? C34 C31 C32 106.9(2) . . ? C33 C31 C32 111.3(2) . . ? C24 C31 C32 109.66(18) . . ? C37 C35 C26 107.57(18) . . ? C37 C35 C38 110.53(18) . . ? C26 C35 C38 114.60(18) . . ? C37 C35 C36 109.24(19) . . ? C26 C35 C36 110.12(17) . . ? C38 C35 C36 104.71(18) . . ? O3 C40 C41 107.1(2) . . ? O4 C41 C40 106.9(2) . . ? O5 C44 C45 111.0(2) . . ? O5 C44 Na1 47.76(10) . . ? C45 C44 Na1 85.14(14) . . ? O6 C45 C44 107.27(19) . . ? O1S C1S O1SA 43.6(4) . . ? C1S O1S C2S 118.0(5) . . ? C2S C2S O1S 114.7(9) 3_565 . ? C2SA O1SA C1S 118.8(12) . . ? O1SA C2SA C2SA 112.4(19) . 3_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Na1 O1 C1 14.1(2) . . . . ? O5 Na1 O1 C1 -150.8(2) . . . . ? O3 Na1 O1 C1 116.3(2) . . . . ? O6 Na1 O1 C1 -81.9(2) . . . . ? O4 Na1 O1 C1 86.8(3) . . . . ? C44 Na1 O1 C1 -136.26(19) . . . . ? O1 Na1 O2 C20 13.8(2) . . . . ? O5 Na1 O2 C20 103.2(3) . . . . ? O3 Na1 O2 C20 -83.9(2) . . . . ? O6 Na1 O2 C20 127.8(2) . . . . ? O4 Na1 O2 C20 -149.7(2) . . . . ? C44 Na1 O2 C20 145.09(19) . . . . ? O2 Na1 O3 C39 123.08(18) . . . . ? O1 Na1 O3 C39 37.82(19) . . . . ? O5 Na1 O3 C39 -58.74(19) . . . . ? O6 Na1 O3 C39 -114.63(19) . . . . ? O4 Na1 O3 C39 -151.39(19) . . . . ? C44 Na1 O3 C39 -83.32(19) . . . . ? O2 Na1 O3 C40 -100.76(17) . . . . ? O1 Na1 O3 C40 173.97(16) . . . . ? O5 Na1 O3 C40 77.41(17) . . . . ? O6 Na1 O3 C40 21.5(2) . . . . ? O4 Na1 O3 C40 -15.24(16) . . . . ? C44 Na1 O3 C40 52.83(17) . . . . ? O2 Na1 O4 C42 -39.95(17) . . . . ? O1 Na1 O4 C42 -111.5(3) . . . . ? O5 Na1 O4 C42 125.74(17) . . . . ? O3 Na1 O4 C42 -143.64(18) . . . . ? O6 Na1 O4 C42 58.16(17) . . . . ? C44 Na1 O4 C42 107.05(18) . . . . ? O2 Na1 O4 C41 85.50(16) . . . . ? O1 Na1 O4 C41 13.9(3) . . . . ? O5 Na1 O4 C41 -108.82(16) . . . . ? O3 Na1 O4 C41 -18.19(15) . . . . ? O6 Na1 O4 C41 -176.40(16) . . . . ? C44 Na1 O4 C41 -127.50(16) . . . . ? O2 Na1 O5 C44 61.9(3) . . . . ? O1 Na1 O5 C44 149.69(13) . . . . ? O3 Na1 O5 C44 -111.20(14) . . . . ? O6 Na1 O5 C44 35.58(13) . . . . ? O4 Na1 O5 C44 -44.89(14) . . . . ? O2 Na1 O5 C43 -65.1(3) . . . . ? O1 Na1 O5 C43 22.67(16) . . . . ? O3 Na1 O5 C43 121.77(15) . . . . ? O6 Na1 O5 C43 -91.44(16) . . . . ? O4 Na1 O5 C43 -171.92(15) . . . . ? C44 Na1 O5 C43 -127.0(2) . . . . ? O2 Na1 O6 C46 -22.5(2) . . . . ? O1 Na1 O6 C46 64.0(2) . . . . ? O5 Na1 O6 C46 150.9(2) . . . . ? O3 Na1 O6 C46 -146.16(19) . . . . ? O4 Na1 O6 C46 -112.6(2) . . . . ? C44 Na1 O6 C46 170.8(2) . . . . ? O2 Na1 O6 C45 177.64(15) . . . . ? O1 Na1 O6 C45 -95.84(16) . . . . ? O5 Na1 O6 C45 -9.00(15) . . . . ? O3 Na1 O6 C45 54.0(2) . . . . ? O4 Na1 O6 C45 87.52(16) . . . . ? C44 Na1 O6 C45 10.94(15) . . . . ? Na1 O1 C1 C2 157.26(14) . . . . ? Na1 O1 C1 As1 -26.2(3) . . . . ? C20 As1 C1 O1 12.6(2) . . . . ? C20 As1 C1 C2 -170.46(13) . . . . ? O1 C1 C2 C3 81.7(3) . . . . ? As1 C1 C2 C3 -95.4(2) . . . . ? O1 C1 C2 C7 -105.6(2) . . . . ? As1 C1 C2 C7 77.2(2) . . . . ? C7 C2 C3 C4 -5.6(3) . . . . ? C1 C2 C3 C4 167.28(19) . . . . ? C7 C2 C3 C8 172.14(19) . . . . ? C1 C2 C3 C8 -15.0(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C8 C3 C4 C5 -178.3(2) . . . . ? C3 C4 C5 C6 4.5(3) . . . . ? C3 C4 C5 C12 -178.7(2) . . . . ? C4 C5 C6 C7 -2.3(3) . . . . ? C12 C5 C6 C7 -179.0(2) . . . . ? C5 C6 C7 C2 -3.7(3) . . . . ? C5 C6 C7 C16 175.8(2) . . . . ? C3 C2 C7 C6 7.8(3) . . . . ? C1 C2 C7 C6 -164.94(19) . . . . ? C3 C2 C7 C16 -171.7(2) . . . . ? C1 C2 C7 C16 15.6(3) . . . . ? C2 C3 C8 C11 175.7(2) . . . . ? C4 C3 C8 C11 -6.6(3) . . . . ? C2 C3 C8 C9 -65.2(3) . . . . ? C4 C3 C8 C9 112.4(2) . . . . ? C2 C3 C8 C10 57.8(3) . . . . ? C4 C3 C8 C10 -124.5(2) . . . . ? C6 C5 C12 C14 104.2(3) . . . . ? C4 C5 C12 C14 -72.3(3) . . . . ? C6 C5 C12 C13 -134.9(3) . . . . ? C4 C5 C12 C13 48.6(3) . . . . ? C6 C5 C12 C15 -14.0(3) . . . . ? C4 C5 C12 C15 169.5(2) . . . . ? C6 C7 C16 C19 74.5(2) . . . . ? C2 C7 C16 C19 -106.0(2) . . . . ? C6 C7 C16 C18 -162.37(19) . . . . ? C2 C7 C16 C18 17.1(3) . . . . ? C6 C7 C16 C17 -42.6(2) . . . . ? C2 C7 C16 C17 136.9(2) . . . . ? Na1 O2 C20 C21 157.70(15) . . . . ? Na1 O2 C20 As1 -26.1(3) . . . . ? C1 As1 C20 O2 12.5(2) . . . . ? C1 As1 C20 C21 -170.83(13) . . . . ? O2 C20 C21 C22 82.4(3) . . . . ? As1 C20 C21 C22 -94.5(2) . . . . ? O2 C20 C21 C26 -108.4(2) . . . . ? As1 C20 C21 C26 74.7(2) . . . . ? C26 C21 C22 C23 -8.0(3) . . . . ? C20 C21 C22 C23 161.45(19) . . . . ? C26 C21 C22 C27 169.73(19) . . . . ? C20 C21 C22 C27 -20.8(3) . . . . ? C21 C22 C23 C24 -0.1(3) . . . . ? C27 C22 C23 C24 -177.9(2) . . . . ? C22 C23 C24 C25 6.5(3) . . . . ? C22 C23 C24 C31 -178.1(2) . . . . ? C23 C24 C25 C26 -4.6(3) . . . . ? C31 C24 C25 C26 179.91(19) . . . . ? C24 C25 C26 C21 -3.2(3) . . . . ? C24 C25 C26 C35 175.3(2) . . . . ? C22 C21 C26 C25 9.8(3) . . . . ? C20 C21 C26 C25 -159.45(19) . . . . ? C22 C21 C26 C35 -168.5(2) . . . . ? C20 C21 C26 C35 22.2(3) . . . . ? C23 C22 C27 C29 -0.3(3) . . . . ? C21 C22 C27 C29 -178.0(2) . . . . ? C23 C22 C27 C30 -118.1(2) . . . . ? C21 C22 C27 C30 64.2(3) . . . . ? C23 C22 C27 C28 117.8(2) . . . . ? C21 C22 C27 C28 -59.9(3) . . . . ? C25 C24 C31 C34 -24.0(3) . . . . ? C23 C24 C31 C34 160.8(2) . . . . ? C25 C24 C31 C33 95.2(3) . . . . ? C23 C24 C31 C33 -80.0(3) . . . . ? C25 C24 C31 C32 -143.9(2) . . . . ? C23 C24 C31 C32 40.9(3) . . . . ? C25 C26 C35 C37 70.7(2) . . . . ? C21 C26 C35 C37 -110.9(2) . . . . ? C25 C26 C35 C38 -166.00(19) . . . . ? C21 C26 C35 C38 12.4(3) . . . . ? C25 C26 C35 C36 -48.3(2) . . . . ? C21 C26 C35 C36 130.1(2) . . . . ? C39 O3 C40 C41 -175.9(2) . . . . ? Na1 O3 C40 C41 46.1(3) . . . . ? C42 O4 C41 C40 174.4(2) . . . . ? Na1 O4 C41 C40 48.3(2) . . . . ? O3 C40 C41 O4 -60.7(3) . . . . ? C43 O5 C44 C45 68.0(2) . . . . ? Na1 O5 C44 C45 -61.8(2) . . . . ? C43 O5 C44 Na1 129.80(19) . . . . ? O2 Na1 C44 O5 -156.86(14) . . . . ? O1 Na1 C44 O5 -34.71(15) . . . . ? O3 Na1 C44 O5 71.56(14) . . . . ? O6 Na1 C44 O5 -133.72(16) . . . . ? O4 Na1 C44 O5 133.12(14) . . . . ? O2 Na1 C44 C45 -32.5(2) . . . . ? O1 Na1 C44 C45 89.63(15) . . . . ? O5 Na1 C44 C45 124.3(2) . . . . ? O3 Na1 C44 C45 -164.10(14) . . . . ? O6 Na1 C44 C45 -9.38(12) . . . . ? O4 Na1 C44 C45 -102.53(14) . . . . ? C46 O6 C45 C44 178.4(2) . . . . ? Na1 O6 C45 C44 -18.0(2) . . . . ? O5 C44 C45 O6 53.5(3) . . . . ? Na1 C44 C45 O6 12.57(16) . . . . ? O1SA C1S O1S C2S 10.1(8) . . . . ? C1S O1S C2S C2S 176.6(8) . . . 3_565 ? O1S C1S O1SA C2SA -10.7(8) . . . . ? C1S O1SA C2SA C2SA -174.8(10) . . . 3_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.801 _refine_diff_density_min -0.498 _refine_diff_density_rms 0.060 data_compound_9 _database_code_CSD 195263 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 As Na O4' _chemical_formula_weight 398.25 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5803(10) _cell_length_b 7.6097(7) _cell_length_c 19.678(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.446(10) _cell_angle_gamma 90.00 _cell_volume 1832.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 1.896 _exptl_absorpt_correction_type Difabs _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type CAD4 _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 4196 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0502 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 26.30 _reflns_number_total 3715 _reflns_number_gt 2640 _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^)+(0.0701P)^2^+0.4897P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3715 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0793 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1199 _refine_ls_wR_factor_gt 0.1089 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _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 Na1 Na -0.06575(15) 0.6813(3) 0.00906(8) 0.0683(6) Uani 1 1 d . . . As1 As -0.13479(3) 0.41060(5) -0.203218(16) 0.03263(14) Uani 1 1 d . A . O1 O 0.0809(2) 0.3613(4) -0.11701(13) 0.0510(8) Uani 1 1 d . . . O2 O -0.1045(2) 0.4208(4) -0.05528(12) 0.0499(8) Uani 1 1 d . . . O3 O -0.0309(7) 0.921(3) -0.0742(4) 0.055(5) Uani 0.52(3) 1 d P A 1 O3' O -0.0466(8) 0.818(3) -0.0884(6) 0.041(4) Uani 0.48(3) 1 d P A 2 O4 O -0.2187(2) 0.8483(5) -0.03315(15) 0.0586(8) Uani 1 1 d . A . C1 C 0.0229(3) 0.3863(5) -0.17651(17) 0.0317(8) Uani 1 1 d . . . C2 C 0.0780(3) 0.3811(4) -0.23643(17) 0.0281(7) Uani 1 1 d . . . C3 C 0.0347(3) 0.4662(5) -0.29962(17) 0.0319(8) Uani 1 1 d . . . H3 H -0.0291 0.5320 -0.3050 0.038 Uiso 1 1 calc R . . C4 C 0.0864(3) 0.4526(6) -0.35420(19) 0.0394(9) Uani 1 1 d . . . H4 H 0.0572 0.5091 -0.3963 0.047 Uiso 1 1 calc R . . C5 C 0.1809(3) 0.3560(6) -0.3464(2) 0.0440(10) Uani 1 1 d . . . H5 H 0.2145 0.3460 -0.3836 0.053 Uiso 1 1 calc R . . C6 C 0.2262(3) 0.2738(5) -0.2839(2) 0.0437(10) Uani 1 1 d . . . H6 H 0.2907 0.2101 -0.2786 0.052 Uiso 1 1 calc R . . C7 C 0.1745(3) 0.2871(5) -0.22905(18) 0.0358(8) Uani 1 1 d . . . H7 H 0.2049 0.2322 -0.1868 0.043 Uiso 1 1 calc R . . C8 C -0.1699(3) 0.4212(5) -0.11365(17) 0.0347(8) Uani 1 1 d . . . C9 C -0.2888(3) 0.4225(5) -0.11343(18) 0.0325(8) Uani 1 1 d . A . C10 C -0.3696(3) 0.4721(5) -0.1722(2) 0.0424(9) Uani 1 1 d . . . H10 H -0.3496 0.5066 -0.2128 0.051 Uiso 1 1 calc R A . C11 C -0.4784(3) 0.4702(6) -0.1702(2) 0.0483(10) Uani 1 1 d . A . H11 H -0.5314 0.5049 -0.2092 0.058 Uiso 1 1 calc R . . C12 C -0.5090(4) 0.4165(6) -0.1100(2) 0.0494(10) Uani 1 1 d . . . H12 H -0.5825 0.4133 -0.1090 0.059 Uiso 1 1 calc R A . C13 C -0.4309(4) 0.3684(6) -0.0524(2) 0.0499(11) Uani 1 1 d . A . H13 H -0.4515 0.3334 -0.0120 0.060 Uiso 1 1 calc R . . C14 C -0.3215(3) 0.3712(5) -0.0536(2) 0.0421(10) Uani 1 1 d . . . H14 H -0.2692 0.3384 -0.0139 0.050 Uiso 1 1 calc R A . C15 C -0.3169(3) 0.8363(6) -0.0113(2) 0.0508(10) Uani 1 1 d . . . H15A H -0.3436 0.9523 -0.0056 0.076 Uiso 1 1 calc R A . H15B H -0.3044 0.7746 0.0324 0.076 Uiso 1 1 calc R . . H15C H -0.3700 0.7739 -0.0458 0.076 Uiso 1 1 calc R . . C16 C -0.2255(4) 0.9325(6) -0.0948(2) 0.0517(11) Uani 1 1 d . . . H16A H -0.2499 1.0520 -0.0904 0.062 Uiso 1 1 calc R A . H16B H -0.2807 0.8748 -0.1304 0.062 Uiso 1 1 calc R . . C17 C -0.1240(4) 0.9387(7) -0.1184(3) 0.0636(14) Uani 1 1 d . A . H17A H -0.1283 0.8480 -0.1535 0.076 Uiso 1 1 calc R B 1 H17B H -0.1223 1.0505 -0.1417 0.076 Uiso 1 1 calc R B 1 C18 C 0.0561(4) 0.8606(8) -0.1076(3) 0.0726(16) Uani 1 1 d . . . H18A H 0.1258 0.8740 -0.0755 0.109 Uiso 1 1 calc R A 1 H18B H 0.0544 0.9296 -0.1486 0.109 Uiso 1 1 calc R A 1 H18C H 0.0446 0.7392 -0.1204 0.109 Uiso 1 1 calc R A 1 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 Na1 0.0637(11) 0.1148(16) 0.0273(8) 0.0195(9) 0.0123(7) 0.0580(12) As1 0.0315(2) 0.0440(2) 0.02295(19) 0.00076(17) 0.00730(13) 0.00041(19) O1 0.0446(16) 0.081(2) 0.0261(13) 0.0097(13) 0.0058(11) 0.0216(15) O2 0.0469(16) 0.076(2) 0.0268(12) 0.0079(14) 0.0092(11) 0.0283(15) O3 0.045(4) 0.085(13) 0.036(3) -0.006(4) 0.010(3) 0.004(5) O3' 0.044(4) 0.046(8) 0.032(4) 0.008(4) 0.010(3) 0.007(4) O4 0.0344(15) 0.085(2) 0.0555(18) 0.0271(17) 0.0093(13) 0.0138(16) C1 0.0349(18) 0.033(2) 0.0251(16) 0.0043(14) 0.0034(14) 0.0059(15) C2 0.0279(16) 0.028(2) 0.0272(16) 0.0032(13) 0.0048(13) -0.0016(14) C3 0.0243(16) 0.038(2) 0.0323(18) 0.0057(15) 0.0041(14) -0.0014(15) C4 0.0341(19) 0.056(3) 0.0293(18) 0.0073(17) 0.0100(15) -0.0048(18) C5 0.036(2) 0.059(3) 0.041(2) 0.0038(19) 0.0178(17) -0.0013(19) C6 0.033(2) 0.047(2) 0.055(2) 0.002(2) 0.0167(17) 0.0086(18) C7 0.0320(18) 0.038(2) 0.0358(18) 0.0051(16) 0.0053(15) 0.0068(17) C8 0.043(2) 0.0346(19) 0.0273(17) 0.0060(16) 0.0093(15) 0.0109(18) C9 0.0395(19) 0.0261(18) 0.0340(17) 0.0045(15) 0.0126(15) 0.0096(16) C10 0.046(2) 0.047(2) 0.038(2) 0.0082(18) 0.0161(17) 0.0121(19) C11 0.038(2) 0.050(2) 0.059(3) 0.006(2) 0.0158(19) 0.0066(19) C12 0.048(2) 0.048(2) 0.059(3) -0.009(2) 0.025(2) -0.004(2) C13 0.061(3) 0.050(3) 0.048(2) -0.0011(19) 0.031(2) -0.004(2) C14 0.056(2) 0.041(2) 0.0331(19) 0.0005(16) 0.0177(18) 0.0060(19) C15 0.040(2) 0.058(3) 0.057(3) -0.003(2) 0.0165(19) 0.008(2) C16 0.048(2) 0.059(3) 0.044(2) 0.016(2) 0.0044(19) 0.012(2) C17 0.060(3) 0.065(3) 0.068(3) 0.030(3) 0.020(3) 0.014(3) C18 0.053(3) 0.110(5) 0.063(3) 0.014(3) 0.030(2) 0.011(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 Na1 O1 2.201(3) 3_565 ? Na1 O3' 2.243(7) . ? Na1 O2 2.261(3) 3_565 ? Na1 O4 2.295(3) . ? Na1 O2 2.342(4) . ? Na1 O3 2.554(17) . ? Na1 Na1 3.279(4) 3_565 ? As1 C8 1.916(3) . ? As1 C1 1.939(3) . ? O1 C1 1.242(4) . ? O1 Na1 2.201(3) 3_565 ? O2 C8 1.248(4) . ? O2 Na1 2.261(3) 3_565 ? O3 C17 1.293(8) . ? O3 C18 1.473(10) . ? O3' C17 1.367(10) . ? O4 C16 1.357(5) . ? O4 C15 1.402(4) . ? C1 C2 1.501(4) . ? C2 C7 1.386(5) . ? C2 C3 1.396(5) . ? C3 C4 1.383(5) . ? C4 C5 1.376(6) . ? C5 C6 1.379(5) . ? C6 C7 1.388(5) . ? C8 C9 1.496(5) . ? C9 C14 1.391(5) . ? C9 C10 1.403(5) . ? C10 C11 1.379(5) . ? C11 C12 1.389(6) . ? C12 C13 1.367(6) . ? C13 C14 1.382(6) . ? C16 C17 1.458(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Na1 O3' 160.7(6) 3_565 . ? O1 Na1 O2 81.23(10) 3_565 3_565 ? O3' Na1 O2 102.9(2) . 3_565 ? O1 Na1 O4 100.22(11) 3_565 . ? O3' Na1 O4 71.4(2) . . ? O2 Na1 O4 166.45(18) 3_565 . ? O1 Na1 O2 110.08(14) 3_565 . ? O3' Na1 O2 88.9(6) . . ? O2 Na1 O2 89.17(12) 3_565 . ? O4 Na1 O2 102.80(13) . . ? O1 Na1 O3 142.2(5) 3_565 . ? O3' Na1 O3 18.7(2) . . ? O2 Na1 O3 102.42(18) 3_565 . ? O4 Na1 O3 68.1(2) . . ? O2 Na1 O3 107.6(5) . . ? O1 Na1 Na1 98.05(11) 3_565 3_565 ? O3' Na1 Na1 98.1(4) . 3_565 ? O2 Na1 Na1 45.57(8) 3_565 3_565 ? O4 Na1 Na1 145.96(15) . 3_565 ? O2 Na1 Na1 43.60(8) . 3_565 ? O3 Na1 Na1 111.3(4) . 3_565 ? C8 As1 C1 101.24(14) . . ? C1 O1 Na1 140.3(3) . 3_565 ? C8 O2 Na1 137.0(2) . 3_565 ? C8 O2 Na1 120.4(3) . . ? Na1 O2 Na1 90.83(12) 3_565 . ? C17 O3 C18 112.5(8) . . ? C17 O3 Na1 104.1(10) . . ? C18 O3 Na1 108.7(11) . . ? C17 O3' Na1 118.3(5) . . ? C16 O4 C15 115.3(3) . . ? C16 O4 Na1 117.3(3) . . ? C15 O4 Na1 125.3(3) . . ? O1 C1 C2 117.3(3) . . ? O1 C1 As1 127.6(3) . . ? C2 C1 As1 114.8(2) . . ? C7 C2 C3 119.0(3) . . ? C7 C2 C1 119.0(3) . . ? C3 C2 C1 122.1(3) . . ? C4 C3 C2 120.0(3) . . ? C5 C4 C3 120.3(3) . . ? C4 C5 C6 120.6(3) . . ? C5 C6 C7 119.3(3) . . ? C2 C7 C6 120.9(3) . . ? O2 C8 C9 116.3(3) . . ? O2 C8 As1 127.1(3) . . ? C9 C8 As1 116.6(2) . . ? C14 C9 C10 118.3(4) . . ? C14 C9 C8 119.5(3) . . ? C10 C9 C8 122.2(3) . . ? C11 C10 C9 120.5(4) . . ? C10 C11 C12 120.1(4) . . ? C13 C12 C11 119.9(4) . . ? C12 C13 C14 120.6(4) . . ? C13 C14 C9 120.7(4) . . ? O4 C16 C17 114.9(4) . . ? O3 C17 O3' 36.5(4) . . ? O3 C17 C16 120.4(5) . . ? O3' C17 C16 115.4(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Na1 O2 C8 130.7(3) 3_565 . . . ? O3' Na1 O2 C8 -46.0(3) . . . . ? O2 Na1 O2 C8 -148.9(3) 3_565 . . . ? O4 Na1 O2 C8 24.7(3) . . . . ? O3 Na1 O2 C8 -46.1(3) . . . . ? Na1 Na1 O2 C8 -148.9(3) 3_565 . . . ? O1 Na1 O2 Na1 -80.35(12) 3_565 . . 3_565 ? O3' Na1 O2 Na1 102.9(2) . . . 3_565 ? O2 Na1 O2 Na1 0.0 3_565 . . 3_565 ? O4 Na1 O2 Na1 173.58(13) . . . 3_565 ? O3 Na1 O2 Na1 102.76(19) . . . 3_565 ? O1 Na1 O3 C17 -110.1(11) 3_565 . . . ? O3' Na1 O3 C17 64.6(11) . . . . ? O2 Na1 O3 C17 158.2(10) 3_565 . . . ? O4 Na1 O3 C17 -32.0(9) . . . . ? O2 Na1 O3 C17 65.1(11) . . . . ? Na1 Na1 O3 C17 111.3(9) 3_565 . . . ? O1 Na1 O3 C18 129.8(8) 3_565 . . . ? O3' Na1 O3 C18 -55.6(13) . . . . ? O2 Na1 O3 C18 38.1(10) 3_565 . . . ? O4 Na1 O3 C18 -152.1(10) . . . . ? O2 Na1 O3 C18 -55.0(9) . . . . ? Na1 Na1 O3 C18 -8.8(10) 3_565 . . . ? O1 Na1 O3' C17 -60.3(19) 3_565 . . . ? O2 Na1 O3' C17 -160.8(13) 3_565 . . . ? O4 Na1 O3' C17 6.4(12) . . . . ? O2 Na1 O3' C17 110.3(14) . . . . ? O3 Na1 O3' C17 -70.2(13) . . . . ? Na1 Na1 O3' C17 153.1(13) 3_565 . . . ? O1 Na1 O4 C16 166.3(3) 3_565 . . . ? O3' Na1 O4 C16 4.2(7) . . . . ? O2 Na1 O4 C16 71.3(6) 3_565 . . . ? O2 Na1 O4 C16 -80.2(3) . . . . ? O3 Na1 O4 C16 23.8(6) . . . . ? Na1 Na1 O4 C16 -72.3(4) 3_565 . . . ? O1 Na1 O4 C15 -31.1(4) 3_565 . . . ? O3' Na1 O4 C15 166.8(7) . . . . ? O2 Na1 O4 C15 -126.1(5) 3_565 . . . ? O2 Na1 O4 C15 82.4(4) . . . . ? O3 Na1 O4 C15 -173.6(6) . . . . ? Na1 Na1 O4 C15 90.3(4) 3_565 . . . ? Na1 O1 C1 C2 -171.0(3) 3_565 . . . ? Na1 O1 C1 As1 2.8(6) 3_565 . . . ? C8 As1 C1 O1 8.3(4) . . . . ? C8 As1 C1 C2 -177.8(2) . . . . ? O1 C1 C2 C7 24.4(5) . . . . ? As1 C1 C2 C7 -150.2(3) . . . . ? O1 C1 C2 C3 -156.4(4) . . . . ? As1 C1 C2 C3 29.0(4) . . . . ? C7 C2 C3 C4 1.5(5) . . . . ? C1 C2 C3 C4 -177.8(3) . . . . ? C2 C3 C4 C5 -0.2(6) . . . . ? C3 C4 C5 C6 -1.0(6) . . . . ? C4 C5 C6 C7 1.0(6) . . . . ? C3 C2 C7 C6 -1.5(5) . . . . ? C1 C2 C7 C6 177.8(3) . . . . ? C5 C6 C7 C2 0.2(6) . . . . ? Na1 O2 C8 C9 150.3(3) 3_565 . . . ? Na1 O2 C8 C9 -78.9(4) . . . . ? Na1 O2 C8 As1 -27.0(6) 3_565 . . . ? Na1 O2 C8 As1 103.8(3) . . . . ? C1 As1 C8 O2 3.1(4) . . . . ? C1 As1 C8 C9 -174.1(3) . . . . ? O2 C8 C9 C14 -19.1(5) . . . . ? As1 C8 C9 C14 158.4(3) . . . . ? O2 C8 C9 C10 161.7(4) . . . . ? As1 C8 C9 C10 -20.8(5) . . . . ? C14 C9 C10 C11 0.2(6) . . . . ? C8 C9 C10 C11 179.4(4) . . . . ? C9 C10 C11 C12 -0.9(7) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C11 C12 C13 C14 -0.6(7) . . . . ? C12 C13 C14 C9 -0.2(6) . . . . ? C10 C9 C14 C13 0.4(6) . . . . ? C8 C9 C14 C13 -178.9(4) . . . . ? C15 O4 C16 C17 -177.8(4) . . . . ? Na1 O4 C16 C17 -13.5(6) . . . . ? C18 O3 C17 O3' 64.7(14) . . . . ? Na1 O3 C17 O3' -52.9(12) . . . . ? C18 O3 C17 C16 157.2(10) . . . . ? Na1 O3 C17 C16 39.7(14) . . . . ? Na1 O3' C17 O3 91.8(16) . . . . ? Na1 O3' C17 C16 -15.6(17) . . . . ? O4 C16 C17 O3 -22.2(15) . . . . ? O4 C16 C17 O3' 18.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.487 _refine_diff_density_min -0.863 _refine_diff_density_rms 0.084 data_compound_7 _database_code_CSD 195264 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H20 As Li O3' _chemical_formula_weight 366.2 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' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 8.5317(3) _cell_length_b 9.7835(5) _cell_length_c 11.7665(6) _cell_angle_alpha 112.465(3) _cell_angle_beta 102.759(3) _cell_angle_gamma 96.788(3) _cell_volume 862.55(7) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 376 _exptl_absorpt_coefficient_mu 1.980 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.5881 _exptl_absorpt_correction_T_max 0.6929 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _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 10780 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6662 _reflns_number_gt 6132 _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^)+(0.0352P)^2^+0.8788P] 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 SHELXL _refine_ls_extinction_coef 0.011(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.48(2) _refine_ls_number_reflns 6662 _refine_ls_number_parameters 421 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group As1 As 0.08647(4) 0.07422(3) 0.93327(3) 0.0178(2) Uani 1 1 d . . . As2 As -0.39696(4) -0.62500(3) 0.98176(3) 0.0178(2) Uani 1 1 d . . . O1 O -0.0181(10) -0.2428(8) 0.7638(7) 0.0203(15) Uani 1 1 d . . . O2 O -0.0430(10) -0.1397(8) 1.0223(7) 0.0190(15) Uani 1 1 d . . . O3 O -0.2975(10) -0.3066(8) 1.1520(8) 0.0217(16) Uani 1 1 d . . . O4 O -0.2728(9) -0.4113(8) 0.8949(7) 0.0146(14) Uani 1 1 d . . . C1 C 0.0544(11) -0.1164(12) 0.7846(8) 0.0122(18) Uani 1 1 d U . . C2 C 0.1182(13) -0.0983(11) 0.6795(10) 0.016(2) Uani 1 1 d . . . C3 C 0.2384(13) 0.0299(13) 0.7028(11) 0.022(2) Uani 1 1 d . . . H3 H 0.2807 0.1110 0.7861 0.026 Uiso 1 1 calc R . . C4 C 0.2938(13) 0.0345(14) 0.5995(11) 0.027(3) Uani 1 1 d . . . H4 H 0.3713 0.1220 0.6140 0.032 Uiso 1 1 calc R . . C5 C 0.2418(15) -0.0784(14) 0.4832(11) 0.031(3) Uani 1 1 d . . . H5 H 0.2784 -0.0696 0.4152 0.037 Uiso 1 1 calc R . . C6 C 0.129(2) -0.2159(14) 0.4599(12) 0.043(3) Uani 1 1 d . . . H6 H 0.0997 -0.3033 0.3805 0.051 Uiso 1 1 calc R . . C7 C 0.0649(15) -0.2133(12) 0.5594(11) 0.035(3) Uani 1 1 d . . . H7 H -0.0206 -0.2961 0.5427 0.042 Uiso 1 1 calc R . . C8 C 0.0012(10) -0.0074(10) 1.0390(7) 0.0096(16) Uani 1 1 d . . . C9 C -0.0095(11) 0.1207(11) 1.1629(7) 0.0121(17) Uani 1 1 d . . . C10 C -0.0482(14) 0.2543(12) 1.1751(11) 0.024(2) Uani 1 1 d . . . H10 H -0.0715 0.2764 1.1020 0.029 Uiso 1 1 calc R . . C11 C -0.0546(14) 0.3556(13) 1.2867(12) 0.025(2) Uani 1 1 d . . . H11 H -0.0873 0.4466 1.2913 0.030 Uiso 1 1 calc R . . C12 C -0.0130(15) 0.3297(14) 1.3999(11) 0.027(2) Uani 1 1 d . . . H12 H -0.0156 0.4041 1.4797 0.032 Uiso 1 1 calc R . . C13 C 0.0285(12) 0.2040(11) 1.3937(8) 0.022(2) Uani 1 1 d . . . H13 H 0.0554 0.1868 1.4691 0.027 Uiso 1 1 calc R . . C14 C 0.0339(12) 0.0915(11) 1.2746(10) 0.021(2) Uani 1 1 d . . . H14 H 0.0655 -0.0001 1.2698 0.025 Uiso 1 1 calc R . . C15 C -0.3670(13) -0.4385(12) 1.1352(10) 0.022(2) Uani 1 1 d . . . C16 C -0.4312(14) -0.4504(13) 1.2387(11) 0.020(2) Uani 1 1 d . . . C17 C -0.3778(15) -0.3289(11) 1.3614(9) 0.034(3) Uani 1 1 d . . . H17 H -0.3062 -0.2372 1.3777 0.041 Uiso 1 1 calc R . . C18 C -0.433(2) -0.3478(16) 1.4583(13) 0.044(3) Uani 1 1 d . . . H18 H -0.3839 -0.2749 1.5445 0.053 Uiso 1 1 calc R . . C19 C -0.5523(16) -0.4628(13) 1.4354(11) 0.032(3) Uani 1 1 d . . . H19 H -0.6007 -0.4622 1.5010 0.038 Uiso 1 1 calc R . . C20 C -0.6076(13) -0.5870(11) 1.3127(10) 0.021(2) Uani 1 1 d . . . H20 H -0.6882 -0.6733 1.2962 0.025 Uiso 1 1 calc R . . C21 C -0.5415(13) -0.5796(12) 1.2180(10) 0.019(2) Uani 1 1 d . . . H21 H -0.5720 -0.6646 1.1369 0.023 Uiso 1 1 calc R . . C22 C -0.3133(12) -0.5529(11) 0.8761(10) 0.022(2) Uani 1 1 d . . . C23 C -0.3109(12) -0.6625(12) 0.7515(10) 0.019(2) Uani 1 1 d . . . C24 C -0.3450(12) -0.6410(12) 0.6407(9) 0.022(2) Uani 1 1 d . . . H24 H -0.3709 -0.5478 0.6445 0.026 Uiso 1 1 calc R . . C25 C -0.3434(13) -0.7459(12) 0.5276(10) 0.026(2) Uani 1 1 d . . . H25 H -0.3752 -0.7300 0.4518 0.031 Uiso 1 1 calc R . . C26 C -0.2917(14) -0.8863(11) 0.5221(10) 0.023(2) Uani 1 1 d . . . H26 H -0.2879 -0.9601 0.4424 0.027 Uiso 1 1 calc R . . C27 C -0.2499(13) -0.9116(12) 0.6285(11) 0.020(2) Uani 1 1 d . . . H27 H -0.2154 -1.0017 0.6246 0.024 Uiso 1 1 calc R . . C28 C -0.2585(12) -0.7994(11) 0.7486(9) 0.0137(18) Uani 1 1 d . . . H28 H -0.2301 -0.8149 0.8248 0.016 Uiso 1 1 calc R . . Li1 Li -0.055(2) -0.322(2) 0.876(2) 0.024(4) Uani 1 1 d . . . Li2 Li -0.246(2) -0.2219(19) 1.0385(18) 0.016(3) Uani 1 1 d . . . O1S O 0.0792(9) -0.4695(8) 0.8835(7) 0.0182(15) Uani 1 1 d . . . O2S O -0.3926(10) -0.0852(9) 1.0306(8) 0.0218(16) Uani 1 1 d . . . C1S C 0.2689(14) -0.4895(14) 0.7487(11) 0.033(3) Uani 1 1 d . . . H1S1 H 0.2551 -0.3927 0.7459 0.049 Uiso 1 1 calc R . . H1S2 H 0.2860 -0.5565 0.6681 0.049 Uiso 1 1 calc R . . H1S3 H 0.3646 -0.4712 0.8207 0.049 Uiso 1 1 calc R . . C2S C 0.1201(13) -0.5616(12) 0.7661(9) 0.024(2) Uani 1 1 d . . . H2S1 H 0.1353 -0.6594 0.7683 0.028 Uiso 1 1 calc R . . H2S2 H 0.0254 -0.5842 0.6907 0.028 Uiso 1 1 calc R . . C3S C 0.1796(14) -0.4762(13) 0.9984(11) 0.028(3) Uani 1 1 d . . . H3S1 H 0.2959 -0.4261 1.0168 0.034 Uiso 1 1 calc R . . H3S2 H 0.1751 -0.5835 0.9833 0.034 Uiso 1 1 calc R . . C4S C 0.1186(13) -0.3993(13) 1.1104(10) 0.022(2) Uani 1 1 d . . . H4S1 H 0.1084 -0.2978 1.1178 0.033 Uiso 1 1 calc R . . H4S2 H 0.1967 -0.3907 1.1890 0.033 Uiso 1 1 calc R . . H4S3 H 0.0106 -0.4589 1.0983 0.033 Uiso 1 1 calc R . . C5S C -0.4278(14) -0.1520(14) 0.8071(11) 0.028(3) Uani 1 1 d . . . H5S1 H -0.3107 -0.1068 0.8274 0.041 Uiso 1 1 calc R . . H5S2 H -0.4909 -0.1392 0.7329 0.041 Uiso 1 1 calc R . . H5S3 H -0.4420 -0.2604 0.7869 0.041 Uiso 1 1 calc R . . C6S C -0.4895(14) -0.0739(14) 0.9223(10) 0.024(2) Uani 1 1 d . . . H6S1 H -0.4823 0.0343 0.9395 0.029 Uiso 1 1 calc R . . H6S2 H -0.6063 -0.1224 0.9038 0.029 Uiso 1 1 calc R . . C7S C -0.4141(12) 0.0127(13) 1.1478(11) 0.023(2) Uani 1 1 d . . . H7S1 H -0.4220 0.1123 1.1464 0.028 Uiso 1 1 calc R . . H7S2 H -0.3170 0.0293 1.2195 0.028 Uiso 1 1 calc R . . C8S C -0.5700(13) -0.0538(12) 1.1701(10) 0.026(2) Uani 1 1 d . . . H8S1 H -0.6646 -0.0802 1.0950 0.039 Uiso 1 1 calc R . . H8S2 H -0.5892 0.0212 1.2463 0.039 Uiso 1 1 calc R . . H8S3 H -0.5561 -0.1452 1.1833 0.039 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 As1 0.0218(4) 0.0125(4) 0.0209(5) 0.0078(4) 0.0086(4) 0.0033(3) As2 0.0212(4) 0.0140(4) 0.0199(5) 0.0080(4) 0.0086(4) 0.0019(3) O1 0.024(3) 0.019(3) 0.013(3) 0.003(3) 0.004(3) 0.001(3) O2 0.024(3) 0.014(3) 0.017(3) 0.004(3) 0.007(3) 0.007(3) O3 0.029(4) 0.012(3) 0.033(4) 0.015(3) 0.016(3) 0.003(3) O4 0.012(3) 0.011(3) 0.027(4) 0.014(3) 0.009(3) 0.000(2) C1 0.012(4) 0.022(4) 0.010(3) 0.012(3) 0.007(3) 0.006(3) C2 0.014(4) 0.013(4) 0.020(5) 0.005(4) 0.005(4) 0.007(3) C3 0.018(4) 0.028(5) 0.027(5) 0.018(4) 0.012(4) 0.001(4) C4 0.019(5) 0.041(6) 0.037(6) 0.031(5) 0.013(5) 0.007(5) C5 0.035(6) 0.040(6) 0.036(6) 0.031(5) 0.022(5) 0.006(4) C6 0.074(8) 0.020(4) 0.023(5) -0.005(3) 0.029(5) -0.007(4) C7 0.044(6) 0.034(5) 0.045(6) 0.026(5) 0.030(5) 0.003(4) C8 0.010(3) 0.018(4) 0.005(3) 0.007(3) 0.005(3) 0.008(3) C9 0.015(3) 0.014(4) 0.004(3) 0.001(3) 0.002(2) 0.000(3) C10 0.023(5) 0.024(5) 0.034(5) 0.023(4) 0.006(4) 0.003(4) C11 0.030(5) 0.015(5) 0.025(5) 0.006(4) 0.003(4) 0.007(4) C12 0.028(5) 0.039(6) 0.013(4) 0.012(4) 0.006(3) 0.004(4) C13 0.023(4) 0.023(4) 0.007(3) -0.005(3) 0.002(3) -0.003(3) C14 0.025(5) 0.016(5) 0.035(6) 0.018(4) 0.018(4) 0.010(4) C15 0.019(4) 0.014(4) 0.032(5) 0.011(4) 0.002(4) 0.005(3) C16 0.022(5) 0.024(5) 0.018(5) 0.014(4) 0.009(4) 0.003(4) C17 0.052(6) 0.014(4) 0.014(4) -0.010(3) 0.007(4) -0.009(4) C18 0.054(6) 0.049(7) 0.026(5) 0.015(5) 0.015(5) -0.010(5) C19 0.041(6) 0.030(5) 0.018(5) 0.002(4) 0.013(4) 0.007(4) C20 0.020(5) 0.016(5) 0.023(5) 0.006(4) 0.004(4) 0.002(4) C21 0.020(4) 0.017(4) 0.014(4) 0.004(3) -0.001(3) 0.007(3) C22 0.014(4) 0.009(3) 0.041(5) 0.011(3) 0.004(4) 0.000(3) C23 0.010(3) 0.013(4) 0.040(5) 0.015(3) 0.010(3) 0.006(3) C24 0.019(5) 0.022(5) 0.014(5) 0.002(4) -0.002(4) 0.001(4) C25 0.033(5) 0.027(4) 0.034(5) 0.025(4) 0.014(4) 0.015(4) C26 0.031(5) 0.008(3) 0.027(5) 0.000(3) 0.014(4) 0.008(3) C27 0.020(4) 0.017(4) 0.029(5) 0.009(4) 0.015(4) 0.009(3) C28 0.014(4) 0.011(4) 0.011(3) -0.001(3) 0.005(3) 0.004(3) Li1 0.022(7) 0.023(8) 0.027(8) 0.008(7) 0.013(6) 0.009(6) Li2 0.021(7) 0.008(6) 0.023(7) 0.010(5) 0.008(6) 0.002(5) O1S 0.020(3) 0.016(3) 0.017(3) 0.007(3) 0.001(3) 0.006(3) O2S 0.020(4) 0.027(4) 0.021(4) 0.008(3) 0.011(3) 0.011(3) C1S 0.025(5) 0.054(6) 0.038(6) 0.033(5) 0.015(4) 0.014(4) C2S 0.030(4) 0.023(4) 0.012(4) 0.001(3) 0.006(3) 0.012(3) C3S 0.029(5) 0.026(5) 0.030(5) 0.018(5) -0.003(4) 0.010(4) C4S 0.026(5) 0.025(5) 0.017(5) 0.008(4) 0.011(4) 0.003(4) C5S 0.028(5) 0.029(6) 0.029(6) 0.017(5) 0.003(5) 0.013(4) C6S 0.028(5) 0.031(6) 0.019(4) 0.008(4) 0.014(4) 0.014(4) C7S 0.012(3) 0.023(4) 0.035(5) 0.009(3) 0.015(3) -0.001(2) C8S 0.017(4) 0.024(4) 0.025(5) -0.002(3) 0.008(3) -0.001(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 As1 C8 1.934(8) . ? As1 C1 1.946(10) . ? As2 C22 1.869(10) . ? As2 C15 1.955(11) . ? O1 C1 1.222(13) . ? O1 Li1 1.83(2) . ? O2 C8 1.230(12) . ? O2 Li2 1.903(18) . ? O2 Li1 1.92(2) . ? O3 C15 1.276(13) . ? O3 Li2 1.919(18) . ? O4 C22 1.306(12) . ? O4 Li2 1.918(19) . ? O4 Li1 2.054(19) . ? C1 C2 1.517(13) . ? C1 Li1 2.78(2) . ? C2 C7 1.360(16) . ? C2 C3 1.417(15) . ? C3 C4 1.412(13) . ? C4 C5 1.323(17) . ? C5 C6 1.453(17) . ? C6 C7 1.389(15) . ? C8 C9 1.547(11) . ? C9 C10 1.349(15) . ? C9 C14 1.430(13) . ? C10 C11 1.326(15) . ? C11 C12 1.427(16) . ? C12 C13 1.299(16) . ? C13 C14 1.428(14) . ? C15 C16 1.479(14) . ? C16 C21 1.388(15) . ? C16 C17 1.405(15) . ? C17 C18 1.393(17) . ? C18 C19 1.320(18) . ? C19 C20 1.417(15) . ? C20 C21 1.376(14) . ? C22 C23 1.455(14) . ? C23 C24 1.373(15) . ? C23 C28 1.452(14) . ? C24 C25 1.339(15) . ? C25 C26 1.475(14) . ? C26 C27 1.348(16) . ? C27 C28 1.444(13) . ? Li1 O1S 1.96(2) . ? Li1 Li2 2.759(8) . ? Li2 O2S 1.948(19) . ? O1S C3S 1.461(13) . ? O1S C2S 1.475(12) . ? O2S C6S 1.408(14) . ? O2S C7S 1.413(13) . ? C1S C2S 1.471(15) . ? C3S C4S 1.488(14) . ? C5S C6S 1.522(14) . ? C7S C8S 1.531(13) . ? 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 C8 As1 C1 98.1(4) . . ? C22 As2 C15 102.4(4) . . ? C1 O1 Li1 130.2(9) . . ? C8 O2 Li2 124.6(8) . . ? C8 O2 Li1 128.2(8) . . ? Li2 O2 Li1 92.3(8) . . ? C15 O3 Li2 133.7(10) . . ? C22 O4 Li2 133.2(8) . . ? C22 O4 Li1 122.2(8) . . ? Li2 O4 Li1 87.9(7) . . ? O1 C1 C2 118.0(9) . . ? O1 C1 As1 128.3(7) . . ? C2 C1 As1 113.6(7) . . ? O1 C1 Li1 30.2(6) . . ? C2 C1 Li1 145.0(7) . . ? As1 C1 Li1 100.5(5) . . ? C7 C2 C3 118.4(10) . . ? C7 C2 C1 118.7(9) . . ? C3 C2 C1 122.7(10) . . ? C4 C3 C2 118.6(11) . . ? C5 C4 C3 122.4(10) . . ? C4 C5 C6 119.8(9) . . ? C7 C6 C5 116.7(10) . . ? C2 C7 C6 123.5(10) . . ? O2 C8 C9 118.3(7) . . ? O2 C8 As1 130.4(6) . . ? C9 C8 As1 111.3(6) . . ? C10 C9 C14 118.9(9) . . ? C10 C9 C8 126.9(9) . . ? C14 C9 C8 114.1(8) . . ? C11 C10 C9 121.5(11) . . ? C10 C11 C12 120.9(11) . . ? C13 C12 C11 119.8(10) . . ? C12 C13 C14 120.7(10) . . ? C13 C14 C9 118.0(9) . . ? O3 C15 C16 117.4(10) . . ? O3 C15 As2 124.7(8) . . ? C16 C15 As2 117.8(8) . . ? C21 C16 C17 119.2(10) . . ? C21 C16 C15 121.5(10) . . ? C17 C16 C15 119.3(10) . . ? C18 C17 C16 117.6(10) . . ? C19 C18 C17 122.7(12) . . ? C18 C19 C20 119.8(10) . . ? C21 C20 C19 118.4(9) . . ? C20 C21 C16 121.2(10) . . ? O4 C22 C23 114.4(9) . . ? O4 C22 As2 126.8(8) . . ? C23 C22 As2 118.4(7) . . ? C24 C23 C28 118.9(10) . . ? C24 C23 C22 124.7(10) . . ? C28 C23 C22 116.3(10) . . ? C25 C24 C23 122.7(11) . . ? C24 C25 C26 119.2(10) . . ? C27 C26 C25 120.9(9) . . ? C26 C27 C28 118.9(10) . . ? C27 C28 C23 119.2(10) . . ? O1 Li1 O2 100.3(9) . . ? O1 Li1 O1S 112.2(10) . . ? O2 Li1 O1S 123.6(12) . . ? O1 Li1 O4 129.9(12) . . ? O2 Li1 O4 87.6(8) . . ? O1S Li1 O4 103.2(9) . . ? O1 Li1 Li2 124.2(7) . . ? O2 Li1 Li2 43.6(5) . . ? O1S Li1 Li2 123.2(7) . . ? O4 Li1 Li2 44.0(5) . . ? O1 Li1 C1 19.6(4) . . ? O2 Li1 C1 82.5(7) . . ? O1S Li1 C1 116.8(8) . . ? O4 Li1 C1 137.4(9) . . ? Li2 Li1 C1 114.4(5) . . ? O2 Li2 O4 92.2(8) . . ? O2 Li2 O3 132.6(11) . . ? O4 Li2 O3 96.6(7) . . ? O2 Li2 O2S 107.6(8) . . ? O4 Li2 O2S 121.4(10) . . ? O3 Li2 O2S 107.0(9) . . ? O2 Li2 Li1 44.1(6) . . ? O4 Li2 Li1 48.1(5) . . ? O3 Li2 Li1 126.1(6) . . ? O2S Li2 Li1 125.6(6) . . ? C3S O1S C2S 112.6(8) . . ? C3S O1S Li1 127.4(9) . . ? C2S O1S Li1 118.3(8) . . ? C6S O2S C7S 113.6(8) . . ? C6S O2S Li2 129.2(8) . . ? C7S O2S Li2 117.2(9) . . ? C1S C2S O1S 114.5(9) . . ? O1S C3S C4S 110.4(9) . . ? O2S C6S C5S 109.4(8) . . ? O2S C7S C8S 111.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 O1 C1 C2 158.6(10) . . . . ? Li1 O1 C1 As1 -26.6(17) . . . . ? C8 As1 C1 O1 8.2(10) . . . . ? C8 As1 C1 C2 -176.8(7) . . . . ? C8 As1 C1 Li1 -5.0(6) . . . . ? O1 C1 C2 C7 13.1(15) . . . . ? As1 C1 C2 C7 -162.5(9) . . . . ? Li1 C1 C2 C7 31.7(18) . . . . ? O1 C1 C2 C3 -163.2(10) . . . . ? As1 C1 C2 C3 21.2(12) . . . . ? Li1 C1 C2 C3 -144.6(12) . . . . ? C7 C2 C3 C4 1.8(16) . . . . ? C1 C2 C3 C4 178.1(10) . . . . ? C2 C3 C4 C5 -2.3(17) . . . . ? C3 C4 C5 C6 -3(2) . . . . ? C4 C5 C6 C7 8(2) . . . . ? C3 C2 C7 C6 3.8(19) . . . . ? C1 C2 C7 C6 -172.6(13) . . . . ? C5 C6 C7 C2 -9(2) . . . . ? Li2 O2 C8 C9 49.5(13) . . . . ? Li1 O2 C8 C9 176.7(10) . . . . ? Li2 O2 C8 As1 -130.6(9) . . . . ? Li1 O2 C8 As1 -3.4(15) . . . . ? C1 As1 C8 O2 6.7(10) . . . . ? C1 As1 C8 C9 -173.4(6) . . . . ? O2 C8 C9 C10 -144.4(11) . . . . ? As1 C8 C9 C10 35.8(12) . . . . ? O2 C8 C9 C14 38.3(12) . . . . ? As1 C8 C9 C14 -141.6(7) . . . . ? C14 C9 C10 C11 -3.3(17) . . . . ? C8 C9 C10 C11 179.5(10) . . . . ? C9 C10 C11 C12 2.9(19) . . . . ? C10 C11 C12 C13 -1.4(18) . . . . ? C11 C12 C13 C14 0.4(18) . . . . ? C12 C13 C14 C9 -0.8(16) . . . . ? C10 C9 C14 C13 2.1(14) . . . . ? C8 C9 C14 C13 179.7(9) . . . . ? Li2 O3 C15 C16 -161.5(10) . . . . ? Li2 O3 C15 As2 17.8(18) . . . . ? C22 As2 C15 O3 -3.4(11) . . . . ? C22 As2 C15 C16 175.9(8) . . . . ? O3 C15 C16 C21 164.4(11) . . . . ? As2 C15 C16 C21 -14.9(14) . . . . ? O3 C15 C16 C17 -16.4(16) . . . . ? As2 C15 C16 C17 164.3(9) . . . . ? C21 C16 C17 C18 2.9(19) . . . . ? C15 C16 C17 C18 -176.4(13) . . . . ? C16 C17 C18 C19 -11(2) . . . . ? C17 C18 C19 C20 12(2) . . . . ? C18 C19 C20 C21 -4(2) . . . . ? C19 C20 C21 C16 -4.0(17) . . . . ? C17 C16 C21 C20 4.3(17) . . . . ? C15 C16 C21 C20 -176.5(11) . . . . ? Li2 O4 C22 C23 -177.2(10) . . . . ? Li1 O4 C22 C23 -54.9(13) . . . . ? Li2 O4 C22 As2 11.0(15) . . . . ? Li1 O4 C22 As2 133.3(9) . . . . ? C15 As2 C22 O4 -10.2(10) . . . . ? C15 As2 C22 C23 178.3(8) . . . . ? O4 C22 C23 C24 -31.2(14) . . . . ? As2 C22 C23 C24 141.4(9) . . . . ? O4 C22 C23 C28 144.9(9) . . . . ? As2 C22 C23 C28 -42.5(12) . . . . ? C28 C23 C24 C25 4.9(15) . . . . ? C22 C23 C24 C25 -179.1(11) . . . . ? C23 C24 C25 C26 -4.4(16) . . . . ? C24 C25 C26 C27 1.5(17) . . . . ? C25 C26 C27 C28 0.8(16) . . . . ? C26 C27 C28 C23 -0.3(15) . . . . ? C24 C23 C28 C27 -2.4(15) . . . . ? C22 C23 C28 C27 -178.7(8) . . . . ? C1 O1 Li1 O2 25.3(16) . . . . ? C1 O1 Li1 O1S -107.6(13) . . . . ? C1 O1 Li1 O4 120.8(14) . . . . ? C1 O1 Li1 Li2 65.2(14) . . . . ? C8 O2 Li1 O1 -9.3(14) . . . . ? Li2 O2 Li1 O1 129.6(6) . . . . ? C8 O2 Li1 O1S 116.2(13) . . . . ? Li2 O2 Li1 O1S -104.8(11) . . . . ? C8 O2 Li1 O4 -139.5(8) . . . . ? Li2 O2 Li1 O4 -0.5(12) . . . . ? C8 O2 Li1 Li2 -139.0(14) . . . . ? C8 O2 Li1 C1 -1.0(11) . . . . ? Li2 O2 Li1 C1 137.9(5) . . . . ? C22 O4 Li1 O1 117.2(13) . . . . ? Li2 O4 Li1 O1 -100.9(13) . . . . ? C22 O4 Li1 O2 -141.4(8) . . . . ? Li2 O4 Li1 O2 0.5(12) . . . . ? C22 O4 Li1 O1S -17.5(14) . . . . ? Li2 O4 Li1 O1S 124.5(7) . . . . ? C22 O4 Li1 Li2 -142.0(12) . . . . ? C22 O4 Li1 C1 142.4(11) . . . . ? Li2 O4 Li1 C1 -75.6(15) . . . . ? C2 C1 Li1 O1 -34.1(16) . . . . ? As1 C1 Li1 O1 159.1(14) . . . . ? O1 C1 Li1 O2 -154.9(16) . . . . ? C2 C1 Li1 O2 171.0(12) . . . . ? As1 C1 Li1 O2 4.2(7) . . . . ? O1 C1 Li1 O1S 81.1(14) . . . . ? C2 C1 Li1 O1S 47.0(18) . . . . ? As1 C1 Li1 O1S -119.8(9) . . . . ? O1 C1 Li1 O4 -76.8(17) . . . . ? C2 C1 Li1 O4 -110.9(16) . . . . ? As1 C1 Li1 O4 82.3(13) . . . . ? O1 C1 Li1 Li2 -124.5(13) . . . . ? C2 C1 Li1 Li2 -158.6(11) . . . . ? As1 C1 Li1 Li2 34.6(5) . . . . ? C8 O2 Li2 O4 141.8(7) . . . . ? Li1 O2 Li2 O4 0.6(13) . . . . ? C8 O2 Li2 O3 -117.2(13) . . . . ? Li1 O2 Li2 O3 101.6(13) . . . . ? C8 O2 Li2 O2S 17.7(14) . . . . ? Li1 O2 Li2 O2S -123.4(7) . . . . ? C8 O2 Li2 Li1 141.2(13) . . . . ? C22 O4 Li2 O2 133.8(8) . . . . ? Li1 O4 Li2 O2 -0.5(12) . . . . ? C22 O4 Li2 O3 0.5(14) . . . . ? Li1 O4 Li2 O3 -133.8(6) . . . . ? C22 O4 Li2 O2S -114.0(12) . . . . ? Li1 O4 Li2 O2S 111.6(9) . . . . ? C22 O4 Li2 Li1 134.3(13) . . . . ? C15 O3 Li2 O2 -115.4(15) . . . . ? C15 O3 Li2 O4 -16.3(16) . . . . ? C15 O3 Li2 O2S 109.5(13) . . . . ? C15 O3 Li2 Li1 -57.9(14) . . . . ? O1 Li1 Li2 O2 -66.4(10) . . . . ? O1S Li1 Li2 O2 105.7(14) . . . . ? O4 Li1 Li2 O2 179.2(17) . . . . ? C1 Li1 Li2 O2 -46.8(7) . . . . ? O1 Li1 Li2 O4 114.4(14) . . . . ? O2 Li1 Li2 O4 -179.2(17) . . . . ? O1S Li1 Li2 O4 -73.5(10) . . . . ? C1 Li1 Li2 O4 134.0(12) . . . . ? O1 Li1 Li2 O3 176.8(15) . . . . ? O2 Li1 Li2 O3 -116.8(14) . . . . ? O1S Li1 Li2 O3 -11.1(7) . . . . ? O4 Li1 Li2 O3 62.4(8) . . . . ? C1 Li1 Li2 O3 -163.6(11) . . . . ? O1 Li1 Li2 O2S 11.8(7) . . . . ? O2 Li1 Li2 O2S 78.1(9) . . . . ? O1S Li1 Li2 O2S -176.1(14) . . . . ? O4 Li1 Li2 O2S -102.6(12) . . . . ? C1 Li1 Li2 O2S 31.3(6) . . . . ? O1 Li1 O1S C3S 131.6(11) . . . . ? O2 Li1 O1S C3S 11.5(17) . . . . ? O4 Li1 O1S C3S -84.5(12) . . . . ? Li2 Li1 O1S C3S -41.3(12) . . . . ? C1 Li1 O1S C3S 110.6(11) . . . . ? O1 Li1 O1S C2S -31.9(13) . . . . ? O2 Li1 O1S C2S -152.1(10) . . . . ? O4 Li1 O1S C2S 112.0(9) . . . . ? Li2 Li1 O1S C2S 155.2(7) . . . . ? C1 Li1 O1S C2S -52.9(12) . . . . ? O2 Li2 O2S C6S 80.7(13) . . . . ? O4 Li2 O2S C6S -23.2(15) . . . . ? O3 Li2 O2S C6S -132.3(10) . . . . ? Li1 Li2 O2S C6S 35.1(12) . . . . ? O2 Li2 O2S C7S -102.9(10) . . . . ? O4 Li2 O2S C7S 153.2(9) . . . . ? O3 Li2 O2S C7S 44.1(12) . . . . ? Li1 Li2 O2S C7S -148.5(6) . . . . ? C3S O1S C2S C1S -79.3(12) . . . . ? Li1 O1S C2S C1S 86.6(12) . . . . ? C2S O1S C3S C4S -172.3(9) . . . . ? Li1 O1S C3S C4S 23.4(14) . . . . ? C7S O2S C6S C5S 166.0(9) . . . . ? Li2 O2S C6S C5S -17.4(15) . . . . ? C6S O2S C7S C8S 80.5(12) . . . . ? Li2 O2S C7S C8S -96.4(11) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.647 _refine_diff_density_min -0.559 _refine_diff_density_rms 0.085 data_compound_6 _database_code_CSD 195265 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C18 H20 As Li O4' _chemical_formula_weight 382.20 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'As' 'As' 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.5633(3) _cell_length_b 7.5209(6) _cell_length_c 18.9855(8) _cell_angle_alpha 90.00 _cell_angle_beta 105.605(2) _cell_angle_gamma 90.00 _cell_volume 1727.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method ? _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.984 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.6923 _exptl_absorpt_correction_T_max 0.8262 _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Kappa CCD' _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34967 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_sigmaI/netI 0.0482 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 28.73 _reflns_number_total 4451 _reflns_number_observed 3714 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-92 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 7 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0297P)^2^+0.9423P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.006(1) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4451 _refine_ls_number_parameters 218 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0501 _refine_ls_R_factor_obs 0.0340 _refine_ls_wR_factor_all 0.1102 _refine_ls_wR_factor_obs 0.0683 _refine_ls_goodness_of_fit_all 1.047 _refine_ls_goodness_of_fit_obs 1.085 _refine_ls_restrained_S_all 1.591 _refine_ls_restrained_S_obs 1.085 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group As1 As 0.640356(14) 0.10159(3) 0.200295(10) 0.01368(8) Uani 1 d . . O1 O 0.42148(11) 0.1467(2) 0.10577(7) 0.0168(3) Uani 1 d . . O2 O 0.60027(10) 0.0829(2) 0.04471(7) 0.0127(3) Uani 1 d . . O3 O 0.29982(11) 0.3288(2) -0.02241(7) 0.0185(3) Uani 1 d . . O4 O 0.46657(10) 0.2980(2) -0.08057(7) 0.0173(3) Uani 1 d . . C1 C 0.32489(15) 0.2173(3) 0.21936(10) 0.0153(4) Uani 1 d . . H1 H 0.29186(15) 0.2709(3) 0.17334(10) 0.018 Uiso 1 calc R . C2 C 0.2730(2) 0.2295(3) 0.27506(11) 0.0187(4) Uani 1 d . . H2 H 0.2050(2) 0.2916(3) 0.26732(11) 0.022 Uiso 1 calc R . C3 C 0.3212(2) 0.1503(3) 0.34248(11) 0.0194(4) Uani 1 d . . H3 H 0.2864(2) 0.1595(3) 0.38102(11) 0.023 Uiso 1 calc R . C4 C 0.4197(2) 0.0580(3) 0.35329(11) 0.0184(4) Uani 1 d . . H4 H 0.4516(2) 0.0024(3) 0.39904(11) 0.022 Uiso 1 calc R . C5 C 0.47216(15) 0.0461(3) 0.29775(10) 0.0145(4) Uani 1 d . . H5 H 0.53983(15) -0.0171(3) 0.30572(10) 0.017 Uiso 1 calc R . C6 C 0.42576(15) 0.1267(2) 0.23026(10) 0.0127(4) Uani 1 d . . C7 C 0.48051(15) 0.1237(2) 0.16890(10) 0.0125(4) Uani 1 d . . C8 C 0.66955(14) 0.0886(2) 0.10648(10) 0.0116(3) Uani 1 d . . C9 C 0.78983(14) 0.0890(2) 0.10843(10) 0.0121(3) Uani 1 d . . C10 C 0.8723(2) 0.0316(3) 0.16948(11) 0.0161(4) Uani 1 d . . H10 H 0.8527(2) -0.0100(3) 0.21155(11) 0.019 Uiso 1 calc R . C11 C 0.9827(2) 0.0350(3) 0.16904(11) 0.0191(4) Uani 1 d . . H11 H 1.0382(2) -0.0041(3) 0.21076(11) 0.023 Uiso 1 calc R . C12 C 1.0123(2) 0.0955(3) 0.10770(12) 0.0201(4) Uani 1 d . . H12 H 1.0878(2) 0.0976(3) 0.10747(12) 0.024 Uiso 1 calc R . C13 C 0.9312(2) 0.1527(3) 0.04682(11) 0.0188(4) Uani 1 d . . H13 H 0.9513(2) 0.1944(3) 0.00494(11) 0.023 Uiso 1 calc R . C14 C 0.8210(2) 0.1490(3) 0.04698(10) 0.0159(4) Uani 1 d . . H14 H 0.7660(2) 0.1877(3) 0.00496(10) 0.019 Uiso 1 calc R . C15 C 0.1979(2) 0.3066(3) -0.00424(11) 0.0218(4) Uani 1 d . . H15A H 0.1719(2) 0.4223(3) 0.00810(11) 0.026 Uiso 1 calc R . H15B H 0.2087(2) 0.2265(3) 0.03781(11) 0.026 Uiso 1 calc R . H15C H 0.1429(2) 0.2557(3) -0.04610(11) 0.026 Uiso 1 calc R . C16 C 0.2841(2) 0.3999(3) -0.09423(11) 0.0179(4) Uani 1 d . . H16A H 0.2365(2) 0.5068(3) -0.10065(11) 0.021 Uiso 1 calc R . H16B H 0.2480(2) 0.3107(3) -0.13136(11) 0.021 Uiso 1 calc R . C17 C 0.3954(2) 0.4471(3) -0.10287(11) 0.0202(4) Uani 1 d . . H17A H 0.3898(2) 0.4768(3) -0.15454(11) 0.024 Uiso 1 calc R . H17B H 0.4252(2) 0.5518(3) -0.07232(11) 0.024 Uiso 1 calc R . C18 C 0.5644(2) 0.3133(3) -0.10445(11) 0.0209(4) Uani 1 d . . H18A H 0.6103(2) 0.2074(3) -0.08954(11) 0.025 Uiso 1 calc R . H18B H 0.6057(2) 0.4191(3) -0.08240(11) 0.025 Uiso 1 calc R . H18C H 0.5444(2) 0.3241(3) -0.15785(11) 0.025 Uiso 1 calc R . Li1 Li 0.4406(3) 0.1540(5) 0.0077(2) 0.0169(7) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 As1 0.01040(10) 0.02153(12) 0.00884(10) -0.00046(8) 0.00211(7) 0.00082(8) O1 0.0145(6) 0.0245(8) 0.0107(6) 0.0009(5) 0.0022(5) 0.0043(5) O2 0.0124(6) 0.0140(7) 0.0111(6) -0.0008(5) 0.0021(5) -0.0005(5) O3 0.0151(6) 0.0258(8) 0.0143(6) 0.0048(6) 0.0038(5) 0.0036(6) O4 0.0157(6) 0.0174(7) 0.0200(7) 0.0061(6) 0.0068(5) 0.0028(5) C1 0.0138(8) 0.0170(10) 0.0143(9) -0.0008(7) 0.0025(7) 0.0012(7) C2 0.0137(9) 0.0220(11) 0.0212(10) -0.0027(8) 0.0060(8) 0.0016(7) C3 0.0185(9) 0.0249(11) 0.0185(10) -0.0022(8) 0.0115(8) -0.0026(8) C4 0.0190(9) 0.0224(11) 0.0145(9) 0.0023(8) 0.0056(8) -0.0023(8) C5 0.0136(8) 0.0156(9) 0.0143(9) 0.0012(7) 0.0042(7) 0.0008(7) C6 0.0126(8) 0.0126(9) 0.0133(9) -0.0012(7) 0.0042(7) -0.0016(6) C7 0.0133(8) 0.0104(9) 0.0137(9) -0.0008(7) 0.0033(7) 0.0004(6) C8 0.0131(8) 0.0100(9) 0.0113(8) -0.0006(7) 0.0028(7) 0.0006(7) C9 0.0125(8) 0.0113(9) 0.0129(8) -0.0018(7) 0.0040(7) -0.0007(7) C10 0.0158(9) 0.0156(9) 0.0168(9) 0.0010(8) 0.0045(7) 0.0013(7) C11 0.0124(9) 0.0197(10) 0.0230(10) 0.0013(8) 0.0007(8) 0.0025(7) C12 0.0122(9) 0.0224(10) 0.0270(11) -0.0019(9) 0.0077(8) -0.0006(8) C13 0.0183(9) 0.0211(10) 0.0198(10) 0.0014(8) 0.0098(8) -0.0023(7) C14 0.0149(9) 0.0185(10) 0.0143(9) 0.0024(7) 0.0038(7) 0.0010(7) C15 0.0165(9) 0.0288(12) 0.0215(10) -0.0012(9) 0.0078(8) 0.0019(8) C16 0.0187(9) 0.0172(10) 0.0157(9) 0.0041(8) 0.0010(7) 0.0036(8) C17 0.0242(10) 0.0153(10) 0.0211(10) 0.0073(8) 0.0058(8) 0.0033(8) C18 0.0184(9) 0.0260(12) 0.0200(10) 0.0040(9) 0.0083(8) 0.0001(8) Li1 0.0166(15) 0.020(2) 0.0126(15) -0.0002(13) 0.0017(12) 0.0008(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 As1 C8 1.915(2) . ? As1 C7 1.942(2) . ? O1 C7 1.240(2) . ? O1 Li1 1.942(3) . ? O2 C8 1.259(2) . ? O2 Li1 2.012(3) . ? O2 Li1 2.038(4) 3_655 ? O3 C15 1.423(2) . ? O3 C16 1.428(2) . ? O3 Li1 2.153(4) . ? O4 C18 1.424(2) . ? O4 C17 1.426(2) . ? O4 Li1 2.092(4) . ? C1 C2 1.387(3) . ? C1 C6 1.404(2) . ? C2 C3 1.394(3) . ? C3 C4 1.386(3) . ? C4 C5 1.388(3) . ? C5 C6 1.396(3) . ? C6 C7 1.504(2) . ? C8 C9 1.502(2) . ? C9 C10 1.399(3) . ? C9 C14 1.402(2) . ? C10 C11 1.390(3) . ? C11 C12 1.390(3) . ? C12 C13 1.387(3) . ? C13 C14 1.386(3) . ? C16 C17 1.494(3) . ? Li1 O2 2.038(4) 3_655 ? Li1 Li1 2.814(7) 3_655 ? 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 C8 As1 C7 99.19(7) . . ? C7 O1 Li1 137.3(2) . . ? C8 O2 Li1 133.70(15) . . ? C8 O2 Li1 120.32(15) . 3_655 ? Li1 O2 Li1 88.02(15) . 3_655 ? C15 O3 C16 111.91(15) . . ? C15 O3 Li1 126.3(2) . . ? C16 O3 Li1 112.00(14) . . ? C18 O4 C17 111.56(15) . . ? C18 O4 Li1 129.10(15) . . ? C17 O4 Li1 115.09(14) . . ? C2 C1 C6 120.7(2) . . ? C1 C2 C3 119.7(2) . . ? C4 C3 C2 120.0(2) . . ? C3 C4 C5 120.5(2) . . ? C4 C5 C6 120.2(2) . . ? C5 C6 C1 118.9(2) . . ? C5 C6 C7 122.7(2) . . ? C1 C6 C7 118.4(2) . . ? O1 C7 C6 117.9(2) . . ? O1 C7 As1 127.50(13) . . ? C6 C7 As1 114.47(12) . . ? O2 C8 C9 117.5(2) . . ? O2 C8 As1 127.64(13) . . ? C9 C8 As1 114.85(12) . . ? C10 C9 C14 118.6(2) . . ? C10 C9 C8 122.4(2) . . ? C14 C9 C8 119.0(2) . . ? C11 C10 C9 120.5(2) . . ? C12 C11 C10 120.2(2) . . ? C13 C12 C11 119.9(2) . . ? C14 C13 C12 120.1(2) . . ? C13 C14 C9 120.8(2) . . ? O3 C16 C17 107.5(2) . . ? O4 C17 C16 108.1(2) . . ? O1 Li1 O2 91.49(14) . . ? O1 Li1 O2 111.3(2) . 3_655 ? O2 Li1 O2 91.98(15) . 3_655 ? O1 Li1 O4 150.3(2) . . ? O2 Li1 O4 93.54(14) . . ? O2 Li1 O4 97.75(14) 3_655 . ? O1 Li1 O3 88.11(14) . . ? O2 Li1 O3 157.8(2) . . ? O2 Li1 O3 108.9(2) 3_655 . ? O4 Li1 O3 76.46(12) . . ? O1 Li1 Li1 106.4(2) . 3_655 ? O2 Li1 Li1 46.37(10) . 3_655 ? O2 Li1 Li1 45.61(11) 3_655 3_655 ? O4 Li1 Li1 98.2(2) . 3_655 ? O3 Li1 Li1 153.6(2) . 3_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -0.3(3) . . . . ? C1 C2 C3 C4 -0.8(3) . . . . ? C2 C3 C4 C5 1.1(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C4 C5 C6 C7 177.9(2) . . . . ? C2 C1 C6 C5 1.1(3) . . . . ? C2 C1 C6 C7 -177.7(2) . . . . ? Li1 O1 C7 C6 -178.9(2) . . . . ? Li1 O1 C7 As1 6.3(3) . . . . ? C5 C6 C7 O1 157.8(2) . . . . ? C1 C6 C7 O1 -23.4(3) . . . . ? C5 C6 C7 As1 -26.7(2) . . . . ? C1 C6 C7 As1 152.05(14) . . . . ? C8 As1 C7 O1 -8.5(2) . . . . ? C8 As1 C7 C6 176.55(13) . . . . ? Li1 O2 C8 C9 -157.3(2) . . . . ? Li1 O2 C8 C9 82.5(2) 3_655 . . . ? Li1 O2 C8 As1 21.5(3) . . . . ? Li1 O2 C8 As1 -98.7(2) 3_655 . . . ? C7 As1 C8 O2 -4.7(2) . . . . ? C7 As1 C8 C9 174.05(13) . . . . ? O2 C8 C9 C10 -156.3(2) . . . . ? As1 C8 C9 C10 24.8(2) . . . . ? O2 C8 C9 C14 23.8(3) . . . . ? As1 C8 C9 C14 -155.17(14) . . . . ? C14 C9 C10 C11 0.2(3) . . . . ? C8 C9 C10 C11 -179.7(2) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C10 C11 C12 C13 0.1(3) . . . . ? C11 C12 C13 C14 -0.2(3) . . . . ? C12 C13 C14 C9 0.4(3) . . . . ? C10 C9 C14 C13 -0.4(3) . . . . ? C8 C9 C14 C13 179.5(2) . . . . ? C15 O3 C16 C17 170.4(2) . . . . ? Li1 O3 C16 C17 -41.3(2) . . . . ? C18 O4 C17 C16 164.8(2) . . . . ? Li1 O4 C17 C16 -36.1(2) . . . . ? O3 C16 C17 O4 49.7(2) . . . . ? C7 O1 Li1 O2 5.4(3) . . . . ? C7 O1 Li1 O2 98.1(2) . . . 3_655 ? C7 O1 Li1 O4 -94.4(4) . . . . ? C7 O1 Li1 O3 -152.4(2) . . . . ? C7 O1 Li1 Li1 50.0(3) . . . 3_655 ? C8 O2 Li1 O1 -20.3(3) . . . . ? Li1 O2 Li1 O1 111.4(2) 3_655 . . . ? C8 O2 Li1 O2 -131.7(2) . . . 3_655 ? Li1 O2 Li1 O2 0.0 3_655 . . 3_655 ? C8 O2 Li1 O4 130.4(2) . . . . ? Li1 O2 Li1 O4 -97.89(15) 3_655 . . . ? C8 O2 Li1 O3 68.3(5) . . . . ? Li1 O2 Li1 O3 -160.0(5) 3_655 . . . ? C8 O2 Li1 Li1 -131.7(2) . . . 3_655 ? Li1 O2 Li1 Li1 0.0 3_655 . . 3_655 ? C18 O4 Li1 O1 105.0(4) . . . . ? C17 O4 Li1 O1 -49.6(4) . . . . ? C18 O4 Li1 O2 5.7(2) . . . . ? C17 O4 Li1 O2 -148.86(15) . . . . ? C18 O4 Li1 O2 -86.7(2) . . . 3_655 ? C17 O4 Li1 O2 118.7(2) . . . 3_655 ? C18 O4 Li1 O3 165.6(2) . . . . ? C17 O4 Li1 O3 11.0(2) . . . . ? C18 O4 Li1 Li1 -40.7(3) . . . 3_655 ? C17 O4 Li1 Li1 164.7(2) . . . 3_655 ? C15 O3 Li1 O1 -45.1(2) . . . . ? C16 O3 Li1 O1 172.05(14) . . . . ? C15 O3 Li1 O2 -134.4(4) . . . . ? C16 O3 Li1 O2 82.7(5) . . . . ? C15 O3 Li1 O2 66.8(2) . . . 3_655 ? C16 O3 Li1 O2 -76.1(2) . . . 3_655 ? C15 O3 Li1 O4 160.5(2) . . . . ? C16 O3 Li1 O4 17.6(2) . . . . ? C15 O3 Li1 Li1 79.5(5) . . . 3_655 ? C16 O3 Li1 Li1 -63.3(5) . . . 3_655 ? _refine_diff_density_max 0.444 _refine_diff_density_min -0.453 _refine_diff_density_rms 0.081 data_compound_5 _database_code_CSD 195266 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 Li O3 Sb' _chemical_formula_weight 529.29 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' 'Sb' 'Sb' -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.7360(5) _cell_length_b 17.3904(8) _cell_length_c 12.5818(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.619(3) _cell_angle_gamma 90.00 _cell_volume 2538.9(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used n/a _cell_measurement_theta_min n/a _cell_measurement_theta_max n/a _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1090 _exptl_absorpt_coefficient_mu 0.554 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.8973 _exptl_absorpt_correction_T_max 0.9216 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 20437 _diffrn_reflns_av_R_equivalents 0.0573 _diffrn_reflns_av_sigmaI/netI 0.0870 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.94 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5803 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics RES2INS _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^)+(0.0113P)^2^+4.0900P] 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 SHELXL _refine_ls_extinction_coef 0.0044(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5803 _refine_ls_number_parameters 290 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0777 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.0977 _refine_ls_wR_factor_gt 0.0903 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.053 _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 Sb1 Sb 0.90573(2) 0.197631(14) 0.64632(2) 0.02267(11) Uani 1 1 d . . . O1 O 0.8106(2) 0.03425(15) 0.6107(2) 0.0230(6) Uani 1 1 d . A . O2 O 1.0235(2) 0.07519(14) 0.5307(2) 0.0219(6) Uani 1 1 d . . . O3 O 0.8108(3) 0.04470(19) 0.3471(3) 0.0462(9) Uani 1 1 d . A . C1 C 0.8111(3) 0.0919(2) 0.6684(3) 0.0175(7) Uani 1 1 d . . . C2 C 0.7348(3) 0.0923(2) 0.7579(3) 0.0185(7) Uani 1 1 d . . . C3 C 0.8053(3) 0.1134(2) 0.8674(3) 0.0230(8) Uani 1 1 d . . . H3B H 0.8668 0.0748 0.8872 0.028 Uiso 1 1 calc R . . H3A H 0.8424 0.1642 0.8621 0.028 Uiso 1 1 calc R . . C4 C 0.7267(3) 0.1164(2) 0.9544(3) 0.0266(9) Uani 1 1 d . . . H4 H 0.7731 0.1301 1.0251 0.032 Uiso 1 1 calc R . . C5 C 0.6697(4) 0.0381(3) 0.9632(4) 0.0332(10) Uani 1 1 d . . . H5B H 0.7296 -0.0014 0.9847 0.040 Uiso 1 1 calc R . . H5A H 0.6186 0.0402 1.0190 0.040 Uiso 1 1 calc R . . C6 C 0.5995(4) 0.0163(2) 0.8554(4) 0.0311(9) Uani 1 1 d . . . H6 H 0.5633 -0.0353 0.8614 0.037 Uiso 1 1 calc R . . C7 C 0.6779(3) 0.0137(2) 0.7682(3) 0.0256(9) Uani 1 1 d . . . H7B H 0.7382 -0.0259 0.7868 0.031 Uiso 1 1 calc R . . H7A H 0.6319 -0.0005 0.6985 0.031 Uiso 1 1 calc R . . C8 C 0.6398(3) 0.1533(2) 0.7286(3) 0.0213(8) Uani 1 1 d . . . H8B H 0.6755 0.2043 0.7222 0.026 Uiso 1 1 calc R . . H8A H 0.5937 0.1404 0.6583 0.026 Uiso 1 1 calc R . . C9 C 0.5608(3) 0.1562(2) 0.8155(3) 0.0233(8) Uani 1 1 d . . . H9 H 0.4992 0.1956 0.7956 0.028 Uiso 1 1 calc R . . C10 C 0.6323(3) 0.1776(2) 0.9232(3) 0.0254(9) Uani 1 1 d . . . H10B H 0.5818 0.1806 0.9795 0.030 Uiso 1 1 calc R . . H10A H 0.6684 0.2286 0.9176 0.030 Uiso 1 1 calc R . . C11 C 0.5052(3) 0.0767(2) 0.8238(4) 0.0306(10) Uani 1 1 d . . . H11B H 0.4527 0.0782 0.8784 0.037 Uiso 1 1 calc R . . H11A H 0.4594 0.0628 0.7538 0.037 Uiso 1 1 calc R . . C12 C 1.0244(3) 0.1454(2) 0.5571(3) 0.0175(7) Uani 1 1 d . . . C13 C 1.1236(3) 0.1940(2) 0.5253(3) 0.0172(7) Uani 1 1 d . . . C14 C 1.1252(4) 0.1833(3) 0.4048(3) 0.0340(10) Uani 1 1 d . . . H14B H 1.0518 0.2020 0.3637 0.041 Uiso 1 1 calc R . . H14A H 1.1333 0.1281 0.3885 0.041 Uiso 1 1 calc R . . C15 C 1.2273(4) 0.2289(3) 0.3711(3) 0.0444(13) Uani 1 1 d . . . H15 H 1.2283 0.2219 0.2923 0.053 Uiso 1 1 calc R . . C16 C 1.2146(4) 0.3139(3) 0.3954(4) 0.0441(13) Uani 1 1 d . . . H16B H 1.1416 0.3338 0.3551 0.053 Uiso 1 1 calc R . . H16A H 1.2791 0.3432 0.3726 0.053 Uiso 1 1 calc R . . C17 C 1.2147(4) 0.3248(2) 0.5162(4) 0.0327(10) Uani 1 1 d . . . H17 H 1.2067 0.3806 0.5324 0.039 Uiso 1 1 calc R . . C18 C 1.1122(3) 0.2796(2) 0.5503(4) 0.0308(10) Uani 1 1 d . . . H18B H 1.1113 0.2866 0.6283 0.037 Uiso 1 1 calc R . . H18A H 1.0388 0.2997 0.5111 0.037 Uiso 1 1 calc R . . C19 C 1.2385(3) 0.1643(2) 0.5875(3) 0.0247(8) Uani 1 1 d . . . H19B H 1.2384 0.1705 0.6657 0.030 Uiso 1 1 calc R . . H19A H 1.2472 0.1089 0.5725 0.030 Uiso 1 1 calc R . . C20 C 1.3396(3) 0.2092(3) 0.5538(4) 0.0321(10) Uani 1 1 d . . . H20 H 1.4137 0.1896 0.5944 0.039 Uiso 1 1 calc R . . C21 C 1.3393(4) 0.1980(3) 0.4340(4) 0.0464(13) Uani 1 1 d . . . H21B H 1.3470 0.1426 0.4183 0.056 Uiso 1 1 calc R . . H21A H 1.4057 0.2254 0.4116 0.056 Uiso 1 1 calc R . . C22 C 1.3273(3) 0.2947(3) 0.5763(3) 0.0305(9) Uani 1 1 d . . . H22B H 1.3295 0.3030 0.6544 0.037 Uiso 1 1 calc R . . H22A H 1.3925 0.3233 0.5534 0.037 Uiso 1 1 calc R . . C23 C 0.8390(5) 0.0103(3) 0.2493(4) 0.0463(12) Uani 1 1 d . . . H23A H 0.7701 0.0131 0.1934 0.056 Uiso 1 1 calc R . . H23B H 0.8567 -0.0448 0.2633 0.056 Uiso 1 1 calc R . . C24 C 0.9354(4) 0.0454(3) 0.2070(4) 0.0509(13) Uani 1 1 d . . . H24A H 0.9170 0.0992 0.1882 0.061 Uiso 1 1 calc R . . H24B H 0.9499 0.0174 0.1428 0.061 Uiso 1 1 calc R . . H24C H 1.0043 0.0434 0.2616 0.061 Uiso 1 1 calc R . . C25 C 0.7549(5) 0.1174(3) 0.3318(5) 0.0633(17) Uani 1 1 d . . . C26 C 0.6338(12) 0.0971(11) 0.3743(17) 0.095(7) Uani 0.50 1 d P A 1 H26A H 0.5844 0.0677 0.3191 0.114 Uiso 0.50 1 calc PR A 1 H26B H 0.5948 0.1449 0.3892 0.114 Uiso 0.50 1 calc PR A 1 H26C H 0.6495 0.0665 0.4403 0.114 Uiso 0.50 1 calc PR A 1 Li1 Li 0.8870(5) 0.0142(4) 0.4893(5) 0.0235(14) Uani 1 1 d . . . C26A C 0.6302(12) 0.1112(8) 0.3004(11) 0.051(3) Uani 0.50 1 d P A 2 H26D H 0.6123 0.1057 0.2221 0.061 Uiso 0.50 1 calc PR A 2 H26E H 0.5928 0.1575 0.3230 0.061 Uiso 0.50 1 calc PR A 2 H26F H 0.6017 0.0660 0.3350 0.061 Uiso 0.50 1 calc PR A 2 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 Sb1 0.02128(14) 0.01330(13) 0.03599(17) -0.00562(12) 0.01260(10) -0.00108(11) O1 0.0228(12) 0.0173(13) 0.0309(15) -0.0077(12) 0.0107(11) -0.0047(11) O2 0.0246(13) 0.0112(12) 0.0323(15) -0.0015(11) 0.0118(11) 0.0007(10) O3 0.067(2) 0.0326(18) 0.0359(19) 0.0001(15) -0.0028(16) 0.0134(17) C1 0.0124(15) 0.0156(17) 0.0247(19) 0.0013(16) 0.0038(14) -0.0008(13) C2 0.0182(16) 0.0129(16) 0.0259(19) -0.0042(16) 0.0082(14) -0.0006(14) C3 0.0186(17) 0.025(2) 0.026(2) -0.0009(17) 0.0044(15) 0.0063(15) C4 0.031(2) 0.028(2) 0.021(2) 0.0014(18) 0.0054(16) 0.0071(17) C5 0.041(2) 0.030(2) 0.033(2) 0.0081(19) 0.020(2) 0.0130(19) C6 0.035(2) 0.0215(19) 0.042(2) 0.001(2) 0.0229(19) -0.0051(18) C7 0.0269(19) 0.0168(18) 0.037(2) -0.0032(18) 0.0162(17) -0.0019(15) C8 0.0162(16) 0.0210(19) 0.026(2) -0.0011(16) 0.0026(15) 0.0012(14) C9 0.0200(17) 0.0215(19) 0.030(2) -0.0003(17) 0.0082(16) 0.0073(15) C10 0.0292(19) 0.0211(19) 0.029(2) 0.0001(17) 0.0136(17) 0.0073(16) C11 0.0232(19) 0.033(2) 0.040(2) -0.002(2) 0.0188(18) -0.0031(17) C12 0.0173(16) 0.0153(17) 0.0195(18) 0.0015(15) 0.0012(14) 0.0013(14) C13 0.0178(15) 0.0155(16) 0.0186(17) 0.0026(16) 0.0033(13) -0.0010(14) C14 0.050(2) 0.035(3) 0.0149(18) 0.0051(19) 0.0000(17) -0.022(2) C15 0.067(3) 0.054(3) 0.015(2) -0.005(2) 0.017(2) -0.035(3) C16 0.052(3) 0.043(3) 0.034(2) 0.018(2) -0.005(2) -0.026(2) C17 0.035(2) 0.0163(19) 0.048(3) 0.0011(19) 0.010(2) -0.0096(17) C18 0.0252(19) 0.0190(19) 0.049(3) 0.0019(19) 0.0098(19) -0.0059(16) C19 0.0214(18) 0.030(2) 0.022(2) 0.0077(18) 0.0015(15) -0.0014(16) C20 0.0169(17) 0.041(3) 0.038(2) 0.007(2) 0.0040(16) -0.0052(17) C21 0.051(3) 0.045(3) 0.054(3) -0.011(3) 0.040(2) -0.020(2) C22 0.0261(19) 0.037(2) 0.029(2) 0.000(2) 0.0041(16) -0.0192(19) C23 0.072(3) 0.043(3) 0.023(2) 0.003(2) 0.007(2) 0.004(3) C24 0.050(3) 0.052(3) 0.047(3) -0.006(3) -0.004(2) 0.010(3) C25 0.058(3) 0.047(3) 0.082(4) 0.024(3) 0.004(3) 0.021(3) C26 0.036(6) 0.082(13) 0.170(19) -0.090(15) 0.023(11) -0.006(7) Li1 0.025(3) 0.020(3) 0.025(3) 0.000(3) 0.005(3) 0.002(3) C26A 0.044(6) 0.028(5) 0.076(9) -0.020(7) -0.003(7) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sb1 C12 2.119(4) . ? Sb1 C1 2.187(3) . ? O1 C1 1.236(4) . ? O1 Li1 1.916(7) . ? O2 C12 1.266(4) . ? O2 Li1 1.914(7) 3_756 ? O2 Li1 1.926(7) . ? O3 C25 1.425(6) . ? O3 C23 1.450(6) . ? O3 Li1 1.950(7) . ? C1 C2 1.541(5) . ? C2 C7 1.534(5) . ? C2 C3 1.542(5) . ? C2 C8 1.543(5) . ? C3 C4 1.536(5) . ? C4 C5 1.528(6) . ? C4 C10 1.543(5) . ? C5 C6 1.525(6) . ? C6 C11 1.535(6) . ? C6 C7 1.535(5) . ? C8 C9 1.537(5) . ? C9 C10 1.530(6) . ? C9 C11 1.538(5) . ? C12 C13 1.539(5) . ? C13 C18 1.531(5) . ? C13 C14 1.531(5) . ? C13 C19 1.543(5) . ? C14 C15 1.547(6) . ? C15 C16 1.522(7) . ? C15 C21 1.527(7) . ? C16 C17 1.531(6) . ? C17 C22 1.514(6) . ? C17 C18 1.550(5) . ? C19 C20 1.532(5) . ? C20 C21 1.519(6) . ? C20 C22 1.526(6) . ? C23 C24 1.455(7) . ? C25 C26A 1.462(14) . ? C25 C26 1.631(16) . ? Li1 O2 1.914(7) 3_756 ? Li1 Li1 2.671(12) 3_756 ? 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 C12 Sb1 C1 95.36(13) . . ? C1 O1 Li1 130.8(3) . . ? C12 O2 Li1 146.6(3) . 3_756 ? C12 O2 Li1 125.2(3) . . ? Li1 O2 Li1 88.1(3) 3_756 . ? C25 O3 C23 114.2(4) . . ? C25 O3 Li1 120.3(4) . . ? C23 O3 Li1 122.3(3) . . ? O1 C1 C2 118.7(3) . . ? O1 C1 Sb1 124.4(3) . . ? C2 C1 Sb1 116.8(2) . . ? C7 C2 C3 108.6(3) . . ? C7 C2 C1 111.5(3) . . ? C3 C2 C1 111.2(3) . . ? C7 C2 C8 108.9(3) . . ? C3 C2 C8 108.7(3) . . ? C1 C2 C8 107.9(3) . . ? C4 C3 C2 110.2(3) . . ? C5 C4 C3 109.8(3) . . ? C5 C4 C10 109.2(3) . . ? C3 C4 C10 109.0(3) . . ? C6 C5 C4 110.0(3) . . ? C5 C6 C11 109.4(3) . . ? C5 C6 C7 110.0(3) . . ? C11 C6 C7 108.7(3) . . ? C2 C7 C6 110.5(3) . . ? C9 C8 C2 110.1(3) . . ? C10 C9 C8 109.2(3) . . ? C10 C9 C11 109.9(3) . . ? C8 C9 C11 109.0(3) . . ? C9 C10 C4 109.6(3) . . ? C6 C11 C9 109.6(3) . . ? O2 C12 C13 116.0(3) . . ? O2 C12 Sb1 124.9(3) . . ? C13 C12 Sb1 119.0(2) . . ? C18 C13 C14 109.6(3) . . ? C18 C13 C12 112.8(3) . . ? C14 C13 C12 108.3(3) . . ? C18 C13 C19 108.5(3) . . ? C14 C13 C19 108.8(3) . . ? C12 C13 C19 108.8(3) . . ? C13 C14 C15 109.6(3) . . ? C16 C15 C21 109.9(4) . . ? C16 C15 C14 109.8(4) . . ? C21 C15 C14 108.6(4) . . ? C15 C16 C17 109.5(4) . . ? C22 C17 C16 108.9(4) . . ? C22 C17 C18 110.0(3) . . ? C16 C17 C18 109.1(4) . . ? C13 C18 C17 109.9(3) . . ? C20 C19 C13 110.1(3) . . ? C21 C20 C22 108.8(4) . . ? C21 C20 C19 108.8(3) . . ? C22 C20 C19 110.3(3) . . ? C20 C21 C15 110.1(4) . . ? C17 C22 C20 110.1(3) . . ? O3 C23 C24 115.2(4) . . ? O3 C25 C26A 113.1(7) . . ? O3 C25 C26 99.7(8) . . ? C26A C25 C26 35.5(8) . . ? O2 Li1 O1 125.8(4) 3_756 . ? O2 Li1 O2 91.9(3) 3_756 . ? O1 Li1 O2 98.9(3) . . ? O2 Li1 O3 106.6(3) 3_756 . ? O1 Li1 O3 118.5(3) . . ? O2 Li1 O3 110.3(3) . . ? O2 Li1 Li1 46.1(2) 3_756 3_756 ? O1 Li1 Li1 122.0(4) . 3_756 ? O2 Li1 Li1 45.7(2) . 3_756 ? O3 Li1 Li1 117.0(4) . 3_756 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Li1 O1 C1 C2 176.9(3) . . . . ? Li1 O1 C1 Sb1 0.7(5) . . . . ? C12 Sb1 C1 O1 -21.4(3) . . . . ? C12 Sb1 C1 C2 162.4(3) . . . . ? O1 C1 C2 C7 6.2(5) . . . . ? Sb1 C1 C2 C7 -177.4(2) . . . . ? O1 C1 C2 C3 127.6(3) . . . . ? Sb1 C1 C2 C3 -56.0(3) . . . . ? O1 C1 C2 C8 -113.3(4) . . . . ? Sb1 C1 C2 C8 63.1(3) . . . . ? C7 C2 C3 C4 -59.1(4) . . . . ? C1 C2 C3 C4 177.9(3) . . . . ? C8 C2 C3 C4 59.3(4) . . . . ? C2 C3 C4 C5 59.5(4) . . . . ? C2 C3 C4 C10 -60.0(4) . . . . ? C3 C4 C5 C6 -59.0(4) . . . . ? C10 C4 C5 C6 60.5(4) . . . . ? C4 C5 C6 C11 -60.6(4) . . . . ? C4 C5 C6 C7 58.8(4) . . . . ? C3 C2 C7 C6 58.9(4) . . . . ? C1 C2 C7 C6 -178.3(3) . . . . ? C8 C2 C7 C6 -59.4(4) . . . . ? C5 C6 C7 C2 -59.3(4) . . . . ? C11 C6 C7 C2 60.5(4) . . . . ? C7 C2 C8 C9 58.9(4) . . . . ? C3 C2 C8 C9 -59.3(4) . . . . ? C1 C2 C8 C9 -180.0(3) . . . . ? C2 C8 C9 C10 60.4(4) . . . . ? C2 C8 C9 C11 -59.8(4) . . . . ? C8 C9 C10 C4 -60.5(4) . . . . ? C11 C9 C10 C4 59.0(4) . . . . ? C5 C4 C10 C9 -59.6(4) . . . . ? C3 C4 C10 C9 60.4(4) . . . . ? C5 C6 C11 C9 59.3(4) . . . . ? C7 C6 C11 C9 -60.8(4) . . . . ? C10 C9 C11 C6 -59.0(4) . . . . ? C8 C9 C11 C6 60.7(4) . . . . ? Li1 O2 C12 C13 34.8(7) 3_756 . . . ? Li1 O2 C12 C13 -146.1(3) . . . . ? Li1 O2 C12 Sb1 -142.3(5) 3_756 . . . ? Li1 O2 C12 Sb1 36.8(5) . . . . ? C1 Sb1 C12 O2 1.9(3) . . . . ? C1 Sb1 C12 C13 -175.1(3) . . . . ? O2 C12 C13 C18 174.4(3) . . . . ? Sb1 C12 C13 C18 -8.3(4) . . . . ? O2 C12 C13 C14 53.0(4) . . . . ? Sb1 C12 C13 C14 -129.8(3) . . . . ? O2 C12 C13 C19 -65.1(4) . . . . ? Sb1 C12 C13 C19 112.2(3) . . . . ? C18 C13 C14 C15 58.9(5) . . . . ? C12 C13 C14 C15 -177.7(4) . . . . ? C19 C13 C14 C15 -59.6(5) . . . . ? C13 C14 C15 C16 -59.7(5) . . . . ? C13 C14 C15 C21 60.5(5) . . . . ? C21 C15 C16 C17 -58.9(5) . . . . ? C14 C15 C16 C17 60.5(5) . . . . ? C15 C16 C17 C22 59.9(5) . . . . ? C15 C16 C17 C18 -60.2(5) . . . . ? C14 C13 C18 C17 -59.3(4) . . . . ? C12 C13 C18 C17 -180.0(3) . . . . ? C19 C13 C18 C17 59.4(4) . . . . ? C22 C17 C18 C13 -59.7(5) . . . . ? C16 C17 C18 C13 59.8(5) . . . . ? C18 C13 C19 C20 -59.5(4) . . . . ? C14 C13 C19 C20 59.7(4) . . . . ? C12 C13 C19 C20 177.4(3) . . . . ? C13 C19 C20 C21 -60.1(5) . . . . ? C13 C19 C20 C22 59.2(4) . . . . ? C22 C20 C21 C15 -59.2(4) . . . . ? C19 C20 C21 C15 61.0(5) . . . . ? C16 C15 C21 C20 59.0(5) . . . . ? C14 C15 C21 C20 -61.2(5) . . . . ? C16 C17 C22 C20 -61.1(4) . . . . ? C18 C17 C22 C20 58.5(5) . . . . ? C21 C20 C22 C17 60.7(4) . . . . ? C19 C20 C22 C17 -58.5(4) . . . . ? C25 O3 C23 C24 73.8(6) . . . . ? Li1 O3 C23 C24 -86.0(5) . . . . ? C23 O3 C25 C26A 84.9(8) . . . . ? Li1 O3 C25 C26A -114.8(8) . . . . ? C23 O3 C25 C26 119.3(8) . . . . ? Li1 O3 C25 C26 -80.4(8) . . . . ? C1 O1 Li1 O2 130.5(4) . . . 3_756 ? C1 O1 Li1 O2 31.8(5) . . . . ? C1 O1 Li1 O3 -87.2(5) . . . . ? C1 O1 Li1 Li1 74.4(6) . . . 3_756 ? C12 O2 Li1 O2 -179.5(4) . . . 3_756 ? Li1 O2 Li1 O2 0.0 3_756 . . 3_756 ? C12 O2 Li1 O1 -52.8(4) . . . . ? Li1 O2 Li1 O1 126.6(4) 3_756 . . . ? C12 O2 Li1 O3 72.1(5) . . . . ? Li1 O2 Li1 O3 -108.5(4) 3_756 . . . ? C12 O2 Li1 Li1 -179.5(4) . . . 3_756 ? C25 O3 Li1 O2 -168.2(4) . . . 3_756 ? C23 O3 Li1 O2 -9.5(5) . . . 3_756 ? C25 O3 Li1 O1 43.0(6) . . . . ? C23 O3 Li1 O1 -158.3(4) . . . . ? C25 O3 Li1 O2 -69.8(5) . . . . ? C23 O3 Li1 O2 88.9(5) . . . . ? C25 O3 Li1 Li1 -119.5(5) . . . 3_756 ? C23 O3 Li1 Li1 39.2(6) . . . 3_756 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.013 _refine_diff_density_min -0.707 _refine_diff_density_rms 0.102