# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1966 data_Compound_1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H69 Na O8 S' _chemical_formula_weight 708.98 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 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 10.598(3) _cell_length_b 16.124(6) _cell_length_c 24.430(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.41(3) _cell_angle_gamma 90.00 _cell_volume 4171.0(24) _cell_formula_units_Z 4 _cell_measurement_temperature 126(2) _cell_measurement_reflns_used 28 _cell_measurement_theta_min 11 _cell_measurement_theta_max 13 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.80 _exptl_crystal_size_min 0.80 _exptl_crystal_density_meas n/d _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method n/d _exptl_crystal_F_000 1552 _exptl_absorpt_coefficient_mu 0.133 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.89 _exptl_absorpt_correction_T_max 0.90 _exptl_special_details ; ? ; _diffrn_ambient_temperature 126(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 'Siemens P4' _diffrn_measurement_method 'Wyckoff' _diffrn_standards_number 3 _diffrn_standards_interval_count 197 _diffrn_standards_interval_time ? _diffrn_standards_decay_% stable _diffrn_reflns_number 8533 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0890 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 25.51 _reflns_number_total 7768 _reflns_number_observed 4511 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens P4' _computing_cell_refinement 'Siemens P4' _computing_data_reduction 'XDISK, SHELXTL-Plus, Siemens (1994)' _computing_structure_solution 'XS-94 (Sheldrick, 1994)' _computing_structure_refinement 'XL-93 (Sheldrick, 1994)' _computing_molecular_graphics 'XP, SHELXTL-Plus, Siemens (1994)' _computing_publication_material 'XCIF, SHELXTL-Plus, Siemens (1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 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^)+(0.0511P)^2^+1.7821P] 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 none,riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0001(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7765 _refine_ls_number_parameters 435 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1277 _refine_ls_R_factor_obs 0.0654 _refine_ls_wR_factor_all 0.1687 _refine_ls_wR_factor_obs 0.1332 _refine_ls_goodness_of_fit_all 1.015 _refine_ls_goodness_of_fit_obs 1.070 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.070 _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 Na1 Na 0.81796(13) 0.66927(10) 0.13872(6) 0.0429(4) Uani 1 d . . S1 S 0.48340(8) 0.35531(5) 0.11654(4) 0.0360(2) Uani 1 d . . C1 C 0.4241(3) 0.2533(2) 0.11323(13) 0.0282(7) Uani 1 d . . C2 C 0.5064(3) 0.1831(2) 0.10835(13) 0.0281(7) Uani 1 d . . C3 C 0.4550(3) 0.1034(2) 0.10468(14) 0.0322(7) Uani 1 d . . H3A H 0.5110(3) 0.0581(2) 0.10016(14) 0.039 Uiso 1 calc R . C4 C 0.3272(3) 0.0865(2) 0.10726(14) 0.0361(8) Uani 1 d . . C5 C 0.2487(3) 0.1548(2) 0.11214(14) 0.0358(8) Uani 1 d . . H5A H 0.1605(3) 0.1451(2) 0.11366(14) 0.043 Uiso 1 calc R . C6 C 0.2909(3) 0.2367(2) 0.11498(13) 0.0294(7) Uani 1 d . . C7 C 0.6522(3) 0.1900(2) 0.10655(14) 0.0312(7) Uani 1 d . . C8 C 0.6908(3) 0.2394(2) 0.05595(14) 0.0373(8) Uani 1 d . . H8A H 0.6513(3) 0.2943(2) 0.05626(14) 0.056 Uiso 1 calc R . H8B H 0.6628(3) 0.2097(2) 0.02261(14) 0.056 Uiso 1 calc R . H8C H 0.7828(3) 0.2455(2) 0.05679(14) 0.056 Uiso 1 calc R . C9 C 0.7081(3) 0.2296(2) 0.15962(15) 0.0393(8) Uani 1 d . . H9A H 0.6694(3) 0.2840(2) 0.16490(15) 0.059 Uiso 1 calc R . H9B H 0.7995(3) 0.2361(2) 0.15689(15) 0.059 Uiso 1 calc R . H9C H 0.6909(3) 0.1937(2) 0.19084(15) 0.059 Uiso 1 calc R . C10 C 0.7181(4) 0.1062(2) 0.1021(2) 0.0481(10) Uani 1 d . . H10A H 0.6974(4) 0.0713(2) 0.1333(2) 0.072 Uiso 1 calc R . H10B H 0.8096(4) 0.1145(2) 0.1021(2) 0.072 Uiso 1 calc R . H10C H 0.6894(4) 0.0788(2) 0.0680(2) 0.072 Uiso 1 calc R . C11 C 0.2722(4) -0.0013(2) 0.1033(2) 0.0489(10) Uani 1 d . . C12 C 0.3739(5) -0.0671(3) 0.0955(3) 0.099(2) Uani 1 d . . H12A H 0.4374(5) -0.0638(3) 0.1258(3) 0.149 Uiso 1 calc R . H12B H 0.4143(5) -0.0574(3) 0.0608(3) 0.149 Uiso 1 calc R . H12C H 0.3350(5) -0.1223(3) 0.0950(3) 0.149 Uiso 1 calc R . C13 C 0.2083(6) -0.0224(3) 0.1564(2) 0.081(2) Uani 1 d . . H13A H 0.2702(6) -0.0186(3) 0.1873(2) 0.122 Uiso 1 calc R . H13B H 0.1744(6) -0.0788(3) 0.1541(2) 0.122 Uiso 1 calc R . H13C H 0.1393(6) 0.0169(3) 0.1619(2) 0.122 Uiso 1 calc R . C14 C 0.1747(5) -0.0076(3) 0.0560(2) 0.076(2) Uani 1 d . . H14A H 0.2147(5) 0.0058(3) 0.0216(2) 0.115 Uiso 1 calc R . H14B H 0.1059(5) 0.0316(3) 0.0618(2) 0.115 Uiso 1 calc R . H14C H 0.1409(5) -0.0641(3) 0.0541(2) 0.115 Uiso 1 calc R . C15 C 0.1894(3) 0.3056(2) 0.1186(2) 0.0366(8) Uani 1 d . . C16 C 0.0542(3) 0.2699(3) 0.1183(2) 0.0564(11) Uani 1 d . . H16A H 0.0385(3) 0.2368(3) 0.0850(2) 0.085 Uiso 1 calc R . H16B H -0.0068(3) 0.3155(3) 0.1190(2) 0.085 Uiso 1 calc R . H16C H 0.0452(3) 0.2347(3) 0.1506(2) 0.085 Uiso 1 calc R . C17 C 0.2063(4) 0.3567(3) 0.1715(2) 0.0475(9) Uani 1 d . . H17A H 0.2051(4) 0.3195(3) 0.2033(2) 0.071 Uiso 1 calc R . H17B H 0.1374(4) 0.3970(3) 0.1734(2) 0.071 Uiso 1 calc R . H17C H 0.2873(4) 0.3861(3) 0.1717(2) 0.071 Uiso 1 calc R . C18 C 0.1908(4) 0.3636(2) 0.0683(2) 0.0472(10) Uani 1 d . . H18A H 0.1797(4) 0.3307(2) 0.0348(2) 0.071 Uiso 1 calc R . H18B H 0.2718(4) 0.3930(2) 0.0682(2) 0.071 Uiso 1 calc R . H18C H 0.1220(4) 0.4040(2) 0.0702(2) 0.071 Uiso 1 calc R . C19 C 0.8034(5) 0.8922(2) 0.0927(2) 0.0651(14) Uani 1 d . . H19A H 0.7588(5) 0.9419(2) 0.0781(2) 0.078 Uiso 1 calc R . H19B H 0.8784(5) 0.8823(2) 0.0707(2) 0.078 Uiso 1 calc R . C20 C 0.8428(5) 0.9049(2) 0.1517(2) 0.0619(13) Uani 1 d . . H20A H 0.8930(5) 0.9565(2) 0.1561(2) 0.074 Uiso 1 calc R . H20B H 0.7676(5) 0.9095(2) 0.1742(2) 0.074 Uiso 1 calc R . C21 C 0.9525(4) 0.8374(2) 0.2251(2) 0.0483(10) Uani 1 d . . H21A H 0.8768(4) 0.8323(2) 0.2472(2) 0.058 Uiso 1 calc R . H21B H 0.9943(4) 0.8909(2) 0.2342(2) 0.058 Uiso 1 calc R . C22 C 1.0410(4) 0.7674(2) 0.2376(2) 0.0470(9) Uani 1 d . . H22A H 1.1164(4) 0.7725(2) 0.2153(2) 0.056 Uiso 1 calc R . H22B H 1.0690(4) 0.7690(2) 0.2767(2) 0.056 Uiso 1 calc R . C23 C 1.0535(4) 0.6223(2) 0.2433(2) 0.0462(9) Uani 1 d . . H23A H 1.0900(4) 0.6325(2) 0.2806(2) 0.055 Uiso 1 calc R . H23B H 1.1237(4) 0.6142(2) 0.2183(2) 0.055 Uiso 1 calc R . C24 C 0.9722(4) 0.5469(2) 0.2431(2) 0.0466(10) Uani 1 d . . H24A H 1.0218(4) 0.4986(2) 0.2569(2) 0.056 Uiso 1 calc R . H24B H 0.9007(4) 0.5554(2) 0.2673(2) 0.056 Uiso 1 calc R . C25 C 0.8483(4) 0.4601(2) 0.1840(2) 0.0443(9) Uani 1 d . . H25A H 0.7755(4) 0.4657(2) 0.2078(2) 0.053 Uiso 1 calc R . H25B H 0.8971(4) 0.4104(2) 0.1958(2) 0.053 Uiso 1 calc R . C26 C 0.8031(4) 0.4510(2) 0.1261(2) 0.0444(9) Uani 1 d . . H26A H 0.8756(4) 0.4445(2) 0.1021(2) 0.053 Uiso 1 calc R . H26B H 0.7484(4) 0.4014(2) 0.1217(2) 0.053 Uiso 1 calc R . C27 C 0.6793(4) 0.5184(2) 0.0573(2) 0.0503(10) Uani 1 d . . H27A H 0.6335(4) 0.4652(2) 0.0525(2) 0.060 Uiso 1 calc R . H27B H 0.7465(4) 0.5205(2) 0.0304(2) 0.060 Uiso 1 calc R . C28 C 0.5908(4) 0.5889(3) 0.0482(2) 0.0552(12) Uani 1 d . . H28A H 0.5518(4) 0.5865(3) 0.0107(2) 0.066 Uiso 1 calc R . H28B H 0.5227(4) 0.5863(3) 0.0747(2) 0.066 Uiso 1 calc R . C29 C 0.5924(4) 0.7340(3) 0.0351(2) 0.0541(11) Uani 1 d . . H29A H 0.5209(4) 0.7459(3) 0.0587(2) 0.065 Uiso 1 calc R . H29B H 0.5580(4) 0.7228(3) -0.0024(2) 0.065 Uiso 1 calc R . C30 C 0.6790(5) 0.8058(3) 0.0348(2) 0.0551(11) Uani 1 d . . H30A H 0.7517(5) 0.7933(3) 0.0120(2) 0.066 Uiso 1 calc R . H30B H 0.6344(5) 0.8549(3) 0.0192(2) 0.066 Uiso 1 calc R . C31 C 0.5760(5) 0.6072(4) 0.2184(2) 0.087(2) Uani 1 d D . H31A H 0.6052(5) 0.5926(4) 0.2562(2) 0.105 Uiso 1 calc R . H31B H 0.5834(5) 0.5575(4) 0.1949(2) 0.105 Uiso 1 calc R . C32 C 0.4428(5) 0.6366(5) 0.2176(3) 0.127(3) Uani 1 d D . H32A H 0.3888(5) 0.6020(5) 0.1926(3) 0.152 Uiso 1 calc R . H32B H 0.4092(5) 0.6340(5) 0.2547(3) 0.152 Uiso 1 calc R . C33 C 0.4459(5) 0.7229(4) 0.1980(3) 0.120(3) Uani 1 d D . H33A H 0.4189(5) 0.7264(4) 0.1587(3) 0.144 Uiso 1 calc R . H33B H 0.3906(5) 0.7589(4) 0.2194(3) 0.144 Uiso 1 calc R . C34 C 0.5795(5) 0.7469(4) 0.2064(2) 0.081(2) Uani 1 d D . H34A H 0.6024(5) 0.7902(4) 0.1799(2) 0.097 Uiso 1 calc R . H34B H 0.5959(5) 0.7685(4) 0.2440(2) 0.097 Uiso 1 calc R . C35 C 1.0463(4) 0.5936(3) 0.0631(2) 0.0662(14) Uani 1 d D . H35A H 1.0156(4) 0.5761(3) 0.0261(2) 0.079 Uiso 1 calc R . H35B H 1.0281(4) 0.5487(3) 0.0894(2) 0.079 Uiso 1 calc R . C36 C 1.1832(4) 0.6105(3) 0.0637(3) 0.112(3) Uani 1 d D . H36A H 1.2294(4) 0.5720(3) 0.0890(3) 0.134 Uiso 1 calc R . H36B H 1.2157(4) 0.6038(3) 0.0266(3) 0.134 Uiso 1 calc R . C37 C 1.1986(4) 0.6967(3) 0.0825(2) 0.0714(15) Uani 1 d D . H37A H 1.2643(4) 0.7256(3) 0.0621(2) 0.086 Uiso 1 calc R . H37B H 1.2215(4) 0.6989(3) 0.1222(2) 0.086 Uiso 1 calc R . C38 C 1.0725(4) 0.7338(3) 0.0707(2) 0.0650(13) Uani 1 d D . H38A H 1.0571(4) 0.7803(3) 0.0960(2) 0.078 Uiso 1 calc R . H38B H 1.0653(4) 0.7548(3) 0.0326(2) 0.078 Uiso 1 calc R . O1 O 0.7221(3) 0.8223(2) 0.08979(11) 0.0522(7) Uani 1 d . . O2 O 0.9169(3) 0.8350(2) 0.16851(11) 0.0485(7) Uani 1 d . . O3 O 0.9786(2) 0.6910(2) 0.22567(10) 0.0379(6) Uani 1 d . . O4 O 0.9259(2) 0.53173(15) 0.18857(10) 0.0393(6) Uani 1 d . . O5 O 0.7337(2) 0.52402(15) 0.11159(11) 0.0416(6) Uani 1 d . . O6 O 0.6608(2) 0.6637(2) 0.05556(11) 0.0442(6) Uani 1 d . . O7 O 0.6496(3) 0.6732(2) 0.19820(14) 0.0701(10) Uani 1 d . . O8 O 0.9857(3) 0.6683(2) 0.07842(13) 0.0549(8) 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 Na1 0.0353(7) 0.0562(9) 0.0377(8) -0.0025(7) 0.0071(6) 0.0007(7) S1 0.0329(4) 0.0286(4) 0.0465(5) 0.0010(4) 0.0040(4) -0.0023(4) C1 0.0246(15) 0.033(2) 0.027(2) 0.0041(13) 0.0003(12) 0.0004(13) C2 0.028(2) 0.031(2) 0.025(2) 0.0017(13) -0.0006(13) 0.0015(13) C3 0.038(2) 0.027(2) 0.031(2) 0.0010(13) 0.0002(14) 0.0008(14) C4 0.043(2) 0.034(2) 0.031(2) 0.0028(14) -0.001(2) -0.0064(15) C5 0.028(2) 0.042(2) 0.036(2) 0.007(2) -0.0003(14) -0.0102(15) C6 0.025(2) 0.035(2) 0.028(2) 0.0024(14) 0.0000(13) 0.0012(13) C7 0.027(2) 0.036(2) 0.031(2) 0.0024(14) 0.0040(13) 0.0038(13) C8 0.031(2) 0.053(2) 0.029(2) 0.002(2) 0.0039(14) 0.001(2) C9 0.028(2) 0.054(2) 0.036(2) 0.007(2) 0.0007(15) -0.003(2) C10 0.040(2) 0.051(2) 0.054(3) 0.003(2) 0.006(2) 0.015(2) C11 0.057(3) 0.036(2) 0.053(3) 0.000(2) -0.003(2) -0.015(2) C12 0.092(4) 0.030(2) 0.175(7) -0.011(3) 0.014(4) -0.013(3) C13 0.117(5) 0.059(3) 0.068(4) 0.010(3) 0.005(3) -0.044(3) C14 0.103(4) 0.057(3) 0.068(3) 0.000(2) -0.021(3) -0.042(3) C15 0.028(2) 0.039(2) 0.042(2) 0.000(2) 0.0023(15) 0.0046(14) C16 0.029(2) 0.062(3) 0.078(3) 0.003(2) 0.003(2) 0.005(2) C17 0.042(2) 0.057(2) 0.044(2) 0.000(2) 0.010(2) 0.013(2) C18 0.045(2) 0.047(2) 0.050(2) 0.008(2) -0.001(2) 0.018(2) C19 0.110(4) 0.035(2) 0.049(3) 0.007(2) -0.003(3) 0.014(2) C20 0.106(4) 0.034(2) 0.045(3) -0.002(2) -0.005(3) 0.009(2) C21 0.069(3) 0.043(2) 0.033(2) -0.006(2) 0.007(2) -0.008(2) C22 0.053(2) 0.054(2) 0.034(2) -0.003(2) -0.001(2) -0.012(2) C23 0.048(2) 0.054(2) 0.035(2) -0.004(2) -0.011(2) 0.007(2) C24 0.061(3) 0.046(2) 0.032(2) 0.005(2) -0.006(2) 0.011(2) C25 0.048(2) 0.035(2) 0.050(2) 0.010(2) 0.003(2) -0.001(2) C26 0.049(2) 0.034(2) 0.050(2) 0.001(2) -0.001(2) -0.008(2) C27 0.059(3) 0.047(2) 0.043(2) -0.003(2) -0.009(2) -0.022(2) C28 0.043(2) 0.078(3) 0.043(2) 0.014(2) -0.015(2) -0.023(2) C29 0.054(2) 0.077(3) 0.031(2) 0.005(2) -0.008(2) 0.024(2) C30 0.083(3) 0.054(2) 0.028(2) 0.007(2) -0.005(2) 0.025(2) C31 0.060(3) 0.121(5) 0.082(4) 0.029(4) 0.022(3) 0.007(3) C32 0.048(3) 0.191(9) 0.144(7) 0.045(6) 0.023(4) 0.001(5) C33 0.063(4) 0.192(8) 0.102(6) -0.032(6) -0.010(4) 0.052(5) C34 0.081(4) 0.106(5) 0.056(3) -0.005(3) 0.014(3) 0.033(3) C35 0.062(3) 0.050(2) 0.088(4) -0.027(2) 0.022(3) -0.014(2) C36 0.061(3) 0.066(4) 0.211(9) -0.031(4) 0.037(4) 0.000(3) C37 0.053(3) 0.087(4) 0.074(4) 0.003(3) 0.001(2) -0.030(3) C38 0.081(3) 0.052(2) 0.065(3) 0.002(2) 0.034(3) -0.004(2) O1 0.077(2) 0.050(2) 0.0299(15) 0.0003(12) 0.0011(14) 0.0126(15) O2 0.074(2) 0.0403(14) 0.0310(14) -0.0041(11) 0.0033(13) 0.0028(13) O3 0.0365(13) 0.0426(14) 0.0341(14) -0.0036(11) -0.0045(11) -0.0005(11) O4 0.0479(15) 0.0379(13) 0.0318(14) 0.0017(10) -0.0020(11) -0.0034(11) O5 0.0468(15) 0.0375(13) 0.040(2) 0.0036(11) -0.0058(12) -0.0077(11) O6 0.0401(14) 0.052(2) 0.040(2) 0.0031(12) -0.0104(11) 0.0020(12) O7 0.044(2) 0.104(3) 0.064(2) 0.006(2) 0.022(2) 0.011(2) O8 0.043(2) 0.057(2) 0.066(2) -0.0076(15) 0.0183(14) -0.0036(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O7 2.349(3) . ? Na1 O8 2.356(3) . ? Na1 O6 2.574(3) . ? Na1 O5 2.583(3) . ? Na1 O3 2.688(3) . ? Na1 O4 2.756(3) . ? Na1 O1 2.907(3) . ? Na1 O2 2.951(3) . ? S1 C1 1.761(3) . ? C1 C6 1.439(4) . ? C1 C2 1.437(4) . ? C2 C3 1.397(4) . ? C2 C7 1.552(4) . ? C3 C4 1.386(5) . ? C4 C5 1.388(5) . ? C4 C11 1.532(5) . ? C5 C6 1.395(4) . ? C6 C15 1.552(4) . ? C7 C10 1.527(5) . ? C7 C8 1.540(4) . ? C7 C9 1.541(5) . ? C11 C14 1.522(6) . ? C11 C13 1.526(6) . ? C11 C12 1.530(6) . ? C15 C17 1.537(5) . ? C15 C18 1.544(5) . ? C15 C16 1.543(5) . ? C19 O1 1.418(5) . ? C19 C20 1.499(6) . ? C20 O2 1.424(5) . ? C21 O2 1.417(4) . ? C21 C22 1.492(5) . ? C22 O3 1.422(4) . ? C23 O3 1.419(4) . ? C23 C24 1.490(5) . ? C24 O4 1.422(4) . ? C25 O4 1.420(4) . ? C25 C26 1.482(5) . ? C26 O5 1.425(4) . ? C27 O5 1.427(4) . ? C27 C28 1.485(6) . ? C28 O6 1.423(4) . ? C29 O6 1.424(4) . ? C29 C30 1.478(6) . ? C30 O1 1.426(4) . ? C31 O7 1.420(6) . ? C31 C32 1.489(5) . ? C32 C33 1.474(5) . ? C33 C34 1.474(5) . ? C34 O7 1.421(6) . ? C35 O8 1.423(5) . ? C35 C36 1.476(4) . ? C36 C37 1.471(4) . ? C37 C38 1.481(4) . ? C38 O8 1.419(5) . ? 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 O7 Na1 O8 178.75(14) . . ? O7 Na1 O6 90.33(12) . . ? O8 Na1 O6 89.23(11) . . ? O7 Na1 O5 85.38(12) . . ? O8 Na1 O5 95.48(11) . . ? O6 Na1 O5 63.92(9) . . ? O7 Na1 O3 88.85(11) . . ? O8 Na1 O3 91.47(11) . . ? O6 Na1 O3 174.49(10) . . ? O5 Na1 O3 121.42(10) . . ? O7 Na1 O4 93.45(12) . . ? O8 Na1 O4 87.76(10) . . ? O6 Na1 O4 124.29(10) . . ? O5 Na1 O4 61.07(9) . . ? O3 Na1 O4 61.20(8) . . ? O7 Na1 O1 88.29(12) . . ? O8 Na1 O1 90.47(11) . . ? O6 Na1 O1 60.12(9) . . ? O5 Na1 O1 123.58(10) . . ? O3 Na1 O1 114.40(9) . . ? O4 Na1 O1 175.20(10) . . ? O7 Na1 O2 95.43(12) . . ? O8 Na1 O2 83.71(10) . . ? O6 Na1 O2 115.98(10) . . ? O5 Na1 O2 179.19(10) . . ? O3 Na1 O2 58.70(8) . . ? O4 Na1 O2 118.89(9) . . ? O1 Na1 O2 56.43(9) . . ? C6 C1 C2 117.1(3) . . ? C6 C1 S1 121.4(2) . . ? C2 C1 S1 121.5(2) . . ? C3 C2 C1 119.6(3) . . ? C3 C2 C7 116.8(3) . . ? C1 C2 C7 123.7(3) . . ? C4 C3 C2 123.8(3) . . ? C3 C4 C5 116.0(3) . . ? C3 C4 C11 123.3(3) . . ? C5 C4 C11 120.7(3) . . ? C4 C5 C6 124.3(3) . . ? C5 C6 C1 119.2(3) . . ? C5 C6 C15 117.3(3) . . ? C1 C6 C15 123.5(3) . . ? C10 C7 C8 105.2(3) . . ? C10 C7 C9 105.4(3) . . ? C8 C7 C9 110.9(3) . . ? C10 C7 C2 113.4(3) . . ? C8 C7 C2 111.0(3) . . ? C9 C7 C2 110.7(3) . . ? C14 C11 C13 108.7(4) . . ? C14 C11 C12 108.5(4) . . ? C13 C11 C12 107.0(4) . . ? C14 C11 C4 110.7(3) . . ? C13 C11 C4 109.5(3) . . ? C12 C11 C4 112.4(4) . . ? C17 C15 C18 109.9(3) . . ? C17 C15 C16 106.3(3) . . ? C18 C15 C16 105.2(3) . . ? C17 C15 C6 112.0(3) . . ? C18 C15 C6 111.0(3) . . ? C16 C15 C6 112.2(3) . . ? O1 C19 C20 107.5(4) . . ? O2 C20 C19 107.3(3) . . ? O2 C21 C22 108.5(3) . . ? O3 C22 C21 109.3(3) . . ? O3 C23 C24 108.7(3) . . ? O4 C24 C23 108.6(3) . . ? O4 C25 C26 108.6(3) . . ? O5 C26 C25 107.3(3) . . ? O5 C27 C28 108.5(3) . . ? O6 C28 C27 107.9(3) . . ? O6 C29 C30 108.6(3) . . ? O1 C30 C29 108.4(3) . . ? O7 C31 C32 106.9(5) . . ? C33 C32 C31 105.7(5) . . ? C34 C33 C32 103.7(5) . . ? O7 C34 C33 105.4(5) . . ? O8 C35 C36 107.2(3) . . ? C37 C36 C35 105.9(4) . . ? C36 C37 C38 103.5(4) . . ? O8 C38 C37 104.9(3) . . ? C19 O1 C30 111.4(3) . . ? C19 O1 Na1 116.9(2) . . ? C30 O1 Na1 108.7(2) . . ? C21 O2 C20 112.3(3) . . ? C21 O2 Na1 110.1(2) . . ? C20 O2 Na1 117.4(2) . . ? C22 O3 C23 111.4(3) . . ? C22 O3 Na1 123.2(2) . . ? C23 O3 Na1 117.7(2) . . ? C25 O4 C24 112.9(3) . . ? C25 O4 Na1 113.1(2) . . ? C24 O4 Na1 113.4(2) . . ? C27 O5 C26 111.2(3) . . ? C27 O5 Na1 114.7(2) . . ? C26 O5 Na1 121.1(2) . . ? C28 O6 C29 112.0(3) . . ? C28 O6 Na1 116.5(2) . . ? C29 O6 Na1 123.5(2) . . ? C31 O7 C34 106.3(4) . . ? C31 O7 Na1 129.6(3) . . ? C34 O7 Na1 121.7(3) . . ? C38 O8 C35 107.0(3) . . ? C38 O8 Na1 126.1(3) . . ? C35 O8 Na1 122.0(3) . . ? _refine_diff_density_max 0.237 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.051 #===END data_Compound_2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C42 H61 K O7 S' _chemical_formula_weight 749.07 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 10.029(2) _cell_length_b 13.819(3) _cell_length_c 15.207(3) _cell_angle_alpha 92.41(3) _cell_angle_beta 91.39(3) _cell_angle_gamma 106.17(3) _cell_volume 2021.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 20 _cell_measurement_theta_min 10 _cell_measurement_theta_max 23 _exptl_crystal_description cube _exptl_crystal_colour colorless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method ? _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.231 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.93 _exptl_absorpt_correction_T_max 0.93 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Rigaku AFC5S' _diffrn_measurement_method 'omega' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.1 _diffrn_reflns_number 4973 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1264 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 0 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 22.50 _reflns_number_total 4973 _reflns_number_observed 2775 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN, Molecular Structure Corporation' _computing_cell_refinement 'TEXSAN, Molecular Structure Corporation' _computing_data_reduction 'XPREP, SHELXTL-Plus, Siemens (1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, SHELXTL-Plus, Siemens (1994)' _computing_publication_material 'XCIF, SHELXTL-Plus, Siemens (1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 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 'w=1/[&Gs&^2&0(Fo&^2&0)+(0.0908P)&^2&0+0.4400P]' _refine_p_factor 'where P=(Fo&^2&0+2Fc&^2&0)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4973 _refine_ls_number_parameters 452 _refine_ls_number_restraints 26 _refine_ls_R_factor_all 0.1509 _refine_ls_R_factor_obs 0.0642 _refine_ls_wR_factor_all 0.1945 _refine_ls_wR_factor_obs 0.1554 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.138 _refine_ls_restrained_S_all 1.037 _refine_ls_restrained_S_obs 1.154 _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 S1 S 0.1531(2) 0.21452(12) 0.22085(12) 0.0483(5) Uani 1 d . . K1 K -0.1742(2) 0.12414(11) 0.22426(10) 0.0495(5) Uani 1 d . . C1 C 0.1583(6) 0.3435(4) 0.2351(4) 0.0322(15) Uani 1 d . . C2 C 0.1562(6) 0.3900(4) 0.3206(4) 0.034(2) Uani 1 d . . C3 C 0.1299(6) 0.4838(4) 0.3276(4) 0.0339(15) Uani 1 d . . H3A H 0.1240(6) 0.5126(4) 0.3854(4) 0.041 Uiso 1 d R . C4 C 0.1125(5) 0.5387(4) 0.2560(4) 0.0297(14) Uani 1 d . . C5 C 0.1325(6) 0.4978(4) 0.1743(4) 0.0332(15) Uani 1 d . . H5A H 0.1264(6) 0.5352(4) 0.1233(4) 0.040 Uiso 1 d R . C6 C 0.1606(6) 0.4053(4) 0.1612(4) 0.0314(14) Uani 1 d . . C7 C 0.1884(6) 0.3444(4) 0.4086(4) 0.038(2) Uani 1 d . . C8 C 0.2049(7) 0.4197(5) 0.4882(4) 0.057(2) Uani 1 d . . H8A H 0.2787(7) 0.4791(5) 0.4782(4) 0.085 Uiso 1 d R . H8B H 0.1197(7) 0.4377(5) 0.4948(4) 0.085 Uiso 1 d R . H8C H 0.2264(7) 0.3901(5) 0.5408(4) 0.085 Uiso 1 d R . C9 C 0.3270(7) 0.3174(5) 0.4034(5) 0.057(2) Uani 1 d . . H9A H 0.3225(7) 0.2696(5) 0.3549(5) 0.085 Uiso 1 d R . H9B H 0.4007(7) 0.3774(5) 0.3951(5) 0.085 Uiso 1 d R . H9C H 0.3447(7) 0.2885(5) 0.4573(5) 0.085 Uiso 1 d R . C10 C 0.0693(7) 0.2509(5) 0.4294(4) 0.055(2) Uani 1 d . . H10A H 0.0551(7) 0.2007(5) 0.3818(4) 0.083 Uiso 1 d R . H10B H 0.0925(7) 0.2234(5) 0.4827(4) 0.083 Uiso 1 d R . H10C H -0.0141(7) 0.2710(5) 0.4367(4) 0.083 Uiso 1 d R . C11 C 0.0757(6) 0.6393(4) 0.2653(4) 0.035(2) Uani 1 d . . C12 C 0.1123(8) 0.6890(5) 0.3576(5) 0.063(2) Uani 1 d . . H12A H 0.0630(8) 0.6438(5) 0.3997(5) 0.095 Uiso 1 d R . H12B H 0.2105(8) 0.7026(5) 0.3693(5) 0.095 Uiso 1 d R . H12C H 0.0869(8) 0.7510(5) 0.3621(5) 0.095 Uiso 1 d R . C13 C -0.0786(7) 0.6215(6) 0.2472(6) 0.078(3) Uani 1 d . . H13A H -0.1292(7) 0.5739(6) 0.2871(6) 0.117 Uiso 1 d R . H13B H -0.1020(7) 0.6840(6) 0.2555(6) 0.117 Uiso 1 d R . H13C H -0.1025(7) 0.5952(6) 0.1877(6) 0.117 Uiso 1 d R . C14 C 0.1568(9) 0.7142(5) 0.2009(5) 0.076(3) Uani 1 d . . H14A H 0.2545(9) 0.7251(5) 0.2126(5) 0.114 Uiso 1 d R . H14B H 0.1333(9) 0.6881(5) 0.1413(5) 0.114 Uiso 1 d R . H14C H 0.1339(9) 0.7769(5) 0.2091(5) 0.114 Uiso 1 d R . C15 C 0.1925(6) 0.3753(4) 0.0673(4) 0.039(2) Uani 1 d . . C16 C 0.2170(8) 0.4635(5) 0.0058(4) 0.059(2) Uani 1 d . . H16A H 0.2933(8) 0.5177(5) 0.0296(4) 0.089 Uiso 1 d R . H16B H 0.2385(8) 0.4421(5) -0.0517(4) 0.089 Uiso 1 d R . H16C H 0.1350(8) 0.4862(5) 0.0016(4) 0.089 Uiso 1 d R . C17 C 0.3282(7) 0.3442(5) 0.0670(4) 0.053(2) Uani 1 d . . H17A H 0.4023(7) 0.3982(5) 0.0934(4) 0.080 Uiso 1 d R . H17B H 0.3171(7) 0.2851(5) 0.1003(4) 0.080 Uiso 1 d R . H17C H 0.3498(7) 0.3298(5) 0.0076(4) 0.080 Uiso 1 d R . C18 C 0.0709(7) 0.2908(5) 0.0251(4) 0.058(2) Uani 1 d . . H18A H 0.0928(7) 0.2728(5) -0.0333(4) 0.087 Uiso 1 d R . H18B H 0.0536(7) 0.2327(5) 0.0602(4) 0.087 Uiso 1 d R . H18C H -0.0103(7) 0.3145(5) 0.0225(4) 0.087 Uiso 1 d R . O1 O -0.1745(4) 0.0180(3) 0.3783(3) 0.0481(12) Uani 1 d . . O2 O -0.2889(4) 0.1643(3) 0.3847(3) 0.0452(11) Uani 1 d . . O3 O -0.3280(4) 0.2621(3) 0.2335(3) 0.0459(11) Uani 1 d . . O4 O -0.2892(4) 0.1758(3) 0.0686(3) 0.0423(11) Uani 1 d . . O5 O -0.1929(4) 0.0204(3) 0.0582(3) 0.0465(11) Uani 1 d . . O6 O -0.1213(4) -0.0635(3) 0.2160(3) 0.0432(11) Uani 1 d . . C19 C -0.2425(6) 0.0282(5) 0.4556(4) 0.042(2) Uani 1 d . . C20 C -0.3038(6) 0.1066(5) 0.4581(5) 0.045(2) Uani 1 d . . C21 C -0.3399(7) 0.2512(5) 0.3891(5) 0.056(2) Uani 1 d . . H21A H -0.3134(7) 0.2873(5) 0.4450(5) 0.067 Uiso 1 d R . H21B H -0.4394(7) 0.2317(5) 0.3824(5) 0.067 Uiso 1 d R . C22 C -0.2816(8) 0.3159(5) 0.3151(5) 0.059(2) Uani 1 d . . H22A H -0.3066(8) 0.3781(5) 0.3181(5) 0.070 Uiso 1 d R . H22B H -0.1822(8) 0.3314(5) 0.3201(5) 0.070 Uiso 1 d R . C23 C -0.2821(7) 0.3209(5) 0.1597(5) 0.053(2) Uani 1 d . . H23A H -0.1828(7) 0.3364(5) 0.1580(5) 0.064 Uiso 1 d R . H23B H -0.3068(7) 0.3831(5) 0.1647(5) 0.064 Uiso 1 d R . C24 C -0.3441(7) 0.2606(5) 0.0769(5) 0.051(2) Uani 1 d . . H24A H -0.4433(7) 0.2381(5) 0.0810(5) 0.062 Uiso 1 d R . H24B H -0.3225(7) 0.3015(5) 0.0268(5) 0.062 Uiso 1 d R . C25 C -0.3326(7) 0.1118(5) -0.0056(4) 0.043(2) Uani 1 d . . C26 C -0.2781(6) 0.0291(5) -0.0107(4) 0.040(2) Uani 1 d . . C27 C -0.1494(7) -0.0704(4) 0.0601(4) 0.048(2) Uani 1 d . . H27A H -0.1060(7) -0.0805(4) 0.0062(4) 0.058 Uiso 1 d R . H27B H -0.2288(7) -0.1273(4) 0.0664(4) 0.058 Uiso 1 d R . C28 C -0.0497(7) -0.0606(5) 0.1371(4) 0.047(2) Uani 1 d . . H28A H -0.0062(7) -0.1143(5) 0.1342(4) 0.057 Uiso 1 d R . H28B H 0.0214(7) 0.0023(5) 0.1354(4) 0.057 Uiso 1 d R . C29 C -0.0295(6) -0.0511(5) 0.2910(4) 0.043(2) Uani 1 d . . H29A H 0.0362(6) 0.0145(5) 0.2923(4) 0.052 Uiso 1 d R . H29B H 0.0208(6) -0.1008(5) 0.2869(4) 0.052 Uiso 1 d R . C30 C -0.1103(7) -0.0620(5) 0.3729(4) 0.046(2) Uani 1 d . . H30A H -0.1789(7) -0.1264(5) 0.3710(4) 0.055 Uiso 1 d R . H30B H -0.0496(7) -0.0571(5) 0.4237(4) 0.055 Uiso 1 d R . C31 C -0.2492(7) -0.0318(5) 0.5256(5) 0.051(2) Uani 1 d . . H31A H -0.2074(7) -0.0864(5) 0.5228(5) 0.062 Uiso 1 d R . C32 C -0.3198(7) -0.0151(6) 0.6003(5) 0.059(2) Uani 1 d . . H32A H -0.3246(7) -0.0565(6) 0.6499(5) 0.071 Uiso 1 d R . C33 C -0.3811(7) 0.0605(6) 0.6025(5) 0.061(2) Uani 1 d . . H33A H -0.4287(7) 0.0722(6) 0.6541(5) 0.073 Uiso 1 d R . C34 C -0.3776(7) 0.1219(5) 0.5308(5) 0.052(2) Uani 1 d . . H34A H -0.4233(7) 0.1743(5) 0.5324(5) 0.062 Uiso 1 d R . C35 C -0.4219(7) 0.1254(5) -0.0722(5) 0.046(2) Uani 1 d . . H35A H -0.4592(7) 0.1823(5) -0.0684(5) 0.055 Uiso 1 d R . C36 C -0.4583(7) 0.0570(6) -0.1424(5) 0.056(2) Uani 1 d . . H36A H -0.5202(7) 0.0662(6) -0.1884(5) 0.067 Uiso 1 d R . C37 C -0.4058(8) -0.0248(5) -0.1483(5) 0.055(2) Uani 1 d . . H37A H -0.4317(8) -0.0721(5) -0.1980(5) 0.066 Uiso 1 d R . C38 C -0.3168(7) -0.0395(5) -0.0828(5) 0.046(2) Uani 1 d . . H38A H -0.2807(7) -0.0969(5) -0.0869(5) 0.055 Uiso 1 d R . O1S O 0.5894(8) 0.7126(6) 0.3396(5) 0.149(3) Uiso 1 d D . C1S C 0.5922(15) 0.7343(8) 0.2484(6) 0.091(5) Uiso 0.75(3) d PD 1 C2S C 0.5405(14) 0.6346(13) 0.1973(6) 0.090(5) Uiso 0.75(3) d PD 1 C3S C 0.5065(10) 0.5548(6) 0.2671(8) 0.059(4) Uiso 0.75(3) d PD 1 C4S C 0.4970(13) 0.6147(8) 0.3517(7) 0.087(5) Uiso 0.75(3) d PD 1 C1S' C 0.5454(25) 0.7583(12) 0.2655(12) 0.039(10) Uiso 0.25(3) d PD 2 C2S' C 0.5518(33) 0.6884(31) 0.1874(6) 0.081(14) Uiso 0.25(3) d PD 2 C3S' C 0.5416(44) 0.5861(22) 0.2263(19) 0.097(17) Uiso 0.25(3) d PD 2 C4S' C 0.5473(38) 0.6049(8) 0.3248(18) 0.088(14) Uiso 0.25(3) d PD 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 S1 0.0620(12) 0.0287(9) 0.0551(12) 0.0013(8) 0.0093(9) 0.0136(8) K1 0.0584(10) 0.0473(9) 0.0526(11) 0.0061(7) 0.0070(8) 0.0300(8) C1 0.035(4) 0.026(3) 0.037(4) -0.001(3) 0.004(3) 0.010(3) C2 0.029(4) 0.036(4) 0.038(4) 0.005(3) -0.001(3) 0.011(3) C3 0.037(4) 0.033(4) 0.032(4) -0.001(3) 0.002(3) 0.012(3) C4 0.025(3) 0.029(3) 0.034(4) 0.002(3) 0.004(3) 0.005(3) C5 0.036(4) 0.031(3) 0.032(4) 0.004(3) 0.001(3) 0.007(3) C6 0.030(3) 0.034(3) 0.029(4) -0.003(3) -0.003(3) 0.010(3) C7 0.042(4) 0.042(4) 0.036(4) 0.010(3) 0.002(3) 0.020(3) C8 0.072(5) 0.060(5) 0.043(5) 0.005(4) -0.006(4) 0.026(4) C9 0.052(5) 0.063(5) 0.061(5) 0.018(4) 0.001(4) 0.022(4) C10 0.060(5) 0.049(4) 0.057(5) 0.021(4) 0.009(4) 0.014(4) C11 0.040(4) 0.031(3) 0.035(4) -0.003(3) 0.003(3) 0.011(3) C12 0.089(6) 0.045(4) 0.060(5) -0.011(4) -0.005(4) 0.028(4) C13 0.049(5) 0.080(6) 0.112(7) -0.020(5) -0.013(5) 0.035(4) C14 0.116(7) 0.042(4) 0.083(6) 0.017(4) 0.032(5) 0.040(5) C15 0.052(4) 0.036(4) 0.035(4) 0.001(3) 0.005(3) 0.021(3) C16 0.086(6) 0.061(5) 0.039(5) 0.003(4) 0.013(4) 0.033(4) C17 0.062(5) 0.061(5) 0.046(5) 0.005(3) 0.014(4) 0.029(4) C18 0.068(5) 0.061(5) 0.048(5) -0.018(4) -0.005(4) 0.027(4) O1 0.047(3) 0.044(3) 0.060(3) 0.017(2) 0.012(2) 0.021(2) O2 0.048(3) 0.038(3) 0.055(3) 0.004(2) 0.006(2) 0.021(2) O3 0.056(3) 0.036(2) 0.047(3) -0.002(2) 0.000(2) 0.015(2) O4 0.042(3) 0.033(2) 0.053(3) 0.000(2) -0.002(2) 0.012(2) O5 0.047(3) 0.043(3) 0.053(3) -0.004(2) -0.001(2) 0.020(2) O6 0.043(3) 0.040(3) 0.048(3) 0.006(2) 0.006(2) 0.013(2) C19 0.034(4) 0.042(4) 0.046(5) -0.001(3) 0.003(3) 0.003(3) C20 0.034(4) 0.044(4) 0.052(5) -0.006(4) -0.002(3) 0.006(3) C21 0.058(5) 0.054(5) 0.058(5) -0.008(4) 0.004(4) 0.023(4) C22 0.070(5) 0.045(4) 0.069(6) 0.001(4) -0.005(4) 0.031(4) C23 0.061(5) 0.042(4) 0.063(5) 0.004(4) 0.004(4) 0.025(4) C24 0.056(4) 0.037(4) 0.066(5) 0.007(4) 0.000(4) 0.020(3) C25 0.044(4) 0.039(4) 0.040(5) 0.009(3) 0.013(4) 0.002(3) C26 0.037(4) 0.037(4) 0.047(5) 0.010(3) 0.009(3) 0.010(3) C27 0.061(5) 0.028(4) 0.059(5) 0.003(3) 0.015(4) 0.017(3) C28 0.050(4) 0.045(4) 0.053(5) 0.004(3) 0.010(4) 0.024(3) C29 0.045(4) 0.036(4) 0.054(5) 0.003(3) -0.001(4) 0.022(3) C30 0.052(4) 0.037(4) 0.052(5) 0.011(3) -0.004(4) 0.016(3) C31 0.045(4) 0.052(4) 0.052(5) 0.009(4) -0.002(4) 0.004(3) C32 0.054(5) 0.071(5) 0.045(5) -0.001(4) 0.003(4) 0.006(4) C33 0.048(5) 0.075(6) 0.045(5) -0.014(4) 0.008(4) -0.003(4) C34 0.045(4) 0.057(5) 0.050(5) -0.015(4) -0.001(4) 0.010(4) C35 0.043(4) 0.045(4) 0.048(5) 0.014(4) 0.007(4) 0.007(3) C36 0.056(5) 0.072(5) 0.037(5) 0.017(4) 0.003(4) 0.010(4) C37 0.066(5) 0.060(5) 0.029(5) 0.003(4) 0.007(4) -0.001(4) C38 0.051(4) 0.035(4) 0.049(5) 0.002(4) 0.015(4) 0.006(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 S1 C1 1.773(5) . ? S1 K1 3.174(2) . ? K1 O3 2.767(4) . ? K1 O6 2.786(4) . ? K1 O4 2.812(4) . ? K1 O1 2.815(4) . ? K1 O2 2.821(4) . ? K1 O5 2.826(4) . ? K1 C29 3.330(6) . ? K1 C23 3.367(7) . ? K1 C28 3.377(6) . ? K1 C22 3.383(7) . ? C1 C2 1.428(8) . ? C1 C6 1.438(8) . ? C2 C3 1.393(7) . ? C2 C7 1.567(8) . ? C3 C4 1.388(8) . ? C4 C5 1.385(7) . ? C4 C11 1.535(8) . ? C5 C6 1.391(7) . ? C6 C15 1.536(8) . ? C7 C8 1.538(8) . ? C7 C9 1.540(8) . ? C7 C10 1.545(8) . ? C11 C13 1.514(8) . ? C11 C12 1.526(8) . ? C11 C14 1.532(8) . ? C15 C16 1.536(8) . ? C15 C17 1.536(8) . ? C15 C18 1.539(8) . ? O1 C19 1.395(7) . ? O1 C30 1.426(7) . ? O2 C20 1.386(7) . ? O2 C21 1.430(7) . ? O3 C22 1.418(8) . ? O3 C23 1.423(7) . ? O4 C25 1.387(7) . ? O4 C24 1.430(7) . ? O5 C26 1.366(7) . ? O5 C27 1.440(7) . ? O6 C28 1.410(7) . ? O6 C29 1.422(7) . ? C19 C31 1.369(9) . ? C19 C20 1.387(9) . ? C20 C34 1.386(9) . ? C21 C22 1.495(9) . ? C23 C24 1.500(9) . ? C25 C35 1.389(9) . ? C25 C26 1.397(8) . ? C26 C38 1.393(8) . ? C27 C28 1.498(9) . ? C29 C30 1.493(8) . ? C31 C32 1.397(9) . ? C32 C33 1.350(10) . ? C33 C34 1.404(9) . ? C35 C36 1.368(9) . ? C36 C37 1.374(9) . ? C37 C38 1.379(9) . ? O1S C1S 1.430(8) . ? O1S C1S' 1.433(8) . ? O1S C4S 1.433(8) . ? O1S C4S' 1.436(8) . ? C1S C2S 1.504(11) . ? C2S C3S 1.54(2) . ? C3S C4S 1.519(11) . ? C1S' C2S' 1.513(11) . ? C2S' C3S' 1.53(2) . ? C3S' C4S' 1.507(11) . ? 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 S1 K1 97.3(2) . . ? O3 K1 O6 158.13(13) . . ? O3 K1 O4 60.56(13) . . ? O6 K1 O4 115.16(14) . . ? O3 K1 O1 114.11(13) . . ? O6 K1 O1 59.83(13) . . ? O4 K1 O1 155.58(13) . . ? O3 K1 O2 59.86(13) . . ? O6 K1 O2 112.70(13) . . ? O4 K1 O2 117.48(13) . . ? O1 K1 O2 54.65(12) . . ? O3 K1 O5 114.13(14) . . ? O6 K1 O5 61.49(13) . . ? O4 K1 O5 54.65(12) . . ? O1 K1 O5 119.29(13) . . ? O2 K1 O5 151.73(13) . . ? O3 K1 S1 116.46(10) . . ? O6 K1 S1 85.41(10) . . ? O4 K1 S1 107.68(10) . . ? O1 K1 S1 96.00(10) . . ? O2 K1 S1 113.98(11) . . ? O5 K1 S1 93.64(10) . . ? O3 K1 C29 158.2(2) . . ? O6 K1 C29 24.91(13) . . ? O4 K1 C29 138.63(14) . . ? O1 K1 C29 44.09(14) . . ? O2 K1 C29 98.39(14) . . ? O5 K1 C29 83.99(14) . . ? S1 K1 C29 72.03(12) . . ? O3 K1 C23 24.41(14) . . ? O6 K1 C23 159.2(2) . . ? O4 K1 C23 44.02(15) . . ? O1 K1 C23 137.53(15) . . ? O2 K1 C23 82.88(15) . . ? O5 K1 C23 98.1(2) . . ? S1 K1 C23 101.23(13) . . ? C29 K1 C23 173.1(2) . . ? O3 K1 C28 158.1(2) . . ? O6 K1 C28 24.10(13) . . ? O4 K1 C28 98.30(15) . . ? O1 K1 C28 82.49(14) . . ? O2 K1 C28 136.54(14) . . ? O5 K1 C28 44.08(14) . . ? S1 K1 C28 73.45(12) . . ? C29 K1 C28 40.8(2) . . ? C23 K1 C28 139.6(2) . . ? O3 K1 C22 24.11(14) . . ? O6 K1 C22 156.5(2) . . ? O4 K1 C22 83.2(2) . . ? O1 K1 C22 97.2(2) . . ? O2 K1 C22 43.77(15) . . ? O5 K1 C22 137.7(2) . . ? S1 K1 C22 103.59(14) . . ? C29 K1 C22 138.0(2) . . ? C23 K1 C22 41.1(2) . . ? C28 K1 C22 177.0(2) . . ? C2 C1 C6 116.9(5) . . ? C2 C1 S1 121.5(4) . . ? C6 C1 S1 121.6(4) . . ? C3 C2 C1 119.0(5) . . ? C3 C2 C7 116.8(5) . . ? C1 C2 C7 124.1(5) . . ? C4 C3 C2 124.1(5) . . ? C5 C4 C3 115.6(5) . . ? C5 C4 C11 121.4(5) . . ? C3 C4 C11 123.0(5) . . ? C4 C5 C6 124.2(5) . . ? C5 C6 C1 118.8(5) . . ? C5 C6 C15 117.4(5) . . ? C1 C6 C15 123.7(5) . . ? C8 C7 C9 106.1(5) . . ? C8 C7 C10 106.4(5) . . ? C9 C7 C10 110.6(5) . . ? C8 C7 C2 112.3(5) . . ? C9 C7 C2 110.1(5) . . ? C10 C7 C2 111.2(5) . . ? C13 C11 C12 108.3(5) . . ? C13 C11 C14 109.4(6) . . ? C12 C11 C14 106.9(5) . . ? C13 C11 C4 109.7(5) . . ? C12 C11 C4 111.8(5) . . ? C14 C11 C4 110.7(5) . . ? C16 C15 C6 112.4(5) . . ? C16 C15 C17 104.9(5) . . ? C6 C15 C17 110.7(5) . . ? C16 C15 C18 106.4(5) . . ? C6 C15 C18 111.2(5) . . ? C17 C15 C18 111.0(5) . . ? C19 O1 C30 116.6(5) . . ? C19 O1 K1 127.1(4) . . ? C30 O1 K1 116.0(3) . . ? C20 O2 C21 117.2(5) . . ? C20 O2 K1 126.4(3) . . ? C21 O2 K1 116.4(4) . . ? C22 O3 C23 112.8(5) . . ? C22 O3 K1 103.1(3) . . ? C23 O3 K1 102.1(3) . . ? C25 O4 C24 116.5(5) . . ? C25 O4 K1 124.9(4) . . ? C24 O4 K1 115.7(4) . . ? C26 O5 C27 117.5(5) . . ? C26 O5 K1 124.6(3) . . ? C27 O5 K1 113.9(4) . . ? C28 O6 C29 111.4(5) . . ? C28 O6 K1 102.1(3) . . ? C29 O6 K1 99.5(3) . . ? C31 C19 C20 120.7(6) . . ? C31 C19 O1 124.4(6) . . ? C20 C19 O1 114.8(6) . . ? O2 C20 C34 124.0(6) . . ? O2 C20 C19 116.3(6) . . ? C34 C20 C19 119.6(7) . . ? O2 C21 C22 108.2(5) . . ? O3 C22 C21 109.6(6) . . ? O3 C22 K1 52.8(3) . . ? C21 C22 K1 89.5(4) . . ? O3 C23 C24 109.1(5) . . ? O3 C23 K1 53.5(3) . . ? C24 C23 K1 89.2(4) . . ? O4 C24 C23 108.0(5) . . ? O4 C25 C35 125.0(6) . . ? O4 C25 C26 114.8(6) . . ? C35 C25 C26 120.2(6) . . ? O5 C26 C38 124.9(6) . . ? O5 C26 C25 116.4(6) . . ? C38 C26 C25 118.7(6) . . ? O5 C27 C28 108.4(5) . . ? O6 C28 C27 109.5(5) . . ? O6 C28 K1 53.8(3) . . ? C27 C28 K1 88.4(3) . . ? O6 C29 C30 109.8(5) . . ? O6 C29 K1 55.6(2) . . ? C30 C29 K1 90.9(3) . . ? O1 C30 C29 107.6(5) . . ? C19 C31 C32 120.0(7) . . ? C33 C32 C31 119.4(7) . . ? C32 C33 C34 121.6(7) . . ? C20 C34 C33 118.5(7) . . ? C36 C35 C25 119.9(7) . . ? C35 C36 C37 120.5(7) . . ? C36 C37 C38 120.4(7) . . ? C37 C38 C26 120.3(6) . . ? C1S O1S C4S 110.3(9) . . ? C1S' O1S C4S' 109.5(9) . . ? O1S C1S C2S 106.6(8) . . ? C1S C2S C3S 105.4(5) . . ? C4S C3S C2S 104.1(5) . . ? O1S C4S C3S 103.8(8) . . ? O1S C1S' C2S' 104.6(8) . . ? C1S' C2S' C3S' 105.1(5) . . ? C4S' C3S' C2S' 105.8(5) . . ? O1S C4S' C3S' 105.6(9) . . ? _refine_diff_density_max 0.513 _refine_diff_density_min -0.354 _refine_diff_density_rms 0.061 #===END data_Compound_3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H69 K O8 S' _chemical_formula_weight 725.09 _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' 0.0181 0.0091 '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' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.3868 1.0657 '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 10.680(5) _cell_length_b 16.110(1) _cell_length_c 24.857(1) _cell_angle_alpha 90.00 _cell_angle_beta 92.72(4) _cell_angle_gamma 90.00 _cell_volume 4271.9(38) _cell_formula_units_Z 4 _cell_measurement_temperature 213(1) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 22 _cell_measurement_theta_max 53 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.127 _exptl_crystal_density_method ? _exptl_crystal_F_000 1584 _exptl_absorpt_coefficient_mu 1.897 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(1) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Siemens R3m/V' _diffrn_measurement_method 'omega' _diffrn_measurement_time 'constant; 15.00&^o&0/min. in &Gw' _diffrn_measurement_range 0.90 _diffrn_standards_number 2 _diffrn_standards_interval_count 198 _diffrn_standards_interval_time ? _diffrn_standards_decay_% No _diffrn_reflns_number 4865 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1031 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.27 _diffrn_reflns_theta_max 52.60 _reflns_number_total 4865 _reflns_number_observed 3214 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Siemens XSCANS' _computing_cell_refinement 'Siemens XSCANS' _computing_data_reduction 'Siemens SHELXTL 5.0' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Siemens SHELXTL 5.0' _computing_publication_material 'Siemens SHELXTL 5.0' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 5 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^)+(0.1528P)^2^+4.9246P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme_1 0.1528 _refine_ls_weighting_scheme_2 4.9246 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef N/A _refine_ls_number_reflns 4860 _refine_ls_number_parameters 438 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_obs 0.0999 _refine_ls_wR_factor_all 0.2788 _refine_ls_wR_factor_obs 0.2416 _refine_ls_goodness_of_fit_all 1.068 _refine_ls_goodness_of_fit_obs 1.171 _refine_ls_restrained_S_all 1.084 _refine_ls_restrained_S_obs 1.169 _refine_ls_shift/esd_max -0.001 _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 K1 K -0.1854(2) 1.82480(9) 0.13951(6) 0.0326(5) Uani 1 d . . S1 S -0.5108(2) 2.14313(10) 0.11904(8) 0.0349(6) Uani 1 d . . C1 C -0.5718(7) 2.2434(4) 0.1152(3) 0.026(2) Uani 1 d . . C2 C -0.7051(6) 2.2599(4) 0.1149(3) 0.023(2) Uani 1 d . . C3 C -0.7458(7) 2.3415(4) 0.1117(3) 0.031(2) Uani 1 d . . H3A H -0.8342(7) 2.3509(4) 0.1138(3) 0.038 Uiso 1 d R . C4 C -0.6700(7) 2.4098(4) 0.1056(3) 0.034(2) Uani 1 d . . C5 C -0.5441(7) 2.3934(4) 0.1057(3) 0.031(2) Uani 1 d . . H5A H -0.4885(7) 2.4399(4) 0.1031(3) 0.037 Uiso 1 d R . C6 C -0.4914(7) 2.3149(4) 0.1088(3) 0.027(2) Uani 1 d . . C7 C -0.8036(7) 2.1897(5) 0.1193(3) 0.039(2) Uani 1 d . . C8 C -0.7882(8) 2.1416(5) 0.1720(3) 0.049(2) Uani 1 d . . H8A H -0.7060(8) 2.1175(5) 0.1752(3) 0.074 Uiso 1 d R . H8B H -0.7991(8) 2.1789(5) 0.2015(3) 0.074 Uiso 1 d R . H8C H -0.8501(8) 2.0985(5) 0.1726(3) 0.074 Uiso 1 d R . C9 C -0.7994(8) 2.1305(5) 0.0710(3) 0.048(2) Uani 1 d . . H9A H -0.7180(8) 2.1053(5) 0.0704(3) 0.073 Uiso 1 d R . H9B H -0.8618(8) 2.0882(5) 0.0744(3) 0.073 Uiso 1 d R . H9C H -0.8161(8) 2.1607(5) 0.0381(3) 0.073 Uiso 1 d R . C10 C -0.9389(7) 2.2262(5) 0.1169(4) 0.057(3) Uani 1 d . . H10A H -0.9992(7) 2.1823(5) 0.1194(4) 0.085 Uiso 1 d R . H10B H -0.9473(7) 2.2643(5) 0.1462(4) 0.085 Uiso 1 d R . H10C H -0.9534(7) 2.2550(5) 0.0833(4) 0.085 Uiso 1 d R . C11 C -0.7254(6) 2.4978(4) 0.1014(3) 0.049(2) Uani 1 d D . C12 C -0.6243(11) 2.5624(6) 0.0954(8) 0.123(9) Uani 0.83(2) d PD 1 H12A H -0.5710(11) 2.5519(6) 0.0662(8) 0.185 Uiso 0.83(2) d PR 1 H12B H -0.6617(11) 2.6163(6) 0.0912(8) 0.185 Uiso 0.83(2) d PR 1 H12C H -0.5756(11) 2.5603(6) 0.1289(8) 0.185 Uiso 0.83(2) d PR 1 C13 C -0.8188(13) 2.5021(7) 0.0539(5) 0.088(6) Uani 0.83(2) d PD 1 H13A H -0.7674(13) 2.4911(7) 0.0241(5) 0.132 Uiso 0.83(2) d PR 1 H13B H -0.8860(13) 2.4625(7) 0.0540(5) 0.132 Uiso 0.83(2) d PR 1 H13C H -0.8529(13) 2.5571(7) 0.0506(5) 0.132 Uiso 0.83(2) d PR 1 C14 C -0.7914(15) 2.5187(7) 0.1521(4) 0.081(5) Uani 0.83(2) d PD 1 H14A H -0.8566(15) 2.4777(7) 0.1527(4) 0.121 Uiso 0.83(2) d PR 1 H14B H -0.7421(15) 2.5168(7) 0.1854(4) 0.121 Uiso 0.83(2) d PR 1 H14C H -0.8281(15) 2.5728(7) 0.1477(4) 0.121 Uiso 0.83(2) d PR 1 C12' C -0.6942(58) 2.5374(31) 0.0486(13) 0.055(17) Uiso 0.17(2) d PD 2 H12D H -0.6392(58) 2.5009(31) 0.0303(13) 0.083 Uiso 0.17(2) d PR 2 H12E H -0.7656(58) 2.5505(31) 0.0252(13) 0.083 Uiso 0.17(2) d PR 2 H12F H -0.6504(58) 2.5875(31) 0.0584(13) 0.083 Uiso 0.17(2) d PR 2 C13' C -0.8669(9) 2.4958(47) 0.0966(38) 0.104(28) Uiso 0.17(2) d PD 2 H13D H -0.8944(9) 2.4805(47) 0.0606(38) 0.156 Uiso 0.17(2) d PR 2 H13E H -0.8952(9) 2.4551(47) 0.1215(38) 0.156 Uiso 0.17(2) d PR 2 H13F H -0.9009(9) 2.5491(47) 0.1051(38) 0.156 Uiso 0.17(2) d PR 2 C14' C -0.6869(55) 2.5463(29) 0.1516(14) 0.052(17) Uiso 0.17(2) d PD 2 H14D H -0.6037(55) 2.5672(29) 0.1476(14) 0.078 Uiso 0.17(2) d PR 2 H14E H -0.7444(55) 2.5919(29) 0.1534(14) 0.078 Uiso 0.17(2) d PR 2 H14F H -0.6890(55) 2.5142(29) 0.1841(14) 0.078 Uiso 0.17(2) d PR 2 C15 C -0.3453(7) 2.3074(4) 0.1086(3) 0.032(2) Uani 1 d . . C16 C -0.2826(8) 2.3936(5) 0.1046(3) 0.047(2) Uiso 1 d . . H16A H -0.1931(8) 2.3878(5) 0.1046(3) 0.071 Uiso 1 d R . H16B H -0.3125(8) 2.4194(5) 0.0716(3) 0.071 Uiso 1 d R . H16C H -0.3043(8) 2.4274(5) 0.1345(3) 0.071 Uiso 1 d R . C17 C -0.3072(7) 2.2593(5) 0.0584(3) 0.038(2) Uani 1 d . . H17A H -0.2176(7) 2.2544(5) 0.0585(3) 0.057 Uiso 1 d R . H17B H -0.3440(7) 2.2049(5) 0.0583(3) 0.057 Uiso 1 d R . H17C H -0.3369(7) 2.2891(5) 0.0269(3) 0.057 Uiso 1 d R . C18 C -0.2884(7) 2.2690(5) 0.1605(3) 0.038(2) Uani 1 d . . H18A H -0.1990(7) 2.2655(5) 0.1585(3) 0.057 Uiso 1 d R . H18B H -0.3083(7) 2.3024(5) 0.1910(3) 0.057 Uiso 1 d R . H18C H -0.3224(7) 2.2143(5) 0.1646(3) 0.057 Uiso 1 d R . O1 O -0.2910(6) 1.6821(3) 0.0899(2) 0.052(2) Uani 1 d . . O2 O -0.0879(6) 1.6664(3) 0.1683(2) 0.046(2) Uani 1 d . . O3 O -0.0250(5) 1.8086(3) 0.2277(2) 0.0395(14) Uani 1 d . . O4 O -0.0714(5) 1.9677(3) 0.1877(2) 0.0369(13) Uani 1 d . . O5 O -0.2674(5) 1.9796(3) 0.1088(2) 0.0376(13) Uani 1 d . . O6 O -0.3407(5) 1.8408(3) 0.0510(2) 0.0415(14) Uani 1 d . . C19 C -0.3303(10) 1.6976(5) 0.0350(3) 0.058(3) Uani 1 d . . H19A H -0.3748(10) 1.6503(5) 0.0205(3) 0.069 Uiso 1 d R . H19B H -0.2592(10) 1.7075(5) 0.0137(3) 0.069 Uiso 1 d R . C20 C -0.4119(8) 1.7713(6) 0.0333(4) 0.058(3) Uani 1 d . . H20A H -0.4455(8) 1.7807(6) -0.0026(4) 0.070 Uiso 1 d R . H20B H -0.4804(8) 1.7630(6) 0.0564(4) 0.070 Uiso 1 d R . C21 C -0.4038(8) 1.9179(5) 0.0430(4) 0.055(3) Uani 1 d . . H21A H -0.4718(8) 1.9214(5) 0.0668(4) 0.066 Uiso 1 d R . H21B H -0.4376(8) 1.9213(5) 0.0066(4) 0.066 Uiso 1 d R . C22 C -0.3155(8) 1.9859(5) 0.0547(3) 0.048(2) Uani 1 d . . H22A H -0.2481(8) 1.9831(5) 0.0305(3) 0.057 Uiso 1 d R . H22B H -0.3575(8) 2.0381(5) 0.0494(3) 0.057 Uiso 1 d R . C23 C -0.1896(8) 2.0481(4) 0.1242(4) 0.048(2) Uani 1 d . . H23A H -0.2354(8) 2.0989(4) 0.1185(4) 0.057 Uiso 1 d R . H23B H -0.1177(8) 2.0492(4) 0.1025(4) 0.057 Uiso 1 d R . C24 C -0.1468(8) 2.0399(5) 0.1817(3) 0.043(2) Uani 1 d . . H24A H -0.1011(8) 2.0884(5) 0.1936(3) 0.051 Uiso 1 d R . H24B H -0.2192(8) 2.0347(5) 0.2029(3) 0.051 Uiso 1 d R . C25 C -0.0322(9) 1.9529(5) 0.2413(3) 0.049(2) Uani 1 d . . H25A H -0.1050(9) 1.9426(5) 0.2615(3) 0.059 Uiso 1 d R . H25B H 0.0114(9) 2.0001(5) 0.2567(3) 0.059 Uiso 1 d R . C26 C 0.0486(8) 1.8766(5) 0.2442(3) 0.050(2) Uani 1 d . . H26A H 0.1153(8) 1.8838(5) 0.2200(3) 0.060 Uiso 1 d R . H26B H 0.0844(8) 1.8680(5) 0.2799(3) 0.060 Uiso 1 d R . C27 C 0.0358(8) 1.7309(5) 0.2364(3) 0.051(2) Uani 1 d . . H27A H 0.0653(8) 1.7268(5) 0.2734(3) 0.061 Uiso 1 d R . H27B H 0.1068(8) 1.7270(5) 0.2142(3) 0.061 Uiso 1 d R . C28 C -0.0510(9) 1.6633(5) 0.2237(3) 0.051(2) Uani 1 d . . H28A H -0.0122(9) 1.6107(5) 0.2319(3) 0.061 Uiso 1 d R . H28B H -0.1232(9) 1.6686(5) 0.2449(3) 0.061 Uiso 1 d R . C29 C -0.1700(11) 1.6001(5) 0.1517(4) 0.075(3) Uani 1 d . . H29A H -0.2429(11) 1.6001(5) 0.1728(4) 0.090 Uiso 1 d R . H29B H -0.1282(11) 1.5477(5) 0.1567(4) 0.090 Uiso 1 d R . C30 C -0.2087(11) 1.6123(5) 0.0944(4) 0.073(3) Uani 1 d . . H30A H -0.1361(11) 1.6212(5) 0.0738(4) 0.088 Uiso 1 d R . H30B H -0.2520(11) 1.5640(5) 0.0807(4) 0.088 Uiso 1 d R . O7 O -0.3832(8) 1.8462(6) 0.2047(4) 0.129(4) Uani 1 d D . C31 C -0.4408(16) 1.9220(10) 0.2143(8) 0.101(7) Uiso 0.68(2) d PD 1 H31A H -0.4188(16) 1.9625(10) 0.1874(8) 0.151 Uiso 0.68(2) calc PR 1 H31B H -0.4145(16) 1.9430(10) 0.2496(8) 0.151 Uiso 0.68(2) calc PR 1 C32 C -0.5807(13) 1.9062(12) 0.2112(8) 0.115(8) Uiso 0.68(2) d PD 1 H32A H -0.6231(13) 1.9439(12) 0.2347(8) 0.172 Uiso 0.68(2) calc PR 1 H32B H -0.6147(13) 1.9139(12) 0.1746(8) 0.172 Uiso 0.68(2) calc PR 1 C33 C -0.5943(12) 1.8339(12) 0.2257(8) 0.094(7) Uiso 0.68(2) d PD 1 H33A H -0.6632(12) 1.8082(12) 0.2050(8) 0.141 Uiso 0.68(2) calc PR 1 H33B H -0.6128(12) 1.8321(12) 0.2635(8) 0.141 Uiso 0.68(2) calc PR 1 C34 C -0.4738(16) 1.7886(11) 0.2166(12) 0.140(12) Uiso 0.68(2) d PD 1 H34A H -0.4475(16) 1.7577(11) 0.2487(12) 0.210 Uiso 0.68(2) calc PR 1 H34B H -0.4861(16) 1.7497(11) 0.1870(12) 0.210 Uiso 0.68(2) calc PR 1 C31' C -0.4826(21) 1.8996(18) 0.2133(39) 0.553(150) Uiso 0.32(2) d PD 2 H31C H -0.4785(21) 1.9477(18) 0.1899(39) 0.829 Uiso 0.32(2) calc PR 2 H31D H -0.4791(21) 1.9185(18) 0.2504(39) 0.829 Uiso 0.32(2) calc PR 2 C32' C -0.6022(13) 1.8525(23) 0.2011(43) 1.074(409) Uiso 0.32(2) d PD 2 H32C H -0.6584(13) 1.8593(23) 0.2303(43) 1.611 Uiso 0.32(2) calc PR 2 H32D H -0.6436(13) 1.8737(23) 0.1683(43) 1.611 Uiso 0.32(2) calc PR 2 C33' C -0.5765(20) 1.7792(19) 0.1956(15) 0.080(13) Uiso 0.32(2) d PD 2 H33C H -0.5960(20) 1.7619(19) 0.1587(15) 0.120 Uiso 0.32(2) calc PR 2 H33D H -0.6252(20) 1.7455(19) 0.2193(15) 0.120 Uiso 0.32(2) calc PR 2 C34' C -0.4385(24) 1.7682(12) 0.2093(18) 0.084(14) Uiso 0.32(2) d PD 2 H34C H -0.4254(24) 1.7473(12) 0.2457(18) 0.126 Uiso 0.32(2) calc PR 2 H34D H -0.4022(24) 1.7292(12) 0.1847(18) 0.126 Uiso 0.32(2) calc PR 2 O8 O -0.0040(6) 1.8193(4) 0.0651(3) 0.083(2) Uani 1 d . . C35 C 0.0895(12) 1.7580(6) 0.0675(4) 0.082(4) Uani 1 d . . H35A H 0.0948(12) 1.7325(6) 0.0328(4) 0.098 Uiso 1 d R . H35B H 0.0688(12) 1.7162(6) 0.0932(4) 0.098 Uiso 1 d R . C36 C 0.2071(12) 1.7979(7) 0.0842(5) 0.091(4) Uani 1 d . . H36A H 0.2241(12) 1.7923(7) 0.1223(5) 0.109 Uiso 1 d R . H36B H 0.2754(12) 1.7740(7) 0.0657(5) 0.109 Uiso 1 d R . C37 C 0.1923(13) 1.8855(7) 0.0687(6) 0.112(5) Uani 1 d . . H37A H 0.2125(13) 1.9206(7) 0.0991(6) 0.134 Uiso 1 d R . H37B H 0.2454(13) 1.9000(7) 0.0401(6) 0.134 Uiso 1 d R . C38 C 0.0587(11) 1.8934(8) 0.0511(6) 0.111(5) Uani 1 d . . H38A H 0.0216(11) 1.9394(8) 0.0691(6) 0.133 Uiso 1 d R . H38B H 0.0502(11) 1.9026(8) 0.0129(6) 0.133 Uiso 1 d 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 K1 0.0372(10) 0.0316(9) 0.0288(10) -0.0004(7) -0.0015(8) -0.0028(8) S1 0.0297(11) 0.0229(9) 0.0526(14) -0.0003(9) 0.0069(10) 0.0033(9) C1 0.029(4) 0.027(4) 0.022(4) -0.009(3) 0.004(4) -0.004(4) C2 0.018(4) 0.026(4) 0.024(4) -0.002(3) 0.006(3) 0.002(3) C3 0.022(4) 0.043(5) 0.030(5) -0.006(4) 0.005(4) 0.005(4) C4 0.038(5) 0.028(4) 0.034(5) -0.001(3) -0.003(4) 0.003(4) C5 0.028(5) 0.028(4) 0.036(5) 0.006(3) 0.001(4) -0.004(4) C6 0.026(4) 0.029(4) 0.027(4) 0.002(3) 0.007(4) 0.003(4) C7 0.027(5) 0.048(5) 0.042(5) 0.001(4) 0.004(4) -0.010(4) C8 0.043(5) 0.061(5) 0.045(6) 0.002(4) 0.011(5) -0.017(5) C9 0.043(5) 0.042(5) 0.062(6) -0.012(4) 0.008(5) -0.019(4) C10 0.027(5) 0.063(6) 0.080(7) -0.005(5) 0.002(5) -0.010(5) C11 0.052(6) 0.031(4) 0.065(6) 0.004(4) 0.005(5) 0.019(4) C12 0.099(12) 0.023(6) 0.249(26) 0.041(9) 0.023(14) 0.013(7) C13 0.125(14) 0.064(8) 0.072(10) 0.001(7) -0.034(10) 0.055(9) C14 0.122(14) 0.050(7) 0.072(9) -0.009(6) 0.020(9) 0.050(9) C15 0.022(4) 0.040(4) 0.033(5) -0.001(4) 0.007(4) -0.005(4) C17 0.025(4) 0.058(5) 0.033(5) 0.009(4) 0.011(4) 0.000(4) C18 0.024(4) 0.058(5) 0.031(5) -0.014(4) -0.004(4) 0.004(4) O1 0.082(5) 0.047(3) 0.029(3) -0.004(3) 0.003(3) -0.023(3) O2 0.077(4) 0.035(3) 0.027(3) 0.006(2) 0.007(3) 0.000(3) O3 0.040(3) 0.043(3) 0.035(3) 0.003(2) -0.005(3) 0.000(3) O4 0.044(3) 0.043(3) 0.024(3) -0.003(2) 0.001(3) -0.002(3) O5 0.038(3) 0.035(3) 0.038(3) -0.001(2) -0.011(3) 0.003(3) O6 0.036(3) 0.049(3) 0.039(3) -0.007(3) -0.009(3) -0.004(3) C19 0.093(8) 0.048(5) 0.032(6) -0.006(4) -0.002(5) -0.031(6) C20 0.045(6) 0.094(7) 0.034(5) -0.010(5) -0.013(5) -0.034(6) C21 0.041(6) 0.075(6) 0.048(6) -0.005(5) -0.005(5) 0.026(5) C22 0.051(6) 0.044(5) 0.047(6) -0.003(4) -0.010(5) 0.021(5) C23 0.036(5) 0.028(4) 0.080(8) -0.001(4) 0.013(5) 0.007(4) C24 0.053(6) 0.036(4) 0.041(6) -0.011(4) 0.010(5) -0.001(4) C25 0.061(6) 0.053(5) 0.034(6) -0.007(4) -0.007(5) -0.003(5) C26 0.046(5) 0.074(6) 0.029(5) 0.006(4) -0.012(4) -0.016(5) C27 0.055(6) 0.067(6) 0.031(5) 0.017(4) 0.006(5) 0.019(6) C28 0.072(7) 0.048(5) 0.033(6) 0.013(4) 0.014(5) 0.012(5) C29 0.135(10) 0.034(5) 0.055(7) 0.009(4) 0.002(7) -0.009(6) C30 0.132(10) 0.027(5) 0.060(7) -0.007(4) 0.002(7) -0.012(6) O7 0.096(7) 0.161(9) 0.134(8) -0.012(7) 0.059(6) -0.052(7) O8 0.061(5) 0.090(5) 0.099(6) 0.029(4) 0.029(4) 0.012(4) C35 0.111(10) 0.070(7) 0.068(8) -0.003(6) 0.048(8) 0.017(8) C36 0.087(9) 0.097(9) 0.086(9) -0.014(7) -0.022(8) 0.036(8) C37 0.102(11) 0.084(8) 0.146(13) 0.036(8) -0.027(10) -0.012(8) C38 0.075(9) 0.098(9) 0.160(13) 0.076(9) 0.015(9) 0.019(8) _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 K1 O6 2.704(6) . ? K1 O3 2.730(6) . ? K1 O5 2.740(5) . ? K1 O8 2.742(7) . ? K1 O7 2.744(8) . ? K1 O1 2.819(5) . ? K1 O2 2.835(5) . ? K1 O4 2.843(5) . ? K1 C34' 3.40(3) . ? S1 C1 1.742(7) . ? C1 C2 1.448(10) . ? C1 C6 1.450(9) . ? C2 C3 1.386(9) . ? C2 C7 1.554(10) . ? C3 C4 1.378(9) . ? C4 C5 1.370(10) . ? C4 C11 1.538(10) . ? C5 C6 1.385(9) . ? C6 C15 1.565(10) . ? C7 C8 1.523(11) . ? C7 C9 1.536(11) . ? C7 C10 1.559(11) . ? C11 C12 1.511(7) . ? C11 C14 1.511(7) . ? C11 C12' 1.511(7) . ? C11 C14' 1.511(7) . ? C11 C13' 1.511(7) . ? C11 C13 1.511(7) . ? C15 C18 1.532(10) . ? C15 C17 1.538(10) . ? C15 C16 1.547(10) . ? O1 C19 1.430(10) . ? O1 C30 1.428(11) . ? O2 C28 1.414(9) . ? O2 C29 1.430(11) . ? O3 C26 1.397(9) . ? O3 C27 1.422(9) . ? O4 C25 1.397(9) . ? O4 C24 1.417(9) . ? O5 C23 1.423(9) . ? O5 C22 1.420(9) . ? O6 C20 1.411(9) . ? O6 C21 1.422(9) . ? C19 C20 1.473(12) . ? C21 C22 1.465(11) . ? C23 C24 1.486(11) . ? C25 C26 1.502(11) . ? C27 C28 1.456(12) . ? C29 C30 1.477(12) . ? O7 C34 1.383(12) . ? O7 C31 1.394(12) . ? O7 C31' 1.392(13) . ? O7 C34' 1.394(13) . ? C31 C32 1.51(2) . ? C32 C33 1.23(2) . ? C33 C34 1.51(2) . ? C31' C32' 1.50(2) . ? C32' C33' 1.22(2) . ? C33' C34' 1.51(2) . ? O8 C35 1.404(11) . ? O8 C38 1.421(12) . ? C35 C36 1.454(15) . ? C36 C37 1.47(2) . ? C37 C38 1.48(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 K1 O3 179.0(2) . . ? O6 K1 O5 60.70(15) . . ? O3 K1 O5 119.4(2) . . ? O6 K1 O8 83.1(2) . . ? O3 K1 O8 95.8(2) . . ? O5 K1 O8 93.9(2) . . ? O6 K1 O7 90.5(3) . . ? O3 K1 O7 90.5(3) . . ? O5 K1 O7 78.8(3) . . ? O8 K1 O7 172.1(3) . . ? O6 K1 O1 60.3(2) . . ? O3 K1 O1 119.7(2) . . ? O5 K1 O1 120.3(2) . . ? O8 K1 O1 87.7(2) . . ? O7 K1 O1 93.3(2) . . ? O6 K1 O2 119.7(2) . . ? O3 K1 O2 60.2(2) . . ? O5 K1 O2 176.8(2) . . ? O8 K1 O2 83.0(2) . . ? O7 K1 O2 104.3(3) . . ? O1 K1 O2 60.7(2) . . ? O6 K1 O4 120.0(2) . . ? O3 K1 O4 59.92(15) . . ? O5 K1 O4 60.3(2) . . ? O8 K1 O4 90.5(2) . . ? O7 K1 O4 88.6(2) . . ? O1 K1 O4 178.1(2) . . ? O2 K1 O4 118.5(2) . . ? O6 K1 C34' 88.2(6) . . ? O3 K1 C34' 92.8(6) . . ? O5 K1 C34' 97.8(4) . . ? O8 K1 C34' 159.8(6) . . ? O7 K1 C34' 23.2(5) . . ? O1 K1 C34' 72.2(6) . . ? O2 K1 C34' 85.5(4) . . ? O4 K1 C34' 109.6(6) . . ? C2 C1 C6 116.1(6) . . ? C2 C1 S1 122.4(5) . . ? C6 C1 S1 121.4(5) . . ? C3 C2 C1 118.7(6) . . ? C3 C2 C7 118.9(6) . . ? C1 C2 C7 122.3(6) . . ? C4 C3 C2 125.4(7) . . ? C5 C4 C3 115.3(7) . . ? C5 C4 C11 123.5(7) . . ? C3 C4 C11 121.2(7) . . ? C4 C5 C6 124.9(7) . . ? C5 C6 C1 119.4(6) . . ? C5 C6 C15 118.2(6) . . ? C1 C6 C15 122.3(6) . . ? C8 C7 C9 110.6(7) . . ? C8 C7 C2 112.6(6) . . ? C9 C7 C2 110.6(6) . . ? C8 C7 C10 106.8(6) . . ? C9 C7 C10 105.4(7) . . ? C2 C7 C10 110.6(6) . . ? C12 C11 C14 107.0(10) . . ? C12' C11 C14' 115.9(31) . . ? C12' C11 C13' 101.6(40) . . ? C14' C11 C13' 107.9(39) . . ? C12 C11 C13 109.9(10) . . ? C14 C11 C13 108.9(9) . . ? C12 C11 C4 111.5(6) . . ? C14 C11 C4 110.0(6) . . ? C12' C11 C4 110.3(20) . . ? C14' C11 C4 109.4(21) . . ? C13' C11 C4 111.4(30) . . ? C13 C11 C4 109.4(7) . . ? C18 C15 C17 111.7(6) . . ? C18 C15 C16 105.1(6) . . ? C17 C15 C16 105.5(6) . . ? C18 C15 C6 112.6(6) . . ? C17 C15 C6 110.1(6) . . ? C16 C15 C6 111.4(6) . . ? C19 O1 C30 111.4(7) . . ? C19 O1 K1 111.6(4) . . ? C30 O1 K1 112.1(5) . . ? C28 O2 C29 113.1(6) . . ? C28 O2 K1 111.1(4) . . ? C29 O2 K1 112.8(5) . . ? C26 O3 C27 113.5(6) . . ? C26 O3 K1 118.9(4) . . ? C27 O3 K1 118.1(5) . . ? C25 O4 C24 112.6(6) . . ? C25 O4 K1 111.5(4) . . ? C24 O4 K1 113.0(4) . . ? C23 O5 C22 112.4(6) . . ? C23 O5 K1 117.1(4) . . ? C22 O5 K1 115.2(4) . . ? C20 O6 C21 113.9(7) . . ? C20 O6 K1 118.5(5) . . ? C21 O6 K1 117.7(5) . . ? O1 C19 C20 108.3(7) . . ? O6 C20 C19 108.7(7) . . ? O6 C21 C22 109.2(7) . . ? O5 C22 C21 109.5(7) . . ? O5 C23 C24 109.9(6) . . ? O4 C24 C23 108.8(6) . . ? O4 C25 C26 109.3(6) . . ? O3 C26 C25 108.3(7) . . ? O3 C27 C28 110.1(7) . . ? O2 C28 C27 109.3(6) . . ? O2 C29 C30 108.6(7) . . ? O1 C30 C29 108.9(8) . . ? C34 O7 C31 103.4(15) . . ? C31' O7 C34' 102.4(16) . . ? C34 O7 K1 127.5(12) . . ? C31 O7 K1 124.7(9) . . ? C31' O7 K1 141.5(35) . . ? C34' O7 K1 106.1(17) . . ? O7 C31 C32 106.7(11) . . ? C33 C32 C31 105.9(8) . . ? C32 C33 C34 107.5(8) . . ? O7 C34 C33 108.6(12) . . ? O7 C31' C32' 107.7(13) . . ? C33' C32' C31' 108.5(8) . . ? C32' C33' C34' 108.0(9) . . ? O7 C34' C33' 106.8(12) . . ? O7 C34' K1 50.7(13) . . ? C33' C34' K1 130.1(20) . . ? C35 O8 C38 105.0(8) . . ? C35 O8 K1 121.2(5) . . ? C38 O8 K1 119.7(7) . . ? O8 C35 C36 107.7(9) . . ? C35 C36 C37 105.6(10) . . ? C36 C37 C38 104.6(10) . . ? O8 C38 C37 108.3(9) . . ? _refine_diff_density_max 0.722 _refine_diff_density_min -0.818 _refine_diff_density_rms 0.093 #===END data_Compound_4 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H69 K O8 Se' _chemical_formula_weight 771.99 _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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 '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 10.778(2) _cell_length_b 16.129(3) _cell_length_c 25.169(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.60(3) _cell_angle_gamma 90.00 _cell_volume 4366.7(14) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 10 _cell_measurement_theta_max 22 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method ? _exptl_crystal_F_000 1656 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type 'Psi Scans' _exptl_absorpt_correction_T_min 0.7129 _exptl_absorpt_correction_T_max 1.0000 _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'Rigaku AFC5S' _diffrn_measurement_method 'omega' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% -1.7 _diffrn_reflns_number 8114 _diffrn_reflns_av_R_equivalents 0.0472 _diffrn_reflns_av_sigmaI/netI 0.0974 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7674 _reflns_number_observed 4424 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'TEXSAN, Molecular Structure Corporation' _computing_cell_refinement 'TEXSAN, Molecular Structure Corporation' _computing_data_reduction 'XPREP, SHELXTL-Plus, Siemens (1994)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'XP, SHELXTL-Plus, Siemens (1994)' _computing_publication_material 'XCIF, SHELXTL-Plus, Siemens (1994)' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 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 'w=1/[&Gs&^2&0(Fo&^2&0)+(0.0617P)&^2&0+2.9628P]' _refine_p_factor 'where P=(Fo&^2&0+2Fc&^2&0)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7672 _refine_ls_number_parameters 432 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1350 _refine_ls_R_factor_obs 0.0575 _refine_ls_wR_factor_all 0.1578 _refine_ls_wR_factor_obs 0.1280 _refine_ls_goodness_of_fit_all 1.008 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.013 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max -0.002 _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 K1 K -0.17863(10) 1.82544(6) 0.13947(4) 0.0501(3) Uani 1 d . . O1 O -0.2800(4) 1.6803(2) 0.08964(14) 0.0714(11) Uani 1 d . . O2 O -0.0801(4) 1.6675(2) 0.16834(14) 0.0661(11) Uani 1 d . . O3 O -0.0202(3) 1.8112(2) 0.22848(14) 0.0612(10) Uani 1 d . . O4 O -0.0700(3) 1.9701(2) 0.18804(13) 0.0558(9) Uani 1 d . . O5 O -0.2614(3) 1.9799(2) 0.10746(13) 0.0545(9) Uani 1 d . . O6 O -0.3326(3) 1.8395(2) 0.05026(14) 0.0631(10) Uani 1 d . . C19 C -0.3223(7) 1.6957(4) 0.0356(2) 0.080(2) Uani 1 d . . H19A H -0.3678(7) 1.6473(4) 0.0211(2) 0.095 Uiso 1 calc R . H19B H -0.2509(7) 1.7052(4) 0.0141(2) 0.095 Uiso 1 calc R . C20 C -0.4044(6) 1.7694(4) 0.0330(2) 0.079(2) Uani 1 d . . H20A H -0.4388(6) 1.7778(4) -0.0036(2) 0.095 Uiso 1 calc R . H20B H -0.4736(6) 1.7614(4) 0.0559(2) 0.095 Uiso 1 calc R . C21 C -0.3974(5) 1.9159(4) 0.0420(2) 0.072(2) Uani 1 d . . H21A H -0.4658(5) 1.9195(4) 0.0657(2) 0.086 Uiso 1 calc R . H21B H -0.4321(5) 1.9194(4) 0.0051(2) 0.086 Uiso 1 calc R . C22 C -0.3079(5) 1.9846(3) 0.0533(2) 0.063(2) Uani 1 d . . H22A H -0.2391(5) 1.9804(3) 0.0298(2) 0.076 Uiso 1 calc R . H22B H -0.3495(5) 2.0380(3) 0.0467(2) 0.076 Uiso 1 calc R . C23 C -0.1871(5) 2.0501(3) 0.1231(2) 0.0600(15) Uani 1 d . . H23A H -0.2352(5) 2.1013(3) 0.1174(2) 0.072 Uiso 1 calc R . H23B H -0.1139(5) 2.0530(3) 0.1020(2) 0.072 Uiso 1 calc R . C24 C -0.1478(5) 2.0410(3) 0.1806(2) 0.0581(14) Uani 1 d . . H24A H -0.1025(5) 2.0907(3) 0.1932(2) 0.070 Uiso 1 calc R . H24B H -0.2212(5) 2.0348(3) 0.2014(2) 0.070 Uiso 1 calc R . C25 C -0.0274(6) 1.9557(4) 0.2421(2) 0.070(2) Uani 1 d . . H25A H -0.0987(6) 1.9482(4) 0.2639(2) 0.084 Uiso 1 calc R . H25B H 0.0203(6) 2.0037(4) 0.2558(2) 0.084 Uiso 1 calc R . C26 C 0.0521(6) 1.8805(4) 0.2453(2) 0.071(2) Uani 1 d . . H26A H 0.1219(6) 1.8872(4) 0.2226(2) 0.086 Uiso 1 calc R . H26B H 0.0857(6) 1.8723(4) 0.2821(2) 0.086 Uiso 1 calc R . C27 C 0.0448(6) 1.7344(4) 0.2371(2) 0.073(2) Uani 1 d . . H27A H 0.0760(6) 1.7303(4) 0.2744(2) 0.087 Uiso 1 calc R . H27B H 0.1160(6) 1.7321(4) 0.2148(2) 0.087 Uiso 1 calc R . C28 C -0.0415(6) 1.6638(4) 0.2236(2) 0.073(2) Uani 1 d . . H28A H 0.0009(6) 1.6111(4) 0.2316(2) 0.088 Uiso 1 calc R . H28B H -0.1142(6) 1.6672(4) 0.2450(2) 0.088 Uiso 1 calc R . C29 C -0.1580(7) 1.6005(4) 0.1521(3) 0.090(2) Uani 1 d . . H29A H -0.2309(7) 1.5989(4) 0.1735(3) 0.108 Uiso 1 calc R . H29B H -0.1130(7) 1.5480(4) 0.1571(3) 0.108 Uiso 1 calc R . C30 C -0.1982(8) 1.6121(3) 0.0942(3) 0.090(2) Uani 1 d . . H30A H -0.1255(8) 1.6224(3) 0.0736(3) 0.108 Uiso 1 calc R . H30B H -0.2401(8) 1.5620(3) 0.0802(3) 0.108 Uiso 1 calc R . O7 O -0.3781(6) 1.8417(5) 0.2014(3) 0.143(2) Uani 1 d . . C31 C -0.4400(10) 1.9123(8) 0.2137(5) 0.190(6) Uani 1 d . . H31A H -0.4308(10) 1.9536(8) 0.1857(5) 0.228 Uiso 1 calc R . H31B H -0.4032(10) 1.9351(8) 0.2472(5) 0.228 Uiso 1 calc R . C32 C -0.5665(12) 1.8968(11) 0.2188(7) 0.248(9) Uani 1 d . . H32A H -0.6175(12) 1.9247(11) 0.1906(7) 0.297 Uiso 1 calc R . H32B H -0.5921(12) 1.9158(11) 0.2535(7) 0.297 Uiso 1 calc R . C33 C -0.5774(13) 1.8105(12) 0.2143(8) 0.269(12) Uani 1 d . . H33A H -0.6294(13) 1.7963(12) 0.1822(8) 0.323 Uiso 1 calc R . H33B H -0.6171(13) 1.7881(12) 0.2452(8) 0.323 Uiso 1 calc R . C34 C -0.4521(13) 1.7737(7) 0.2112(4) 0.165(4) Uani 1 d . . H34A H -0.4246(13) 1.7466(7) 0.2448(4) 0.198 Uiso 1 calc R . H34B H -0.4509(13) 1.7332(7) 0.1822(4) 0.198 Uiso 1 calc R . O8 O 0.0102(5) 1.8260(4) 0.0701(2) 0.121(2) Uani 1 d . . C35 C 0.0991(9) 1.7641(5) 0.0677(4) 0.123(3) Uani 1 d . . H35A H 0.0966(9) 1.7395(5) 0.0320(4) 0.147 Uiso 1 calc R . H35B H 0.0850(9) 1.7203(5) 0.0936(4) 0.147 Uiso 1 calc R . C36 C 0.2174(9) 1.8047(6) 0.0801(4) 0.138(3) Uani 1 d . . H36A H 0.2454(9) 1.7950(6) 0.1174(4) 0.166 Uiso 1 calc R . H36B H 0.2806(9) 1.7831(6) 0.0574(4) 0.166 Uiso 1 calc R . C37 C 0.1987(9) 1.8915(6) 0.0707(5) 0.155(4) Uani 1 d . . H37A H 0.2248(9) 1.9237(6) 0.1025(5) 0.186 Uiso 1 calc R . H37B H 0.2460(9) 1.9102(6) 0.0410(5) 0.186 Uiso 1 calc R . C38 C 0.0683(9) 1.9005(5) 0.0582(4) 0.148(4) Uani 1 d . . H38A H 0.0354(9) 1.9457(5) 0.0792(4) 0.178 Uiso 1 calc R . H38B H 0.0527(9) 1.9137(5) 0.0204(4) 0.178 Uiso 1 calc R . Se1 Se -0.51696(5) 2.13504(3) 0.11999(2) 0.0501(2) Uani 1 d . . C1 C -0.5798(4) 2.2470(3) 0.1147(2) 0.0387(11) Uani 1 d . . C2 C -0.7108(4) 2.2640(3) 0.1145(2) 0.0424(11) Uani 1 d . . C3 C -0.7503(5) 2.3461(3) 0.1105(2) 0.0496(13) Uani 1 d . . H3A H -0.8360(5) 2.3563(3) 0.1114(2) 0.060 Uiso 1 calc R . C4 C -0.6730(5) 2.4139(3) 0.1054(2) 0.0508(13) Uani 1 d . . C5 C -0.5476(5) 2.3962(3) 0.1054(2) 0.0480(12) Uani 1 d . . H5A H -0.4925(5) 2.4409(3) 0.1021(2) 0.058 Uiso 1 calc R . C6 C -0.4967(4) 2.3165(3) 0.1098(2) 0.0418(11) Uani 1 d . . C7 C -0.8133(5) 2.1968(3) 0.1176(2) 0.0517(13) Uani 1 d . . C8 C -0.8000(5) 2.1475(3) 0.1702(2) 0.066(2) Uani 1 d . . H8A H -0.7180(5) 2.1225(3) 0.1740(2) 0.080 Uiso 1 calc R . H8B H -0.8627(5) 2.1044(3) 0.1698(2) 0.080 Uiso 1 calc R . H8C H -0.8108(5) 2.1846(3) 0.1999(2) 0.080 Uiso 1 calc R . C9 C -0.8131(5) 2.1370(3) 0.0693(2) 0.066(2) Uani 1 d . . H9A H -0.7320(5) 2.1112(3) 0.0682(2) 0.080 Uiso 1 calc R . H9B H -0.8313(5) 2.1680(3) 0.0367(2) 0.080 Uiso 1 calc R . H9C H -0.8758(5) 2.0946(3) 0.0727(2) 0.080 Uiso 1 calc R . C10 C -0.9451(5) 2.2338(4) 0.1152(3) 0.076(2) Uani 1 d . . H10A H -0.9591(5) 2.2657(4) 0.0827(3) 0.092 Uiso 1 calc R . H10B H -0.9537(5) 2.2696(4) 0.1457(3) 0.092 Uiso 1 calc R . H10C H -1.0057(5) 2.1893(4) 0.1157(3) 0.092 Uiso 1 calc R . C11 C -0.7247(5) 2.5026(3) 0.1002(2) 0.063(2) Uani 1 d D . C12 C -0.6253(8) 2.5665(6) 0.0906(4) 0.101(4) Uiso 0.736(10) d PD 1 H12A H -0.5853(8) 2.5527(6) 0.0583(4) 0.121 Uiso 0.736(10) calc PR 1 H12B H -0.5639(8) 2.5667(6) 0.1205(4) 0.121 Uiso 0.736(10) calc PR 1 H12C H -0.6631(8) 2.6209(6) 0.0869(4) 0.121 Uiso 0.736(10) calc PR 1 C13 C -0.8206(8) 2.5076(6) 0.0536(3) 0.085(3) Uiso 0.736(10) d PD 1 H13A H -0.7825(8) 2.4918(6) 0.0212(3) 0.102 Uiso 0.736(10) calc PR 1 H13B H -0.8518(8) 2.5638(6) 0.0502(3) 0.102 Uiso 0.736(10) calc PR 1 H13C H -0.8888(8) 2.4702(6) 0.0596(3) 0.102 Uiso 0.736(10) calc PR 1 C14 C -0.7835(9) 2.5272(5) 0.1509(3) 0.083(3) Uiso 0.736(10) d PD 1 H14A H -0.7218(9) 2.5239(5) 0.1806(3) 0.100 Uiso 0.736(10) calc PR 1 H14B H -0.8518(9) 2.4899(5) 0.1570(3) 0.100 Uiso 0.736(10) calc PR 1 H14C H -0.8145(9) 2.5835(5) 0.1476(3) 0.100 Uiso 0.736(10) calc PR 1 C12' C -0.6590(28) 2.5634(16) 0.1382(11) 0.124(13) Uiso 0.264(10) d PD 2 H12D H -0.6608(28) 2.5427(16) 0.1743(11) 0.149 Uiso 0.264(10) calc PR 2 H12E H -0.7008(28) 2.6167(16) 0.1355(11) 0.149 Uiso 0.264(10) calc PR 2 H12F H -0.5734(28) 2.5698(16) 0.1291(11) 0.149 Uiso 0.264(10) calc PR 2 C13' C -0.7231(31) 2.5350(17) 0.0438(5) 0.109(11) Uiso 0.264(10) d PD 2 H13D H -0.7649(31) 2.4958(17) 0.0195(5) 0.130 Uiso 0.264(10) calc PR 2 H13E H -0.6377(31) 2.5420(17) 0.0345(5) 0.130 Uiso 0.264(10) calc PR 2 H13F H -0.7657(31) 2.5880(17) 0.0412(5) 0.130 Uiso 0.264(10) calc PR 2 C14' C -0.8583(15) 2.5071(25) 0.1155(17) 0.175(18) Uiso 0.264(10) d PD 2 H14D H -0.9091(15) 2.4699(25) 0.0930(17) 0.210 Uiso 0.264(10) calc PR 2 H14E H -0.8887(15) 2.5634(25) 0.1108(17) 0.210 Uiso 0.264(10) calc PR 2 H14F H -0.8625(15) 2.4908(25) 0.1524(17) 0.210 Uiso 0.264(10) calc PR 2 C15 C -0.3523(4) 2.3091(3) 0.1093(2) 0.0473(12) Uani 1 d . . C16 C -0.2884(5) 2.3948(3) 0.1055(2) 0.071(2) Uani 1 d . . H16A H -0.3080(5) 2.4286(3) 0.1357(2) 0.086 Uiso 1 calc R . H16B H -0.3182(5) 2.4221(3) 0.0728(2) 0.086 Uiso 1 calc R . H16C H -0.1991(5) 2.3873(3) 0.1056(2) 0.086 Uiso 1 calc R . C17 C -0.3156(4) 2.2609(3) 0.0600(2) 0.0551(14) Uani 1 d . . H17A H -0.3533(4) 2.2869(3) 0.0282(2) 0.066 Uiso 1 calc R . H17B H -0.3446(4) 2.2041(3) 0.0621(2) 0.066 Uiso 1 calc R . H17C H -0.2259(4) 2.2613(3) 0.0586(2) 0.066 Uiso 1 calc R . C18 C -0.2954(4) 2.2709(3) 0.1614(2) 0.0541(13) Uani 1 d . . H18A H -0.3207(4) 2.3029(3) 0.1914(2) 0.065 Uiso 1 calc R . H18B H -0.2055(4) 2.2714(3) 0.1610(2) 0.065 Uiso 1 calc R . H18C H -0.3242(4) 2.2142(3) 0.1645(2) 0.065 Uiso 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 K1 0.0533(7) 0.0433(6) 0.0526(7) 0.0005(5) -0.0055(5) -0.0013(5) O1 0.103(3) 0.059(3) 0.051(2) 0.000(2) -0.001(2) -0.020(2) O2 0.098(3) 0.050(2) 0.050(2) 0.008(2) 0.006(2) 0.003(2) O3 0.063(2) 0.064(2) 0.055(2) 0.009(2) -0.013(2) -0.001(2) O4 0.060(2) 0.053(2) 0.053(2) -0.004(2) -0.004(2) -0.003(2) O5 0.056(2) 0.047(2) 0.060(2) 0.001(2) -0.002(2) 0.003(2) O6 0.058(2) 0.066(2) 0.063(2) -0.005(2) -0.017(2) -0.003(2) C19 0.106(5) 0.070(4) 0.061(4) -0.011(3) -0.013(4) -0.026(4) C20 0.077(5) 0.094(5) 0.063(4) -0.009(4) -0.019(3) -0.027(4) C21 0.054(4) 0.094(5) 0.066(4) -0.006(3) -0.015(3) 0.014(3) C22 0.074(4) 0.064(4) 0.052(4) 0.007(3) 0.001(3) 0.027(3) C23 0.059(3) 0.040(3) 0.081(4) -0.001(3) 0.002(3) 0.007(3) C24 0.058(3) 0.046(3) 0.071(4) -0.011(3) 0.008(3) -0.006(3) C25 0.087(5) 0.069(4) 0.054(4) -0.005(3) -0.007(3) -0.018(3) C26 0.071(4) 0.083(4) 0.058(4) 0.005(3) -0.022(3) -0.007(3) C27 0.075(4) 0.082(4) 0.060(4) 0.018(3) -0.005(3) 0.016(4) C28 0.103(5) 0.057(3) 0.061(4) 0.014(3) 0.004(4) 0.022(3) C29 0.147(7) 0.046(3) 0.076(5) 0.009(3) 0.004(4) -0.012(4) C30 0.152(7) 0.040(3) 0.078(5) -0.011(3) 0.004(5) -0.010(4) O7 0.112(5) 0.162(6) 0.161(6) 0.000(5) 0.064(4) -0.021(5) C31 0.123(9) 0.198(13) 0.259(15) -0.083(11) 0.090(9) -0.032(9) C32 0.117(11) 0.281(19) 0.357(22) -0.070(18) 0.109(12) -0.033(12) C33 0.109(11) 0.321(23) 0.368(24) 0.179(20) -0.063(13) -0.088(14) C34 0.189(13) 0.159(10) 0.147(9) 0.041(8) 0.006(9) -0.041(10) O8 0.086(4) 0.105(4) 0.177(6) 0.035(4) 0.047(4) 0.008(3) C35 0.141(8) 0.077(5) 0.157(8) 0.001(5) 0.058(7) 0.017(6) C36 0.106(7) 0.126(8) 0.182(10) -0.011(7) -0.002(7) 0.032(6) C37 0.129(9) 0.102(7) 0.232(12) 0.074(7) 0.001(8) -0.005(6) C38 0.108(7) 0.103(6) 0.238(12) 0.080(7) 0.034(7) 0.028(6) Se1 0.0449(3) 0.0348(2) 0.0706(4) -0.0012(3) 0.0028(2) 0.0039(2) C1 0.034(3) 0.037(3) 0.044(3) -0.002(2) -0.001(2) 0.005(2) C2 0.037(3) 0.040(3) 0.050(3) -0.006(2) 0.001(2) 0.001(2) C3 0.038(3) 0.055(3) 0.056(3) -0.003(2) -0.001(2) 0.013(2) C4 0.054(3) 0.041(3) 0.057(3) 0.002(2) -0.001(3) 0.009(2) C5 0.052(3) 0.037(2) 0.055(3) -0.002(2) 0.002(2) -0.006(2) C6 0.044(3) 0.039(3) 0.043(3) -0.002(2) 0.003(2) -0.003(2) C7 0.041(3) 0.049(3) 0.066(4) -0.003(3) 0.004(3) -0.008(2) C8 0.060(4) 0.063(4) 0.078(4) 0.000(3) 0.016(3) -0.016(3) C9 0.056(3) 0.062(3) 0.080(4) -0.010(3) -0.002(3) -0.021(3) C10 0.038(3) 0.085(4) 0.107(5) -0.002(4) 0.008(3) -0.008(3) C11 0.070(4) 0.045(3) 0.073(4) 0.005(3) -0.002(3) 0.011(3) C15 0.033(3) 0.051(3) 0.058(3) 0.000(2) 0.001(2) -0.006(2) C16 0.054(3) 0.069(4) 0.092(5) -0.002(3) 0.010(3) -0.017(3) C17 0.039(3) 0.070(3) 0.056(3) -0.001(3) 0.002(3) -0.002(3) C18 0.034(3) 0.066(3) 0.061(3) -0.011(3) -0.007(2) -0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O6 2.717(4) . ? K1 O3 2.740(4) . ? K1 O7 2.746(6) . ? K1 O5 2.750(3) . ? K1 O8 2.763(5) . ? K1 O2 2.837(4) . ? K1 O1 2.841(4) . ? K1 O4 2.852(3) . ? O1 C30 1.410(7) . ? O1 C19 1.429(6) . ? O2 C29 1.414(7) . ? O2 C28 1.427(6) . ? O3 C26 1.412(6) . ? O3 C27 1.433(6) . ? O4 C24 1.422(6) . ? O4 C25 1.427(6) . ? O5 C22 1.424(6) . ? O5 C23 1.429(6) . ? O6 C20 1.423(6) . ? O6 C21 1.424(6) . ? C19 C20 1.481(8) . ? C21 C22 1.485(8) . ? C23 C24 1.489(7) . ? C25 C26 1.484(8) . ? C27 C28 1.495(8) . ? C29 C30 1.506(8) . ? O7 C31 1.365(11) . ? O7 C34 1.387(11) . ? C31 C32 1.400(14) . ? C32 C33 1.40(2) . ? C33 C34 1.48(2) . ? O8 C35 1.388(8) . ? O8 C38 1.396(9) . ? C35 C36 1.451(11) . ? C36 C37 1.431(11) . ? C37 C38 1.428(11) . ? Se1 C1 1.930(4) . ? C1 C2 1.438(6) . ? C1 C6 1.445(6) . ? C2 C3 1.392(6) . ? C2 C7 1.554(6) . ? C3 C4 1.385(7) . ? C4 C5 1.382(7) . ? C4 C11 1.538(7) . ? C5 C6 1.399(6) . ? C6 C15 1.561(6) . ? C7 C10 1.539(7) . ? C7 C8 1.542(7) . ? C7 C9 1.553(7) . ? C11 C14 1.513(5) . ? C11 C12' 1.514(6) . ? C11 C13' 1.514(6) . ? C11 C14' 1.515(6) . ? C11 C13 1.515(5) . ? C11 C12 1.517(5) . ? C15 C17 1.537(7) . ? C15 C18 1.539(7) . ? C15 C16 1.550(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 K1 O3 179.10(12) . . ? O6 K1 O7 90.1(2) . . ? O3 K1 O7 90.8(2) . . ? O6 K1 O5 60.79(10) . . ? O3 K1 O5 119.30(11) . . ? O7 K1 O5 80.1(2) . . ? O6 K1 O8 85.0(2) . . ? O3 K1 O8 94.1(2) . . ? O7 K1 O8 172.8(2) . . ? O5 K1 O8 92.87(14) . . ? O6 K1 O2 119.09(11) . . ? O3 K1 O2 60.76(11) . . ? O7 K1 O2 103.5(2) . . ? O5 K1 O2 176.31(12) . . ? O8 K1 O2 83.46(14) . . ? O6 K1 O1 60.39(11) . . ? O3 K1 O1 119.66(12) . . ? O7 K1 O1 92.1(2) . . ? O5 K1 O1 120.55(12) . . ? O8 K1 O1 90.1(2) . . ? O2 K1 O1 60.05(12) . . ? O6 K1 O4 119.93(11) . . ? O3 K1 O4 59.99(10) . . ? O7 K1 O4 89.6(2) . . ? O5 K1 O4 60.07(10) . . ? O8 K1 O4 88.24(15) . . ? O2 K1 O4 119.22(12) . . ? O1 K1 O4 178.28(12) . . ? C30 O1 C19 111.9(5) . . ? C30 O1 K1 112.7(3) . . ? C19 O1 K1 111.6(3) . . ? C29 O2 C28 112.5(4) . . ? C29 O2 K1 114.0(3) . . ? C28 O2 K1 111.6(3) . . ? C26 O3 C27 112.6(4) . . ? C26 O3 K1 118.9(3) . . ? C27 O3 K1 118.0(3) . . ? C24 O4 C25 114.1(4) . . ? C24 O4 K1 112.2(3) . . ? C25 O4 K1 112.0(3) . . ? C22 O5 C23 112.3(4) . . ? C22 O5 K1 114.6(3) . . ? C23 O5 K1 118.1(3) . . ? C20 O6 C21 113.0(4) . . ? C20 O6 K1 118.6(3) . . ? C21 O6 K1 117.5(3) . . ? O1 C19 C20 109.6(5) . . ? O6 C20 C19 108.2(5) . . ? O6 C21 C22 108.2(4) . . ? O5 C22 C21 109.2(5) . . ? O5 C23 C24 108.1(4) . . ? O4 C24 C23 109.7(4) . . ? O4 C25 C26 109.6(5) . . ? O3 C26 C25 109.0(5) . . ? O3 C27 C28 109.5(5) . . ? O2 C28 C27 109.2(5) . . ? O2 C29 C30 108.3(5) . . ? O1 C30 C29 108.4(5) . . ? C31 O7 C34 108.9(8) . . ? C31 O7 K1 128.3(7) . . ? C34 O7 K1 120.3(7) . . ? O7 C31 C32 111.4(11) . . ? C31 C32 C33 104.3(13) . . ? C32 C33 C34 109.3(11) . . ? O7 C34 C33 103.2(10) . . ? C35 O8 C38 106.8(6) . . ? C35 O8 K1 124.3(5) . . ? C38 O8 K1 119.8(5) . . ? O8 C35 C36 105.4(7) . . ? C37 C36 C35 107.0(8) . . ? C38 C37 C36 105.2(8) . . ? O8 C38 C37 108.3(7) . . ? C2 C1 C6 117.7(4) . . ? C2 C1 Se1 121.3(3) . . ? C6 C1 Se1 121.0(3) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 C7 116.9(4) . . ? C1 C2 C7 124.6(4) . . ? C4 C3 C2 125.1(4) . . ? C5 C4 C3 115.5(4) . . ? C5 C4 C11 122.8(5) . . ? C3 C4 C11 121.7(4) . . ? C4 C5 C6 124.6(4) . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C15 117.1(4) . . ? C1 C6 C15 124.3(4) . . ? C10 C7 C8 105.6(4) . . ? C10 C7 C9 104.8(4) . . ? C8 C7 C9 110.4(4) . . ? C10 C7 C2 112.6(4) . . ? C8 C7 C2 112.1(4) . . ? C9 C7 C2 110.9(4) . . ? C12' C11 C13' 109.7(17) . . ? C12' C11 C14' 102.9(19) . . ? C13' C11 C14' 106.8(20) . . ? C14 C11 C13 109.7(6) . . ? C14 C11 C12 107.1(6) . . ? C13 C11 C12 107.2(6) . . ? C14 C11 C4 109.9(5) . . ? C12' C11 C4 113.4(13) . . ? C13' C11 C4 112.0(12) . . ? C14' C11 C4 111.5(16) . . ? C13 C11 C4 109.9(5) . . ? C12 C11 C4 112.9(5) . . ? C17 C15 C18 112.1(4) . . ? C17 C15 C16 105.2(4) . . ? C18 C15 C16 104.8(4) . . ? C17 C15 C6 110.6(4) . . ? C18 C15 C6 111.6(4) . . ? C16 C15 C6 112.3(4) . . ? _refine_diff_density_max 0.474 _refine_diff_density_min -0.368 _refine_diff_density_rms 0.065 #===END