# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry, 1999 # CCDC Number: 182/1324 data_rem218 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H72 K4 Li4 O8' _chemical_formula_weight 769.06 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' 'Li' 'Li' -0.0003 0.0001 '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' 'O' 'O' 0.0106 0.0060 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 11.5194(6) _cell_length_b 17.1506(10) _cell_length_c 13.0058(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.166(2) _cell_angle_gamma 90.00 _cell_volume 2412.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 10011 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 29.00 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.62 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.059 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.405 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7874 _exptl_absorpt_correction_T_max 0.9162 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(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 'Siemens SMART CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10325 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0262 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4372 _reflns_number_gt 3351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Siemens SMART' _computing_cell_refinement 'local programs' _computing_data_reduction 'Siemens SAINT' _computing_structure_solution 'Siemens SHELXTL' _computing_structure_refinement 'Siemens SHELXTL' _computing_molecular_graphics 'Siemens SHELXTL' _computing_publication_material 'SHELXTL and local programs' _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^)+(0.0537P)^2^+0.0508P] 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 4372 _refine_ls_number_parameters 266 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0880 _refine_ls_wR_factor_gt 0.0853 _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 K1 K 0.80487(3) 0.36146(2) 0.43194(3) 0.03428(12) Uani 1 1 d . . . K2 K 0.68029(3) 0.36129(2) 0.11477(3) 0.03899(12) Uani 1 1 d . . . Li1 Li 0.9845(3) 0.2500 0.3781(3) 0.0318(9) Uani 1 2 d S . . Li2 Li 0.9068(3) 0.2500 0.1792(3) 0.0320(9) Uani 1 2 d S . . Li3 Li 0.5434(2) 0.32121(16) 0.2729(2) 0.0313(6) Uani 1 1 d . . . O1 O 0.61094(13) 0.2500 0.39250(12) 0.0269(3) Uani 1 2 d S . . C1 C 0.5641(2) 0.2500 0.47963(18) 0.0309(5) Uani 1 2 d S . . C2 C 0.6073(2) 0.32187(13) 0.55121(16) 0.0548(5) Uani 1 1 d . . . H2A H 0.6971 0.3193 0.5885 0.082 Uiso 1 1 calc R . . H2B H 0.5662 0.3239 0.6058 0.082 Uiso 1 1 calc R . . H2C H 0.5865 0.3688 0.5054 0.082 Uiso 1 1 calc R . . C3 C 0.4225(2) 0.2500 0.4328(3) 0.0704(10) Uani 1 2 d S . . H3A H 0.3940 0.2077 0.3793 0.106 Uiso 0.50 1 calc PR . . H3B H 0.3933 0.3001 0.3969 0.106 Uiso 0.50 1 calc PR . . H3C H 0.3898 0.2422 0.4923 0.106 Uiso 0.50 1 calc PR . . O2 O 0.96947(13) 0.2500 0.51351(12) 0.0326(4) Uani 1 2 d S . . C4 C 1.0564(2) 0.2500 0.61918(18) 0.0315(5) Uani 1 2 d S . . C5 C 1.04014(18) 0.32249(12) 0.68139(15) 0.0498(5) Uani 1 1 d . . . H5A H 1.0531 0.3693 0.6436 0.075 Uiso 1 1 calc R . . H5B H 1.1005 0.3214 0.7560 0.075 Uiso 1 1 calc R . . H5C H 0.9563 0.3232 0.6845 0.075 Uiso 1 1 calc R . . C6 C 1.1872(2) 0.2500 0.6145(2) 0.0477(7) Uani 1 2 d S . . H6A H 1.2470 0.2399 0.6878 0.072 Uiso 0.50 1 calc PR . . H6B H 1.2045 0.3009 0.5887 0.072 Uiso 0.50 1 calc PR . . H6C H 1.1939 0.2092 0.5641 0.072 Uiso 0.50 1 calc PR . . O3 O 0.51308(13) 0.2500 0.15350(12) 0.0297(4) Uani 1 2 d S . . C7 C 0.3987(2) 0.2500 0.06593(19) 0.0355(6) Uani 1 2 d S . . C8 C 0.4187(7) 0.2612(15) -0.0428(7) 0.083(7) Uani 0.325(9) 1 d P A -1 H8A H 0.4758 0.2212 -0.0509 0.125 Uiso 0.325(9) 1 calc PR A -1 H8B H 0.4538 0.3130 -0.0447 0.125 Uiso 0.325(9) 1 calc PR A -1 H8C H 0.3394 0.2565 -0.1030 0.125 Uiso 0.325(9) 1 calc PR A -1 C9 C 0.3361(18) 0.1665(10) 0.058(2) 0.081(6) Uani 0.325(9) 1 d P A -1 H9A H 0.3912 0.1267 0.0457 0.121 Uiso 0.325(9) 1 calc PR A -1 H9B H 0.2573 0.1660 -0.0036 0.121 Uiso 0.325(9) 1 calc PR A -1 H9C H 0.3211 0.1553 0.1260 0.121 Uiso 0.325(9) 1 calc PR A -1 C10 C 0.3052(19) 0.2998(14) 0.0803(18) 0.137(15) Uani 0.325(9) 1 d P A -1 H10A H 0.2983 0.2900 0.1523 0.206 Uiso 0.325(9) 1 calc PR A -1 H10B H 0.2256 0.2889 0.0229 0.206 Uiso 0.325(9) 1 calc PR A -1 H10C H 0.3277 0.3544 0.0756 0.206 Uiso 0.325(9) 1 calc PR A -1 C11 C 0.3047(13) 0.2500 0.125(2) 0.138(15) Uani 0.350(17) 2 d SP A 2 H11A H 0.3118 0.2988 0.1664 0.207 Uiso 0.175(9) 1 calc PR A 2 H11B H 0.3213 0.2058 0.1763 0.207 Uiso 0.175(9) 1 calc PR A 2 H11C H 0.2209 0.2454 0.0718 0.207 Uiso 0.175(9) 1 calc PR A 2 C12 C 0.3891(8) 0.1785(5) 0.0004(7) 0.078(7) Uani 0.350(17) 1 d P A 2 H12A H 0.3991 0.1327 0.0477 0.117 Uiso 0.350(17) 1 calc PR A 2 H12B H 0.4540 0.1786 -0.0324 0.117 Uiso 0.350(17) 1 calc PR A 2 H12C H 0.3079 0.1767 -0.0578 0.117 Uiso 0.350(17) 1 calc PR A 2 O4 O 0.79008(14) 0.2500 0.04232(12) 0.0361(4) Uani 1 2 d S . . C13 C 0.8064(2) 0.2500 -0.05929(19) 0.0426(7) Uani 1 2 d S . . C14 C 0.7504(3) 0.32273(18) -0.12288(19) 0.0887(9) Uani 1 1 d . . . H14A H 0.6606 0.3221 -0.1401 0.133 Uiso 1 1 calc R . . H14B H 0.7687 0.3243 -0.1911 0.133 Uiso 1 1 calc R . . H14C H 0.7856 0.3689 -0.0787 0.133 Uiso 1 1 calc R . . C15 C 0.9446(3) 0.2500 -0.0429(3) 0.0719(10) Uani 1 2 d S . . H15A H 0.9816 0.2007 -0.0092 0.108 Uiso 0.50 1 calc PR . . H15B H 0.9852 0.2934 0.0049 0.108 Uiso 0.50 1 calc PR . . H15C H 0.9555 0.2559 -0.1140 0.108 Uiso 0.50 1 calc PR . . O5 O 0.61011(10) 0.41721(6) 0.27385(9) 0.0340(3) Uani 1 1 d . . . C16 C 0.56607(15) 0.49229(10) 0.27788(15) 0.0397(4) Uani 1 1 d . . . C17 C 0.6519(2) 0.53493(13) 0.3800(2) 0.0781(8) Uani 1 1 d . . . H17A H 0.6547 0.5062 0.4460 0.117 Uiso 1 1 calc R . . H17B H 0.6204 0.5877 0.3827 0.117 Uiso 1 1 calc R . . H17C H 0.7354 0.5380 0.3764 0.117 Uiso 1 1 calc R . . C18 C 0.43669(16) 0.48985(12) 0.28637(17) 0.0476(5) Uani 1 1 d . . . H18A H 0.3799 0.4628 0.2224 0.071 Uiso 1 1 calc R . . H18B H 0.4073 0.5432 0.2890 0.071 Uiso 1 1 calc R . . H18C H 0.4402 0.4620 0.3532 0.071 Uiso 1 1 calc R . . C19 C 0.5597(3) 0.53742(15) 0.1758(2) 0.0912(10) Uani 1 1 d . . . H19A H 0.6420 0.5393 0.1696 0.137 Uiso 1 1 calc R . . H19B H 0.5309 0.5906 0.1807 0.137 Uiso 1 1 calc R . . H19C H 0.5021 0.5115 0.1112 0.137 Uiso 1 1 calc R . . O6 O 0.92621(9) 0.33529(6) 0.27820(9) 0.0291(3) Uani 1 1 d . . . C20 C 1.00458(14) 0.39845(10) 0.27798(14) 0.0344(4) Uani 1 1 d . . . C21 C 1.0304(2) 0.44769(12) 0.38119(17) 0.0544(5) Uani 1 1 d . . . H21A H 0.9537 0.4727 0.3806 0.082 Uiso 1 1 calc R . . H21B H 1.0919 0.4878 0.3834 0.082 Uiso 1 1 calc R . . H21C H 1.0623 0.4142 0.4459 0.082 Uiso 1 1 calc R . . C22 C 1.1269(2) 0.36730(14) 0.2737(3) 0.0791(8) Uani 1 1 d . . . H22A H 1.1667 0.3347 0.3381 0.119 Uiso 1 1 calc R . . H22B H 1.1813 0.4111 0.2731 0.119 Uiso 1 1 calc R . . H22C H 1.1114 0.3361 0.2071 0.119 Uiso 1 1 calc R . . C23 C 0.9445(2) 0.45149(13) 0.17924(18) 0.0636(6) Uani 1 1 d . . . H23A H 0.9222 0.4206 0.1118 0.095 Uiso 1 1 calc R . . H23B H 1.0029 0.4925 0.1772 0.095 Uiso 1 1 calc R . . H23C H 0.8699 0.4753 0.1855 0.095 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 K1 0.02937(18) 0.0348(2) 0.0376(2) -0.00015(17) 0.01010(15) 0.00338(16) K2 0.0376(2) 0.0427(2) 0.0417(2) 0.00314(18) 0.02001(17) 0.00349(18) Li1 0.0300(19) 0.033(2) 0.030(2) 0.000 0.0084(16) 0.000 Li2 0.0295(18) 0.035(2) 0.032(2) 0.000 0.0113(16) 0.000 Li3 0.0341(13) 0.0282(15) 0.0328(14) 0.0019(12) 0.0131(11) 0.0013(12) O1 0.0288(7) 0.0291(9) 0.0248(8) 0.000 0.0117(6) 0.000 C1 0.0291(11) 0.0393(14) 0.0267(11) 0.000 0.0129(9) 0.000 C2 0.0777(14) 0.0538(13) 0.0445(11) -0.0132(10) 0.0359(11) -0.0074(11) C3 0.0332(14) 0.128(3) 0.0553(19) 0.000 0.0227(14) 0.000 O2 0.0298(8) 0.0398(10) 0.0247(8) 0.000 0.0048(6) 0.000 C4 0.0303(11) 0.0335(14) 0.0258(12) 0.000 0.0033(9) 0.000 C5 0.0548(11) 0.0500(13) 0.0381(10) -0.0092(9) 0.0080(9) 0.0034(10) C6 0.0311(13) 0.0566(19) 0.0486(16) 0.000 0.0050(12) 0.000 O3 0.0272(8) 0.0362(9) 0.0240(8) 0.000 0.0066(6) 0.000 C7 0.0274(11) 0.0454(16) 0.0302(12) 0.000 0.0054(10) 0.000 C8 0.054(4) 0.143(18) 0.037(4) 0.047(10) -0.004(3) -0.028(10) C9 0.045(8) 0.075(8) 0.086(9) 0.013(7) -0.024(7) -0.031(6) C10 0.057(12) 0.20(3) 0.10(2) -0.11(2) -0.035(10) 0.065(14) C11 0.003(5) 0.34(5) 0.062(12) 0.000 -0.004(6) 0.000 C12 0.058(6) 0.071(9) 0.064(8) -0.036(7) -0.032(6) 0.009(7) O4 0.0343(8) 0.0523(11) 0.0242(8) 0.000 0.0131(7) 0.000 C13 0.0391(13) 0.0672(19) 0.0240(12) 0.000 0.0142(10) 0.000 C14 0.107(2) 0.119(2) 0.0488(14) 0.0360(15) 0.0380(14) 0.0440(19) C15 0.0519(17) 0.120(3) 0.0531(19) 0.000 0.0300(15) 0.000 O5 0.0344(6) 0.0243(6) 0.0452(7) 0.0016(5) 0.0162(5) 0.0046(5) C16 0.0378(9) 0.0246(10) 0.0608(12) 0.0050(9) 0.0224(9) 0.0053(8) C17 0.0456(12) 0.0449(14) 0.136(2) -0.0370(15) 0.0210(14) -0.0042(11) C18 0.0383(9) 0.0393(11) 0.0671(13) -0.0036(10) 0.0204(9) 0.0067(9) C19 0.118(2) 0.0560(16) 0.134(2) 0.0535(16) 0.087(2) 0.0454(15) O6 0.0288(5) 0.0261(6) 0.0325(6) 0.0009(5) 0.0106(5) -0.0018(5) C20 0.0313(8) 0.0311(10) 0.0424(9) 0.0001(8) 0.0149(7) -0.0051(8) C21 0.0647(13) 0.0409(12) 0.0554(12) -0.0081(10) 0.0177(10) -0.0190(10) C22 0.0455(12) 0.0609(16) 0.147(3) -0.0180(16) 0.0545(15) -0.0121(11) C23 0.0754(15) 0.0498(13) 0.0583(13) 0.0170(11) 0.0136(11) -0.0227(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 K1 O2 2.6435(11) . ? K1 O5 2.6447(12) . ? K1 O6 2.8425(11) . ? K1 O1 2.8492(11) . ? K2 O4 2.6366(11) . ? K2 O5 2.6472(12) . ? K2 O3 2.8768(11) . ? K2 O6 2.9309(11) . ? Li1 O2 1.828(4) . ? Li1 O6 1.918(3) 4_565 ? Li1 O6 1.918(3) . ? Li2 O4 1.824(4) . ? Li2 O6 1.910(3) . ? Li2 O6 1.910(3) 4_565 ? Li3 O5 1.815(3) . ? Li3 O3 1.911(3) . ? Li3 O1 1.919(3) . ? O1 C1 1.413(3) . ? O1 Li3 1.919(3) 4_565 ? O1 K1 2.8492(11) 4_565 ? C1 C2 1.521(2) . ? C1 C2 1.521(2) 4_565 ? C1 C3 1.531(3) . ? O2 C4 1.394(3) . ? O2 Li1 1.828(4) 4_565 ? O2 K1 2.6435(11) 4_565 ? C4 C6 1.528(3) . ? C4 C5 1.530(2) . ? C4 C5 1.530(2) 4_565 ? O3 C7 1.413(3) . ? O3 Li3 1.911(3) 4_565 ? O3 K2 2.8768(11) 4_565 ? C7 C10 1.437(19) 4_565 ? C7 C10 1.437(19) . ? C7 C12 1.476(7) . ? C7 C12 1.476(7) 4_565 ? C7 C8 1.521(8) 4_565 ? C7 C8 1.521(8) . ? C7 C11 1.53(2) . ? C7 C9 1.591(19) . ? C7 C9 1.591(19) 4_565 ? O4 C13 1.398(3) . ? O4 K2 2.6366(11) 4_565 ? C13 C14 1.513(3) 4_565 ? C13 C14 1.513(3) . ? C13 C15 1.531(4) . ? O5 C16 1.392(2) . ? C16 C19 1.517(3) . ? C16 C18 1.533(2) . ? C16 C17 1.540(3) . ? O6 C20 1.4108(19) . ? O6 Li1 1.918(3) 4_565 ? C20 C21 1.526(3) . ? C20 C22 1.526(3) . ? C20 C23 1.531(3) . ? 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 O2 K1 O5 150.73(4) . . ? O2 K1 O6 73.11(4) . . ? O5 K1 O6 90.07(3) . . ? O2 K1 O1 89.80(3) . . ? O5 K1 O1 72.56(3) . . ? O6 K1 O1 108.21(4) . . ? O4 K2 O5 148.75(4) . . ? O4 K2 O3 90.85(3) . . ? O5 K2 O3 72.55(3) . . ? O4 K2 O6 71.72(4) . . ? O5 K2 O6 88.14(3) . . ? O3 K2 O6 108.07(4) . . ? O2 Li1 O6 121.71(13) . 4_565 ? O2 Li1 O6 121.71(13) . . ? O6 Li1 O6 99.42(18) 4_565 . ? O4 Li2 O6 122.23(12) . . ? O4 Li2 O6 122.23(12) . 4_565 ? O6 Li2 O6 99.93(18) . 4_565 ? O5 Li3 O3 122.95(15) . . ? O5 Li3 O1 121.30(15) . . ? O3 Li3 O1 99.29(13) . . ? C1 O1 Li3 119.34(12) . 4_565 ? C1 O1 Li3 119.34(12) . . ? Li3 O1 Li3 79.06(17) 4_565 . ? C1 O1 K1 110.38(8) . . ? Li3 O1 K1 130.28(10) 4_565 . ? Li3 O1 K1 78.02(8) . . ? C1 O1 K1 110.38(8) . 4_565 ? Li3 O1 K1 78.02(8) 4_565 4_565 ? Li3 O1 K1 130.28(10) . 4_565 ? K1 O1 K1 84.28(4) . 4_565 ? O1 C1 C2 110.83(12) . . ? O1 C1 C2 110.84(12) . 4_565 ? C2 C1 C2 108.2(2) . 4_565 ? O1 C1 C3 109.26(19) . . ? C2 C1 C3 108.81(14) . . ? C2 C1 C3 108.81(14) 4_565 . ? C4 O2 Li1 132.48(18) . 4_565 ? C4 O2 Li1 132.48(18) . . ? Li1 O2 Li1 0.00(2) 4_565 . ? C4 O2 K1 124.61(7) . 4_565 ? Li1 O2 K1 84.62(9) 4_565 4_565 ? Li1 O2 K1 84.62(9) . 4_565 ? C4 O2 K1 124.61(7) . . ? Li1 O2 K1 84.62(9) 4_565 . ? Li1 O2 K1 84.62(9) . . ? K1 O2 K1 92.63(5) 4_565 . ? O2 C4 C6 110.13(19) . . ? O2 C4 C5 110.11(13) . . ? C6 C4 C5 108.87(14) . . ? O2 C4 C5 110.11(13) . 4_565 ? C6 C4 C5 108.87(14) . 4_565 ? C5 C4 C5 108.7(2) . 4_565 ? C7 O3 Li3 120.89(12) . . ? C7 O3 Li3 120.89(12) . 4_565 ? Li3 O3 Li3 79.47(17) . 4_565 ? C7 O3 K2 110.68(9) . . ? Li3 O3 K2 76.83(8) . . ? Li3 O3 K2 128.35(10) 4_565 . ? C7 O3 K2 110.68(9) . 4_565 ? Li3 O3 K2 128.35(10) . 4_565 ? Li3 O3 K2 76.83(8) 4_565 4_565 ? K2 O3 K2 83.13(4) . 4_565 ? O3 C7 C10 115.3(7) . 4_565 ? O3 C7 C10 115.3(7) . . ? O3 C7 C12 109.2(3) . . ? O3 C7 C12 109.2(3) . 4_565 ? C12 C7 C12 112.4(9) . 4_565 ? O3 C7 C8 110.6(3) . 4_565 ? C10 C7 C8 114.0(11) 4_565 4_565 ? O3 C7 C8 110.6(3) . . ? C10 C7 C8 114.0(11) . . ? O3 C7 C11 102.6(8) . . ? C12 C7 C11 111.5(6) . . ? C12 C7 C11 111.5(6) 4_565 . ? O3 C7 C9 109.2(6) . . ? C10 C7 C9 101.6(10) . . ? C8 C7 C9 105.2(12) . . ? O3 C7 C9 109.2(6) . 4_565 ? C10 C7 C9 101.6(10) 4_565 4_565 ? C8 C7 C9 105.2(12) 4_565 4_565 ? C13 O4 Li2 128.92(18) . . ? C13 O4 K2 125.14(7) . 4_565 ? Li2 O4 K2 86.24(9) . 4_565 ? C13 O4 K2 125.14(7) . . ? Li2 O4 K2 86.24(9) . . ? K2 O4 K2 92.75(5) 4_565 . ? O4 C13 C14 110.23(14) . 4_565 ? O4 C13 C14 110.23(14) . . ? C14 C13 C14 111.1(3) 4_565 . ? O4 C13 C15 109.9(2) . . ? C14 C13 C15 107.65(16) 4_565 . ? C14 C13 C15 107.65(16) . . ? C16 O5 Li3 132.90(13) . . ? C16 O5 K1 121.86(10) . . ? Li3 O5 K1 85.47(9) . . ? C16 O5 K2 125.32(10) . . ? Li3 O5 K2 84.75(9) . . ? K1 O5 K2 94.06(4) . . ? O5 C16 C19 110.34(16) . . ? O5 C16 C18 110.71(15) . . ? C19 C16 C18 108.80(17) . . ? O5 C16 C17 109.74(15) . . ? C19 C16 C17 109.6(2) . . ? C18 C16 C17 107.59(16) . . ? C20 O6 Li2 120.84(13) . . ? C20 O6 Li1 120.82(13) . 4_565 ? Li2 O6 Li1 78.76(13) . 4_565 ? C20 O6 Li1 120.82(13) . . ? Li2 O6 Li1 78.76(13) . . ? Li1 O6 Li1 0.00(19) 4_565 . ? C20 O6 K1 110.51(9) . . ? Li2 O6 K1 128.58(11) . . ? Li1 O6 K1 77.64(11) 4_565 . ? Li1 O6 K1 77.64(11) . . ? C20 O6 K2 109.93(9) . . ? Li2 O6 K2 76.62(11) . . ? Li1 O6 K2 129.23(11) 4_565 . ? Li1 O6 K2 129.23(11) . . ? K1 O6 K2 84.23(3) . . ? O6 C20 C21 110.74(14) . . ? O6 C20 C22 109.32(15) . . ? C21 C20 C22 108.86(17) . . ? O6 C20 C23 110.71(14) . . ? C21 C20 C23 107.69(16) . . ? C22 C20 C23 109.48(18) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.231 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.039