Supplementary Material (ESI) for Dalton Transactions his journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Marcus L. Cole' 'Cameron Jones' 'Peter C. Junk' _publ_contact_author_name 'Dr Peter Junk' _publ_contact_author_address ; Dr Peter Junk School of Chemistry Monash University Box 23 Clayton Victoria 3800 AUSTRALIA ; _publ_contact_author_email 'PETER.JUNK@SCI.MONASH.EDU.AU' _publ_section_title ; Ether and Crown Ether Adduct Complexes of Sodium and Potassium Cyclopentadienide and Methylcyclopentadienide - Molecular Structures of [Na(dme)Cp]09[K(dme)0.5Cp]009[Na(15-Crown-5)Cp, [Na(18-Crown-6)CpMe] and the "Naked Cp-" Complex [K(15-Crown-5)2][Cp] ; data_COMPOUND_1#d:\junkie\xtals\bonocpxs\marcus\nacpdme\pj269 _database_code_CSD 172086 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H15 Na O2' _chemical_formula_weight 178.20 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 29.799(13) _cell_length_b 8.149(3) _cell_length_c 9.379(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2277.7(17) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.039 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9697 _exptl_absorpt_correction_T_max 0.9898 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10030 _diffrn_reflns_av_R_equivalents 0.1673 _diffrn_reflns_av_sigmaI/netI 0.1724 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 23.32 _reflns_number_total 3239 _reflns_number_gt 749 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0867P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 3(2) _refine_ls_number_reflns 3239 _refine_ls_number_parameters 221 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2679 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.2395 _refine_ls_wR_factor_gt 0.1538 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 1.289 _refine_ls_shift/su_mean 0.218 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.15297(10) 0.3449(3) 0.3540(9) 0.0905(11) Uani 1 1 d . . . O1 O 0.1875(3) 0.6173(9) 0.356(2) 0.144(3) Uani 1 1 d . . . C1 C 0.0910(10) 0.338(6) 0.126(4) 0.23(2) Uani 1 1 d . . . H1 H 0.0627 0.3836 0.1412 0.278 Uiso 1 1 calc R . . Na2 Na 0.09565(11) 0.2204(3) 0.8538(9) 0.0918(12) Uani 1 1 d . . . O2 O 0.2353(3) 0.3294(13) 0.362(2) 0.158(4) Uani 1 1 d . . . C2 C 0.1058(10) 0.177(4) 0.154(2) 0.165(13) Uani 1 1 d . . . H2 H 0.0901 0.0937 0.2006 0.198 Uiso 1 1 calc R . . O3 O 0.0131(3) 0.2306(12) 0.850(2) 0.159(4) Uani 1 1 d . . . C3 C 0.1489(9) 0.168(3) 0.097(2) 0.115(10) Uani 1 1 d . . . H3 H 0.1658 0.0721 0.0876 0.139 Uiso 1 1 calc R . . O4 O 0.0627(3) -0.0534(11) 0.855(3) 0.157(3) Uani 1 1 d . . . C4 C 0.1610(7) 0.304(3) 0.0613(19) 0.101(6) Uani 1 1 d . . . H4 H 0.1901 0.3263 0.0305 0.122 Uiso 1 1 calc R . . C5 C 0.1305(12) 0.415(3) 0.069(2) 0.129(9) Uani 1 1 d . . . H5 H 0.1334 0.5246 0.0434 0.155 Uiso 1 1 calc R . . C6 C 0.0878(7) 0.289(4) 0.5638(15) 0.100(6) Uani 1 1 d . . . H6 H 0.0579 0.2908 0.5353 0.120 Uiso 1 1 calc R . . C7 C 0.1109(10) 0.155(3) 0.5618(17) 0.107(8) Uani 1 1 d . . . H7 H 0.1008 0.0532 0.5296 0.129 Uiso 1 1 calc R . . C8 C 0.1507(8) 0.186(4) 0.613(3) 0.142(13) Uani 1 1 d . . . H8 H 0.1744 0.1126 0.6207 0.170 Uiso 1 1 calc R . . C9 C 0.1511(12) 0.359(4) 0.6553(18) 0.158(14) Uani 1 1 d . . . H9 H 0.1734 0.4185 0.7017 0.190 Uiso 1 1 calc R . . C10 C 0.1069(11) 0.414(4) 0.605(2) 0.147(10) Uani 1 1 d . . . H10 H 0.0957 0.5204 0.6043 0.177 Uiso 1 1 calc R . . C11 C 0.1635(5) 0.7621(13) 0.387(5) 0.202(12) Uani 1 1 d . . . H11A H 0.1468 0.7476 0.4737 0.303 Uiso 1 1 calc R . . H11B H 0.1433 0.7858 0.3103 0.303 Uiso 1 1 calc R . . H11C H 0.1842 0.8516 0.3985 0.303 Uiso 1 1 calc R . . C12 C 0.2331(6) 0.6131(18) 0.349(4) 0.188(7) Uani 1 1 d . . . H12A H 0.2444 0.6891 0.4205 0.226 Uiso 1 1 calc R . . H12B H 0.2417 0.6565 0.2570 0.226 Uiso 1 1 calc R . . C13 C 0.2556(5) 0.468(2) 0.368(3) 0.207(11) Uani 1 1 d . . . H13A H 0.2792 0.4648 0.2964 0.249 Uiso 1 1 calc R . . H13B H 0.2703 0.4733 0.4597 0.249 Uiso 1 1 calc R . . C14 C 0.2603(4) 0.1889(15) 0.381(4) 0.183(9) Uani 1 1 d . . . H14A H 0.2900 0.2057 0.3436 0.275 Uiso 1 1 calc R . . H14B H 0.2463 0.0994 0.3312 0.275 Uiso 1 1 calc R . . H14C H 0.2621 0.1637 0.4805 0.275 Uiso 1 1 calc R . . C15 C -0.0113(5) 0.3726(16) 0.886(4) 0.219(12) Uani 1 1 d . . . H15A H -0.0333 0.3937 0.8131 0.328 Uiso 1 1 calc R . . H15B H 0.0089 0.4642 0.8923 0.328 Uiso 1 1 calc R . . H15C H -0.0261 0.3569 0.9755 0.328 Uiso 1 1 calc R . . C16 C -0.0057(5) 0.090(2) 0.880(3) 0.197(11) Uani 1 1 d . . . H16A H -0.0341 0.0848 0.8293 0.236 Uiso 1 1 calc R . . H16B H -0.0125 0.0884 0.9811 0.236 Uiso 1 1 calc R . . C17 C 0.0193(7) -0.0558(19) 0.847(5) 0.199(9) Uani 1 1 d . . . H17A H 0.0088 -0.1420 0.9098 0.238 Uiso 1 1 calc R . . H17B H 0.0114 -0.0881 0.7505 0.238 Uiso 1 1 calc R . . C18 C 0.0874(6) -0.1993(13) 0.859(4) 0.252(11) Uani 1 1 d . . . H18A H 0.0852 -0.2463 0.9531 0.378 Uiso 1 1 calc R . . H18B H 0.1183 -0.1766 0.8380 0.378 Uiso 1 1 calc R . . H18C H 0.0756 -0.2752 0.7906 0.378 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 Na1 0.084(2) 0.105(2) 0.083(2) 0.004(6) -0.002(5) -0.0038(19) O1 0.122(7) 0.112(6) 0.198(8) 0.022(16) 0.011(17) -0.029(5) C1 0.11(2) 0.38(5) 0.21(3) -0.16(3) -0.09(2) 0.15(3) Na2 0.085(2) 0.108(2) 0.083(3) 0.015(6) -0.007(5) -0.0097(18) O2 0.086(6) 0.166(8) 0.221(12) 0.084(15) 0.003(13) -0.011(6) C2 0.099(19) 0.30(4) 0.099(15) 0.070(19) 0.015(14) -0.10(2) O3 0.078(6) 0.172(8) 0.226(12) 0.039(19) -0.013(14) 0.002(5) C3 0.19(3) 0.079(14) 0.080(14) -0.013(11) -0.030(15) -0.016(14) O4 0.125(7) 0.142(7) 0.205(8) -0.003(18) 0.006(19) -0.038(6) C4 0.091(14) 0.132(17) 0.081(12) 0.006(12) -0.001(9) 0.012(15) C5 0.20(3) 0.087(12) 0.103(15) 0.012(13) -0.072(17) -0.007(16) C6 0.099(15) 0.150(16) 0.052(9) -0.035(11) 0.011(9) -0.018(15) C7 0.15(3) 0.082(11) 0.091(14) 0.013(10) 0.044(15) 0.016(14) C8 0.059(15) 0.24(4) 0.13(2) 0.065(19) 0.006(12) 0.061(18) C9 0.25(4) 0.18(3) 0.040(11) -0.026(14) 0.019(16) -0.11(2) C10 0.22(3) 0.14(2) 0.083(15) 0.039(15) 0.010(16) 0.04(2) C11 0.199(16) 0.102(8) 0.30(3) 0.03(2) 0.02(2) 0.028(9) C12 0.159(16) 0.171(14) 0.236(19) 0.04(3) 0.00(3) -0.096(12) C13 0.112(13) 0.182(16) 0.33(3) 0.11(3) -0.11(2) -0.051(12) C14 0.117(11) 0.196(12) 0.24(3) 0.07(2) 0.024(18) 0.052(10) C15 0.176(15) 0.184(12) 0.30(3) -0.02(2) -0.05(2) 0.093(12) C16 0.127(16) 0.26(2) 0.20(3) 0.06(2) 0.059(18) -0.086(16) C17 0.20(2) 0.147(13) 0.25(2) 0.03(3) -0.01(4) -0.070(15) C18 0.32(2) 0.076(8) 0.35(3) 0.00(3) -0.09(4) 0.059(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Na1 O1 2.447(7) . ? Na1 O2 2.457(8) . ? Na1 C2 2.72(2) . ? Na1 C8 2.75(2) . ? Na1 C4 2.78(2) . ? Na1 C10 2.78(2) . ? Na1 C7 2.788(18) . ? Na1 C6 2.802(18) . ? Na1 C3 2.814(18) . ? Na1 C5 2.81(2) . ? Na1 C9 2.83(2) . ? Na1 C1 2.82(3) . ? O1 C12 1.361(13) . ? O1 C11 1.409(15) . ? C1 C2 1.41(4) . ? C1 C5 1.43(4) . ? C1 Na2 2.73(3) 1_554 ? Na2 O4 2.438(8) . ? Na2 O3 2.463(9) . ? Na2 C1 2.73(3) 1_556 ? Na2 C9 2.73(2) . ? Na2 C5 2.77(2) 1_556 ? Na2 C6 2.787(18) . ? Na2 C8 2.81(2) . ? Na2 C3 2.81(2) 1_556 ? Na2 C7 2.828(19) . ? Na2 C4 2.84(2) 1_556 ? Na2 C10 2.84(2) . ? Na2 C2 2.85(2) 1_556 ? O2 C13 1.281(12) . ? O2 C14 1.378(11) . ? C2 C3 1.39(3) . ? C2 Na2 2.85(2) 1_554 ? O3 C16 1.304(14) . ? O3 C15 1.405(17) . ? C3 C4 1.22(3) . ? C3 Na2 2.81(2) 1_554 ? O4 C17 1.295(16) . ? O4 C18 1.400(11) . ? C4 C5 1.29(3) . ? C4 Na2 2.84(2) 1_554 ? C5 Na2 2.77(2) 1_554 ? C6 C10 1.23(3) . ? C6 C7 1.29(3) . ? C7 C8 1.31(2) . ? C8 C9 1.46(3) . ? C9 C10 1.47(3) . ? C12 C13 1.372(15) . ? C16 C17 1.44(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 O1 Na1 O2 68.1(3) . . ? O1 Na1 C2 133.0(8) . . ? O2 Na1 C2 120.7(9) . . ? O1 Na1 C8 115.4(10) . . ? O2 Na1 C8 88.5(6) . . ? C2 Na1 C8 111.1(9) . . ? O1 Na1 C4 94.7(8) . . ? O2 Na1 C4 86.4(7) . . ? C2 Na1 C4 45.7(6) . . ? C8 Na1 C4 144.9(10) . . ? O1 Na1 C10 90.9(9) . . ? O2 Na1 C10 118.6(9) . . ? C2 Na1 C10 115.5(10) . . ? C8 Na1 C10 48.4(7) . . ? C4 Na1 C10 154.6(8) . . ? O1 Na1 C7 133.4(7) . . ? O2 Na1 C7 113.6(8) . . ? C2 Na1 C7 88.2(5) . . ? C8 Na1 C7 27.3(5) . . ? C4 Na1 C7 131.5(7) . . ? C10 Na1 C7 45.5(7) . . ? O1 Na1 C6 115.6(7) . . ? O2 Na1 C6 131.5(7) . . ? C2 Na1 C6 92.5(6) . . ? C8 Na1 C6 44.5(6) . . ? C4 Na1 C6 137.3(6) . . ? C10 Na1 C6 25.4(6) . . ? C7 Na1 C6 26.7(6) . . ? O1 Na1 C3 119.5(8) . . ? O2 Na1 C3 92.4(7) . . ? C2 Na1 C3 29.1(6) . . ? C8 Na1 C3 120.9(8) . . ? C4 Na1 C3 25.1(5) . . ? C10 Na1 C3 143.9(9) . . ? C7 Na1 C3 107.1(7) . . ? C6 Na1 C3 119.2(7) . . ? O1 Na1 C5 85.7(7) . . ? O2 Na1 C5 106.1(9) . . ? C2 Na1 C5 47.4(7) . . ? C8 Na1 C5 158.1(9) . . ? C4 Na1 C5 26.6(7) . . ? C10 Na1 C5 130.1(8) . . ? C7 Na1 C5 132.0(8) . . ? C6 Na1 C5 122.3(9) . . ? C3 Na1 C5 44.0(6) . . ? O1 Na1 C9 87.8(8) . . ? O2 Na1 C9 89.6(9) . . ? C2 Na1 C9 134.5(6) . . ? C8 Na1 C9 30.4(7) . . ? C4 Na1 C9 174.0(10) . . ? C10 Na1 C9 30.3(7) . . ? C7 Na1 C9 46.8(6) . . ? C6 Na1 C9 44.9(7) . . ? C3 Na1 C9 151.2(9) . . ? C5 Na1 C9 159.3(11) . . ? O1 Na1 C1 107.4(12) . . ? O2 Na1 C1 132.4(9) . . ? C2 Na1 C1 29.5(8) . . ? C8 Na1 C1 130.0(11) . . ? C4 Na1 C1 46.1(8) . . ? C10 Na1 C1 108.7(9) . . ? C7 Na1 C1 102.9(11) . . ? C6 Na1 C1 94.3(9) . . ? C3 Na1 C1 46.7(7) . . ? C5 Na1 C1 29.5(9) . . ? C9 Na1 C1 138.0(10) . . ? C12 O1 C11 122.5(11) . . ? C12 O1 Na1 113.4(7) . . ? C11 O1 Na1 123.2(8) . . ? C2 C1 C5 102.6(19) . . ? C2 C1 Na2 80.1(15) . 1_554 ? C5 C1 Na2 76.4(16) . 1_554 ? C2 C1 Na1 71.0(15) . . ? C5 C1 Na1 74.7(13) . . ? Na2 C1 Na1 132.9(9) 1_554 . ? O4 Na2 O3 68.1(3) . . ? O4 Na2 C1 107.4(13) . 1_556 ? O3 Na2 C1 87.1(8) . 1_556 ? O4 Na2 C9 128.6(9) . . ? O3 Na2 C9 125.5(10) . . ? C1 Na2 C9 121.5(11) 1_556 . ? O4 Na2 C5 132.3(9) . 1_556 ? O3 Na2 C5 111.4(9) . 1_556 ? C1 Na2 C5 30.2(8) 1_556 1_556 ? C9 Na2 C5 92.0(6) . 1_556 ? O4 Na2 C6 98.7(8) . . ? O3 Na2 C6 84.1(7) . . ? C1 Na2 C6 146.9(10) 1_556 . ? C9 Na2 C6 45.8(6) . . ? C5 Na2 C6 129.0(8) 1_556 . ? O4 Na2 C8 98.5(10) . . ? O3 Na2 C8 125.3(8) . . ? C1 Na2 C8 144.8(10) 1_556 . ? C9 Na2 C8 30.6(7) . . ? C5 Na2 C8 115.2(10) 1_556 . ? C6 Na2 C8 44.2(6) . . ? O4 Na2 C3 94.9(7) . 1_556 ? O3 Na2 C3 125.4(8) . 1_556 ? C1 Na2 C3 47.5(7) 1_556 1_556 ? C9 Na2 C3 105.9(8) . 1_556 ? C5 Na2 C3 44.3(7) 1_556 1_556 ? C6 Na2 C3 150.4(7) . 1_556 ? C8 Na2 C3 107.9(6) . 1_556 ? O4 Na2 C7 83.9(8) . . ? O3 Na2 C7 98.9(9) . . ? C1 Na2 C7 168.6(11) 1_556 . ? C9 Na2 C7 47.3(6) . . ? C5 Na2 C7 139.1(7) 1_556 . ? C6 Na2 C7 26.6(5) . . ? C8 Na2 C7 26.8(5) . . ? C3 Na2 C7 131.8(8) 1_556 . ? O4 Na2 C4 119.7(8) . 1_556 ? O3 Na2 C4 133.4(7) . 1_556 ? C1 Na2 C4 46.3(7) 1_556 1_556 ? C9 Na2 C4 87.3(6) . 1_556 ? C5 Na2 C4 26.5(7) 1_556 1_556 ? C6 Na2 C4 132.8(6) . 1_556 ? C8 Na2 C4 100.1(8) . 1_556 ? C3 Na2 C4 24.9(5) 1_556 1_556 ? C7 Na2 C4 126.9(8) . 1_556 ? O4 Na2 C10 123.9(10) . . ? O3 Na2 C10 95.1(9) . . ? C1 Na2 C10 125.5(12) 1_556 . ? C9 Na2 C10 30.5(7) . . ? C5 Na2 C10 103.8(9) 1_556 . ? C6 Na2 C10 25.2(6) . . ? C8 Na2 C10 47.4(7) . . ? C3 Na2 C10 133.3(9) 1_556 . ? C7 Na2 C10 44.7(7) . . ? C4 Na2 C10 110.5(9) 1_556 . ? O4 Na2 C2 85.7(9) . 1_556 ? O3 Na2 C2 97.1(8) . 1_556 ? C1 Na2 C2 29.2(8) 1_556 1_556 ? C9 Na2 C2 131.3(7) . 1_556 ? C5 Na2 C2 46.5(7) 1_556 1_556 ? C6 Na2 C2 175.5(8) . 1_556 ? C8 Na2 C2 136.0(8) . 1_556 ? C3 Na2 C2 28.5(6) 1_556 1_556 ? C7 Na2 C2 156.2(9) . 1_556 ? C4 Na2 C2 44.0(6) 1_556 1_556 ? C10 Na2 C2 150.3(10) . 1_556 ? C13 O2 C14 118.0(12) . . ? C13 O2 Na1 115.3(9) . . ? C14 O2 Na1 125.9(8) . . ? C3 C2 C1 105(2) . . ? C3 C2 Na1 79.3(12) . . ? C1 C2 Na1 79.5(16) . . ? C3 C2 Na2 74.0(11) . 1_554 ? C1 C2 Na2 70.6(16) . 1_554 ? Na1 C2 Na2 132.3(8) . 1_554 ? C16 O3 C15 116.9(16) . . ? C16 O3 Na2 113.4(10) . . ? C15 O3 Na2 122.7(9) . . ? C4 C3 C2 109(2) . . ? C4 C3 Na1 75.7(13) . . ? C2 C3 Na1 71.5(12) . . ? C4 C3 Na2 78.7(13) . 1_554 ? C2 C3 Na2 77.5(12) . 1_554 ? Na1 C3 Na2 129.8(8) . 1_554 ? C17 O4 C18 121.0(12) . . ? C17 O4 Na2 114.6(10) . . ? C18 O4 Na2 124.4(8) . . ? C3 C4 C5 115(3) . . ? C3 C4 Na1 79.2(12) . . ? C5 C4 Na1 78.2(13) . . ? C3 C4 Na2 76.5(14) . 1_554 ? C5 C4 Na2 74.0(14) . 1_554 ? Na1 C4 Na2 130.4(8) . 1_554 ? C4 C5 C1 107(3) . . ? C4 C5 Na2 79.6(15) . 1_554 ? C1 C5 Na2 73.4(15) . 1_554 ? C4 C5 Na1 75.2(13) . . ? C1 C5 Na1 75.8(15) . . ? Na2 C5 Na1 131.8(9) 1_554 . ? C10 C6 C7 117(2) . . ? C10 C6 Na2 79.7(13) . . ? C7 C6 Na2 78.5(13) . . ? C10 C6 Na1 76.4(14) . . ? C7 C6 Na1 76.1(11) . . ? Na2 C6 Na1 131.3(8) . . ? C6 C7 C8 108(2) . . ? C6 C7 Na1 77.2(11) . . ? C8 C7 Na1 74.8(12) . . ? C6 C7 Na2 74.9(11) . . ? C8 C7 Na2 75.7(12) . . ? Na1 C7 Na2 130.1(8) . . ? C7 C8 C9 107(2) . . ? C7 C8 Na1 77.9(11) . . ? C9 C8 Na1 77.7(12) . . ? C7 C8 Na2 77.5(12) . . ? C9 C8 Na2 71.9(13) . . ? Na1 C8 Na2 132.7(8) . . ? C8 C9 C10 101(2) . . ? C8 C9 Na2 77.5(12) . . ? C10 C9 Na2 78.6(14) . . ? C8 C9 Na1 71.9(11) . . ? C10 C9 Na1 73.1(11) . . ? Na2 C9 Na1 132.5(9) . . ? C6 C10 C9 105(3) . . ? C6 C10 Na1 78.2(15) . . ? C9 C10 Na1 76.6(13) . . ? C6 C10 Na2 75.1(14) . . ? C9 C10 Na2 70.9(12) . . ? Na1 C10 Na2 130.0(10) . . ? O1 C12 C13 120.3(13) . . ? O2 C13 C12 121.6(14) . . ? O3 C16 C17 117.3(18) . . ? O4 C17 C16 120(2) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.169 _refine_diff_density_min -0.144 _refine_diff_density_rms 0.039 #===END data_COMPOUND_2#d:\junkie\xtals\bonocpxs\marcus\kcpdme\pj285a _database_code_CSD 172087 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H40 K4 O4' _chemical_formula_weight 597.00 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' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.972(3) _cell_length_b 11.280(4) _cell_length_c 17.045(6) _cell_angle_alpha 83.372(5) _cell_angle_beta 83.498(4) _cell_angle_gamma 82.935(7) _cell_volume 1692.0(10) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.172 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 632 _exptl_absorpt_coefficient_mu 0.553 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8091 _exptl_absorpt_correction_T_max 0.9217 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7399 _diffrn_reflns_av_R_equivalents 0.0987 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.21 _diffrn_reflns_theta_max 23.27 _reflns_number_total 4528 _reflns_number_gt 1817 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1758P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4528 _refine_ls_number_parameters 464 _refine_ls_number_restraints 205 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.0971 _refine_ls_wR_factor_ref 0.3152 _refine_ls_wR_factor_gt 0.2543 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.984 _refine_ls_shift/su_max 0.558 _refine_ls_shift/su_mean 0.090 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 0.4101(3) 0.3147(2) 0.35316(15) 0.0604(8) Uani 1 1 d . . . O1 O 0.3501(11) 0.3592(9) 0.5145(5) 0.086(3) Uani 1 1 d . A . C1 C 0.4608(16) 0.3584(13) 0.5687(8) 0.101(5) Uani 1 1 d . . . H1A H 0.4359 0.4261 0.5990 0.152 Uiso 1 1 calc R A . H1B H 0.5583 0.3631 0.5396 0.152 Uiso 1 1 calc R . . H1C H 0.4625 0.2856 0.6039 0.152 Uiso 1 1 calc R . . K2 K 0.4646(3) 0.8265(2) 0.18354(18) 0.0759(10) Uani 1 1 d . . . O2 O 0.1549(10) 0.2213(7) 0.4541(5) 0.075(3) Uani 1 1 d . A . C2 C 0.2064(16) 0.3416(14) 0.5544(7) 0.088(5) Uani 1 1 d . . . H2A H 0.1660 0.4115 0.5815 0.105 Uiso 1 1 calc R A . H2B H 0.2151 0.2725 0.5938 0.105 Uiso 1 1 calc R . . K3 K 0.0897(3) 0.6853(2) 0.14677(16) 0.0617(8) Uani 1 1 d . . . O3 O 0.3439(10) 0.7761(8) 0.0480(5) 0.073(3) Uani 1 1 d . A . C3 C 0.1022(15) 0.3218(11) 0.4953(8) 0.080(4) Uani 1 1 d . A . H3A H 0.0033 0.3109 0.5227 0.097 Uiso 1 1 calc R . . H3B H 0.0913 0.3927 0.4574 0.097 Uiso 1 1 calc R . . K4 K 0.0355(3) 0.1732(2) 0.31623(18) 0.0756(10) Uani 1 1 d . . . O4 O 0.1525(11) 0.6392(9) -0.0132(5) 0.086(3) Uani 1 1 d . A . C4 C 0.171(3) 0.1080(15) 0.4997(12) 0.175(10) Uani 1 1 d . . . H4A H 0.2671 0.0965 0.5211 0.263 Uiso 1 1 calc R A . H4B H 0.1660 0.0457 0.4665 0.263 Uiso 1 1 calc R . . H4C H 0.0918 0.1050 0.5424 0.263 Uiso 1 1 calc R . . C5 C 0.334(2) 0.8868(14) -0.0020(10) 0.147(8) Uani 1 1 d . . . H5A H 0.4059 0.8799 -0.0481 0.221 Uiso 1 1 calc R A . H5B H 0.3566 0.9499 0.0266 0.221 Uiso 1 1 calc R . . H5C H 0.2344 0.9050 -0.0182 0.221 Uiso 1 1 calc R . . C6 C 0.3983(14) 0.6769(13) 0.0054(7) 0.076(4) Uani 1 1 d . . . H6A H 0.4118 0.6059 0.0429 0.092 Uiso 1 1 calc R A . H6B H 0.4967 0.6903 -0.0218 0.092 Uiso 1 1 calc R . . C7 C 0.3003(16) 0.6534(15) -0.0533(8) 0.097(5) Uani 1 1 d . A . H7A H 0.2942 0.7199 -0.0948 0.117 Uiso 1 1 calc R . . H7B H 0.3412 0.5810 -0.0775 0.117 Uiso 1 1 calc R . . C8 C 0.0429(16) 0.6321(14) -0.0647(8) 0.108(6) Uani 1 1 d . . . H8A H 0.0254 0.7078 -0.0962 0.161 Uiso 1 1 calc R A . H8B H -0.0495 0.6133 -0.0343 0.161 Uiso 1 1 calc R . . H8C H 0.0779 0.5704 -0.0990 0.161 Uiso 1 1 calc R . . C1A C 0.136(3) 0.460(2) 0.2541(17) 0.062(7) Uani 0.59(3) 1 d PDU A 1 H1A1 H 0.0478 0.4224 0.2583 0.075 Uiso 0.59(3) 1 calc PR A 1 C2A C 0.174(3) 0.543(3) 0.2965(15) 0.074(9) Uani 0.59(3) 1 d PDU A 1 H2A1 H 0.1078 0.5755 0.3365 0.089 Uiso 0.59(3) 1 calc PR A 1 C3A C 0.315(3) 0.5779(18) 0.2781(12) 0.051(6) Uani 0.59(3) 1 d PDU A 1 H3A1 H 0.3625 0.6303 0.3027 0.061 Uiso 0.59(3) 1 calc PR A 1 C4A C 0.368(2) 0.517(2) 0.2154(12) 0.047(6) Uani 0.59(3) 1 d PDU A 1 H4A1 H 0.4605 0.5233 0.1853 0.056 Uiso 0.59(3) 1 calc PR A 1 C5A C 0.263(3) 0.446(3) 0.204(2) 0.105(11) Uani 0.59(3) 1 d PDU A 1 H5A1 H 0.2768 0.3933 0.1649 0.127 Uiso 0.59(3) 1 calc PR A 1 C6A C 0.7001(17) 0.1325(14) 0.3516(10) 0.065(4) Uani 0.91(2) 1 d PU . 5 H6A1 H 0.6820 0.0523 0.3590 0.078 Uiso 0.91(2) 1 calc PR . 5 C7A C 0.7192(19) 0.2005(14) 0.4111(11) 0.074(5) Uani 0.91(2) 1 d PU . 5 H7A1 H 0.7154 0.1769 0.4653 0.089 Uiso 0.91(2) 1 calc PR . 5 C8A C 0.7462(17) 0.3159(15) 0.3707(12) 0.073(5) Uani 0.91(2) 1 d PU . 5 H8A1 H 0.7664 0.3810 0.3951 0.087 Uiso 0.91(2) 1 calc PR . 5 C9A C 0.7383(15) 0.3160(13) 0.2947(11) 0.066(4) Uani 0.91(2) 1 d PU . 5 H9A H 0.7488 0.3821 0.2573 0.079 Uiso 0.91(2) 1 calc PR . 5 C10A C 0.7122(18) 0.2038(15) 0.2774(9) 0.063(4) Uani 0.91(2) 1 d PU . 5 H10A H 0.7044 0.1801 0.2277 0.076 Uiso 0.91(2) 1 calc PR . 5 C11A C 0.7515(17) 0.6813(16) 0.1276(14) 0.057(5) Uani 0.80(3) 1 d PU . 3 H11A H 0.7311 0.6156 0.1039 0.068 Uiso 0.80(3) 1 calc PR . 3 C12A C 0.7571(15) 0.6834(15) 0.2133(12) 0.057(5) Uani 0.80(3) 1 d PU . 3 H12A H 0.7446 0.6201 0.2527 0.068 Uiso 0.80(3) 1 calc PR . 3 C13A C 0.7851(18) 0.8008(18) 0.2239(11) 0.058(5) Uani 0.80(3) 1 d PU . 3 H13A H 0.7933 0.8295 0.2721 0.069 Uiso 0.80(3) 1 calc PR . 3 C14A C 0.799(2) 0.8674(14) 0.1479(12) 0.050(5) Uani 0.80(3) 1 d PU . 3 H14A H 0.8163 0.9476 0.1390 0.060 Uiso 0.80(3) 1 calc PR . 3 C15A C 0.7815(18) 0.7933(19) 0.0861(11) 0.065(6) Uani 0.80(3) 1 d PU . 3 H15A H 0.7886 0.8146 0.0316 0.078 Uiso 0.80(3) 1 calc PR . 3 C16A C 0.331(3) 0.999(3) 0.3100(15) 0.045(7) Uani 0.45(3) 1 d PU . 7 H16A H 0.3788 0.9940 0.3562 0.054 Uiso 0.45(3) 1 calc PR . 7 C17A C 0.348(3) 1.073(3) 0.2398(18) 0.052(8) Uani 0.45(3) 1 d PU . 7 H17A H 0.4190 1.1274 0.2291 0.062 Uiso 0.45(3) 1 calc PR . 7 C18A C 0.234(4) 1.054(3) 0.1802(17) 0.061(9) Uani 0.45(3) 1 d PU . 7 H18A H 0.2224 1.0920 0.1295 0.073 Uiso 0.45(3) 1 calc PR . 7 C19A C 0.150(2) 0.960(3) 0.2267(18) 0.033(6) Uani 0.45(3) 1 d PU . 7 H19A H 0.0672 0.9265 0.2139 0.039 Uiso 0.45(3) 1 calc PR . 7 C20A C 0.223(5) 0.934(4) 0.291(3) 0.085(12) Uani 0.45(3) 1 d PU . 7 H20A H 0.1995 0.8674 0.3255 0.102 Uiso 0.45(3) 1 calc PR . 7 C1B C 0.348(4) 0.538(4) 0.244(2) 0.082(13) Uani 0.41(3) 1 d PDU A 2 H1B1 H 0.4357 0.5762 0.2365 0.098 Uiso 0.41(3) 1 calc PR A 2 C2B C 0.240(4) 0.563(2) 0.3039(14) 0.029(6) Uani 0.41(3) 1 d PDU A 2 H2B1 H 0.2379 0.6151 0.3426 0.035 Uiso 0.41(3) 1 calc PR A 2 C3B C 0.134(3) 0.493(2) 0.2922(15) 0.042(9) Uani 0.41(3) 1 d PDU A 2 H3B1 H 0.0411 0.4890 0.3217 0.050 Uiso 0.41(3) 1 calc PR A 2 C4B C 0.186(3) 0.428(2) 0.2307(15) 0.040(8) Uani 0.41(3) 1 d PDU A 2 H4B1 H 0.1343 0.3713 0.2135 0.049 Uiso 0.41(3) 1 calc PR A 2 C5B C 0.323(4) 0.456(3) 0.1972(19) 0.059(10) Uani 0.41(3) 1 d PDU A 2 H5B1 H 0.3834 0.4268 0.1539 0.070 Uiso 0.41(3) 1 calc PR A 2 C6B C 0.753(10) 0.201(6) 0.384(5) 0.01(2) Uiso 0.09(2) 1 d PD . 6 H6B1 H 0.7878 0.1381 0.4201 0.016 Uiso 0.09(2) 1 calc PR . 6 C7B C 0.745(8) 0.314(5) 0.404(4) 0.000(18) Uiso 0.09(2) 1 d PD . 6 H7B1 H 0.7527 0.3498 0.4491 0.000 Uiso 0.09(2) 1 calc PR . 6 C8B C 0.719(8) 0.350(6) 0.328(4) 0.01(2) Uiso 0.09(2) 1 d PD . 6 H8B1 H 0.6784 0.4293 0.3155 0.010 Uiso 0.09(2) 1 calc PR . 6 C9B C 0.749(8) 0.277(7) 0.271(4) 0.00(2) Uiso 0.09(2) 1 d PD . 6 H9B H 0.7840 0.2914 0.2173 0.000 Uiso 0.09(2) 1 calc PR . 6 C10B C 0.71(3) 0.175(13) 0.315(6) 0.12(13) Uiso 0.09(2) 1 d PD . 6 H10B H 0.6759 0.1086 0.3012 0.142 Uiso 0.09(2) 1 calc PR . 6 C11B C 0.788(7) 0.759(5) 0.208(3) 0.041(16) Uiso 0.20(3) 1 d PD . 4 H11B H 0.7921 0.7432 0.2629 0.049 Uiso 0.20(3) 1 calc PR . 4 C12B C 0.759(6) 0.672(4) 0.167(4) 0.026(14) Uiso 0.20(3) 1 d PD . 4 H12B H 0.7369 0.5953 0.1869 0.031 Uiso 0.20(3) 1 calc PR . 4 C13B C 0.769(7) 0.716(5) 0.090(3) 0.06(2) Uiso 0.20(3) 1 d PD . 4 H13B H 0.7708 0.6810 0.0430 0.071 Uiso 0.20(3) 1 calc PR . 4 C14B C 0.776(5) 0.829(4) 0.105(3) 0.017(11) Uiso 0.20(3) 1 d PD . 4 H14B H 0.7537 0.8884 0.0644 0.021 Uiso 0.20(3) 1 calc PR . 4 C15B C 0.811(15) 0.868(7) 0.172(5) 0.14(6) Uiso 0.20(3) 1 d PD . 4 H15B H 0.8382 0.9387 0.1861 0.163 Uiso 0.20(3) 1 calc PR . 4 C16B C 0.252(4) 0.939(3) 0.3172(16) 0.088(12) Uani 0.55(3) 1 d PDU . 8 H16B H 0.2608 0.9041 0.3688 0.106 Uiso 0.55(3) 1 calc PR . 8 C17B C 0.337(4) 1.018(3) 0.2734(18) 0.087(12) Uani 0.55(3) 1 d PDU . 8 H17B H 0.4252 1.0355 0.2910 0.104 Uiso 0.55(3) 1 calc PR . 8 C18B C 0.293(3) 1.070(2) 0.2041(17) 0.073(9) Uani 0.55(3) 1 d PDU . 8 H18B H 0.3298 1.1311 0.1684 0.088 Uiso 0.55(3) 1 calc PR . 8 C19B C 0.176(3) 1.006(2) 0.2035(15) 0.074(10) Uani 0.55(3) 1 d PDU . 8 H19B H 0.1161 1.0164 0.1618 0.088 Uiso 0.55(3) 1 calc PR . 8 C20B C 0.152(3) 0.925(2) 0.2672(16) 0.055(8) Uani 0.55(3) 1 d PDU . 8 H20B H 0.0809 0.8703 0.2748 0.066 Uiso 0.55(3) 1 calc PR . 8 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 0.0415(18) 0.0811(19) 0.0533(16) 0.0079(14) -0.0062(13) 0.0017(14) O1 0.081(8) 0.128(9) 0.051(5) -0.016(5) 0.004(5) -0.023(7) C1 0.095(12) 0.137(13) 0.083(10) -0.036(10) -0.032(9) -0.013(10) K2 0.0459(19) 0.079(2) 0.106(2) -0.0382(19) -0.0147(17) 0.0128(15) O2 0.096(8) 0.059(5) 0.068(6) -0.001(5) -0.009(5) -0.009(5) C2 0.093(12) 0.124(13) 0.046(7) -0.013(9) 0.000(8) -0.015(10) K3 0.0412(18) 0.0764(19) 0.0620(17) 0.0109(15) -0.0077(13) 0.0005(14) O3 0.078(7) 0.083(6) 0.060(5) 0.001(5) -0.015(5) -0.017(5) C3 0.079(11) 0.072(9) 0.084(10) -0.005(8) -0.001(9) 0.007(8) K4 0.0451(18) 0.080(2) 0.105(2) -0.0371(19) -0.0146(16) 0.0120(14) O4 0.082(8) 0.111(8) 0.069(6) -0.014(6) -0.023(6) -0.005(6) C4 0.30(3) 0.077(12) 0.147(19) 0.008(12) -0.030(19) -0.042(15) C5 0.25(3) 0.089(12) 0.105(13) 0.023(10) -0.027(14) -0.035(13) C6 0.062(10) 0.109(11) 0.060(8) -0.005(9) -0.002(7) -0.021(8) C7 0.072(11) 0.131(14) 0.087(11) -0.029(11) 0.011(9) -0.002(9) C8 0.082(12) 0.157(16) 0.086(11) -0.035(11) -0.034(9) 0.022(10) C1A 0.053(10) 0.069(10) 0.066(11) 0.003(8) -0.013(8) -0.008(8) C2A 0.067(11) 0.071(12) 0.081(11) -0.001(8) -0.013(8) 0.004(9) C3A 0.065(10) 0.050(9) 0.040(9) -0.001(7) -0.017(7) -0.011(7) C4A 0.036(8) 0.062(10) 0.036(9) 0.014(7) 0.003(6) -0.004(7) C5A 0.107(13) 0.098(13) 0.108(13) -0.007(9) -0.011(10) -0.001(10) C6A 0.050(7) 0.060(7) 0.082(8) 0.001(7) -0.016(6) 0.001(6) C7A 0.063(8) 0.085(9) 0.068(8) -0.004(7) -0.007(7) 0.014(6) C8A 0.057(7) 0.079(8) 0.085(9) -0.020(7) -0.019(7) 0.002(6) C9A 0.062(7) 0.050(7) 0.077(8) -0.004(7) 0.015(6) 0.008(6) C10A 0.066(8) 0.068(8) 0.055(7) -0.005(6) -0.009(6) -0.005(6) C11A 0.041(7) 0.065(8) 0.062(9) -0.014(7) -0.003(7) 0.007(6) C12A 0.050(7) 0.059(8) 0.058(9) 0.000(7) 0.000(6) -0.003(6) C13A 0.051(8) 0.058(8) 0.065(8) -0.007(7) -0.011(6) -0.004(6) C14A 0.050(8) 0.047(8) 0.054(8) 0.001(6) -0.016(6) -0.005(5) C15A 0.069(9) 0.065(9) 0.063(8) -0.027(7) -0.012(7) 0.005(7) C16A 0.044(10) 0.058(11) 0.032(9) -0.005(8) -0.007(7) 0.000(7) C17A 0.045(11) 0.052(11) 0.056(12) -0.009(9) 0.000(8) 0.005(8) C18A 0.066(12) 0.059(12) 0.057(12) -0.015(8) -0.019(9) 0.008(8) C19A 0.025(8) 0.037(10) 0.038(10) -0.010(8) 0.003(7) -0.009(7) C20A 0.089(15) 0.080(14) 0.084(14) -0.010(9) -0.015(10) 0.003(9) C1B 0.079(16) 0.082(15) 0.081(16) -0.006(10) -0.006(10) 0.001(9) C2B 0.039(10) 0.029(9) 0.023(9) -0.011(7) -0.019(8) 0.001(7) C3B 0.040(11) 0.039(11) 0.040(11) 0.012(8) -0.003(8) -0.001(8) C4B 0.049(12) 0.037(11) 0.039(11) -0.009(8) -0.012(8) -0.009(8) C5B 0.063(13) 0.047(12) 0.058(12) 0.001(8) -0.003(9) 0.020(9) C16B 0.095(15) 0.081(14) 0.090(15) -0.026(9) -0.015(9) 0.008(9) C17B 0.073(13) 0.091(14) 0.093(15) -0.007(10) -0.012(9) 0.002(9) C18B 0.077(12) 0.061(11) 0.078(12) -0.013(9) -0.001(9) 0.005(8) C19B 0.070(13) 0.069(13) 0.076(13) 0.006(9) -0.002(9) -0.004(9) C20B 0.038(10) 0.064(11) 0.067(11) -0.017(8) -0.011(8) -0.007(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 C8B 2.83(7) . ? K1 O1 2.832(8) . ? K1 O2 2.932(9) . ? K1 C1B 2.99(5) . ? K1 C9A 3.002(14) . ? K1 C10B 3.0(3) . ? K1 C10A 3.054(16) . ? K1 C5B 3.07(4) . ? K1 C8A 3.066(15) . ? K1 C2B 3.10(2) . ? K1 C4A 3.10(2) . ? K1 C4B 3.12(3) . ? O1 C2 1.413(14) . ? O1 C1 1.430(14) . ? K2 O3 2.804(8) . ? K2 C17B 2.84(3) . ? K2 C20A 2.91(4) . ? K2 C11B 2.97(6) . ? K2 C12A 2.970(14) . ? K2 C14B 2.96(4) . ? K2 C11A 2.998(15) . ? K2 C12B 2.99(5) . ? K2 C13A 3.004(16) . ? K2 C18B 3.02(3) . ? K2 C14A 3.071(18) . ? K2 C17A 3.06(3) . ? O2 C4 1.418(18) . ? O2 C3 1.406(13) . ? O2 K4 2.824(9) . ? C2 C3 1.503(16) . ? K3 O4 2.815(9) . ? K3 C11B 2.85(6) 1_455 ? K3 O3 2.897(9) . ? K3 C12B 2.97(5) 1_455 ? K3 C2A 2.98(3) . ? K3 C1A 2.97(2) . ? K3 C5A 3.06(4) . ? K3 C12A 3.072(14) 1_455 ? K3 C13B 3.10(6) 1_455 ? K3 C11A 3.095(15) 1_455 ? K3 C15B 3.06(13) 1_455 ? K3 C13A 3.098(18) 1_455 ? O3 C6 1.410(14) . ? O3 C5 1.427(16) . ? K4 C6B 2.66(9) 1_455 ? K4 C9B 2.84(6) 1_455 ? K4 C10B 2.9(3) 1_455 ? K4 C19B 2.92(3) 1_545 ? K4 C9A 2.978(14) 1_455 ? K4 C8A 2.994(16) 1_455 ? K4 C10A 3.017(16) 1_455 ? K4 C19A 3.01(2) 1_545 ? K4 C20B 3.04(2) 1_545 ? K4 C18B 3.03(3) 1_545 ? K4 C20A 3.05(5) 1_545 ? O4 C8 1.407(14) . ? O4 C7 1.440(15) . ? C6 C7 1.471(16) . ? C1A C5A 1.351(10) . ? C1A C2A 1.352(10) . ? C2A C3A 1.359(10) . ? C3A C4A 1.345(10) . ? C4A C5A 1.357(10) . ? C6A C7A 1.377(19) . ? C6A C10A 1.42(3) . ? C6A K4 3.082(15) 1_655 ? C7A C8A 1.44(2) . ? C7A K4 3.102(18) 1_655 ? C8A C9A 1.31(2) . ? C8A K4 2.994(16) 1_655 ? C9A C10A 1.385(18) . ? C9A K4 2.978(14) 1_655 ? C10A K4 3.017(16) 1_655 ? C11A C15A 1.42(2) . ? C11A C12A 1.47(2) . ? C11A K3 3.095(15) 1_655 ? C12A C13A 1.41(2) . ? C12A K3 3.072(14) 1_655 ? C13A C14A 1.42(2) . ? C13A K3 3.098(18) 1_655 ? C14A C15A 1.45(2) . ? C14A K3 3.117(18) 1_655 ? C15A K3 3.119(16) 1_655 ? C16A C20A 1.37(4) . ? C16A C17A 1.38(4) . ? C16A K4 3.10(3) 1_565 ? C17A C18A 1.57(4) . ? C17A K4 3.09(3) 1_565 ? C18A C19A 1.48(4) . ? C18A K4 3.09(3) 1_565 ? C19A C20A 1.32(5) . ? C19A K4 3.01(2) 1_565 ? C20A K4 3.05(5) 1_565 ? C1B C5B 1.350(10) . ? C1B C2B 1.351(10) . ? C2B C3B 1.352(10) . ? C3B C4B 1.351(10) . ? C4B C5B 1.352(10) . ? C6B C7B 1.340(10) . ? C6B C10B 1.342(10) . ? C6B K4 2.66(9) 1_655 ? C7B C8B 1.341(10) . ? C7B K4 3.19(7) 1_655 ? C8B C9B 1.341(10) . ? C8B K4 3.27(7) 1_655 ? C9B C10B 1.342(11) . ? C9B K4 2.84(6) 1_655 ? C10B K4 2.9(3) 1_655 ? C11B C12B 1.341(10) . ? C11B C15B 1.343(11) . ? C11B K3 2.85(6) 1_655 ? C12B C13B 1.340(10) . ? C12B K3 2.97(5) 1_655 ? C13B C14B 1.340(10) . ? C13B K3 3.10(6) 1_655 ? C14B C15B 1.343(11) . ? C14B K3 3.18(4) 1_655 ? C15B K3 3.06(13) 1_655 ? C16B C20B 1.342(10) . ? C16B C17B 1.342(10) . ? C16B K4 3.08(3) 1_565 ? C17B C18B 1.338(10) . ? C17B K4 3.10(3) 1_565 ? C18B C19B 1.345(10) . ? C18B K4 3.03(3) 1_565 ? C19B C20B 1.351(10) . ? C19B K4 2.92(3) 1_565 ? C20B K4 3.04(2) 1_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C8B K1 O1 99.5(12) . . ? C8B K1 O2 150.2(12) . . ? O1 K1 O2 58.7(2) . . ? C8B K1 C1B 87.8(15) . . ? O1 K1 C1B 111.5(7) . . ? O2 K1 C1B 118.0(7) . . ? C8B K1 C9A 13.8(11) . . ? O1 K1 C9A 112.2(4) . . ? O2 K1 C9A 153.9(3) . . ? C1B K1 C9A 88.0(7) . . ? C8B K1 C10B 40(2) . . ? O1 K1 C10B 113.7(16) . . ? O2 K1 C10B 125.7(17) . . ? C1B K1 C10B 114.2(18) . . ? C9A K1 C10B 31.1(17) . . ? C8B K1 C10A 38.8(13) . . ? O1 K1 C10A 124.8(4) . . ? O2 K1 C10A 135.1(4) . . ? C1B K1 C10A 102.3(7) . . ? C9A K1 C10A 26.4(3) . . ? C10B K1 C10A 12.8(15) . . ? C8B K1 C5B 95.8(14) . . ? O1 K1 C5B 133.5(6) . . ? O2 K1 C5B 113.9(6) . . ? C1B K1 C5B 25.7(3) . . ? C9A K1 C5B 90.2(6) . . ? C10B K1 C5B 106.3(16) . . ? C10A K1 C5B 93.5(6) . . ? C8B K1 C8A 15.5(11) . . ? O1 K1 C8A 87.8(4) . . ? O2 K1 C8A 134.7(4) . . ? C1B K1 C8A 101.6(8) . . ? C9A K1 C8A 24.8(4) . . ? C10B K1 C8A 38.5(17) . . ? C10A K1 C8A 42.4(4) . . ? C5B K1 C8A 111.3(7) . . ? C8B K1 C2B 104.8(15) . . ? O1 K1 C2B 89.6(5) . . ? O2 K1 C2B 95.7(7) . . ? C1B K1 C2B 25.6(3) . . ? C9A K1 C2B 109.1(7) . . ? C10B K1 C2B 138.4(18) . . ? C10A K1 C2B 127.3(7) . . ? C5B K1 C2B 43.9(6) . . ? C8A K1 C2B 115.1(7) . . ? C8B K1 C4A 85.5(13) . . ? O1 K1 C4A 122.1(5) . . ? O2 K1 C4A 122.6(4) . . ? C1B K1 C4A 10.6(5) . . ? C9A K1 C4A 83.3(5) . . ? C10B K1 C4A 106.6(17) . . ? C10A K1 C4A 94.2(5) . . ? C5B K1 C4A 17.5(6) . . ? C8A K1 C4A 100.3(5) . . ? C2B K1 C4A 35.2(5) . . ? C8B K1 C4B 121.0(13) . . ? O1 K1 C4B 120.2(5) . . ? O2 K1 C4B 88.7(5) . . ? C1B K1 C4B 39.6(8) . . ? C9A K1 C4B 115.1(6) . . ? C10B K1 C4B 125.8(16) . . ? C10A K1 C4B 113.8(6) . . ? C5B K1 C4B 25.2(3) . . ? C8A K1 C4B 136.4(6) . . ? C2B K1 C4B 41.5(5) . . ? C4A K1 C4B 37.4(6) . . ? C2 O1 C1 111.9(10) . . ? C2 O1 K1 118.9(7) . . ? C1 O1 K1 125.8(8) . . ? O3 K2 C17B 122.6(6) . . ? O3 K2 C20A 109.2(10) . . ? C17B K2 C20A 29.3(11) . . ? O3 K2 C11B 122.0(10) . . ? C17B K2 C11B 111.0(11) . . ? C20A K2 C11B 128.6(14) . . ? O3 K2 C12A 114.2(5) . . ? C17B K2 C12A 122.7(7) . . ? C20A K2 C12A 131.6(10) . . ? C11B K2 C12A 17.8(11) . . ? O3 K2 C14B 94.5(12) . . ? C17B K2 C14B 119.3(12) . . ? C20A K2 C14B 148.3(14) . . ? C11B K2 C14B 36.4(15) . . ? C12A K2 C14B 46.2(9) . . ? O3 K2 C11A 87.7(4) . . ? C17B K2 C11A 145.2(7) . . ? C20A K2 C11A 159.9(10) . . ? C11B K2 C11A 35.0(9) . . ? C12A K2 C11A 28.5(4) . . ? C14B K2 C11A 33.2(8) . . ? O3 K2 C12B 99.1(11) . . ? C17B K2 C12B 136.7(12) . . ? C20A K2 C12B 147.1(15) . . ? C11B K2 C12B 26.0(4) . . ? C12A K2 C12B 15.8(10) . . ? C14B K2 C12B 38.5(11) . . ? C11A K2 C12B 12.9(9) . . ? O3 K2 C13A 130.8(4) . . ? C17B K2 C13A 100.4(8) . . ? C20A K2 C13A 119.8(10) . . ? C11B K2 C13A 10.9(9) . . ? C12A K2 C13A 27.4(4) . . ? C14B K2 C13A 39.6(11) . . ? C11A K2 C13A 45.2(5) . . ? C12B K2 C13A 36.8(8) . . ? O3 K2 C18B 99.2(7) . . ? C17B K2 C18B 26.2(3) . . ? C20A K2 C18B 41.6(9) . . ? C11B K2 C18B 125.1(12) . . ? C12A K2 C18B 141.4(7) . . ? C14B K2 C18B 115.5(10) . . ? C11A K2 C18B 148.6(6) . . ? C12B K2 C18B 149.3(10) . . ? C13A K2 C18B 114.5(7) . . ? O3 K2 C14A 111.6(4) . . ? C17B K2 C14A 104.0(7) . . ? C20A K2 C14A 131.6(10) . . ? C11B K2 C14A 29.0(14) . . ? C12A K2 C14A 44.6(4) . . ? C14B K2 C14A 17.8(10) . . ? C11A K2 C14A 43.8(4) . . ? C12B K2 C14A 43.7(9) . . ? C13A K2 C14A 27.0(4) . . ? C18B K2 C14A 106.2(6) . . ? O3 K2 C17A 114.8(6) . . ? C17B K2 C17A 15.0(6) . . ? C20A K2 C17A 40.8(9) . . ? C11B K2 C17A 111.6(11) . . ? C12A K2 C17A 126.6(7) . . ? C14B K2 C17A 110.3(11) . . ? C11A K2 C17A 141.2(6) . . ? C12B K2 C17A 137.3(10) . . ? C13A K2 C17A 100.8(7) . . ? C18B K2 C17A 15.7(6) . . ? C14A K2 C17A 97.5(6) . . ? C4 O2 C3 117.2(12) . . ? C4 O2 K4 104.0(9) . . ? C3 O2 K4 123.4(7) . . ? C4 O2 K1 121.4(11) . . ? C3 O2 K1 99.8(7) . . ? K4 O2 K1 89.0(2) . . ? O1 C2 C3 109.3(10) . . ? O4 K3 C11B 120.0(10) . 1_455 ? O4 K3 O3 58.7(3) . . ? C11B K3 O3 141.4(13) 1_455 . ? O4 K3 C12B 99.4(12) . 1_455 ? C11B K3 C12B 26.6(4) 1_455 1_455 ? O3 K3 C12B 146.6(12) . 1_455 ? O4 K3 C2A 131.7(5) . . ? C11B K3 C2A 95.0(13) 1_455 . ? O3 K3 C2A 113.5(5) . . ? C12B K3 C2A 99.9(13) 1_455 . ? O4 K3 C1A 110.7(7) . . ? C11B K3 C1A 97.2(14) 1_455 . ? O3 K3 C1A 120.0(5) . . ? C12B K3 C1A 90.2(11) 1_455 . ? C2A K3 C1A 26.3(2) . . ? O4 K3 C5A 91.9(6) . . ? C11B K3 C5A 122.7(14) 1_455 . ? O3 K3 C5A 95.3(6) . . ? C12B K3 C5A 111.4(11) 1_455 . ? C2A K3 C5A 39.8(7) . . ? C1A K3 C5A 25.8(3) . . ? O4 K3 C12A 114.9(4) . 1_455 ? C11B K3 C12A 17.3(11) 1_455 1_455 ? O3 K3 C12A 155.8(3) . 1_455 ? C12B K3 C12A 15.5(10) 1_455 1_455 ? C2A K3 C12A 88.3(6) . 1_455 ? C1A K3 C12A 84.2(6) . 1_455 ? C5A K3 C12A 108.5(6) . 1_455 ? O4 K3 C13B 77.9(10) . 1_455 ? C11B K3 C13B 42.3(12) 1_455 1_455 ? O3 K3 C13B 121.6(12) . 1_455 ? C12B K3 C13B 25.4(4) 1_455 1_455 ? C2A K3 C13B 124.6(13) . 1_455 ? C1A K3 C13B 110.4(13) . 1_455 ? C5A K3 C13B 125.2(12) . 1_455 ? C12A K3 C13B 39.5(10) 1_455 1_455 ? O4 K3 C11A 87.7(5) . 1_455 ? C11B K3 C11A 34.8(9) 1_455 1_455 ? O3 K3 C11A 135.1(5) . 1_455 ? C12B K3 C11A 12.5(10) 1_455 1_455 ? C2A K3 C11A 111.2(7) . 1_455 ? C1A K3 C11A 98.4(6) . 1_455 ? C5A K3 C11A 116.4(6) . 1_455 ? C12A K3 C11A 27.6(4) 1_455 1_455 ? C13B K3 C11A 13.4(10) 1_455 1_455 ? O4 K3 C15B 111.9(13) . 1_455 ? C11B K3 C15B 25.9(10) 1_455 1_455 ? O3 K3 C15B 115.5(15) . 1_455 ? C12B K3 C15B 45.4(15) 1_455 1_455 ? C2A K3 C15B 113.2(15) . 1_455 ? C1A K3 C15B 121.8(16) . 1_455 ? C5A K3 C15B 147.6(16) . 1_455 ? C12A K3 C15B 42.3(14) 1_455 1_455 ? C13B K3 C15B 46.2(11) 1_455 1_455 ? C11A K3 C15B 46.9(13) 1_455 1_455 ? O4 K3 C13A 125.8(4) . 1_455 ? C11B K3 C13A 9.8(10) 1_455 1_455 ? O3 K3 C13A 134.8(4) . 1_455 ? C12B K3 C13A 36.3(9) 1_455 1_455 ? C2A K3 C13A 94.3(5) . 1_455 ? C1A K3 C13A 100.9(7) . 1_455 ? C5A K3 C13A 126.7(7) . 1_455 ? C12A K3 C13A 26.5(4) 1_455 1_455 ? C13B K3 C13A 49.6(9) 1_455 1_455 ? C11A K3 C13A 43.8(5) 1_455 1_455 ? C15B K3 C13A 20.9(15) 1_455 1_455 ? C6 O3 C5 112.4(11) . . ? C6 O3 K2 123.9(7) . . ? C5 O3 K2 105.1(8) . . ? C6 O3 K3 101.1(6) . . ? C5 O3 K3 124.0(10) . . ? K2 O3 K3 90.1(2) . . ? O2 C3 C2 112.4(11) . . ? C6B K4 C9B 43(2) 1_455 1_455 ? C6B K4 O2 92.5(17) 1_455 . ? C9B K4 O2 123.8(12) 1_455 . ? C6B K4 C10B 28(2) 1_455 1_455 ? C9B K4 C10B 27.1(14) 1_455 1_455 ? O2 K4 C10B 120(3) . 1_455 ? C6B K4 C19B 129.9(15) 1_455 1_545 ? C9B K4 C19B 109.9(13) 1_455 1_545 ? O2 K4 C19B 126.2(6) . 1_545 ? C10B K4 C19B 106(3) 1_455 1_545 ? C6B K4 C9A 38.6(19) 1_455 1_455 ? C9B K4 C9A 12.1(11) 1_455 1_455 ? O2 K4 C9A 112.0(4) . 1_455 ? C10B K4 C9A 32(3) 1_455 1_455 ? C19B K4 C9A 121.8(6) 1_545 1_455 ? C6B K4 C8A 25.4(15) 1_455 1_455 ? C9B K4 C8A 36.0(12) 1_455 1_455 ? O2 K4 C8A 88.4(4) . 1_455 ? C10B K4 C8A 40(3) 1_455 1_455 ? C19B K4 C8A 144.3(6) 1_545 1_455 ? C9A K4 C8A 25.3(4) 1_455 1_455 ? C6B K4 C10A 38.3(18) 1_455 1_455 ? C9B K4 C10A 17.7(16) 1_455 1_455 ? O2 K4 C10A 129.5(4) . 1_455 ? C10B K4 C10A 12.9(16) 1_455 1_455 ? C19B K4 C10A 101.2(6) 1_545 1_455 ? C9A K4 C10A 26.7(4) 1_455 1_455 ? C8A K4 C10A 43.2(4) 1_455 1_455 ? C6B K4 C19A 121.1(14) 1_455 1_545 ? C9B K4 C19A 110.6(14) 1_455 1_545 ? O2 K4 C19A 123.6(6) . 1_545 ? C10B K4 C19A 101(3) 1_455 1_545 ? C19B K4 C19A 12.8(5) 1_545 1_545 ? C9A K4 C19A 122.6(6) 1_455 1_545 ? C8A K4 C19A 140.7(5) 1_455 1_545 ? C10A K4 C19A 98.6(5) 1_455 1_545 ? C6B K4 C20B 116.5(14) 1_455 1_545 ? C9B K4 C20B 117.5(16) 1_455 1_545 ? O2 K4 C20B 112.6(5) . 1_545 ? C10B K4 C20B 102(3) 1_455 1_545 ? C19B K4 C20B 26.1(2) 1_545 1_545 ? C9A K4 C20B 129.0(6) 1_455 1_545 ? C8A K4 C20B 140.2(5) 1_455 1_545 ? C10A K4 C20B 102.8(5) 1_455 1_545 ? C19A K4 C20B 14.3(5) 1_545 1_545 ? C6B K4 C18B 155.7(16) 1_455 1_545 ? C9B K4 C18B 124.7(13) 1_455 1_545 ? O2 K4 C18B 108.4(7) . 1_545 ? C10B K4 C18B 130(3) 1_455 1_545 ? C19B K4 C18B 26.0(3) 1_545 1_545 ? C9A K4 C18B 134.3(7) 1_455 1_545 ? C8A K4 C18B 159.2(7) 1_455 1_545 ? C10A K4 C18B 122.0(7) 1_455 1_545 ? C19A K4 C18B 36.1(6) 1_545 1_545 ? C20B K4 C18B 44.3(6) 1_545 1_545 ? C6B K4 C20A 125.8(16) 1_455 1_545 ? C9B K4 C20A 132.9(17) 1_455 1_545 ? O2 K4 C20A 98.6(9) . 1_545 ? C10B K4 C20A 116(3) 1_455 1_545 ? C19B K4 C20A 32.7(10) 1_545 1_545 ? C9A K4 C20A 144.3(9) 1_455 1_545 ? C8A K4 C20A 151.1(8) 1_455 1_545 ? C10A K4 C20A 117.8(9) 1_455 1_545 ? C19A K4 C20A 25.2(9) 1_545 1_545 ? C20B K4 C20A 15.4(8) 1_545 1_545 ? C18B K4 C20A 40.6(8) 1_545 1_545 ? C8 O4 C7 113.7(11) . . ? C8 O4 K3 124.9(9) . . ? C7 O4 K3 119.5(7) . . ? O3 C6 C7 114.7(12) . . ? O4 C7 C6 108.3(11) . . ? C5A C1A C2A 99(2) . . ? C5A C1A K3 80.5(19) . . ? C2A C1A K3 77.0(15) . . ? C5A C1A K1 71.1(19) . . ? C2A C1A K1 76.2(15) . . ? K3 C1A K1 136.9(7) . . ? C5A C1A K4 107(2) . . ? C2A C1A K4 130(2) . . ? K3 C1A K4 148.2(8) . . ? K1 C1A K4 73.0(5) . . ? C1A C2A C3A 117(2) . . ? C1A C2A K3 76.7(15) . . ? C3A C2A K3 87.6(15) . . ? C1A C2A K1 80.0(15) . . ? C3A C2A K1 73.5(14) . . ? K3 C2A K1 138.9(8) . . ? C4A C3A C2A 102.4(19) . . ? C4A C3A K1 75.6(12) . . ? C2A C3A K1 82.1(15) . . ? C4A C3A K3 76.7(12) . . ? C2A C3A K3 67.5(14) . . ? K1 C3A K3 132.7(6) . . ? C4A C3A K2 89.6(15) . . ? C2A C3A K2 136.1(18) . . ? K1 C3A K2 141.6(9) . . ? K3 C3A K2 74.8(5) . . ? C3A C4A C5A 107.9(19) . . ? C3A C4A K1 79.5(12) . . ? C5A C4A K1 78.8(18) . . ? C3A C4A K3 79.1(12) . . ? C5A C4A K3 71.9(18) . . ? K1 C4A K3 136.0(6) . . ? C1A C5A C4A 114(2) . . ? C1A C5A K3 73.6(18) . . ? C4A C5A K3 83.1(18) . . ? C1A C5A K1 85(2) . . ? C4A C5A K1 76.1(17) . . ? K3 C5A K1 140.9(9) . . ? C7A C6A C10A 109.4(14) . . ? C7A C6A K4 78.0(9) . 1_655 ? C10A C6A K4 74.0(8) . 1_655 ? C7A C6A K1 77.9(9) . . ? C10A C6A K1 74.5(8) . . ? K4 C6A K1 130.6(5) 1_655 . ? C6A C7A C8A 104.7(16) . . ? C6A C7A K4 76.3(10) . 1_655 ? C8A C7A K4 72.2(11) . 1_655 ? C6A C7A K1 76.6(9) . . ? C8A C7A K1 74.3(8) . . ? K4 C7A K1 129.2(6) 1_655 . ? C9A C8A C7A 109.9(16) . . ? C9A C8A K4 76.7(9) . 1_655 ? C7A C8A K4 80.6(10) . 1_655 ? C9A C8A K1 74.8(9) . . ? C7A C8A K1 78.9(9) . . ? K4 C8A K1 136.4(6) 1_655 . ? C8A C9A C10A 110.5(15) . . ? C8A C9A K4 78.0(10) . 1_655 ? C10A C9A K4 78.2(9) . 1_655 ? C8A C9A K1 80.3(9) . . ? C10A C9A K1 78.9(9) . . ? K4 C9A K1 140.4(5) 1_655 . ? C9A C10A C6A 105.5(13) . . ? C9A C10A K4 75.1(9) . 1_655 ? C6A C10A K4 79.1(8) . 1_655 ? C9A C10A K1 74.7(9) . . ? C6A C10A K1 78.9(8) . . ? K4 C10A K1 135.9(5) 1_655 . ? C15A C11A C12A 110.5(15) . . ? C15A C11A K2 81.9(9) . . ? C12A C11A K2 74.7(8) . . ? C15A C11A K3 77.8(9) . 1_655 ? C12A C11A K3 75.3(8) . 1_655 ? K2 C11A K3 134.7(6) . 1_655 ? C13A C12A C11A 106.3(14) . . ? C13A C12A K2 77.7(9) . . ? C11A C12A K2 76.8(8) . . ? C13A C12A K3 77.8(9) . 1_655 ? C11A C12A K3 77.1(8) . 1_655 ? K2 C12A K3 137.1(6) . 1_655 ? C12A C13A C14A 107.9(16) . . ? C12A C13A K2 75.0(9) . . ? C14A C13A K2 79.1(10) . . ? C12A C13A K3 75.7(9) . 1_655 ? C14A C13A K3 77.5(10) . 1_655 ? K2 C13A K3 134.3(7) . 1_655 ? C13A C14A C15A 110.8(15) . . ? C13A C14A K2 73.9(9) . . ? C15A C14A K2 78.7(10) . . ? C13A C14A K3 76.1(10) . 1_655 ? C15A C14A K3 76.6(9) . 1_655 ? K2 C14A K3 130.7(5) . 1_655 ? C11A C15A C14A 104.4(16) . . ? C11A C15A K3 75.9(9) . 1_655 ? C14A C15A K3 76.5(10) . 1_655 ? C11A C15A K2 71.5(10) . . ? C14A C15A K2 74.2(10) . . ? K3 C15A K2 128.3(6) 1_655 . ? C20A C16A C17A 99(3) . . ? C20A C16A K4 75(2) . 1_565 ? C17A C16A K4 76.7(15) . 1_565 ? C20A C16A K2 69(2) . . ? C17A C16A K2 75.3(14) . . ? K4 C16A K2 129.7(8) 1_565 . ? C16A C17A C18A 113(2) . . ? C16A C17A K2 78.8(14) . . ? C18A C17A K2 76.2(14) . . ? C16A C17A K4 77.5(15) . 1_565 ? C18A C17A K4 75.2(14) . 1_565 ? K2 C17A K4 131.7(10) . 1_565 ? C19A C18A C17A 101(2) . . ? C19A C18A K4 73.1(14) . 1_565 ? C17A C18A K4 75.5(14) . 1_565 ? C19A C18A K2 75.7(15) . . ? C17A C18A K2 74.3(14) . . ? K4 C18A K2 130.8(10) 1_565 . ? C20A C19A C18A 103(3) . . ? C20A C19A K4 79(2) . 1_565 ? C18A C19A K4 78.9(15) . 1_565 ? C20A C19A K2 70(2) . . ? C18A C19A K2 76.5(14) . . ? K4 C19A K2 134.5(7) 1_565 . ? C19A C20A C16A 125(3) . . ? C19A C20A K2 85(2) . . ? C16A C20A K2 85(2) . . ? C19A C20A K4 76(2) . 1_565 ? C16A C20A K4 79(2) . 1_565 ? K2 C20A K4 141.1(14) . 1_565 ? C5B C1B C2B 117(3) . . ? C5B C1B K1 80(2) . . ? C2B C1B K1 82(2) . . ? C5B C1B K3 79(2) . . ? C2B C1B K3 79(2) . . ? K1 C1B K3 141.7(12) . . ? C1B C2B C3B 102(2) . . ? C1B C2B K1 73(2) . . ? C3B C2B K1 81.0(15) . . ? C1B C2B K3 77(2) . . ? C3B C2B K3 73.9(14) . . ? K1 C2B K3 134.9(6) . . ? C4B C3B C2B 109(2) . . ? C4B C3B K3 78.4(16) . . ? C2B C3B K3 81.6(14) . . ? C4B C3B K1 75.1(17) . . ? C2B C3B K1 74.2(15) . . ? K3 C3B K1 135.3(7) . . ? C3B C4B C5B 112(2) . . ? C3B C4B K1 80.1(17) . . ? C5B C4B K1 75.2(19) . . ? C3B C4B K3 76.8(16) . . ? C5B C4B K3 80.8(19) . . ? K1 C4B K3 137.2(8) . . ? C3B C4B K4 94.3(18) . . ? C5B C4B K4 136(2) . . ? K1 C4B K4 75.9(6) . . ? K3 C4B K4 140.9(10) . . ? C1B C5B C4B 100(3) . . ? C1B C5B K1 74(2) . . ? C4B C5B K1 79.5(19) . . ? C1B C5B K3 77(2) . . ? C4B C5B K3 74.7(18) . . ? K1 C5B K3 136.2(9) . . ? C7B C6B C10B 123(10) . . ? C7B C6B K4 101(5) . 1_655 ? C10B C6B K4 85(10) . 1_655 ? C7B C6B K1 76(4) . . ? C10B C6B K1 68(10) . . ? K4 C6B K1 143(3) 1_655 . ? C8B C7B C6B 87(6) . . ? C8B C7B K4 81(4) . 1_655 ? C6B C7B K4 55(5) . 1_655 ? C8B C7B K1 61(4) . . ? C6B C7B K1 80(5) . . ? K4 C7B K1 122.9(18) 1_655 . ? C7B C8B C9B 122(6) . . ? C7B C8B K1 94(5) . . ? C9B C8B K1 94(5) . . ? C7B C8B K4 75(4) . 1_655 ? C9B C8B K4 60(4) . 1_655 ? K1 C8B K4 135(2) . 1_655 ? C10B C9B C8B 98(9) . . ? C10B C9B K4 78(10) . 1_655 ? C8B C9B K4 96(5) . 1_655 ? C10B C9B K1 70(10) . . ? C8B C9B K1 62(4) . . ? K4 C9B K1 137(2) 1_655 . ? C9B C10B C6B 98(7) . . ? C9B C10B K4 75(10) . 1_655 ? C6B C10B K4 67(10) . 1_655 ? C9B C10B K1 85(10) . . ? C6B C10B K1 88(10) . . ? K4 C10B K1 145(4) 1_655 . ? C12B C11B C15B 120(5) . . ? C12B C11B K3 82(3) . 1_655 ? C15B C11B K3 86(7) . 1_655 ? C12B C11B K2 78(3) . . ? C15B C11B K2 86(6) . . ? K3 C11B K2 150(2) 1_655 . ? C13B C12B C11B 107(4) . . ? C13B C12B K3 83(3) . 1_655 ? C11B C12B K3 72(3) . 1_655 ? C13B C12B K2 86(4) . . ? C11B C12B K2 76(3) . . ? K3 C12B K2 141.7(15) 1_655 . ? C12B C13B C14B 94(4) . . ? C12B C13B K3 71(3) . 1_655 ? C14B C13B K3 81(3) . 1_655 ? C12B C13B K2 69(3) . . ? C14B C13B K2 68(3) . . ? K3 C13B K2 126.4(15) 1_655 . ? C13B C14B C15B 129(5) . . ? C13B C14B K2 88(3) . . ? C15B C14B K2 87(6) . . ? C13B C14B K3 75(3) . 1_655 ? C15B C14B K3 73(6) . 1_655 ? K2 C14B K3 132.7(15) . 1_655 ? C11B C15B C14B 87(4) . . ? C11B C15B K3 68(6) . 1_655 ? C14B C15B K3 83(6) . 1_655 ? C11B C15B K2 69(6) . . ? C14B C15B K2 68(5) . . ? K3 C15B K2 128.6(18) 1_655 . ? C20B C16B C17B 102(3) . . ? C20B C16B K4 75.9(16) . 1_565 ? C17B C16B K4 78(2) . 1_565 ? C20B C16B K2 79.5(17) . . ? C17B C16B K2 67(2) . . ? K4 C16B K2 131.5(9) 1_565 . ? C18B C17B C16B 119(3) . . ? C18B C17B K2 84.5(19) . . ? C16B C17B K2 87(2) . . ? C18B C17B K4 74.5(18) . 1_565 ? C16B C17B K4 77(2) . 1_565 ? K2 C17B K4 142.3(12) . 1_565 ? C17B C18B C19B 96(3) . . ? C17B C18B K2 69.4(19) . . ? C19B C18B K2 80.3(16) . . ? C17B C18B K4 80.3(19) . 1_565 ? C19B C18B K4 72.6(16) . 1_565 ? K2 C18B K4 136.6(8) . 1_565 ? C18B C19B C20B 116(2) . . ? C18B C19B K4 81.4(17) . 1_565 ? C20B C19B K4 81.9(15) . 1_565 ? C18B C19B K2 74.3(16) . . ? C20B C19B K2 79.1(16) . . ? K4 C19B K2 138.1(9) 1_565 . ? C16B C20B C19B 106(2) . . ? C16B C20B K4 78.8(17) . 1_565 ? C19B C20B K4 72.0(15) . 1_565 ? C16B C20B K2 75.6(17) . . ? C19B C20B K2 75.9(15) . . ? K4 C20B K2 131.0(8) 1_565 . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.530 _refine_diff_density_min -0.352 _refine_diff_density_rms 0.099 #===END data_COMPOUND_5#d:\junkie\xtals\bonocx\marcus\nacp15\pj275 _database_code_CSD 172088 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H25 Na O5' _chemical_formula_weight 308.34 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 15.2065(16) _cell_length_b 14.8447(16) _cell_length_c 15.5194(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3503.3(7) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.169 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.107 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9586 _exptl_absorpt_correction_T_max 0.9687 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15138 _diffrn_reflns_av_R_equivalents 0.0760 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.32 _diffrn_reflns_theta_max 23.27 _reflns_number_total 2517 _reflns_number_gt 1397 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1166P)^2^+1.1738P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0011(12) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2517 _refine_ls_number_parameters 327 _refine_ls_number_restraints 180 _refine_ls_R_factor_all 0.1132 _refine_ls_R_factor_gt 0.0699 _refine_ls_wR_factor_ref 0.2333 _refine_ls_wR_factor_gt 0.1930 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.118 _refine_ls_shift/su_max 0.113 _refine_ls_shift/su_mean 0.016 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.18029(9) 0.36972(10) 0.41467(9) 0.0726(6) Uani 1 1 d . A . O1A O 0.1821(7) 0.2899(11) 0.5576(9) 0.136(4) Uani 0.517(6) 1 d PU A 2 C1 C 0.3627(3) 0.3225(4) 0.4051(3) 0.0913(13) Uani 1 1 d . . . H1 H 0.3845 0.2866 0.4493 0.110 Uiso 1 1 calc R A . O4A O 0.0984(10) 0.5040(9) 0.3708(9) 0.144(4) Uani 0.517(6) 1 d PU A 2 C5 C 0.3682(3) 0.4159(4) 0.4000(3) 0.0907(13) Uani 1 1 d . A . H5 H 0.3947 0.4536 0.4402 0.109 Uiso 1 1 calc R . . O2A O 0.0642(5) 0.2541(6) 0.4282(7) 0.129(3) Uani 0.517(6) 1 d PU A 2 C2 C 0.3188(3) 0.2927(3) 0.3322(3) 0.0919(13) Uani 1 1 d . A . H2 H 0.3061 0.2331 0.3185 0.110 Uiso 1 1 calc R . . C4 C 0.3279(3) 0.4425(4) 0.3254(3) 0.0945(14) Uani 1 1 d . . . H4 H 0.3219 0.5015 0.3062 0.113 Uiso 1 1 calc R A . C3 C 0.2974(3) 0.3667(4) 0.2837(3) 0.0962(14) Uani 1 1 d . A . H3 H 0.2675 0.3659 0.2315 0.115 Uiso 1 1 calc R . . O1B O 0.1630(9) 0.2425(9) 0.5182(9) 0.130(4) Uani 0.483(6) 1 d PU A 1 C8B C 0.1793(16) 0.5420(16) 0.5455(14) 0.137(6) Uani 0.483(6) 1 d PU A 1 H8B1 H 0.1663 0.5735 0.5987 0.164 Uiso 0.483(6) 1 calc PR A 1 H8B2 H 0.2411 0.5524 0.5336 0.164 Uiso 0.483(6) 1 calc PR A 1 O5B O 0.1676(11) 0.4147(14) 0.5704(10) 0.150(5) Uani 0.483(6) 1 d PU A 1 C4A C 0.0098(14) 0.2897(16) 0.3081(12) 0.116(6) Uani 0.517(6) 1 d PU A 2 H4A1 H -0.0143 0.2650 0.2553 0.140 Uiso 0.517(6) 1 calc PR A 2 H4A2 H -0.0365 0.3226 0.3374 0.140 Uiso 0.517(6) 1 calc PR A 2 O3B O 0.0457(5) 0.4226(6) 0.3454(5) 0.109(3) Uani 0.483(6) 1 d PU A 1 C10A C 0.2013(13) 0.3582(12) 0.6183(11) 0.120(5) Uani 0.517(6) 1 d PU A 2 H10A H 0.2556 0.3411 0.6467 0.144 Uiso 0.517(6) 1 calc PR A 2 H10B H 0.1554 0.3560 0.6618 0.144 Uiso 0.517(6) 1 calc PR A 2 C3B C 0.0117(11) 0.2510(13) 0.3321(12) 0.094(4) Uani 0.483(6) 1 d PU A 1 H3B1 H -0.0248 0.2490 0.3833 0.113 Uiso 0.483(6) 1 calc PR A 1 H3B2 H -0.0051 0.2031 0.2929 0.113 Uiso 0.483(6) 1 calc PR A 1 C6A C 0.0465(10) 0.5161(12) 0.3207(11) 0.114(5) Uani 0.517(6) 1 d PU A 2 H6A1 H 0.0597 0.5669 0.2835 0.137 Uiso 0.517(6) 1 calc PR A 2 H6A2 H -0.0120 0.5221 0.3449 0.137 Uiso 0.517(6) 1 calc PR A 2 O3A O 0.0746(9) 0.3438(11) 0.2903(7) 0.152(4) Uani 0.517(6) 1 d PU A 2 C1B C 0.1103(10) 0.2023(11) 0.5444(15) 0.105(4) Uani 0.483(6) 1 d PU A 1 H1B1 H 0.0658 0.2366 0.5748 0.125 Uiso 0.483(6) 1 calc PR A 1 H1B2 H 0.1297 0.1508 0.5779 0.125 Uiso 0.483(6) 1 calc PR A 1 O5A O 0.1566(8) 0.4632(11) 0.5444(9) 0.126(4) Uani 0.517(6) 1 d PU A 2 O4B O 0.1423(6) 0.5362(7) 0.4255(9) 0.107(3) Uani 0.483(6) 1 d PU A 1 C6B C 0.0725(11) 0.5650(12) 0.3776(15) 0.116(5) Uani 0.483(6) 1 d PU A 1 H6B1 H 0.0816 0.6267 0.3590 0.139 Uiso 0.483(6) 1 calc PR A 1 H6B2 H 0.0189 0.5624 0.4113 0.139 Uiso 0.483(6) 1 calc PR A 1 C5A C 0.0645(15) 0.4075(15) 0.2684(13) 0.157(6) Uani 0.517(6) 1 d PU A 2 H5A1 H 0.0143 0.4014 0.2302 0.188 Uiso 0.517(6) 1 calc PR A 2 H5A2 H 0.1144 0.4184 0.2309 0.188 Uiso 0.517(6) 1 calc PR A 2 O2B O 0.0898(8) 0.2499(9) 0.3489(10) 0.159(4) Uani 0.483(6) 1 d PU A 1 C7B C 0.1433(11) 0.5762(8) 0.4957(14) 0.101(4) Uani 0.483(6) 1 d PU A 1 H7B1 H 0.1688 0.6354 0.4873 0.121 Uiso 0.483(6) 1 calc PR A 1 H7B2 H 0.0831 0.5845 0.5149 0.121 Uiso 0.483(6) 1 calc PR A 1 C10B C 0.1798(12) 0.3075(15) 0.6228(10) 0.113(4) Uani 0.483(6) 1 d PU A 1 H10C H 0.1232 0.3139 0.6511 0.135 Uiso 0.483(6) 1 calc PR A 1 H10D H 0.2172 0.2722 0.6604 0.135 Uiso 0.483(6) 1 calc PR A 1 C4B C 0.0103(8) 0.3526(10) 0.2845(8) 0.088(3) Uani 0.483(6) 1 d PU A 1 H4B1 H 0.0459 0.3511 0.2327 0.105 Uiso 0.483(6) 1 calc PR A 1 H4B2 H -0.0495 0.3679 0.2682 0.105 Uiso 0.483(6) 1 calc PR A 1 C9B C 0.2255(10) 0.4127(16) 0.6111(10) 0.121(5) Uani 0.483(6) 1 d PU A 1 H9B1 H 0.2238 0.4509 0.6618 0.145 Uiso 0.483(6) 1 calc PR A 1 H9B2 H 0.2816 0.4149 0.5814 0.145 Uiso 0.483(6) 1 calc PR A 1 C7A C 0.0894(15) 0.5713(9) 0.4380(12) 0.120(4) Uani 0.517(6) 1 d PU A 2 H7A1 H 0.0320 0.5708 0.4654 0.145 Uiso 0.517(6) 1 calc PR A 2 H7A2 H 0.1043 0.6316 0.4189 0.145 Uiso 0.517(6) 1 calc PR A 2 C2A C 0.1023(11) 0.1817(11) 0.4867(14) 0.115(4) Uani 0.517(6) 1 d PU A 2 H2A1 H 0.1524 0.1528 0.4596 0.138 Uiso 0.517(6) 1 calc PR A 2 H2A2 H 0.0584 0.1362 0.4996 0.138 Uiso 0.517(6) 1 calc PR A 2 C8A C 0.1641(18) 0.526(2) 0.495(2) 0.189(10) Uani 0.517(6) 1 d PU A 2 H8A1 H 0.2095 0.5076 0.4547 0.226 Uiso 0.517(6) 1 calc PR A 2 H8A2 H 0.1891 0.5743 0.5289 0.226 Uiso 0.517(6) 1 calc PR A 2 C9A C 0.2141(11) 0.4879(17) 0.5832(11) 0.135(5) Uani 0.517(6) 1 d PU A 2 H9A1 H 0.2007 0.5321 0.6273 0.162 Uiso 0.517(6) 1 calc PR A 2 H9A2 H 0.2666 0.5025 0.5506 0.162 Uiso 0.517(6) 1 calc PR A 2 C1A C 0.1386(13) 0.2455(14) 0.5928(12) 0.123(4) Uani 0.517(6) 1 d PU A 2 H1A1 H 0.0905 0.2770 0.6209 0.148 Uiso 0.517(6) 1 calc PR A 2 H1A2 H 0.1691 0.2071 0.6336 0.148 Uiso 0.517(6) 1 calc PR A 2 C3A C 0.047(2) 0.205(2) 0.372(2) 0.218(11) Uani 0.517(6) 1 d PU A 2 H3A1 H 0.0015 0.1618 0.3874 0.262 Uiso 0.517(6) 1 calc PR A 2 H3A2 H 0.0979 0.1742 0.3487 0.262 Uiso 0.517(6) 1 calc PR A 2 C2B C 0.0831(12) 0.1768(10) 0.4339(14) 0.139(5) Uani 0.517(6) 1 d PU A 1 H2B1 H 0.1192 0.1254 0.4183 0.167 Uiso 0.517(6) 1 calc PR A 1 H2B2 H 0.0229 0.1554 0.4347 0.167 Uiso 0.517(6) 1 calc PR A 1 C5B C 0.0642(12) 0.4843(15) 0.2771(14) 0.153(6) Uani 0.517(6) 1 d PU A 1 H5B1 H 0.0156 0.4964 0.2383 0.184 Uiso 0.517(6) 1 calc PR A 1 H5B2 H 0.1190 0.4738 0.2467 0.184 Uiso 0.517(6) 1 calc PR A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0669(9) 0.0816(11) 0.0694(10) -0.0006(7) 0.0037(7) 0.0058(7) O1A 0.116(6) 0.175(9) 0.118(7) 0.025(7) 0.015(6) 0.009(6) C1 0.073(3) 0.100(4) 0.101(4) 0.007(3) 0.003(2) 0.013(3) O4A 0.147(7) 0.147(8) 0.139(7) -0.001(6) 0.028(6) 0.053(7) C5 0.075(3) 0.100(4) 0.097(3) -0.004(3) 0.007(2) 0.001(3) O2A 0.114(5) 0.103(5) 0.170(7) -0.031(5) 0.024(5) -0.009(4) C2 0.071(3) 0.095(3) 0.109(4) -0.007(3) 0.015(3) 0.004(2) C4 0.078(3) 0.103(3) 0.103(4) 0.025(3) 0.021(3) 0.008(3) C3 0.072(3) 0.138(4) 0.079(3) 0.010(3) 0.007(2) -0.004(3) O1B 0.128(7) 0.114(7) 0.148(8) 0.041(6) 0.037(7) 0.012(6) C8B 0.158(10) 0.127(10) 0.125(9) -0.032(9) 0.003(8) -0.025(9) O5B 0.150(8) 0.179(10) 0.121(8) -0.016(8) 0.018(6) 0.026(8) C4A 0.113(9) 0.121(11) 0.115(9) -0.009(8) -0.012(7) 0.000(9) O3B 0.105(5) 0.112(6) 0.110(5) 0.011(5) 0.000(4) 0.015(4) C10A 0.145(9) 0.100(8) 0.115(9) 0.022(8) -0.016(7) -0.017(8) C3B 0.089(7) 0.094(9) 0.098(8) -0.018(7) -0.007(6) -0.025(7) C6A 0.120(8) 0.125(9) 0.096(7) 0.022(7) 0.020(7) 0.053(7) O3A 0.135(7) 0.200(9) 0.121(6) -0.025(7) -0.015(5) 0.024(7) C1B 0.101(7) 0.099(8) 0.113(9) 0.034(7) 0.012(8) -0.001(6) O5A 0.124(6) 0.127(8) 0.127(7) -0.022(6) 0.018(5) -0.019(6) O4B 0.077(5) 0.094(5) 0.151(8) -0.008(6) 0.027(5) 0.011(4) C6B 0.114(8) 0.088(8) 0.145(10) 0.015(8) 0.010(8) 0.003(7) C5A 0.165(10) 0.150(10) 0.156(11) -0.033(9) 0.034(8) -0.003(10) O2B 0.134(7) 0.157(8) 0.185(9) -0.025(7) 0.006(7) 0.000(6) C7B 0.100(7) 0.064(6) 0.138(9) -0.013(7) 0.020(7) -0.001(6) C10B 0.132(9) 0.140(10) 0.067(6) 0.020(8) 0.010(6) -0.004(8) C4B 0.063(5) 0.115(8) 0.086(6) -0.011(6) -0.032(5) 0.013(6) C9B 0.120(8) 0.140(10) 0.103(8) -0.023(8) -0.026(7) -0.020(8) C7A 0.144(9) 0.080(7) 0.137(9) 0.003(7) 0.031(8) 0.016(7) C2A 0.122(8) 0.117(8) 0.105(8) -0.001(8) 0.005(8) -0.013(7) C8A 0.187(13) 0.189(14) 0.189(14) -0.002(11) 0.002(11) -0.006(10) C9A 0.131(8) 0.154(10) 0.120(8) -0.031(8) -0.008(7) -0.008(8) C1A 0.132(8) 0.124(9) 0.113(8) 0.043(8) 0.016(8) 0.019(7) C3A 0.220(14) 0.212(15) 0.222(14) -0.005(11) -0.001(11) -0.006(10) C2B 0.171(10) 0.089(7) 0.156(10) 0.023(8) -0.024(8) -0.025(7) C5B 0.157(10) 0.148(10) 0.155(10) 0.050(9) -0.031(8) 0.036(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 Na1 O3B 2.442(7) . ? Na1 O4A 2.447(13) . ? Na1 O2B 2.469(13) . ? Na1 O2A 2.471(8) . ? Na1 O5A 2.472(12) . ? Na1 O1B 2.494(11) . ? Na1 O5B 2.514(14) . ? Na1 O1A 2.515(12) . ? Na1 O3A 2.541(11) . ? Na1 O4B 2.544(10) . ? Na1 C3 2.703(5) . ? Na1 C2 2.717(4) . ? O1A C1A 1.082(19) . ? O1A C10A 1.41(2) . ? C1 C2 1.386(6) . ? C1 C5 1.391(6) . ? O4A C6A 1.122(18) . ? O4A C7A 1.45(2) . ? C5 C4 1.368(6) . ? O2A C3A 1.17(3) . ? O2A C2A 1.52(2) . ? C2 C3 1.371(6) . ? C4 C3 1.378(6) . ? O1B C1B 1.079(15) . ? O1B C10B 1.91(2) . ? C8B C7B 1.07(3) . ? C8B O5B 1.94(3) . ? O5B C9B 1.084(18) . ? C4A O3A 1.30(2) . ? C4A C3A 1.70(4) . ? O3B C5B 1.429(17) . ? O3B C4B 1.505(15) . ? C10A C9A 2.01(3) . ? C3B O2B 1.22(2) . ? C3B C4B 1.68(2) . ? C6A C5A 1.83(2) . ? O3A C5A 1.02(2) . ? C1B C2B 1.81(3) . ? O5A C9A 1.123(17) . ? O5A C8A 1.21(3) . ? O4B C7B 1.24(2) . ? O4B C6B 1.36(2) . ? C6B C5B 1.97(3) . ? O2B C2B 1.71(2) . ? C10B C9B 1.72(3) . ? C7A C8A 1.59(4) . ? C2A C1A 1.98(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 O3B Na1 O4A 35.8(4) . . ? O3B Na1 O2B 65.3(4) . . ? O4A Na1 O2B 100.8(5) . . ? O3B Na1 O2A 70.3(3) . . ? O4A Na1 O2A 103.0(4) . . ? O2B Na1 O2A 30.3(3) . . ? O3B Na1 O5A 93.2(4) . . ? O4A Na1 O5A 72.2(5) . . ? O2B Na1 O5A 131.3(4) . . ? O2A Na1 O5A 102.5(4) . . ? O3B Na1 O1B 116.0(4) . . ? O4A Na1 O1B 138.0(4) . . ? O2B Na1 O1B 70.3(6) . . ? O2A Na1 O1B 49.0(5) . . ? O5A Na1 O1B 83.4(5) . . ? O3B Na1 O5B 105.9(5) . . ? O4A Na1 O5B 90.7(5) . . ? O2B Na1 O5B 123.1(6) . . ? O2A Na1 O5B 92.7(5) . . ? O5A Na1 O5B 19.4(4) . . ? O1B Na1 O5B 64.8(6) . . ? O3B Na1 O1A 123.3(3) . . ? O4A Na1 O1A 129.4(4) . . ? O2B Na1 O1A 91.8(5) . . ? O2A Na1 O1A 66.8(4) . . ? O5A Na1 O1A 63.1(6) . . ? O1B Na1 O1A 22.5(3) . . ? O5B Na1 O1A 43.8(6) . . ? O3B Na1 O3A 35.3(3) . . ? O4A Na1 O3A 65.8(5) . . ? O2B Na1 O3A 39.2(5) . . ? O2A Na1 O3A 60.5(5) . . ? O5A Na1 O3A 127.7(4) . . ? O1B Na1 O3A 108.0(6) . . ? O5B Na1 O3A 136.2(5) . . ? O1A Na1 O3A 127.3(5) . . ? O3B Na1 O4B 61.7(4) . . ? O4A Na1 O4B 27.3(4) . . ? O2B Na1 O4B 126.9(4) . . ? O2A Na1 O4B 120.5(3) . . ? O5A Na1 O4B 50.8(5) . . ? O1B Na1 O4B 132.0(4) . . ? O5B Na1 O4B 70.2(6) . . ? O1A Na1 O4B 113.7(5) . . ? O3A Na1 O4B 93.1(5) . . ? O3B Na1 C3 103.1(2) . . ? O4A Na1 C3 98.0(3) . . ? O2B Na1 C3 92.6(3) . . ? O2A Na1 C3 121.6(3) . . ? O5A Na1 C3 135.9(3) . . ? O1B Na1 C3 122.8(3) . . ? O5B Na1 C3 141.0(4) . . ? O1A Na1 C3 130.4(3) . . ? O3A Na1 C3 81.0(3) . . ? O4B Na1 C3 102.4(3) . . ? O3B Na1 C2 125.3(2) . . ? O4A Na1 C2 127.3(3) . . ? O2B Na1 C2 86.2(3) . . ? O2A Na1 C2 107.6(2) . . ? O5A Na1 C2 137.2(3) . . ? O1B Na1 C2 93.8(3) . . ? O5B Na1 C2 128.6(4) . . ? O1A Na1 C2 102.1(3) . . ? O3A Na1 C2 93.9(3) . . ? O4B Na1 C2 128.0(2) . . ? C3 Na1 C2 29.30(13) . . ? C1A O1A C10A 103(2) . . ? C1A O1A Na1 136.5(17) . . ? C10A O1A Na1 104.6(10) . . ? C2 C1 C5 107.4(4) . . ? C2 C1 Na1 69.8(2) . . ? C5 C1 Na1 79.5(3) . . ? C6A O4A C7A 108.7(16) . . ? C6A O4A Na1 133.0(15) . . ? C7A O4A Na1 114.1(13) . . ? C4 C5 C1 108.0(5) . . ? C4 C5 Na1 72.4(2) . . ? C1 C5 Na1 72.9(2) . . ? C3A O2A C2A 95(2) . . ? C3A O2A Na1 122.3(19) . . ? C2A O2A Na1 105.7(8) . . ? C3 C2 C1 107.9(5) . . ? C3 C2 Na1 74.8(2) . . ? C1 C2 Na1 81.6(3) . . ? C5 C4 C3 108.2(5) . . ? C5 C4 Na1 80.4(3) . . ? C3 C4 Na1 69.8(3) . . ? C2 C3 C4 108.5(4) . . ? C2 C3 Na1 75.9(2) . . ? C4 C3 Na1 81.6(3) . . ? C1B O1B C10B 93.3(16) . . ? C1B O1B Na1 137.7(12) . . ? C10B O1B Na1 98.7(9) . . ? C7B C8B O5B 123.9(17) . . ? C9B O5B C8B 94(2) . . ? C9B O5B Na1 119.4(13) . . ? C8B O5B Na1 93.5(10) . . ? O3A C4A C3A 109.3(19) . . ? C5B O3B C4B 92.7(12) . . ? C5B O3B Na1 111.5(8) . . ? C4B O3B Na1 110.7(6) . . ? O1A C10A C9A 121.7(13) . . ? O2B C3B C4B 96.8(14) . . ? O4A C6A C5A 93.5(14) . . ? C5A O3A C4A 122(2) . . ? C5A O3A Na1 102.1(18) . . ? C4A O3A Na1 114.2(11) . . ? O1B C1B C2B 85.9(18) . . ? C9A O5A C8A 91(2) . . ? C9A O5A Na1 120.4(11) . . ? C8A O5A Na1 84.3(18) . . ? C7B O4B C6B 109.7(16) . . ? C7B O4B Na1 121.3(12) . . ? C6B O4B Na1 116.5(12) . . ? O4B C6B C5B 106.9(15) . . ? O3A C5A C6A 134.1(19) . . ? C3B O2B C2B 96.7(15) . . ? C3B O2B Na1 128.6(12) . . ? C2B O2B Na1 99.9(10) . . ? C8B C7B O4B 114.3(16) . . ? C9B C10B O1B 115.1(11) . . ? O3B C4B C3B 109.9(9) . . ? O5B C9B C10B 76.0(19) . . ? O4A C7A C8A 92.3(17) . . ? O2A C2A C1A 105.3(11) . . ? O5A C8A C7A 128(2) . . ? O5A C9A C10A 76.0(17) . . ? O1A C1A C2A 92.4(17) . . ? O2A C3A C4A 93(2) . . ? O2B C2B C1B 125.8(12) . . ? O3B C5B C6B 79.4(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.27 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.207 _refine_diff_density_min -0.202 _refine_diff_density_rms 0.043 #===END data_COMPOUND_8#d:\junkie\xtals\bonocx\marcus\nacpme18\pj305 _database_code_CSD 172089 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H31 Na O6' _chemical_formula_weight 366.42 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 19.623(3) _cell_length_b 9.8461(17) _cell_length_c 10.8445(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2095.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.162 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 792 _exptl_absorpt_coefficient_mu 0.103 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9699 _exptl_absorpt_correction_T_max 0.9818 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8839 _diffrn_reflns_av_R_equivalents 0.0783 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 23.20 _reflns_number_total 2639 _reflns_number_gt 1755 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1615P)^2^+0.4594P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.1(12) _refine_ls_number_reflns 2639 _refine_ls_number_parameters 227 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1129 _refine_ls_R_factor_gt 0.0862 _refine_ls_wR_factor_ref 0.2734 _refine_ls_wR_factor_gt 0.2428 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.002 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na1 Na 0.10395(13) 0.8471(3) 0.0699(3) 0.0944(9) Uani 1 1 d . . . O1 O 0.1288(5) 1.1052(6) 0.0447(7) 0.148(3) Uani 1 1 d . A 1 C1 C 0.1898(7) 0.9387(11) -0.2498(13) 0.159(4) Uani 1 1 d . . . H1A H 0.2323 0.9811 -0.2285 0.238 Uiso 1 1 calc R A . H1B H 0.1535 1.0035 -0.2419 0.238 Uiso 1 1 calc R . . H1C H 0.1918 0.9067 -0.3333 0.238 Uiso 1 1 calc R . . O2 O 0.1912(3) 0.9658(6) 0.2301(5) 0.1142(19) Uani 1 1 d . A 1 C2 C 0.1770(4) 0.8212(8) -0.1648(8) 0.095(2) Uani 1 1 d . A . O3 O 0.1531(3) 0.7064(7) 0.2948(6) 0.126(2) Uani 1 1 d . A . C3 C 0.1230(3) 0.7324(8) -0.1709(8) 0.0895(19) Uani 1 1 d . A . H3 H 0.0867 0.7396 -0.2257 0.107 Uiso 1 1 calc R . . O4 O 0.0213(5) 0.6183(7) 0.2373(8) 0.144(3) Uani 1 1 d . . . C4 C 0.1302(4) 0.6337(8) -0.0861(8) 0.097(2) Uani 1 1 d . A . H4 H 0.1003 0.5620 -0.0719 0.116 Uiso 1 1 calc R . . O5 O -0.0414(3) 0.7471(10) 0.0378(8) 0.161(3) Uani 1 1 d . A 1 C5 C 0.1906(6) 0.6590(11) -0.0239(7) 0.115(3) Uani 1 1 d . A . H5 H 0.2086 0.6076 0.0403 0.138 Uiso 1 1 calc R . . O6 O 0.0042(5) 1.0092(10) -0.0232(8) 0.168(3) Uani 1 1 d . A 1 C6 C 0.2200(4) 0.7766(10) -0.0755(8) 0.103(2) Uani 1 1 d . A . H6 H 0.2611 0.8163 -0.0526 0.123 Uiso 1 1 calc R . . C7 C 0.1760(9) 1.1687(11) 0.1334(11) 0.148(5) Uani 1 1 d . A 1 H7A H 0.1994 1.2445 0.0951 0.178 Uiso 1 1 calc R A 1 H7B H 0.1510 1.2025 0.2042 0.178 Uiso 1 1 calc R A 1 C8 C 0.2245(7) 1.0670(19) 0.1717(14) 0.196(9) Uani 1 1 d . . . H8A H 0.2483 1.0312 0.1004 0.235 Uiso 1 1 calc R A 1 H8B H 0.2579 1.1071 0.2267 0.235 Uiso 1 1 calc R A 1 C9 C 0.2387(5) 0.8703(16) 0.2862(15) 0.157(5) Uani 1 1 d . A 1 H9A H 0.2632 0.8208 0.2228 0.188 Uiso 1 1 calc R A 1 H9B H 0.2716 0.9185 0.3367 0.188 Uiso 1 1 calc R A 1 C10 C 0.1997(8) 0.7784(18) 0.3606(12) 0.168(5) Uani 1 1 d . . . H10A H 0.2305 0.7155 0.4011 0.202 Uiso 1 1 calc R A 1 H10B H 0.1763 0.8296 0.4242 0.202 Uiso 1 1 calc R A 1 C11 C 0.1174(7) 0.5927(16) 0.3538(13) 0.169(6) Uani 1 1 d . . . H11A H 0.0958 0.6247 0.4289 0.203 Uiso 1 1 calc R A . H11B H 0.1504 0.5237 0.3764 0.203 Uiso 1 1 calc R . . C12 C 0.0644(11) 0.5307(13) 0.2717(14) 0.171(6) Uani 1 1 d . A . H12A H 0.0863 0.4913 0.1999 0.206 Uiso 1 1 calc R . . H12B H 0.0412 0.4585 0.3157 0.206 Uiso 1 1 calc R . . C13 C -0.0303(11) 0.5565(13) 0.1604(13) 0.187(8) Uani 1 1 d . A 1 H13A H -0.0578 0.4942 0.2086 0.225 Uiso 1 1 calc R A 1 H13B H -0.0091 0.5062 0.0937 0.225 Uiso 1 1 calc R A 1 C14 C -0.0751(8) 0.671(2) 0.1082(17) 0.228(11) Uani 1 1 d . . . H14A H -0.1130 0.6323 0.0631 0.273 Uiso 1 1 calc R A 1 H14B H -0.0935 0.7247 0.1757 0.273 Uiso 1 1 calc R A 1 C15 C -0.0844(5) 0.8588(17) -0.0191(16) 0.170(6) Uani 1 1 d . A 1 H15A H -0.1201 0.8192 -0.0696 0.204 Uiso 1 1 calc R A 1 H15B H -0.1058 0.9122 0.0454 0.204 Uiso 1 1 calc R A 1 C16 C -0.0395(9) 0.949(3) -0.0974(14) 0.223(10) Uani 1 1 d . A 1 H16A H -0.0154 0.8946 -0.1581 0.267 Uiso 1 1 calc R A 1 H16B H -0.0669 1.0157 -0.1403 0.267 Uiso 1 1 calc R A 1 C17 C 0.0397(8) 1.1286(19) -0.073(2) 0.242(12) Uani 1 1 d . A 1 H17A H 0.0638 1.1010 -0.1471 0.291 Uiso 1 1 calc R A 1 H17B H 0.0057 1.1949 -0.0974 0.291 Uiso 1 1 calc R A 1 C18 C 0.0868(9) 1.1934(12) 0.0063(16) 0.167(5) Uani 1 1 d . A 1 H18A H 0.1108 1.2646 -0.0379 0.200 Uiso 1 1 calc R A 1 H18B H 0.0631 1.2342 0.0754 0.200 Uiso 1 1 calc R A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Na1 0.0976(16) 0.0912(16) 0.0945(19) -0.0264(15) 0.0069(15) 0.0164(12) O1 0.249(8) 0.072(3) 0.124(5) 0.000(3) 0.048(6) 0.021(5) C1 0.186(10) 0.128(7) 0.161(11) -0.006(7) 0.041(8) -0.001(7) O2 0.089(3) 0.143(4) 0.111(4) -0.040(3) 0.014(3) -0.036(4) C2 0.104(5) 0.092(5) 0.089(5) -0.018(4) 0.009(4) 0.020(4) O3 0.149(5) 0.145(5) 0.082(4) 0.004(4) -0.009(4) 0.045(4) C3 0.072(4) 0.091(4) 0.105(5) -0.019(4) -0.009(4) 0.007(4) O4 0.202(8) 0.084(3) 0.145(6) -0.016(4) 0.049(5) -0.019(5) C4 0.108(5) 0.088(5) 0.094(6) -0.012(4) 0.019(5) 0.009(4) O5 0.079(3) 0.232(7) 0.173(7) -0.078(7) 0.031(4) -0.043(5) C5 0.160(8) 0.125(7) 0.060(4) -0.017(5) -0.003(5) 0.073(6) O6 0.189(7) 0.195(7) 0.120(5) -0.025(5) -0.045(6) 0.092(6) C6 0.093(5) 0.123(6) 0.093(6) -0.036(5) -0.005(4) 0.025(5) C7 0.232(14) 0.100(6) 0.113(7) -0.030(6) 0.077(9) -0.062(8) C8 0.148(9) 0.242(16) 0.197(14) -0.156(13) 0.098(10) -0.129(11) C9 0.060(5) 0.231(13) 0.178(12) -0.082(11) -0.044(6) 0.022(7) C10 0.139(9) 0.237(15) 0.129(10) -0.037(11) -0.044(8) 0.090(11) C11 0.205(12) 0.172(11) 0.132(10) 0.100(10) 0.038(9) 0.065(10) C12 0.270(18) 0.110(8) 0.135(11) 0.012(8) 0.073(12) -0.004(10) C13 0.30(2) 0.129(9) 0.139(10) -0.039(8) 0.057(11) -0.147(12) C14 0.158(11) 0.34(2) 0.188(16) -0.157(18) 0.083(12) -0.160(16) C15 0.071(5) 0.254(14) 0.184(13) -0.079(11) -0.036(7) 0.050(8) C16 0.160(12) 0.39(3) 0.117(9) 0.008(14) -0.025(10) 0.153(16) C17 0.170(11) 0.185(14) 0.37(3) 0.195(19) -0.067(15) 0.000(10) C18 0.203(13) 0.093(7) 0.205(14) 0.020(8) 0.042(11) 0.026(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 Na1 O1 2.602(6) . ? Na1 O2 2.705(6) . ? Na1 C5 2.712(7) . ? Na1 O6 2.721(8) . ? Na1 C4 2.746(7) . ? Na1 C6 2.855(8) . ? Na1 C3 2.870(8) . ? Na1 C2 2.933(8) . ? Na1 O3 2.965(7) . ? O1 C18 1.268(15) . ? O1 C7 1.475(15) . ? C1 C2 1.500(14) . ? O2 C8 1.350(16) . ? O2 C9 1.457(14) . ? C2 C6 1.357(11) . ? C2 C3 1.375(11) . ? O3 C10 1.360(15) . ? O3 C11 1.467(15) . ? C3 C4 1.346(11) . ? O4 C12 1.264(18) . ? O4 C13 1.446(18) . ? C4 C5 1.386(13) . ? O5 C14 1.26(2) . ? O5 C15 1.518(17) . ? C5 C6 1.409(13) . ? O6 C16 1.32(2) . ? O6 C17 1.471(17) . ? C7 C8 1.44(2) . ? C9 C10 1.43(2) . ? C11 C12 1.50(2) . ? C13 C14 1.54(2) . ? C15 C16 1.51(2) . ? C17 C18 1.41(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 O1 Na1 O2 61.8(3) . . ? O1 Na1 C5 120.6(3) . . ? O2 Na1 C5 98.0(3) . . ? O1 Na1 O6 61.5(3) . . ? O2 Na1 O6 116.1(3) . . ? C5 Na1 O6 135.4(3) . . ? O1 Na1 C4 130.3(3) . . ? O2 Na1 C4 127.4(3) . . ? C5 Na1 C4 29.4(3) . . ? O6 Na1 C4 110.8(3) . . ? O1 Na1 C6 91.7(3) . . ? O2 Na1 C6 87.4(2) . . ? C5 Na1 C6 29.2(3) . . ? O6 Na1 C6 120.7(3) . . ? C4 Na1 C6 47.5(2) . . ? O1 Na1 C3 105.3(3) . . ? O2 Na1 C3 132.2(2) . . ? C5 Na1 C3 46.2(2) . . ? O6 Na1 C3 89.2(2) . . ? C4 Na1 C3 27.6(2) . . ? C6 Na1 C3 45.4(2) . . ? O1 Na1 C2 84.4(2) . . ? O2 Na1 C2 106.6(2) . . ? C5 Na1 C2 46.2(3) . . ? O6 Na1 C2 94.6(3) . . ? C4 Na1 C2 46.1(2) . . ? C6 Na1 C2 27.1(2) . . ? C3 Na1 C2 27.4(2) . . ? O1 Na1 O3 118.8(3) . . ? O2 Na1 O3 57.9(2) . . ? C5 Na1 O3 77.7(2) . . ? O6 Na1 O3 144.4(3) . . ? C4 Na1 O3 95.1(2) . . ? C6 Na1 O3 94.7(2) . . ? C3 Na1 O3 121.5(2) . . ? C2 Na1 O3 121.0(2) . . ? C18 O1 C7 109.4(11) . . ? C18 O1 Na1 125.6(9) . . ? C7 O1 Na1 117.6(7) . . ? C8 O2 C9 111.2(11) . . ? C8 O2 Na1 108.9(7) . . ? C9 O2 Na1 113.2(5) . . ? C6 C2 C3 107.9(8) . . ? C6 C2 C1 125.7(9) . . ? C3 C2 C1 126.2(9) . . ? C6 C2 Na1 73.2(5) . . ? C3 C2 Na1 73.7(4) . . ? C1 C2 Na1 123.2(5) . . ? C10 O3 C11 119.3(12) . . ? C10 O3 Na1 114.0(8) . . ? C11 O3 Na1 124.1(7) . . ? C4 C3 C2 110.2(7) . . ? C4 C3 Na1 71.1(4) . . ? C2 C3 Na1 78.9(4) . . ? C12 O4 C13 110.6(12) . . ? C3 C4 C5 107.0(8) . . ? C3 C4 Na1 81.3(4) . . ? C5 C4 Na1 73.9(4) . . ? C14 O5 C15 112.7(14) . . ? C4 C5 C6 107.7(7) . . ? C4 C5 Na1 76.7(4) . . ? C6 C5 Na1 81.0(4) . . ? C16 O6 C17 116.5(15) . . ? C16 O6 Na1 115.4(9) . . ? C17 O6 Na1 105.3(7) . . ? C2 C6 C5 107.2(7) . . ? C2 C6 Na1 79.7(4) . . ? C5 C6 Na1 69.8(4) . . ? C8 C7 O1 107.9(8) . . ? O2 C8 C7 109.1(9) . . ? C10 C9 O2 107.5(8) . . ? O3 C10 C9 113.2(10) . . ? O3 C11 C12 112.5(9) . . ? O4 C12 C11 111.2(11) . . ? O4 C13 C14 107.6(9) . . ? O5 C14 C13 111.1(13) . . ? C16 C15 O5 109.2(8) . . ? O6 C16 C15 107.5(12) . . ? C18 C17 O6 116.6(14) . . ? O1 C18 C17 108.4(11) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.20 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.294 _refine_diff_density_min -0.206 _refine_diff_density_rms 0.051 #===END data_COMPOUND_9#d:\junkie\xtals\bonocx\marcus\kcp15c5\pj320c _database_code_CSD 172090 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C25 H45 K O10' _chemical_formula_weight 544.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'K' 'K' 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.793(3) _cell_length_b 9.119(3) _cell_length_c 9.377(3) _cell_angle_alpha 84.667(6) _cell_angle_beta 89.760(5) _cell_angle_gamma 78.841(7) _cell_volume 734.3(4) _cell_formula_units_Z 1 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 294 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.9341 _exptl_absorpt_correction_T_max 0.9447 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3278 _diffrn_reflns_av_R_equivalents 0.0678 _diffrn_reflns_av_sigmaI/netI 0.0825 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.26 _reflns_number_total 2079 _reflns_number_gt 1290 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1676P)^2^+0.0000P] 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 2079 _refine_ls_number_parameters 187 _refine_ls_number_restraints 35 _refine_ls_R_factor_all 0.1244 _refine_ls_R_factor_gt 0.0825 _refine_ls_wR_factor_ref 0.2506 _refine_ls_wR_factor_gt 0.2144 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.083 _refine_ls_shift/su_mean 0.009 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 1.0000 0.0000 0.5000 0.0439(6) Uani 1 2 d S . . O1 O 0.8020(5) 0.2516(4) 0.3463(4) 0.0636(13) Uani 1 1 d . . . C1 C 0.6609(8) 0.2853(7) 0.5578(7) 0.0673(19) Uani 1 1 d . . . H1A H 0.7227 0.3580 0.5795 0.081 Uiso 1 1 calc R . . H1B H 0.5575 0.3185 0.5936 0.081 Uiso 1 1 calc R . . O2 O 0.9025(5) 0.0005(5) 0.1896(4) 0.0669(13) Uani 1 1 d . . . C2 C 0.6509(8) 0.2854(8) 0.4040(8) 0.080(2) Uani 1 1 d . . . H2A H 0.5918 0.2113 0.3802 0.096 Uiso 1 1 calc R . . H2B H 0.5976 0.3831 0.3625 0.096 Uiso 1 1 calc R . . O3 O 0.9595(4) -0.2765(4) 0.3739(4) 0.0541(11) Uani 1 1 d . . . C3 C 0.8085(10) 0.2590(9) 0.1926(8) 0.089(3) Uani 1 1 d . . . H3A H 0.7277 0.3407 0.1533 0.107 Uiso 1 1 calc R . . H3B H 0.9073 0.2831 0.1629 0.107 Uiso 1 1 calc R . . O4 O 0.7389(5) -0.1542(4) 0.5720(4) 0.0533(11) Uani 1 1 d . . . C4 C 0.7910(9) 0.1276(8) 0.1332(7) 0.077(2) Uani 1 1 d . . . H4A H 0.8018 0.1415 0.0301 0.092 Uiso 1 1 calc R . . H4B H 0.6876 0.1089 0.1528 0.092 Uiso 1 1 calc R . . O5 O 0.7260(5) 0.1447(4) 0.6326(4) 0.0589(11) Uani 1 1 d . . . C5 C 0.8679(8) -0.1335(8) 0.1474(7) 0.0695(19) Uani 1 1 d . . . H5A H 0.8783 -0.1346 0.0445 0.083 Uiso 1 1 calc R . . H5B H 0.7616 -0.1388 0.1714 0.083 Uiso 1 1 calc R . . C6 C 0.9762(8) -0.2676(8) 0.2218(6) 0.0659(18) Uani 1 1 d . . . H6A H 0.9552 -0.3586 0.1868 0.079 Uiso 1 1 calc R . . H6B H 1.0824 -0.2610 0.1984 0.079 Uiso 1 1 calc R . . C7 C 0.8351(7) -0.3447(7) 0.4247(7) 0.0596(17) Uani 1 1 d . . . H7A H 0.8621 -0.4525 0.4201 0.071 Uiso 1 1 calc R . . H7B H 0.7433 -0.3060 0.3655 0.071 Uiso 1 1 calc R . . C8 C 0.8035(7) -0.3108(6) 0.5755(6) 0.0520(15) Uani 1 1 d . . . H8A H 0.7312 -0.3696 0.6179 0.062 Uiso 1 1 calc R . . H8B H 0.8988 -0.3348 0.6319 0.062 Uiso 1 1 calc R . . C9 C 0.7014(7) -0.1044(6) 0.7090(6) 0.0536(15) Uani 1 1 d . . . H9A H 0.7951 -0.1139 0.7663 0.064 Uiso 1 1 calc R . . H9B H 0.6344 -0.1648 0.7585 0.064 Uiso 1 1 calc R . . C10 C 0.6208(7) 0.0563(6) 0.6880(7) 0.0555(16) Uani 1 1 d . . . H10A H 0.5338 0.0668 0.6221 0.067 Uiso 1 1 calc R . . H10B H 0.5814 0.0896 0.7787 0.067 Uiso 1 1 calc R . . C11 C 0.5831(18) 0.4530(19) -0.0945(16) 0.057(4) Uani 0.50 1 d PDU . . H11 H 0.6201 0.4033 -0.1736 0.068 Uiso 0.50 1 calc PR . . C12 C 0.647(2) 0.5642(16) -0.0442(15) 0.096(5) Uani 0.50 1 d PDU . . H12 H 0.7360 0.5936 -0.0805 0.115 Uiso 0.50 1 calc PR . . C13 C 0.5637(19) 0.6266(18) 0.0654(16) 0.080(5) Uani 0.50 1 d PDU . . H13 H 0.5788 0.7024 0.1205 0.096 Uiso 0.50 1 calc PR . . C14 C 0.450(4) 0.541(3) 0.068(3) 0.123(11) Uani 0.50 1 d PDU . . H14 H 0.3657 0.5637 0.1280 0.148 Uiso 0.50 1 calc PR . . C15 C 0.4584(18) 0.423(2) -0.0157(18) 0.078(5) Uani 0.50 1 d PDU . . H15 H 0.4000 0.3480 -0.0180 0.094 Uiso 0.50 1 calc PR . . 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 0.0287(9) 0.0472(10) 0.0493(10) -0.0010(7) 0.0131(7) 0.0068(7) O1 0.055(3) 0.067(3) 0.055(2) -0.0003(19) 0.002(2) 0.020(2) C1 0.055(4) 0.049(4) 0.086(5) -0.004(3) 0.025(4) 0.016(3) O2 0.069(3) 0.064(3) 0.055(2) -0.001(2) 0.001(2) 0.014(2) C2 0.062(5) 0.070(5) 0.094(6) 0.007(4) -0.004(4) 0.017(3) O3 0.040(2) 0.064(2) 0.054(2) -0.0118(19) 0.0099(18) 0.0021(18) C3 0.100(6) 0.080(5) 0.071(5) 0.011(4) -0.010(4) 0.015(4) O4 0.051(2) 0.047(2) 0.055(2) -0.0041(17) 0.0155(19) 0.0059(18) C4 0.089(6) 0.074(5) 0.057(4) 0.004(3) -0.017(4) 0.007(4) O5 0.045(2) 0.049(2) 0.077(3) -0.003(2) 0.017(2) 0.0010(18) C5 0.062(4) 0.088(5) 0.053(4) -0.016(3) -0.001(3) 0.005(4) C6 0.060(4) 0.077(4) 0.055(4) -0.016(3) 0.013(3) 0.004(3) C7 0.040(3) 0.057(4) 0.078(4) -0.010(3) 0.007(3) 0.001(3) C8 0.044(3) 0.036(3) 0.071(4) 0.002(3) 0.012(3) 0.001(2) C9 0.043(3) 0.066(4) 0.048(3) 0.001(3) 0.013(3) -0.004(3) C10 0.050(4) 0.054(3) 0.062(4) -0.017(3) 0.015(3) -0.005(3) C11 0.054(7) 0.079(8) 0.016(5) -0.002(5) 0.003(5) 0.039(6) C12 0.086(9) 0.095(9) 0.084(8) 0.027(7) 0.016(7) 0.022(7) C13 0.095(9) 0.061(7) 0.069(8) -0.024(6) -0.016(7) 0.029(7) C14 0.118(14) 0.127(14) 0.105(14) -0.001(9) -0.005(9) 0.023(9) C15 0.078(9) 0.075(8) 0.086(9) -0.002(7) -0.047(8) -0.026(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag K1 O5 2.854(4) 2_756 ? K1 O5 2.854(4) . ? K1 O1 2.869(4) 2_756 ? K1 O1 2.869(4) . ? K1 O3 2.964(4) 2_756 ? K1 O3 2.964(4) . ? K1 O4 2.960(4) 2_756 ? K1 O4 2.960(4) . ? K1 O2 3.037(4) . ? K1 O2 3.037(4) 2_756 ? K1 C9 3.495(6) 2_756 ? O1 C2 1.422(8) . ? O1 C3 1.438(8) . ? C1 O5 1.420(7) . ? C1 C2 1.445(9) . ? O2 C5 1.406(8) . ? O2 C4 1.427(7) . ? O3 C7 1.420(7) . ? O3 C6 1.430(7) . ? C3 C4 1.403(10) . ? O4 C9 1.419(6) . ? O4 C8 1.429(6) . ? O5 C10 1.408(7) . ? C5 C6 1.512(8) . ? C7 C8 1.488(8) . ? C9 C10 1.495(7) . ? C11 C12 1.370(10) . ? C11 C15 1.378(10) . ? C12 C13 1.362(10) . ? C13 C14 1.380(10) . ? C14 C15 1.387(10) . ? C15 C15 1.76(4) 2_665 ? 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 O5 K1 O5 180.00(11) 2_756 . ? O5 K1 O1 60.69(12) 2_756 2_756 ? O5 K1 O1 119.31(12) . 2_756 ? O5 K1 O1 119.31(12) 2_756 . ? O5 K1 O1 60.69(12) . . ? O1 K1 O1 180.0 2_756 . ? O5 K1 O3 112.83(11) 2_756 2_756 ? O5 K1 O3 67.17(11) . 2_756 ? O1 K1 O3 108.32(11) 2_756 2_756 ? O1 K1 O3 71.68(11) . 2_756 ? O5 K1 O3 67.17(11) 2_756 . ? O5 K1 O3 112.83(12) . . ? O1 K1 O3 71.68(11) 2_756 . ? O1 K1 O3 108.32(11) . . ? O3 K1 O3 180.00(6) 2_756 . ? O5 K1 O4 57.92(11) 2_756 2_756 ? O5 K1 O4 122.08(11) . 2_756 ? O1 K1 O4 92.74(12) 2_756 2_756 ? O1 K1 O4 87.26(12) . 2_756 ? O3 K1 O4 56.93(10) 2_756 2_756 ? O3 K1 O4 123.07(10) . 2_756 ? O5 K1 O4 122.08(11) 2_756 . ? O5 K1 O4 57.92(11) . . ? O1 K1 O4 87.26(12) 2_756 . ? O1 K1 O4 92.74(12) . . ? O3 K1 O4 123.07(10) 2_756 . ? O3 K1 O4 56.93(10) . . ? O4 K1 O4 180.00(11) 2_756 . ? O5 K1 O2 75.97(12) 2_756 . ? O5 K1 O2 104.03(12) . . ? O1 K1 O2 122.81(11) 2_756 . ? O1 K1 O2 57.19(11) . . ? O3 K1 O2 122.54(11) 2_756 . ? O3 K1 O2 57.46(11) . . ? O4 K1 O2 94.05(12) 2_756 . ? O4 K1 O2 85.95(12) . . ? O5 K1 O2 104.03(12) 2_756 2_756 ? O5 K1 O2 75.97(12) . 2_756 ? O1 K1 O2 57.19(11) 2_756 2_756 ? O1 K1 O2 122.81(11) . 2_756 ? O3 K1 O2 57.46(11) 2_756 2_756 ? O3 K1 O2 122.54(11) . 2_756 ? O4 K1 O2 85.95(12) 2_756 2_756 ? O4 K1 O2 94.05(12) . 2_756 ? O2 K1 O2 180.00(4) . 2_756 ? O5 K1 C9 42.30(12) 2_756 2_756 ? O5 K1 C9 137.70(12) . 2_756 ? O1 K1 C9 94.22(13) 2_756 2_756 ? O1 K1 C9 85.78(13) . 2_756 ? O3 K1 C9 78.76(12) 2_756 2_756 ? O3 K1 C9 101.24(12) . 2_756 ? O4 K1 C9 23.57(12) 2_756 2_756 ? O4 K1 C9 156.43(12) . 2_756 ? O2 K1 C9 73.47(13) . 2_756 ? O2 K1 C9 106.53(13) 2_756 2_756 ? C2 O1 C3 115.4(5) . . ? C2 O1 K1 113.5(3) . . ? C3 O1 K1 116.3(3) . . ? O5 C1 C2 115.2(5) . . ? C5 O2 C4 111.2(5) . . ? C5 O2 K1 117.1(3) . . ? C4 O2 K1 115.9(4) . . ? O1 C2 C1 110.0(6) . . ? C7 O3 C6 114.2(5) . . ? C7 O3 K1 117.3(3) . . ? C6 O3 K1 113.3(4) . . ? C4 C3 O1 115.1(6) . . ? C9 O4 C8 113.8(4) . . ? C9 O4 K1 99.9(3) . . ? C8 O4 K1 105.2(3) . . ? C3 C4 O2 112.0(6) . . ? C10 O5 C1 116.5(5) . . ? C10 O5 K1 118.4(3) . . ? C1 O5 K1 112.0(3) . . ? O2 C5 C6 110.4(5) . . ? O3 C6 C5 112.1(5) . . ? O3 C7 C8 108.7(5) . . ? O4 C8 C7 107.1(4) . . ? O4 C9 C10 107.9(4) . . ? O5 C10 C9 109.3(5) . . ? C12 C11 C15 112.9(13) . . ? C13 C12 C11 111.8(18) . . ? C12 C13 C14 97(2) . . ? C13 C14 C15 122(3) . . ? C11 C15 C14 95.6(18) . . ? C11 C15 C15 59.6(11) . 2_665 ? C14 C15 C15 36.0(18) . 2_665 ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.540 _refine_diff_density_min -0.383 _refine_diff_density_rms 0.085 #===END