# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1748 data_rs0027 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H74 N12 O Zn4' _chemical_formula_weight 1468.98 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' 'N' 'N' 0.0061 0.0033 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Ia3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, -z+1/2' '-x+1/2, y, -z' '-x, -y+1/2, z' 'z, x, y' 'z, -x, -y+1/2' '-z+1/2, x, -y' '-z, -x+1/2, y' 'y, z, x' 'y, -z, -x+1/2' '-y+1/2, z, -x' '-y, -z+1/2, x' 'x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, -z+1' '-x+1, y+1/2, -z+1/2' '-x+1/2, -y+1, z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1' '-z+1, x+1/2, -y+1/2' '-z+1/2, -x+1, y+1/2' 'y+1/2, z+1/2, x+1/2' 'y+1/2, -z+1/2, -x+1' '-y+1, z+1/2, -x+1/2' '-y+1/2, -z+1, x+1/2' '-x, -y, -z' '-x, y, z-1/2' 'x-1/2, -y, z' 'x, y-1/2, -z' '-z, -x, -y' '-z, x, y-1/2' 'z-1/2, -x, y' 'z, x-1/2, -y' '-y, -z, -x' '-y, z, x-1/2' 'y-1/2, -z, x' 'y, z-1/2, -x' '-x+1/2, -y+1/2, -z+1/2' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' 'x+1/2, y, -z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y' 'z, -x+1/2, y+1/2' 'z+1/2, x, -y+1/2' '-y+1/2, -z+1/2, -x+1/2' '-y+1/2, z+1/2, x' 'y, -z+1/2, x+1/2' 'y+1/2, z, -x+1/2' _cell_length_a 30.8060(7) _cell_length_b 30.8060(7) _cell_length_c 30.8060(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 29235.2(12) _cell_formula_units_Z 16 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.335 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 12160 _exptl_absorpt_coefficient_mu 1.350 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.7290 _exptl_absorpt_correction_T_max 0.7466 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _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 8240 _diffrn_reflns_av_R_equivalents 0.0886 _diffrn_reflns_av_sigmaI/netI 0.1698 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 25.02 _reflns_number_total 4297 _reflns_number_gt 1963 _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^)+(0.1442P)^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 0.00144(13) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4297 _refine_ls_number_parameters 276 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1941 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2608 _refine_ls_wR_factor_gt 0.1987 _refine_ls_goodness_of_fit_ref 0.993 _refine_ls_restrained_S_all 0.993 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0979(3) 0.2008(3) 0.0630(3) 0.056(2) Uani 1 1 d . . . N1 N 0.1423(2) 0.1992(2) 0.0638(2) 0.0560(18) Uani 1 1 d . . . O1 O 0.15548(16) 0.15548(16) 0.15548(16) 0.051(2) Uani 1 3 d S . . Zn1A Zn 0.09837(3) 0.17921(3) 0.15502(3) 0.0536(5) Uani 1 1 d . . . Zn2 Zn 0.19113(3) 0.19113(3) 0.19113(3) 0.0626(6) Uani 1 3 d S . . C2 C 0.0779(3) 0.2262(3) 0.0311(3) 0.071(3) Uani 1 1 d . . . H2A H 0.0472 0.2260 0.0283 0.085 Uiso 1 1 calc R . . N2 N 0.1509(2) 0.2252(2) 0.2314(2) 0.0548(17) Uani 1 1 d . . . C3 C 0.1025(4) 0.2513(3) 0.0038(3) 0.086(3) Uani 1 1 d . . . H3A H 0.0887 0.2690 -0.0174 0.103 Uiso 1 1 calc R . . N3 N 0.1001(2) 0.2402(2) 0.1775(2) 0.0583(18) Uani 1 1 d . . . C4 C 0.1472(4) 0.2512(3) 0.0070(3) 0.085(3) Uani 1 1 d . . . H4A H 0.1643 0.2693 -0.0111 0.102 Uiso 1 1 calc R . . N4 N 0.0766(2) 0.1784(2) 0.0944(2) 0.0610(19) Uani 1 1 d . . . C5 C 0.1658(3) 0.2248(3) 0.0364(3) 0.067(2) Uani 1 1 d . . . H5A H 0.1966 0.2240 0.0381 0.081 Uiso 1 1 calc R . . C6 C 0.0287(3) 0.1752(3) 0.0903(3) 0.068(3) Uani 1 1 d . . . H6A H 0.0166 0.2050 0.0883 0.082 Uiso 1 1 calc R . . H6B H 0.0170 0.1618 0.1170 0.082 Uiso 1 1 calc R . . C7 C 0.0128(3) 0.1495(3) 0.0518(3) 0.058(2) Uani 1 1 d . . . C8 C 0.0393(3) 0.1200(3) 0.0293(3) 0.068(2) Uani 1 1 d . . . H8A H 0.0689 0.1165 0.0376 0.082 Uiso 1 1 calc R . . C9 C 0.0230(4) 0.0963(3) -0.0042(3) 0.082(3) Uani 1 1 d . . . H9A H 0.0412 0.0761 -0.0187 0.098 Uiso 1 1 calc R . . C10 C -0.0192(4) 0.1011(3) -0.0173(3) 0.079(3) Uani 1 1 d . . . H10A H -0.0300 0.0856 -0.0417 0.095 Uiso 1 1 calc R . . C11 C -0.0457(4) 0.1289(4) 0.0055(3) 0.088(3) Uani 1 1 d . . . H11A H -0.0754 0.1314 -0.0025 0.106 Uiso 1 1 calc R . . C12 C -0.0301(3) 0.1534(3) 0.0401(3) 0.072(3) Uani 1 1 d . . . H12A H -0.0488 0.1725 0.0554 0.086 Uiso 1 1 calc R . . C13 C 0.1632(3) 0.2302(3) 0.2735(3) 0.062(2) Uani 1 1 d . . . H13A H 0.1863 0.2125 0.2837 0.075 Uiso 1 1 calc R . . C14 C 0.1455(3) 0.2581(3) 0.3016(3) 0.071(3) Uani 1 1 d . . . H14A H 0.1551 0.2595 0.3309 0.085 Uiso 1 1 calc R . . C15 C 0.1130(3) 0.2846(3) 0.2867(3) 0.075(3) Uani 1 1 d . . . H15A H 0.1005 0.3056 0.3055 0.090 Uiso 1 1 calc R . . C16 C 0.0987(3) 0.2810(3) 0.2454(3) 0.063(2) Uani 1 1 d . . . H16A H 0.0767 0.3000 0.2352 0.076 Uiso 1 1 calc R . . C17 C 0.1162(3) 0.2496(3) 0.2174(3) 0.057(2) Uani 1 1 d . . . C18 C 0.0699(3) 0.2714(3) 0.1587(3) 0.066(2) Uani 1 1 d . . . H18A H 0.0468 0.2775 0.1802 0.079 Uiso 1 1 calc R . . H18B H 0.0559 0.2580 0.1330 0.079 Uiso 1 1 calc R . . C19 C 0.0900(3) 0.3132(3) 0.1452(3) 0.065(2) Uani 1 1 d . . . C20 C 0.0707(4) 0.3517(3) 0.1547(3) 0.084(3) Uani 1 1 d . . . H20A H 0.0446 0.3522 0.1710 0.101 Uiso 1 1 calc R . . C21 C 0.0897(5) 0.3913(4) 0.1402(5) 0.111(4) Uani 1 1 d . . . H21A H 0.0764 0.4183 0.1467 0.133 Uiso 1 1 calc R . . C22 C 0.1273(5) 0.3898(5) 0.1168(5) 0.121(5) Uani 1 1 d . . . H22A H 0.1397 0.4158 0.1057 0.146 Uiso 1 1 calc R . . C23 C 0.1470(4) 0.3514(5) 0.1094(4) 0.117(5) Uani 1 1 d . . . H23A H 0.1742 0.3508 0.0950 0.140 Uiso 1 1 calc R . . C24 C 0.1282(4) 0.3134(3) 0.1222(3) 0.082(3) Uani 1 1 d . . . H24A H 0.1418 0.2866 0.1152 0.099 Uiso 1 1 calc R . . C25 C 0.0017(8) 0.3053(6) -0.0897(7) 0.095(4) Uiso 0.33 1 d PG A -1 C26 C -0.0039(9) 0.2929(7) -0.1327(6) 0.095(4) Uiso 0.33 1 d PG A -1 C28 C -0.0062(10) 0.2492(8) -0.1435(5) 0.095(4) Uiso 0.33 1 d PG A -1 C27 C -0.0029(8) 0.2178(6) -0.1113(7) 0.095(4) Uiso 0.33 1 d PG A -1 C29 C 0.0026(11) 0.2301(7) -0.0683(6) 0.095(4) Uiso 0.33 1 d PG A -1 C30 C 0.0049(11) 0.2739(9) -0.0574(5) 0.095(4) Uiso 0.33 1 d PG 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 C1 0.059(6) 0.062(5) 0.046(5) -0.013(4) -0.002(4) 0.005(5) N1 0.067(5) 0.054(4) 0.048(4) 0.002(3) 0.002(4) 0.000(4) O1 0.051(2) 0.051(2) 0.051(2) -0.001(2) -0.001(2) -0.001(2) Zn1A 0.0511(7) 0.0578(7) 0.0518(7) -0.0016(5) -0.0034(4) 0.0016(5) Zn2 0.0626(6) 0.0626(6) 0.0626(6) -0.0032(5) -0.0032(5) -0.0032(5) C2 0.084(7) 0.058(5) 0.071(6) -0.004(5) -0.017(6) 0.018(5) N2 0.063(4) 0.051(4) 0.050(4) -0.003(3) -0.003(3) -0.002(4) C3 0.115(9) 0.074(7) 0.068(6) 0.024(6) -0.004(6) 0.029(7) N3 0.064(4) 0.054(4) 0.057(4) -0.003(4) -0.006(4) 0.003(4) C4 0.100(8) 0.082(7) 0.072(7) 0.018(6) 0.022(6) 0.015(6) N4 0.052(4) 0.070(5) 0.061(5) -0.009(4) -0.003(4) 0.003(4) C5 0.082(6) 0.059(5) 0.061(6) 0.006(5) 0.010(5) 0.001(5) C6 0.057(6) 0.081(6) 0.066(6) -0.010(5) -0.004(5) 0.010(5) C7 0.052(5) 0.070(6) 0.051(5) 0.003(4) -0.006(4) -0.001(5) C8 0.065(6) 0.076(6) 0.064(6) -0.004(5) -0.004(5) 0.000(5) C9 0.092(8) 0.076(7) 0.077(7) -0.018(6) 0.004(6) -0.005(6) C10 0.089(8) 0.084(7) 0.065(6) -0.005(6) -0.006(6) -0.031(6) C11 0.075(7) 0.117(9) 0.072(7) 0.008(7) -0.014(6) -0.001(7) C12 0.063(6) 0.090(7) 0.062(6) -0.013(5) -0.011(5) 0.002(5) C13 0.067(6) 0.063(6) 0.057(6) -0.001(5) -0.006(5) -0.010(5) C14 0.083(7) 0.085(7) 0.043(5) -0.012(5) 0.000(5) -0.007(6) C15 0.082(7) 0.085(7) 0.059(6) -0.016(5) 0.003(5) 0.004(6) C16 0.057(5) 0.065(6) 0.067(6) -0.005(5) 0.004(5) 0.001(5) C17 0.062(5) 0.052(5) 0.058(6) -0.004(4) -0.001(5) -0.009(5) C18 0.068(6) 0.055(5) 0.074(6) -0.001(5) -0.013(5) 0.010(5) C19 0.076(7) 0.061(6) 0.057(5) -0.006(5) -0.017(5) 0.018(5) C20 0.088(7) 0.077(7) 0.087(7) -0.011(6) -0.014(6) 0.002(6) C21 0.119(11) 0.087(9) 0.127(11) 0.018(8) -0.029(9) -0.002(8) C22 0.118(12) 0.086(10) 0.160(14) 0.050(9) -0.033(10) -0.014(9) C23 0.101(10) 0.128(12) 0.121(11) 0.055(9) 0.001(8) -0.002(9) C24 0.093(8) 0.071(7) 0.083(7) 0.018(6) 0.002(6) 0.011(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 N4 1.356(10) . ? C1 N1 1.369(10) . ? C1 C2 1.401(11) . ? N1 C5 1.364(10) . ? N1 Zn1A 2.069(7) 9 ? O1 Zn2 1.902(8) . ? O1 Zn1A 1.905(3) 5 ? O1 Zn1A 1.905(3) . ? O1 Zn1A 1.905(3) 9 ? Zn1A N4 1.984(7) . ? Zn1A N3 2.002(7) . ? Zn1A N1 2.069(7) 5 ? Zn1A Zn2 3.0885(16) . ? Zn1A Zn1A 3.1308(16) 5 ? Zn1A Zn1A 3.1308(16) 9 ? Zn2 N2 2.045(7) 5 ? Zn2 N2 2.045(7) . ? Zn2 N2 2.045(7) 9 ? Zn2 Zn1A 3.0885(16) 5 ? Zn2 Zn1A 3.0885(16) 9 ? C2 C3 1.372(13) . ? N2 C13 1.360(10) . ? N2 C17 1.374(10) . ? C3 C4 1.380(13) . ? N3 C17 1.357(10) . ? N3 C18 1.458(10) . ? C4 C5 1.344(13) . ? N4 C6 1.486(10) . ? C6 C7 1.508(11) . ? C7 C12 1.376(11) . ? C7 C8 1.404(11) . ? C8 C9 1.361(12) . ? C9 C10 1.370(13) . ? C10 C11 1.377(14) . ? C11 C12 1.390(13) . ? C13 C14 1.337(12) . ? C14 C15 1.371(13) . ? C15 C16 1.352(12) . ? C16 C17 1.405(11) . ? C18 C19 1.488(12) . ? C19 C20 1.359(12) . ? C19 C24 1.374(14) . ? C20 C21 1.424(15) . ? C21 C22 1.366(18) . ? C22 C23 1.348(18) . ? C23 C24 1.364(16) . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C26 C28 1.3900 . ? C28 C27 1.3900 . ? C27 C29 1.3900 . ? C29 C30 1.3900 . ? 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 N4 C1 N1 116.9(7) . . ? N4 C1 C2 124.9(8) . . ? N1 C1 C2 118.1(8) . . ? C5 N1 C1 119.9(7) . . ? C5 N1 Zn1A 114.1(6) . 9 ? C1 N1 Zn1A 125.5(6) . 9 ? Zn2 O1 Zn1A 108.4(2) . 5 ? Zn2 O1 Zn1A 108.4(2) . . ? Zn1A O1 Zn1A 110.5(2) 5 . ? Zn2 O1 Zn1A 108.4(2) . 9 ? Zn1A O1 Zn1A 110.5(2) 5 9 ? Zn1A O1 Zn1A 110.5(2) . 9 ? O1 Zn1A N4 108.3(3) . . ? O1 Zn1A N3 109.4(3) . . ? N4 Zn1A N3 110.2(3) . . ? O1 Zn1A N1 105.05(19) . 5 ? N4 Zn1A N1 116.0(3) . 5 ? N3 Zn1A N1 107.6(3) . 5 ? O1 Zn1A Zn2 35.8(2) . . ? N4 Zn1A Zn2 130.8(2) . . ? N3 Zn1A Zn2 74.87(19) . . ? N1 Zn1A Zn2 107.74(17) 5 . ? O1 Zn1A Zn1A 34.75(11) . 5 ? N4 Zn1A Zn1A 113.7(2) . 5 ? N3 Zn1A Zn1A 130.46(19) . 5 ? N1 Zn1A Zn1A 72.13(19) 5 5 ? Zn2 Zn1A Zn1A 59.55(2) . 5 ? O1 Zn1A Zn1A 34.75(11) . 9 ? N4 Zn1A Zn1A 75.0(2) . 9 ? N3 Zn1A Zn1A 113.20(19) . 9 ? N1 Zn1A Zn1A 130.20(19) 5 9 ? Zn2 Zn1A Zn1A 59.55(2) . 9 ? Zn1A Zn1A Zn1A 60.0 5 9 ? O1 Zn2 N2 107.26(18) . 5 ? O1 Zn2 N2 107.26(18) . . ? N2 Zn2 N2 111.59(17) 5 . ? O1 Zn2 N2 107.26(18) . 9 ? N2 Zn2 N2 111.59(17) 5 9 ? N2 Zn2 N2 111.59(17) . 9 ? O1 Zn2 Zn1A 35.82(3) . 5 ? N2 Zn2 Zn1A 73.65(18) 5 5 ? N2 Zn2 Zn1A 109.22(18) . 5 ? N2 Zn2 Zn1A 132.40(19) 9 5 ? O1 Zn2 Zn1A 35.82(3) . . ? N2 Zn2 Zn1A 132.40(19) 5 . ? N2 Zn2 Zn1A 73.65(18) . . ? N2 Zn2 Zn1A 109.22(18) 9 . ? Zn1A Zn2 Zn1A 60.91(4) 5 . ? O1 Zn2 Zn1A 35.82(3) . 9 ? N2 Zn2 Zn1A 109.22(18) 5 9 ? N2 Zn2 Zn1A 132.40(19) . 9 ? N2 Zn2 Zn1A 73.65(18) 9 9 ? Zn1A Zn2 Zn1A 60.91(4) 5 9 ? Zn1A Zn2 Zn1A 60.91(4) . 9 ? C3 C2 C1 120.3(9) . . ? C13 N2 C17 117.1(7) . . ? C13 N2 Zn2 117.8(6) . . ? C17 N2 Zn2 124.1(5) . . ? C2 C3 C4 120.3(9) . . ? C17 N3 C18 116.9(7) . . ? C17 N3 Zn1A 121.5(5) . . ? C18 N3 Zn1A 117.6(5) . . ? C5 C4 C3 118.4(10) . . ? C1 N4 C6 116.9(7) . . ? C1 N4 Zn1A 120.1(5) . . ? C6 N4 Zn1A 114.7(5) . . ? C4 C5 N1 122.7(9) . . ? N4 C6 C7 115.1(7) . . ? C12 C7 C8 119.1(8) . . ? C12 C7 C6 118.1(8) . . ? C8 C7 C6 122.7(8) . . ? C9 C8 C7 120.4(9) . . ? C8 C9 C10 121.2(10) . . ? C9 C10 C11 118.6(9) . . ? C10 C11 C12 121.6(10) . . ? C7 C12 C11 119.1(9) . . ? C14 C13 N2 125.2(9) . . ? C13 C14 C15 117.6(9) . . ? C16 C15 C14 120.3(9) . . ? C15 C16 C17 120.7(9) . . ? N3 C17 N2 116.9(7) . . ? N3 C17 C16 124.3(8) . . ? N2 C17 C16 118.7(8) . . ? N3 C18 C19 114.5(7) . . ? C20 C19 C24 118.7(10) . . ? C20 C19 C18 120.9(9) . . ? C24 C19 C18 120.3(8) . . ? C19 C20 C21 120.1(11) . . ? C22 C21 C20 119.0(12) . . ? C23 C22 C21 120.0(13) . . ? C22 C23 C24 120.9(13) . . ? C23 C24 C19 121.1(11) . . ? C26 C25 C30 120.0 . . ? C28 C26 C25 120.0 . . ? C26 C28 C27 120.0 . . ? C28 C27 C29 120.0 . . ? C30 C29 C27 120.0 . . ? C29 C30 C25 120.0 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.301 _refine_diff_density_min -1.446 _refine_diff_density_rms 0.385 data_rs0004 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound X' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H59 Li3 N12 O3 Zn3' _chemical_formula_weight 1020.96 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' 'N' 'N' 0.0061 0.0033 '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' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M P213 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' 'x+1/2, -y+1/2, -z' 'z+1/2, -x+1/2, -y' 'y+1/2, -z+1/2, -x' '-x, y+1/2, -z+1/2' '-z, x+1/2, -y+1/2' '-y, z+1/2, -x+1/2' '-x+1/2, -y, z+1/2' '-z+1/2, -x, y+1/2' '-y+1/2, -z, x+1/2' _cell_length_a 16.964(2) _cell_length_b 16.964(2) _cell_length_c 16.964(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4882.0(10) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 23059 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 22.465 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.389 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2120 _exptl_absorpt_coefficient_mu 1.513 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8276 _exptl_absorpt_correction_T_max 0.8276 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20356 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0256 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 22.44 _reflns_number_total 2128 _reflns_number_gt 1986 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _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^)+(0.1541P)^2^+4.5598P] 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 0.0092(19) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.05(4) _refine_ls_number_reflns 2128 _refine_ls_number_parameters 205 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2168 _refine_ls_wR_factor_gt 0.2093 _refine_ls_goodness_of_fit_ref 1.190 _refine_ls_restrained_S_all 1.190 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.33355(7) 0.80550(7) 0.27074(7) 0.0575(5) Uani 1 1 d . . . O1 O 0.2822(3) 0.7178(3) 0.2178(3) 0.0341(19) Uani 1 3 d S . . N1 N 0.3526(4) 0.7865(4) 0.3879(4) 0.0462(18) Uani 1 1 d . . . C1 C 0.4248(6) 0.8124(6) 0.4189(5) 0.057(2) Uani 1 1 d . . . H1A H 0.4641 0.8312 0.3838 0.068 Uiso 1 1 calc R . . Li1 Li 0.3726(7) 0.6373(7) 0.2349(7) 0.035(2) Uani 1 1 d . . . N2 N 0.2287(5) 0.7361(5) 0.4043(4) 0.0559(19) Uani 1 1 d . . . C2 C 0.4398(8) 0.8116(8) 0.4951(8) 0.089(4) Uani 1 1 d . . . H2B H 0.4879 0.8315 0.5157 0.106 Uiso 1 1 calc R . . O2 O 0.3736(3) 0.6264(3) 0.1264(3) 0.041(2) Uani 1 3 d S . . N3 N 0.4722(4) 0.6990(5) 0.2689(5) 0.0540(19) Uani 1 1 d . . . C3 C 0.3812(10) 0.7798(8) 0.5450(7) 0.094(4) Uani 1 1 d . . . H3A H 0.3914 0.7768 0.6000 0.112 Uiso 1 1 calc R . . N4 N 0.4333(4) 0.8110(5) 0.2012(5) 0.0535(19) Uani 1 1 d . . . C4 C 0.3141(7) 0.7545(6) 0.5187(5) 0.062(3) Uani 1 1 d . . . H4A H 0.2759 0.7342 0.5543 0.075 Uiso 1 1 calc R . . C5 C 0.2977(5) 0.7571(5) 0.4370(4) 0.0411(18) Uani 1 1 d . . . C6 C 0.1682(8) 0.7085(7) 0.4586(6) 0.077(3) Uani 1 1 d . . . H6A H 0.1162 0.7249 0.4395 0.115 Uiso 1 1 calc R . . H6B H 0.1775 0.7313 0.5109 0.115 Uiso 1 1 calc R . . H6C H 0.1703 0.6509 0.4620 0.115 Uiso 1 1 calc R . . C7 C 0.5268(6) 0.6587(7) 0.3093(7) 0.070(3) Uani 1 1 d . . . H7A H 0.5142 0.6079 0.3290 0.084 Uiso 1 1 calc R . . C8 C 0.6005(8) 0.6891(13) 0.3228(9) 0.107(5) Uani 1 1 d . . . H8A H 0.6374 0.6600 0.3532 0.128 Uiso 1 1 calc R . . C9 C 0.6210(7) 0.7601(12) 0.2932(9) 0.100(5) Uani 1 1 d . . . H9A H 0.6723 0.7803 0.3026 0.119 Uiso 1 1 calc R . . C10 C 0.5711(7) 0.8009(9) 0.2518(8) 0.084(4) Uani 1 1 d . . . H10A H 0.5863 0.8504 0.2305 0.101 Uiso 1 1 calc R . . C11 C 0.4926(5) 0.7713(6) 0.2380(6) 0.055(2) Uani 1 1 d . . . C12 C 0.4524(7) 0.8875(7) 0.1668(8) 0.077(3) Uani 1 1 d . . . H12A H 0.5017 0.8833 0.1369 0.116 Uiso 1 1 calc R . . H12B H 0.4587 0.9265 0.2090 0.116 Uiso 1 1 calc R . . H12C H 0.4098 0.9039 0.1315 0.116 Uiso 1 1 calc R . . C13 C 0.4237(5) 0.5763(5) 0.0763(5) 0.064(5) Uani 1 3 d S . . C14 C 0.4932(9) 0.6276(11) 0.0484(15) 0.141(8) Uani 1 1 d . . . H14A H 0.5287 0.5959 0.0156 0.212 Uiso 1 1 calc R . . H14B H 0.5221 0.6476 0.0943 0.212 Uiso 1 1 calc R . . H14C H 0.4731 0.6721 0.0175 0.212 Uiso 1 1 calc R . . O3 O 0.3921(16) 1.0951(14) -0.1159(15) 0.049(6) Uiso 0.33 1 d PD A -1 C20 C 0.357(2) 1.062(3) -0.045(2) 0.090(11) Uiso 0.33 1 d PD A -1 H20A H 0.3266 1.1024 -0.0159 0.108 Uiso 0.33 1 calc PR A -1 H20B H 0.3211 1.0178 -0.0582 0.108 Uiso 0.33 1 calc PR A -1 C21 C 0.422(2) 1.034(2) 0.0027(14) 0.062(10) Uiso 0.33 1 d PD A -1 H21A H 0.4255 1.0654 0.0517 0.074 Uiso 0.33 1 calc PR A -1 H21B H 0.4130 0.9781 0.0174 0.074 Uiso 0.33 1 calc PR A -1 C22 C 0.4914(15) 1.041(4) -0.041(3) 0.073(12) Uiso 0.33 1 d PD A -1 H22A H 0.5060 0.9895 -0.0639 0.088 Uiso 0.33 1 calc PR A -1 H22B H 0.5349 1.0588 -0.0062 0.088 Uiso 0.33 1 calc PR A -1 C23 C 0.477(3) 1.098(3) -0.102(3) 0.112(15) Uiso 0.33 1 d PD A -1 H23A H 0.5064 1.0841 -0.1509 0.134 Uiso 0.33 1 calc PR A -1 H23B H 0.4935 1.1515 -0.0853 0.134 Uiso 0.33 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 Zn1 0.0577(8) 0.0566(8) 0.0584(8) -0.0010(5) -0.0025(5) -0.0004(5) O1 0.0341(19) 0.0341(19) 0.0341(19) 0.002(2) -0.002(2) -0.002(2) N1 0.052(4) 0.053(4) 0.034(3) -0.010(3) -0.014(3) 0.010(3) C1 0.059(5) 0.066(6) 0.046(5) 0.000(4) -0.006(4) -0.014(5) Li1 0.036(6) 0.037(6) 0.032(6) 0.010(5) 0.005(5) 0.001(5) N2 0.052(4) 0.077(5) 0.039(4) -0.008(4) 0.011(3) -0.006(4) C2 0.081(8) 0.095(8) 0.089(9) -0.020(8) -0.040(7) -0.002(7) O2 0.041(2) 0.041(2) 0.041(2) -0.006(2) 0.006(2) 0.006(2) N3 0.041(4) 0.069(5) 0.052(4) -0.017(4) -0.002(3) 0.006(4) C3 0.144(13) 0.085(9) 0.051(6) 0.007(6) -0.010(8) 0.008(9) N4 0.045(4) 0.055(4) 0.061(4) -0.005(4) 0.011(4) -0.015(4) C4 0.081(7) 0.069(6) 0.038(5) 0.001(4) -0.014(5) -0.010(5) C5 0.049(5) 0.041(4) 0.033(4) 0.001(3) 0.005(4) 0.001(4) C6 0.088(8) 0.086(8) 0.056(6) -0.015(5) 0.014(6) -0.017(7) C7 0.056(6) 0.085(7) 0.069(6) -0.024(6) -0.010(5) 0.019(5) C8 0.059(8) 0.164(15) 0.097(10) -0.025(11) -0.037(7) 0.045(9) C9 0.043(6) 0.148(14) 0.108(11) -0.010(10) -0.003(7) -0.004(8) C10 0.042(5) 0.116(10) 0.094(9) -0.030(8) 0.020(6) -0.016(6) C11 0.032(4) 0.070(6) 0.064(5) -0.031(5) 0.005(4) -0.008(4) C12 0.072(7) 0.066(7) 0.094(8) -0.002(6) 0.020(6) -0.022(5) C13 0.064(5) 0.064(5) 0.064(5) -0.021(4) 0.021(4) 0.021(4) C14 0.089(10) 0.117(12) 0.22(2) -0.029(14) 0.105(13) 0.006(9) _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 Zn1 O1 1.944(4) . ? Zn1 N1 2.039(6) . ? Zn1 N2 2.050(7) 9_655 ? Zn1 N4 2.065(7) . ? Zn1 Li1 2.755(12) 9_655 ? Zn1 Li1 2.992(12) . ? Zn1 Zn1 3.0070(19) 9_655 ? Zn1 Zn1 3.0070(19) 11_564 ? O1 Zn1 1.944(4) 9_655 ? O1 Zn1 1.944(4) 11_564 ? O1 Li1 2.074(13) 11_564 ? O1 Li1 2.074(13) 9_655 ? O1 Li1 2.074(13) . ? N1 C5 1.345(11) . ? N1 C1 1.404(12) . ? C1 C2 1.317(16) . ? Li1 O2 1.849(14) . ? Li1 N3 2.071(14) . ? Li1 N4 2.160(13) 11_564 ? Li1 Li1 2.47(2) 11_564 ? Li1 Li1 2.47(2) 9_655 ? Li1 Zn1 2.755(12) 11_564 ? N2 C5 1.345(12) . ? N2 C6 1.456(14) . ? N2 Zn1 2.050(7) 11_564 ? C2 C3 1.41(2) . ? O2 C13 1.474(19) . ? O2 Li1 1.849(14) 11_564 ? O2 Li1 1.849(14) 9_655 ? N3 C7 1.339(13) . ? N3 C11 1.377(13) . ? C3 C4 1.296(19) . ? N4 C11 1.363(13) . ? N4 C12 1.459(14) . ? N4 Li1 2.160(13) 9_655 ? C4 C5 1.414(13) . ? C7 C8 1.37(2) . ? C8 C9 1.35(2) . ? C9 C10 1.30(2) . ? C10 C11 1.441(14) . ? C13 C14 1.541(16) 9_655 ? C13 C14 1.541(16) . ? C13 C14 1.541(16) 11_564 ? O3 C20 1.46(3) . ? O3 C23 1.46(3) . ? C20 C21 1.44(4) . ? C21 C22 1.40(5) . ? C22 C23 1.45(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Zn1 N1 113.6(2) . . ? O1 Zn1 N2 111.7(3) . 9_655 ? N1 Zn1 N2 102.5(3) . 9_655 ? O1 Zn1 N4 97.9(3) . . ? N1 Zn1 N4 115.7(3) . . ? N2 Zn1 N4 116.0(3) 9_655 . ? O1 Zn1 Li1 48.7(3) . 9_655 ? N1 Zn1 Li1 139.7(3) . 9_655 ? N2 Zn1 Li1 117.6(4) 9_655 9_655 ? N4 Zn1 Li1 50.8(3) . 9_655 ? O1 Zn1 Li1 43.6(3) . . ? N1 Zn1 Li1 90.7(3) . . ? N2 Zn1 Li1 155.2(3) 9_655 . ? N4 Zn1 Li1 75.2(3) . . ? Li1 Zn1 Li1 50.7(5) 9_655 . ? O1 Zn1 Zn1 39.32(13) . 9_655 ? N1 Zn1 Zn1 131.8(2) . 9_655 ? N2 Zn1 Zn1 73.2(2) 9_655 9_655 ? N4 Zn1 Zn1 108.4(2) . 9_655 ? Li1 Zn1 Zn1 62.4(3) 9_655 9_655 ? Li1 Zn1 Zn1 82.3(2) . 9_655 ? O1 Zn1 Zn1 39.32(13) . 11_564 ? N1 Zn1 Zn1 77.2(2) . 11_564 ? N2 Zn1 Zn1 107.5(2) 9_655 11_564 ? N4 Zn1 Zn1 129.0(2) . 11_564 ? Li1 Zn1 Zn1 86.4(2) 9_655 11_564 ? Li1 Zn1 Zn1 54.7(2) . 11_564 ? Zn1 Zn1 Zn1 60.0 9_655 11_564 ? Zn1 O1 Zn1 101.4(3) . 9_655 ? Zn1 O1 Zn1 101.4(3) . 11_564 ? Zn1 O1 Zn1 101.4(3) 9_655 11_564 ? Zn1 O1 Li1 158.8(5) . 11_564 ? Zn1 O1 Li1 86.5(3) 9_655 11_564 ? Zn1 O1 Li1 96.2(4) 11_564 11_564 ? Zn1 O1 Li1 86.5(3) . 9_655 ? Zn1 O1 Li1 96.2(4) 9_655 9_655 ? Zn1 O1 Li1 158.8(5) 11_564 9_655 ? Li1 O1 Li1 73.0(6) 11_564 9_655 ? Zn1 O1 Li1 96.2(4) . . ? Zn1 O1 Li1 158.8(5) 9_655 . ? Zn1 O1 Li1 86.5(3) 11_564 . ? Li1 O1 Li1 73.0(6) 11_564 . ? Li1 O1 Li1 73.0(6) 9_655 . ? C5 N1 C1 119.1(7) . . ? C5 N1 Zn1 123.6(5) . . ? C1 N1 Zn1 117.0(6) . . ? C2 C1 N1 122.2(10) . . ? O2 Li1 N3 108.7(6) . . ? O2 Li1 O1 86.2(6) . . ? N3 Li1 O1 108.0(6) . . ? O2 Li1 N4 123.0(7) . 11_564 ? N3 Li1 N4 125.9(7) . 11_564 ? O1 Li1 N4 91.2(5) . 11_564 ? O2 Li1 Li1 48.1(3) . 11_564 ? N3 Li1 Li1 145.5(7) . 11_564 ? O1 Li1 Li1 53.5(3) . 11_564 ? N4 Li1 Li1 86.3(7) 11_564 11_564 ? O2 Li1 Li1 48.1(3) . 9_655 ? N3 Li1 Li1 85.5(7) . 9_655 ? O1 Li1 Li1 53.5(3) . 9_655 ? N4 Li1 Li1 140.7(6) 11_564 9_655 ? Li1 Li1 Li1 60.000(1) 11_564 9_655 ? O2 Li1 Zn1 117.3(6) . 11_564 ? N3 Li1 Zn1 120.6(6) . 11_564 ? O1 Li1 Zn1 44.8(3) . 11_564 ? N4 Li1 Zn1 47.8(3) 11_564 11_564 ? Li1 Li1 Zn1 69.6(4) 11_564 11_564 ? Li1 Li1 Zn1 98.1(3) 9_655 11_564 ? O2 Li1 Zn1 107.4(5) . . ? N3 Li1 Zn1 69.0(4) . . ? O1 Li1 Zn1 40.2(2) . . ? N4 Li1 Zn1 106.2(5) 11_564 . ? Li1 Li1 Zn1 92.2(2) 11_564 . ? Li1 Li1 Zn1 59.7(3) 9_655 . ? Zn1 Li1 Zn1 62.9(3) 11_564 . ? C5 N2 C6 115.9(7) . . ? C5 N2 Zn1 119.1(6) . 11_564 ? C6 N2 Zn1 109.6(7) . 11_564 ? C1 C2 C3 117.2(11) . . ? C13 O2 Li1 129.6(4) . . ? C13 O2 Li1 129.6(4) . 11_564 ? Li1 O2 Li1 83.7(7) . 11_564 ? C13 O2 Li1 129.6(4) . 9_655 ? Li1 O2 Li1 83.7(7) . 9_655 ? Li1 O2 Li1 83.7(7) 11_564 9_655 ? C7 N3 C11 118.3(9) . . ? C7 N3 Li1 116.7(8) . . ? C11 N3 Li1 123.3(7) . . ? C4 C3 C2 122.5(11) . . ? C11 N4 C12 117.3(8) . . ? C11 N4 Zn1 108.7(6) . . ? C12 N4 Zn1 116.8(7) . . ? C11 N4 Li1 112.3(7) . 9_655 ? C12 N4 Li1 115.1(8) . 9_655 ? Zn1 N4 Li1 81.4(4) . 9_655 ? C3 C4 C5 120.0(11) . . ? N2 C5 N1 116.4(7) . . ? N2 C5 C4 124.6(8) . . ? N1 C5 C4 118.9(8) . . ? N3 C7 C8 121.6(14) . . ? C9 C8 C7 120.5(12) . . ? C10 C9 C8 120.5(12) . . ? C9 C10 C11 120.2(14) . . ? N4 C11 N3 115.4(7) . . ? N4 C11 C10 125.7(11) . . ? N3 C11 C10 118.7(10) . . ? O2 C13 C14 107.0(8) . 9_655 ? O2 C13 C14 107.0(8) . . ? C14 C13 C14 111.8(7) 9_655 . ? O2 C13 C14 107.0(8) . 11_564 ? C14 C13 C14 111.8(7) 9_655 11_564 ? C14 C13 C14 111.8(7) . 11_564 ? C20 O3 C23 107(3) . . ? C21 C20 O3 106(2) . . ? C22 C21 C20 108.8(17) . . ? C21 C22 C23 107.3(18) . . ? C22 C23 O3 105(2) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 22.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.913 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.325