# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Matthias Driess' _publ_contact_author_email MATTHIAS.DRIESS@TU-BERLIN.DE _publ_section_title ; One-pot synthesis of lithium alkylzinc alkoxo heterocubanes with a LiZn3O4 core as suitable organometallic precursors for Li-containing ZnO nanocrystals ; loop_ _publ_author_name 'Matthias Driess' 'Yilmaz Aksu' 'Surajit Jana' # Attachment 'JANA23.CIF' data_jana23 _database_code_depnum_ccdc_archive 'CCDC 703246' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H45 Li O5 Zn3' _chemical_formula_weight 556.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.9460(4) _cell_length_b 17.7288(5) _cell_length_c 18.2916(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5495.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7186 _cell_measurement_theta_min 3.1969 _cell_measurement_theta_max 28.9569 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2336 _exptl_absorpt_coefficient_mu 2.619 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5605 _exptl_absorpt_correction_T_max 0.6947 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28361 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0769 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.20 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4828 _reflns_number_gt 2723 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0275P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4828 _refine_ls_number_parameters 264 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0627 _refine_ls_R_factor_gt 0.0291 _refine_ls_wR_factor_ref 0.0620 _refine_ls_wR_factor_gt 0.0557 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.62785(2) 0.25211(2) 0.72456(2) 0.03696(13) Uani 1 1 d . . . Zn2 Zn 0.51757(2) 0.17447(2) 0.61385(2) 0.03168(12) Uani 1 1 d . . . Zn3 Zn 0.57133(2) 0.08917(2) 0.75010(2) 0.03059(11) Uani 1 1 d . . . Li1 Li 0.6768(3) 0.1316(3) 0.6346(3) 0.0359(15) Uani 1 1 d . . . O1 O 0.57499(11) 0.07761(12) 0.63961(11) 0.0274(6) Uani 1 1 d . . . O2 O 0.67478(10) 0.14648(12) 0.74060(11) 0.0304(6) Uani 1 1 d . . . O3 O 0.62397(11) 0.22758(12) 0.61571(12) 0.0320(6) Uani 1 1 d . . . O4 O 0.52113(11) 0.19412(11) 0.72574(11) 0.0282(6) Uani 1 1 d . . . C1 C 0.6639(2) 0.3437(2) 0.7738(2) 0.0643(13) Uani 1 1 d . . . H1A H 0.7217 0.3462 0.7719 0.096 Uiso 1 1 calc R . . H1B H 0.6466 0.3429 0.8249 0.096 Uiso 1 1 calc R . . H1C H 0.6416 0.3880 0.7493 0.096 Uiso 1 1 calc R . . C2 C 0.43152(18) 0.1846(2) 0.54307(19) 0.0514(11) Uani 1 1 d . . . H2A H 0.3980 0.2274 0.5568 0.077 Uiso 1 1 calc R . . H2B H 0.3999 0.1383 0.5428 0.077 Uiso 1 1 calc R . . H2C H 0.4535 0.1932 0.4942 0.077 Uiso 1 1 calc R . . C3 C 0.5289(2) 0.0201(2) 0.82423(19) 0.0489(11) Uani 1 1 d . . . H3A H 0.5601 -0.0264 0.8246 0.073 Uiso 1 1 calc R . . H3B H 0.4739 0.0082 0.8126 0.073 Uiso 1 1 calc R . . H3C H 0.5317 0.0441 0.8724 0.073 Uiso 1 1 calc R . . C4 C 0.56187(18) 0.00693(19) 0.60400(19) 0.0332(9) Uani 1 1 d . . . H4 H 0.5678 0.0149 0.5502 0.040 Uiso 1 1 calc R . . C5 C 0.6232(2) -0.04971(19) 0.6279(2) 0.0514(11) Uani 1 1 d . . . H5A H 0.6760 -0.0292 0.6189 0.077 Uiso 1 1 calc R . . H5B H 0.6164 -0.0966 0.6002 0.077 Uiso 1 1 calc R . . H5C H 0.6169 -0.0601 0.6802 0.077 Uiso 1 1 calc R . . C6 C 0.47856(19) -0.0214(2) 0.6183(2) 0.0489(10) Uani 1 1 d . . . H6A H 0.4721 -0.0316 0.6706 0.073 Uiso 1 1 calc R . . H6B H 0.4695 -0.0679 0.5905 0.073 Uiso 1 1 calc R . . H6C H 0.4404 0.0170 0.6030 0.073 Uiso 1 1 calc R . . C7 C 0.7374(2) 0.1369(2) 0.7922(2) 0.0472(11) Uani 1 1 d . . . H7 H 0.7797 0.1743 0.7803 0.057 Uiso 1 1 calc R . . C8 C 0.7717(2) 0.0588(3) 0.7840(2) 0.0710(14) Uani 1 1 d . . . H8A H 0.7312 0.0212 0.7954 0.106 Uiso 1 1 calc R . . H8B H 0.8163 0.0528 0.8176 0.106 Uiso 1 1 calc R . . H8C H 0.7898 0.0517 0.7336 0.106 Uiso 1 1 calc R . . C9 C 0.7095(2) 0.1521(3) 0.8687(2) 0.0772(15) Uani 1 1 d . . . H9A H 0.6892 0.2038 0.8719 0.116 Uiso 1 1 calc R . . H9B H 0.7536 0.1459 0.9028 0.116 Uiso 1 1 calc R . . H9C H 0.6674 0.1165 0.8813 0.116 Uiso 1 1 calc R . . C10 C 0.6447(2) 0.2823(2) 0.5617(2) 0.0447(10) Uani 1 1 d . . . H10 H 0.6412 0.2579 0.5126 0.054 Uiso 1 1 calc R . . C11 C 0.5877(2) 0.3483(2) 0.5634(3) 0.0729(14) Uani 1 1 d . . . H11A H 0.5339 0.3299 0.5553 0.109 Uiso 1 1 calc R . . H11B H 0.6017 0.3843 0.5248 0.109 Uiso 1 1 calc R . . H11C H 0.5907 0.3733 0.6111 0.109 Uiso 1 1 calc R . . C12 C 0.72874(19) 0.3082(2) 0.5733(2) 0.0623(13) Uani 1 1 d . . . H12A H 0.7339 0.3304 0.6221 0.094 Uiso 1 1 calc R . . H12B H 0.7424 0.3459 0.5363 0.094 Uiso 1 1 calc R . . H12C H 0.7644 0.2649 0.5690 0.094 Uiso 1 1 calc R . . C13 C 0.45318(18) 0.2203(2) 0.7656(2) 0.0362(10) Uani 1 1 d . . . H13 H 0.4117 0.1803 0.7634 0.043 Uiso 1 1 calc R . . C14 C 0.4205(2) 0.2905(2) 0.7313(2) 0.0576(12) Uani 1 1 d . . . H14A H 0.4593 0.3312 0.7353 0.086 Uiso 1 1 calc R . . H14B H 0.3719 0.3052 0.7566 0.086 Uiso 1 1 calc R . . H14C H 0.4089 0.2808 0.6797 0.086 Uiso 1 1 calc R . . C15 C 0.4745(2) 0.2331(2) 0.84535(19) 0.0508(11) Uani 1 1 d . . . H15A H 0.4981 0.1871 0.8655 0.076 Uiso 1 1 calc R . . H15B H 0.4268 0.2457 0.8730 0.076 Uiso 1 1 calc R . . H15C H 0.5124 0.2747 0.8490 0.076 Uiso 1 1 calc R . . O5 O 0.75317(12) 0.09806(15) 0.56407(14) 0.0489(7) Uani 1 1 d . . . C16 C 0.7341(2) 0.0952(3) 0.4885(2) 0.0830(17) Uani 1 1 d . . . H16A H 0.6998 0.0511 0.4786 0.100 Uiso 1 1 calc R . . H16B H 0.7051 0.1413 0.4742 0.100 Uiso 1 1 calc R . . C17 C 0.8045(3) 0.0893(4) 0.4479(3) 0.131(2) Uani 1 1 d . . . H17A H 0.8134 0.1360 0.4194 0.157 Uiso 1 1 calc R . . H17B H 0.8012 0.0464 0.4134 0.157 Uiso 1 1 calc R . . C18 C 0.8693(3) 0.0776(3) 0.4993(3) 0.0861(17) Uani 1 1 d . . . H18A H 0.9077 0.1196 0.4963 0.103 Uiso 1 1 calc R . . H18B H 0.8971 0.0298 0.4884 0.103 Uiso 1 1 calc R . . C19 C 0.83304(19) 0.0746(2) 0.5730(2) 0.0613(13) Uani 1 1 d . . . H19A H 0.8353 0.0227 0.5928 0.074 Uiso 1 1 calc R . . H19B H 0.8611 0.1088 0.6070 0.074 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 Zn1 0.0317(2) 0.0366(3) 0.0426(3) -0.0090(2) 0.00381(19) -0.0049(2) Zn2 0.0300(2) 0.0347(3) 0.0303(2) 0.0012(2) -0.00175(19) 0.0012(2) Zn3 0.0297(2) 0.0343(3) 0.0277(2) 0.0003(2) 0.00138(19) 0.00088(19) Li1 0.032(3) 0.043(4) 0.033(4) -0.004(3) 0.004(3) 0.002(3) O1 0.0274(12) 0.0265(15) 0.0283(14) -0.0050(11) 0.0008(10) 0.0001(11) O2 0.0201(11) 0.0438(15) 0.0273(15) -0.0027(12) -0.0039(10) 0.0023(11) O3 0.0304(13) 0.0341(16) 0.0316(15) 0.0049(12) 0.0044(11) -0.0034(11) O4 0.0226(11) 0.0319(14) 0.0300(15) -0.0043(11) 0.0041(10) 0.0008(10) C1 0.054(2) 0.058(3) 0.082(4) -0.027(3) 0.009(2) -0.012(2) C2 0.046(2) 0.067(3) 0.041(3) -0.001(2) -0.0073(19) 0.003(2) C3 0.053(2) 0.048(3) 0.046(3) 0.007(2) 0.006(2) 0.001(2) C4 0.042(2) 0.026(2) 0.032(2) -0.0081(19) 0.0006(18) -0.0011(18) C5 0.057(3) 0.031(2) 0.066(3) -0.006(2) 0.004(2) 0.009(2) C6 0.052(2) 0.043(3) 0.052(3) -0.009(2) -0.001(2) -0.018(2) C7 0.030(2) 0.068(3) 0.043(3) 0.001(2) -0.0088(19) -0.003(2) C8 0.049(3) 0.095(4) 0.069(3) 0.014(3) -0.016(2) 0.025(3) C9 0.061(3) 0.128(5) 0.042(3) -0.014(3) -0.015(2) 0.007(3) C10 0.047(2) 0.049(3) 0.038(3) 0.012(2) 0.0059(19) -0.004(2) C11 0.080(3) 0.042(3) 0.096(4) 0.029(3) 0.005(3) 0.000(2) C12 0.053(3) 0.070(4) 0.064(3) 0.010(3) 0.012(2) -0.028(2) C13 0.0263(19) 0.035(2) 0.047(3) -0.011(2) 0.0085(18) 0.0029(16) C14 0.050(2) 0.058(3) 0.065(3) -0.010(2) 0.005(2) 0.023(2) C15 0.048(2) 0.061(3) 0.043(3) -0.017(2) 0.018(2) 0.002(2) O5 0.0291(14) 0.079(2) 0.0382(17) -0.0043(16) 0.0057(12) 0.0101(13) C16 0.065(3) 0.142(5) 0.042(3) -0.012(3) 0.003(2) 0.017(3) C17 0.091(4) 0.238(8) 0.063(4) -0.029(5) 0.028(4) -0.003(5) C18 0.059(3) 0.114(5) 0.085(4) -0.001(3) 0.033(3) 0.018(3) C19 0.035(2) 0.091(4) 0.058(3) -0.011(3) 0.009(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C1 1.955(4) . ? Zn1 O3 2.039(2) . ? Zn1 O2 2.056(2) . ? Zn1 O4 2.0804(19) . ? Zn1 Li1 2.821(6) . ? Zn1 Zn3 3.0790(6) . ? Zn1 Zn2 3.0803(5) . ? Zn2 C2 1.958(3) . ? Zn2 O1 2.029(2) . ? Zn2 O3 2.0345(19) . ? Zn2 O4 2.077(2) . ? Zn2 Li1 2.828(5) . ? Zn2 Zn3 3.0542(6) . ? Zn3 C3 1.963(3) . ? Zn3 O1 2.032(2) . ? Zn3 O2 2.0336(19) . ? Zn3 O4 2.094(2) . ? Zn3 Li1 2.867(5) . ? Li1 O5 1.923(6) . ? Li1 O3 1.953(6) . ? Li1 O2 1.956(6) . ? Li1 O1 1.975(6) . ? O1 C4 1.430(4) . ? O2 C7 1.431(4) . ? O3 C10 1.428(4) . ? O4 C13 1.440(3) . ? C4 C5 1.510(4) . ? C4 C6 1.521(4) . ? C7 C9 1.501(5) . ? C7 C8 1.510(5) . ? C10 C12 1.511(4) . ? C10 C11 1.517(5) . ? C13 C14 1.498(5) . ? C13 C15 1.519(4) . ? O5 C16 1.420(4) . ? O5 C19 1.425(4) . ? C16 C17 1.410(5) . ? C17 C18 1.461(6) . ? C18 C19 1.482(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 O3 129.59(14) . . ? C1 Zn1 O2 124.74(13) . . ? O3 Zn1 O2 87.56(8) . . ? C1 Zn1 O4 132.65(12) . . ? O3 Zn1 O4 82.92(8) . . ? O2 Zn1 O4 83.37(8) . . ? C1 Zn1 Li1 143.70(15) . . ? O3 Zn1 Li1 43.82(13) . . ? O2 Zn1 Li1 43.91(13) . . ? O4 Zn1 Li1 83.52(12) . . ? C1 Zn1 Zn3 143.76(13) . . ? O3 Zn1 Zn3 86.45(6) . . ? O2 Zn1 Zn3 40.88(5) . . ? O4 Zn1 Zn3 42.64(5) . . ? Li1 Zn1 Zn3 57.95(12) . . ? C1 Zn1 Zn2 149.76(12) . . ? O3 Zn1 Zn2 40.82(5) . . ? O2 Zn1 Zn2 85.49(6) . . ? O4 Zn1 Zn2 42.15(6) . . ? Li1 Zn1 Zn2 57.07(11) . . ? Zn3 Zn1 Zn2 59.455(13) . . ? C2 Zn2 O1 126.03(13) . . ? C2 Zn2 O3 128.95(13) . . ? O1 Zn2 O3 87.87(8) . . ? C2 Zn2 O4 131.13(12) . . ? O1 Zn2 O4 84.21(8) . . ? O3 Zn2 O4 83.11(8) . . ? C2 Zn2 Li1 145.47(16) . . ? O1 Zn2 Li1 44.28(14) . . ? O3 Zn2 Li1 43.67(14) . . ? O4 Zn2 Li1 83.39(12) . . ? C2 Zn2 Zn3 143.81(11) . . ? O1 Zn2 Zn3 41.28(6) . . ? O3 Zn2 Zn3 87.19(6) . . ? O4 Zn2 Zn3 43.14(6) . . ? Li1 Zn2 Zn3 58.18(12) . . ? C2 Zn2 Zn1 147.72(12) . . ? O1 Zn2 Zn1 86.25(6) . . ? O3 Zn2 Zn1 40.92(6) . . ? O4 Zn2 Zn1 42.23(5) . . ? Li1 Zn2 Zn1 56.84(12) . . ? Zn3 Zn2 Zn1 60.251(13) . . ? C3 Zn3 O1 129.44(12) . . ? C3 Zn3 O2 133.32(12) . . ? O1 Zn3 O2 86.51(8) . . ? C3 Zn3 O4 123.54(12) . . ? O1 Zn3 O4 83.70(8) . . ? O2 Zn3 O4 83.57(8) . . ? C3 Zn3 Li1 154.25(16) . . ? O1 Zn3 Li1 43.52(13) . . ? O2 Zn3 Li1 43.01(13) . . ? O4 Zn3 Li1 82.14(13) . . ? C3 Zn3 Zn2 139.76(10) . . ? O1 Zn3 Zn2 41.20(6) . . ? O2 Zn3 Zn2 86.56(6) . . ? O4 Zn3 Zn2 42.71(6) . . ? Li1 Zn3 Zn2 56.96(11) . . ? C3 Zn3 Zn1 143.48(11) . . ? O1 Zn3 Zn1 86.23(6) . . ? O2 Zn3 Zn1 41.42(6) . . ? O4 Zn3 Zn1 42.30(5) . . ? Li1 Zn3 Zn1 56.50(12) . . ? Zn2 Zn3 Zn1 60.295(13) . . ? O5 Li1 O3 117.3(3) . . ? O5 Li1 O2 135.9(3) . . ? O3 Li1 O2 92.9(3) . . ? O5 Li1 O1 118.0(3) . . ? O3 Li1 O1 91.8(2) . . ? O2 Li1 O1 90.3(2) . . ? O5 Li1 Zn1 145.5(3) . . ? O3 Li1 Zn1 46.29(14) . . ? O2 Li1 Zn1 46.78(14) . . ? O1 Li1 Zn1 94.8(2) . . ? O5 Li1 Zn2 129.4(3) . . ? O3 Li1 Zn2 46.00(12) . . ? O2 Li1 Zn2 94.6(2) . . ? O1 Li1 Zn2 45.85(12) . . ? Zn1 Li1 Zn2 66.09(12) . . ? O5 Li1 Zn3 146.4(3) . . ? O3 Li1 Zn3 94.2(2) . . ? O2 Li1 Zn3 45.16(13) . . ? O1 Li1 Zn3 45.14(13) . . ? Zn1 Li1 Zn3 65.55(12) . . ? Zn2 Li1 Zn3 64.86(11) . . ? C4 O1 Li1 122.7(2) . . ? C4 O1 Zn2 124.15(18) . . ? Li1 O1 Zn2 89.87(19) . . ? C4 O1 Zn3 122.46(19) . . ? Li1 O1 Zn3 91.34(18) . . ? Zn2 O1 Zn3 97.53(9) . . ? C7 O2 Li1 128.7(2) . . ? C7 O2 Zn3 121.6(2) . . ? Li1 O2 Zn3 91.84(18) . . ? C7 O2 Zn1 119.3(2) . . ? Li1 O2 Zn1 89.31(19) . . ? Zn3 O2 Zn1 97.69(8) . . ? C10 O3 Li1 127.0(2) . . ? C10 O3 Zn2 121.40(19) . . ? Li1 O3 Zn2 90.32(18) . . ? C10 O3 Zn1 121.5(2) . . ? Li1 O3 Zn1 89.89(19) . . ? Zn2 O3 Zn1 98.26(9) . . ? C13 O4 Zn2 122.02(18) . . ? C13 O4 Zn1 122.72(18) . . ? Zn2 O4 Zn1 95.62(8) . . ? C13 O4 Zn3 120.25(19) . . ? Zn2 O4 Zn3 94.16(8) . . ? Zn1 O4 Zn3 95.06(8) . . ? O1 C4 C5 110.1(3) . . ? O1 C4 C6 110.8(3) . . ? C5 C4 C6 111.7(3) . . ? O2 C7 C9 111.1(3) . . ? O2 C7 C8 109.1(3) . . ? C9 C7 C8 112.2(4) . . ? O3 C10 C12 110.0(3) . . ? O3 C10 C11 110.7(3) . . ? C12 C10 C11 111.3(3) . . ? O4 C13 C14 110.5(3) . . ? O4 C13 C15 110.1(3) . . ? C14 C13 C15 111.5(3) . . ? C16 O5 C19 108.5(3) . . ? C16 O5 Li1 120.7(3) . . ? C19 O5 Li1 130.8(3) . . ? C17 C16 O5 108.8(4) . . ? C16 C17 C18 107.9(4) . . ? C17 C18 C19 106.2(3) . . ? O5 C19 C18 106.2(3) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.402 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.068 # Attachment 'compound2.CIF' data_compound2 _database_code_depnum_ccdc_archive 'CCDC 703247' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H53 Li O5 Zn3' _chemical_formula_weight 612.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 orthorhombic _symmetry_space_group_name_H-M Pccn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 20.6243(4) _cell_length_b 18.2357(4) _cell_length_c 16.3338(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6143.1(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 9919 _cell_measurement_theta_min 2.9750 _cell_measurement_theta_max 28.8379 _exptl_crystal_description 'transparent plates' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 2.350 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7195 _exptl_absorpt_correction_T_max 0.7990 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET) (compiled Jan 12 2007,17:49:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28304 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0417 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5406 _reflns_number_gt 3672 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET) (compiled May 8 2007,13:10:02) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0305P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5406 _refine_ls_number_parameters 323 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0520 _refine_ls_R_factor_gt 0.0271 _refine_ls_wR_factor_ref 0.0659 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.544170(14) 0.077637(17) 0.760637(19) 0.02159(9) Uani 1 1 d . . . Zn2 Zn 0.691984(14) 0.079656(18) 0.77028(2) 0.02489(10) Uani 1 1 d . . . Zn3 Zn 0.624442(15) -0.018750(17) 0.645886(19) 0.02535(10) Uani 1 1 d . . . O1 O 0.68773(8) -0.02942(10) 0.74123(11) 0.0224(4) Uani 1 1 d . . . O2 O 0.55170(8) -0.03064(9) 0.72961(10) 0.0213(4) Uani 1 1 d . . . O3 O 0.61507(8) 0.06189(10) 0.84606(10) 0.0228(4) Uani 1 1 d . . . O4 O 0.62082(8) 0.09170(9) 0.68046(11) 0.0220(4) Uani 1 1 d . . . Li1 Li 0.6158(2) -0.0458(3) 0.8191(3) 0.0281(11) Uani 1 1 d . . . O5 O 0.61420(10) -0.12863(11) 0.89952(12) 0.0411(6) Uani 1 1 d . C . C16 C 0.62098(14) 0.15037(15) 0.62051(17) 0.0290(7) Uani 1 1 d . . . C8 C 0.49381(13) -0.07191(16) 0.71008(17) 0.0273(7) Uani 1 1 d . . . C4 C 0.74604(14) -0.07160(16) 0.73343(18) 0.0322(7) Uani 1 1 d . . . C10 C 0.45637(14) -0.03226(16) 0.64367(18) 0.0360(8) Uani 1 1 d . . . H10A H 0.4424 0.0158 0.6640 0.054 Uiso 1 1 calc R . . H10B H 0.4182 -0.0613 0.6284 0.054 Uiso 1 1 calc R . . H10C H 0.4842 -0.0256 0.5956 0.054 Uiso 1 1 calc R . . C11 C 0.45437(14) -0.07780(18) 0.78835(18) 0.0393(8) Uani 1 1 d . . . H11A H 0.4796 -0.1039 0.8299 0.059 Uiso 1 1 calc R . . H11B H 0.4142 -0.1047 0.7773 0.059 Uiso 1 1 calc R . . H11C H 0.4439 -0.0285 0.8083 0.059 Uiso 1 1 calc R . . C12 C 0.61168(13) 0.09940(17) 0.92350(17) 0.0318(8) Uani 1 1 d . . . C17 C 0.61508(14) 0.22328(15) 0.66482(19) 0.0386(8) Uani 1 1 d . . . H17A H 0.5748 0.2241 0.6966 0.058 Uiso 1 1 calc R . . H17B H 0.6145 0.2632 0.6247 0.058 Uiso 1 1 calc R . . H17C H 0.6521 0.2296 0.7017 0.058 Uiso 1 1 calc R . . C9 C 0.51371(15) -0.14721(16) 0.6796(2) 0.0427(9) Uani 1 1 d . . . H9A H 0.5387 -0.1421 0.6289 0.064 Uiso 1 1 calc R . . H9B H 0.4749 -0.1767 0.6690 0.064 Uiso 1 1 calc R . . H9C H 0.5404 -0.1715 0.7212 0.064 Uiso 1 1 calc R . . C5 C 0.78813(14) -0.03794(18) 0.66623(19) 0.0454(9) Uani 1 1 d . . . H5A H 0.7636 -0.0365 0.6148 0.068 Uiso 1 1 calc R . . H5B H 0.8272 -0.0677 0.6588 0.068 Uiso 1 1 calc R . . H5C H 0.8005 0.0120 0.6819 0.068 Uiso 1 1 calc R . . C19 C 0.56299(15) 0.13886(17) 0.56394(18) 0.0401(8) Uani 1 1 d . . . H19A H 0.5664 0.0908 0.5375 0.060 Uiso 1 1 calc R . . H19B H 0.5624 0.1773 0.5220 0.060 Uiso 1 1 calc R . . H19C H 0.5229 0.1411 0.5960 0.060 Uiso 1 1 calc R . . C7 C 0.78182(14) -0.06914(19) 0.81551(19) 0.0440(9) Uani 1 1 d . . . H7A H 0.7915 -0.0181 0.8297 0.066 Uiso 1 1 calc R . . H7B H 0.8224 -0.0969 0.8112 0.066 Uiso 1 1 calc R . . H7C H 0.7545 -0.0909 0.8582 0.066 Uiso 1 1 calc R . . C1 C 0.46543(13) 0.13802(17) 0.77073(19) 0.0378(8) Uani 1 1 d . . . H1A H 0.4443 0.1420 0.7172 0.057 Uiso 1 1 calc R . . H1B H 0.4772 0.1870 0.7903 0.057 Uiso 1 1 calc R . . H1C H 0.4356 0.1150 0.8097 0.057 Uiso 1 1 calc R . . C3 C 0.63383(16) -0.05860(17) 0.53449(18) 0.0435(9) Uani 1 1 d . . . H3A H 0.6513 -0.1085 0.5375 0.065 Uiso 1 1 calc R . . H3B H 0.6635 -0.0275 0.5030 0.065 Uiso 1 1 calc R . . H3C H 0.5914 -0.0596 0.5076 0.065 Uiso 1 1 calc R . . C13 C 0.55102(15) 0.0732(2) 0.96662(18) 0.0532(10) Uani 1 1 d . . . H13A H 0.5129 0.0858 0.9336 0.080 Uiso 1 1 calc R . . H13B H 0.5478 0.0969 1.0203 0.080 Uiso 1 1 calc R . . H13C H 0.5531 0.0199 0.9738 0.080 Uiso 1 1 calc R . . C18 C 0.68360(14) 0.14678(18) 0.57213(19) 0.0466(9) Uani 1 1 d . . . H18A H 0.7204 0.1545 0.6090 0.070 Uiso 1 1 calc R . . H18B H 0.6834 0.1850 0.5299 0.070 Uiso 1 1 calc R . . H18C H 0.6874 0.0985 0.5461 0.070 Uiso 1 1 calc R . . C2 C 0.76890(14) 0.14035(17) 0.7883(2) 0.0475(9) Uani 1 1 d . . . H2A H 0.7557 0.1884 0.8094 0.071 Uiso 1 1 calc R . . H2B H 0.7921 0.1467 0.7364 0.071 Uiso 1 1 calc R . . H2C H 0.7974 0.1163 0.8281 0.071 Uiso 1 1 calc R . . C15 C 0.67169(15) 0.0812(2) 0.97308(19) 0.0485(9) Uani 1 1 d . . . H15A H 0.6751 0.0279 0.9795 0.073 Uiso 1 1 calc R . . H15B H 0.6686 0.1042 1.0271 0.073 Uiso 1 1 calc R . . H15C H 0.7102 0.0996 0.9446 0.073 Uiso 1 1 calc R . . C14 C 0.60913(15) 0.18249(17) 0.9091(2) 0.0466(9) Uani 1 1 d . . . H14A H 0.6477 0.1979 0.8785 0.070 Uiso 1 1 calc R . . H14B H 0.6080 0.2079 0.9619 0.070 Uiso 1 1 calc R . . H14C H 0.5701 0.1947 0.8776 0.070 Uiso 1 1 calc R . . C6 C 0.72900(16) -0.15007(16) 0.7119(2) 0.0476(9) Uani 1 1 d . . . H6A H 0.7029 -0.1715 0.7560 0.071 Uiso 1 1 calc R . . H6B H 0.7689 -0.1786 0.7051 0.071 Uiso 1 1 calc R . . H6C H 0.7042 -0.1509 0.6608 0.071 Uiso 1 1 calc R . . C23 C 0.64123(18) -0.1275(2) 0.9808(2) 0.0579(10) Uani 1 1 d . . . H23A H 0.6817 -0.0983 0.9826 0.069 Uiso 1 1 calc R A 1 H23B H 0.6100 -0.1072 1.0208 0.069 Uiso 1 1 calc R A 1 C20 C 0.5935(2) -0.2031(2) 0.8825(3) 0.0718(13) Uani 1 1 d . . . H20A H 0.5470 -0.2093 0.8959 0.086 Uiso 1 1 calc R B 1 H20B H 0.5999 -0.2149 0.8239 0.086 Uiso 1 1 calc R B 1 C22 C 0.6538(13) -0.2036(18) 0.9966(14) 0.060(7) Uani 0.36(2) 1 d P C 1 H22A H 0.7010 -0.2105 1.0046 0.071 Uiso 0.36(2) 1 calc PR C 1 H22B H 0.6318 -0.2179 1.0481 0.071 Uiso 0.36(2) 1 calc PR C 1 C21 C 0.6327(12) -0.2500(5) 0.9330(9) 0.122(7) Uani 0.64(2) 1 d P C 1 H21A H 0.6069 -0.2914 0.9549 0.146 Uiso 0.64(2) 1 calc PR C 1 H21B H 0.6699 -0.2698 0.9018 0.146 Uiso 0.64(2) 1 calc PR C 1 C22A C 0.6339(10) -0.2044(12) 1.0167(10) 0.101(6) Uani 0.64(2) 1 d P C 2 H22C H 0.6747 -0.2324 1.0112 0.121 Uiso 0.64(2) 1 calc PR C 2 H22D H 0.6220 -0.2019 1.0753 0.121 Uiso 0.64(2) 1 calc PR C 2 C21A C 0.5868(10) -0.2354(9) 0.9733(13) 0.056(6) Uani 0.36(2) 1 d P C 2 H21C H 0.5439 -0.2231 0.9968 0.067 Uiso 0.36(2) 1 calc PR C 2 H21D H 0.5918 -0.2894 0.9730 0.067 Uiso 0.36(2) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.01934(18) 0.02090(19) 0.02452(19) -0.00195(16) -0.00035(14) -0.00034(13) Zn2 0.01933(19) 0.0218(2) 0.0336(2) -0.00062(17) 0.00088(14) -0.00234(13) Zn3 0.0333(2) 0.02201(18) 0.02078(18) -0.00195(15) 0.00113(15) 0.00256(15) O1 0.0218(11) 0.0179(11) 0.0276(11) -0.0002(9) 0.0010(8) 0.0050(8) O2 0.0197(11) 0.0190(11) 0.0251(11) -0.0030(9) -0.0058(8) -0.0047(7) O3 0.0229(11) 0.0270(11) 0.0186(10) -0.0050(8) -0.0004(8) -0.0024(8) O4 0.0253(11) 0.0205(10) 0.0201(10) 0.0037(8) 0.0043(8) 0.0020(8) Li1 0.030(3) 0.031(3) 0.023(3) 0.008(2) -0.007(2) 0.004(2) O5 0.0598(15) 0.0293(13) 0.0344(13) 0.0119(11) -0.0085(11) -0.0075(11) C16 0.0359(18) 0.0225(16) 0.0287(17) 0.0110(13) 0.0028(15) 0.0009(14) C8 0.0262(17) 0.0283(18) 0.0272(17) 0.0003(15) -0.0084(13) -0.0070(13) C4 0.0286(18) 0.0285(18) 0.0394(19) 0.0033(16) 0.0035(15) 0.0133(13) C10 0.0376(19) 0.035(2) 0.0357(19) -0.0017(16) -0.0180(15) -0.0028(14) C11 0.0325(19) 0.045(2) 0.0409(19) 0.0068(17) 0.0000(15) -0.0164(15) C12 0.036(2) 0.0392(19) 0.0205(17) -0.0097(14) -0.0047(14) -0.0004(14) C17 0.049(2) 0.0241(17) 0.043(2) 0.0071(15) -0.0010(16) -0.0023(14) C9 0.054(2) 0.0270(19) 0.047(2) -0.0048(17) -0.0149(17) -0.0101(15) C5 0.034(2) 0.053(2) 0.049(2) 0.0019(19) 0.0168(16) 0.0102(15) C19 0.056(2) 0.034(2) 0.0300(18) 0.0105(16) -0.0082(16) -0.0007(16) C7 0.0274(19) 0.055(2) 0.050(2) 0.0053(19) -0.0048(16) 0.0144(15) C1 0.0241(18) 0.0332(19) 0.056(2) -0.0040(17) 0.0000(15) 0.0006(13) C3 0.063(2) 0.035(2) 0.0325(19) -0.0077(16) 0.0018(16) 0.0080(16) C13 0.057(2) 0.077(3) 0.0260(19) -0.010(2) 0.0106(16) 0.003(2) C18 0.050(2) 0.042(2) 0.048(2) 0.0205(18) 0.0182(18) 0.0049(16) C2 0.029(2) 0.031(2) 0.083(3) 0.0001(19) -0.0016(17) -0.0069(14) C15 0.061(2) 0.053(2) 0.0308(19) -0.0014(19) -0.0207(17) -0.0048(18) C14 0.063(2) 0.033(2) 0.044(2) -0.0166(17) -0.0062(17) 0.0017(16) C6 0.050(2) 0.0240(19) 0.068(3) -0.0052(18) 0.0012(18) 0.0145(15) C23 0.071(3) 0.062(3) 0.041(2) 0.010(2) -0.007(2) -0.007(2) C20 0.103(3) 0.043(3) 0.069(3) 0.019(2) -0.025(2) -0.024(2) C22 0.082(12) 0.061(12) 0.035(12) 0.021(11) -0.029(11) 0.022(10) C21 0.243(19) 0.050(5) 0.073(8) 0.007(5) -0.070(10) 0.029(7) C22A 0.208(16) 0.052(7) 0.043(7) 0.018(5) 0.030(7) 0.015(10) C21A 0.082(11) 0.019(8) 0.067(11) 0.016(7) -0.028(8) -0.021(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 Zn1 C1 1.969(3) . ? Zn1 O3 2.0415(17) . ? Zn1 O2 2.0445(17) . ? Zn1 O4 2.0689(17) . ? Zn1 Li1 2.857(4) . ? Zn1 Zn2 3.0528(4) . ? Zn1 Zn3 3.0567(4) . ? Zn2 C2 1.957(3) . ? Zn2 O3 2.0380(17) . ? Zn2 O1 2.0468(18) . ? Zn2 O4 2.0868(17) . ? Zn2 Li1 2.887(5) . ? Zn2 Zn3 3.0478(4) . ? Zn3 C3 1.969(3) . ? Zn3 O1 2.0413(17) . ? Zn3 O2 2.0415(17) . ? Zn3 O4 2.0931(17) . ? Zn3 Li1 2.877(5) . ? O1 C4 1.433(3) . ? O1 Li1 1.976(5) . ? O2 C8 1.447(3) . ? O2 Li1 1.990(5) . ? O3 C12 1.440(3) . ? O3 Li1 2.013(5) . ? O4 C16 1.450(3) . ? Li1 O5 2.002(5) . ? O5 C23 1.440(4) . ? O5 C20 1.451(4) . ? C16 C18 1.516(4) . ? C16 C17 1.519(4) . ? C16 C19 1.526(4) . ? C8 C10 1.515(4) . ? C8 C9 1.517(4) . ? C8 C11 1.519(4) . ? C4 C6 1.515(4) . ? C4 C5 1.528(4) . ? C4 C7 1.531(4) . ? C12 C13 1.513(4) . ? C12 C15 1.516(4) . ? C12 C14 1.534(4) . ? C23 C22 1.44(3) . ? C23 C22A 1.53(2) . ? C20 C21 1.438(10) . ? C20 C21A 1.603(17) . ? C22 C21 1.41(3) . ? C22A C21A 1.33(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 C1 Zn1 O3 127.75(10) . . ? C1 Zn1 O2 128.57(10) . . ? O3 Zn1 O2 88.81(7) . . ? C1 Zn1 O4 127.87(10) . . ? O3 Zn1 O4 84.42(7) . . ? O2 Zn1 O4 84.53(7) . . ? C1 Zn1 Li1 147.07(13) . . ? O3 Zn1 Li1 44.79(11) . . ? O2 Zn1 Li1 44.15(11) . . ? O4 Zn1 Li1 85.05(10) . . ? C1 Zn1 Zn2 144.35(9) . . ? O3 Zn1 Zn2 41.51(5) . . ? O2 Zn1 Zn2 87.05(5) . . ? O4 Zn1 Zn2 42.95(5) . . ? Li1 Zn1 Zn2 58.38(9) . . ? C1 Zn1 Zn3 145.05(9) . . ? O3 Zn1 Zn3 87.15(5) . . ? O2 Zn1 Zn3 41.54(5) . . ? O4 Zn1 Zn3 43.05(5) . . ? Li1 Zn1 Zn3 58.10(10) . . ? Zn2 Zn1 Zn3 59.848(10) . . ? C2 Zn2 O3 129.02(11) . . ? C2 Zn2 O1 128.27(10) . . ? O3 Zn2 O1 87.30(7) . . ? C2 Zn2 O4 128.06(11) . . ? O3 Zn2 O4 84.05(7) . . ? O1 Zn2 O4 84.79(7) . . ? C2 Zn2 Li1 147.97(13) . . ? O3 Zn2 Li1 44.20(11) . . ? O1 Zn2 Li1 43.15(11) . . ? O4 Zn2 Li1 83.97(10) . . ? C2 Zn2 Zn3 143.51(10) . . ? O3 Zn2 Zn3 87.45(5) . . ? O1 Zn2 Zn3 41.73(5) . . ? O4 Zn2 Zn3 43.27(5) . . ? Li1 Zn2 Zn3 57.91(10) . . ? C2 Zn2 Zn1 145.51(9) . . ? O3 Zn2 Zn1 41.60(5) . . ? O1 Zn2 Zn1 86.19(5) . . ? O4 Zn2 Zn1 42.50(5) . . ? Li1 Zn2 Zn1 57.42(9) . . ? Zn3 Zn2 Zn1 60.139(10) . . ? C3 Zn3 O1 127.37(10) . . ? C3 Zn3 O2 130.70(11) . . ? O1 Zn3 O2 87.06(7) . . ? C3 Zn3 O4 127.45(11) . . ? O1 Zn3 O4 84.76(7) . . ? O2 Zn3 O4 83.99(7) . . ? C3 Zn3 Li1 148.36(14) . . ? O1 Zn3 Li1 43.36(10) . . ? O2 Zn3 Li1 43.77(10) . . ? O4 Zn3 Li1 84.13(11) . . ? C3 Zn3 Zn2 142.04(10) . . ? O1 Zn3 Zn2 41.87(5) . . ? O2 Zn3 Zn2 87.24(5) . . ? O4 Zn3 Zn2 43.10(5) . . ? Li1 Zn3 Zn2 58.25(10) . . ? C3 Zn3 Zn1 146.32(9) . . ? O1 Zn3 Zn1 86.18(5) . . ? O2 Zn3 Zn1 41.61(5) . . ? O4 Zn3 Zn1 42.43(5) . . ? Li1 Zn3 Zn1 57.48(9) . . ? Zn2 Zn3 Zn1 60.013(10) . . ? C4 O1 Li1 127.3(2) . . ? C4 O1 Zn3 121.32(16) . . ? Li1 O1 Zn3 91.46(15) . . ? C4 O1 Zn2 120.41(16) . . ? Li1 O1 Zn2 91.73(16) . . ? Zn3 O1 Zn2 96.41(7) . . ? C8 O2 Li1 129.6(2) . . ? C8 O2 Zn3 120.93(15) . . ? Li1 O2 Zn3 91.04(15) . . ? C8 O2 Zn1 119.62(15) . . ? Li1 O2 Zn1 90.16(16) . . ? Zn3 O2 Zn1 96.85(7) . . ? C12 O3 Li1 131.0(2) . . ? C12 O3 Zn2 119.73(15) . . ? Li1 O3 Zn2 90.91(15) . . ? C12 O3 Zn1 119.93(15) . . ? Li1 O3 Zn1 89.61(14) . . ? Zn2 O3 Zn1 96.89(7) . . ? C16 O4 Zn1 121.37(14) . . ? C16 O4 Zn2 123.42(15) . . ? Zn1 O4 Zn2 94.55(7) . . ? C16 O4 Zn3 121.85(15) . . ? Zn1 O4 Zn3 94.52(7) . . ? Zn2 O4 Zn3 93.63(7) . . ? O1 Li1 O2 90.3(2) . . ? O1 Li1 O5 123.3(2) . . ? O2 Li1 O5 125.1(3) . . ? O1 Li1 O3 90.0(2) . . ? O2 Li1 O3 91.1(2) . . ? O5 Li1 O3 126.3(3) . . ? O1 Li1 Zn1 93.10(17) . . ? O2 Li1 Zn1 45.69(11) . . ? O5 Li1 Zn1 143.6(2) . . ? O3 Li1 Zn1 45.60(10) . . ? O1 Li1 Zn3 45.18(11) . . ? O2 Li1 Zn3 45.20(11) . . ? O5 Li1 Zn3 140.9(2) . . ? O3 Li1 Zn3 92.78(17) . . ? Zn1 Li1 Zn3 64.42(10) . . ? O1 Li1 Zn2 45.12(11) . . ? O2 Li1 Zn2 92.79(17) . . ? O5 Li1 Zn2 142.0(2) . . ? O3 Li1 Zn2 44.89(11) . . ? Zn1 Li1 Zn2 64.20(10) . . ? Zn3 Li1 Zn2 63.84(10) . . ? C23 O5 C20 107.7(3) . . ? C23 O5 Li1 126.0(2) . . ? C20 O5 Li1 125.8(2) . . ? O4 C16 C18 108.8(2) . . ? O4 C16 C17 108.9(2) . . ? C18 C16 C17 110.8(2) . . ? O4 C16 C19 107.8(2) . . ? C18 C16 C19 110.3(3) . . ? C17 C16 C19 110.3(2) . . ? O2 C8 C10 109.3(2) . . ? O2 C8 C9 108.6(2) . . ? C10 C8 C9 109.6(2) . . ? O2 C8 C11 107.0(2) . . ? C10 C8 C11 111.3(2) . . ? C9 C8 C11 110.9(3) . . ? O1 C4 C6 109.4(2) . . ? O1 C4 C5 109.0(2) . . ? C6 C4 C5 110.2(3) . . ? O1 C4 C7 108.1(2) . . ? C6 C4 C7 110.0(3) . . ? C5 C4 C7 110.1(3) . . ? O3 C12 C13 107.4(2) . . ? O3 C12 C15 109.0(2) . . ? C13 C12 C15 110.9(3) . . ? O3 C12 C14 109.6(2) . . ? C13 C12 C14 110.8(3) . . ? C15 C12 C14 109.1(2) . . ? C22 C23 O5 102.9(10) . . ? C22 C23 C22A 20.2(15) . . ? O5 C23 C22A 107.6(8) . . ? C21 C20 O5 106.3(5) . . ? C21 C20 C21A 45.4(6) . . ? O5 C20 C21A 101.0(7) . . ? C21 C22 C23 113.0(13) . . ? C22 C21 C20 103.9(12) . . ? C21A C22A C23 105.0(12) . . ? C22A C21A C20 105.9(13) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.454 _refine_diff_density_min -0.399 _refine_diff_density_rms 0.066