# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hevia, Eva' _publ_contact_author_email eva.hevia@strath.ac.uk loop_ _publ_author_name S.Baillie V.Blair D.Blakemore D.Hay A.R.Kennedy D.Pryde ; E.Hevia ; data_savep21 _database_code_depnum_ccdc_archive 'CCDC 853494' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H88 Li2 N4 O4 Zn2' _chemical_formula_weight 905.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' O O 0.0106 0.0060 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.3706(4) _cell_length_b 16.5165(4) _cell_length_c 17.8453(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.038(3) _cell_angle_gamma 90.00 _cell_volume 4944.5(2) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 13335 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 30.35 _exptl_crystal_description chunk _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.217 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1960 _exptl_absorpt_coefficient_mu 1.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.65 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ; CrysAlisPro. Absorption correction using spherical harmonics implemented in SCALE3 ABSPACK scaling algorithm ; _exptl_special_details ; Crystals twinned. Initially gave cell twice as large. Both parts of twin indexed in CrysAlisPro and raw data processed to give an hklf 5 formated file. Matrice for 2nd twin -1 0 -0.5 0 -1 0 0 0 1 BASF refined to 0.32576 Final result presented is much superior to other treatments. Attempts to refine with an even smaller cell (with c halved) failed. Solution is completely disordered. ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Gemini S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 32501 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.71 _diffrn_reflns_theta_max 26.00 _reflns_number_total 32506 _reflns_number_gt 21835 _reflns_threshold_expression I>2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; One t-buty group treated as disordered by rotation about Zn-C. Two sites refined to occupancy 0.65 : 0.35. DFIX restraints applied to these C-C distances (1.54 A) and pairs of major and minor disordered sites were constrained to have similar displacement parameters. 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^)+(0.1099P)^2^+15.8182P] 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 32506 _refine_ls_number_parameters 551 _refine_ls_number_restraints 43 _refine_ls_R_factor_all 0.1261 _refine_ls_R_factor_gt 0.0846 _refine_ls_wR_factor_ref 0.2390 _refine_ls_wR_factor_gt 0.2052 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.106 _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 0.98612(2) 0.20872(3) 0.98546(3) 0.01748(13) Uani 1 1 d . A . Zn2 Zn 0.99708(2) 0.20849(3) 0.48522(3) 0.01720(13) Uani 1 1 d . . . Li1 Li 0.8633(3) 0.1074(4) 0.8622(4) 0.0227(16) Uani 1 1 d . . . Li2 Li 0.8670(3) 0.1108(4) 0.3646(4) 0.0196(15) Uani 1 1 d . . . O1 O 0.87763(15) 0.06287(17) 0.75467(17) 0.0237(7) Uani 1 1 d . . . O2 O 0.75755(14) 0.04659(17) 0.84548(17) 0.0231(7) Uani 1 1 d . . . O3 O 0.75899(14) 0.05940(17) 0.35228(17) 0.0248(7) Uani 1 1 d . . . O4 O 0.87747(16) 0.05431(17) 0.25656(18) 0.0259(7) Uani 1 1 d U . . C1 C 0.9985(2) 0.0851(2) 0.9923(2) 0.0192(9) Uani 1 1 d . . . N2 N 0.88251(17) 0.22986(19) 0.9017(2) 0.0191(8) Uani 1 1 d . . . C24 C 1.0034(2) 0.0845(2) 0.4908(3) 0.0211(9) Uani 1 1 d . . . N4 N 0.89642(17) 0.23425(19) 0.3988(2) 0.0190(8) Uani 1 1 d . . . N1 N 0.94102(17) 0.0394(2) 0.9442(2) 0.0192(8) Uani 1 1 d . . . C2 C 1.0556(2) 0.0413(2) 1.0466(2) 0.0192(9) Uani 1 1 d . . . H2 H 1.0964 0.0718 1.0807 0.023 Uiso 1 1 calc R . . C3 C 0.8969(2) 0.2850(2) 0.8415(3) 0.0207(9) Uani 1 1 d . . . C4 C 0.9099(2) 0.3733(2) 0.8687(3) 0.0271(10) Uani 1 1 d . . . H4A H 0.9618 0.3779 0.9080 0.032 Uiso 1 1 calc R . . H4B H 0.9121 0.4081 0.8241 0.032 Uiso 1 1 calc R . . C5 C 0.8435(2) 0.4034(3) 0.9037(3) 0.0306(12) Uani 1 1 d . . . H5A H 0.8567 0.4584 0.9252 0.037 Uiso 1 1 calc R . . H5B H 0.7929 0.4066 0.8626 0.037 Uiso 1 1 calc R . . C6 C 0.8331(2) 0.3467(2) 0.9679(3) 0.0283(11) Uani 1 1 d . . . H6A H 0.7866 0.3645 0.9861 0.034 Uiso 1 1 calc R . . H6B H 0.8809 0.3500 1.0124 0.034 Uiso 1 1 calc R . . C7 C 0.8207(2) 0.2585(2) 0.9401(3) 0.0215(9) Uani 1 1 d . . . C8 C 0.9738(2) 0.2549(3) 0.8221(3) 0.0271(10) Uani 1 1 d . . . H8A H 1.0187 0.2595 0.8682 0.041 Uiso 1 1 calc R . . H8B H 0.9842 0.2881 0.7802 0.041 Uiso 1 1 calc R . . H8C H 0.9671 0.1982 0.8054 0.041 Uiso 1 1 calc R . . C9 C 0.8302(2) 0.2826(3) 0.7645(3) 0.0273(10) Uani 1 1 d . . . H9A H 0.8104 0.2270 0.7543 0.041 Uiso 1 1 calc R . . H9B H 0.8517 0.3011 0.7218 0.041 Uiso 1 1 calc R . . H9C H 0.7863 0.3182 0.7687 0.041 Uiso 1 1 calc R . . C10 C 0.8283(2) 0.2043(3) 1.0120(3) 0.0269(10) Uani 1 1 d . . . H10A H 0.8246 0.1473 0.9963 0.040 Uiso 1 1 calc R . . H10B H 0.7852 0.2171 1.0363 0.040 Uiso 1 1 calc R . . H10C H 0.8798 0.2142 1.0492 0.040 Uiso 1 1 calc R . . C11 C 0.7341(2) 0.2482(2) 0.8898(3) 0.0250(10) Uani 1 1 d . . . H11A H 0.7239 0.2872 0.8469 0.038 Uiso 1 1 calc R . . H11B H 0.6969 0.2578 0.9217 0.038 Uiso 1 1 calc R . . H11C H 0.7269 0.1931 0.8688 0.038 Uiso 1 1 calc R . . C12 C 1.0654(2) 0.2811(3) 1.0616(3) 0.0264(10) Uani 1 1 d D . . C13 C 1.0638(5) 0.3706(4) 1.0521(6) 0.054(2) Uani 0.650(5) 1 d PD A 1 H13A H 1.0146 0.3922 1.0615 0.081 Uiso 0.650(5) 1 calc PR A 1 H13B H 1.0658 0.3842 0.9992 0.081 Uiso 0.650(5) 1 calc PR A 1 H13C H 1.1098 0.3944 1.0893 0.081 Uiso 0.650(5) 1 calc PR A 1 C14 C 1.1488(4) 0.2523(6) 1.0611(6) 0.056(2) Uani 0.650(5) 1 d P A 1 H14A H 1.1885 0.2810 1.1013 0.084 Uiso 0.650(5) 1 calc PR A 1 H14B H 1.1582 0.2635 1.0102 0.084 Uiso 0.650(5) 1 calc PR A 1 H14C H 1.1532 0.1940 1.0713 0.084 Uiso 0.650(5) 1 calc PR A 1 C15 C 1.0540(5) 0.2592(5) 1.1405(4) 0.046(2) Uani 0.650(5) 1 d P A 1 H15A H 1.0537 0.2001 1.1458 0.069 Uiso 0.650(5) 1 calc PR A 1 H15B H 1.0031 0.2812 1.1455 0.069 Uiso 0.650(5) 1 calc PR A 1 H15C H 1.0977 0.2820 1.1812 0.069 Uiso 0.650(5) 1 calc PR A 1 C16 C 0.8733(3) 0.0971(3) 0.6781(3) 0.0350(12) Uani 1 1 d . . . H16A H 0.9249 0.1220 0.6771 0.042 Uiso 1 1 calc R . . H16B H 0.8313 0.1391 0.6648 0.042 Uiso 1 1 calc R . . C17 C 0.8540(2) 0.0279(3) 0.6215(3) 0.0317(11) Uani 1 1 d . . . H17A H 0.8754 0.0374 0.5759 0.038 Uiso 1 1 calc R . . H17B H 0.7958 0.0187 0.6036 0.038 Uiso 1 1 calc R . . C18 C 0.8958(3) -0.0427(3) 0.6699(3) 0.0286(11) Uani 1 1 d . . . H18A H 0.9532 -0.0440 0.6715 0.034 Uiso 1 1 calc R . . H18B H 0.8711 -0.0949 0.6495 0.034 Uiso 1 1 calc R . . C19 C 0.8836(2) -0.0247(2) 0.7495(3) 0.0249(10) Uani 1 1 d . . . H19A H 0.8342 -0.0509 0.7554 0.030 Uiso 1 1 calc R . . H19B H 0.9291 -0.0452 0.7908 0.030 Uiso 1 1 calc R . . C20 C 0.6962(2) 0.0556(3) 0.7737(3) 0.0282(11) Uani 1 1 d . . . H20A H 0.6994 0.0115 0.7371 0.034 Uiso 1 1 calc R . . H20B H 0.7013 0.1082 0.7490 0.034 Uiso 1 1 calc R . . C21 C 0.6186(2) 0.0512(3) 0.7971(3) 0.0287(11) Uani 1 1 d . . . H21A H 0.5744 0.0323 0.7536 0.034 Uiso 1 1 calc R . . H21B H 0.6044 0.1045 0.8152 0.034 Uiso 1 1 calc R . . C22 C 0.6378(2) -0.0103(3) 0.8630(3) 0.0353(13) Uani 1 1 d . . . H22A H 0.6049 -0.0008 0.8999 0.042 Uiso 1 1 calc R . . H22B H 0.6287 -0.0662 0.8427 0.042 Uiso 1 1 calc R . . C23 C 0.7249(3) 0.0040(3) 0.9012(3) 0.0418(14) Uani 1 1 d . . . H23A H 0.7312 0.0369 0.9488 0.050 Uiso 1 1 calc R . . H23B H 0.7529 -0.0482 0.9156 0.050 Uiso 1 1 calc R . . N3 N 0.93997(17) 0.0422(2) 0.4484(2) 0.0198(8) Uani 1 1 d . . . C25 C 1.0614(2) 0.0385(2) 0.5419(3) 0.0203(10) Uani 1 1 d . . . H25 H 1.1062 0.0669 0.5726 0.024 Uiso 1 1 calc R . . C26 C 0.9166(2) 0.2788(2) 0.3347(3) 0.0238(10) Uani 1 1 d . . . C27 C 0.9358(2) 0.3685(3) 0.3539(3) 0.0338(12) Uani 1 1 d . . . H27A H 0.9875 0.3726 0.3934 0.041 Uiso 1 1 calc R . . H27B H 0.9411 0.3968 0.3066 0.041 Uiso 1 1 calc R . . C28 C 0.8717(3) 0.4108(3) 0.3844(3) 0.0418(14) Uani 1 1 d . . . H28A H 0.8212 0.4133 0.3431 0.050 Uiso 1 1 calc R . . H28B H 0.8886 0.4668 0.4003 0.050 Uiso 1 1 calc R . . C29 C 0.8590(2) 0.3635(3) 0.4541(3) 0.0329(12) Uani 1 1 d . . . H29A H 0.8156 0.3893 0.4723 0.039 Uiso 1 1 calc R . . H29B H 0.9082 0.3659 0.4970 0.039 Uiso 1 1 calc R . . C30 C 0.8373(2) 0.2740(3) 0.4339(3) 0.0250(10) Uani 1 1 d . . . C31 C 0.9903(2) 0.2383(3) 0.3199(3) 0.0292(11) Uani 1 1 d . . . H31A H 1.0353 0.2443 0.3659 0.044 Uiso 1 1 calc R . . H31B H 1.0034 0.2639 0.2753 0.044 Uiso 1 1 calc R . . H31C H 0.9795 0.1806 0.3091 0.044 Uiso 1 1 calc R . . C32 C 0.8509(2) 0.2743(3) 0.2572(3) 0.0280(11) Uani 1 1 d . . . H32A H 0.8277 0.2199 0.2508 0.042 Uiso 1 1 calc R . . H32B H 0.8743 0.2861 0.2140 0.042 Uiso 1 1 calc R . . H32C H 0.8092 0.3141 0.2578 0.042 Uiso 1 1 calc R . . C33 C 0.8389(2) 0.2282(3) 0.5094(3) 0.0311(12) Uani 1 1 d . . . H33A H 0.8271 0.1708 0.4977 0.047 Uiso 1 1 calc R . . H33B H 0.7987 0.2511 0.5330 0.047 Uiso 1 1 calc R . . H33C H 0.8918 0.2335 0.5455 0.047 Uiso 1 1 calc R . . C34 C 0.7501(2) 0.2687(3) 0.3829(3) 0.0299(11) Uani 1 1 d . . . H34A H 0.7450 0.2999 0.3352 0.045 Uiso 1 1 calc R . . H34B H 0.7138 0.2908 0.4117 0.045 Uiso 1 1 calc R . . H34C H 0.7364 0.2119 0.3697 0.045 Uiso 1 1 calc R . . C35 C 1.0752(2) 0.2784(3) 0.5656(3) 0.0264(10) Uani 1 1 d . . . C36 C 1.1509(2) 0.2296(3) 0.5985(3) 0.0339(12) Uani 1 1 d . . . H36A H 1.1714 0.2092 0.5559 0.051 Uiso 1 1 calc R . . H36B H 1.1388 0.1840 0.6286 0.051 Uiso 1 1 calc R . . H36C H 1.1911 0.2643 0.6322 0.051 Uiso 1 1 calc R . . C37 C 1.0398(3) 0.2963(4) 0.6338(3) 0.0559(17) Uani 1 1 d . . . H37A H 1.0796 0.3239 0.6748 0.084 Uiso 1 1 calc R . . H37B H 1.0243 0.2453 0.6540 0.084 Uiso 1 1 calc R . . H37C H 0.9928 0.3310 0.6163 0.084 Uiso 1 1 calc R . . C38 C 1.1001(2) 0.3585(3) 0.5368(3) 0.0403(14) Uani 1 1 d . . . H38A H 1.0532 0.3932 0.5187 0.060 Uiso 1 1 calc R . . H38B H 1.1245 0.3484 0.4939 0.060 Uiso 1 1 calc R . . H38C H 1.1388 0.3856 0.5792 0.060 Uiso 1 1 calc R . . C39 C 0.6975(2) 0.0673(3) 0.2805(3) 0.0292(11) Uani 1 1 d . . . H39A H 0.7044 0.0260 0.2425 0.035 Uiso 1 1 calc R . . H39B H 0.6992 0.1217 0.2576 0.035 Uiso 1 1 calc R . . C40 C 0.6195(2) 0.0547(3) 0.3018(3) 0.0323(12) Uani 1 1 d . . . H40A H 0.5783 0.0316 0.2579 0.039 Uiso 1 1 calc R . . H40B H 0.5995 0.1060 0.3185 0.039 Uiso 1 1 calc R . . C41 C 0.6434(2) -0.0055(3) 0.3690(3) 0.0364(13) Uani 1 1 d . . . H41A H 0.6062 -0.0032 0.4027 0.044 Uiso 1 1 calc R . . H41B H 0.6452 -0.0616 0.3500 0.044 Uiso 1 1 calc R . . C42 C 0.7254(2) 0.0242(3) 0.4112(3) 0.0354(12) Uani 1 1 d . . . H42A H 0.7218 0.0653 0.4506 0.042 Uiso 1 1 calc R . . H42B H 0.7588 -0.0213 0.4375 0.042 Uiso 1 1 calc R . . C43 C 0.8838(2) -0.0335(3) 0.2583(3) 0.0274(10) Uani 1 1 d U . . H43A H 0.8330 -0.0583 0.2619 0.033 Uiso 1 1 calc R . . H43B H 0.9268 -0.0514 0.3033 0.033 Uiso 1 1 calc R . . C44 C 0.9026(2) -0.0573(3) 0.1830(3) 0.0294(11) Uani 1 1 d U . . H44A H 0.8840 -0.1129 0.1672 0.035 Uiso 1 1 calc R . . H44B H 0.9605 -0.0536 0.1873 0.035 Uiso 1 1 calc R . . C45 C 0.8557(3) 0.0058(3) 0.1264(3) 0.0340(11) Uani 1 1 d U . . H45A H 0.8782 0.0131 0.0812 0.041 Uiso 1 1 calc R . . H45B H 0.7987 -0.0092 0.1079 0.041 Uiso 1 1 calc R . . C46 C 0.8669(3) 0.0811(3) 0.1769(3) 0.0328(11) Uani 1 1 d U . . H46A H 0.9143 0.1117 0.1718 0.039 Uiso 1 1 calc R . . H46B H 0.8196 0.1167 0.1609 0.039 Uiso 1 1 calc R . . C14A C 1.0305(8) 0.3557(9) 1.0979(9) 0.046(2) Uani 0.350(5) 1 d PD A 2 H14D H 0.9932 0.3361 1.1266 0.069 Uiso 0.350(5) 1 calc PR A 2 H14E H 1.0025 0.3920 1.0562 0.069 Uiso 0.350(5) 1 calc PR A 2 H14F H 1.0742 0.3851 1.1332 0.069 Uiso 0.350(5) 1 calc PR A 2 C13A C 1.1197(8) 0.3284(9) 1.0193(10) 0.054(2) Uani 0.350(5) 1 d P A 2 H13D H 1.1664 0.3494 1.0578 0.081 Uiso 0.350(5) 1 calc PR A 2 H13E H 1.0897 0.3735 0.9900 0.081 Uiso 0.350(5) 1 calc PR A 2 H13F H 1.1372 0.2918 0.9837 0.081 Uiso 0.350(5) 1 calc PR A 2 C15A C 1.1157(7) 0.2342(9) 1.1273(9) 0.056(2) Uani 0.350(5) 1 d PD A 2 H15D H 1.1506 0.2712 1.1637 0.084 Uiso 0.350(5) 1 calc PR A 2 H15E H 1.1482 0.1953 1.1075 0.084 Uiso 0.350(5) 1 calc PR A 2 H15F H 1.0814 0.2050 1.1540 0.084 Uiso 0.350(5) 1 calc PR A 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 0.01476(19) 0.0200(2) 0.0159(3) 0.0007(2) 0.00081(19) 0.00036(18) Zn2 0.01501(19) 0.0197(2) 0.0150(3) -0.0009(2) 0.00042(19) 0.00033(18) Li1 0.015(3) 0.032(4) 0.020(4) -0.003(4) 0.001(3) -0.001(3) Li2 0.015(3) 0.027(4) 0.012(4) 0.004(3) -0.004(3) 0.004(3) O1 0.0283(14) 0.0259(16) 0.0170(18) 0.0008(15) 0.0059(13) 0.0005(12) O2 0.0184(13) 0.0298(16) 0.0191(18) 0.0022(14) 0.0010(12) -0.0016(11) O3 0.0171(12) 0.0379(18) 0.0164(17) 0.0072(15) -0.0012(12) -0.0031(12) O4 0.0313(14) 0.0272(16) 0.0197(18) -0.0011(15) 0.0072(13) 0.0001(12) C1 0.0190(17) 0.020(2) 0.018(3) 0.0007(19) 0.0039(17) -0.0017(15) N2 0.0160(14) 0.0186(18) 0.022(2) 0.0008(16) 0.0048(14) 0.0027(13) C24 0.0207(17) 0.023(2) 0.019(3) -0.002(2) 0.0043(18) 0.0006(16) N4 0.0152(14) 0.0193(17) 0.018(2) 0.0000(16) -0.0039(14) 0.0009(13) N1 0.0202(16) 0.0210(18) 0.016(2) 0.0019(17) 0.0044(14) 0.0054(14) C2 0.0187(18) 0.025(2) 0.011(2) -0.004(2) -0.0019(16) -0.0002(16) C3 0.0255(17) 0.020(2) 0.016(2) 0.005(2) 0.0037(17) -0.0018(17) C4 0.030(2) 0.021(2) 0.028(3) 0.005(2) 0.003(2) -0.0017(17) C5 0.033(2) 0.017(2) 0.035(3) -0.002(2) -0.002(2) 0.0019(18) C6 0.0231(19) 0.030(2) 0.030(3) -0.010(2) 0.0034(19) 0.0024(17) C7 0.0160(17) 0.025(2) 0.023(3) -0.004(2) 0.0037(17) 0.0017(15) C8 0.029(2) 0.032(2) 0.021(3) 0.007(2) 0.0095(19) -0.0004(18) C9 0.033(2) 0.027(2) 0.018(3) 0.003(2) 0.0003(18) 0.0003(19) C10 0.0190(17) 0.038(3) 0.025(3) 0.006(2) 0.0068(17) 0.0052(19) C11 0.0190(18) 0.027(2) 0.026(3) -0.004(2) 0.0008(18) 0.0033(17) C12 0.0237(19) 0.029(2) 0.026(3) -0.003(2) 0.0052(18) -0.0030(18) C13 0.049(4) 0.041(5) 0.061(6) -0.009(4) -0.007(4) -0.016(3) C14 0.027(3) 0.072(5) 0.062(6) -0.029(5) 0.000(3) -0.018(3) C15 0.048(4) 0.064(5) 0.027(5) -0.018(4) 0.013(3) -0.027(4) C16 0.042(3) 0.035(3) 0.028(3) 0.001(3) 0.010(2) 0.002(2) C17 0.033(2) 0.045(3) 0.019(3) -0.003(3) 0.009(2) -0.005(2) C18 0.031(2) 0.029(3) 0.031(3) -0.009(2) 0.016(2) -0.0045(19) C19 0.0242(19) 0.021(2) 0.028(3) 0.001(2) 0.0053(19) -0.0002(17) C20 0.0180(18) 0.038(3) 0.024(3) 0.000(2) -0.0030(18) -0.0036(18) C21 0.0193(18) 0.034(3) 0.032(3) -0.006(2) 0.0049(19) -0.0023(17) C22 0.032(2) 0.029(3) 0.050(4) -0.003(3) 0.019(2) -0.0065(19) C23 0.033(2) 0.053(3) 0.040(4) 0.018(3) 0.010(2) -0.004(2) N3 0.0171(15) 0.0255(19) 0.016(2) 0.0009(17) 0.0021(14) 0.0026(13) C25 0.0175(17) 0.021(2) 0.022(3) 0.000(2) 0.0039(18) -0.0007(16) C26 0.0225(18) 0.022(2) 0.024(3) 0.003(2) 0.0006(18) -0.0012(16) C27 0.035(2) 0.025(2) 0.037(3) 0.003(2) 0.003(2) -0.0059(19) C28 0.051(3) 0.024(3) 0.046(4) -0.003(3) 0.003(3) 0.002(2) C29 0.031(2) 0.029(3) 0.033(3) -0.012(3) -0.001(2) 0.0058(18) C30 0.0167(17) 0.030(2) 0.028(3) -0.001(2) 0.0041(17) 0.0056(16) C31 0.025(2) 0.040(3) 0.022(3) 0.006(2) 0.0059(19) 0.0011(19) C32 0.031(2) 0.028(3) 0.024(3) 0.004(2) 0.0044(19) 0.0022(18) C33 0.0196(18) 0.051(3) 0.024(3) -0.003(3) 0.0080(18) 0.0077(19) C34 0.0177(18) 0.040(3) 0.031(3) 0.004(2) 0.0037(18) 0.0098(17) C35 0.0237(18) 0.031(3) 0.022(3) -0.008(2) 0.0011(17) -0.0061(18) C36 0.027(2) 0.037(3) 0.028(3) -0.002(2) -0.009(2) -0.0093(19) C37 0.035(2) 0.090(5) 0.041(4) -0.031(4) 0.007(2) -0.011(3) C38 0.032(2) 0.026(3) 0.052(4) -0.005(3) -0.009(2) -0.0025(19) C39 0.0223(19) 0.037(3) 0.023(3) -0.003(2) -0.0039(19) -0.0008(18) C40 0.0197(19) 0.038(3) 0.035(3) 0.004(3) 0.000(2) -0.0031(18) C41 0.029(2) 0.037(3) 0.041(4) 0.010(3) 0.005(2) -0.0043(19) C42 0.026(2) 0.053(3) 0.024(3) 0.013(3) 0.003(2) -0.002(2) C43 0.027(2) 0.028(2) 0.027(3) 0.002(2) 0.0057(19) -0.0016(18) C44 0.027(2) 0.029(2) 0.032(3) -0.010(2) 0.0078(19) -0.0042(18) C45 0.036(2) 0.044(3) 0.023(3) -0.004(2) 0.010(2) -0.002(2) C46 0.043(2) 0.042(3) 0.013(3) 0.007(2) 0.006(2) 0.005(2) C14A 0.048(4) 0.064(5) 0.027(5) -0.018(4) 0.013(3) -0.027(4) C13A 0.049(4) 0.041(5) 0.061(6) -0.009(4) -0.007(4) -0.016(3) C15A 0.027(3) 0.072(5) 0.062(6) -0.029(5) 0.000(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N2 2.049(3) . ? Zn1 C12 2.050(4) . ? Zn1 C1 2.054(4) . ? Zn1 Li1 3.123(7) . ? Zn2 C24 2.051(4) . ? Zn2 N4 2.054(3) . ? Zn2 C35 2.055(4) . ? Zn2 Li2 3.134(6) . ? Li1 O2 2.047(7) . ? Li1 N1 2.049(7) . ? Li1 O1 2.130(8) . ? Li1 N2 2.139(8) . ? Li2 O3 2.018(6) . ? Li2 N3 2.036(7) . ? Li2 N4 2.151(7) . ? Li2 O4 2.192(8) . ? O1 C19 1.455(5) . ? O1 C16 1.463(5) . ? O2 C20 1.445(5) . ? O2 C23 1.448(5) . ? O3 C39 1.446(5) . ? O3 C42 1.450(5) . ? O4 C43 1.454(5) . ? O4 C46 1.455(5) . ? C1 N1 1.364(5) . ? C1 C2 1.395(5) . ? N2 C3 1.477(5) . ? N2 C7 1.494(5) . ? C24 N3 1.358(5) . ? C24 C25 1.395(5) . ? N4 C26 1.475(5) . ? N4 C30 1.488(5) . ? N1 C2 1.341(5) 3_757 ? C2 N1 1.341(5) 3_757 ? C2 H2 0.9500 . ? C3 C4 1.536(5) . ? C3 C8 1.547(5) . ? C3 C9 1.551(5) . ? C4 C5 1.529(6) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.526(6) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.535(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C10 1.542(6) . ? C7 C11 1.548(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 C15A 1.486(13) . ? C12 C13 1.487(8) . ? C12 C15 1.516(9) . ? C12 C14 1.527(8) . ? C12 C13A 1.561(16) . ? C12 C14A 1.583(12) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.505(6) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 C18 1.518(6) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.520(6) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.513(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.524(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.508(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? N3 C25 1.345(5) 3_756 ? C25 N3 1.345(5) 3_756 ? C25 H25 0.9500 . ? C26 C31 1.528(5) . ? C26 C27 1.539(6) . ? C26 C32 1.550(5) . ? C27 C28 1.528(6) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.532(7) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.546(6) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C33 1.539(6) . ? C30 C34 1.553(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C38 1.522(6) . ? C35 C36 1.524(6) . ? C35 C37 1.528(6) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.514(6) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 C41 1.530(6) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.510(6) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.514(6) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.531(6) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.518(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C14A H14D 0.9800 . ? C14A H14E 0.9800 . ? C14A H14F 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C15A H15D 0.9800 . ? C15A H15E 0.9800 . ? C15A H15F 0.9800 . ? 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 N2 Zn1 C12 134.11(15) . . ? N2 Zn1 C1 105.76(14) . . ? C12 Zn1 C1 119.90(16) . . ? N2 Zn1 Li1 42.91(15) . . ? C12 Zn1 Li1 176.45(19) . . ? C1 Zn1 Li1 63.32(17) . . ? C24 Zn2 N4 105.53(14) . . ? C24 Zn2 C35 120.66(17) . . ? N4 Zn2 C35 133.40(15) . . ? C24 Zn2 Li2 62.59(16) . . ? N4 Zn2 Li2 43.03(15) . . ? C35 Zn2 Li2 175.42(16) . . ? O2 Li1 N1 103.6(3) . . ? O2 Li1 O1 90.5(3) . . ? N1 Li1 O1 104.2(3) . . ? O2 Li1 N2 124.7(3) . . ? N1 Li1 N2 105.4(3) . . ? O1 Li1 N2 125.3(4) . . ? O2 Li1 Zn1 142.1(3) . . ? N1 Li1 Zn1 65.68(19) . . ? O1 Li1 Zn1 127.0(3) . . ? N2 Li1 Zn1 40.71(14) . . ? O3 Li2 N3 103.3(3) . . ? O3 Li2 N4 125.1(3) . . ? N3 Li2 N4 105.2(3) . . ? O3 Li2 O4 90.7(3) . . ? N3 Li2 O4 103.3(3) . . ? N4 Li2 O4 125.8(3) . . ? O3 Li2 Zn2 140.9(3) . . ? N3 Li2 Zn2 65.25(19) . . ? N4 Li2 Zn2 40.65(13) . . ? O4 Li2 Zn2 127.8(2) . . ? C19 O1 C16 108.2(3) . . ? C19 O1 Li1 115.3(3) . . ? C16 O1 Li1 136.0(3) . . ? C20 O2 C23 109.2(3) . . ? C20 O2 Li1 120.4(3) . . ? C23 O2 Li1 129.3(3) . . ? C39 O3 C42 109.6(3) . . ? C39 O3 Li2 120.7(3) . . ? C42 O3 Li2 128.8(3) . . ? C43 O4 C46 108.2(3) . . ? C43 O4 Li2 115.4(3) . . ? C46 O4 Li2 135.4(3) . . ? N1 C1 C2 115.0(3) . . ? N1 C1 Zn1 117.7(3) . . ? C2 C1 Zn1 127.0(3) . . ? C3 N2 C7 114.6(3) . . ? C3 N2 Zn1 110.7(2) . . ? C7 N2 Zn1 108.6(3) . . ? C3 N2 Li1 112.6(3) . . ? C7 N2 Li1 112.4(3) . . ? Zn1 N2 Li1 96.4(2) . . ? N3 C24 C25 115.3(3) . . ? N3 C24 Zn2 117.5(3) . . ? C25 C24 Zn2 126.6(3) . . ? C26 N4 C30 115.8(3) . . ? C26 N4 Zn2 111.0(2) . . ? C30 N4 Zn2 108.8(3) . . ? C26 N4 Li2 109.9(3) . . ? C30 N4 Li2 113.4(3) . . ? Zn2 N4 Li2 96.3(2) . . ? C2 N1 C1 118.1(3) 3_757 . ? C2 N1 Li1 129.2(3) 3_757 . ? C1 N1 Li1 112.6(3) . . ? N1 C2 C1 126.9(4) 3_757 . ? N1 C2 H2 116.5 3_757 . ? C1 C2 H2 116.5 . . ? N2 C3 C4 113.2(4) . . ? N2 C3 C8 106.5(3) . . ? C4 C3 C8 108.1(3) . . ? N2 C3 C9 113.6(3) . . ? C4 C3 C9 108.6(3) . . ? C8 C3 C9 106.4(4) . . ? C5 C4 C3 111.9(3) . . ? C5 C4 H4A 109.2 . . ? C3 C4 H4A 109.2 . . ? C5 C4 H4B 109.2 . . ? C3 C4 H4B 109.2 . . ? H4A C4 H4B 107.9 . . ? C6 C5 C4 110.9(3) . . ? C6 C5 H5A 109.5 . . ? C4 C5 H5A 109.5 . . ? C6 C5 H5B 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 108.1 . . ? C5 C6 C7 112.0(4) . . ? C5 C6 H6A 109.2 . . ? C7 C6 H6A 109.2 . . ? C5 C6 H6B 109.2 . . ? C7 C6 H6B 109.2 . . ? H6A C6 H6B 107.9 . . ? N2 C7 C6 113.0(3) . . ? N2 C7 C10 106.4(3) . . ? C6 C7 C10 107.9(4) . . ? N2 C7 C11 113.8(4) . . ? C6 C7 C11 109.0(3) . . ? C10 C7 C11 106.3(3) . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C7 C11 H11A 109.5 . . ? C7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15A C12 C13 126.8(7) . . ? C15A C12 C15 48.2(7) . . ? C13 C12 C15 109.9(6) . . ? C15A C12 C14 58.5(7) . . ? C13 C12 C14 107.4(5) . . ? C15 C12 C14 106.5(6) . . ? C15A C12 C13A 109.7(9) . . ? C13 C12 C13A 56.2(7) . . ? C15 C12 C13A 144.0(7) . . ? C14 C12 C13A 57.3(7) . . ? C15A C12 C14A 107.0(9) . . ? C13 C12 C14A 43.6(6) . . ? C15 C12 C14A 69.5(7) . . ? C14 C12 C14A 135.2(6) . . ? C13A C12 C14A 98.8(8) . . ? C15A C12 Zn1 112.0(6) . . ? C13 C12 Zn1 120.9(4) . . ? C15 C12 Zn1 104.4(3) . . ? C14 C12 Zn1 106.8(4) . . ? C13A C12 Zn1 111.0(6) . . ? C14A C12 Zn1 117.5(5) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? O1 C16 C17 106.3(4) . . ? O1 C16 H16A 110.5 . . ? C17 C16 H16A 110.5 . . ? O1 C16 H16B 110.5 . . ? C17 C16 H16B 110.5 . . ? H16A C16 H16B 108.7 . . ? C16 C17 C18 102.2(4) . . ? C16 C17 H17A 111.3 . . ? C18 C17 H17A 111.3 . . ? C16 C17 H17B 111.3 . . ? C18 C17 H17B 111.3 . . ? H17A C17 H17B 109.2 . . ? C17 C18 C19 102.7(4) . . ? C17 C18 H18A 111.2 . . ? C19 C18 H18A 111.2 . . ? C17 C18 H18B 111.2 . . ? C19 C18 H18B 111.2 . . ? H18A C18 H18B 109.1 . . ? O1 C19 C18 106.4(3) . . ? O1 C19 H19A 110.5 . . ? C18 C19 H19A 110.5 . . ? O1 C19 H19B 110.5 . . ? C18 C19 H19B 110.5 . . ? H19A C19 H19B 108.6 . . ? O2 C20 C21 104.8(4) . . ? O2 C20 H20A 110.8 . . ? C21 C20 H20A 110.8 . . ? O2 C20 H20B 110.8 . . ? C21 C20 H20B 110.8 . . ? H20A C20 H20B 108.9 . . ? C20 C21 C22 102.2(3) . . ? C20 C21 H21A 111.3 . . ? C22 C21 H21A 111.3 . . ? C20 C21 H21B 111.3 . . ? C22 C21 H21B 111.3 . . ? H21A C21 H21B 109.2 . . ? C23 C22 C21 103.8(4) . . ? C23 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? C23 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? O2 C23 C22 106.9(4) . . ? O2 C23 H23A 110.3 . . ? C22 C23 H23A 110.3 . . ? O2 C23 H23B 110.3 . . ? C22 C23 H23B 110.3 . . ? H23A C23 H23B 108.6 . . ? C25 N3 C24 118.5(3) 3_756 . ? C25 N3 Li2 128.2(3) 3_756 . ? C24 N3 Li2 112.5(3) . . ? N3 C25 C24 126.2(4) 3_756 . ? N3 C25 H25 116.9 3_756 . ? C24 C25 H25 116.9 . . ? N4 C26 C31 107.1(3) . . ? N4 C26 C27 112.9(4) . . ? C31 C26 C27 108.5(3) . . ? N4 C26 C32 113.6(3) . . ? C31 C26 C32 106.3(4) . . ? C27 C26 C32 108.1(3) . . ? C28 C27 C26 112.6(3) . . ? C28 C27 H27A 109.1 . . ? C26 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C26 C27 H27B 109.1 . . ? H27A C27 H27B 107.8 . . ? C27 C28 C29 109.2(4) . . ? C27 C28 H28A 109.8 . . ? C29 C28 H28A 109.8 . . ? C27 C28 H28B 109.8 . . ? C29 C28 H28B 109.8 . . ? H28A C28 H28B 108.3 . . ? C28 C29 C30 112.1(4) . . ? C28 C29 H29A 109.2 . . ? C30 C29 H29A 109.2 . . ? C28 C29 H29B 109.2 . . ? C30 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? N4 C30 C33 107.1(3) . . ? N4 C30 C29 111.5(3) . . ? C33 C30 C29 108.5(4) . . ? N4 C30 C34 113.8(4) . . ? C33 C30 C34 106.2(3) . . ? C29 C30 C34 109.4(3) . . ? C26 C31 H31A 109.5 . . ? C26 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C26 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C26 C32 H32A 109.5 . . ? C26 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C26 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C30 C33 H33A 109.5 . . ? C30 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C30 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C30 C34 H34A 109.5 . . ? C30 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C30 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C38 C35 C36 107.3(3) . . ? C38 C35 C37 108.1(4) . . ? C36 C35 C37 106.2(4) . . ? C38 C35 Zn2 116.6(3) . . ? C36 C35 Zn2 108.6(3) . . ? C37 C35 Zn2 109.5(3) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C35 C38 H38A 109.5 . . ? C35 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C35 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O3 C39 C40 105.5(4) . . ? O3 C39 H39A 110.6 . . ? C40 C39 H39A 110.6 . . ? O3 C39 H39B 110.6 . . ? C40 C39 H39B 110.6 . . ? H39A C39 H39B 108.8 . . ? C39 C40 C41 102.0(3) . . ? C39 C40 H40A 111.4 . . ? C41 C40 H40A 111.4 . . ? C39 C40 H40B 111.4 . . ? C41 C40 H40B 111.4 . . ? H40A C40 H40B 109.2 . . ? C42 C41 C40 102.0(4) . . ? C42 C41 H41A 111.4 . . ? C40 C41 H41A 111.4 . . ? C42 C41 H41B 111.4 . . ? C40 C41 H41B 111.4 . . ? H41A C41 H41B 109.2 . . ? O3 C42 C41 105.9(4) . . ? O3 C42 H42A 110.6 . . ? C41 C42 H42A 110.6 . . ? O3 C42 H42B 110.6 . . ? C41 C42 H42B 110.6 . . ? H42A C42 H42B 108.7 . . ? O4 C43 C44 105.9(4) . . ? O4 C43 H43A 110.6 . . ? C44 C43 H43A 110.6 . . ? O4 C43 H43B 110.6 . . ? C44 C43 H43B 110.6 . . ? H43A C43 H43B 108.7 . . ? C43 C44 C45 102.0(4) . . ? C43 C44 H44A 111.4 . . ? C45 C44 H44A 111.4 . . ? C43 C44 H44B 111.4 . . ? C45 C44 H44B 111.4 . . ? H44A C44 H44B 109.2 . . ? C46 C45 C44 101.6(4) . . ? C46 C45 H45A 111.4 . . ? C44 C45 H45A 111.4 . . ? C46 C45 H45B 111.4 . . ? C44 C45 H45B 111.4 . . ? H45A C45 H45B 109.3 . . ? O4 C46 C45 107.2(4) . . ? O4 C46 H46A 110.3 . . ? C45 C46 H46A 110.3 . . ? O4 C46 H46B 110.3 . . ? C45 C46 H46B 110.3 . . ? H46A C46 H46B 108.5 . . ? C12 C14A H14D 109.5 . . ? C12 C14A H14E 109.5 . . ? H14D C14A H14E 109.5 . . ? C12 C14A H14F 109.5 . . ? H14D C14A H14F 109.5 . . ? H14E C14A H14F 109.5 . . ? C12 C13A H13D 109.5 . . ? C12 C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C12 C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C12 C15A H15D 109.5 . . ? C12 C15A H15E 109.5 . . ? H15D C15A H15E 109.5 . . ? C12 C15A H15F 109.5 . . ? H15D C15A H15F 109.5 . . ? H15E C15A H15F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Zn1 Li1 O2 -85.8(5) . . . . ? C12 Zn1 Li1 O2 -120(3) . . . . ? C1 Zn1 Li1 O2 84.9(5) . . . . ? N2 Zn1 Li1 N1 -166.6(3) . . . . ? C12 Zn1 Li1 N1 160(3) . . . . ? C1 Zn1 Li1 N1 4.13(18) . . . . ? N2 Zn1 Li1 O1 103.6(4) . . . . ? C12 Zn1 Li1 O1 70(3) . . . . ? C1 Zn1 Li1 O1 -85.7(4) . . . . ? C12 Zn1 Li1 N2 -34(3) . . . . ? C1 Zn1 Li1 N2 170.8(3) . . . . ? C24 Zn2 Li2 O3 87.9(5) . . . . ? N4 Zn2 Li2 O3 -88.2(5) . . . . ? C35 Zn2 Li2 O3 -48(3) . . . . ? C24 Zn2 Li2 N3 7.38(19) . . . . ? N4 Zn2 Li2 N3 -168.7(3) . . . . ? C35 Zn2 Li2 N3 -129(2) . . . . ? C24 Zn2 Li2 N4 176.1(3) . . . . ? C35 Zn2 Li2 N4 40(2) . . . . ? C24 Zn2 Li2 O4 -80.5(3) . . . . ? N4 Zn2 Li2 O4 103.4(4) . . . . ? C35 Zn2 Li2 O4 144(2) . . . . ? O2 Li1 O1 C19 -62.0(3) . . . . ? N1 Li1 O1 C19 42.2(4) . . . . ? N2 Li1 O1 C19 163.3(3) . . . . ? Zn1 Li1 O1 C19 112.3(4) . . . . ? O2 Li1 O1 C16 108.5(4) . . . . ? N1 Li1 O1 C16 -147.3(4) . . . . ? N2 Li1 O1 C16 -26.3(6) . . . . ? Zn1 Li1 O1 C16 -77.3(5) . . . . ? N1 Li1 O2 C20 -156.3(3) . . . . ? O1 Li1 O2 C20 -51.6(4) . . . . ? N2 Li1 O2 C20 83.7(5) . . . . ? Zn1 Li1 O2 C20 136.0(5) . . . . ? N1 Li1 O2 C23 36.6(5) . . . . ? O1 Li1 O2 C23 141.3(4) . . . . ? N2 Li1 O2 C23 -83.5(6) . . . . ? Zn1 Li1 O2 C23 -31.2(7) . . . . ? N3 Li2 O3 C39 -155.2(3) . . . . ? N4 Li2 O3 C39 85.0(5) . . . . ? O4 Li2 O3 C39 -51.4(4) . . . . ? Zn2 Li2 O3 C39 137.8(4) . . . . ? N3 Li2 O3 C42 36.6(5) . . . . ? N4 Li2 O3 C42 -83.1(5) . . . . ? O4 Li2 O3 C42 140.5(4) . . . . ? Zn2 Li2 O3 C42 -30.4(7) . . . . ? O3 Li2 O4 C43 -66.5(3) . . . . ? N3 Li2 O4 C43 37.3(4) . . . . ? N4 Li2 O4 C43 157.5(3) . . . . ? Zn2 Li2 O4 C43 106.2(4) . . . . ? O3 Li2 O4 C46 101.1(4) . . . . ? N3 Li2 O4 C46 -155.1(4) . . . . ? N4 Li2 O4 C46 -34.9(6) . . . . ? Zn2 Li2 O4 C46 -86.2(5) . . . . ? N2 Zn1 C1 N1 0.1(3) . . . . ? C12 Zn1 C1 N1 175.3(3) . . . . ? Li1 Zn1 C1 N1 -6.4(3) . . . . ? N2 Zn1 C1 C2 -172.9(3) . . . . ? C12 Zn1 C1 C2 2.2(4) . . . . ? Li1 Zn1 C1 C2 -179.5(4) . . . . ? C12 Zn1 N2 C3 60.1(3) . . . . ? C1 Zn1 N2 C3 -125.7(3) . . . . ? Li1 Zn1 N2 C3 -117.1(3) . . . . ? C12 Zn1 N2 C7 -66.5(3) . . . . ? C1 Zn1 N2 C7 107.7(3) . . . . ? Li1 Zn1 N2 C7 116.3(3) . . . . ? C12 Zn1 N2 Li1 177.2(3) . . . . ? C1 Zn1 N2 Li1 -8.6(3) . . . . ? O2 Li1 N2 C3 -112.6(4) . . . . ? N1 Li1 N2 C3 128.2(3) . . . . ? O1 Li1 N2 C3 7.7(5) . . . . ? Zn1 Li1 N2 C3 115.6(3) . . . . ? O2 Li1 N2 C7 18.7(6) . . . . ? N1 Li1 N2 C7 -100.5(3) . . . . ? O1 Li1 N2 C7 139.0(4) . . . . ? Zn1 Li1 N2 C7 -113.2(3) . . . . ? O2 Li1 N2 Zn1 131.8(4) . . . . ? N1 Li1 N2 Zn1 12.6(3) . . . . ? O1 Li1 N2 Zn1 -107.9(3) . . . . ? N4 Zn2 C24 N3 -8.6(4) . . . . ? C35 Zn2 C24 N3 164.9(3) . . . . ? Li2 Zn2 C24 N3 -11.4(3) . . . . ? N4 Zn2 C24 C25 -179.1(3) . . . . ? C35 Zn2 C24 C25 -5.6(4) . . . . ? Li2 Zn2 C24 C25 178.1(4) . . . . ? C24 Zn2 N4 C26 -117.7(3) . . . . ? C35 Zn2 N4 C26 70.0(3) . . . . ? Li2 Zn2 N4 C26 -114.1(3) . . . . ? C24 Zn2 N4 C30 113.8(3) . . . . ? C35 Zn2 N4 C30 -58.5(3) . . . . ? Li2 Zn2 N4 C30 117.4(3) . . . . ? C24 Zn2 N4 Li2 -3.6(3) . . . . ? C35 Zn2 N4 Li2 -175.9(3) . . . . ? O3 Li2 N4 C26 -115.5(4) . . . . ? N3 Li2 N4 C26 125.7(3) . . . . ? O4 Li2 N4 C26 6.3(4) . . . . ? Zn2 Li2 N4 C26 115.0(3) . . . . ? O3 Li2 N4 C30 15.9(5) . . . . ? N3 Li2 N4 C30 -103.0(3) . . . . ? O4 Li2 N4 C30 137.6(3) . . . . ? Zn2 Li2 N4 C30 -113.6(3) . . . . ? O3 Li2 N4 Zn2 129.5(4) . . . . ? N3 Li2 N4 Zn2 10.6(3) . . . . ? O4 Li2 N4 Zn2 -108.7(3) . . . . ? C2 C1 N1 C2 0.2(6) . . . 3_757 ? Zn1 C1 N1 C2 -173.7(3) . . . 3_757 ? C2 C1 N1 Li1 -176.7(3) . . . . ? Zn1 C1 N1 Li1 9.5(4) . . . . ? O2 Li1 N1 C2 36.1(5) . . . 3_757 ? O1 Li1 N1 C2 -57.9(5) . . . 3_757 ? N2 Li1 N1 C2 168.6(3) . . . 3_757 ? Zn1 Li1 N1 C2 177.6(4) . . . 3_757 ? O2 Li1 N1 C1 -147.4(3) . . . . ? O1 Li1 N1 C1 118.5(3) . . . . ? N2 Li1 N1 C1 -15.0(4) . . . . ? Zn1 Li1 N1 C1 -6.0(3) . . . . ? N1 C1 C2 N1 -0.2(7) . . . 3_757 ? Zn1 C1 C2 N1 173.0(3) . . . 3_757 ? C7 N2 C3 C4 49.3(4) . . . . ? Zn1 N2 C3 C4 -73.9(3) . . . . ? Li1 N2 C3 C4 179.4(3) . . . . ? C7 N2 C3 C8 167.9(3) . . . . ? Zn1 N2 C3 C8 44.7(4) . . . . ? Li1 N2 C3 C8 -61.9(4) . . . . ? C7 N2 C3 C9 -75.3(4) . . . . ? Zn1 N2 C3 C9 161.5(3) . . . . ? Li1 N2 C3 C9 54.9(4) . . . . ? N2 C3 C4 C5 -51.5(4) . . . . ? C8 C3 C4 C5 -169.2(4) . . . . ? C9 C3 C4 C5 75.7(5) . . . . ? C3 C4 C5 C6 53.6(5) . . . . ? C4 C5 C6 C7 -53.5(4) . . . . ? C3 N2 C7 C6 -49.1(5) . . . . ? Zn1 N2 C7 C6 75.3(4) . . . . ? Li1 N2 C7 C6 -179.3(3) . . . . ? C3 N2 C7 C10 -167.3(3) . . . . ? Zn1 N2 C7 C10 -43.0(3) . . . . ? Li1 N2 C7 C10 62.4(4) . . . . ? C3 N2 C7 C11 76.1(4) . . . . ? Zn1 N2 C7 C11 -159.6(3) . . . . ? Li1 N2 C7 C11 -54.2(4) . . . . ? C5 C6 C7 N2 51.1(4) . . . . ? C5 C6 C7 C10 168.4(3) . . . . ? C5 C6 C7 C11 -76.6(4) . . . . ? N2 Zn1 C12 C15A 160.8(7) . . . . ? C1 Zn1 C12 C15A -12.7(8) . . . . ? Li1 Zn1 C12 C15A -167(3) . . . . ? N2 Zn1 C12 C13 -13.8(6) . . . . ? C1 Zn1 C12 C13 172.6(5) . . . . ? Li1 Zn1 C12 C13 18(3) . . . . ? N2 Zn1 C12 C15 110.5(4) . . . . ? C1 Zn1 C12 C15 -63.1(4) . . . . ? Li1 Zn1 C12 C15 142(3) . . . . ? N2 Zn1 C12 C14 -136.9(5) . . . . ? C1 Zn1 C12 C14 49.5(5) . . . . ? Li1 Zn1 C12 C14 -105(3) . . . . ? N2 Zn1 C12 C13A -76.2(7) . . . . ? C1 Zn1 C12 C13A 110.3(7) . . . . ? Li1 Zn1 C12 C13A -44(3) . . . . ? N2 Zn1 C12 C14A 36.4(8) . . . . ? C1 Zn1 C12 C14A -137.2(7) . . . . ? Li1 Zn1 C12 C14A 68(3) . . . . ? C19 O1 C16 C17 15.3(4) . . . . ? Li1 O1 C16 C17 -155.6(3) . . . . ? O1 C16 C17 C18 -32.8(4) . . . . ? C16 C17 C18 C19 37.0(4) . . . . ? C16 O1 C19 C18 8.6(4) . . . . ? Li1 O1 C19 C18 -178.4(3) . . . . ? C17 C18 C19 O1 -28.7(4) . . . . ? C23 O2 C20 C21 24.3(5) . . . . ? Li1 O2 C20 C21 -145.1(3) . . . . ? O2 C20 C21 C22 -35.4(4) . . . . ? C20 C21 C22 C23 33.2(5) . . . . ? C20 O2 C23 C22 -2.9(5) . . . . ? Li1 O2 C23 C22 165.4(4) . . . . ? C21 C22 C23 O2 -19.5(5) . . . . ? C25 C24 N3 C25 -0.6(6) . . . 3_756 ? Zn2 C24 N3 C25 -172.2(3) . . . 3_756 ? C25 C24 N3 Li2 -171.5(4) . . . . ? Zn2 C24 N3 Li2 17.0(4) . . . . ? O3 Li2 N3 C25 39.2(5) . . . 3_756 ? N4 Li2 N3 C25 171.9(3) . . . 3_756 ? O4 Li2 N3 C25 -54.7(5) . . . 3_756 ? Zn2 Li2 N3 C25 179.5(4) . . . 3_756 ? O3 Li2 N3 C24 -151.0(3) . . . . ? N4 Li2 N3 C24 -18.4(4) . . . . ? O4 Li2 N3 C24 115.1(3) . . . . ? Zn2 Li2 N3 C24 -10.7(3) . . . . ? N3 C24 C25 N3 0.7(7) . . . 3_756 ? Zn2 C24 C25 N3 171.3(3) . . . 3_756 ? C30 N4 C26 C31 167.4(3) . . . . ? Zn2 N4 C26 C31 42.8(4) . . . . ? Li2 N4 C26 C31 -62.5(4) . . . . ? C30 N4 C26 C27 48.0(4) . . . . ? Zn2 N4 C26 C27 -76.6(3) . . . . ? Li2 N4 C26 C27 178.1(3) . . . . ? C30 N4 C26 C32 -75.5(4) . . . . ? Zn2 N4 C26 C32 159.9(3) . . . . ? Li2 N4 C26 C32 54.6(4) . . . . ? N4 C26 C27 C28 -50.7(5) . . . . ? C31 C26 C27 C28 -169.3(4) . . . . ? C32 C26 C27 C28 75.8(5) . . . . ? C26 C27 C28 C29 54.6(5) . . . . ? C27 C28 C29 C30 -56.1(5) . . . . ? C26 N4 C30 C33 -167.7(3) . . . . ? Zn2 N4 C30 C33 -42.0(3) . . . . ? Li2 N4 C30 C33 63.9(4) . . . . ? C26 N4 C30 C29 -49.1(5) . . . . ? Zn2 N4 C30 C29 76.6(4) . . . . ? Li2 N4 C30 C29 -177.5(3) . . . . ? C26 N4 C30 C34 75.3(4) . . . . ? Zn2 N4 C30 C34 -159.0(3) . . . . ? Li2 N4 C30 C34 -53.1(5) . . . . ? C28 C29 C30 N4 53.2(5) . . . . ? C28 C29 C30 C33 171.0(3) . . . . ? C28 C29 C30 C34 -73.6(5) . . . . ? C24 Zn2 C35 C38 146.2(3) . . . . ? N4 Zn2 C35 C38 -42.4(4) . . . . ? Li2 Zn2 C35 C38 -80(2) . . . . ? C24 Zn2 C35 C36 24.9(4) . . . . ? N4 Zn2 C35 C36 -163.7(3) . . . . ? Li2 Zn2 C35 C36 159(2) . . . . ? C24 Zn2 C35 C37 -90.7(4) . . . . ? N4 Zn2 C35 C37 80.6(4) . . . . ? Li2 Zn2 C35 C37 43(2) . . . . ? C42 O3 C39 C40 13.6(5) . . . . ? Li2 O3 C39 C40 -156.7(3) . . . . ? O3 C39 C40 C41 -32.2(5) . . . . ? C39 C40 C41 C42 38.1(5) . . . . ? C39 O3 C42 C41 11.2(5) . . . . ? Li2 O3 C42 C41 -179.6(4) . . . . ? C40 C41 C42 O3 -30.8(5) . . . . ? C46 O4 C43 C44 17.3(4) . . . . ? Li2 O4 C43 C44 -171.8(3) . . . . ? O4 C43 C44 C45 -34.7(4) . . . . ? C43 C44 C45 C46 37.8(4) . . . . ? C43 O4 C46 C45 7.4(4) . . . . ? Li2 O4 C46 C45 -160.8(3) . . . . ? C44 C45 C46 O4 -28.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.773 _refine_diff_density_min -1.018 _refine_diff_density_rms 0.103 #===END data_vb16 _database_code_depnum_ccdc_archive 'CCDC 853495' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H54 Li N5 Zn' _chemical_formula_sum 'C25 H54 Li N5 Zn' _chemical_formula_weight 497.04 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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' _cell_length_a 13.0384(8) _cell_length_b 14.2144(8) _cell_length_c 16.4829(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3054.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 2636 _cell_measurement_theta_min 2.8512 _cell_measurement_theta_max 30.2567 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 0.822 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.99350 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Gemini, S' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 10176 _diffrn_reflns_av_R_equivalents 0.0469 _diffrn_reflns_av_sigmaI/netI 0.1311 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.86 _diffrn_reflns_theta_max 26.99 _reflns_number_total 5924 _reflns_number_gt 3580 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET) (compiled Apr 28 2010,14:27:37) ; _computing_structure_solution ? _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^)+(0.0112P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.498(11) _refine_ls_number_reflns 5924 _refine_ls_number_parameters 335 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0447 _refine_ls_wR_factor_ref 0.0580 _refine_ls_wR_factor_gt 0.0534 _refine_ls_goodness_of_fit_ref 0.787 _refine_ls_restrained_S_all 0.786 _refine_ls_shift/su_max 0.002 _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 0.90290(3) 0.52651(3) 0.89774(2) 0.03143(10) Uani 1 1 d . . . Li1 Li 0.4261(4) 0.5362(4) 0.7911(3) 0.0352(15) Uani 1 1 d . . . N1 N 0.7777(2) 0.55081(19) 0.82861(14) 0.0311(7) Uani 1 1 d . A . N2 N 0.5749(2) 0.54763(19) 0.76886(15) 0.0373(8) Uani 1 1 d . A . N3 N 0.4005(2) 0.4750(2) 0.90564(14) 0.0476(6) Uani 1 1 d DU A . N4 N 0.3190(2) 0.44357(18) 0.74474(17) 0.0407(8) Uani 1 1 d DU A . N5 N 0.3387(2) 0.64672(18) 0.74284(16) 0.0322(7) Uani 1 1 d DU A . C1 C 0.7563(2) 0.4990(2) 0.75259(16) 0.0281(9) Uani 1 1 d . A . H1 H 0.7840 0.4340 0.7601 0.034 Uiso 1 1 calc R . . C2 C 0.6421(3) 0.4894(2) 0.74255(17) 0.0353(9) Uani 1 1 d . . . H2 H 0.6178 0.4356 0.7143 0.042 Uiso 1 1 calc R A . C3 C 0.6107(3) 0.6194(2) 0.81929(19) 0.0404(9) Uani 1 1 d . A . H3 H 0.5685 0.6722 0.8309 0.048 Uiso 1 1 calc R . . C4 C 0.7066(3) 0.6133(2) 0.85167(19) 0.0376(10) Uani 1 1 d . . . H4 H 0.7243 0.6563 0.8935 0.045 Uiso 1 1 calc R A . C5 C 0.8128(2) 0.5417(2) 0.67795(17) 0.0315(8) Uani 1 1 d . . . C6 C 0.7792(3) 0.6426(2) 0.66185(19) 0.0454(11) Uani 1 1 d . A . H6A H 0.7963 0.6819 0.7088 0.068 Uiso 1 1 calc R . . H6B H 0.7050 0.6443 0.6526 0.068 Uiso 1 1 calc R . . H6C H 0.8147 0.6667 0.6137 0.068 Uiso 1 1 calc R . . C7 C 0.7885(2) 0.4810(2) 0.60315(17) 0.0468(9) Uani 1 1 d . A . H7A H 0.8280 0.5038 0.5566 0.070 Uiso 1 1 calc R . . H7B H 0.7150 0.4850 0.5909 0.070 Uiso 1 1 calc R . . H7C H 0.8068 0.4154 0.6143 0.070 Uiso 1 1 calc R . . C8 C 0.9289(2) 0.5411(2) 0.69201(17) 0.0407(9) Uani 1 1 d . A . H8A H 0.9450 0.5773 0.7410 0.061 Uiso 1 1 calc R . . H8B H 0.9635 0.5694 0.6452 0.061 Uiso 1 1 calc R . . H8C H 0.9525 0.4761 0.6988 0.061 Uiso 1 1 calc R . . C9 C 0.9302(3) 0.3875(2) 0.91570(19) 0.0403(11) Uani 1 1 d . . . C10 C 0.8292(3) 0.3379(2) 0.9330(2) 0.0556(12) Uani 1 1 d . . . H10A H 0.8414 0.2701 0.9385 0.083 Uiso 1 1 calc R . . H10B H 0.7815 0.3491 0.8881 0.083 Uiso 1 1 calc R . . H10C H 0.7998 0.3624 0.9834 0.083 Uiso 1 1 calc R . . C11 C 0.9792(3) 0.3380(2) 0.8432(2) 0.0563(12) Uani 1 1 d . . . H11A H 0.9933 0.2723 0.8573 0.085 Uiso 1 1 calc R . . H11B H 1.0435 0.3696 0.8290 0.085 Uiso 1 1 calc R . . H11C H 0.9322 0.3402 0.7968 0.085 Uiso 1 1 calc R . . C12 C 0.9973(4) 0.3747(3) 0.9902(2) 0.0823(16) Uani 1 1 d . . . H12A H 1.0663 0.3989 0.9790 0.123 Uiso 1 1 calc R . . H12B H 1.0015 0.3076 1.0038 0.123 Uiso 1 1 calc R . . H12C H 0.9675 0.4092 1.0360 0.123 Uiso 1 1 calc R . . C13 C 0.9684(3) 0.6472(2) 0.93799(18) 0.0375(10) Uani 1 1 d . . . C14 C 1.0823(3) 0.6287(3) 0.9525(2) 0.0639(12) Uani 1 1 d . . . H14A H 1.1151 0.6862 0.9725 0.096 Uiso 1 1 calc R . . H14B H 1.1148 0.6094 0.9016 0.096 Uiso 1 1 calc R . . H14C H 1.0902 0.5786 0.9929 0.096 Uiso 1 1 calc R . . C15 C 0.9237(3) 0.6790(2) 1.01917(17) 0.0499(11) Uani 1 1 d . . . H15A H 0.8499 0.6902 1.0131 0.075 Uiso 1 1 calc R . . H15B H 0.9574 0.7373 1.0365 0.075 Uiso 1 1 calc R . . H15C H 0.9350 0.6300 1.0600 0.075 Uiso 1 1 calc R . . C16 C 0.9601(3) 0.7287(2) 0.87850(19) 0.0714(15) Uani 1 1 d . . . H16A H 0.9990 0.7825 0.8992 0.107 Uiso 1 1 calc R . . H16B H 0.8879 0.7464 0.8722 0.107 Uiso 1 1 calc R . . H16C H 0.9879 0.7095 0.8258 0.107 Uiso 1 1 calc R . . C17 C 0.490(2) 0.416(3) 0.922(2) 0.072(3) Uani 0.671(6) 1 d PD A 1 H17A H 0.4821 0.3904 0.9772 0.108 Uiso 0.671(6) 1 d PR A 1 H17B H 0.5536 0.4526 0.9193 0.108 Uiso 0.671(6) 1 d PR A 1 H17C H 0.4932 0.3640 0.8832 0.108 Uiso 0.671(6) 1 d PR A 1 C18 C 0.3933(11) 0.5377(18) 0.9760(12) 0.084(5) Uani 0.671(6) 1 d PD A 1 H18A H 0.4589 0.5702 0.9837 0.125 Uiso 0.671(6) 1 calc PR A 1 H18B H 0.3773 0.5007 1.0246 0.125 Uiso 0.671(6) 1 calc PR A 1 H18C H 0.3390 0.5841 0.9668 0.125 Uiso 0.671(6) 1 calc PR A 1 C19 C 0.3012(5) 0.4266(5) 0.8959(4) 0.0543(17) Uani 0.671(6) 1 d PDU A 1 H19A H 0.2445 0.4726 0.9004 0.065 Uiso 0.671(6) 1 calc PR A 1 H19B H 0.2926 0.3789 0.9391 0.065 Uiso 0.671(6) 1 calc PR A 1 C20 C 0.2981(6) 0.3795(4) 0.8134(4) 0.0513(18) Uani 0.671(6) 1 d PDU A 1 H20A H 0.3493 0.3281 0.8126 0.062 Uiso 0.671(6) 1 calc PR A 1 H20B H 0.2296 0.3509 0.8057 0.062 Uiso 0.671(6) 1 calc PR A 1 C21 C 0.3494(17) 0.3911(6) 0.6723(6) 0.070(4) Uani 0.671(6) 1 d PD A 1 H21A H 0.2946 0.3474 0.6572 0.104 Uiso 0.671(6) 1 calc PR A 1 H21B H 0.4123 0.3557 0.6837 0.104 Uiso 0.671(6) 1 calc PR A 1 H21C H 0.3619 0.4351 0.6276 0.104 Uiso 0.671(6) 1 calc PR A 1 C22 C 0.2315(5) 0.5087(4) 0.7305(4) 0.0421(17) Uani 0.671(6) 1 d PDU A 1 H22A H 0.1992 0.5254 0.7829 0.050 Uiso 0.671(6) 1 calc PR A 1 H22B H 0.1793 0.4774 0.6963 0.050 Uiso 0.671(6) 1 calc PR A 1 C23 C 0.2690(5) 0.5965(4) 0.6888(4) 0.0402(17) Uani 0.671(6) 1 d PDU A 1 H23A H 0.3050 0.5797 0.6380 0.048 Uiso 0.671(6) 1 calc PR A 1 H23B H 0.2100 0.6373 0.6748 0.048 Uiso 0.671(6) 1 calc PR A 1 C24 C 0.2847(7) 0.7047(5) 0.8013(6) 0.0367(19) Uani 0.671(6) 1 d PD A 1 H24A H 0.2417 0.7504 0.7726 0.055 Uiso 0.671(6) 1 calc PR A 1 H24B H 0.3345 0.7382 0.8352 0.055 Uiso 0.671(6) 1 calc PR A 1 H24C H 0.2415 0.6648 0.8356 0.055 Uiso 0.671(6) 1 calc PR A 1 C25 C 0.4034(7) 0.7124(4) 0.6944(4) 0.0450(19) Uani 0.671(6) 1 d PD A 1 H25A H 0.4511 0.7454 0.7305 0.068 Uiso 0.671(6) 1 calc PR A 1 H25B H 0.3594 0.7583 0.6669 0.068 Uiso 0.671(6) 1 calc PR A 1 H25C H 0.4423 0.6767 0.6539 0.068 Uiso 0.671(6) 1 calc PR A 1 C17A C 0.495(4) 0.426(5) 0.930(5) 0.072(3) Uani 0.329(6) 1 d PD A 2 H17D H 0.5230 0.3976 0.8804 0.108 Uiso 0.329(6) 1 d PR A 2 H17E H 0.4835 0.3761 0.9705 0.108 Uiso 0.329(6) 1 d PR A 2 H17F H 0.5435 0.4719 0.9515 0.108 Uiso 0.329(6) 1 d PR A 2 C18A C 0.352(3) 0.534(4) 0.968(3) 0.084(5) Uani 0.329(6) 1 d PD A 2 H18D H 0.3911 0.5927 0.9741 0.125 Uiso 0.329(6) 1 calc PR A 2 H18E H 0.3524 0.5001 1.0202 0.125 Uiso 0.329(6) 1 calc PR A 2 H18F H 0.2817 0.5483 0.9525 0.125 Uiso 0.329(6) 1 calc PR A 2 C19A C 0.3431(10) 0.3867(7) 0.8826(9) 0.0543(17) Uani 0.329(6) 1 d PDU A 2 H19C H 0.3084 0.3606 0.9311 0.065 Uiso 0.329(6) 1 calc PR A 2 H19D H 0.3920 0.3390 0.8622 0.065 Uiso 0.329(6) 1 calc PR A 2 C20A C 0.2638(9) 0.4085(11) 0.8173(7) 0.0513(18) Uani 0.329(6) 1 d PDU A 2 H20C H 0.2245 0.3511 0.8036 0.062 Uiso 0.329(6) 1 calc PR A 2 H20D H 0.2151 0.4568 0.8370 0.062 Uiso 0.329(6) 1 calc PR A 2 C21A C 0.351(4) 0.3610(14) 0.6969(16) 0.070(4) Uani 0.329(6) 1 d PD A 2 H21D H 0.2929 0.3386 0.6644 0.104 Uiso 0.329(6) 1 calc PR A 2 H21E H 0.3733 0.3108 0.7337 0.104 Uiso 0.329(6) 1 calc PR A 2 H21F H 0.4076 0.3785 0.6610 0.104 Uiso 0.329(6) 1 calc PR A 2 C22A C 0.2476(12) 0.4981(8) 0.6937(7) 0.0421(17) Uani 0.329(6) 1 d PDU A 2 H22C H 0.1790 0.4683 0.6947 0.050 Uiso 0.329(6) 1 calc PR A 2 H22D H 0.2723 0.4983 0.6369 0.050 Uiso 0.329(6) 1 calc PR A 2 C23A C 0.2396(8) 0.5988(9) 0.7244(9) 0.0402(17) Uani 0.329(6) 1 d PDU A 2 H23C H 0.2026 0.6365 0.6833 0.048 Uiso 0.329(6) 1 calc PR A 2 H23D H 0.1973 0.5987 0.7743 0.048 Uiso 0.329(6) 1 calc PR A 2 C24A C 0.3183(15) 0.7259(11) 0.7968(14) 0.0367(19) Uani 0.329(6) 1 d PD A 2 H24D H 0.2760 0.7046 0.8424 0.055 Uiso 0.329(6) 1 calc PR A 2 H24E H 0.2818 0.7751 0.7669 0.055 Uiso 0.329(6) 1 calc PR A 2 H24F H 0.3833 0.7510 0.8174 0.055 Uiso 0.329(6) 1 calc PR A 2 C25A C 0.3966(16) 0.6706(10) 0.6708(8) 0.0450(19) Uani 0.329(6) 1 d PD A 2 H25D H 0.4645 0.6939 0.6865 0.068 Uiso 0.329(6) 1 calc PR A 2 H25E H 0.3602 0.7195 0.6404 0.068 Uiso 0.329(6) 1 calc PR A 2 H25F H 0.4044 0.6145 0.6367 0.068 Uiso 0.329(6) 1 calc PR A 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 0.0318(2) 0.0298(2) 0.03261(17) -0.0026(2) -0.0014(2) -0.0020(3) Li1 0.037(4) 0.030(3) 0.039(3) 0.000(3) -0.002(3) 0.000(4) N1 0.0306(18) 0.0303(19) 0.0324(15) -0.0087(14) 0.0020(14) 0.0030(15) N2 0.032(2) 0.0267(18) 0.0531(17) -0.0048(15) 0.0010(15) 0.0042(16) N3 0.0576(18) 0.0382(15) 0.0469(14) 0.007(2) -0.003(2) 0.004(2) N4 0.035(2) 0.0271(19) 0.0604(18) -0.0038(16) 0.0053(16) 0.0029(15) N5 0.0319(19) 0.0250(17) 0.0399(16) -0.0011(15) 0.0020(16) 0.0018(14) C1 0.025(2) 0.023(2) 0.0361(17) -0.0018(16) 0.0010(17) 0.0021(16) C2 0.034(2) 0.031(2) 0.0402(18) -0.0078(18) -0.0056(17) -0.003(2) C3 0.034(3) 0.023(2) 0.064(2) -0.0055(18) 0.003(2) 0.010(2) C4 0.039(3) 0.028(2) 0.046(2) -0.0162(18) -0.005(2) -0.001(2) C5 0.034(2) 0.022(2) 0.0382(18) -0.0003(19) -0.0041(18) -0.0046(19) C6 0.046(3) 0.033(2) 0.057(2) 0.004(2) -0.002(2) -0.003(2) C7 0.054(2) 0.044(2) 0.0419(16) -0.002(2) -0.001(2) -0.001(2) C8 0.026(2) 0.046(2) 0.0497(18) 0.003(2) 0.0075(16) -0.004(2) C9 0.048(3) 0.038(2) 0.035(2) -0.0003(18) -0.004(2) 0.002(2) C10 0.075(4) 0.041(3) 0.052(2) 0.004(2) 0.007(2) -0.001(3) C11 0.056(3) 0.041(3) 0.072(3) 0.010(2) 0.005(2) 0.016(2) C12 0.109(4) 0.051(3) 0.087(3) 0.006(2) -0.053(3) 0.004(3) C13 0.041(3) 0.042(2) 0.0293(19) -0.0044(18) 0.0129(19) -0.002(2) C14 0.042(3) 0.075(3) 0.075(3) -0.031(2) 0.006(3) -0.022(3) C15 0.050(3) 0.044(2) 0.055(2) -0.0235(19) 0.009(2) -0.020(2) C16 0.115(4) 0.053(3) 0.046(2) 0.005(2) -0.013(2) -0.046(3) C17 0.079(5) 0.065(7) 0.073(8) 0.025(5) 0.009(3) 0.017(5) C18 0.121(13) 0.077(4) 0.053(4) 0.017(3) 0.026(9) 0.054(13) C19 0.046(4) 0.048(4) 0.069(3) 0.028(3) 0.011(4) 0.005(3) C20 0.038(5) 0.020(4) 0.097(3) 0.006(3) 0.001(3) 0.002(3) C21 0.075(4) 0.054(7) 0.080(7) -0.035(6) -0.001(8) -0.004(9) C22 0.032(3) 0.032(3) 0.062(4) -0.005(3) -0.003(4) -0.001(2) C23 0.040(4) 0.034(3) 0.047(4) -0.004(3) -0.008(3) 0.007(3) C24 0.029(6) 0.031(4) 0.050(3) 0.000(3) 0.007(4) -0.014(3) C25 0.049(3) 0.047(5) 0.039(4) 0.008(3) 0.017(4) 0.019(5) C17A 0.079(5) 0.065(7) 0.073(8) 0.025(5) 0.009(3) 0.017(5) C18A 0.121(13) 0.077(4) 0.053(4) 0.017(3) 0.026(9) 0.054(13) C19A 0.046(4) 0.048(4) 0.069(3) 0.028(3) 0.011(4) 0.005(3) C20A 0.038(5) 0.020(4) 0.097(3) 0.006(3) 0.001(3) 0.002(3) C21A 0.075(4) 0.054(7) 0.080(7) -0.035(6) -0.001(8) -0.004(9) C22A 0.032(3) 0.032(3) 0.062(4) -0.005(3) -0.003(4) -0.001(2) C23A 0.040(4) 0.034(3) 0.047(4) -0.004(3) -0.008(3) 0.007(3) C24A 0.029(6) 0.031(4) 0.050(3) 0.000(3) 0.007(4) -0.014(3) C25A 0.049(3) 0.047(5) 0.039(4) 0.008(3) 0.017(4) 0.019(5) _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 N1 2.021(3) . ? Zn1 C13 2.028(4) . ? Zn1 C9 2.029(3) . ? Li1 N2 1.981(6) . ? Li1 N4 2.066(6) . ? Li1 N5 2.097(6) . ? Li1 N3 2.105(5) . ? Li1 C3 2.723(7) . ? Li1 C22 2.754(9) . ? Li1 C23 2.788(8) . ? N1 C4 1.338(4) . ? N1 C1 1.480(3) . ? N2 C2 1.281(4) . ? N2 C3 1.397(4) . ? N3 C17 1.465(7) . ? N3 C18 1.466(7) . ? N3 C18A 1.471(10) . ? N3 C17A 1.473(10) . ? N3 C19 1.475(5) . ? N3 C19A 1.510(8) . ? N4 C21 1.462(6) . ? N4 C21A 1.474(10) . ? N4 C22A 1.476(8) . ? N4 C20 1.478(6) . ? N4 C20A 1.482(9) . ? N4 C22 1.488(5) . ? N5 C25A 1.448(9) . ? N5 C24 1.451(6) . ? N5 C24A 1.459(9) . ? N5 C23 1.459(5) . ? N5 C25 1.490(6) . ? N5 C23A 1.492(9) . ? C1 C2 1.504(4) . ? C1 C5 1.557(4) . ? C1 H1 1.0000 . ? C2 H2 0.9500 . ? C3 C4 1.362(5) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.524(4) . ? C5 C8 1.531(4) . ? C5 C7 1.538(4) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C12 1.520(4) . ? C9 C10 1.521(5) . ? C9 C11 1.527(4) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C16 1.521(4) . ? C13 C14 1.527(5) . ? C13 C15 1.528(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C17 H17D 0.8531 . ? C17 H17E 0.9780 . ? C17 H17F 1.1623 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.516(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.506(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C17A H17A 0.9393 . ? C17A H17B 0.8741 . ? C17A H17C 1.1670 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A H18D 0.9800 . ? C18A H18E 0.9800 . ? C18A H18F 0.9800 . ? C19A C20A 1.525(9) . ? C19A H19C 0.9900 . ? C19A H19D 0.9900 . ? C20A H20C 0.9900 . ? C20A H20D 0.9900 . ? C21A H21D 0.9800 . ? C21A H21E 0.9800 . ? C21A H21F 0.9800 . ? C22A C23A 1.521(9) . ? C22A H22C 0.9900 . ? C22A H22D 0.9900 . ? C23A H23C 0.9900 . ? C23A H23D 0.9900 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? 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 N1 Zn1 C13 112.35(13) . . ? N1 Zn1 C9 112.98(13) . . ? C13 Zn1 C9 134.58(16) . . ? N2 Li1 N4 130.2(3) . . ? N2 Li1 N5 113.6(3) . . ? N4 Li1 N5 88.3(2) . . ? N2 Li1 N3 110.8(3) . . ? N4 Li1 N3 87.8(2) . . ? N5 Li1 N3 124.3(3) . . ? N2 Li1 C3 29.53(13) . . ? N4 Li1 C3 159.7(3) . . ? N5 Li1 C3 102.7(2) . . ? N3 Li1 C3 99.6(2) . . ? N2 Li1 C22 147.8(3) . . ? N4 Li1 C22 32.10(16) . . ? N5 Li1 C22 57.90(19) . . ? N3 Li1 C22 97.0(3) . . ? C3 Li1 C22 159.7(3) . . ? N2 Li1 C23 125.6(3) . . ? N4 Li1 C23 58.40(19) . . ? N5 Li1 C23 30.83(15) . . ? N3 Li1 C23 123.6(3) . . ? C3 Li1 C23 128.3(3) . . ? C22 Li1 C23 31.53(14) . . ? C4 N1 C1 116.1(3) . . ? C4 N1 Zn1 120.8(2) . . ? C1 N1 Zn1 123.0(2) . . ? C2 N2 C3 116.4(3) . . ? C2 N2 Li1 132.9(3) . . ? C3 N2 Li1 106.1(3) . . ? C17 N3 C18 104.6(16) . . ? C17 N3 C18A 122(2) . . ? C18 N3 C17A 97(3) . . ? C18A N3 C17A 116(3) . . ? C17 N3 C19 116.9(17) . . ? C18 N3 C19 108.3(8) . . ? C18A N3 C19 88.1(17) . . ? C17A N3 C19 123(4) . . ? C17 N3 C19A 88.0(16) . . ? C18 N3 C19A 132.2(12) . . ? C18A N3 C19A 116(2) . . ? C17A N3 C19A 95(3) . . ? C17 N3 Li1 106.2(17) . . ? C18 N3 Li1 118.0(13) . . ? C18A N3 Li1 118(3) . . ? C17A N3 Li1 108(3) . . ? C19 N3 Li1 103.5(3) . . ? C19A N3 Li1 101.3(6) . . ? C21 N4 C22A 88.5(8) . . ? C21A N4 C22A 107.0(17) . . ? C21 N4 C20 111.2(5) . . ? C21A N4 C20 88.3(11) . . ? C22A N4 C20 130.1(7) . . ? C21 N4 C20A 128.3(8) . . ? C21A N4 C20A 107.5(13) . . ? C22A N4 C20A 109.3(8) . . ? C21 N4 C22 113.3(8) . . ? C21A N4 C22 128.8(19) . . ? C20 N4 C22 111.3(4) . . ? C20A N4 C22 88.0(5) . . ? C21 N4 Li1 116.3(9) . . ? C21A N4 Li1 121(2) . . ? C22A N4 Li1 107.6(6) . . ? C20 N4 Li1 103.5(4) . . ? C20A N4 Li1 104.1(7) . . ? C22 N4 Li1 100.4(4) . . ? C25A N5 C24 131.7(7) . . ? C25A N5 C24A 114.5(9) . . ? C25A N5 C23 86.5(8) . . ? C24 N5 C23 112.4(5) . . ? C24A N5 C23 129.4(10) . . ? C24 N5 C25 105.9(4) . . ? C24A N5 C25 87.0(7) . . ? C23 N5 C25 109.4(4) . . ? C25A N5 C23A 113.1(9) . . ? C24 N5 C23A 88.5(5) . . ? C24A N5 C23A 108.5(8) . . ? C25 N5 C23A 131.9(7) . . ? C25A N5 Li1 101.7(8) . . ? C24 N5 Li1 115.9(5) . . ? C24A N5 Li1 116.5(11) . . ? C23 N5 Li1 101.8(3) . . ? C25 N5 Li1 111.4(4) . . ? C23A N5 Li1 101.9(6) . . ? N1 C1 C2 108.9(2) . . ? N1 C1 C5 112.7(2) . . ? C2 C1 C5 114.6(2) . . ? N1 C1 H1 106.7 . . ? C2 C1 H1 106.7 . . ? C5 C1 H1 106.7 . . ? N2 C2 C1 125.6(3) . . ? N2 C2 H2 117.2 . . ? C1 C2 H2 117.2 . . ? C4 C3 N2 119.6(3) . . ? C4 C3 Li1 148.3(3) . . ? C4 C3 H3 120.2 . . ? N2 C3 H3 120.2 . . ? Li1 C3 H3 82.3 . . ? N1 C4 C3 124.5(3) . . ? N1 C4 H4 117.7 . . ? C3 C4 H4 117.7 . . ? C6 C5 C8 108.4(3) . . ? C6 C5 C7 109.2(3) . . ? C8 C5 C7 108.8(3) . . ? C6 C5 C1 111.6(3) . . ? C8 C5 C1 110.2(2) . . ? C7 C5 C1 108.5(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C12 C9 C10 107.0(3) . . ? C12 C9 C11 109.6(3) . . ? C10 C9 C11 107.1(3) . . ? C12 C9 Zn1 109.7(2) . . ? C10 C9 Zn1 109.1(2) . . ? C11 C9 Zn1 114.1(2) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C14 107.6(3) . . ? C16 C13 C15 108.2(3) . . ? C14 C13 C15 106.5(3) . . ? C16 C13 Zn1 113.8(2) . . ? C14 C13 Zn1 108.4(2) . . ? C15 C13 Zn1 112.1(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N3 C17 H17A 107.5 . . ? N3 C17 H17B 110.9 . . ? H17A C17 H17B 109.5 . . ? N3 C17 H17C 110.0 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N3 C17 H17D 115.0 . . ? H17A C17 H17D 133.5 . . ? H17B C17 H17D 72.4 . . ? N3 C17 H17E 114.4 . . ? H17B C17 H17E 115.0 . . ? H17C C17 H17E 95.9 . . ? H17D C17 H17E 121.7 . . ? N3 C17 H17F 99.3 . . ? H17A C17 H17F 86.2 . . ? H17C C17 H17F 139.8 . . ? H17D C17 H17F 104.1 . . ? H17E C17 H17F 96.4 . . ? N3 C18 H18A 109.5 . . ? N3 C18 H18B 109.5 . . ? N3 C18 H18C 109.5 . . ? N3 C19 C20 109.1(5) . . ? N3 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? N3 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N4 C20 C19 114.2(5) . . ? N4 C20 H20A 108.7 . . ? C19 C20 H20A 108.7 . . ? N4 C20 H20B 108.7 . . ? C19 C20 H20B 108.7 . . ? H20A C20 H20B 107.6 . . ? N4 C21 H21A 109.5 . . ? N4 C21 H21B 109.5 . . ? N4 C21 H21C 109.5 . . ? N4 C22 C23 109.8(5) . . ? N4 C22 Li1 47.5(3) . . ? C23 C22 Li1 75.5(4) . . ? N4 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? Li1 C22 H22A 92.3 . . ? N4 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? Li1 C22 H22B 154.7 . . ? H22A C22 H22B 108.2 . . ? N5 C23 C22 109.2(5) . . ? N5 C23 Li1 47.4(3) . . ? C22 C23 Li1 73.0(4) . . ? N5 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? Li1 C23 H23A 95.1 . . ? N5 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? Li1 C23 H23B 153.0 . . ? H23A C23 H23B 108.3 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? N5 C25 H25C 109.5 . . ? N3 C17A H17A 109.3 . . ? N3 C17A H17B 117.8 . . ? H17A C17A H17B 123.9 . . ? N3 C17A H17C 99.3 . . ? H17A C17A H17C 98.3 . . ? H17B C17A H17C 102.3 . . ? N3 C17A H17D 106.1 . . ? H17A C17A H17D 122.8 . . ? H17B C17A H17D 71.5 . . ? N3 C17A H17E 113.7 . . ? H17B C17A H17E 125.9 . . ? H17C C17A H17E 84.7 . . ? H17D C17A H17E 109.5 . . ? N3 C17A H17F 108.6 . . ? H17A C17A H17F 99.9 . . ? H17C C17A H17F 139.1 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? N3 C18A H18D 109.5 . . ? N3 C18A H18E 109.5 . . ? H18D C18A H18E 109.5 . . ? N3 C18A H18F 109.5 . . ? H18D C18A H18F 109.5 . . ? H18E C18A H18F 109.5 . . ? N3 C19A C20A 110.2(10) . . ? N3 C19A H19C 109.6 . . ? C20A C19A H19C 109.6 . . ? N3 C19A H19D 109.6 . . ? C20A C19A H19D 109.6 . . ? H19C C19A H19D 108.1 . . ? N4 C20A C19A 108.0(10) . . ? N4 C20A H20C 110.1 . . ? C19A C20A H20C 110.1 . . ? N4 C20A H20D 110.1 . . ? C19A C20A H20D 110.1 . . ? H20C C20A H20D 108.4 . . ? N4 C21A H21D 109.5 . . ? N4 C21A H21E 109.5 . . ? H21D C21A H21E 109.5 . . ? N4 C21A H21F 109.5 . . ? H21D C21A H21F 109.5 . . ? H21E C21A H21F 109.5 . . ? N4 C22A C23A 110.3(10) . . ? N4 C22A H22C 109.6 . . ? C23A C22A H22C 109.6 . . ? N4 C22A H22D 109.6 . . ? C23A C22A H22D 109.6 . . ? H22C C22A H22D 108.1 . . ? N5 C23A C22A 116.0(11) . . ? N5 C23A H23C 108.3 . . ? C22A C23A H23C 108.3 . . ? N5 C23A H23D 108.3 . . ? C22A C23A H23D 108.3 . . ? H23C C23A H23D 107.4 . . ? N5 C24A H24D 109.5 . . ? N5 C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? N5 C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? N5 C25A H25D 109.5 . . ? N5 C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? N5 C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 Zn1 N1 C4 -45.4(3) . . . . ? C9 Zn1 N1 C4 131.7(3) . . . . ? C13 Zn1 N1 C1 137.3(2) . . . . ? C9 Zn1 N1 C1 -45.6(2) . . . . ? N4 Li1 N2 C2 -23.5(6) . . . . ? N5 Li1 N2 C2 -132.6(4) . . . . ? N3 Li1 N2 C2 81.9(4) . . . . ? C3 Li1 N2 C2 154.0(5) . . . . ? C22 Li1 N2 C2 -65.9(7) . . . . ? C23 Li1 N2 C2 -99.7(5) . . . . ? N4 Li1 N2 C3 -177.5(3) . . . . ? N5 Li1 N2 C3 73.4(3) . . . . ? N3 Li1 N2 C3 -72.0(3) . . . . ? C22 Li1 N2 C3 140.2(6) . . . . ? C23 Li1 N2 C3 106.3(3) . . . . ? N2 Li1 N3 C17 -27.3(16) . . . . ? N4 Li1 N3 C17 105.3(16) . . . . ? N5 Li1 N3 C17 -168.3(16) . . . . ? C3 Li1 N3 C17 -55.7(16) . . . . ? C22 Li1 N3 C17 136.1(16) . . . . ? C23 Li1 N3 C17 154.3(16) . . . . ? N2 Li1 N3 C18 89.5(7) . . . . ? N4 Li1 N3 C18 -137.9(7) . . . . ? N5 Li1 N3 C18 -51.5(8) . . . . ? C3 Li1 N3 C18 61.1(7) . . . . ? C22 Li1 N3 C18 -107.1(7) . . . . ? C23 Li1 N3 C18 -88.8(7) . . . . ? N2 Li1 N3 C18A 114.0(17) . . . . ? N4 Li1 N3 C18A -113.4(17) . . . . ? N5 Li1 N3 C18A -27.0(17) . . . . ? C3 Li1 N3 C18A 85.6(17) . . . . ? C22 Li1 N3 C18A -82.6(17) . . . . ? C23 Li1 N3 C18A -64.4(18) . . . . ? N2 Li1 N3 C17A -19(3) . . . . ? N4 Li1 N3 C17A 113(3) . . . . ? N5 Li1 N3 C17A -160(3) . . . . ? C3 Li1 N3 C17A -48(3) . . . . ? C22 Li1 N3 C17A 144(3) . . . . ? C23 Li1 N3 C17A 162(3) . . . . ? N2 Li1 N3 C19 -151.0(4) . . . . ? N4 Li1 N3 C19 -18.4(4) . . . . ? N5 Li1 N3 C19 68.0(5) . . . . ? C3 Li1 N3 C19 -179.4(3) . . . . ? C22 Li1 N3 C19 12.4(4) . . . . ? C23 Li1 N3 C19 30.7(5) . . . . ? N2 Li1 N3 C19A -118.5(6) . . . . ? N4 Li1 N3 C19A 14.1(6) . . . . ? N5 Li1 N3 C19A 100.5(6) . . . . ? C3 Li1 N3 C19A -146.9(6) . . . . ? C22 Li1 N3 C19A 44.9(6) . . . . ? C23 Li1 N3 C19A 63.1(7) . . . . ? N2 Li1 N4 C21 -14.9(7) . . . . ? N5 Li1 N4 C21 105.1(6) . . . . ? N3 Li1 N4 C21 -130.5(6) . . . . ? C3 Li1 N4 C21 -18.5(10) . . . . ? C22 Li1 N4 C21 122.7(6) . . . . ? C23 Li1 N4 C21 97.1(6) . . . . ? N2 Li1 N4 C21A 11.1(14) . . . . ? N5 Li1 N4 C21A 131.0(13) . . . . ? N3 Li1 N4 C21A -104.5(13) . . . . ? C3 Li1 N4 C21A 7.5(16) . . . . ? C22 Li1 N4 C21A 148.6(13) . . . . ? C23 Li1 N4 C21A 123.1(14) . . . . ? N2 Li1 N4 C22A -112.1(7) . . . . ? N5 Li1 N4 C22A 7.8(7) . . . . ? N3 Li1 N4 C22A 132.3(7) . . . . ? C3 Li1 N4 C22A -115.7(10) . . . . ? C22 Li1 N4 C22A 25.4(6) . . . . ? C23 Li1 N4 C22A -0.1(7) . . . . ? N2 Li1 N4 C20 107.3(4) . . . . ? N5 Li1 N4 C20 -132.7(3) . . . . ? N3 Li1 N4 C20 -8.3(4) . . . . ? C3 Li1 N4 C20 103.8(8) . . . . ? C22 Li1 N4 C20 -115.1(4) . . . . ? C23 Li1 N4 C20 -140.6(4) . . . . ? N2 Li1 N4 C20A 131.9(6) . . . . ? N5 Li1 N4 C20A -108.1(6) . . . . ? N3 Li1 N4 C20A 16.3(6) . . . . ? C3 Li1 N4 C20A 128.3(9) . . . . ? C22 Li1 N4 C20A -90.5(6) . . . . ? C23 Li1 N4 C20A -116.0(6) . . . . ? N2 Li1 N4 C22 -137.6(4) . . . . ? N5 Li1 N4 C22 -17.6(3) . . . . ? N3 Li1 N4 C22 106.8(3) . . . . ? C3 Li1 N4 C22 -141.1(7) . . . . ? C23 Li1 N4 C22 -25.5(4) . . . . ? N2 Li1 N5 C25A 31.7(8) . . . . ? N4 Li1 N5 C25A -102.1(7) . . . . ? N3 Li1 N5 C25A 171.8(8) . . . . ? C3 Li1 N5 C25A 60.7(8) . . . . ? C22 Li1 N5 C25A -113.0(8) . . . . ? C23 Li1 N5 C25A -88.8(7) . . . . ? N2 Li1 N5 C24 -117.2(4) . . . . ? N4 Li1 N5 C24 109.0(4) . . . . ? N3 Li1 N5 C24 22.9(5) . . . . ? C3 Li1 N5 C24 -88.2(4) . . . . ? C22 Li1 N5 C24 98.1(4) . . . . ? C23 Li1 N5 C24 122.3(4) . . . . ? N2 Li1 N5 C24A -93.5(7) . . . . ? N4 Li1 N5 C24A 132.7(7) . . . . ? N3 Li1 N5 C24A 46.5(8) . . . . ? C3 Li1 N5 C24A -64.6(7) . . . . ? C22 Li1 N5 C24A 121.8(7) . . . . ? C23 Li1 N5 C24A 145.9(8) . . . . ? N2 Li1 N5 C23 120.5(4) . . . . ? N4 Li1 N5 C23 -13.3(4) . . . . ? N3 Li1 N5 C23 -99.4(4) . . . . ? C3 Li1 N5 C23 149.5(3) . . . . ? C22 Li1 N5 C23 -24.2(4) . . . . ? N2 Li1 N5 C25 4.1(4) . . . . ? N4 Li1 N5 C25 -129.7(3) . . . . ? N3 Li1 N5 C25 144.1(4) . . . . ? C3 Li1 N5 C25 33.0(4) . . . . ? C22 Li1 N5 C25 -140.7(4) . . . . ? C23 Li1 N5 C25 -116.5(4) . . . . ? N2 Li1 N5 C23A 148.6(6) . . . . ? N4 Li1 N5 C23A 14.9(6) . . . . ? N3 Li1 N5 C23A -71.3(6) . . . . ? C3 Li1 N5 C23A 177.6(6) . . . . ? C22 Li1 N5 C23A 3.9(6) . . . . ? C23 Li1 N5 C23A 28.1(5) . . . . ? C4 N1 C1 C2 -29.8(3) . . . . ? Zn1 N1 C1 C2 147.6(2) . . . . ? C4 N1 C1 C5 98.6(3) . . . . ? Zn1 N1 C1 C5 -84.0(3) . . . . ? C3 N2 C2 C1 -8.2(5) . . . . ? Li1 N2 C2 C1 -160.1(3) . . . . ? N1 C1 C2 N2 29.7(4) . . . . ? C5 C1 C2 N2 -97.6(4) . . . . ? C2 N2 C3 C4 -14.0(4) . . . . ? Li1 N2 C3 C4 145.0(3) . . . . ? C2 N2 C3 Li1 -159.0(4) . . . . ? N2 Li1 C3 C4 -71.8(5) . . . . ? N4 Li1 C3 C4 -66.2(10) . . . . ? N5 Li1 C3 C4 172.4(5) . . . . ? N3 Li1 C3 C4 43.8(6) . . . . ? C22 Li1 C3 C4 -172.0(7) . . . . ? C23 Li1 C3 C4 -168.2(5) . . . . ? N4 Li1 C3 N2 5.6(7) . . . . ? N5 Li1 C3 N2 -115.8(3) . . . . ? N3 Li1 C3 N2 115.6(3) . . . . ? C22 Li1 C3 N2 -100.2(8) . . . . ? C23 Li1 C3 N2 -96.5(4) . . . . ? C1 N1 C4 C3 12.6(5) . . . . ? Zn1 N1 C4 C3 -164.9(3) . . . . ? N2 C3 C4 N1 11.7(5) . . . . ? Li1 C3 C4 N1 61.5(7) . . . . ? N1 C1 C5 C6 -61.5(3) . . . . ? C2 C1 C5 C6 63.9(4) . . . . ? N1 C1 C5 C8 59.1(3) . . . . ? C2 C1 C5 C8 -175.6(3) . . . . ? N1 C1 C5 C7 178.1(2) . . . . ? C2 C1 C5 C7 -56.6(3) . . . . ? N1 Zn1 C9 C12 -159.2(3) . . . . ? C13 Zn1 C9 C12 17.0(4) . . . . ? N1 Zn1 C9 C10 -42.4(3) . . . . ? C13 Zn1 C9 C10 133.9(2) . . . . ? N1 Zn1 C9 C11 77.4(3) . . . . ? C13 Zn1 C9 C11 -106.4(3) . . . . ? N1 Zn1 C13 C16 -33.6(3) . . . . ? C9 Zn1 C13 C16 150.1(3) . . . . ? N1 Zn1 C13 C14 -153.3(2) . . . . ? C9 Zn1 C13 C14 30.5(3) . . . . ? N1 Zn1 C13 C15 89.5(3) . . . . ? C9 Zn1 C13 C15 -86.8(3) . . . . ? C17 N3 C19 C20 -75.4(17) . . . . ? C18 N3 C19 C20 166.9(13) . . . . ? C18A N3 C19 C20 159(3) . . . . ? C17A N3 C19 C20 -81(4) . . . . ? C19A N3 C19 C20 -48.8(11) . . . . ? Li1 N3 C19 C20 41.0(6) . . . . ? C21 N4 C20 C19 160.5(11) . . . . ? C21A N4 C20 C19 156(2) . . . . ? C22A N4 C20 C19 -92.6(9) . . . . ? C20A N4 C20 C19 -59.5(18) . . . . ? C22 N4 C20 C19 -72.1(8) . . . . ? Li1 N4 C20 C19 34.9(7) . . . . ? N3 C19 C20 N4 -54.6(9) . . . . ? C21 N4 C22 C23 -78.5(10) . . . . ? C21A N4 C22 C23 -98.8(19) . . . . ? C22A N4 C22 C23 -63.0(17) . . . . ? C20 N4 C22 C23 155.3(5) . . . . ? C20A N4 C22 C23 150.2(10) . . . . ? Li1 N4 C22 C23 46.2(6) . . . . ? C21 N4 C22 Li1 -124.7(8) . . . . ? C21A N4 C22 Li1 -145.0(18) . . . . ? C22A N4 C22 Li1 -109.2(19) . . . . ? C20 N4 C22 Li1 109.1(4) . . . . ? C20A N4 C22 Li1 104.0(7) . . . . ? N2 Li1 C22 N4 75.4(6) . . . . ? N5 Li1 C22 N4 159.1(4) . . . . ? N3 Li1 C22 N4 -74.5(3) . . . . ? C3 Li1 C22 N4 141.1(7) . . . . ? C23 Li1 C22 N4 135.4(6) . . . . ? N2 Li1 C22 C23 -60.0(8) . . . . ? N4 Li1 C22 C23 -135.4(6) . . . . ? N5 Li1 C22 C23 23.7(4) . . . . ? N3 Li1 C22 C23 150.1(5) . . . . ? C3 Li1 C22 C23 5.6(10) . . . . ? C25A N5 C23 C22 143.5(9) . . . . ? C24 N5 C23 C22 -82.4(8) . . . . ? C24A N5 C23 C22 -97.3(13) . . . . ? C25 N5 C23 C22 160.2(6) . . . . ? C23A N5 C23 C22 -50.9(14) . . . . ? Li1 N5 C23 C22 42.2(6) . . . . ? C25A N5 C23 Li1 101.3(7) . . . . ? C24 N5 C23 Li1 -124.7(5) . . . . ? C24A N5 C23 Li1 -139.5(12) . . . . ? C25 N5 C23 Li1 117.9(4) . . . . ? C23A N5 C23 Li1 -93.1(16) . . . . ? N4 C22 C23 N5 -64.6(8) . . . . ? Li1 C22 C23 N5 -31.2(5) . . . . ? N4 C22 C23 Li1 -33.4(4) . . . . ? N2 Li1 C23 N5 -76.1(5) . . . . ? N4 Li1 C23 N5 164.4(4) . . . . ? N3 Li1 C23 N5 102.0(4) . . . . ? C3 Li1 C23 N5 -39.1(4) . . . . ? C22 Li1 C23 N5 138.4(6) . . . . ? N2 Li1 C23 C22 145.4(5) . . . . ? N4 Li1 C23 C22 26.0(4) . . . . ? N5 Li1 C23 C22 -138.4(6) . . . . ? N3 Li1 C23 C22 -36.4(6) . . . . ? C3 Li1 C23 C22 -177.5(4) . . . . ? C17 N3 C19A C20A -148.7(19) . . . . ? C18 N3 C19A C20A 103.3(17) . . . . ? C18A N3 C19A C20A 86(3) . . . . ? C17A N3 C19A C20A -152(3) . . . . ? C19 N3 C19A C20A 54.8(10) . . . . ? Li1 N3 C19A C20A -42.6(12) . . . . ? C21 N4 C20A C19A 97.5(16) . . . . ? C21A N4 C20A C19A 86(2) . . . . ? C22A N4 C20A C19A -158.6(10) . . . . ? C20 N4 C20A C19A 47.7(14) . . . . ? C22 N4 C20A C19A -144.0(12) . . . . ? Li1 N4 C20A C19A -43.9(12) . . . . ? N3 C19A C20A N4 61.7(16) . . . . ? C21 N4 C22A C23A -146.2(14) . . . . ? C21A N4 C22A C23A -160(2) . . . . ? C20 N4 C22A C23A 97.0(13) . . . . ? C20A N4 C22A C23A 83.5(16) . . . . ? C22 N4 C22A C23A 48.0(12) . . . . ? Li1 N4 C22A C23A -29.0(14) . . . . ? C25A N5 C23A C22A 71.6(16) . . . . ? C24 N5 C23A C22A -153.0(13) . . . . ? C24A N5 C23A C22A -160.2(15) . . . . ? C23 N5 C23A C22A 56.0(12) . . . . ? C25 N5 C23A C22A 96.8(14) . . . . ? Li1 N5 C23A C22A -36.7(13) . . . . ? N4 C22A C23A N5 47.0(18) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.801 _refine_diff_density_min -0.353 _refine_diff_density_rms 0.048 #===END data_vb24 _database_code_depnum_ccdc_archive 'CCDC 853496' #TrackingRef '- CIF.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H70 N8 Zn3' _chemical_formula_sum 'C40 H70 N8 Zn3' _chemical_formula_weight 859.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Zn Zn 0.2839 1.4301 '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' 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.469(2) _cell_length_b 12.6321(5) _cell_length_c 16.5424(11) _cell_angle_alpha 90.00 _cell_angle_beta 125.028(10) _cell_angle_gamma 90.00 _cell_volume 4700.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 4386 _cell_measurement_theta_min 2.9382 _cell_measurement_theta_max 30.0669 _exptl_crystal_description 'cut needle' _exptl_crystal_colour red _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1824 _exptl_absorpt_coefficient_mu 1.552 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.93531 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Oxford Diffraction Xcalibur, E' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15271 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0607 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 29.00 _reflns_number_total 6041 _reflns_number_gt 4389 _reflns_threshold_expression I>2\s(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET) (compiled Aug 27 2010,11:50:40) ; _computing_structure_solution ? _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^)+(0.0313P)^2^+0.4997P] 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 6041 _refine_ls_number_parameters 240 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0682 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0840 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 0.186457(11) 0.89879(2) 0.278635(18) 0.02130(8) Uani 1 1 d . . . Zn2 Zn 0.0000 0.46526(3) 0.2500 0.02214(10) Uani 1 2 d S . . N1 N 0.05817(8) 0.59680(15) 0.24946(13) 0.0238(4) Uani 1 1 d . . . N2 N 0.12783(8) 0.75414(15) 0.24336(13) 0.0230(4) Uani 1 1 d . . . N3 N 0.11798(8) 0.97062(16) 0.12929(13) 0.0242(4) Uani 1 1 d . . . N4 N 0.03990(8) 1.07071(18) -0.05234(14) 0.0318(5) Uani 1 1 d . . . C1 C 0.03500(10) 0.6860(2) 0.19849(16) 0.0278(6) Uani 1 1 d . . . H1 H -0.0068 0.6958 0.1616 0.033 Uiso 1 1 calc R . . C2 C 0.06911(10) 0.7648(2) 0.19693(16) 0.0274(5) Uani 1 1 d . . . H2 H 0.0504 0.8284 0.1620 0.033 Uiso 1 1 calc R . . C3 C 0.15140(10) 0.66351(18) 0.29173(16) 0.0235(5) Uani 1 1 d . . . H3 H 0.1928 0.6517 0.3244 0.028 Uiso 1 1 calc R . . C4 C 0.11693(10) 0.58582(18) 0.29558(16) 0.0243(5) Uani 1 1 d . . . H4 H 0.1357 0.5230 0.3321 0.029 Uiso 1 1 calc R . . C5 C 0.08442(10) 0.9164(2) 0.04490(16) 0.0268(5) Uani 1 1 d . . . H5 H 0.0871 0.8413 0.0465 0.032 Uiso 1 1 calc R . . C6 C 0.04613(10) 0.9664(2) -0.04420(17) 0.0294(6) Uani 1 1 d . . . H6 H 0.0233 0.9244 -0.1021 0.035 Uiso 1 1 calc R . . C7 C 0.07436(10) 1.1246(2) 0.03139(17) 0.0323(6) Uani 1 1 d . . . H7 H 0.0722 1.1997 0.0292 0.039 Uiso 1 1 calc R . . C8 C 0.11300(10) 1.07587(19) 0.12115(17) 0.0271(5) Uani 1 1 d . . . H8 H 0.1367 1.1182 0.1786 0.032 Uiso 1 1 calc R . . C9 C 0.25188(10) 0.86232(18) 0.26259(16) 0.0238(5) Uani 1 1 d . . . C10 C 0.23255(12) 0.7907(2) 0.17445(19) 0.0402(7) Uani 1 1 d . . . H10A H 0.2018 0.8264 0.1133 0.060 Uiso 1 1 calc R . . H10B H 0.2167 0.7243 0.1810 0.060 Uiso 1 1 calc R . . H10C H 0.2669 0.7754 0.1725 0.060 Uiso 1 1 calc R . . C11 C 0.30341(11) 0.8080(2) 0.35559(19) 0.0398(7) Uani 1 1 d . . . H11A H 0.2909 0.7376 0.3617 0.060 Uiso 1 1 calc R . . H11B H 0.3151 0.8505 0.4137 0.060 Uiso 1 1 calc R . . H11C H 0.3373 0.8012 0.3510 0.060 Uiso 1 1 calc R . . C12 C 0.27535(11) 0.9655(2) 0.24896(19) 0.0350(6) Uani 1 1 d . . . H12A H 0.3079 0.9499 0.2424 0.052 Uiso 1 1 calc R . . H12B H 0.2900 1.0113 0.3064 0.052 Uiso 1 1 calc R . . H12C H 0.2432 1.0016 0.1893 0.052 Uiso 1 1 calc R . . C13 C 0.18079(12) 0.9683(2) 0.38332(18) 0.0325(6) Uani 1 1 d . . . C14 C 0.23724(17) 1.0355(3) 0.4480(2) 0.0720(12) Uani 1 1 d . . . H14A H 0.2375 1.0929 0.4083 0.108 Uiso 1 1 calc R . . H14B H 0.2724 0.9908 0.4737 0.108 Uiso 1 1 calc R . . H14C H 0.2378 1.0657 0.5031 0.108 Uiso 1 1 calc R . . C15 C 0.12718(17) 1.0390(3) 0.3456(2) 0.0744(12) Uani 1 1 d . . . H15A H 0.0907 0.9973 0.3047 0.112 Uiso 1 1 calc R . . H15B H 0.1274 1.0964 0.3059 0.112 Uiso 1 1 calc R . . H15C H 0.1288 1.0691 0.4016 0.112 Uiso 1 1 calc R . . C16 C 0.18024(14) 0.8851(2) 0.44894(19) 0.0468(8) Uani 1 1 d . . . H16A H 0.1816 0.9199 0.5031 0.070 Uiso 1 1 calc R . . H16B H 0.2149 0.8389 0.4760 0.070 Uiso 1 1 calc R . . H16C H 0.1438 0.8429 0.4101 0.070 Uiso 1 1 calc R . . C17 C 0.04159(11) 0.4077(2) 0.38798(19) 0.0379(7) Uani 1 1 d . . . C18 C -0.00421(13) 0.3457(3) 0.3943(2) 0.0544(9) Uani 1 1 d . . . H18A H 0.0153 0.3149 0.4603 0.082 Uiso 1 1 calc R . . H18B H -0.0212 0.2890 0.3449 0.082 Uiso 1 1 calc R . . H18C H -0.0359 0.3936 0.3817 0.082 Uiso 1 1 calc R . . C19 C 0.09003(13) 0.3297(3) 0.4080(3) 0.0698(11) Uani 1 1 d . . . H19A H 0.1199 0.3670 0.4041 0.105 Uiso 1 1 calc R . . H19B H 0.0722 0.2730 0.3587 0.105 Uiso 1 1 calc R . . H19C H 0.1090 0.2993 0.4741 0.105 Uiso 1 1 calc R . . C20 C 0.06907(15) 0.4912(3) 0.46821(19) 0.0713(12) Uani 1 1 d . . . H20A H 0.0894 0.4569 0.5329 0.107 Uiso 1 1 calc R . . H20B H 0.0378 0.5379 0.4592 0.107 Uiso 1 1 calc R . . H20C H 0.0978 0.5330 0.4644 0.107 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 0.02376(15) 0.02200(15) 0.02066(13) 0.00357(11) 0.01422(12) 0.00139(11) Zn2 0.0205(2) 0.0197(2) 0.02477(19) 0.000 0.01215(16) 0.000 N1 0.0226(10) 0.0256(11) 0.0240(9) 0.0030(9) 0.0138(8) -0.0018(8) N2 0.0240(10) 0.0212(11) 0.0256(10) 0.0023(8) 0.0153(8) 0.0014(8) N3 0.0243(10) 0.0245(11) 0.0250(10) 0.0031(9) 0.0147(9) 0.0012(8) N4 0.0222(11) 0.0428(14) 0.0271(11) 0.0067(10) 0.0121(9) 0.0049(9) C1 0.0159(12) 0.0362(15) 0.0279(12) 0.0090(11) 0.0105(10) 0.0017(10) C2 0.0251(13) 0.0283(14) 0.0282(12) 0.0102(11) 0.0149(11) 0.0060(10) C3 0.0187(12) 0.0233(13) 0.0289(12) 0.0030(10) 0.0139(10) 0.0029(9) C4 0.0253(13) 0.0203(13) 0.0289(12) 0.0063(10) 0.0165(10) 0.0047(10) C5 0.0283(13) 0.0261(14) 0.0295(12) -0.0003(11) 0.0186(11) -0.0008(10) C6 0.0231(13) 0.0384(16) 0.0250(12) -0.0022(12) 0.0129(10) -0.0019(11) C7 0.0317(14) 0.0276(15) 0.0338(14) 0.0073(11) 0.0165(12) 0.0048(11) C8 0.0265(13) 0.0251(13) 0.0245(12) 0.0004(10) 0.0116(10) -0.0016(10) C9 0.0248(12) 0.0189(12) 0.0318(12) 0.0016(10) 0.0187(11) -0.0011(9) C10 0.0509(17) 0.0374(17) 0.0491(16) -0.0113(13) 0.0385(14) -0.0070(13) C11 0.0316(15) 0.0368(16) 0.0515(16) 0.0121(13) 0.0241(13) 0.0077(12) C12 0.0345(15) 0.0295(15) 0.0482(15) 0.0061(13) 0.0280(13) -0.0014(12) C13 0.0467(16) 0.0313(15) 0.0332(13) 0.0012(12) 0.0309(13) 0.0012(12) C14 0.110(3) 0.074(3) 0.066(2) -0.042(2) 0.070(2) -0.045(2) C15 0.117(3) 0.079(3) 0.074(2) 0.029(2) 0.082(2) 0.056(2) C16 0.070(2) 0.0482(19) 0.0351(14) 0.0037(14) 0.0374(15) 0.0004(15) C17 0.0265(14) 0.0434(18) 0.0381(14) 0.0173(13) 0.0153(12) 0.0019(12) C18 0.0457(19) 0.065(2) 0.0587(19) 0.0314(17) 0.0338(16) 0.0083(16) C19 0.046(2) 0.075(3) 0.092(2) 0.060(2) 0.0422(19) 0.0254(18) C20 0.069(2) 0.094(3) 0.0231(14) 0.0100(17) 0.0102(15) -0.018(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 C9 2.015(2) . ? Zn1 C13 2.026(2) . ? Zn1 N3 2.2650(18) . ? Zn1 N2 2.2791(19) . ? Zn2 C17 2.013(2) . ? Zn2 C17 2.013(2) 2 ? Zn2 N1 2.3087(19) . ? Zn2 N1 2.3087(19) 2 ? N1 C1 1.330(3) . ? N1 C4 1.339(3) . ? N2 C3 1.332(3) . ? N2 C2 1.337(3) . ? N3 C8 1.335(3) . ? N3 C5 1.338(3) . ? N4 C6 1.326(3) . ? N4 C7 1.332(3) . ? C1 C2 1.378(3) . ? C1 H1 0.9500 . ? C2 H2 0.9500 . ? C3 C4 1.390(3) . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C6 1.378(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.379(3) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C9 C12 1.528(3) . ? C9 C10 1.529(3) . ? C9 C11 1.530(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.517(4) . ? C13 C16 1.517(3) . ? C13 C14 1.538(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C20 1.515(4) . ? C17 C19 1.531(4) . ? C17 C18 1.535(4) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? 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 C9 Zn1 C13 136.36(10) . . ? C9 Zn1 N3 101.13(8) . . ? C13 Zn1 N3 109.60(9) . . ? C9 Zn1 N2 109.61(8) . . ? C13 Zn1 N2 100.18(9) . . ? N3 Zn1 N2 91.12(7) . . ? C17 Zn2 C17 137.65(17) . 2 ? C17 Zn2 N1 108.71(9) . . ? C17 Zn2 N1 101.49(9) 2 . ? C17 Zn2 N1 101.49(9) . 2 ? C17 Zn2 N1 108.71(9) 2 2 ? N1 Zn2 N1 87.94(10) . 2 ? C1 N1 C4 115.50(19) . . ? C1 N1 Zn2 122.13(15) . . ? C4 N1 Zn2 122.27(15) . . ? C3 N2 C2 116.2(2) . . ? C3 N2 Zn1 120.45(15) . . ? C2 N2 Zn1 120.54(15) . . ? C8 N3 C5 115.81(19) . . ? C8 N3 Zn1 118.80(15) . . ? C5 N3 Zn1 125.18(16) . . ? C6 N4 C7 115.4(2) . . ? N1 C1 C2 122.8(2) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? N2 C2 C1 121.7(2) . . ? N2 C2 H2 119.2 . . ? C1 C2 H2 119.2 . . ? N2 C3 C4 121.7(2) . . ? N2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? N1 C4 C3 122.1(2) . . ? N1 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? N3 C5 C6 121.8(2) . . ? N3 C5 H5 119.1 . . ? C6 C5 H5 119.1 . . ? N4 C6 C5 122.6(2) . . ? N4 C6 H6 118.7 . . ? C5 C6 H6 118.7 . . ? N4 C7 C8 122.7(2) . . ? N4 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? N3 C8 C7 121.6(2) . . ? N3 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C12 C9 C10 108.02(19) . . ? C12 C9 C11 107.8(2) . . ? C10 C9 C11 107.9(2) . . ? C12 C9 Zn1 107.95(16) . . ? C10 C9 Zn1 114.40(16) . . ? C11 C9 Zn1 110.51(16) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C16 107.2(2) . . ? C15 C13 C14 108.3(3) . . ? C16 C13 C14 107.7(2) . . ? C15 C13 Zn1 115.85(18) . . ? C16 C13 Zn1 110.40(18) . . ? C14 C13 Zn1 107.00(18) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C20 C17 C19 108.9(3) . . ? C20 C17 C18 108.1(2) . . ? C19 C17 C18 107.5(2) . . ? C20 C17 Zn2 114.5(2) . . ? C19 C17 Zn2 109.6(2) . . ? C18 C17 Zn2 107.91(17) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 Zn2 N1 C1 -139.27(19) . . . . ? C17 Zn2 N1 C1 70.84(19) 2 . . . ? N1 Zn2 N1 C1 -37.84(15) 2 . . . ? C17 Zn2 N1 C4 44.75(19) . . . . ? C17 Zn2 N1 C4 -105.13(18) 2 . . . ? N1 Zn2 N1 C4 146.19(19) 2 . . . ? C9 Zn1 N2 C3 56.34(18) . . . . ? C13 Zn1 N2 C3 -91.28(18) . . . . ? N3 Zn1 N2 C3 158.58(17) . . . . ? C9 Zn1 N2 C2 -143.24(16) . . . . ? C13 Zn1 N2 C2 69.15(18) . . . . ? N3 Zn1 N2 C2 -41.00(16) . . . . ? C9 Zn1 N3 C8 -101.33(18) . . . . ? C13 Zn1 N3 C8 47.22(19) . . . . ? N2 Zn1 N3 C8 148.44(18) . . . . ? C9 Zn1 N3 C5 73.09(19) . . . . ? C13 Zn1 N3 C5 -138.37(19) . . . . ? N2 Zn1 N3 C5 -37.15(18) . . . . ? C4 N1 C1 C2 -3.3(3) . . . . ? Zn2 N1 C1 C2 -179.53(17) . . . . ? C3 N2 C2 C1 -0.5(3) . . . . ? Zn1 N2 C2 C1 -161.75(18) . . . . ? N1 C1 C2 N2 3.2(4) . . . . ? C2 N2 C3 C4 -1.6(3) . . . . ? Zn1 N2 C3 C4 159.65(17) . . . . ? C1 N1 C4 C3 1.1(3) . . . . ? Zn2 N1 C4 C3 177.35(16) . . . . ? N2 C3 C4 N1 1.3(4) . . . . ? C8 N3 C5 C6 -1.5(3) . . . . ? Zn1 N3 C5 C6 -176.11(17) . . . . ? C7 N4 C6 C5 1.6(4) . . . . ? N3 C5 C6 N4 -0.1(4) . . . . ? C6 N4 C7 C8 -1.5(4) . . . . ? C5 N3 C8 C7 1.7(3) . . . . ? Zn1 N3 C8 C7 176.60(18) . . . . ? N4 C7 C8 N3 -0.2(4) . . . . ? C13 Zn1 C9 C12 -70.3(2) . . . . ? N3 Zn1 C9 C12 64.24(16) . . . . ? N2 Zn1 C9 C12 159.47(14) . . . . ? C13 Zn1 C9 C10 169.39(17) . . . . ? N3 Zn1 C9 C10 -56.04(18) . . . . ? N2 Zn1 C9 C10 39.20(19) . . . . ? C13 Zn1 C9 C11 47.3(2) . . . . ? N3 Zn1 C9 C11 -178.09(16) . . . . ? N2 Zn1 C9 C11 -82.85(17) . . . . ? C9 Zn1 C13 C15 142.6(2) . . . . ? N3 Zn1 C13 C15 10.5(3) . . . . ? N2 Zn1 C13 C15 -84.4(2) . . . . ? C9 Zn1 C13 C16 -95.3(2) . . . . ? N3 Zn1 C13 C16 132.61(18) . . . . ? N2 Zn1 C13 C16 37.7(2) . . . . ? C9 Zn1 C13 C14 21.7(3) . . . . ? N3 Zn1 C13 C14 -110.4(2) . . . . ? N2 Zn1 C13 C14 154.7(2) . . . . ? C17 Zn2 C17 C20 176.2(2) 2 . . . ? N1 Zn2 C17 C20 43.1(2) . . . . ? N1 Zn2 C17 C20 -48.6(2) 2 . . . ? C17 Zn2 C17 C19 53.53(19) 2 . . . ? N1 Zn2 C17 C19 -79.6(2) . . . . ? N1 Zn2 C17 C19 -171.3(2) 2 . . . ? C17 Zn2 C17 C18 -63.28(19) 2 . . . ? N1 Zn2 C17 C18 163.59(19) . . . . ? N1 Zn2 C17 C18 71.9(2) 2 . . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.553 _refine_diff_density_min -0.360 _refine_diff_density_rms 0.077