Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Wheatley, Andrew E. H.' 'Boss, Sally R.' 'Haigh, Robert' 'Linton, David J.' _publ_contact_author_name 'Dr Andrew E H Wheatley' _publ_contact_author_address ; Chemistry University of Cambridge Lensfield Road Cambridge Cambs CB2 1EW UNITED KINGDOM ; _publ_contact_author_email 'AEHW2@CAM.AC.UK' _publ_section_title ; Towards an understanding of the oxygen scavenging properties of lithium zincates: the synthesis, structural characterisation and oxophilic derivatisation of [Ph(2-C5H4N)N]2ZnRLi·nthf (R = But, Bun; n = 1, 2) ; data_aw0128 _database_code_CSD 183652 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common AW0128 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H64 Li2 N8 O4 Zn2' _chemical_formula_weight 1057.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9618(3) _cell_length_b 12.7891(3) _cell_length_c 19.3890(6) _cell_angle_alpha 77.647(13) _cell_angle_beta 73.211(15) _cell_angle_gamma 74.019(14) _cell_volume 2700.70(29) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 17090 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1108 _exptl_absorpt_coefficient_mu 0.940 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.8641 _exptl_absorpt_correction_T_max 0.9545 _exptl_absorpt_process_details 'Sortav Blessing (1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30519 _diffrn_reflns_av_R_equivalents 0.0536 _diffrn_reflns_av_sigmaI/netI 0.0627 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.48 _reflns_number_total 12229 _reflns_number_gt 9177 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0795P)^2^+0.0948P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12229 _refine_ls_number_parameters 698 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0712 _refine_ls_R_factor_gt 0.0429 _refine_ls_wR_factor_ref 0.1509 _refine_ls_wR_factor_gt 0.1141 _refine_ls_goodness_of_fit_ref 1.164 _refine_ls_restrained_S_all 1.164 _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 -0.58777(3) 0.10417(2) 0.487367(17) 0.02388(10) Uani 1 1 d . . . N1 N -0.54127(19) 0.24726(18) 0.45219(13) 0.0272(5) Uani 1 1 d . . . C2 C -0.8344(3) 0.4493(3) 0.48409(19) 0.0395(8) Uani 1 1 d . . . H2A H -0.9087 0.4584 0.5197 0.047 Uiso 1 1 calc R . . O1 O 0.05631(15) 0.40721(14) 0.04135(10) 0.0231(4) Uani 1 1 d . . . Li1 Li -0.3451(4) 0.0472(4) 0.3756(3) 0.0292(10) Uiso 1 1 d . . . Zn2 Zn -0.03193(3) 0.42698(2) -0.037068(17) 0.02381(10) Uani 1 1 d . . . N2 N -0.33811(19) 0.16590(18) 0.43020(13) 0.0263(5) Uani 1 1 d . . . C3 C -0.8204(3) 0.5231(3) 0.4217(2) 0.0482(9) Uani 1 1 d . . . H3A H -0.8848 0.5835 0.4137 0.058 Uiso 1 1 calc R . . Li2 Li -0.0648(4) 0.3850(4) 0.1292(3) 0.0304(11) Uani 1 1 d . . . O2 O -0.48129(15) -0.01473(14) 0.42765(10) 0.0229(4) Uani 1 1 d . . . N3 N -0.75890(19) 0.10991(19) 0.49606(13) 0.0276(5) Uani 1 1 d . . . C4 C -0.7127(3) 0.5096(3) 0.3704(2) 0.0538(10) Uani 1 1 d . . . H4A H -0.7024 0.5620 0.3276 0.065 Uiso 1 1 calc R . . O3 O -0.0709(2) 0.22827(19) 0.17711(12) 0.0423(6) Uani 1 1 d . . . N4 N -0.8027(2) 0.08049(19) 0.62183(14) 0.0302(5) Uani 1 1 d . . . C5 C -0.6186(3) 0.4206(3) 0.38040(19) 0.0406(8) Uani 1 1 d . . . H5A H -0.5453 0.4115 0.3440 0.049 Uiso 1 1 calc R . . O4 O -0.3374(2) 0.1357(2) 0.27065(12) 0.0463(6) Uani 1 1 d . . . N5 N -0.1883(2) 0.3837(2) -0.00472(13) 0.0285(5) Uani 1 1 d . . . C6 C -0.6315(2) 0.3443(2) 0.44389(17) 0.0295(6) Uani 1 1 d . . . N6 N -0.2312(2) 0.44305(19) 0.10669(13) 0.0285(5) Uani 1 1 d . . . C7 C -0.4267(2) 0.2572(2) 0.44236(15) 0.0266(6) Uani 1 1 d . . . N7 N 0.0825(2) 0.36139(19) -0.12126(13) 0.0277(5) Uani 1 1 d . . . C8 C -0.3991(3) 0.3553(3) 0.44915(18) 0.0376(7) Uani 1 1 d . . . H8A H -0.4610 0.4198 0.4566 0.045 Uiso 1 1 calc R . . N8 N 0.0466(2) 0.52399(19) -0.20007(13) 0.0295(5) Uani 1 1 d . . . C9 C -0.2831(3) 0.3566(3) 0.4449(2) 0.0438(8) Uani 1 1 d . . . H9A H -0.2642 0.4219 0.4493 0.053 Uiso 1 1 calc R . . C10 C -0.1933(3) 0.2617(3) 0.43412(19) 0.0403(8) Uani 1 1 d . . . H10A H -0.1123 0.2605 0.4313 0.048 Uiso 1 1 calc R . . C11 C -0.2254(2) 0.1706(2) 0.42780(16) 0.0318(7) Uani 1 1 d . . . H11A H -0.1641 0.1055 0.4212 0.038 Uiso 1 1 calc R . . C1 C -0.7401(3) 0.3606(2) 0.49580(17) 0.0319(7) Uani 1 1 d . . . H1A H -0.7502 0.3106 0.5399 0.038 Uiso 1 1 calc R . . C12 C -0.8804(3) 0.0968(2) 0.68686(18) 0.0347(7) Uani 1 1 d . . . H12A H -0.8508 0.0709 0.7294 0.042 Uiso 1 1 calc R . . C13 C -0.9992(3) 0.1485(3) 0.6953(2) 0.0425(8) Uani 1 1 d . . . H13A H -1.0508 0.1576 0.7422 0.051 Uiso 1 1 calc R . . C14 C -1.0413(3) 0.1868(3) 0.6328(2) 0.0439(9) Uani 1 1 d . . . H14A H -1.1235 0.2219 0.6367 0.053 Uiso 1 1 calc R . . C15 C -0.9654(2) 0.1745(2) 0.56561(19) 0.0365(7) Uani 1 1 d . . . H15A H -0.9943 0.2018 0.5229 0.044 Uiso 1 1 calc R . . C16 C -0.8430(2) 0.1203(2) 0.56036(17) 0.0281(6) Uani 1 1 d . . . C17 C -0.7960(2) 0.1232(2) 0.43115(16) 0.0276(6) Uani 1 1 d . . . C18 C -0.8663(3) 0.0584(3) 0.42246(18) 0.0365(7) Uani 1 1 d . . . H18A H -0.8960 0.0077 0.4626 0.044 Uiso 1 1 calc R . . C19 C -0.8932(3) 0.0663(3) 0.3571(2) 0.0430(8) Uani 1 1 d . . . H19A H -0.9422 0.0220 0.3528 0.052 Uiso 1 1 calc R . . C20 C -0.8499(3) 0.1377(3) 0.2975(2) 0.0443(8) Uani 1 1 d . . . H20A H -0.8674 0.1418 0.2520 0.053 Uiso 1 1 calc R . . C21 C -0.7811(3) 0.2028(3) 0.3048(2) 0.0472(9) Uani 1 1 d . . . H21A H -0.7515 0.2529 0.2643 0.057 Uiso 1 1 calc R . . C22 C -0.7547(3) 0.1963(3) 0.37052(18) 0.0390(8) Uani 1 1 d . . . H22A H -0.7074 0.2423 0.3746 0.047 Uiso 1 1 calc R . . C27 C -0.3123(3) 0.4885(3) 0.16314(17) 0.0378(7) Uani 1 1 d . . . H27A H -0.2831 0.5066 0.1987 0.045 Uiso 1 1 calc R . . C28 C -0.4341(3) 0.5102(3) 0.17241(19) 0.0473(9) Uani 1 1 d . . . H28A H -0.4877 0.5425 0.2130 0.057 Uiso 1 1 calc R C . C29 C -0.4760(3) 0.4833(3) 0.1206(2) 0.0502(9) Uani 1 1 d . . . H29A H -0.5598 0.4965 0.1254 0.060 Uiso 1 1 calc R . . C30 C -0.3972(3) 0.4379(3) 0.06269(18) 0.0402(8) Uani 1 1 d . . . H30A H -0.4261 0.4189 0.0274 0.048 Uiso 1 1 calc R C . C31 C -0.2725(2) 0.4190(2) 0.05493(16) 0.0281(6) Uani 1 1 d . . . C32 C -0.2221(2) 0.3344(2) -0.05213(17) 0.0313(6) Uani 1 1 d . . . C33 C -0.2767(3) 0.2453(3) -0.0257(2) 0.0479(9) Uani 1 1 d . . . H33A H -0.2944 0.2191 0.0250 0.058 Uiso 1 1 calc R . . C34 C -0.3052(4) 0.1948(4) -0.0727(3) 0.0627(11) Uani 1 1 d . . . H34A H -0.3433 0.1350 -0.0539 0.075 Uiso 1 1 calc R . . C35 C -0.2791(3) 0.2304(4) -0.1460(2) 0.0606(11) Uani 1 1 d . . . H35A H -0.2991 0.1954 -0.1779 0.073 Uiso 1 1 calc R . . C36 C -0.2240(3) 0.3168(3) -0.1736(2) 0.0478(9) Uani 1 1 d . . . H36A H -0.2046 0.3407 -0.2246 0.057 Uiso 1 1 calc R . . C37 C -0.1965(2) 0.3695(3) -0.12661(17) 0.0336(7) Uani 1 1 d . . . H37A H -0.1598 0.4302 -0.1459 0.040 Uiso 1 1 calc R . . C38 C 0.0255(3) 0.5755(3) -0.26417(17) 0.0370(7) Uani 1 1 d . . . H38A H 0.0007 0.6534 -0.2700 0.044 Uiso 1 1 calc R . . C39 C 0.0368(3) 0.5248(3) -0.32257(18) 0.0442(8) Uani 1 1 d . . . H39A H 0.0182 0.5654 -0.3665 0.053 Uiso 1 1 calc R . . C40 C 0.0768(3) 0.4114(3) -0.31368(18) 0.0444(8) Uani 1 1 d . . . H40A H 0.0881 0.3728 -0.3528 0.053 Uiso 1 1 calc R . . C41 C 0.1002(3) 0.3545(3) -0.24917(17) 0.0365(7) Uani 1 1 d . . . H41A H 0.1298 0.2770 -0.2439 0.044 Uiso 1 1 calc R . . C42 C 0.0800(2) 0.4121(2) -0.19037(15) 0.0273(6) Uani 1 1 d . . . C43 C 0.1451(3) 0.2494(2) -0.11217(16) 0.0309(6) Uani 1 1 d . . . C44 C 0.2675(3) 0.2182(3) -0.1435(2) 0.0497(9) Uani 1 1 d . . . H44A H 0.3089 0.2717 -0.1736 0.060 Uiso 1 1 calc R . . C45 C 0.3287(3) 0.1114(3) -0.1316(2) 0.0603(11) Uani 1 1 d . . . H45A H 0.4118 0.0916 -0.1544 0.072 Uiso 1 1 calc R . . C46 C 0.2718(3) 0.0315(3) -0.0870(2) 0.0529(9) Uani 1 1 d . . . H46A H 0.3155 -0.0423 -0.0788 0.063 Uiso 1 1 calc R . . C47 C 0.1515(3) 0.0605(3) -0.0548(2) 0.0482(9) Uani 1 1 d . . . H47A H 0.1116 0.0067 -0.0236 0.058 Uiso 1 1 calc R . . C48 C 0.0877(3) 0.1691(2) -0.06777(18) 0.0379(7) Uani 1 1 d . . . H48A H 0.0042 0.1883 -0.0460 0.045 Uiso 1 1 calc R . . C49 C 0.1761(2) 0.3393(2) 0.02950(16) 0.0296(6) Uani 1 1 d . . . H49A H 0.2263 0.3718 -0.0158 0.036 Uiso 1 1 calc R . . H49B H 0.1737 0.2656 0.0224 0.036 Uiso 1 1 calc R . . C50 C 0.2332(3) 0.3268(3) 0.0909(2) 0.0443(8) Uani 1 1 d . . . H50A H 0.1837 0.2934 0.1361 0.053 Uiso 1 1 calc R . . H50B H 0.2348 0.4005 0.0985 0.053 Uiso 1 1 calc R . . C51 C 0.3617(3) 0.2554(3) 0.0775(3) 0.0611(11) Uani 1 1 d . . . H51A H 0.4085 0.2835 0.0293 0.073 Uiso 1 1 calc R . . H51B H 0.3997 0.2622 0.1149 0.073 Uiso 1 1 calc R . . C52 C 0.3673(4) 0.1347(4) 0.0795(3) 0.0886(16) Uani 1 1 d . . . H52A H 0.4512 0.0937 0.0704 0.133 Uiso 1 1 calc R . . H52B H 0.3313 0.1270 0.0420 0.133 Uiso 1 1 calc R . . H52C H 0.3231 0.1056 0.1275 0.133 Uiso 1 1 calc R . . C23 C -0.5369(2) -0.0713(2) 0.39433(16) 0.0294(6) Uani 1 1 d . B . H23A H -0.5733 -0.0184 0.3570 0.035 Uiso 1 1 calc R . . H23B H -0.6021 -0.0992 0.4319 0.035 Uiso 1 1 calc R . . C24 C -0.4491(3) -0.1660(3) 0.3592(2) 0.0437(8) Uani 1 1 d D . . H24A H -0.4106 -0.2176 0.3961 0.052 Uiso 1 1 calc R A 1 H24B H -0.3856 -0.1377 0.3204 0.052 Uiso 1 1 calc R A 1 C25 C -0.509(2) -0.2277(18) 0.3266(13) 0.101(9) Uani 0.50 1 d PD B 1 H25A H -0.5052 -0.1964 0.2749 0.122 Uiso 0.50 1 calc PR B 1 H25B H -0.5938 -0.2209 0.3532 0.122 Uiso 0.50 1 calc PR B 1 C25' C -0.508(2) -0.2453(14) 0.3415(8) 0.046(4) Uani 0.50 1 d PD B 2 H25C H -0.4432 -0.3024 0.3170 0.055 Uiso 0.50 1 calc PR B 2 H25D H -0.5499 -0.2825 0.3880 0.055 Uiso 0.50 1 calc PR B 2 C26 C -0.4390(8) -0.3539(6) 0.3328(5) 0.068(3) Uani 0.50 1 d P B 1 H26A H -0.4759 -0.3950 0.3118 0.102 Uiso 0.50 1 calc PR B 1 H26B H -0.4434 -0.3843 0.3841 0.102 Uiso 0.50 1 calc PR B 1 H26C H -0.3548 -0.3598 0.3062 0.102 Uiso 0.50 1 calc PR B 1 C26' C -0.5883(11) -0.2006(11) 0.2981(7) 0.107(4) Uani 0.50 1 d P B 2 H26D H -0.6223 -0.2586 0.2920 0.160 Uiso 0.50 1 calc PR B 2 H26E H -0.5467 -0.1683 0.2503 0.160 Uiso 0.50 1 calc PR B 2 H26F H -0.6528 -0.1435 0.3213 0.160 Uiso 0.50 1 calc PR B 2 C53 C -0.4373(13) 0.1339(16) 0.2447(12) 0.071(6) Uani 0.50 1 d PD C 1 H53A H -0.4308 0.1752 0.1954 0.107 Uiso 0.50 1 calc PR C 1 H53B H -0.5120 0.1676 0.2772 0.107 Uiso 0.50 1 calc PR C 1 H53C H -0.4374 0.0577 0.2436 0.107 Uiso 0.50 1 calc PR C 1 C54 C -0.2555(6) 0.1729(6) 0.2092(3) 0.0300(14) Uani 0.50 1 d PD C 1 H54A H -0.2960 0.2413 0.1827 0.036 Uiso 0.50 1 calc PR C 1 H54B H -0.2221 0.1168 0.1760 0.036 Uiso 0.50 1 calc PR C 1 C55 C -0.1545(19) 0.1950(16) 0.2343(11) 0.033(3) Uani 0.50 1 d PD C 1 H55A H -0.1886 0.2522 0.2667 0.039 Uiso 0.50 1 calc PR C 1 H55B H -0.1169 0.1270 0.2625 0.039 Uiso 0.50 1 calc PR C 1 C56 C 0.0096(7) 0.1292(11) 0.1394(8) 0.045(3) Uani 0.50 1 d PD C 1 H56D H -0.0052 0.0607 0.1705 0.067 Uiso 0.50 1 calc PR C 1 H56E H 0.0941 0.1306 0.1310 0.067 Uiso 0.50 1 calc PR C 1 H56F H -0.0088 0.1334 0.0927 0.067 Uiso 0.50 1 calc PR C 1 C53' C -0.4582(12) 0.1666(17) 0.2587(12) 0.053(4) Uani 0.50 1 d PD C 2 H53D H -0.4563 0.2075 0.2096 0.080 Uiso 0.50 1 calc PR C 2 H53E H -0.5121 0.2128 0.2948 0.080 Uiso 0.50 1 calc PR C 2 H53F H -0.4873 0.1001 0.2637 0.080 Uiso 0.50 1 calc PR C 2 C54' C -0.2921(8) 0.2298(9) 0.2418(7) 0.085(3) Uani 0.50 1 d PD C 2 H54C H -0.3466 0.2915 0.2669 0.102 Uiso 0.50 1 calc PR C 2 H54D H -0.2931 0.2488 0.1897 0.102 Uiso 0.50 1 calc PR C 2 C55' C -0.171(2) 0.2206(19) 0.2478(12) 0.054(4) Uani 0.50 1 d PD C 2 H55C H -0.1465 0.1493 0.2778 0.065 Uiso 0.50 1 calc PR C 2 H55D H -0.1743 0.2790 0.2751 0.065 Uiso 0.50 1 calc PR C 2 C56' C -0.0464(13) 0.1458(12) 0.1427(8) 0.084(5) Uani 0.50 1 d PD C 2 H56A H -0.0556 0.0793 0.1778 0.126 Uiso 0.50 1 calc PR C 2 H56B H 0.0364 0.1358 0.1130 0.126 Uiso 0.50 1 calc PR C 2 H56C H -0.1013 0.1598 0.1110 0.126 Uiso 0.50 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02149(16) 0.02282(17) 0.0262(2) -0.00008(13) -0.00583(13) -0.00586(13) N1 0.0230(11) 0.0210(11) 0.0344(14) -0.0001(10) -0.0041(10) -0.0062(9) C2 0.0311(15) 0.0367(18) 0.050(2) -0.0125(16) -0.0106(15) -0.0010(13) O1 0.0233(9) 0.0217(9) 0.0220(10) 0.0003(8) -0.0056(8) -0.0038(7) Zn2 0.02480(17) 0.02437(18) 0.02028(18) -0.00137(13) -0.00377(13) -0.00574(13) N2 0.0244(11) 0.0263(12) 0.0271(13) -0.0007(10) -0.0056(10) -0.0072(10) C3 0.0402(18) 0.0332(18) 0.070(3) 0.0027(17) -0.0252(18) -0.0017(15) Li2 0.033(2) 0.034(3) 0.024(3) 0.003(2) -0.007(2) -0.014(2) O2 0.0237(9) 0.0237(9) 0.0230(10) -0.0033(8) -0.0078(8) -0.0059(8) N3 0.0218(11) 0.0278(12) 0.0310(14) 0.0028(10) -0.0077(10) -0.0062(10) C4 0.049(2) 0.042(2) 0.065(3) 0.0216(18) -0.0227(19) -0.0129(17) O3 0.0522(13) 0.0416(13) 0.0360(13) 0.0072(11) -0.0099(11) -0.0262(11) N4 0.0288(12) 0.0260(12) 0.0327(15) -0.0048(11) -0.0043(11) -0.0042(10) C5 0.0368(16) 0.0363(17) 0.044(2) 0.0086(15) -0.0107(15) -0.0116(14) O4 0.0523(14) 0.0548(15) 0.0356(13) 0.0118(11) -0.0145(11) -0.0286(12) N5 0.0264(11) 0.0326(13) 0.0268(13) -0.0053(10) -0.0044(10) -0.0085(10) C6 0.0318(15) 0.0231(14) 0.0361(17) -0.0009(12) -0.0126(13) -0.0085(12) N6 0.0264(11) 0.0329(13) 0.0242(13) -0.0010(10) -0.0038(10) -0.0088(10) C7 0.0302(14) 0.0250(14) 0.0240(15) 0.0004(11) -0.0053(12) -0.0096(12) N7 0.0304(12) 0.0254(12) 0.0224(13) -0.0019(10) -0.0035(10) -0.0028(10) C8 0.0393(17) 0.0294(16) 0.047(2) -0.0074(14) -0.0128(15) -0.0089(13) N8 0.0319(12) 0.0303(13) 0.0247(13) -0.0030(10) -0.0054(10) -0.0072(10) C9 0.0438(18) 0.0343(17) 0.062(2) -0.0061(16) -0.0190(17) -0.0176(15) C10 0.0343(16) 0.0416(18) 0.051(2) 0.0055(16) -0.0219(15) -0.0165(14) C11 0.0272(14) 0.0326(16) 0.0331(17) 0.0029(13) -0.0095(13) -0.0067(12) C1 0.0330(15) 0.0277(15) 0.0335(17) -0.0031(13) -0.0077(13) -0.0062(12) C12 0.0392(16) 0.0258(15) 0.0337(18) -0.0066(13) 0.0010(14) -0.0075(13) C13 0.0369(17) 0.0312(17) 0.052(2) -0.0143(16) 0.0066(16) -0.0080(14) C14 0.0274(15) 0.0316(17) 0.064(3) -0.0085(17) 0.0010(16) -0.0040(13) C15 0.0246(14) 0.0272(15) 0.051(2) -0.0007(14) -0.0068(14) -0.0020(12) C16 0.0241(13) 0.0208(13) 0.0376(17) -0.0020(12) -0.0051(12) -0.0068(11) C17 0.0228(13) 0.0258(14) 0.0332(17) 0.0008(12) -0.0113(12) -0.0031(11) C18 0.0325(15) 0.0354(17) 0.044(2) 0.0049(14) -0.0157(14) -0.0131(13) C19 0.0424(17) 0.0371(18) 0.059(2) -0.0040(16) -0.0258(17) -0.0121(15) C20 0.0498(19) 0.0441(19) 0.046(2) -0.0024(16) -0.0264(16) -0.0099(16) C21 0.052(2) 0.052(2) 0.044(2) 0.0092(17) -0.0221(17) -0.0230(17) C22 0.0409(17) 0.0420(18) 0.0402(19) 0.0058(15) -0.0173(15) -0.0207(15) C27 0.0346(16) 0.0480(19) 0.0271(17) -0.0079(15) -0.0003(13) -0.0095(14) C28 0.0326(16) 0.065(2) 0.036(2) -0.0136(17) 0.0003(15) -0.0026(16) C29 0.0242(15) 0.071(3) 0.049(2) -0.0085(19) -0.0042(15) -0.0050(16) C30 0.0287(15) 0.052(2) 0.039(2) -0.0006(16) -0.0122(14) -0.0087(15) C31 0.0260(13) 0.0287(15) 0.0263(16) 0.0046(12) -0.0059(12) -0.0081(12) C32 0.0282(14) 0.0357(16) 0.0318(17) -0.0062(13) -0.0096(12) -0.0066(12) C33 0.060(2) 0.049(2) 0.042(2) -0.0046(17) -0.0113(17) -0.0267(18) C34 0.070(3) 0.066(3) 0.068(3) -0.017(2) -0.013(2) -0.037(2) C35 0.056(2) 0.076(3) 0.065(3) -0.032(2) -0.017(2) -0.020(2) C36 0.0391(17) 0.066(2) 0.039(2) -0.0211(18) -0.0114(15) -0.0011(17) C37 0.0262(14) 0.0401(17) 0.0337(18) -0.0087(14) -0.0075(13) -0.0036(13) C38 0.0455(18) 0.0315(16) 0.0330(18) 0.0017(14) -0.0115(14) -0.0099(14) C39 0.065(2) 0.045(2) 0.0255(18) 0.0024(15) -0.0155(16) -0.0194(17) C40 0.064(2) 0.045(2) 0.0281(18) -0.0081(15) -0.0089(16) -0.0191(17) C41 0.0488(18) 0.0314(16) 0.0275(17) -0.0051(13) -0.0040(14) -0.0111(14) C42 0.0267(13) 0.0298(15) 0.0237(15) -0.0045(12) -0.0020(11) -0.0078(12) C43 0.0390(16) 0.0267(15) 0.0248(16) -0.0051(12) -0.0068(13) -0.0039(13) C44 0.0405(18) 0.0386(19) 0.052(2) 0.0010(16) 0.0049(16) -0.0020(15) C45 0.045(2) 0.045(2) 0.067(3) -0.003(2) 0.0026(19) 0.0072(17) C46 0.057(2) 0.0280(17) 0.063(3) -0.0022(17) -0.0141(19) 0.0028(16) C47 0.053(2) 0.0296(17) 0.055(2) 0.0022(16) -0.0080(18) -0.0101(16) C48 0.0345(16) 0.0320(16) 0.042(2) -0.0023(14) -0.0059(14) -0.0062(13) C49 0.0260(14) 0.0266(15) 0.0308(17) -0.0014(12) -0.0060(12) -0.0002(12) C50 0.0394(17) 0.0431(19) 0.051(2) -0.0081(17) -0.0200(16) 0.0000(15) C51 0.0390(19) 0.068(3) 0.072(3) -0.002(2) -0.0291(19) 0.0037(18) C52 0.058(3) 0.064(3) 0.130(5) -0.017(3) -0.031(3) 0.020(2) C23 0.0322(14) 0.0346(16) 0.0257(16) -0.0023(12) -0.0096(12) -0.0137(13) C24 0.0468(18) 0.0429(19) 0.050(2) -0.0181(17) -0.0174(16) -0.0093(15) C25 0.070(11) 0.118(19) 0.15(2) -0.099(15) -0.018(14) -0.030(12) C25' 0.084(10) 0.034(5) 0.026(4) -0.002(4) -0.018(5) -0.021(5) C26 0.100(7) 0.045(4) 0.066(6) -0.021(4) -0.004(5) -0.035(5) C26' 0.115(9) 0.129(11) 0.107(10) -0.044(8) -0.027(8) -0.057(9) C53 0.078(11) 0.089(13) 0.054(11) 0.033(9) -0.024(8) -0.054(11) C54 0.038(4) 0.037(4) 0.017(3) -0.004(3) -0.003(3) -0.016(3) C55 0.036(6) 0.033(5) 0.024(6) -0.001(4) -0.002(4) -0.007(4) C56 0.032(4) 0.042(5) 0.059(6) -0.027(4) 0.010(4) -0.013(4) C53' 0.034(4) 0.077(10) 0.047(7) -0.004(6) -0.015(4) -0.009(5) C54' 0.059(6) 0.078(7) 0.104(9) 0.039(6) -0.022(6) -0.032(5) C55' 0.046(7) 0.072(13) 0.033(8) 0.017(6) 0.000(5) -0.024(8) C56' 0.133(13) 0.053(7) 0.054(7) -0.001(5) 0.004(10) -0.035(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.983(2) . ? Zn1 N3 1.987(2) . ? Zn1 O2 2.0274(18) . ? Zn1 O2 2.0410(19) 2_456 ? Zn1 Zn1 2.9502(8) 2_456 ? Zn1 Li1 2.979(5) 2_456 ? Zn1 Li1 3.087(5) . ? N1 C7 1.366(3) . ? N1 C6 1.417(4) . ? C2 C3 1.366(5) . ? C2 C1 1.395(4) . ? O1 C49 1.439(3) . ? O1 Li2 1.916(5) . ? O1 Zn2 2.0262(18) . ? O1 Zn2 2.0461(18) 2_565 ? Li1 O2 1.929(5) . ? Li1 N4 2.055(5) 2_456 ? Li1 N2 2.059(5) . ? Li1 O4 2.096(5) . ? Li1 Zn1 2.979(5) 2_456 ? Zn2 N7 1.976(2) . ? Zn2 N5 1.985(2) . ? Zn2 O1 2.0461(18) 2_565 ? Zn2 Zn2 2.9507(6) 2_565 ? Zn2 Li2 2.968(4) 2_565 ? Zn2 Li2 3.078(5) . ? N2 C11 1.353(3) . ? N2 C7 1.355(4) . ? C3 C4 1.374(5) . ? Li2 O3 2.033(5) . ? Li2 N6 2.062(5) . ? Li2 N8 2.071(5) 2_565 ? Li2 Zn2 2.968(4) 2_565 ? O2 C23 1.448(3) . ? O2 Zn1 2.0410(19) 2_456 ? N3 C16 1.363(4) . ? N3 C17 1.414(4) . ? C4 C5 1.388(5) . ? O3 C56' 1.289(15) . ? O3 C55 1.34(2) . ? O3 C55' 1.542(18) . ? O3 C56 1.545(11) . ? N4 C12 1.351(4) . ? N4 C16 1.360(4) . ? N4 Li1 2.055(5) 2_456 ? C5 C6 1.396(4) . ? O4 C54 1.394(6) . ? O4 C54' 1.397(9) . ? O4 C53 1.432(18) . ? O4 C53' 1.463(16) . ? N5 C31 1.362(4) . ? N5 C32 1.417(4) . ? C6 C1 1.389(4) . ? N6 C27 1.351(4) . ? N6 C31 1.359(4) . ? C7 C8 1.422(4) . ? N7 C42 1.363(4) . ? N7 C43 1.421(4) . ? C8 C9 1.372(4) . ? N8 C38 1.335(4) . ? N8 C42 1.363(4) . ? N8 Li2 2.071(5) 2_565 ? C9 C10 1.389(5) . ? C10 C11 1.362(4) . ? C12 C13 1.370(4) . ? C13 C14 1.387(5) . ? C14 C15 1.369(5) . ? C15 C16 1.421(4) . ? C17 C18 1.395(4) . ? C17 C22 1.396(4) . ? C18 C19 1.373(5) . ? C19 C20 1.379(5) . ? C20 C21 1.374(4) . ? C21 C22 1.379(5) . ? C27 C28 1.370(4) . ? C28 C29 1.384(5) . ? C29 C30 1.361(5) . ? C30 C31 1.412(4) . ? C32 C37 1.387(4) . ? C32 C33 1.398(4) . ? C33 C34 1.384(5) . ? C34 C35 1.367(6) . ? C35 C36 1.373(5) . ? C36 C37 1.396(4) . ? C38 C39 1.378(4) . ? C39 C40 1.385(5) . ? C40 C41 1.369(5) . ? C41 C42 1.415(4) . ? C43 C48 1.392(4) . ? C43 C44 1.393(4) . ? C44 C45 1.366(5) . ? C45 C46 1.386(5) . ? C46 C47 1.373(5) . ? C47 C48 1.397(5) . ? C49 C50 1.497(4) . ? C50 C51 1.537(5) . ? C51 C52 1.518(6) . ? C23 C24 1.508(4) . ? C24 C25 1.520(11) . ? C24 C25' 1.520(11) . ? C25 C26 1.60(3) . ? C25' C26' 1.39(2) . ? C54 C55 1.54(2) . ? C54' C55' 1.46(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Zn1 N3 114.82(9) . . ? N1 Zn1 O2 112.59(8) . . ? N3 Zn1 O2 109.70(8) . . ? N1 Zn1 O2 113.33(8) . 2_456 ? N3 Zn1 O2 116.12(8) . 2_456 ? O2 Zn1 O2 87.04(8) . 2_456 ? N1 Zn1 Zn1 122.54(6) . 2_456 ? N3 Zn1 Zn1 122.43(7) . 2_456 ? O2 Zn1 Zn1 43.70(5) . 2_456 ? O2 Zn1 Zn1 43.34(5) 2_456 2_456 ? N1 Zn1 Li1 141.09(12) . 2_456 ? N3 Zn1 Li1 76.45(11) . 2_456 ? O2 Zn1 Li1 96.04(11) . 2_456 ? O2 Zn1 Li1 39.96(10) 2_456 2_456 ? Zn1 Zn1 Li1 62.75(9) 2_456 2_456 ? N1 Zn1 Li1 76.31(11) . . ? N3 Zn1 Li1 137.61(11) . . ? O2 Zn1 Li1 37.58(10) . . ? O2 Zn1 Li1 92.55(11) 2_456 . ? Zn1 Zn1 Li1 59.08(9) 2_456 . ? Li1 Zn1 Li1 121.83(9) 2_456 . ? C7 N1 C6 118.3(2) . . ? C7 N1 Zn1 122.18(18) . . ? C6 N1 Zn1 119.20(16) . . ? C3 C2 C1 120.3(3) . . ? C49 O1 Li2 122.6(2) . . ? C49 O1 Zn2 116.91(16) . . ? Li2 O1 Zn2 102.63(16) . . ? C49 O1 Zn2 119.24(15) . 2_565 ? Li2 O1 Zn2 96.95(17) . 2_565 ? Zn2 O1 Zn2 92.87(7) . 2_565 ? O2 Li1 N4 105.5(2) . 2_456 ? O2 Li1 N2 109.1(2) . . ? N4 Li1 N2 109.2(2) 2_456 . ? O2 Li1 O4 120.5(2) . . ? N4 Li1 O4 111.7(2) 2_456 . ? N2 Li1 O4 100.6(2) . . ? O2 Li1 Zn1 42.82(11) . 2_456 ? N4 Li1 Zn1 73.98(16) 2_456 2_456 ? N2 Li1 Zn1 93.10(18) . 2_456 ? O4 Li1 Zn1 162.1(2) . 2_456 ? O2 Li1 Zn1 39.87(11) . . ? N4 Li1 Zn1 131.9(2) 2_456 . ? N2 Li1 Zn1 71.73(15) . . ? O4 Li1 Zn1 115.3(2) . . ? Zn1 Li1 Zn1 58.17(9) 2_456 . ? N7 Zn2 N5 115.45(9) . . ? N7 Zn2 O1 108.12(9) . . ? N5 Zn2 O1 115.87(9) . . ? N7 Zn2 O1 116.38(8) . 2_565 ? N5 Zn2 O1 110.79(9) . 2_565 ? O1 Zn2 O1 87.13(7) . 2_565 ? N7 Zn2 Zn2 121.44(7) . 2_565 ? N5 Zn2 Zn2 123.08(7) . 2_565 ? O1 Zn2 Zn2 43.83(5) . 2_565 ? O1 Zn2 Zn2 43.30(5) 2_565 2_565 ? N7 Zn2 Li2 76.69(12) . 2_565 ? N5 Zn2 Li2 137.16(12) . 2_565 ? O1 Zn2 Li2 96.12(10) . 2_565 ? O1 Zn2 Li2 39.86(11) 2_565 2_565 ? Zn2 Zn2 Li2 62.68(9) 2_565 2_565 ? N7 Zn2 Li2 136.22(12) . . ? N5 Zn2 Li2 79.41(11) . . ? O1 Zn2 Li2 37.41(10) . . ? O1 Zn2 Li2 92.43(10) 2_565 . ? Zn2 Zn2 Li2 58.93(8) 2_565 . ? Li2 Zn2 Li2 121.61(9) 2_565 . ? C11 N2 C7 117.8(2) . . ? C11 N2 Li1 113.9(2) . . ? C7 N2 Li1 123.5(2) . . ? C2 C3 C4 119.6(3) . . ? O1 Li2 O3 118.4(3) . . ? O1 Li2 N6 109.1(2) . . ? O3 Li2 N6 101.7(2) . . ? O1 Li2 N8 105.9(2) . 2_565 ? O3 Li2 N8 111.5(2) . 2_565 ? N6 Li2 N8 110.1(2) . 2_565 ? O1 Li2 Zn2 43.19(11) . 2_565 ? O3 Li2 Zn2 159.7(2) . 2_565 ? N6 Li2 Zn2 94.21(18) . 2_565 ? N8 Li2 Zn2 73.77(14) 2_565 2_565 ? O1 Li2 Zn2 39.97(11) . . ? O3 Li2 Zn2 115.2(2) . . ? N6 Li2 Zn2 71.17(15) . . ? N8 Li2 Zn2 131.9(2) 2_565 . ? Zn2 Li2 Zn2 58.39(9) 2_565 . ? C23 O2 Li1 123.4(2) . . ? C23 O2 Zn1 118.46(15) . . ? Li1 O2 Zn1 102.55(16) . . ? C23 O2 Zn1 116.31(16) . 2_456 ? Li1 O2 Zn1 97.21(16) . 2_456 ? Zn1 O2 Zn1 92.96(7) . 2_456 ? C16 N3 C17 119.5(2) . . ? C16 N3 Zn1 121.68(19) . . ? C17 N3 Zn1 117.88(17) . . ? C3 C4 C5 121.0(3) . . ? C56' O3 C55 97.7(9) . . ? C56' O3 C55' 112.8(10) . . ? C55 O3 C55' 15.3(13) . . ? C56' O3 C56 23.7(8) . . ? C55 O3 C56 110.1(8) . . ? C55' O3 C56 124.9(10) . . ? C56' O3 Li2 124.9(7) . . ? C55 O3 Li2 127.6(8) . . ? C55' O3 Li2 113.8(9) . . ? C56 O3 Li2 121.0(6) . . ? C12 N4 C16 118.6(2) . . ? C12 N4 Li1 115.8(2) . 2_456 ? C16 N4 Li1 121.8(2) . 2_456 ? C4 C5 C6 120.1(3) . . ? C54 O4 C54' 41.6(5) . . ? C54 O4 C53 105.1(8) . . ? C54' O4 C53 113.7(9) . . ? C54 O4 C53' 110.9(10) . . ? C54' O4 C53' 104.4(9) . . ? C53 O4 C53' 20.4(13) . . ? C54 O4 Li1 140.9(3) . . ? C54' O4 Li1 126.8(6) . . ? C53 O4 Li1 111.4(8) . . ? C53' O4 Li1 108.3(9) . . ? C31 N5 C32 118.8(2) . . ? C31 N5 Zn2 121.07(18) . . ? C32 N5 Zn2 118.95(18) . . ? C1 C6 C5 118.1(3) . . ? C1 C6 N1 120.5(3) . . ? C5 C6 N1 121.1(3) . . ? C27 N6 C31 118.1(2) . . ? C27 N6 Li2 110.6(2) . . ? C31 N6 Li2 129.1(2) . . ? N2 C7 N1 116.8(2) . . ? N2 C7 C8 120.1(2) . . ? N1 C7 C8 123.0(3) . . ? C42 N7 C43 117.6(2) . . ? C42 N7 Zn2 120.14(19) . . ? C43 N7 Zn2 120.15(18) . . ? C9 C8 C7 119.9(3) . . ? C38 N8 C42 118.1(2) . . ? C38 N8 Li2 118.8(2) . 2_565 ? C42 N8 Li2 121.7(2) . 2_565 ? C8 C9 C10 119.5(3) . . ? C11 C10 C9 117.7(3) . . ? N2 C11 C10 124.9(3) . . ? C6 C1 C2 120.9(3) . . ? N4 C12 C13 124.1(3) . . ? C12 C13 C14 117.5(3) . . ? C15 C14 C13 120.5(3) . . ? C14 C15 C16 119.3(3) . . ? N4 C16 N3 116.2(2) . . ? N4 C16 C15 119.9(3) . . ? N3 C16 C15 123.8(3) . . ? C18 C17 C22 117.0(3) . . ? C18 C17 N3 122.1(3) . . ? C22 C17 N3 120.6(2) . . ? C19 C18 C17 121.3(3) . . ? C18 C19 C20 120.8(3) . . ? C21 C20 C19 118.9(3) . . ? C20 C21 C22 120.6(3) . . ? C21 C22 C17 121.3(3) . . ? N6 C27 C28 124.2(3) . . ? C27 C28 C29 117.6(3) . . ? C30 C29 C28 120.0(3) . . ? C29 C30 C31 120.2(3) . . ? N6 C31 N5 116.5(2) . . ? N6 C31 C30 119.8(3) . . ? N5 C31 C30 123.6(3) . . ? C37 C32 C33 117.9(3) . . ? C37 C32 N5 121.0(3) . . ? C33 C32 N5 121.0(3) . . ? C34 C33 C32 120.7(4) . . ? C35 C34 C33 120.5(4) . . ? C34 C35 C36 120.0(3) . . ? C35 C36 C37 120.0(3) . . ? C32 C37 C36 120.8(3) . . ? N8 C38 C39 125.3(3) . . ? C38 C39 C40 116.4(3) . . ? C41 C40 C39 120.7(3) . . ? C40 C41 C42 119.5(3) . . ? N8 C42 N7 116.5(2) . . ? N8 C42 C41 119.9(3) . . ? N7 C42 C41 123.4(3) . . ? C48 C43 C44 118.0(3) . . ? C48 C43 N7 121.0(3) . . ? C44 C43 N7 120.9(3) . . ? C45 C44 C43 120.8(3) . . ? C44 C45 C46 121.2(3) . . ? C47 C46 C45 119.2(3) . . ? C46 C47 C48 120.0(3) . . ? C43 C48 C47 120.8(3) . . ? O1 C49 C50 113.3(2) . . ? C49 C50 C51 113.0(3) . . ? C52 C51 C50 113.3(3) . . ? O2 C23 C24 112.5(2) . . ? C23 C24 C25 112.5(10) . . ? C23 C24 C25' 114.1(10) . . ? C25 C24 C25' 12.4(13) . . ? C24 C25 C26 108.3(14) . . ? C26' C25' C24 116.8(12) . . ? O4 C54 C55 108.3(8) . . ? O3 C55 C54 111.0(14) . . ? O4 C54' C55' 115.3(12) . . ? C54' C55' O3 118.3(18) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.640 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.208 data_aw0118 _database_code_CSD 183653 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aw0118 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H35 Li1 N4 O2 Zn1' _chemical_formula_weight 555.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.715(2) _cell_length_b 12.228(2) _cell_length_c 12.323(3) _cell_angle_alpha 107.10(3) _cell_angle_beta 106.27(3) _cell_angle_gamma 111.01(3) _cell_volume 1420.3(9) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9559 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 0.897 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 1.075 _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16302 _diffrn_reflns_av_R_equivalents 0.0559 _diffrn_reflns_av_sigmaI/netI 0.0803 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6373 _reflns_number_gt 4686 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0440P)^2^+0.3787P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6373 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0780 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1094 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 -0.07969(3) 0.51168(3) -0.42701(2) 0.02220(11) Uani 1 1 d . . . Li1 Li -0.0548(5) 0.6619(4) -0.5757(4) 0.0291(10) Uani 1 1 d . . . O1 O -0.10027(16) 0.48604(16) -0.60311(14) 0.0217(4) Uani 1 1 d . . . O2 O -0.0942(2) 0.70075(19) -0.72171(17) 0.0404(5) Uani 1 1 d . . . N1 N -0.1526(2) 0.7229(2) -0.47486(19) 0.0269(5) Uani 1 1 d . . . N2 N -0.0538(2) 0.6799(2) -0.31324(18) 0.0246(5) Uani 1 1 d . . . N4 N -0.2160(2) 0.3608(2) -0.42551(18) 0.0242(5) Uani 1 1 d . . . N3 N -0.1531(2) 0.2201(2) -0.53168(19) 0.0259(5) Uani 1 1 d . . . C16 C -0.2497(3) 0.2363(2) -0.4999(2) 0.0230(6) Uani 1 1 d . . . C17 C -0.2968(3) 0.3800(2) -0.3628(2) 0.0256(6) Uani 1 1 d . . . C12 C -0.1870(3) 0.1014(3) -0.6160(2) 0.0312(6) Uani 1 1 d . . . H12A H -0.1192 0.0912 -0.6389 0.037 Uiso 1 1 calc R . . C21 C -0.4242(3) 0.4862(3) -0.3081(3) 0.0444(8) Uani 1 1 d . . . H21A H -0.4623 0.5412 -0.3185 0.053 Uiso 1 1 calc R . . C18 C -0.3117(3) 0.3278(3) -0.2778(2) 0.0324(7) Uani 1 1 d . . . H18A H -0.2730 0.2733 -0.2666 0.039 Uiso 1 1 calc R . . C1 C -0.2305(3) 0.7710(3) -0.5237(3) 0.0344(7) Uani 1 1 d . . . H1A H -0.2494 0.7598 -0.6075 0.041 Uiso 1 1 calc R . . C14 C -0.4106(3) 0.0091(3) -0.6355(3) 0.0362(7) Uani 1 1 d . . . H14A H -0.4983 -0.0633 -0.6702 0.043 Uiso 1 1 calc R . . C2 C -0.2840(3) 0.8343(3) -0.4611(3) 0.0390(7) Uani 1 1 d . . . H2A H -0.3380 0.8666 -0.4995 0.047 Uiso 1 1 calc R . . C23 C -0.2178(3) 0.3758(3) -0.7115(2) 0.0269(6) Uani 1 1 d . . . H23A H -0.2219 0.2946 -0.7084 0.032 Uiso 1 1 calc R . . H23B H -0.2079 0.3764 -0.7886 0.032 Uiso 1 1 calc R . . C8 C 0.1071(3) 0.6923(3) -0.0017(2) 0.0370(7) Uani 1 1 d . . . H8A H 0.1076 0.6330 0.0336 0.044 Uiso 1 1 calc R . . C22 C -0.3546(3) 0.4590(3) -0.3767(3) 0.0332(7) Uani 1 1 d . . . H22A H -0.3462 0.4950 -0.4345 0.040 Uiso 1 1 calc R . . C24 C -0.3486(3) 0.3750(3) -0.7200(2) 0.0340(7) Uani 1 1 d . . . H24A H -0.3481 0.4520 -0.7312 0.041 Uiso 1 1 calc R . . H24B H -0.3545 0.3827 -0.6397 0.041 Uiso 1 1 calc R . . C20 C -0.4388(3) 0.4339(3) -0.2246(3) 0.0467(8) Uani 1 1 d . . . H20A H -0.4873 0.4522 -0.1778 0.056 Uiso 1 1 calc R . . C3 C -0.2563(3) 0.8497(3) -0.3389(3) 0.0412(8) Uani 1 1 d . . . H3A H -0.2921 0.8929 -0.2920 0.049 Uiso 1 1 calc R . . C9 C 0.1895(3) 0.8243(3) 0.0729(3) 0.0458(8) Uani 1 1 d . . . H9A H 0.2466 0.8562 0.1593 0.055 Uiso 1 1 calc R . . C27 C -0.1679(5) 0.6206(4) -0.8511(3) 0.0824(15) Uani 1 1 d . . . H27A H -0.2582 0.5535 -0.8691 0.099 Uiso 1 1 calc R . . H27B H -0.1197 0.5756 -0.8813 0.099 Uiso 1 1 calc R . . C10 C 0.1880(4) 0.9093(3) 0.0207(3) 0.0532(9) Uani 1 1 d . . . H10A H 0.2442 1.0006 0.0716 0.064 Uiso 1 1 calc R . . C19 C -0.3822(3) 0.3547(3) -0.2095(3) 0.0427(8) Uani 1 1 d . . . H19A H -0.3917 0.3185 -0.1521 0.051 Uiso 1 1 calc R . . C25 C -0.4736(3) 0.2521(3) -0.8278(3) 0.0544(9) Uani 1 1 d . . . H25A H -0.4734 0.1755 -0.8159 0.065 Uiso 1 1 calc R . . H25B H -0.5553 0.2552 -0.8228 0.065 Uiso 1 1 calc R . . C11 C 0.1053(3) 0.8630(3) -0.1050(3) 0.0428(8) Uani 1 1 d . . . H11A H 0.1055 0.9231 -0.1394 0.051 Uiso 1 1 calc R . . C29 C -0.0898(4) 0.8381(4) -0.8207(3) 0.0594(10) Uani 1 1 d . . . H29A H -0.1409 0.8846 -0.8016 0.071 Uiso 1 1 calc R . . H29B H -0.0270 0.8849 -0.8506 0.071 Uiso 1 1 calc R . . C30 C -0.0137(4) 0.8284(3) -0.7067(3) 0.0656(11) Uani 1 1 d . . . H30A H 0.0765 0.8411 -0.7011 0.079 Uiso 1 1 calc R . . H30B H -0.0009 0.8956 -0.6291 0.079 Uiso 1 1 calc R . . C28 C -0.1838(5) 0.7008(4) -0.9164(4) 0.0762(13) Uani 1 1 d . . . H28A H -0.2785 0.6850 -0.9487 0.091 Uiso 1 1 calc R . . H28B H -0.1596 0.6805 -0.9880 0.091 Uiso 1 1 calc R . . C26 C -0.4844(4) 0.2323(5) -0.9556(3) 0.0888(15) Uani 1 1 d . . . H26A H -0.5662 0.1504 -1.0183 0.133 Uiso 1 1 calc R . . H26B H -0.4044 0.2284 -0.9623 0.133 Uiso 1 1 calc R . . H26C H -0.4898 0.3050 -0.9706 0.133 Uiso 1 1 calc R . . C13 C -0.3125(3) -0.0056(3) -0.6711(3) 0.0363(7) Uani 1 1 d . . . H13A H -0.3318 -0.0870 -0.7314 0.044 Uiso 1 1 calc R . . C15 C -0.3806(3) 0.1281(3) -0.5505(2) 0.0319(6) Uani 1 1 d . . . H15A H -0.4472 0.1384 -0.5254 0.038 Uiso 1 1 calc R . . C7 C 0.0237(3) 0.6451(3) -0.1275(2) 0.0294(6) Uani 1 1 d . . . H7A H -0.0331 0.5537 -0.1772 0.035 Uiso 1 1 calc R . . C6 C 0.0213(3) 0.7288(3) -0.1829(2) 0.0260(6) Uani 1 1 d . . . C4 C -0.1779(3) 0.8028(3) -0.2858(3) 0.0367(7) Uani 1 1 d . . . H4A H -0.1587 0.8138 -0.2020 0.044 Uiso 1 1 calc R . . C5 C -0.1254(3) 0.7379(2) -0.3556(2) 0.0242(6) Uani 1 1 d . . . 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 0.02169(18) 0.01995(17) 0.02504(16) 0.00928(12) 0.01101(12) 0.00988(13) Li1 0.027(2) 0.030(3) 0.033(2) 0.017(2) 0.0140(19) 0.013(2) O1 0.0189(9) 0.0197(9) 0.0230(8) 0.0075(7) 0.0080(7) 0.0081(8) O2 0.0488(13) 0.0306(11) 0.0365(11) 0.0186(9) 0.0159(10) 0.0128(10) N1 0.0252(12) 0.0285(13) 0.0282(11) 0.0118(10) 0.0111(9) 0.0148(11) N2 0.0272(12) 0.0224(12) 0.0242(11) 0.0091(9) 0.0107(9) 0.0131(10) N4 0.0226(12) 0.0211(12) 0.0299(11) 0.0114(9) 0.0145(9) 0.0091(10) N3 0.0263(13) 0.0201(12) 0.0301(11) 0.0098(9) 0.0133(10) 0.0102(10) C16 0.0223(14) 0.0240(14) 0.0262(13) 0.0149(11) 0.0120(11) 0.0104(12) C17 0.0186(14) 0.0235(14) 0.0277(13) 0.0080(11) 0.0087(11) 0.0069(12) C12 0.0336(17) 0.0270(15) 0.0352(15) 0.0119(12) 0.0175(13) 0.0162(14) C21 0.0379(19) 0.0367(18) 0.059(2) 0.0149(16) 0.0247(16) 0.0205(16) C18 0.0284(16) 0.0295(16) 0.0324(15) 0.0125(12) 0.0127(12) 0.0083(13) C1 0.0360(17) 0.0403(18) 0.0337(15) 0.0198(13) 0.0140(13) 0.0228(15) C14 0.0271(16) 0.0229(15) 0.0430(17) 0.0108(13) 0.0098(13) 0.0036(13) C2 0.0403(18) 0.0415(18) 0.0459(17) 0.0219(14) 0.0187(14) 0.0280(16) C23 0.0220(14) 0.0251(14) 0.0256(13) 0.0087(11) 0.0060(11) 0.0087(12) C8 0.0420(19) 0.0411(18) 0.0342(15) 0.0218(14) 0.0169(14) 0.0216(16) C22 0.0265(16) 0.0312(16) 0.0394(15) 0.0134(13) 0.0163(13) 0.0114(13) C24 0.0249(16) 0.0364(17) 0.0331(15) 0.0106(13) 0.0110(12) 0.0122(14) C20 0.0341(18) 0.044(2) 0.0478(18) 0.0034(15) 0.0266(15) 0.0113(16) C3 0.054(2) 0.0429(19) 0.0445(17) 0.0187(15) 0.0279(15) 0.0354(17) C9 0.050(2) 0.048(2) 0.0245(15) 0.0121(14) 0.0071(14) 0.0180(17) C27 0.136(4) 0.040(2) 0.0376(19) 0.0163(17) 0.019(2) 0.025(2) C10 0.066(2) 0.0295(17) 0.0338(16) 0.0064(14) 0.0065(16) 0.0102(17) C19 0.0379(18) 0.0422(19) 0.0340(16) 0.0121(14) 0.0183(14) 0.0071(16) C25 0.0263(18) 0.058(2) 0.0482(19) 0.0044(16) 0.0068(14) 0.0126(17) C11 0.061(2) 0.0239(16) 0.0313(15) 0.0102(12) 0.0123(14) 0.0162(16) C29 0.070(3) 0.055(2) 0.063(2) 0.0390(19) 0.0263(19) 0.032(2) C30 0.072(3) 0.042(2) 0.058(2) 0.0314(18) 0.0118(19) 0.006(2) C28 0.086(3) 0.065(3) 0.054(2) 0.031(2) 0.008(2) 0.028(2) C26 0.049(2) 0.115(4) 0.047(2) 0.010(2) 0.0070(18) 0.014(3) C13 0.0398(18) 0.0223(15) 0.0354(15) 0.0052(12) 0.0132(13) 0.0120(14) C15 0.0250(15) 0.0300(16) 0.0392(15) 0.0150(13) 0.0152(12) 0.0108(13) C7 0.0308(16) 0.0251(14) 0.0290(14) 0.0107(11) 0.0122(12) 0.0117(13) C6 0.0267(15) 0.0245(14) 0.0268(13) 0.0092(11) 0.0132(11) 0.0127(12) C4 0.050(2) 0.0395(18) 0.0346(15) 0.0179(13) 0.0224(14) 0.0308(16) C5 0.0216(14) 0.0183(13) 0.0286(13) 0.0081(11) 0.0110(11) 0.0072(11) _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 N4 1.969(2) . ? Zn1 N2 1.976(2) . ? Zn1 O1 2.0239(17) 2_564 ? Zn1 O1 2.0293(16) . ? Zn1 Li1 2.951(4) . ? Zn1 Zn1 2.9605(9) 2_564 ? Zn1 Li1 3.065(5) 2_564 ? Li1 O1 1.916(5) . ? Li1 O2 1.968(5) . ? Li1 N1 2.068(5) . ? Li1 N3 2.077(5) 2_564 ? Li1 Zn1 3.065(5) 2_564 ? O1 C23 1.441(3) . ? O1 Zn1 2.0239(17) 2_564 ? O2 C27 1.397(4) . ? O2 C30 1.427(4) . ? N1 C1 1.352(3) . ? N1 C5 1.354(3) . ? N2 C5 1.371(3) . ? N2 C6 1.406(3) . ? N4 C16 1.364(3) . ? N4 C17 1.417(3) . ? N3 C12 1.346(3) . ? N3 C16 1.356(3) . ? N3 Li1 2.077(5) 2_564 ? C16 C15 1.419(4) . ? C17 C22 1.387(4) . ? C17 C18 1.398(4) . ? C12 C13 1.369(4) . ? C21 C22 1.380(4) . ? C21 C20 1.380(5) . ? C18 C19 1.386(4) . ? C1 C2 1.361(4) . ? C14 C15 1.367(4) . ? C14 C13 1.389(4) . ? C2 C3 1.387(4) . ? C23 C24 1.502(4) . ? C8 C9 1.376(4) . ? C8 C7 1.383(4) . ? C24 C25 1.525(4) . ? C20 C19 1.381(4) . ? C3 C4 1.364(4) . ? C9 C10 1.377(4) . ? C27 C28 1.468(5) . ? C10 C11 1.382(4) . ? C25 C26 1.481(5) . ? C11 C6 1.403(4) . ? C29 C28 1.485(5) . ? C29 C30 1.501(4) . ? C7 C6 1.391(4) . ? C4 C5 1.411(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Zn1 N2 112.66(9) . . ? N4 Zn1 O1 114.38(8) . 2_564 ? N2 Zn1 O1 111.03(9) . 2_564 ? N4 Zn1 O1 112.99(9) . . ? N2 Zn1 O1 117.10(8) . . ? O1 Zn1 O1 86.16(7) 2_564 . ? N4 Zn1 Li1 140.25(11) . . ? N2 Zn1 Li1 77.38(11) . . ? O1 Zn1 Li1 95.17(10) 2_564 . ? O1 Zn1 Li1 40.14(10) . . ? N4 Zn1 Zn1 123.36(7) . 2_564 ? N2 Zn1 Zn1 123.89(7) . 2_564 ? O1 Zn1 Zn1 43.15(5) 2_564 2_564 ? O1 Zn1 Zn1 43.01(5) . 2_564 ? Li1 Zn1 Zn1 62.46(9) . 2_564 ? N4 Zn1 Li1 77.93(11) . 2_564 ? N2 Zn1 Li1 138.51(10) . 2_564 ? O1 Zn1 Li1 37.67(10) 2_564 2_564 ? O1 Zn1 Li1 91.70(9) . 2_564 ? Li1 Zn1 Li1 121.07(8) . 2_564 ? Zn1 Zn1 Li1 58.61(8) 2_564 2_564 ? O1 Li1 O2 119.1(2) . . ? O1 Li1 N1 107.9(2) . . ? O2 Li1 N1 107.6(2) . . ? O1 Li1 N3 108.9(2) . 2_564 ? O2 Li1 N3 104.4(2) . 2_564 ? N1 Li1 N3 108.6(2) . 2_564 ? O1 Li1 Zn1 43.07(10) . . ? O2 Li1 Zn1 159.2(2) . . ? N1 Li1 Zn1 75.56(14) . . ? N3 Li1 Zn1 93.64(16) 2_564 . ? O1 Li1 Zn1 40.22(10) . 2_564 ? O2 Li1 Zn1 117.1(2) . 2_564 ? N1 Li1 Zn1 134.08(19) . 2_564 ? N3 Li1 Zn1 71.14(14) 2_564 2_564 ? Zn1 Li1 Zn1 58.93(8) . 2_564 ? C23 O1 Li1 121.83(19) . . ? C23 O1 Zn1 116.77(14) . 2_564 ? Li1 O1 Zn1 102.11(16) . 2_564 ? C23 O1 Zn1 120.22(15) . . ? Li1 O1 Zn1 96.79(15) . . ? Zn1 O1 Zn1 93.84(7) 2_564 . ? C27 O2 C30 106.7(2) . . ? C27 O2 Li1 132.3(2) . . ? C30 O2 Li1 119.2(2) . . ? C1 N1 C5 118.2(2) . . ? C1 N1 Li1 116.9(2) . . ? C5 N1 Li1 123.9(2) . . ? C5 N2 C6 118.9(2) . . ? C5 N2 Zn1 121.40(16) . . ? C6 N2 Zn1 118.74(16) . . ? C16 N4 C17 118.5(2) . . ? C16 N4 Zn1 121.24(17) . . ? C17 N4 Zn1 119.41(16) . . ? C12 N3 C16 118.2(2) . . ? C12 N3 Li1 113.2(2) . 2_564 ? C16 N3 Li1 125.4(2) . 2_564 ? N3 C16 N4 116.4(2) . . ? N3 C16 C15 119.9(2) . . ? N4 C16 C15 123.5(2) . . ? C22 C17 C18 118.1(3) . . ? C22 C17 N4 121.0(2) . . ? C18 C17 N4 120.7(2) . . ? N3 C12 C13 124.5(3) . . ? C22 C21 C20 120.4(3) . . ? C19 C18 C17 120.6(3) . . ? N1 C1 C2 124.5(3) . . ? C15 C14 C13 119.9(3) . . ? C1 C2 C3 117.3(3) . . ? O1 C23 C24 113.4(2) . . ? C9 C8 C7 120.7(3) . . ? C21 C22 C17 121.1(3) . . ? C23 C24 C25 113.2(2) . . ? C21 C20 C19 119.4(3) . . ? C4 C3 C2 120.1(3) . . ? C8 C9 C10 119.2(3) . . ? O2 C27 C28 109.1(3) . . ? C9 C10 C11 120.5(3) . . ? C20 C19 C18 120.4(3) . . ? C26 C25 C24 115.3(3) . . ? C10 C11 C6 121.2(3) . . ? C28 C29 C30 104.8(3) . . ? O2 C30 C29 106.2(3) . . ? C27 C28 C29 105.5(3) . . ? C12 C13 C14 117.5(3) . . ? C14 C15 C16 119.8(3) . . ? C8 C7 C6 121.3(3) . . ? C7 C6 C11 117.1(2) . . ? C7 C6 N2 121.0(2) . . ? C11 C6 N2 121.7(2) . . ? C3 C4 C5 120.0(3) . . ? N1 C5 N2 116.1(2) . . ? N1 C5 C4 119.8(2) . . ? N2 C5 C4 124.0(2) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.658 _refine_diff_density_min -0.645 _refine_diff_density_rms 0.101 data_aw0123 _database_code_CSD 183654 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aw0123 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H35 Li N4 O Zn' _chemical_formula_weight 539.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.6358(5) _cell_length_b 17.4699(9) _cell_length_c 16.9408(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.230(3) _cell_angle_gamma 90.00 _cell_volume 2847.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 220(2) _cell_measurement_reflns_used 15492 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 0.891 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details 'Sortav Blessing (1995) ' _exptl_absorpt_correction_T_min 0.988 _exptl_absorpt_correction_T_max 1.028 _exptl_special_details ; ? ; _diffrn_ambient_temperature 220(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18191 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.70 _diffrn_reflns_theta_max 27.43 _reflns_number_total 6446 _reflns_number_gt 4645 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+3.4440P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6446 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0597 _refine_ls_wR_factor_ref 0.1309 _refine_ls_wR_factor_gt 0.1198 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 0.67507(4) 0.17093(2) 0.21101(2) 0.03566(13) Uani 1 1 d . . . Li1 Li 0.7984(6) 0.3070(3) 0.2286(4) 0.0440(14) Uani 1 1 d . . . N1 N 0.8850(3) 0.19073(16) 0.21872(15) 0.0367(6) Uani 1 1 d . . . O1 O 0.8828(3) 0.37818(18) 0.29648(18) 0.0690(8) Uani 1 1 d . . . C1 C 0.8980(4) 0.3079(3) 0.0502(2) 0.0599(11) Uani 1 1 d . . . H1A H 0.8473 0.3504 0.0303 0.072 Uiso 1 1 calc R . . N2 N 0.8675(3) 0.28019(18) 0.12093(16) 0.0455(7) Uani 1 1 d . . . C2 C 0.9978(5) 0.2784(3) 0.0055(2) 0.0696(13) Uani 1 1 d . . . H2A H 1.0152 0.2992 -0.0442 0.084 Uiso 1 1 calc R . . N3 N 0.5904(3) 0.28813(15) 0.22992(15) 0.0344(6) Uani 1 1 d . . . C3 C 1.0729(4) 0.2163(3) 0.0362(2) 0.0693(13) Uani 1 1 d . . . H3A H 1.1445 0.1953 0.0076 0.083 Uiso 1 1 calc R . . N4 N 0.6080(3) 0.19759(15) 0.32458(14) 0.0351(6) Uani 1 1 d . . . C4 C 1.0439(4) 0.1856(2) 0.1076(2) 0.0535(10) Uani 1 1 d . . . H4A H 1.0946 0.1435 0.1284 0.064 Uiso 1 1 calc R . . C5 C 0.9367(3) 0.2182(2) 0.14933(19) 0.0396(8) Uani 1 1 d . . . C6 C 0.9707(3) 0.14569(19) 0.27083(19) 0.0373(7) Uani 1 1 d . . . C7 C 1.1122(3) 0.1603(2) 0.2865(2) 0.0472(9) Uani 1 1 d . . . H7A H 1.1542 0.2012 0.2608 0.057 Uiso 1 1 calc R . . C8 C 1.1912(4) 0.1156(3) 0.3392(2) 0.0578(10) Uani 1 1 d . . . H8A H 1.2863 0.1263 0.3485 0.069 Uiso 1 1 calc R . . C9 C 1.1333(4) 0.0557(2) 0.3781(2) 0.0563(10) Uani 1 1 d . . . H9A H 1.1880 0.0251 0.4133 0.068 Uiso 1 1 calc R . . C10 C 0.9939(4) 0.0415(2) 0.3647(2) 0.0568(10) Uani 1 1 d . . . H10A H 0.9526 0.0014 0.3920 0.068 Uiso 1 1 calc R . . C11 C 0.9124(4) 0.0852(2) 0.3113(2) 0.0475(9) Uani 1 1 d . . . H11A H 0.8174 0.0739 0.3024 0.057 Uiso 1 1 calc R . . C12 C 0.5872(4) 0.1704(2) 0.39739(19) 0.0453(8) Uani 1 1 d . . . H12A H 0.6328 0.1251 0.4138 0.054 Uiso 1 1 calc R . . C13 C 0.5026(4) 0.2059(2) 0.4486(2) 0.0524(10) Uani 1 1 d . . . H13A H 0.4912 0.1860 0.4994 0.063 Uiso 1 1 calc R . . C14 C 0.4347(4) 0.2718(2) 0.4230(2) 0.0507(9) Uani 1 1 d . . . H14A H 0.3749 0.2967 0.4567 0.061 Uiso 1 1 calc R . . C15 C 0.4527(4) 0.3014(2) 0.34983(19) 0.0419(8) Uani 1 1 d . . . H15A H 0.4041 0.3455 0.3324 0.050 Uiso 1 1 calc R . . C16 C 0.5459(3) 0.26447(18) 0.30078(18) 0.0329(7) Uani 1 1 d . . . C17 C 0.5094(3) 0.34128(17) 0.18426(17) 0.0326(7) Uani 1 1 d . . . C18 C 0.3675(3) 0.3325(2) 0.1682(2) 0.0427(8) Uani 1 1 d . . . H18A H 0.3216 0.2905 0.1898 0.051 Uiso 1 1 calc R . . C19 C 0.2926(4) 0.3840(2) 0.1214(2) 0.0491(9) Uani 1 1 d . . . H19A H 0.1967 0.3764 0.1111 0.059 Uiso 1 1 calc R . . C20 C 0.3563(4) 0.4465(2) 0.0895(2) 0.0463(8) Uani 1 1 d . . . H20A H 0.3045 0.4822 0.0586 0.056 Uiso 1 1 calc R . . C21 C 0.4971(4) 0.4555(2) 0.10380(19) 0.0448(8) Uani 1 1 d . . . H21A H 0.5424 0.4973 0.0814 0.054 Uiso 1 1 calc R . . C22 C 0.5731(4) 0.40412(19) 0.15058(19) 0.0396(8) Uani 1 1 d . . . H22A H 0.6692 0.4116 0.1599 0.047 Uiso 1 1 calc R . . C23 C 0.5757(3) 0.09780(19) 0.13774(19) 0.0378(7) Uani 1 1 d . . . C24 C 0.5794(5) 0.0164(2) 0.1707(3) 0.0627(11) Uani 1 1 d . . . H24A H 0.5299 -0.0176 0.1337 0.094 Uiso 1 1 calc R . . H24B H 0.5354 0.0155 0.2209 0.094 Uiso 1 1 calc R . . H24C H 0.6751 -0.0003 0.1786 0.094 Uiso 1 1 calc R . . C25 C 0.6452(4) 0.0981(3) 0.0586(2) 0.0579(10) Uani 1 1 d . . . H25A H 0.5971 0.0627 0.0224 0.087 Uiso 1 1 calc R . . H25B H 0.7416 0.0825 0.0669 0.087 Uiso 1 1 calc R . . H25C H 0.6411 0.1492 0.0363 0.087 Uiso 1 1 calc R . . C26 C 0.4245(4) 0.1222(2) 0.1233(2) 0.0550(10) Uani 1 1 d . . . H26A H 0.3769 0.0862 0.0875 0.082 Uiso 1 1 calc R . . H26B H 0.4208 0.1730 0.1002 0.082 Uiso 1 1 calc R . . H26C H 0.3796 0.1228 0.1732 0.082 Uiso 1 1 calc R . . C27 C 1.0268(5) 0.3888(3) 0.3139(3) 0.0832(15) Uani 1 1 d . . . H27A H 1.0735 0.4039 0.2663 0.100 Uiso 1 1 calc R . . H27B H 1.0697 0.3417 0.3350 0.100 Uiso 1 1 calc R . . C28 C 1.0361(6) 0.4519(4) 0.3750(3) 0.1002(19) Uani 1 1 d . . . H28A H 1.1088 0.4406 0.4162 0.120 Uiso 1 1 calc R . . H28B H 1.0573 0.5010 0.3504 0.120 Uiso 1 1 calc R . . C29 C 0.9012(6) 0.4543(3) 0.4080(3) 0.0936(17) Uani 1 1 d . . . H29A H 0.9000 0.4227 0.4557 0.112 Uiso 1 1 calc R . . H29B H 0.8761 0.5069 0.4214 0.112 Uiso 1 1 calc R . . C30 C 0.8097(6) 0.4250(6) 0.3478(5) 0.177(5) Uani 1 1 d . . . H30A H 0.7655 0.4674 0.3179 0.213 Uiso 1 1 calc R . . H30B H 0.7365 0.3951 0.3713 0.213 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0317(2) 0.0359(2) 0.0395(2) -0.00333(17) 0.00285(14) -0.00085(18) Li1 0.032(3) 0.041(3) 0.059(4) -0.002(3) 0.008(2) 0.001(2) N1 0.0281(14) 0.0413(16) 0.0409(15) 0.0008(12) 0.0035(11) 0.0007(11) O1 0.0457(16) 0.078(2) 0.083(2) -0.0376(17) 0.0000(14) -0.0034(15) C1 0.060(3) 0.067(3) 0.053(2) 0.013(2) 0.0027(19) -0.005(2) N2 0.0401(16) 0.0508(19) 0.0459(17) 0.0062(14) 0.0040(12) -0.0009(14) C2 0.069(3) 0.094(4) 0.048(2) 0.012(2) 0.017(2) -0.019(3) N3 0.0330(14) 0.0335(15) 0.0374(14) 0.0026(11) 0.0072(11) 0.0028(12) C3 0.054(3) 0.096(4) 0.061(3) -0.007(3) 0.027(2) -0.006(3) N4 0.0396(15) 0.0323(14) 0.0334(14) 0.0019(11) 0.0024(11) -0.0021(12) C4 0.043(2) 0.062(3) 0.057(2) -0.0041(19) 0.0127(17) 0.0034(18) C5 0.0318(17) 0.044(2) 0.0430(18) -0.0054(15) 0.0042(13) -0.0063(15) C6 0.0302(17) 0.0401(18) 0.0417(18) -0.0068(14) 0.0028(13) 0.0022(14) C7 0.0331(18) 0.052(2) 0.056(2) -0.0012(17) 0.0000(15) 0.0003(16) C8 0.035(2) 0.069(3) 0.068(3) -0.008(2) -0.0084(18) 0.0044(19) C9 0.051(2) 0.058(3) 0.058(2) 0.000(2) -0.0133(18) 0.013(2) C10 0.056(2) 0.050(2) 0.063(2) 0.0113(19) -0.0066(19) 0.0015(19) C11 0.0347(19) 0.051(2) 0.055(2) 0.0022(18) -0.0048(15) 0.0011(17) C12 0.051(2) 0.043(2) 0.0409(19) 0.0080(16) -0.0062(15) -0.0042(18) C13 0.061(2) 0.063(3) 0.0335(18) 0.0058(17) 0.0064(16) -0.014(2) C14 0.050(2) 0.061(3) 0.043(2) -0.0115(18) 0.0138(16) -0.0039(19) C15 0.0424(19) 0.0406(19) 0.0436(19) -0.0046(15) 0.0096(15) 0.0016(15) C16 0.0280(15) 0.0334(17) 0.0372(17) -0.0012(13) 0.0004(12) -0.0049(13) C17 0.0351(16) 0.0285(17) 0.0344(16) -0.0015(13) 0.0039(12) 0.0022(13) C18 0.0398(18) 0.0341(18) 0.055(2) 0.0040(16) 0.0044(15) -0.0033(16) C19 0.0349(19) 0.048(2) 0.064(2) -0.0014(18) -0.0072(16) 0.0039(17) C20 0.050(2) 0.040(2) 0.047(2) 0.0035(16) -0.0060(16) 0.0086(17) C21 0.055(2) 0.0364(19) 0.0430(19) 0.0096(15) 0.0053(16) -0.0019(17) C22 0.0382(18) 0.0393(19) 0.0412(18) 0.0019(15) 0.0024(14) -0.0050(15) C23 0.0382(18) 0.0347(18) 0.0404(18) -0.0017(14) 0.0004(14) -0.0005(14) C24 0.073(3) 0.042(2) 0.072(3) 0.003(2) -0.011(2) -0.009(2) C25 0.064(3) 0.066(3) 0.044(2) -0.0104(19) 0.0053(18) 0.004(2) C26 0.040(2) 0.062(3) 0.062(2) -0.007(2) -0.0042(17) -0.0014(18) C27 0.057(3) 0.099(4) 0.094(4) -0.030(3) 0.008(2) -0.015(3) C28 0.089(4) 0.126(5) 0.086(4) -0.027(3) 0.004(3) -0.054(4) C29 0.098(4) 0.096(4) 0.088(4) -0.032(3) 0.018(3) -0.023(3) C30 0.067(4) 0.271(11) 0.193(7) -0.183(8) -0.001(4) 0.008(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 C23 1.989(3) . ? Zn1 N1 2.049(3) . ? Zn1 N4 2.116(2) . ? Zn1 N3 2.234(3) . ? Zn1 C16 2.597(3) . ? Zn1 Li1 2.667(6) . ? Li1 O1 1.851(7) . ? Li1 N3 2.032(6) . ? Li1 N2 2.032(6) . ? Li1 N1 2.206(6) . ? Li1 C5 2.487(7) . ? N1 C5 1.388(4) . ? N1 C6 1.414(4) . ? O1 C30 1.412(6) . ? O1 C27 1.414(5) . ? C1 N2 1.341(5) . ? C1 C2 1.359(6) . ? N2 C5 1.346(4) . ? C2 C3 1.389(7) . ? N3 C16 1.362(4) . ? N3 C17 1.415(4) . ? C3 C4 1.367(6) . ? N4 C12 1.347(4) . ? N4 C16 1.363(4) . ? C4 C5 1.405(5) . ? C6 C11 1.395(5) . ? C6 C7 1.397(5) . ? C7 C8 1.382(5) . ? C8 C9 1.371(6) . ? C9 C10 1.373(5) . ? C10 C11 1.392(5) . ? C12 C13 1.372(5) . ? C13 C14 1.383(5) . ? C14 C15 1.363(5) . ? C15 C16 1.414(4) . ? C17 C18 1.388(4) . ? C17 C22 1.395(4) . ? C18 C19 1.377(5) . ? C19 C20 1.378(5) . ? C20 C21 1.374(5) . ? C21 C22 1.380(5) . ? C23 C26 1.524(5) . ? C23 C24 1.528(5) . ? C23 C25 1.533(5) . ? C27 C28 1.512(7) . ? C28 C29 1.444(7) . ? C29 C30 1.407(7) . ? 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 C23 Zn1 N1 125.96(12) . . ? C23 Zn1 N4 123.22(12) . . ? N1 Zn1 N4 104.83(10) . . ? C23 Zn1 N3 120.75(12) . . ? N1 Zn1 N3 101.72(10) . . ? N4 Zn1 N3 62.30(10) . . ? C23 Zn1 C16 122.66(11) . . ? N1 Zn1 C16 111.12(10) . . ? N4 Zn1 C16 31.57(10) . . ? N3 Zn1 C16 31.61(9) . . ? C23 Zn1 Li1 146.94(16) . . ? N1 Zn1 Li1 53.88(14) . . ? N4 Zn1 Li1 81.90(14) . . ? N3 Zn1 Li1 47.99(13) . . ? C16 Zn1 Li1 66.34(13) . . ? O1 Li1 N3 120.1(3) . . ? O1 Li1 N2 123.9(3) . . ? N3 Li1 N2 110.2(3) . . ? O1 Li1 N1 120.7(3) . . ? N3 Li1 N1 103.2(3) . . ? N2 Li1 N1 64.8(2) . . ? O1 Li1 C5 121.6(3) . . ? N3 Li1 C5 117.6(3) . . ? N2 Li1 C5 32.72(14) . . ? N1 Li1 C5 33.73(13) . . ? O1 Li1 Zn1 147.8(3) . . ? N3 Li1 Zn1 54.77(15) . . ? N2 Li1 Zn1 82.0(2) . . ? N1 Li1 Zn1 48.61(14) . . ? C5 Li1 Zn1 68.44(17) . . ? C5 N1 C6 119.8(3) . . ? C5 N1 Zn1 113.9(2) . . ? C6 N1 Zn1 119.1(2) . . ? C5 N1 Li1 84.3(2) . . ? C6 N1 Li1 132.5(3) . . ? Zn1 N1 Li1 77.52(17) . . ? C30 O1 C27 108.3(4) . . ? C30 O1 Li1 123.7(3) . . ? C27 O1 Li1 127.6(3) . . ? N2 C1 C2 124.0(4) . . ? C1 N2 C5 118.8(3) . . ? C1 N2 Li1 144.9(3) . . ? C5 N2 Li1 92.6(3) . . ? C1 C2 C3 117.2(4) . . ? C16 N3 C17 119.3(2) . . ? C16 N3 Li1 114.8(3) . . ? C17 N3 Li1 113.7(3) . . ? C16 N3 Zn1 89.08(19) . . ? C17 N3 Zn1 135.9(2) . . ? Li1 N3 Zn1 77.24(18) . . ? C4 C3 C2 120.7(4) . . ? C12 N4 C16 119.2(3) . . ? C12 N4 Zn1 145.5(2) . . ? C16 N4 Zn1 94.08(18) . . ? C3 C4 C5 118.6(4) . . ? N2 C5 N1 112.8(3) . . ? N2 C5 C4 120.7(3) . . ? N1 C5 C4 126.5(3) . . ? N2 C5 Li1 54.7(2) . . ? N1 C5 Li1 62.0(2) . . ? C4 C5 Li1 163.0(3) . . ? C11 C6 C7 117.4(3) . . ? C11 C6 N1 119.4(3) . . ? C7 C6 N1 123.1(3) . . ? C8 C7 C6 121.0(4) . . ? C9 C8 C7 121.2(4) . . ? C8 C9 C10 118.6(4) . . ? C9 C10 C11 121.3(4) . . ? C10 C11 C6 120.5(3) . . ? N4 C12 C13 123.0(3) . . ? C12 C13 C14 117.7(3) . . ? C15 C14 C13 121.3(3) . . ? C14 C15 C16 118.6(3) . . ? N3 C16 N4 111.5(3) . . ? N3 C16 C15 128.4(3) . . ? N4 C16 C15 120.0(3) . . ? N3 C16 Zn1 59.31(16) . . ? N4 C16 Zn1 54.35(15) . . ? C15 C16 Zn1 166.6(2) . . ? C18 C17 C22 117.3(3) . . ? C18 C17 N3 122.8(3) . . ? C22 C17 N3 119.9(3) . . ? C19 C18 C17 121.3(3) . . ? C18 C19 C20 120.9(3) . . ? C21 C20 C19 118.6(3) . . ? C20 C21 C22 120.9(3) . . ? C21 C22 C17 121.1(3) . . ? C26 C23 C24 108.7(3) . . ? C26 C23 C25 108.7(3) . . ? C24 C23 C25 108.7(3) . . ? C26 C23 Zn1 110.1(2) . . ? C24 C23 Zn1 111.7(2) . . ? C25 C23 Zn1 109.0(2) . . ? O1 C27 C28 105.0(4) . . ? C29 C28 C27 105.5(4) . . ? C30 C29 C28 104.5(5) . . ? C29 C30 O1 110.1(5) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.456 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.060 data_aw0121 _database_code_CSD 183655 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common aw0121 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H43 Li N4 O2 Zn' _chemical_formula_weight 612.03 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 12.3776(7) _cell_length_b 18.8123(6) _cell_length_c 14.0799(8) _cell_angle_alpha 90.00 _cell_angle_beta 100.231(2) _cell_angle_gamma 90.00 _cell_volume 3226.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13607 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 25.028 _exptl_crystal_description blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.796 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.983 _exptl_absorpt_correction_T_max 1.027 _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements (Blessing 1995) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method CCD _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19551 _diffrn_reflns_av_R_equivalents 0.1123 _diffrn_reflns_av_sigmaI/netI 0.1160 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.52 _diffrn_reflns_theta_max 25.04 _reflns_number_total 5670 _reflns_number_gt 3588 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction ; 'HKL Denzo and Scalepack (Otwinowski & Minor 1997' ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+2.4448P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5670 _refine_ls_number_parameters 406 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1057 _refine_ls_R_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.1010 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _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 0.37577(3) 0.15364(2) 0.70983(3) 0.03665(14) Uani 1 1 d . . . Li1 Li 0.3078(5) 0.1930(3) 0.5049(4) 0.0362(14) Uani 1 1 d . . . O1 O 0.14929(19) 0.21107(13) 0.47597(16) 0.0435(6) Uani 1 1 d . . . N2 N 0.2533(2) 0.08870(13) 0.64699(19) 0.0353(7) Uani 1 1 d . . . C1 C 0.3691(3) 0.04893(19) 0.4414(3) 0.0515(10) Uani 1 1 d . . . H1A H 0.4155 0.0729 0.4048 0.062 Uiso 1 1 calc R . . O2 O 0.33996(18) 0.23775(12) 0.38729(15) 0.0398(6) Uani 1 1 d . . . N1 N 0.3356(2) 0.08539(14) 0.5134(2) 0.0429(8) Uani 1 1 d . . . C2 C 0.3416(4) -0.01959(19) 0.4170(3) 0.0551(11) Uani 1 1 d . . . H2A H 0.3668 -0.0427 0.3651 0.066 Uiso 1 1 calc R . . N4 N 0.3965(2) 0.24516(13) 0.62523(18) 0.0304(6) Uani 1 1 d . . . C3 C 0.2748(4) -0.05403(19) 0.4721(3) 0.0551(11) Uani 1 1 d . . . H3A H 0.2525 -0.1017 0.4572 0.066 Uiso 1 1 calc R . . N3 N 0.2799(2) 0.24830(13) 0.73058(19) 0.0325(7) Uani 1 1 d . . . C4 C 0.2411(3) -0.02028(17) 0.5471(3) 0.0440(10) Uani 1 1 d . . . H4A H 0.1956 -0.0443 0.5844 0.053 Uiso 1 1 calc R . . C5 C 0.2737(3) 0.05051(17) 0.5695(3) 0.0372(9) Uani 1 1 d . . . C6 C 0.1707(3) 0.06840(16) 0.6976(2) 0.0344(9) Uani 1 1 d . . . C7 C 0.0678(3) 0.04193(17) 0.6537(3) 0.0425(9) Uani 1 1 d . . . H7A H 0.0521 0.0368 0.5855 0.051 Uiso 1 1 calc R . . C8 C -0.0107(3) 0.02329(19) 0.7069(3) 0.0516(11) Uani 1 1 d . . . H8A H -0.0782 0.0034 0.6754 0.062 Uiso 1 1 calc R . . C9 C 0.0076(3) 0.03325(19) 0.8057(3) 0.0530(11) Uani 1 1 d . . . H9A H -0.0469 0.0206 0.8424 0.064 Uiso 1 1 calc R . . C10 C 0.1060(3) 0.06165(19) 0.8499(3) 0.0490(10) Uani 1 1 d . . . H10A H 0.1189 0.0693 0.9177 0.059 Uiso 1 1 calc R . . C11 C 0.1862(3) 0.07931(17) 0.7975(3) 0.0418(9) Uani 1 1 d . . . H11A H 0.2533 0.0992 0.8298 0.050 Uiso 1 1 calc R . . C12 C 0.2045(3) 0.27872(18) 0.7746(2) 0.0410(9) Uani 1 1 d . . . H12A H 0.1704 0.2507 0.8170 0.049 Uiso 1 1 calc R . . C13 C 0.1743(3) 0.34876(19) 0.7613(3) 0.0463(10) Uani 1 1 d . . . H13A H 0.1218 0.3692 0.7948 0.056 Uiso 1 1 calc R . . C14 C 0.2227(3) 0.38896(18) 0.6973(3) 0.0432(9) Uani 1 1 d . . . H14A H 0.2036 0.4376 0.6867 0.052 Uiso 1 1 calc R . . C15 C 0.2979(3) 0.35833(16) 0.6496(2) 0.0363(8) Uani 1 1 d . . . H15A H 0.3298 0.3851 0.6044 0.044 Uiso 1 1 calc R . . C16 C 0.3274(3) 0.28705(16) 0.6681(2) 0.0291(8) Uani 1 1 d . . . C17 C 0.4950(3) 0.27107(16) 0.6033(2) 0.0314(8) Uani 1 1 d . . . C18 C 0.5428(3) 0.33665(18) 0.6325(2) 0.0370(8) Uani 1 1 d . . . H18A H 0.5063 0.3681 0.6692 0.044 Uiso 1 1 calc R . . C19 C 0.6426(3) 0.3566(2) 0.6090(3) 0.0499(10) Uani 1 1 d . . . H19A H 0.6736 0.4013 0.6303 0.060 Uiso 1 1 calc R . . C20 C 0.6974(3) 0.3129(2) 0.5552(3) 0.0566(11) Uani 1 1 d . . . H20A H 0.7649 0.3273 0.5380 0.068 Uiso 1 1 calc R . . C21 C 0.6523(3) 0.2476(2) 0.5269(3) 0.0513(11) Uani 1 1 d . . . H21A H 0.6895 0.2166 0.4903 0.062 Uiso 1 1 calc R . . C22 C 0.5537(3) 0.22666(19) 0.5510(2) 0.0399(9) Uani 1 1 d . . . H22A H 0.5251 0.1810 0.5317 0.048 Uiso 1 1 calc R . . C23 C 0.5048(3) 0.11428(18) 0.7981(3) 0.0483(10) Uani 1 1 d D . . H23A H 0.5700 0.1215 0.7675 0.058 Uiso 1 1 calc R A 1 H23B H 0.5160 0.1431 0.8579 0.058 Uiso 1 1 calc R A 1 C27 C 0.3107(3) 0.31178(18) 0.3725(3) 0.0464(10) Uani 1 1 d . . . H27A H 0.3673 0.3428 0.4101 0.056 Uiso 1 1 calc R . . H27B H 0.2391 0.3217 0.3920 0.056 Uiso 1 1 calc R . . C28 C 0.3040(3) 0.3235(2) 0.2659(3) 0.0523(11) Uani 1 1 d . . . H28A H 0.3145 0.3742 0.2511 0.063 Uiso 1 1 calc R . . H28B H 0.2330 0.3069 0.2289 0.063 Uiso 1 1 calc R . . C29 C 0.3979(3) 0.2786(2) 0.2455(3) 0.0540(11) Uani 1 1 d . . . H29A H 0.4686 0.3043 0.2617 0.065 Uiso 1 1 calc R . . H29B H 0.3866 0.2640 0.1768 0.065 Uiso 1 1 calc R . . C30 C 0.3948(3) 0.2150(2) 0.3110(3) 0.0516(10) Uani 1 1 d . . . H30A H 0.3545 0.1752 0.2748 0.062 Uiso 1 1 calc R . . H30B H 0.4703 0.1989 0.3376 0.062 Uiso 1 1 calc R . . C31 C 0.0931(3) 0.1817(2) 0.3857(3) 0.0597(12) Uani 1 1 d . . . H31A H 0.1357 0.1419 0.3650 0.072 Uiso 1 1 calc R . . H31B H 0.0829 0.2185 0.3347 0.072 Uiso 1 1 calc R . . C32 C -0.0126(3) 0.1568(2) 0.4039(3) 0.0553(10) Uani 1 1 d . . . H32A H -0.0071 0.1074 0.4288 0.066 Uiso 1 1 calc R . . H32B H -0.0687 0.1585 0.3443 0.066 Uiso 1 1 calc R . . C33 C -0.0408(3) 0.2073(2) 0.4785(3) 0.0552(11) Uani 1 1 d . . . H33A H -0.0866 0.1838 0.5202 0.066 Uiso 1 1 calc R . . H33B H -0.0805 0.2494 0.4477 0.066 Uiso 1 1 calc R . . C34 C 0.0696(3) 0.22799(19) 0.5356(3) 0.0407(9) Uani 1 1 d . . . H34A H 0.0714 0.2794 0.5506 0.049 Uiso 1 1 calc R . . H34B H 0.0851 0.2011 0.5969 0.049 Uiso 1 1 calc R . . C26A C 0.5960(9) -0.0601(5) 0.9237(8) 0.102(4) Uani 0.50 1 d PD B 1 H26A H 0.6562 -0.0712 0.9768 0.153 Uiso 0.50 1 calc PR B 1 H26B H 0.6018 -0.0901 0.8679 0.153 Uiso 0.50 1 calc PR B 1 H26C H 0.5256 -0.0689 0.9442 0.153 Uiso 0.50 1 calc PR B 1 C25A C 0.6027(10) 0.0159(6) 0.8964(11) 0.078(4) Uani 0.50 1 d PD B 1 H25A H 0.6686 0.0234 0.8668 0.094 Uiso 0.50 1 calc PR B 1 H25B H 0.6101 0.0459 0.9550 0.094 Uiso 0.50 1 calc PR B 1 C24A C 0.5025(15) 0.0378(6) 0.8267(9) 0.041(4) Uani 0.50 1 d PD B 1 H24A H 0.4369 0.0292 0.8563 0.049 Uiso 0.50 1 calc PR B 1 H24B H 0.4960 0.0078 0.7682 0.049 Uiso 0.50 1 calc PR B 1 C26 C 0.6543(9) 0.0119(6) 0.9486(6) 0.064(3) Uani 0.50 1 d PD B 2 H26D H 0.7251 -0.0112 0.9718 0.096 Uiso 0.50 1 calc PR B 2 H26E H 0.6001 -0.0050 0.9864 0.096 Uiso 0.50 1 calc PR B 2 H26F H 0.6626 0.0635 0.9558 0.096 Uiso 0.50 1 calc PR B 2 C25 C 0.6151(9) -0.0066(5) 0.8409(6) 0.056(3) Uani 0.50 1 d PD B 2 H25C H 0.6034 -0.0586 0.8351 0.067 Uiso 0.50 1 calc PR B 2 H25D H 0.6741 0.0058 0.8047 0.067 Uiso 0.50 1 calc PR B 2 C24 C 0.5076(17) 0.0316(6) 0.7929(10) 0.044(4) Uani 0.50 1 d PD B 2 H24C H 0.4468 0.0130 0.8230 0.053 Uiso 0.50 1 calc PR B 2 H24D H 0.4920 0.0177 0.7240 0.053 Uiso 0.50 1 calc PR B 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 0.0412(3) 0.0319(2) 0.0343(2) 0.00101(19) -0.00027(18) -0.0022(2) Li1 0.040(4) 0.036(3) 0.031(3) -0.002(2) 0.003(3) 0.004(3) O1 0.0309(14) 0.0665(17) 0.0324(14) -0.0124(12) 0.0038(12) -0.0066(12) N2 0.0414(19) 0.0284(15) 0.0353(17) -0.0021(13) 0.0049(15) -0.0022(13) C1 0.058(3) 0.044(2) 0.056(3) -0.003(2) 0.020(2) 0.003(2) O2 0.0406(15) 0.0483(15) 0.0318(14) 0.0045(11) 0.0099(12) 0.0051(12) N1 0.051(2) 0.0330(16) 0.046(2) -0.0051(14) 0.0116(17) 0.0000(15) C2 0.072(3) 0.041(2) 0.053(3) -0.013(2) 0.013(2) 0.008(2) N4 0.0316(17) 0.0296(15) 0.0307(16) -0.0031(12) 0.0076(13) 0.0002(13) C3 0.076(3) 0.030(2) 0.058(3) -0.0130(19) 0.006(2) -0.003(2) N3 0.0348(17) 0.0345(15) 0.0288(16) -0.0047(13) 0.0075(14) -0.0040(13) C4 0.057(3) 0.0276(19) 0.045(2) -0.0031(17) 0.002(2) -0.0053(18) C5 0.037(2) 0.031(2) 0.041(2) 0.0055(17) -0.0006(18) 0.0049(17) C6 0.039(2) 0.0233(17) 0.038(2) 0.0002(15) -0.0013(18) -0.0003(16) C7 0.047(3) 0.036(2) 0.042(2) 0.0009(17) 0.001(2) 0.0016(18) C8 0.046(3) 0.040(2) 0.068(3) -0.006(2) 0.007(2) -0.0056(19) C9 0.055(3) 0.040(2) 0.071(3) 0.002(2) 0.028(2) 0.000(2) C10 0.061(3) 0.043(2) 0.043(3) -0.0022(18) 0.013(2) -0.002(2) C11 0.048(2) 0.036(2) 0.040(2) -0.0025(17) 0.0025(19) -0.0049(18) C12 0.042(2) 0.046(2) 0.036(2) -0.0091(17) 0.0100(19) -0.0097(19) C13 0.035(2) 0.048(2) 0.059(3) -0.020(2) 0.0167(19) -0.003(2) C14 0.040(2) 0.033(2) 0.057(3) -0.0073(18) 0.007(2) 0.0021(18) C15 0.035(2) 0.033(2) 0.041(2) -0.0006(16) 0.0056(17) -0.0027(16) C16 0.0260(19) 0.0318(19) 0.028(2) -0.0042(15) 0.0014(15) -0.0026(16) C17 0.033(2) 0.0365(19) 0.0237(19) 0.0016(15) 0.0017(16) 0.0039(16) C18 0.035(2) 0.043(2) 0.034(2) 0.0035(16) 0.0096(16) 0.0015(18) C19 0.044(3) 0.050(2) 0.056(3) 0.010(2) 0.011(2) -0.003(2) C20 0.039(3) 0.071(3) 0.062(3) 0.020(2) 0.015(2) 0.003(2) C21 0.042(3) 0.075(3) 0.039(2) 0.006(2) 0.0123(19) 0.020(2) C22 0.038(2) 0.047(2) 0.033(2) -0.0020(17) -0.0007(17) 0.0094(18) C23 0.037(2) 0.050(2) 0.056(3) 0.0049(19) 0.0010(19) -0.0046(19) C27 0.045(2) 0.043(2) 0.052(3) 0.0045(18) 0.009(2) 0.0059(19) C28 0.046(3) 0.063(3) 0.047(3) 0.0189(19) 0.004(2) 0.001(2) C29 0.047(3) 0.071(3) 0.046(3) 0.005(2) 0.013(2) -0.005(2) C30 0.053(3) 0.065(3) 0.041(2) -0.001(2) 0.020(2) 0.009(2) C31 0.048(3) 0.088(3) 0.043(3) -0.027(2) 0.006(2) -0.012(2) C32 0.045(3) 0.069(3) 0.049(3) -0.012(2) 0.001(2) -0.009(2) C33 0.033(2) 0.085(3) 0.047(3) -0.007(2) 0.007(2) 0.003(2) C34 0.033(2) 0.050(2) 0.040(2) -0.0067(17) 0.0099(18) 0.0023(18) C26A 0.093(9) 0.114(9) 0.102(9) 0.025(7) 0.024(7) 0.053(8) C25A 0.059(8) 0.063(8) 0.111(14) 0.043(9) 0.009(9) 0.022(7) C24A 0.037(6) 0.055(6) 0.030(9) 0.024(5) 0.002(6) 0.007(5) C26 0.073(8) 0.066(7) 0.048(7) 0.017(5) -0.003(5) 0.041(6) C25 0.070(7) 0.052(6) 0.041(6) 0.003(4) -0.002(5) 0.021(5) C24 0.057(8) 0.049(6) 0.025(8) 0.010(5) 0.003(7) -0.006(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 C23 1.985(4) . ? Zn1 N2 2.024(3) . ? Zn1 N4 2.135(3) . ? Zn1 N3 2.188(3) . ? Zn1 Li1 2.952(5) . ? Li1 O2 1.961(6) . ? Li1 O1 1.961(6) . ? Li1 N1 2.054(6) . ? Li1 N4 2.092(6) . ? O1 C34 1.440(4) . ? O1 C31 1.445(4) . ? N2 C5 1.367(4) . ? N2 C6 1.399(4) . ? C1 N1 1.349(4) . ? C1 C2 1.361(5) . ? O2 C30 1.434(4) . ? O2 C27 1.445(4) . ? N1 C5 1.363(4) . ? C2 C3 1.390(5) . ? N4 C16 1.379(4) . ? N4 C17 1.397(4) . ? C3 C4 1.360(5) . ? N3 C12 1.337(4) . ? N3 C16 1.354(4) . ? C4 C5 1.411(4) . ? C6 C11 1.401(5) . ? C6 C7 1.404(5) . ? C7 C8 1.373(5) . ? C8 C9 1.382(5) . ? C9 C10 1.373(5) . ? C10 C11 1.379(5) . ? C12 C13 1.373(5) . ? C13 C14 1.391(5) . ? C14 C15 1.368(4) . ? C15 C16 1.402(4) . ? C17 C18 1.398(4) . ? C17 C22 1.400(4) . ? C18 C19 1.387(5) . ? C19 C20 1.376(5) . ? C20 C21 1.378(5) . ? C21 C22 1.381(5) . ? C23 C24A 1.496(11) . ? C23 C24 1.559(11) . ? C27 C28 1.505(5) . ? C28 C29 1.506(5) . ? C29 C30 1.515(5) . ? C31 C32 1.455(5) . ? C32 C33 1.503(5) . ? C33 C34 1.508(5) . ? C26A C25A 1.486(11) . ? C25A C24A 1.496(12) . ? C26 C25 1.547(10) . ? C25 C24 1.557(11) . ? 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 C23 Zn1 N2 120.36(13) . . ? C23 Zn1 N4 119.17(13) . . ? N2 Zn1 N4 113.44(10) . . ? C23 Zn1 N3 127.96(13) . . ? N2 Zn1 N3 99.66(10) . . ? N4 Zn1 N3 62.61(10) . . ? C23 Zn1 Li1 139.80(16) . . ? N2 Zn1 Li1 70.31(13) . . ? N4 Zn1 Li1 45.09(13) . . ? N3 Zn1 Li1 81.89(13) . . ? O2 Li1 O1 95.5(3) . . ? O2 Li1 N1 114.5(3) . . ? O1 Li1 N1 109.5(3) . . ? O2 Li1 N4 109.1(3) . . ? O1 Li1 N4 116.7(3) . . ? N1 Li1 N4 110.9(3) . . ? O2 Li1 Zn1 150.2(3) . . ? O1 Li1 Zn1 110.3(2) . . ? N1 Li1 Zn1 71.34(18) . . ? N4 Li1 Zn1 46.29(13) . . ? C34 O1 C31 108.9(3) . . ? C34 O1 Li1 132.9(3) . . ? C31 O1 Li1 115.1(3) . . ? C5 N2 C6 121.2(3) . . ? C5 N2 Zn1 115.8(2) . . ? C6 N2 Zn1 120.0(2) . . ? N1 C1 C2 125.0(4) . . ? C30 O2 C27 108.7(3) . . ? C30 O2 Li1 134.3(3) . . ? C27 O2 Li1 116.9(3) . . ? C1 N1 C5 118.1(3) . . ? C1 N1 Li1 121.9(3) . . ? C5 N1 Li1 113.7(3) . . ? C1 C2 C3 116.6(4) . . ? C16 N4 C17 122.0(3) . . ? C16 N4 Li1 110.2(3) . . ? C17 N4 Li1 109.8(2) . . ? C16 N4 Zn1 94.08(18) . . ? C17 N4 Zn1 126.9(2) . . ? Li1 N4 Zn1 88.62(17) . . ? C4 C3 C2 120.7(3) . . ? C12 N3 C16 119.3(3) . . ? C12 N3 Zn1 148.2(2) . . ? C16 N3 Zn1 92.47(19) . . ? C3 C4 C5 120.0(4) . . ? N1 C5 N2 114.4(3) . . ? N1 C5 C4 119.5(3) . . ? N2 C5 C4 126.1(3) . . ? N2 C6 C11 119.3(3) . . ? N2 C6 C7 124.1(3) . . ? C11 C6 C7 116.5(3) . . ? C8 C7 C6 121.7(4) . . ? C7 C8 C9 120.5(4) . . ? C10 C9 C8 118.9(4) . . ? C9 C10 C11 121.1(4) . . ? C10 C11 C6 121.2(4) . . ? N3 C12 C13 122.9(3) . . ? C12 C13 C14 118.2(3) . . ? C15 C14 C13 119.9(3) . . ? C14 C15 C16 119.3(3) . . ? N3 C16 N4 110.6(3) . . ? N3 C16 C15 120.5(3) . . ? N4 C16 C15 128.8(3) . . ? N4 C17 C18 125.7(3) . . ? N4 C17 C22 117.6(3) . . ? C18 C17 C22 116.7(3) . . ? C19 C18 C17 121.2(3) . . ? C20 C19 C18 121.1(4) . . ? C19 C20 C21 118.5(4) . . ? C20 C21 C22 120.9(4) . . ? C21 C22 C17 121.5(3) . . ? C24A C23 C24 18.9(9) . . ? C24A C23 Zn1 118.4(7) . . ? C24 C23 Zn1 111.4(7) . . ? O2 C27 C28 104.6(3) . . ? C27 C28 C29 101.6(3) . . ? C28 C29 C30 102.8(3) . . ? O2 C30 C29 106.7(3) . . ? O1 C31 C32 106.0(3) . . ? C31 C32 C33 104.3(3) . . ? C32 C33 C34 103.5(3) . . ? O1 C34 C33 106.4(3) . . ? C26A C25A C24A 110.8(12) . . ? C25A C24A C23 112.8(14) . . ? C26 C25 C24 114.6(9) . . ? C25 C24 C23 117.7(14) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.283 _refine_diff_density_min -0.504 _refine_diff_density_rms 0.063