# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 182 _journal_volume ? _journal_page_first ? _journal_year ? loop_ _publ_author_name 'Redshaw, Carl' 'Jana, Surajit' 'Shang, Congxiao' 'Elsegood, Mark' 'Lu, Xuesong' 'Guo, Zhengxiao' _publ_contact_author_name 'Redshaw, Carl' _publ_contact_author_email carl.redshaw@uea.ac.uk _publ_section_title ; Enhancement of H2 uptake via fluorination but not lithiation for Zn4N8 and Zn4N6O type clusters. ; # Attachment '- Redshaw.CIF' data_1 _database_code_depnum_ccdc_archive 'CCDC 790909' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H28 F20 N8 Zn4, 0.5(C7 H8)' _chemical_formula_sum 'C35.50 H32 F20 N8 Zn4' _chemical_formula_weight 1212.17 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' 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 41.8755(9) _cell_length_b 10.1152(2) _cell_length_c 21.2258(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.1503(10) _cell_angle_gamma 90.00 _cell_volume 8543.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 69533 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4808 _exptl_absorpt_coefficient_mu 2.346 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.651 _exptl_absorpt_correction_T_max 0.933 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 49302 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -51 _diffrn_reflns_limit_h_max 54 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.56 _reflns_number_total 9797 _reflns_number_gt 7162 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0000P)^2^+139.2028P] 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 9797 _refine_ls_number_parameters 585 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1082 _refine_ls_R_factor_gt 0.0763 _refine_ls_wR_factor_ref 0.1427 _refine_ls_wR_factor_gt 0.1305 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.158582(18) 0.65353(7) 0.15892(3) 0.02934(17) Uani 1 1 d . . . Zn2 Zn 0.181063(17) 0.44892(7) 0.06801(3) 0.02513(16) Uani 1 1 d . . . Zn3 Zn 0.105982(17) 0.37840(7) 0.07856(4) 0.02753(17) Uani 1 1 d . . . Zn4 Zn 0.124339(18) 0.65456(7) -0.00395(3) 0.02918(17) Uani 1 1 d . . . C1 C 0.17013(16) 0.7919(7) 0.2320(3) 0.0375(16) Uani 1 1 d . . . C2 C 0.19591(17) 0.8840(7) 0.2388(3) 0.0368(15) Uani 1 1 d . . . F2 F 0.21906(10) 0.8615(4) 0.2076(2) 0.0466(10) Uani 1 1 d . . . C3 C 0.20048(18) 0.9985(7) 0.2759(3) 0.0418(17) Uani 1 1 d . . . F3 F 0.22603(12) 1.0826(4) 0.2791(2) 0.0571(12) Uani 1 1 d . . . C4 C 0.1778(2) 1.0251(8) 0.3099(3) 0.054(2) Uani 1 1 d . . . F4 F 0.18152(14) 1.1354(5) 0.3459(2) 0.0715(15) Uani 1 1 d . . . C5 C 0.15238(19) 0.9341(8) 0.3063(3) 0.0457(19) Uani 1 1 d . . . F5 F 0.13104(12) 0.9613(6) 0.3414(2) 0.0715(15) Uani 1 1 d . . . C6 C 0.14977(18) 0.8241(7) 0.2690(3) 0.0415(17) Uani 1 1 d . . . F6 F 0.12426(11) 0.7400(5) 0.2690(2) 0.0583(12) Uani 1 1 d . . . C7 C 0.22354(15) 0.3446(6) 0.0755(3) 0.0254(12) Uani 1 1 d . . . C8 C 0.22687(15) 0.2147(6) 0.0959(3) 0.0293(13) Uani 1 1 d . . . F8 F 0.20124(9) 0.1513(4) 0.11058(18) 0.0350(8) Uani 1 1 d . . . C9 C 0.25525(15) 0.1377(7) 0.1032(3) 0.0320(14) Uani 1 1 d . . . F9 F 0.25685(10) 0.0103(4) 0.12109(19) 0.0440(10) Uani 1 1 d . . . C10 C 0.28222(16) 0.1957(7) 0.0900(3) 0.0350(15) Uani 1 1 d . . . F10 F 0.31039(9) 0.1249(4) 0.09618(19) 0.0474(10) Uani 1 1 d . . . C11 C 0.28034(16) 0.3246(7) 0.0689(3) 0.0350(15) Uani 1 1 d . . . F11 F 0.30646(9) 0.3809(4) 0.05412(19) 0.0432(10) Uani 1 1 d . . . C12 C 0.25144(16) 0.3950(6) 0.0632(3) 0.0316(14) Uani 1 1 d . . . F12 F 0.25098(9) 0.5226(4) 0.04170(19) 0.0403(9) Uani 1 1 d . . . C13 C 0.07637(15) 0.2252(6) 0.0866(3) 0.0275(13) Uani 1 1 d . . . C14 C 0.09025(16) 0.1133(6) 0.1203(3) 0.0337(14) Uani 1 1 d . . . F14 F 0.12438(10) 0.1044(4) 0.1483(2) 0.0578(12) Uani 1 1 d . . . C15 C 0.07224(17) 0.0039(6) 0.1290(3) 0.0347(15) Uani 1 1 d . . . F15 F 0.08773(11) -0.1006(4) 0.1631(2) 0.0610(13) Uani 1 1 d . . . C16 C 0.03847(18) 0.0062(6) 0.1027(4) 0.0380(16) Uani 1 1 d . . . F16 F 0.02017(11) -0.0990(4) 0.1098(2) 0.0558(12) Uani 1 1 d . . . C17 C 0.02320(16) 0.1144(7) 0.0676(4) 0.0406(16) Uani 1 1 d . . . F17 F -0.01089(10) 0.1167(5) 0.0404(3) 0.0670(14) Uani 1 1 d . . . C18 C 0.04233(16) 0.2194(7) 0.0603(3) 0.0359(15) Uani 1 1 d . . . F18 F 0.02539(10) 0.3233(4) 0.0234(3) 0.0627(14) Uani 1 1 d . . . C19 C 0.09755(15) 0.7615(6) -0.0822(3) 0.0296(13) Uani 1 1 d . . . C20 C 0.09334(16) 0.7268(7) -0.1467(3) 0.0345(15) Uani 1 1 d . . . F20 F 0.10835(11) 0.6142(4) -0.15981(19) 0.0482(10) Uani 1 1 d . . . C21 C 0.07461(17) 0.7961(7) -0.2010(3) 0.0386(16) Uani 1 1 d . . . F21 F 0.07129(12) 0.7555(5) -0.26360(19) 0.0578(12) Uani 1 1 d . . . C22 C 0.05898(18) 0.9112(7) -0.1919(4) 0.0437(18) Uani 1 1 d . . . F22 F 0.04081(12) 0.9830(5) -0.2441(2) 0.0628(13) Uani 1 1 d . . . C23 C 0.06282(17) 0.9542(7) -0.1279(4) 0.0392(16) Uani 1 1 d . . . F23 F 0.04836(11) 1.0673(4) -0.1186(2) 0.0542(11) Uani 1 1 d . . . C24 C 0.08150(16) 0.8765(6) -0.0759(3) 0.0314(14) Uani 1 1 d . . . F24 F 0.08477(10) 0.9240(4) -0.01303(19) 0.0413(9) Uani 1 1 d . . . N1 N 0.18662(13) 0.6445(5) 0.0955(2) 0.0282(11) Uani 1 1 d . . . H1 H 0.2090 0.6647 0.1172 0.034 Uiso 1 1 calc R . . N2 N 0.17271(13) 0.7310(5) 0.0375(2) 0.0305(12) Uani 1 1 d . . . C25 C 0.19302(17) 0.7201(7) -0.0078(3) 0.0384(16) Uani 1 1 d . . . H25A H 0.2160 0.7503 0.0148 0.058 Uiso 1 1 calc R . . H25B H 0.1830 0.7749 -0.0471 0.058 Uiso 1 1 calc R . . H25C H 0.1936 0.6277 -0.0214 0.058 Uiso 1 1 calc R . . C26 C 0.17264(19) 0.8705(6) 0.0577(4) 0.0416(17) Uani 1 1 d . . . H26A H 0.1588 0.8800 0.0870 0.062 Uiso 1 1 calc R . . H26B H 0.1634 0.9257 0.0182 0.062 Uiso 1 1 calc R . . H26C H 0.1957 0.8985 0.0811 0.062 Uiso 1 1 calc R . . N3 N 0.15542(12) 0.3802(5) 0.1311(2) 0.0269(11) Uani 1 1 d . . . H3 H 0.1620 0.2930 0.1417 0.032 Uiso 1 1 calc R . . N4 N 0.16599(13) 0.4570(5) 0.1928(2) 0.0293(11) Uani 1 1 d . . . C27 C 0.14919(18) 0.4058(7) 0.2396(3) 0.0392(16) Uani 1 1 d . . . H27A H 0.1249 0.4001 0.2172 0.059 Uiso 1 1 calc R . . H27B H 0.1535 0.4656 0.2777 0.059 Uiso 1 1 calc R . . H27C H 0.1580 0.3178 0.2550 0.059 Uiso 1 1 calc R . . C28 C 0.20286(16) 0.4416(7) 0.2247(3) 0.0389(16) Uani 1 1 d . . . H28A H 0.2081 0.3483 0.2355 0.058 Uiso 1 1 calc R . . H28B H 0.2100 0.4943 0.2655 0.058 Uiso 1 1 calc R . . H28C H 0.2147 0.4722 0.1943 0.058 Uiso 1 1 calc R . . N5 N 0.13925(12) 0.4660(5) -0.0140(2) 0.0275(11) Uani 1 1 d . . . H5 H 0.1455 0.4594 -0.0522 0.033 Uiso 1 1 calc R . . N6 N 0.11419(12) 0.3647(5) -0.0147(2) 0.0273(11) Uani 1 1 d . . . C29 C 0.08433(17) 0.3805(7) -0.0740(3) 0.0365(15) Uani 1 1 d . . . H29A H 0.0759 0.4713 -0.0759 0.055 Uiso 1 1 calc R . . H29B H 0.0668 0.3186 -0.0715 0.055 Uiso 1 1 calc R . . H29C H 0.0906 0.3620 -0.1140 0.055 Uiso 1 1 calc R . . C30 C 0.12857(16) 0.2314(6) -0.0183(3) 0.0327(14) Uani 1 1 d . . . H30A H 0.1344 0.2237 -0.0594 0.049 Uiso 1 1 calc R . . H30B H 0.1120 0.1636 -0.0175 0.049 Uiso 1 1 calc R . . H30C H 0.1488 0.2191 0.0198 0.049 Uiso 1 1 calc R . . N7 N 0.11313(12) 0.6612(5) 0.0844(3) 0.0312(12) Uani 1 1 d . . . H7 H 0.1044 0.7451 0.0866 0.037 Uiso 1 1 calc R . . N8 N 0.08673(13) 0.5675(5) 0.0861(3) 0.0336(12) Uani 1 1 d . . . C31 C 0.07828(19) 0.5822(7) 0.1489(4) 0.0460(18) Uani 1 1 d . . . H31A H 0.0989 0.5763 0.1867 0.069 Uiso 1 1 calc R . . H31B H 0.0628 0.5117 0.1520 0.069 Uiso 1 1 calc R . . H31C H 0.0676 0.6683 0.1493 0.069 Uiso 1 1 calc R . . C32 C 0.05567(17) 0.6045(7) 0.0320(4) 0.0443(18) Uani 1 1 d . . . H32A H 0.0501 0.6970 0.0373 0.067 Uiso 1 1 calc R . . H32B H 0.0371 0.5476 0.0340 0.067 Uiso 1 1 calc R . . H32C H 0.0594 0.5931 -0.0110 0.067 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 0.0293(4) 0.0325(4) 0.0275(4) -0.0034(3) 0.0107(3) -0.0006(3) Zn2 0.0226(3) 0.0257(4) 0.0279(4) 0.0000(3) 0.0090(3) 0.0010(3) Zn3 0.0236(4) 0.0261(4) 0.0332(4) 0.0018(3) 0.0093(3) 0.0000(3) Zn4 0.0301(4) 0.0279(4) 0.0297(4) 0.0056(3) 0.0095(3) 0.0028(3) C1 0.031(4) 0.053(4) 0.027(3) -0.002(3) 0.006(3) 0.013(3) C2 0.037(4) 0.046(4) 0.025(3) 0.001(3) 0.008(3) 0.007(3) F2 0.040(2) 0.054(3) 0.050(2) -0.016(2) 0.0213(19) -0.010(2) C3 0.042(4) 0.049(4) 0.028(3) 0.005(3) 0.001(3) 0.006(3) F3 0.069(3) 0.043(3) 0.047(3) -0.009(2) 0.000(2) -0.004(2) C4 0.076(6) 0.046(5) 0.025(4) 0.000(3) -0.006(4) 0.031(4) F4 0.105(4) 0.056(3) 0.041(3) -0.013(2) 0.005(3) 0.026(3) C5 0.039(4) 0.067(5) 0.026(3) 0.003(3) 0.004(3) 0.026(4) F5 0.071(3) 0.100(4) 0.052(3) 0.008(3) 0.032(3) 0.046(3) C6 0.040(4) 0.049(4) 0.032(4) 0.004(3) 0.007(3) 0.008(3) F6 0.046(3) 0.077(3) 0.060(3) 0.007(2) 0.029(2) 0.002(2) C7 0.028(3) 0.027(3) 0.020(3) -0.003(2) 0.005(2) 0.000(3) C8 0.023(3) 0.041(4) 0.023(3) -0.003(3) 0.006(2) -0.002(3) F8 0.0307(19) 0.031(2) 0.044(2) 0.0075(16) 0.0130(17) 0.0039(16) C9 0.028(3) 0.039(4) 0.026(3) -0.005(3) 0.003(3) 0.007(3) F9 0.045(2) 0.043(2) 0.041(2) 0.0106(18) 0.0090(19) 0.0214(19) C10 0.024(3) 0.049(4) 0.029(3) -0.005(3) 0.004(3) 0.012(3) F10 0.030(2) 0.065(3) 0.044(2) -0.004(2) 0.0067(18) 0.019(2) C11 0.028(3) 0.048(4) 0.028(3) -0.013(3) 0.007(3) -0.005(3) F11 0.0230(19) 0.063(3) 0.046(2) -0.016(2) 0.0141(17) -0.0084(18) C12 0.034(4) 0.031(3) 0.026(3) -0.008(3) 0.004(3) -0.007(3) F12 0.033(2) 0.038(2) 0.053(2) -0.0022(18) 0.0189(18) -0.0083(17) C13 0.024(3) 0.028(3) 0.030(3) 0.000(3) 0.008(3) -0.007(3) C14 0.035(4) 0.029(3) 0.039(4) 0.001(3) 0.013(3) 0.002(3) F14 0.032(2) 0.042(2) 0.092(3) 0.021(2) 0.009(2) 0.0044(19) C15 0.034(4) 0.030(3) 0.041(4) 0.008(3) 0.013(3) 0.010(3) F15 0.053(3) 0.036(2) 0.090(4) 0.023(2) 0.017(3) 0.006(2) C16 0.041(4) 0.027(3) 0.049(4) 0.008(3) 0.019(3) 0.000(3) F16 0.049(3) 0.039(2) 0.082(3) 0.010(2) 0.024(2) -0.013(2) C17 0.024(3) 0.042(4) 0.053(4) -0.004(3) 0.008(3) -0.005(3) F17 0.030(2) 0.054(3) 0.106(4) 0.019(3) 0.006(2) -0.007(2) C18 0.028(3) 0.033(4) 0.047(4) 0.007(3) 0.011(3) 0.004(3) F18 0.031(2) 0.047(3) 0.094(4) 0.028(2) -0.003(2) 0.000(2) C19 0.027(3) 0.028(3) 0.034(3) 0.008(3) 0.011(3) 0.000(3) C20 0.031(4) 0.037(4) 0.039(4) 0.010(3) 0.016(3) 0.004(3) F20 0.063(3) 0.047(2) 0.040(2) 0.0100(19) 0.025(2) 0.017(2) C21 0.034(4) 0.045(4) 0.035(4) 0.008(3) 0.009(3) 0.003(3) F21 0.073(3) 0.068(3) 0.033(2) 0.008(2) 0.017(2) 0.010(2) C22 0.036(4) 0.048(4) 0.045(4) 0.022(3) 0.010(3) 0.004(3) F22 0.060(3) 0.069(3) 0.052(3) 0.028(2) 0.006(2) 0.022(2) C23 0.031(4) 0.034(4) 0.056(5) 0.006(3) 0.020(3) 0.001(3) F23 0.057(3) 0.036(2) 0.070(3) 0.010(2) 0.020(2) 0.015(2) C24 0.029(3) 0.030(3) 0.038(4) 0.002(3) 0.015(3) -0.006(3) F24 0.043(2) 0.037(2) 0.042(2) -0.0009(17) 0.0101(18) 0.0047(18) N1 0.030(3) 0.031(3) 0.025(3) 0.000(2) 0.012(2) -0.004(2) N2 0.036(3) 0.029(3) 0.029(3) 0.000(2) 0.014(2) 0.000(2) C25 0.040(4) 0.045(4) 0.032(3) 0.006(3) 0.015(3) -0.001(3) C26 0.055(5) 0.020(3) 0.051(4) 0.000(3) 0.016(4) 0.002(3) N3 0.029(3) 0.023(3) 0.027(3) 0.000(2) 0.006(2) 0.000(2) N4 0.030(3) 0.034(3) 0.025(3) 0.005(2) 0.011(2) 0.003(2) C27 0.044(4) 0.052(4) 0.024(3) 0.009(3) 0.014(3) 0.002(3) C28 0.036(4) 0.047(4) 0.032(4) 0.003(3) 0.008(3) 0.009(3) N5 0.021(3) 0.032(3) 0.030(3) -0.003(2) 0.009(2) -0.004(2) N6 0.025(3) 0.027(3) 0.027(3) 0.001(2) 0.005(2) 0.000(2) C29 0.038(4) 0.037(4) 0.031(3) -0.004(3) 0.004(3) -0.005(3) C30 0.029(3) 0.030(3) 0.035(3) -0.006(3) 0.004(3) 0.003(3) N7 0.029(3) 0.026(3) 0.038(3) 0.004(2) 0.011(2) 0.003(2) N8 0.025(3) 0.037(3) 0.039(3) 0.006(2) 0.009(2) 0.001(2) C31 0.047(4) 0.041(4) 0.061(5) -0.003(4) 0.033(4) -0.007(3) C32 0.028(4) 0.038(4) 0.063(5) 0.005(3) 0.008(3) 0.008(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 C1 2.033(7) . ? Zn1 N1 2.046(5) . ? Zn1 N7 2.063(5) . ? Zn1 N4 2.104(5) . ? Zn2 C7 2.031(6) . ? Zn2 N1 2.055(5) . ? Zn2 N5 2.056(5) . ? Zn2 N3 2.080(5) . ? Zn3 N3 2.023(5) . ? Zn3 C13 2.025(6) . ? Zn3 N8 2.101(5) . ? Zn3 N6 2.117(5) . ? Zn4 C19 2.007(6) . ? Zn4 N5 2.039(5) . ? Zn4 N7 2.071(5) . ? Zn4 N2 2.089(5) . ? C1 C6 1.367(9) . ? C1 C2 1.399(10) . ? C2 F2 1.353(7) . ? C2 C3 1.379(10) . ? C3 F3 1.352(8) . ? C3 C4 1.387(11) . ? C4 F4 1.333(8) . ? C4 C5 1.391(12) . ? C5 C6 1.350(10) . ? C5 F5 1.358(8) . ? C6 F6 1.366(8) . ? C7 C12 1.373(8) . ? C7 C8 1.377(9) . ? C8 F8 1.367(7) . ? C8 C9 1.388(8) . ? C9 F9 1.339(7) . ? C9 C10 1.378(9) . ? C10 F10 1.351(7) . ? C10 C11 1.372(10) . ? C11 F11 1.354(7) . ? C11 C12 1.377(9) . ? C12 F12 1.367(7) . ? C13 C18 1.361(8) . ? C13 C14 1.368(9) . ? C14 F14 1.369(7) . ? C14 C15 1.383(9) . ? C15 F15 1.331(7) . ? C15 C16 1.349(9) . ? C16 F16 1.347(7) . ? C16 C17 1.365(9) . ? C17 F17 1.363(7) . ? C17 C18 1.368(9) . ? C18 F18 1.369(7) . ? C19 C24 1.371(9) . ? C19 C20 1.371(9) . ? C20 C21 1.368(9) . ? C20 F20 1.370(7) . ? C21 F21 1.356(8) . ? C21 C22 1.378(10) . ? C22 F22 1.345(7) . ? C22 C23 1.388(10) . ? C23 F23 1.338(8) . ? C23 C24 1.381(9) . ? C24 F24 1.385(7) . ? N1 N2 1.473(7) . ? N2 C25 1.474(8) . ? N2 C26 1.475(8) . ? N3 N4 1.468(7) . ? N4 C27 1.479(7) . ? N4 C28 1.489(8) . ? N5 N6 1.463(7) . ? N6 C29 1.482(8) . ? N6 C30 1.489(8) . ? C32 N8 1.490(8) . ? N7 N8 1.465(7) . ? N8 C31 1.490(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Zn1 N1 118.9(2) . . ? C1 Zn1 N7 120.2(2) . . ? N1 Zn1 N7 94.5(2) . . ? C1 Zn1 N4 114.5(2) . . ? N1 Zn1 N4 97.43(19) . . ? N7 Zn1 N4 107.5(2) . . ? C7 Zn2 N1 117.3(2) . . ? C7 Zn2 N5 127.2(2) . . ? N1 Zn2 N5 98.7(2) . . ? C7 Zn2 N3 113.0(2) . . ? N1 Zn2 N3 100.08(19) . . ? N5 Zn2 N3 95.65(19) . . ? N3 Zn3 C13 120.6(2) . . ? N3 Zn3 N8 107.5(2) . . ? C13 Zn3 N8 115.5(2) . . ? N3 Zn3 N6 94.56(19) . . ? C13 Zn3 N6 108.1(2) . . ? N8 Zn3 N6 108.0(2) . . ? C19 Zn4 N5 121.9(2) . . ? C19 Zn4 N7 120.4(2) . . ? N5 Zn4 N7 106.7(2) . . ? C19 Zn4 N2 111.6(2) . . ? N5 Zn4 N2 95.85(19) . . ? N7 Zn4 N2 94.01(19) . . ? C6 C1 C2 112.4(6) . . ? C6 C1 Zn1 124.1(6) . . ? C2 C1 Zn1 122.0(5) . . ? F2 C2 C3 115.3(6) . . ? F2 C2 C1 119.0(6) . . ? C3 C2 C1 125.7(6) . . ? F3 C3 C2 121.7(7) . . ? F3 C3 C4 120.7(7) . . ? C2 C3 C4 117.7(7) . . ? F4 C4 C3 119.0(9) . . ? F4 C4 C5 122.4(8) . . ? C3 C4 C5 118.6(7) . . ? C6 C5 F5 122.8(8) . . ? C6 C5 C4 119.9(7) . . ? F5 C5 C4 117.3(7) . . ? C5 C6 F6 115.7(7) . . ? C5 C6 C1 125.6(8) . . ? F6 C6 C1 118.7(7) . . ? C12 C7 C8 113.9(6) . . ? C12 C7 Zn2 124.7(5) . . ? C8 C7 Zn2 121.4(4) . . ? F8 C8 C7 120.6(5) . . ? F8 C8 C9 114.6(6) . . ? C7 C8 C9 124.8(6) . . ? F9 C9 C10 119.7(6) . . ? F9 C9 C8 122.5(6) . . ? C10 C9 C8 117.7(6) . . ? F10 C10 C11 119.7(6) . . ? F10 C10 C9 120.0(6) . . ? C11 C10 C9 120.2(6) . . ? F11 C11 C10 120.4(6) . . ? F11 C11 C12 120.9(6) . . ? C10 C11 C12 118.7(6) . . ? F12 C12 C7 119.3(6) . . ? F12 C12 C11 116.0(6) . . ? C7 C12 C11 124.6(6) . . ? C18 C13 C14 113.5(6) . . ? C18 C13 Zn3 126.1(5) . . ? C14 C13 Zn3 120.4(5) . . ? C13 C14 F14 119.8(6) . . ? C13 C14 C15 124.8(6) . . ? F14 C14 C15 115.4(6) . . ? F15 C15 C16 120.6(6) . . ? F15 C15 C14 120.9(6) . . ? C16 C15 C14 118.4(6) . . ? F16 C16 C15 120.0(6) . . ? F16 C16 C17 120.5(6) . . ? C15 C16 C17 119.5(6) . . ? F17 C17 C16 119.7(6) . . ? F17 C17 C18 120.8(6) . . ? C16 C17 C18 119.5(6) . . ? C13 C18 C17 124.2(6) . . ? C13 C18 F18 119.5(6) . . ? C17 C18 F18 116.3(6) . . ? C24 C19 C20 113.6(6) . . ? C24 C19 Zn4 122.8(5) . . ? C20 C19 Zn4 123.6(5) . . ? C21 C20 F20 115.8(6) . . ? C21 C20 C19 124.8(6) . . ? F20 C20 C19 119.4(6) . . ? F21 C21 C20 121.8(6) . . ? F21 C21 C22 119.0(6) . . ? C20 C21 C22 119.2(7) . . ? F22 C22 C21 120.8(7) . . ? F22 C22 C23 120.1(7) . . ? C21 C22 C23 119.1(6) . . ? F23 C23 C24 122.6(6) . . ? F23 C23 C22 119.5(6) . . ? C24 C23 C22 117.9(6) . . ? C19 C24 C23 125.3(6) . . ? C19 C24 F24 118.9(6) . . ? C23 C24 F24 115.7(6) . . ? N2 N1 Zn1 111.4(3) . . ? N2 N1 Zn2 110.7(3) . . ? Zn1 N1 Zn2 101.1(2) . . ? N1 N2 C25 110.0(5) . . ? N1 N2 C26 111.2(5) . . ? C25 N2 C26 108.3(5) . . ? N1 N2 Zn4 102.2(3) . . ? C25 N2 Zn4 112.2(4) . . ? C26 N2 Zn4 112.8(4) . . ? N4 N3 Zn3 118.0(3) . . ? N4 N3 Zn2 108.9(3) . . ? Zn3 N3 Zn2 107.1(2) . . ? N3 N4 C27 109.9(5) . . ? N3 N4 C28 109.4(5) . . ? C27 N4 C28 107.5(5) . . ? N3 N4 Zn1 102.9(3) . . ? C27 N4 Zn1 120.7(4) . . ? C28 N4 Zn1 106.0(4) . . ? N6 N5 Zn4 114.5(3) . . ? N6 N5 Zn2 111.7(3) . . ? Zn4 N5 Zn2 101.4(2) . . ? N5 N6 C29 110.3(4) . . ? N5 N6 C30 109.6(4) . . ? C29 N6 C30 107.6(5) . . ? N5 N6 Zn3 105.6(3) . . ? C29 N6 Zn3 116.6(4) . . ? C30 N6 Zn3 107.0(4) . . ? N8 N7 Zn1 118.7(4) . . ? N8 N7 Zn4 112.7(4) . . ? Zn1 N7 Zn4 106.1(2) . . ? N7 N8 C32 107.6(5) . . ? N7 N8 C31 110.4(5) . . ? C32 N8 C31 105.7(5) . . ? N7 N8 Zn3 106.1(3) . . ? C32 N8 Zn3 115.7(4) . . ? C31 N8 Zn3 111.3(4) . . ? 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 N1 Zn1 C1 C6 167.1(5) . . . . ? N7 Zn1 C1 C6 51.9(7) . . . . ? N4 Zn1 C1 C6 -78.4(6) . . . . ? N1 Zn1 C1 C2 2.2(6) . . . . ? N7 Zn1 C1 C2 -113.0(5) . . . . ? N4 Zn1 C1 C2 116.7(5) . . . . ? C6 C1 C2 F2 176.7(6) . . . . ? Zn1 C1 C2 F2 -16.8(9) . . . . ? C6 C1 C2 C3 -2.6(10) . . . . ? Zn1 C1 C2 C3 163.9(5) . . . . ? F2 C2 C3 F3 1.3(9) . . . . ? C1 C2 C3 F3 -179.4(6) . . . . ? F2 C2 C3 C4 -178.8(6) . . . . ? C1 C2 C3 C4 0.5(10) . . . . ? F3 C3 C4 F4 0.2(10) . . . . ? C2 C3 C4 F4 -179.7(6) . . . . ? F3 C3 C4 C5 -178.5(6) . . . . ? C2 C3 C4 C5 1.6(10) . . . . ? F4 C4 C5 C6 179.9(6) . . . . ? C3 C4 C5 C6 -1.4(10) . . . . ? F4 C4 C5 F5 -0.2(10) . . . . ? C3 C4 C5 F5 178.5(6) . . . . ? F5 C5 C6 F6 -0.6(10) . . . . ? C4 C5 C6 F6 179.4(6) . . . . ? F5 C5 C6 C1 179.2(6) . . . . ? C4 C5 C6 C1 -0.9(11) . . . . ? C2 C1 C6 C5 2.8(10) . . . . ? Zn1 C1 C6 C5 -163.4(6) . . . . ? C2 C1 C6 F6 -177.5(6) . . . . ? Zn1 C1 C6 F6 16.3(9) . . . . ? N1 Zn2 C7 C12 -35.9(6) . . . . ? N5 Zn2 C7 C12 91.3(5) . . . . ? N3 Zn2 C7 C12 -151.5(5) . . . . ? N1 Zn2 C7 C8 142.3(4) . . . . ? N5 Zn2 C7 C8 -90.6(5) . . . . ? N3 Zn2 C7 C8 26.6(5) . . . . ? C12 C7 C8 F8 179.4(5) . . . . ? Zn2 C7 C8 F8 1.1(8) . . . . ? C12 C7 C8 C9 -0.6(9) . . . . ? Zn2 C7 C8 C9 -178.9(5) . . . . ? F8 C8 C9 F9 2.2(8) . . . . ? C7 C8 C9 F9 -177.8(5) . . . . ? F8 C8 C9 C10 -179.3(5) . . . . ? C7 C8 C9 C10 0.8(9) . . . . ? F9 C9 C10 F10 -1.2(9) . . . . ? C8 C9 C10 F10 -179.8(5) . . . . ? F9 C9 C10 C11 177.2(5) . . . . ? C8 C9 C10 C11 -1.3(9) . . . . ? F10 C10 C11 F11 0.2(9) . . . . ? C9 C10 C11 F11 -178.2(5) . . . . ? F10 C10 C11 C12 -179.7(5) . . . . ? C9 C10 C11 C12 1.8(9) . . . . ? C8 C7 C12 F12 179.0(5) . . . . ? Zn2 C7 C12 F12 -2.8(8) . . . . ? C8 C7 C12 C11 1.1(9) . . . . ? Zn2 C7 C12 C11 179.4(5) . . . . ? F11 C11 C12 F12 0.3(8) . . . . ? C10 C11 C12 F12 -179.7(5) . . . . ? F11 C11 C12 C7 178.3(5) . . . . ? C10 C11 C12 C7 -1.8(9) . . . . ? N3 Zn3 C13 C18 171.7(5) . . . . ? N8 Zn3 C13 C18 39.6(6) . . . . ? N6 Zn3 C13 C18 -81.4(6) . . . . ? N3 Zn3 C13 C14 -9.0(6) . . . . ? N8 Zn3 C13 C14 -141.1(5) . . . . ? N6 Zn3 C13 C14 97.9(5) . . . . ? C18 C13 C14 F14 178.8(6) . . . . ? Zn3 C13 C14 F14 -0.6(8) . . . . ? C18 C13 C14 C15 -1.1(10) . . . . ? Zn3 C13 C14 C15 179.5(5) . . . . ? C13 C14 C15 F15 -179.4(6) . . . . ? F14 C14 C15 F15 0.8(9) . . . . ? C13 C14 C15 C16 -0.2(10) . . . . ? F14 C14 C15 C16 179.9(6) . . . . ? F15 C15 C16 F16 -1.2(10) . . . . ? C14 C15 C16 F16 179.6(6) . . . . ? F15 C15 C16 C17 -179.7(6) . . . . ? C14 C15 C16 C17 1.1(10) . . . . ? F16 C16 C17 F17 0.9(11) . . . . ? C15 C16 C17 F17 179.4(6) . . . . ? F16 C16 C17 C18 -179.2(6) . . . . ? C15 C16 C17 C18 -0.7(11) . . . . ? C14 C13 C18 C17 1.5(10) . . . . ? Zn3 C13 C18 C17 -179.1(6) . . . . ? C14 C13 C18 F18 -177.9(6) . . . . ? Zn3 C13 C18 F18 1.5(9) . . . . ? F17 C17 C18 C13 179.2(6) . . . . ? C16 C17 C18 C13 -0.7(11) . . . . ? F17 C17 C18 F18 -1.4(10) . . . . ? C16 C17 C18 F18 178.7(6) . . . . ? N5 Zn4 C19 C24 166.3(5) . . . . ? N7 Zn4 C19 C24 27.0(6) . . . . ? N2 Zn4 C19 C24 -81.6(5) . . . . ? N5 Zn4 C19 C20 -13.3(6) . . . . ? N7 Zn4 C19 C20 -152.6(5) . . . . ? N2 Zn4 C19 C20 98.8(6) . . . . ? C24 C19 C20 C21 -1.2(10) . . . . ? Zn4 C19 C20 C21 178.4(5) . . . . ? C24 C19 C20 F20 179.5(5) . . . . ? Zn4 C19 C20 F20 -0.9(9) . . . . ? F20 C20 C21 F21 -0.1(10) . . . . ? C19 C20 C21 F21 -179.5(6) . . . . ? F20 C20 C21 C22 -179.4(6) . . . . ? C19 C20 C21 C22 1.3(11) . . . . ? F21 C21 C22 F22 -0.3(10) . . . . ? C20 C21 C22 F22 178.9(6) . . . . ? F21 C21 C22 C23 -178.9(6) . . . . ? C20 C21 C22 C23 0.3(10) . . . . ? F22 C22 C23 F23 -0.1(10) . . . . ? C21 C22 C23 F23 178.5(6) . . . . ? F22 C22 C23 C24 179.5(6) . . . . ? C21 C22 C23 C24 -1.9(10) . . . . ? C20 C19 C24 C23 -0.5(9) . . . . ? Zn4 C19 C24 C23 179.8(5) . . . . ? C20 C19 C24 F24 -178.0(5) . . . . ? Zn4 C19 C24 F24 2.3(8) . . . . ? F23 C23 C24 C19 -178.4(6) . . . . ? C22 C23 C24 C19 2.0(10) . . . . ? F23 C23 C24 F24 -0.8(9) . . . . ? C22 C23 C24 F24 179.6(6) . . . . ? C1 Zn1 N1 N2 -89.3(4) . . . . ? N7 Zn1 N1 N2 39.0(4) . . . . ? N4 Zn1 N1 N2 147.3(4) . . . . ? C1 Zn1 N1 Zn2 153.0(2) . . . . ? N7 Zn1 N1 Zn2 -78.7(2) . . . . ? N4 Zn1 N1 Zn2 29.6(2) . . . . ? C7 Zn2 N1 N2 112.7(4) . . . . ? N5 Zn2 N1 N2 -27.4(4) . . . . ? N3 Zn2 N1 N2 -124.7(3) . . . . ? C7 Zn2 N1 Zn1 -129.2(2) . . . . ? N5 Zn2 N1 Zn1 90.7(2) . . . . ? N3 Zn2 N1 Zn1 -6.6(2) . . . . ? Zn1 N1 N2 C25 -178.8(4) . . . . ? Zn2 N1 N2 C25 -67.2(5) . . . . ? Zn1 N1 N2 C26 61.2(5) . . . . ? Zn2 N1 N2 C26 172.8(4) . . . . ? Zn1 N1 N2 Zn4 -59.4(3) . . . . ? Zn2 N1 N2 Zn4 52.2(3) . . . . ? C19 Zn4 N2 N1 176.3(3) . . . . ? N5 Zn4 N2 N1 -56.0(3) . . . . ? N7 Zn4 N2 N1 51.3(3) . . . . ? C19 Zn4 N2 C25 -65.9(5) . . . . ? N5 Zn4 N2 C25 61.8(4) . . . . ? N7 Zn4 N2 C25 169.2(4) . . . . ? C19 Zn4 N2 C26 56.8(5) . . . . ? N5 Zn4 N2 C26 -175.5(4) . . . . ? N7 Zn4 N2 C26 -68.2(4) . . . . ? C13 Zn3 N3 N4 -98.6(4) . . . . ? N8 Zn3 N3 N4 36.8(4) . . . . ? N6 Zn3 N3 N4 147.2(4) . . . . ? C13 Zn3 N3 Zn2 138.2(2) . . . . ? N8 Zn3 N3 Zn2 -86.4(2) . . . . ? N6 Zn3 N3 Zn2 24.0(2) . . . . ? C7 Zn2 N3 N4 94.3(4) . . . . ? N1 Zn2 N3 N4 -31.3(4) . . . . ? N5 Zn2 N3 N4 -131.2(3) . . . . ? C7 Zn2 N3 Zn3 -137.1(2) . . . . ? N1 Zn2 N3 Zn3 97.3(2) . . . . ? N5 Zn2 N3 Zn3 -2.6(2) . . . . ? Zn3 N3 N4 C27 60.3(5) . . . . ? Zn2 N3 N4 C27 -177.5(4) . . . . ? Zn3 N3 N4 C28 178.1(4) . . . . ? Zn2 N3 N4 C28 -59.7(5) . . . . ? Zn3 N3 N4 Zn1 -69.5(4) . . . . ? Zn2 N3 N4 Zn1 52.7(3) . . . . ? C1 Zn1 N4 N3 179.2(3) . . . . ? N1 Zn1 N4 N3 -54.3(3) . . . . ? N7 Zn1 N4 N3 42.9(4) . . . . ? C1 Zn1 N4 C27 56.3(5) . . . . ? N1 Zn1 N4 C27 -177.1(5) . . . . ? N7 Zn1 N4 C27 -79.9(5) . . . . ? C1 Zn1 N4 C28 -65.9(4) . . . . ? N1 Zn1 N4 C28 60.7(4) . . . . ? N7 Zn1 N4 C28 157.8(4) . . . . ? C19 Zn4 N5 N6 -85.2(4) . . . . ? N7 Zn4 N5 N6 58.8(4) . . . . ? N2 Zn4 N5 N6 154.8(4) . . . . ? C19 Zn4 N5 Zn2 154.4(2) . . . . ? N7 Zn4 N5 Zn2 -61.5(2) . . . . ? N2 Zn4 N5 Zn2 34.4(2) . . . . ? C7 Zn2 N5 N6 91.7(4) . . . . ? N1 Zn2 N5 N6 -134.1(3) . . . . ? N3 Zn2 N5 N6 -32.9(4) . . . . ? C7 Zn2 N5 Zn4 -146.0(2) . . . . ? N1 Zn2 N5 Zn4 -11.7(2) . . . . ? N3 Zn2 N5 Zn4 89.4(2) . . . . ? Zn4 N5 N6 C29 65.0(5) . . . . ? Zn2 N5 N6 C29 179.6(4) . . . . ? Zn4 N5 N6 C30 -176.7(4) . . . . ? Zn2 N5 N6 C30 -62.2(5) . . . . ? Zn4 N5 N6 Zn3 -61.8(4) . . . . ? Zn2 N5 N6 Zn3 52.7(4) . . . . ? N3 Zn3 N6 N5 -48.1(3) . . . . ? C13 Zn3 N6 N5 -172.4(3) . . . . ? N8 Zn3 N6 N5 62.0(4) . . . . ? N3 Zn3 N6 C29 -171.0(4) . . . . ? C13 Zn3 N6 C29 64.8(5) . . . . ? N8 Zn3 N6 C29 -60.9(4) . . . . ? N3 Zn3 N6 C30 68.6(4) . . . . ? C13 Zn3 N6 C30 -55.7(4) . . . . ? N8 Zn3 N6 C30 178.7(4) . . . . ? C1 Zn1 N7 N8 -104.4(5) . . . . ? N1 Zn1 N7 N8 128.2(4) . . . . ? N4 Zn1 N7 N8 29.0(4) . . . . ? C1 Zn1 N7 Zn4 127.6(3) . . . . ? N1 Zn1 N7 Zn4 0.2(2) . . . . ? N4 Zn1 N7 Zn4 -99.1(2) . . . . ? C19 Zn4 N7 N8 85.8(4) . . . . ? N5 Zn4 N7 N8 -58.9(4) . . . . ? N2 Zn4 N7 N8 -156.2(4) . . . . ? C19 Zn4 N7 Zn1 -142.7(2) . . . . ? N5 Zn4 N7 Zn1 72.6(3) . . . . ? N2 Zn4 N7 Zn1 -24.7(2) . . . . ? Zn1 N7 N8 C32 173.4(4) . . . . ? Zn4 N7 N8 C32 -61.7(5) . . . . ? Zn1 N7 N8 C31 58.5(6) . . . . ? Zn4 N7 N8 C31 -176.6(4) . . . . ? Zn1 N7 N8 Zn3 -62.2(4) . . . . ? Zn4 N7 N8 Zn3 62.7(4) . . . . ? N3 Zn3 N8 N7 37.6(4) . . . . ? C13 Zn3 N8 N7 175.5(3) . . . . ? N6 Zn3 N8 N7 -63.4(4) . . . . ? N3 Zn3 N8 C32 156.8(4) . . . . ? C13 Zn3 N8 C32 -65.2(5) . . . . ? N6 Zn3 N8 C32 55.9(5) . . . . ? N3 Zn3 N8 C31 -82.5(4) . . . . ? C13 Zn3 N8 C31 55.4(5) . . . . ? N6 Zn3 N8 C31 176.5(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 F8 0.93 2.42 3.123(6) 132.0 . N3 H3 F14 0.93 2.51 3.146(6) 126.3 . N5 H5 F10 0.93 2.47 3.260(6) 143.4 7 N7 H7 F15 0.93 2.50 3.291(7) 142.6 1_565 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.032 0.250 211 41 ' ' 2 0.500 -0.033 0.750 211 41 ' ' 3 0.000 0.467 0.750 211 41 ' ' 4 0.000 0.532 0.250 211 41 ' ' _platon_squeeze_details ; Half a toluene per cluster, 4 per cell. ; _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.071 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.133 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 790910' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H28 F20 N6 O Zn4, C2 H3 N' _chemical_formula_sum 'C47 H31 F20 N7 O Zn4' _chemical_formula_weight 1351.27 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 10.6416(19) _cell_length_b 13.399(2) _cell_length_c 34.942(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.088(2) _cell_angle_gamma 90.00 _cell_volume 4962.6(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6977 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 23.56 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2680 _exptl_absorpt_coefficient_mu 2.031 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.823 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6710 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 43133 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.0676 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10393 _reflns_number_gt 7686 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0463P)^2^+119.8667P] 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 SHELXL _refine_ls_extinction_coef 0.0054(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 10393 _refine_ls_number_parameters 717 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1335 _refine_ls_R_factor_gt 0.1067 _refine_ls_wR_factor_ref 0.2629 _refine_ls_wR_factor_gt 0.2492 _refine_ls_goodness_of_fit_ref 1.146 _refine_ls_restrained_S_all 1.146 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.90661(12) 0.67650(9) 0.91346(4) 0.0294(3) Uani 1 1 d . . . Zn2 Zn 0.81625(12) 0.73781(9) 0.82325(4) 0.0292(3) Uani 1 1 d . . . Zn3 Zn 0.69785(12) 0.85458(9) 0.89507(4) 0.0299(3) Uani 1 1 d . . . Zn4 Zn 0.62988(12) 0.62623(9) 0.87565(4) 0.0291(3) Uani 1 1 d . . . O1 O 0.8618(7) 0.7953(5) 0.8773(2) 0.0289(16) Uani 1 1 d . . . H1 H 0.9314 0.8456 0.8778 0.035 Uiso 1 1 calc R . . N1 N 0.9003(8) 0.5693(6) 0.8683(3) 0.0281(19) Uani 1 1 d . . . N2 N 0.7845(8) 0.6021(6) 0.8450(3) 0.0262(18) Uani 1 1 d . . . H2 H 0.7642 0.5570 0.8252 0.031 Uiso 1 1 calc R . . C1 C 1.0072(10) 0.5667(8) 0.8448(3) 0.029(2) Uani 1 1 d . . . C2 C 1.1088(10) 0.6292(9) 0.8533(3) 0.033(2) Uani 1 1 d . . . H2A H 1.1106 0.6721 0.8750 0.040 Uiso 1 1 calc R . . C3 C 1.2068(11) 0.6292(9) 0.8306(3) 0.037(3) Uani 1 1 d . . . H3 H 1.2764 0.6723 0.8368 0.044 Uiso 1 1 calc R . . C4 C 1.2074(11) 0.5672(9) 0.7982(4) 0.036(3) Uani 1 1 d . . . H4A H 1.2748 0.5686 0.7821 0.044 Uiso 1 1 calc R . . C5 C 1.1053(11) 0.5039(10) 0.7909(4) 0.044(3) Uani 1 1 d . . . H5 H 1.1039 0.4589 0.7698 0.052 Uiso 1 1 calc R . . C6 C 1.0045(12) 0.5047(11) 0.8138(4) 0.048(3) Uani 1 1 d . . . H6A H 0.9341 0.4621 0.8079 0.058 Uiso 1 1 calc R . . C7 C 0.8778(13) 0.4693(9) 0.8851(4) 0.043(3) Uani 1 1 d . . . H7A H 0.8061 0.4732 0.9008 0.065 Uiso 1 1 calc R . . H7B H 0.9532 0.4481 0.9011 0.065 Uiso 1 1 calc R . . H7C H 0.8591 0.4209 0.8643 0.065 Uiso 1 1 calc R . . N3 N 0.6278(9) 0.7907(7) 0.8180(3) 0.033(2) Uani 1 1 d . . . N4 N 0.5922(9) 0.7717(7) 0.8567(3) 0.034(2) Uani 1 1 d . . . H4 H 0.5072 0.7862 0.8580 0.041 Uiso 1 1 calc R . . C8 C 0.6085(10) 0.8990(9) 0.8084(3) 0.033(2) Uani 1 1 d . . . C9 C 0.4898(13) 0.9367(10) 0.8054(4) 0.052(4) Uani 1 1 d . . . H9 H 0.4193 0.8948 0.8083 0.062 Uiso 1 1 calc R . . C10 C 0.4735(13) 1.0395(11) 0.7980(5) 0.064(5) Uani 1 1 d . . . H10 H 0.3911 1.0672 0.7947 0.077 Uiso 1 1 calc R . . C11 C 0.5795(12) 1.1007(9) 0.7954(4) 0.044(3) Uani 1 1 d . . . H11 H 0.5701 1.1704 0.7911 0.053 Uiso 1 1 calc R . . C12 C 0.6972(14) 1.0573(10) 0.7992(4) 0.048(3) Uani 1 1 d . . . H12 H 0.7698 1.0982 0.7981 0.058 Uiso 1 1 calc R . . C13 C 0.7121(13) 0.9555(9) 0.8045(3) 0.040(3) Uani 1 1 d . . . H13 H 0.7934 0.9258 0.8055 0.048 Uiso 1 1 calc R . . C14 C 0.5516(10) 0.7280(9) 0.7893(4) 0.038(3) Uani 1 1 d . . . H14A H 0.5635 0.6574 0.7960 0.057 Uiso 1 1 calc R . . H14B H 0.5789 0.7400 0.7637 0.057 Uiso 1 1 calc R . . H14C H 0.4621 0.7453 0.7895 0.057 Uiso 1 1 calc R . . N5 N 0.6904(9) 0.7598(7) 0.9436(3) 0.036(2) Uani 1 1 d . . . N6 N 0.7281(8) 0.6634(6) 0.9271(3) 0.029(2) Uani 1 1 d . . . H6 H 0.7221 0.6123 0.9449 0.035 Uiso 1 1 calc R . . C15 C 0.7730(12) 0.7870(9) 0.9778(3) 0.037(3) Uani 1 1 d . . . C16 C 0.8218(14) 0.7158(11) 1.0046(4) 0.054(4) Uani 1 1 d . . . H16 H 0.8002 0.6475 1.0008 0.065 Uiso 1 1 calc R . . C17 C 0.8997(14) 0.7428(12) 1.0359(4) 0.054(4) Uani 1 1 d . . . H17 H 0.9342 0.6934 1.0533 0.065 Uiso 1 1 calc R . . C18 C 0.9282(19) 0.8418(12) 1.0422(5) 0.081(6) Uani 1 1 d . . . H18 H 0.9816 0.8617 1.0641 0.097 Uiso 1 1 calc R . . C19 C 0.878(3) 0.9118(15) 1.0163(6) 0.143(13) Uani 1 1 d . . . H19 H 0.8959 0.9805 1.0209 0.172 Uiso 1 1 calc R . . C20 C 0.805(2) 0.8849(13) 0.9844(5) 0.105(9) Uani 1 1 d . . . H20 H 0.7744 0.9345 0.9665 0.126 Uiso 1 1 calc R . . C21 C 0.5580(11) 0.7556(9) 0.9534(4) 0.041(3) Uani 1 1 d . . . H21A H 0.5478 0.6995 0.9708 0.061 Uiso 1 1 calc R . . H21B H 0.5018 0.7465 0.9298 0.061 Uiso 1 1 calc R . . H21C H 0.5368 0.8180 0.9659 0.061 Uiso 1 1 calc R . . C22 C 1.0638(10) 0.6890(8) 0.9485(3) 0.033(2) Uani 1 1 d . . . C23 C 1.1132(11) 0.6073(9) 0.9699(4) 0.039(3) Uani 1 1 d . . . F23 F 1.0568(8) 0.5185(5) 0.9647(2) 0.052(2) Uani 1 1 d . . . C24 C 1.2184(13) 0.6120(10) 0.9950(4) 0.043(3) Uani 1 1 d . . . F24 F 1.2676(8) 0.5321(7) 1.0145(2) 0.062(2) Uani 1 1 d . . . C25 C 1.2784(13) 0.7008(11) 0.9999(4) 0.048(3) Uani 1 1 d . . . F25 F 1.3855(7) 0.7079(7) 1.0241(2) 0.063(2) Uani 1 1 d . . . C26 C 1.2336(12) 0.7858(10) 0.9805(4) 0.045(3) Uani 1 1 d . . . F26 F 1.2943(9) 0.8757(7) 0.9854(3) 0.072(3) Uani 1 1 d . . . C27 C 1.1265(11) 0.7756(9) 0.9553(3) 0.037(3) Uani 1 1 d . . . F27 F 1.0834(8) 0.8592(6) 0.9364(3) 0.058(2) Uani 1 1 d . . . C28 C 0.9266(11) 0.7644(8) 0.7815(3) 0.035(3) Uani 1 1 d . . . C29 C 1.0285(11) 0.8269(9) 0.7858(4) 0.039(3) Uani 1 1 d . . . F29 F 1.0440(7) 0.8874(6) 0.8172(2) 0.0491(19) Uani 1 1 d . . . C30 C 1.1158(10) 0.8388(8) 0.7595(4) 0.035(3) Uani 1 1 d . . . F30 F 1.2173(8) 0.9024(7) 0.7645(2) 0.062(2) Uani 1 1 d . . . C31 C 1.1024(11) 0.7812(8) 0.7265(4) 0.035(3) Uani 1 1 d . . . F31 F 1.1875(7) 0.7903(5) 0.7001(2) 0.052(2) Uani 1 1 d . . . C32 C 1.0047(12) 0.7153(8) 0.7205(4) 0.038(3) Uani 1 1 d . . . F32 F 0.9913(9) 0.6578(6) 0.6887(2) 0.060(2) Uani 1 1 d . . . C33 C 0.9193(12) 0.7099(8) 0.7480(4) 0.037(3) Uani 1 1 d . . . F33 F 0.8236(7) 0.6421(6) 0.7420(2) 0.0479(18) Uani 1 1 d . . . C34 C 0.6924(10) 1.0031(8) 0.9003(3) 0.032(2) Uani 1 1 d . . . C35 C 0.5869(12) 1.0517(9) 0.9091(4) 0.042(3) Uani 1 1 d . . . F35 F 0.4866(7) 0.9961(6) 0.9191(3) 0.055(2) Uani 1 1 d . . . C36 C 0.5688(12) 1.1532(9) 0.9075(4) 0.043(3) Uani 1 1 d . . . F36 F 0.4615(7) 1.1968(6) 0.9157(3) 0.064(3) Uani 1 1 d . . . C37 C 0.6690(13) 1.2117(8) 0.8982(4) 0.042(3) Uani 1 1 d . . . F37 F 0.6575(8) 1.3121(5) 0.8969(3) 0.060(2) Uani 1 1 d . . . C38 C 0.7790(12) 1.1690(8) 0.8903(4) 0.040(3) Uani 1 1 d . . . F38 F 0.8776(8) 1.2256(5) 0.8817(2) 0.053(2) Uani 1 1 d . . . C39 C 0.7894(12) 1.0653(9) 0.8912(4) 0.039(3) Uani 1 1 d . . . F39 F 0.8988(6) 1.0242(5) 0.8821(2) 0.0429(17) Uani 1 1 d . . . C40 C 0.4996(11) 0.5172(8) 0.8702(3) 0.033(2) Uani 1 1 d . . . C41 C 0.4132(12) 0.5025(10) 0.8952(4) 0.043(3) Uani 1 1 d . . . F41 F 0.4113(9) 0.5605(7) 0.9271(3) 0.071(3) Uani 1 1 d . . . C42 C 0.3197(14) 0.4278(10) 0.8911(5) 0.055(4) Uani 1 1 d . . . F42 F 0.2349(10) 0.4211(8) 0.9171(3) 0.094(4) Uani 1 1 d . . . C43 C 0.3134(12) 0.3679(10) 0.8605(5) 0.055(4) Uani 1 1 d . . . F43 F 0.2276(9) 0.2932(6) 0.8556(3) 0.076(3) Uani 1 1 d . . . C44 C 0.4014(13) 0.3789(9) 0.8340(4) 0.045(3) Uani 1 1 d . . . F44 F 0.3929(9) 0.3190(7) 0.8032(3) 0.076(3) Uani 1 1 d . . . C45 C 0.4899(11) 0.4531(9) 0.8397(4) 0.038(3) Uani 1 1 d . . . F45 F 0.5711(8) 0.4613(7) 0.8113(2) 0.060(2) Uani 1 1 d . . . N7 N 0.3181(18) 0.8396(9) 0.8741(5) 0.109(8) Uani 1 1 d . . . C46 C 0.2684(15) 0.9118(15) 0.8761(5) 0.068(5) Uani 1 1 d . . . C47 C 0.2173(15) 1.0184(12) 0.8756(7) 0.085(6) Uani 1 1 d . . . H47A H 0.2860 1.0648 0.8834 0.127 Uiso 1 1 calc R . . H47B H 0.1517 1.0237 0.8935 0.127 Uiso 1 1 calc R . . H47C H 0.1813 1.0351 0.8496 0.127 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 0.0302(7) 0.0220(6) 0.0357(7) -0.0004(5) 0.0005(5) 0.0012(5) Zn2 0.0273(6) 0.0241(6) 0.0363(7) 0.0016(5) 0.0037(5) -0.0024(5) Zn3 0.0318(7) 0.0177(6) 0.0397(7) -0.0007(5) 0.0006(5) 0.0003(5) Zn4 0.0293(6) 0.0209(6) 0.0373(7) -0.0002(5) 0.0047(5) -0.0047(5) O1 0.033(4) 0.016(3) 0.038(4) 0.002(3) 0.004(3) 0.000(3) N1 0.026(4) 0.019(4) 0.039(5) -0.001(4) 0.002(4) 0.000(3) N2 0.020(4) 0.024(4) 0.035(5) -0.001(4) 0.003(4) -0.002(3) C1 0.030(5) 0.019(5) 0.037(6) -0.003(4) 0.006(5) 0.001(4) C2 0.028(5) 0.037(6) 0.036(6) -0.009(5) 0.005(5) 0.001(5) C3 0.034(6) 0.034(6) 0.041(7) -0.002(5) 0.000(5) 0.009(5) C4 0.029(6) 0.035(6) 0.046(7) -0.001(5) 0.007(5) 0.003(5) C5 0.031(6) 0.045(7) 0.056(8) -0.009(6) 0.008(6) 0.006(5) C6 0.029(6) 0.052(8) 0.064(9) -0.025(7) 0.006(6) -0.001(6) C7 0.048(7) 0.025(6) 0.056(8) 0.008(5) -0.002(6) 0.003(5) N3 0.036(5) 0.020(4) 0.041(5) 0.003(4) -0.003(4) -0.002(4) N4 0.031(5) 0.037(5) 0.036(5) 0.000(4) 0.005(4) 0.006(4) C8 0.028(5) 0.037(6) 0.033(6) -0.001(5) -0.006(5) -0.004(5) C9 0.040(7) 0.042(7) 0.072(10) 0.020(7) 0.000(7) 0.003(6) C10 0.033(7) 0.045(8) 0.111(14) 0.028(9) -0.009(8) 0.010(6) C11 0.051(8) 0.029(6) 0.053(8) 0.013(6) 0.005(6) 0.014(5) C12 0.056(8) 0.042(7) 0.049(8) 0.012(6) 0.015(6) -0.007(6) C13 0.052(7) 0.031(6) 0.037(7) 0.010(5) 0.002(6) 0.002(5) C14 0.025(5) 0.039(7) 0.049(7) -0.003(6) -0.007(5) -0.006(5) N5 0.037(5) 0.023(5) 0.047(6) -0.012(4) 0.008(4) -0.002(4) N6 0.036(5) 0.016(4) 0.038(5) 0.001(4) 0.011(4) 0.005(4) C15 0.048(7) 0.032(6) 0.034(6) 0.007(5) 0.016(5) 0.013(5) C16 0.063(9) 0.049(8) 0.047(8) 0.008(6) -0.014(7) -0.007(7) C17 0.063(9) 0.055(9) 0.043(8) 0.009(7) -0.003(7) -0.001(7) C18 0.114(15) 0.046(9) 0.071(11) -0.008(8) -0.053(11) -0.007(9) C19 0.28(4) 0.043(10) 0.092(16) 0.013(10) -0.09(2) -0.023(16) C20 0.18(2) 0.041(9) 0.073(12) -0.012(8) -0.074(14) 0.016(12) C21 0.040(6) 0.035(6) 0.048(7) 0.007(5) 0.012(5) 0.023(5) C22 0.030(6) 0.027(6) 0.043(7) -0.007(5) 0.006(5) 0.005(4) C23 0.034(6) 0.040(7) 0.042(7) 0.000(5) 0.006(5) -0.003(5) F23 0.063(5) 0.035(4) 0.058(5) 0.012(4) -0.003(4) -0.009(4) C24 0.048(7) 0.044(7) 0.037(7) 0.008(6) 0.003(6) 0.005(6) F24 0.065(5) 0.057(5) 0.060(5) 0.013(4) -0.013(4) 0.010(4) C25 0.044(7) 0.056(8) 0.041(7) -0.003(6) -0.006(6) 0.005(6) F25 0.043(4) 0.087(7) 0.055(5) 0.002(5) -0.011(4) -0.004(4) C26 0.032(6) 0.048(8) 0.053(8) -0.014(6) 0.004(6) -0.009(6) F26 0.064(6) 0.058(5) 0.090(7) -0.012(5) -0.011(5) -0.012(5) C27 0.034(6) 0.038(6) 0.039(6) 0.000(5) -0.003(5) -0.001(5) F27 0.068(5) 0.031(4) 0.073(6) -0.001(4) -0.015(4) -0.005(4) C28 0.039(6) 0.024(5) 0.040(6) 0.003(5) -0.003(5) 0.004(5) C29 0.038(6) 0.034(6) 0.045(7) -0.003(5) 0.002(5) 0.001(5) F29 0.039(4) 0.051(4) 0.058(5) -0.017(4) 0.004(3) -0.012(3) C30 0.025(5) 0.023(5) 0.056(7) 0.005(5) 0.000(5) -0.009(4) F30 0.069(6) 0.059(5) 0.061(5) 0.007(4) 0.014(4) -0.021(4) C31 0.035(6) 0.024(5) 0.049(7) 0.011(5) 0.020(5) 0.009(5) F31 0.053(4) 0.038(4) 0.072(5) 0.006(4) 0.033(4) 0.000(3) C32 0.042(7) 0.025(6) 0.046(7) -0.002(5) 0.010(5) 0.002(5) F32 0.079(6) 0.055(5) 0.049(5) -0.019(4) 0.025(4) -0.009(4) C33 0.044(7) 0.025(6) 0.041(7) 0.004(5) 0.000(5) -0.003(5) F33 0.044(4) 0.045(4) 0.056(5) -0.016(4) 0.009(3) -0.017(3) C34 0.026(5) 0.028(6) 0.041(6) 0.000(5) -0.001(5) -0.003(4) C35 0.044(7) 0.025(6) 0.055(8) 0.000(5) -0.007(6) -0.005(5) F35 0.033(4) 0.037(4) 0.096(6) -0.005(4) 0.006(4) 0.002(3) C36 0.039(7) 0.034(6) 0.055(8) -0.006(6) -0.008(6) 0.010(5) F36 0.033(4) 0.036(4) 0.122(8) -0.012(5) 0.001(4) 0.012(3) C37 0.061(8) 0.016(5) 0.048(7) 0.003(5) 0.000(6) -0.003(5) F37 0.070(5) 0.026(4) 0.084(6) 0.008(4) 0.006(5) 0.010(4) C38 0.045(7) 0.022(6) 0.052(8) 0.003(5) 0.001(6) -0.004(5) F38 0.065(5) 0.029(4) 0.065(5) 0.009(4) 0.010(4) -0.011(3) C39 0.049(7) 0.026(6) 0.043(7) -0.005(5) -0.001(6) -0.002(5) F39 0.031(4) 0.033(4) 0.066(5) -0.003(3) 0.012(3) 0.001(3) C40 0.039(6) 0.022(5) 0.036(6) 0.006(5) 0.002(5) 0.007(5) C41 0.035(6) 0.039(7) 0.056(8) -0.008(6) 0.004(6) -0.011(5) F41 0.083(6) 0.068(6) 0.069(6) -0.024(5) 0.041(5) -0.032(5) C42 0.052(8) 0.036(7) 0.080(11) -0.003(7) 0.028(8) -0.015(6) F42 0.084(7) 0.088(8) 0.117(9) -0.010(7) 0.052(7) -0.045(6) C43 0.036(7) 0.036(7) 0.093(12) -0.001(7) -0.003(7) -0.013(6) F43 0.064(6) 0.047(5) 0.115(8) 0.000(5) 0.003(5) -0.034(4) C44 0.049(8) 0.027(6) 0.058(8) -0.003(6) -0.005(6) -0.008(5) F44 0.075(6) 0.058(6) 0.094(7) -0.035(5) 0.000(5) -0.021(5) C45 0.032(6) 0.026(6) 0.057(8) -0.005(5) 0.003(5) 0.001(5) F45 0.058(5) 0.063(5) 0.061(5) -0.028(4) 0.019(4) -0.014(4) N7 0.151(16) 0.028(7) 0.129(14) -0.043(8) -0.097(13) 0.038(9) C46 0.048(9) 0.090(14) 0.066(10) -0.010(9) 0.002(8) -0.028(9) C47 0.044(9) 0.047(9) 0.16(2) -0.013(11) -0.003(11) 0.012(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 C22 1.989(12) . ? Zn1 N6 2.007(9) . ? Zn1 O1 2.061(7) . ? Zn1 N1 2.131(9) . ? Zn2 C28 1.983(12) . ? Zn2 N2 2.010(9) . ? Zn2 O1 2.059(8) . ? Zn2 N3 2.120(10) . ? Zn3 C34 2.000(11) . ? Zn3 N4 2.007(10) . ? Zn3 O1 2.062(7) . ? Zn3 N5 2.125(10) . ? Zn4 C40 2.011(12) . ? Zn4 N6 2.059(10) . ? Zn4 N2 2.067(9) . ? Zn4 N4 2.085(10) . ? N1 C1 1.462(14) . ? N1 N2 1.482(12) . ? N1 C7 1.490(14) . ? C1 C6 1.362(16) . ? C1 C2 1.379(15) . ? C2 C3 1.366(16) . ? C3 C4 1.403(17) . ? C4 C5 1.385(17) . ? C5 C6 1.394(17) . ? N3 N4 1.459(13) . ? N3 C14 1.491(14) . ? N3 C8 1.500(14) . ? C8 C13 1.353(17) . ? C8 C9 1.355(17) . ? C9 C10 1.409(19) . ? C10 C11 1.404(19) . ? C11 C12 1.377(18) . ? C12 C13 1.385(18) . ? N5 C15 1.466(16) . ? N5 C21 1.479(15) . ? N5 N6 1.484(12) . ? C15 C20 1.37(2) . ? C15 C16 1.404(17) . ? C16 C17 1.362(19) . ? C17 C18 1.37(2) . ? C18 C19 1.38(2) . ? C19 C20 1.35(2) . ? C22 C27 1.349(16) . ? C22 C23 1.402(17) . ? C23 F23 1.338(14) . ? C23 C24 1.360(18) . ? C24 F24 1.350(14) . ? C24 C25 1.355(19) . ? C25 F25 1.359(15) . ? C25 C26 1.389(19) . ? C26 F26 1.371(15) . ? C26 C27 1.383(17) . ? C27 F27 1.359(14) . ? C28 C29 1.368(17) . ? C28 C33 1.376(17) . ? C29 F29 1.363(14) . ? C29 C30 1.373(17) . ? C30 F30 1.375(13) . ? C30 C31 1.382(17) . ? C31 F31 1.355(13) . ? C31 C32 1.367(17) . ? C32 F32 1.348(14) . ? C32 C33 1.382(17) . ? C33 F33 1.367(13) . ? C34 C35 1.356(17) . ? C34 C39 1.384(16) . ? C35 F35 1.373(15) . ? C35 C36 1.374(17) . ? C36 F36 1.335(14) . ? C36 C37 1.385(18) . ? C37 F37 1.352(13) . ? C37 C38 1.354(18) . ? C38 F38 1.349(14) . ? C38 C39 1.395(16) . ? C39 F39 1.352(14) . ? C40 C41 1.336(17) . ? C40 C45 1.367(17) . ? C41 F41 1.361(15) . ? C41 C42 1.410(17) . ? C42 C43 1.33(2) . ? C42 F42 1.339(16) . ? C43 F43 1.355(14) . ? C43 C44 1.38(2) . ? C44 F44 1.342(15) . ? C44 C45 1.371(17) . ? C45 F45 1.376(15) . ? N7 C46 1.11(2) . ? C46 C47 1.53(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 C22 Zn1 N6 128.6(4) . . ? C22 Zn1 O1 116.6(4) . . ? N6 Zn1 O1 92.3(3) . . ? C22 Zn1 N1 118.8(4) . . ? N6 Zn1 N1 98.5(4) . . ? O1 Zn1 N1 94.4(3) . . ? C28 Zn2 N2 124.8(4) . . ? C28 Zn2 O1 120.1(4) . . ? N2 Zn2 O1 91.5(3) . . ? C28 Zn2 N3 119.6(4) . . ? N2 Zn2 N3 98.4(3) . . ? O1 Zn2 N3 95.6(3) . . ? C34 Zn3 N4 126.3(4) . . ? C34 Zn3 O1 116.3(4) . . ? N4 Zn3 O1 91.4(3) . . ? C34 Zn3 N5 121.3(4) . . ? N4 Zn3 N5 98.2(4) . . ? O1 Zn3 N5 95.9(3) . . ? C40 Zn4 N6 123.4(4) . . ? C40 Zn4 N2 114.3(4) . . ? N6 Zn4 N2 97.2(3) . . ? C40 Zn4 N4 122.5(4) . . ? N6 Zn4 N4 96.9(4) . . ? N2 Zn4 N4 97.0(4) . . ? Zn2 O1 Zn1 107.2(3) . . ? Zn2 O1 Zn3 106.5(3) . . ? Zn1 O1 Zn3 105.6(3) . . ? C1 N1 N2 110.4(8) . . ? C1 N1 C7 111.1(9) . . ? N2 N1 C7 109.1(8) . . ? C1 N1 Zn1 117.2(6) . . ? N2 N1 Zn1 100.2(6) . . ? C7 N1 Zn1 108.1(7) . . ? N1 N2 Zn2 108.5(6) . . ? N1 N2 Zn4 115.0(6) . . ? Zn2 N2 Zn4 102.9(4) . . ? C6 C1 C2 120.3(11) . . ? C6 C1 N1 119.9(10) . . ? C2 C1 N1 119.8(9) . . ? C3 C2 C1 119.8(11) . . ? C2 C3 C4 121.9(12) . . ? C5 C4 C3 116.8(11) . . ? C4 C5 C6 121.4(12) . . ? C1 C6 C5 119.8(12) . . ? N4 N3 C14 110.7(9) . . ? N4 N3 C8 109.6(9) . . ? C14 N3 C8 109.9(9) . . ? N4 N3 Zn2 100.5(6) . . ? C14 N3 Zn2 108.9(7) . . ? C8 N3 Zn2 116.9(7) . . ? N3 N4 Zn3 110.3(7) . . ? N3 N4 Zn4 113.5(6) . . ? Zn3 N4 Zn4 103.0(4) . . ? C13 C8 C9 123.0(12) . . ? C13 C8 N3 117.8(10) . . ? C9 C8 N3 119.1(11) . . ? C8 C9 C10 118.5(13) . . ? C11 C10 C9 119.8(12) . . ? C12 C11 C10 118.5(12) . . ? C11 C12 C13 121.4(13) . . ? C8 C13 C12 118.7(13) . . ? C15 N5 C21 109.6(9) . . ? C15 N5 N6 111.7(9) . . ? C21 N5 N6 110.6(9) . . ? C15 N5 Zn3 116.1(7) . . ? C21 N5 Zn3 108.1(7) . . ? N6 N5 Zn3 100.4(6) . . ? N5 N6 Zn1 108.1(6) . . ? N5 N6 Zn4 114.5(6) . . ? Zn1 N6 Zn4 103.4(4) . . ? C20 C15 C16 117.9(13) . . ? C20 C15 N5 119.8(11) . . ? C16 C15 N5 122.3(11) . . ? C17 C16 C15 121.2(14) . . ? C16 C17 C18 119.7(14) . . ? C17 C18 C19 119.0(15) . . ? C20 C19 C18 121.5(17) . . ? C19 C20 C15 120.7(16) . . ? C27 C22 C23 114.9(11) . . ? C27 C22 Zn1 123.9(9) . . ? C23 C22 Zn1 121.2(9) . . ? F23 C23 C24 117.5(11) . . ? F23 C23 C22 118.7(11) . . ? C24 C23 C22 123.8(12) . . ? F24 C24 C25 118.3(12) . . ? F24 C24 C23 123.4(12) . . ? C25 C24 C23 118.3(12) . . ? C24 C25 F25 120.0(13) . . ? C24 C25 C26 121.3(12) . . ? F25 C25 C26 118.7(13) . . ? F26 C26 C27 121.3(13) . . ? F26 C26 C25 121.4(12) . . ? C27 C26 C25 117.3(12) . . ? C22 C27 F27 118.9(10) . . ? C22 C27 C26 124.3(12) . . ? F27 C27 C26 116.8(11) . . ? C29 C28 C33 113.7(11) . . ? C29 C28 Zn2 123.0(9) . . ? C33 C28 Zn2 122.5(9) . . ? F29 C29 C28 119.4(11) . . ? F29 C29 C30 115.4(11) . . ? C28 C29 C30 125.1(12) . . ? C29 C30 F30 123.8(11) . . ? C29 C30 C31 117.9(10) . . ? F30 C30 C31 118.3(10) . . ? F31 C31 C32 119.9(11) . . ? F31 C31 C30 119.5(11) . . ? C32 C31 C30 120.6(10) . . ? F32 C32 C31 121.3(11) . . ? F32 C32 C33 121.0(11) . . ? C31 C32 C33 117.7(11) . . ? F33 C33 C28 117.9(11) . . ? F33 C33 C32 117.1(11) . . ? C28 C33 C32 125.0(11) . . ? C35 C34 C39 114.3(11) . . ? C35 C34 Zn3 122.0(9) . . ? C39 C34 Zn3 123.3(9) . . ? C34 C35 F35 118.4(10) . . ? C34 C35 C36 125.6(12) . . ? F35 C35 C36 116.0(12) . . ? F36 C36 C35 123.0(13) . . ? F36 C36 C37 119.5(11) . . ? C35 C36 C37 117.5(12) . . ? F37 C37 C38 119.4(12) . . ? F37 C37 C36 120.1(12) . . ? C38 C37 C36 120.5(11) . . ? F38 C38 C37 120.8(10) . . ? F38 C38 C39 120.3(12) . . ? C37 C38 C39 118.9(12) . . ? F39 C39 C34 119.0(10) . . ? F39 C39 C38 117.9(11) . . ? C34 C39 C38 123.1(12) . . ? C41 C40 C45 114.1(11) . . ? C41 C40 Zn4 123.6(9) . . ? C45 C40 Zn4 122.3(9) . . ? C40 C41 F41 120.7(11) . . ? C40 C41 C42 124.0(13) . . ? F41 C41 C42 115.2(12) . . ? C43 C42 F42 121.0(13) . . ? C43 C42 C41 119.5(13) . . ? F42 C42 C41 119.5(13) . . ? C42 C43 F43 122.1(14) . . ? C42 C43 C44 118.9(12) . . ? F43 C43 C44 118.9(14) . . ? F44 C44 C45 123.1(13) . . ? F44 C44 C43 118.2(12) . . ? C45 C44 C43 118.6(13) . . ? C40 C45 C44 124.9(12) . . ? C40 C45 F45 120.2(10) . . ? C44 C45 F45 114.9(11) . . ? N7 C46 C47 171(2) . . ? 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 C28 Zn2 O1 Zn1 -112.8(4) . . . . ? N2 Zn2 O1 Zn1 19.5(4) . . . . ? N3 Zn2 O1 Zn1 118.1(4) . . . . ? C28 Zn2 O1 Zn3 134.5(4) . . . . ? N2 Zn2 O1 Zn3 -93.1(3) . . . . ? N3 Zn2 O1 Zn3 5.4(4) . . . . ? C22 Zn1 O1 Zn2 132.8(4) . . . . ? N6 Zn1 O1 Zn2 -91.3(4) . . . . ? N1 Zn1 O1 Zn2 7.4(4) . . . . ? C22 Zn1 O1 Zn3 -114.0(4) . . . . ? N6 Zn1 O1 Zn3 21.9(4) . . . . ? N1 Zn1 O1 Zn3 120.7(4) . . . . ? C34 Zn3 O1 Zn2 -112.1(4) . . . . ? N4 Zn3 O1 Zn2 20.2(4) . . . . ? N5 Zn3 O1 Zn2 118.6(4) . . . . ? C34 Zn3 O1 Zn1 134.1(4) . . . . ? N4 Zn3 O1 Zn1 -93.6(4) . . . . ? N5 Zn3 O1 Zn1 4.9(4) . . . . ? C22 Zn1 N1 C1 -47.5(9) . . . . ? N6 Zn1 N1 C1 169.2(7) . . . . ? O1 Zn1 N1 C1 76.2(7) . . . . ? C22 Zn1 N1 N2 -166.9(6) . . . . ? N6 Zn1 N1 N2 49.8(6) . . . . ? O1 Zn1 N1 N2 -43.2(6) . . . . ? C22 Zn1 N1 C7 79.0(8) . . . . ? N6 Zn1 N1 C7 -64.3(8) . . . . ? O1 Zn1 N1 C7 -157.4(7) . . . . ? C1 N1 N2 Zn2 -58.4(8) . . . . ? C7 N1 N2 Zn2 179.2(7) . . . . ? Zn1 N1 N2 Zn2 65.9(6) . . . . ? C1 N1 N2 Zn4 -172.8(6) . . . . ? C7 N1 N2 Zn4 64.7(9) . . . . ? Zn1 N1 N2 Zn4 -48.6(6) . . . . ? C28 Zn2 N2 N1 72.0(8) . . . . ? O1 Zn2 N2 N1 -56.9(6) . . . . ? N3 Zn2 N2 N1 -152.8(6) . . . . ? C28 Zn2 N2 Zn4 -165.8(4) . . . . ? O1 Zn2 N2 Zn4 65.3(4) . . . . ? N3 Zn2 N2 Zn4 -30.6(4) . . . . ? C40 Zn4 N2 N1 -103.6(7) . . . . ? N6 Zn4 N2 N1 28.0(7) . . . . ? N4 Zn4 N2 N1 125.9(6) . . . . ? C40 Zn4 N2 Zn2 138.7(4) . . . . ? N6 Zn4 N2 Zn2 -89.7(4) . . . . ? N4 Zn4 N2 Zn2 8.2(4) . . . . ? N2 N1 C1 C6 -61.6(13) . . . . ? C7 N1 C1 C6 59.7(14) . . . . ? Zn1 N1 C1 C6 -175.4(10) . . . . ? N2 N1 C1 C2 116.5(11) . . . . ? C7 N1 C1 C2 -122.2(11) . . . . ? Zn1 N1 C1 C2 2.7(13) . . . . ? C6 C1 C2 C3 0.3(18) . . . . ? N1 C1 C2 C3 -177.8(10) . . . . ? C1 C2 C3 C4 0.3(18) . . . . ? C2 C3 C4 C5 -1.6(18) . . . . ? C3 C4 C5 C6 2.4(19) . . . . ? C2 C1 C6 C5 0(2) . . . . ? N1 C1 C6 C5 178.6(11) . . . . ? C4 C5 C6 C1 -2(2) . . . . ? C28 Zn2 N3 N4 -169.9(6) . . . . ? N2 Zn2 N3 N4 51.9(6) . . . . ? O1 Zn2 N3 N4 -40.5(6) . . . . ? C28 Zn2 N3 C14 73.7(8) . . . . ? N2 Zn2 N3 C14 -64.5(8) . . . . ? O1 Zn2 N3 C14 -156.8(7) . . . . ? C28 Zn2 N3 C8 -51.5(9) . . . . ? N2 Zn2 N3 C8 170.3(8) . . . . ? O1 Zn2 N3 C8 78.0(8) . . . . ? C14 N3 N4 Zn3 178.9(7) . . . . ? C8 N3 N4 Zn3 -59.8(9) . . . . ? Zn2 N3 N4 Zn3 63.9(6) . . . . ? C14 N3 N4 Zn4 63.9(10) . . . . ? C8 N3 N4 Zn4 -174.7(6) . . . . ? Zn2 N3 N4 Zn4 -51.1(7) . . . . ? C34 Zn3 N4 N3 68.0(8) . . . . ? O1 Zn3 N4 N3 -56.6(7) . . . . ? N5 Zn3 N4 N3 -152.7(7) . . . . ? C34 Zn3 N4 Zn4 -170.6(4) . . . . ? O1 Zn3 N4 Zn4 64.8(4) . . . . ? N5 Zn3 N4 Zn4 -31.3(4) . . . . ? C40 Zn4 N4 N3 -94.4(8) . . . . ? N6 Zn4 N4 N3 128.5(7) . . . . ? N2 Zn4 N4 N3 30.4(7) . . . . ? C40 Zn4 N4 Zn3 146.4(5) . . . . ? N6 Zn4 N4 Zn3 9.3(4) . . . . ? N2 Zn4 N4 Zn3 -88.8(4) . . . . ? N4 N3 C8 C13 112.2(12) . . . . ? C14 N3 C8 C13 -126.0(11) . . . . ? Zn2 N3 C8 C13 -1.3(14) . . . . ? N4 N3 C8 C9 -65.4(14) . . . . ? C14 N3 C8 C9 56.4(15) . . . . ? Zn2 N3 C8 C9 -178.9(10) . . . . ? C13 C8 C9 C10 0(2) . . . . ? N3 C8 C9 C10 177.4(13) . . . . ? C8 C9 C10 C11 -3(3) . . . . ? C9 C10 C11 C12 2(2) . . . . ? C10 C11 C12 C13 1(2) . . . . ? C9 C8 C13 C12 3(2) . . . . ? N3 C8 C13 C12 -174.2(11) . . . . ? C11 C12 C13 C8 -4(2) . . . . ? C34 Zn3 N5 C15 -46.4(9) . . . . ? N4 Zn3 N5 C15 171.6(7) . . . . ? O1 Zn3 N5 C15 79.3(8) . . . . ? C34 Zn3 N5 C21 77.2(8) . . . . ? N4 Zn3 N5 C21 -64.9(8) . . . . ? O1 Zn3 N5 C21 -157.2(7) . . . . ? C34 Zn3 N5 N6 -166.9(6) . . . . ? N4 Zn3 N5 N6 51.1(6) . . . . ? O1 Zn3 N5 N6 -41.3(6) . . . . ? C15 N5 N6 Zn1 -59.0(10) . . . . ? C21 N5 N6 Zn1 178.6(7) . . . . ? Zn3 N5 N6 Zn1 64.6(6) . . . . ? C15 N5 N6 Zn4 -173.6(7) . . . . ? C21 N5 N6 Zn4 64.0(10) . . . . ? Zn3 N5 N6 Zn4 -50.0(7) . . . . ? C22 Zn1 N6 N5 69.2(8) . . . . ? O1 Zn1 N6 N5 -58.0(7) . . . . ? N1 Zn1 N6 N5 -152.8(7) . . . . ? C22 Zn1 N6 Zn4 -169.0(4) . . . . ? O1 Zn1 N6 Zn4 63.8(4) . . . . ? N1 Zn1 N6 Zn4 -31.0(4) . . . . ? C40 Zn4 N6 N5 -107.8(7) . . . . ? N2 Zn4 N6 N5 126.8(7) . . . . ? N4 Zn4 N6 N5 28.8(7) . . . . ? C40 Zn4 N6 Zn1 134.9(4) . . . . ? N2 Zn4 N6 Zn1 9.4(4) . . . . ? N4 Zn4 N6 Zn1 -88.5(4) . . . . ? C21 N5 C15 C20 -93.9(18) . . . . ? N6 N5 C15 C20 143.2(16) . . . . ? Zn3 N5 C15 C20 28.9(19) . . . . ? C21 N5 C15 C16 86.1(14) . . . . ? N6 N5 C15 C16 -36.9(15) . . . . ? Zn3 N5 C15 C16 -151.2(11) . . . . ? C20 C15 C16 C17 -1(2) . . . . ? N5 C15 C16 C17 179.1(13) . . . . ? C15 C16 C17 C18 2(3) . . . . ? C16 C17 C18 C19 -1(3) . . . . ? C17 C18 C19 C20 -2(5) . . . . ? C18 C19 C20 C15 3(5) . . . . ? C16 C15 C20 C19 -1(4) . . . . ? N5 C15 C20 C19 178(2) . . . . ? N6 Zn1 C22 C27 -103.4(11) . . . . ? O1 Zn1 C22 C27 13.8(12) . . . . ? N1 Zn1 C22 C27 125.7(10) . . . . ? N6 Zn1 C22 C23 72.6(11) . . . . ? O1 Zn1 C22 C23 -170.2(9) . . . . ? N1 Zn1 C22 C23 -58.3(11) . . . . ? C27 C22 C23 F23 -179.7(11) . . . . ? Zn1 C22 C23 F23 3.9(16) . . . . ? C27 C22 C23 C24 -1.9(18) . . . . ? Zn1 C22 C23 C24 -178.3(10) . . . . ? F23 C23 C24 F24 0.1(19) . . . . ? C22 C23 C24 F24 -177.7(12) . . . . ? F23 C23 C24 C25 178.5(12) . . . . ? C22 C23 C24 C25 1(2) . . . . ? F24 C24 C25 F25 0(2) . . . . ? C23 C24 C25 F25 -178.4(12) . . . . ? F24 C24 C25 C26 179.4(12) . . . . ? C23 C24 C25 C26 1(2) . . . . ? C24 C25 C26 F26 -180.0(13) . . . . ? F25 C25 C26 F26 -1(2) . . . . ? C24 C25 C26 C27 -1(2) . . . . ? F25 C25 C26 C27 178.2(12) . . . . ? C23 C22 C27 F27 -178.5(11) . . . . ? Zn1 C22 C27 F27 -2.3(17) . . . . ? C23 C22 C27 C26 1.6(19) . . . . ? Zn1 C22 C27 C26 177.9(10) . . . . ? F26 C26 C27 C22 178.6(12) . . . . ? C25 C26 C27 C22 0(2) . . . . ? F26 C26 C27 F27 -1.2(19) . . . . ? C25 C26 C27 F27 180.0(12) . . . . ? N2 Zn2 C28 C29 -121.5(10) . . . . ? O1 Zn2 C28 C29 -5.5(11) . . . . ? N3 Zn2 C28 C29 111.8(10) . . . . ? N2 Zn2 C28 C33 47.9(11) . . . . ? O1 Zn2 C28 C33 163.9(8) . . . . ? N3 Zn2 C28 C33 -78.8(10) . . . . ? C33 C28 C29 F29 177.8(10) . . . . ? Zn2 C28 C29 F29 -11.9(16) . . . . ? C33 C28 C29 C30 1.8(18) . . . . ? Zn2 C28 C29 C30 172.0(10) . . . . ? F29 C29 C30 F30 3.7(17) . . . . ? C28 C29 C30 F30 179.9(11) . . . . ? F29 C29 C30 C31 -178.2(10) . . . . ? C28 C29 C30 C31 -2.0(19) . . . . ? C29 C30 C31 F31 -179.4(10) . . . . ? F30 C30 C31 F31 -1.2(16) . . . . ? C29 C30 C31 C32 0.5(17) . . . . ? F30 C30 C31 C32 178.7(11) . . . . ? F31 C31 C32 F32 0.6(17) . . . . ? C30 C31 C32 F32 -179.2(11) . . . . ? F31 C31 C32 C33 -179.0(10) . . . . ? C30 C31 C32 C33 1.1(17) . . . . ? C29 C28 C33 F33 177.2(10) . . . . ? Zn2 C28 C33 F33 6.9(15) . . . . ? C29 C28 C33 C32 0.0(17) . . . . ? Zn2 C28 C33 C32 -170.3(10) . . . . ? F32 C32 C33 F33 1.7(17) . . . . ? C31 C32 C33 F33 -178.6(10) . . . . ? F32 C32 C33 C28 179.0(11) . . . . ? C31 C32 C33 C28 -1.4(19) . . . . ? N4 Zn3 C34 C35 61.8(12) . . . . ? O1 Zn3 C34 C35 175.3(10) . . . . ? N5 Zn3 C34 C35 -69.0(11) . . . . ? N4 Zn3 C34 C39 -110.9(10) . . . . ? O1 Zn3 C34 C39 2.5(12) . . . . ? N5 Zn3 C34 C39 118.2(10) . . . . ? C39 C34 C35 F35 -178.7(11) . . . . ? Zn3 C34 C35 F35 7.9(17) . . . . ? C39 C34 C35 C36 4(2) . . . . ? Zn3 C34 C35 C36 -169.6(11) . . . . ? C34 C35 C36 F36 178.4(12) . . . . ? F35 C35 C36 F36 1(2) . . . . ? C34 C35 C36 C37 -4(2) . . . . ? F35 C35 C36 C37 178.7(11) . . . . ? F36 C36 C37 F37 -1(2) . . . . ? C35 C36 C37 F37 -178.9(12) . . . . ? F36 C36 C37 C38 179.2(12) . . . . ? C35 C36 C37 C38 1(2) . . . . ? F37 C37 C38 F38 1(2) . . . . ? C36 C37 C38 F38 -179.1(12) . . . . ? F37 C37 C38 C39 -179.1(12) . . . . ? C36 C37 C38 C39 1(2) . . . . ? C35 C34 C39 F39 179.9(11) . . . . ? Zn3 C34 C39 F39 -6.8(16) . . . . ? C35 C34 C39 C38 -1.5(19) . . . . ? Zn3 C34 C39 C38 171.8(10) . . . . ? F38 C38 C39 F39 -2.1(18) . . . . ? C37 C38 C39 F39 178.0(11) . . . . ? F38 C38 C39 C34 179.3(11) . . . . ? C37 C38 C39 C34 -1(2) . . . . ? N6 Zn4 C40 C41 42.4(12) . . . . ? N2 Zn4 C40 C41 159.9(10) . . . . ? N4 Zn4 C40 C41 -83.7(11) . . . . ? N6 Zn4 C40 C45 -139.6(9) . . . . ? N2 Zn4 C40 C45 -22.1(11) . . . . ? N4 Zn4 C40 C45 94.4(10) . . . . ? C45 C40 C41 F41 179.8(12) . . . . ? Zn4 C40 C41 F41 -2.0(18) . . . . ? C45 C40 C41 C42 0(2) . . . . ? Zn4 C40 C41 C42 178.5(11) . . . . ? C40 C41 C42 C43 -1(2) . . . . ? F41 C41 C42 C43 179.3(14) . . . . ? C40 C41 C42 F42 -177.9(14) . . . . ? F41 C41 C42 F42 3(2) . . . . ? F42 C42 C43 F43 -5(2) . . . . ? C41 C42 C43 F43 178.3(13) . . . . ? F42 C42 C43 C44 178.6(14) . . . . ? C41 C42 C43 C44 2(2) . . . . ? C42 C43 C44 F44 -179.2(14) . . . . ? F43 C43 C44 F44 4(2) . . . . ? C42 C43 C44 C45 -2(2) . . . . ? F43 C43 C44 C45 -178.4(12) . . . . ? C41 C40 C45 C44 -0.2(18) . . . . ? Zn4 C40 C45 C44 -178.5(10) . . . . ? C41 C40 C45 F45 178.5(11) . . . . ? Zn4 C40 C45 F45 0.3(16) . . . . ? F44 C44 C45 C40 178.3(12) . . . . ? C43 C44 C45 C40 1(2) . . . . ? F44 C44 C45 F45 -0.5(19) . . . . ? C43 C44 C45 F45 -177.8(12) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 F39 1.00 2.42 3.094(10) 123.8 . O1 H1 F27 1.00 2.50 3.113(11) 119.1 . O1 H1 F29 1.00 2.59 3.228(11) 122.0 . N2 H2 F45 0.93 2.43 3.103(11) 128.9 . N4 H4 N7 0.93 2.25 3.16(2) 166.5 . N6 H6 F24 0.93 2.40 3.318(12) 170.9 3_767 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 2.850 _refine_diff_density_min -1.103 _refine_diff_density_rms 0.188 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 790911' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C45 H28 F20 N6 O Zn4, 3(C2 H3 N)' _chemical_formula_sum 'C51 H37 F20 N9 O Zn4' _chemical_formula_weight 1433.38 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' F F 0.0171 0.0103 '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' O O 0.0106 0.0060 '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 _symmetry_space_group_name_Hall '-P 2yn' 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 10.5846(4) _cell_length_b 13.3665(5) _cell_length_c 39.0083(16) _cell_angle_alpha 90.00 _cell_angle_beta 93.707(2) _cell_angle_gamma 90.00 _cell_volume 5507.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8273 _cell_measurement_theta_min 2.40 _cell_measurement_theta_max 28.23 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.729 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 1.837 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.405 _exptl_absorpt_correction_T_max 0.947 _exptl_absorpt_process_details 'SADABS v2004/1, Sheldrick, G.M., (2004)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 55922 _diffrn_reflns_av_R_equivalents 0.0425 _diffrn_reflns_av_sigmaI/netI 0.0378 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -51 _diffrn_reflns_limit_l_max 52 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 28.33 _reflns_number_total 13709 _reflns_number_gt 11100 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0283P)^2^+5.5781P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except NH & OH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13709 _refine_ls_number_parameters 784 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.43979(3) 0.441744(19) 0.379407(7) 0.01980(6) Uani 1 1 d . . . Zn2 Zn 0.65338(2) 0.26773(2) 0.396054(7) 0.01952(6) Uani 1 1 d . . . Zn3 Zn 0.56658(2) 0.32199(2) 0.315234(7) 0.01984(6) Uani 1 1 d . . . Zn4 Zn 0.37781(2) 0.211021(19) 0.363192(7) 0.01855(6) Uani 1 1 d . . . O1 O 0.60696(15) 0.38463(12) 0.36267(4) 0.0199(3) Uani 1 1 d . . . H1 H 0.658(3) 0.421(2) 0.3629(7) 0.024 Uiso 1 1 d . . . N1 N 0.43223(18) 0.34773(14) 0.42291(5) 0.0199(4) Uani 1 1 d . . . N2 N 0.47308(19) 0.25104(14) 0.40837(5) 0.0195(4) Uani 1 1 d . . . H2 H 0.469(3) 0.210(2) 0.4229(7) 0.023 Uiso 1 1 d . . . C1 C 0.5148(2) 0.37185(18) 0.45384(6) 0.0221(5) Uani 1 1 d . . . C2 C 0.5790(2) 0.4612(2) 0.45558(7) 0.0284(5) Uani 1 1 d . . . H2A H 0.5667 0.5086 0.4375 0.034 Uiso 1 1 calc R . . C3 C 0.6621(3) 0.4823(2) 0.48370(7) 0.0357(6) Uani 1 1 d . . . H3 H 0.7065 0.5440 0.4848 0.043 Uiso 1 1 calc R . . C4 C 0.6800(3) 0.4142(2) 0.50986(7) 0.0403(7) Uani 1 1 d . . . H4A H 0.7386 0.4277 0.5288 0.048 Uiso 1 1 calc R . . C5 C 0.6120(3) 0.3254(2) 0.50854(7) 0.0473(8) Uani 1 1 d . . . H5 H 0.6225 0.2789 0.5269 0.057 Uiso 1 1 calc R . . C6 C 0.5292(3) 0.3041(2) 0.48066(7) 0.0378(7) Uani 1 1 d . . . H6A H 0.4824 0.2434 0.4799 0.045 Uiso 1 1 calc R . . C7 C 0.2984(2) 0.34059(19) 0.43192(6) 0.0256(5) Uani 1 1 d . . . H7A H 0.2894 0.2848 0.4479 0.038 Uiso 1 1 calc R . . H7B H 0.2439 0.3292 0.4110 0.038 Uiso 1 1 calc R . . H7C H 0.2737 0.4031 0.4428 0.038 Uiso 1 1 calc R . . N3 N 0.65086(18) 0.15753(14) 0.35690(5) 0.0189(4) Uani 1 1 d . . . N4 N 0.53627(18) 0.18707(15) 0.33557(5) 0.0193(4) Uani 1 1 d . . . H4 H 0.523(2) 0.140(2) 0.3205(7) 0.023 Uiso 1 1 d . . . C8 C 0.7608(2) 0.15346(17) 0.33543(6) 0.0200(5) Uani 1 1 d . . . C9 C 0.7595(2) 0.0894(2) 0.30749(7) 0.0332(6) Uani 1 1 d . . . H9 H 0.6890 0.0466 0.3026 0.040 Uiso 1 1 calc R . . C10 C 0.8609(3) 0.0877(2) 0.28676(8) 0.0377(7) Uani 1 1 d . . . H10 H 0.8596 0.0438 0.2676 0.045 Uiso 1 1 calc R . . C11 C 0.9632(2) 0.1493(2) 0.29375(7) 0.0294(6) Uani 1 1 d . . . H11 H 1.0327 0.1481 0.2795 0.035 Uiso 1 1 calc R . . C12 C 0.9644(2) 0.2129(2) 0.32158(7) 0.0287(5) Uani 1 1 d . . . H12 H 1.0353 0.2553 0.3265 0.034 Uiso 1 1 calc R . . C13 C 0.8631(2) 0.21551(19) 0.34242(6) 0.0246(5) Uani 1 1 d . . . H13 H 0.8643 0.2600 0.3614 0.030 Uiso 1 1 calc R . . C14 C 0.6301(2) 0.05821(17) 0.37293(7) 0.0260(5) Uani 1 1 d . . . H14A H 0.6068 0.0091 0.3550 0.039 Uiso 1 1 calc R . . H14B H 0.5618 0.0635 0.3886 0.039 Uiso 1 1 calc R . . H14C H 0.7081 0.0367 0.3857 0.039 Uiso 1 1 calc R . . N5 N 0.37723(18) 0.37366(15) 0.31057(5) 0.0203(4) Uani 1 1 d . . . N6 N 0.33646(19) 0.35494(15) 0.34571(5) 0.0193(4) Uani 1 1 d . . . H6 H 0.257(3) 0.367(2) 0.3450(7) 0.023 Uiso 1 1 d . . . C15 C 0.3590(2) 0.47997(18) 0.30188(6) 0.0216(5) Uani 1 1 d . . . C16 C 0.2391(3) 0.5213(2) 0.29726(8) 0.0380(7) Uani 1 1 d . . . H16 H 0.1665 0.4798 0.2982 0.046 Uiso 1 1 calc R . . C17 C 0.2247(3) 0.6228(2) 0.29125(9) 0.0471(8) Uani 1 1 d . . . H17 H 0.1422 0.6505 0.2879 0.057 Uiso 1 1 calc R . . C18 C 0.3290(3) 0.6842(2) 0.29012(7) 0.0364(6) Uani 1 1 d . . . H18 H 0.3189 0.7540 0.2865 0.044 Uiso 1 1 calc R . . C19 C 0.4483(3) 0.6427(2) 0.29437(7) 0.0307(6) Uani 1 1 d . . . H19 H 0.5208 0.6842 0.2934 0.037 Uiso 1 1 calc R . . C20 C 0.4633(2) 0.54113(19) 0.30002(6) 0.0262(5) Uani 1 1 d . . . H20 H 0.5459 0.5133 0.3026 0.031 Uiso 1 1 calc R . . C21 C 0.3059(2) 0.3085(2) 0.28542(6) 0.0281(5) Uani 1 1 d . . . H21A H 0.2149 0.3204 0.2866 0.042 Uiso 1 1 calc R . . H21B H 0.3249 0.2383 0.2908 0.042 Uiso 1 1 calc R . . H21C H 0.3307 0.3239 0.2622 0.042 Uiso 1 1 calc R . . C22 C 0.4325(2) 0.58993(18) 0.38522(6) 0.0240(5) Uani 1 1 d . . . C23 C 0.3252(2) 0.63760(19) 0.39489(6) 0.0271(5) Uani 1 1 d . . . F23 F 0.22457(14) 0.58188(12) 0.40369(4) 0.0358(4) Uani 1 1 d . . . C24 C 0.3120(3) 0.7400(2) 0.39683(7) 0.0342(6) Uani 1 1 d . . . F24 F 0.20405(18) 0.78189(14) 0.40666(6) 0.0545(5) Uani 1 1 d . . . C25 C 0.4110(3) 0.79989(19) 0.38877(7) 0.0359(6) Uani 1 1 d . . . F25 F 0.4013(2) 0.89975(12) 0.39039(5) 0.0553(5) Uani 1 1 d . . . C26 C 0.5217(3) 0.75684(19) 0.37922(7) 0.0329(6) Uani 1 1 d . . . F26 F 0.62019(18) 0.81488(12) 0.37176(5) 0.0455(4) Uani 1 1 d . . . C27 C 0.5293(3) 0.65356(19) 0.37776(7) 0.0283(5) Uani 1 1 d . . . F27 F 0.64098(15) 0.61512(12) 0.36811(5) 0.0399(4) Uani 1 1 d . . . C28 C 0.8079(2) 0.2910(2) 0.42672(6) 0.0248(5) Uani 1 1 d . . . C29 C 0.8665(2) 0.3827(2) 0.43090(6) 0.0295(6) Uani 1 1 d . . . F29 F 0.82245(15) 0.46195(12) 0.41166(4) 0.0376(4) Uani 1 1 d . . . C30 C 0.9683(3) 0.4009(2) 0.45385(7) 0.0377(7) Uani 1 1 d . . . F30 F 1.02155(18) 0.49210(16) 0.45688(5) 0.0560(5) Uani 1 1 d . . . C31 C 1.0150(3) 0.3240(3) 0.47386(7) 0.0406(7) Uani 1 1 d . . . F31 F 1.11381(17) 0.33910(18) 0.49689(5) 0.0604(6) Uani 1 1 d . . . C32 C 0.9615(3) 0.2305(3) 0.47100(7) 0.0397(7) Uani 1 1 d . . . F32 F 1.00802(19) 0.15407(18) 0.49066(5) 0.0633(6) Uani 1 1 d . . . C33 C 0.8598(3) 0.2163(2) 0.44739(7) 0.0313(6) Uani 1 1 d . . . F33 F 0.80839(17) 0.12323(13) 0.44537(4) 0.0426(4) Uani 1 1 d . . . C34 C 0.6792(2) 0.34782(17) 0.27731(6) 0.0216(5) Uani 1 1 d . . . C35 C 0.6707(2) 0.29286(18) 0.24737(6) 0.0251(5) Uani 1 1 d . . . F35 F 0.57518(15) 0.22567(12) 0.24194(4) 0.0394(4) Uani 1 1 d . . . C36 C 0.7551(3) 0.3009(2) 0.22195(7) 0.0296(6) Uani 1 1 d . . . F36 F 0.74239(17) 0.24539(14) 0.19326(4) 0.0463(4) Uani 1 1 d . . . C37 C 0.8548(2) 0.3660(2) 0.22665(7) 0.0289(6) Uani 1 1 d . . . F37 F 0.93886(15) 0.37617(13) 0.20237(4) 0.0407(4) Uani 1 1 d . . . C38 C 0.8677(2) 0.42309(19) 0.25610(7) 0.0271(5) Uani 1 1 d . . . F38 F 0.96396(15) 0.48846(13) 0.26003(5) 0.0432(4) Uani 1 1 d . . . C39 C 0.7801(2) 0.41274(19) 0.28021(6) 0.0247(5) Uani 1 1 d . . . F39 F 0.79523(15) 0.47152(13) 0.30878(4) 0.0383(4) Uani 1 1 d . . . C40 C 0.2477(2) 0.10109(17) 0.35838(6) 0.0224(5) Uani 1 1 d . . . C41 C 0.2405(2) 0.03553(19) 0.33089(7) 0.0272(5) Uani 1 1 d . . . F41 F 0.32233(16) 0.04560(13) 0.30555(4) 0.0421(4) Uani 1 1 d . . . C42 C 0.1534(3) -0.0405(2) 0.32676(8) 0.0354(6) Uani 1 1 d . . . F42 F 0.14955(19) -0.10109(14) 0.29884(5) 0.0570(5) Uani 1 1 d . . . C43 C 0.0671(3) -0.0543(2) 0.35106(9) 0.0421(7) Uani 1 1 d . . . F43 F -0.01949(19) -0.12799(15) 0.34749(6) 0.0652(6) Uani 1 1 d . . . C44 C 0.0693(3) 0.0083(2) 0.37888(9) 0.0422(7) Uani 1 1 d . . . F44 F -0.0157(2) -0.00470(18) 0.40282(6) 0.0735(7) Uani 1 1 d . . . C45 C 0.1593(3) 0.0832(2) 0.38184(7) 0.0310(6) Uani 1 1 d . . . F45 F 0.15524(18) 0.14235(14) 0.41006(5) 0.0508(5) Uani 1 1 d . . . N7 N 0.6448(7) 0.8194(5) 0.46130(14) 0.131(2) Uani 1 1 d . . . C46 C 0.7330(6) 0.8043(5) 0.44789(12) 0.0942(18) Uani 1 1 d . . . C47 C 0.8484(6) 0.7858(7) 0.43120(14) 0.160(4) Uani 1 1 d . . . H47A H 0.9160 0.8286 0.4414 0.240 Uiso 1 1 calc R . . H47B H 0.8351 0.8007 0.4066 0.240 Uiso 1 1 calc R . . H47C H 0.8726 0.7154 0.4342 0.240 Uiso 1 1 calc R . . N8 N 0.4482(4) 0.0600(2) 0.45295(8) 0.0718(10) Uani 1 1 d . . . C48 C 0.3742(4) 0.0168(3) 0.46572(9) 0.0607(10) Uani 1 1 d . . . C49 C 0.2781(6) -0.0387(4) 0.48228(15) 0.1054(19) Uani 1 1 d . . . H49A H 0.2107 0.0070 0.4884 0.158 Uiso 1 1 calc R . . H49B H 0.3159 -0.0705 0.5031 0.158 Uiso 1 1 calc R . . H49C H 0.2426 -0.0902 0.4666 0.158 Uiso 1 1 calc R . . N9 N 0.0533(2) 0.4259(2) 0.36141(8) 0.0463(7) Uani 1 1 d . . . C50 C 0.0149(3) 0.5049(2) 0.36002(8) 0.0396(7) Uani 1 1 d . . . C51 C -0.0330(3) 0.6069(3) 0.35831(11) 0.0597(10) Uani 1 1 d . . . H51A H 0.0117 0.6474 0.3762 0.090 Uiso 1 1 calc R . . H51B H -0.1238 0.6068 0.3619 0.090 Uiso 1 1 calc R . . H51C H -0.0192 0.6354 0.3357 0.090 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 0.02216(13) 0.01550(13) 0.02188(13) -0.00148(10) 0.00237(10) -0.00078(10) Zn2 0.01912(13) 0.01890(13) 0.02049(13) -0.00207(10) 0.00095(10) -0.00049(10) Zn3 0.01949(13) 0.02040(14) 0.01999(13) 0.00097(10) 0.00410(10) -0.00090(10) Zn4 0.01837(13) 0.01733(13) 0.02020(13) -0.00185(10) 0.00318(10) -0.00311(10) O1 0.0189(8) 0.0165(8) 0.0245(8) -0.0003(6) 0.0016(7) -0.0042(6) N1 0.0205(10) 0.0177(9) 0.0219(10) -0.0030(7) 0.0037(8) 0.0011(7) N2 0.0258(10) 0.0139(9) 0.0191(9) 0.0001(7) 0.0033(8) -0.0008(8) C1 0.0255(12) 0.0233(12) 0.0177(11) -0.0052(9) 0.0041(9) 0.0018(9) C2 0.0295(13) 0.0290(13) 0.0269(13) -0.0054(10) 0.0029(10) -0.0043(11) C3 0.0325(14) 0.0416(16) 0.0328(15) -0.0132(12) 0.0006(11) -0.0066(12) C4 0.0411(17) 0.0487(18) 0.0296(14) -0.0172(13) -0.0098(12) 0.0085(14) C5 0.075(2) 0.0395(17) 0.0256(14) -0.0040(12) -0.0117(14) 0.0086(16) C6 0.0584(19) 0.0294(14) 0.0247(13) -0.0036(11) -0.0045(13) -0.0037(13) C7 0.0260(12) 0.0249(12) 0.0270(12) -0.0028(10) 0.0093(10) -0.0006(10) N3 0.0186(9) 0.0167(9) 0.0218(9) -0.0005(7) 0.0040(7) 0.0007(7) N4 0.0175(9) 0.0200(10) 0.0205(9) -0.0037(8) 0.0008(7) 0.0001(7) C8 0.0212(11) 0.0169(11) 0.0223(11) -0.0003(9) 0.0055(9) 0.0031(9) C9 0.0252(13) 0.0348(15) 0.0402(15) -0.0174(12) 0.0065(11) -0.0060(11) C10 0.0331(15) 0.0436(17) 0.0374(15) -0.0205(13) 0.0089(12) -0.0006(12) C11 0.0216(12) 0.0388(15) 0.0286(13) -0.0018(11) 0.0072(10) 0.0029(11) C12 0.0218(12) 0.0327(14) 0.0322(13) -0.0019(11) 0.0048(10) -0.0049(10) C13 0.0245(12) 0.0256(12) 0.0240(12) -0.0013(10) 0.0032(9) -0.0027(10) C14 0.0308(13) 0.0170(11) 0.0306(13) 0.0026(10) 0.0048(10) -0.0001(10) N5 0.0206(10) 0.0221(10) 0.0182(9) 0.0003(7) 0.0018(7) -0.0015(8) N6 0.0171(9) 0.0207(10) 0.0202(9) 0.0002(7) 0.0026(8) -0.0013(8) C15 0.0223(11) 0.0261(12) 0.0163(10) 0.0036(9) 0.0011(9) 0.0026(9) C16 0.0235(13) 0.0376(16) 0.0521(18) 0.0163(13) -0.0033(12) 0.0012(11) C17 0.0320(15) 0.0463(18) 0.063(2) 0.0246(16) 0.0032(14) 0.0144(14) C18 0.0473(17) 0.0260(14) 0.0361(15) 0.0121(11) 0.0056(13) 0.0108(12) C19 0.0356(14) 0.0259(13) 0.0309(14) 0.0054(10) 0.0037(11) -0.0027(11) C20 0.0240(12) 0.0265(13) 0.0282(13) 0.0028(10) 0.0024(10) 0.0012(10) C21 0.0280(13) 0.0342(14) 0.0219(12) -0.0038(10) -0.0009(10) -0.0054(11) C22 0.0293(13) 0.0199(11) 0.0223(12) -0.0013(9) -0.0029(10) -0.0003(10) C23 0.0297(13) 0.0239(12) 0.0267(12) -0.0031(10) -0.0042(10) -0.0011(10) F23 0.0266(8) 0.0338(9) 0.0468(10) -0.0041(7) 0.0013(7) -0.0007(7) C24 0.0359(15) 0.0263(13) 0.0396(15) -0.0064(11) -0.0040(12) 0.0105(11) F24 0.0482(11) 0.0368(10) 0.0785(14) -0.0108(9) 0.0057(10) 0.0174(8) C25 0.0528(18) 0.0164(12) 0.0370(15) -0.0015(11) -0.0076(13) 0.0032(12) F25 0.0731(14) 0.0179(8) 0.0737(14) -0.0017(8) -0.0032(11) 0.0033(8) C26 0.0448(16) 0.0218(13) 0.0312(14) 0.0041(10) -0.0041(12) -0.0087(11) F26 0.0570(11) 0.0272(9) 0.0523(11) 0.0057(8) 0.0035(9) -0.0171(8) C27 0.0334(14) 0.0218(12) 0.0296(13) 0.0000(10) 0.0011(11) 0.0008(10) F27 0.0338(9) 0.0279(8) 0.0594(11) 0.0009(8) 0.0138(8) -0.0034(7) C28 0.0198(11) 0.0336(13) 0.0211(11) -0.0043(10) 0.0016(9) -0.0014(10) C29 0.0263(13) 0.0372(15) 0.0255(13) -0.0053(11) 0.0046(10) -0.0019(11) F29 0.0368(9) 0.0309(9) 0.0451(9) -0.0017(7) 0.0025(7) -0.0064(7) C30 0.0243(13) 0.0517(18) 0.0376(16) -0.0121(13) 0.0051(12) -0.0116(13) F30 0.0446(11) 0.0632(13) 0.0596(12) -0.0170(10) -0.0017(9) -0.0282(10) C31 0.0220(13) 0.070(2) 0.0289(14) -0.0102(14) -0.0028(11) -0.0074(14) F31 0.0338(10) 0.1051(18) 0.0402(10) -0.0063(11) -0.0127(8) -0.0171(10) C32 0.0304(15) 0.060(2) 0.0283(14) 0.0054(13) -0.0023(11) 0.0021(14) F32 0.0502(12) 0.0836(16) 0.0530(12) 0.0227(11) -0.0200(9) 0.0045(11) C33 0.0294(13) 0.0384(15) 0.0261(13) 0.0008(11) 0.0004(10) -0.0028(11) F33 0.0471(10) 0.0373(9) 0.0422(10) 0.0075(8) -0.0075(8) -0.0027(8) C34 0.0220(11) 0.0205(11) 0.0224(11) 0.0062(9) 0.0033(9) 0.0003(9) C35 0.0236(12) 0.0217(12) 0.0302(13) 0.0008(10) 0.0037(10) -0.0032(9) F35 0.0376(9) 0.0392(9) 0.0426(9) -0.0121(7) 0.0107(7) -0.0170(7) C36 0.0354(14) 0.0260(13) 0.0281(13) -0.0014(10) 0.0078(11) 0.0043(11) F36 0.0548(11) 0.0489(11) 0.0371(9) -0.0159(8) 0.0188(8) -0.0064(9) C37 0.0254(13) 0.0301(14) 0.0328(14) 0.0096(11) 0.0150(11) 0.0068(10) F37 0.0388(9) 0.0416(10) 0.0447(10) 0.0090(8) 0.0258(8) 0.0046(7) C38 0.0184(11) 0.0264(13) 0.0364(14) 0.0075(10) 0.0012(10) -0.0039(10) F38 0.0270(8) 0.0455(10) 0.0578(11) 0.0020(8) 0.0068(8) -0.0153(7) C39 0.0233(12) 0.0255(12) 0.0251(12) 0.0011(10) 0.0000(10) 0.0004(10) F39 0.0368(9) 0.0435(10) 0.0343(9) -0.0105(7) 0.0008(7) -0.0128(7) C40 0.0201(11) 0.0182(11) 0.0288(12) -0.0002(9) 0.0009(9) -0.0025(9) C41 0.0245(12) 0.0246(13) 0.0325(13) -0.0022(10) 0.0015(10) -0.0021(10) F41 0.0430(10) 0.0451(10) 0.0395(9) -0.0172(8) 0.0139(8) -0.0131(8) C42 0.0368(15) 0.0248(13) 0.0440(16) -0.0105(12) -0.0020(12) -0.0062(11) F42 0.0607(12) 0.0449(11) 0.0652(13) -0.0300(10) 0.0031(10) -0.0169(9) C43 0.0332(15) 0.0279(15) 0.065(2) -0.0018(14) 0.0009(14) -0.0155(12) F43 0.0568(13) 0.0473(12) 0.0923(16) -0.0125(11) 0.0099(11) -0.0353(10) C44 0.0353(16) 0.0389(17) 0.0543(19) 0.0009(14) 0.0167(14) -0.0158(13) F44 0.0667(14) 0.0776(16) 0.0814(15) -0.0148(12) 0.0440(12) -0.0439(12) C45 0.0306(14) 0.0263(13) 0.0365(14) -0.0042(11) 0.0065(11) -0.0059(11) F45 0.0546(11) 0.0527(11) 0.0481(10) -0.0208(9) 0.0279(9) -0.0251(9) N7 0.175(6) 0.143(5) 0.079(3) 0.009(3) 0.021(4) -0.015(5) C46 0.112(5) 0.125(5) 0.044(3) 0.013(3) -0.005(3) -0.036(4) C47 0.111(5) 0.306(11) 0.060(3) 0.059(5) -0.011(3) -0.072(6) N8 0.122(3) 0.0414(17) 0.0541(19) 0.0086(15) 0.018(2) -0.0155(19) C48 0.108(3) 0.0335(18) 0.0417(19) 0.0063(15) 0.009(2) -0.006(2) C49 0.132(5) 0.077(3) 0.112(4) 0.011(3) 0.048(4) -0.029(3) N9 0.0296(13) 0.0432(16) 0.0664(18) -0.0133(13) 0.0052(12) -0.0035(11) C50 0.0246(14) 0.0400(17) 0.0536(18) -0.0083(14) -0.0007(13) -0.0028(12) C51 0.0409(19) 0.0400(19) 0.096(3) -0.0052(19) -0.0108(19) 0.0030(15) _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 C22 1.996(2) . ? Zn1 N6 2.0210(19) . ? Zn1 O1 2.0710(16) . ? Zn1 N1 2.1174(19) . ? Zn2 C28 1.987(2) . ? Zn2 N2 2.010(2) . ? Zn2 O1 2.0726(17) . ? Zn2 N3 2.1207(19) . ? Zn3 C34 1.989(2) . ? Zn3 N4 2.004(2) . ? Zn3 O1 2.0508(17) . ? Zn3 N5 2.1166(19) . ? Zn4 C40 2.015(2) . ? Zn4 N2 2.044(2) . ? Zn4 N4 2.0762(19) . ? Zn4 N6 2.078(2) . ? N1 C1 1.479(3) . ? N1 C7 1.484(3) . ? N1 N2 1.487(3) . ? C1 C2 1.373(3) . ? C1 C6 1.385(4) . ? C2 C3 1.389(4) . ? C3 C4 1.371(4) . ? C4 C5 1.386(5) . ? C5 C6 1.382(4) . ? N3 C8 1.478(3) . ? N3 N4 1.479(3) . ? N3 C14 1.490(3) . ? C8 C13 1.377(3) . ? C8 C9 1.385(3) . ? C9 C10 1.385(4) . ? C10 C11 1.374(4) . ? C11 C12 1.378(4) . ? C12 C13 1.388(3) . ? N5 C15 1.471(3) . ? N5 C21 1.481(3) . ? N5 N6 1.485(3) . ? C15 C20 1.380(3) . ? C15 C16 1.385(3) . ? C16 C17 1.383(4) . ? C17 C18 1.379(4) . ? C18 C19 1.379(4) . ? C19 C20 1.383(4) . ? C22 C23 1.377(4) . ? C22 C27 1.377(4) . ? C23 F23 1.361(3) . ? C23 C24 1.379(4) . ? C24 F24 1.349(3) . ? C24 C25 1.371(4) . ? C25 F25 1.341(3) . ? C25 C26 1.378(4) . ? C26 F26 1.347(3) . ? C26 C27 1.384(4) . ? C27 F27 1.364(3) . ? C28 C33 1.375(4) . ? C28 C29 1.378(4) . ? C29 F29 1.363(3) . ? C29 C30 1.377(4) . ? C30 F30 1.346(3) . ? C30 C31 1.364(5) . ? C31 F31 1.349(3) . ? C31 C32 1.373(5) . ? C32 F32 1.351(4) . ? C32 C33 1.384(4) . ? C33 F33 1.359(3) . ? C34 C39 1.376(3) . ? C34 C35 1.378(3) . ? C35 F35 1.359(3) . ? C35 C36 1.381(3) . ? C36 F36 1.342(3) . ? C36 C37 1.370(4) . ? C37 F37 1.348(3) . ? C37 C38 1.379(4) . ? C38 F38 1.343(3) . ? C38 C39 1.370(3) . ? C39 F39 1.365(3) . ? C40 C45 1.371(4) . ? C40 C41 1.383(3) . ? C41 F41 1.362(3) . ? C41 C42 1.375(4) . ? C42 F42 1.355(3) . ? C42 C43 1.371(4) . ? C43 F43 1.346(3) . ? C43 C44 1.369(4) . ? C44 F44 1.349(3) . ? C44 C45 1.382(4) . ? C45 F45 1.358(3) . ? N7 C46 1.118(8) . ? C46 C47 1.442(9) . ? N8 C48 1.115(5) . ? C48 C49 1.445(6) . ? N9 C50 1.131(4) . ? C50 C51 1.455(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C22 Zn1 N6 128.34(9) . . ? C22 Zn1 O1 116.22(9) . . ? N6 Zn1 O1 91.19(7) . . ? C22 Zn1 N1 119.62(9) . . ? N6 Zn1 N1 97.68(8) . . ? O1 Zn1 N1 96.38(7) . . ? C28 Zn2 N2 129.09(9) . . ? C28 Zn2 O1 114.36(9) . . ? N2 Zn2 O1 92.50(7) . . ? C28 Zn2 N3 120.92(9) . . ? N2 Zn2 N3 97.30(7) . . ? O1 Zn2 N3 94.57(7) . . ? C34 Zn3 N4 124.71(9) . . ? C34 Zn3 O1 120.02(8) . . ? N4 Zn3 O1 92.27(7) . . ? C34 Zn3 N5 119.27(8) . . ? N4 Zn3 N5 98.79(8) . . ? O1 Zn3 N5 94.90(7) . . ? C40 Zn4 N2 124.57(9) . . ? C40 Zn4 N4 114.19(9) . . ? N2 Zn4 N4 96.76(8) . . ? C40 Zn4 N6 121.09(9) . . ? N2 Zn4 N6 97.03(8) . . ? N4 Zn4 N6 97.61(8) . . ? Zn3 O1 Zn1 107.60(7) . . ? Zn3 O1 Zn2 106.63(7) . . ? Zn1 O1 Zn2 104.63(7) . . ? C1 N1 C7 110.08(18) . . ? C1 N1 N2 109.25(17) . . ? C7 N1 N2 109.88(17) . . ? C1 N1 Zn1 118.26(14) . . ? C7 N1 Zn1 108.30(14) . . ? N2 N1 Zn1 100.55(12) . . ? N1 N2 Zn2 107.38(13) . . ? N1 N2 Zn4 114.64(14) . . ? Zn2 N2 Zn4 104.24(9) . . ? C2 C1 C6 120.1(2) . . ? C2 C1 N1 119.6(2) . . ? C6 C1 N1 120.3(2) . . ? C1 C2 C3 120.1(3) . . ? C4 C3 C2 120.2(3) . . ? C3 C4 C5 119.6(3) . . ? C6 C5 C4 120.5(3) . . ? C5 C6 C1 119.5(3) . . ? C8 N3 N4 109.75(17) . . ? C8 N3 C14 110.35(18) . . ? N4 N3 C14 109.65(17) . . ? C8 N3 Zn2 117.38(14) . . ? N4 N3 Zn2 101.03(12) . . ? C14 N3 Zn2 108.19(14) . . ? N3 N4 Zn3 108.44(13) . . ? N3 N4 Zn4 114.18(13) . . ? Zn3 N4 Zn4 102.83(9) . . ? C13 C8 C9 119.7(2) . . ? C13 C8 N3 120.2(2) . . ? C9 C8 N3 120.0(2) . . ? C8 C9 C10 120.0(2) . . ? C11 C10 C9 120.4(2) . . ? C10 C11 C12 119.5(2) . . ? C11 C12 C13 120.6(2) . . ? C8 C13 C12 119.7(2) . . ? C15 N5 C21 111.18(19) . . ? C15 N5 N6 109.50(17) . . ? C21 N5 N6 110.26(17) . . ? C15 N5 Zn3 116.41(14) . . ? C21 N5 Zn3 107.73(15) . . ? N6 N5 Zn3 101.29(13) . . ? N5 N6 Zn1 109.05(13) . . ? N5 N6 Zn4 113.04(13) . . ? Zn1 N6 Zn4 102.96(9) . . ? C20 C15 C16 119.1(2) . . ? C20 C15 N5 119.4(2) . . ? C16 C15 N5 121.4(2) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 120.6(3) . . ? C17 C18 C19 119.1(3) . . ? C18 C19 C20 120.5(3) . . ? C15 C20 C19 120.4(2) . . ? C23 C22 C27 114.2(2) . . ? C23 C22 Zn1 121.96(19) . . ? C27 C22 Zn1 123.66(19) . . ? F23 C23 C22 119.3(2) . . ? F23 C23 C24 116.5(2) . . ? C22 C23 C24 124.3(3) . . ? F24 C24 C25 119.8(2) . . ? F24 C24 C23 121.2(3) . . ? C25 C24 C23 119.0(3) . . ? F25 C25 C24 120.5(3) . . ? F25 C25 C26 119.8(3) . . ? C24 C25 C26 119.6(2) . . ? F26 C26 C25 120.1(2) . . ? F26 C26 C27 121.2(3) . . ? C25 C26 C27 118.7(3) . . ? F27 C27 C22 119.7(2) . . ? F27 C27 C26 116.2(2) . . ? C22 C27 C26 124.1(3) . . ? C33 C28 C29 114.6(2) . . ? C33 C28 Zn2 121.4(2) . . ? C29 C28 Zn2 123.8(2) . . ? F29 C29 C30 116.5(3) . . ? F29 C29 C28 119.4(2) . . ? C30 C29 C28 124.1(3) . . ? F30 C30 C31 119.9(3) . . ? F30 C30 C29 121.5(3) . . ? C31 C30 C29 118.6(3) . . ? F31 C31 C30 120.4(3) . . ? F31 C31 C32 119.2(3) . . ? C30 C31 C32 120.4(3) . . ? F32 C32 C31 120.6(3) . . ? F32 C32 C33 120.9(3) . . ? C31 C32 C33 118.5(3) . . ? F33 C33 C28 119.2(2) . . ? F33 C33 C32 117.1(3) . . ? C28 C33 C32 123.7(3) . . ? C39 C34 C35 114.4(2) . . ? C39 C34 Zn3 123.24(18) . . ? C35 C34 Zn3 121.92(18) . . ? F35 C35 C34 119.4(2) . . ? F35 C35 C36 116.7(2) . . ? C34 C35 C36 123.9(2) . . ? F36 C36 C37 119.8(2) . . ? F36 C36 C35 121.4(2) . . ? C37 C36 C35 118.8(2) . . ? F37 C37 C36 120.5(2) . . ? F37 C37 C38 119.7(2) . . ? C36 C37 C38 119.8(2) . . ? F38 C38 C39 121.9(2) . . ? F38 C38 C37 119.3(2) . . ? C39 C38 C37 118.8(2) . . ? F39 C39 C38 117.0(2) . . ? F39 C39 C34 118.7(2) . . ? C38 C39 C34 124.3(2) . . ? C45 C40 C41 113.7(2) . . ? C45 C40 Zn4 123.84(19) . . ? C41 C40 Zn4 122.49(18) . . ? F41 C41 C42 116.2(2) . . ? F41 C41 C40 119.6(2) . . ? C42 C41 C40 124.2(2) . . ? F42 C42 C43 119.3(2) . . ? F42 C42 C41 121.4(3) . . ? C43 C42 C41 119.4(3) . . ? F43 C43 C44 120.4(3) . . ? F43 C43 C42 120.4(3) . . ? C44 C43 C42 119.2(3) . . ? F44 C44 C43 119.4(3) . . ? F44 C44 C45 121.5(3) . . ? C43 C44 C45 119.0(3) . . ? F45 C45 C40 119.9(2) . . ? F45 C45 C44 115.6(2) . . ? C40 C45 C44 124.5(3) . . ? N7 C46 C47 178.8(7) . . ? N8 C48 C49 179.8(6) . . ? N9 C50 C51 179.3(4) . . ? 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 C34 Zn3 O1 Zn1 135.08(9) . . . . ? N4 Zn3 O1 Zn1 -91.99(8) . . . . ? N5 Zn3 O1 Zn1 7.03(8) . . . . ? C34 Zn3 O1 Zn2 -113.12(10) . . . . ? N4 Zn3 O1 Zn2 19.81(8) . . . . ? N5 Zn3 O1 Zn2 118.83(8) . . . . ? C22 Zn1 O1 Zn3 -115.39(9) . . . . ? N6 Zn1 O1 Zn3 19.19(8) . . . . ? N1 Zn1 O1 Zn3 117.05(8) . . . . ? C22 Zn1 O1 Zn2 131.45(9) . . . . ? N6 Zn1 O1 Zn2 -93.97(8) . . . . ? N1 Zn1 O1 Zn2 3.90(8) . . . . ? C28 Zn2 O1 Zn3 133.82(9) . . . . ? N2 Zn2 O1 Zn3 -90.73(8) . . . . ? N3 Zn2 O1 Zn3 6.80(8) . . . . ? C28 Zn2 O1 Zn1 -112.33(9) . . . . ? N2 Zn2 O1 Zn1 23.11(8) . . . . ? N3 Zn2 O1 Zn1 120.65(8) . . . . ? C22 Zn1 N1 C1 -47.43(18) . . . . ? N6 Zn1 N1 C1 169.75(15) . . . . ? O1 Zn1 N1 C1 77.67(16) . . . . ? C22 Zn1 N1 C7 78.62(17) . . . . ? N6 Zn1 N1 C7 -64.21(15) . . . . ? O1 Zn1 N1 C7 -156.28(14) . . . . ? C22 Zn1 N1 N2 -166.17(13) . . . . ? N6 Zn1 N1 N2 51.00(13) . . . . ? O1 Zn1 N1 N2 -41.08(13) . . . . ? C1 N1 N2 Zn2 -60.20(18) . . . . ? C7 N1 N2 Zn2 178.93(14) . . . . ? Zn1 N1 N2 Zn2 64.92(12) . . . . ? C1 N1 N2 Zn4 -175.50(14) . . . . ? C7 N1 N2 Zn4 63.6(2) . . . . ? Zn1 N1 N2 Zn4 -50.38(14) . . . . ? C28 Zn2 N2 N1 65.61(18) . . . . ? O1 Zn2 N2 N1 -58.96(13) . . . . ? N3 Zn2 N2 N1 -153.90(13) . . . . ? C28 Zn2 N2 Zn4 -172.37(10) . . . . ? O1 Zn2 N2 Zn4 63.06(9) . . . . ? N3 Zn2 N2 Zn4 -31.88(9) . . . . ? C40 Zn4 N2 N1 -107.01(16) . . . . ? N4 Zn4 N2 N1 127.35(14) . . . . ? N6 Zn4 N2 N1 28.78(15) . . . . ? C40 Zn4 N2 Zn2 135.89(10) . . . . ? N4 Zn4 N2 Zn2 10.25(10) . . . . ? N6 Zn4 N2 Zn2 -88.32(9) . . . . ? C7 N1 C1 C2 -115.5(2) . . . . ? N2 N1 C1 C2 123.8(2) . . . . ? Zn1 N1 C1 C2 9.7(3) . . . . ? C7 N1 C1 C6 65.7(3) . . . . ? N2 N1 C1 C6 -55.1(3) . . . . ? Zn1 N1 C1 C6 -169.1(2) . . . . ? C6 C1 C2 C3 2.3(4) . . . . ? N1 C1 C2 C3 -176.6(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 -1.8(4) . . . . ? C3 C4 C5 C6 1.7(5) . . . . ? C4 C5 C6 C1 0.3(5) . . . . ? C2 C1 C6 C5 -2.3(4) . . . . ? N1 C1 C6 C5 176.5(3) . . . . ? C28 Zn2 N3 C8 -45.19(19) . . . . ? N2 Zn2 N3 C8 169.95(15) . . . . ? O1 Zn2 N3 C8 76.84(15) . . . . ? C28 Zn2 N3 N4 -164.44(13) . . . . ? N2 Zn2 N3 N4 50.70(13) . . . . ? O1 Zn2 N3 N4 -42.42(12) . . . . ? C28 Zn2 N3 C14 80.43(17) . . . . ? N2 Zn2 N3 C14 -64.43(16) . . . . ? O1 Zn2 N3 C14 -157.55(15) . . . . ? C8 N3 N4 Zn3 -59.73(18) . . . . ? C14 N3 N4 Zn3 178.91(14) . . . . ? Zn2 N3 N4 Zn3 64.87(12) . . . . ? C8 N3 N4 Zn4 -173.70(13) . . . . ? C14 N3 N4 Zn4 64.94(19) . . . . ? Zn2 N3 N4 Zn4 -49.10(14) . . . . ? C34 Zn3 N4 N3 73.28(16) . . . . ? O1 Zn3 N4 N3 -56.25(13) . . . . ? N5 Zn3 N4 N3 -151.57(13) . . . . ? C34 Zn3 N4 Zn4 -165.47(9) . . . . ? O1 Zn3 N4 Zn4 65.00(8) . . . . ? N5 Zn3 N4 Zn4 -30.31(9) . . . . ? C40 Zn4 N4 N3 -105.38(15) . . . . ? N2 Zn4 N4 N3 27.43(15) . . . . ? N6 Zn4 N4 N3 125.49(14) . . . . ? C40 Zn4 N4 Zn3 137.37(9) . . . . ? N2 Zn4 N4 Zn3 -89.82(9) . . . . ? N6 Zn4 N4 Zn3 8.24(9) . . . . ? N4 N3 C8 C13 118.3(2) . . . . ? C14 N3 C8 C13 -120.7(2) . . . . ? Zn2 N3 C8 C13 3.8(3) . . . . ? N4 N3 C8 C9 -59.6(3) . . . . ? C14 N3 C8 C9 61.4(3) . . . . ? Zn2 N3 C8 C9 -174.07(19) . . . . ? C13 C8 C9 C10 0.2(4) . . . . ? N3 C8 C9 C10 178.1(2) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C9 C10 C11 C12 0.0(5) . . . . ? C10 C11 C12 C13 -0.3(4) . . . . ? C9 C8 C13 C12 -0.5(4) . . . . ? N3 C8 C13 C12 -178.4(2) . . . . ? C11 C12 C13 C8 0.6(4) . . . . ? C34 Zn3 N5 C15 -52.06(18) . . . . ? N4 Zn3 N5 C15 169.59(15) . . . . ? O1 Zn3 N5 C15 76.53(15) . . . . ? C34 Zn3 N5 C21 73.56(17) . . . . ? N4 Zn3 N5 C21 -64.79(16) . . . . ? O1 Zn3 N5 C21 -157.85(15) . . . . ? C34 Zn3 N5 N6 -170.69(12) . . . . ? N4 Zn3 N5 N6 50.96(13) . . . . ? O1 Zn3 N5 N6 -42.10(13) . . . . ? C15 N5 N6 Zn1 -59.21(19) . . . . ? C21 N5 N6 Zn1 178.16(15) . . . . ? Zn3 N5 N6 Zn1 64.29(13) . . . . ? C15 N5 N6 Zn4 -173.08(14) . . . . ? C21 N5 N6 Zn4 64.3(2) . . . . ? Zn3 N5 N6 Zn4 -49.59(14) . . . . ? C22 Zn1 N6 N5 70.36(17) . . . . ? O1 Zn1 N6 N5 -55.08(14) . . . . ? N1 Zn1 N6 N5 -151.69(13) . . . . ? C22 Zn1 N6 Zn4 -169.35(10) . . . . ? O1 Zn1 N6 Zn4 65.21(8) . . . . ? N1 Zn1 N6 Zn4 -31.40(9) . . . . ? C40 Zn4 N6 N5 -95.29(16) . . . . ? N2 Zn4 N6 N5 126.82(14) . . . . ? N4 Zn4 N6 N5 28.99(15) . . . . ? C40 Zn4 N6 Zn1 147.20(9) . . . . ? N2 Zn4 N6 Zn1 9.31(9) . . . . ? N4 Zn4 N6 Zn1 -88.52(9) . . . . ? C21 N5 C15 C20 -129.0(2) . . . . ? N6 N5 C15 C20 108.9(2) . . . . ? Zn3 N5 C15 C20 -5.2(3) . . . . ? C21 N5 C15 C16 54.4(3) . . . . ? N6 N5 C15 C16 -67.7(3) . . . . ? Zn3 N5 C15 C16 178.2(2) . . . . ? C20 C15 C16 C17 -0.7(4) . . . . ? N5 C15 C16 C17 175.9(3) . . . . ? C15 C16 C17 C18 -0.7(5) . . . . ? C16 C17 C18 C19 1.3(5) . . . . ? C17 C18 C19 C20 -0.6(4) . . . . ? C16 C15 C20 C19 1.4(4) . . . . ? N5 C15 C20 C19 -175.3(2) . . . . ? C18 C19 C20 C15 -0.8(4) . . . . ? N6 Zn1 C22 C23 62.6(2) . . . . ? O1 Zn1 C22 C23 177.42(18) . . . . ? N1 Zn1 C22 C23 -67.6(2) . . . . ? N6 Zn1 C22 C27 -112.7(2) . . . . ? O1 Zn1 C22 C27 2.1(2) . . . . ? N1 Zn1 C22 C27 117.1(2) . . . . ? C27 C22 C23 F23 -178.4(2) . . . . ? Zn1 C22 C23 F23 5.9(3) . . . . ? C27 C22 C23 C24 0.7(4) . . . . ? Zn1 C22 C23 C24 -175.0(2) . . . . ? F23 C23 C24 F24 -0.6(4) . . . . ? C22 C23 C24 F24 -179.7(2) . . . . ? F23 C23 C24 C25 179.0(2) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? F24 C24 C25 F25 -0.3(4) . . . . ? C23 C24 C25 F25 -180.0(3) . . . . ? F24 C24 C25 C26 179.1(3) . . . . ? C23 C24 C25 C26 -0.6(4) . . . . ? F25 C25 C26 F26 0.4(4) . . . . ? C24 C25 C26 F26 -179.0(2) . . . . ? F25 C25 C26 C27 180.0(2) . . . . ? C24 C25 C26 C27 0.5(4) . . . . ? C23 C22 C27 F27 179.5(2) . . . . ? Zn1 C22 C27 F27 -4.8(3) . . . . ? C23 C22 C27 C26 -0.7(4) . . . . ? Zn1 C22 C27 C26 174.9(2) . . . . ? F26 C26 C27 F27 -0.6(4) . . . . ? C25 C26 C27 F27 179.9(2) . . . . ? F26 C26 C27 C22 179.7(2) . . . . ? C25 C26 C27 C22 0.1(4) . . . . ? N2 Zn2 C28 C33 72.4(2) . . . . ? O1 Zn2 C28 C33 -172.13(19) . . . . ? N3 Zn2 C28 C33 -60.2(2) . . . . ? N2 Zn2 C28 C29 -103.1(2) . . . . ? O1 Zn2 C28 C29 12.3(2) . . . . ? N3 Zn2 C28 C29 124.3(2) . . . . ? C33 C28 C29 F29 -179.9(2) . . . . ? Zn2 C28 C29 F29 -4.1(3) . . . . ? C33 C28 C29 C30 -0.5(4) . . . . ? Zn2 C28 C29 C30 175.3(2) . . . . ? F29 C29 C30 F30 -0.3(4) . . . . ? C28 C29 C30 F30 -179.8(2) . . . . ? F29 C29 C30 C31 179.5(2) . . . . ? C28 C29 C30 C31 0.0(4) . . . . ? F30 C30 C31 F31 0.5(4) . . . . ? C29 C30 C31 F31 -179.3(2) . . . . ? F30 C30 C31 C32 -180.0(3) . . . . ? C29 C30 C31 C32 0.2(4) . . . . ? F31 C31 C32 F32 -0.8(4) . . . . ? C30 C31 C32 F32 179.6(3) . . . . ? F31 C31 C32 C33 179.7(3) . . . . ? C30 C31 C32 C33 0.1(4) . . . . ? C29 C28 C33 F33 179.6(2) . . . . ? Zn2 C28 C33 F33 3.7(3) . . . . ? C29 C28 C33 C32 0.8(4) . . . . ? Zn2 C28 C33 C32 -175.1(2) . . . . ? F32 C32 C33 F33 1.0(4) . . . . ? C31 C32 C33 F33 -179.5(3) . . . . ? F32 C32 C33 C28 179.8(3) . . . . ? C31 C32 C33 C28 -0.7(4) . . . . ? N4 Zn3 C34 C39 -122.2(2) . . . . ? O1 Zn3 C34 C39 -5.1(2) . . . . ? N5 Zn3 C34 C39 110.8(2) . . . . ? N4 Zn3 C34 C35 50.0(2) . . . . ? O1 Zn3 C34 C35 167.10(18) . . . . ? N5 Zn3 C34 C35 -77.0(2) . . . . ? C39 C34 C35 F35 179.4(2) . . . . ? Zn3 C34 C35 F35 6.6(3) . . . . ? C39 C34 C35 C36 -0.1(4) . . . . ? Zn3 C34 C35 C36 -172.9(2) . . . . ? F35 C35 C36 F36 0.4(4) . . . . ? C34 C35 C36 F36 180.0(2) . . . . ? F35 C35 C36 C37 -178.5(2) . . . . ? C34 C35 C36 C37 1.1(4) . . . . ? F36 C36 C37 F37 1.3(4) . . . . ? C35 C36 C37 F37 -179.7(2) . . . . ? F36 C36 C37 C38 179.9(2) . . . . ? C35 C36 C37 C38 -1.2(4) . . . . ? F37 C37 C38 F38 0.2(4) . . . . ? C36 C37 C38 F38 -178.3(2) . . . . ? F37 C37 C38 C39 179.0(2) . . . . ? C36 C37 C38 C39 0.4(4) . . . . ? F38 C38 C39 F39 -0.5(4) . . . . ? C37 C38 C39 F39 -179.2(2) . . . . ? F38 C38 C39 C34 179.3(2) . . . . ? C37 C38 C39 C34 0.6(4) . . . . ? C35 C34 C39 F39 179.0(2) . . . . ? Zn3 C34 C39 F39 -8.3(3) . . . . ? C35 C34 C39 C38 -0.8(4) . . . . ? Zn3 C34 C39 C38 172.0(2) . . . . ? N2 Zn4 C40 C45 39.7(3) . . . . ? N4 Zn4 C40 C45 157.5(2) . . . . ? N6 Zn4 C40 C45 -86.4(2) . . . . ? N2 Zn4 C40 C41 -139.55(19) . . . . ? N4 Zn4 C40 C41 -21.8(2) . . . . ? N6 Zn4 C40 C41 94.4(2) . . . . ? C45 C40 C41 F41 179.5(2) . . . . ? Zn4 C40 C41 F41 -1.2(3) . . . . ? C45 C40 C41 C42 0.5(4) . . . . ? Zn4 C40 C41 C42 179.8(2) . . . . ? F41 C41 C42 F42 -0.4(4) . . . . ? C40 C41 C42 F42 178.6(3) . . . . ? F41 C41 C42 C43 -179.2(3) . . . . ? C40 C41 C42 C43 -0.2(4) . . . . ? F42 C42 C43 F43 0.9(5) . . . . ? C41 C42 C43 F43 179.7(3) . . . . ? F42 C42 C43 C44 -178.6(3) . . . . ? C41 C42 C43 C44 0.2(5) . . . . ? F43 C43 C44 F44 0.3(5) . . . . ? C42 C43 C44 F44 179.7(3) . . . . ? F43 C43 C44 C45 180.0(3) . . . . ? C42 C43 C44 C45 -0.5(5) . . . . ? C41 C40 C45 F45 -179.7(2) . . . . ? Zn4 C40 C45 F45 1.0(4) . . . . ? C41 C40 C45 C44 -0.8(4) . . . . ? Zn4 C40 C45 C44 179.9(2) . . . . ? F44 C44 C45 F45 -0.5(5) . . . . ? C43 C44 C45 F45 179.8(3) . . . . ? F44 C44 C45 C40 -179.4(3) . . . . ? C43 C44 C45 C40 0.9(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 F29 0.73(3) 2.55(3) 3.059(2) 128(3) . O1 H1 F27 0.73(3) 2.61(3) 3.108(2) 128(3) . N2 H2 N8 0.79(3) 2.34(3) 3.110(4) 164(3) . N4 H4 F41 0.86(3) 2.51(3) 3.120(2) 128(2) . N6 H6 N9 0.86(3) 2.42(3) 3.240(3) 161(2) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.506 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.074 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 790912' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C12 H16 N6 Zn' _chemical_formula_sum 'C12 H16 N6 Zn' _chemical_formula_weight 309.68 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Fddd _symmetry_space_group_name_Hall '-F 2uv 2vw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+3/4, -y+3/4, z' '-x+3/4, y, -z+3/4' 'x, -y+3/4, -z+3/4' 'x, y+1/2, z+1/2' '-x+3/4, -y+5/4, z+1/2' '-x+3/4, y+1/2, -z+5/4' 'x, -y+5/4, -z+5/4' 'x+1/2, y, z+1/2' '-x+5/4, -y+3/4, z+1/2' '-x+5/4, y, -z+5/4' 'x+1/2, -y+3/4, -z+5/4' 'x+1/2, y+1/2, z' '-x+5/4, -y+5/4, z' '-x+5/4, y+1/2, -z+3/4' 'x+1/2, -y+5/4, -z+3/4' '-x, -y, -z' 'x-3/4, y-3/4, -z' 'x-3/4, -y, z-3/4' '-x, y-3/4, z-3/4' '-x, -y+1/2, -z+1/2' 'x-3/4, y-1/4, -z+1/2' 'x-3/4, -y+1/2, z-1/4' '-x, y-1/4, z-1/4' '-x+1/2, -y, -z+1/2' 'x-1/4, y-3/4, -z+1/2' 'x-1/4, -y, z-1/4' '-x+1/2, y-3/4, z-1/4' '-x+1/2, -y+1/2, -z' 'x-1/4, y-1/4, -z' 'x-1/4, -y+1/2, z-3/4' '-x+1/2, y-1/4, z-3/4' _cell_length_a 7.6932(5) _cell_length_b 16.0210(11) _cell_length_c 22.1017(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2724.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 3370 _cell_measurement_theta_min 4.39 _cell_measurement_theta_max 32.90 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.510 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.900 _exptl_absorpt_process_details 'SADABS v2008/1, Sheldrick, G.M., (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8457 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2 SMX' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker APEX 2 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2 _diffrn_reflns_number 4496 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.39 _diffrn_reflns_theta_max 33.00 _reflns_number_total 734 _reflns_number_gt 715 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX 2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0428P)^2^+5.1142P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'all non-H atoms found by direct methods' _atom_sites_solution_hydrogens 'geom except NH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 734 _refine_ls_number_parameters 50 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0268 _refine_ls_R_factor_gt 0.0262 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.1250 0.6250 0.6250 0.01390(17) Uani 1 4 d S . . N1 N 0.02250(18) 0.69964(8) 0.56324(6) 0.0164(3) Uani 1 1 d . . . H1 H -0.020(3) 0.7427(14) 0.5745(9) 0.020 Uiso 1 1 d . . . C1 C 0.03973(19) 0.69356(9) 0.50464(7) 0.0133(3) Uani 1 1 d . . . C2 C -0.0328(2) 0.76162(10) 0.46448(7) 0.0197(3) Uani 1 1 d . . . H2A H -0.0894 0.8041 0.4895 0.030 Uiso 1 1 calc R . . H2B H -0.1179 0.7375 0.4365 0.030 Uiso 1 1 calc R . . H2C H 0.0619 0.7873 0.4414 0.030 Uiso 1 1 calc R . . C3 C 0.1250 0.6250 0.47558(11) 0.0132(4) Uani 1 2 d S . . C4 C 0.1250 0.6250 0.41142(11) 0.0153(5) Uani 1 2 d S . . N2 N 0.1250 0.6250 0.35908(10) 0.0205(4) Uani 1 2 d S . . 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 0.0201(2) 0.0139(2) 0.0077(2) 0.000 0.000 0.000 N1 0.0247(7) 0.0121(6) 0.0125(6) -0.0028(5) 0.0001(5) 0.0065(5) C1 0.0164(7) 0.0106(6) 0.0130(7) 0.0005(5) -0.0021(5) -0.0005(6) C2 0.0276(8) 0.0154(7) 0.0161(8) 0.0023(6) -0.0031(6) 0.0054(6) C3 0.0187(10) 0.0105(10) 0.0103(10) 0.000 0.000 -0.0008(7) C4 0.0208(11) 0.0088(9) 0.0163(13) 0.000 0.000 -0.0017(7) N2 0.0349(12) 0.0155(9) 0.0111(10) 0.000 0.000 -0.0023(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N1 1.9787(13) . ? N1 C1 1.3056(19) . ? C1 C3 1.4316(18) . ? C1 C2 1.513(2) . ? C3 C4 1.418(3) . ? C4 N2 1.157(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 N1 133.03(8) 11_455 14_455 ? N1 Zn1 N1 92.76(8) 11_455 8 ? N1 Zn1 N1 105.63(8) 14_455 8 ? N1 Zn1 N1 92.76(8) 14_455 . ? N1 Zn1 N1 133.03(8) 8 . ? C1 N1 Zn1 126.78(11) . . ? N1 C1 C3 123.29(15) . . ? N1 C1 C2 119.39(13) . . ? C3 C1 C2 117.32(15) . . ? C4 C3 C1 116.66(11) . . ? C1 C3 C1 126.7(2) . 14_455 ? N2 C4 C3 180.000(1) . . ? 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 N1 Zn1 N1 C1 133.17(15) 11_455 . . . ? N1 Zn1 N1 C1 -3.13(10) 14_455 . . . ? N1 Zn1 N1 C1 -117.59(14) 8 . . . ? Zn1 N1 C1 C3 6.3(2) . . . . ? Zn1 N1 C1 C2 -173.69(11) . . . . ? N1 C1 C3 C4 176.65(11) . . . . ? C2 C1 C3 C4 -3.41(14) . . . . ? N1 C1 C3 C1 -3.35(11) . . . 14_455 ? C2 C1 C3 C1 176.59(14) . . . 14_455 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 N2 0.80(2) 2.39(2) 3.1948(15) 175.5(19) 31_566 _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 33.00 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 0.507 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.078 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 790913' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H70 O8 Zn7' _chemical_formula_sum 'C28 H70 O8 Zn7' _chemical_formula_weight 992.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 17.0725(2) _cell_length_b 15.6207(3) _cell_length_c 15.3372(2) _cell_angle_alpha 90.00 _cell_angle_beta 93.2230(8) _cell_angle_gamma 90.00 _cell_volume 4083.72(11) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 79782 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.614 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2048 _exptl_absorpt_coefficient_mu 4.079 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.511 _exptl_absorpt_correction_T_max 0.736 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 43518 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.52 _reflns_number_total 9353 _reflns_number_gt 7992 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0000P)^2^+8.6453P] 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 9353 _refine_ls_number_parameters 414 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.0426 _refine_ls_R_factor_gt 0.0322 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0636 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.092 _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 0.5000 0.5000 0.0000 0.01758(10) Uani 1 2 d S . . Zn2 Zn 0.412478(18) 0.32483(2) 0.00110(2) 0.02132(8) Uani 1 1 d . A . Zn3 Zn 0.385302(18) 0.45593(2) 0.14625(2) 0.02045(8) Uani 1 1 d . . . Zn4 Zn 0.320023(18) 0.48968(2) -0.04097(2) 0.02067(8) Uani 1 1 d . . . O1 O 0.47852(10) 0.39881(13) 0.08920(12) 0.0194(4) Uani 1 1 d . . . C1 C 0.54024(18) 0.3557(2) 0.1390(2) 0.0334(8) Uani 1 1 d . . . H1A H 0.5812 0.3981 0.1567 0.040 Uiso 1 1 calc R . . H1B H 0.5643 0.3131 0.1009 0.040 Uiso 1 1 calc R . . C2 C 0.5157(2) 0.3121(3) 0.2171(3) 0.0545(12) Uani 1 1 d . . . H2A H 0.4988 0.3545 0.2592 0.082 Uiso 1 1 calc R . . H2B H 0.5598 0.2791 0.2434 0.082 Uiso 1 1 calc R . . H2C H 0.4721 0.2733 0.2012 0.082 Uiso 1 1 calc R . . O2 O 0.31963(11) 0.39155(13) 0.04826(12) 0.0213(4) Uani 1 1 d . . . C3 C 0.24668(16) 0.3505(2) 0.0650(2) 0.0268(7) Uani 1 1 d . . . H3A H 0.2230 0.3269 0.0097 0.032 Uiso 1 1 calc R . . H3B H 0.2100 0.3934 0.0870 0.032 Uiso 1 1 calc R . . C4 C 0.2582(2) 0.2796(2) 0.1307(2) 0.0416(9) Uani 1 1 d . . . H4A H 0.2925 0.2357 0.1078 0.062 Uiso 1 1 calc R . . H4B H 0.2073 0.2541 0.1419 0.062 Uiso 1 1 calc R . . H4C H 0.2823 0.3027 0.1852 0.062 Uiso 1 1 calc R . . O3 O 0.39537(10) 0.54756(12) 0.05110(12) 0.0179(4) Uani 1 1 d . . . C5 C 0.38361(17) 0.6377(2) 0.0648(2) 0.0266(6) Uani 1 1 d . . . H5A H 0.3687 0.6649 0.0079 0.032 Uiso 1 1 calc R . . H5B H 0.4338 0.6635 0.0871 0.032 Uiso 1 1 calc R . . C6 C 0.3221(2) 0.6568(2) 0.1270(3) 0.0462(10) Uani 1 1 d . . . H6A H 0.2725 0.6306 0.1060 0.069 Uiso 1 1 calc R . . H6B H 0.3153 0.7189 0.1314 0.069 Uiso 1 1 calc R . . H6C H 0.3381 0.6335 0.1846 0.069 Uiso 1 1 calc R . . O4 O 0.41973(11) 0.42973(13) -0.08044(12) 0.0204(4) Uani 1 1 d . . . C7 C 0.42884(19) 0.4165(2) -0.17145(19) 0.0324(7) Uani 1 1 d D . . H7A H 0.4776 0.3836 -0.1789 0.039 Uiso 1 1 calc R . . H7B H 0.4345 0.4728 -0.2002 0.039 Uiso 1 1 calc R . . C8 C 0.3617(2) 0.3698(3) -0.2154(2) 0.0410(9) Uani 1 1 d D . . H8A H 0.3583 0.3123 -0.1904 0.061 Uiso 1 1 calc R . . H8B H 0.3695 0.3654 -0.2780 0.061 Uiso 1 1 calc R . . H8C H 0.3129 0.4010 -0.2067 0.061 Uiso 1 1 calc R . . C9 C 0.4244(2) 0.2044(2) -0.0324(3) 0.0406(8) Uani 1 1 d DU . . H9A H 0.3713 0.1790 -0.0385 0.049 Uiso 0.744(14) 1 calc PR A 1 H9B H 0.4457 0.2036 -0.0912 0.049 Uiso 0.744(14) 1 calc PR A 1 H9C H 0.3907 0.1706 0.0052 0.049 Uiso 0.256(14) 1 calc PR A 2 H9D H 0.4014 0.1989 -0.0929 0.049 Uiso 0.256(14) 1 calc PR A 2 C10 C 0.4737(4) 0.1468(3) 0.0241(5) 0.048(2) Uani 0.744(14) 1 d PDU A 1 H10A H 0.4735 0.0893 -0.0014 0.072 Uiso 0.744(14) 1 calc PR A 1 H10B H 0.4527 0.1443 0.0823 0.072 Uiso 0.744(14) 1 calc PR A 1 H10C H 0.5276 0.1687 0.0291 0.072 Uiso 0.744(14) 1 calc PR A 1 C10X C 0.4998(7) 0.1617(10) -0.0304(14) 0.040(5) Uani 0.256(14) 1 d PDU A 2 H10D H 0.4926 0.1023 -0.0498 0.060 Uiso 0.256(14) 1 calc PR A 2 H10E H 0.5234 0.1625 0.0293 0.060 Uiso 0.256(14) 1 calc PR A 2 H10F H 0.5344 0.1915 -0.0693 0.060 Uiso 0.256(14) 1 calc PR A 2 C11 C 0.35801(19) 0.4612(2) 0.26910(19) 0.0302(7) Uani 1 1 d . . . H11A H 0.3029 0.4807 0.2704 0.036 Uiso 1 1 calc R . . H11B H 0.3603 0.4024 0.2930 0.036 Uiso 1 1 calc R . . C12 C 0.4082(2) 0.5186(3) 0.3301(2) 0.0442(9) Uani 1 1 d . . . H12A H 0.4627 0.4987 0.3322 0.066 Uiso 1 1 calc R . . H12B H 0.3885 0.5164 0.3889 0.066 Uiso 1 1 calc R . . H12C H 0.4057 0.5777 0.3086 0.066 Uiso 1 1 calc R . . C13 C 0.23328(17) 0.5418(2) -0.1112(2) 0.0329(7) Uani 1 1 d . . . H13A H 0.2165 0.5941 -0.0809 0.039 Uiso 1 1 calc R . . H13B H 0.2532 0.5599 -0.1678 0.039 Uiso 1 1 calc R . . C14 C 0.16183(18) 0.4856(3) -0.1296(2) 0.0399(9) Uani 1 1 d . . . H14A H 0.1768 0.4349 -0.1623 0.060 Uiso 1 1 calc R . . H14B H 0.1217 0.5178 -0.1641 0.060 Uiso 1 1 calc R . . H14C H 0.1408 0.4679 -0.0743 0.060 Uiso 1 1 calc R . . Zn5 Zn 0.0000 0.5000 0.5000 0.01737(10) Uani 1 2 d S . . Zn6 Zn 0.182250(18) 0.52449(2) 0.50133(2) 0.02150(8) Uani 1 1 d . . . Zn7 Zn 0.084171(19) 0.52515(2) 0.32820(2) 0.02141(8) Uani 1 1 d . . . Zn8 Zn 0.073248(18) 0.67709(2) 0.45523(2) 0.01971(8) Uani 1 1 d . . . O5 O 0.09720(11) 0.44925(13) 0.43791(12) 0.0199(4) Uani 1 1 d . . . C15 C 0.10687(19) 0.3598(2) 0.4226(2) 0.0309(7) Uani 1 1 d . . . H15A H 0.0661 0.3406 0.3784 0.037 Uiso 1 1 calc R . . H15B H 0.0990 0.3282 0.4774 0.037 Uiso 1 1 calc R . . C16 C 0.1858(2) 0.3384(2) 0.3916(3) 0.0436(9) Uani 1 1 d . . . H16A H 0.1942 0.3698 0.3376 0.065 Uiso 1 1 calc R . . H16B H 0.1888 0.2767 0.3804 0.065 Uiso 1 1 calc R . . H16C H 0.2263 0.3544 0.4364 0.065 Uiso 1 1 calc R . . O6 O 0.16006(10) 0.60594(13) 0.39772(12) 0.0199(4) Uani 1 1 d . . . C17 C 0.21989(16) 0.6480(2) 0.35152(19) 0.0253(6) Uani 1 1 d . . . H17A H 0.1949 0.6831 0.3039 0.030 Uiso 1 1 calc R . . H17B H 0.2530 0.6044 0.3247 0.030 Uiso 1 1 calc R . . C18 C 0.2707(2) 0.7043(2) 0.4098(2) 0.0391(8) Uani 1 1 d . . . H18A H 0.2383 0.7478 0.4364 0.059 Uiso 1 1 calc R . . H18B H 0.3100 0.7324 0.3754 0.059 Uiso 1 1 calc R . . H18C H 0.2972 0.6695 0.4558 0.059 Uiso 1 1 calc R . . O7 O -0.00025(10) 0.58786(13) 0.39451(12) 0.0191(4) Uani 1 1 d . . . C19 C -0.06922(17) 0.6167(2) 0.3455(2) 0.0299(7) Uani 1 1 d . . . H19A H -0.1060 0.6420 0.3860 0.036 Uiso 1 1 calc R . . H19B H -0.0956 0.5669 0.3166 0.036 Uiso 1 1 calc R . . C20 C -0.0514(2) 0.6818(2) 0.2775(2) 0.0362(8) Uani 1 1 d . . . H20A H -0.0280 0.7325 0.3060 0.054 Uiso 1 1 calc R . . H20B H -0.1001 0.6979 0.2447 0.054 Uiso 1 1 calc R . . H20C H -0.0146 0.6573 0.2375 0.054 Uiso 1 1 calc R . . O8 O 0.08694(11) 0.58617(13) 0.55180(11) 0.0190(4) Uani 1 1 d . . . C21 C 0.09632(19) 0.6045(2) 0.64370(19) 0.0309(7) Uani 1 1 d . . . H21A H 0.1355 0.5646 0.6710 0.037 Uiso 1 1 calc R . . H21B H 0.0458 0.5941 0.6706 0.037 Uiso 1 1 calc R . . C22 C 0.1218(2) 0.6938(3) 0.6629(2) 0.0470(10) Uani 1 1 d . . . H22A H 0.1713 0.7051 0.6355 0.070 Uiso 1 1 calc R . . H22B H 0.1294 0.7016 0.7262 0.070 Uiso 1 1 calc R . . H22C H 0.0816 0.7337 0.6396 0.070 Uiso 1 1 calc R . . C23 C 0.27803(19) 0.4885(2) 0.5682(2) 0.0348(8) Uani 1 1 d . . . H23A H 0.2633 0.4432 0.6093 0.042 Uiso 1 1 calc R . . H23B H 0.3132 0.4619 0.5268 0.042 Uiso 1 1 calc R . . C24 C 0.3251(2) 0.5554(3) 0.6201(3) 0.0509(10) Uani 1 1 d . . . H24A H 0.3438 0.5990 0.5803 0.076 Uiso 1 1 calc R . . H24B H 0.3701 0.5281 0.6513 0.076 Uiso 1 1 calc R . . H24C H 0.2918 0.5825 0.6622 0.076 Uiso 1 1 calc R . . C25 C 0.0816(2) 0.4863(2) 0.2060(2) 0.0373(8) Uani 1 1 d . . . H25A H 0.1043 0.4280 0.2049 0.045 Uiso 1 1 calc R . . H25B H 0.0261 0.4819 0.1842 0.045 Uiso 1 1 calc R . . C26 C 0.1236(3) 0.5407(3) 0.1447(2) 0.0530(11) Uani 1 1 d . . . H26A H 0.1038 0.5995 0.1471 0.079 Uiso 1 1 calc R . . H26B H 0.1149 0.5184 0.0852 0.079 Uiso 1 1 calc R . . H26C H 0.1799 0.5402 0.1612 0.079 Uiso 1 1 calc R . . C27 C 0.06386(18) 0.8025(2) 0.4555(2) 0.0278(7) Uani 1 1 d . . . H27A H 0.1072 0.8258 0.4941 0.033 Uiso 1 1 calc R . . H27B H 0.0719 0.8233 0.3957 0.033 Uiso 1 1 calc R . . C28 C -0.0136(2) 0.8406(2) 0.4847(2) 0.0395(8) Uani 1 1 d . . . H28A H -0.0573 0.8197 0.4463 0.059 Uiso 1 1 calc R . . H28B H -0.0113 0.9032 0.4814 0.059 Uiso 1 1 calc R . . H28C H -0.0215 0.8233 0.5450 0.059 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 0.0147(2) 0.0183(2) 0.0198(2) 0.00220(18) 0.00149(16) -0.00064(17) Zn2 0.02026(16) 0.01747(18) 0.02640(17) -0.00136(14) 0.00272(13) 0.00012(13) Zn3 0.02095(16) 0.02199(18) 0.01862(15) 0.00081(13) 0.00289(12) -0.00075(13) Zn4 0.01658(15) 0.02264(19) 0.02253(16) 0.00095(13) -0.00112(12) 0.00099(13) O1 0.0167(9) 0.0208(11) 0.0207(9) 0.0035(8) 0.0012(7) 0.0007(8) C1 0.0237(15) 0.036(2) 0.0400(18) 0.0145(15) -0.0067(13) 0.0005(13) C2 0.040(2) 0.070(3) 0.054(2) 0.036(2) 0.0042(18) 0.017(2) O2 0.0165(9) 0.0215(11) 0.0262(10) 0.0002(8) 0.0036(8) -0.0029(8) C3 0.0181(13) 0.0258(17) 0.0368(16) 0.0002(14) 0.0054(12) -0.0067(12) C4 0.043(2) 0.037(2) 0.045(2) 0.0151(17) 0.0036(16) -0.0160(16) O3 0.0165(9) 0.0159(10) 0.0214(9) 0.0010(8) 0.0027(7) 0.0005(7) C5 0.0260(15) 0.0182(16) 0.0359(16) 0.0005(13) 0.0035(12) 0.0022(12) C6 0.054(2) 0.028(2) 0.060(2) 0.0000(18) 0.0276(19) 0.0090(17) O4 0.0188(9) 0.0234(11) 0.0190(9) -0.0011(8) 0.0016(7) 0.0004(8) C7 0.0357(17) 0.044(2) 0.0185(14) -0.0025(14) 0.0053(12) -0.0007(15) C8 0.043(2) 0.051(3) 0.0286(17) -0.0120(16) -0.0022(14) 0.0008(17) C9 0.0387(19) 0.0243(19) 0.058(2) -0.0096(17) -0.0071(16) 0.0020(15) C10 0.058(4) 0.027(3) 0.057(4) -0.007(3) -0.015(3) 0.007(2) C10X 0.040(7) 0.025(8) 0.056(12) -0.013(7) 0.005(7) 0.012(6) C11 0.0336(16) 0.0307(19) 0.0271(15) 0.0026(14) 0.0088(13) 0.0065(14) C12 0.042(2) 0.065(3) 0.0258(16) -0.0102(17) 0.0028(14) 0.0054(19) C13 0.0211(15) 0.038(2) 0.0389(18) 0.0025(15) -0.0032(13) 0.0041(13) C14 0.0258(16) 0.056(3) 0.0361(18) -0.0004(17) -0.0102(14) -0.0011(16) Zn5 0.0173(2) 0.0186(2) 0.0164(2) -0.00015(17) 0.00306(16) -0.00323(17) Zn6 0.01797(15) 0.02134(19) 0.02496(16) 0.00236(14) -0.00090(12) -0.00035(13) Zn7 0.02416(17) 0.02312(19) 0.01736(15) -0.00125(13) 0.00484(12) -0.00296(13) Zn8 0.01934(15) 0.01687(18) 0.02316(16) -0.00060(13) 0.00331(12) -0.00100(12) O5 0.0218(9) 0.0160(10) 0.0224(9) -0.0006(8) 0.0048(8) -0.0017(8) C15 0.0350(17) 0.0193(17) 0.0395(17) -0.0028(14) 0.0117(14) -0.0013(13) C16 0.0368(19) 0.029(2) 0.065(2) -0.0117(18) 0.0067(17) 0.0058(15) O6 0.0178(9) 0.0200(11) 0.0223(9) 0.0019(8) 0.0054(7) -0.0023(8) C17 0.0222(14) 0.0264(17) 0.0284(15) 0.0054(13) 0.0104(12) -0.0013(12) C18 0.0311(17) 0.037(2) 0.050(2) -0.0011(17) 0.0090(15) -0.0127(15) O7 0.0178(9) 0.0216(11) 0.0179(9) 0.0024(8) 0.0006(7) -0.0009(8) C19 0.0219(14) 0.038(2) 0.0291(15) 0.0055(14) -0.0055(12) 0.0029(13) C20 0.0356(18) 0.040(2) 0.0321(17) 0.0122(15) -0.0054(14) 0.0011(15) O8 0.0210(9) 0.0206(11) 0.0152(9) -0.0025(8) 0.0009(7) -0.0024(8) C21 0.0337(17) 0.039(2) 0.0206(14) -0.0054(14) 0.0026(12) -0.0119(14) C22 0.068(3) 0.043(2) 0.0297(17) -0.0096(16) 0.0002(17) -0.020(2) C23 0.0298(17) 0.032(2) 0.0412(18) 0.0036(15) -0.0098(14) 0.0054(14) C24 0.040(2) 0.055(3) 0.055(2) 0.009(2) -0.0223(18) -0.0089(18) C25 0.050(2) 0.039(2) 0.0235(15) -0.0068(15) 0.0089(14) -0.0116(17) C26 0.091(3) 0.042(2) 0.0266(17) 0.0006(17) 0.0172(19) -0.007(2) C27 0.0300(16) 0.0206(16) 0.0334(16) 0.0020(13) 0.0079(13) 0.0008(13) C28 0.0421(19) 0.0255(19) 0.052(2) 0.0045(16) 0.0132(16) 0.0074(15) _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 O4 2.1011(19) . ? Zn1 O3 2.1247(18) . ? Zn1 O1 2.1356(19) . ? Zn1 Zn4 3.1056(3) . ? Zn1 Zn2 3.1182(3) . ? Zn1 Zn3 3.1359(3) . ? Zn2 C9 1.964(3) . ? Zn2 O2 2.0619(19) . ? Zn2 O1 2.0643(19) . ? Zn2 O4 2.069(2) . ? Zn2 Zn4 3.0699(5) . ? Zn2 Zn3 3.0792(5) . ? Zn3 C11 1.968(3) . ? Zn3 O3 2.0583(19) . ? Zn3 O1 2.0619(19) . ? Zn3 O2 2.0828(19) . ? Zn3 Zn4 3.0669(4) . ? Zn4 C13 1.959(3) . ? Zn4 O2 2.055(2) . ? Zn4 O4 2.0633(19) . ? Zn4 O3 2.0645(19) . ? O1 C1 1.434(3) . ? C1 C2 1.460(5) . ? O2 C3 1.436(3) . ? C3 C4 1.503(5) . ? O3 C5 1.439(3) . ? C5 C6 1.488(4) . ? O4 C7 1.428(3) . ? C7 C8 1.488(4) . ? C9 C10X 1.448(11) . ? C9 C10 1.479(6) . ? C11 C12 1.525(5) . ? C13 C14 1.517(4) . ? Zn5 O5 2.1135(18) . ? Zn5 O7 2.1214(19) . ? Zn5 O8 2.1244(19) . ? Zn5 Zn7 3.0965(3) . ? Zn5 Zn8 3.1280(3) . ? Zn5 Zn6 3.1338(3) . ? Zn6 C23 1.963(3) . ? Zn6 O6 2.0542(19) . ? Zn6 O5 2.0681(19) . ? Zn6 O8 2.0777(19) . ? Zn6 Zn7 3.0586(5) . ? Zn6 Zn8 3.0818(5) . ? Zn7 C25 1.968(3) . ? Zn7 O7 2.0582(19) . ? Zn7 O5 2.0602(19) . ? Zn7 O6 2.0622(19) . ? Zn7 Zn8 3.0829(5) . ? Zn8 C27 1.966(3) . ? Zn8 O8 2.0559(19) . ? Zn8 O7 2.0623(19) . ? Zn8 O6 2.0874(19) . ? O5 C15 1.428(4) . ? C15 C16 1.492(4) . ? O6 C17 1.435(3) . ? C17 C18 1.496(4) . ? O7 C19 1.434(3) . ? C19 C20 1.498(4) . ? O8 C21 1.439(3) . ? C21 C22 1.486(5) . ? C23 C24 1.517(5) . ? C25 C26 1.482(5) . ? C27 C28 1.539(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 O4 Zn1 O4 180.0 . 3_665 ? O4 Zn1 O3 97.75(7) . 3_665 ? O4 Zn1 O3 82.25(7) . . ? O3 Zn1 O3 180.00(5) 3_665 . ? O4 Zn1 O1 81.93(7) . . ? O3 Zn1 O1 98.96(7) 3_665 . ? O3 Zn1 O1 81.05(7) . . ? O4 Zn1 O1 98.07(7) . 3_665 ? O4 Zn1 O1 81.93(7) 3_665 3_665 ? O3 Zn1 O1 81.04(7) 3_665 3_665 ? O3 Zn1 O1 98.95(7) . 3_665 ? O1 Zn1 O1 180.0 . 3_665 ? O4 Zn1 Zn4 41.31(5) . . ? O4 Zn1 Zn4 138.69(5) 3_665 . ? O3 Zn1 Zn4 138.59(5) 3_665 . ? O3 Zn1 Zn4 41.41(5) . . ? O1 Zn1 Zn4 83.55(5) . . ? O1 Zn1 Zn4 96.45(5) 3_665 . ? O4 Zn1 Zn4 138.69(5) . 3_665 ? O4 Zn1 Zn4 41.31(5) 3_665 3_665 ? O1 Zn1 Zn4 96.45(5) . 3_665 ? Zn4 Zn1 Zn4 180.0 . 3_665 ? O4 Zn1 Zn2 41.22(5) . . ? O4 Zn1 Zn2 138.78(5) 3_665 . ? O3 Zn1 Zn2 96.21(5) 3_665 . ? O3 Zn1 Zn2 83.79(5) . . ? O1 Zn1 Zn2 41.19(5) . . ? O1 Zn1 Zn2 138.81(5) 3_665 . ? Zn4 Zn1 Zn2 59.108(9) . . ? Zn4 Zn1 Zn2 120.893(9) 3_665 . ? O4 Zn1 Zn2 138.78(5) . 3_665 ? O4 Zn1 Zn2 41.22(5) 3_665 3_665 ? O3 Zn1 Zn2 83.79(5) 3_665 3_665 ? O3 Zn1 Zn2 96.21(5) . 3_665 ? Zn4 Zn1 Zn2 120.892(9) . 3_665 ? Zn4 Zn1 Zn2 59.107(9) 3_665 3_665 ? Zn2 Zn1 Zn2 180.0 . 3_665 ? O4 Zn1 Zn3 83.82(5) . . ? O4 Zn1 Zn3 96.18(5) 3_665 . ? O3 Zn1 Zn3 139.36(5) 3_665 . ? O3 Zn1 Zn3 40.64(5) . . ? O1 Zn1 Zn3 40.77(5) . . ? O1 Zn1 Zn3 139.23(5) 3_665 . ? Zn4 Zn1 Zn3 58.858(8) . . ? Zn4 Zn1 Zn3 121.142(8) 3_665 . ? Zn2 Zn1 Zn3 58.990(9) . . ? Zn2 Zn1 Zn3 121.011(9) 3_665 . ? O1 Zn1 Zn3 139.23(5) . 3_665 ? Zn4 Zn1 Zn3 58.857(8) 3_665 3_665 ? Zn2 Zn1 Zn3 58.988(9) 3_665 3_665 ? Zn3 Zn1 Zn3 180.0 . 3_665 ? C9 Zn2 O2 132.01(12) . . ? C9 Zn2 O1 130.29(12) . . ? O2 Zn2 O1 83.67(7) . . ? C9 Zn2 O4 126.13(13) . . ? O2 Zn2 O4 83.40(8) . . ? O1 Zn2 O4 84.45(7) . . ? C9 Zn2 Zn4 143.92(10) . . ? O2 Zn2 Zn4 41.70(5) . . ? O1 Zn2 Zn4 85.61(5) . . ? O4 Zn2 Zn4 41.95(5) . . ? C9 Zn2 Zn3 148.05(12) . . ? O2 Zn2 Zn3 42.28(5) . . ? O1 Zn2 Zn3 41.70(5) . . ? O4 Zn2 Zn3 85.81(5) . . ? Zn4 Zn2 Zn3 59.835(11) . . ? C9 Zn2 Zn1 141.47(11) . . ? O2 Zn2 Zn1 86.36(6) . . ? O1 Zn2 Zn1 42.94(5) . . ? O4 Zn2 Zn1 42.00(5) . . ? Zn4 Zn2 Zn1 60.243(9) . . ? Zn3 Zn2 Zn1 60.793(9) . . ? C11 Zn3 O3 133.09(11) . . ? C11 Zn3 O1 130.89(11) . . ? O3 Zn3 O1 84.42(7) . . ? C11 Zn3 O2 124.36(11) . . ? O3 Zn3 O2 83.52(8) . . ? O1 Zn3 O2 83.22(7) . . ? C11 Zn3 Zn4 142.75(9) . . ? O3 Zn3 Zn4 42.01(5) . . ? O1 Zn3 Zn4 85.73(5) . . ? O2 Zn3 Zn4 41.82(6) . . ? C11 Zn3 Zn2 140.69(10) . . ? O3 Zn3 Zn2 85.86(5) . . ? O1 Zn3 Zn2 41.76(5) . . ? O2 Zn3 Zn2 41.76(5) . . ? Zn4 Zn3 Zn2 59.931(11) . . ? C11 Zn3 Zn1 150.06(10) . . ? O3 Zn3 Zn1 42.25(5) . . ? O1 Zn3 Zn1 42.56(5) . . ? O2 Zn3 Zn1 85.54(5) . . ? Zn4 Zn3 Zn1 60.078(8) . . ? Zn2 Zn3 Zn1 60.218(8) . . ? C13 Zn4 O2 130.22(11) . . ? C13 Zn4 O4 129.64(11) . . ? O2 Zn4 O4 83.71(8) . . ? C13 Zn4 O3 128.07(12) . . ? O2 Zn4 O3 84.06(8) . . ? O4 Zn4 O3 84.65(7) . . ? C13 Zn4 Zn3 144.11(10) . . ? O2 Zn4 Zn3 42.52(5) . . ? O4 Zn4 Zn3 86.23(5) . . ? O3 Zn4 Zn3 41.86(5) . . ? C13 Zn4 Zn2 145.92(11) . . ? O2 Zn4 Zn2 41.87(5) . . ? O4 Zn4 Zn2 42.10(5) . . ? O3 Zn4 Zn2 86.01(5) . . ? Zn3 Zn4 Zn2 60.234(11) . . ? C13 Zn4 Zn1 142.97(10) . . ? O2 Zn4 Zn1 86.80(5) . . ? O4 Zn4 Zn1 42.24(5) . . ? O3 Zn4 Zn1 42.91(5) . . ? Zn3 Zn4 Zn1 61.063(8) . . ? Zn2 Zn4 Zn1 60.649(8) . . ? C1 O1 Zn3 122.59(18) . . ? C1 O1 Zn2 116.35(19) . . ? Zn3 O1 Zn2 96.53(7) . . ? C1 O1 Zn1 122.77(17) . . ? Zn3 O1 Zn1 96.66(8) . . ? Zn2 O1 Zn1 95.86(7) . . ? O1 C1 C2 114.9(3) . . ? C3 O2 Zn4 119.13(17) . . ? C3 O2 Zn2 121.90(18) . . ? Zn4 O2 Zn2 96.43(8) . . ? C3 O2 Zn3 121.59(17) . . ? Zn4 O2 Zn3 95.66(8) . . ? Zn2 O2 Zn3 95.96(8) . . ? O2 C3 C4 111.5(2) . . ? C5 O3 Zn3 124.01(17) . . ? C5 O3 Zn4 116.19(16) . . ? Zn3 O3 Zn4 96.13(8) . . ? C5 O3 Zn1 121.52(16) . . ? Zn3 O3 Zn1 97.11(8) . . ? Zn4 O3 Zn1 95.68(8) . . ? O3 C5 C6 113.5(3) . . ? C7 O4 Zn4 119.29(18) . . ? C7 O4 Zn2 119.32(19) . . ? Zn4 O4 Zn2 95.95(8) . . ? C7 O4 Zn1 123.10(17) . . ? Zn4 O4 Zn1 96.45(8) . . ? Zn2 O4 Zn1 96.78(8) . . ? O4 C7 C8 112.9(3) . . ? C10X C9 Zn2 122.7(6) . . ? C10 C9 Zn2 119.5(3) . . ? C12 C11 Zn3 117.2(2) . . ? C14 C13 Zn4 115.9(2) . . ? O5 Zn5 O5 180.0 . 3_566 ? O5 Zn5 O7 97.64(7) . 3_566 ? O5 Zn5 O7 82.36(7) . . ? O7 Zn5 O7 180.0 3_566 . ? O5 Zn5 O8 98.26(7) . 3_566 ? O7 Zn5 O8 98.82(7) . 3_566 ? O5 Zn5 O8 81.74(7) . . ? O7 Zn5 O8 81.18(7) . . ? O8 Zn5 O8 180.00(8) 3_566 . ? O5 Zn5 Zn7 138.55(5) . 3_566 ? O7 Zn5 Zn7 138.58(5) . 3_566 ? O8 Zn5 Zn7 83.68(5) 3_566 3_566 ? O8 Zn5 Zn7 96.32(5) . 3_566 ? O5 Zn5 Zn7 41.45(5) . . ? O7 Zn5 Zn7 41.42(5) . . ? O8 Zn5 Zn7 96.32(5) 3_566 . ? O8 Zn5 Zn7 83.68(5) . . ? Zn7 Zn5 Zn7 180.0 3_566 . ? O5 Zn5 Zn8 84.21(5) . . ? O7 Zn5 Zn8 139.10(5) 3_566 . ? O7 Zn5 Zn8 40.90(5) . . ? O8 Zn5 Zn8 139.27(5) 3_566 . ? O8 Zn5 Zn8 40.73(5) . . ? Zn7 Zn5 Zn8 120.625(9) 3_566 . ? Zn7 Zn5 Zn8 59.375(9) . . ? O5 Zn5 Zn8 95.79(5) . 3_566 ? Zn7 Zn5 Zn8 120.626(9) . 3_566 ? Zn8 Zn5 Zn8 180.0 . 3_566 ? O5 Zn5 Zn6 40.91(5) . . ? O5 Zn5 Zn6 139.09(5) 3_566 . ? O7 Zn5 Zn6 96.58(5) 3_566 . ? O7 Zn5 Zn6 83.42(5) . . ? O8 Zn5 Zn6 138.79(5) 3_566 . ? O8 Zn5 Zn6 41.21(5) . . ? Zn7 Zn5 Zn6 121.201(9) 3_566 . ? Zn7 Zn5 Zn6 58.799(8) . . ? Zn8 Zn5 Zn6 58.964(9) . . ? Zn8 Zn5 Zn6 121.036(9) 3_566 . ? O5 Zn5 Zn6 139.09(5) . 3_566 ? O8 Zn5 Zn6 41.21(5) 3_566 3_566 ? Zn7 Zn5 Zn6 58.800(9) 3_566 3_566 ? Zn7 Zn5 Zn6 121.200(8) . 3_566 ? Zn8 Zn5 Zn6 121.035(9) . 3_566 ? Zn8 Zn5 Zn6 58.965(9) 3_566 3_566 ? Zn6 Zn5 Zn6 180.0 . 3_566 ? C23 Zn6 O6 133.90(12) . . ? C23 Zn6 O5 128.70(12) . . ? O6 Zn6 O5 83.92(8) . . ? C23 Zn6 O8 125.82(12) . . ? O6 Zn6 O8 83.50(7) . . ? O5 Zn6 O8 83.97(7) . . ? C23 Zn6 Zn7 148.63(11) . . ? O6 Zn6 Zn7 42.11(5) . . ? O5 Zn6 Zn7 42.09(5) . . ? O8 Zn6 Zn7 85.40(5) . . ? C23 Zn6 Zn8 144.68(11) . . ? O6 Zn6 Zn8 42.33(5) . . ? O5 Zn6 Zn8 86.14(6) . . ? O8 Zn6 Zn8 41.53(5) . . ? Zn7 Zn6 Zn8 60.273(11) . . ? C23 Zn6 Zn5 140.01(11) . . ? O6 Zn6 Zn5 86.03(5) . . ? O5 Zn6 Zn5 42.01(5) . . ? O8 Zn6 Zn5 42.35(5) . . ? Zn7 Zn6 Zn5 59.991(8) . . ? Zn8 Zn6 Zn5 60.424(8) . . ? C25 Zn7 O7 129.71(13) . . ? C25 Zn7 O5 126.57(13) . . ? O7 Zn7 O5 85.22(7) . . ? C25 Zn7 O6 131.35(11) . . ? O7 Zn7 O6 83.70(7) . . ? O5 Zn7 O6 83.91(8) . . ? C25 Zn7 Zn6 143.83(12) . . ? O7 Zn7 Zn6 86.39(5) . . ? O5 Zn7 Zn6 42.29(5) . . ? O6 Zn7 Zn6 41.91(5) . . ? C25 Zn7 Zn8 147.18(12) . . ? O7 Zn7 Zn8 41.62(5) . . ? O5 Zn7 Zn8 86.24(5) . . ? O6 Zn7 Zn8 42.33(5) . . ? Zn6 Zn7 Zn8 60.236(11) . . ? C25 Zn7 Zn5 141.70(10) . . ? O7 Zn7 Zn5 42.99(5) . . ? O5 Zn7 Zn5 42.77(5) . . ? O6 Zn7 Zn5 86.89(5) . . ? Zn6 Zn7 Zn5 61.211(8) . . ? Zn8 Zn7 Zn5 60.822(8) . . ? C27 Zn8 O8 133.87(11) . . ? C27 Zn8 O7 128.83(11) . . ? O8 Zn8 O7 84.26(7) . . ? C27 Zn8 O6 126.27(10) . . ? O8 Zn8 O6 83.22(7) . . ? O7 Zn8 O6 82.98(7) . . ? C27 Zn8 Zn6 144.95(9) . . ? O8 Zn8 Zn6 42.06(5) . . ? O7 Zn8 Zn6 85.70(5) . . ? O6 Zn8 Zn6 41.51(5) . . ? C27 Zn8 Zn7 140.94(9) . . ? O8 Zn8 Zn7 85.12(5) . . ? O7 Zn8 Zn7 41.52(5) . . ? O6 Zn8 Zn7 41.71(5) . . ? Zn6 Zn8 Zn7 59.491(11) . . ? C27 Zn8 Zn5 147.92(9) . . ? O8 Zn8 Zn5 42.40(5) . . ? O7 Zn8 Zn5 42.34(5) . . ? O6 Zn8 Zn5 85.64(5) . . ? Zn6 Zn8 Zn5 60.612(9) . . ? Zn7 Zn8 Zn5 59.803(9) . . ? C15 O5 Zn7 115.91(18) . . ? C15 O5 Zn6 123.29(18) . . ? Zn7 O5 Zn6 95.61(8) . . ? C15 O5 Zn5 122.82(16) . . ? Zn7 O5 Zn5 95.78(8) . . ? Zn6 O5 Zn5 97.08(8) . . ? O5 C15 C16 112.8(3) . . ? C17 O6 Zn6 124.09(17) . . ? C17 O6 Zn7 117.97(16) . . ? Zn6 O6 Zn7 95.98(8) . . ? C17 O6 Zn8 120.44(18) . . ? Zn6 O6 Zn8 96.16(7) . . ? Zn7 O6 Zn8 95.96(7) . . ? O6 C17 C18 112.3(2) . . ? C19 O7 Zn7 117.87(17) . . ? C19 O7 Zn8 119.03(19) . . ? Zn7 O7 Zn8 96.87(7) . . ? C19 O7 Zn5 124.75(17) . . ? Zn7 O7 Zn5 95.60(8) . . ? Zn8 O7 Zn5 96.77(7) . . ? O7 C19 C20 112.7(2) . . ? C21 O8 Zn8 124.75(19) . . ? C21 O8 Zn6 114.27(18) . . ? Zn8 O8 Zn6 96.41(7) . . ? C21 O8 Zn5 121.99(17) . . ? Zn8 O8 Zn5 96.87(7) . . ? Zn6 O8 Zn5 96.45(8) . . ? O8 C21 C22 113.4(3) . . ? C24 C23 Zn6 118.6(3) . . ? C26 C25 Zn7 116.2(3) . . ? C28 C27 Zn8 117.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.722 _refine_diff_density_min -0.546 _refine_diff_density_rms 0.095 #===END data_6 _database_code_depnum_ccdc_archive 'CCDC 790914' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H43 Cl N8 Zn4' _chemical_formula_sum 'C14 H43 Cl N8 Zn4' _chemical_formula_weight 620.49 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 _symmetry_space_group_name_Hall '-P 2ybc' 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 17.7876(19) _cell_length_b 11.0855(13) _cell_length_c 14.1353(14) _cell_angle_alpha 90.00 _cell_angle_beta 108.948(5) _cell_angle_gamma 90.00 _cell_volume 2636.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 43525 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 3.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.496 _exptl_absorpt_correction_T_max 0.731 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 12549 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 22.50 _reflns_number_total 3427 _reflns_number_gt 2313 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0758P)^2^+27.2731P] 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 3427 _refine_ls_number_parameters 306 _refine_ls_number_restraints 271 _refine_ls_R_factor_all 0.1254 _refine_ls_R_factor_gt 0.0840 _refine_ls_wR_factor_ref 0.2279 _refine_ls_wR_factor_gt 0.1910 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.33676(9) 0.98882(15) 0.42481(10) 0.0790(5) Uani 1 1 d D . . Cl1 Cl 0.4174(2) 0.9805(4) 0.3303(2) 0.0969(12) Uani 1 1 d . . . Zn2 Zn 0.33209(11) 0.95144(18) 0.64731(11) 0.0967(7) Uani 1 1 d D . . C9 C 0.3747(11) 0.9140(18) 0.7948(9) 0.124(6) Uani 1 1 d D . . H9A H 0.3320 0.9280 0.8243 0.149 Uiso 1 1 calc R . . H9B H 0.3890 0.8274 0.8033 0.149 Uiso 1 1 calc R . . C10 C 0.4433(12) 0.9842(16) 0.8497(11) 0.133(7) Uani 1 1 d D . . H10A H 0.4610 0.9597 0.9201 0.199 Uiso 1 1 calc R A . H10B H 0.4292 1.0700 0.8447 0.199 Uiso 1 1 calc R . . H10C H 0.4862 0.9707 0.8216 0.199 Uiso 1 1 calc R . . Zn3 Zn 0.22095(11) 1.17867(17) 0.47660(14) 0.1032(7) Uani 1 1 d DU . . C11 C 0.1719(13) 1.3454(16) 0.4737(19) 0.182(9) Uani 1 1 d DU . . H11A H 0.1863 1.3758 0.5432 0.218 Uiso 1 1 calc R . . H11B H 0.1958 1.4007 0.4363 0.218 Uiso 1 1 calc R . . C12 C 0.0867(15) 1.350(3) 0.429(3) 0.32(2) Uani 1 1 d DU . . H12A H 0.0688 1.4339 0.4266 0.483 Uiso 1 1 calc R A . H12B H 0.0620 1.3022 0.4694 0.483 Uiso 1 1 calc R . . H12C H 0.0714 1.3171 0.3612 0.483 Uiso 1 1 calc R . . Zn4 Zn 0.17531(10) 0.87087(19) 0.43000(13) 0.1021(7) Uani 1 1 d DU . . C13 C 0.0760(19) 0.766(4) 0.386(3) 0.135(10) Uani 0.66(3) 1 d PDU A 1 H13A H 0.0293 0.8192 0.3584 0.162 Uiso 0.66(3) 1 calc PR A 1 H13B H 0.0793 0.7125 0.3318 0.162 Uiso 0.66(3) 1 calc PR A 1 C14 C 0.0627(17) 0.693(3) 0.463(2) 0.150(12) Uani 0.66(3) 1 d PDU A 1 H14A H 0.0165 0.6403 0.4339 0.224 Uiso 0.66(3) 1 calc PR A 1 H14B H 0.0527 0.7446 0.5141 0.224 Uiso 0.66(3) 1 calc PR A 1 H14C H 0.1097 0.6427 0.4947 0.224 Uiso 0.66(3) 1 calc PR A 1 C13X C 0.092(4) 0.741(6) 0.377(6) 0.130(15) Uani 0.34(3) 1 d PDU A 2 H13C H 0.0876 0.6925 0.4340 0.156 Uiso 0.34(3) 1 calc PR A 2 H13D H 0.0398 0.7794 0.3443 0.156 Uiso 0.34(3) 1 calc PR A 2 C14X C 0.109(3) 0.660(4) 0.306(4) 0.16(2) Uani 0.34(3) 1 d PDU A 2 H14D H 0.0610 0.6170 0.2683 0.234 Uiso 0.34(3) 1 calc PR A 2 H14E H 0.1502 0.6023 0.3423 0.234 Uiso 0.34(3) 1 calc PR A 2 H14F H 0.1288 0.7074 0.2602 0.234 Uiso 0.34(3) 1 calc PR A 2 N1 N 0.2930(5) 0.8309(9) 0.4544(7) 0.084(3) Uani 1 1 d D A . H1 H 0.2976 0.7718 0.4100 0.101 Uiso 1 1 calc R . . N2 N 0.3341(6) 0.7944(9) 0.5560(7) 0.084(3) Uani 1 1 d D A . C1 C 0.4192(7) 0.7696(14) 0.5694(10) 0.098(5) Uani 1 1 d D . . H1A H 0.4229 0.7057 0.5231 0.148 Uiso 1 1 calc R A . H1B H 0.4464 0.7436 0.6384 0.148 Uiso 1 1 calc R . . H1C H 0.4445 0.8431 0.5556 0.148 Uiso 1 1 calc R . . C2 C 0.2992(8) 0.6801(12) 0.5802(10) 0.097(4) Uani 1 1 d D . . H2A H 0.2434 0.6937 0.5742 0.146 Uiso 1 1 calc R A . H2B H 0.3288 0.6554 0.6488 0.146 Uiso 1 1 calc R . . H2C H 0.3026 0.6166 0.5336 0.146 Uiso 1 1 calc R . . N3 N 0.3752(6) 1.0625(9) 0.5623(6) 0.082(3) Uani 1 1 d D A . H3 H 0.4304 1.0613 0.5862 0.099 Uiso 1 1 calc R . . N4 N 0.3477(6) 1.1851(10) 0.5576(8) 0.095(4) Uani 1 1 d D A . C3 C 0.3744(10) 1.2408(14) 0.6598(10) 0.115(5) Uani 1 1 d D . . H3A H 0.3581 1.1892 0.7061 0.172 Uiso 1 1 calc R A . H3B H 0.3500 1.3206 0.6569 0.172 Uiso 1 1 calc R . . H3C H 0.4324 1.2489 0.6834 0.172 Uiso 1 1 calc R . . C4 C 0.3845(9) 1.2592(14) 0.4947(11) 0.115(5) Uani 1 1 d D . . H4A H 0.4415 1.2690 0.5302 0.172 Uiso 1 1 calc R A . H4B H 0.3591 1.3387 0.4822 0.172 Uiso 1 1 calc R . . H4C H 0.3769 1.2182 0.4309 0.172 Uiso 1 1 calc R . . N5 N 0.2356(6) 1.0847(10) 0.3591(7) 0.095(4) Uani 1 1 d D A . H5 H 0.2425 1.1373 0.3113 0.114 Uiso 1 1 calc R . . N6 N 0.1712(7) 1.0033(10) 0.3148(8) 0.101(4) Uani 1 1 d D A . C5 C 0.0928(8) 1.0654(18) 0.2739(12) 0.135(7) Uani 1 1 d D . . H5A H 0.0770 1.0978 0.3292 0.202 Uiso 1 1 calc R A . H5B H 0.0527 1.0076 0.2357 0.202 Uiso 1 1 calc R . . H5C H 0.0972 1.1315 0.2300 0.202 Uiso 1 1 calc R . . C6 C 0.1865(10) 0.9369(16) 0.2309(10) 0.129(6) Uani 1 1 d D . . H6A H 0.1873 0.9941 0.1784 0.194 Uiso 1 1 calc R A . H6B H 0.1443 0.8773 0.2034 0.194 Uiso 1 1 calc R . . H6C H 0.2379 0.8957 0.2559 0.194 Uiso 1 1 calc R . . N7 N 0.192(2) 1.0178(12) 0.5246(14) 0.131(7) Uani 0.566(16) 1 d PDU A 1 H7 H 0.1382 1.0350 0.5109 0.157 Uiso 0.566(16) 1 calc PR A 1 N8 N 0.2095(10) 1.005(2) 0.6277(15) 0.142(7) Uani 0.566(16) 1 d PDU A 1 C7 C 0.199(3) 1.108(3) 0.690(3) 0.180(16) Uani 0.566(16) 1 d PDU A 1 H7A H 0.2291 1.1775 0.6786 0.269 Uiso 0.566(16) 1 calc PR A 1 H7B H 0.2192 1.0850 0.7606 0.269 Uiso 0.566(16) 1 calc PR A 1 H7C H 0.1428 1.1284 0.6712 0.269 Uiso 0.566(16) 1 calc PR A 1 C8 C 0.1624(19) 0.900(3) 0.649(2) 0.141(11) Uani 0.566(16) 1 d PDU A 1 H8A H 0.1689 0.8294 0.6115 0.212 Uiso 0.566(16) 1 calc PR A 1 H8B H 0.1061 0.9225 0.6293 0.212 Uiso 0.566(16) 1 calc PR A 1 H8C H 0.1819 0.8822 0.7210 0.212 Uiso 0.566(16) 1 calc PR A 1 N7X N 0.2121(9) 0.943(3) 0.5697(13) 0.129(7) Uani 0.434(16) 1 d PDU A 2 H7X H 0.1901 0.8948 0.6079 0.154 Uiso 0.434(16) 1 calc PR A 2 N8X N 0.1742(17) 1.056(2) 0.5617(19) 0.134(7) Uani 0.434(16) 1 d PDU A 2 C7X C 0.194(4) 1.118(5) 0.661(3) 0.164(13) Uani 0.434(16) 1 d PDU A 2 H7D H 0.2522 1.1236 0.6911 0.246 Uiso 0.434(16) 1 calc PR A 2 H7E H 0.1728 1.0711 0.7054 0.246 Uiso 0.434(16) 1 calc PR A 2 H7F H 0.1712 1.1988 0.6520 0.246 Uiso 0.434(16) 1 calc PR A 2 C8X C 0.0854(16) 1.042(4) 0.525(3) 0.154(13) Uani 0.434(16) 1 d PDU A 2 H8D H 0.0688 1.0054 0.4576 0.231 Uiso 0.434(16) 1 calc PR A 2 H8E H 0.0603 1.1207 0.5215 0.231 Uiso 0.434(16) 1 calc PR A 2 H8F H 0.0692 0.9890 0.5703 0.231 Uiso 0.434(16) 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 0.0726(10) 0.1031(13) 0.0568(8) 0.0032(8) 0.0149(7) -0.0020(9) Cl1 0.084(2) 0.136(3) 0.070(2) 0.004(2) 0.0240(18) -0.003(2) Zn2 0.0920(12) 0.1312(16) 0.0623(9) 0.0062(9) 0.0186(8) 0.0024(11) C9 0.157(17) 0.153(16) 0.067(9) -0.003(10) 0.042(10) 0.003(14) C10 0.19(2) 0.126(15) 0.064(9) -0.004(9) 0.012(11) -0.010(14) Zn3 0.0986(14) 0.1000(14) 0.1063(13) -0.0005(10) 0.0271(10) 0.0134(10) C11 0.175(18) 0.145(11) 0.22(2) 0.012(15) 0.053(17) 0.095(15) C12 0.20(2) 0.25(3) 0.43(5) -0.06(3) -0.02(3) 0.14(2) Zn4 0.0795(12) 0.1261(16) 0.0942(12) -0.0038(11) 0.0191(9) -0.0106(11) C13 0.077(17) 0.14(2) 0.17(2) 0.020(15) 0.023(16) -0.014(15) C14 0.11(2) 0.15(3) 0.17(3) 0.006(19) 0.032(19) -0.037(16) C13X 0.07(3) 0.14(3) 0.18(3) 0.016(19) 0.04(2) -0.019(19) C14X 0.09(3) 0.12(4) 0.26(5) -0.04(3) 0.05(3) -0.04(3) N1 0.074(7) 0.103(9) 0.067(6) 0.005(6) 0.011(5) -0.001(6) N2 0.085(8) 0.095(9) 0.063(6) 0.007(6) 0.010(6) -0.002(6) C1 0.091(11) 0.111(12) 0.073(9) 0.016(8) -0.001(7) -0.009(9) C2 0.101(11) 0.096(11) 0.083(9) 0.013(8) 0.014(8) 0.008(9) N3 0.074(7) 0.096(9) 0.071(7) -0.001(6) 0.016(5) -0.005(6) N4 0.094(9) 0.091(9) 0.090(8) 0.000(7) 0.013(7) -0.010(7) C3 0.138(14) 0.108(12) 0.089(10) -0.035(9) 0.024(10) -0.012(11) C4 0.099(12) 0.115(13) 0.119(13) 0.004(11) 0.021(10) 0.001(10) N5 0.094(9) 0.117(10) 0.070(7) 0.000(7) 0.019(6) -0.001(8) N6 0.097(9) 0.124(10) 0.068(7) -0.008(7) 0.006(6) 0.012(8) C5 0.087(12) 0.181(19) 0.115(13) 0.015(13) 0.005(10) 0.035(12) C6 0.145(16) 0.150(16) 0.074(10) -0.010(10) 0.008(10) -0.006(13) N7 0.180(19) 0.135(9) 0.107(11) -0.002(8) 0.087(14) -0.015(13) N8 0.196(19) 0.137(16) 0.108(11) -0.002(8) 0.071(15) 0.003(14) C7 0.24(4) 0.20(3) 0.14(2) -0.02(2) 0.11(3) 0.04(3) C8 0.14(3) 0.18(2) 0.14(2) 0.053(19) 0.09(2) 0.034(19) N7X 0.173(19) 0.145(12) 0.084(12) 0.012(10) 0.064(15) 0.019(14) N8X 0.153(16) 0.157(13) 0.119(16) -0.009(9) 0.080(15) 0.016(14) C7X 0.22(3) 0.18(3) 0.114(19) -0.002(17) 0.07(2) 0.05(3) C8X 0.149(17) 0.18(4) 0.18(3) -0.03(3) 0.12(2) 0.000(17) _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 N3 2.012(8) . ? Zn1 N1 2.014(9) . ? Zn1 N5 2.036(9) . ? Zn1 Cl1 2.257(4) . ? Zn2 C9 2.017(12) . ? Zn2 N3 2.036(9) . ? Zn2 N7X 2.061(14) . ? Zn2 N2 2.175(10) . ? Zn2 N8 2.188(15) . ? C9 C10 1.44(2) . ? Zn3 N7 2.033(12) . ? Zn3 C11 2.039(14) . ? Zn3 N5 2.047(9) . ? Zn3 N8X 2.154(16) . ? Zn3 N4 2.173(10) . ? C11 C12 1.44(2) . ? Zn4 N7X 2.031(13) . ? Zn4 C13X 2.031(18) . ? Zn4 C13 2.035(16) . ? Zn4 N1 2.056(9) . ? Zn4 N7 2.067(12) . ? Zn4 N6 2.176(10) . ? C13 C14 1.44(3) . ? C13X C14X 1.44(3) . ? N1 N2 1.441(11) . ? N2 C1 1.490(13) . ? N2 C2 1.499(13) . ? N3 N4 1.438(12) . ? N4 C3 1.500(13) . ? N4 C4 1.507(14) . ? N5 N6 1.433(13) . ? N6 C5 1.492(14) . ? N6 C6 1.495(14) . ? N7 N8 1.395(16) . ? N8 C7 1.487(17) . ? N8 C8 1.515(17) . ? N7X N8X 1.409(17) . ? N8X C7X 1.500(18) . ? N8X C8X 1.502(18) . ? 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 N3 Zn1 N1 100.6(4) . . ? N3 Zn1 N5 101.6(4) . . ? N1 Zn1 N5 101.8(4) . . ? N3 Zn1 Cl1 120.4(3) . . ? N1 Zn1 Cl1 116.8(3) . . ? N5 Zn1 Cl1 112.9(3) . . ? C9 Zn2 N3 130.3(6) . . ? C9 Zn2 N7X 121.2(9) . . ? N3 Zn2 N7X 103.7(9) . . ? C9 Zn2 N2 112.1(6) . . ? N3 Zn2 N2 93.0(4) . . ? N7X Zn2 N2 82.0(6) . . ? C9 Zn2 N8 102.2(7) . . ? N3 Zn2 N8 108.2(7) . . ? N7X Zn2 N8 29.3(7) . . ? N2 Zn2 N8 110.4(7) . . ? C10 C9 Zn2 114.4(12) . . ? N7 Zn3 C11 130.4(11) . . ? N7 Zn3 N5 86.4(5) . . ? C11 Zn3 N5 127.7(8) . . ? N7 Zn3 N8X 22.1(8) . . ? C11 Zn3 N8X 110.1(10) . . ? N5 Zn3 N8X 107.8(8) . . ? N7 Zn3 N4 100.7(10) . . ? C11 Zn3 N4 110.2(7) . . ? N5 Zn3 N4 93.4(4) . . ? N8X Zn3 N4 104.4(9) . . ? C12 C11 Zn3 115.0(16) . . ? N7X Zn4 C13X 127(2) . . ? N7X Zn4 C13 119.5(14) . . ? C13X Zn4 C13 13(3) . . ? N7X Zn4 N1 86.1(6) . . ? C13X Zn4 N1 119(2) . . ? C13 Zn4 N1 131.6(14) . . ? N7X Zn4 N7 29.3(9) . . ? C13X Zn4 N7 137.2(17) . . ? C13 Zn4 N7 125.0(15) . . ? N1 Zn4 N7 97.9(10) . . ? N7X Zn4 N6 112.6(10) . . ? C13X Zn4 N6 111(3) . . ? C13 Zn4 N6 110.1(12) . . ? N1 Zn4 N6 93.2(4) . . ? N7 Zn4 N6 85.1(5) . . ? C14 C13 Zn4 116(2) . . ? C14X C13X Zn4 113(2) . . ? N2 N1 Zn1 110.2(7) . . ? N2 N1 Zn4 112.8(7) . . ? Zn1 N1 Zn4 102.7(4) . . ? N1 N2 C1 110.2(9) . . ? N1 N2 C2 110.6(9) . . ? C1 N2 C2 107.1(10) . . ? N1 N2 Zn2 105.4(7) . . ? C1 N2 Zn2 106.5(8) . . ? C2 N2 Zn2 116.9(8) . . ? N4 N3 Zn1 109.6(7) . . ? N4 N3 Zn2 114.3(7) . . ? Zn1 N3 Zn2 104.5(4) . . ? N3 N4 C3 110.3(10) . . ? N3 N4 C4 109.7(10) . . ? C3 N4 C4 106.4(11) . . ? N3 N4 Zn3 105.8(7) . . ? C3 N4 Zn3 118.0(9) . . ? C4 N4 Zn3 106.4(8) . . ? N6 N5 Zn1 109.5(7) . . ? N6 N5 Zn3 112.3(7) . . ? Zn1 N5 Zn3 102.8(4) . . ? N5 N6 C5 113.2(11) . . ? N5 N6 C6 109.3(11) . . ? C5 N6 C6 107.9(10) . . ? N5 N6 Zn4 105.7(7) . . ? C5 N6 Zn4 113.7(10) . . ? C6 N6 Zn4 106.9(9) . . ? N8 N7 Zn3 116.4(13) . . ? N8 N7 Zn4 122.0(13) . . ? Zn3 N7 Zn4 118.3(7) . . ? N7 N8 C7 121(2) . . ? N7 N8 C8 109.8(17) . . ? C7 N8 C8 106.5(18) . . ? N7 N8 Zn2 92.2(17) . . ? C7 N8 Zn2 116(2) . . ? C8 N8 Zn2 111.2(16) . . ? N8X N7X Zn4 106.1(16) . . ? N8X N7X Zn2 112.8(18) . . ? Zn4 N7X Zn2 119.1(9) . . ? N7X N8X C7X 112(2) . . ? N7X N8X C8X 110.8(19) . . ? C7X N8X C8X 106(2) . . ? N7X N8X Zn3 110.2(19) . . ? C7X N8X Zn3 102(3) . . ? C8X N8X Zn3 115(2) . . ? 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 N3 Zn2 C9 C10 5.3(19) . . . . ? N7X Zn2 C9 C10 -146.0(15) . . . . ? N2 Zn2 C9 C10 120.0(14) . . . . ? N8 Zn2 C9 C10 -121.8(16) . . . . ? N7 Zn3 C11 C12 -50(3) . . . . ? N5 Zn3 C11 C12 74(3) . . . . ? N8X Zn3 C11 C12 -60(3) . . . . ? N4 Zn3 C11 C12 -175(2) . . . . ? N7X Zn4 C13 C14 -34(4) . . . . ? C13X Zn4 C13 C14 96(18) . . . . ? N1 Zn4 C13 C14 79(3) . . . . ? N7 Zn4 C13 C14 -69(4) . . . . ? N6 Zn4 C13 C14 -167(3) . . . . ? N7X Zn4 C13X C14X -145(5) . . . . ? C13 Zn4 C13X C14X 158(23) . . . . ? N1 Zn4 C13X C14X -36(8) . . . . ? N7 Zn4 C13X C14X 177(4) . . . . ? N6 Zn4 C13X C14X 71(7) . . . . ? N3 Zn1 N1 N2 -27.9(8) . . . . ? N5 Zn1 N1 N2 -132.3(7) . . . . ? Cl1 Zn1 N1 N2 104.4(7) . . . . ? N3 Zn1 N1 Zn4 92.5(5) . . . . ? N5 Zn1 N1 Zn4 -11.9(5) . . . . ? Cl1 Zn1 N1 Zn4 -135.2(3) . . . . ? N7X Zn4 N1 N2 37.4(12) . . . . ? C13X Zn4 N1 N2 -94(3) . . . . ? C13 Zn4 N1 N2 -89.5(17) . . . . ? N7 Zn4 N1 N2 64.3(9) . . . . ? N6 Zn4 N1 N2 149.8(8) . . . . ? N7X Zn4 N1 Zn1 -81.2(10) . . . . ? C13X Zn4 N1 Zn1 148(3) . . . . ? C13 Zn4 N1 Zn1 151.9(15) . . . . ? N7 Zn4 N1 Zn1 -54.3(6) . . . . ? N6 Zn4 N1 Zn1 31.2(5) . . . . ? Zn1 N1 N2 C1 -64.6(11) . . . . ? Zn4 N1 N2 C1 -178.7(8) . . . . ? Zn1 N1 N2 C2 177.2(8) . . . . ? Zn4 N1 N2 C2 63.1(11) . . . . ? Zn1 N1 N2 Zn2 49.9(7) . . . . ? Zn4 N1 N2 Zn2 -64.2(7) . . . . ? C9 Zn2 N2 N1 172.8(8) . . . . ? N3 Zn2 N2 N1 -51.1(7) . . . . ? N7X Zn2 N2 N1 52.4(10) . . . . ? N8 Zn2 N2 N1 59.6(9) . . . . ? C9 Zn2 N2 C1 -70.1(9) . . . . ? N3 Zn2 N2 C1 66.0(8) . . . . ? N7X Zn2 N2 C1 169.4(11) . . . . ? N8 Zn2 N2 C1 176.7(8) . . . . ? C9 Zn2 N2 C2 49.5(10) . . . . ? N3 Zn2 N2 C2 -174.4(8) . . . . ? N7X Zn2 N2 C2 -71.0(12) . . . . ? N8 Zn2 N2 C2 -63.7(10) . . . . ? N1 Zn1 N3 N4 -132.1(7) . . . . ? N5 Zn1 N3 N4 -27.5(8) . . . . ? Cl1 Zn1 N3 N4 98.0(7) . . . . ? N1 Zn1 N3 Zn2 -9.2(5) . . . . ? N5 Zn1 N3 Zn2 95.3(5) . . . . ? Cl1 Zn1 N3 Zn2 -139.2(3) . . . . ? C9 Zn2 N3 N4 -88.7(11) . . . . ? N7X Zn2 N3 N4 66.3(9) . . . . ? N2 Zn2 N3 N4 148.7(7) . . . . ? N8 Zn2 N3 N4 36.1(9) . . . . ? C9 Zn2 N3 Zn1 151.6(8) . . . . ? N7X Zn2 N3 Zn1 -53.5(8) . . . . ? N2 Zn2 N3 Zn1 29.0(5) . . . . ? N8 Zn2 N3 Zn1 -83.6(7) . . . . ? Zn1 N3 N4 C3 178.8(9) . . . . ? Zn2 N3 N4 C3 62.0(11) . . . . ? Zn1 N3 N4 C4 -64.3(10) . . . . ? Zn2 N3 N4 C4 178.8(8) . . . . ? Zn1 N3 N4 Zn3 50.1(8) . . . . ? Zn2 N3 N4 Zn3 -66.8(7) . . . . ? N7 Zn3 N4 N3 34.9(8) . . . . ? C11 Zn3 N4 N3 175.5(10) . . . . ? N5 Zn3 N4 N3 -52.1(7) . . . . ? N8X Zn3 N4 N3 57.2(10) . . . . ? N7 Zn3 N4 C3 -89.1(11) . . . . ? C11 Zn3 N4 C3 51.4(13) . . . . ? N5 Zn3 N4 C3 -176.2(10) . . . . ? N8X Zn3 N4 C3 -66.8(13) . . . . ? N7 Zn3 N4 C4 151.5(9) . . . . ? C11 Zn3 N4 C4 -67.9(12) . . . . ? N5 Zn3 N4 C4 64.5(9) . . . . ? N8X Zn3 N4 C4 173.9(10) . . . . ? N3 Zn1 N5 N6 -129.1(7) . . . . ? N1 Zn1 N5 N6 -25.5(8) . . . . ? Cl1 Zn1 N5 N6 100.5(7) . . . . ? N3 Zn1 N5 Zn3 -9.5(6) . . . . ? N1 Zn1 N5 Zn3 94.1(5) . . . . ? Cl1 Zn1 N5 Zn3 -139.9(3) . . . . ? N7 Zn3 N5 N6 46.4(12) . . . . ? C11 Zn3 N5 N6 -94.2(12) . . . . ? N8X Zn3 N5 N6 40.6(11) . . . . ? N4 Zn3 N5 N6 146.9(8) . . . . ? N7 Zn3 N5 Zn1 -71.2(11) . . . . ? C11 Zn3 N5 Zn1 148.2(9) . . . . ? N8X Zn3 N5 Zn1 -77.0(9) . . . . ? N4 Zn3 N5 Zn1 29.3(6) . . . . ? Zn1 N5 N6 C5 174.1(9) . . . . ? Zn3 N5 N6 C5 60.5(12) . . . . ? Zn1 N5 N6 C6 -65.6(11) . . . . ? Zn3 N5 N6 C6 -179.2(9) . . . . ? Zn1 N5 N6 Zn4 49.1(8) . . . . ? Zn3 N5 N6 Zn4 -64.5(8) . . . . ? N7X Zn4 N6 N5 34.2(9) . . . . ? C13X Zn4 N6 N5 -176.2(19) . . . . ? C13 Zn4 N6 N5 170.3(15) . . . . ? N1 Zn4 N6 N5 -52.9(7) . . . . ? N7 Zn4 N6 N5 44.7(12) . . . . ? N7X Zn4 N6 C5 -90.5(11) . . . . ? C13X Zn4 N6 C5 59(2) . . . . ? C13 Zn4 N6 C5 45.6(17) . . . . ? N1 Zn4 N6 C5 -177.6(10) . . . . ? N7 Zn4 N6 C5 -79.9(14) . . . . ? N7X Zn4 N6 C6 150.6(10) . . . . ? C13X Zn4 N6 C6 -60(2) . . . . ? C13 Zn4 N6 C6 -73.3(17) . . . . ? N1 Zn4 N6 C6 63.4(9) . . . . ? N7 Zn4 N6 C6 161.1(13) . . . . ? C11 Zn3 N7 N8 -71(3) . . . . ? N5 Zn3 N7 N8 150(2) . . . . ? N8X Zn3 N7 N8 -44(2) . . . . ? N4 Zn3 N7 N8 58(2) . . . . ? C11 Zn3 N7 Zn4 129.2(14) . . . . ? N5 Zn3 N7 Zn4 -9.4(16) . . . . ? N8X Zn3 N7 Zn4 156(4) . . . . ? N4 Zn3 N7 Zn4 -102.3(16) . . . . ? N7X Zn4 N7 N8 -13.0(15) . . . . ? C13X Zn4 N7 N8 71(5) . . . . ? C13 Zn4 N7 N8 76(3) . . . . ? N1 Zn4 N7 N8 -80(2) . . . . ? N6 Zn4 N7 N8 -173(2) . . . . ? N7X Zn4 N7 Zn3 146(4) . . . . ? C13X Zn4 N7 Zn3 -130(5) . . . . ? C13 Zn4 N7 Zn3 -125.3(19) . . . . ? N1 Zn4 N7 Zn3 78.4(17) . . . . ? N6 Zn4 N7 Zn3 -14.2(16) . . . . ? Zn3 N7 N8 C7 38(3) . . . . ? Zn4 N7 N8 C7 -163(3) . . . . ? Zn3 N7 N8 C8 162.2(19) . . . . ? Zn4 N7 N8 C8 -39(3) . . . . ? Zn3 N7 N8 Zn2 -84.3(19) . . . . ? Zn4 N7 N8 Zn2 75(2) . . . . ? C9 Zn2 N8 N7 -176.5(11) . . . . ? N3 Zn2 N8 N7 43.3(12) . . . . ? N7X Zn2 N8 N7 -42.3(18) . . . . ? N2 Zn2 N8 N7 -57.1(12) . . . . ? C9 Zn2 N8 C7 58(2) . . . . ? N3 Zn2 N8 C7 -83(2) . . . . ? N7X Zn2 N8 C7 -168(3) . . . . ? N2 Zn2 N8 C7 177.1(18) . . . . ? C9 Zn2 N8 C8 -64.3(16) . . . . ? N3 Zn2 N8 C8 155.5(14) . . . . ? N7X Zn2 N8 C8 70(2) . . . . ? N2 Zn2 N8 C8 55.1(16) . . . . ? C13X Zn4 N7X N8X -102(4) . . . . ? C13 Zn4 N7X N8X -90(2) . . . . ? N1 Zn4 N7X N8X 133.3(17) . . . . ? N7 Zn4 N7X N8X 19.6(19) . . . . ? N6 Zn4 N7X N8X 41.4(18) . . . . ? C13X Zn4 N7X Zn2 129(3) . . . . ? C13 Zn4 N7X Zn2 141.5(19) . . . . ? N1 Zn4 N7X Zn2 4.9(15) . . . . ? N7 Zn4 N7X Zn2 -109(3) . . . . ? N6 Zn4 N7X Zn2 -87.0(16) . . . . ? C9 Zn2 N7X N8X 95(2) . . . . ? N3 Zn2 N7X N8X -62.4(17) . . . . ? N2 Zn2 N7X N8X -153.6(18) . . . . ? N8 Zn2 N7X N8X 40.4(15) . . . . ? C9 Zn2 N7X Zn4 -139.3(13) . . . . ? N3 Zn2 N7X Zn4 62.9(17) . . . . ? N2 Zn2 N7X Zn4 -28.3(15) . . . . ? N8 Zn2 N7X Zn4 166(3) . . . . ? Zn4 N7X N8X C7X 178(3) . . . . ? Zn2 N7X N8X C7X -50(3) . . . . ? Zn4 N7X N8X C8X 60(3) . . . . ? Zn2 N7X N8X C8X -168(2) . . . . ? Zn4 N7X N8X Zn3 -68.6(18) . . . . ? Zn2 N7X N8X Zn3 63(2) . . . . ? N7 Zn3 N8X N7X 25(2) . . . . ? C11 Zn3 N8X N7X -175.9(15) . . . . ? N5 Zn3 N8X N7X 40.9(19) . . . . ? N4 Zn3 N8X N7X -57.6(18) . . . . ? N7 Zn3 N8X C7X 144(4) . . . . ? C11 Zn3 N8X C7X -57(2) . . . . ? N5 Zn3 N8X C7X 160(2) . . . . ? N4 Zn3 N8X C7X 61(2) . . . . ? N7 Zn3 N8X C8X -101(4) . . . . ? C11 Zn3 N8X C8X 58(2) . . . . ? N5 Zn3 N8X C8X -85(2) . . . . ? N4 Zn3 N8X C8X 176.2(19) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3 Cl1 0.93 2.62 3.537(11) 169.1 3_676 _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.446 _refine_diff_density_min -0.671 _refine_diff_density_rms 0.117 #===END data_7 _database_code_depnum_ccdc_archive 'CCDC 790915' #TrackingRef '- Redshaw.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H82 Li2 N12 O2 Zn8' _chemical_formula_sum 'C28 H82 Li2 N12 O2 Zn8' _chemical_formula_weight 1155.9 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1483(3) _cell_length_b 10.8241(3) _cell_length_c 13.5695(5) _cell_angle_alpha 111.0290(18) _cell_angle_beta 91.4522(17) _cell_angle_gamma 117.6991(19) _cell_volume 1198.09(7) _cell_formula_units_Z 1 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 31841 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.602 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 596 _exptl_absorpt_coefficient_mu 3.969 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.769 _exptl_absorpt_correction_T_max 0.925 _exptl_absorpt_process_details 'SADABS v2007/2, Sheldrick, G.M., (2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator '10cm confocal mirrors' _diffrn_measurement_device_type 'Bruker-Nonius APEX II CCD camera on \K-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm' _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 22176 _diffrn_reflns_av_R_equivalents 0.0555 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 27.54 _reflns_number_total 5464 _reflns_number_gt 4080 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Otwinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0000P)^2^+4.1345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except H11A&B coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5464 _refine_ls_number_parameters 251 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0836 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.0966 _refine_ls_wR_factor_gt 0.0850 _refine_ls_goodness_of_fit_ref 1.172 _refine_ls_restrained_S_all 1.172 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.44818(6) 0.56128(6) 0.73266(5) 0.02403(14) Uani 1 1 d . . . Zn2 Zn 0.65770(6) 0.42372(6) 0.64066(4) 0.02366(14) Uani 1 1 d . . . Zn3 Zn 0.76184(6) 0.76672(6) 0.68452(4) 0.02177(14) Uani 1 1 d . . . Zn4 Zn 0.77878(6) 0.68748(6) 0.88708(4) 0.02438(14) Uani 1 1 d . . . O1 O 0.5710(3) 0.5505(3) 0.6195(3) 0.0225(7) Uani 1 1 d . . . N1 N 0.5516(4) 0.5059(4) 0.8298(3) 0.0259(9) Uani 1 1 d . . . H1 H 0.5047 0.4978 0.8870 0.031 Uiso 1 1 calc R . . N2 N 0.5478(5) 0.3628(4) 0.7643(3) 0.0276(9) Uani 1 1 d . . . C1 C 0.3883(6) 0.2335(6) 0.7222(5) 0.0380(13) Uani 1 1 d . . . H1A H 0.3873 0.1386 0.6784 0.057 Uiso 1 1 calc R . . H1B H 0.3304 0.2534 0.6771 0.057 Uiso 1 1 calc R . . H1C H 0.3415 0.2227 0.7830 0.057 Uiso 1 1 calc R . . C2 C 0.6370(6) 0.3309(6) 0.8294(4) 0.0347(12) Uani 1 1 d . . . H2A H 0.7435 0.4154 0.8553 0.052 Uiso 1 1 calc R . . H2B H 0.6331 0.2348 0.7843 0.052 Uiso 1 1 calc R . . H2C H 0.5933 0.3212 0.8916 0.052 Uiso 1 1 calc R . . N3 N 0.7413(4) 0.8351(4) 0.8396(3) 0.0226(8) Uani 1 1 d . . . H3 H 0.8140 0.9376 0.8815 0.027 Uiso 1 1 calc R . . N4 N 0.5849(4) 0.8054(5) 0.8423(3) 0.0254(9) Uani 1 1 d . . . C3 C 0.5549(6) 0.9030(6) 0.8027(4) 0.0305(11) Uani 1 1 d . . . H3A H 0.6240 1.0114 0.8513 0.046 Uiso 1 1 calc R . . H3B H 0.4486 0.8780 0.8012 0.046 Uiso 1 1 calc R . . H3C H 0.5722 0.8842 0.7293 0.046 Uiso 1 1 calc R . . C4 C 0.5645(6) 0.8376(6) 0.9541(4) 0.0336(12) Uani 1 1 d . . . H4A H 0.5900 0.7772 0.9816 0.050 Uiso 1 1 calc R . . H4B H 0.4579 0.8097 0.9547 0.050 Uiso 1 1 calc R . . H4C H 0.6321 0.9472 1.0004 0.050 Uiso 1 1 calc R . . N5 N 0.8559(4) 0.6000(4) 0.7513(3) 0.0228(8) Uani 1 1 d . . . H5 H 0.9180 0.5650 0.7676 0.027 Uiso 1 1 calc R . . N6 N 0.9352(4) 0.7165(4) 0.7102(3) 0.0241(9) Uani 1 1 d . . . C5 C 0.9738(6) 0.6519(6) 0.6070(4) 0.0294(11) Uani 1 1 d . . . H5A H 1.0362 0.6088 0.6178 0.044 Uiso 1 1 calc R . . H5B H 1.0313 0.7334 0.5831 0.044 Uiso 1 1 calc R . . H5C H 0.8794 0.5708 0.5517 0.044 Uiso 1 1 calc R . . C6 C 1.0771(5) 0.8453(6) 0.7908(4) 0.0314(12) Uani 1 1 d . . . H6A H 1.0526 0.8860 0.8603 0.047 Uiso 1 1 calc R . . H6B H 1.1263 0.9265 0.7654 0.047 Uiso 1 1 calc R . . H6C H 1.1467 0.8089 0.8004 0.047 Uiso 1 1 calc R . . C7 C 0.2266(6) 0.4929(7) 0.6987(5) 0.0359(12) Uani 1 1 d . . . H7A H 0.2156 0.5685 0.6800 0.043 Uiso 1 1 calc R . . H7B H 0.1737 0.3934 0.6339 0.043 Uiso 1 1 calc R . . C8 C 0.1478(7) 0.4743(8) 0.7898(5) 0.0458(15) Uani 1 1 d . . . H8A H 0.1616 0.4029 0.8112 0.069 Uiso 1 1 calc R . . H8B H 0.0384 0.4336 0.7651 0.069 Uiso 1 1 calc R . . H8C H 0.1925 0.5744 0.8521 0.069 Uiso 1 1 calc R . . C9 C 0.6349(6) 0.2446(6) 0.5109(4) 0.0326(12) Uani 1 1 d . . . H9A H 0.5267 0.1605 0.4854 0.039 Uiso 1 1 calc R . . H9B H 0.6653 0.2760 0.4511 0.039 Uiso 1 1 calc R . . C10 C 0.7361(7) 0.1884(7) 0.5416(5) 0.0434(14) Uani 1 1 d . . . H10A H 0.8419 0.2741 0.5719 0.065 Uiso 1 1 calc R . . H10B H 0.7319 0.1068 0.4768 0.065 Uiso 1 1 calc R . . H10C H 0.6993 0.1483 0.5958 0.065 Uiso 1 1 calc R . . C11 C 0.7930(6) 0.8659(6) 0.5808(4) 0.0284(11) Uani 1 1 d . . . H11A H 0.801(6) 0.811(6) 0.512(5) 0.034 Uiso 1 1 d . . . H11B H 0.707(6) 0.875(6) 0.560(4) 0.034 Uiso 1 1 d . . . C12 C 0.9398(7) 1.0232(6) 0.6293(5) 0.0415(14) Uani 1 1 d . . . H12A H 0.9313 1.0888 0.6976 0.062 Uiso 1 1 calc R . . H12B H 0.9551 1.0710 0.5782 0.062 Uiso 1 1 calc R . . H12C H 1.0271 1.0107 0.6431 0.062 Uiso 1 1 calc R . . C13 C 0.9016(6) 0.7635(6) 1.0353(4) 0.0318(12) Uani 1 1 d . . . H13A H 0.9503 0.8768 1.0709 0.038 Uiso 1 1 calc R . . H13B H 0.8311 0.7212 1.0787 0.038 Uiso 1 1 calc R . . C14 C 1.0270(6) 0.7215(6) 1.0372(4) 0.0354(12) Uani 1 1 d . . . H14A H 0.9800 0.6095 1.0048 0.053 Uiso 1 1 calc R . . H14B H 1.0819 0.7639 1.1125 0.053 Uiso 1 1 calc R . . H14C H 1.0989 0.7644 0.9957 0.053 Uiso 1 1 calc R . . Li1 Li 0.4409(12) 0.3766(11) 0.4884(8) 0.047(3) 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 0.0220(3) 0.0261(3) 0.0236(3) 0.0108(2) 0.0060(2) 0.0117(2) Zn2 0.0253(3) 0.0225(3) 0.0235(3) 0.0096(2) 0.0031(2) 0.0125(2) Zn3 0.0199(3) 0.0224(3) 0.0236(3) 0.0111(2) 0.0043(2) 0.0102(2) Zn4 0.0259(3) 0.0255(3) 0.0216(3) 0.0096(2) 0.0024(2) 0.0132(2) O1 0.0223(16) 0.0225(17) 0.0221(17) 0.0097(14) 0.0034(14) 0.0108(14) N1 0.030(2) 0.022(2) 0.023(2) 0.0100(17) 0.0065(18) 0.0109(18) N2 0.031(2) 0.022(2) 0.029(2) 0.0127(18) 0.0064(18) 0.0113(18) C1 0.039(3) 0.025(3) 0.041(3) 0.014(2) 0.009(3) 0.009(2) C2 0.049(3) 0.031(3) 0.036(3) 0.018(2) 0.013(3) 0.026(3) N3 0.0200(19) 0.020(2) 0.023(2) 0.0081(17) 0.0017(16) 0.0075(16) N4 0.024(2) 0.028(2) 0.025(2) 0.0081(18) 0.0063(17) 0.0166(18) C3 0.031(3) 0.032(3) 0.036(3) 0.013(2) 0.009(2) 0.022(2) C4 0.035(3) 0.034(3) 0.030(3) 0.009(2) 0.012(2) 0.020(2) N5 0.023(2) 0.025(2) 0.026(2) 0.0126(17) 0.0050(17) 0.0147(17) N6 0.0192(19) 0.024(2) 0.027(2) 0.0092(18) 0.0027(17) 0.0109(17) C5 0.027(3) 0.036(3) 0.028(3) 0.012(2) 0.010(2) 0.019(2) C6 0.023(2) 0.031(3) 0.040(3) 0.017(2) 0.006(2) 0.012(2) C7 0.030(3) 0.042(3) 0.039(3) 0.022(3) 0.005(2) 0.018(3) C8 0.037(3) 0.060(4) 0.051(4) 0.027(3) 0.018(3) 0.029(3) C9 0.027(3) 0.028(3) 0.029(3) 0.004(2) 0.003(2) 0.009(2) C10 0.051(4) 0.036(3) 0.046(4) 0.014(3) 0.018(3) 0.025(3) C11 0.023(3) 0.029(3) 0.032(3) 0.016(2) 0.006(2) 0.010(2) C12 0.042(3) 0.032(3) 0.038(3) 0.018(3) 0.006(3) 0.008(3) C13 0.030(3) 0.033(3) 0.026(3) 0.004(2) -0.004(2) 0.018(2) C14 0.043(3) 0.044(3) 0.026(3) 0.012(2) 0.002(2) 0.029(3) Li1 0.056(6) 0.030(5) 0.040(6) 0.020(4) -0.007(5) 0.007(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 C7 1.993(5) . ? Zn1 O1 2.007(3) . ? Zn1 N1 2.069(4) . ? Zn1 N4 2.188(4) . ? Zn2 C9 2.006(5) . ? Zn2 O1 2.032(3) . ? Zn2 N5 2.040(4) . ? Zn2 N2 2.167(4) . ? Zn3 C11 2.006(5) . ? Zn3 N3 2.016(4) . ? Zn3 O1 2.056(3) . ? Zn3 N6 2.123(4) . ? Zn4 C13 2.002(5) . ? Zn4 N1 2.093(4) . ? Zn4 N3 2.099(4) . ? Zn4 N5 2.101(4) . ? O1 Li1 1.902(10) . ? O1 Li1 1.921(10) 2_666 ? N1 N2 1.464(5) . ? N2 C1 1.476(6) . ? N2 C2 1.480(6) . ? N3 N4 1.470(5) . ? N4 C4 1.473(6) . ? N4 C3 1.482(6) . ? N5 N6 1.460(5) . ? N6 C6 1.474(6) . ? N6 C5 1.478(6) . ? C7 C8 1.512(8) . ? C9 C10 1.530(8) . ? C11 C12 1.530(7) . ? C13 C14 1.540(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 C7 Zn1 O1 123.40(19) . . ? C7 Zn1 N1 126.5(2) . . ? O1 Zn1 N1 97.14(14) . . ? C7 Zn1 N4 111.4(2) . . ? O1 Zn1 N4 100.43(14) . . ? N1 Zn1 N4 91.08(15) . . ? C7 Zn1 Li1 93.1(3) . . ? O1 Zn1 Li1 34.6(2) . . ? N1 Zn1 Li1 107.5(2) . . ? N4 Zn1 Li1 131.5(2) . . ? C9 Zn2 O1 118.88(18) . . ? C9 Zn2 N5 126.60(18) . . ? O1 Zn2 N5 98.05(14) . . ? C9 Zn2 N2 114.23(19) . . ? O1 Zn2 N2 100.81(14) . . ? N5 Zn2 N2 92.78(15) . . ? C9 Zn2 Li1 76.9(3) . . ? O1 Zn2 Li1 44.5(2) . . ? N5 Zn2 Li1 139.3(2) . . ? N2 Zn2 Li1 107.5(3) . . ? C11 Zn3 N3 131.86(19) . . ? C11 Zn3 O1 110.99(17) . . ? N3 Zn3 O1 98.94(14) . . ? C11 Zn3 N6 113.01(19) . . ? N3 Zn3 N6 96.27(15) . . ? O1 Zn3 N6 101.10(14) . . ? C11 Zn3 Li1 62.8(3) . 2_666 ? N3 Zn3 Li1 129.2(3) . 2_666 ? O1 Zn3 Li1 48.4(2) . 2_666 ? N6 Zn3 Li1 124.0(3) . 2_666 ? C13 Zn4 N1 122.4(2) . . ? C13 Zn4 N3 120.93(19) . . ? N1 Zn4 N3 95.90(15) . . ? C13 Zn4 N5 118.60(18) . . ? N1 Zn4 N5 96.08(15) . . ? N3 Zn4 N5 97.03(15) . . ? Li1 O1 Li1 72.2(5) . 2_666 ? Li1 O1 Zn1 108.6(4) . . ? Li1 O1 Zn1 120.5(4) 2_666 . ? Li1 O1 Zn2 87.0(3) . . ? Li1 O1 Zn2 135.3(4) 2_666 . ? Zn1 O1 Zn2 103.34(14) . . ? Li1 O1 Zn3 144.7(4) . . ? Li1 O1 Zn3 78.3(3) 2_666 . ? Zn1 O1 Zn3 102.73(14) . . ? Zn2 O1 Zn3 101.27(13) . . ? N2 N1 Zn1 109.8(3) . . ? N2 N1 Zn4 109.4(3) . . ? Zn1 N1 Zn4 104.58(17) . . ? N1 N2 C1 110.2(4) . . ? N1 N2 C2 110.6(4) . . ? C1 N2 C2 109.6(4) . . ? N1 N2 Zn2 99.9(3) . . ? C1 N2 Zn2 114.1(3) . . ? C2 N2 Zn2 112.0(3) . . ? N4 N3 Zn3 109.8(3) . . ? N4 N3 Zn4 110.3(3) . . ? Zn3 N3 Zn4 101.27(16) . . ? N3 N4 C4 109.7(4) . . ? N3 N4 C3 110.4(4) . . ? C4 N4 C3 109.6(4) . . ? N3 N4 Zn1 101.5(2) . . ? C4 N4 Zn1 112.8(3) . . ? C3 N4 Zn1 112.5(3) . . ? N6 N5 Zn2 109.5(3) . . ? N6 N5 Zn4 110.0(3) . . ? Zn2 N5 Zn4 103.09(16) . . ? N5 N6 C6 109.7(4) . . ? N5 N6 C5 111.0(4) . . ? C6 N6 C5 109.1(4) . . ? N5 N6 Zn3 100.1(2) . . ? C6 N6 Zn3 115.7(3) . . ? C5 N6 Zn3 111.0(3) . . ? C8 C7 Zn1 114.4(4) . . ? C10 C9 Zn2 109.4(4) . . ? C12 C11 Zn3 109.7(4) . . ? C12 C11 Li1 177.5(5) . 2_666 ? Zn3 C11 Li1 69.0(3) . 2_666 ? C14 C13 Zn4 114.9(3) . . ? O1 Li1 O1 107.8(5) . 2_666 ? O1 Li1 Li1 54.3(4) . 2_666 ? O1 Li1 Li1 53.5(4) 2_666 2_666 ? O1 Li1 C11 142.4(6) . 2_666 ? O1 Li1 C11 101.2(4) 2_666 2_666 ? Li1 Li1 C11 146.6(8) 2_666 2_666 ? O1 Li1 Zn3 154.4(5) . 2_666 ? O1 Li1 Zn3 53.2(3) 2_666 2_666 ? Li1 Li1 Zn3 104.6(6) 2_666 2_666 ? C11 Li1 Zn3 48.2(2) 2_666 2_666 ? 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 C7 Zn1 O1 Li1 -32.6(4) . . . . ? N1 Zn1 O1 Li1 110.6(4) . . . . ? N4 Zn1 O1 Li1 -157.0(4) . . . . ? C7 Zn1 O1 Li1 47.2(4) . . . 2_666 ? N1 Zn1 O1 Li1 -169.6(4) . . . 2_666 ? N4 Zn1 O1 Li1 -77.2(4) . . . 2_666 ? Li1 Zn1 O1 Li1 79.8(5) . . . 2_666 ? C7 Zn1 O1 Zn2 -123.9(2) . . . . ? N1 Zn1 O1 Zn2 19.24(16) . . . . ? N4 Zn1 O1 Zn2 111.67(15) . . . . ? Li1 Zn1 O1 Zn2 -91.3(4) . . . . ? C7 Zn1 O1 Zn3 131.0(2) . . . . ? N1 Zn1 O1 Zn3 -85.80(15) . . . . ? N4 Zn1 O1 Zn3 6.63(16) . . . . ? Li1 Zn1 O1 Zn3 163.6(4) . . . . ? C9 Zn2 O1 Li1 21.7(4) . . . . ? N5 Zn2 O1 Li1 161.6(4) . . . . ? N2 Zn2 O1 Li1 -104.0(4) . . . . ? C9 Zn2 O1 Li1 -39.0(5) . . . 2_666 ? N5 Zn2 O1 Li1 101.0(5) . . . 2_666 ? N2 Zn2 O1 Li1 -164.6(5) . . . 2_666 ? Li1 Zn2 O1 Li1 -60.7(7) . . . 2_666 ? C9 Zn2 O1 Zn1 130.1(2) . . . . ? N5 Zn2 O1 Zn1 -89.94(16) . . . . ? N2 Zn2 O1 Zn1 4.46(17) . . . . ? Li1 Zn2 O1 Zn1 108.4(4) . . . . ? C9 Zn2 O1 Zn3 -123.8(2) . . . . ? N5 Zn2 O1 Zn3 16.21(16) . . . . ? N2 Zn2 O1 Zn3 110.62(15) . . . . ? Li1 Zn2 O1 Zn3 -145.4(4) . . . . ? C11 Zn3 O1 Li1 27.6(7) . . . . ? N3 Zn3 O1 Li1 169.2(7) . . . . ? N6 Zn3 O1 Li1 -92.5(7) . . . . ? Li1 Zn3 O1 Li1 33.5(10) 2_666 . . . ? C11 Zn3 O1 Li1 -5.9(4) . . . 2_666 ? N3 Zn3 O1 Li1 135.7(4) . . . 2_666 ? N6 Zn3 O1 Li1 -126.0(4) . . . 2_666 ? C11 Zn3 O1 Zn1 -124.9(2) . . . . ? N3 Zn3 O1 Zn1 16.75(16) . . . . ? N6 Zn3 O1 Zn1 114.99(15) . . . . ? Li1 Zn3 O1 Zn1 -119.0(4) 2_666 . . . ? C11 Zn3 O1 Zn2 128.49(19) . . . . ? N3 Zn3 O1 Zn2 -89.89(15) . . . . ? N6 Zn3 O1 Zn2 8.36(17) . . . . ? Li1 Zn3 O1 Zn2 134.4(4) 2_666 . . . ? C7 Zn1 N1 N2 88.5(4) . . . . ? O1 Zn1 N1 N2 -53.0(3) . . . . ? N4 Zn1 N1 N2 -153.6(3) . . . . ? Li1 Zn1 N1 N2 -19.1(4) . . . . ? C7 Zn1 N1 Zn4 -154.2(2) . . . . ? O1 Zn1 N1 Zn4 64.33(17) . . . . ? N4 Zn1 N1 Zn4 -36.32(18) . . . . ? Li1 Zn1 N1 Zn4 98.2(2) . . . . ? C13 Zn4 N1 N2 -96.6(3) . . . . ? N3 Zn4 N1 N2 130.8(3) . . . . ? N5 Zn4 N1 N2 33.1(3) . . . . ? C13 Zn4 N1 Zn1 145.87(19) . . . . ? N3 Zn4 N1 Zn1 13.23(19) . . . . ? N5 Zn4 N1 Zn1 -84.51(18) . . . . ? Zn1 N1 N2 C1 -65.2(4) . . . . ? Zn4 N1 N2 C1 -179.4(3) . . . . ? Zn1 N1 N2 C2 173.4(3) . . . . ? Zn4 N1 N2 C2 59.1(4) . . . . ? Zn1 N1 N2 Zn2 55.2(3) . . . . ? Zn4 N1 N2 Zn2 -59.0(3) . . . . ? C9 Zn2 N2 N1 -166.3(3) . . . . ? O1 Zn2 N2 N1 -37.6(3) . . . . ? N5 Zn2 N2 N1 61.1(3) . . . . ? Li1 Zn2 N2 N1 -83.1(3) . . . . ? C9 Zn2 N2 C1 -48.8(4) . . . . ? O1 Zn2 N2 C1 79.9(3) . . . . ? N5 Zn2 N2 C1 178.7(3) . . . . ? Li1 Zn2 N2 C1 34.4(4) . . . . ? C9 Zn2 N2 C2 76.6(4) . . . . ? O1 Zn2 N2 C2 -154.7(3) . . . . ? N5 Zn2 N2 C2 -56.0(3) . . . . ? Li1 Zn2 N2 C2 159.8(4) . . . . ? C11 Zn3 N3 N4 79.6(3) . . . . ? O1 Zn3 N3 N4 -49.3(3) . . . . ? N6 Zn3 N3 N4 -151.6(3) . . . . ? Li1 Zn3 N3 N4 -6.9(4) 2_666 . . . ? C11 Zn3 N3 Zn4 -163.9(2) . . . . ? O1 Zn3 N3 Zn4 67.25(16) . . . . ? N6 Zn3 N3 Zn4 -35.07(17) . . . . ? Li1 Zn3 N3 Zn4 109.6(3) 2_666 . . . ? C13 Zn4 N3 N4 -103.5(3) . . . . ? N1 Zn4 N3 N4 30.1(3) . . . . ? N5 Zn4 N3 N4 127.0(3) . . . . ? C13 Zn4 N3 Zn3 140.3(2) . . . . ? N1 Zn4 N3 Zn3 -86.07(17) . . . . ? N5 Zn4 N3 Zn3 10.82(17) . . . . ? Zn3 N3 N4 C4 173.1(3) . . . . ? Zn4 N3 N4 C4 62.4(4) . . . . ? Zn3 N3 N4 C3 -66.0(4) . . . . ? Zn4 N3 N4 C3 -176.7(3) . . . . ? Zn3 N3 N4 Zn1 53.5(3) . . . . ? Zn4 N3 N4 Zn1 -57.2(3) . . . . ? C7 Zn1 N4 N3 -170.2(3) . . . . ? O1 Zn1 N4 N3 -37.9(3) . . . . ? N1 Zn1 N4 N3 59.5(3) . . . . ? Li1 Zn1 N4 N3 -55.1(4) . . . . ? C7 Zn1 N4 C4 72.5(4) . . . . ? O1 Zn1 N4 C4 -155.2(3) . . . . ? N1 Zn1 N4 C4 -57.8(3) . . . . ? Li1 Zn1 N4 C4 -172.5(4) . . . . ? C7 Zn1 N4 C3 -52.2(4) . . . . ? O1 Zn1 N4 C3 80.1(3) . . . . ? N1 Zn1 N4 C3 177.6(3) . . . . ? Li1 Zn1 N4 C3 62.9(4) . . . . ? C9 Zn2 N5 N6 83.9(3) . . . . ? O1 Zn2 N5 N6 -51.6(3) . . . . ? N2 Zn2 N5 N6 -152.9(3) . . . . ? Li1 Zn2 N5 N6 -31.7(5) . . . . ? C9 Zn2 N5 Zn4 -159.0(2) . . . . ? O1 Zn2 N5 Zn4 65.51(17) . . . . ? N2 Zn2 N5 Zn4 -35.82(17) . . . . ? Li1 Zn2 N5 Zn4 85.3(4) . . . . ? C13 Zn4 N5 N6 -99.7(3) . . . . ? N1 Zn4 N5 N6 128.1(3) . . . . ? N3 Zn4 N5 N6 31.3(3) . . . . ? C13 Zn4 N5 Zn2 143.5(2) . . . . ? N1 Zn4 N5 Zn2 11.34(18) . . . . ? N3 Zn4 N5 Zn2 -85.40(17) . . . . ? Zn2 N5 N6 C6 179.0(3) . . . . ? Zn4 N5 N6 C6 66.4(4) . . . . ? Zn2 N5 N6 C5 -60.4(4) . . . . ? Zn4 N5 N6 C5 -173.0(3) . . . . ? Zn2 N5 N6 Zn3 56.9(2) . . . . ? Zn4 N5 N6 Zn3 -55.7(3) . . . . ? C11 Zn3 N6 N5 -159.7(3) . . . . ? N3 Zn3 N6 N5 59.4(3) . . . . ? O1 Zn3 N6 N5 -41.0(3) . . . . ? Li1 Zn3 N6 N5 -87.9(4) 2_666 . . . ? C11 Zn3 N6 C6 82.6(4) . . . . ? N3 Zn3 N6 C6 -58.3(4) . . . . ? O1 Zn3 N6 C6 -158.7(3) . . . . ? Li1 Zn3 N6 C6 154.4(4) 2_666 . . . ? C11 Zn3 N6 C5 -42.4(4) . . . . ? N3 Zn3 N6 C5 176.7(3) . . . . ? O1 Zn3 N6 C5 76.3(3) . . . . ? Li1 Zn3 N6 C5 29.4(4) 2_666 . . . ? O1 Zn1 C7 C8 165.7(4) . . . . ? N1 Zn1 C7 C8 33.5(5) . . . . ? N4 Zn1 C7 C8 -74.9(4) . . . . ? Li1 Zn1 C7 C8 147.9(4) . . . . ? O1 Zn2 C9 C10 168.3(3) . . . . ? N5 Zn2 C9 C10 40.8(5) . . . . ? N2 Zn2 C9 C10 -72.9(4) . . . . ? Li1 Zn2 C9 C10 -176.3(4) . . . . ? N3 Zn3 C11 C12 58.1(5) . . . . ? O1 Zn3 C11 C12 -177.4(3) . . . . ? N6 Zn3 C11 C12 -64.6(4) . . . . ? Li1 Zn3 C11 C12 177.7(5) 2_666 . . . ? N3 Zn3 C11 Li1 -119.6(4) . . . 2_666 ? O1 Zn3 C11 Li1 5.0(3) . . . 2_666 ? N6 Zn3 C11 Li1 117.7(3) . . . 2_666 ? N1 Zn4 C13 C14 107.4(4) . . . . ? N3 Zn4 C13 C14 -131.1(4) . . . . ? N5 Zn4 C13 C14 -11.8(5) . . . . ? Li1 O1 Li1 O1 0.0 2_666 . . 2_666 ? Zn1 O1 Li1 O1 117.0(5) . . . 2_666 ? Zn2 O1 Li1 O1 -139.9(5) . . . 2_666 ? Zn3 O1 Li1 O1 -34.6(10) . . . 2_666 ? Zn1 O1 Li1 Li1 117.0(5) . . . 2_666 ? Zn2 O1 Li1 Li1 -139.9(5) . . . 2_666 ? Zn3 O1 Li1 Li1 -34.6(10) . . . 2_666 ? Li1 O1 Li1 C11 -138.7(13) 2_666 . . 2_666 ? Zn1 O1 Li1 C11 -21.7(10) . . . 2_666 ? Zn2 O1 Li1 C11 81.3(9) . . . 2_666 ? Zn3 O1 Li1 C11 -173.3(5) . . . 2_666 ? Li1 O1 Li1 Zn3 -38.4(9) 2_666 . . 2_666 ? Zn1 O1 Li1 Zn3 78.6(13) . . . 2_666 ? Zn2 O1 Li1 Zn3 -178.3(13) . . . 2_666 ? Zn3 O1 Li1 Zn3 -72.9(16) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.784 _refine_diff_density_min -0.660 _refine_diff_density_rms 0.137 #===END