# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Zhongmin Su' _publ_contact_author_email 'zmsu@nenu.edu.cn, zmsu@hotmail.com' loop_ _publ_author_name 'Zhongmin Su' 'Shun-li Li' data_IFMC-10 _database_code_depnum_ccdc_archive 'CCDC 855123' #TrackingRef '- crystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IFMC-10 _chemical_melting_point 320 _chemical_formula_moiety C51H41NO13Zn2.C3H7NO _chemical_formula_sum 'C54 H48 N2 O14 Zn2' _chemical_formula_weight 1079.68 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 25.502(4) _cell_length_b 25.502(4) _cell_length_c 49.611(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 32265(8) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 98 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.889 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8928 _exptl_absorpt_coefficient_mu 0.638 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.821 _exptl_absorpt_correction_T_max 0.853 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 135406 _diffrn_reflns_av_R_equivalents 0.0934 _diffrn_reflns_av_sigmaI/netI 0.1179 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -64 _diffrn_reflns_limit_l_max 64 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18397 _reflns_number_gt 4927 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg and Putz, 2008)' _computing_publication_material SHELXL-97 _refine_special_details ; dfix 1.5 0.01 c33 c36 The above restraint in the refinement was used to fix the organic ligand. 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^)+(0.1612P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18397 _refine_ls_number_parameters 567 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2846 _refine_ls_R_factor_gt 0.0906 _refine_ls_wR_factor_ref 0.3250 _refine_ls_wR_factor_gt 0.2611 _refine_ls_goodness_of_fit_ref 0.894 _refine_ls_restrained_S_all 0.894 _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 0.84998(4) 0.72789(3) 0.065901(14) 0.1191(4) Uani 1 1 d . . . Zn2 Zn 0.78291(4) 0.27248(4) 0.577519(16) 0.1356(4) Uani 1 1 d . . . C1 C 0.8306(2) 0.2202(2) 0.23081(10) 0.0867(14) Uani 1 1 d . . . C2 C 0.8173(2) 0.2670(2) 0.24356(11) 0.0886(15) Uani 1 1 d . . . C3 C 0.8253(2) 0.2745(2) 0.27116(11) 0.0857(14) Uani 1 1 d . . . C4 C 0.8436(2) 0.2328(2) 0.28633(10) 0.0870(15) Uani 1 1 d . . . C5 C 0.85298(19) 0.1842(2) 0.27427(10) 0.0831(14) Uani 1 1 d . . . C6 C 0.84830(19) 0.1788(2) 0.24671(10) 0.0808(14) Uani 1 1 d . . . C7 C 0.8692(2) 0.1364(2) 0.29167(12) 0.1139(19) Uani 1 1 d . . . H7A H 0.8708 0.1466 0.3103 0.171 Uiso 1 1 calc R . . H7B H 0.9030 0.1240 0.2860 0.171 Uiso 1 1 calc R . . H7C H 0.8438 0.1089 0.2895 0.171 Uiso 1 1 calc R . . C8 C 0.8261(3) 0.2138(3) 0.20033(10) 0.123(2) Uani 1 1 d . . . H8A H 0.8133 0.2458 0.1925 0.184 Uiso 1 1 calc R . . H8B H 0.8022 0.1858 0.1963 0.184 Uiso 1 1 calc R . . H8C H 0.8599 0.2057 0.1929 0.184 Uiso 1 1 calc R . . C9 C 0.8149(3) 0.3269(2) 0.28362(12) 0.119(2) Uani 1 1 d . . . H9A H 0.8025 0.3507 0.2700 0.179 Uiso 1 1 calc R . . H9B H 0.8467 0.3403 0.2913 0.179 Uiso 1 1 calc R . . H9C H 0.7889 0.3234 0.2975 0.179 Uiso 1 1 calc R . . C11 C 0.7955(3) 0.2336(2) 0.35537(12) 0.1011(17) Uani 1 1 d . . . C12 C 0.8339(3) 0.2496(3) 0.37263(13) 0.120(2) Uani 1 1 d . . . H12 H 0.8673 0.2569 0.3661 0.144 Uiso 1 1 calc R . . C13 C 0.8231(3) 0.2549(3) 0.40032(13) 0.130(2) Uani 1 1 d . . . H13 H 0.8495 0.2663 0.4119 0.157 Uiso 1 1 calc R . . C14 C 0.7748(3) 0.2435(2) 0.41043(12) 0.1068(19) Uani 1 1 d . . . C15 C 0.7376(3) 0.2281(3) 0.39272(14) 0.136(2) Uani 1 1 d . . . H15 H 0.7039 0.2213 0.3990 0.163 Uiso 1 1 calc R . . C16 C 0.7482(3) 0.2221(3) 0.36514(12) 0.131(2) Uani 1 1 d . . . H16 H 0.7221 0.2100 0.3536 0.158 Uiso 1 1 calc R . . C17 C 0.8032(4) 0.2515(4) 0.45828(15) 0.170(3) Uani 1 1 d . . . H17 H 0.8381 0.2506 0.4528 0.204 Uiso 1 1 calc R . . C18 C 0.7896(5) 0.2566(4) 0.48616(17) 0.177(3) Uani 1 1 d . . . H18 H 0.8166 0.2595 0.4987 0.212 Uiso 1 1 calc R . . C19 C 0.7392(4) 0.2573(3) 0.49514(16) 0.131(3) Uani 1 1 d . . . C20 C 0.7011(4) 0.2512(3) 0.47652(15) 0.133(2) Uani 1 1 d . . . H20 H 0.6663 0.2500 0.4820 0.159 Uiso 1 1 calc R . . C21 C 0.7128(4) 0.2466(3) 0.44960(13) 0.129(2) Uani 1 1 d . . . H21 H 0.6854 0.2423 0.4374 0.155 Uiso 1 1 calc R . . C22 C 0.7634(3) 0.2480(2) 0.43983(12) 0.1110(19) Uani 1 1 d . . . O2 O 0.6830(3) 0.2634(2) 0.53171(10) 0.167(2) Uani 1 1 d . . . C24 C 0.8255(3) 0.3865(3) 0.20231(13) 0.115(2) Uani 1 1 d . . . C25 C 0.7799(2) 0.3941(3) 0.18832(12) 0.1117(19) Uani 1 1 d . . . H25 H 0.7523 0.3707 0.1904 0.134 Uiso 1 1 calc R . . C26 C 0.7747(3) 0.4357(3) 0.17143(14) 0.122(2) Uani 1 1 d . . . H26 H 0.7433 0.4399 0.1621 0.146 Uiso 1 1 calc R . . C27 C 0.8136(3) 0.4712(3) 0.16764(14) 0.130(2) Uani 1 1 d . . . C28 C 0.8625(3) 0.4629(3) 0.18066(17) 0.164(3) Uani 1 1 d . . . H28 H 0.8910 0.4847 0.1773 0.197 Uiso 1 1 calc R . . C29 C 0.8667(3) 0.4210(3) 0.19864(16) 0.152(3) Uani 1 1 d . . . H29 H 0.8976 0.4163 0.2083 0.182 Uiso 1 1 calc R . . C30 C 0.8113(4) 0.5174(3) 0.14920(15) 0.134(2) Uani 1 1 d . . . C31 C 0.8542(3) 0.5356(3) 0.13395(16) 0.148(3) Uani 1 1 d . . . H31 H 0.8869 0.5195 0.1352 0.177 Uiso 1 1 calc R . . C32 C 0.8466(4) 0.5783(3) 0.11698(16) 0.153(3) Uani 1 1 d . . . H32 H 0.8744 0.5905 0.1066 0.183 Uiso 1 1 calc R . . C33 C 0.7991(4) 0.6027(3) 0.11517(15) 0.136(3) Uani 1 1 d D . . C34 C 0.7574(3) 0.5834(3) 0.12947(16) 0.138(2) Uani 1 1 d . . . H34 H 0.7246 0.5987 0.1275 0.165 Uiso 1 1 calc R . . C35 C 0.7634(3) 0.5426(3) 0.14640(15) 0.131(2) Uani 1 1 d . . . H35 H 0.7349 0.5310 0.1564 0.157 Uiso 1 1 calc R . . C37 C 0.8138(3) 0.0637(3) 0.20803(15) 0.114(2) Uani 1 1 d . . . C38 C 0.8552(3) 0.0327(3) 0.20387(14) 0.131(2) Uani 1 1 d . . . H38 H 0.8862 0.0397 0.2131 0.157 Uiso 1 1 calc R . . C39 C 0.8534(3) -0.0103(3) 0.18600(15) 0.126(2) Uani 1 1 d . . . H39 H 0.8821 -0.0326 0.1848 0.151 Uiso 1 1 calc R . . C40 C 0.8098(3) -0.0195(3) 0.17042(14) 0.120(2) Uani 1 1 d . . . C41 C 0.7689(4) 0.0140(4) 0.1745(2) 0.173(4) Uani 1 1 d . . . H41 H 0.7383 0.0092 0.1646 0.208 Uiso 1 1 calc R . . C42 C 0.7710(3) 0.0550(3) 0.19287(19) 0.164(3) Uani 1 1 d . . . H42 H 0.7421 0.0770 0.1947 0.197 Uiso 1 1 calc R . . C43 C 0.8068(4) -0.0635(3) 0.15155(15) 0.119(2) Uani 1 1 d . . . C44 C 0.8489(4) -0.0812(3) 0.13803(16) 0.145(3) Uani 1 1 d . . . H44 H 0.8808 -0.0642 0.1406 0.174 Uiso 1 1 calc R . . C45 C 0.8472(5) -0.1245(3) 0.12006(14) 0.161(4) Uani 1 1 d . . . H45 H 0.8771 -0.1370 0.1115 0.194 Uiso 1 1 calc R . . C46 C 0.7972(5) -0.1475(3) 0.11590(15) 0.147(3) Uani 1 1 d . . . C47 C 0.7547(4) -0.1286(4) 0.1288(2) 0.172(4) Uani 1 1 d . . . H47 H 0.7219 -0.1432 0.1255 0.206 Uiso 1 1 calc R . . C48 C 0.7595(4) -0.0880(3) 0.14652(18) 0.161(3) Uani 1 1 d . . . H48 H 0.7298 -0.0765 0.1556 0.193 Uiso 1 1 calc R . . C49 C 0.7975(6) -0.1945(3) 0.09727(17) 0.153(4) Uani 1 1 d . . . C50 C 0.8513(3) 0.2392(2) 0.31665(11) 0.1059(18) Uani 1 1 d . . . H50A H 0.8779 0.2152 0.3232 0.127 Uiso 1 1 calc R . . H50B H 0.8617 0.2747 0.3210 0.127 Uiso 1 1 calc R . . C51 C 0.7954(2) 0.3123(2) 0.22672(13) 0.1113(19) Uani 1 1 d . . . H51A H 0.7783 0.2987 0.2107 0.134 Uiso 1 1 calc R . . H51B H 0.7697 0.3318 0.2371 0.134 Uiso 1 1 calc R . . C52 C 0.8598(2) 0.1282(3) 0.23356(12) 0.1078(18) Uani 1 1 d . . . H52A H 0.8822 0.1338 0.2180 0.129 Uiso 1 1 calc R . . H52B H 0.8782 0.1053 0.2460 0.129 Uiso 1 1 calc R . . O1 O 0.8389(3) -0.2117(2) 0.08732(12) 0.169(3) Uani 1 1 d . . . O1W O 0.8550(6) 0.2738(6) 0.5837(3) 0.230(6) Uiso 0.50 1 d P . . O3 O 0.8349(3) 0.6643(2) 0.08364(12) 0.177(3) Uani 1 1 d . . . O2W O 0.9279(5) 0.7223(5) 0.0619(2) 0.182(4) Uiso 0.50 1 d P . . O5 O 0.7530(3) -0.2138(2) 0.09332(13) 0.194(3) Uani 1 1 d . . . O7 O 0.80099(17) 0.22709(17) 0.32837(7) 0.1153(13) Uani 1 1 d . . . O8 O 0.83700(15) 0.34493(17) 0.21946(9) 0.1257(15) Uani 1 1 d . . . O9 O 0.81193(16) 0.10436(17) 0.22537(9) 0.1206(14) Uani 1 1 d . . . O6 O 0.7673(3) 0.2695(3) 0.54000(12) 0.195(3) Uani 1 1 d . . . O4 O 0.7527(3) 0.6694(2) 0.09491(12) 0.187(3) Uani 1 1 d . . . C23 C 0.7307(6) 0.2624(3) 0.52445(17) 0.159(4) Uani 1 1 d . . . C36 C 0.8004(6) 0.6474(3) 0.09560(19) 0.166(4) Uani 1 1 d 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 0.1694(8) 0.0996(6) 0.0882(5) 0.0114(4) -0.0105(4) -0.0134(5) Zn2 0.1609(8) 0.1414(8) 0.1046(6) -0.0106(5) 0.0121(5) -0.0092(5) C1 0.090(4) 0.095(4) 0.076(3) 0.008(3) -0.002(3) -0.005(3) C2 0.079(3) 0.098(4) 0.090(4) 0.025(3) -0.005(3) -0.017(3) C3 0.092(4) 0.085(4) 0.081(4) 0.008(3) 0.005(3) 0.001(3) C4 0.096(4) 0.099(4) 0.067(3) -0.001(3) -0.001(3) -0.007(3) C5 0.079(3) 0.091(4) 0.079(4) 0.012(3) -0.010(3) -0.006(3) C6 0.084(4) 0.086(4) 0.073(3) -0.009(3) -0.001(3) -0.002(3) C7 0.129(5) 0.112(5) 0.100(4) 0.002(4) -0.011(4) 0.010(4) C8 0.149(6) 0.153(6) 0.066(4) 0.005(3) -0.011(3) 0.004(4) C9 0.139(5) 0.108(5) 0.111(5) -0.006(4) 0.009(4) 0.009(4) C11 0.112(5) 0.111(5) 0.080(4) 0.005(3) -0.002(4) -0.007(4) C12 0.139(6) 0.135(5) 0.086(4) -0.015(4) 0.004(4) -0.019(4) C13 0.158(7) 0.159(6) 0.074(4) -0.007(4) 0.003(4) -0.036(5) C14 0.154(6) 0.096(4) 0.070(4) -0.013(3) 0.003(4) 0.002(4) C15 0.140(6) 0.183(7) 0.086(5) -0.003(5) 0.004(4) -0.009(5) C16 0.126(6) 0.192(7) 0.076(4) -0.005(4) -0.005(4) -0.017(5) C17 0.186(8) 0.248(10) 0.075(5) -0.015(5) -0.009(5) 0.010(7) C18 0.203(10) 0.233(10) 0.093(6) 0.002(6) -0.020(6) 0.003(8) C19 0.186(8) 0.108(5) 0.098(6) -0.006(4) 0.042(6) -0.008(5) C20 0.199(8) 0.113(5) 0.086(5) -0.002(4) 0.019(5) 0.000(5) C21 0.174(8) 0.133(6) 0.081(5) -0.011(4) 0.013(5) 0.000(5) C22 0.156(6) 0.101(4) 0.076(4) 0.004(3) 0.002(5) 0.009(4) O2 0.274(8) 0.149(4) 0.078(3) -0.005(3) 0.045(4) 0.012(5) C24 0.107(5) 0.114(5) 0.124(5) 0.039(4) -0.004(4) -0.019(4) C25 0.092(4) 0.123(5) 0.120(5) 0.036(4) -0.025(4) -0.016(4) C26 0.101(5) 0.127(5) 0.138(5) 0.058(5) -0.019(4) -0.029(4) C27 0.135(6) 0.128(6) 0.127(5) 0.050(5) -0.016(5) 0.003(5) C28 0.129(6) 0.169(7) 0.193(8) 0.097(6) -0.038(6) -0.040(5) C29 0.116(5) 0.159(7) 0.180(7) 0.080(6) -0.041(5) -0.041(5) C30 0.143(7) 0.118(5) 0.141(6) 0.032(5) -0.047(5) -0.002(5) C31 0.138(6) 0.149(7) 0.157(7) 0.065(6) -0.001(5) -0.044(5) C32 0.188(9) 0.130(6) 0.141(6) 0.052(5) -0.019(6) -0.052(6) C33 0.182(8) 0.095(5) 0.130(6) 0.022(5) -0.048(6) 0.010(6) C34 0.144(7) 0.134(6) 0.135(6) 0.028(5) 0.003(5) -0.014(5) C35 0.143(7) 0.122(5) 0.128(5) 0.043(5) -0.008(5) -0.011(5) C37 0.093(5) 0.099(5) 0.150(6) -0.015(4) -0.007(5) 0.010(4) C38 0.105(5) 0.149(6) 0.138(6) -0.046(5) -0.006(4) -0.012(5) C39 0.109(5) 0.134(6) 0.134(6) -0.030(5) 0.000(4) 0.007(4) C40 0.126(6) 0.114(5) 0.120(5) -0.017(4) -0.008(5) 0.005(5) C41 0.146(7) 0.142(7) 0.232(10) -0.057(7) -0.066(6) 0.024(6) C42 0.135(7) 0.109(6) 0.250(10) -0.071(6) -0.059(7) 0.029(5) C43 0.138(6) 0.096(5) 0.124(5) -0.018(4) -0.011(5) 0.005(5) C44 0.170(8) 0.142(7) 0.123(6) -0.011(5) 0.003(5) -0.034(6) C45 0.281(12) 0.110(6) 0.093(5) -0.022(4) 0.020(6) -0.017(7) C46 0.251(12) 0.097(6) 0.094(5) 0.005(4) -0.058(6) -0.051(7) C47 0.177(9) 0.133(7) 0.206(10) -0.058(7) -0.035(7) 0.017(6) C48 0.163(8) 0.115(6) 0.205(9) -0.050(6) -0.058(6) 0.022(5) C49 0.282(15) 0.085(6) 0.093(6) 0.000(5) -0.044(7) -0.027(7) C50 0.128(5) 0.114(5) 0.076(3) -0.014(3) -0.010(4) 0.003(4) C51 0.117(5) 0.101(4) 0.116(5) 0.030(4) -0.009(4) -0.006(4) C52 0.097(4) 0.126(5) 0.101(4) -0.004(4) -0.007(3) 0.000(4) O1 0.299(9) 0.099(4) 0.110(4) -0.002(3) 0.012(5) -0.010(4) O3 0.293(9) 0.101(4) 0.137(5) 0.053(3) -0.013(5) -0.036(4) O5 0.260(8) 0.142(5) 0.179(6) -0.061(4) -0.057(5) -0.019(5) O7 0.125(3) 0.157(4) 0.064(2) -0.001(2) 0.004(2) -0.015(3) O8 0.102(3) 0.132(3) 0.143(4) 0.069(3) -0.022(2) -0.025(3) O9 0.103(3) 0.113(3) 0.146(4) -0.049(3) 0.001(3) 0.006(2) O6 0.268(8) 0.240(7) 0.077(4) -0.014(4) 0.018(4) -0.028(6) O4 0.265(8) 0.133(5) 0.164(5) 0.067(4) -0.033(5) -0.005(5) C23 0.274(14) 0.130(6) 0.073(6) -0.004(5) 0.040(7) -0.006(8) C36 0.268(14) 0.100(7) 0.131(8) 0.038(5) -0.077(8) -0.001(8) _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 O3 1.885(5) . ? Zn1 O1 1.893(6) 1_565 ? Zn1 O2 1.907(6) 6_654 ? Zn1 O2W 2.002(12) . ? Zn2 O1W 1.865(16) . ? Zn2 O6 1.905(7) . ? Zn2 O5 1.922(7) 6_645 ? Zn2 O4 1.940(7) 6_655 ? C1 C6 1.393(7) . ? C1 C2 1.394(7) . ? C1 C8 1.525(7) . ? C2 C3 1.397(7) . ? C2 C51 1.530(7) . ? C3 C4 1.383(7) . ? C3 C9 1.498(7) . ? C4 C5 1.397(7) . ? C4 C50 1.525(7) . ? C5 C6 1.380(6) . ? C5 C7 1.550(7) . ? C6 C52 1.476(7) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C11 C16 1.332(8) . ? C11 O7 1.357(7) . ? C11 C12 1.363(8) . ? C12 C13 1.408(8) . ? C12 H12 0.9300 . ? C13 C14 1.363(8) . ? C13 H13 0.9300 . ? C14 C15 1.350(8) . ? C14 C22 1.492(8) . ? C15 C16 1.403(9) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.370(10) . ? C17 C18 1.432(11) . ? C17 H17 0.9300 . ? C18 C19 1.361(11) . ? C18 H18 0.9300 . ? C19 C20 1.350(10) . ? C19 C23 1.476(11) . ? C20 C21 1.374(9) . ? C20 H20 0.9300 . ? C21 C22 1.378(9) . ? C21 H21 0.9300 . ? O2 C23 1.268(13) . ? O2 Zn1 1.907(6) 6_655 ? C24 C25 1.369(8) . ? C24 C29 1.383(8) . ? C24 O8 1.390(7) . ? C25 C26 1.357(8) . ? C25 H25 0.9300 . ? C26 C27 1.356(8) . ? C26 H26 0.9300 . ? C27 C28 1.421(9) . ? C27 C30 1.494(9) . ? C28 C29 1.395(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C35 1.386(9) . ? C30 C31 1.409(10) . ? C31 C32 1.390(10) . ? C31 H31 0.9300 . ? C32 C33 1.363(10) . ? C32 H32 0.9300 . ? C33 C34 1.369(10) . ? C33 C36 1.499(8) . ? C34 C35 1.347(9) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C37 C38 1.336(9) . ? C37 C42 1.343(9) . ? C37 O9 1.347(7) . ? C38 C39 1.411(9) . ? C38 H38 0.9300 . ? C39 C40 1.374(9) . ? C39 H39 0.9300 . ? C40 C41 1.364(9) . ? C40 C43 1.463(9) . ? C41 C42 1.388(10) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.345(10) . ? C43 C48 1.380(10) . ? C44 C45 1.420(10) . ? C44 H44 0.9300 . ? C45 C46 1.419(12) . ? C45 H45 0.9300 . ? C46 C47 1.347(12) . ? C46 C49 1.514(12) . ? C47 C48 1.365(10) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 O1 1.245(13) . ? C49 O5 1.253(12) . ? C50 O7 1.441(7) . ? C50 H50A 0.9700 . ? C50 H50B 0.9700 . ? C51 O8 1.397(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 O9 1.424(7) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? O1 Zn1 1.893(6) 1_545 ? O3 C36 1.146(13) . ? O5 Zn2 1.922(7) 6_644 ? O6 C23 1.225(12) . ? O4 C36 1.340(13) . ? O4 Zn2 1.940(7) 6_654 ? 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 O3 Zn1 O1 114.1(3) . 1_565 ? O3 Zn1 O2 115.2(3) . 6_654 ? O1 Zn1 O2 109.8(3) 1_565 6_654 ? O3 Zn1 O2W 100.8(4) . . ? O1 Zn1 O2W 105.1(4) 1_565 . ? O2 Zn1 O2W 111.0(4) 6_654 . ? O1W Zn2 O6 111.5(5) . . ? O1W Zn2 O5 114.7(5) . 6_645 ? O6 Zn2 O5 105.6(3) . 6_645 ? O1W Zn2 O4 112.0(5) . 6_655 ? O6 Zn2 O4 111.5(3) . 6_655 ? O5 Zn2 O4 101.0(3) 6_645 6_655 ? C6 C1 C2 118.1(5) . . ? C6 C1 C8 120.3(5) . . ? C2 C1 C8 121.6(5) . . ? C1 C2 C3 121.7(5) . . ? C1 C2 C51 119.2(5) . . ? C3 C2 C51 119.1(5) . . ? C4 C3 C2 118.6(5) . . ? C4 C3 C9 121.4(5) . . ? C2 C3 C9 120.0(5) . . ? C3 C4 C5 120.4(5) . . ? C3 C4 C50 119.9(5) . . ? C5 C4 C50 119.7(5) . . ? C6 C5 C4 119.9(5) . . ? C6 C5 C7 119.8(5) . . ? C4 C5 C7 120.3(5) . . ? C5 C6 C1 120.9(5) . . ? C5 C6 C52 120.5(5) . . ? C1 C6 C52 118.5(5) . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C3 C9 H9A 109.5 . . ? C3 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C3 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C16 C11 O7 115.2(6) . . ? C16 C11 C12 119.2(6) . . ? O7 C11 C12 125.6(6) . . ? C11 C12 C13 120.1(7) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 121.0(7) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C15 C14 C13 117.2(6) . . ? C15 C14 C22 121.5(7) . . ? C13 C14 C22 121.3(7) . . ? C14 C15 C16 122.1(7) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C11 C16 C15 120.3(7) . . ? C11 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C22 C17 C18 118.2(8) . . ? C22 C17 H17 120.9 . . ? C18 C17 H17 120.9 . . ? C19 C18 C17 123.0(8) . . ? C19 C18 H18 118.5 . . ? C17 C18 H18 118.5 . . ? C20 C19 C18 117.1(7) . . ? C20 C19 C23 125.3(10) . . ? C18 C19 C23 117.6(11) . . ? C19 C20 C21 121.3(8) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 122.9(8) . . ? C20 C21 H21 118.6 . . ? C22 C21 H21 118.6 . . ? C17 C22 C21 117.4(7) . . ? C17 C22 C14 120.9(8) . . ? C21 C22 C14 121.6(7) . . ? C23 O2 Zn1 132.7(7) . 6_655 ? C25 C24 C29 119.2(6) . . ? C25 C24 O8 126.7(6) . . ? C29 C24 O8 114.0(6) . . ? C26 C25 C24 120.5(6) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C27 C26 C25 122.3(6) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 118.7(6) . . ? C26 C27 C30 125.7(7) . . ? C28 C27 C30 115.4(7) . . ? C29 C28 C27 118.2(6) . . ? C29 C28 H28 120.9 . . ? C27 C28 H28 120.9 . . ? C24 C29 C28 120.9(6) . . ? C24 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C35 C30 C31 118.6(7) . . ? C35 C30 C27 117.4(8) . . ? C31 C30 C27 124.0(8) . . ? C32 C31 C30 118.3(8) . . ? C32 C31 H31 120.9 . . ? C30 C31 H31 120.9 . . ? C33 C32 C31 121.5(8) . . ? C33 C32 H32 119.3 . . ? C31 C32 H32 119.3 . . ? C32 C33 C34 119.4(7) . . ? C32 C33 C36 111.8(10) . . ? C34 C33 C36 128.7(10) . . ? C35 C34 C33 120.9(8) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C30 121.3(7) . . ? C34 C35 H35 119.3 . . ? C30 C35 H35 119.3 . . ? C38 C37 C42 117.3(7) . . ? C38 C37 O9 125.5(7) . . ? C42 C37 O9 117.1(6) . . ? C37 C38 C39 122.1(7) . . ? C37 C38 H38 118.9 . . ? C39 C38 H38 118.9 . . ? C40 C39 C38 120.9(7) . . ? C40 C39 H39 119.6 . . ? C38 C39 H39 119.6 . . ? C41 C40 C39 115.3(7) . . ? C41 C40 C43 122.3(8) . . ? C39 C40 C43 122.3(7) . . ? C40 C41 C42 122.7(7) . . ? C40 C41 H41 118.6 . . ? C42 C41 H41 118.6 . . ? C37 C42 C41 121.5(7) . . ? C37 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C44 C43 C48 117.1(7) . . ? C44 C43 C40 122.2(8) . . ? C48 C43 C40 120.7(8) . . ? C43 C44 C45 123.3(8) . . ? C43 C44 H44 118.4 . . ? C45 C44 H44 118.4 . . ? C46 C45 C44 116.2(9) . . ? C46 C45 H45 121.9 . . ? C44 C45 H45 121.9 . . ? C47 C46 C45 120.4(8) . . ? C47 C46 C49 125.2(11) . . ? C45 C46 C49 114.3(11) . . ? C46 C47 C48 120.2(9) . . ? C46 C47 H47 119.9 . . ? C48 C47 H47 119.9 . . ? C47 C48 C43 122.7(9) . . ? C47 C48 H48 118.6 . . ? C43 C48 H48 118.6 . . ? O1 C49 O5 124.6(9) . . ? O1 C49 C46 121.7(12) . . ? O5 C49 C46 113.6(12) . . ? O7 C50 C4 105.2(4) . . ? O7 C50 H50A 110.7 . . ? C4 C50 H50A 110.7 . . ? O7 C50 H50B 110.7 . . ? C4 C50 H50B 110.7 . . ? H50A C50 H50B 108.8 . . ? O8 C51 C2 108.2(5) . . ? O8 C51 H51A 110.1 . . ? C2 C51 H51A 110.1 . . ? O8 C51 H51B 110.1 . . ? C2 C51 H51B 110.1 . . ? H51A C51 H51B 108.4 . . ? O9 C52 C6 109.1(5) . . ? O9 C52 H52A 109.9 . . ? C6 C52 H52A 109.9 . . ? O9 C52 H52B 109.9 . . ? C6 C52 H52B 109.9 . . ? H52A C52 H52B 108.3 . . ? C49 O1 Zn1 129.5(8) . 1_545 ? C36 O3 Zn1 136.2(9) . . ? C49 O5 Zn2 143.2(8) . 6_644 ? C11 O7 C50 117.7(5) . . ? C24 O8 C51 116.9(4) . . ? C37 O9 C52 118.7(5) . . ? C23 O6 Zn2 141.3(7) . . ? C36 O4 Zn2 139.1(6) . 6_654 ? O6 C23 O2 123.3(9) . . ? O6 C23 C19 121.4(12) . . ? O2 C23 C19 115.0(12) . . ? O3 C36 O4 121.9(8) . . ? O3 C36 C33 129.6(13) . . ? O4 C36 C33 108.4(11) . . ? 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 C6 C1 C2 C3 5.3(8) . . . . ? C8 C1 C2 C3 -174.8(5) . . . . ? C6 C1 C2 C51 -177.2(5) . . . . ? C8 C1 C2 C51 2.6(8) . . . . ? C1 C2 C3 C4 -4.5(8) . . . . ? C51 C2 C3 C4 178.1(5) . . . . ? C1 C2 C3 C9 174.5(5) . . . . ? C51 C2 C3 C9 -2.9(7) . . . . ? C2 C3 C4 C5 -1.1(7) . . . . ? C9 C3 C4 C5 180.0(5) . . . . ? C2 C3 C4 C50 -178.2(5) . . . . ? C9 C3 C4 C50 2.8(8) . . . . ? C3 C4 C5 C6 5.6(7) . . . . ? C50 C4 C5 C6 -177.3(5) . . . . ? C3 C4 C5 C7 -175.0(5) . . . . ? C50 C4 C5 C7 2.1(7) . . . . ? C4 C5 C6 C1 -4.7(7) . . . . ? C7 C5 C6 C1 175.9(5) . . . . ? C4 C5 C6 C52 177.9(5) . . . . ? C7 C5 C6 C52 -1.5(7) . . . . ? C2 C1 C6 C5 -0.7(7) . . . . ? C8 C1 C6 C5 179.5(5) . . . . ? C2 C1 C6 C52 176.8(5) . . . . ? C8 C1 C6 C52 -3.0(8) . . . . ? C16 C11 C12 C13 -1.4(10) . . . . ? O7 C11 C12 C13 180.0(6) . . . . ? C11 C12 C13 C14 1.0(11) . . . . ? C12 C13 C14 C15 -1.4(11) . . . . ? C12 C13 C14 C22 178.8(6) . . . . ? C13 C14 C15 C16 2.3(11) . . . . ? C22 C14 C15 C16 -178.0(6) . . . . ? O7 C11 C16 C15 -179.0(6) . . . . ? C12 C11 C16 C15 2.2(11) . . . . ? C14 C15 C16 C11 -2.7(12) . . . . ? C22 C17 C18 C19 1.0(15) . . . . ? C17 C18 C19 C20 2.2(14) . . . . ? C17 C18 C19 C23 179.6(8) . . . . ? C18 C19 C20 C21 -2.6(12) . . . . ? C23 C19 C20 C21 -179.8(7) . . . . ? C19 C20 C21 C22 -0.2(11) . . . . ? C18 C17 C22 C21 -3.7(12) . . . . ? C18 C17 C22 C14 179.1(7) . . . . ? C20 C21 C22 C17 3.4(11) . . . . ? C20 C21 C22 C14 -179.4(6) . . . . ? C15 C14 C22 C17 164.6(8) . . . . ? C13 C14 C22 C17 -15.7(10) . . . . ? C15 C14 C22 C21 -12.5(10) . . . . ? C13 C14 C22 C21 167.3(7) . . . . ? C29 C24 C25 C26 -1.2(11) . . . . ? O8 C24 C25 C26 -177.6(7) . . . . ? C24 C25 C26 C27 -0.2(11) . . . . ? C25 C26 C27 C28 3.6(12) . . . . ? C25 C26 C27 C30 179.1(8) . . . . ? C26 C27 C28 C29 -5.6(13) . . . . ? C30 C27 C28 C29 178.5(8) . . . . ? C25 C24 C29 C28 -1.0(13) . . . . ? O8 C24 C29 C28 175.8(8) . . . . ? C27 C28 C29 C24 4.3(14) . . . . ? C26 C27 C30 C35 34.9(12) . . . . ? C28 C27 C30 C35 -149.5(8) . . . . ? C26 C27 C30 C31 -142.8(8) . . . . ? C28 C27 C30 C31 32.8(12) . . . . ? C35 C30 C31 C32 0.6(11) . . . . ? C27 C30 C31 C32 178.3(7) . . . . ? C30 C31 C32 C33 0.7(12) . . . . ? C31 C32 C33 C34 -2.9(13) . . . . ? C31 C32 C33 C36 -179.9(7) . . . . ? C32 C33 C34 C35 3.7(12) . . . . ? C36 C33 C34 C35 -179.8(8) . . . . ? C33 C34 C35 C30 -2.4(12) . . . . ? C31 C30 C35 C34 0.2(12) . . . . ? C27 C30 C35 C34 -177.6(7) . . . . ? C42 C37 C38 C39 -5.1(12) . . . . ? O9 C37 C38 C39 177.7(7) . . . . ? C37 C38 C39 C40 5.3(12) . . . . ? C38 C39 C40 C41 -2.8(11) . . . . ? C38 C39 C40 C43 179.6(7) . . . . ? C39 C40 C41 C42 0.7(14) . . . . ? C43 C40 C41 C42 178.3(9) . . . . ? C38 C37 C42 C41 2.9(13) . . . . ? O9 C37 C42 C41 -179.7(8) . . . . ? C40 C41 C42 C37 -0.8(16) . . . . ? C41 C40 C43 C44 148.7(9) . . . . ? C39 C40 C43 C44 -33.8(11) . . . . ? C41 C40 C43 C48 -30.1(12) . . . . ? C39 C40 C43 C48 147.4(8) . . . . ? C48 C43 C44 C45 -2.6(12) . . . . ? C40 C43 C44 C45 178.6(7) . . . . ? C43 C44 C45 C46 2.8(12) . . . . ? C44 C45 C46 C47 -0.4(12) . . . . ? C44 C45 C46 C49 -178.2(6) . . . . ? C45 C46 C47 C48 -1.9(14) . . . . ? C49 C46 C47 C48 175.6(7) . . . . ? C46 C47 C48 C43 2.2(15) . . . . ? C44 C43 C48 C47 0.0(13) . . . . ? C40 C43 C48 C47 178.9(8) . . . . ? C47 C46 C49 O1 -175.7(9) . . . . ? C45 C46 C49 O1 2.0(11) . . . . ? C47 C46 C49 O5 3.8(13) . . . . ? C45 C46 C49 O5 -178.6(7) . . . . ? C3 C4 C50 O7 86.7(6) . . . . ? C5 C4 C50 O7 -90.4(6) . . . . ? C1 C2 C51 O8 -93.8(6) . . . . ? C3 C2 C51 O8 83.7(6) . . . . ? C5 C6 C52 O9 106.7(6) . . . . ? C1 C6 C52 O9 -70.8(6) . . . . ? O5 C49 O1 Zn1 -4.5(15) . . . 1_545 ? C46 C49 O1 Zn1 174.9(4) . . . 1_545 ? O1 Zn1 O3 C36 51.4(12) 1_565 . . . ? O2 Zn1 O3 C36 -76.9(11) 6_654 . . . ? O2W Zn1 O3 C36 163.5(11) . . . . ? O1 C49 O5 Zn2 8.1(17) . . . 6_644 ? C46 C49 O5 Zn2 -171.3(7) . . . 6_644 ? C16 C11 O7 C50 179.7(6) . . . . ? C12 C11 O7 C50 -1.6(9) . . . . ? C4 C50 O7 C11 -175.0(5) . . . . ? C25 C24 O8 C51 -11.3(10) . . . . ? C29 C24 O8 C51 172.2(6) . . . . ? C2 C51 O8 C24 175.4(5) . . . . ? C38 C37 O9 C52 22.0(10) . . . . ? C42 C37 O9 C52 -155.1(7) . . . . ? C6 C52 O9 C37 166.0(5) . . . . ? O1W Zn2 O6 C23 169.5(12) . . . . ? O5 Zn2 O6 C23 44.3(13) 6_645 . . . ? O4 Zn2 O6 C23 -64.5(12) 6_655 . . . ? Zn2 O6 C23 O2 14.0(19) . . . . ? Zn2 O6 C23 C19 -172.2(7) . . . . ? Zn1 O2 C23 O6 -2.7(15) 6_655 . . . ? Zn1 O2 C23 C19 -176.9(5) 6_655 . . . ? C20 C19 C23 O6 -177.7(9) . . . . ? C18 C19 C23 O6 5.1(13) . . . . ? C20 C19 C23 O2 -3.4(12) . . . . ? C18 C19 C23 O2 179.4(8) . . . . ? Zn1 O3 C36 O4 15.2(17) . . . . ? Zn1 O3 C36 C33 -160.3(7) . . . . ? Zn2 O4 C36 O3 1.8(17) 6_654 . . . ? Zn2 O4 C36 C33 178.1(6) 6_654 . . . ? C32 C33 C36 O3 -4.0(15) . . . . ? C34 C33 C36 O3 179.3(10) . . . . ? C32 C33 C36 O4 -179.9(8) . . . . ? C34 C33 C36 O4 3.4(13) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.944 _refine_diff_density_min -0.279 _refine_diff_density_rms 0.077 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.000 0.250 0.125 933.5 36.0 2 0.000 0.750 -0.125 933.5 36.1 3 -0.033 0.748 0.203 13656.2 414.8 4 0.500 0.250 0.375 930.8 36.1 5 0.500 0.750 0.625 930.7 36.0 _platon_squeeze_details ; One DMF solvent molecule was removed by the SQUEEZE process ; data_IFMC-11 _database_code_depnum_ccdc_archive 'CCDC 855124' #TrackingRef '- crystal.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common IFMC-11 _chemical_melting_point 315 _chemical_formula_moiety C39H35NO13Zn2.0.2(C3H7NO) _chemical_formula_sum 'C39.63 H36.38 N1.19 O13.19 Zn2' _chemical_formula_weight 870.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' '-y+3/4, x+1/4, z+1/4' 'y+1/4, -x+1/4, z+1/4' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-y+5/4, x+3/4, z+3/4' 'y+3/4, -x+3/4, z+3/4' '-x, -y, -z' 'x, y-1/2, -z' 'y-3/4, -x-1/4, -z-1/4' '-y-1/4, x-1/4, -z-1/4' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' 'y-1/4, -x+1/4, -z+1/4' '-y+1/4, x+1/4, -z+1/4' _cell_length_a 24.337(3) _cell_length_b 24.337(3) _cell_length_c 39.257(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 23252(4) _cell_formula_units_Z 16 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 125 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.995 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 7167 _exptl_absorpt_coefficient_mu 0.870 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.777 _exptl_absorpt_correction_T_max 0.797 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX CCD area-detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 99484 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13128 _reflns_number_gt 4653 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker, 1997)' _computing_cell_refinement SMART _computing_data_reduction 'SAINT (Bruker, 1999)' _computing_structure_solution 'SHELXS-97(Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Diamond (Brandenburg and Putz, 2008)' _computing_publication_material SHELXL-97 _refine_special_details ; dfix 1.5 0.01 c28 c29 isor 0.01 c28 c27 c29 The above restraints in the refinement were used to fix the organic ligand. 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^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13128 _refine_ls_number_parameters 459 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.2642 _refine_ls_R_factor_gt 0.1497 _refine_ls_wR_factor_ref 0.4431 _refine_ls_wR_factor_gt 0.3887 _refine_ls_goodness_of_fit_ref 1.227 _refine_ls_restrained_S_all 1.228 _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 0.52669(4) 0.63694(6) 0.83952(3) 0.1295(6) Uani 1 1 d . . . Zn2 Zn 0.54541(6) 0.50542(6) 0.85141(3) 0.1461(7) Uani 1 1 d . . . C1 C 0.5208(4) 0.5568(7) 0.7857(3) 0.133(4) Uani 1 1 d . . . C2 C 0.5089(4) 0.5464(6) 0.7478(2) 0.133(4) Uani 1 1 d . . . H2 H 0.5020 0.5769 0.7342 0.160 Uiso 1 1 calc R . . C3 C 0.5077(4) 0.4981(5) 0.7330(2) 0.117(3) Uani 1 1 d . . . H3 H 0.5153 0.4683 0.7470 0.140 Uiso 1 1 calc R . . C4 C 0.4964(3) 0.4850(4) 0.69831(19) 0.100(2) Uani 1 1 d . . . C5 C 0.5034(3) 0.4349(4) 0.6863(2) 0.100(2) Uani 1 1 d . . . H5 H 0.5142 0.4077 0.7015 0.120 Uiso 1 1 calc R . . C6 C 0.4958(4) 0.4198(4) 0.65263(19) 0.105(3) Uani 1 1 d . . . H6 H 0.5011 0.3838 0.6454 0.126 Uiso 1 1 calc R . . C7 C 0.4798(3) 0.4609(4) 0.62997(18) 0.092(2) Uani 1 1 d . . . C8 C 0.4717(3) 0.5127(4) 0.64048(18) 0.095(2) Uani 1 1 d . . . H8 H 0.4593 0.5395 0.6255 0.114 Uiso 1 1 calc R . . C9 C 0.4825(3) 0.5252(4) 0.67461(19) 0.097(2) Uani 1 1 d . . . H9 H 0.4802 0.5616 0.6817 0.116 Uiso 1 1 calc R . . C10 C 0.4806(3) 0.3986(3) 0.58129(16) 0.0835(19) Uani 1 1 d . . . H10A H 0.4557 0.3713 0.5905 0.100 Uiso 1 1 calc R . . H10B H 0.5181 0.3872 0.5860 0.100 Uiso 1 1 calc R . . C11 C 0.4720(3) 0.4048(3) 0.54371(17) 0.0819(19) Uani 1 1 d . . . C12 C 0.4190(3) 0.4003(3) 0.52983(17) 0.0784(18) Uani 1 1 d . . . C13 C 0.4107(3) 0.4060(3) 0.49543(19) 0.0818(19) Uani 1 1 d . . . C14 C 0.4540(3) 0.4217(3) 0.47433(18) 0.091(2) Uani 1 1 d . . . C15 C 0.5074(3) 0.4296(3) 0.48789(16) 0.0765(17) Uani 1 1 d . . . C16 C 0.5160(3) 0.4197(3) 0.52294(17) 0.0791(18) Uani 1 1 d . . . C17 C 0.5732(3) 0.4230(3) 0.53671(19) 0.097(2) Uani 1 1 d . . . H17A H 0.5980 0.4335 0.5188 0.145 Uiso 1 1 calc R . . H17B H 0.5839 0.3878 0.5455 0.145 Uiso 1 1 calc R . . H17C H 0.5746 0.4498 0.5546 0.145 Uiso 1 1 calc R . . C18 C 0.3697(3) 0.3874(3) 0.5531(2) 0.099(2) Uani 1 1 d . . . H18A H 0.3822 0.3832 0.5761 0.148 Uiso 1 1 calc R . . H18B H 0.3525 0.3540 0.5456 0.148 Uiso 1 1 calc R . . H18C H 0.3437 0.4170 0.5519 0.148 Uiso 1 1 calc R . . C19 C 0.4444(3) 0.4309(4) 0.43550(17) 0.111(3) Uani 1 1 d . . . H19A H 0.4785 0.4410 0.4249 0.166 Uiso 1 1 calc R . . H19B H 0.4181 0.4598 0.4323 0.166 Uiso 1 1 calc R . . H19C H 0.4308 0.3977 0.4254 0.166 Uiso 1 1 calc R . . C20 C 0.3555(3) 0.3950(3) 0.47973(19) 0.090(2) Uani 1 1 d . . . H20A H 0.3596 0.3765 0.4580 0.108 Uiso 1 1 calc R . . H20B H 0.3335 0.3720 0.4946 0.108 Uiso 1 1 calc R . . C21 C 0.2801(3) 0.4480(4) 0.4573(2) 0.093(2) Uani 1 1 d . . . C22 C 0.2537(4) 0.4033(5) 0.4493(3) 0.146(4) Uani 1 1 d . . . H22 H 0.2683 0.3690 0.4546 0.176 Uiso 1 1 calc R . . C23 C 0.2041(5) 0.4077(6) 0.4330(3) 0.158(5) Uani 1 1 d . . . H23 H 0.1853 0.3754 0.4280 0.190 Uiso 1 1 calc R . . C24 C 0.1823(4) 0.4522(6) 0.4242(2) 0.113(3) Uani 1 1 d . . . C25 C 0.2088(5) 0.4990(6) 0.4303(3) 0.150(4) Uani 1 1 d . . . H25 H 0.1944 0.5326 0.4234 0.179 Uiso 1 1 calc R . . C26 C 0.2600(4) 0.4957(5) 0.4480(3) 0.131(3) Uani 1 1 d . . . H26 H 0.2794 0.5277 0.4529 0.157 Uiso 1 1 calc R . . C27 C 0.1297(5) 0.4526(5) 0.4047(2) 0.126(3) Uani 1 1 d U . . H27 H 0.1169 0.4869 0.3979 0.152 Uiso 1 1 calc R . . C28 C 0.1019(5) 0.4138(7) 0.3968(3) 0.161(4) Uani 1 1 d DU . . H28 H 0.1136 0.3789 0.4031 0.193 Uiso 1 1 calc R . . C30 C 0.5521(3) 0.4500(3) 0.46587(17) 0.086(2) Uani 1 1 d . . . H30A H 0.5370 0.4719 0.4474 0.104 Uiso 1 1 calc R . . H30B H 0.5770 0.4728 0.4789 0.104 Uiso 1 1 calc R . . C31 C 0.6277(3) 0.4144(3) 0.43401(19) 0.090(2) Uani 1 1 d . . . C32 C 0.6450(3) 0.4646(3) 0.4255(2) 0.099(2) Uani 1 1 d . . . H32 H 0.6236 0.4953 0.4303 0.119 Uiso 1 1 calc R . . C33 C 0.6963(4) 0.4705(3) 0.4090(3) 0.120(3) Uani 1 1 d . . . H33 H 0.7091 0.5055 0.4040 0.144 Uiso 1 1 calc R . . C34 C 0.7266(4) 0.4271(4) 0.4005(2) 0.105(3) Uani 1 1 d . . . C35 C 0.7043(4) 0.3733(3) 0.4050(2) 0.115(3) Uani 1 1 d . . . H35 H 0.7216 0.3426 0.3958 0.138 Uiso 1 1 calc R . . C36 C 0.6563(4) 0.3682(4) 0.4234(3) 0.125(3) Uani 1 1 d . . . H36 H 0.6430 0.3334 0.4288 0.150 Uiso 1 1 calc R . . C37 C 0.7821(3) 0.4352(4) 0.3851(2) 0.104(3) Uani 1 1 d . . . H37 H 0.7928 0.4712 0.3807 0.125 Uiso 1 1 calc R . . C38 C 0.8163(3) 0.3972(4) 0.3773(2) 0.106(3) Uani 1 1 d . . . H38 H 0.8047 0.3612 0.3807 0.128 Uiso 1 1 calc R . . O1 O 0.5314(3) 0.5126(4) 0.80341(18) 0.142(3) Uani 1 1 d . . . O2 O 0.5173(3) 0.6054(4) 0.79512(16) 0.144(3) Uani 1 1 d . . . O1W O 0.5157(6) 0.7219(6) 0.8299(4) 0.146(5) Uiso 0.50 1 d P . . O2W O 0.5537(9) 0.4323(10) 0.8501(5) 0.213(8) Uiso 0.50 1 d P . . O7 O 0.4701(2) 0.4509(2) 0.59582(11) 0.0951(15) Uani 1 1 d . . . O9 O 0.5804(2) 0.4037(2) 0.45260(13) 0.1000(16) Uani 1 1 d . . . O8 O 0.3292(3) 0.4489(3) 0.47505(17) 0.1244(19) Uani 1 1 d . . . C39 C 0.8740(3) 0.4050(4) 0.3632(2) 0.091(2) Uani 1 1 d . . . O5 O 0.9018(2) 0.3662(3) 0.35758(13) 0.1034(16) Uani 1 1 d . . . O6 O 0.8866(3) 0.4555(4) 0.3604(2) 0.160(3) Uani 1 1 d . . . O3 O 0.0330(3) 0.3668(6) 0.3671(2) 0.198(4) Uani 1 1 d . . . O4 O 0.0286(4) 0.4620(5) 0.3723(2) 0.190(4) Uani 1 1 d . . . C29 C 0.0478(5) 0.4192(8) 0.3768(3) 0.147(4) Uani 1 1 d DU . . 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 0.0707(7) 0.2079(14) 0.1098(8) -0.0243(7) -0.0099(5) 0.0267(7) Zn2 0.1492(12) 0.1707(13) 0.1184(9) 0.0249(7) -0.0226(7) -0.0718(9) C1 0.082(6) 0.213(15) 0.104(8) -0.034(8) -0.008(5) 0.003(8) C2 0.106(7) 0.217(13) 0.077(6) 0.013(6) -0.005(5) 0.020(8) C3 0.100(7) 0.161(9) 0.088(6) 0.005(6) 0.006(5) 0.007(6) C4 0.085(5) 0.139(8) 0.076(5) 0.007(5) -0.002(4) 0.009(5) C5 0.109(6) 0.110(7) 0.081(5) 0.020(4) -0.008(4) 0.016(5) C6 0.125(7) 0.108(6) 0.082(5) 0.025(4) -0.010(4) 0.010(5) C7 0.077(5) 0.122(7) 0.075(5) 0.014(4) 0.019(3) 0.002(5) C8 0.111(6) 0.097(6) 0.077(5) 0.007(4) 0.008(4) 0.017(5) C9 0.074(5) 0.122(7) 0.094(6) -0.005(5) 0.006(4) 0.005(4) C10 0.086(5) 0.089(5) 0.076(4) 0.017(4) 0.012(3) 0.012(4) C11 0.084(5) 0.080(5) 0.082(4) 0.013(3) 0.004(4) 0.008(4) C12 0.073(5) 0.076(4) 0.087(5) 0.006(3) 0.022(3) -0.001(3) C13 0.053(4) 0.087(5) 0.106(5) -0.006(4) 0.011(4) 0.006(3) C14 0.109(6) 0.084(5) 0.081(4) 0.003(4) 0.011(4) 0.006(4) C15 0.066(4) 0.094(5) 0.069(4) -0.002(3) 0.008(3) 0.003(4) C16 0.066(4) 0.078(4) 0.094(5) 0.007(3) 0.013(3) 0.012(3) C17 0.074(5) 0.119(6) 0.098(5) 0.009(4) -0.003(4) 0.003(4) C18 0.069(5) 0.102(6) 0.125(6) 0.012(4) 0.025(4) -0.009(4) C19 0.103(6) 0.163(8) 0.065(4) 0.002(4) -0.001(4) 0.020(5) C20 0.094(5) 0.068(5) 0.106(5) 0.003(4) 0.001(4) 0.010(4) C21 0.049(4) 0.098(6) 0.131(6) -0.007(5) -0.035(4) -0.003(4) C22 0.111(8) 0.126(8) 0.202(11) -0.045(8) -0.059(8) 0.009(6) C23 0.142(11) 0.153(12) 0.179(11) -0.060(9) -0.050(8) -0.008(9) C24 0.099(7) 0.122(8) 0.119(7) -0.004(6) -0.022(5) 0.000(7) C25 0.099(8) 0.156(11) 0.194(11) 0.027(9) -0.018(7) 0.016(8) C26 0.077(6) 0.137(9) 0.179(9) 0.004(7) -0.040(6) -0.017(6) C27 0.127(7) 0.132(7) 0.120(6) -0.004(5) 0.007(5) -0.009(6) C28 0.150(8) 0.186(8) 0.146(7) -0.016(7) -0.009(6) -0.013(7) C30 0.082(5) 0.093(5) 0.085(4) 0.003(4) 0.023(4) 0.018(4) C31 0.070(5) 0.090(6) 0.109(5) 0.016(4) 0.013(4) 0.006(4) C32 0.077(5) 0.087(6) 0.133(6) 0.033(5) 0.032(4) 0.028(4) C33 0.113(7) 0.068(5) 0.179(9) 0.037(5) 0.045(6) 0.018(5) C34 0.105(6) 0.099(6) 0.112(6) 0.024(4) 0.030(5) 0.014(5) C35 0.098(6) 0.080(6) 0.167(8) 0.011(5) 0.061(6) 0.012(5) C36 0.094(6) 0.083(6) 0.199(10) 0.023(6) 0.063(6) 0.015(5) C37 0.098(6) 0.090(5) 0.125(6) 0.016(4) 0.056(5) 0.026(5) C38 0.089(6) 0.119(7) 0.111(6) 0.013(5) 0.011(5) -0.019(5) O1 0.142(6) 0.187(8) 0.099(4) -0.006(4) -0.027(4) -0.004(5) O2 0.149(6) 0.199(8) 0.085(4) -0.020(5) -0.024(4) 0.042(6) O7 0.110(4) 0.108(4) 0.068(3) 0.011(2) -0.003(2) 0.012(3) O9 0.084(3) 0.088(3) 0.128(4) 0.007(3) 0.044(3) 0.010(3) O8 0.105(4) 0.121(5) 0.147(5) -0.008(4) -0.006(4) -0.004(4) C39 0.083(6) 0.090(6) 0.099(5) 0.008(4) 0.015(4) 0.004(5) O5 0.075(3) 0.115(4) 0.120(4) -0.015(3) 0.022(3) 0.001(3) O6 0.131(6) 0.136(6) 0.214(8) 0.013(5) 0.084(5) 0.001(5) O3 0.120(6) 0.331(15) 0.142(6) -0.013(7) -0.036(5) -0.006(7) O4 0.167(8) 0.254(12) 0.149(7) 0.014(7) -0.045(5) 0.069(8) C29 0.139(8) 0.172(8) 0.130(7) 0.004(7) -0.009(6) -0.008(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 O3 1.813(8) 6 ? Zn1 O5 1.880(5) 6_655 ? Zn1 O2 1.918(7) . ? Zn1 O1W 2.119(14) . ? Zn2 O2W 1.79(2) . ? Zn2 O1 1.923(7) . ? Zn2 O6 1.941(8) 6_655 ? Zn2 O4 2.130(8) 6 ? C1 O2 1.242(14) . ? C1 O1 1.304(15) . ? C1 C2 1.539(14) . ? C2 C3 1.311(13) . ? C2 H2 0.9300 . ? C3 C4 1.424(12) . ? C3 H3 0.9300 . ? C4 C5 1.319(11) . ? C4 C9 1.393(11) . ? C5 C6 1.383(11) . ? C5 H5 0.9300 . ? C6 C7 1.394(10) . ? C6 H6 0.9300 . ? C7 C8 1.340(11) . ? C7 O7 1.383(9) . ? C8 C9 1.399(10) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 O7 1.417(9) . ? C10 C11 1.498(9) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C16 1.393(9) . ? C11 C12 1.405(10) . ? C12 C13 1.372(10) . ? C12 C18 1.539(9) . ? C13 C14 1.393(10) . ? C13 C20 1.503(10) . ? C14 C15 1.417(10) . ? C14 C19 1.558(10) . ? C15 C16 1.412(9) . ? C15 C30 1.476(9) . ? C16 C17 1.497(10) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 O8 1.472(9) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.301(12) . ? C21 C26 1.312(12) . ? C21 O8 1.383(8) . ? C22 C23 1.372(15) . ? C22 H22 0.9300 . ? C23 C24 1.252(15) . ? C23 H23 0.9300 . ? C24 C25 1.330(14) . ? C24 C27 1.492(14) . ? C25 C26 1.429(14) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.203(14) . ? C27 H27 0.9300 . ? C28 C29 1.538(9) . ? C28 H28 0.9300 . ? C30 O9 1.420(8) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.336(10) . ? C31 C36 1.387(11) . ? C31 O9 1.388(8) . ? C32 C33 1.411(11) . ? C32 H32 0.9300 . ? C33 C34 1.333(11) . ? C33 H33 0.9300 . ? C34 C35 1.428(12) . ? C34 C37 1.492(11) . ? C35 C36 1.379(11) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 C38 1.281(11) . ? C37 H37 0.9300 . ? C38 C39 1.521(11) . ? C38 H38 0.9300 . ? O1W O1W 1.57(3) 2_665 ? C39 O5 1.185(9) . ? C39 O6 1.270(10) . ? O5 Zn1 1.880(5) 6_654 ? O6 Zn2 1.941(8) 6_654 ? O3 C29 1.377(16) . ? O3 Zn1 1.813(8) 6_554 ? O4 C29 1.156(15) . ? O4 Zn2 2.130(8) 6_554 ? 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 O3 Zn1 O5 120.9(3) 6 6_655 ? O3 Zn1 O2 115.3(4) 6 . ? O5 Zn1 O2 115.9(3) 6_655 . ? O3 Zn1 O1W 93.2(6) 6 . ? O5 Zn1 O1W 102.9(5) 6_655 . ? O2 Zn1 O1W 102.3(5) . . ? O2W Zn2 O1 94.7(7) . . ? O2W Zn2 O6 113.4(8) . 6_655 ? O1 Zn2 O6 106.5(4) . 6_655 ? O2W Zn2 O4 118.4(8) . 6 ? O1 Zn2 O4 101.1(4) . 6 ? O6 Zn2 O4 117.9(4) 6_655 6 ? O2 C1 O1 129.8(10) . . ? O2 C1 C2 115.5(13) . . ? O1 C1 C2 114.6(12) . . ? C3 C2 C1 125.5(12) . . ? C3 C2 H2 117.2 . . ? C1 C2 H2 117.2 . . ? C2 C3 C4 129.0(10) . . ? C2 C3 H3 115.5 . . ? C4 C3 H3 115.5 . . ? C5 C4 C9 116.2(7) . . ? C5 C4 C3 121.6(9) . . ? C9 C4 C3 121.9(10) . . ? C4 C5 C6 124.7(8) . . ? C4 C5 H5 117.6 . . ? C6 C5 H5 117.6 . . ? C5 C6 C7 117.2(9) . . ? C5 C6 H6 121.4 . . ? C7 C6 H6 121.4 . . ? C8 C7 O7 116.1(7) . . ? C8 C7 C6 121.2(8) . . ? O7 C7 C6 122.7(8) . . ? C7 C8 C9 118.2(8) . . ? C7 C8 H8 120.9 . . ? C9 C8 H8 120.9 . . ? C4 C9 C8 122.1(8) . . ? C4 C9 H9 118.9 . . ? C8 C9 H9 118.9 . . ? O7 C10 C11 106.3(5) . . ? O7 C10 H10A 110.5 . . ? C11 C10 H10A 110.5 . . ? O7 C10 H10B 110.5 . . ? C11 C10 H10B 110.5 . . ? H10A C10 H10B 108.7 . . ? C16 C11 C12 119.9(6) . . ? C16 C11 C10 119.7(6) . . ? C12 C11 C10 120.2(6) . . ? C13 C12 C11 120.6(6) . . ? C13 C12 C18 119.3(7) . . ? C11 C12 C18 120.1(6) . . ? C12 C13 C14 120.1(7) . . ? C12 C13 C20 121.1(6) . . ? C14 C13 C20 118.8(7) . . ? C13 C14 C15 120.5(7) . . ? C13 C14 C19 120.5(7) . . ? C15 C14 C19 119.0(7) . . ? C16 C15 C14 118.6(6) . . ? C16 C15 C30 121.3(6) . . ? C14 C15 C30 120.1(6) . . ? C11 C16 C15 120.1(6) . . ? C11 C16 C17 121.2(6) . . ? C15 C16 C17 118.7(6) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C12 C18 H18A 109.5 . . ? C12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C14 C19 H19A 109.5 . . ? C14 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C14 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? O8 C20 C13 106.3(6) . . ? O8 C20 H20A 110.5 . . ? C13 C20 H20A 110.5 . . ? O8 C20 H20B 110.5 . . ? C13 C20 H20B 110.5 . . ? H20A C20 H20B 108.7 . . ? C22 C21 C26 119.3(8) . . ? C22 C21 O8 124.2(9) . . ? C26 C21 O8 116.6(8) . . ? C21 C22 C23 118.8(11) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C24 C23 C22 124.6(12) . . ? C24 C23 H23 117.7 . . ? C22 C23 H23 117.7 . . ? C23 C24 C25 119.1(10) . . ? C23 C24 C27 120.6(12) . . ? C25 C24 C27 120.1(11) . . ? C24 C25 C26 117.6(11) . . ? C24 C25 H25 121.2 . . ? C26 C25 H25 121.2 . . ? C21 C26 C25 120.6(10) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? C28 C27 C24 127.7(12) . . ? C28 C27 H27 116.2 . . ? C24 C27 H27 116.2 . . ? C27 C28 C29 123.2(15) . . ? C27 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? O9 C30 C15 107.7(6) . . ? O9 C30 H30A 110.2 . . ? C15 C30 H30A 110.2 . . ? O9 C30 H30B 110.2 . . ? C15 C30 H30B 110.2 . . ? H30A C30 H30B 108.5 . . ? C32 C31 C36 120.5(7) . . ? C32 C31 O9 124.5(7) . . ? C36 C31 O9 115.0(7) . . ? C31 C32 C33 119.2(7) . . ? C31 C32 H32 120.4 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 121.6(8) . . ? C34 C33 H33 119.2 . . ? C32 C33 H33 119.2 . . ? C33 C34 C35 119.0(8) . . ? C33 C34 C37 119.9(8) . . ? C35 C34 C37 121.1(8) . . ? C36 C35 C34 118.0(8) . . ? C36 C35 H35 121.0 . . ? C34 C35 H35 121.0 . . ? C35 C36 C31 120.7(8) . . ? C35 C36 H36 119.7 . . ? C31 C36 H36 119.7 . . ? C38 C37 C34 126.0(8) . . ? C38 C37 H37 117.0 . . ? C34 C37 H37 117.0 . . ? C37 C38 C39 126.6(9) . . ? C37 C38 H38 116.7 . . ? C39 C38 H38 116.7 . . ? C1 O1 Zn2 129.1(8) . . ? C1 O2 Zn1 129.9(8) . . ? O1W O1W Zn1 155.9(14) 2_665 . ? C7 O7 C10 121.2(6) . . ? C31 O9 C30 116.5(6) . . ? C21 O8 C20 115.1(6) . . ? O5 C39 O6 128.1(8) . . ? O5 C39 C38 119.8(8) . . ? O6 C39 C38 112.1(8) . . ? C39 O5 Zn1 129.2(6) . 6_654 ? C39 O6 Zn2 134.1(7) . 6_654 ? C29 O3 Zn1 114.9(9) . 6_554 ? C29 O4 Zn2 137.5(11) . 6_554 ? O4 C29 O3 133.2(13) . . ? O4 C29 C28 120.1(15) . . ? O3 C29 C28 106.6(12) . . ? 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 O2 C1 C2 C3 -176.6(11) . . . . ? O1 C1 C2 C3 1.4(15) . . . . ? C1 C2 C3 C4 179.1(9) . . . . ? C2 C3 C4 C5 171.5(10) . . . . ? C2 C3 C4 C9 -2.4(15) . . . . ? C9 C4 C5 C6 -2.5(13) . . . . ? C3 C4 C5 C6 -176.8(8) . . . . ? C4 C5 C6 C7 0.2(14) . . . . ? C5 C6 C7 C8 -0.6(12) . . . . ? C5 C6 C7 O7 -178.9(7) . . . . ? O7 C7 C8 C9 -178.3(7) . . . . ? C6 C7 C8 C9 3.2(12) . . . . ? C5 C4 C9 C8 5.3(12) . . . . ? C3 C4 C9 C8 179.5(8) . . . . ? C7 C8 C9 C4 -5.7(12) . . . . ? O7 C10 C11 C16 90.2(8) . . . . ? O7 C10 C11 C12 -84.3(8) . . . . ? C16 C11 C12 C13 5.4(11) . . . . ? C10 C11 C12 C13 179.9(7) . . . . ? C16 C11 C12 C18 -176.2(6) . . . . ? C10 C11 C12 C18 -1.7(10) . . . . ? C11 C12 C13 C14 -6.3(11) . . . . ? C18 C12 C13 C14 175.2(7) . . . . ? C11 C12 C13 C20 173.0(6) . . . . ? C18 C12 C13 C20 -5.4(10) . . . . ? C12 C13 C14 C15 2.7(11) . . . . ? C20 C13 C14 C15 -176.6(6) . . . . ? C12 C13 C14 C19 -177.1(7) . . . . ? C20 C13 C14 C19 3.5(10) . . . . ? C13 C14 C15 C16 1.8(10) . . . . ? C19 C14 C15 C16 -178.4(7) . . . . ? C13 C14 C15 C30 -175.6(6) . . . . ? C19 C14 C15 C30 4.3(10) . . . . ? C12 C11 C16 C15 -0.8(10) . . . . ? C10 C11 C16 C15 -175.3(6) . . . . ? C12 C11 C16 C17 -177.9(6) . . . . ? C10 C11 C16 C17 7.5(10) . . . . ? C14 C15 C16 C11 -2.7(10) . . . . ? C30 C15 C16 C11 174.6(6) . . . . ? C14 C15 C16 C17 174.5(7) . . . . ? C30 C15 C16 C17 -8.2(10) . . . . ? C12 C13 C20 O8 99.2(8) . . . . ? C14 C13 C20 O8 -81.5(8) . . . . ? C26 C21 C22 C23 -3.6(18) . . . . ? O8 C21 C22 C23 177.1(10) . . . . ? C21 C22 C23 C24 2(2) . . . . ? C22 C23 C24 C25 1(2) . . . . ? C22 C23 C24 C27 176.4(11) . . . . ? C23 C24 C25 C26 -2.5(18) . . . . ? C27 C24 C25 C26 -177.6(10) . . . . ? C22 C21 C26 C25 2.4(17) . . . . ? O8 C21 C26 C25 -178.3(9) . . . . ? C24 C25 C26 C21 0.7(17) . . . . ? C23 C24 C27 C28 3.6(19) . . . . ? C25 C24 C27 C28 178.7(13) . . . . ? C24 C27 C28 C29 179.5(10) . . . . ? C16 C15 C30 O9 89.5(8) . . . . ? C14 C15 C30 O9 -93.2(8) . . . . ? C36 C31 C32 C33 -7.5(14) . . . . ? O9 C31 C32 C33 174.6(8) . . . . ? C31 C32 C33 C34 3.0(15) . . . . ? C32 C33 C34 C35 6.4(15) . . . . ? C32 C33 C34 C37 -176.2(9) . . . . ? C33 C34 C35 C36 -11.1(15) . . . . ? C37 C34 C35 C36 171.5(10) . . . . ? C34 C35 C36 C31 6.8(16) . . . . ? C32 C31 C36 C35 2.6(15) . . . . ? O9 C31 C36 C35 -179.4(9) . . . . ? C33 C34 C37 C38 176.3(10) . . . . ? C35 C34 C37 C38 -6.4(15) . . . . ? C34 C37 C38 C39 -176.9(8) . . . . ? O2 C1 O1 Zn2 0.5(17) . . . . ? C2 C1 O1 Zn2 -177.2(6) . . . . ? O2W Zn2 O1 C1 179.3(11) . . . . ? O6 Zn2 O1 C1 -64.6(9) 6_655 . . . ? O4 Zn2 O1 C1 59.1(10) 6 . . . ? O1 C1 O2 Zn1 0.7(18) . . . . ? C2 C1 O2 Zn1 178.3(6) . . . . ? O3 Zn1 O2 C1 -82.5(11) 6 . . . ? O5 Zn1 O2 C1 66.9(10) 6_655 . . . ? O1W Zn1 O2 C1 178.0(10) . . . . ? O3 Zn1 O1W O1W -12.8(19) 6 . . 2_665 ? O5 Zn1 O1W O1W -135.4(18) 6_655 . . 2_665 ? O2 Zn1 O1W O1W 104.0(18) . . . 2_665 ? C8 C7 O7 C10 175.8(7) . . . . ? C6 C7 O7 C10 -5.7(10) . . . . ? C11 C10 O7 C7 -173.3(6) . . . . ? C32 C31 O9 C30 -6.2(11) . . . . ? C36 C31 O9 C30 175.8(8) . . . . ? C15 C30 O9 C31 -173.4(6) . . . . ? C22 C21 O8 C20 9.8(13) . . . . ? C26 C21 O8 C20 -169.5(8) . . . . ? C13 C20 O8 C21 173.1(6) . . . . ? C37 C38 C39 O5 178.9(9) . . . . ? C37 C38 C39 O6 1.9(13) . . . . ? O6 C39 O5 Zn1 -4.8(14) . . . 6_654 ? C38 C39 O5 Zn1 178.7(5) . . . 6_654 ? O5 C39 O6 Zn2 -8.1(16) . . . 6_654 ? C38 C39 O6 Zn2 168.6(7) . . . 6_654 ? Zn2 O4 C29 O3 8(3) 6_554 . . . ? Zn2 O4 C29 C28 -173.4(8) 6_554 . . . ? Zn1 O3 C29 O4 4(2) 6_554 . . . ? Zn1 O3 C29 C28 -174.5(7) 6_554 . . . ? C27 C28 C29 O4 -10(2) . . . . ? C27 C28 C29 O3 169.3(12) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.649 _refine_diff_density_min -0.979 _refine_diff_density_rms 0.135 # SQUEEZE RESULTS (APPEND TO CIF) 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 1 0.000 0.250 0.125 424.9 16.2 2 0.000 0.750 -0.125 424.9 13.0 3 -0.055 0.736 0.265 8830.6 79.1 4 0.127 0.416 0.149 7.9 0.2 5 0.127 0.916 0.851 7.7 0.4 6 0.166 0.123 0.101 7.1 0.3 7 0.166 0.623 0.899 7.3 0.1 8 0.338 0.372 0.399 8.8 0.6 9 0.338 0.872 0.601 8.6 0.8 10 0.378 0.088 0.351 8.2 0.8 11 0.501 0.250 0.375 421.8 12.8 12 0.500 0.750 0.625 423.5 16.0 13 0.373 0.584 0.649 6.8 0.4 14 0.627 0.416 0.351 7.8 0.5 15 0.627 0.916 0.649 7.9 0.2 16 0.666 0.123 0.399 7.3 0.1 17 0.666 0.623 0.601 7.1 0.3 18 0.834 0.377 0.101 7.2 0.7 19 0.834 0.877 0.899 7.4 0.6 20 0.873 0.084 0.149 6.8 0.4 21 0.873 0.584 0.851 6.5 0.7 _platon_squeeze_details ; 0.2 DMF solvent molecule was removed by the SQUEEZE process ;