# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email zhangjp7@mail.sysu.edu.cn _publ_contact_author_name 'Zhang, Jie-Peng' loop_ _publ_author_name 'Xiao-Min Liu' 'Lin-Hua Xie' 'Jian-Bin Lin' 'Rui-Biao Lin' 'Jie-Peng Zhang' 'Xiao-Ming Chen' data_1a _database_code_depnum_ccdc_archive 'CCDC 822607' #TrackingRef '- 1a-2b.R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C21 H23 N5 O6 Zn' _chemical_formula_weight 506.81 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 Orthorhombic _symmetry_space_group_name_H-M Fdd2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' 'x+1/4, -y+1/4, z+1/4' '-x+1/4, y+1/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/4, -y+3/4, z+3/4' '-x+1/4, y+3/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' 'x+3/4, -y+1/4, z+3/4' '-x+3/4, y+1/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+3/4, -y+3/4, z+1/4' '-x+3/4, y+3/4, z+1/4' _cell_length_a 28.942(3) _cell_length_b 58.653(5) _cell_length_c 21.5267(19) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 36542(6) _cell_formula_units_Z 64 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.474 _exptl_crystal_density_method . _exptl_crystal_F_000 16768 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7984 _exptl_absorpt_correction_T_max 0.8235 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33623 _diffrn_reflns_av_R_equivalents 0.0506 _diffrn_reflns_av_sigmaI/netI 0.0725 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 35 _diffrn_reflns_limit_k_min -69 _diffrn_reflns_limit_k_max 72 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.23 _diffrn_reflns_theta_max 26.00 _reflns_number_total 15614 _reflns_number_gt 9096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0950P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.461(9) _refine_ls_number_reflns 15614 _refine_ls_number_parameters 974 _refine_ls_number_restraints 73 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0664 _refine_ls_wR_factor_ref 0.1868 _refine_ls_wR_factor_gt 0.1687 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.003 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 0.872750(15) 1.257425(7) 0.97408(3) 0.06958(14) Uani 1 1 d . . . Zn2 Zn 0.616331(14) 1.109214(6) 0.97080(2) 0.06194(13) Uani 1 1 d . . . Zn3 Zn 0.872263(14) 1.001823(6) 0.72810(3) 0.05927(12) Uani 1 1 d . . . Zn4 Zn 1.114850(15) 0.864014(6) 0.73392(3) 0.06816(15) Uani 1 1 d . . . C1 C 0.85696(14) 1.22209(6) 1.0697(2) 0.0906(16) Uani 1 1 d . . . H1A H 0.8876 1.2252 1.0794 0.109 Uiso 1 1 calc R . . C2 C 0.83300(14) 1.20569(7) 1.1042(2) 0.0932(16) Uani 1 1 d . . . H2B H 0.8480 1.1980 1.1361 0.112 Uiso 1 1 calc R . . C3 C 0.78780(15) 1.20089(6) 1.0916(3) 0.0959(18) Uani 1 1 d . . . C4 C 0.76652(15) 1.21213(7) 1.0416(3) 0.1011(18) Uani 1 1 d . . . H4A H 0.7359 1.2092 1.0312 0.121 Uiso 1 1 calc R . . C5 C 0.79169(14) 1.22734(7) 1.0092(2) 0.0905(16) Uani 1 1 d . . . H5A H 0.7777 1.2342 0.9752 0.109 Uiso 1 1 calc R . . C6 C 0.69861(12) 1.13552(5) 1.01770(19) 0.0647(13) Uani 1 1 d . . . H6B H 0.7155 1.1259 0.9919 0.078 Uiso 1 1 calc R . . C7 C 0.72253(13) 1.15123(5) 1.05150(19) 0.0658(12) Uani 1 1 d . . . H7B H 0.7546 1.1517 1.0504 0.079 Uiso 1 1 calc R . . C8 C 0.69867(16) 1.16604(6) 1.0864(3) 0.1002(18) Uani 1 1 d . . . C9 C 0.65049(16) 1.16450(7) 1.0880(2) 0.1059(18) Uani 1 1 d . . . H9A H 0.6332 1.1750 1.1106 0.127 Uiso 1 1 calc R . . C10 C 0.62785(14) 1.14627(8) 1.0537(3) 0.1108(19) Uani 1 1 d . . . H10B H 0.5961 1.1442 1.0568 0.133 Uiso 1 1 calc R . . C11 C 0.68669(14) 1.09150(5) 0.89643(19) 0.0644(12) Uani 1 1 d . . . C12 C 0.71770(12) 1.07371(5) 0.87213(18) 0.0593(12) Uani 1 1 d . . . C13 C 0.75109(18) 1.07871(6) 0.8291(2) 0.0953(17) Uani 1 1 d . . . H13A H 0.7547 1.0938 0.8170 0.114 Uiso 1 1 calc R . . C14 C 0.78034(14) 1.06223(6) 0.8020(2) 0.0853(15) Uani 1 1 d . . . H14B H 0.8036 1.0665 0.7744 0.102 Uiso 1 1 calc R . . C15 C 0.77339(13) 1.03942(6) 0.81769(19) 0.0634(12) Uani 1 1 d . . . C16 C 0.73867(13) 1.03441(6) 0.85959(19) 0.0659(13) Uani 1 1 d . . . H16B H 0.7327 1.0193 0.8699 0.079 Uiso 1 1 calc R . . C17 C 0.71264(13) 1.05167(5) 0.88639(19) 0.0655(13) Uani 1 1 d . . . H17A H 0.6905 1.0477 0.9158 0.079 Uiso 1 1 calc R . . C18 C 0.80016(13) 1.02133(5) 0.79085(19) 0.0640(12) Uani 1 1 d . . . C19 C 0.94120(18) 1.02791(8) 0.6893(3) 0.1277(9) Uani 1 1 d U . . C20 C 0.96963(16) 1.04410(7) 0.6479(3) 0.1182(11) Uani 1 1 d U . . C21 C 0.9784(2) 1.03858(8) 0.5870(3) 0.148(2) Uani 1 1 d . . . H21A H 0.9651 1.0257 0.5693 0.177 Uiso 1 1 calc R . . C22 C 1.0071(2) 1.05236(8) 0.5525(3) 0.140(2) Uani 1 1 d . . . H22A H 1.0158 1.0475 0.5130 0.168 Uiso 1 1 calc R . . C23 C 1.02271(17) 1.07212(7) 0.5729(3) 0.1051(11) Uani 1 1 d U . . C24 C 1.01330(19) 1.07596(7) 0.6346(2) 0.1076(18) Uani 1 1 d . . . H24A H 1.0257 1.0890 0.6525 0.129 Uiso 1 1 calc R . . C25 C 0.98778(19) 1.06244(7) 0.6710(3) 0.1093(19) Uani 1 1 d . . . H25A H 0.9831 1.0662 0.7125 0.131 Uiso 1 1 calc R . . C26 C 1.05314(18) 1.08616(8) 0.5404(3) 0.1212(9) Uani 1 1 d U . . C27 C 0.86842(14) 0.96716(7) 0.6257(2) 0.0809(15) Uani 1 1 d . . . H27A H 0.8996 0.9708 0.6228 0.097 Uiso 1 1 calc R . . C28 C 0.85184(14) 0.95132(5) 0.5857(2) 0.0758(14) Uani 1 1 d . . . H28A H 0.8707 0.9450 0.5552 0.091 Uiso 1 1 calc R . . C29 C 0.80613(14) 0.94474(5) 0.59153(19) 0.0687(13) Uani 1 1 d . . . C30 C 0.77944(13) 0.95524(5) 0.63676(19) 0.0660(13) Uani 1 1 d . . . H30A H 0.7486 0.9513 0.6418 0.079 Uiso 1 1 calc R . . C31 C 0.79875(13) 0.97122(6) 0.6732(2) 0.0685(13) Uani 1 1 d . . . H31A H 0.7804 0.9781 0.7031 0.082 Uiso 1 1 calc R . . C32 C 0.72019(14) 0.91098(6) 0.58598(19) 0.0695(13) Uani 1 1 d . . . C33 C 0.74211(13) 0.89718(5) 0.62963(19) 0.0692(13) Uani 1 1 d . . . H33A H 0.7740 0.8981 0.6343 0.083 Uiso 1 1 calc R . . C34 C 0.71769(13) 0.88242(6) 0.6655(2) 0.0710(13) Uani 1 1 d . . . H34A H 0.7344 0.8735 0.6934 0.085 Uiso 1 1 calc R . . C35 C 0.64842(15) 0.89371(6) 0.6216(2) 0.0807(14) Uani 1 1 d . . . H35A H 0.6164 0.8929 0.6181 0.097 Uiso 1 1 calc R . . C36 C 0.67164(14) 0.90876(6) 0.5852(2) 0.0848(15) Uani 1 1 d . . . H36A H 0.6548 0.9180 0.5585 0.102 Uiso 1 1 calc R . . C37 C 0.87516(12) 0.96741(6) 0.8314(2) 0.0707(14) Uani 1 1 d . . . H37A H 0.8435 0.9699 0.8332 0.085 Uiso 1 1 calc R . . C38 C 0.89415(15) 0.95179(6) 0.8688(2) 0.0858(15) Uani 1 1 d . . . H38A H 0.8754 0.9439 0.8965 0.103 Uiso 1 1 calc R . . C39 C 0.94118(14) 0.94713(5) 0.8673(2) 0.0670(13) Uani 1 1 d . . . C40 C 0.96704(15) 0.96009(6) 0.8280(2) 0.0784(14) Uani 1 1 d . . . H40A H 0.9989 0.9581 0.8265 0.094 Uiso 1 1 calc R . . C41 C 0.94677(14) 0.97579(6) 0.7910(2) 0.0789(15) Uani 1 1 d . . . H41A H 0.9656 0.9842 0.7647 0.095 Uiso 1 1 calc R . . C42 C 1.03099(15) 0.91374(6) 0.8704(2) 0.0755(14) Uani 1 1 d . . . C43 C 1.00622(14) 0.89935(6) 0.8280(2) 0.0836(15) Uani 1 1 d . . . H43A H 0.9742 0.9000 0.8253 0.100 Uiso 1 1 calc R . . C44 C 1.03193(16) 0.88425(6) 0.7906(3) 0.0950(18) Uani 1 1 d . . . H44A H 1.0166 0.8744 0.7637 0.114 Uiso 1 1 calc R . . C45 C 1.09794(15) 0.89756(7) 0.8299(3) 0.0992(18) Uani 1 1 d . . . H45A H 1.1301 0.8978 0.8287 0.119 Uiso 1 1 calc R . . C46 C 1.07741(16) 0.91280(8) 0.8727(3) 0.113(2) Uani 1 1 d . . . H46A H 1.0947 0.9215 0.9004 0.135 Uiso 1 1 calc R . . C47 C 1.19528(15) 0.88927(6) 0.6808(2) 0.0777(15) Uani 1 1 d . . . H47A H 1.2133 0.8788 0.7022 0.093 Uiso 1 1 calc R . . C48 C 1.21707(14) 0.90541(7) 0.6471(2) 0.0859(15) Uani 1 1 d . . . H48A H 1.2492 0.9056 0.6460 0.103 Uiso 1 1 calc R . . C49 C 1.19392(15) 0.92068(6) 0.6161(2) 0.0824(15) Uani 1 1 d . . . C50 C 1.14672(16) 0.91936(7) 0.6203(3) 0.121(2) Uani 1 1 d . . . H50A H 1.1288 0.9303 0.6002 0.145 Uiso 1 1 calc R . . C51 C 1.12662(14) 0.90364(7) 0.6510(3) 0.1004(19) Uani 1 1 d . . . H51A H 1.0945 0.9029 0.6504 0.120 Uiso 1 1 calc R . . C52 C 1.28588(15) 0.95484(7) 0.6091(2) 0.0869(15) Uani 1 1 d . . . C53 C 1.33289(17) 0.95643(6) 0.5970(2) 0.0900(17) Uani 1 1 d . . . H53A H 1.3477 0.9473 0.5678 0.108 Uiso 1 1 calc R . . C54 C 1.35593(14) 0.97276(6) 0.6317(2) 0.0760(15) Uani 1 1 d . . . H54A H 1.3874 0.9742 0.6243 0.091 Uiso 1 1 calc R . . C55 C 1.29495(15) 0.98267(7) 0.6815(2) 0.0852(16) Uani 1 1 d . . . H55A H 1.2816 0.9917 0.7121 0.102 Uiso 1 1 calc R . . C56 C 1.26613(17) 0.96830(7) 0.6535(2) 0.0893(16) Uani 1 1 d . . . H56A H 1.2349 0.9675 0.6635 0.107 Uiso 1 1 calc R . . C57 C 1.0541(2) 0.83989(8) 0.6733(3) 0.1180(8) Uani 1 1 d U . . C58 C 1.02151(18) 0.82623(7) 0.6349(3) 0.1039(11) Uani 1 1 d U . . C59 C 1.0052(2) 0.80536(7) 0.6552(3) 0.127(2) Uani 1 1 d . . . H59A H 1.0124 0.8005 0.6952 0.153 Uiso 1 1 calc R . . C60 C 0.97935(18) 0.79201(7) 0.6191(2) 0.1056(18) Uani 1 1 d . . . H60A H 0.9709 0.7776 0.6333 0.127 Uiso 1 1 calc R . . C61 C 0.96506(13) 0.79883(6) 0.56216(18) 0.0590(11) Uani 1 1 d . . . C62 C 0.98186(19) 0.81993(7) 0.5413(2) 0.1054(19) Uani 1 1 d . . . H62A H 0.9741 0.8253 0.5020 0.126 Uiso 1 1 calc R . . C63 C 1.01084(19) 0.83296(7) 0.5807(3) 0.120(2) Uani 1 1 d . . . H63A H 1.0224 0.8468 0.5665 0.144 Uiso 1 1 calc R . . C64 C 0.93299(15) 0.78389(8) 0.5219(2) 0.0925(17) Uani 1 1 d . . . C65 C 1.18684(14) 0.84722(6) 0.8047(2) 0.0712(13) Uani 1 1 d . . . C66 C 1.21774(14) 0.82833(6) 0.82961(19) 0.0645(12) Uani 1 1 d . . . C67 C 1.21259(14) 0.80602(5) 0.8115(2) 0.0658(13) Uani 1 1 d . . . H67A H 1.1892 0.8020 0.7840 0.079 Uiso 1 1 calc R . . C68 C 1.24138(14) 0.79001(6) 0.8335(2) 0.0715(14) Uani 1 1 d . . . H68A H 1.2383 0.7751 0.8197 0.086 Uiso 1 1 calc R . . C69 C 1.27571(14) 0.79519(6) 0.8764(2) 0.0756(14) Uani 1 1 d . . . C70 C 1.28016(17) 0.81718(7) 0.8976(3) 0.1000(18) Uani 1 1 d . . . H70A H 1.3017 0.8207 0.9282 0.120 Uiso 1 1 calc R . . C71 C 1.25129(14) 0.83452(6) 0.8722(2) 0.0725(13) Uani 1 1 d . . . H71A H 1.2549 0.8497 0.8839 0.087 Uiso 1 1 calc R . . C72 C 1.30875(16) 0.77768(6) 0.9048(3) 0.0961(18) Uani 1 1 d . . . N1 N 0.65241(11) 1.13287(5) 1.01876(19) 0.0830(13) Uani 1 1 d . . . N2 N 0.71862(14) 1.18273(6) 1.1233(2) 0.1275(18) Uani 1 1 d . . . H2A H 0.7015 1.1922 1.1434 0.153 Uiso 1 1 calc R . . N3 N 0.76787(12) 1.18410(6) 1.1277(2) 0.1120(15) Uani 1 1 d . . . H3A H 0.7838 1.1752 1.1511 0.134 Uiso 1 1 calc R . . N4 N 0.83636(12) 1.23341(5) 1.02265(18) 0.0818(12) Uani 1 1 d . . . N5 N 0.84369(11) 0.97784(5) 0.66867(17) 0.0699(11) Uani 1 1 d . . . N6 N 0.78733(15) 0.92885(5) 0.5517(2) 0.1110(16) Uani 1 1 d . . . H6A H 0.8052 0.9206 0.5290 0.133 Uiso 1 1 calc R . . N7 N 0.74062(13) 0.92603(5) 0.5480(2) 0.0949(13) Uani 1 1 d . . . H7A H 0.7246 0.9338 0.5218 0.114 Uiso 1 1 calc R . . N8 N 0.67059(11) 0.87937(5) 0.66440(17) 0.0731(11) Uani 1 1 d . . . N9 N 0.90171(10) 0.97996(5) 0.78996(17) 0.0698(11) Uani 1 1 d . . . N10 N 0.95882(12) 0.93082(5) 0.90433(17) 0.0789(12) Uani 1 1 d . . . H10A H 0.9406 0.9223 0.9256 0.095 Uiso 1 1 calc R . . N11 N 1.00808(13) 0.92766(5) 0.9085(2) 0.0930(14) Uani 1 1 d . . . H11A H 1.0232 0.9350 0.9364 0.112 Uiso 1 1 calc R . . N12 N 1.07912(11) 0.88392(5) 0.79353(18) 0.0704(11) Uani 1 1 d . . . N13 N 1.15086(11) 0.88749(5) 0.68532(16) 0.0647(10) Uani 1 1 d . . . N14 N 1.21294(16) 0.93636(8) 0.5840(3) 0.143(2) Uani 1 1 d . . . H14A H 1.1946 0.9460 0.5668 0.171 Uiso 1 1 calc R . . N15 N 1.26102(15) 0.93979(7) 0.5734(2) 0.1160(17) Uani 1 1 d . . . H15A H 1.2747 0.9324 0.5443 0.139 Uiso 1 1 calc R . . N16 N 1.33885(11) 0.98602(5) 0.67283(17) 0.0731(11) Uani 1 1 d . . . O1 O 0.68718(12) 1.11089(4) 0.87466(16) 0.1120(12) Uani 1 1 d . . . O2 O 0.66152(9) 1.08605(4) 0.94313(13) 0.0695(9) Uani 1 1 d . . . O3 O 0.83140(10) 1.02717(4) 0.75200(14) 0.0803(10) Uani 1 1 d . . . O4 O 0.79156(10) 1.00120(4) 0.80421(15) 0.0882(10) Uani 1 1 d . . . O5 O 0.93839(13) 1.03278(6) 0.7480(2) 0.1435(12) Uani 1 1 d U . . O6 O 0.91617(11) 1.01543(5) 0.6661(2) 0.1332(10) Uani 1 1 d U . . O7 O 1.06301(13) 1.08351(6) 0.48753(19) 0.1303(10) Uani 1 1 d U . . O8 O 1.07300(13) 1.10179(6) 0.5580(2) 0.1456(10) Uani 1 1 d U . . O9 O 1.07425(13) 0.85611(6) 0.6566(2) 0.1370(10) Uani 1 1 d U . . O10 O 1.05665(13) 0.83539(5) 0.7330(2) 0.1261(10) Uani 1 1 d U . . O11 O 0.90950(10) 0.76910(5) 0.54766(16) 0.0965(11) Uani 1 1 d . . . O12 O 0.93453(12) 0.78727(6) 0.46305(18) 0.1172(13) Uani 1 1 d . . . O13 O 1.16018(9) 0.84080(4) 0.75681(14) 0.0744(9) Uani 1 1 d . . . O14 O 1.18669(12) 0.86609(4) 0.82565(16) 0.1062(12) Uani 1 1 d . . . O15 O 1.32976(12) 0.78112(5) 0.95200(19) 0.1102(13) Uani 1 1 d . . . O16 O 1.31384(14) 0.75962(5) 0.8733(2) 0.1574(18) 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 0.0543(2) 0.0670(2) 0.0874(3) 0.0027(3) -0.0177(2) -0.0011(2) Zn2 0.0505(2) 0.0542(2) 0.0812(3) 0.0016(2) 0.0086(2) -0.00025(18) Zn3 0.0469(2) 0.05621(19) 0.0747(3) 0.0006(3) 0.0091(2) -0.00300(18) Zn4 0.0523(2) 0.0571(2) 0.0951(4) -0.0006(3) -0.0087(3) -0.00032(19) C1 0.054(2) 0.075(2) 0.143(4) 0.037(3) -0.033(3) -0.012(2) C2 0.063(2) 0.094(2) 0.122(4) 0.045(3) -0.022(3) -0.033(2) C3 0.069(3) 0.057(2) 0.161(5) -0.019(3) -0.004(3) -0.010(2) C4 0.054(2) 0.095(3) 0.154(5) 0.010(3) -0.017(3) -0.027(2) C5 0.046(2) 0.097(3) 0.128(4) 0.006(3) -0.032(2) 0.003(2) C6 0.0368(19) 0.067(2) 0.090(3) 0.005(2) 0.005(2) 0.0001(17) C7 0.049(2) 0.063(2) 0.085(3) -0.007(2) 0.016(2) -0.0040(18) C8 0.084(3) 0.074(2) 0.142(5) 0.000(3) 0.015(3) -0.047(2) C9 0.069(3) 0.095(3) 0.154(4) -0.050(3) 0.044(3) -0.027(2) C10 0.049(2) 0.122(3) 0.161(5) -0.066(3) 0.029(3) -0.008(2) C11 0.064(2) 0.0553(18) 0.074(3) 0.0123(19) 0.002(2) 0.0116(17) C12 0.0431(19) 0.0617(19) 0.073(3) -0.0130(19) 0.004(2) 0.0022(16) C13 0.119(4) 0.056(2) 0.111(4) 0.020(2) 0.036(3) 0.005(2) C14 0.067(3) 0.078(2) 0.110(4) 0.016(3) 0.033(3) 0.010(2) C15 0.052(2) 0.0591(18) 0.079(3) 0.019(2) 0.007(2) 0.0153(16) C16 0.061(2) 0.0559(19) 0.081(3) -0.003(2) -0.006(2) 0.0080(18) C17 0.060(2) 0.0591(19) 0.078(3) 0.014(2) 0.005(2) -0.0064(18) C18 0.058(2) 0.0558(18) 0.079(3) -0.005(2) 0.003(2) -0.0008(17) C19 0.0726(16) 0.1022(16) 0.2083(17) 0.0062(16) 0.0577(16) -0.0098(14) C20 0.069(2) 0.0863(19) 0.199(2) 0.017(2) 0.051(2) -0.0035(16) C21 0.158(4) 0.109(3) 0.176(6) -0.020(4) 0.062(4) -0.081(3) C22 0.143(4) 0.142(4) 0.134(5) -0.015(4) 0.035(4) -0.078(3) C23 0.082(2) 0.1039(19) 0.129(2) 0.0436(19) 0.0042(18) -0.0406(16) C24 0.137(4) 0.103(3) 0.082(4) 0.027(3) 0.009(3) -0.053(3) C25 0.125(4) 0.113(3) 0.090(4) 0.016(3) -0.007(3) -0.048(3) C26 0.1025(16) 0.1189(15) 0.1422(15) 0.0559(14) 0.0079(15) -0.0496(13) C27 0.058(2) 0.093(3) 0.092(3) -0.018(2) 0.031(2) 0.009(2) C28 0.058(2) 0.061(2) 0.108(3) -0.030(2) 0.029(2) -0.0107(18) C29 0.071(2) 0.0540(18) 0.081(3) -0.009(2) 0.027(2) -0.0130(18) C30 0.050(2) 0.0523(17) 0.096(3) -0.014(2) 0.015(2) -0.0140(16) C31 0.050(2) 0.070(2) 0.086(3) -0.001(2) 0.013(2) -0.0054(18) C32 0.076(2) 0.0572(19) 0.075(3) -0.004(2) -0.027(2) -0.0200(19) C33 0.052(2) 0.071(2) 0.085(3) -0.009(2) 0.007(2) -0.0205(18) C34 0.045(2) 0.081(2) 0.087(3) -0.004(2) -0.015(2) 0.0067(19) C35 0.058(2) 0.093(3) 0.091(3) 0.007(3) -0.012(2) -0.021(2) C36 0.066(3) 0.071(2) 0.118(4) 0.031(2) 0.012(3) -0.004(2) C37 0.042(2) 0.063(2) 0.107(3) 0.023(2) 0.019(2) 0.0071(16) C38 0.055(2) 0.079(2) 0.123(4) 0.033(3) 0.018(3) 0.005(2) C39 0.063(2) 0.058(2) 0.080(3) -0.006(2) 0.007(2) 0.0113(18) C40 0.062(2) 0.076(2) 0.097(3) -0.001(2) -0.005(2) 0.023(2) C41 0.060(2) 0.063(2) 0.113(4) 0.011(2) 0.016(3) -0.002(2) C42 0.074(3) 0.075(2) 0.078(3) 0.003(2) -0.003(2) 0.023(2) C43 0.051(2) 0.090(3) 0.109(4) 0.024(3) -0.009(2) 0.015(2) C44 0.070(3) 0.067(2) 0.148(5) -0.010(3) -0.008(3) 0.004(2) C45 0.051(2) 0.100(3) 0.147(5) -0.030(3) -0.023(3) 0.003(2) C46 0.068(3) 0.134(4) 0.136(5) -0.018(4) -0.036(3) 0.042(3) C47 0.064(3) 0.085(3) 0.085(3) -0.006(2) -0.012(2) 0.001(2) C48 0.044(2) 0.099(3) 0.115(4) -0.023(3) 0.006(2) -0.018(2) C49 0.073(3) 0.0597(19) 0.115(4) 0.028(2) -0.004(3) -0.0287(19) C50 0.057(3) 0.114(3) 0.192(5) 0.079(3) -0.023(3) -0.021(3) C51 0.050(2) 0.071(2) 0.181(5) 0.048(3) 0.003(3) -0.0076(19) C52 0.066(3) 0.106(3) 0.089(3) 0.029(3) -0.026(2) -0.035(2) C53 0.094(3) 0.072(2) 0.104(4) 0.023(2) 0.007(3) -0.011(2) C54 0.049(2) 0.069(2) 0.110(4) 0.002(2) 0.003(3) 0.001(2) C55 0.072(3) 0.089(3) 0.094(4) 0.012(3) 0.003(3) 0.005(2) C56 0.078(3) 0.095(3) 0.094(4) -0.002(3) 0.012(3) -0.026(2) C57 0.1063(16) 0.1069(14) 0.1409(15) -0.0415(14) 0.0003(15) -0.0364(14) C58 0.086(2) 0.101(2) 0.125(2) -0.029(2) 0.0010(19) -0.0308(17) C59 0.183(5) 0.087(3) 0.112(4) 0.002(3) -0.079(4) -0.036(3) C60 0.128(4) 0.093(3) 0.096(4) 0.007(3) -0.021(3) -0.055(3) C61 0.054(2) 0.072(2) 0.052(2) -0.0146(19) 0.0059(19) -0.0061(18) C62 0.127(4) 0.086(3) 0.103(4) -0.015(3) -0.035(4) -0.007(3) C63 0.134(4) 0.086(3) 0.139(5) -0.006(3) 0.044(4) -0.053(3) C64 0.047(2) 0.111(3) 0.119(4) 0.004(3) 0.003(3) -0.003(2) C65 0.068(2) 0.0553(19) 0.090(3) 0.006(2) -0.018(2) 0.0065(19) C66 0.067(2) 0.064(2) 0.063(3) -0.004(2) -0.014(2) 0.0015(19) C67 0.062(2) 0.0511(18) 0.084(3) 0.003(2) -0.004(2) -0.0017(18) C68 0.076(3) 0.0566(19) 0.082(3) 0.005(2) -0.020(2) -0.010(2) C69 0.069(3) 0.060(2) 0.097(3) 0.005(2) -0.025(2) 0.008(2) C70 0.094(3) 0.083(3) 0.123(4) 0.004(3) -0.042(3) 0.017(2) C71 0.067(2) 0.066(2) 0.084(3) -0.017(2) -0.026(2) 0.011(2) C72 0.066(3) 0.053(2) 0.169(5) 0.002(3) 0.012(3) 0.008(2) N1 0.0517(19) 0.0654(18) 0.132(3) 0.005(2) 0.017(2) -0.0005(16) N2 0.094(3) 0.115(3) 0.174(4) -0.052(3) 0.013(3) -0.054(2) N3 0.072(2) 0.130(3) 0.134(4) 0.005(3) 0.029(2) -0.062(2) N4 0.0568(19) 0.0697(18) 0.119(3) 0.004(2) -0.024(2) -0.0076(17) N5 0.0502(18) 0.0651(17) 0.094(3) 0.0018(17) -0.0204(18) -0.0098(15) N6 0.106(3) 0.079(2) 0.149(4) -0.030(2) 0.032(3) -0.029(2) N7 0.077(2) 0.097(2) 0.111(3) -0.007(2) 0.001(2) -0.0456(19) N8 0.061(2) 0.0658(17) 0.093(3) -0.0043(19) -0.0076(19) 0.0014(16) N9 0.0448(17) 0.0636(17) 0.101(3) 0.0172(18) 0.0100(18) -0.0032(15) N10 0.058(2) 0.091(2) 0.088(3) 0.020(2) 0.0113(19) 0.0142(18) N11 0.084(3) 0.098(2) 0.097(3) -0.016(2) -0.016(2) 0.035(2) N12 0.0452(17) 0.0593(16) 0.107(3) 0.0057(19) -0.0050(19) 0.0093(15) N13 0.0459(17) 0.0698(17) 0.078(2) 0.0036(17) 0.0009(17) -0.0036(15) N14 0.094(3) 0.136(3) 0.198(5) 0.030(4) -0.056(3) -0.003(3) N15 0.097(3) 0.119(3) 0.132(4) 0.016(3) 0.008(3) -0.037(3) N16 0.0506(18) 0.0722(18) 0.096(3) -0.0030(19) 0.0268(18) -0.0048(16) O1 0.122(2) 0.0795(16) 0.135(3) 0.0435(17) 0.067(2) 0.0474(16) O2 0.0578(15) 0.0575(13) 0.093(2) -0.0045(14) 0.0150(15) 0.0074(12) O3 0.0781(18) 0.0738(15) 0.089(2) -0.0060(16) 0.0212(17) 0.0077(14) O4 0.0839(19) 0.0650(14) 0.116(2) -0.0143(16) 0.0323(18) 0.0132(14) O5 0.090(2) 0.152(2) 0.1883(19) 0.037(2) 0.027(2) -0.027(2) O6 0.0836(17) 0.0936(16) 0.222(2) -0.0030(17) 0.0706(17) -0.0216(14) O7 0.107(2) 0.1256(18) 0.1584(17) 0.0535(16) 0.0302(18) -0.0168(17) O8 0.134(2) 0.1444(17) 0.158(2) 0.0617(16) -0.009(2) -0.0775(15) O9 0.124(2) 0.1318(17) 0.156(2) -0.0523(16) 0.0134(19) -0.0592(15) O10 0.116(2) 0.1087(17) 0.1536(17) -0.0373(16) -0.0332(18) -0.0142(17) O11 0.0819(19) 0.0959(17) 0.112(3) 0.0155(18) -0.0197(19) -0.0393(16) O12 0.076(2) 0.148(3) 0.128(3) -0.013(3) -0.010(2) -0.028(2) O13 0.0645(16) 0.0687(14) 0.090(2) -0.0133(15) -0.0180(16) 0.0061(13) O14 0.138(3) 0.0626(14) 0.118(2) -0.0364(16) -0.056(2) 0.0378(16) O15 0.079(2) 0.100(2) 0.152(3) 0.002(2) -0.026(2) 0.0194(17) O16 0.142(3) 0.101(2) 0.229(5) -0.038(3) -0.067(3) 0.051(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O15 1.925(3) 13_455 ? Zn1 N16 2.007(3) 4_755 ? Zn1 O11 2.027(3) 5 ? Zn1 N4 2.046(3) . ? Zn1 C64 2.552(5) 5 ? Zn2 O2 1.978(2) . ? Zn2 N8 2.004(3) 4_655 ? Zn2 N1 2.020(3) . ? Zn2 O7 2.187(3) 9_455 ? Zn2 O8 2.299(4) 9_455 ? Zn3 O3 1.968(3) . ? Zn3 O6 2.009(4) . ? Zn3 N9 2.036(3) . ? Zn3 N5 2.073(3) . ? Zn4 O13 1.954(3) . ? Zn4 N13 2.019(3) . ? Zn4 N12 2.020(3) . ? Zn4 O9 2.089(4) . ? Zn4 O10 2.378(3) . ? C1 N4 1.350(5) . ? C1 C2 1.399(6) . ? C2 C3 1.366(6) . ? C3 N3 1.382(6) . ? C3 C4 1.403(7) . ? C4 C5 1.346(6) . ? C5 N4 1.372(5) . ? C6 N1 1.346(5) . ? C6 C7 1.363(5) . ? C7 C8 1.340(6) . ? C8 N2 1.387(6) . ? C8 C9 1.398(6) . ? C9 C10 1.455(6) . ? C10 N1 1.300(6) . ? C11 O1 1.230(4) . ? C11 O2 1.282(5) . ? C11 C12 1.472(5) . ? C12 C17 1.337(4) . ? C12 C13 1.371(6) . ? C13 C14 1.411(6) . ? C14 C15 1.395(5) . ? C15 C16 1.382(5) . ? C15 C18 1.435(5) . ? C16 C17 1.388(5) . ? C18 O4 1.241(4) . ? C18 O3 1.278(5) . ? C19 O6 1.145(6) . ? C19 O5 1.297(8) . ? C19 C20 1.542(7) . ? C20 C25 1.296(7) . ? C20 C21 1.373(9) . ? C21 C22 1.377(7) . ? C22 C23 1.319(7) . ? C23 C24 1.374(7) . ? C23 C26 1.394(7) . ? C24 C25 1.337(7) . ? C26 O8 1.146(6) . ? C26 O7 1.183(7) . ? C27 N5 1.327(5) . ? C27 C28 1.354(6) . ? C28 C29 1.384(5) . ? C29 N6 1.378(5) . ? C29 C30 1.387(5) . ? C30 C31 1.344(5) . ? C31 N5 1.361(5) . ? C32 N7 1.340(5) . ? C32 C33 1.393(5) . ? C32 C36 1.411(6) . ? C33 C34 1.359(5) . ? C34 N8 1.375(5) . ? C35 C36 1.359(6) . ? C35 N8 1.402(5) . ? C37 C38 1.338(6) . ? C37 N9 1.389(5) . ? C38 C39 1.389(6) . ? C39 N10 1.345(5) . ? C39 C40 1.362(6) . ? C40 C41 1.351(6) . ? C41 N9 1.327(5) . ? C42 N11 1.334(5) . ? C42 C46 1.346(6) . ? C42 C43 1.435(6) . ? C43 C44 1.410(6) . ? C44 N12 1.368(5) . ? C45 N12 1.244(5) . ? C45 C46 1.415(7) . ? C47 N13 1.293(5) . ? C47 C48 1.349(6) . ? C48 C49 1.303(6) . ? C49 N14 1.274(6) . ? C49 C50 1.371(6) . ? C50 C51 1.274(6) . ? C51 N13 1.391(5) . ? C52 C56 1.365(6) . ? C52 N15 1.374(6) . ? C52 C53 1.388(6) . ? C53 C54 1.387(6) . ? C54 N16 1.277(5) . ? C55 N16 1.299(5) . ? C55 C56 1.330(6) . ? C57 O9 1.172(6) . ? C57 O10 1.316(7) . ? C57 C58 1.488(7) . ? C58 C63 1.269(8) . ? C58 C59 1.384(6) . ? C59 C60 1.334(7) . ? C60 C61 1.353(6) . ? C61 C62 1.403(6) . ? C61 C64 1.543(6) . ? C62 C63 1.417(7) . ? C64 O11 1.234(5) . ? C64 O12 1.283(6) . ? C64 Zn1 2.552(5) 5_544 ? C65 O14 1.195(4) . ? C65 O13 1.342(5) . ? C65 C66 1.521(5) . ? C66 C67 1.373(5) . ? C66 C71 1.384(5) . ? C67 C68 1.342(5) . ? C68 C69 1.390(6) . ? C69 C70 1.374(5) . ? C69 C72 1.531(6) . ? C70 C71 1.426(6) . ? C72 O15 1.201(6) . ? C72 O16 1.266(6) . ? N2 N3 1.431(5) . ? N6 N7 1.365(5) . ? N8 Zn2 2.004(3) 8_644 ? N10 N11 1.440(5) . ? N14 N15 1.424(6) . ? N16 Zn1 2.007(3) 8_744 ? O7 Zn2 2.187(3) 9_554 ? O8 Zn2 2.299(4) 9_554 ? O11 Zn1 2.027(3) 5_544 ? O15 Zn1 1.925(3) 13_545 ? 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 O15 Zn1 N16 132.36(16) 13_455 4_755 ? O15 Zn1 O11 106.75(14) 13_455 5 ? N16 Zn1 O11 110.50(13) 4_755 5 ? O15 Zn1 N4 106.89(14) 13_455 . ? N16 Zn1 N4 97.77(13) 4_755 . ? O11 Zn1 N4 95.93(14) 5 . ? O15 Zn1 C64 95.86(14) 13_455 5 ? N16 Zn1 C64 102.94(14) 4_755 5 ? O11 Zn1 C64 28.43(14) 5 5 ? N4 Zn1 C64 124.36(16) . 5 ? O2 Zn2 N8 125.14(13) . 4_655 ? O2 Zn2 N1 106.50(12) . . ? N8 Zn2 N1 100.37(13) 4_655 . ? O2 Zn2 O7 92.44(12) . 9_455 ? N8 Zn2 O7 97.48(14) 4_655 9_455 ? N1 Zn2 O7 138.93(16) . 9_455 ? O2 Zn2 O8 118.45(12) . 9_455 ? N8 Zn2 O8 108.39(14) 4_655 9_455 ? N1 Zn2 O8 89.71(14) . 9_455 ? O7 Zn2 O8 49.46(14) 9_455 9_455 ? O3 Zn3 O6 104.70(12) . . ? O3 Zn3 N9 123.81(13) . . ? O6 Zn3 N9 114.85(14) . . ? O3 Zn3 N5 115.73(12) . . ? O6 Zn3 N5 96.41(15) . . ? N9 Zn3 N5 98.24(12) . . ? O13 Zn4 N13 105.03(12) . . ? O13 Zn4 N12 125.90(13) . . ? N13 Zn4 N12 101.49(12) . . ? O13 Zn4 O9 115.07(13) . . ? N13 Zn4 O9 91.65(14) . . ? N12 Zn4 O9 110.28(14) . . ? O13 Zn4 O10 89.18(11) . . ? N13 Zn4 O10 147.43(14) . . ? N12 Zn4 O10 92.90(13) . . ? O9 Zn4 O10 55.85(15) . . ? N4 C1 C2 121.2(4) . . ? C3 C2 C1 120.7(4) . . ? C2 C3 N3 115.7(4) . . ? C2 C3 C4 118.5(4) . . ? N3 C3 C4 125.7(4) . . ? C5 C4 C3 118.1(4) . . ? C4 C5 N4 124.9(4) . . ? N1 C6 C7 125.0(4) . . ? C8 C7 C6 118.4(4) . . ? C7 C8 N2 124.3(4) . . ? C7 C8 C9 119.1(4) . . ? N2 C8 C9 116.5(4) . . ? C8 C9 C10 118.9(4) . . ? N1 C10 C9 119.5(4) . . ? O1 C11 O2 122.4(3) . . ? O1 C11 C12 120.9(4) . . ? O2 C11 C12 116.6(3) . . ? C17 C12 C13 116.0(3) . . ? C17 C12 C11 122.5(3) . . ? C13 C12 C11 121.2(3) . . ? C12 C13 C14 123.8(4) . . ? C15 C14 C13 118.0(4) . . ? C16 C15 C14 117.9(3) . . ? C16 C15 C18 119.9(3) . . ? C14 C15 C18 122.2(4) . . ? C15 C16 C17 120.7(3) . . ? C12 C17 C16 123.4(4) . . ? O4 C18 O3 123.3(3) . . ? O4 C18 C15 120.1(4) . . ? O3 C18 C15 116.6(3) . . ? O6 C19 O5 121.8(5) . . ? O6 C19 C20 118.6(6) . . ? O5 C19 C20 117.5(5) . . ? C25 C20 C21 119.2(5) . . ? C25 C20 C19 120.3(6) . . ? C21 C20 C19 120.4(5) . . ? C20 C21 C22 119.2(5) . . ? C23 C22 C21 122.9(6) . . ? C22 C23 C24 113.4(5) . . ? C22 C23 C26 124.6(6) . . ? C24 C23 C26 120.9(5) . . ? C25 C24 C23 125.3(5) . . ? C20 C25 C24 119.4(5) . . ? O8 C26 O7 107.5(5) . . ? O8 C26 C23 128.6(6) . . ? O7 C26 C23 123.9(5) . . ? N5 C27 C28 125.2(4) . . ? C27 C28 C29 118.2(4) . . ? N6 C29 C28 120.7(4) . . ? N6 C29 C30 121.1(4) . . ? C28 C29 C30 118.2(3) . . ? C31 C30 C29 119.2(4) . . ? C30 C31 N5 123.7(4) . . ? N7 C32 C33 126.4(4) . . ? N7 C32 C36 119.5(4) . . ? C33 C32 C36 114.1(4) . . ? C34 C33 C32 121.1(4) . . ? C33 C34 N8 126.1(4) . . ? C36 C35 N8 122.8(4) . . ? C35 C36 C32 123.0(4) . . ? C38 C37 N9 121.5(3) . . ? C37 C38 C39 121.5(4) . . ? N10 C39 C40 123.8(4) . . ? N10 C39 C38 119.9(4) . . ? C40 C39 C38 116.3(4) . . ? C41 C40 C39 120.5(4) . . ? N9 C41 C40 124.3(4) . . ? N11 C42 C46 119.9(4) . . ? N11 C42 C43 120.2(4) . . ? C46 C42 C43 119.9(4) . . ? C44 C43 C42 118.0(4) . . ? N12 C44 C43 120.6(4) . . ? N12 C45 C46 129.2(4) . . ? C42 C46 C45 114.9(4) . . ? N13 C47 C48 124.1(4) . . ? C49 C48 C47 121.2(4) . . ? N14 C49 C48 123.5(4) . . ? N14 C49 C50 120.5(4) . . ? C48 C49 C50 116.0(4) . . ? C51 C50 C49 122.0(5) . . ? C50 C51 N13 122.5(4) . . ? C56 C52 N15 122.9(4) . . ? C56 C52 C53 120.2(4) . . ? N15 C52 C53 116.8(4) . . ? C54 C53 C52 114.6(4) . . ? N16 C54 C53 127.5(4) . . ? N16 C55 C56 130.1(4) . . ? C55 C56 C52 114.9(4) . . ? O9 C57 O10 115.7(5) . . ? O9 C57 C58 125.6(6) . . ? O10 C57 C58 118.1(5) . . ? C63 C58 C59 118.9(5) . . ? C63 C58 C57 119.8(5) . . ? C59 C58 C57 121.1(5) . . ? C60 C59 C58 121.7(5) . . ? C59 C60 C61 121.8(4) . . ? C60 C61 C62 116.4(4) . . ? C60 C61 C64 121.6(4) . . ? C62 C61 C64 122.0(4) . . ? C61 C62 C63 119.2(5) . . ? C58 C63 C62 121.8(5) . . ? O11 C64 O12 124.8(4) . . ? O11 C64 C61 118.6(4) . . ? O12 C64 C61 116.5(4) . . ? O11 C64 Zn1 51.5(2) . 5_544 ? O12 C64 Zn1 73.7(3) . 5_544 ? C61 C64 Zn1 169.5(3) . 5_544 ? O14 C65 O13 123.2(4) . . ? O14 C65 C66 122.9(4) . . ? O13 C65 C66 113.9(3) . . ? C67 C66 C71 120.9(4) . . ? C67 C66 C65 122.0(4) . . ? C71 C66 C65 117.1(3) . . ? C68 C67 C66 119.9(4) . . ? C67 C68 C69 121.7(3) . . ? C70 C69 C68 119.5(4) . . ? C70 C69 C72 116.0(4) . . ? C68 C69 C72 124.4(3) . . ? C69 C70 C71 119.2(4) . . ? C66 C71 C70 118.6(3) . . ? O15 C72 O16 122.3(4) . . ? O15 C72 C69 122.8(4) . . ? O16 C72 C69 114.8(5) . . ? C10 N1 C6 118.9(4) . . ? C10 N1 Zn2 115.4(3) . . ? C6 N1 Zn2 125.7(3) . . ? C8 N2 N3 119.5(4) . . ? C3 N3 N2 114.7(4) . . ? C1 N4 C5 116.5(4) . . ? C1 N4 Zn1 119.7(3) . . ? C5 N4 Zn1 123.8(3) . . ? C27 N5 C31 115.5(3) . . ? C27 N5 Zn3 122.4(3) . . ? C31 N5 Zn3 122.1(3) . . ? N7 N6 C29 120.7(4) . . ? C32 N7 N6 118.7(4) . . ? C34 N8 C35 112.8(3) . . ? C34 N8 Zn2 126.5(3) . 8_644 ? C35 N8 Zn2 120.5(3) . 8_644 ? C41 N9 C37 115.8(3) . . ? C41 N9 Zn3 122.6(3) . . ? C37 N9 Zn3 121.5(2) . . ? C39 N10 N11 120.2(3) . . ? C42 N11 N10 122.2(4) . . ? C45 N12 C44 117.2(4) . . ? C45 N12 Zn4 123.2(3) . . ? C44 N12 Zn4 119.4(3) . . ? C47 N13 C51 114.0(3) . . ? C47 N13 Zn4 127.4(3) . . ? C51 N13 Zn4 118.6(3) . . ? C49 N14 N15 127.6(4) . . ? C52 N15 N14 120.8(4) . . ? C54 N16 C55 112.7(4) . . ? C54 N16 Zn1 123.2(3) . 8_744 ? C55 N16 Zn1 123.9(3) . 8_744 ? C11 O2 Zn2 116.1(2) . . ? C18 O3 Zn3 113.2(2) . . ? C19 O6 Zn3 111.3(4) . . ? C26 O7 Zn2 103.8(3) . 9_554 ? C26 O8 Zn2 98.9(4) . 9_554 ? C57 O9 Zn4 102.5(4) . . ? C57 O10 Zn4 84.6(3) . . ? C64 O11 Zn1 100.1(3) . 5_544 ? C65 O13 Zn4 112.6(2) . . ? C72 O15 Zn1 114.5(3) . 13_545 ? 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 C8 N2 N3 C3 100.8(5) . . . . ? C29 N6 N7 C32 -89.6(5) . . . . ? C39 N10 N11 C42 -89.3(5) . . . . ? C49 N14 N15 C52 -96.2(6) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.599 _refine_diff_density_min -0.311 _refine_diff_density_rms 0.073 # 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 -0.002 0.000 0.476 1371.9 285.3 2 -0.002 0.000 0.976 1371.9 285.3 3 0.006 0.250 0.226 1371.8 279.9 4 -0.010 0.250 0.726 1371.8 279.9 5 -0.002 0.500 0.476 1371.9 285.3 6 -0.002 0.500 0.976 1371.9 285.3 7 0.006 0.750 0.726 1371.8 279.9 8 -0.010 0.750 0.226 1371.8 279.9 _platon_squeeze_details ; ; data_1b _database_code_depnum_ccdc_archive 'CCDC 822608' #TrackingRef '- 1a-2b.R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H22 N4 O6 Zn' _chemical_formula_weight 479.79 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 Orthorhombic _symmetry_space_group_name_H-M Pnna loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z' '-x+1/2, y+1/2, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z' 'x-1/2, -y-1/2, z-1/2' '-x, y-1/2, z-1/2' _cell_length_a 29.50(2) _cell_length_b 14.724(13) _cell_length_c 10.274(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4463(7) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method . _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7631 _exptl_absorpt_correction_T_max 0.8121 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15206 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_sigmaI/netI 0.0959 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 26.00 _reflns_number_total 4324 _reflns_number_gt 1660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0580P)^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 4324 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1532 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1677 _refine_ls_wR_factor_gt 0.1476 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.47203(3) 1.2500 0.7500 0.0620(3) Uani 1 2 d S . . Zn2 Zn 0.75755(3) 0.7500 0.7500 0.0627(3) Uani 1 2 d S . . C1 C 0.4368(2) 1.1164(5) 0.9059(6) 0.0659(17) Uani 1 1 d . . . C2 C 0.40202(18) 1.0532(4) 0.9658(6) 0.0649(17) Uani 1 1 d . . . C3 C 0.35731(18) 1.0542(5) 0.9246(6) 0.0758(19) Uani 1 1 d . . . H3A H 0.3485 1.0933 0.8582 0.091 Uiso 1 1 calc R . . C4 C 0.3260(2) 0.9979(6) 0.9814(8) 0.097(3) Uani 1 1 d . . . H4A H 0.2961 0.9995 0.9529 0.116 Uiso 1 1 calc R . . C5 C 0.3379(2) 0.9390(5) 1.0798(8) 0.084(2) Uani 1 1 d . . . C6 C 0.3821(2) 0.9389(5) 1.1212(7) 0.088(2) Uani 1 1 d . . . H6A H 0.3908 0.9000 1.1880 0.105 Uiso 1 1 calc R . . C7 C 0.41401(19) 0.9956(5) 1.0656(6) 0.076(2) Uani 1 1 d . . . H7A H 0.4437 0.9949 1.0957 0.091 Uiso 1 1 calc R . . C8 C 0.3041(4) 0.8753(7) 1.1383(12) 0.132(5) Uani 1 1 d . . . C9 C 0.5461(2) 1.2229(4) 0.5600(7) 0.084(2) Uani 1 1 d . . . H9A H 0.5451 1.2860 0.5565 0.101 Uiso 1 1 calc R . . C10 C 0.5785(2) 1.1790(5) 0.4879(8) 0.100(2) Uani 1 1 d . . . H10A H 0.5993 1.2122 0.4394 0.120 Uiso 1 1 calc R . . C11 C 0.5801(2) 1.0844(6) 0.4876(7) 0.088(2) Uani 1 1 d . . . C12 C 0.5499(2) 1.0388(5) 0.5703(7) 0.0771(19) Uani 1 1 d . . . H12A H 0.5511 0.9759 0.5780 0.092 Uiso 1 1 calc R . . C13 C 0.51858(19) 1.0871(5) 0.6395(6) 0.0689(17) Uani 1 1 d . . . H13A H 0.4983 1.0552 0.6916 0.083 Uiso 1 1 calc R . . C14 C 0.64817(19) 0.9067(5) 0.4884(7) 0.077(2) Uani 1 1 d . . . C15 C 0.6722(2) 0.9532(5) 0.5829(7) 0.0757(19) Uani 1 1 d . . . H15A H 0.6675 1.0146 0.5994 0.091 Uiso 1 1 calc R . . C16 C 0.70327(18) 0.9030(5) 0.6506(6) 0.0741(19) Uani 1 1 d . . . H16A H 0.7194 0.9331 0.7153 0.089 Uiso 1 1 calc R . . C17 C 0.68899(18) 0.7744(4) 0.5431(6) 0.0728(19) Uani 1 1 d . . . H17A H 0.6948 0.7132 0.5284 0.087 Uiso 1 1 calc R . . C18 C 0.65654(18) 0.8151(5) 0.4702(6) 0.0758(19) Uani 1 1 d . . . H18A H 0.6402 0.7821 0.4089 0.091 Uiso 1 1 calc R . . N1 N 0.51546(14) 1.1791(4) 0.6365(5) 0.0664(14) Uani 1 1 d . . . N2 N 0.61103(17) 1.0412(5) 0.4115(6) 0.0977(19) Uani 1 1 d . . . H2A H 0.6283 1.0722 0.3608 0.117 Uiso 1 1 calc R . . N3 N 0.61482(17) 0.9473(5) 0.4151(6) 0.0955(18) Uani 1 1 d . . . H3B H 0.5962 0.9144 0.3712 0.115 Uiso 1 1 calc R . . N4 N 0.71279(14) 0.8164(3) 0.6338(5) 0.0673(14) Uani 1 1 d . . . O1 O 0.42526(12) 1.1593(3) 0.8068(4) 0.0754(12) Uani 1 1 d . . . O2 O 0.47516(14) 1.1203(4) 0.9540(5) 0.1080(17) Uani 1 1 d . . . O3 O 0.3102(2) 0.8508(4) 1.2495(8) 0.157(3) Uani 1 1 d . . . O4 O 0.2717(2) 0.8527(6) 1.0803(9) 0.233(5) 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 0.0508(5) 0.0514(7) 0.0838(7) 0.0021(6) 0.000 0.000 Zn2 0.0488(5) 0.0558(7) 0.0835(7) -0.0179(6) 0.000 0.000 C1 0.060(4) 0.071(5) 0.067(5) 0.004(4) -0.001(3) -0.007(3) C2 0.060(4) 0.057(4) 0.077(5) -0.012(4) 0.022(3) -0.015(3) C3 0.058(4) 0.086(6) 0.083(5) 0.004(4) 0.001(3) -0.001(4) C4 0.060(4) 0.103(7) 0.126(7) -0.026(5) 0.015(5) -0.024(4) C5 0.070(5) 0.062(5) 0.119(7) -0.018(5) 0.027(4) -0.017(4) C6 0.092(5) 0.061(5) 0.111(6) 0.022(4) 0.028(4) 0.010(4) C7 0.061(4) 0.082(5) 0.086(5) 0.033(4) 0.005(4) -0.016(3) C8 0.132(8) 0.094(8) 0.169(11) -0.037(8) 0.106(9) -0.049(6) C9 0.073(4) 0.046(5) 0.132(6) 0.018(4) 0.009(4) 0.005(3) C10 0.076(4) 0.078(6) 0.147(7) 0.022(5) 0.047(4) 0.036(4) C11 0.075(5) 0.084(6) 0.106(6) 0.019(5) -0.002(4) 0.028(4) C12 0.079(4) 0.058(5) 0.095(5) -0.012(4) -0.004(4) 0.023(4) C13 0.068(4) 0.052(5) 0.086(5) 0.008(4) 0.001(3) -0.002(3) C14 0.063(4) 0.088(6) 0.080(5) 0.003(5) 0.005(4) 0.033(4) C15 0.087(4) 0.049(5) 0.091(5) -0.028(4) -0.003(4) 0.005(4) C16 0.059(4) 0.078(6) 0.085(5) -0.017(4) -0.003(3) 0.001(4) C17 0.059(3) 0.055(5) 0.104(5) -0.017(4) -0.019(3) 0.018(3) C18 0.062(4) 0.069(5) 0.097(5) -0.029(4) -0.004(3) 0.008(3) N1 0.056(3) 0.057(4) 0.086(4) 0.002(3) -0.001(3) 0.005(3) N2 0.104(4) 0.076(5) 0.113(5) 0.016(4) 0.033(4) 0.044(4) N3 0.093(4) 0.084(5) 0.110(5) -0.006(4) 0.002(4) 0.027(4) N4 0.061(3) 0.045(4) 0.096(4) -0.025(3) -0.002(3) 0.000(3) O1 0.077(3) 0.062(3) 0.088(3) 0.019(2) 0.009(2) 0.003(2) O2 0.083(3) 0.125(5) 0.116(4) 0.037(3) -0.012(3) -0.050(3) O3 0.140(5) 0.075(4) 0.255(8) 0.011(6) 0.115(6) -0.016(3) O4 0.168(6) 0.275(11) 0.255(10) -0.093(7) 0.080(6) -0.169(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 O1 2.007(4) . ? Zn1 O1 2.007(4) 4_576 ? Zn1 N1 2.022(5) 4_576 ? Zn1 N1 2.022(5) . ? Zn2 N4 2.031(5) . ? Zn2 N4 2.031(5) 4_566 ? Zn2 O3 2.149(6) 6_657 ? Zn2 O3 2.149(6) 7_675 ? Zn2 O4 2.345(10) 7_675 ? Zn2 O4 2.345(10) 6_657 ? Zn2 C8 2.571(9) 6_657 ? Zn2 C8 2.571(9) 7_675 ? C1 O2 1.236(6) . ? C1 O1 1.246(6) . ? C1 C2 1.516(8) . ? C2 C7 1.376(8) . ? C2 C3 1.385(7) . ? C3 C4 1.372(9) . ? C4 C5 1.378(9) . ? C5 C6 1.372(8) . ? C5 C8 1.494(11) . ? C6 C7 1.381(8) . ? C8 O4 1.176(13) . ? C8 O3 1.211(13) . ? C8 Zn2 2.571(9) 6_557 ? C9 N1 1.361(7) . ? C9 C10 1.372(8) . ? C10 C11 1.393(9) . ? C11 N2 1.360(8) . ? C11 C12 1.404(8) . ? C12 C13 1.364(7) . ? C13 N1 1.358(7) . ? C14 N3 1.376(7) . ? C14 C15 1.384(8) . ? C14 C18 1.383(9) . ? C15 C16 1.369(8) . ? C16 N4 1.316(7) . ? C17 N4 1.321(6) . ? C17 C18 1.355(7) . ? N2 N3 1.386(8) . ? O3 Zn2 2.149(6) 6_557 ? O4 Zn2 2.345(10) 6_557 ? 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 O1 Zn1 O1 93.1(2) . 4_576 ? O1 Zn1 N1 127.68(19) . 4_576 ? O1 Zn1 N1 105.1(2) 4_576 4_576 ? O1 Zn1 N1 105.1(2) . . ? O1 Zn1 N1 127.68(19) 4_576 . ? N1 Zn1 N1 101.4(3) 4_576 . ? N4 Zn2 N4 98.9(3) . 4_566 ? N4 Zn2 O3 98.0(2) . 6_657 ? N4 Zn2 O3 143.3(3) 4_566 6_657 ? N4 Zn2 O3 143.3(3) . 7_675 ? N4 Zn2 O3 98.0(2) 4_566 7_675 ? O3 Zn2 O3 87.4(4) 6_657 7_675 ? N4 Zn2 O4 89.4(2) . 7_675 ? N4 Zn2 O4 104.0(3) 4_566 7_675 ? O3 Zn2 O4 108.6(3) 6_657 7_675 ? O3 Zn2 O4 54.8(3) 7_675 7_675 ? N4 Zn2 O4 104.0(3) . 6_657 ? N4 Zn2 O4 89.4(2) 4_566 6_657 ? O3 Zn2 O4 54.8(3) 6_657 6_657 ? O3 Zn2 O4 108.6(3) 7_675 6_657 ? O4 Zn2 O4 159.5(4) 7_675 6_657 ? N4 Zn2 C8 105.3(3) . 6_657 ? N4 Zn2 C8 115.5(3) 4_566 6_657 ? O3 Zn2 C8 27.9(3) 6_657 6_657 ? O3 Zn2 C8 96.3(3) 7_675 6_657 ? O4 Zn2 C8 134.4(4) 7_675 6_657 ? O4 Zn2 C8 27.2(3) 6_657 6_657 ? N4 Zn2 C8 115.5(3) . 7_675 ? N4 Zn2 C8 105.3(3) 4_566 7_675 ? O3 Zn2 C8 96.3(3) 6_657 7_675 ? O3 Zn2 C8 27.9(3) 7_675 7_675 ? O4 Zn2 C8 27.2(3) 7_675 7_675 ? O4 Zn2 C8 134.4(4) 6_657 7_675 ? C8 Zn2 C8 115.4(6) 6_657 7_675 ? O2 C1 O1 123.6(6) . . ? O2 C1 C2 119.1(6) . . ? O1 C1 C2 117.3(6) . . ? C7 C2 C3 118.6(6) . . ? C7 C2 C1 120.4(6) . . ? C3 C2 C1 120.9(6) . . ? C4 C3 C2 120.3(7) . . ? C3 C4 C5 121.4(7) . . ? C6 C5 C4 118.1(7) . . ? C6 C5 C8 120.6(9) . . ? C4 C5 C8 121.3(9) . . ? C5 C6 C7 121.2(6) . . ? C2 C7 C6 120.4(6) . . ? O4 C8 O3 120.9(10) . . ? O4 C8 C5 121.2(13) . . ? O3 C8 C5 117.9(12) . . ? O4 C8 Zn2 65.6(7) . 6_557 ? O3 C8 Zn2 56.2(5) . 6_557 ? C5 C8 Zn2 170.5(9) . 6_557 ? N1 C9 C10 123.4(6) . . ? C9 C10 C11 119.8(7) . . ? N2 C11 C10 119.5(7) . . ? N2 C11 C12 123.4(8) . . ? C10 C11 C12 117.1(7) . . ? C13 C12 C11 119.8(7) . . ? N1 C13 C12 123.6(6) . . ? N3 C14 C15 122.3(7) . . ? N3 C14 C18 118.5(7) . . ? C15 C14 C18 119.1(6) . . ? C16 C15 C14 115.6(6) . . ? N4 C16 C15 126.8(6) . . ? N4 C17 C18 124.0(6) . . ? C17 C18 C14 118.8(6) . . ? C13 N1 C9 116.2(5) . . ? C13 N1 Zn1 123.0(4) . . ? C9 N1 Zn1 120.6(5) . . ? C11 N2 N3 120.4(6) . . ? C14 N3 N2 120.4(6) . . ? C16 N4 C17 115.6(5) . . ? C16 N4 Zn2 121.9(4) . . ? C17 N4 Zn2 122.3(4) . . ? C1 O1 Zn1 112.8(4) . . ? C8 O3 Zn2 95.8(8) . 6_557 ? C8 O4 Zn2 87.2(9) . 6_557 ? 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 C11 N2 N3 C14 -98.7(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.308 _refine_diff_density_min -0.320 _refine_diff_density_rms 0.070 # 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 0.750 0.361 0.250 330.1 59.8 2 0.022 0.750 0.250 151.6 31.0 3 0.478 0.250 0.250 150.1 29.7 4 0.250 0.138 0.750 330.0 59.8 5 0.522 0.750 0.750 151.6 30.9 6 0.978 0.250 0.750 150.0 29.7 _platon_squeeze_details ; ; data_2a _database_code_depnum_ccdc_archive 'CCDC 822609' #TrackingRef '- 1a-2b.R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C29 H29 N4 O10.50 Zn2' _chemical_formula_weight 732.30 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.877(7) _cell_length_b 17.619(12) _cell_length_c 20.499(14) _cell_angle_alpha 110.788(12) _cell_angle_beta 93.326(13) _cell_angle_gamma 90.408(12) _cell_volume 3665(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method . _exptl_crystal_F_000 1500 _exptl_absorpt_coefficient_mu 1.363 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7628 _exptl_absorpt_correction_T_max 0.8013 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28005 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.1211 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 14215 _reflns_number_gt 7436 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0130P)^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 14215 _refine_ls_number_parameters 721 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0544 _refine_ls_wR_factor_ref 0.1469 _refine_ls_wR_factor_gt 0.1346 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.004 _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 0.81675(5) 0.56118(4) 0.77262(3) 0.02770(16) Uani 1 1 d . . . Zn2 Zn 0.82175(5) 0.44178(3) 0.84484(3) 0.02797(16) Uani 1 1 d . . . Zn3 Zn 0.85660(5) 0.06026(4) 0.27563(3) 0.02762(16) Uani 1 1 d . . . Zn4 Zn 0.86766(5) -0.05801(4) 0.34917(3) 0.02795(16) Uani 1 1 d . . . C1 C 0.8203(5) 0.6204(3) 0.9272(3) 0.0356(14) Uani 1 1 d . . . C2 C 0.8198(5) 0.6876(3) 0.9965(3) 0.0344(13) Uani 1 1 d . . . C3 C 0.8009(5) 0.7669(3) 1.0024(3) 0.0440(16) Uani 1 1 d . . . H3A H 0.7833 0.7787 0.9622 0.053 Uiso 1 1 calc R . . C4 C 0.8072(5) 0.8274(3) 1.0646(3) 0.0442(16) Uani 1 1 d . . . H4B H 0.7951 0.8804 1.0669 0.053 Uiso 1 1 calc R . . C5 C 0.8314(5) 0.8121(3) 1.1253(3) 0.0365(14) Uani 1 1 d . . . C6 C 0.8464(5) 0.7332(3) 1.1211(3) 0.0419(15) Uani 1 1 d . . . H6A H 0.8603 0.7219 1.1618 0.050 Uiso 1 1 calc R . . C7 C 0.8411(5) 0.6704(3) 1.0571(3) 0.0406(15) Uani 1 1 d . . . H7A H 0.8518 0.6172 1.0547 0.049 Uiso 1 1 calc R . . C8 C 0.8436(5) 0.8796(3) 1.1954(3) 0.0352(14) Uani 1 1 d . . . C9 C 0.5838(5) 0.5008(3) 0.8042(3) 0.0335(13) Uani 1 1 d . . . C10 C 0.4457(5) 0.5023(3) 0.8055(3) 0.0368(14) Uani 1 1 d . . . C11 C 0.3805(6) 0.5586(4) 0.7860(4) 0.065(2) Uani 1 1 d . . . H11A H 0.4229 0.5954 0.7716 0.078 Uiso 1 1 calc R . . C12 C 0.2557(5) 0.5615(4) 0.7872(4) 0.062(2) Uani 1 1 d . . . H12A H 0.2138 0.6000 0.7737 0.075 Uiso 1 1 calc R . . C13 C 0.1916(5) 0.5084(3) 0.8082(3) 0.0371(14) Uani 1 1 d . . . C14 C 0.2546(6) 0.4543(4) 0.8289(4) 0.067(2) Uani 1 1 d . . . H14A H 0.2120 0.4187 0.8444 0.081 Uiso 1 1 calc R . . C15 C 0.3800(5) 0.4509(4) 0.8275(4) 0.073(3) Uani 1 1 d . . . H15A H 0.4211 0.4128 0.8418 0.087 Uiso 1 1 calc R . . C16 C 0.0546(5) 0.5117(4) 0.8098(3) 0.0414(15) Uani 1 1 d . . . C17 C 0.8287(5) 0.3802(3) 0.6942(3) 0.0338(13) Uani 1 1 d . . . C18 C 0.8429(5) 0.3140(3) 0.6266(3) 0.0368(14) Uani 1 1 d . . . C19 C 0.8511(6) 0.3301(3) 0.5656(3) 0.0498(17) Uani 1 1 d . . . H19A H 0.8469 0.3834 0.5674 0.060 Uiso 1 1 calc R . . C20 C 0.8652(6) 0.2688(4) 0.5023(3) 0.0508(17) Uani 1 1 d . . . H20A H 0.8739 0.2812 0.4623 0.061 Uiso 1 1 calc R . . C21 C 0.8662(5) 0.1888(3) 0.4986(3) 0.0398(14) Uani 1 1 d . . . C22 C 0.8608(5) 0.1721(3) 0.5600(3) 0.0416(15) Uani 1 1 d . . . H22A H 0.8649 0.1188 0.5584 0.050 Uiso 1 1 calc R . . C23 C 0.8494(5) 0.2334(3) 0.6222(3) 0.0403(15) Uani 1 1 d . . . H23A H 0.8459 0.2212 0.6627 0.048 Uiso 1 1 calc R . . C24 C 0.8723(5) 0.1212(4) 0.4292(3) 0.0383(14) Uani 1 1 d . . . C25 C 0.8432(5) 0.3944(3) 0.9697(3) 0.0412(15) Uani 1 1 d . . . H25A H 0.8401 0.4501 0.9934 0.049 Uiso 1 1 calc R . . C26 C 0.8595(5) 0.3462(4) 1.0082(3) 0.0472(16) Uani 1 1 d . . . H26A H 0.8672 0.3686 1.0568 0.057 Uiso 1 1 calc R . . C27 C 0.8645(5) 0.2633(4) 0.9742(3) 0.0454(16) Uani 1 1 d . . . C28 C 0.8487(6) 0.2324(3) 0.9015(3) 0.0497(17) Uani 1 1 d . . . H28A H 0.8490 0.1767 0.8772 0.060 Uiso 1 1 calc R . . C29 C 0.8328(5) 0.2853(4) 0.8662(3) 0.0440(15) Uani 1 1 d . . . H29A H 0.8227 0.2643 0.8177 0.053 Uiso 1 1 calc R . . C30 C 0.9060(6) 0.2056(4) 1.1216(3) 0.0513(18) Uani 1 1 d . . . C31 C 0.8167(6) 0.1477(4) 1.1088(3) 0.0541(19) Uani 1 1 d . . . H31A H 0.7667 0.1326 1.0676 0.065 Uiso 1 1 calc R . . C32 C 0.8001(6) 0.1118(4) 1.1561(3) 0.057(2) Uani 1 1 d . . . H32A H 0.7392 0.0711 1.1451 0.068 Uiso 1 1 calc R . . C33 C 0.9481(6) 0.1909(4) 1.2316(3) 0.059(2) Uani 1 1 d . . . H33A H 0.9934 0.2069 1.2744 0.071 Uiso 1 1 calc R . . C34 C 0.9698(6) 0.2294(4) 1.1874(3) 0.064(2) Uani 1 1 d . . . H34A H 1.0275 0.2721 1.2004 0.077 Uiso 1 1 calc R . . C35 C 0.6271(5) 0.0065(4) 0.3075(3) 0.0432(16) Uani 1 1 d . . . C36 C 0.4886(5) 0.0052(4) 0.3082(3) 0.0425(16) Uani 1 1 d . . . C37 C 0.4181(5) 0.0548(4) 0.2844(3) 0.058(2) Uani 1 1 d . . . H37A H 0.4564 0.0901 0.2668 0.070 Uiso 1 1 calc R . . C38 C 0.2897(5) 0.0540(4) 0.2858(4) 0.063(2) Uani 1 1 d . . . H38A H 0.2434 0.0894 0.2706 0.076 Uiso 1 1 calc R . . C39 C 0.2333(5) 0.0007(4) 0.3098(3) 0.0399(15) Uani 1 1 d . . . C40 C 0.3016(6) -0.0493(4) 0.3323(4) 0.072(2) Uani 1 1 d . . . H40A H 0.2630 -0.0858 0.3486 0.087 Uiso 1 1 calc R . . C41 C 0.4298(6) -0.0474(4) 0.3315(4) 0.074(2) Uani 1 1 d . . . H41A H 0.4756 -0.0827 0.3472 0.088 Uiso 1 1 calc R . . C42 C 0.0976(6) 0.0005(4) 0.3116(3) 0.0433(15) Uani 1 1 d . . . C43 C 0.8375(5) -0.1088(4) 0.4694(3) 0.0428(15) Uani 1 1 d . . . H43A H 0.8462 -0.0533 0.4945 0.051 Uiso 1 1 calc R . . C44 C 0.8143(6) -0.1588(4) 0.5058(3) 0.0597(19) Uani 1 1 d . . . H44A H 0.8095 -0.1380 0.5540 0.072 Uiso 1 1 calc R . . C45 C 0.7984(7) -0.2400(4) 0.4692(4) 0.062(2) Uani 1 1 d . . . C46 C 0.8151(7) -0.2699(4) 0.3957(4) 0.071(2) Uani 1 1 d . . . H46A H 0.8102 -0.3253 0.3700 0.085 Uiso 1 1 calc R . . C47 C 0.8382(6) -0.2156(4) 0.3644(3) 0.0505(17) Uani 1 1 d . . . H47A H 0.8473 -0.2348 0.3165 0.061 Uiso 1 1 calc R . . C48 C 0.7502(7) -0.3036(5) 0.6109(4) 0.065(2) Uani 1 1 d . . . C49 C 0.6757(7) -0.2874(5) 0.6676(4) 0.081(3) Uani 1 1 d . . . H49A H 0.6090 -0.2536 0.6721 0.097 Uiso 1 1 calc R . . C50 C 0.7041(7) -0.3231(4) 0.7170(4) 0.074(2) Uani 1 1 d . . . H50A H 0.6549 -0.3131 0.7547 0.088 Uiso 1 1 calc R . . C51 C 0.8672(6) -0.3824(4) 0.6584(3) 0.0498(17) Uani 1 1 d . . . H51A H 0.9338 -0.4162 0.6544 0.060 Uiso 1 1 calc R . . C52 C 0.8484(6) -0.3491(4) 0.6084(3) 0.0579(19) Uani 1 1 d . . . H52A H 0.9027 -0.3578 0.5732 0.070 Uiso 1 1 calc R . . N1 N 0.8313(4) 0.3670(3) 0.8994(2) 0.0332(11) Uani 1 1 d . . . N2 N 0.8878(5) 0.2110(3) 1.0091(3) 0.0567(15) Uani 1 1 d . . . H2A H 0.8739 0.1596 0.9888 0.068 Uiso 1 1 calc R . . N3 N 0.9340(5) 0.2430(3) 1.0773(3) 0.0689(19) Uani 1 1 d . . . H3B H 0.9801 0.2863 1.0914 0.083 Uiso 1 1 calc R . . N4 N 0.8638(4) 0.1301(3) 1.2165(2) 0.0360(12) Uani 1 1 d . . . N5 N 0.8485(4) -0.1345(3) 0.4001(2) 0.0364(11) Uani 1 1 d . . . N6 N 0.7691(7) -0.2976(4) 0.4993(4) 0.098(2) Uani 1 1 d . . . H6B H 0.7834 -0.3483 0.4794 0.118 Uiso 1 1 calc R . . N7 N 0.7162(6) -0.2682(4) 0.5625(4) 0.091(2) Uani 1 1 d . . . H7B H 0.6644 -0.2297 0.5714 0.109 Uiso 1 1 calc R . . N8 N 0.7994(4) -0.3710(3) 0.7119(2) 0.0377(12) Uani 1 1 d . . . O1 O 0.8313(4) 0.6405(2) 0.87415(19) 0.0474(11) Uani 1 1 d . . . O2 O 0.8120(4) 0.5487(2) 0.92521(19) 0.0455(11) Uani 1 1 d . . . O3 O 0.8443(4) 0.9506(2) 1.1950(2) 0.0586(13) Uani 1 1 d . . . O4 O 0.8531(4) 0.8623(2) 1.2490(2) 0.0481(11) Uani 1 1 d . . . O5 O 0.6363(3) 0.5505(2) 0.7845(2) 0.0506(12) Uani 1 1 d . . . O6 O 0.6365(3) 0.4496(2) 0.8251(2) 0.0483(11) Uani 1 1 d . . . O7 O 0.0035(3) 0.4720(3) 0.8407(2) 0.0543(12) Uani 1 1 d . . . O8 O 0.0010(4) 0.5539(3) 0.7794(2) 0.0559(12) Uani 1 1 d . . . O9 O 0.8134(4) 0.4500(2) 0.69399(19) 0.0513(11) Uani 1 1 d . . . O10 O 0.8319(4) 0.3614(2) 0.74738(19) 0.0496(11) Uani 1 1 d . . . O11 O 0.8673(4) 0.1391(2) 0.3750(2) 0.0592(13) Uani 1 1 d . . . O12 O 0.8770(4) 0.0499(2) 0.4291(2) 0.0501(11) Uani 1 1 d . . . O13 O 0.6733(4) 0.0528(3) 0.2810(3) 0.0657(14) Uani 1 1 d . . . O14 O 0.6839(4) -0.0378(3) 0.3333(2) 0.0568(13) Uani 1 1 d . . . O15 O 0.0401(4) 0.0424(3) 0.2844(2) 0.0602(13) Uani 1 1 d . . . O16 O 0.0511(3) -0.0446(2) 0.3405(2) 0.0523(12) 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 0.0301(4) 0.0296(4) 0.0266(4) 0.0135(3) 0.0040(3) 0.0025(3) Zn2 0.0333(4) 0.0275(4) 0.0259(4) 0.0126(3) 0.0040(3) 0.0031(3) Zn3 0.0317(4) 0.0289(4) 0.0259(4) 0.0138(3) 0.0044(3) 0.0021(3) Zn4 0.0316(4) 0.0292(4) 0.0263(4) 0.0134(3) 0.0049(3) 0.0025(3) C1 0.039(4) 0.035(3) 0.028(3) 0.006(3) 0.002(3) -0.006(3) C2 0.042(4) 0.035(3) 0.025(3) 0.009(3) 0.002(3) -0.004(3) C3 0.070(5) 0.038(4) 0.023(3) 0.009(3) 0.005(3) 0.008(3) C4 0.068(5) 0.028(3) 0.039(4) 0.017(3) -0.003(3) 0.008(3) C5 0.048(4) 0.032(3) 0.026(3) 0.005(3) 0.004(3) 0.003(3) C6 0.068(4) 0.039(4) 0.023(3) 0.016(3) 0.004(3) 0.002(3) C7 0.068(4) 0.022(3) 0.027(3) 0.002(3) 0.006(3) -0.003(3) C8 0.039(4) 0.032(3) 0.033(4) 0.008(3) 0.007(3) 0.002(3) C9 0.030(3) 0.041(3) 0.028(3) 0.010(3) 0.007(3) 0.007(3) C10 0.028(3) 0.044(4) 0.042(4) 0.019(3) 0.004(3) 0.005(3) C11 0.042(4) 0.073(5) 0.107(6) 0.066(5) 0.006(4) -0.001(3) C12 0.032(4) 0.075(5) 0.110(6) 0.069(5) 0.008(4) 0.013(3) C13 0.028(3) 0.039(3) 0.044(4) 0.015(3) 0.007(3) 0.002(3) C14 0.038(4) 0.075(5) 0.119(7) 0.070(5) 0.016(4) 0.001(3) C15 0.030(4) 0.084(5) 0.150(8) 0.096(6) 0.013(4) 0.011(3) C16 0.029(4) 0.052(4) 0.035(4) 0.004(3) 0.006(3) -0.007(3) C17 0.034(3) 0.036(3) 0.032(4) 0.013(3) -0.002(3) 0.001(2) C18 0.053(4) 0.025(3) 0.033(4) 0.010(3) 0.008(3) 0.005(3) C19 0.088(5) 0.028(3) 0.035(4) 0.011(3) 0.008(3) 0.004(3) C20 0.091(5) 0.040(4) 0.030(4) 0.021(3) 0.015(3) 0.013(3) C21 0.048(4) 0.037(3) 0.029(4) 0.005(3) 0.001(3) 0.004(3) C22 0.062(4) 0.033(3) 0.033(4) 0.016(3) 0.001(3) -0.004(3) C23 0.060(4) 0.034(3) 0.024(3) 0.007(3) 0.003(3) 0.001(3) C24 0.039(4) 0.045(4) 0.028(4) 0.009(3) 0.003(3) 0.004(3) C25 0.064(4) 0.033(3) 0.019(3) 0.001(3) 0.003(3) 0.003(3) C26 0.068(5) 0.051(4) 0.030(4) 0.022(3) 0.004(3) 0.009(3) C27 0.050(4) 0.053(4) 0.042(4) 0.030(3) -0.004(3) -0.006(3) C28 0.074(5) 0.029(3) 0.051(4) 0.021(3) 0.000(4) 0.004(3) C29 0.058(4) 0.047(4) 0.028(4) 0.015(3) 0.005(3) 0.007(3) C30 0.066(5) 0.052(4) 0.051(4) 0.039(4) -0.004(3) -0.009(3) C31 0.061(5) 0.061(4) 0.050(4) 0.036(4) -0.023(3) -0.029(3) C32 0.068(5) 0.059(4) 0.054(5) 0.039(4) -0.023(4) -0.029(3) C33 0.086(5) 0.053(4) 0.045(4) 0.030(4) -0.026(4) -0.026(4) C34 0.090(6) 0.064(5) 0.051(5) 0.043(4) -0.025(4) -0.040(4) C35 0.026(4) 0.049(4) 0.052(4) 0.015(3) 0.004(3) 0.000(3) C36 0.027(3) 0.056(4) 0.060(4) 0.038(4) 0.009(3) 0.004(3) C37 0.038(4) 0.074(5) 0.089(6) 0.061(5) 0.011(4) 0.002(3) C38 0.025(4) 0.092(6) 0.101(6) 0.069(5) 0.004(4) 0.006(3) C39 0.027(3) 0.051(4) 0.049(4) 0.026(3) 0.007(3) 0.005(3) C40 0.038(4) 0.088(6) 0.127(7) 0.079(6) 0.022(4) 0.002(4) C41 0.036(4) 0.094(6) 0.126(7) 0.081(6) 0.012(4) 0.018(4) C42 0.040(4) 0.043(4) 0.047(4) 0.015(3) 0.009(3) -0.003(3) C43 0.061(4) 0.039(4) 0.034(4) 0.020(3) 0.012(3) 0.004(3) C44 0.084(6) 0.068(5) 0.036(4) 0.030(4) 0.004(4) 0.005(4) C45 0.090(6) 0.062(5) 0.051(5) 0.042(4) -0.002(4) -0.009(4) C46 0.121(7) 0.046(4) 0.055(5) 0.030(4) 0.002(4) -0.008(4) C47 0.089(5) 0.042(4) 0.027(4) 0.021(3) -0.002(3) -0.006(3) C48 0.068(5) 0.084(6) 0.068(5) 0.060(5) -0.001(4) -0.009(4) C49 0.071(6) 0.094(6) 0.117(7) 0.082(6) 0.027(5) 0.028(4) C50 0.086(6) 0.077(6) 0.091(6) 0.067(5) 0.022(5) 0.016(4) C51 0.054(4) 0.061(4) 0.047(4) 0.031(4) 0.019(3) 0.018(3) C52 0.061(5) 0.079(5) 0.055(5) 0.048(4) 0.019(4) 0.015(4) N1 0.040(3) 0.030(3) 0.032(3) 0.015(2) 0.004(2) 0.001(2) N2 0.092(5) 0.043(3) 0.045(4) 0.029(3) -0.008(3) -0.006(3) N3 0.097(5) 0.073(4) 0.052(4) 0.047(3) -0.027(3) -0.037(3) N4 0.038(3) 0.039(3) 0.038(3) 0.026(2) -0.007(2) -0.007(2) N5 0.042(3) 0.040(3) 0.033(3) 0.020(2) 0.003(2) 0.004(2) N6 0.166(8) 0.080(5) 0.074(5) 0.059(4) 0.007(5) -0.005(5) N7 0.115(6) 0.104(6) 0.091(6) 0.076(5) 0.034(4) 0.030(4) N8 0.038(3) 0.038(3) 0.044(3) 0.023(3) 0.004(2) 0.007(2) O1 0.075(3) 0.043(3) 0.024(2) 0.011(2) 0.005(2) -0.006(2) O2 0.073(3) 0.027(2) 0.031(2) 0.0024(19) 0.011(2) 0.0007(19) O3 0.108(4) 0.032(2) 0.031(3) 0.007(2) -0.005(2) -0.001(2) O4 0.077(3) 0.036(2) 0.027(2) 0.006(2) 0.005(2) 0.004(2) O5 0.029(2) 0.067(3) 0.073(3) 0.045(3) 0.012(2) 0.004(2) O6 0.027(2) 0.058(3) 0.070(3) 0.035(2) 0.000(2) 0.0098(19) O7 0.032(3) 0.079(3) 0.060(3) 0.033(3) 0.008(2) -0.003(2) O8 0.034(3) 0.071(3) 0.075(3) 0.040(3) 0.010(2) 0.014(2) O9 0.084(3) 0.036(2) 0.030(3) 0.007(2) 0.003(2) 0.012(2) O10 0.082(3) 0.041(3) 0.025(2) 0.010(2) 0.007(2) 0.013(2) O11 0.105(4) 0.039(3) 0.029(3) 0.007(2) 0.007(2) 0.005(2) O12 0.079(3) 0.035(2) 0.032(3) 0.007(2) 0.006(2) 0.004(2) O13 0.030(3) 0.081(3) 0.110(4) 0.062(3) 0.008(2) 0.003(2) O14 0.029(3) 0.082(3) 0.079(4) 0.051(3) 0.007(2) 0.009(2) O15 0.029(3) 0.086(4) 0.087(4) 0.057(3) 0.007(2) 0.012(2) O16 0.027(2) 0.066(3) 0.072(3) 0.035(3) 0.006(2) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 2.008(4) . ? Zn1 O8 2.009(4) 1_655 ? Zn1 N8 2.011(4) 1_565 ? Zn1 O9 2.047(4) . ? Zn1 O1 2.051(4) . ? Zn1 Zn2 2.9703(17) . ? Zn2 O10 2.007(4) . ? Zn2 N1 2.008(4) . ? Zn2 O2 2.024(4) . ? Zn2 O6 2.047(4) . ? Zn2 O7 2.058(4) 1_655 ? Zn3 O13 2.010(4) . ? Zn3 O11 2.013(4) . ? Zn3 N4 2.015(4) 1_554 ? Zn3 O15 2.031(4) 1_655 ? Zn3 O3 2.047(4) 1_544 ? Zn3 Zn4 2.9736(17) . ? Zn4 N5 1.993(4) . ? Zn4 O12 2.019(4) . ? Zn4 O4 2.031(4) 1_544 ? Zn4 O16 2.033(4) 1_655 ? Zn4 O14 2.061(4) . ? C1 O2 1.251(6) . ? C1 O1 1.269(6) . ? C1 C2 1.492(7) . ? C2 C3 1.377(7) . ? C2 C7 1.387(7) . ? C3 C4 1.339(7) . ? C3 H3A 0.9300 . ? C4 C5 1.375(7) . ? C4 H4B 0.9300 . ? C5 C6 1.373(7) . ? C5 C8 1.503(7) . ? C6 C7 1.381(7) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 O4 1.240(6) . ? C8 O3 1.254(6) . ? C9 O5 1.236(6) . ? C9 O6 1.256(6) . ? C9 C10 1.504(7) . ? C10 C15 1.361(7) . ? C10 C11 1.381(7) . ? C11 C12 1.361(8) . ? C11 H11A 0.9300 . ? C12 C13 1.363(7) . ? C12 H12A 0.9300 . ? C13 C14 1.349(8) . ? C13 C16 1.494(7) . ? C14 C15 1.367(8) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 O7 1.243(6) . ? C16 O8 1.256(7) . ? C17 O9 1.244(6) . ? C17 O10 1.245(6) . ? C17 C18 1.477(7) . ? C18 C19 1.384(7) . ? C18 C23 1.394(7) . ? C19 C20 1.381(7) . ? C19 H19A 0.9300 . ? C20 C21 1.384(7) . ? C20 H20A 0.9300 . ? C21 C22 1.396(7) . ? C21 C24 1.502(7) . ? C22 C23 1.360(7) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 O11 1.256(6) . ? C24 O12 1.257(6) . ? C25 N1 1.345(6) . ? C25 C26 1.357(7) . ? C25 H25A 0.9300 . ? C26 C27 1.380(8) . ? C26 H26A 0.9300 . ? C27 N2 1.369(7) . ? C27 C28 1.391(8) . ? C28 C29 1.375(7) . ? C28 H28A 0.9300 . ? C29 N1 1.356(7) . ? C29 H29A 0.9300 . ? C30 N3 1.344(7) . ? C30 C31 1.349(7) . ? C30 C34 1.399(8) . ? C31 C32 1.353(7) . ? C31 H31A 0.9300 . ? C32 N4 1.315(7) . ? C32 H32A 0.9300 . ? C33 N4 1.342(7) . ? C33 C34 1.341(7) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 O14 1.237(7) . ? C35 O13 1.247(7) . ? C35 C36 1.507(7) . ? C36 C41 1.356(7) . ? C36 C37 1.363(7) . ? C37 C38 1.399(8) . ? C37 H37A 0.9300 . ? C38 C39 1.361(7) . ? C38 H38A 0.9300 . ? C39 C40 1.341(8) . ? C39 C42 1.479(8) . ? C40 C41 1.396(8) . ? C40 H40A 0.9300 . ? C41 H41A 0.9300 . ? C42 O15 1.227(7) . ? C42 O16 1.264(6) . ? C43 N5 1.342(6) . ? C43 C44 1.372(7) . ? C43 H43A 0.9300 . ? C44 C45 1.362(9) . ? C44 H44A 0.9300 . ? C45 N6 1.406(8) . ? C45 C46 1.432(9) . ? C46 C47 1.358(7) . ? C46 H46A 0.9300 . ? C47 N5 1.354(7) . ? C47 H47A 0.9300 . ? C48 C52 1.332(9) . ? C48 N7 1.383(8) . ? C48 C49 1.402(9) . ? C49 C50 1.391(8) . ? C49 H49A 0.9300 . ? C50 N8 1.327(7) . ? C50 H50A 0.9300 . ? C51 N8 1.315(6) . ? C51 C52 1.357(8) . ? C51 H51A 0.9300 . ? C52 H52A 0.9300 . ? N2 N3 1.371(6) . ? N2 H2A 0.8600 . ? N3 H3B 0.8600 . ? N4 Zn3 2.015(4) 1_556 ? N6 N7 1.375(8) . ? N6 H6B 0.8600 . ? N7 H7B 0.8600 . ? N8 Zn1 2.011(4) 1_545 ? O3 Zn3 2.047(4) 1_566 ? O4 Zn4 2.031(4) 1_566 ? O7 Zn2 2.058(4) 1_455 ? O8 Zn1 2.009(4) 1_455 ? O15 Zn3 2.031(4) 1_455 ? O16 Zn4 2.033(4) 1_455 ? 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 O5 Zn1 O8 163.48(16) . 1_655 ? O5 Zn1 N8 96.65(17) . 1_565 ? O8 Zn1 N8 99.85(18) 1_655 1_565 ? O5 Zn1 O9 91.39(18) . . ? O8 Zn1 O9 87.33(18) 1_655 . ? N8 Zn1 O9 97.46(18) 1_565 . ? O5 Zn1 O1 87.15(17) . . ? O8 Zn1 O1 87.33(18) 1_655 . ? N8 Zn1 O1 106.62(18) 1_565 . ? O9 Zn1 O1 155.89(15) . . ? O5 Zn1 Zn2 79.66(11) . . ? O8 Zn1 Zn2 84.11(12) 1_655 . ? N8 Zn1 Zn2 171.45(14) 1_565 . ? O9 Zn1 Zn2 75.04(12) . . ? O1 Zn1 Zn2 81.03(12) . . ? O10 Zn2 N1 100.29(18) . . ? O10 Zn2 O2 160.69(16) . . ? N1 Zn2 O2 98.99(18) . . ? O10 Zn2 O6 89.52(17) . . ? N1 Zn2 O6 103.69(16) . . ? O2 Zn2 O6 87.05(17) . . ? O10 Zn2 O7 86.97(17) . 1_655 ? N1 Zn2 O7 103.34(17) . 1_655 ? O2 Zn2 O7 87.48(17) . 1_655 ? O6 Zn2 O7 152.93(16) . 1_655 ? O10 Zn2 Zn1 83.08(12) . . ? N1 Zn2 Zn1 176.02(13) . . ? O2 Zn2 Zn1 77.61(12) . . ? O6 Zn2 Zn1 78.33(11) . . ? O7 Zn2 Zn1 74.60(12) 1_655 . ? O13 Zn3 O11 88.50(19) . . ? O13 Zn3 N4 99.65(18) . 1_554 ? O11 Zn3 N4 104.92(19) . 1_554 ? O13 Zn3 O15 162.57(17) . 1_655 ? O11 Zn3 O15 89.40(19) . 1_655 ? N4 Zn3 O15 97.61(17) 1_554 1_655 ? O13 Zn3 O3 88.4(2) . 1_544 ? O11 Zn3 O3 158.20(16) . 1_544 ? N4 Zn3 O3 96.88(18) 1_554 1_544 ? O15 Zn3 O3 87.19(19) 1_655 1_544 ? O13 Zn3 Zn4 85.24(12) . . ? O11 Zn3 Zn4 81.07(13) . . ? N4 Zn3 Zn4 172.26(14) 1_554 . ? O15 Zn3 Zn4 77.34(12) 1_655 . ? O3 Zn3 Zn4 77.17(12) 1_544 . ? N5 Zn4 O12 101.13(19) . . ? N5 Zn4 O4 99.95(18) . 1_544 ? O12 Zn4 O4 158.58(16) . 1_544 ? N5 Zn4 O16 107.21(17) . 1_655 ? O12 Zn4 O16 88.20(17) . 1_655 ? O4 Zn4 O16 89.20(17) 1_544 1_655 ? N5 Zn4 O14 98.30(17) . . ? O12 Zn4 O14 87.63(18) . . ? O4 Zn4 O14 85.60(18) 1_544 . ? O16 Zn4 O14 154.49(17) 1_655 . ? N5 Zn4 Zn3 171.49(13) . . ? O12 Zn4 Zn3 77.43(13) . . ? O4 Zn4 Zn3 81.16(12) 1_544 . ? O16 Zn4 Zn3 81.20(12) 1_655 . ? O14 Zn4 Zn3 73.32(11) . . ? O2 C1 O1 124.6(5) . . ? O2 C1 C2 118.5(5) . . ? O1 C1 C2 117.0(5) . . ? C3 C2 C7 118.5(5) . . ? C3 C2 C1 122.1(5) . . ? C7 C2 C1 119.4(5) . . ? C4 C3 C2 121.7(5) . . ? C4 C3 H3A 119.2 . . ? C2 C3 H3A 119.2 . . ? C3 C4 C5 120.8(5) . . ? C3 C4 H4B 119.6 . . ? C5 C4 H4B 119.6 . . ? C6 C5 C4 118.7(5) . . ? C6 C5 C8 119.8(5) . . ? C4 C5 C8 121.5(5) . . ? C5 C6 C7 121.0(5) . . ? C5 C6 H6A 119.5 . . ? C7 C6 H6A 119.5 . . ? C6 C7 C2 119.3(5) . . ? C6 C7 H7A 120.4 . . ? C2 C7 H7A 120.4 . . ? O4 C8 O3 124.5(5) . . ? O4 C8 C5 119.0(5) . . ? O3 C8 C5 116.5(5) . . ? O5 C9 O6 125.3(5) . . ? O5 C9 C10 118.1(5) . . ? O6 C9 C10 116.6(5) . . ? C15 C10 C11 117.2(5) . . ? C15 C10 C9 122.3(5) . . ? C11 C10 C9 120.5(5) . . ? C12 C11 C10 121.5(6) . . ? C12 C11 H11A 119.3 . . ? C10 C11 H11A 119.3 . . ? C11 C12 C13 120.3(6) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? C14 C13 C12 118.7(5) . . ? C14 C13 C16 120.9(5) . . ? C12 C13 C16 120.4(5) . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14A 119.4 . . ? C15 C14 H14A 119.4 . . ? C10 C15 C14 121.1(5) . . ? C10 C15 H15A 119.4 . . ? C14 C15 H15A 119.4 . . ? O7 C16 O8 125.7(6) . . ? O7 C16 C13 117.4(6) . . ? O8 C16 C13 116.9(5) . . ? O9 C17 O10 124.8(5) . . ? O9 C17 C18 118.1(5) . . ? O10 C17 C18 117.0(5) . . ? C19 C18 C23 117.7(5) . . ? C19 C18 C17 121.2(5) . . ? C23 C18 C17 121.1(5) . . ? C20 C19 C18 121.7(5) . . ? C20 C19 H19A 119.2 . . ? C18 C19 H19A 119.2 . . ? C19 C20 C21 119.7(5) . . ? C19 C20 H20A 120.2 . . ? C21 C20 H20A 120.2 . . ? C20 C21 C22 119.1(5) . . ? C20 C21 C24 120.2(5) . . ? C22 C21 C24 120.7(5) . . ? C23 C22 C21 120.4(5) . . ? C23 C22 H22A 119.8 . . ? C21 C22 H22A 119.8 . . ? C22 C23 C18 121.4(5) . . ? C22 C23 H23A 119.3 . . ? C18 C23 H23A 119.3 . . ? O11 C24 O12 124.3(6) . . ? O11 C24 C21 118.1(5) . . ? O12 C24 C21 117.5(5) . . ? N1 C25 C26 124.4(5) . . ? N1 C25 H25A 117.8 . . ? C26 C25 H25A 117.8 . . ? C25 C26 C27 118.9(6) . . ? C25 C26 H26A 120.6 . . ? C27 C26 H26A 120.6 . . ? N2 C27 C26 122.4(6) . . ? N2 C27 C28 119.1(6) . . ? C26 C27 C28 118.4(5) . . ? C29 C28 C27 119.1(6) . . ? C29 C28 H28A 120.4 . . ? C27 C28 H28A 120.4 . . ? N1 C29 C28 122.6(5) . . ? N1 C29 H29A 118.7 . . ? C28 C29 H29A 118.7 . . ? N3 C30 C31 124.8(6) . . ? N3 C30 C34 119.0(5) . . ? C31 C30 C34 116.2(5) . . ? C30 C31 C32 119.7(6) . . ? C30 C31 H31A 120.2 . . ? C32 C31 H31A 120.2 . . ? N4 C32 C31 124.8(5) . . ? N4 C32 H32A 117.6 . . ? C31 C32 H32A 117.6 . . ? N4 C33 C34 122.6(6) . . ? N4 C33 H33A 118.7 . . ? C34 C33 H33A 118.7 . . ? C33 C34 C30 120.4(6) . . ? C33 C34 H34A 119.8 . . ? C30 C34 H34A 119.8 . . ? O14 C35 O13 126.4(6) . . ? O14 C35 C36 117.5(5) . . ? O13 C35 C36 116.2(5) . . ? C41 C36 C37 117.7(6) . . ? C41 C36 C35 120.3(5) . . ? C37 C36 C35 122.0(5) . . ? C36 C37 C38 121.7(5) . . ? C36 C37 H37A 119.1 . . ? C38 C37 H37A 119.1 . . ? C39 C38 C37 119.2(6) . . ? C39 C38 H38A 120.4 . . ? C37 C38 H38A 120.4 . . ? C40 C39 C38 119.6(6) . . ? C40 C39 C42 121.4(5) . . ? C38 C39 C42 118.9(5) . . ? C39 C40 C41 120.9(6) . . ? C39 C40 H40A 119.6 . . ? C41 C40 H40A 119.6 . . ? C36 C41 C40 120.9(6) . . ? C36 C41 H41A 119.6 . . ? C40 C41 H41A 119.6 . . ? O15 C42 O16 125.8(6) . . ? O15 C42 C39 117.9(5) . . ? O16 C42 C39 116.2(5) . . ? N5 C43 C44 124.4(6) . . ? N5 C43 H43A 117.8 . . ? C44 C43 H43A 117.8 . . ? C45 C44 C43 118.2(6) . . ? C45 C44 H44A 120.9 . . ? C43 C44 H44A 120.9 . . ? C44 C45 N6 124.1(7) . . ? C44 C45 C46 118.8(6) . . ? N6 C45 C46 117.0(7) . . ? C47 C46 C45 118.6(6) . . ? C47 C46 H46A 120.7 . . ? C45 C46 H46A 120.7 . . ? N5 C47 C46 122.6(6) . . ? N5 C47 H47A 118.7 . . ? C46 C47 H47A 118.7 . . ? C52 C48 N7 125.2(7) . . ? C52 C48 C49 118.8(6) . . ? N7 C48 C49 116.0(7) . . ? C50 C49 C48 118.3(7) . . ? C50 C49 H49A 120.8 . . ? C48 C49 H49A 120.8 . . ? N8 C50 C49 121.8(7) . . ? N8 C50 H50A 119.1 . . ? C49 C50 H50A 119.1 . . ? N8 C51 C52 125.6(6) . . ? N8 C51 H51A 117.2 . . ? C52 C51 H51A 117.2 . . ? C48 C52 C51 118.4(6) . . ? C48 C52 H52A 120.8 . . ? C51 C52 H52A 120.8 . . ? C25 N1 C29 116.5(5) . . ? C25 N1 Zn2 122.6(4) . . ? C29 N1 Zn2 120.8(4) . . ? C27 N2 N3 118.1(5) . . ? C27 N2 H2A 121.0 . . ? N3 N2 H2A 121.0 . . ? C30 N3 N2 119.1(5) . . ? C30 N3 H3B 120.5 . . ? N2 N3 H3B 120.5 . . ? C32 N4 C33 116.0(5) . . ? C32 N4 Zn3 122.2(4) . 1_556 ? C33 N4 Zn3 121.0(4) . 1_556 ? C43 N5 C47 117.3(5) . . ? C43 N5 Zn4 122.4(4) . . ? C47 N5 Zn4 120.2(4) . . ? N7 N6 C45 116.1(7) . . ? N7 N6 H6B 121.9 . . ? C45 N6 H6B 121.9 . . ? N6 N7 C48 116.8(7) . . ? N6 N7 H7B 121.6 . . ? C48 N7 H7B 121.6 . . ? C51 N8 C50 116.9(5) . . ? C51 N8 Zn1 121.9(4) . 1_545 ? C50 N8 Zn1 120.1(4) . 1_545 ? C1 O1 Zn1 124.6(4) . . ? C1 O2 Zn2 131.0(4) . . ? C8 O3 Zn3 130.7(4) . 1_566 ? C8 O4 Zn4 126.4(4) . 1_566 ? C9 O5 Zn1 128.0(4) . . ? C9 O6 Zn2 127.2(4) . . ? C16 O7 Zn2 132.5(4) . 1_455 ? C16 O8 Zn1 122.3(4) . 1_455 ? C17 O9 Zn1 132.3(4) . . ? C17 O10 Zn2 123.9(4) . . ? C24 O11 Zn3 126.3(4) . . ? C24 O12 Zn4 130.8(4) . . ? C35 O13 Zn3 120.7(4) . . ? C35 O14 Zn4 134.3(4) . . ? C42 O15 Zn3 130.9(4) . 1_455 ? C42 O16 Zn4 124.7(4) . 1_455 ? 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 C27 N2 N3 C30 149.4(6) . . . . ? C45 N6 N7 C48 -142.9(7) . . . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.065 _refine_diff_density_min -0.620 _refine_diff_density_rms 0.102 # 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 -0.052 -0.008 -0.017 1481.9 209.6 _platon_squeeze_details ; ; data_2b _database_code_depnum_ccdc_archive 'CCDC 822610' #TrackingRef '- 1a-2b.R2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H30 N5 O10.50 Zn2' _chemical_formula_weight 759.33 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9028(13) _cell_length_b 10.9453(13) _cell_length_c 15.8533(18) _cell_angle_alpha 88.159(2) _cell_angle_beta 80.542(2) _cell_angle_gamma 85.314(2) _cell_volume 1859.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas . _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method . _exptl_crystal_F_000 778 _exptl_absorpt_coefficient_mu 1.347 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7125 _exptl_absorpt_correction_T_max 0.7651 _exptl_absorpt_process_details 'Blessing, R. H. (1995) Acta Cryst. A51, 33-38.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13655 _diffrn_reflns_av_R_equivalents 0.0276 _diffrn_reflns_av_sigmaI/netI 0.0490 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7217 _reflns_number_gt 5202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0570P)^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 7217 _refine_ls_number_parameters 425 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0574 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1105 _refine_ls_wR_factor_gt 0.1038 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 0.28242(3) 0.15772(3) 0.40630(2) 0.03398(11) Uani 1 1 d . . . Zn2 Zn 0.32970(3) 0.16287(3) 0.21524(2) 0.03352(11) Uani 1 1 d . . . C1 C 0.3031(3) 0.3954(3) 0.3064(2) 0.0463(8) Uani 1 1 d . A . C2 C 0.3053(3) 0.5333(3) 0.3055(2) 0.0446(8) Uani 1 1 d . . . C3 C 0.2854(4) 0.5952(3) 0.3806(2) 0.0732(13) Uani 1 1 d . . . H3A H 0.2700 0.5518 0.4321 0.088 Uiso 1 1 calc R . . C4 C 0.2877(4) 0.7211(3) 0.3810(2) 0.0728(13) Uani 1 1 d . . . H4A H 0.2739 0.7612 0.4330 0.087 Uiso 1 1 calc R . . C5 C 0.3098(3) 0.7875(3) 0.3071(2) 0.0447(8) Uani 1 1 d . . . C6 C 0.3307(4) 0.7256(3) 0.2314(2) 0.0748(13) Uani 1 1 d . . . H6A H 0.3474 0.7689 0.1799 0.090 Uiso 1 1 calc R . . C7 C 0.3270(4) 0.6007(3) 0.2312(2) 0.0742(13) Uani 1 1 d . . . H7A H 0.3396 0.5608 0.1792 0.089 Uiso 1 1 calc R . . C8 C 0.3120(3) 0.9246(3) 0.3079(2) 0.0468(8) Uani 1 1 d . . . C9 C 0.5419(3) 0.1529(3) 0.3094(2) 0.0451(8) Uani 1 1 d . A . C10 C 0.6793(3) 0.1564(3) 0.3116(2) 0.0462(8) Uani 1 1 d . . . C11 C 0.7618(3) 0.1729(4) 0.2366(2) 0.0650(11) Uani 1 1 d . . . H11A H 0.7327 0.1811 0.1846 0.078 Uiso 1 1 calc R . . C12 C 0.8874(3) 0.1772(4) 0.2391(2) 0.0646(11) Uani 1 1 d . . . H12A H 0.9422 0.1896 0.1887 0.077 Uiso 1 1 calc R . . C13 C 0.9329(3) 0.1632(3) 0.3161(2) 0.0454(8) Uani 1 1 d . . . C14 C 0.8486(3) 0.1479(3) 0.3911(2) 0.0451(8) Uani 1 1 d . . . H14A H 0.8771 0.1407 0.4433 0.054 Uiso 1 1 calc R . . C15 C 0.7247(3) 0.1435(3) 0.3888(2) 0.0456(8) Uani 1 1 d . . . H15A H 0.6698 0.1317 0.4393 0.055 Uiso 1 1 calc R . . C16 C 1.0692(3) 0.1661(3) 0.3175(2) 0.0437(8) Uani 1 1 d . . . C17 C 0.2330(5) 0.1664(5) -0.2888(3) 0.0824(14) Uani 1 1 d . . . C18 C 0.3490(4) 0.1668(4) -0.3364(3) 0.0794(13) Uani 1 1 d . A . H18A H 0.4197 0.1697 -0.3110 0.095 Uiso 1 1 calc R . . C19 C 0.3568(4) 0.1625(3) -0.4230(2) 0.0582(10) Uani 1 1 d . . . H19A H 0.4360 0.1595 -0.4557 0.070 Uiso 1 1 calc R A . C20 C 0.1474(4) 0.1631(3) -0.4165(2) 0.0572(9) Uani 1 1 d . . . H20A H 0.0782 0.1610 -0.4435 0.069 Uiso 1 1 calc R A . C21 C 0.1283(4) 0.1667(4) -0.3286(2) 0.0713(12) Uani 1 1 d . A . H21A H 0.0484 0.1693 -0.2969 0.086 Uiso 1 1 calc R . . C1A C 0.3863(9) 0.2727(8) 0.0423(5) 0.078(3) Uani 0.496(5) 1 d P A 1 H1AA H 0.4263 0.3259 0.0712 0.093 Uiso 0.496(5) 1 calc PR A 1 C2A C 0.3755(11) 0.3009(9) -0.0403(5) 0.097(4) Uani 0.496(5) 1 d P A 1 H2AA H 0.4109 0.3693 -0.0673 0.116 Uiso 0.496(5) 1 calc PR A 1 C3A C 0.3121(17) 0.2278(14) -0.0829(8) 0.080(3) Uani 0.496(5) 1 d P A 1 C4A C 0.268(2) 0.1239(18) -0.0412(11) 0.082(4) Uani 0.496(5) 1 d P A 1 H4AA H 0.2312 0.0668 -0.0691 0.099 Uiso 0.496(5) 1 calc PR A 1 C5A C 0.2808(9) 0.1083(9) 0.0445(5) 0.071(3) Uani 0.496(5) 1 d P A 1 H5AA H 0.2393 0.0448 0.0737 0.085 Uiso 0.496(5) 1 calc PR A 1 C1B C 0.2556(9) 0.2174(9) 0.0486(5) 0.070(3) Uani 0.504(5) 1 d P A 2 H1BA H 0.1945 0.2689 0.0806 0.084 Uiso 0.504(5) 1 calc PR A 2 C2B C 0.2441(14) 0.202(2) -0.0375(9) 0.085(4) Uani 0.504(5) 1 d P A 2 H2BA H 0.1796 0.2436 -0.0613 0.102 Uiso 0.504(5) 1 calc PR A 2 C3B C 0.3325(14) 0.1238(19) -0.0853(8) 0.084(4) Uani 0.504(5) 1 d P A 2 C4B C 0.4135(11) 0.0585(13) -0.0423(6) 0.151(6) Uani 0.504(5) 1 d P A 2 H4BA H 0.4654 -0.0048 -0.0699 0.181 Uiso 0.504(5) 1 calc PR A 2 C5B C 0.4218(10) 0.0822(10) 0.0397(5) 0.110(5) Uani 0.504(5) 1 d P A 2 H5BA H 0.4838 0.0394 0.0651 0.132 Uiso 0.504(5) 1 calc PR A 2 N1 N 0.3407(3) 0.1681(3) 0.08718(17) 0.0500(7) Uani 1 1 d . . . N2 N 0.2595(3) 0.1624(2) -0.46485(16) 0.0425(6) Uani 1 1 d . . . N3A N 0.2047(15) 0.2041(10) -0.1991(8) 0.095(4) Uani 0.504(5) 1 d P A 1 H3AA H 0.1331 0.1946 -0.1686 0.114 Uiso 0.504(5) 1 calc PR A 1 N4A N 0.3001(10) 0.2566(10) -0.1647(5) 0.121(4) Uani 0.496(5) 1 d P A 1 H4AB H 0.3486 0.3051 -0.1949 0.145 Uiso 0.496(5) 1 calc PR A 1 N3B N 0.2234(14) 0.1319(10) -0.1999(7) 0.092(4) Uani 0.496(5) 1 d P A 2 H3BA H 0.1515 0.1357 -0.1678 0.110 Uiso 0.496(5) 1 calc PR A 2 N4B N 0.3275(9) 0.0931(10) -0.1662(5) 0.127(5) Uani 0.504(5) 1 d P A 2 H4BB H 0.3882 0.0503 -0.1957 0.152 Uiso 0.504(5) 1 calc PR A 2 O1 O 1.1402(2) 0.1740(3) 0.24778(16) 0.0625(7) Uani 1 1 d . . . O2 O 1.1026(2) 0.1605(2) 0.38969(15) 0.0584(7) Uani 1 1 d . . . O3 O 0.5088(2) 0.1482(2) 0.23736(16) 0.0615(7) Uani 1 1 d . . . O4 O 0.4696(2) 0.1554(3) 0.37947(16) 0.0620(7) Uani 1 1 d . . . O5 O 0.3270(3) 0.3449(2) 0.23506(16) 0.0641(7) Uani 1 1 d . . . O6 O 0.2781(3) 0.3420(2) 0.37625(15) 0.0616(7) Uani 1 1 d . . . O7 O 0.3259(3) 0.9793(2) 0.23655(17) 0.0657(7) Uani 1 1 d . . . O8 O 0.2995(2) 0.9738(2) 0.37872(16) 0.0625(7) 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 0.0372(2) 0.0359(2) 0.0301(2) -0.00278(15) -0.00771(15) -0.00458(15) Zn2 0.0377(2) 0.03476(19) 0.0293(2) -0.00203(14) -0.00810(15) -0.00417(15) C1 0.050(2) 0.0380(17) 0.053(2) -0.0050(16) -0.0113(17) -0.0039(15) C2 0.056(2) 0.0324(16) 0.0463(19) -0.0030(14) -0.0102(16) -0.0070(14) C3 0.132(4) 0.043(2) 0.043(2) 0.0015(17) -0.006(2) -0.016(2) C4 0.130(4) 0.040(2) 0.048(2) -0.0129(17) -0.007(2) -0.011(2) C5 0.057(2) 0.0322(16) 0.0464(19) -0.0060(14) -0.0114(16) -0.0036(14) C6 0.140(4) 0.0380(19) 0.045(2) 0.0002(17) -0.008(2) -0.012(2) C7 0.139(4) 0.041(2) 0.041(2) -0.0067(16) -0.005(2) -0.013(2) C8 0.050(2) 0.0319(16) 0.062(2) -0.0073(16) -0.0155(18) -0.0037(14) C9 0.0353(18) 0.0500(19) 0.052(2) -0.0057(16) -0.0116(17) -0.0043(15) C10 0.0351(18) 0.059(2) 0.0456(19) -0.0027(16) -0.0095(15) -0.0039(15) C11 0.043(2) 0.114(3) 0.041(2) 0.011(2) -0.0159(17) -0.015(2) C12 0.038(2) 0.112(3) 0.044(2) 0.009(2) -0.0058(17) -0.014(2) C13 0.0368(18) 0.059(2) 0.0427(19) -0.0012(16) -0.0130(15) -0.0061(15) C14 0.0395(19) 0.061(2) 0.0368(18) -0.0020(15) -0.0116(15) -0.0035(16) C15 0.0399(19) 0.060(2) 0.0365(18) -0.0022(15) -0.0045(15) -0.0054(16) C16 0.0376(18) 0.0474(18) 0.047(2) -0.0023(15) -0.0098(16) -0.0050(14) C17 0.094(4) 0.119(4) 0.037(2) -0.005(2) -0.021(2) -0.003(3) C18 0.074(3) 0.118(4) 0.052(3) -0.001(2) -0.027(2) -0.011(3) C19 0.066(3) 0.072(3) 0.041(2) -0.0028(18) -0.0186(19) -0.009(2) C20 0.061(3) 0.070(2) 0.040(2) -0.0041(17) -0.0082(18) -0.0002(19) C21 0.074(3) 0.096(3) 0.039(2) 0.002(2) -0.001(2) 0.004(2) C1A 0.119(8) 0.070(6) 0.050(5) -0.004(4) -0.020(5) -0.032(5) C2A 0.175(11) 0.083(6) 0.038(5) 0.002(4) -0.019(6) -0.043(7) C3A 0.109(10) 0.094(10) 0.038(6) -0.002(6) -0.016(6) -0.013(8) C4A 0.096(13) 0.095(10) 0.067(10) -0.002(10) -0.039(9) -0.020(9) C5A 0.097(7) 0.075(6) 0.046(5) 0.003(4) -0.017(5) -0.029(6) C1B 0.092(7) 0.076(6) 0.037(4) -0.008(4) -0.008(4) 0.025(5) C2B 0.075(9) 0.136(13) 0.041(7) -0.008(9) -0.026(6) 0.043(10) C3B 0.084(9) 0.122(13) 0.040(6) -0.015(7) -0.014(5) 0.034(8) C4B 0.144(11) 0.254(16) 0.042(6) -0.043(7) -0.033(6) 0.114(11) C5B 0.117(9) 0.168(10) 0.037(5) -0.035(5) -0.027(5) 0.087(8) N1 0.0556(19) 0.0636(18) 0.0328(15) -0.0037(14) -0.0128(14) -0.0031(15) N2 0.0482(17) 0.0462(15) 0.0337(15) -0.0020(12) -0.0076(13) -0.0052(13) N3A 0.128(10) 0.117(9) 0.040(5) -0.010(7) -0.021(5) 0.004(8) N4A 0.169(10) 0.169(10) 0.039(4) 0.012(5) -0.035(5) -0.070(8) N3B 0.107(8) 0.125(10) 0.037(4) -0.013(7) -0.018(4) 0.043(9) N4B 0.126(8) 0.207(12) 0.043(5) -0.037(6) -0.038(5) 0.081(7) O1 0.0344(13) 0.102(2) 0.0507(15) 0.0042(14) -0.0058(12) -0.0074(13) O2 0.0366(13) 0.0912(19) 0.0506(15) -0.0023(13) -0.0155(11) -0.0068(12) O3 0.0414(14) 0.097(2) 0.0501(15) -0.0084(14) -0.0180(12) -0.0079(13) O4 0.0389(14) 0.097(2) 0.0512(15) -0.0062(14) -0.0061(12) -0.0106(13) O5 0.101(2) 0.0328(12) 0.0563(16) -0.0078(11) -0.0032(15) -0.0099(12) O6 0.098(2) 0.0361(12) 0.0519(15) 0.0054(11) -0.0143(14) -0.0117(12) O7 0.098(2) 0.0314(12) 0.0688(18) -0.0002(12) -0.0142(15) -0.0108(12) O8 0.091(2) 0.0339(12) 0.0657(17) -0.0120(12) -0.0186(15) -0.0048(12) _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 2.014(2) . ? Zn1 O2 2.018(2) 1_455 ? Zn1 N2 2.018(3) 1_556 ? Zn1 O6 2.056(2) . ? Zn1 O8 2.060(2) 1_545 ? Zn1 Zn2 2.9873(6) . ? Zn2 N1 2.013(3) . ? Zn2 O5 2.024(2) . ? Zn2 O7 2.030(2) 1_545 ? Zn2 O3 2.033(2) . ? Zn2 O1 2.040(2) 1_455 ? C1 O6 1.235(4) . ? C1 O5 1.254(4) . ? C1 C2 1.512(4) . ? C2 C3 1.365(5) . ? C2 C7 1.366(4) . ? C3 C4 1.381(5) . ? C4 C5 1.357(5) . ? C5 C6 1.373(5) . ? C5 C8 1.503(4) . ? C6 C7 1.372(5) . ? C8 O8 1.244(4) . ? C8 O7 1.255(4) . ? C9 O4 1.252(4) . ? C9 O3 1.257(4) . ? C9 C10 1.508(4) . ? C10 C11 1.384(5) . ? C10 C15 1.393(4) . ? C11 C12 1.381(5) . ? C12 C13 1.391(4) . ? C13 C14 1.393(4) . ? C13 C16 1.492(4) . ? C14 C15 1.362(4) . ? C16 O1 1.245(4) . ? C16 O2 1.256(4) . ? C17 C18 1.362(6) . ? C17 C21 1.391(6) . ? C17 N3B 1.436(12) . ? C17 N3A 1.470(12) . ? C18 C19 1.364(5) . ? C19 N2 1.340(4) . ? C20 N2 1.331(4) . ? C20 C21 1.376(5) . ? C1A C2A 1.357(11) . ? C1A N1 1.410(8) . ? C2A C3A 1.361(14) . ? C3A N4A 1.349(12) . ? C3A C4A 1.38(2) . ? C4A C5A 1.392(16) . ? C5A N1 1.248(9) . ? C1B N1 1.269(8) . ? C1B C2B 1.407(14) . ? C2B C3B 1.38(2) . ? C3B N4B 1.347(12) . ? C3B C4B 1.349(15) . ? C4B C5B 1.352(11) . ? C5B N1 1.387(9) . ? N2 Zn1 2.018(3) 1_554 ? N3A N4A 1.419(16) . ? N3B N4B 1.364(14) . ? O1 Zn2 2.040(2) 1_655 ? O2 Zn1 2.018(2) 1_655 ? O7 Zn2 2.030(2) 1_565 ? O8 Zn1 2.060(2) 1_565 ? 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 O2 160.58(10) . 1_455 ? O4 Zn1 N2 99.51(11) . 1_556 ? O2 Zn1 N2 99.90(10) 1_455 1_556 ? O4 Zn1 O6 87.11(11) . . ? O2 Zn1 O6 88.71(11) 1_455 . ? N2 Zn1 O6 100.62(10) 1_556 . ? O4 Zn1 O8 87.94(11) . 1_545 ? O2 Zn1 O8 87.77(10) 1_455 1_545 ? N2 Zn1 O8 104.66(10) 1_556 1_545 ? O6 Zn1 O8 154.71(10) . 1_545 ? O4 Zn1 Zn2 77.55(7) . . ? O2 Zn1 Zn2 83.04(7) 1_455 . ? N2 Zn1 Zn2 176.10(8) 1_556 . ? O6 Zn1 Zn2 76.80(7) . . ? O8 Zn1 Zn2 77.92(7) 1_545 . ? N1 Zn2 O5 98.77(11) . . ? N1 Zn2 O7 99.49(11) . 1_545 ? O5 Zn2 O7 161.72(11) . 1_545 ? N1 Zn2 O3 105.78(11) . . ? O5 Zn2 O3 87.61(11) . . ? O7 Zn2 O3 88.31(11) 1_545 . ? N1 Zn2 O1 98.45(11) . 1_455 ? O5 Zn2 O1 89.27(11) . 1_455 ? O7 Zn2 O1 87.17(11) 1_545 1_455 ? O3 Zn2 O1 155.76(10) . 1_455 ? N1 Zn2 Zn1 173.59(9) . . ? O5 Zn2 Zn1 81.22(7) . . ? O7 Zn2 Zn1 80.53(8) 1_545 . ? O3 Zn2 Zn1 80.64(7) . . ? O1 Zn2 Zn1 75.13(7) 1_455 . ? O6 C1 O5 125.6(3) . . ? O6 C1 C2 118.1(3) . . ? O5 C1 C2 116.3(3) . . ? C3 C2 C7 117.6(3) . . ? C3 C2 C1 120.1(3) . . ? C7 C2 C1 122.3(3) . . ? C2 C3 C4 121.0(3) . . ? C5 C4 C3 121.2(3) . . ? C4 C5 C6 118.0(3) . . ? C4 C5 C8 121.0(3) . . ? C6 C5 C8 121.0(3) . . ? C7 C6 C5 120.6(3) . . ? C2 C7 C6 121.6(3) . . ? O8 C8 O7 125.7(3) . . ? O8 C8 C5 117.5(3) . . ? O7 C8 C5 116.8(3) . . ? O4 C9 O3 125.1(3) . . ? O4 C9 C10 117.5(3) . . ? O3 C9 C10 117.5(3) . . ? C11 C10 C15 119.2(3) . . ? C11 C10 C9 120.2(3) . . ? C15 C10 C9 120.6(3) . . ? C12 C11 C10 119.9(3) . . ? C11 C12 C13 120.9(3) . . ? C12 C13 C14 118.5(3) . . ? C12 C13 C16 120.1(3) . . ? C14 C13 C16 121.3(3) . . ? C15 C14 C13 120.7(3) . . ? C14 C15 C10 120.8(3) . . ? O1 C16 O2 125.3(3) . . ? O1 C16 C13 118.0(3) . . ? O2 C16 C13 116.6(3) . . ? C18 C17 C21 120.3(4) . . ? C18 C17 N3B 118.1(7) . . ? C21 C17 N3B 119.4(7) . . ? C18 C17 N3A 123.2(7) . . ? C21 C17 N3A 113.8(7) . . ? N3B C17 N3A 31.9(5) . . ? C17 C18 C19 117.0(4) . . ? N2 C19 C18 125.3(4) . . ? N2 C20 C21 123.6(4) . . ? C20 C21 C17 117.5(4) . . ? C2A C1A N1 124.3(8) . . ? C1A C2A C3A 119.1(9) . . ? N4A C3A C2A 119.1(10) . . ? N4A C3A C4A 122.9(11) . . ? C2A C3A C4A 117.9(10) . . ? C3A C4A C5A 117.1(12) . . ? N1 C5A C4A 128.6(9) . . ? N1 C1B C2B 126.8(8) . . ? C3B C2B C1B 117.3(10) . . ? N4B C3B C4B 118.7(11) . . ? N4B C3B C2B 123.7(10) . . ? C4B C3B C2B 116.4(11) . . ? C3B C4B C5B 122.0(10) . . ? C4B C5B N1 122.2(8) . . ? C5A N1 C1B 57.2(5) . . ? C5A N1 C5B 70.8(6) . . ? C1B N1 C5B 114.4(5) . . ? C5A N1 C1A 112.3(5) . . ? C1B N1 C1A 72.1(6) . . ? C5B N1 C1A 96.7(7) . . ? C5A N1 Zn2 126.6(4) . . ? C1B N1 Zn2 123.9(4) . . ? C5B N1 Zn2 118.4(4) . . ? C1A N1 Zn2 117.9(4) . . ? C20 N2 C19 116.1(3) . . ? C20 N2 Zn1 122.1(2) . 1_554 ? C19 N2 Zn1 121.7(2) . 1_554 ? N4A N3A C17 117.5(11) . . ? C3A N4A N3A 117.9(10) . . ? N4B N3B C17 120.4(11) . . ? C3B N4B N3B 118.2(9) . . ? C16 O1 Zn2 132.8(2) . 1_655 ? C16 O2 Zn1 123.3(2) . 1_655 ? C9 O3 Zn2 125.5(2) . . ? C9 O4 Zn1 130.9(2) . . ? C1 O5 Zn2 125.6(2) . . ? C1 O6 Zn1 130.3(2) . . ? C8 O7 Zn2 126.7(2) . 1_565 ? C8 O8 Zn1 128.8(2) . 1_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 N3A N4A C3A -142.0(13) . . . . ? C17 N3B N4B C3B 144.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.528 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.082 # 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 -0.003 0.055 -0.002 695.0 101.7 _platon_squeeze_details ; ;