# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 917619' #TrackingRef 'complex_2-917619.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H66 N12 O13 Zn2' _chemical_formula_weight 1630.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' H H 0.0000 0.0000 '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 9.887(5) _cell_length_b 12.748(4) _cell_length_c 15.965(5) _cell_angle_alpha 100.459(4) _cell_angle_beta 95.864(19) _cell_angle_gamma 102.289(19) _cell_volume 1912.6(13) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5222 _cell_measurement_theta_min 2.8006 _cell_measurement_theta_max 27.5205 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.702 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7665 _exptl_absorpt_correction_T_max 0.8723 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _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 Mercury70_(2x2_bin_mode) _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23707 _diffrn_reflns_av_R_equivalents 0.0290 _diffrn_reflns_av_unetI/netI 0.0349 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 27.58 _reflns_number_total 8728 _reflns_number_gt 7004 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Some restraints were applied and listed as follows: DELU 0.002 N2 C10 SIMU 0.002 N2 C10 ; _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^)+(0.1056P)^2^+0.9081P] 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 8728 _refine_ls_number_parameters 532 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1802 _refine_ls_wR_factor_gt 0.1667 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.064 _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 0.74883(4) -0.31651(2) 0.45334(2) 0.03970(14) Uani 1 1 d . . . O1 O 0.8513(3) -0.2425(2) 0.37449(19) 0.0736(8) Uani 1 1 d . . . O2 O 0.8991(4) -0.3909(2) 0.3027(2) 0.0786(9) Uani 1 1 d . . . O3 O 0.6568(3) -1.20065(17) 0.49145(17) 0.0556(6) Uani 1 1 d . . . O4 O 0.6988(3) -1.14221(18) 0.63272(16) 0.0546(6) Uani 1 1 d . . . O5 O 1.4320(7) 0.3419(6) -0.0968(5) 0.0865(19) Uani 0.50 1 d P . . O6 O 1.3377(6) -0.3190(4) -0.0123(4) 0.1413(18) Uani 1 1 d . . . O7A O 0.6731(8) -0.5159(5) 0.1617(4) 0.124(2) Uani 0.80 1 d P A 1 O7B O 0.725(3) -0.560(2) 0.1995(17) 0.125(8) Uani 0.20 1 d P B 2 N1 N 1.4141(5) 0.0317(4) -0.1461(3) 0.0983(14) Uani 1 1 d . . . N2 N 1.2516(3) 0.1082(3) -0.01930(19) 0.0571(6) Uani 1 1 d U . . N3 N 1.2255(5) 0.3276(3) 0.0227(3) 0.0796(11) Uani 1 1 d . . . N4 N 0.5650(3) -0.4177(2) 0.36557(17) 0.0439(6) Uani 1 1 d . . . N5 N 0.7291(2) -0.47277(18) 0.47817(15) 0.0334(5) Uani 1 1 d . . . N6 N 0.9146(3) -0.29638(19) 0.56027(18) 0.0423(6) Uani 1 1 d . . . C1 C 0.8985(3) -0.2937(3) 0.3132(2) 0.0499(8) Uani 1 1 d . . . C2 C 0.9588(3) -0.2252(3) 0.2525(2) 0.0427(7) Uani 1 1 d . . . C3 C 1.0338(4) -0.2660(3) 0.1923(2) 0.0536(8) Uani 1 1 d . . . H3 H 1.0438 -0.3377 0.1875 0.064 Uiso 1 1 calc R . . C4 C 1.0952(4) -0.2022(3) 0.1384(2) 0.0520(8) Uani 1 1 d . . . H4 H 1.1465 -0.2312 0.0984 0.062 Uiso 1 1 calc R . . C5 C 1.0807(3) -0.0954(2) 0.14371(18) 0.0395(6) Uani 1 1 d . . . C6 C 0.9444(4) -0.1186(3) 0.2580(2) 0.0558(9) Uani 1 1 d . . . H6 H 0.8933 -0.0897 0.2984 0.067 Uiso 1 1 calc R . . C7 C 1.0052(4) -0.0541(3) 0.2041(2) 0.0557(9) Uani 1 1 d . . . H7 H 0.9947 0.0174 0.2088 0.067 Uiso 1 1 calc R . . C8 C 1.1432(3) -0.0247(3) 0.08586(18) 0.0392(6) Uani 1 1 d . . . C9 C 1.2222(3) -0.0622(3) 0.02611(19) 0.0410(6) Uani 1 1 d . . . H9 H 1.2385 -0.1320 0.0219 0.049 Uiso 1 1 calc R . . C10 C 1.2770(3) 0.0037(3) -0.0272(2) 0.0479(6) Uani 1 1 d U . . C11 C 1.1189(3) 0.0758(2) 0.09426(17) 0.0341(6) Uani 1 1 d . . . H11 H 1.0651 0.0995 0.1350 0.041 Uiso 1 1 calc R . . C12 C 1.1729(3) 0.1422(3) 0.0434(2) 0.0441(7) Uani 1 1 d . . . C13 C 1.1428(4) 0.2523(3) 0.0551(2) 0.0550(8) Uani 1 1 d . . . C14 C 1.0341(4) 0.2755(4) 0.0970(3) 0.0670(11) Uani 1 1 d . . . H14 H 0.9784 0.2210 0.1185 0.080 Uiso 1 1 calc R . . C15 C 1.0073(6) 0.3770(5) 0.1074(3) 0.0904(17) Uani 1 1 d . . . H15 H 0.9348 0.3933 0.1362 0.108 Uiso 1 1 calc R . . C16 C 1.0907(8) 0.4543(5) 0.0739(3) 0.104(2) Uani 1 1 d . . . H16 H 1.0744 0.5243 0.0792 0.124 Uiso 1 1 calc R . . C17 C 1.1982(8) 0.4292(4) 0.0325(4) 0.1025(19) Uani 1 1 d . . . H17 H 1.2541 0.4830 0.0104 0.123 Uiso 1 1 calc R . . C18 C 1.3622(3) -0.0356(3) -0.0931(2) 0.0542(9) Uani 1 1 d . . . C19 C 1.3883(4) -0.1345(3) -0.0977(2) 0.0570(9) Uani 1 1 d . . . H19 H 1.3506 -0.1795 -0.0619 0.068 Uiso 1 1 calc R . . C20 C 1.4692(5) -0.1693(5) -0.1543(3) 0.0845(15) Uani 1 1 d . . . H20 H 1.4867 -0.2386 -0.1569 0.101 Uiso 1 1 calc R . . C21 C 1.5267(5) -0.1061(5) -0.2083(3) 0.0870(17) Uani 1 1 d . . . H21 H 1.5831 -0.1312 -0.2467 0.104 Uiso 1 1 calc R . . C22 C 1.4992(6) -0.0063(6) -0.2042(3) 0.0934(17) Uani 1 1 d . . . H22 H 1.5371 0.0380 -0.2403 0.112 Uiso 1 1 calc R . . C23 C 0.6831(3) -1.1257(2) 0.5604(2) 0.0404(7) Uani 1 1 d . . . C24 C 0.6898(3) -1.0109(2) 0.54533(19) 0.0364(6) Uani 1 1 d . . . C25 C 0.6566(3) -0.9925(2) 0.4636(2) 0.0404(6) Uani 1 1 d . . . H25 H 0.6324 -1.0514 0.4166 0.049 Uiso 1 1 calc R . . C26 C 0.6589(3) -0.8879(2) 0.45123(19) 0.0394(6) Uani 1 1 d . . . H26 H 0.6312 -0.8776 0.3964 0.047 Uiso 1 1 calc R . . C27 C 0.7022(3) -0.7972(2) 0.51945(19) 0.0361(6) Uani 1 1 d . . . C28 C 0.7368(3) -0.8154(2) 0.6013(2) 0.0413(6) Uani 1 1 d . . . H28 H 0.7656 -0.7562 0.6478 0.050 Uiso 1 1 calc R . . C29 C 0.7288(3) -0.9209(2) 0.6141(2) 0.0403(6) Uani 1 1 d . . . H29 H 0.7497 -0.9319 0.6695 0.048 Uiso 1 1 calc R . . C30 C 0.7113(3) -0.6841(2) 0.50526(18) 0.0366(6) Uani 1 1 d . . . C31 C 0.8169(3) -0.5957(2) 0.55224(19) 0.0377(6) Uani 1 1 d . . . H31 H 0.8831 -0.6070 0.5933 0.045 Uiso 1 1 calc R . . C32 C 0.8225(3) -0.4910(2) 0.53748(18) 0.0340(6) Uani 1 1 d . . . C33 C 0.6278(3) -0.5563(2) 0.43270(17) 0.0347(6) Uani 1 1 d . . . C34 C 0.6159(3) -0.6631(2) 0.44472(19) 0.0371(6) Uani 1 1 d . . . H34 H 0.5443 -0.7200 0.4123 0.044 Uiso 1 1 calc R . . C35 C 0.5301(3) -0.5238(2) 0.37036(18) 0.0368(6) Uani 1 1 d . . . C36 C 0.4103(3) -0.5962(3) 0.3225(2) 0.0481(7) Uani 1 1 d . . . H36 H 0.3862 -0.6691 0.3279 0.058 Uiso 1 1 calc R . . C37 C 0.3286(4) -0.5562(3) 0.2668(2) 0.0607(9) Uani 1 1 d . . . H37 H 0.2474 -0.6021 0.2340 0.073 Uiso 1 1 calc R . . C38 C 0.3672(5) -0.4484(3) 0.2598(3) 0.0687(11) Uani 1 1 d . . . H38 H 0.3145 -0.4215 0.2207 0.082 Uiso 1 1 calc R . . C39 C 0.4844(4) -0.3810(3) 0.3113(2) 0.0604(9) Uani 1 1 d . . . H39 H 0.5083 -0.3073 0.3082 0.072 Uiso 1 1 calc R . . C40 C 0.9270(3) -0.3898(2) 0.58606(19) 0.0366(6) Uani 1 1 d . . . C41 C 1.0258(4) -0.3898(3) 0.6522(2) 0.0504(8) Uani 1 1 d . . . H41 H 1.0333 -0.4552 0.6682 0.060 Uiso 1 1 calc R . . C42 C 1.1153(4) -0.2909(3) 0.6955(3) 0.0590(9) Uani 1 1 d . . . H42 H 1.1839 -0.2892 0.7405 0.071 Uiso 1 1 calc R . . C43 C 1.1009(4) -0.1956(3) 0.6707(3) 0.0567(9) Uani 1 1 d . . . H43 H 1.1583 -0.1283 0.6993 0.068 Uiso 1 1 calc R . . C44 C 1.0004(4) -0.2016(3) 0.6029(3) 0.0536(8) Uani 1 1 d . . . H44 H 0.9917 -0.1370 0.5858 0.064 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0534(2) 0.02469(18) 0.0455(2) 0.01254(14) 0.01607(16) 0.01032(14) O1 0.098(2) 0.0584(16) 0.0690(17) 0.0242(13) 0.0442(16) 0.0044(14) O2 0.109(2) 0.0574(17) 0.092(2) 0.0446(16) 0.0406(18) 0.0316(16) O3 0.0693(15) 0.0285(11) 0.0684(16) 0.0033(10) 0.0035(12) 0.0193(10) O4 0.0779(16) 0.0359(12) 0.0569(14) 0.0194(10) 0.0170(12) 0.0171(11) O5 0.081(4) 0.080(4) 0.114(5) 0.048(4) 0.037(4) 0.020(3) O6 0.156(4) 0.105(4) 0.175(5) 0.042(3) 0.051(4) 0.033(3) O7A 0.148(5) 0.101(4) 0.106(5) 0.001(3) 0.016(4) 0.015(4) O7B 0.130(19) 0.14(2) 0.103(17) 0.021(15) -0.006(14) 0.034(16) N1 0.096(3) 0.130(4) 0.071(3) 0.022(3) 0.028(2) 0.024(3) N2 0.0587(14) 0.0582(14) 0.0512(14) 0.0115(12) 0.0095(12) 0.0063(12) N3 0.120(3) 0.053(2) 0.073(2) 0.0255(17) 0.019(2) 0.025(2) N4 0.0602(16) 0.0323(12) 0.0422(14) 0.0107(10) 0.0068(12) 0.0154(11) N5 0.0417(12) 0.0232(10) 0.0365(12) 0.0081(9) 0.0098(10) 0.0070(9) N6 0.0431(13) 0.0252(11) 0.0573(16) 0.0071(10) 0.0114(11) 0.0045(9) C1 0.0497(17) 0.0528(19) 0.0505(19) 0.0232(15) 0.0089(15) 0.0084(14) C2 0.0453(16) 0.0435(16) 0.0413(16) 0.0154(13) 0.0078(13) 0.0089(13) C3 0.082(2) 0.0373(16) 0.0497(18) 0.0148(14) 0.0191(17) 0.0212(16) C4 0.076(2) 0.0465(18) 0.0433(17) 0.0132(14) 0.0248(16) 0.0252(16) C5 0.0451(15) 0.0417(15) 0.0338(14) 0.0114(12) 0.0081(12) 0.0107(12) C6 0.068(2) 0.053(2) 0.063(2) 0.0238(17) 0.0350(18) 0.0264(17) C7 0.074(2) 0.0472(19) 0.064(2) 0.0280(16) 0.0327(18) 0.0289(17) C8 0.0397(14) 0.0433(16) 0.0344(14) 0.0107(12) 0.0049(11) 0.0073(12) C9 0.0452(16) 0.0398(15) 0.0385(15) 0.0073(12) 0.0061(12) 0.0114(12) C10 0.0464(14) 0.0529(15) 0.0411(14) 0.0083(12) 0.0054(12) 0.0062(12) C11 0.0383(14) 0.0372(14) 0.0307(13) 0.0112(11) 0.0097(11) 0.0117(11) C12 0.0457(16) 0.0473(17) 0.0380(15) 0.0110(13) 0.0029(12) 0.0077(13) C13 0.068(2) 0.052(2) 0.0423(18) 0.0101(15) -0.0046(16) 0.0144(16) C14 0.072(2) 0.065(2) 0.058(2) -0.0070(19) -0.0060(19) 0.028(2) C15 0.117(4) 0.084(4) 0.072(3) -0.002(3) -0.017(3) 0.059(3) C16 0.182(6) 0.077(3) 0.057(3) -0.005(2) -0.027(3) 0.078(4) C17 0.176(6) 0.057(3) 0.075(3) 0.023(2) 0.007(4) 0.028(3) C18 0.0450(17) 0.071(2) 0.0393(17) 0.0013(16) 0.0040(14) 0.0084(16) C19 0.057(2) 0.059(2) 0.051(2) -0.0033(16) 0.0144(16) 0.0147(16) C20 0.069(3) 0.097(4) 0.074(3) -0.024(3) 0.008(2) 0.026(2) C21 0.062(3) 0.127(5) 0.056(3) -0.020(3) 0.013(2) 0.018(3) C22 0.085(3) 0.128(5) 0.062(3) 0.008(3) 0.028(2) 0.016(3) C23 0.0398(14) 0.0242(13) 0.0586(19) 0.0084(12) 0.0131(13) 0.0080(10) C24 0.0368(14) 0.0246(12) 0.0504(16) 0.0117(11) 0.0119(12) 0.0072(10) C25 0.0459(15) 0.0266(13) 0.0448(16) 0.0013(11) 0.0083(13) 0.0041(11) C26 0.0469(15) 0.0300(14) 0.0404(15) 0.0078(11) 0.0073(12) 0.0065(11) C27 0.0385(14) 0.0236(12) 0.0451(15) 0.0090(11) 0.0061(12) 0.0036(10) C28 0.0525(17) 0.0233(13) 0.0440(16) 0.0054(11) 0.0013(13) 0.0042(11) C29 0.0509(16) 0.0279(13) 0.0420(16) 0.0093(11) 0.0022(13) 0.0093(11) C30 0.0452(15) 0.0248(12) 0.0408(15) 0.0098(11) 0.0087(12) 0.0068(11) C31 0.0419(14) 0.0264(13) 0.0440(15) 0.0104(11) 0.0022(12) 0.0059(11) C32 0.0403(14) 0.0248(12) 0.0362(14) 0.0056(10) 0.0092(11) 0.0050(10) C33 0.0403(14) 0.0293(13) 0.0357(14) 0.0087(11) 0.0092(11) 0.0076(11) C34 0.0424(14) 0.0243(12) 0.0425(15) 0.0065(11) 0.0063(12) 0.0038(10) C35 0.0471(15) 0.0319(13) 0.0334(14) 0.0074(11) 0.0092(12) 0.0115(11) C36 0.0549(18) 0.0412(17) 0.0446(17) 0.0052(13) 0.0013(14) 0.0095(14) C37 0.065(2) 0.061(2) 0.0488(19) 0.0008(17) -0.0108(17) 0.0184(18) C38 0.087(3) 0.064(2) 0.058(2) 0.0141(19) -0.012(2) 0.033(2) C39 0.081(3) 0.0453(19) 0.060(2) 0.0189(16) 0.0006(19) 0.0234(18) C40 0.0384(14) 0.0261(13) 0.0447(15) 0.0057(11) 0.0117(12) 0.0050(10) C41 0.0556(19) 0.0381(16) 0.0530(19) 0.0123(14) 0.0009(15) 0.0023(14) C42 0.0527(19) 0.053(2) 0.059(2) 0.0007(16) -0.0011(16) -0.0004(15) C43 0.0492(18) 0.0365(17) 0.072(2) -0.0056(16) 0.0120(17) -0.0036(13) C44 0.0520(18) 0.0270(14) 0.077(2) 0.0057(15) 0.0135(17) 0.0016(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.933(2) 1_565 ? Zn1 O1 1.946(2) . ? Zn1 N5 2.074(2) . ? Zn1 N6 2.181(3) . ? Zn1 N4 2.181(3) . ? O1 C1 1.262(5) . ? O2 C1 1.221(4) . ? O3 C23 1.283(4) . ? O3 Zn1 1.933(2) 1_545 ? O4 C23 1.210(4) . ? N1 C18 1.372(6) . ? N1 C22 1.403(7) . ? N2 C10 1.393(5) . ? N2 C12 1.393(4) . ? N3 C13 1.338(5) . ? N3 C17 1.363(6) . ? N4 C39 1.330(4) . ? N4 C35 1.341(4) . ? N5 C33 1.335(3) . ? N5 C32 1.340(4) . ? N6 C44 1.338(4) . ? N6 C40 1.354(4) . ? C1 C2 1.504(4) . ? C2 C3 1.368(5) . ? C2 C6 1.385(5) . ? C3 C4 1.386(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(4) . ? C4 H4 0.9300 . ? C5 C7 1.377(5) . ? C5 C8 1.493(4) . ? C6 C7 1.389(5) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C11 1.339(4) . ? C8 C9 1.377(4) . ? C9 C10 1.373(4) . ? C9 H9 0.9300 . ? C10 C18 1.495(5) . ? C11 C12 1.343(4) . ? C11 H11 0.9300 . ? C12 C13 1.480(5) . ? C13 C14 1.379(6) . ? C14 C15 1.359(6) . ? C14 H14 0.9300 . ? C15 C16 1.369(9) . ? C15 H15 0.9300 . ? C16 C17 1.372(9) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.330(5) . ? C19 C20 1.344(6) . ? C19 H19 0.9300 . ? C20 C21 1.368(8) . ? C20 H20 0.9300 . ? C21 C22 1.348(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.516(4) . ? C24 C25 1.386(4) . ? C24 C29 1.392(4) . ? C25 C26 1.379(4) . ? C25 H25 0.9300 . ? C26 C27 1.394(4) . ? C26 H26 0.9300 . ? C27 C28 1.389(4) . ? C27 C30 1.485(4) . ? C28 C29 1.384(4) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C34 1.382(4) . ? C30 C31 1.399(4) . ? C31 C32 1.388(4) . ? C31 H31 0.9300 . ? C32 C40 1.496(4) . ? C33 C34 1.391(4) . ? C33 C35 1.490(4) . ? C34 H34 0.9300 . ? C35 C36 1.390(4) . ? C36 C37 1.377(5) . ? C36 H36 0.9300 . ? C37 C38 1.375(6) . ? C37 H37 0.9300 . ? C38 C39 1.372(6) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.364(5) . ? C41 C42 1.391(5) . ? C41 H41 0.9300 . ? C42 C43 1.375(6) . ? C42 H42 0.9300 . ? C43 C44 1.372(6) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 95.74(12) 1_565 . ? O3 Zn1 N5 132.05(10) 1_565 . ? O1 Zn1 N5 131.94(11) . . ? O3 Zn1 N6 103.28(10) 1_565 . ? O1 Zn1 N6 101.30(12) . . ? N5 Zn1 N6 75.68(9) . . ? O3 Zn1 N4 93.82(10) 1_565 . ? O1 Zn1 N4 100.80(12) . . ? N5 Zn1 N4 74.94(9) . . ? N6 Zn1 N4 150.41(9) . . ? C1 O1 Zn1 122.4(2) . . ? C23 O3 Zn1 131.1(2) . 1_545 ? C18 N1 C22 117.6(5) . . ? C10 N2 C12 118.5(3) . . ? C13 N3 C17 117.4(5) . . ? C39 N4 C35 118.9(3) . . ? C39 N4 Zn1 124.9(2) . . ? C35 N4 Zn1 116.1(2) . . ? C33 N5 C32 119.8(2) . . ? C33 N5 Zn1 120.37(19) . . ? C32 N5 Zn1 119.78(17) . . ? C44 N6 C40 118.3(3) . . ? C44 N6 Zn1 126.3(2) . . ? C40 N6 Zn1 115.41(19) . . ? O2 C1 O1 124.4(3) . . ? O2 C1 C2 120.8(3) . . ? O1 C1 C2 114.8(3) . . ? C3 C2 C6 118.5(3) . . ? C3 C2 C1 120.3(3) . . ? C6 C2 C1 121.1(3) . . ? C2 C3 C4 121.0(3) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 120.7(3) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C7 C5 C4 118.5(3) . . ? C7 C5 C8 119.2(3) . . ? C4 C5 C8 122.3(3) . . ? C2 C6 C7 120.9(3) . . ? C2 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C5 C7 C6 120.5(3) . . ? C5 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C11 C8 C9 121.6(3) . . ? C11 C8 C5 117.5(3) . . ? C9 C8 C5 120.9(3) . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 N2 118.9(3) . . ? C9 C10 C18 120.8(3) . . ? N2 C10 C18 120.3(3) . . ? C8 C11 C12 119.5(3) . . ? C8 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 N2 121.6(3) . . ? C11 C12 C13 117.4(3) . . ? N2 C12 C13 121.0(3) . . ? N3 C13 C14 121.9(4) . . ? N3 C13 C12 116.8(4) . . ? C14 C13 C12 121.3(4) . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 117.7(6) . . ? C14 C15 H15 121.2 . . ? C16 C15 H15 121.2 . . ? C15 C16 C17 120.4(5) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? N3 C17 C16 121.8(5) . . ? N3 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 N1 121.5(4) . . ? C19 C18 C10 119.1(3) . . ? N1 C18 C10 119.4(4) . . ? C18 C19 C20 119.8(4) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C19 C20 C21 122.1(5) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C22 C21 C20 118.1(5) . . ? C22 C21 H21 121.0 . . ? C20 C21 H21 121.0 . . ? C21 C22 N1 121.0(5) . . ? C21 C22 H22 119.5 . . ? N1 C22 H22 119.5 . . ? O4 C23 O3 124.7(3) . . ? O4 C23 C24 120.8(3) . . ? O3 C23 C24 114.4(3) . . ? C25 C24 C29 118.4(3) . . ? C25 C24 C23 121.3(3) . . ? C29 C24 C23 120.3(3) . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25 119.7 . . ? C24 C25 H25 119.7 . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 118.2(3) . . ? C28 C27 C30 120.8(2) . . ? C26 C27 C30 121.0(3) . . ? C29 C28 C27 120.6(3) . . ? C29 C28 H28 119.7 . . ? C27 C28 H28 119.7 . . ? C28 C29 C24 121.0(3) . . ? C28 C29 H29 119.5 . . ? C24 C29 H29 119.5 . . ? C34 C30 C31 117.9(2) . . ? C34 C30 C27 120.9(2) . . ? C31 C30 C27 121.2(3) . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? N5 C32 C31 121.2(2) . . ? N5 C32 C40 114.3(2) . . ? C31 C32 C40 124.5(3) . . ? N5 C33 C34 121.8(3) . . ? N5 C33 C35 114.0(2) . . ? C34 C33 C35 124.2(2) . . ? C30 C34 C33 119.5(2) . . ? C30 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? N4 C35 C36 122.4(3) . . ? N4 C35 C33 114.5(2) . . ? C36 C35 C33 123.1(3) . . ? C37 C36 C35 117.6(3) . . ? C37 C36 H36 121.2 . . ? C35 C36 H36 121.2 . . ? C38 C37 C36 120.0(3) . . ? C38 C37 H37 120.0 . . ? C36 C37 H37 120.0 . . ? C39 C38 C37 119.0(3) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? N4 C39 C38 122.1(3) . . ? N4 C39 H39 119.0 . . ? C38 C39 H39 119.0 . . ? N6 C40 C41 122.0(3) . . ? N6 C40 C32 114.6(3) . . ? C41 C40 C32 123.4(3) . . ? C40 C41 C42 119.2(3) . . ? C40 C41 H41 120.4 . . ? C42 C41 H41 120.4 . . ? C43 C42 C41 119.0(3) . . ? C43 C42 H42 120.5 . . ? C41 C42 H42 120.5 . . ? C44 C43 C42 118.8(3) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? N6 C44 C43 122.7(3) . . ? N6 C44 H44 118.7 . . ? C43 C44 H44 118.7 . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.58 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.849 _refine_diff_density_min -0.558 _refine_diff_density_rms 0.077 data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 917620' #TrackingRef 'complex_3-917620.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H57.75 N12 O8.88 Zn2' _chemical_formula_weight 1555.95 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 15.120(4) _cell_length_b 15.143(4) _cell_length_c 17.514(5) _cell_angle_alpha 69.388(7) _cell_angle_beta 86.529(8) _cell_angle_gamma 79.694(9) _cell_volume 3692.7(16) _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 prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1602 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7616 _exptl_absorpt_correction_T_max 0.7867 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _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 Saturn70_(4x4_bin_mode) _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26975 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_unetI/netI 0.0420 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.00 _reflns_number_total 12537 _reflns_number_gt 10156 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Some restraints were applied and listed as follows: FLAT C82 C83 C84 C85 C86 C87 ISOR C83 C84 C86 C87 DFIX 1.40 0.002 C82 C83 C84 C85 C85 C86 DFIX 1.40 0.002 C83 C84 C86 C87 C87 C82 DELU 0.002 C82 C83 C82 C87 SIMU 0.002 C82 C83 C82 C87 DELU 0.002 C85 C84 C85 C86 SIMU 0.002 C85 C84 C85 C86 SIMU 0.002 C44 O2 C44 O3 DELU 0.002 C44 O2 C44 O3 OMIT 1 -2 1 OMIT 2 -3 1 OMIT 1 5 4 OMIT 1 1 2 OMIT 0 0 2 OMIT 1 2 1 OMIT 0 2 1 OMIT 0 -1 1 OMIT 1 -3 1 OMIT 2 4 3 OMIT 2 -4 1 OMIT 1 2 0 OMIT -2 50 EADP ZN1 O3 EADP ZN1 O4 DELU 0.002 O4 C44 SIMU 0.002 O4 C44 DELU 0.002 O7 C88 SIMU 0.002 O7 C88 DELU 0.002 O8 C88 SIMU 0.002 O8 C88 DELU 0.002 O5 C66 SIMU 0.002 O5 C66 DELU 0.002 O6 C66 SIMU 0.002 O6 C66 ; _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^)+(0.1252P)^2^+8.7768P] 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 12537 _refine_ls_number_parameters 1006 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0819 _refine_ls_wR_factor_ref 0.2335 _refine_ls_wR_factor_gt 0.2196 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.93068(4) 0.68106(4) 0.33031(3) 0.03785(19) Uani 1 1 d . . . Zn2 Zn 1.42685(4) 0.42571(4) 0.30704(4) 0.0413(2) Uani 1 1 d . . . O1 O 0.0518(3) 0.6917(3) 0.2871(2) 0.0559(10) Uani 1 1 d . . . O2 O -0.0029(3) 0.8331(4) 0.1969(3) 0.0743(14) Uani 1 1 d . . . O3 O 0.8965(2) 1.5674(2) 0.4319(2) 0.03785(19) Uani 1 1 d U . . O4 O 0.9477(2) 1.5317(2) 0.3270(2) 0.03785(19) Uani 1 1 d U . . O5 O 1.4337(5) -0.4745(4) 0.3494(5) 0.1102(18) Uani 1 1 d U . . O6 O 1.3383(5) -0.5376(5) 0.4426(5) 0.126(2) Uani 1 1 d U . . O7 O 0.4895(4) 0.5361(5) 0.1680(4) 0.1160(19) Uani 1 1 d U . . O8 O 0.5491(3) 0.4047(4) 0.2592(3) 0.0819(13) Uani 1 1 d U . . O9 O 0.0757(6) 1.0299(9) -0.0513(5) 0.103(4) Uani 0.50 1 d P . . O10 O 1.449(2) 0.308(2) 0.1223(18) 0.129(10) Uani 0.25 1 d P . . O11 O 1.446(3) -0.387(3) 0.987(2) 0.092(15) Uani 0.13 1 d P . . N1 N 0.8159(3) 0.7231(3) 0.2586(3) 0.0441(10) Uani 1 1 d . . . N2 N 0.5863(3) 0.8549(3) 0.0347(3) 0.0472(11) Uani 1 1 d . . . N3 N 0.5549(4) 1.0474(4) -0.2665(3) 0.0679(15) Uani 1 1 d . . . N4 N 0.9058(3) 0.7749(3) 0.3958(3) 0.0403(9) Uani 1 1 d . . . N5 N 0.8371(3) 0.9230(3) 0.6125(3) 0.0421(10) Uani 1 1 d . . . N6 N 0.7819(4) 0.8237(5) 0.9114(4) 0.0802(19) Uani 1 1 d . . . N7 N 1.4152(3) 0.2854(3) 0.3766(3) 0.0410(9) Uani 1 1 d . . . N8 N 1.3477(3) -0.0116(3) 0.5925(2) 0.0407(9) Uani 1 1 d . . . N9 N 1.2453(5) -0.1115(9) 0.8821(4) 0.107(3) Uani 1 1 d . . . N10 N 1.3086(3) 0.4644(3) 0.2409(3) 0.0453(10) Uani 1 1 d . . . N11 N 1.0728(3) 0.6192(4) 0.0235(3) 0.0552(12) Uani 1 1 d . . . N12 N 1.0352(4) 0.8282(5) -0.2725(3) 0.0774(18) Uani 1 1 d . . . C1 C 0.8171(4) 0.7605(5) 0.1781(4) 0.0565(15) Uani 1 1 d . . . H1 H 0.8720 0.7702 0.1524 0.068 Uiso 1 1 calc R . . C2 C 0.7406(4) 0.7859(5) 0.1299(4) 0.0588(16) Uani 1 1 d . . . H2 H 0.7453 0.8117 0.0735 0.071 Uiso 1 1 calc R . . C3 C 0.6582(3) 0.7733(4) 0.1652(3) 0.0466(12) Uani 1 1 d . . . C4 C 0.6577(4) 0.7322(6) 0.2493(4) 0.083(2) Uani 1 1 d . . . H4 H 0.6039 0.7205 0.2765 0.100 Uiso 1 1 calc R . . C5 C 0.7360(4) 0.7086(6) 0.2927(4) 0.080(2) Uani 1 1 d . . . H5 H 0.7333 0.6810 0.3492 0.096 Uiso 1 1 calc R . . C6 C 0.5757(3) 0.8014(4) 0.1128(3) 0.0443(12) Uani 1 1 d . . . C7 C 0.4937(3) 0.7753(4) 0.1446(3) 0.0466(13) Uani 1 1 d . . . H7 H 0.4893 0.7375 0.1991 0.056 Uiso 1 1 calc R . . C8 C 0.4185(3) 0.8060(4) 0.0943(3) 0.0425(11) Uani 1 1 d . . . C9 C 0.4308(3) 0.8580(4) 0.0129(3) 0.0426(12) Uani 1 1 d . . . H9 H 0.3827 0.8779 -0.0232 0.051 Uiso 1 1 calc R . . C10 C 0.5148(3) 0.8805(4) -0.0149(3) 0.0431(12) Uani 1 1 d . . . C11 C 0.5284(3) 0.9389(4) -0.1022(3) 0.0465(12) Uani 1 1 d . . . C12 C 0.5991(4) 0.9887(4) -0.1256(3) 0.0490(13) Uani 1 1 d . . . H12 H 0.6398 0.9867 -0.0871 0.059 Uiso 1 1 calc R . . C13 C 0.6087(4) 1.0416(4) -0.2072(4) 0.0572(15) Uani 1 1 d . . . H13 H 0.6563 1.0756 -0.2215 0.069 Uiso 1 1 calc R . . C14 C 0.4889(5) 0.9989(7) -0.2440(4) 0.089(3) Uani 1 1 d . . . H14 H 0.4505 1.0005 -0.2841 0.107 Uiso 1 1 calc R . . C15 C 0.4724(5) 0.9449(6) -0.1632(4) 0.079(2) Uani 1 1 d . . . H15 H 0.4235 0.9129 -0.1508 0.095 Uiso 1 1 calc R . . C16 C 0.3271(3) 0.7905(4) 0.1267(3) 0.0408(11) Uani 1 1 d . . . C17 C 0.2522(3) 0.8542(4) 0.0881(3) 0.0525(14) Uani 1 1 d . . . H17 H 0.2594 0.9042 0.0400 0.063 Uiso 1 1 calc R . . C18 C 0.1663(4) 0.8449(5) 0.1197(3) 0.0542(14) Uani 1 1 d . . . H18 H 0.1170 0.8879 0.0918 0.065 Uiso 1 1 calc R . . C19 C 0.1533(3) 0.7728(4) 0.1919(3) 0.0434(12) Uani 1 1 d . . . C20 C 0.2288(4) 0.7077(4) 0.2315(3) 0.0461(12) Uani 1 1 d . . . H20 H 0.2215 0.6579 0.2798 0.055 Uiso 1 1 calc R . . C21 C 0.3145(3) 0.7168(4) 0.1994(3) 0.0462(12) Uani 1 1 d . . . H21 H 0.3639 0.6732 0.2265 0.055 Uiso 1 1 calc R . . C22 C 0.0607(4) 0.7670(5) 0.2263(3) 0.0497(13) Uani 1 1 d . . . C23 C 0.8704(4) 0.7485(4) 0.4710(3) 0.0478(13) Uani 1 1 d . . . H23 H 0.8565 0.6871 0.4936 0.057 Uiso 1 1 calc R . . C24 C 0.8535(4) 0.8076(4) 0.5163(3) 0.0513(14) Uani 1 1 d . . . H24 H 0.8284 0.7861 0.5680 0.062 Uiso 1 1 calc R . . C25 C 0.8741(3) 0.8998(3) 0.4846(3) 0.0380(11) Uani 1 1 d . . . C26 C 0.9105(4) 0.9268(4) 0.4072(3) 0.0435(12) Uani 1 1 d . . . H26 H 0.9254 0.9876 0.3835 0.052 Uiso 1 1 calc R . . C27 C 0.9248(4) 0.8639(4) 0.3653(3) 0.0462(12) Uani 1 1 d . . . H27 H 0.9488 0.8842 0.3130 0.055 Uiso 1 1 calc R . . C28 C 0.8595(3) 0.9629(3) 0.5339(3) 0.0389(11) Uani 1 1 d . . . C29 C 0.8705(3) 1.0580(3) 0.5004(3) 0.0396(11) Uani 1 1 d . . . H29 H 0.8851 1.0837 0.4455 0.048 Uiso 1 1 calc R . . C30 C 0.8600(3) 1.1151(3) 0.5484(3) 0.0374(10) Uani 1 1 d . . . C31 C 0.8386(3) 1.0727(4) 0.6298(3) 0.0424(11) Uani 1 1 d . . . H31 H 0.8310 1.1082 0.6643 0.051 Uiso 1 1 calc R . . C32 C 0.8289(3) 0.9774(4) 0.6595(3) 0.0418(11) Uani 1 1 d . . . C33 C 0.8102(4) 0.9268(4) 0.7474(3) 0.0483(13) Uani 1 1 d . . . C34 C 0.8448(4) 0.9479(4) 0.8085(4) 0.0593(15) Uani 1 1 d . . . H34 H 0.8778 0.9975 0.7959 0.071 Uiso 1 1 calc R . . C35 C 0.8296(5) 0.8940(5) 0.8897(4) 0.075(2) Uani 1 1 d . . . H35 H 0.8542 0.9081 0.9306 0.090 Uiso 1 1 calc R . . C36 C 0.7477(5) 0.8051(5) 0.8515(5) 0.072(2) Uani 1 1 d . . . H36 H 0.7129 0.7570 0.8657 0.087 Uiso 1 1 calc R . . C37 C 0.7607(4) 0.8520(4) 0.7707(4) 0.0599(16) Uani 1 1 d . . . H37 H 0.7367 0.8345 0.7315 0.072 Uiso 1 1 calc R . . C38 C 0.8721(3) 1.2175(3) 0.5118(3) 0.0383(11) Uani 1 1 d . . . C39 C 0.9029(6) 1.2520(4) 0.4336(4) 0.076(2) Uani 1 1 d . . . H39 H 0.9152 1.2114 0.4035 0.092 Uiso 1 1 calc R . . C40 C 0.9163(6) 1.3460(4) 0.3982(4) 0.077(2) Uani 1 1 d . . . H40 H 0.9367 1.3675 0.3447 0.093 Uiso 1 1 calc R . . C41 C 0.9002(3) 1.4072(4) 0.4401(3) 0.0441(12) Uani 1 1 d . . . C42 C 0.8714(5) 1.3739(4) 0.5190(4) 0.0614(16) Uani 1 1 d . . . H42 H 0.8612 1.4144 0.5492 0.074 Uiso 1 1 calc R . . C43 C 0.8575(5) 1.2798(4) 0.5543(3) 0.0601(16) Uani 1 1 d . . . H43 H 0.8378 1.2584 0.6080 0.072 Uiso 1 1 calc R . . C44 C 0.9167(3) 1.5085(4) 0.3970(3) 0.0417(7) Uani 1 1 d U . . C45 C 1.3964(4) 0.2585(4) 0.4557(3) 0.0526(14) Uani 1 1 d . . . H45 H 1.3922 0.3033 0.4815 0.063 Uiso 1 1 calc R . . C46 C 1.3827(4) 0.1673(4) 0.5012(3) 0.0525(14) Uani 1 1 d . . . H46 H 1.3694 0.1521 0.5564 0.063 Uiso 1 1 calc R . . C47 C 1.3885(3) 0.0979(3) 0.4656(3) 0.0371(10) Uani 1 1 d . . . C48 C 1.4110(4) 0.1254(4) 0.3839(3) 0.0457(12) Uani 1 1 d . . . H48 H 1.4172 0.0816 0.3569 0.055 Uiso 1 1 calc R . . C49 C 1.4241(4) 0.2183(4) 0.3423(3) 0.0477(13) Uani 1 1 d . . . H49 H 1.4400 0.2350 0.2875 0.057 Uiso 1 1 calc R . . C50 C 1.3718(3) -0.0007(3) 0.5155(3) 0.0367(10) Uani 1 1 d . . . C51 C 1.3818(3) -0.0741(3) 0.4849(3) 0.0408(11) Uani 1 1 d . . . H51 H 1.3983 -0.0629 0.4307 0.049 Uiso 1 1 calc R . . C52 C 1.3673(3) -0.1648(3) 0.5345(3) 0.0394(11) Uani 1 1 d . . . C53 C 1.3427(4) -0.1757(4) 0.6152(3) 0.0454(12) Uani 1 1 d . . . H53 H 1.3330 -0.2350 0.6513 0.054 Uiso 1 1 calc R . . C54 C 1.3329(3) -0.0983(4) 0.6412(3) 0.0415(11) Uani 1 1 d . . . C55 C 1.3037(4) -0.1055(4) 0.7255(3) 0.0507(13) Uani 1 1 d . . . C56 C 1.3147(5) -0.1915(6) 0.7911(4) 0.074(2) Uani 1 1 d . . . H56 H 1.3423 -0.2485 0.7847 0.089 Uiso 1 1 calc R . . C57 C 1.2826(7) -0.1886(9) 0.8671(5) 0.101(3) Uani 1 1 d . . . H57 H 1.2883 -0.2464 0.9106 0.122 Uiso 1 1 calc R . . C58 C 1.2372(5) -0.0315(9) 0.8192(5) 0.098(3) Uani 1 1 d . . . H58 H 1.2111 0.0245 0.8281 0.117 Uiso 1 1 calc R . . C59 C 1.2639(4) -0.0240(6) 0.7419(4) 0.0663(17) Uani 1 1 d . . . H59 H 1.2556 0.0353 0.7003 0.080 Uiso 1 1 calc R . . C60 C 1.3770(4) -0.2468(4) 0.5043(3) 0.0469(12) Uani 1 1 d . . . C61 C 1.4074(6) -0.2380(5) 0.4265(4) 0.076(2) Uani 1 1 d . . . H61 H 1.4233 -0.1805 0.3924 0.091 Uiso 1 1 calc R . . C62 C 1.4145(6) -0.3148(6) 0.3986(5) 0.087(2) Uani 1 1 d . . . H62 H 1.4372 -0.3079 0.3466 0.105 Uiso 1 1 calc R . . C63 C 1.3892(5) -0.3991(5) 0.4450(5) 0.070(2) Uani 1 1 d . . . C64 C 1.3609(6) -0.4092(5) 0.5227(5) 0.089(3) Uani 1 1 d . . . H64 H 1.3445 -0.4667 0.5562 0.107 Uiso 1 1 calc R . . C65 C 1.3562(6) -0.3344(4) 0.5522(4) 0.077(2) Uani 1 1 d . . . H65 H 1.3384 -0.3439 0.6059 0.093 Uiso 1 1 calc R . . C66 C 1.3890(8) -0.4764(7) 0.4102(8) 0.1090(18) Uani 1 1 d U . . C67 C 1.2282(3) 0.4631(4) 0.2788(3) 0.0454(12) Uani 1 1 d . . . H67 H 1.2272 0.4398 0.3355 0.054 Uiso 1 1 calc R . . C68 C 1.1474(3) 0.4949(4) 0.2373(3) 0.0468(12) Uani 1 1 d . . . H68 H 1.0935 0.4916 0.2659 0.056 Uiso 1 1 calc R . . C69 C 1.1467(3) 0.5315(4) 0.1531(3) 0.0465(13) Uani 1 1 d . . . C70 C 1.2290(4) 0.5320(7) 0.1150(4) 0.087(3) Uani 1 1 d . . . H70 H 1.2319 0.5545 0.0583 0.105 Uiso 1 1 calc R . . C71 C 1.3072(4) 0.4994(7) 0.1602(4) 0.082(2) Uani 1 1 d . . . H71 H 1.3618 0.5021 0.1326 0.099 Uiso 1 1 calc R . . C72 C 1.0626(3) 0.5655(4) 0.1033(3) 0.0482(13) Uani 1 1 d . . . C73 C 0.9811(3) 0.5399(4) 0.1348(3) 0.0451(12) Uani 1 1 d . . . H73 H 0.9757 0.5063 0.1902 0.054 Uiso 1 1 calc R . . C74 C 0.9066(3) 0.5649(4) 0.0830(3) 0.0467(12) Uani 1 1 d . . . C75 C 0.9190(3) 0.6176(4) 0.0015(3) 0.0500(13) Uani 1 1 d . . . H75 H 0.8716 0.6344 -0.0352 0.060 Uiso 1 1 calc R . . C76 C 1.0008(4) 0.6453(4) -0.0257(3) 0.0526(14) Uani 1 1 d . . . C77 C 1.0126(4) 0.7081(5) -0.1119(3) 0.0552(15) Uani 1 1 d . . . C78 C 1.0671(5) 0.7748(7) -0.1305(4) 0.087(3) Uani 1 1 d . . . H78 H 1.0986 0.7815 -0.0894 0.105 Uiso 1 1 calc R . . C79 C 1.0758(5) 0.8329(7) -0.2108(4) 0.102(3) Uani 1 1 d . . . H79 H 1.1132 0.8784 -0.2215 0.122 Uiso 1 1 calc R . . C80 C 0.9822(4) 0.7618(5) -0.2551(4) 0.0641(17) Uani 1 1 d . . . H80 H 0.9532 0.7556 -0.2978 0.077 Uiso 1 1 calc R . . C81 C 0.9686(4) 0.7017(4) -0.1759(3) 0.0553(15) Uani 1 1 d . . . H81 H 0.9300 0.6575 -0.1662 0.066 Uiso 1 1 calc R . . C82 C 0.8193(3) 0.5393(4) 0.1102(3) 0.0726(14) Uani 1 1 d DU . . C83 C 0.8095(3) 0.4657(5) 0.1836(3) 0.0816(16) Uani 1 1 d DU . . H83 H 0.8604 0.4296 0.2138 0.098 Uiso 1 1 calc R . . C84 C 0.7247(3) 0.4451(6) 0.2127(4) 0.0909(18) Uani 1 1 d DU . . H84 H 0.7197 0.3997 0.2642 0.109 Uiso 1 1 calc R . . C85 C 0.6473(4) 0.4915(5) 0.1661(4) 0.0851(16) Uani 1 1 d DU . . C86 C 0.6566(4) 0.5719(5) 0.0973(4) 0.0897(18) Uani 1 1 d DU . . H86 H 0.6053 0.6103 0.0692 0.108 Uiso 1 1 calc R . . C87 C 0.7408(3) 0.5961(5) 0.0697(4) 0.0785(15) Uani 1 1 d DU . . H87 H 0.7447 0.6503 0.0241 0.094 Uiso 1 1 calc R . . C88 C 0.5593(5) 0.4680(6) 0.1979(5) 0.0863(14) Uani 1 1 d U . . 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 0.0337(3) 0.0320(3) 0.0452(3) -0.0100(2) 0.0028(2) -0.0069(2) Zn2 0.0324(3) 0.0328(3) 0.0550(4) -0.0094(3) -0.0028(2) -0.0074(2) O1 0.045(2) 0.062(3) 0.065(2) -0.023(2) 0.0188(18) -0.0223(18) O2 0.036(2) 0.097(4) 0.070(3) -0.009(3) 0.0086(19) -0.002(2) O3 0.0337(3) 0.0320(3) 0.0452(3) -0.0100(2) 0.0028(2) -0.0069(2) O4 0.0337(3) 0.0320(3) 0.0452(3) -0.0100(2) 0.0028(2) -0.0069(2) O5 0.120(4) 0.084(3) 0.151(5) -0.078(3) -0.052(3) 0.013(3) O6 0.141(5) 0.084(3) 0.173(5) -0.072(4) -0.037(4) 0.001(3) O7 0.063(3) 0.122(4) 0.124(4) 0.007(3) -0.005(3) -0.018(2) O8 0.046(2) 0.096(3) 0.088(3) -0.006(2) 0.0097(19) -0.0275(19) O9 0.053(5) 0.148(10) 0.046(5) 0.025(6) 0.009(4) 0.020(6) O10 0.15(3) 0.13(2) 0.13(2) -0.079(19) -0.022(19) 0.004(19) O11 0.08(3) 0.12(4) 0.044(19) 0.03(2) -0.014(17) -0.05(2) N1 0.031(2) 0.048(3) 0.049(2) -0.012(2) 0.0004(18) -0.0058(18) N2 0.032(2) 0.056(3) 0.048(2) -0.011(2) 0.0023(18) -0.0084(19) N3 0.068(3) 0.082(4) 0.050(3) -0.015(3) 0.014(3) -0.024(3) N4 0.038(2) 0.033(2) 0.050(2) -0.0151(19) 0.0000(18) -0.0074(17) N5 0.044(2) 0.034(2) 0.045(2) -0.0076(19) -0.0009(18) -0.0078(18) N6 0.078(4) 0.067(4) 0.062(4) 0.006(3) 0.020(3) 0.009(3) N7 0.037(2) 0.034(2) 0.048(2) -0.0082(19) 0.0005(18) -0.0082(17) N8 0.036(2) 0.039(2) 0.043(2) -0.0104(19) -0.0023(17) -0.0063(17) N9 0.084(5) 0.209(10) 0.059(4) -0.063(6) 0.026(4) -0.074(6) N10 0.031(2) 0.051(3) 0.049(2) -0.011(2) -0.0021(17) -0.0054(18) N11 0.037(2) 0.070(3) 0.047(3) -0.004(2) -0.0009(19) -0.012(2) N12 0.055(3) 0.105(5) 0.052(3) -0.003(3) 0.004(3) -0.013(3) C1 0.035(3) 0.075(4) 0.054(3) -0.010(3) 0.004(2) -0.021(3) C2 0.039(3) 0.083(4) 0.044(3) -0.003(3) 0.001(2) -0.022(3) C3 0.034(3) 0.056(3) 0.045(3) -0.011(2) 0.000(2) -0.009(2) C4 0.032(3) 0.140(7) 0.057(4) -0.006(4) 0.005(3) -0.023(4) C5 0.040(3) 0.129(7) 0.045(3) 0.002(4) -0.001(3) -0.018(4) C6 0.030(2) 0.047(3) 0.050(3) -0.010(2) 0.001(2) -0.004(2) C7 0.033(3) 0.050(3) 0.046(3) -0.004(2) 0.002(2) -0.008(2) C8 0.035(3) 0.042(3) 0.049(3) -0.014(2) 0.006(2) -0.009(2) C9 0.031(2) 0.056(3) 0.040(3) -0.014(2) 0.003(2) -0.011(2) C10 0.034(3) 0.051(3) 0.044(3) -0.015(2) 0.007(2) -0.013(2) C11 0.037(3) 0.055(3) 0.045(3) -0.014(2) 0.006(2) -0.012(2) C12 0.038(3) 0.051(3) 0.056(3) -0.016(3) 0.006(2) -0.011(2) C13 0.056(3) 0.048(3) 0.065(4) -0.014(3) 0.016(3) -0.018(3) C14 0.081(5) 0.143(8) 0.042(3) -0.015(4) 0.000(3) -0.052(5) C15 0.062(4) 0.136(7) 0.044(3) -0.020(4) 0.009(3) -0.057(4) C16 0.032(2) 0.048(3) 0.044(3) -0.014(2) 0.004(2) -0.015(2) C17 0.035(3) 0.063(4) 0.045(3) 0.001(3) 0.003(2) -0.012(2) C18 0.034(3) 0.070(4) 0.048(3) -0.007(3) -0.002(2) -0.010(3) C19 0.035(3) 0.056(3) 0.045(3) -0.021(2) 0.005(2) -0.017(2) C20 0.047(3) 0.040(3) 0.050(3) -0.011(2) 0.011(2) -0.017(2) C21 0.033(3) 0.043(3) 0.057(3) -0.010(2) 0.003(2) -0.008(2) C22 0.043(3) 0.069(4) 0.046(3) -0.026(3) 0.009(2) -0.023(3) C23 0.060(3) 0.034(3) 0.054(3) -0.018(2) 0.008(3) -0.019(2) C24 0.071(4) 0.038(3) 0.049(3) -0.017(2) 0.013(3) -0.021(3) C25 0.039(3) 0.028(2) 0.045(3) -0.009(2) -0.008(2) -0.0037(19) C26 0.052(3) 0.030(3) 0.046(3) -0.009(2) 0.000(2) -0.010(2) C27 0.051(3) 0.037(3) 0.048(3) -0.011(2) 0.004(2) -0.009(2) C28 0.041(3) 0.031(2) 0.044(3) -0.011(2) -0.006(2) -0.007(2) C29 0.049(3) 0.030(2) 0.038(2) -0.008(2) -0.003(2) -0.007(2) C30 0.040(3) 0.028(2) 0.043(3) -0.011(2) -0.003(2) -0.0056(19) C31 0.051(3) 0.033(3) 0.042(3) -0.012(2) 0.001(2) -0.005(2) C32 0.043(3) 0.035(3) 0.044(3) -0.010(2) 0.001(2) -0.006(2) C33 0.048(3) 0.041(3) 0.048(3) -0.009(2) 0.006(2) 0.000(2) C34 0.071(4) 0.053(3) 0.048(3) -0.015(3) 0.007(3) -0.005(3) C35 0.094(5) 0.073(5) 0.044(3) -0.014(3) 0.007(3) 0.003(4) C36 0.060(4) 0.052(4) 0.081(5) 0.001(4) 0.020(4) -0.007(3) C37 0.057(4) 0.043(3) 0.064(4) -0.003(3) 0.011(3) -0.005(3) C38 0.042(3) 0.029(2) 0.042(3) -0.011(2) -0.003(2) -0.004(2) C39 0.132(7) 0.034(3) 0.064(4) -0.021(3) 0.040(4) -0.021(4) C40 0.123(6) 0.041(3) 0.066(4) -0.017(3) 0.041(4) -0.027(4) C41 0.045(3) 0.032(3) 0.052(3) -0.010(2) -0.002(2) -0.008(2) C42 0.099(5) 0.036(3) 0.056(3) -0.021(3) -0.005(3) -0.016(3) C43 0.106(5) 0.036(3) 0.039(3) -0.007(2) 0.001(3) -0.023(3) C44 0.0381(13) 0.0352(12) 0.0482(12) -0.0106(10) -0.0004(11) -0.0048(12) C45 0.067(4) 0.037(3) 0.055(3) -0.017(3) 0.006(3) -0.012(3) C46 0.074(4) 0.037(3) 0.044(3) -0.014(2) 0.010(3) -0.010(3) C47 0.033(2) 0.031(2) 0.044(3) -0.009(2) -0.0022(19) -0.0053(19) C48 0.062(3) 0.035(3) 0.042(3) -0.013(2) 0.000(2) -0.014(2) C49 0.061(3) 0.042(3) 0.041(3) -0.012(2) 0.002(2) -0.014(2) C50 0.032(2) 0.032(2) 0.042(3) -0.009(2) -0.0040(19) -0.0057(19) C51 0.040(3) 0.038(3) 0.041(3) -0.009(2) -0.004(2) -0.006(2) C52 0.038(3) 0.033(3) 0.044(3) -0.008(2) -0.008(2) -0.008(2) C53 0.049(3) 0.034(3) 0.045(3) -0.002(2) -0.004(2) -0.012(2) C54 0.039(3) 0.041(3) 0.040(3) -0.007(2) -0.004(2) -0.009(2) C55 0.047(3) 0.062(4) 0.044(3) -0.015(3) 0.003(2) -0.017(3) C56 0.079(5) 0.094(5) 0.044(3) -0.003(3) 0.000(3) -0.042(4) C57 0.104(7) 0.153(9) 0.047(4) -0.004(5) -0.003(4) -0.082(7) C58 0.072(5) 0.168(10) 0.075(5) -0.071(6) 0.019(4) -0.024(5) C59 0.054(4) 0.095(5) 0.057(4) -0.033(4) 0.005(3) -0.018(3) C60 0.050(3) 0.034(3) 0.055(3) -0.012(2) -0.014(2) -0.006(2) C61 0.121(6) 0.060(4) 0.063(4) -0.031(3) 0.020(4) -0.045(4) C62 0.120(7) 0.083(6) 0.082(5) -0.052(5) 0.011(5) -0.029(5) C63 0.078(5) 0.041(3) 0.095(5) -0.032(4) -0.035(4) 0.008(3) C64 0.137(8) 0.032(3) 0.095(6) -0.013(4) -0.024(5) -0.019(4) C65 0.126(7) 0.038(3) 0.062(4) -0.005(3) -0.008(4) -0.021(4) C66 0.119(4) 0.080(3) 0.154(5) -0.077(4) -0.050(3) 0.011(3) C67 0.033(3) 0.050(3) 0.043(3) -0.005(2) 0.000(2) -0.008(2) C68 0.031(2) 0.054(3) 0.050(3) -0.011(2) 0.005(2) -0.009(2) C69 0.028(2) 0.054(3) 0.049(3) -0.007(2) 0.001(2) -0.010(2) C70 0.035(3) 0.154(8) 0.044(3) 0.001(4) 0.000(3) -0.019(4) C71 0.027(3) 0.150(7) 0.051(4) -0.014(4) 0.004(2) -0.010(4) C72 0.034(3) 0.055(3) 0.047(3) -0.007(2) 0.002(2) -0.008(2) C73 0.036(3) 0.047(3) 0.043(3) -0.004(2) 0.001(2) -0.007(2) C74 0.034(3) 0.049(3) 0.052(3) -0.013(2) 0.000(2) -0.005(2) C75 0.032(3) 0.058(3) 0.050(3) -0.006(3) -0.001(2) -0.006(2) C76 0.036(3) 0.061(4) 0.050(3) -0.006(3) 0.001(2) -0.007(2) C77 0.033(3) 0.070(4) 0.047(3) -0.002(3) 0.002(2) -0.004(3) C78 0.059(4) 0.136(7) 0.053(4) 0.001(4) -0.005(3) -0.049(4) C79 0.074(5) 0.149(8) 0.059(4) 0.014(5) -0.003(4) -0.063(5) C80 0.059(4) 0.075(4) 0.049(3) -0.017(3) -0.003(3) 0.004(3) C81 0.046(3) 0.056(3) 0.051(3) -0.010(3) -0.003(2) 0.010(3) C82 0.042(2) 0.090(3) 0.067(3) 0.000(2) -0.0035(19) -0.020(2) C83 0.047(2) 0.097(3) 0.074(3) 0.007(2) -0.005(2) -0.020(2) C84 0.054(3) 0.122(4) 0.070(3) 0.010(3) -0.001(2) -0.035(3) C85 0.052(2) 0.117(4) 0.067(3) 0.003(3) -0.002(2) -0.037(3) C86 0.056(3) 0.119(4) 0.071(3) 0.006(3) -0.003(2) -0.034(3) C87 0.047(2) 0.094(3) 0.071(3) 0.004(2) -0.003(2) -0.018(2) C88 0.048(2) 0.101(3) 0.091(3) -0.004(2) 0.006(2) -0.027(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 O1 1.951(4) 1_655 ? Zn1 N1 2.074(4) . ? Zn1 N4 2.093(4) . ? Zn1 O3 2.109(3) 1_545 ? Zn1 O4 2.252(3) 1_545 ? Zn1 C44 2.501(5) 1_545 ? Zn2 O5 1.923(5) 1_565 ? Zn2 O8 2.002(5) 1_655 ? Zn2 N10 2.069(4) . ? Zn2 N7 2.078(4) . ? O1 C22 1.278(7) . ? O1 Zn1 1.951(4) 1_455 ? O2 C22 1.242(7) . ? O3 C44 1.236(6) . ? O3 Zn1 2.109(3) 1_565 ? O4 C44 1.238(6) . ? O4 Zn1 2.252(3) 1_565 ? O5 C66 1.220(14) . ? O5 Zn2 1.923(5) 1_545 ? O6 C66 1.264(14) . ? O7 C88 1.322(10) . ? O8 C88 1.185(9) . ? O8 Zn2 2.002(5) 1_455 ? N1 C1 1.322(7) . ? N1 C5 1.334(7) . ? N2 C6 1.339(7) . ? N2 C10 1.342(7) . ? N3 C14 1.304(9) . ? N3 C13 1.328(8) . ? N4 C27 1.341(7) . ? N4 C23 1.342(7) . ? N5 C32 1.340(7) . ? N5 C28 1.345(6) . ? N6 C35 1.324(10) . ? N6 C36 1.331(10) . ? N7 C45 1.328(7) . ? N7 C49 1.334(7) . ? N8 C50 1.336(6) . ? N8 C54 1.340(6) . ? N9 C57 1.308(13) . ? N9 C58 1.312(13) . ? N10 C71 1.323(8) . ? N10 C67 1.349(6) . ? N11 C76 1.344(7) . ? N11 C72 1.363(7) . ? N12 C79 1.303(10) . ? N12 C80 1.336(9) . ? C1 C2 1.388(8) . ? C1 H1 0.9300 . ? C2 C3 1.371(7) . ? C2 H2 0.9300 . ? C3 C4 1.383(8) . ? C3 C6 1.500(7) . ? C4 C5 1.369(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.394(7) . ? C7 C8 1.389(7) . ? C7 H7 0.9300 . ? C8 C9 1.384(7) . ? C8 C16 1.488(7) . ? C9 C10 1.389(7) . ? C9 H9 0.9300 . ? C10 C11 1.496(7) . ? C11 C15 1.372(8) . ? C11 C12 1.376(7) . ? C12 C13 1.384(8) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.395(9) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.383(7) . ? C16 C21 1.396(7) . ? C17 C18 1.391(7) . ? C17 H17 0.9300 . ? C18 C19 1.379(8) . ? C18 H18 0.9300 . ? C19 C20 1.403(8) . ? C19 C22 1.496(7) . ? C20 C21 1.392(7) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C23 C24 1.374(8) . ? C23 H23 0.9300 . ? C24 C25 1.394(7) . ? C24 H24 0.9300 . ? C25 C26 1.380(7) . ? C25 C28 1.480(7) . ? C26 C27 1.376(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.388(7) . ? C29 C30 1.387(7) . ? C29 H29 0.9300 . ? C30 C31 1.387(7) . ? C30 C38 1.495(7) . ? C31 C32 1.384(7) . ? C31 H31 0.9300 . ? C32 C33 1.493(7) . ? C33 C34 1.375(9) . ? C33 C37 1.397(8) . ? C34 C35 1.398(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.361(9) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.369(8) . ? C38 C43 1.376(8) . ? C39 C40 1.385(8) . ? C39 H39 0.9300 . ? C40 C41 1.354(8) . ? C40 H40 0.9300 . ? C41 C42 1.366(8) . ? C41 C44 1.513(7) . ? C42 C43 1.388(8) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 Zn1 2.501(5) 1_565 ? C45 C46 1.374(8) . ? C45 H45 0.9300 . ? C46 C47 1.386(7) . ? C46 H46 0.9300 . ? C47 C48 1.382(7) . ? C47 C50 1.500(7) . ? C48 C49 1.383(7) . ? C48 H48 0.9300 . ? C49 H49 0.9300 . ? C50 C51 1.376(7) . ? C51 C52 1.391(7) . ? C51 H51 0.9300 . ? C52 C53 1.399(7) . ? C52 C60 1.493(7) . ? C53 C54 1.381(8) . ? C53 H53 0.9300 . ? C54 C55 1.487(7) . ? C55 C59 1.390(9) . ? C55 C56 1.391(9) . ? C56 C57 1.403(12) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C59 1.360(10) . ? C58 H58 0.9300 . ? C59 H59 0.9300 . ? C60 C65 1.378(8) . ? C60 C61 1.380(9) . ? C61 C62 1.397(10) . ? C61 H61 0.9300 . ? C62 C63 1.358(11) . ? C62 H62 0.9300 . ? C63 C64 1.365(11) . ? C63 C66 1.500(11) . ? C64 C65 1.390(10) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? C67 C68 1.380(7) . ? C67 H67 0.9300 . ? C68 C69 1.381(7) . ? C68 H68 0.9300 . ? C69 C70 1.376(8) . ? C69 C72 1.492(7) . ? C70 C71 1.378(8) . ? C70 H70 0.9300 . ? C71 H71 0.9300 . ? C72 C73 1.382(7) . ? C73 C74 1.402(7) . ? C73 H73 0.9300 . ? C74 C75 1.389(7) . ? C74 C82 1.447(7) . ? C75 C76 1.381(7) . ? C75 H75 0.9300 . ? C76 C77 1.494(7) . ? C77 C78 1.356(9) . ? C77 C81 1.378(9) . ? C78 C79 1.385(9) . ? C78 H78 0.9300 . ? C79 H79 0.9300 . ? C80 C81 1.393(8) . ? C80 H80 0.9300 . ? C81 H81 0.9300 . ? C82 C83 1.395(2) . ? C82 C87 1.400(2) . ? C83 C84 1.397(2) . ? C83 H83 0.9300 . ? C84 C85 1.395(2) . ? C84 H84 0.9300 . ? C85 C86 1.401(2) . ? C85 C88 1.466(8) . ? C86 C87 1.399(2) . ? C86 H86 0.9300 . ? C87 H87 0.9300 . ? 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 N1 124.07(17) 1_655 . ? O1 Zn1 N4 104.83(17) 1_655 . ? N1 Zn1 N4 101.05(17) . . ? O1 Zn1 O3 125.18(15) 1_655 1_545 ? N1 Zn1 O3 102.49(15) . 1_545 ? N4 Zn1 O3 91.38(15) . 1_545 ? O1 Zn1 O4 89.99(15) 1_655 1_545 ? N1 Zn1 O4 91.30(15) . 1_545 ? N4 Zn1 O4 150.07(14) . 1_545 ? O3 Zn1 O4 59.17(12) 1_545 1_545 ? O1 Zn1 C44 109.79(17) 1_655 1_545 ? N1 Zn1 C44 97.36(17) . 1_545 ? N4 Zn1 C44 120.84(17) . 1_545 ? O3 Zn1 C44 29.57(15) 1_545 1_545 ? O4 Zn1 C44 29.62(14) 1_545 1_545 ? O5 Zn2 O8 103.0(3) 1_565 1_655 ? O5 Zn2 N10 107.3(2) 1_565 . ? O8 Zn2 N10 123.8(2) 1_655 . ? O5 Zn2 N7 125.5(3) 1_565 . ? O8 Zn2 N7 100.07(19) 1_655 . ? N10 Zn2 N7 99.15(17) . . ? C22 O1 Zn1 116.8(4) . 1_455 ? C44 O3 Zn1 93.1(3) . 1_565 ? C44 O4 Zn1 86.4(3) . 1_565 ? C66 O5 Zn2 115.9(7) . 1_545 ? C88 O8 Zn2 112.3(5) . 1_455 ? C1 N1 C5 116.2(5) . . ? C1 N1 Zn1 123.4(3) . . ? C5 N1 Zn1 120.3(4) . . ? C6 N2 C10 117.5(4) . . ? C14 N3 C13 115.8(5) . . ? C27 N4 C23 116.6(4) . . ? C27 N4 Zn1 121.9(4) . . ? C23 N4 Zn1 121.5(3) . . ? C32 N5 C28 117.7(4) . . ? C35 N6 C36 116.9(6) . . ? C45 N7 C49 117.0(4) . . ? C45 N7 Zn2 122.4(4) . . ? C49 N7 Zn2 120.6(3) . . ? C50 N8 C54 117.6(4) . . ? C57 N9 C58 115.6(7) . . ? C71 N10 C67 116.7(4) . . ? C71 N10 Zn2 122.2(4) . . ? C67 N10 Zn2 120.8(3) . . ? C76 N11 C72 117.8(5) . . ? C79 N12 C80 116.3(6) . . ? N1 C1 C2 123.4(5) . . ? N1 C1 H1 118.3 . . ? C2 C1 H1 118.3 . . ? C3 C2 C1 120.3(5) . . ? C3 C2 H2 119.8 . . ? C1 C2 H2 119.8 . . ? C2 C3 C4 116.0(5) . . ? C2 C3 C6 120.1(5) . . ? C4 C3 C6 123.9(5) . . ? C5 C4 C3 120.3(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? N1 C5 C4 123.7(6) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? N2 C6 C7 122.9(5) . . ? N2 C6 C3 115.3(4) . . ? C7 C6 C3 121.7(5) . . ? C8 C7 C6 119.5(5) . . ? C8 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C9 C8 C7 117.2(5) . . ? C9 C8 C16 120.7(5) . . ? C7 C8 C16 122.0(5) . . ? C8 C9 C10 120.2(5) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? N2 C10 C9 122.5(5) . . ? N2 C10 C11 116.7(4) . . ? C9 C10 C11 120.7(5) . . ? C15 C11 C12 116.4(5) . . ? C15 C11 C10 122.2(5) . . ? C12 C11 C10 121.4(5) . . ? C11 C12 C13 119.1(6) . . ? C11 C12 H12 120.4 . . ? C13 C12 H12 120.4 . . ? N3 C13 C12 124.7(6) . . ? N3 C13 H13 117.7 . . ? C12 C13 H13 117.7 . . ? N3 C14 C15 123.9(7) . . ? N3 C14 H14 118.0 . . ? C15 C14 H14 118.0 . . ? C11 C15 C14 120.0(6) . . ? C11 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C21 118.1(5) . . ? C17 C16 C8 120.1(5) . . ? C21 C16 C8 121.7(4) . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C19 C18 C17 120.9(5) . . ? C19 C18 H18 119.6 . . ? C17 C18 H18 119.6 . . ? C18 C19 C20 118.2(5) . . ? C18 C19 C22 119.8(5) . . ? C20 C19 C22 122.0(5) . . ? C21 C20 C19 120.7(5) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C16 120.7(5) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? O2 C22 O1 123.0(5) . . ? O2 C22 C19 120.7(5) . . ? O1 C22 C19 116.3(5) . . ? N4 C23 C24 123.4(5) . . ? N4 C23 H23 118.3 . . ? C24 C23 H23 118.3 . . ? C23 C24 C25 119.8(5) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C26 C25 C24 116.7(5) . . ? C26 C25 C28 122.8(4) . . ? C24 C25 C28 120.4(5) . . ? C27 C26 C25 120.1(5) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? N4 C27 C26 123.3(5) . . ? N4 C27 H27 118.3 . . ? C26 C27 H27 118.3 . . ? N5 C28 C29 122.1(5) . . ? N5 C28 C25 116.7(4) . . ? C29 C28 C25 121.2(4) . . ? C30 C29 C28 120.3(5) . . ? C30 C29 H29 119.8 . . ? C28 C29 H29 119.8 . . ? C29 C30 C31 117.2(4) . . ? C29 C30 C38 120.0(4) . . ? C31 C30 C38 122.9(4) . . ? C32 C31 C30 119.7(5) . . ? C32 C31 H31 120.2 . . ? C30 C31 H31 120.2 . . ? N5 C32 C31 123.0(5) . . ? N5 C32 C33 115.0(4) . . ? C31 C32 C33 122.0(5) . . ? C34 C33 C37 117.3(5) . . ? C34 C33 C32 121.8(5) . . ? C37 C33 C32 120.8(5) . . ? C33 C34 C35 119.1(7) . . ? C33 C34 H34 120.5 . . ? C35 C34 H34 120.5 . . ? N6 C35 C34 123.3(7) . . ? N6 C35 H35 118.4 . . ? C34 C35 H35 118.4 . . ? N6 C36 C37 124.2(7) . . ? N6 C36 H36 117.9 . . ? C37 C36 H36 117.9 . . ? C36 C37 C33 119.3(7) . . ? C36 C37 H37 120.4 . . ? C33 C37 H37 120.4 . . ? C39 C38 C43 116.8(5) . . ? C39 C38 C30 119.9(5) . . ? C43 C38 C30 123.2(5) . . ? C38 C39 C40 121.5(6) . . ? C38 C39 H39 119.3 . . ? C40 C39 H39 119.3 . . ? C41 C40 C39 121.1(6) . . ? C41 C40 H40 119.4 . . ? C39 C40 H40 119.4 . . ? C40 C41 C42 118.6(5) . . ? C40 C41 C44 117.7(5) . . ? C42 C41 C44 123.7(5) . . ? C41 C42 C43 120.2(5) . . ? C41 C42 H42 119.9 . . ? C43 C42 H42 119.9 . . ? C38 C43 C42 121.7(5) . . ? C38 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? O3 C44 O4 121.3(5) . . ? O3 C44 C41 118.8(5) . . ? O4 C44 C41 119.8(5) . . ? O3 C44 Zn1 57.4(2) . 1_565 ? O4 C44 Zn1 64.0(3) . 1_565 ? C41 C44 Zn1 174.9(4) . 1_565 ? N7 C45 C46 122.8(5) . . ? N7 C45 H45 118.6 . . ? C46 C45 H45 118.6 . . ? C45 C46 C47 120.8(5) . . ? C45 C46 H46 119.6 . . ? C47 C46 H46 119.6 . . ? C48 C47 C46 116.2(5) . . ? C48 C47 C50 123.6(5) . . ? C46 C47 C50 120.2(4) . . ? C47 C48 C49 119.7(5) . . ? C47 C48 H48 120.1 . . ? C49 C48 H48 120.1 . . ? N7 C49 C48 123.5(5) . . ? N7 C49 H49 118.3 . . ? C48 C49 H49 118.3 . . ? N8 C50 C51 123.0(5) . . ? N8 C50 C47 114.2(4) . . ? C51 C50 C47 122.8(4) . . ? C50 C51 C52 120.4(5) . . ? C50 C51 H51 119.8 . . ? C52 C51 H51 119.8 . . ? C51 C52 C53 116.3(5) . . ? C51 C52 C60 122.5(5) . . ? C53 C52 C60 121.2(5) . . ? C54 C53 C52 120.0(5) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? N8 C54 C53 122.7(5) . . ? N8 C54 C55 115.3(5) . . ? C53 C54 C55 122.0(5) . . ? C59 C55 C56 116.8(6) . . ? C59 C55 C54 120.2(5) . . ? C56 C55 C54 123.0(6) . . ? C55 C56 C57 117.2(9) . . ? C55 C56 H56 121.4 . . ? C57 C56 H56 121.4 . . ? N9 C57 C56 125.5(9) . . ? N9 C57 H57 117.2 . . ? C56 C57 H57 117.2 . . ? N9 C58 C59 125.1(10) . . ? N9 C58 H58 117.5 . . ? C59 C58 H58 117.5 . . ? C58 C59 C55 119.7(8) . . ? C58 C59 H59 120.2 . . ? C55 C59 H59 120.2 . . ? C65 C60 C61 116.8(6) . . ? C65 C60 C52 122.0(6) . . ? C61 C60 C52 121.3(5) . . ? C60 C61 C62 120.6(7) . . ? C60 C61 H61 119.7 . . ? C62 C61 H61 119.7 . . ? C63 C62 C61 122.0(7) . . ? C63 C62 H62 119.0 . . ? C61 C62 H62 119.0 . . ? C62 C63 C64 117.8(6) . . ? C62 C63 C66 120.5(9) . . ? C64 C63 C66 121.6(8) . . ? C63 C64 C65 120.8(7) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C60 C65 C64 121.9(7) . . ? C60 C65 H65 119.0 . . ? C64 C65 H65 119.0 . . ? O5 C66 O6 123.1(9) . . ? O5 C66 C63 118.7(11) . . ? O6 C66 C63 118.1(11) . . ? N10 C67 C68 123.0(5) . . ? N10 C67 H67 118.5 . . ? C68 C67 H67 118.5 . . ? C67 C68 C69 119.8(5) . . ? C67 C68 H68 120.1 . . ? C69 C68 H68 120.1 . . ? C70 C69 C68 116.8(5) . . ? C70 C69 C72 119.8(5) . . ? C68 C69 C72 123.4(5) . . ? C69 C70 C71 120.4(6) . . ? C69 C70 H70 119.8 . . ? C71 C70 H70 119.8 . . ? N10 C71 C70 123.3(5) . . ? N10 C71 H71 118.4 . . ? C70 C71 H71 118.4 . . ? N11 C72 C73 122.3(5) . . ? N11 C72 C69 115.2(4) . . ? C73 C72 C69 122.3(5) . . ? C72 C73 C74 119.8(5) . . ? C72 C73 H73 120.1 . . ? C74 C73 H73 120.1 . . ? C75 C74 C73 116.9(5) . . ? C75 C74 C82 119.5(5) . . ? C73 C74 C82 123.6(5) . . ? C76 C75 C74 120.8(5) . . ? C76 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? N11 C76 C75 122.3(5) . . ? N11 C76 C77 116.7(5) . . ? C75 C76 C77 121.0(5) . . ? C78 C77 C81 117.0(6) . . ? C78 C77 C76 121.1(6) . . ? C81 C77 C76 121.9(6) . . ? C77 C78 C79 119.8(7) . . ? C77 C78 H78 120.1 . . ? C79 C78 H78 120.1 . . ? N12 C79 C78 124.4(8) . . ? N12 C79 H79 117.8 . . ? C78 C79 H79 117.8 . . ? N12 C80 C81 122.9(6) . . ? N12 C80 H80 118.6 . . ? C81 C80 H80 118.6 . . ? C77 C81 C80 119.5(6) . . ? C77 C81 H81 120.2 . . ? C80 C81 H81 120.2 . . ? C83 C82 C87 117.4(5) . . ? C83 C82 C74 121.2(4) . . ? C87 C82 C74 120.8(4) . . ? C82 C83 C84 121.3(5) . . ? C82 C83 H83 119.4 . . ? C84 C83 H83 119.4 . . ? C85 C84 C83 121.3(6) . . ? C85 C84 H84 119.4 . . ? C83 C84 H84 119.4 . . ? C84 C85 C86 116.4(6) . . ? C84 C85 C88 120.2(5) . . ? C86 C85 C88 122.3(5) . . ? C87 C86 C85 121.8(6) . . ? C87 C86 H86 119.1 . . ? C85 C86 H86 119.1 . . ? C86 C87 C82 120.5(6) . . ? C86 C87 H87 119.8 . . ? C82 C87 H87 119.8 . . ? O8 C88 O7 117.8(7) . . ? O8 C88 C85 123.9(7) . . ? O7 C88 C85 115.8(7) . . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 1.384 _refine_diff_density_min -2.598 _refine_diff_density_rms 0.093 data_complex_4 _database_code_depnum_ccdc_archive 'CCDC 917621' #TrackingRef 'complex_4-917621.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H44 N6 O19 Zn2' _chemical_formula_weight 1307.77 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5313(3) _cell_length_b 16.9991(6) _cell_length_c 13.9952(5) _cell_angle_alpha 90.00 _cell_angle_beta 92.608(3) _cell_angle_gamma 90.00 _cell_volume 2740.52(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7006 _cell_measurement_theta_min 2.1351 _cell_measurement_theta_max 27.4971 _exptl_crystal_description yellow _exptl_crystal_colour block _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.585 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1340 _exptl_absorpt_coefficient_mu 0.963 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8307 _exptl_absorpt_correction_T_max 0.8690 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _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 Saturn70_(4x4_bin_mode) _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17122 _diffrn_reflns_av_R_equivalents 0.0197 _diffrn_reflns_av_unetI/netI 0.0180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4690 _reflns_number_gt 4423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Some restraints were applied and listed as follows: OMIT 1 1 1 OMIT 0 0 4 OMIT 2 1 0 OMIT -2 2 4 OMIT 2 0 2 OMIT -2 50 ; _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^)+(0.0416P)^2^+2.0223P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4690 _refine_ls_number_parameters 427 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0332 _refine_ls_R_factor_gt 0.0310 _refine_ls_wR_factor_ref 0.0817 _refine_ls_wR_factor_gt 0.0801 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.762996(19) 0.067168(12) 0.087872(15) 0.02348(9) Uani 1 1 d . . . O1 O -0.07009(18) 0.10715(12) -0.68706(14) 0.0636(6) Uani 1 1 d . . . H1A H -0.1255 0.1330 -0.7144 0.114(15) Uiso 1 1 d R A . O3 O 0.64197(12) 0.13307(8) 0.14712(11) 0.0310(3) Uani 1 1 d . . . O4 O 0.78103(13) 0.19956(10) 0.22632(12) 0.0422(4) Uani 1 1 d . . . O5 O 0.70076(15) 0.46954(9) 0.34471(13) 0.0437(4) Uani 1 1 d . . . O6 O 0.52169(19) 0.49917(11) 0.37728(17) 0.0689(6) Uani 1 1 d . . . O7 O 0.20034(15) 0.33903(11) 0.24023(16) 0.0578(5) Uani 1 1 d . . . H7A H 0.1311 0.3271 0.2368 0.086(12) Uiso 1 1 d R . . O8 O 0.23266(16) 0.22597(12) 0.16762(18) 0.0679(6) Uani 1 1 d . . . O9 O -0.02734(18) 0.30487(14) 0.2447(2) 0.0805(7) Uani 1 1 d . . . O10 O 0.3561(5) 0.1748(3) -0.0536(5) 0.0942(18) Uani 0.50 1 d P . . N1 N 0.67466(15) 0.03170(10) -0.03662(12) 0.0271(4) Uani 1 1 d . . . N2 N 0.55025(15) -0.10469(10) -0.34070(12) 0.0271(4) Uani 1 1 d . . . N3 N 0.64634(15) -0.34326(10) -0.52851(12) 0.0275(4) Uani 1 1 d . . . C1 C 0.56843(18) 0.05833(12) -0.06295(15) 0.0272(4) Uani 1 1 d . . . H1 H 0.5319 0.0927 -0.0223 0.033 Uiso 1 1 calc R . . C2 C 0.51116(18) 0.03702(12) -0.14731(14) 0.0274(4) Uani 1 1 d . . . H2 H 0.4371 0.0564 -0.1624 0.033 Uiso 1 1 calc R . . C3 C 0.56435(17) -0.01361(11) -0.21003(14) 0.0250(4) Uani 1 1 d . . . C4 C 0.67394(19) -0.04119(13) -0.18238(15) 0.0322(5) Uani 1 1 d . . . H4 H 0.7123 -0.0757 -0.2217 0.039 Uiso 1 1 calc R . . C5 C 0.72590(19) -0.01745(13) -0.09662(15) 0.0328(5) Uani 1 1 d . . . H5 H 0.7997 -0.0363 -0.0796 0.039 Uiso 1 1 calc R . . C6 C 0.50590(18) -0.03966(12) -0.30154(14) 0.0259(4) Uani 1 1 d . . . C7 C 0.41107(18) -0.00005(12) -0.34330(14) 0.0288(4) Uani 1 1 d . . . H7 H 0.3850 0.0462 -0.3160 0.035 Uiso 1 1 calc R . . C8 C 0.35517(18) -0.02959(12) -0.42583(14) 0.0287(4) Uani 1 1 d . . . C9 C 0.39833(19) -0.09921(13) -0.46309(15) 0.0312(5) Uani 1 1 d . . . H9 H 0.3619 -0.1222 -0.5168 0.037 Uiso 1 1 calc R . . C10 C 0.49569(18) -0.13395(12) -0.41964(14) 0.0268(4) Uani 1 1 d . . . C11 C 0.54642(18) -0.20694(12) -0.45795(14) 0.0276(4) Uani 1 1 d . . . C12 C 0.48002(19) -0.26344(13) -0.50679(16) 0.0343(5) Uani 1 1 d . . . H12 H 0.4004 -0.2563 -0.5167 0.041 Uiso 1 1 calc R . . C13 C 0.53260(18) -0.33019(12) -0.54057(16) 0.0325(5) Uani 1 1 d . . . H13 H 0.4869 -0.3675 -0.5730 0.039 Uiso 1 1 calc R . . C14 C 0.71058(19) -0.28876(13) -0.48097(16) 0.0351(5) Uani 1 1 d . . . H14 H 0.7900 -0.2973 -0.4722 0.042 Uiso 1 1 calc R . . C15 C 0.66451(19) -0.22098(13) -0.44471(16) 0.0344(5) Uani 1 1 d . . . H15 H 0.7120 -0.1850 -0.4117 0.041 Uiso 1 1 calc R . . C16 C 0.25331(19) 0.01088(12) -0.47251(15) 0.0307(5) Uani 1 1 d . A . C17 C 0.1852(2) 0.06024(16) -0.42020(17) 0.0467(7) Uani 1 1 d . . . H17 H 0.2032 0.0677 -0.3554 0.056 Uiso 1 1 calc R . . C18 C 0.0910(3) 0.09853(19) -0.4625(2) 0.0584(8) Uani 1 1 d . A . H18 H 0.0463 0.1317 -0.4263 0.070 Uiso 1 1 calc R . . C19 C 0.0625(2) 0.08788(15) -0.55859(18) 0.0441(6) Uani 1 1 d . . . C20 C 0.1281(2) 0.03734(14) -0.61140(16) 0.0394(5) Uani 1 1 d . A . H20 H 0.1081 0.0287 -0.6757 0.047 Uiso 1 1 calc R . . C21 C 0.2230(2) -0.00032(14) -0.56915(16) 0.0361(5) Uani 1 1 d . . . H21 H 0.2674 -0.0336 -0.6055 0.043 Uiso 1 1 calc R A . C23 C 0.67811(18) 0.19100(11) 0.19787(14) 0.0261(4) Uani 1 1 d . . . C24 C 0.59189(17) 0.25298(11) 0.22296(13) 0.0231(4) Uani 1 1 d . . . C25 C 0.47456(17) 0.24361(11) 0.19997(14) 0.0258(4) Uani 1 1 d . . . H25 H 0.4488 0.1994 0.1661 0.031 Uiso 1 1 calc R . . C26 C 0.39494(18) 0.30019(12) 0.22733(14) 0.0277(4) Uani 1 1 d . . . C27 C 0.43403(18) 0.36791(12) 0.27484(15) 0.0289(4) Uani 1 1 d . . . H27 H 0.3809 0.4055 0.2932 0.035 Uiso 1 1 calc R . . C28 C 0.55206(18) 0.37950(11) 0.29491(14) 0.0266(4) Uani 1 1 d . . . C29 C 0.63017(18) 0.32126(11) 0.27040(14) 0.0256(4) Uani 1 1 d . . . H29 H 0.7089 0.3278 0.2858 0.031 Uiso 1 1 calc R . . C30 C 0.5922(2) 0.45494(13) 0.34308(15) 0.0333(5) Uani 1 1 d . . . C31 C 0.26904(19) 0.28394(13) 0.20810(17) 0.0366(5) Uani 1 1 d . . . O2A O -0.1127(4) 0.1628(3) -0.5504(3) 0.0571(17) Uani 0.563(10) 1 d P A 1 C22A C -0.0501(10) 0.1221(6) -0.5961(8) 0.0409(19) Uani 0.563(10) 1 d P A 1 O2B O -0.0423(8) 0.2094(4) -0.5879(5) 0.091(4) Uani 0.437(10) 1 d P A 2 C22B C -0.0189(13) 0.1437(9) -0.6133(12) 0.053(3) Uani 0.437(10) 1 d P A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.02585(15) 0.01850(14) 0.02577(14) 0.00150(8) -0.00227(9) -0.00035(8) O1 0.0647(13) 0.0623(13) 0.0604(12) -0.0135(10) -0.0326(10) 0.0258(10) O3 0.0309(8) 0.0225(7) 0.0399(8) -0.0057(6) 0.0049(6) -0.0004(6) O4 0.0302(9) 0.0436(9) 0.0514(10) -0.0093(8) -0.0145(7) 0.0093(7) O5 0.0437(10) 0.0322(9) 0.0541(10) -0.0135(7) -0.0095(8) -0.0082(7) O6 0.0705(14) 0.0402(11) 0.0980(16) -0.0385(11) 0.0259(12) -0.0077(10) O7 0.0282(10) 0.0471(11) 0.0986(16) -0.0188(10) 0.0087(9) 0.0037(8) O8 0.0356(10) 0.0499(12) 0.1160(18) -0.0320(12) -0.0213(11) 0.0022(8) O9 0.0460(12) 0.0623(14) 0.133(2) -0.0288(14) 0.0037(13) -0.0110(10) O10 0.088(3) 0.051(3) 0.140(5) -0.003(3) -0.043(3) 0.013(2) N1 0.0291(9) 0.0241(9) 0.0277(9) -0.0005(7) -0.0031(7) -0.0031(7) N2 0.0320(9) 0.0226(8) 0.0263(8) -0.0022(7) -0.0015(7) 0.0019(7) N3 0.0289(9) 0.0241(9) 0.0292(9) -0.0034(7) -0.0005(7) 0.0027(7) C1 0.0287(11) 0.0255(10) 0.0274(10) -0.0045(8) 0.0013(8) 0.0007(8) C2 0.0256(10) 0.0258(10) 0.0304(10) -0.0006(8) -0.0014(8) 0.0004(8) C3 0.0303(11) 0.0199(9) 0.0246(10) 0.0011(8) 0.0001(8) -0.0031(8) C4 0.0338(12) 0.0315(11) 0.0312(11) -0.0065(9) -0.0003(9) 0.0059(9) C5 0.0302(12) 0.0337(12) 0.0338(11) -0.0024(9) -0.0046(9) 0.0044(9) C6 0.0293(11) 0.0228(10) 0.0254(10) -0.0012(8) 0.0002(8) -0.0005(8) C7 0.0348(12) 0.0231(10) 0.0283(10) -0.0043(8) -0.0012(9) 0.0063(8) C8 0.0324(11) 0.0264(11) 0.0270(10) -0.0018(8) -0.0007(8) 0.0046(9) C9 0.0356(12) 0.0283(11) 0.0289(10) -0.0077(8) -0.0069(9) 0.0056(9) C10 0.0297(11) 0.0237(10) 0.0268(10) -0.0034(8) -0.0013(8) 0.0021(8) C11 0.0321(11) 0.0251(10) 0.0253(10) -0.0035(8) -0.0025(8) 0.0047(8) C12 0.0255(11) 0.0335(12) 0.0434(12) -0.0101(10) -0.0044(9) 0.0046(9) C13 0.0292(11) 0.0274(11) 0.0403(12) -0.0092(9) -0.0037(9) -0.0012(9) C14 0.0275(11) 0.0334(12) 0.0437(13) -0.0106(10) -0.0054(9) 0.0050(9) C15 0.0309(12) 0.0290(11) 0.0424(12) -0.0125(9) -0.0063(9) 0.0009(9) C16 0.0339(12) 0.0280(11) 0.0299(11) -0.0029(8) -0.0029(9) 0.0059(9) C17 0.0504(15) 0.0584(16) 0.0303(12) -0.0142(11) -0.0090(11) 0.0236(12) C18 0.0594(18) 0.0685(19) 0.0459(15) -0.0241(14) -0.0128(13) 0.0372(15) C19 0.0449(14) 0.0443(14) 0.0417(13) -0.0095(11) -0.0135(11) 0.0175(11) C20 0.0444(13) 0.0413(13) 0.0315(11) -0.0069(10) -0.0096(10) 0.0066(11) C21 0.0395(13) 0.0363(12) 0.0321(11) -0.0087(9) -0.0033(10) 0.0111(10) C23 0.0306(11) 0.0230(10) 0.0246(10) 0.0031(8) -0.0011(8) 0.0006(8) C24 0.0268(10) 0.0197(9) 0.0226(9) 0.0020(7) 0.0002(8) 0.0003(8) C25 0.0303(11) 0.0196(9) 0.0271(10) -0.0005(7) -0.0031(8) -0.0022(8) C26 0.0282(11) 0.0244(10) 0.0302(10) 0.0017(8) -0.0011(8) -0.0001(8) C27 0.0334(11) 0.0218(10) 0.0318(11) -0.0002(8) 0.0051(9) 0.0027(8) C28 0.0358(11) 0.0208(10) 0.0232(10) 0.0000(8) 0.0016(8) -0.0031(8) C29 0.0277(10) 0.0245(10) 0.0245(9) 0.0015(8) -0.0011(8) -0.0030(8) C30 0.0487(14) 0.0242(10) 0.0270(10) -0.0025(8) 0.0015(10) -0.0062(10) C31 0.0293(11) 0.0314(12) 0.0486(13) 0.0023(10) -0.0031(10) 0.0034(9) O2A 0.051(3) 0.058(3) 0.061(2) -0.007(2) -0.0047(19) 0.024(2) C22A 0.038(5) 0.038(5) 0.046(4) -0.003(3) -0.008(3) 0.009(3) O2B 0.120(7) 0.065(5) 0.081(5) -0.035(4) -0.059(5) 0.060(5) C22B 0.050(8) 0.052(8) 0.055(7) -0.008(5) -0.018(5) 0.018(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O5 1.9451(15) 2_645 ? Zn1 O3 1.9989(14) . ? Zn1 N3 2.0446(17) 2_654 ? Zn1 N1 2.0676(16) . ? O1 C22A 1.308(12) . ? O1 C22B 1.320(16) . ? O1 H1A 0.8527 . ? O3 C23 1.273(2) . ? O4 C23 1.243(3) . ? O5 C30 1.275(3) . ? O5 Zn1 1.9451(15) 2_655 ? O6 C30 1.221(3) . ? O7 C31 1.319(3) . ? O7 H7A 0.8234 . ? O8 C31 1.203(3) . ? N1 C1 1.342(3) . ? N1 C5 1.341(3) . ? N2 C10 1.342(3) . ? N2 C6 1.345(3) . ? N3 C13 1.333(3) . ? N3 C14 1.343(3) . ? N3 Zn1 2.0446(17) 2_644 ? C1 C2 1.375(3) . ? C1 H1 0.9300 . ? C2 C3 1.392(3) . ? C2 H2 0.9300 . ? C3 C4 1.386(3) . ? C3 C6 1.487(3) . ? C4 C5 1.377(3) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.390(3) . ? C7 C8 1.391(3) . ? C7 H7 0.9300 . ? C8 C9 1.394(3) . ? C8 C16 1.487(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9300 . ? C10 C11 1.482(3) . ? C11 C15 1.387(3) . ? C11 C12 1.389(3) . ? C12 C13 1.380(3) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 C15 1.376(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.382(3) . ? C16 C21 1.395(3) . ? C17 C18 1.377(3) . ? C17 H17 0.9300 . ? C18 C19 1.381(4) . ? C18 H18 0.9300 . ? C19 C20 1.381(3) . ? C19 C22A 1.496(12) . ? C19 C22B 1.517(16) . ? C20 C21 1.378(3) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C23 C24 1.501(3) . ? C24 C25 1.386(3) . ? C24 C29 1.399(3) . ? C25 C26 1.395(3) . ? C25 H25 0.9300 . ? C26 C27 1.394(3) . ? C26 C31 1.490(3) . ? C27 C28 1.391(3) . ? C27 H27 0.9300 . ? C28 C29 1.392(3) . ? C28 C30 1.512(3) . ? C29 H29 0.9300 . ? O2A C22A 1.205(13) . ? O2B C22B 1.206(17) . ? 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 O3 114.56(7) 2_645 . ? O5 Zn1 N3 136.88(7) 2_645 2_654 ? O3 Zn1 N3 97.52(6) . 2_654 ? O5 Zn1 N1 104.28(7) 2_645 . ? O3 Zn1 N1 100.75(6) . . ? N3 Zn1 N1 96.67(7) 2_654 . ? C22A O1 C22B 25.2(6) . . ? C22A O1 H1A 115.6 . . ? C22B O1 H1A 114.1 . . ? C23 O3 Zn1 116.61(13) . . ? C30 O5 Zn1 111.33(14) . 2_655 ? C31 O7 H7A 113.7 . . ? C1 N1 C5 117.46(17) . . ? C1 N1 Zn1 122.80(14) . . ? C5 N1 Zn1 119.68(14) . . ? C10 N2 C6 117.86(17) . . ? C13 N3 C14 117.69(18) . . ? C13 N3 Zn1 126.22(14) . 2_644 ? C14 N3 Zn1 115.73(14) . 2_644 ? N1 C1 C2 122.94(19) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C1 C2 C3 119.76(19) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C4 C3 C2 117.09(18) . . ? C4 C3 C6 120.76(18) . . ? C2 C3 C6 122.13(18) . . ? C5 C4 C3 119.94(19) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? N1 C5 C4 122.80(19) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? N2 C6 C7 122.22(18) . . ? N2 C6 C3 115.44(17) . . ? C7 C6 C3 122.33(18) . . ? C6 C7 C8 120.01(19) . . ? C6 C7 H7 120.0 . . ? C8 C7 H7 120.0 . . ? C7 C8 C9 117.22(18) . . ? C7 C8 C16 121.67(18) . . ? C9 C8 C16 121.12(18) . . ? C10 C9 C8 119.59(18) . . ? C10 C9 H9 120.2 . . ? C8 C9 H9 120.2 . . ? N2 C10 C9 122.96(18) . . ? N2 C10 C11 115.47(17) . . ? C9 C10 C11 121.57(18) . . ? C15 C11 C12 117.56(19) . . ? C15 C11 C10 119.81(18) . . ? C12 C11 C10 122.63(19) . . ? C13 C12 C11 119.8(2) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? N3 C13 C12 122.59(19) . . ? N3 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? N3 C14 C15 123.2(2) . . ? N3 C14 H14 118.4 . . ? C15 C14 H14 118.4 . . ? C14 C15 C11 119.23(19) . . ? C14 C15 H15 120.4 . . ? C11 C15 H15 120.4 . . ? C17 C16 C21 118.2(2) . . ? C17 C16 C8 120.34(19) . . ? C21 C16 C8 121.41(19) . . ? C18 C17 C16 121.0(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C18 C19 C20 119.4(2) . . ? C18 C19 C22A 117.1(5) . . ? C20 C19 C22A 122.8(5) . . ? C18 C19 C22B 121.6(7) . . ? C20 C19 C22B 117.4(7) . . ? C22A C19 C22B 21.9(5) . . ? C21 C20 C19 120.2(2) . . ? C21 C20 H20 119.9 . . ? C19 C20 H20 119.9 . . ? C20 C21 C16 120.8(2) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? O4 C23 O3 123.56(19) . . ? O4 C23 C24 118.41(18) . . ? O3 C23 C24 118.03(17) . . ? C25 C24 C29 119.30(18) . . ? C25 C24 C23 121.00(17) . . ? C29 C24 C23 119.69(17) . . ? C24 C25 C26 120.32(18) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C27 C26 C25 119.85(19) . . ? C27 C26 C31 122.03(19) . . ? C25 C26 C31 118.06(18) . . ? C28 C27 C26 120.36(19) . . ? C28 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C27 C28 C29 119.19(18) . . ? C27 C28 C30 119.15(19) . . ? C29 C28 C30 121.66(19) . . ? C28 C29 C24 120.89(18) . . ? C28 C29 H29 119.6 . . ? C24 C29 H29 119.6 . . ? O6 C30 O5 122.9(2) . . ? O6 C30 C28 120.1(2) . . ? O5 C30 C28 117.0(2) . . ? O8 C31 O7 122.7(2) . . ? O8 C31 C26 123.6(2) . . ? O7 C31 C26 113.71(19) . . ? O2A C22A O1 123.0(10) . . ? O2A C22A C19 124.6(9) . . ? O1 C22A C19 112.2(9) . . ? O2B C22B O1 124.6(13) . . ? O2B C22B C19 124.8(12) . . ? O1 C22B C19 110.2(11) . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.397 _refine_diff_density_min -0.297 _refine_diff_density_rms 0.047 data_complex_5 _database_code_depnum_ccdc_archive 'CCDC 917622' #TrackingRef 'complex_5-917622.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26.50 H16.75 N3.25 O4 Zn' _chemical_formula_weight 510.05 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 monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.242(19) _cell_length_b 7.320(7) _cell_length_c 21.883(17) _cell_angle_alpha 90.00 _cell_angle_beta 122.10(3) _cell_angle_gamma 90.00 _cell_volume 2340(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4711 _cell_measurement_theta_min 2.1976 _cell_measurement_theta_max 27.6649 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.448 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1042 _exptl_absorpt_coefficient_mu 1.089 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7359 _exptl_absorpt_correction_T_max 0.7725 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _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 Mercury70_(2x2_bin_mode) _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21011 _diffrn_reflns_av_R_equivalents 0.0578 _diffrn_reflns_av_unetI/netI 0.0586 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 27.60 _reflns_number_total 5410 _reflns_number_gt 3803 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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. Some restraints were applied and listed as follows: DFIX 1.10 N4 C28 DFIX 1.45 C27 C28 OMIT -2 1 5 OMIT 1 0 2 OMIT -1 1 1 OMIT 0 1 1 ISOR 0.002 O3 O4 ISOR 0.002 C23 C24 DELU 0.002 C23 C24 DELU 0.002 O3 C23 DELU 0.002 O4 C23 DELU 0.002 O3 ZN1 SIMU 0.002 O3 ZN1 DELU 0.002 N4 C28 SIMU 0.002 N4 C28 DELU 0.002 C27 C28 SIMU 0.002 C27 C28 ; _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^)+(0.1123P)^2^+3.8822P] 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 5410 _refine_ls_number_parameters 326 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0786 _refine_ls_wR_factor_ref 0.2284 _refine_ls_wR_factor_gt 0.2040 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.091 _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 0.46869(3) 0.60518(9) 0.19846(3) 0.0425(2) Uani 1 1 d U . . O1 O 0.5802(2) 0.5932(6) 0.29625(19) 0.0547(10) Uani 1 1 d . . . N1 N 1.0411(4) 0.7720(9) 0.9436(3) 0.0734(16) Uani 1 1 d . . . C1 C 0.5903(3) 0.7214(7) 0.3370(2) 0.0406(11) Uani 1 1 d . . . O2 O 0.5290(2) 0.8393(5) 0.3207(2) 0.0518(9) Uani 1 1 d . . . N2 N 1.0964(3) 0.8128(7) 0.7405(2) 0.0468(10) Uani 1 1 d . . . C2 C 0.6779(3) 0.7326(7) 0.4083(2) 0.0403(11) Uani 1 1 d . . . O3 O 0.5065(4) 0.7534(8) 0.1466(3) 0.0869(13) Uani 1 1 d U . . N3 N 1.3485(3) 0.8734(6) 0.6938(2) 0.0411(10) Uani 1 1 d . . . C3 C 0.6814(3) 0.8177(8) 0.4660(3) 0.0474(12) Uani 1 1 d . . . H3 H 0.6285 0.8670 0.4609 0.057 Uiso 1 1 calc R . . O4 O 0.3691(4) 0.7331(9) 0.0543(3) 0.1024(17) Uani 1 1 d U . . C4 C 0.7627(3) 0.8293(9) 0.5307(3) 0.0485(13) Uani 1 1 d . . . H4 H 0.7644 0.8853 0.5695 0.058 Uiso 1 1 calc R . . C5 C 0.8423(3) 0.7596(8) 0.5396(2) 0.0430(12) Uani 1 1 d . . . C6 C 0.8382(3) 0.6777(9) 0.4804(3) 0.0536(15) Uani 1 1 d . . . H6 H 0.8914 0.6336 0.4847 0.064 Uiso 1 1 calc R . . C7 C 0.7563(3) 0.6616(9) 0.4161(3) 0.0502(13) Uani 1 1 d . . . H7 H 0.7539 0.6024 0.3776 0.060 Uiso 1 1 calc R . . C8 C 0.9307(3) 0.7777(8) 0.6091(2) 0.0453(12) Uani 1 1 d . . . C9 C 0.9348(3) 0.7720(8) 0.6737(3) 0.0476(13) Uani 1 1 d . . . H9 H 0.8815 0.7557 0.6739 0.057 Uiso 1 1 calc R . . C10 C 1.0179(3) 0.7903(8) 0.7384(2) 0.0450(12) Uani 1 1 d . . . C11 C 1.0929(3) 0.8166(8) 0.6782(2) 0.0437(12) Uani 1 1 d . . . C12 C 1.0115(3) 0.8020(9) 0.6117(3) 0.0463(13) Uani 1 1 d . . . H12 H 1.0116 0.8086 0.5693 0.056 Uiso 1 1 calc R . . C13 C 1.0247(4) 0.7853(9) 0.8087(3) 0.0501(14) Uani 1 1 d . . . C14 C 0.9500(4) 0.8014(11) 0.8150(3) 0.0673(19) Uani 1 1 d . . . H14 H 0.8920 0.8172 0.7741 0.081 Uiso 1 1 calc R . . C15 C 0.9615(5) 0.7941(13) 0.8821(3) 0.080(2) Uani 1 1 d . . . H15 H 0.9095 0.8055 0.8846 0.096 Uiso 1 1 calc R . . C16 C 1.1124(5) 0.7589(11) 0.9369(3) 0.075(2) Uani 1 1 d . . . H16 H 1.1699 0.7454 0.9787 0.090 Uiso 1 1 calc R . . C17 C 1.1068(4) 0.7641(10) 0.8717(3) 0.0640(17) Uani 1 1 d . . . H17 H 1.1599 0.7531 0.8707 0.077 Uiso 1 1 calc R . . C18 C 1.1807(3) 0.8397(8) 0.6822(3) 0.0434(12) Uani 1 1 d . . . C19 C 1.2581(4) 0.9089(14) 0.7437(3) 0.098(3) Uani 1 1 d . . . H19 H 1.2548 0.9482 0.7826 0.117 Uiso 1 1 calc R . . C20 C 1.3388(4) 0.9187(14) 0.7462(4) 0.094(3) Uani 1 1 d . . . H20 H 1.3902 0.9608 0.7886 0.113 Uiso 1 1 calc R . . C21 C 1.2754(4) 0.8134(12) 0.6351(3) 0.073(2) Uani 1 1 d . . . H21 H 1.2807 0.7799 0.5965 0.088 Uiso 1 1 calc R . . C22 C 1.1919(4) 0.7972(12) 0.6274(3) 0.071(2) Uani 1 1 d . . . H22 H 1.1421 0.7564 0.5839 0.086 Uiso 1 1 calc R . . C23 C 0.4459(6) 0.7866(11) 0.0845(4) 0.0791(15) Uani 1 1 d U . . C24 C 0.4773(5) 0.8980(9) 0.0417(4) 0.0662(16) Uani 1 1 d U . . C25 C 0.5658(5) 0.9234(11) 0.0630(4) 0.078(2) Uani 1 1 d . . . H25 H 0.6120 0.8728 0.1062 0.093 Uiso 1 1 calc R . . C26 C 0.4113(5) 0.9745(10) -0.0205(4) 0.081(2) Uani 1 1 d . . . H26 H 0.3502 0.9596 -0.0354 0.097 Uiso 1 1 calc R . . N4 N 0.7329(5) 0.8920(10) 0.6991(4) 0.076(5) Uani 0.25 1 d PRDU . . C28 C 0.6782(5) 0.9807(10) 0.6630(4) 0.067(4) Uani 0.25 1 d PRDU . . C27 C 0.6040(5) 1.0925(10) 0.6088(4) 0.066(5) Uani 0.25 1 d PRDU . . H27A H 0.6277 1.2086 0.6059 0.099 Uiso 0.25 1 calc PR . . H27B H 0.5595 1.1107 0.6219 0.099 Uiso 0.25 1 calc PR . . H27C H 0.5758 1.0322 0.5629 0.099 Uiso 0.25 1 calc PR . . 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 0.0273(3) 0.0546(4) 0.0306(3) 0.0021(3) 0.0054(2) -0.0023(2) O1 0.039(2) 0.066(3) 0.0341(18) -0.0053(18) 0.0026(16) 0.0023(17) N1 0.080(4) 0.096(5) 0.037(3) -0.006(3) 0.026(3) 0.000(3) C1 0.031(2) 0.049(3) 0.028(2) 0.010(2) 0.0056(19) -0.002(2) O2 0.0284(17) 0.052(2) 0.050(2) 0.0078(18) 0.0040(15) 0.0026(15) N2 0.030(2) 0.068(3) 0.0294(19) -0.001(2) 0.0068(16) 0.006(2) C2 0.026(2) 0.051(3) 0.027(2) 0.006(2) 0.0036(18) 0.002(2) O3 0.099(2) 0.085(2) 0.0799(18) 0.0128(15) 0.0498(15) -0.0092(16) N3 0.0304(19) 0.051(3) 0.0299(19) -0.0011(18) 0.0080(16) 0.0018(17) C3 0.028(2) 0.065(4) 0.040(3) 0.000(3) 0.012(2) 0.006(2) O4 0.100(2) 0.105(2) 0.105(2) 0.0040(18) 0.0563(17) -0.0112(17) C4 0.036(3) 0.071(4) 0.034(2) -0.006(2) 0.016(2) 0.003(2) C5 0.030(2) 0.066(3) 0.025(2) 0.002(2) 0.0085(19) 0.006(2) C6 0.029(2) 0.086(4) 0.032(2) -0.003(3) 0.007(2) 0.014(3) C7 0.037(3) 0.074(4) 0.029(2) -0.008(2) 0.010(2) 0.004(3) C8 0.032(2) 0.068(4) 0.026(2) -0.002(2) 0.0091(19) 0.004(2) C9 0.031(2) 0.074(4) 0.030(2) -0.001(2) 0.011(2) 0.007(2) C10 0.038(3) 0.057(3) 0.027(2) -0.001(2) 0.009(2) 0.011(2) C11 0.030(2) 0.065(3) 0.026(2) -0.005(2) 0.0076(18) 0.000(2) C12 0.031(2) 0.073(4) 0.026(2) -0.002(2) 0.0095(19) 0.000(2) C13 0.045(3) 0.067(4) 0.028(2) -0.003(2) 0.012(2) 0.007(3) C14 0.050(3) 0.113(6) 0.038(3) -0.007(3) 0.022(3) 0.003(4) C15 0.072(5) 0.123(7) 0.050(4) -0.013(4) 0.036(4) -0.002(4) C16 0.071(4) 0.104(6) 0.031(3) -0.002(3) 0.015(3) 0.016(4) C17 0.055(3) 0.093(5) 0.034(3) -0.001(3) 0.017(3) 0.016(3) C18 0.031(2) 0.058(3) 0.032(2) -0.003(2) 0.0096(19) -0.002(2) C19 0.033(3) 0.206(10) 0.044(3) -0.054(5) 0.013(3) -0.018(4) C20 0.032(3) 0.184(9) 0.052(4) -0.058(5) 0.012(3) -0.018(4) C21 0.037(3) 0.141(7) 0.036(3) -0.014(4) 0.016(2) -0.022(4) C22 0.036(3) 0.139(7) 0.030(3) -0.026(3) 0.011(2) -0.027(3) C23 0.086(2) 0.077(2) 0.077(2) 0.0007(17) 0.0449(15) 0.0012(17) C24 0.070(2) 0.065(2) 0.062(2) -0.0039(16) 0.0344(18) -0.0003(17) C25 0.075(5) 0.080(5) 0.056(4) 0.016(3) 0.019(4) 0.002(4) C26 0.070(5) 0.088(5) 0.093(5) -0.001(5) 0.049(4) -0.010(4) N4 0.033(7) 0.048(8) 0.106(12) -0.015(8) 0.010(7) -0.008(5) C28 0.030(6) 0.047(8) 0.101(12) -0.010(8) 0.020(7) -0.010(5) C27 0.033(7) 0.047(8) 0.099(12) -0.006(8) 0.023(7) -0.010(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 1.918(5) . ? Zn1 O1 1.977(4) . ? Zn1 O2 1.996(4) 2_645 ? Zn1 N3 2.025(5) 4_475 ? O1 C1 1.242(6) . ? N1 C16 1.316(9) . ? N1 C15 1.326(8) . ? C1 O2 1.260(6) . ? C1 C2 1.488(6) . ? O2 Zn1 1.996(4) 2_655 ? N2 C11 1.333(6) . ? N2 C10 1.340(7) . ? C2 C7 1.372(7) . ? C2 C3 1.380(7) . ? O3 C23 1.220(9) . ? N3 C20 1.288(8) . ? N3 C21 1.307(7) . ? N3 Zn1 2.025(5) 4_676 ? C3 C4 1.367(7) . ? C3 H3 0.9300 . ? O4 C23 1.189(9) . ? C4 C5 1.377(7) . ? C4 H4 0.9300 . ? C5 C6 1.394(7) . ? C5 C8 1.480(6) . ? C6 C7 1.369(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.377(7) . ? C8 C9 1.376(7) . ? C9 C10 1.385(7) . ? C9 H9 0.9300 . ? C10 C13 1.481(7) . ? C11 C12 1.388(6) . ? C11 C18 1.478(7) . ? C12 H12 0.9300 . ? C13 C17 1.361(7) . ? C13 C14 1.371(8) . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.380(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C22 1.349(7) . ? C18 C19 1.392(7) . ? C19 C20 1.366(9) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.362(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.542(11) . ? C24 C26 1.347(10) . ? C24 C25 1.351(10) . ? C25 C26 1.403(10) 3_675 ? C25 H25 0.9300 . ? C26 C25 1.403(10) 3_675 ? C26 H26 0.9300 . ? N4 C28 1.0693 . ? C28 C27 1.4482 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O1 103.0(2) . . ? O3 Zn1 O2 112.1(2) . 2_645 ? O1 Zn1 O2 93.90(16) . 2_645 ? O3 Zn1 N3 125.9(2) . 4_475 ? O1 Zn1 N3 115.99(18) . 4_475 ? O2 Zn1 N3 101.48(16) 2_645 4_475 ? C1 O1 Zn1 115.4(3) . . ? C16 N1 C15 114.9(5) . . ? O1 C1 O2 122.5(4) . . ? O1 C1 C2 118.1(4) . . ? O2 C1 C2 119.4(5) . . ? C1 O2 Zn1 128.3(3) . 2_655 ? C11 N2 C10 118.1(4) . . ? C7 C2 C3 119.7(4) . . ? C7 C2 C1 119.6(5) . . ? C3 C2 C1 120.7(4) . . ? C23 O3 Zn1 114.4(6) . . ? C20 N3 C21 116.5(5) . . ? C20 N3 Zn1 123.3(4) . 4_676 ? C21 N3 Zn1 120.2(4) . 4_676 ? C4 C3 C2 119.9(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.3(5) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C4 C5 C6 118.2(4) . . ? C4 C5 C8 121.1(4) . . ? C6 C5 C8 120.7(4) . . ? C7 C6 C5 120.5(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C2 120.3(5) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? C12 C8 C9 117.6(4) . . ? C12 C8 C5 121.3(4) . . ? C9 C8 C5 121.1(5) . . ? C8 C9 C10 120.5(5) . . ? C8 C9 H9 119.8 . . ? C10 C9 H9 119.8 . . ? N2 C10 C9 121.6(5) . . ? N2 C10 C13 116.5(4) . . ? C9 C10 C13 121.8(5) . . ? N2 C11 C12 122.8(5) . . ? N2 C11 C18 116.9(4) . . ? C12 C11 C18 120.3(4) . . ? C8 C12 C11 119.3(5) . . ? C8 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C17 C13 C14 115.8(5) . . ? C17 C13 C10 121.4(5) . . ? C14 C13 C10 122.8(5) . . ? C13 C14 C15 119.6(6) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? N1 C15 C14 124.9(7) . . ? N1 C15 H15 117.6 . . ? C14 C15 H15 117.6 . . ? N1 C16 C17 123.8(6) . . ? N1 C16 H16 118.1 . . ? C17 C16 H16 118.1 . . ? C13 C17 C16 120.9(6) . . ? C13 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C22 C18 C19 115.2(5) . . ? C22 C18 C11 123.1(4) . . ? C19 C18 C11 121.7(5) . . ? C20 C19 C18 119.5(6) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N3 C20 C19 124.2(5) . . ? N3 C20 H20 117.9 . . ? C19 C20 H20 117.9 . . ? N3 C21 C22 123.7(5) . . ? N3 C21 H21 118.1 . . ? C22 C21 H21 118.1 . . ? C18 C22 C21 120.7(5) . . ? C18 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? O4 C23 O3 126.6(8) . . ? O4 C23 C24 118.9(8) . . ? O3 C23 C24 114.4(7) . . ? C26 C24 C25 119.0(7) . . ? C26 C24 C23 117.0(7) . . ? C25 C24 C23 124.1(7) . . ? C24 C25 C26 120.6(6) . 3_675 ? C24 C25 H25 119.7 . . ? C26 C25 H25 119.7 3_675 . ? C24 C26 C25 120.5(6) . 3_675 ? C24 C26 H26 119.8 . . ? C25 C26 H26 119.8 3_675 . ? N4 C28 C27 174.8 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.60 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.188 _refine_diff_density_min -0.661 _refine_diff_density_rms 0.110 data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 917623' #TrackingRef 'complex_1-917623.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C88 H58 Cl4 N12 O9 Zn4' _chemical_formula_weight 1830.74 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M p21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 17.8687(18) _cell_length_b 18.2000(14) _cell_length_c 12.7837(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.390(7) _cell_angle_gamma 90.00 _cell_volume 4139.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8912 _cell_measurement_theta_min 2.5144 _cell_measurement_theta_max 27.5438 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.469 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1860 _exptl_absorpt_coefficient_mu 1.340 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5539 _exptl_absorpt_correction_T_max 0.7754 _exptl_absorpt_process_details 'Sphere (Rigaku CrystalClear)' _exptl_special_details ; RIGAKU/MSC(2004), CrystalClear Version 1.3.6, Rigaku/MSC, 9009 New Trails Drive, The Woodlands, TX77381-5209, USA ; _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 Mercury70_(2x2_bin_mode) _diffrn_measurement_method CCD_Profile_fitting _diffrn_detector_area_resol_mean 14.6306 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25754 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_unetI/netI 0.0310 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.51 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7179 _reflns_number_gt 6123 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _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^)+(0.0919P)^2^+8.7616P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0016(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7179 _refine_ls_number_parameters 542 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0603 _refine_ls_wR_factor_ref 0.1757 _refine_ls_wR_factor_gt 0.1658 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _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 0.44195(3) 0.62243(3) 0.70739(4) 0.0432(2) Uani 1 1 d . . . Zn2 Zn 0.06279(3) 1.06703(3) 1.25932(4) 0.0449(2) Uani 1 1 d . . . Cl1 Cl 0.56258(8) 0.63236(10) 0.77200(12) 0.0713(4) Uani 1 1 d . . . Cl2 Cl -0.05437(8) 1.02970(10) 1.29328(11) 0.0685(4) Uani 1 1 d . . . O1 O 0.3689(2) 0.69665(19) 0.7390(3) 0.0590(9) Uani 1 1 d . . . O2 O 0.3791(3) 0.7936(2) 0.6355(3) 0.0664(11) Uani 1 1 d . . . O3 O 0.0878(3) 0.1532(2) 0.3595(4) 0.0805(13) Uani 1 1 d . . . O4 O 0.1829(3) 0.1347(2) 0.2685(3) 0.0769(13) Uani 1 1 d . . . O5 O 0.0315(15) 0.1428(8) 0.6119(17) 0.101(7) Uani 0.25 1 d P . . O6 O -0.1195(16) 1.2127(15) 1.290(2) 0.135(10) Uani 0.25 1 d P . . N1 N 0.4051(2) 0.5555(2) 0.8397(3) 0.0488(10) Uani 1 1 d . . . N2 N 0.3936(2) 0.52811(19) 0.6390(3) 0.0384(8) Uani 1 1 d . . . N3 N 0.4581(2) 0.6325(2) 0.5415(3) 0.0440(9) Uani 1 1 d . . . N4 N 0.1258(2) 0.9836(2) 1.3514(3) 0.0474(10) Uani 1 1 d . . . N5 N 0.1160(2) 1.0049(2) 1.1500(3) 0.0383(8) Uani 1 1 d . . . N6 N 0.0296(2) 1.1180(2) 1.1065(4) 0.0503(10) Uani 1 1 d . . . C1 C 0.3579(3) 0.7636(3) 0.7127(4) 0.0430(10) Uani 1 1 d . . . C2 C 0.3143(2) 0.8059(2) 0.7883(3) 0.0387(10) Uani 1 1 d . . . C3 C 0.3092(3) 0.7811(2) 0.8890(3) 0.0412(10) Uani 1 1 d . . . H3 H 0.3320 0.7369 0.9104 0.049 Uiso 1 1 calc R . . C4 C 0.2708(3) 0.8209(2) 0.9590(3) 0.0416(10) Uani 1 1 d . . . H4 H 0.2685 0.8031 1.0268 0.050 Uiso 1 1 calc R . . C5 C 0.2356(3) 0.8865(2) 0.9305(3) 0.0394(10) Uani 1 1 d . . . C6 C 0.2416(3) 0.9125(3) 0.8283(4) 0.0486(12) Uani 1 1 d . . . H6 H 0.2189 0.9567 0.8069 0.058 Uiso 1 1 calc R . . C7 C 0.2808(3) 0.8732(3) 0.7595(4) 0.0488(12) Uani 1 1 d . . . H7 H 0.2851 0.8917 0.6925 0.059 Uiso 1 1 calc R . . C8 C 0.1949(3) 0.9288(2) 1.0066(3) 0.0372(10) Uani 1 1 d . . . C9 C 0.2052(3) 0.9142(2) 1.1142(3) 0.0384(10) Uani 1 1 d . . . H9 H 0.2393 0.8783 1.1394 0.046 Uiso 1 1 calc R . . C10 C 0.1652(2) 0.9527(2) 1.1835(3) 0.0363(9) Uani 1 1 d . . . C11 C 0.1069(3) 1.0221(2) 1.0478(3) 0.0382(10) Uani 1 1 d . . . C12 C 0.1440(3) 0.9837(2) 0.9741(3) 0.0410(10) Uani 1 1 d . . . H12 H 0.1347 0.9948 0.9031 0.049 Uiso 1 1 calc R . . C13 C 0.1696(3) 0.9396(2) 1.2988(3) 0.0410(10) Uani 1 1 d . . . C14 C 0.2151(3) 0.8868(3) 1.3492(4) 0.0571(14) Uani 1 1 d . . . H14 H 0.2459 0.8574 1.3119 0.069 Uiso 1 1 calc R . . C15 C 0.2140(4) 0.8785(3) 1.4570(4) 0.0677(17) Uani 1 1 d . . . H15 H 0.2448 0.8440 1.4932 0.081 Uiso 1 1 calc R . . C16 C 0.1670(4) 0.9216(4) 1.5098(4) 0.0688(17) Uani 1 1 d . . . H16 H 0.1641 0.9155 1.5815 0.083 Uiso 1 1 calc R . . C17 C 0.1244(3) 0.9741(3) 1.4545(4) 0.0612(15) Uani 1 1 d . . . H17 H 0.0935 1.0041 1.4905 0.073 Uiso 1 1 calc R . . C18 C 0.0544(3) 1.0843(2) 1.0226(4) 0.0431(11) Uani 1 1 d . . . C19 C 0.0335(3) 1.1079(3) 0.9216(4) 0.0542(13) Uani 1 1 d . . . H19 H 0.0508 1.0840 0.8643 0.065 Uiso 1 1 calc R . . C20 C -0.0142(4) 1.1684(3) 0.9075(5) 0.0693(16) Uani 1 1 d . . . H20 H -0.0289 1.1856 0.8402 0.083 Uiso 1 1 calc R . . C21 C -0.0391(4) 1.2024(3) 0.9931(5) 0.0705(17) Uani 1 1 d . . . H21 H -0.0711 1.2427 0.9850 0.085 Uiso 1 1 calc R . . C22 C -0.0160(3) 1.1757(3) 1.0906(5) 0.0639(15) Uani 1 1 d . . . H22 H -0.0329 1.1989 1.1488 0.077 Uiso 1 1 calc R . . C23 C 0.1524(4) 0.1691(3) 0.3353(5) 0.0624(15) Uani 1 1 d . . . C24 C 0.1937(3) 0.2313(3) 0.3920(4) 0.0551(13) Uani 1 1 d . . . C25 C 0.2552(4) 0.2608(3) 0.3500(5) 0.079(2) Uani 1 1 d . . . H25 H 0.2704 0.2413 0.2881 0.094 Uiso 1 1 calc R . . C26 C 0.2950(4) 0.3189(3) 0.3977(5) 0.0735(18) Uani 1 1 d . . . H26 H 0.3353 0.3389 0.3666 0.088 Uiso 1 1 calc R . . C27 C 0.2751(3) 0.3470(3) 0.4911(4) 0.0472(11) Uani 1 1 d . . . C28 C 0.2149(3) 0.3157(3) 0.5358(5) 0.0614(14) Uani 1 1 d . . . H28 H 0.2019 0.3328 0.6002 0.074 Uiso 1 1 calc R . . C29 C 0.1741(3) 0.2593(3) 0.4859(5) 0.0662(16) Uani 1 1 d . . . H29 H 0.1329 0.2399 0.5159 0.079 Uiso 1 1 calc R . . C30 C 0.3180(3) 0.4096(2) 0.5426(4) 0.0441(11) Uani 1 1 d . . . C31 C 0.3561(3) 0.4596(2) 0.4848(4) 0.0435(11) Uani 1 1 d . . . H31 H 0.3564 0.4537 0.4126 0.052 Uiso 1 1 calc R . . C32 C 0.3934(3) 0.5181(2) 0.5347(3) 0.0378(10) Uani 1 1 d . . . C33 C 0.3588(3) 0.4792(2) 0.6962(3) 0.0402(10) Uani 1 1 d . . . C34 C 0.3199(3) 0.4204(2) 0.6507(4) 0.0441(11) Uani 1 1 d . . . H34 H 0.2951 0.3880 0.6918 0.053 Uiso 1 1 calc R . . C35 C 0.3676(3) 0.4942(3) 0.8120(4) 0.0446(11) Uani 1 1 d . . . C36 C 0.3401(4) 0.4478(3) 0.8855(4) 0.0642(15) Uani 1 1 d . . . H36 H 0.3127 0.4060 0.8643 0.077 Uiso 1 1 calc R . . C37 C 0.3542(4) 0.4648(4) 0.9906(5) 0.081(2) Uani 1 1 d . . . H37 H 0.3381 0.4339 1.0418 0.098 Uiso 1 1 calc R . . C38 C 0.3926(4) 0.5285(4) 1.0184(5) 0.0775(19) Uani 1 1 d . . . H38 H 0.4024 0.5415 1.0887 0.093 Uiso 1 1 calc R . . C39 C 0.4161(4) 0.5724(3) 0.9414(4) 0.0646(15) Uani 1 1 d . . . H39 H 0.4408 0.6159 0.9607 0.078 Uiso 1 1 calc R . . C40 C 0.4348(3) 0.5753(2) 0.4810(4) 0.0388(10) Uani 1 1 d . . . C41 C 0.4499(3) 0.5708(3) 0.3761(4) 0.0454(11) Uani 1 1 d . . . H41 H 0.4344 0.5303 0.3353 0.054 Uiso 1 1 calc R . . C42 C 0.4882(3) 0.6274(3) 0.3344(4) 0.0516(12) Uani 1 1 d . . . H42 H 0.4984 0.6258 0.2644 0.062 Uiso 1 1 calc R . . C43 C 0.5115(3) 0.6864(3) 0.3962(5) 0.0590(14) Uani 1 1 d . . . H43 H 0.5379 0.7249 0.3692 0.071 Uiso 1 1 calc R . . C44 C 0.4946(3) 0.6872(3) 0.4991(4) 0.0538(12) Uani 1 1 d . . . H44 H 0.5094 0.7275 0.5407 0.065 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0481(4) 0.0389(3) 0.0434(3) -0.0116(2) 0.0077(2) 0.0004(2) Zn2 0.0462(4) 0.0459(3) 0.0427(3) -0.0160(2) 0.0046(2) 0.0051(2) Cl1 0.0546(8) 0.1021(12) 0.0563(8) -0.0034(7) 0.0011(6) -0.0099(8) Cl2 0.0478(8) 0.1091(12) 0.0500(7) -0.0121(7) 0.0121(6) 0.0025(7) O1 0.075(3) 0.0432(19) 0.063(2) -0.0081(16) 0.0297(19) 0.0102(17) O2 0.098(3) 0.062(2) 0.044(2) -0.0005(17) 0.031(2) 0.014(2) O3 0.071(3) 0.062(3) 0.106(4) -0.026(2) -0.006(3) -0.002(2) O4 0.102(4) 0.066(3) 0.063(3) -0.022(2) 0.010(2) -0.025(2) O5 0.17(2) 0.029(7) 0.114(16) 0.015(9) 0.065(15) -0.011(10) O6 0.13(2) 0.13(2) 0.14(2) -0.076(17) 0.000(17) -0.040(16) N1 0.056(3) 0.052(2) 0.038(2) -0.0077(17) 0.0061(18) -0.0006(19) N2 0.045(2) 0.0352(18) 0.0352(19) -0.0058(15) 0.0052(16) 0.0067(16) N3 0.051(2) 0.036(2) 0.046(2) -0.0036(16) 0.0086(18) 0.0033(17) N4 0.049(2) 0.054(2) 0.041(2) -0.0061(17) 0.0085(17) 0.0112(19) N5 0.042(2) 0.0400(19) 0.0333(19) -0.0089(15) 0.0029(15) -0.0018(16) N6 0.050(2) 0.044(2) 0.058(3) -0.0113(18) 0.006(2) 0.0067(18) C1 0.042(3) 0.048(3) 0.040(2) -0.011(2) 0.007(2) 0.001(2) C2 0.038(2) 0.043(2) 0.035(2) -0.0122(18) 0.0017(18) 0.0016(19) C3 0.051(3) 0.031(2) 0.041(2) -0.0026(18) 0.008(2) 0.0032(19) C4 0.055(3) 0.034(2) 0.036(2) -0.0026(17) 0.011(2) 0.004(2) C5 0.040(2) 0.046(2) 0.032(2) -0.0099(18) 0.0021(18) -0.0011(19) C6 0.057(3) 0.051(3) 0.038(2) -0.003(2) 0.003(2) 0.021(2) C7 0.062(3) 0.057(3) 0.028(2) 0.0001(19) 0.005(2) 0.011(2) C8 0.043(2) 0.032(2) 0.037(2) -0.0102(16) 0.0058(19) -0.0003(18) C9 0.045(3) 0.036(2) 0.035(2) -0.0058(17) 0.0046(19) 0.0026(19) C10 0.039(2) 0.035(2) 0.035(2) -0.0070(17) 0.0030(18) -0.0023(18) C11 0.040(2) 0.037(2) 0.038(2) -0.0087(17) 0.0031(18) -0.0021(18) C12 0.048(3) 0.042(2) 0.033(2) -0.0058(18) 0.0052(19) 0.003(2) C13 0.045(3) 0.045(2) 0.034(2) -0.0075(18) 0.0081(19) -0.001(2) C14 0.071(4) 0.064(3) 0.038(3) -0.001(2) 0.014(2) 0.021(3) C15 0.079(4) 0.082(4) 0.044(3) 0.007(3) 0.015(3) 0.036(3) C16 0.087(4) 0.087(4) 0.034(3) 0.000(3) 0.014(3) 0.027(3) C17 0.066(4) 0.084(4) 0.035(3) -0.006(2) 0.015(2) 0.029(3) C18 0.042(3) 0.040(2) 0.047(3) -0.0075(19) 0.000(2) 0.0007(19) C19 0.058(3) 0.051(3) 0.053(3) -0.004(2) 0.000(2) 0.010(2) C20 0.076(4) 0.061(3) 0.068(4) 0.009(3) -0.011(3) 0.018(3) C21 0.067(4) 0.057(3) 0.086(4) -0.007(3) 0.002(3) 0.020(3) C22 0.062(4) 0.056(3) 0.073(4) -0.016(3) 0.007(3) 0.018(3) C23 0.072(4) 0.046(3) 0.068(4) -0.002(3) -0.003(3) 0.001(3) C24 0.060(3) 0.042(3) 0.061(3) -0.008(2) -0.006(3) -0.003(2) C25 0.116(6) 0.066(4) 0.057(3) -0.024(3) 0.022(4) -0.029(4) C26 0.095(5) 0.065(4) 0.063(4) -0.019(3) 0.022(3) -0.029(3) C27 0.052(3) 0.039(2) 0.050(3) -0.008(2) 0.000(2) 0.003(2) C28 0.058(3) 0.059(3) 0.068(4) -0.025(3) 0.010(3) -0.002(3) C29 0.062(4) 0.051(3) 0.087(4) -0.018(3) 0.016(3) -0.006(3) C30 0.048(3) 0.036(2) 0.048(3) -0.0067(19) 0.003(2) 0.004(2) C31 0.056(3) 0.038(2) 0.036(2) -0.0062(18) 0.001(2) 0.009(2) C32 0.043(2) 0.036(2) 0.034(2) -0.0043(17) 0.0049(18) 0.0082(18) C33 0.046(3) 0.039(2) 0.036(2) -0.0040(18) 0.0033(19) 0.0074(19) C34 0.052(3) 0.036(2) 0.044(3) -0.0026(19) 0.007(2) -0.001(2) C35 0.050(3) 0.048(3) 0.036(2) -0.0011(19) 0.004(2) 0.004(2) C36 0.082(4) 0.065(3) 0.046(3) 0.002(2) 0.006(3) -0.013(3) C37 0.100(5) 0.101(5) 0.044(3) 0.015(3) 0.010(3) -0.019(4) C38 0.094(5) 0.098(5) 0.038(3) -0.009(3) -0.001(3) -0.008(4) C39 0.075(4) 0.076(4) 0.043(3) -0.015(3) 0.006(3) -0.010(3) C40 0.040(2) 0.036(2) 0.041(2) -0.0005(17) 0.0052(19) 0.0067(18) C41 0.047(3) 0.046(3) 0.043(3) 0.0008(19) 0.002(2) 0.011(2) C42 0.053(3) 0.060(3) 0.043(3) 0.008(2) 0.008(2) 0.013(2) C43 0.054(3) 0.056(3) 0.068(4) 0.016(3) 0.013(3) 0.005(3) C44 0.056(3) 0.049(3) 0.057(3) 0.003(2) 0.008(2) -0.002(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 O1 1.947(3) . ? Zn1 N2 2.077(4) . ? Zn1 N3 2.174(4) . ? Zn1 N1 2.233(4) . ? Zn1 Cl1 2.2420(15) . ? Zn2 O3 2.047(4) 1_566 ? Zn2 N5 2.094(4) . ? Zn2 N4 2.170(4) . ? Zn2 N6 2.194(5) . ? Zn2 Cl2 2.2810(16) . ? Zn2 O4 2.468(5) 1_566 ? Zn2 C23 2.583(6) 1_566 ? O1 C1 1.273(6) . ? O2 C1 1.219(6) . ? O3 C23 1.257(8) . ? O3 Zn2 2.047(4) 1_544 ? O4 C23 1.227(7) . ? O4 Zn2 2.468(5) 1_544 ? N1 C35 1.332(6) . ? N1 C39 1.332(7) . ? N2 C33 1.341(6) . ? N2 C32 1.344(5) . ? N3 C44 1.333(6) . ? N3 C40 1.341(6) . ? N4 C17 1.332(6) . ? N4 C13 1.344(6) . ? N5 C10 1.337(6) . ? N5 C11 1.339(6) . ? N6 C22 1.331(7) . ? N6 C18 1.347(6) . ? C1 C2 1.509(6) . ? C2 C3 1.376(6) . ? C2 C7 1.397(6) . ? C3 C4 1.382(6) . ? C3 H3 0.9300 . ? C4 C5 1.383(6) . ? C4 H4 0.9300 . ? C5 C6 1.403(7) . ? C5 C8 1.484(6) . ? C6 C7 1.377(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C12 1.388(6) . ? C8 C9 1.396(6) . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 C13 1.489(6) . ? C11 C12 1.390(6) . ? C11 C18 1.485(6) . ? C12 H12 0.9300 . ? C13 C14 1.378(7) . ? C14 C15 1.388(7) . ? C14 H14 0.9300 . ? C15 C16 1.371(8) . ? C15 H15 0.9300 . ? C16 C17 1.374(8) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.378(7) . ? C19 C20 1.393(8) . ? C19 H19 0.9300 . ? C20 C21 1.367(9) . ? C20 H20 0.9300 . ? C21 C22 1.366(9) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.499(7) . ? C23 Zn2 2.583(6) 1_544 ? C24 C25 1.377(9) . ? C24 C29 1.380(8) . ? C25 C26 1.382(8) . ? C25 H25 0.9300 . ? C26 C27 1.376(8) . ? C26 H26 0.9300 . ? C27 C28 1.387(8) . ? C27 C30 1.491(6) . ? C28 C29 1.380(8) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 C31 1.390(7) . ? C30 C34 1.393(7) . ? C31 C32 1.380(6) . ? C31 H31 0.9300 . ? C32 C40 1.483(6) . ? C33 C34 1.376(6) . ? C33 C35 1.499(6) . ? C34 H34 0.9300 . ? C35 C36 1.388(7) . ? C36 C37 1.379(8) . ? C36 H36 0.9300 . ? C37 C38 1.376(10) . ? C37 H37 0.9300 . ? C38 C39 1.363(9) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C41 1.395(7) . ? C41 C42 1.371(7) . ? C41 H41 0.9300 . ? C42 C43 1.375(8) . ? C42 H42 0.9300 . ? C43 C44 1.376(8) . ? C43 H43 0.9300 . ? C44 H44 0.9300 . ? 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 N2 113.60(16) . . ? O1 Zn1 N3 107.23(15) . . ? N2 Zn1 N3 75.35(14) . . ? O1 Zn1 N1 88.29(16) . . ? N2 Zn1 N1 74.21(14) . . ? N3 Zn1 N1 149.35(14) . . ? O1 Zn1 Cl1 120.53(13) . . ? N2 Zn1 Cl1 124.67(11) . . ? N3 Zn1 Cl1 98.14(12) . . ? N1 Zn1 Cl1 96.12(12) . . ? O3 Zn2 N5 138.15(18) 1_566 . ? O3 Zn2 N4 97.19(17) 1_566 . ? N5 Zn2 N4 74.89(14) . . ? O3 Zn2 N6 104.93(18) 1_566 . ? N5 Zn2 N6 74.68(14) . . ? N4 Zn2 N6 149.56(15) . . ? O3 Zn2 Cl2 105.03(16) 1_566 . ? N5 Zn2 Cl2 116.66(11) . . ? N4 Zn2 Cl2 97.30(13) . . ? N6 Zn2 Cl2 96.86(12) . . ? O3 Zn2 O4 56.65(18) 1_566 1_566 ? N5 Zn2 O4 81.59(15) . 1_566 ? N4 Zn2 O4 85.35(17) . 1_566 ? N6 Zn2 O4 89.56(16) . 1_566 ? Cl2 Zn2 O4 161.66(11) . 1_566 ? O3 Zn2 C23 28.64(19) 1_566 1_566 ? N5 Zn2 C23 109.58(19) . 1_566 ? N4 Zn2 C23 91.60(17) . 1_566 ? N6 Zn2 C23 97.84(17) . 1_566 ? Cl2 Zn2 C23 133.66(16) . 1_566 ? O4 Zn2 C23 28.01(17) 1_566 1_566 ? C1 O1 Zn1 134.3(3) . . ? C23 O3 Zn2 100.1(4) . 1_544 ? C23 O4 Zn2 81.2(4) . 1_544 ? C35 N1 C39 118.4(5) . . ? C35 N1 Zn1 115.6(3) . . ? C39 N1 Zn1 125.9(4) . . ? C33 N2 C32 119.5(4) . . ? C33 N2 Zn1 121.0(3) . . ? C32 N2 Zn1 119.5(3) . . ? C44 N3 C40 118.8(4) . . ? C44 N3 Zn1 125.1(3) . . ? C40 N3 Zn1 115.8(3) . . ? C17 N4 C13 118.9(4) . . ? C17 N4 Zn2 124.8(3) . . ? C13 N4 Zn2 116.3(3) . . ? C10 N5 C11 119.7(4) . . ? C10 N5 Zn2 119.7(3) . . ? C11 N5 Zn2 120.2(3) . . ? C22 N6 C18 118.7(5) . . ? C22 N6 Zn2 125.4(4) . . ? C18 N6 Zn2 115.8(3) . . ? O2 C1 O1 126.2(4) . . ? O2 C1 C2 120.5(4) . . ? O1 C1 C2 113.3(4) . . ? C3 C2 C7 118.0(4) . . ? C3 C2 C1 121.0(4) . . ? C7 C2 C1 120.9(4) . . ? C2 C3 C4 121.0(4) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 121.5(4) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C4 C5 C6 117.7(4) . . ? C4 C5 C8 120.9(4) . . ? C6 C5 C8 121.3(4) . . ? C7 C6 C5 120.5(4) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.8 . . ? C6 C7 C2 121.3(4) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C12 C8 C9 117.0(4) . . ? C12 C8 C5 121.7(4) . . ? C9 C8 C5 121.3(4) . . ? C10 C9 C8 120.5(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? N5 C10 C9 121.3(4) . . ? N5 C10 C13 113.8(4) . . ? C9 C10 C13 124.8(4) . . ? N5 C11 C12 121.4(4) . . ? N5 C11 C18 114.0(4) . . ? C12 C11 C18 124.6(4) . . ? C8 C12 C11 120.0(4) . . ? C8 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? N4 C13 C14 121.8(4) . . ? N4 C13 C10 114.8(4) . . ? C14 C13 C10 123.4(4) . . ? C13 C14 C15 118.5(5) . . ? C13 C14 H14 120.8 . . ? C15 C14 H14 120.8 . . ? C16 C15 C14 119.6(5) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 118.6(5) . . ? C15 C16 H16 120.7 . . ? C17 C16 H16 120.7 . . ? N4 C17 C16 122.6(5) . . ? N4 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? N6 C18 C19 121.5(4) . . ? N6 C18 C11 115.0(4) . . ? C19 C18 C11 123.4(4) . . ? C18 C19 C20 118.4(5) . . ? C18 C19 H19 120.8 . . ? C20 C19 H19 120.8 . . ? C21 C20 C19 119.7(6) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C22 C21 C20 118.4(5) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N6 C22 C21 123.3(5) . . ? N6 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? O4 C23 O3 122.1(6) . . ? O4 C23 C24 119.4(6) . . ? O3 C23 C24 118.5(6) . . ? O4 C23 Zn2 70.8(3) . 1_544 ? O3 C23 Zn2 51.3(3) . 1_544 ? C24 C23 Zn2 169.8(5) . 1_544 ? C25 C24 C29 118.2(5) . . ? C25 C24 C23 118.8(5) . . ? C29 C24 C23 123.0(6) . . ? C24 C25 C26 121.5(6) . . ? C24 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 120.2(6) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 118.5(5) . . ? C26 C27 C30 120.2(5) . . ? C28 C27 C30 121.2(5) . . ? C29 C28 C27 120.8(5) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C24 C29 C28 120.7(6) . . ? C24 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C31 C30 C34 117.8(4) . . ? C31 C30 C27 121.5(4) . . ? C34 C30 C27 120.6(4) . . ? C32 C31 C30 119.9(4) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? N2 C32 C31 121.3(4) . . ? N2 C32 C40 114.2(4) . . ? C31 C32 C40 124.6(4) . . ? N2 C33 C34 121.9(4) . . ? N2 C33 C35 114.0(4) . . ? C34 C33 C35 124.1(4) . . ? C33 C34 C30 119.6(4) . . ? C33 C34 H34 120.2 . . ? C30 C34 H34 120.2 . . ? N1 C35 C36 122.1(5) . . ? N1 C35 C33 114.7(4) . . ? C36 C35 C33 123.2(5) . . ? C37 C36 C35 118.6(6) . . ? C37 C36 H36 120.7 . . ? C35 C36 H36 120.7 . . ? C38 C37 C36 118.8(6) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.6 . . ? C39 C38 C37 119.1(5) . . ? C39 C38 H38 120.5 . . ? C37 C38 H38 120.5 . . ? N1 C39 C38 122.9(6) . . ? N1 C39 H39 118.6 . . ? C38 C39 H39 118.6 . . ? N3 C40 C41 121.5(4) . . ? N3 C40 C32 114.7(4) . . ? C41 C40 C32 123.7(4) . . ? C42 C41 C40 118.6(5) . . ? C42 C41 H41 120.7 . . ? C40 C41 H41 120.7 . . ? C41 C42 C43 119.9(5) . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C42 C43 C44 118.4(5) . . ? C42 C43 H43 120.8 . . ? C44 C43 H43 120.8 . . ? N3 C44 C43 122.7(5) . . ? N3 C44 H44 118.6 . . ? C43 C44 H44 118.6 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.951 _refine_diff_density_min -0.670 _refine_diff_density_rms 0.090