# Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A # This journal is © The Royal Society of Chemistry 2013 # Electronic Supplementary Material (ESI) for Journal of Materials Chemistry A # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 Cd N2 O10, C3 H7 N O, 2(C2 H8 N), 3(H2 O) ' _chemical_formula_sum 'C31 H41 Cd N5 O14 ' _chemical_formula_weight 820.10 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' Cd Cd -0.8075 1.2024 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.217(2) _cell_length_b 10.362(2) _cell_length_c 18.118(4) _cell_angle_alpha 102.53(3) _cell_angle_beta 99.35(3) _cell_angle_gamma 93.79(3) _cell_volume 1837.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.482 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.666 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.847 _exptl_absorpt_correction_T_max 0.869 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SCX-MINI _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 19200 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.1027 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.49 _reflns_number_total 8444 _reflns_number_gt 6547 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _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^)+(0.0606P)^2^+1.5547P] 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 8444 _refine_ls_number_parameters 443 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0963 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1599 _refine_ls_wR_factor_gt 0.1494 _refine_ls_goodness_of_fit_ref 1.098 _refine_ls_restrained_S_all 1.098 _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 C1 C 0.2159(5) -0.0124(5) -0.2488(3) 0.0257(10) Uani 1 1 d . . . C2 C 0.3602(5) 0.0184(4) -0.2108(3) 0.0244(10) Uani 1 1 d . . . C3 C 0.4616(5) -0.0046(5) -0.2538(3) 0.0292(11) Uani 1 1 d . . . H3A H 0.4401 -0.0390 -0.3067 0.035 Uiso 1 1 calc R . . C4 C 0.5945(5) 0.0239(5) -0.2179(3) 0.0284(11) Uani 1 1 d . . . C5 C 0.7043(5) -0.0064(5) -0.2642(3) 0.0372(13) Uani 1 1 d . . . C6 C 0.6250(5) 0.0776(5) -0.1395(3) 0.0313(11) Uani 1 1 d . . . H6 H 0.7139 0.0977 -0.1154 0.038 Uiso 1 1 calc R . . C7 C 0.5252(5) 0.1019(5) -0.0962(3) 0.0266(10) Uani 1 1 d . . . C8 C 0.3934(5) 0.0700(5) -0.1317(3) 0.0288(11) Uani 1 1 d . . . H8 H 0.3263 0.0830 -0.1026 0.035 Uiso 1 1 calc R . . C9 C 0.4921(5) 0.2331(5) 0.0281(3) 0.0371(13) Uani 1 1 d . . . C10 C 0.5428(5) 0.2679(5) 0.1133(3) 0.0321(12) Uani 1 1 d . . . C11 C 0.6781(5) 0.2849(5) 0.1452(3) 0.0358(12) Uani 1 1 d . . . H11 H 0.7416 0.2715 0.1137 0.043 Uiso 1 1 calc R . . C12 C 0.7170(6) 0.3221(5) 0.2245(3) 0.0386(13) Uani 1 1 d . . . H12 H 0.8074 0.3339 0.2458 0.046 Uiso 1 1 calc R . . C13 C 0.6244(6) 0.3420(5) 0.2723(3) 0.0335(12) Uani 1 1 d . . . C14 C 0.6657(6) 0.3920(6) 0.3573(3) 0.0429(14) Uani 1 1 d . . . C15 C 0.4894(6) 0.3230(5) 0.2399(3) 0.0390(13) Uani 1 1 d . . . H15 H 0.4263 0.3349 0.2718 0.047 Uiso 1 1 calc R . . C16 C 0.4479(5) 0.2867(5) 0.1614(3) 0.0375(13) Uani 1 1 d . . . H16 H 0.3574 0.2748 0.1403 0.045 Uiso 1 1 calc R . . C17 C 0.8132(5) 0.3638(5) 0.4726(3) 0.0299(11) Uani 1 1 d . . . C18 C 0.8358(5) 0.4956(5) 0.5135(3) 0.0329(12) Uani 1 1 d . . . H18 H 0.8162 0.5635 0.4886 0.039 Uiso 1 1 calc R . . C19 C 0.8883(5) 0.5255(5) 0.5922(3) 0.0296(11) Uani 1 1 d . . . C20 C 0.9115(5) 0.6708(5) 0.6352(3) 0.0328(11) Uani 1 1 d . . . C21 C 0.9201(5) 0.4238(5) 0.6279(3) 0.0326(12) Uani 1 1 d . . . H21 H 0.9561 0.4439 0.6801 0.039 Uiso 1 1 calc R . . C22 C 0.8994(5) 0.2918(5) 0.5871(3) 0.0327(12) Uani 1 1 d . . . C23 C 0.9306(5) 0.1802(5) 0.6269(3) 0.0342(12) Uani 1 1 d . . . C24 C 0.8454(5) 0.2629(5) 0.5087(3) 0.0312(11) Uani 1 1 d . . . H24 H 0.8311 0.1751 0.4807 0.037 Uiso 1 1 calc R . . C27 C 0.1517(7) 0.3647(8) 0.8619(5) 0.074(2) Uani 1 1 d . . . H27A H 0.1402 0.4484 0.8941 0.111 Uiso 1 1 calc R . . H27B H 0.1437 0.3729 0.8097 0.111 Uiso 1 1 calc R . . H27C H 0.2384 0.3397 0.8787 0.111 Uiso 1 1 calc R . . C28 C 0.0423(8) 0.2540(8) 0.9462(4) 0.076(2) Uani 1 1 d . . . H28A H 0.1281 0.2387 0.9714 0.114 Uiso 1 1 calc R . . H28B H -0.0223 0.1818 0.9452 0.114 Uiso 1 1 calc R . . H28C H 0.0166 0.3356 0.9737 0.114 Uiso 1 1 calc R . . C29 C 0.7015(12) 0.4108(10) 0.8658(8) 0.110(4) Uani 1 1 d . . . H29 H 0.6725 0.4323 0.9126 0.132 Uiso 1 1 calc R . . C31 C 0.6547(13) 0.3453(12) 0.7308(8) 0.147(5) Uani 1 1 d . . . H31A H 0.6370 0.4145 0.7040 0.221 Uiso 1 1 calc R . . H31B H 0.6064 0.2630 0.7010 0.221 Uiso 1 1 calc R . . H31C H 0.7485 0.3362 0.7385 0.221 Uiso 1 1 calc R . . Cd1 Cd -0.04815(3) -0.04702(3) -0.315817(19) 0.02546(13) Uani 1 1 d . . . N1 N 0.5619(4) 0.1527(4) -0.0151(2) 0.0354(10) Uani 1 1 d . . . H1A H 0.6343 0.1299 0.0078 0.042 Uiso 1 1 calc R . . N2 N 0.7591(5) 0.3309(4) 0.3924(2) 0.0379(11) Uani 1 1 d . . . H2A H 0.7895 0.2660 0.3642 0.046 Uiso 1 1 calc R . . N4 N 0.0493(5) 0.2631(5) 0.8670(3) 0.0552(14) Uani 1 1 d . . . H4A H 0.0657 0.1836 0.8404 0.066 Uiso 1 1 calc R . . H4B H -0.0306 0.2809 0.8446 0.066 Uiso 1 1 calc R . . N5 N 0.6130(7) 0.3789(6) 0.8042(5) 0.076(2) Uani 1 1 d . . . O1 O 0.1281(3) 0.0182(4) -0.2086(2) 0.0359(8) Uani 1 1 d . . . O2 O 0.1869(3) -0.0648(3) -0.31945(19) 0.0331(8) Uani 1 1 d . . . O3 O 0.6744(4) -0.0388(5) -0.3353(2) 0.0631(13) Uani 1 1 d . . . O4 O 0.8215(4) 0.0032(4) -0.2277(2) 0.0484(10) Uani 1 1 d . . . O5 O 0.3908(4) 0.2776(5) 0.0014(2) 0.0617(13) Uani 1 1 d . . . O6 O 0.6106(5) 0.4840(5) 0.3916(2) 0.0731(15) Uani 1 1 d . . . O7 O 0.9043(4) 0.0632(3) 0.5871(2) 0.0446(10) Uani 1 1 d . . . O8 O 0.9780(5) 0.2071(4) 0.6957(2) 0.0583(12) Uani 1 1 d . . . O9 O 0.8919(4) 0.7572(3) 0.5963(2) 0.0380(9) Uani 1 1 d . . . O10 O 0.9524(4) 0.7011(4) 0.7058(2) 0.0494(10) Uani 1 1 d . . . O11 O 0.8253(6) 0.4148(7) 0.8668(5) 0.123(3) Uani 1 1 d . . . O1W O 0.9661(6) 0.6428(4) 0.84800(16) 0.0923(18) Uani 1 1 d G . . H1B H 0.9060 0.5847 0.8513 0.138 Uiso 1 1 d G . . H1C H 0.9534 0.6561 0.8028 0.138 Uiso 1 1 d G . . O2W O 0.9098(5) 0.8972(4) 0.89818(17) 0.0748(14) Uani 1 1 d G . . H2B H 0.8826 0.9285 0.8595 0.112 Uiso 1 1 d G . . H2C H 0.9183 0.8150 0.8832 0.112 Uiso 1 1 d G . . O3W O 0.8113(4) 0.0411(5) 0.02356(17) 0.0652(13) Uani 1 1 d G . . H3D H 0.8850 0.0659 0.0545 0.098 Uiso 1 1 d G . . H3E H 0.8247 -0.0102 -0.0174 0.098 Uiso 1 1 d G . . N3 N 0.6911(6) 0.8494(6) 0.5055(4) 0.0765(18) Uiso 1 1 d . . . H3B H 0.6788 0.9348 0.5237 0.092 Uiso 1 1 calc R . . H3C H 0.7547 0.8281 0.5400 0.092 Uiso 1 1 calc R . . C30 C 0.4749(10) 0.3688(10) 0.8030(6) 0.111(3) Uiso 1 1 d . . . H30A H 0.4584 0.3806 0.8546 0.166 Uiso 1 1 calc R . . H30B H 0.4352 0.2827 0.7734 0.166 Uiso 1 1 calc R . . H30C H 0.4365 0.4362 0.7802 0.166 Uiso 1 1 calc R . . C25 C 0.7437(10) 0.8417(10) 0.4346(6) 0.111(3) Uiso 1 1 d . . . H25A H 0.7457 0.7502 0.4099 0.167 Uiso 1 1 calc R . . H25B H 0.8324 0.8866 0.4465 0.167 Uiso 1 1 calc R . . H25C H 0.6875 0.8834 0.4009 0.167 Uiso 1 1 calc R . . C26 C 0.5587(14) 0.7626(15) 0.5032(9) 0.181(6) Uiso 1 1 d . . . H26A H 0.5030 0.7501 0.4536 0.272 Uiso 1 1 calc R . . H26B H 0.5129 0.8067 0.5421 0.272 Uiso 1 1 calc R . . H26C H 0.5790 0.6778 0.5125 0.272 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 C1 0.025(2) 0.023(2) 0.027(2) 0.004(2) -0.003(2) 0.006(2) C2 0.027(2) 0.022(2) 0.023(2) 0.0035(19) 0.0028(19) 0.002(2) C3 0.030(3) 0.029(3) 0.025(2) 0.000(2) 0.002(2) 0.005(2) C4 0.027(3) 0.030(3) 0.029(3) 0.005(2) 0.008(2) 0.005(2) C5 0.036(3) 0.032(3) 0.046(3) 0.005(3) 0.020(3) 0.009(2) C6 0.024(2) 0.033(3) 0.033(3) 0.002(2) 0.000(2) 0.002(2) C7 0.025(2) 0.031(3) 0.022(2) 0.005(2) -0.0016(19) 0.004(2) C8 0.029(3) 0.031(3) 0.026(2) 0.002(2) 0.008(2) 0.003(2) C9 0.040(3) 0.040(3) 0.027(3) 0.002(2) -0.002(2) 0.010(3) C10 0.040(3) 0.027(3) 0.025(2) 0.002(2) -0.002(2) 0.004(2) C11 0.037(3) 0.036(3) 0.032(3) 0.003(2) 0.004(2) 0.009(2) C12 0.042(3) 0.036(3) 0.031(3) 0.002(2) -0.006(2) 0.002(3) C13 0.050(3) 0.022(3) 0.025(2) 0.003(2) -0.001(2) 0.007(2) C14 0.062(4) 0.036(3) 0.028(3) 0.003(2) 0.001(3) 0.015(3) C15 0.046(3) 0.039(3) 0.032(3) 0.006(2) 0.009(2) 0.009(3) C16 0.032(3) 0.038(3) 0.036(3) 0.002(2) -0.001(2) 0.002(2) C17 0.036(3) 0.024(3) 0.025(2) 0.002(2) -0.002(2) 0.005(2) C18 0.047(3) 0.022(3) 0.028(3) 0.003(2) 0.004(2) 0.007(2) C19 0.034(3) 0.024(3) 0.028(2) 0.001(2) 0.003(2) 0.005(2) C20 0.032(3) 0.024(3) 0.038(3) 0.001(2) 0.003(2) 0.004(2) C21 0.041(3) 0.031(3) 0.023(2) 0.004(2) 0.001(2) 0.004(2) C22 0.041(3) 0.027(3) 0.030(3) 0.007(2) 0.004(2) 0.006(2) C23 0.041(3) 0.031(3) 0.033(3) 0.010(2) 0.007(2) 0.009(2) C24 0.041(3) 0.019(2) 0.031(3) 0.000(2) 0.003(2) 0.006(2) C27 0.069(5) 0.074(5) 0.084(6) 0.030(5) 0.013(4) -0.005(4) C28 0.079(5) 0.087(6) 0.071(5) 0.027(4) 0.022(4) 0.026(5) C29 0.107(9) 0.080(7) 0.154(11) 0.057(7) 0.013(8) 0.019(6) C31 0.178(12) 0.116(10) 0.184(14) 0.054(9) 0.096(11) 0.054(9) Cd1 0.0256(2) 0.0240(2) 0.02434(19) 0.00264(13) 0.00116(13) 0.00378(14) N1 0.028(2) 0.048(3) 0.027(2) 0.006(2) -0.0037(18) 0.011(2) N2 0.061(3) 0.027(2) 0.021(2) -0.0013(18) -0.001(2) 0.015(2) N4 0.058(3) 0.052(3) 0.048(3) -0.002(3) 0.005(3) 0.010(3) N5 0.057(4) 0.062(4) 0.128(7) 0.046(4) 0.032(4) 0.021(3) O1 0.0250(18) 0.043(2) 0.036(2) 0.0007(17) 0.0060(15) 0.0046(16) O2 0.0275(18) 0.035(2) 0.0301(18) -0.0008(15) -0.0028(15) 0.0055(16) O3 0.051(3) 0.091(4) 0.039(2) -0.009(2) 0.019(2) 0.000(2) O4 0.029(2) 0.069(3) 0.053(3) 0.018(2) 0.0126(18) 0.015(2) O5 0.061(3) 0.080(3) 0.033(2) -0.006(2) -0.009(2) 0.039(3) O6 0.093(4) 0.076(3) 0.038(2) -0.010(2) -0.011(2) 0.051(3) O7 0.072(3) 0.0214(19) 0.042(2) 0.0093(17) 0.010(2) 0.0105(19) O8 0.092(3) 0.044(3) 0.035(2) 0.0155(19) -0.011(2) 0.009(2) O9 0.048(2) 0.0209(18) 0.039(2) 0.0019(16) -0.0035(17) 0.0041(16) O10 0.069(3) 0.035(2) 0.034(2) -0.0024(17) -0.006(2) 0.004(2) O11 0.057(4) 0.126(6) 0.205(8) 0.079(6) 0.017(4) 0.023(4) O1W 0.130(5) 0.082(4) 0.070(4) 0.026(3) 0.019(3) 0.012(4) O2W 0.090(4) 0.085(4) 0.050(3) 0.017(3) 0.008(3) 0.023(3) O3W 0.046(3) 0.099(4) 0.052(3) 0.019(3) 0.003(2) 0.027(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.255(5) . ? C1 O1 1.258(6) . ? C1 C2 1.504(6) . ? C2 C8 1.394(6) . ? C2 C3 1.397(7) . ? C3 C4 1.390(6) . ? C3 H3A 0.9300 . ? C4 C6 1.384(7) . ? C4 C5 1.516(7) . ? C5 O3 1.240(7) . ? C5 O4 1.257(6) . ? C5 Cd1 2.862(5) 1_655 ? C6 C7 1.388(7) . ? C6 H6 0.9300 . ? C7 C8 1.380(6) . ? C7 N1 1.427(6) . ? C8 H8 0.9300 . ? C9 O5 1.231(6) . ? C9 N1 1.338(7) . ? C9 C10 1.503(7) . ? C10 C11 1.393(7) . ? C10 C16 1.400(7) . ? C11 C12 1.386(7) . ? C11 H11 0.9300 . ? C12 C13 1.380(8) . ? C12 H12 0.9300 . ? C13 C15 1.391(7) . ? C13 C14 1.495(7) . ? C14 O6 1.241(7) . ? C14 N2 1.331(7) . ? C15 C16 1.378(7) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C24 1.379(7) . ? C17 C18 1.390(7) . ? C17 N2 1.426(6) . ? C18 C19 1.399(7) . ? C18 H18 0.9300 . ? C19 C21 1.381(7) . ? C19 C20 1.520(7) . ? C20 O10 1.242(6) . ? C20 O9 1.261(6) . ? C20 Cd1 2.847(5) 1_666 ? C21 C22 1.391(7) . ? C21 H21 0.9300 . ? C22 C24 1.396(7) . ? C22 C23 1.516(7) . ? C23 O8 1.225(6) . ? C23 O7 1.256(6) . ? C23 Cd1 2.779(5) 1_656 ? C24 H24 0.9300 . ? C27 N4 1.463(8) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N4 1.471(8) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 O11 1.260(11) . ? C29 N5 1.282(12) . ? C29 H29 0.9300 . ? C31 N5 1.441(13) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? Cd1 O4 2.240(4) 1_455 ? Cd1 O9 2.268(3) 1_444 ? Cd1 O7 2.303(4) 1_454 ? Cd1 O1 2.367(3) . ? Cd1 O2 2.432(3) . ? Cd1 O8 2.589(4) 1_454 ? Cd1 O10 2.722(4) 1_444 ? Cd1 C23 2.779(5) 1_454 ? Cd1 O3 2.808(4) 1_455 ? Cd1 C20 2.847(5) 1_444 ? Cd1 C5 2.862(5) 1_455 ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C30 1.405(11) . ? O3 Cd1 2.808(4) 1_655 ? O4 Cd1 2.240(4) 1_655 ? O7 Cd1 2.303(4) 1_656 ? O8 Cd1 2.589(4) 1_656 ? O9 Cd1 2.268(3) 1_666 ? O10 Cd1 2.722(4) 1_666 ? O1W H1B 0.8501 . ? O1W H1C 0.8499 . ? O2W H2B 0.8501 . ? O2W H2C 0.8500 . ? O3W H3D 0.8501 . ? O3W H3E 0.8499 . ? N3 C25 1.458(10) . ? N3 C26 1.563(14) . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 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 O2 C1 O1 122.2(4) . . ? O2 C1 C2 119.2(4) . . ? O1 C1 C2 118.5(4) . . ? C8 C2 C3 119.5(4) . . ? C8 C2 C1 119.7(4) . . ? C3 C2 C1 120.9(4) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C6 C4 C3 119.3(4) . . ? C6 C4 C5 120.7(4) . . ? C3 C4 C5 120.0(4) . . ? O3 C5 O4 123.6(5) . . ? O3 C5 C4 118.9(5) . . ? O4 C5 C4 117.5(5) . . ? O3 C5 Cd1 75.0(3) . 1_655 ? O4 C5 Cd1 48.6(2) . 1_655 ? C4 C5 Cd1 166.2(4) . 1_655 ? C4 C6 C7 121.1(4) . . ? C4 C6 H6 119.4 . . ? C7 C6 H6 119.4 . . ? C8 C7 C6 119.5(4) . . ? C8 C7 N1 121.5(4) . . ? C6 C7 N1 118.9(4) . . ? C7 C8 C2 120.4(4) . . ? C7 C8 H8 119.8 . . ? C2 C8 H8 119.8 . . ? O5 C9 N1 123.5(5) . . ? O5 C9 C10 119.9(5) . . ? N1 C9 C10 116.6(4) . . ? C11 C10 C16 119.9(4) . . ? C11 C10 C9 122.8(5) . . ? C16 C10 C9 117.3(5) . . ? C12 C11 C10 119.3(5) . . ? C12 C11 H11 120.3 . . ? C10 C11 H11 120.3 . . ? C13 C12 C11 121.3(5) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C15 119.0(5) . . ? C12 C13 C14 121.6(5) . . ? C15 C13 C14 119.3(5) . . ? O6 C14 N2 123.7(5) . . ? O6 C14 C13 119.6(5) . . ? N2 C14 C13 116.7(5) . . ? C16 C15 C13 120.9(5) . . ? C16 C15 H15 119.5 . . ? C13 C15 H15 119.5 . . ? C15 C16 C10 119.6(5) . . ? C15 C16 H16 120.2 . . ? C10 C16 H16 120.2 . . ? C24 C17 C18 120.5(4) . . ? C24 C17 N2 119.0(4) . . ? C18 C17 N2 120.6(4) . . ? C17 C18 C19 119.6(4) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C21 C19 C18 119.5(4) . . ? C21 C19 C20 122.2(4) . . ? C18 C19 C20 118.2(4) . . ? O10 C20 O9 122.2(5) . . ? O10 C20 C19 120.2(5) . . ? O9 C20 C19 117.6(4) . . ? O10 C20 Cd1 71.5(3) . 1_666 ? O9 C20 Cd1 50.7(2) . 1_666 ? C19 C20 Cd1 167.9(4) . 1_666 ? C19 C21 C22 121.2(4) . . ? C19 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C21 C22 C24 118.9(4) . . ? C21 C22 C23 121.0(4) . . ? C24 C22 C23 120.1(4) . . ? O8 C23 O7 123.2(5) . . ? O8 C23 C22 119.3(5) . . ? O7 C23 C22 117.5(4) . . ? O8 C23 Cd1 68.3(3) . 1_656 ? O7 C23 Cd1 55.1(3) . 1_656 ? C22 C23 Cd1 170.8(4) . 1_656 ? C17 C24 C22 120.4(4) . . ? C17 C24 H24 119.8 . . ? C22 C24 H24 119.8 . . ? N4 C27 H27A 109.5 . . ? N4 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N4 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O11 C29 N5 124.1(12) . . ? O11 C29 H29 117.9 . . ? N5 C29 H29 117.9 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O4 Cd1 O9 116.19(15) 1_455 1_444 ? O4 Cd1 O7 111.65(14) 1_455 1_454 ? O9 Cd1 O7 89.10(13) 1_444 1_454 ? O4 Cd1 O1 84.05(13) 1_455 . ? O9 Cd1 O1 131.37(13) 1_444 . ? O7 Cd1 O1 125.81(14) 1_454 . ? O4 Cd1 O2 138.28(13) 1_455 . ? O9 Cd1 O2 91.61(13) 1_444 . ? O7 Cd1 O2 98.44(13) 1_454 . ? O1 Cd1 O2 54.56(11) . . ? O4 Cd1 O8 83.97(16) 1_455 1_454 ? O9 Cd1 O8 141.67(12) 1_444 1_454 ? O7 Cd1 O8 52.59(12) 1_454 1_454 ? O1 Cd1 O8 80.09(13) . 1_454 ? O2 Cd1 O8 92.78(14) . 1_454 ? O4 Cd1 O10 90.26(14) 1_455 1_444 ? O9 Cd1 O10 51.10(12) 1_444 1_444 ? O7 Cd1 O10 140.20(12) 1_454 1_444 ? O1 Cd1 O10 87.84(12) . 1_444 ? O2 Cd1 O10 83.84(13) . 1_444 ? O8 Cd1 O10 167.08(11) 1_454 1_444 ? O4 Cd1 C23 97.34(15) 1_455 1_454 ? O9 Cd1 C23 115.67(14) 1_444 1_454 ? O7 Cd1 C23 26.57(14) 1_454 1_454 ? O1 Cd1 C23 103.66(15) . 1_454 ? O2 Cd1 C23 97.40(14) . 1_454 ? O8 Cd1 C23 26.07(13) 1_454 1_454 ? O10 Cd1 C23 166.77(13) 1_444 1_454 ? O4 Cd1 O3 50.16(13) 1_455 1_455 ? O9 Cd1 O3 82.28(14) 1_444 1_455 ? O7 Cd1 O3 75.73(15) 1_454 1_455 ? O1 Cd1 O3 133.83(12) . 1_455 ? O2 Cd1 O3 171.55(11) . 1_455 ? O8 Cd1 O3 88.48(15) 1_454 1_455 ? O10 Cd1 O3 96.70(14) 1_444 1_455 ? C23 Cd1 O3 80.16(16) 1_454 1_455 ? O4 Cd1 C20 104.56(16) 1_455 1_444 ? O9 Cd1 C20 25.47(13) 1_444 1_444 ? O7 Cd1 C20 114.56(14) 1_454 1_444 ? O1 Cd1 C20 110.16(14) . 1_444 ? O2 Cd1 C20 87.26(13) . 1_444 ? O8 Cd1 C20 167.02(14) 1_454 1_444 ? O10 Cd1 C20 25.64(13) 1_444 1_444 ? C23 Cd1 C20 141.13(15) 1_454 1_444 ? O3 Cd1 C20 89.64(15) 1_455 1_444 ? O4 Cd1 C5 24.91(15) 1_455 1_455 ? O9 Cd1 C5 99.94(15) 1_444 1_455 ? O7 Cd1 C5 93.94(15) 1_454 1_455 ? O1 Cd1 C5 108.79(14) . 1_455 ? O2 Cd1 C5 163.19(14) . 1_455 ? O8 Cd1 C5 85.74(16) 1_454 1_455 ? O10 Cd1 C5 93.90(14) 1_444 1_455 ? C23 Cd1 C5 88.61(16) 1_454 1_455 ? O3 Cd1 C5 25.25(13) 1_455 1_455 ? C20 Cd1 C5 97.91(15) 1_444 1_455 ? C9 N1 C7 124.8(4) . . ? C9 N1 H1A 117.6 . . ? C7 N1 H1A 117.6 . . ? C14 N2 C17 125.6(4) . . ? C14 N2 H2A 117.2 . . ? C17 N2 H2A 117.2 . . ? C27 N4 C28 113.8(6) . . ? C27 N4 H4A 108.8 . . ? C28 N4 H4A 108.8 . . ? C27 N4 H4B 108.8 . . ? C28 N4 H4B 108.8 . . ? H4A N4 H4B 107.7 . . ? C29 N5 C30 124.2(10) . . ? C29 N5 C31 119.3(9) . . ? C30 N5 C31 116.4(9) . . ? C1 O1 Cd1 93.0(3) . . ? C1 O2 Cd1 90.1(3) . . ? C5 O3 Cd1 79.8(3) . 1_655 ? C5 O4 Cd1 106.5(3) . 1_655 ? C23 O7 Cd1 98.3(3) . 1_656 ? C23 O8 Cd1 85.7(3) . 1_656 ? C20 O9 Cd1 103.9(3) . 1_666 ? C20 O10 Cd1 82.8(3) . 1_666 ? H1B O1W H1C 109.5 . . ? H2B O2W H2C 109.5 . . ? H3D O3W H3E 109.5 . . ? C25 N3 C26 119.1(8) . . ? C25 N3 H3B 107.5 . . ? C26 N3 H3B 107.5 . . ? C25 N3 H3C 107.5 . . ? C26 N3 H3C 107.5 . . ? H3B N3 H3C 107.0 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N3 C25 H25A 109.5 . . ? N3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C8 -176.6(4) . . . . ? O1 C1 C2 C8 5.0(7) . . . . ? O2 C1 C2 C3 3.1(7) . . . . ? O1 C1 C2 C3 -175.3(4) . . . . ? C8 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C4 -179.7(4) . . . . ? C2 C3 C4 C6 -1.3(7) . . . . ? C2 C3 C4 C5 177.5(4) . . . . ? C6 C4 C5 O3 -171.2(5) . . . . ? C3 C4 C5 O3 10.1(8) . . . . ? C6 C4 C5 O4 8.7(7) . . . . ? C3 C4 C5 O4 -170.1(5) . . . . ? C6 C4 C5 Cd1 7.0(18) . . . 1_655 ? C3 C4 C5 Cd1 -171.7(12) . . . 1_655 ? C3 C4 C6 C7 0.7(7) . . . . ? C5 C4 C6 C7 -178.0(5) . . . . ? C4 C6 C7 C8 1.1(8) . . . . ? C4 C6 C7 N1 177.7(5) . . . . ? C6 C7 C8 C2 -2.4(7) . . . . ? N1 C7 C8 C2 -178.9(4) . . . . ? C3 C2 C8 C7 1.9(7) . . . . ? C1 C2 C8 C7 -178.4(4) . . . . ? O5 C9 C10 C11 -145.5(6) . . . . ? N1 C9 C10 C11 34.9(8) . . . . ? O5 C9 C10 C16 32.9(8) . . . . ? N1 C9 C10 C16 -146.8(5) . . . . ? C16 C10 C11 C12 -0.8(8) . . . . ? C9 C10 C11 C12 177.5(5) . . . . ? C10 C11 C12 C13 0.3(8) . . . . ? C11 C12 C13 C15 0.6(8) . . . . ? C11 C12 C13 C14 -175.3(5) . . . . ? C12 C13 C14 O6 132.6(7) . . . . ? C15 C13 C14 O6 -43.2(8) . . . . ? C12 C13 C14 N2 -49.1(7) . . . . ? C15 C13 C14 N2 135.1(6) . . . . ? C12 C13 C15 C16 -0.9(8) . . . . ? C14 C13 C15 C16 175.0(5) . . . . ? C13 C15 C16 C10 0.4(8) . . . . ? C11 C10 C16 C15 0.5(8) . . . . ? C9 C10 C16 C15 -177.9(5) . . . . ? C24 C17 C18 C19 -1.8(8) . . . . ? N2 C17 C18 C19 179.7(5) . . . . ? C17 C18 C19 C21 1.7(8) . . . . ? C17 C18 C19 C20 -179.8(5) . . . . ? C21 C19 C20 O10 -4.7(8) . . . . ? C18 C19 C20 O10 176.9(5) . . . . ? C21 C19 C20 O9 173.0(5) . . . . ? C18 C19 C20 O9 -5.5(7) . . . . ? C21 C19 C20 Cd1 160.0(14) . . . 1_666 ? C18 C19 C20 Cd1 -18.5(19) . . . 1_666 ? C18 C19 C21 C22 -0.8(8) . . . . ? C20 C19 C21 C22 -179.3(5) . . . . ? C19 C21 C22 C24 0.0(8) . . . . ? C19 C21 C22 C23 -178.2(5) . . . . ? C21 C22 C23 O8 -1.9(8) . . . . ? C24 C22 C23 O8 179.9(5) . . . . ? C21 C22 C23 O7 177.2(5) . . . . ? C24 C22 C23 O7 -1.0(8) . . . . ? C21 C22 C23 Cd1 143(2) . . . 1_656 ? C24 C22 C23 Cd1 -35(3) . . . 1_656 ? C18 C17 C24 C22 1.0(8) . . . . ? N2 C17 C24 C22 179.6(5) . . . . ? C21 C22 C24 C17 -0.1(8) . . . . ? C23 C22 C24 C17 178.1(5) . . . . ? O5 C9 N1 C7 -3.7(9) . . . . ? C10 C9 N1 C7 175.9(5) . . . . ? C8 C7 N1 C9 -34.7(8) . . . . ? C6 C7 N1 C9 148.8(5) . . . . ? O6 C14 N2 C17 -2.4(10) . . . . ? C13 C14 N2 C17 179.4(5) . . . . ? C24 C17 N2 C14 143.7(6) . . . . ? C18 C17 N2 C14 -37.8(8) . . . . ? O11 C29 N5 C30 177.2(8) . . . . ? O11 C29 N5 C31 -0.2(14) . . . . ? O2 C1 O1 Cd1 -3.3(5) . . . . ? C2 C1 O1 Cd1 175.1(4) . . . . ? O4 Cd1 O1 C1 176.2(3) 1_455 . . . ? O9 Cd1 O1 C1 56.2(3) 1_444 . . . ? O7 Cd1 O1 C1 -71.3(3) 1_454 . . . ? O2 Cd1 O1 C1 1.7(3) . . . . ? O8 Cd1 O1 C1 -98.9(3) 1_454 . . . ? O10 Cd1 O1 C1 85.7(3) 1_444 . . . ? C23 Cd1 O1 C1 -87.7(3) 1_454 . . . ? O3 Cd1 O1 C1 -177.1(3) 1_455 . . . ? C20 Cd1 O1 C1 72.9(3) 1_444 . . . ? C5 Cd1 O1 C1 179.1(3) 1_455 . . . ? O1 C1 O2 Cd1 3.2(5) . . . . ? C2 C1 O2 Cd1 -175.2(4) . . . . ? O4 Cd1 O2 C1 -10.0(4) 1_455 . . . ? O9 Cd1 O2 C1 -144.1(3) 1_444 . . . ? O7 Cd1 O2 C1 126.6(3) 1_454 . . . ? O1 Cd1 O2 C1 -1.7(3) . . . . ? O8 Cd1 O2 C1 74.0(3) 1_454 . . . ? O10 Cd1 O2 C1 -93.5(3) 1_444 . . . ? C23 Cd1 O2 C1 99.8(3) 1_454 . . . ? O3 Cd1 O2 C1 172.4(8) 1_455 . . . ? C20 Cd1 O2 C1 -119.0(3) 1_444 . . . ? C5 Cd1 O2 C1 -10.4(6) 1_455 . . . ? O4 C5 O3 Cd1 -0.3(5) . . . 1_655 ? C4 C5 O3 Cd1 179.6(5) . . . 1_655 ? O3 C5 O4 Cd1 0.4(7) . . . 1_655 ? C4 C5 O4 Cd1 -179.5(4) . . . 1_655 ? O8 C23 O7 Cd1 5.3(6) . . . 1_656 ? C22 C23 O7 Cd1 -173.7(4) . . . 1_656 ? O7 C23 O8 Cd1 -4.7(6) . . . 1_656 ? C22 C23 O8 Cd1 174.4(5) . . . 1_656 ? O10 C20 O9 Cd1 1.1(6) . . . 1_666 ? C19 C20 O9 Cd1 -176.5(4) . . . 1_666 ? O9 C20 O10 Cd1 -0.9(5) . . . 1_666 ? C19 C20 O10 Cd1 176.6(5) . . . 1_666 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N3 H3C O9 0.90 1.88 2.771(7) 168.9 . O3W H3E O2W 0.85 1.98 2.806 163.1 1_544 O3W H3D O2W 0.85 2.11 2.931(8) 163.0 2_766 O2W H2C O1W 0.85 1.89 2.727 170.3 . O2W H2B O4 0.85 1.94 2.788(5) 179.0 1_566 O1W H1C O10 0.85 1.91 2.756(5) 170.9 . O1W H1B O11 0.85 1.99 2.798(9) 158.7 . N4 H4B O11 0.90 2.12 2.861(8) 139.6 1_455 N4 H4A O1 0.90 1.95 2.844(6) 171.5 1_556 N2 H2A O2 0.86 2.11 2.917(5) 155.8 2_655 N1 H1A O3W 0.86 2.09 2.911(6) 159.8 . _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.166 _refine_diff_density_min -0.741 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 964931' ####################################################################### # # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H12 N2 O10 Zn, C3 H7 N O, 2(C2 H8 N), 3(H2 O)' _chemical_formula_sum 'C31 H41 N5 O14 Zn' _chemical_formula_weight 773.08 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.004(2) _cell_length_b 10.293(2) _cell_length_c 17.914(4) _cell_angle_alpha 103.66(3) _cell_angle_beta 99.58(3) _cell_angle_gamma 93.45(3) _cell_volume 1757.9(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.461 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.824 _exptl_absorpt_correction_T_max 0.857 _exptl_absorpt_process_details Higashi,1995 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type SCX-MINI _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time ? _diffrn_standards_decay_% none _diffrn_reflns_number 18509 _diffrn_reflns_av_R_equivalents 0.0621 _diffrn_reflns_av_sigmaI/netI 0.0869 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8044 _reflns_number_gt 5636 _reflns_threshold_expression >2sigma(I) _computing_data_collection PROCESS-AUTO _computing_cell_refinement PROCESS-AUTO _computing_data_reduction CrystalStructure _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^)+(0.0560P)^2^+0.8377P] 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 8044 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1090 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1461 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _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 C1 C 0.6829(4) 0.4955(4) -0.2836(2) 0.0362(9) Uani 1 1 d . . . C2 C 0.5796(3) 0.5241(3) -0.23073(19) 0.0273(7) Uani 1 1 d . . . C3 C 0.4419(3) 0.4977(3) -0.2638(2) 0.0305(8) Uani 1 1 d . . . H3A H 0.4152 0.4657 -0.3177 0.037 Uiso 1 1 calc R . . C4 C 0.3440(3) 0.5189(3) -0.21709(19) 0.0264(7) Uani 1 1 d . . . C5 C 0.1954(4) 0.4903(3) -0.2529(2) 0.0343(9) Uani 1 1 d . . . C6 C 0.3837(3) 0.5688(3) -0.1369(2) 0.0294(8) Uani 1 1 d . . . H6 H 0.3181 0.5820 -0.1054 0.035 Uiso 1 1 calc R . . C7 C 0.5209(3) 0.5991(3) -0.10323(19) 0.0291(8) Uani 1 1 d . . . C8 C 0.6186(3) 0.5764(3) -0.1509(2) 0.0301(8) Uani 1 1 d . . . H8 H 0.7107 0.5966 -0.1288 0.036 Uiso 1 1 calc R . . C9 C 0.4958(4) 0.7344(4) 0.0251(2) 0.0390(9) Uani 1 1 d . . . C10 C 0.5477(4) 0.7658(4) 0.1112(2) 0.0332(8) Uani 1 1 d . . . C11 C 0.6859(4) 0.7823(4) 0.1441(2) 0.0376(9) Uani 1 1 d . . . H11 H 0.7507 0.7686 0.1121 0.045 Uiso 1 1 calc R . . C12 C 0.7264(4) 0.8193(4) 0.2247(2) 0.0379(9) Uani 1 1 d . . . H12 H 0.8187 0.8311 0.2466 0.046 Uiso 1 1 calc R . . C13 C 0.6312(4) 0.8386(4) 0.2727(2) 0.0359(9) Uani 1 1 d . . . C14 C 0.4940(4) 0.8185(4) 0.2401(2) 0.0384(9) Uani 1 1 d . . . H14 H 0.4294 0.8298 0.2723 0.046 Uiso 1 1 calc R . . C15 C 0.4523(4) 0.7816(4) 0.1599(2) 0.0386(9) Uani 1 1 d . . . H15 H 0.3598 0.7673 0.1384 0.046 Uiso 1 1 calc R . . C16 C 0.6716(4) 0.8910(4) 0.3596(2) 0.0444(10) Uani 1 1 d . . . C17 C 0.8205(4) 0.8676(3) 0.4782(2) 0.0320(8) Uani 1 1 d . . . C18 C 0.8539(4) 0.7667(3) 0.5155(2) 0.0321(8) Uani 1 1 d . . . H18 H 0.8424 0.6773 0.4873 0.038 Uiso 1 1 calc R . . C19 C 0.9046(4) 0.8006(3) 0.5955(2) 0.0309(8) Uani 1 1 d . . . C20 C 0.9376(4) 0.6937(4) 0.6392(2) 0.0362(9) Uani 1 1 d . . . C21 C 0.9216(4) 0.9343(3) 0.6374(2) 0.0317(8) Uani 1 1 d . . . H21 H 0.9555 0.9566 0.6909 0.038 Uiso 1 1 calc R . . C22 C 0.8881(3) 1.0355(3) 0.59987(19) 0.0283(8) Uani 1 1 d . . . C23 C 0.9071(3) 1.1800(3) 0.6459(2) 0.0306(8) Uani 1 1 d . . . C24 C 0.8403(4) 1.0009(3) 0.5200(2) 0.0337(8) Uani 1 1 d . . . H24 H 0.8212 1.0680 0.4941 0.040 Uiso 1 1 calc R . . C25 C 0.6886(6) 0.9214(6) 0.8774(4) 0.0789(16) Uani 1 1 d . . . H25 H 0.6504 0.9388 0.9222 0.095 Uiso 1 1 calc R . . C26 C 0.6578(7) 0.8595(7) 0.7387(4) 0.100(2) Uani 1 1 d . . . H26A H 0.7546 0.8560 0.7498 0.150 Uiso 1 1 calc R . . H26B H 0.6381 0.9287 0.7120 0.150 Uiso 1 1 calc R . . H26C H 0.6148 0.7744 0.7062 0.150 Uiso 1 1 calc R . . C27 C 0.4609(5) 0.8729(6) 0.8052(4) 0.098(2) Uani 1 1 d . . . H27A H 0.4264 0.7809 0.7806 0.147 Uiso 1 1 calc R . . H27B H 0.4198 0.9300 0.7745 0.147 Uiso 1 1 calc R . . H27C H 0.4392 0.8973 0.8566 0.147 Uiso 1 1 calc R . . C28 C 0.7447(8) 0.3507(7) 0.4382(3) 0.124(3) Uani 1 1 d . . . H28A H 0.7352 0.2664 0.3997 0.186 Uiso 1 1 calc R . . H28B H 0.8397 0.3804 0.4574 0.186 Uiso 1 1 calc R . . H28C H 0.7021 0.4163 0.4148 0.186 Uiso 1 1 calc R . . C29 C 0.5381(8) 0.2778(10) 0.4836(5) 0.177(5) Uani 1 1 d . . . H29A H 0.5104 0.2466 0.4279 0.266 Uiso 1 1 calc R . . H29B H 0.4823 0.3458 0.5033 0.266 Uiso 1 1 calc R . . H29C H 0.5279 0.2040 0.5071 0.266 Uiso 1 1 calc R . . O1W O 0.8111(3) 0.5347(3) 0.01839(13) 0.0660(9) Uani 1 1 d G . . H1B H 0.8272 0.4924 -0.0255 0.099 Uiso 1 1 d G . . H1C H 0.8854 0.5557 0.0514 0.099 Uiso 1 1 d G . . O2W O 0.9111(4) 0.4031(3) 0.88877(12) 0.0793(11) Uani 1 1 d G . . H2B H 0.8829 0.4164 0.8440 0.119 Uiso 1 1 d G . . H2C H 0.9302 0.3225 0.8835 0.119 Uiso 1 1 d G . . O3W O 0.9612(4) 0.1446(3) 0.85597(13) 0.1011(14) Uani 1 1 d G . . H3B H 0.9088 0.0867 0.8671 0.152 Uiso 1 1 d G . . H3C H 0.9664 0.1201 0.8079 0.152 Uiso 1 1 d G . . C30 C 0.1510(5) 0.8808(6) 0.8754(3) 0.0734(15) Uani 1 1 d . . . H30A H 0.1353 0.9653 0.9074 0.110 Uiso 1 1 calc R . . H30B H 0.1513 0.8890 0.8231 0.110 Uiso 1 1 calc R . . H30C H 0.2375 0.8557 0.8964 0.110 Uiso 1 1 calc R . . C31 C 0.0376(5) 0.7566(6) 0.9500(3) 0.0738(15) Uani 1 1 d . . . H31A H 0.1241 0.7328 0.9720 0.111 Uiso 1 1 calc R . . H31B H -0.0321 0.6853 0.9453 0.111 Uiso 1 1 calc R . . H31C H 0.0171 0.8376 0.9835 0.111 Uiso 1 1 calc R . . N1 N 0.7686(3) 0.8305(3) 0.39606(16) 0.0367(8) Uani 1 1 d . . . H1A H 0.8017 0.7650 0.3679 0.044 Uiso 1 1 calc R . . N2 N 0.5636(3) 0.6495(3) -0.02151(16) 0.0358(7) Uani 1 1 d . . . H2A H 0.6377 0.6245 0.0001 0.043 Uiso 1 1 calc R . . N3 N 0.6067(4) 0.8885(4) 0.8109(3) 0.0637(11) Uani 1 1 d . . . N4 N 0.6801(5) 0.3340(5) 0.5024(2) 0.0834(15) Uani 1 1 d . . . H4A H 0.6861 0.4150 0.5363 0.100 Uiso 1 1 calc R . . H4B H 0.7286 0.2810 0.5274 0.100 Uiso 1 1 calc R . . N5 N 0.0431(4) 0.7779(4) 0.8741(2) 0.0559(10) Uani 1 1 d . . . H5A H -0.0376 0.8021 0.8543 0.067 Uiso 1 1 calc R . . H5B H 0.0563 0.7000 0.8421 0.067 Uiso 1 1 calc R . . O1 O 0.8064(2) 0.4956(3) -0.25109(15) 0.0393(6) Uani 1 1 d . . . O2 O 0.6430(3) 0.4759(4) -0.35463(16) 0.0700(10) Uani 1 1 d . . . O3 O 0.1612(3) 0.4341(3) -0.32489(16) 0.0437(7) Uani 1 1 d . . . O4 O 0.1077(2) 0.5222(3) -0.21137(17) 0.0462(7) Uani 1 1 d . . . O5 O 0.3947(3) 0.7837(3) -0.00041(16) 0.0639(9) Uani 1 1 d . . . O6 O 0.6159(4) 0.9841(4) 0.39305(17) 0.0839(13) Uani 1 1 d . . . O7 O 0.9125(3) 0.5712(2) 0.60148(15) 0.0389(6) Uani 1 1 d . . . O8 O 0.9865(4) 0.7296(3) 0.70941(17) 0.0731(11) Uani 1 1 d . . . O9 O 0.9426(3) 1.2081(3) 0.71797(15) 0.0518(8) Uani 1 1 d . . . O10 O 0.8871(2) 1.2703(2) 0.60817(14) 0.0333(6) Uani 1 1 d . . . O11 O 0.8156(4) 0.9316(4) 0.8863(3) 0.0993(14) Uani 1 1 d . . . Zn1 Zn 0.94399(4) 0.45780(4) -0.32053(2) 0.02639(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(2) 0.044(2) 0.032(2) 0.0061(17) 0.0090(17) 0.0040(17) C2 0.0256(17) 0.0277(19) 0.0271(18) 0.0042(14) 0.0048(14) 0.0019(14) C3 0.0330(19) 0.0296(19) 0.0258(18) 0.0053(15) -0.0007(15) 0.0028(15) C4 0.0222(16) 0.0241(18) 0.0302(19) 0.0048(14) 0.0005(14) 0.0023(14) C5 0.0265(18) 0.0248(19) 0.048(2) 0.0113(17) -0.0065(17) 0.0017(15) C6 0.0260(17) 0.032(2) 0.0307(19) 0.0075(15) 0.0059(15) 0.0041(15) C7 0.0302(18) 0.0298(19) 0.0243(18) 0.0041(14) 0.0000(15) 0.0054(15) C8 0.0218(17) 0.034(2) 0.0321(19) 0.0064(16) 0.0007(15) 0.0023(15) C9 0.041(2) 0.041(2) 0.030(2) 0.0040(17) -0.0052(17) 0.0110(18) C10 0.039(2) 0.032(2) 0.0253(19) 0.0062(15) -0.0023(16) 0.0061(16) C11 0.042(2) 0.038(2) 0.030(2) 0.0054(17) 0.0008(17) 0.0084(18) C12 0.040(2) 0.035(2) 0.032(2) 0.0043(17) -0.0074(17) 0.0063(17) C13 0.052(2) 0.0267(19) 0.0254(19) 0.0049(15) -0.0024(17) 0.0098(17) C14 0.047(2) 0.038(2) 0.030(2) 0.0063(17) 0.0104(18) 0.0058(18) C15 0.038(2) 0.040(2) 0.034(2) 0.0076(17) -0.0001(17) 0.0013(18) C16 0.064(3) 0.039(2) 0.028(2) 0.0037(17) 0.003(2) 0.016(2) C17 0.040(2) 0.030(2) 0.0235(18) 0.0051(15) 0.0019(16) 0.0047(16) C18 0.046(2) 0.0221(18) 0.0263(19) 0.0041(14) 0.0039(16) 0.0067(16) C19 0.0371(19) 0.0260(19) 0.032(2) 0.0108(15) 0.0062(16) 0.0069(16) C20 0.046(2) 0.031(2) 0.036(2) 0.0163(17) 0.0065(18) 0.0096(17) C21 0.043(2) 0.0275(19) 0.0234(18) 0.0058(15) 0.0037(16) 0.0030(16) C22 0.0319(18) 0.0233(18) 0.0278(18) 0.0056(14) 0.0017(15) 0.0030(15) C23 0.0287(18) 0.0257(19) 0.034(2) 0.0049(16) 0.0004(16) -0.0015(15) C24 0.047(2) 0.0260(19) 0.0277(19) 0.0107(15) -0.0008(17) 0.0055(17) C25 0.078(4) 0.070(4) 0.098(5) 0.031(3) 0.023(4) 0.026(3) C26 0.115(5) 0.098(5) 0.099(5) 0.030(4) 0.041(4) 0.023(4) C27 0.063(4) 0.066(4) 0.177(7) 0.053(4) 0.023(4) 0.015(3) C28 0.210(9) 0.110(6) 0.051(4) 0.021(4) 0.026(5) -0.003(6) C29 0.100(6) 0.238(11) 0.118(7) -0.091(7) 0.007(5) 0.001(6) O1W 0.0497(18) 0.101(3) 0.0528(19) 0.0260(19) 0.0094(15) 0.0284(18) O2W 0.095(3) 0.097(3) 0.056(2) 0.033(2) 0.019(2) 0.020(2) O3W 0.141(4) 0.098(3) 0.069(3) 0.028(2) 0.022(3) 0.012(3) C30 0.057(3) 0.083(4) 0.081(4) 0.033(3) -0.001(3) -0.005(3) C31 0.077(4) 0.084(4) 0.073(4) 0.033(3) 0.025(3) 0.022(3) N1 0.054(2) 0.0310(17) 0.0228(16) 0.0034(13) 0.0007(14) 0.0159(15) N2 0.0351(16) 0.048(2) 0.0207(15) 0.0052(14) -0.0018(13) 0.0124(15) N3 0.057(3) 0.054(3) 0.089(3) 0.029(2) 0.017(2) 0.017(2) N4 0.088(3) 0.112(4) 0.043(2) 0.005(2) -0.004(2) 0.057(3) N5 0.065(2) 0.054(2) 0.043(2) 0.0028(18) 0.0071(19) 0.008(2) O1 0.0267(13) 0.0544(17) 0.0390(15) 0.0133(13) 0.0080(11) 0.0095(12) O2 0.0407(17) 0.132(3) 0.0287(16) 0.0017(18) 0.0085(14) 0.0096(18) O3 0.0368(14) 0.0377(15) 0.0454(17) 0.0050(13) -0.0149(13) 0.0001(12) O4 0.0243(13) 0.0439(17) 0.070(2) 0.0122(14) 0.0102(14) 0.0075(12) O5 0.068(2) 0.081(2) 0.0345(16) 0.0000(15) -0.0085(15) 0.0454(18) O6 0.109(3) 0.090(3) 0.0362(18) -0.0111(17) -0.0133(18) 0.066(2) O7 0.0471(15) 0.0288(14) 0.0448(16) 0.0149(12) 0.0097(13) 0.0100(12) O8 0.128(3) 0.0472(19) 0.0369(18) 0.0162(15) -0.0133(19) 0.013(2) O9 0.080(2) 0.0345(16) 0.0304(15) -0.0007(12) -0.0062(15) 0.0061(15) O10 0.0401(14) 0.0221(13) 0.0356(14) 0.0079(11) -0.0002(11) 0.0035(11) O11 0.065(3) 0.102(3) 0.134(4) 0.040(3) 0.005(3) 0.019(2) Zn1 0.0242(2) 0.0263(2) 0.0273(2) 0.00597(16) 0.00161(16) 0.00310(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.233(4) . ? C1 O1 1.275(4) . ? C1 C2 1.511(5) . ? C2 C8 1.383(5) . ? C2 C3 1.390(5) . ? C3 C4 1.386(5) . ? C3 H3A 0.9300 . ? C4 C6 1.387(5) . ? C4 C5 1.500(5) . ? C5 O4 1.252(4) . ? C5 O3 1.262(4) . ? C5 Zn1 2.568(3) 1_455 ? C6 C7 1.389(5) . ? C6 H6 0.9300 . ? C7 C8 1.397(5) . ? C7 N2 1.415(4) . ? C8 H8 0.9300 . ? C9 O5 1.227(4) . ? C9 N2 1.355(5) . ? C9 C10 1.495(5) . ? C10 C15 1.387(5) . ? C10 C11 1.393(5) . ? C11 C12 1.386(5) . ? C11 H11 0.9300 . ? C12 C13 1.379(5) . ? C12 H12 0.9300 . ? C13 C14 1.382(5) . ? C13 C16 1.499(5) . ? C14 C15 1.380(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O6 1.221(5) . ? C16 N1 1.346(5) . ? C17 C24 1.384(5) . ? C17 C18 1.390(5) . ? C17 N1 1.427(4) . ? C18 C19 1.390(5) . ? C18 H18 0.9300 . ? C19 C21 1.388(5) . ? C19 C20 1.515(5) . ? C20 O8 1.230(4) . ? C20 O7 1.270(4) . ? C21 C22 1.395(5) . ? C21 H21 0.9300 . ? C22 C24 1.384(5) . ? C22 C23 1.505(5) . ? C23 O9 1.239(4) . ? C23 O10 1.279(4) . ? C24 H24 0.9300 . ? C25 O11 1.249(6) . ? C25 N3 1.288(7) . ? C25 H25 0.9300 . ? C26 N3 1.442(7) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 N3 1.442(6) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 N4 1.449(7) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N4 1.454(8) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? O1W H1B 0.8501 . ? O1W H1C 0.8499 . ? O2W H2B 0.8501 . ? O2W H2C 0.8500 . ? O3W H3B 0.8500 . ? O3W H3C 0.8500 . ? C30 N5 1.459(6) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 N5 1.437(6) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? N1 H1A 0.8600 . ? N2 H2A 0.8600 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? O1 Zn1 2.000(2) . ? O3 Zn1 2.213(3) 1_455 ? O4 Zn1 2.266(3) 1_455 ? O7 Zn1 2.020(2) 1_556 ? O10 Zn1 2.035(2) 1_566 ? Zn1 O7 2.020(3) 1_554 ? Zn1 O10 2.035(2) 1_544 ? Zn1 O3 2.213(3) 1_655 ? Zn1 O4 2.266(3) 1_655 ? Zn1 C5 2.568(3) 1_655 ? 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 O2 C1 O1 124.5(3) . . ? O2 C1 C2 118.2(3) . . ? O1 C1 C2 117.2(3) . . ? C8 C2 C3 119.5(3) . . ? C8 C2 C1 121.8(3) . . ? C3 C2 C1 118.7(3) . . ? C4 C3 C2 120.4(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C6 119.8(3) . . ? C3 C4 C5 120.4(3) . . ? C6 C4 C5 119.8(3) . . ? O4 C5 O3 121.2(3) . . ? O4 C5 C4 119.9(3) . . ? O3 C5 C4 118.9(3) . . ? O4 C5 Zn1 61.91(18) . 1_455 ? O3 C5 Zn1 59.48(18) . 1_455 ? C4 C5 Zn1 174.9(3) . 1_455 ? C4 C6 C7 120.4(3) . . ? C4 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? C6 C7 C8 119.3(3) . . ? C6 C7 N2 121.3(3) . . ? C8 C7 N2 119.4(3) . . ? C2 C8 C7 120.5(3) . . ? C2 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? O5 C9 N2 123.0(3) . . ? O5 C9 C10 119.8(3) . . ? N2 C9 C10 117.2(3) . . ? C15 C10 C11 119.4(3) . . ? C15 C10 C9 117.6(3) . . ? C11 C10 C9 123.0(3) . . ? C12 C11 C10 119.6(4) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12 119.6 . . ? C11 C12 H12 119.6 . . ? C12 C13 C14 119.6(3) . . ? C12 C13 C16 122.0(3) . . ? C14 C13 C16 118.3(4) . . ? C15 C14 C13 120.3(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 120.4(4) . . ? C14 C15 H15 119.8 . . ? C10 C15 H15 119.8 . . ? O6 C16 N1 124.0(4) . . ? O6 C16 C13 119.2(4) . . ? N1 C16 C13 116.7(3) . . ? C24 C17 C18 120.3(3) . . ? C24 C17 N1 121.2(3) . . ? C18 C17 N1 118.5(3) . . ? C17 C18 C19 119.5(3) . . ? C17 C18 H18 120.3 . . ? C19 C18 H18 120.3 . . ? C21 C19 C18 120.0(3) . . ? C21 C19 C20 118.7(3) . . ? C18 C19 C20 121.3(3) . . ? O8 C20 O7 123.1(3) . . ? O8 C20 C19 118.5(3) . . ? O7 C20 C19 118.3(3) . . ? C19 C21 C22 120.5(3) . . ? C19 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C24 C22 C21 119.0(3) . . ? C24 C22 C23 120.9(3) . . ? C21 C22 C23 120.0(3) . . ? O9 C23 O10 122.3(3) . . ? O9 C23 C22 119.9(3) . . ? O10 C23 C22 117.9(3) . . ? C22 C24 C17 120.6(3) . . ? C22 C24 H24 119.7 . . ? C17 C24 H24 119.7 . . ? O11 C25 N3 124.9(6) . . ? O11 C25 H25 117.6 . . ? N3 C25 H25 117.6 . . ? N3 C26 H26A 109.5 . . ? N3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 H27A 109.5 . . ? N3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N4 C28 H28A 109.5 . . ? N4 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? N4 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 H29A 109.5 . . ? N4 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N4 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H1B O1W H1C 109.5 . . ? H2B O2W H2C 109.5 . . ? H3B O3W H3C 109.5 . . ? N5 C30 H30A 109.5 . . ? N5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N5 C31 H31A 109.5 . . ? N5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C16 N1 C17 124.5(3) . . ? C16 N1 H1A 117.8 . . ? C17 N1 H1A 117.8 . . ? C9 N2 C7 124.5(3) . . ? C9 N2 H2A 117.7 . . ? C7 N2 H2A 117.7 . . ? C25 N3 C26 121.0(5) . . ? C25 N3 C27 121.8(5) . . ? C26 N3 C27 117.1(5) . . ? C28 N4 C29 117.4(6) . . ? C28 N4 H4A 107.9 . . ? C29 N4 H4A 107.9 . . ? C28 N4 H4B 107.9 . . ? C29 N4 H4B 107.9 . . ? H4A N4 H4B 107.2 . . ? C31 N5 C30 113.2(4) . . ? C31 N5 H5A 108.9 . . ? C30 N5 H5A 108.9 . . ? C31 N5 H5B 108.9 . . ? C30 N5 H5B 108.9 . . ? H5A N5 H5B 107.8 . . ? C1 O1 Zn1 117.6(2) . . ? C5 O3 Zn1 91.1(2) . 1_455 ? C5 O4 Zn1 88.9(2) . 1_455 ? C20 O7 Zn1 107.7(2) . 1_556 ? C23 O10 Zn1 111.2(2) . 1_566 ? O1 Zn1 O7 107.52(11) . 1_554 ? O1 Zn1 O10 107.06(11) . 1_544 ? O7 Zn1 O10 100.78(10) 1_554 1_544 ? O1 Zn1 O3 145.39(10) . 1_655 ? O7 Zn1 O3 97.38(11) 1_554 1_655 ? O10 Zn1 O3 90.97(10) 1_544 1_655 ? O1 Zn1 O4 87.62(10) . 1_655 ? O7 Zn1 O4 121.80(10) 1_554 1_655 ? O10 Zn1 O4 128.52(10) 1_544 1_655 ? O3 Zn1 O4 58.52(10) 1_655 1_655 ? O1 Zn1 C5 116.70(12) . 1_655 ? O7 Zn1 C5 110.77(12) 1_554 1_655 ? O10 Zn1 C5 112.71(11) 1_544 1_655 ? O3 Zn1 C5 29.41(11) 1_655 1_655 ? O4 Zn1 C5 29.17(11) 1_655 1_655 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C8 -165.2(4) . . . . ? O1 C1 C2 C8 13.7(5) . . . . ? O2 C1 C2 C3 14.3(5) . . . . ? O1 C1 C2 C3 -166.8(3) . . . . ? C8 C2 C3 C4 -2.4(5) . . . . ? C1 C2 C3 C4 178.1(3) . . . . ? C2 C3 C4 C6 1.1(5) . . . . ? C2 C3 C4 C5 -179.9(3) . . . . ? C3 C4 C5 O4 -172.8(3) . . . . ? C6 C4 C5 O4 6.1(5) . . . . ? C3 C4 C5 O3 7.1(5) . . . . ? C6 C4 C5 O3 -173.9(3) . . . . ? C3 C4 C5 Zn1 -63(3) . . . 1_455 ? C6 C4 C5 Zn1 116(3) . . . 1_455 ? C3 C4 C6 C7 0.7(5) . . . . ? C5 C4 C6 C7 -178.3(3) . . . . ? C4 C6 C7 C8 -1.2(5) . . . . ? C4 C6 C7 N2 -179.7(3) . . . . ? C3 C2 C8 C7 1.9(5) . . . . ? C1 C2 C8 C7 -178.6(3) . . . . ? C6 C7 C8 C2 -0.1(5) . . . . ? N2 C7 C8 C2 178.4(3) . . . . ? O5 C9 C10 C15 35.3(6) . . . . ? N2 C9 C10 C15 -143.7(4) . . . . ? O5 C9 C10 C11 -143.3(4) . . . . ? N2 C9 C10 C11 37.6(5) . . . . ? C15 C10 C11 C12 -2.5(5) . . . . ? C9 C10 C11 C12 176.1(3) . . . . ? C10 C11 C12 C13 0.6(6) . . . . ? C11 C12 C13 C14 1.3(6) . . . . ? C11 C12 C13 C16 -174.1(3) . . . . ? C12 C13 C14 C15 -1.2(6) . . . . ? C16 C13 C14 C15 174.3(3) . . . . ? C13 C14 C15 C10 -0.7(6) . . . . ? C11 C10 C15 C14 2.5(6) . . . . ? C9 C10 C15 C14 -176.2(3) . . . . ? C12 C13 C16 O6 130.8(5) . . . . ? C14 C13 C16 O6 -44.7(6) . . . . ? C12 C13 C16 N1 -49.3(5) . . . . ? C14 C13 C16 N1 135.2(4) . . . . ? C24 C17 C18 C19 1.4(6) . . . . ? N1 C17 C18 C19 180.0(3) . . . . ? C17 C18 C19 C21 -0.1(5) . . . . ? C17 C18 C19 C20 177.8(3) . . . . ? C21 C19 C20 O8 -4.5(6) . . . . ? C18 C19 C20 O8 177.6(4) . . . . ? C21 C19 C20 O7 175.0(3) . . . . ? C18 C19 C20 O7 -2.9(5) . . . . ? C18 C19 C21 C22 0.0(5) . . . . ? C20 C19 C21 C22 -177.9(3) . . . . ? C19 C21 C22 C24 -1.2(5) . . . . ? C19 C21 C22 C23 -180.0(3) . . . . ? C24 C22 C23 O9 175.8(3) . . . . ? C21 C22 C23 O9 -5.5(5) . . . . ? C24 C22 C23 O10 -5.0(5) . . . . ? C21 C22 C23 O10 173.7(3) . . . . ? C21 C22 C24 C17 2.6(5) . . . . ? C23 C22 C24 C17 -178.7(3) . . . . ? C18 C17 C24 C22 -2.7(6) . . . . ? N1 C17 C24 C22 178.8(3) . . . . ? O6 C16 N1 C17 -0.7(7) . . . . ? C13 C16 N1 C17 179.5(3) . . . . ? C24 C17 N1 C16 -37.9(6) . . . . ? C18 C17 N1 C16 143.5(4) . . . . ? O5 C9 N2 C7 -5.4(6) . . . . ? C10 C9 N2 C7 173.6(3) . . . . ? C6 C7 N2 C9 -35.6(5) . . . . ? C8 C7 N2 C9 145.8(4) . . . . ? O11 C25 N3 C26 0.2(9) . . . . ? O11 C25 N3 C27 177.2(5) . . . . ? O2 C1 O1 Zn1 -1.2(5) . . . . ? C2 C1 O1 Zn1 180.0(2) . . . . ? O4 C5 O3 Zn1 5.5(4) . . . 1_455 ? C4 C5 O3 Zn1 -174.4(3) . . . 1_455 ? O3 C5 O4 Zn1 -5.4(3) . . . 1_455 ? C4 C5 O4 Zn1 174.5(3) . . . 1_455 ? O8 C20 O7 Zn1 7.1(5) . . . 1_556 ? C19 C20 O7 Zn1 -172.4(3) . . . 1_556 ? O9 C23 O10 Zn1 7.2(4) . . . 1_566 ? C22 C23 O10 Zn1 -172.0(2) . . . 1_566 ? C1 O1 Zn1 O7 46.8(3) . . . 1_554 ? C1 O1 Zn1 O10 -60.8(3) . . . 1_544 ? C1 O1 Zn1 O3 -179.2(2) . . . 1_655 ? C1 O1 Zn1 O4 169.5(3) . . . 1_655 ? C1 O1 Zn1 C5 171.9(3) . . . 1_655 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N5 H5B O4 0.90 1.99 2.884(5) 169.4 1_556 N5 H5A O11 0.90 2.10 2.858(6) 141.0 1_455 N4 H4B O10 0.90 1.99 2.784(5) 146.7 1_545 N4 H4A O7 0.90 2.62 3.227(6) 125.4 . N4 H4A O2 0.90 2.03 2.728(5) 133.2 1_556 N2 H2A O1W 0.86 2.03 2.864(4) 163.2 . N1 H1A O3 0.86 2.09 2.902(4) 157.0 2_665 O3W H3C O9 0.85 2.01 2.683(3) 134.9 1_545 O3W H3B O11 0.85 1.93 2.769(6) 168.8 1_545 O2W H2C O3W 0.85 1.84 2.682 171.2 . O2W H2B O1 0.85 2.11 2.942(3) 166.2 1_556 O1W H1C O2W 0.85 2.10 2.939(6) 167.4 2_766 O1W H1B O2W 0.85 1.94 2.771 165.4 1_554 _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.484 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.076 _database_code_depnum_ccdc_archive 'CCDC 964932'