# Electronic Supplementary Material (ESI) for CrystEngComm # 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 _database_code_depnum_ccdc_archive 'CCDC 904151' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H52 N18 O9 Zn2' _chemical_formula_weight 1203.86 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7033(16) _cell_length_b 11.880(4) _cell_length_c 12.457(6) _cell_angle_alpha 115.528(6) _cell_angle_beta 106.801(5) _cell_angle_gamma 91.358(4) _cell_volume 1348.0(8) _cell_formula_units_Z 1 _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 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 622 _exptl_absorpt_coefficient_mu 0.964 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8087 _exptl_absorpt_correction_T_max 0.8610 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9431 _diffrn_reflns_av_R_equivalents 0.0763 _diffrn_reflns_av_sigmaI/netI 0.2744 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.37 _reflns_number_total 4913 _reflns_number_gt 1718 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The distance of O1W---H1A was refined isotropically with restraint of 0.82+-0.02 \%A. For N8 and N9 atoms, the anisotropic displacement ellipsoids were rather elongated which led us to use the SIMU restraint. ; _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^)+(0.0276P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4913 _refine_ls_number_parameters 373 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1829 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1075 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 0.826 _refine_ls_restrained_S_all 0.826 _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 0.31893(9) 0.45765(7) 0.60391(7) 0.0472(3) Uani 1 1 d . . . C1 C 0.5602(8) 0.3762(7) 0.6393(7) 0.0553(19) Uani 1 1 d . . . C2 C 0.7070(7) 0.3905(5) 0.7028(5) 0.0432(16) Uani 1 1 d . . . C3 C 0.7461(7) 0.3636(5) 0.8051(6) 0.0538(18) Uani 1 1 d . . . H3 H 0.6820 0.3387 0.8311 0.065 Uiso 1 1 calc R . . C4 C 0.8768(8) 0.3730(5) 0.8674(6) 0.0564(19) Uani 1 1 d . . . H4 H 0.9012 0.3573 0.9369 0.068 Uiso 1 1 calc R . . C5 C 0.9701(7) 0.4051(5) 0.8282(6) 0.0539(19) Uani 1 1 d . . . H5 H 1.0592 0.4093 0.8691 0.065 Uiso 1 1 calc R . . C6 C 0.9336(7) 0.4317(5) 0.7276(6) 0.0486(18) Uani 1 1 d . . . H6 H 0.9989 0.4547 0.7017 0.058 Uiso 1 1 calc R . . C7 C 0.8024(7) 0.4250(5) 0.6641(5) 0.0383(16) Uani 1 1 d . . . C8 C 0.7732(8) 0.4626(5) 0.5595(6) 0.0454(17) Uani 1 1 d . . . C9 C 0.2182(8) 0.1695(6) 0.4830(6) 0.0541(19) Uani 1 1 d . . . H9 H 0.3016 0.1465 0.4986 0.065 Uiso 1 1 calc R . . C10 C 0.0597(7) 0.2739(6) 0.4800(6) 0.0518(18) Uani 1 1 d . . . H10 H 0.0126 0.3407 0.4955 0.062 Uiso 1 1 calc R . . C11 C 0.0861(7) -0.0482(6) 0.3437(6) 0.070(2) Uani 1 1 d . . . H11A H 0.0247 -0.0852 0.3685 0.083 Uiso 1 1 calc R . . H11B H 0.1697 -0.0768 0.3650 0.083 Uiso 1 1 calc R . . C12 C 0.0327(8) -0.0953(5) 0.2029(6) 0.0518(18) Uani 1 1 d . . . C13 C 0.1233(7) -0.0899(5) 0.1428(6) 0.0480(17) Uani 1 1 d . . . C14 C 0.0746(7) -0.1367(5) 0.0110(7) 0.0491(18) Uani 1 1 d . . . C15 C -0.0592(7) -0.1916(5) -0.0600(6) 0.0488(17) Uani 1 1 d . . . C16 C -0.1434(7) -0.2000(6) 0.0040(8) 0.0582(19) Uani 1 1 d . . . C17 C -0.1006(8) -0.1480(6) 0.1354(8) 0.0548(18) Uani 1 1 d . . . C18 C -0.1954(7) -0.1486(6) 0.2048(7) 0.094(3) Uani 1 1 d . . . H18A H -0.1484 -0.1092 0.2939 0.141 Uiso 1 1 calc R . . H18B H -0.2337 -0.2343 0.1775 0.141 Uiso 1 1 calc R . . H18C H -0.2645 -0.1026 0.1871 0.141 Uiso 1 1 calc R . . C19 C 0.2681(6) -0.0414(5) 0.2134(5) 0.0579(19) Uani 1 1 d . . . H19A H 0.3133 -0.0464 0.1556 0.087 Uiso 1 1 calc R . . H19B H 0.3031 -0.0918 0.2542 0.087 Uiso 1 1 calc R . . H19C H 0.2806 0.0451 0.2756 0.087 Uiso 1 1 calc R . . C20 C -0.1073(6) -0.2396(5) -0.1984(6) 0.068(2) Uani 1 1 d . . . H20A H -0.2002 -0.2733 -0.2312 0.102 Uiso 1 1 calc R . . H20B H -0.0599 -0.3050 -0.2358 0.102 Uiso 1 1 calc R . . H20C H -0.0931 -0.1715 -0.2180 0.102 Uiso 1 1 calc R . . C21 C 0.1677(6) -0.1303(5) -0.0592(5) 0.0535(18) Uani 1 1 d . . . H21A H 0.1212 -0.1091 -0.1256 0.064 Uiso 1 1 calc R . . H21B H 0.2423 -0.0626 -0.0012 0.064 Uiso 1 1 calc R . . C22 C 0.2163(6) -0.3158(6) -0.2309(5) 0.0472(17) Uani 1 1 d . . . H22 H 0.1753 -0.2981 -0.2972 0.057 Uiso 1 1 calc R . . C23 C 0.3207(7) -0.3955(6) -0.1243(6) 0.069(2) Uani 1 1 d . . . H23 H 0.3700 -0.4499 -0.1014 0.082 Uiso 1 1 calc R . . C24 C -0.2823(10) -0.2771(8) -0.0759(8) 0.113(3) Uani 1 1 d . . . H24A H -0.3161 -0.3021 -0.0237 0.135 Uiso 1 1 calc R . . H24B H -0.2736 -0.3540 -0.1437 0.135 Uiso 1 1 calc R . . C25 C -0.4536(9) -0.2607(9) -0.2670(11) 0.087(3) Uani 1 1 d . . . H25 H -0.4374 -0.3279 -0.3329 0.105 Uiso 1 1 calc R . . C26 C -0.5287(12) -0.0974(15) -0.1506(19) 0.188(9) Uani 1 1 d . . . H26 H -0.5795 -0.0339 -0.1300 0.226 Uiso 1 1 calc R . . N1 N 0.1067(7) 0.0903(5) 0.4157(5) 0.0506(15) Uani 1 1 d . . . N2 N 0.0036(6) 0.1542(6) 0.4110(5) 0.0619(16) Uani 1 1 d . . . N3 N 0.1951(6) 0.2893(4) 0.5266(4) 0.0491(14) Uani 1 1 d . . . N4 N 0.2179(5) -0.2477(4) -0.1150(5) 0.0486(14) Uani 1 1 d . . . N5 N 0.2880(7) -0.2988(6) -0.0435(5) 0.082(2) Uani 1 1 d . . . N6 N 0.2786(5) -0.4113(4) -0.2429(5) 0.0452(13) Uani 1 1 d . . . N7 N -0.3878(9) -0.2162(10) -0.1353(11) 0.127(3) Uani 1 1 d . . . N8 N -0.4313(12) -0.1124(10) -0.0586(11) 0.162(4) Uani 1 1 d . . . N9 N -0.5466(15) -0.1832(15) -0.2766(11) 0.219(8) Uani 1 1 d . . . O1 O 0.5014(4) 0.2821(4) 0.5372(4) 0.0704(14) Uani 1 1 d . . . O2 O 0.5027(4) 0.4632(4) 0.6997(4) 0.0621(13) Uani 1 1 d . . . O3 O 0.6619(5) 0.4938(4) 0.5267(4) 0.0536(12) Uani 1 1 d . . . O4 O 0.8593(5) 0.4662(4) 0.5133(4) 0.0616(13) Uani 1 1 d . . . O1W O 0.6210(9) 0.0589(8) 0.4577(8) 0.072(3) Uani 0.50 1 d PD . . H1A H 0.570(6) 0.034(7) 0.486(7) 0.108 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0558(6) 0.0510(5) 0.0431(5) 0.0230(4) 0.0244(4) 0.0233(4) C1 0.080(7) 0.060(5) 0.050(5) 0.034(4) 0.040(5) 0.031(5) C2 0.044(5) 0.048(4) 0.040(4) 0.022(3) 0.014(4) 0.022(3) C3 0.065(6) 0.056(4) 0.052(4) 0.034(4) 0.019(4) 0.020(4) C4 0.067(6) 0.047(4) 0.050(5) 0.029(4) 0.001(4) 0.020(4) C5 0.050(5) 0.049(4) 0.060(5) 0.030(4) 0.005(4) 0.016(4) C6 0.049(5) 0.035(4) 0.062(5) 0.019(3) 0.022(4) 0.014(3) C7 0.038(4) 0.034(4) 0.045(4) 0.016(3) 0.019(4) 0.010(3) C8 0.054(5) 0.044(4) 0.040(4) 0.017(3) 0.020(4) 0.029(4) C9 0.077(6) 0.042(4) 0.055(5) 0.021(4) 0.039(4) 0.035(4) C10 0.058(6) 0.049(5) 0.053(4) 0.018(4) 0.031(4) 0.029(4) C11 0.112(6) 0.051(5) 0.068(5) 0.030(4) 0.056(5) 0.031(4) C12 0.088(6) 0.024(4) 0.052(5) 0.014(3) 0.042(5) 0.023(4) C13 0.061(5) 0.025(4) 0.054(5) 0.009(3) 0.027(4) 0.013(3) C14 0.062(5) 0.022(3) 0.067(5) 0.011(3) 0.042(4) 0.018(3) C15 0.069(6) 0.032(4) 0.058(5) 0.021(3) 0.036(4) 0.025(4) C16 0.051(5) 0.038(4) 0.077(6) 0.020(4) 0.019(5) 0.002(4) C17 0.059(5) 0.040(4) 0.088(6) 0.033(4) 0.048(5) 0.021(4) C18 0.106(7) 0.076(5) 0.124(6) 0.036(5) 0.086(6) 0.024(5) C19 0.064(5) 0.050(4) 0.059(4) 0.016(3) 0.031(4) 0.017(4) C20 0.083(6) 0.050(4) 0.064(5) 0.021(4) 0.023(4) 0.024(4) C21 0.071(5) 0.036(4) 0.056(4) 0.014(3) 0.036(4) 0.019(4) C22 0.062(5) 0.043(4) 0.028(4) 0.011(3) 0.010(3) 0.019(4) C23 0.112(7) 0.068(5) 0.041(5) 0.027(4) 0.041(5) 0.063(5) C24 0.123(9) 0.096(7) 0.136(8) 0.070(6) 0.039(7) 0.033(7) C25 0.048(7) 0.116(8) 0.096(8) 0.059(7) 0.003(6) 0.026(5) C26 0.034(7) 0.29(2) 0.34(2) 0.26(2) 0.013(11) 0.029(10) N1 0.068(5) 0.041(4) 0.046(4) 0.016(3) 0.030(3) 0.013(4) N2 0.069(5) 0.052(4) 0.062(4) 0.019(3) 0.029(4) 0.024(4) N3 0.062(4) 0.044(4) 0.048(3) 0.018(3) 0.030(3) 0.022(3) N4 0.075(4) 0.040(3) 0.037(3) 0.014(3) 0.031(3) 0.025(3) N5 0.126(6) 0.081(5) 0.065(5) 0.043(4) 0.053(4) 0.052(4) N6 0.060(4) 0.038(3) 0.045(4) 0.017(3) 0.030(3) 0.029(3) N7 0.114(8) 0.121(8) 0.154(10) 0.085(7) 0.020(8) 0.001(7) N8 0.141(10) 0.104(7) 0.251(13) 0.062(8) 0.109(11) 0.033(7) N9 0.187(15) 0.283(17) 0.154(10) 0.112(12) 0.003(11) -0.085(12) O1 0.065(4) 0.061(3) 0.072(3) 0.023(3) 0.018(3) 0.018(3) O2 0.059(3) 0.084(3) 0.051(3) 0.035(3) 0.021(3) 0.032(3) O3 0.053(3) 0.072(3) 0.054(3) 0.043(2) 0.022(3) 0.023(3) O4 0.072(4) 0.075(3) 0.062(3) 0.038(3) 0.043(3) 0.034(3) O1W 0.064(8) 0.063(6) 0.057(6) 0.012(5) -0.004(5) 0.056(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 O2 1.966(4) . ? Zn1 O3 2.005(4) 2_666 ? Zn1 N3 2.040(5) . ? Zn1 N6 2.049(5) 1_566 ? Zn1 O4 2.490(4) 2_666 ? Zn1 C8 2.561(6) 2_666 ? C1 O1 1.242(7) . ? C1 O2 1.281(7) . ? C1 C2 1.509(9) . ? C2 C7 1.370(7) . ? C2 C3 1.396(7) . ? C3 C4 1.364(8) . ? C3 H3 0.9300 . ? C4 C5 1.343(8) . ? C4 H4 0.9300 . ? C5 C6 1.373(7) . ? C5 H5 0.9300 . ? C6 C7 1.380(7) . ? C6 H6 0.9300 . ? C7 C8 1.506(8) . ? C8 O4 1.228(6) . ? C8 O3 1.262(7) . ? C8 Zn1 2.561(6) 2_666 ? C9 N1 1.304(7) . ? C9 N3 1.346(6) . ? C9 H9 0.9300 . ? C10 N2 1.315(7) . ? C10 N3 1.371(7) . ? C10 H10 0.9300 . ? C11 N1 1.468(7) . ? C11 C12 1.509(8) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C17 1.394(8) . ? C12 C13 1.402(8) . ? C13 C14 1.407(8) . ? C13 C19 1.497(8) . ? C14 C15 1.409(8) . ? C14 C21 1.524(7) . ? C15 C16 1.392(8) . ? C15 C20 1.479(7) . ? C16 C17 1.397(8) . ? C16 C24 1.528(9) . ? C17 C18 1.513(7) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 N4 1.460(7) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 N6 1.304(7) . ? C22 N4 1.310(6) . ? C22 H22 0.9300 . ? C23 N5 1.296(7) . ? C23 N6 1.339(7) . ? C23 H23 0.9300 . ? C24 N7 1.537(10) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 N9 1.387(18) . ? C25 N7 1.426(11) . ? C25 H25 0.9300 . ? C26 N8 1.387(14) . ? C26 N9 1.406(18) . ? C26 H26 0.9300 . ? N1 N2 1.355(7) . ? N4 N5 1.352(7) . ? N6 Zn1 2.049(5) 1_544 ? N7 N8 1.385(11) . ? O3 Zn1 2.005(4) 2_666 ? O4 Zn1 2.490(4) 2_666 ? O1W H1A 0.840(19) . ? 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 Zn1 O3 103.53(18) . 2_666 ? O2 Zn1 N3 115.6(2) . . ? O3 Zn1 N3 112.45(17) 2_666 . ? O2 Zn1 N6 94.7(2) . 1_566 ? O3 Zn1 N6 119.07(19) 2_666 1_566 ? N3 Zn1 N6 110.25(18) . 1_566 ? O2 Zn1 O4 154.25(15) . 2_666 ? O3 Zn1 O4 57.06(16) 2_666 2_666 ? N3 Zn1 O4 88.98(19) . 2_666 ? N6 Zn1 O4 82.89(18) 1_566 2_666 ? O2 Zn1 C8 130.6(2) . 2_666 ? O3 Zn1 C8 28.96(18) 2_666 2_666 ? N3 Zn1 C8 101.7(2) . 2_666 ? N6 Zn1 C8 101.7(2) 1_566 2_666 ? O4 Zn1 C8 28.10(15) 2_666 2_666 ? O1 C1 O2 123.9(8) . . ? O1 C1 C2 120.3(7) . . ? O2 C1 C2 115.8(6) . . ? C7 C2 C3 118.9(6) . . ? C7 C2 C1 123.9(6) . . ? C3 C2 C1 117.2(6) . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C5 C4 C3 120.0(6) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C4 C5 C6 119.7(7) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C5 C6 C7 121.6(6) . . ? C5 C6 H6 119.2 . . ? C7 C6 H6 119.2 . . ? C2 C7 C6 118.7(6) . . ? C2 C7 C8 123.8(6) . . ? C6 C7 C8 117.4(6) . . ? O4 C8 O3 123.0(6) . . ? O4 C8 C7 119.2(7) . . ? O3 C8 C7 117.8(6) . . ? O4 C8 Zn1 72.7(4) . 2_666 ? O3 C8 Zn1 50.3(3) . 2_666 ? C7 C8 Zn1 167.8(5) . 2_666 ? N1 C9 N3 110.1(6) . . ? N1 C9 H9 125.0 . . ? N3 C9 H9 125.0 . . ? N2 C10 N3 112.6(6) . . ? N2 C10 H10 123.7 . . ? N3 C10 H10 123.7 . . ? N1 C11 C12 113.3(5) . . ? N1 C11 H11A 108.9 . . ? C12 C11 H11A 108.9 . . ? N1 C11 H11B 108.9 . . ? C12 C11 H11B 108.9 . . ? H11A C11 H11B 107.7 . . ? C17 C12 C13 121.8(6) . . ? C17 C12 C11 120.7(6) . . ? C13 C12 C11 117.4(7) . . ? C12 C13 C14 117.7(6) . . ? C12 C13 C19 122.1(6) . . ? C14 C13 C19 120.1(6) . . ? C13 C14 C15 121.9(6) . . ? C13 C14 C21 120.1(6) . . ? C15 C14 C21 118.0(6) . . ? C16 C15 C14 117.9(6) . . ? C16 C15 C20 121.5(7) . . ? C14 C15 C20 120.6(6) . . ? C15 C16 C17 121.8(6) . . ? C15 C16 C24 117.1(7) . . ? C17 C16 C24 121.0(7) . . ? C12 C17 C16 118.7(6) . . ? C12 C17 C18 119.9(7) . . ? C16 C17 C18 121.4(7) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C13 C19 H19A 109.5 . . ? C13 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C13 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C15 C20 H20A 109.5 . . ? C15 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C15 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N4 C21 C14 113.9(4) . . ? N4 C21 H21A 108.8 . . ? C14 C21 H21A 108.8 . . ? N4 C21 H21B 108.8 . . ? C14 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N6 C22 N4 112.5(5) . . ? N6 C22 H22 123.7 . . ? N4 C22 H22 123.7 . . ? N5 C23 N6 115.2(6) . . ? N5 C23 H23 122.4 . . ? N6 C23 H23 122.4 . . ? C16 C24 N7 118.7(6) . . ? C16 C24 H24A 107.6 . . ? N7 C24 H24A 107.6 . . ? C16 C24 H24B 107.6 . . ? N7 C24 H24B 107.6 . . ? H24A C24 H24B 107.1 . . ? N9 C25 N7 105.9(11) . . ? N9 C25 H25 127.1 . . ? N7 C25 H25 127.1 . . ? N8 C26 N9 116.6(16) . . ? N8 C26 H26 121.7 . . ? N9 C26 H26 121.7 . . ? C9 N1 N2 110.2(5) . . ? C9 N1 C11 128.5(7) . . ? N2 N1 C11 121.2(6) . . ? C10 N2 N1 104.1(5) . . ? C9 N3 C10 103.0(5) . . ? C9 N3 Zn1 131.3(5) . . ? C10 N3 Zn1 124.2(5) . . ? C22 N4 N5 107.8(5) . . ? C22 N4 C21 130.5(6) . . ? N5 N4 C21 121.4(5) . . ? C23 N5 N4 103.0(5) . . ? C22 N6 C23 101.4(5) . . ? C22 N6 Zn1 130.3(4) . 1_544 ? C23 N6 Zn1 128.1(5) . 1_544 ? N8 N7 C25 114.3(10) . . ? N8 N7 C24 119.9(12) . . ? C25 N7 C24 125.7(11) . . ? N7 N8 C26 99.4(12) . . ? C25 N9 C26 103.9(13) . . ? C1 O2 Zn1 114.9(5) . . ? C8 O3 Zn1 100.8(4) . 2_666 ? C8 O4 Zn1 79.2(4) . 2_666 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 75.6(8) . . . . ? O2 C1 C2 C7 -107.2(6) . . . . ? O1 C1 C2 C3 -102.8(7) . . . . ? O2 C1 C2 C3 74.5(7) . . . . ? C7 C2 C3 C4 1.0(9) . . . . ? C1 C2 C3 C4 179.5(6) . . . . ? C2 C3 C4 C5 -2.0(9) . . . . ? C3 C4 C5 C6 1.8(9) . . . . ? C4 C5 C6 C7 -0.7(9) . . . . ? C3 C2 C7 C6 0.1(8) . . . . ? C1 C2 C7 C6 -178.3(6) . . . . ? C3 C2 C7 C8 -176.8(5) . . . . ? C1 C2 C7 C8 4.8(9) . . . . ? C5 C6 C7 C2 -0.3(9) . . . . ? C5 C6 C7 C8 176.9(5) . . . . ? C2 C7 C8 O4 -164.8(5) . . . . ? C6 C7 C8 O4 18.2(8) . . . . ? C2 C7 C8 O3 17.8(8) . . . . ? C6 C7 C8 O3 -159.1(5) . . . . ? C2 C7 C8 Zn1 29(2) . . . 2_666 ? C6 C7 C8 Zn1 -148.0(17) . . . 2_666 ? N1 C11 C12 C17 -103.0(7) . . . . ? N1 C11 C12 C13 80.1(8) . . . . ? C17 C12 C13 C14 1.6(9) . . . . ? C11 C12 C13 C14 178.4(5) . . . . ? C17 C12 C13 C19 -175.9(6) . . . . ? C11 C12 C13 C19 0.9(8) . . . . ? C12 C13 C14 C15 -2.3(8) . . . . ? C19 C13 C14 C15 175.3(5) . . . . ? C12 C13 C14 C21 178.5(5) . . . . ? C19 C13 C14 C21 -4.0(8) . . . . ? C13 C14 C15 C16 -0.7(8) . . . . ? C21 C14 C15 C16 178.6(5) . . . . ? C13 C14 C15 C20 179.8(5) . . . . ? C21 C14 C15 C20 -0.9(8) . . . . ? C14 C15 C16 C17 4.5(9) . . . . ? C20 C15 C16 C17 -176.0(6) . . . . ? C14 C15 C16 C24 -171.1(6) . . . . ? C20 C15 C16 C24 8.4(9) . . . . ? C13 C12 C17 C16 2.0(9) . . . . ? C11 C12 C17 C16 -174.7(6) . . . . ? C13 C12 C17 C18 -178.4(5) . . . . ? C11 C12 C17 C18 5.0(9) . . . . ? C15 C16 C17 C12 -5.2(9) . . . . ? C24 C16 C17 C12 170.3(6) . . . . ? C15 C16 C17 C18 175.2(6) . . . . ? C24 C16 C17 C18 -9.4(10) . . . . ? C13 C14 C21 N4 97.3(6) . . . . ? C15 C14 C21 N4 -82.0(7) . . . . ? C15 C16 C24 N7 -79.3(10) . . . . ? C17 C16 C24 N7 105.1(9) . . . . ? N3 C9 N1 N2 0.2(7) . . . . ? N3 C9 N1 C11 175.5(5) . . . . ? C12 C11 N1 C9 -111.1(7) . . . . ? C12 C11 N1 N2 63.7(8) . . . . ? N3 C10 N2 N1 1.3(7) . . . . ? C9 N1 N2 C10 -0.9(6) . . . . ? C11 N1 N2 C10 -176.6(5) . . . . ? N1 C9 N3 C10 0.5(6) . . . . ? N1 C9 N3 Zn1 -165.2(4) . . . . ? N2 C10 N3 C9 -1.2(7) . . . . ? N2 C10 N3 Zn1 165.9(4) . . . . ? O2 Zn1 N3 C9 -31.1(5) . . . . ? O3 Zn1 N3 C9 87.5(5) 2_666 . . . ? N6 Zn1 N3 C9 -137.0(5) 1_566 . . . ? O4 Zn1 N3 C9 140.9(5) 2_666 . . . ? C8 Zn1 N3 C9 115.7(5) 2_666 . . . ? O2 Zn1 N3 C10 165.7(4) . . . . ? O3 Zn1 N3 C10 -75.7(5) 2_666 . . . ? N6 Zn1 N3 C10 59.8(5) 1_566 . . . ? O4 Zn1 N3 C10 -22.2(4) 2_666 . . . ? C8 Zn1 N3 C10 -47.5(5) 2_666 . . . ? N6 C22 N4 N5 1.3(7) . . . . ? N6 C22 N4 C21 176.0(5) . . . . ? C14 C21 N4 C22 126.8(6) . . . . ? C14 C21 N4 N5 -59.1(8) . . . . ? N6 C23 N5 N4 0.5(8) . . . . ? C22 N4 N5 C23 -1.0(7) . . . . ? C21 N4 N5 C23 -176.3(5) . . . . ? N4 C22 N6 C23 -0.9(7) . . . . ? N4 C22 N6 Zn1 -175.6(4) . . . 1_544 ? N5 C23 N6 C22 0.3(8) . . . . ? N5 C23 N6 Zn1 175.1(5) . . . 1_544 ? N9 C25 N7 N8 -1.2(12) . . . . ? N9 C25 N7 C24 175.7(9) . . . . ? C16 C24 N7 N8 -65.0(11) . . . . ? C16 C24 N7 C25 118.4(9) . . . . ? C25 N7 N8 C26 1.0(10) . . . . ? C24 N7 N8 C26 -176.0(7) . . . . ? N9 C26 N8 N7 -0.6(13) . . . . ? N7 C25 N9 C26 0.7(14) . . . . ? N8 C26 N9 C25 -0.1(16) . . . . ? O1 C1 O2 Zn1 -12.2(7) . . . . ? C2 C1 O2 Zn1 170.6(4) . . . . ? O3 Zn1 O2 C1 -69.3(4) 2_666 . . . ? N3 Zn1 O2 C1 54.1(4) . . . . ? N6 Zn1 O2 C1 169.3(4) 1_566 . . . ? O4 Zn1 O2 C1 -107.3(5) 2_666 . . . ? C8 Zn1 O2 C1 -80.9(5) 2_666 . . . ? O4 C8 O3 Zn1 -0.3(7) . . . 2_666 ? C7 C8 O3 Zn1 177.0(4) . . . 2_666 ? O3 C8 O4 Zn1 0.2(6) . . . 2_666 ? C7 C8 O4 Zn1 -177.0(5) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.37 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.456 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.069 data_2 _database_code_depnum_ccdc_archive 'CCDC 904152' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H62 Cd2 N18 O14' _chemical_formula_weight 1388.00 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 20.4940(7) _cell_length_b 13.4394(5) _cell_length_c 23.0775(7) _cell_angle_alpha 90.00 _cell_angle_beta 93.709(3) _cell_angle_gamma 90.00 _cell_volume 6342.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.453 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2832 _exptl_absorpt_coefficient_mu 0.744 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8243 _exptl_absorpt_correction_T_max 0.8715 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12011 _diffrn_reflns_av_R_equivalents 0.0362 _diffrn_reflns_av_sigmaI/netI 0.0988 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5729 _reflns_number_gt 3333 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0929P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5729 _refine_ls_number_parameters 402 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0878 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1752 _refine_ls_wR_factor_gt 0.1675 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.019 _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 Cd1 Cd 0.78897(3) -0.26428(4) 0.76783(2) 0.0372(2) Uani 1 1 d . . . C1 C 0.8620(4) -0.4625(6) 0.7144(5) 0.066(3) Uani 1 1 d . . . C2 C 0.8774(4) -0.5095(5) 0.6576(4) 0.058(2) Uani 1 1 d . . . C3 C 0.9268(5) -0.4655(7) 0.6267(6) 0.086(3) Uani 1 1 d . . . H3 H 0.9479 -0.4085 0.6411 0.103 Uiso 1 1 calc R . . C4 C 0.9441(6) -0.5067(9) 0.5755(6) 0.099(4) Uani 1 1 d . . . H4 H 0.9771 -0.4775 0.5556 0.119 Uiso 1 1 calc R . . C5 C 0.9130(6) -0.5914(9) 0.5529(5) 0.094(4) Uani 1 1 d . . . H5 H 0.9253 -0.6190 0.5183 0.113 Uiso 1 1 calc R . . C6 C 0.8633(5) -0.6342(7) 0.5826(4) 0.069(3) Uani 1 1 d . . . H6 H 0.8423 -0.6907 0.5675 0.082 Uiso 1 1 calc R . . C7 C 0.8442(4) -0.5942(5) 0.6348(3) 0.0464(19) Uani 1 1 d . . . C8 C 0.7913(3) -0.6440(5) 0.6666(3) 0.0364(17) Uani 1 1 d . . . C9 C 0.8746(5) -0.1788(7) 0.6603(5) 0.084(3) Uani 1 1 d . . . H9 H 0.8950 -0.2403 0.6578 0.100 Uiso 1 1 calc R . . C10 C 0.8158(4) -0.0671(6) 0.6884(3) 0.047(2) Uani 1 1 d . . . H10 H 0.7859 -0.0300 0.7080 0.057 Uiso 1 1 calc R . . C11 C 0.8389(4) 0.0614(5) 0.6127(3) 0.0447(19) Uani 1 1 d . . . H11A H 0.8253 0.1118 0.6395 0.054 Uiso 1 1 calc R . . H11B H 0.8043 0.0539 0.5824 0.054 Uiso 1 1 calc R . . C12 C 0.9002(3) 0.0971(5) 0.5856(3) 0.0343(16) Uani 1 1 d . . . C13 C 0.9465(4) 0.1494(5) 0.6198(3) 0.0366(16) Uani 1 1 d . . . C14 C 0.9400(4) 0.1600(7) 0.6836(3) 0.062(2) Uani 1 1 d . . . H14A H 0.9101 0.2130 0.6905 0.092 Uiso 1 1 calc R . . H14B H 0.9819 0.1748 0.7026 0.092 Uiso 1 1 calc R . . H14C H 0.9237 0.0989 0.6988 0.092 Uiso 1 1 calc R . . C15 C 0.9994(3) 0.1929(5) 0.5934(3) 0.0376(16) Uani 1 1 d . . . C16 C 1.0083(3) 0.1771(5) 0.5348(3) 0.0345(16) Uani 1 1 d . . . C17 C 0.9629(3) 0.1195(4) 0.5012(3) 0.0303(15) Uani 1 1 d . . . C18 C 0.9076(3) 0.0821(5) 0.5270(3) 0.0331(16) Uani 1 1 d . . . C19 C 0.8554(4) 0.0267(5) 0.4901(3) 0.0480(19) Uani 1 1 d . . . H19A H 0.8204 0.0715 0.4785 0.072 Uiso 1 1 calc R . . H19B H 0.8386 -0.0270 0.5122 0.072 Uiso 1 1 calc R . . H19C H 0.8740 0.0005 0.4561 0.072 Uiso 1 1 calc R . . C20 C 1.0660(4) 0.2245(6) 0.5080(3) 0.052(2) Uani 1 1 d . . . H20A H 1.0559 0.2924 0.4982 0.079 Uiso 1 1 calc R . . H20B H 1.0755 0.1887 0.4735 0.079 Uiso 1 1 calc R . . H20C H 1.1034 0.2224 0.5353 0.079 Uiso 1 1 calc R . . C21 C 1.0439(4) 0.2648(5) 0.6280(3) 0.0464(18) Uani 1 1 d . . . H21A H 1.0580 0.3159 0.6018 0.056 Uiso 1 1 calc R . . H21B H 1.0188 0.2972 0.6568 0.056 Uiso 1 1 calc R . . C22 C 1.1782(4) 0.1185(6) 0.6799(3) 0.053(2) Uani 1 1 d . . . H22 H 1.2043 0.0618 0.6815 0.063 Uiso 1 1 calc R . . C23 C 1.1433(3) 0.2602(5) 0.6958(3) 0.0388(17) Uani 1 1 d . . . H23 H 1.1382 0.3239 0.7106 0.047 Uiso 1 1 calc R . . C24 C 0.9741(3) 0.0969(5) 0.4391(3) 0.0363(16) Uani 1 1 d . . . H24A H 1.0208 0.0965 0.4344 0.044 Uiso 1 1 calc R . . H24B H 0.9575 0.0308 0.4299 0.044 Uiso 1 1 calc R . . C25 C 0.8924(4) 0.1557(6) 0.3595(3) 0.048(2) Uani 1 1 d . . . H25 H 0.8689 0.0969 0.3544 0.058 Uiso 1 1 calc R . . C26 C 0.9248(5) 0.3001(7) 0.3523(4) 0.074(3) Uani 1 1 d . . . H26 H 0.9276 0.3657 0.3398 0.089 Uiso 1 1 calc R . . N1 N 0.8318(3) -0.1589(4) 0.7012(3) 0.0440(15) Uani 1 1 d . . . N2 N 0.8853(4) -0.1061(6) 0.6248(4) 0.084(3) Uani 1 1 d . . . N3 N 0.8472(3) -0.0332(4) 0.6440(3) 0.0431(15) Uani 1 1 d . . . N4 N 1.1927(3) 0.2012(4) 0.7111(2) 0.0401(14) Uani 1 1 d . . . N5 N 1.1232(4) 0.1257(5) 0.6469(3) 0.063(2) Uani 1 1 d . . . N6 N 1.1027(3) 0.2193(4) 0.6579(2) 0.0375(13) Uani 1 1 d . . . N7 N 0.9431(3) 0.1674(4) 0.3980(2) 0.0362(13) Uani 1 1 d . . . N8 N 0.9656(4) 0.2621(5) 0.3940(4) 0.078(3) Uani 1 1 d . . . N9 N 0.8798(3) 0.2367(4) 0.3300(3) 0.0461(15) Uani 1 1 d . . . O1 O 0.8296(3) -0.3835(4) 0.7096(3) 0.080(2) Uani 1 1 d . . . O2 O 0.8853(3) -0.5017(5) 0.7608(3) 0.0768(18) Uani 1 1 d . . . O3 O 0.7641(3) -0.5988(4) 0.7051(2) 0.0608(16) Uani 1 1 d . . . O4 O 0.7770(3) -0.7329(4) 0.6537(2) 0.0510(13) Uani 1 1 d . . . O1W O 0.8031(5) -0.4351(8) 0.8313(8) 0.261(9) Uani 1 1 d . . . O2W O 1.0000 -0.6194(6) 0.7500 0.064(2) Uani 1 2 d SD . . H2A H 0.967(3) -0.578(6) 0.750(5) 0.096 Uiso 1 1 d D . . O3W O 0.7142(5) -0.7890(8) 0.5470(4) 0.123(3) Uani 1 1 d D . . H3A H 0.713(9) -0.758(10) 0.580(3) 0.185 Uiso 1 1 d D . . O4W O 1.2662(9) 0.2047(15) 0.5222(10) 0.174(8) Uani 0.50 1 d PDU . . H4A H 1.2500 0.2500 0.5000 0.260 Uiso 1 2 d SD . . 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 Cd1 0.0313(3) 0.0469(3) 0.0330(3) -0.0056(2) -0.0007(2) -0.0062(3) C1 0.046(5) 0.042(5) 0.109(9) -0.013(5) -0.012(5) -0.004(4) C2 0.054(6) 0.034(4) 0.089(7) 0.004(4) 0.011(5) -0.003(4) C3 0.057(7) 0.053(6) 0.150(11) 0.010(6) 0.031(7) -0.004(5) C4 0.085(9) 0.083(8) 0.134(11) 0.034(8) 0.046(8) -0.002(7) C5 0.097(9) 0.105(9) 0.086(8) 0.028(7) 0.047(7) 0.012(7) C6 0.079(7) 0.073(6) 0.056(6) 0.012(5) 0.019(5) 0.004(5) C7 0.046(5) 0.042(4) 0.051(5) 0.004(3) 0.004(4) 0.010(4) C8 0.038(4) 0.034(4) 0.036(4) 0.006(3) -0.001(3) -0.003(3) C9 0.103(8) 0.048(5) 0.106(8) 0.025(5) 0.060(7) 0.024(5) C10 0.052(5) 0.049(5) 0.044(5) 0.003(4) 0.021(4) 0.002(4) C11 0.044(5) 0.042(4) 0.049(5) 0.007(3) 0.010(4) 0.006(3) C12 0.032(4) 0.034(4) 0.037(4) 0.005(3) 0.003(3) 0.004(3) C13 0.041(4) 0.037(4) 0.032(4) 0.002(3) 0.004(3) 0.010(3) C14 0.062(6) 0.087(6) 0.035(5) -0.008(4) 0.002(4) -0.002(5) C15 0.034(4) 0.036(4) 0.041(4) -0.001(3) -0.013(3) 0.004(3) C16 0.028(4) 0.037(4) 0.037(4) 0.005(3) -0.003(3) 0.005(3) C17 0.029(4) 0.029(3) 0.032(4) 0.004(3) -0.003(3) 0.010(3) C18 0.025(4) 0.034(4) 0.039(4) 0.005(3) -0.006(3) -0.001(3) C19 0.049(5) 0.053(4) 0.041(4) -0.003(3) -0.006(4) -0.013(4) C20 0.039(4) 0.067(5) 0.052(5) 0.005(4) 0.002(4) -0.014(4) C21 0.039(4) 0.047(4) 0.052(5) -0.004(4) -0.012(3) 0.004(4) C22 0.048(5) 0.047(4) 0.060(5) -0.009(4) -0.019(4) 0.010(4) C23 0.037(4) 0.043(4) 0.036(4) -0.007(3) 0.001(3) -0.003(4) C24 0.034(4) 0.037(4) 0.038(4) 0.006(3) 0.000(3) 0.003(3) C25 0.056(5) 0.043(4) 0.045(5) 0.007(4) -0.011(4) -0.009(4) C26 0.071(7) 0.055(5) 0.091(7) 0.033(5) -0.032(6) -0.012(5) N1 0.052(4) 0.038(3) 0.044(4) 0.004(3) 0.017(3) 0.001(3) N2 0.101(7) 0.063(5) 0.094(6) 0.021(4) 0.061(5) 0.025(5) N3 0.046(4) 0.039(3) 0.046(4) 0.002(3) 0.017(3) 0.006(3) N4 0.028(3) 0.048(4) 0.042(3) -0.004(3) -0.008(3) -0.003(3) N5 0.060(5) 0.049(4) 0.076(5) -0.018(3) -0.027(4) 0.011(3) N6 0.032(3) 0.041(3) 0.038(3) -0.006(3) -0.005(3) -0.001(3) N7 0.036(3) 0.037(3) 0.035(3) 0.007(2) -0.003(3) -0.003(3) N8 0.072(5) 0.056(4) 0.099(6) 0.028(4) -0.044(5) -0.020(4) N9 0.042(4) 0.050(4) 0.044(4) 0.008(3) -0.014(3) -0.004(3) O1 0.082(5) 0.046(3) 0.109(5) -0.021(3) -0.010(4) 0.014(3) O2 0.072(5) 0.074(4) 0.082(5) -0.008(4) -0.009(4) 0.012(3) O3 0.065(4) 0.052(3) 0.069(4) -0.018(3) 0.029(3) -0.009(3) O4 0.059(4) 0.044(3) 0.051(3) -0.007(2) 0.010(3) -0.009(3) O1W 0.119(9) 0.138(9) 0.54(3) -0.176(12) 0.167(13) -0.068(7) O2W 0.062(6) 0.055(5) 0.075(6) 0.000 -0.002(5) 0.000 O3W 0.118(7) 0.151(8) 0.097(6) -0.029(6) -0.030(5) 0.010(6) O4W 0.099(9) 0.201(11) 0.221(12) 0.019(9) 0.015(8) -0.090(9) _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 Cd1 O1 2.283(6) . ? Cd1 N1 2.306(5) . ? Cd1 N9 2.306(6) 6_556 ? Cd1 N4 2.342(6) 3_445 ? Cd1 O4 2.367(5) 4_656 ? Cd1 O3 2.570(5) 4_656 ? C1 O1 1.253(10) . ? C1 O2 1.258(11) . ? C1 C2 1.508(13) . ? C2 C3 1.405(12) . ? C2 C7 1.410(11) . ? C3 C4 1.373(15) . ? C4 C5 1.389(16) . ? C5 C6 1.388(12) . ? C6 C7 1.398(11) . ? C7 C8 1.504(10) . ? C8 O3 1.238(8) . ? C8 O4 1.261(8) . ? C9 N2 1.303(11) . ? C9 N1 1.355(10) . ? C10 N1 1.306(9) . ? C10 N3 1.325(8) . ? C11 N3 1.466(9) . ? C11 C12 1.516(9) . ? C12 C13 1.385(10) . ? C12 C18 1.387(9) . ? C13 C15 1.404(10) . ? C13 C14 1.496(9) . ? C15 C16 1.394(9) . ? C15 C21 1.518(10) . ? C16 C17 1.404(9) . ? C16 C20 1.510(10) . ? C17 C18 1.405(9) . ? C17 C24 1.498(9) . ? C18 C19 1.520(9) . ? C21 N6 1.480(9) . ? C22 N5 1.322(10) . ? C22 N4 1.348(9) . ? C23 N6 1.292(9) . ? C23 N4 1.316(9) . ? C24 N7 1.456(8) . ? C25 N9 1.300(9) . ? C25 N7 1.332(9) . ? C26 N8 1.334(11) . ? C26 N9 1.335(11) . ? N2 N3 1.346(9) . ? N4 Cd1 2.342(6) 3 ? N5 N6 1.356(8) . ? N7 N8 1.358(8) . ? N9 Cd1 2.306(6) 6 ? O3 Cd1 2.570(5) 4_646 ? O4 Cd1 2.367(5) 4_646 ? O4W O4W 1.70(3) 7_756 ? 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 Cd1 N1 82.5(2) . . ? O1 Cd1 N9 99.7(2) . 6_556 ? N1 Cd1 N9 89.4(2) . 6_556 ? O1 Cd1 N4 81.8(2) . 3_445 ? N1 Cd1 N4 95.3(2) . 3_445 ? N9 Cd1 N4 175.2(2) 6_556 3_445 ? O1 Cd1 O4 145.5(2) . 4_656 ? N1 Cd1 O4 131.43(18) . 4_656 ? N9 Cd1 O4 88.4(2) 6_556 4_656 ? N4 Cd1 O4 87.8(2) 3_445 4_656 ? O1 Cd1 O3 157.9(2) . 4_656 ? N1 Cd1 O3 79.41(18) . 4_656 ? N9 Cd1 O3 92.7(2) 6_556 4_656 ? N4 Cd1 O3 87.3(2) 3_445 4_656 ? O4 Cd1 O3 52.26(16) 4_656 4_656 ? O1 C1 O2 126.9(10) . . ? O1 C1 C2 114.6(9) . . ? O2 C1 C2 118.3(8) . . ? C3 C2 C7 119.8(9) . . ? C3 C2 C1 117.6(8) . . ? C7 C2 C1 122.6(7) . . ? C4 C3 C2 120.1(10) . . ? C3 C4 C5 121.1(10) . . ? C6 C5 C4 119.2(10) . . ? C5 C6 C7 121.5(10) . . ? C6 C7 C2 118.4(8) . . ? C6 C7 C8 120.0(7) . . ? C2 C7 C8 121.6(7) . . ? O3 C8 O4 121.7(6) . . ? O3 C8 C7 120.2(6) . . ? O4 C8 C7 118.1(6) . . ? N2 C9 N1 115.6(7) . . ? N1 C10 N3 111.8(6) . . ? N3 C11 C12 113.8(6) . . ? C13 C12 C18 120.9(6) . . ? C13 C12 C11 118.8(6) . . ? C18 C12 C11 120.2(6) . . ? C12 C13 C15 119.1(6) . . ? C12 C13 C14 120.4(6) . . ? C15 C13 C14 120.5(7) . . ? C16 C15 C13 120.6(6) . . ? C16 C15 C21 119.7(6) . . ? C13 C15 C21 119.5(6) . . ? C15 C16 C17 119.7(6) . . ? C15 C16 C20 119.2(6) . . ? C17 C16 C20 121.1(6) . . ? C16 C17 C18 119.2(6) . . ? C16 C17 C24 120.1(6) . . ? C18 C17 C24 120.7(6) . . ? C12 C18 C17 120.2(6) . . ? C12 C18 C19 120.0(6) . . ? C17 C18 C19 119.8(6) . . ? N6 C21 C15 115.1(6) . . ? N5 C22 N4 113.5(7) . . ? N6 C23 N4 112.1(6) . . ? N7 C24 C17 113.8(5) . . ? N9 C25 N7 111.8(6) . . ? N8 C26 N9 114.7(7) . . ? C10 N1 C9 101.2(6) . . ? C10 N1 Cd1 129.1(5) . . ? C9 N1 Cd1 129.3(5) . . ? C9 N2 N3 102.4(6) . . ? C10 N3 N2 109.0(6) . . ? C10 N3 C11 129.2(6) . . ? N2 N3 C11 121.4(6) . . ? C23 N4 C22 102.4(6) . . ? C23 N4 Cd1 129.5(5) . 3 ? C22 N4 Cd1 127.7(5) . 3 ? C22 N5 N6 102.9(6) . . ? C23 N6 N5 109.1(6) . . ? C23 N6 C21 127.5(6) . . ? N5 N6 C21 123.4(6) . . ? C25 N7 N8 108.5(6) . . ? C25 N7 C24 130.2(6) . . ? N8 N7 C24 121.3(6) . . ? C26 N8 N7 102.1(7) . . ? C25 N9 C26 102.9(7) . . ? C25 N9 Cd1 125.9(5) . 6 ? C26 N9 Cd1 130.3(5) . 6 ? C1 O1 Cd1 138.9(7) . . ? C8 O3 Cd1 88.1(4) . 4_646 ? C8 O4 Cd1 97.1(4) . 4_646 ? 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 O2W H2A O2 0.88(2) 1.99(3) 2.857(8) 170(10) . O3W H3A O4 0.87(2) 2.10(12) 2.807(10) 137(16) . _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.186 _refine_diff_density_min -0.959 _refine_diff_density_rms 0.118 data_3 _database_code_depnum_ccdc_archive 'CCDC 904153' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H31 N9 O9 Zn2' _chemical_formula_weight 840.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 '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 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.577(7) _cell_length_b 11.671(3) _cell_length_c 18.655(5) _cell_angle_alpha 90.00 _cell_angle_beta 118.998(4) _cell_angle_gamma 90.00 _cell_volume 3537.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.578 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1720 _exptl_absorpt_coefficient_mu 2.256 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6738 _exptl_absorpt_correction_T_max 0.7284 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26790 _diffrn_reflns_av_R_equivalents 0.1835 _diffrn_reflns_av_sigmaI/netI 0.1450 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.66 _diffrn_reflns_theta_max 68.02 _reflns_number_total 6238 _reflns_number_gt 2734 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The distances of O1W---H1A and O1W---H1B were restrained to 0.89+-0.02 \%A. The distance of H1A...H1B was restrained to 1.44+-0.02 \%A. For C34 and N8 atoms, the anisotropic displacement ellipsoids were rather elongated which led us to use the simu restraints. ; _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^)+(0.0732P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6238 _refine_ls_number_parameters 493 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1787 _refine_ls_R_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.1873 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _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 0.83212(7) -0.00189(10) 0.45980(5) 0.0445(3) Uani 1 1 d . . . Zn2 Zn 1.31368(7) -0.06772(10) 0.92069(6) 0.0480(3) Uani 1 1 d . . . C1 C 0.8954(5) 0.0573(8) 0.6122(4) 0.050(2) Uani 1 1 d . . . C2 C 0.9521(5) 0.0763(7) 0.7017(4) 0.046(2) Uani 1 1 d . . . C3 C 0.9309(5) 0.1504(8) 0.7461(5) 0.061(3) Uani 1 1 d . . . H3 H 0.8812 0.1895 0.7193 0.073 Uiso 1 1 calc R . . C4 C 0.9802(6) 0.1684(9) 0.8278(5) 0.072(3) Uani 1 1 d . . . H4 H 0.9651 0.2198 0.8561 0.087 Uiso 1 1 calc R . . C5 C 1.0536(5) 0.1082(9) 0.8677(4) 0.060(3) Uani 1 1 d . . . H5 H 1.0877 0.1186 0.9237 0.072 Uiso 1 1 calc R . . C6 C 1.0767(5) 0.0323(7) 0.8249(4) 0.043(2) Uani 1 1 d . . . C7 C 1.0268(4) 0.0186(7) 0.7421(4) 0.0403(19) Uani 1 1 d . . . H7 H 1.0430 -0.0296 0.7128 0.048 Uiso 1 1 calc R . . C8 C 1.1582(5) -0.0283(7) 0.8700(4) 0.047(2) Uani 1 1 d . . . C9 C 1.4170(5) 0.0475(7) 1.0673(5) 0.048(2) Uani 1 1 d . . . C10 C 1.4314(5) 0.1379(7) 1.1308(4) 0.045(2) Uani 1 1 d . . . C11 C 1.3714(5) 0.2200(7) 1.1128(4) 0.044(2) Uani 1 1 d . . . H11 H 1.3244 0.2196 1.0616 0.053 Uiso 1 1 calc R . . C12 C 1.3800(5) 0.3026(7) 1.1693(4) 0.0418(19) Uani 1 1 d . . . C13 C 1.4500(5) 0.3011(7) 1.2467(4) 0.049(2) Uani 1 1 d . . . H13 H 1.4560 0.3540 1.2865 0.059 Uiso 1 1 calc R . . C14 C 1.5107(6) 0.2193(8) 1.2632(5) 0.060(3) Uani 1 1 d . . . H14 H 1.5589 0.2201 1.3133 0.072 Uiso 1 1 calc R . . C15 C 1.5002(5) 0.1385(8) 1.2067(4) 0.052(2) Uani 1 1 d . . . H15 H 1.5402 0.0825 1.2197 0.062 Uiso 1 1 calc R . . C16 C 1.3142(5) 0.3902(8) 1.1490(5) 0.053(2) Uani 1 1 d . . . C17 C 0.5941(5) 0.4538(8) 0.1820(5) 0.063(3) Uani 1 1 d . . . H17A H 0.5609 0.4646 0.1239 0.094 Uiso 1 1 calc R . . H17B H 0.5682 0.4901 0.2097 0.094 Uiso 1 1 calc R . . H17C H 0.6001 0.3733 0.1942 0.094 Uiso 1 1 calc R . . C18 C 0.6784(5) 0.5065(7) 0.2105(4) 0.0462(19) Uani 1 1 d . . . C19 C 0.7384(6) 0.5020(7) 0.2930(4) 0.048(2) Uani 1 1 d . . . C20 C 0.8158(6) 0.5505(7) 0.3211(5) 0.049(2) Uani 1 1 d . . . C21 C 0.8304(5) 0.6139(7) 0.2655(4) 0.048(2) Uani 1 1 d . . . C22 C 0.7728(5) 0.6179(7) 0.1819(4) 0.048(2) Uani 1 1 d . . . C23 C 0.6984(5) 0.5577(7) 0.1555(4) 0.049(2) Uani 1 1 d . . . C24 C 0.7861(7) 0.6898(8) 0.1224(5) 0.075(3) Uani 1 1 d . . . H24A H 0.7400 0.6810 0.0684 0.112 Uiso 1 1 calc R . . H24B H 0.8354 0.6654 0.1224 0.112 Uiso 1 1 calc R . . H24C H 0.7913 0.7688 0.1384 0.112 Uiso 1 1 calc R . . C25 C 0.8805(6) 0.5357(9) 0.4091(5) 0.075(3) Uani 1 1 d . . . H25A H 0.9301 0.5740 0.4184 0.112 Uiso 1 1 calc R . . H25B H 0.8915 0.4556 0.4211 0.112 Uiso 1 1 calc R . . H25C H 0.8613 0.5681 0.4441 0.112 Uiso 1 1 calc R . . C26 C 0.7206(6) 0.4323(7) 0.3513(5) 0.053(2) Uani 1 1 d . . . H26A H 0.7446 0.4695 0.4044 0.064 Uiso 1 1 calc R . . H26B H 0.6616 0.4271 0.3302 0.064 Uiso 1 1 calc R . . C27 C 0.7865(5) 0.2453(8) 0.4225(5) 0.051(2) Uani 1 1 d . . . H27 H 0.7923 0.2612 0.4739 0.061 Uiso 1 1 calc R . . C28 C 0.7882(5) 0.1654(8) 0.3229(4) 0.050(2) Uani 1 1 d . . . H28 H 0.7967 0.1098 0.2920 0.060 Uiso 1 1 calc R . . C29 C 0.9132(6) 0.6732(8) 0.2970(5) 0.059(2) Uani 1 1 d . . . H29A H 0.9572 0.6175 0.3230 0.071 Uiso 1 1 calc R . . H29B H 0.9169 0.7075 0.2516 0.071 Uiso 1 1 calc R . . C30 C 0.8679(6) 0.8408(8) 0.3500(5) 0.052(2) Uani 1 1 d . . . H30 H 0.8171 0.8521 0.3036 0.063 Uiso 1 1 calc R . . C31 C 0.9726(5) 0.8547(8) 0.4665(5) 0.050(2) Uani 1 1 d . . . H31 H 1.0085 0.8809 0.5190 0.060 Uiso 1 1 calc R . . C32 C 0.6424(6) 0.5358(7) 0.0641(5) 0.060(3) Uani 1 1 d . . . H32A H 0.5887 0.5693 0.0471 0.072 Uiso 1 1 calc R . . H32B H 0.6655 0.5725 0.0331 0.072 Uiso 1 1 calc R . . C33 C 0.6810(6) 0.3239(9) 0.0839(5) 0.066(3) Uani 1 1 d . . . H33 H 0.7324 0.3290 0.1304 0.079 Uiso 1 1 calc R . . C34 C 0.5696(8) 0.2611(11) -0.0106(7) 0.122(6) Uani 1 1 d . . . H34 H 0.5283 0.2100 -0.0433 0.146 Uiso 1 1 calc R . . N1 N 0.8079(4) 0.1481(6) 0.4018(3) 0.0470(17) Uani 1 1 d . . . N2 N 0.7556(4) 0.3167(5) 0.3597(4) 0.0459(17) Uani 1 1 d . . . N3 N 0.7564(5) 0.2649(6) 0.2929(4) 0.060(2) Uani 1 1 d . . . N4 N 0.9223(5) 0.7631(6) 0.3571(4) 0.0520(18) Uani 1 1 d . . . N5 N 0.9903(4) 0.7712(6) 0.4316(4) 0.059(2) Uani 1 1 d . . . N6 N 0.8963(4) 0.9005(6) 0.4187(4) 0.0482(17) Uani 1 1 d . . . N7 N 0.6330(5) 0.4126(6) 0.0459(4) 0.063(2) Uani 1 1 d . . . N8 N 0.5602(7) 0.3741(9) -0.0152(6) 0.139(6) Uani 1 1 d . . . N9 N 0.6462(5) 0.2283(7) 0.0470(4) 0.074(2) Uani 1 1 d . . . O1 O 0.9185(3) -0.0139(5) 0.5758(3) 0.0543(15) Uani 1 1 d . . . O2 O 0.8288(4) 0.1073(6) 0.5769(3) 0.0657(18) Uani 1 1 d . . . O3 O 1.2004(3) -0.0387(5) 0.8334(3) 0.0581(17) Uani 1 1 d . . . O4 O 1.1812(4) -0.0628(6) 0.9406(3) 0.0743(19) Uani 1 1 d . . . O5 O 1.3458(3) 0.0439(5) 1.0073(3) 0.0661(19) Uani 1 1 d . . . O6 O 1.4722(4) -0.0194(5) 1.0773(3) 0.0599(16) Uani 1 1 d . . . O7 O 1.2660(4) 0.4048(5) 1.0719(3) 0.0568(16) Uani 1 1 d . . . O8 O 1.3081(4) 0.4423(5) 1.2029(3) 0.0641(17) Uani 1 1 d . . . O1W O 1.3695(4) -0.0131(9) 0.8591(4) 0.093(3) Uani 1 1 d D . . H1B H 1.4238(14) -0.015(12) 0.880(6) 0.139 Uiso 1 1 d D . . H1A H 1.347(6) -0.004(11) 0.8051(16) 0.139 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0427(6) 0.0504(6) 0.0322(5) -0.0012(5) 0.0116(4) -0.0039(6) Zn2 0.0409(6) 0.0581(7) 0.0346(5) -0.0043(5) 0.0100(4) 0.0065(6) C1 0.039(5) 0.071(6) 0.032(4) 0.006(4) 0.012(4) -0.009(5) C2 0.044(5) 0.062(6) 0.030(4) -0.002(4) 0.017(3) -0.009(4) C3 0.035(5) 0.091(7) 0.046(5) -0.003(5) 0.013(4) 0.010(5) C4 0.062(7) 0.100(8) 0.045(5) -0.017(5) 0.018(5) 0.010(6) C5 0.037(5) 0.107(8) 0.030(4) -0.012(4) 0.012(4) 0.000(5) C6 0.042(5) 0.052(5) 0.033(4) 0.003(3) 0.016(3) -0.007(4) C7 0.032(4) 0.051(5) 0.037(4) 0.002(4) 0.016(3) -0.003(4) C8 0.041(5) 0.057(6) 0.027(4) -0.004(3) 0.004(3) -0.004(4) C9 0.042(5) 0.050(5) 0.046(5) 0.003(4) 0.018(4) 0.006(4) C10 0.039(5) 0.052(5) 0.040(4) -0.002(4) 0.017(3) -0.001(4) C11 0.040(5) 0.055(5) 0.030(4) -0.004(4) 0.011(3) 0.009(4) C12 0.031(4) 0.049(5) 0.038(4) 0.001(4) 0.012(3) 0.006(4) C13 0.051(5) 0.058(5) 0.032(4) -0.006(4) 0.014(4) 0.007(4) C14 0.051(6) 0.069(7) 0.036(5) -0.006(4) 0.002(4) 0.009(5) C15 0.039(5) 0.059(6) 0.043(5) -0.005(4) 0.008(4) 0.009(4) C16 0.039(5) 0.062(6) 0.056(5) -0.013(5) 0.022(4) -0.005(4) C17 0.052(6) 0.075(7) 0.059(5) 0.009(5) 0.025(4) 0.010(5) C18 0.048(5) 0.048(5) 0.043(4) 0.002(4) 0.023(4) 0.007(4) C19 0.068(6) 0.043(5) 0.039(4) -0.002(4) 0.030(4) 0.005(5) C20 0.058(6) 0.043(5) 0.043(4) 0.000(4) 0.022(4) 0.008(4) C21 0.049(5) 0.052(5) 0.042(4) -0.005(4) 0.021(4) 0.004(4) C22 0.055(6) 0.047(5) 0.036(4) 0.001(4) 0.017(4) -0.001(4) C23 0.057(6) 0.047(5) 0.034(4) 0.009(4) 0.015(4) 0.009(4) C24 0.099(9) 0.062(6) 0.067(6) -0.004(5) 0.043(6) -0.018(6) C25 0.077(7) 0.089(8) 0.038(5) -0.008(4) 0.012(5) -0.003(6) C26 0.075(6) 0.043(5) 0.052(5) -0.002(4) 0.039(4) 0.010(5) C27 0.058(6) 0.061(6) 0.036(4) -0.008(4) 0.025(4) -0.013(5) C28 0.067(6) 0.055(6) 0.038(4) -0.005(4) 0.035(4) -0.003(5) C29 0.061(6) 0.063(6) 0.055(5) -0.017(4) 0.030(5) -0.001(5) C30 0.047(5) 0.068(6) 0.048(5) -0.002(4) 0.028(4) 0.007(5) C31 0.040(5) 0.061(6) 0.042(4) -0.009(4) 0.014(4) -0.005(4) C32 0.069(7) 0.048(6) 0.051(5) 0.006(4) 0.018(4) 0.000(5) C33 0.044(5) 0.074(7) 0.056(5) 0.001(5) 0.005(4) 0.019(5) C34 0.116(11) 0.078(9) 0.082(8) -0.016(7) -0.023(7) 0.018(8) N1 0.050(4) 0.056(5) 0.035(4) -0.010(3) 0.022(3) 0.000(4) N2 0.068(5) 0.040(4) 0.038(4) 0.000(3) 0.033(3) -0.004(3) N3 0.088(6) 0.048(5) 0.047(4) 0.003(4) 0.036(4) 0.003(4) N4 0.056(5) 0.052(4) 0.049(4) -0.007(3) 0.027(4) -0.006(4) N5 0.042(4) 0.067(5) 0.052(4) -0.012(4) 0.010(3) -0.006(4) N6 0.043(4) 0.049(4) 0.046(4) -0.011(3) 0.016(3) -0.005(3) N7 0.062(5) 0.055(5) 0.049(4) -0.004(4) 0.009(4) 0.001(4) N8 0.131(10) 0.086(8) 0.077(6) -0.019(6) -0.046(6) 0.031(7) N9 0.071(6) 0.067(6) 0.054(4) -0.014(4) 0.008(4) 0.001(5) O1 0.052(4) 0.066(4) 0.033(3) -0.013(3) 0.011(2) -0.004(3) O2 0.043(4) 0.100(5) 0.042(3) 0.011(3) 0.011(3) 0.013(3) O3 0.036(3) 0.096(5) 0.036(3) -0.007(3) 0.013(2) 0.004(3) O4 0.062(4) 0.096(5) 0.047(4) 0.019(3) 0.013(3) 0.009(4) O5 0.040(4) 0.086(5) 0.046(3) -0.024(3) 0.001(3) 0.008(3) O6 0.044(4) 0.067(4) 0.059(3) -0.018(3) 0.017(3) 0.005(3) O7 0.059(4) 0.066(4) 0.030(3) -0.007(3) 0.009(3) 0.015(3) O8 0.066(4) 0.075(4) 0.042(3) -0.014(3) 0.018(3) 0.018(3) O1W 0.038(4) 0.178(8) 0.055(4) 0.019(5) 0.017(3) 0.003(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 O7 1.953(6) 2_746 ? Zn1 O1 1.977(5) . ? Zn1 N1 1.991(7) . ? Zn1 N6 2.048(7) 1_545 ? Zn1 C1 2.589(8) . ? Zn2 O5 1.931(5) . ? Zn2 O3 1.968(5) . ? Zn2 O1W 1.988(7) . ? Zn2 N9 1.999(8) 3_756 ? C1 O2 1.231(10) . ? C1 O1 1.272(10) . ? C1 C2 1.497(10) . ? C2 C7 1.390(11) . ? C2 C3 1.381(12) . ? C3 C4 1.360(11) . ? C3 H3 0.9300 . ? C4 C5 1.386(12) . ? C4 H4 0.9300 . ? C5 C6 1.393(11) . ? C5 H5 0.9300 . ? C6 C7 1.372(9) . ? C6 C8 1.506(11) . ? C7 H7 0.9300 . ? C8 O4 1.240(9) . ? C8 O3 1.270(10) . ? C9 O6 1.230(9) . ? C9 O5 1.252(9) . ? C9 C10 1.509(11) . ? C10 C15 1.373(10) . ? C10 C11 1.383(11) . ? C11 C12 1.380(11) . ? C11 H11 0.9300 . ? C12 C13 1.399(10) . ? C12 C16 1.495(11) . ? C13 C14 1.394(12) . ? C13 H13 0.9300 . ? C14 C15 1.355(11) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O8 1.226(10) . ? C16 O7 1.285(9) . ? C17 C18 1.517(12) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.397(10) . ? C18 C23 1.385(11) . ? C19 C20 1.389(12) . ? C19 C26 1.517(11) . ? C20 C21 1.402(12) . ? C20 C25 1.503(10) . ? C21 C22 1.401(10) . ? C21 C29 1.522(12) . ? C22 C23 1.410(12) . ? C22 C24 1.504(12) . ? C23 C32 1.530(10) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 N2 1.474(10) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 N1 1.320(10) . ? C27 N2 1.321(10) . ? C27 H27 0.9300 . ? C28 N3 1.300(10) . ? C28 N1 1.349(9) . ? C28 H28 0.9300 . ? C29 N4 1.484(10) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N4 1.314(10) . ? C30 N6 1.324(10) . ? C30 H30 0.9300 . ? C31 N5 1.300(11) . ? C31 N6 1.365(10) . ? C31 H31 0.9300 . ? C32 N7 1.467(11) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N9 1.306(12) . ? C33 N7 1.326(11) . ? C33 H33 0.9300 . ? C34 N8 1.328(14) . ? C34 N9 1.357(13) . ? C34 H34 0.9300 . ? N2 N3 1.392(9) . ? N4 N5 1.355(9) . ? N6 Zn1 2.048(7) 1_565 ? N7 N8 1.355(11) . ? N9 Zn2 1.999(8) 3_756 ? O7 Zn1 1.953(6) 2_756 ? O1W H1B 0.89(2) . ? O1W H1A 0.89(2) . ? 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 O7 Zn1 O1 115.8(2) 2_746 . ? O7 Zn1 N1 113.2(3) 2_746 . ? O1 Zn1 N1 120.4(3) . . ? O7 Zn1 N6 101.8(3) 2_746 1_545 ? O1 Zn1 N6 93.4(3) . 1_545 ? N1 Zn1 N6 107.8(3) . 1_545 ? O7 Zn1 C1 110.0(2) 2_746 . ? O1 Zn1 C1 28.5(3) . . ? N1 Zn1 C1 103.0(3) . . ? N6 Zn1 C1 121.5(3) 1_545 . ? O5 Zn2 O3 110.4(2) . . ? O5 Zn2 O1W 103.3(3) . . ? O3 Zn2 O1W 96.6(3) . . ? O5 Zn2 N9 117.5(3) . 3_756 ? O3 Zn2 N9 120.2(3) . 3_756 ? O1W Zn2 N9 104.6(4) . 3_756 ? O2 C1 O1 122.4(7) . . ? O2 C1 C2 120.5(8) . . ? O1 C1 C2 117.1(7) . . ? O2 C1 Zn1 74.7(4) . . ? O1 C1 Zn1 48.0(3) . . ? C2 C1 Zn1 164.5(7) . . ? C7 C2 C3 118.6(7) . . ? C7 C2 C1 120.7(7) . . ? C3 C2 C1 120.7(8) . . ? C4 C3 C2 122.4(8) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C3 C4 C5 118.5(8) . . ? C3 C4 H4 120.8 . . ? C5 C4 H4 120.8 . . ? C4 C5 C6 120.7(7) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? C7 C6 C5 119.4(7) . . ? C7 C6 C8 121.5(7) . . ? C5 C6 C8 119.0(6) . . ? C6 C7 C2 120.4(7) . . ? C6 C7 H7 119.8 . . ? C2 C7 H7 119.8 . . ? O4 C8 O3 123.8(8) . . ? O4 C8 C6 118.8(8) . . ? O3 C8 C6 117.4(6) . . ? O6 C9 O5 123.7(8) . . ? O6 C9 C10 120.5(7) . . ? O5 C9 C10 115.7(8) . . ? C15 C10 C11 119.0(7) . . ? C15 C10 C9 122.4(8) . . ? C11 C10 C9 118.6(7) . . ? C12 C11 C10 121.2(7) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 119.0(7) . . ? C11 C12 C16 120.5(7) . . ? C13 C12 C16 120.4(7) . . ? C14 C13 C12 119.0(7) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 120.6(7) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C10 121.2(8) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O8 C16 O7 124.2(8) . . ? O8 C16 C12 121.4(7) . . ? O7 C16 C12 114.4(7) . . ? C18 C17 H17A 109.5 . . ? C18 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C18 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 118.3(8) . . ? C19 C18 C17 120.6(7) . . ? C23 C18 C17 121.1(7) . . ? C20 C19 C18 121.8(7) . . ? C20 C19 C26 119.6(7) . . ? C18 C19 C26 118.3(8) . . ? C19 C20 C21 118.2(7) . . ? C19 C20 C25 119.9(8) . . ? C21 C20 C25 122.0(8) . . ? C22 C21 C20 121.6(8) . . ? C22 C21 C29 119.8(8) . . ? C20 C21 C29 118.4(7) . . ? C21 C22 C23 117.5(7) . . ? C21 C22 C24 122.1(8) . . ? C23 C22 C24 120.3(7) . . ? C18 C23 C22 121.8(7) . . ? C18 C23 C32 118.2(8) . . ? C22 C23 C32 119.6(7) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C19 109.2(6) . . ? N2 C26 H26A 109.8 . . ? C19 C26 H26A 109.8 . . ? N2 C26 H26B 109.8 . . ? C19 C26 H26B 109.8 . . ? H26A C26 H26B 108.3 . . ? N1 C27 N2 110.2(7) . . ? N1 C27 H27 124.9 . . ? N2 C27 H27 124.9 . . ? N3 C28 N1 115.5(7) . . ? N3 C28 H28 122.3 . . ? N1 C28 H28 122.3 . . ? N4 C29 C21 109.7(7) . . ? N4 C29 H29A 109.7 . . ? C21 C29 H29A 109.7 . . ? N4 C29 H29B 109.7 . . ? C21 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? N4 C30 N6 109.8(7) . . ? N4 C30 H30 125.1 . . ? N6 C30 H30 125.1 . . ? N5 C31 N6 113.7(7) . . ? N5 C31 H31 123.2 . . ? N6 C31 H31 123.2 . . ? N7 C32 C23 111.3(6) . . ? N7 C32 H32A 109.4 . . ? C23 C32 H32A 109.4 . . ? N7 C32 H32B 109.4 . . ? C23 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? N9 C33 N7 110.7(8) . . ? N9 C33 H33 124.7 . . ? N7 C33 H33 124.7 . . ? N8 C34 N9 112.7(11) . . ? N8 C34 H34 123.6 . . ? N9 C34 H34 123.6 . . ? C27 N1 C28 103.3(7) . . ? C27 N1 Zn1 128.1(5) . . ? C28 N1 Zn1 126.5(6) . . ? C27 N2 N3 109.4(7) . . ? C27 N2 C26 130.7(7) . . ? N3 N2 C26 119.9(6) . . ? C28 N3 N2 101.7(6) . . ? C30 N4 N5 110.2(7) . . ? C30 N4 C29 127.6(7) . . ? N5 N4 C29 122.1(7) . . ? C31 N5 N4 103.2(7) . . ? C30 N6 C31 103.1(7) . . ? C30 N6 Zn1 128.6(6) . 1_565 ? C31 N6 Zn1 125.6(5) . 1_565 ? C33 N7 N8 109.2(8) . . ? C33 N7 C32 131.9(8) . . ? N8 N7 C32 118.5(8) . . ? C34 N8 N7 103.2(9) . . ? C33 N9 C34 103.7(9) . . ? C33 N9 Zn2 128.7(6) . 3_756 ? C34 N9 Zn2 126.7(8) . 3_756 ? C1 O1 Zn1 103.5(5) . . ? C8 O3 Zn2 105.2(4) . . ? C9 O5 Zn2 122.3(6) . . ? C16 O7 Zn1 117.0(5) . 2_756 ? Zn2 O1W H1B 123(7) . . ? Zn2 O1W H1A 127(7) . . ? H1B O1W H1A 108(9) . . ? 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 O7 Zn1 C1 O2 -66.8(6) 2_746 . . . ? O1 Zn1 C1 O2 -174.4(9) . . . . ? N1 Zn1 C1 O2 54.1(6) . . . . ? N6 Zn1 C1 O2 174.7(5) 1_545 . . . ? O7 Zn1 C1 O1 107.5(5) 2_746 . . . ? N1 Zn1 C1 O1 -131.6(5) . . . . ? N6 Zn1 C1 O1 -11.0(6) 1_545 . . . ? O7 Zn1 C1 C2 124(2) 2_746 . . . ? O1 Zn1 C1 C2 17(2) . . . . ? N1 Zn1 C1 C2 -115(2) . . . . ? N6 Zn1 C1 C2 6(2) 1_545 . . . ? O2 C1 C2 C7 178.9(8) . . . . ? O1 C1 C2 C7 0.4(12) . . . . ? Zn1 C1 C2 C7 -13(3) . . . . ? O2 C1 C2 C3 -0.2(13) . . . . ? O1 C1 C2 C3 -178.7(8) . . . . ? Zn1 C1 C2 C3 167.6(19) . . . . ? C7 C2 C3 C4 -0.3(14) . . . . ? C1 C2 C3 C4 178.8(9) . . . . ? C2 C3 C4 C5 -1.2(16) . . . . ? C3 C4 C5 C6 0.8(16) . . . . ? C4 C5 C6 C7 1.1(14) . . . . ? C4 C5 C6 C8 177.9(9) . . . . ? C5 C6 C7 C2 -2.6(12) . . . . ? C8 C6 C7 C2 -179.4(7) . . . . ? C3 C2 C7 C6 2.3(12) . . . . ? C1 C2 C7 C6 -176.9(7) . . . . ? C7 C6 C8 O4 -144.0(8) . . . . ? C5 C6 C8 O4 39.3(11) . . . . ? C7 C6 C8 O3 37.5(11) . . . . ? C5 C6 C8 O3 -139.2(8) . . . . ? O6 C9 C10 C15 -10.6(13) . . . . ? O5 C9 C10 C15 167.0(8) . . . . ? O6 C9 C10 C11 172.2(8) . . . . ? O5 C9 C10 C11 -10.2(12) . . . . ? C15 C10 C11 C12 0.7(13) . . . . ? C9 C10 C11 C12 177.9(8) . . . . ? C10 C11 C12 C13 -1.3(13) . . . . ? C10 C11 C12 C16 -179.5(8) . . . . ? C11 C12 C13 C14 2.7(13) . . . . ? C16 C12 C13 C14 -179.1(8) . . . . ? C12 C13 C14 C15 -3.5(14) . . . . ? C13 C14 C15 C10 2.9(15) . . . . ? C11 C10 C15 C14 -1.4(14) . . . . ? C9 C10 C15 C14 -178.6(8) . . . . ? C11 C12 C16 O8 159.0(8) . . . . ? C13 C12 C16 O8 -19.1(13) . . . . ? C11 C12 C16 O7 -20.9(12) . . . . ? C13 C12 C16 O7 160.9(8) . . . . ? C23 C18 C19 C20 2.1(12) . . . . ? C17 C18 C19 C20 -179.4(8) . . . . ? C23 C18 C19 C26 -172.0(7) . . . . ? C17 C18 C19 C26 6.5(11) . . . . ? C18 C19 C20 C21 5.6(12) . . . . ? C26 C19 C20 C21 179.6(7) . . . . ? C18 C19 C20 C25 -175.3(8) . . . . ? C26 C19 C20 C25 -1.2(12) . . . . ? C19 C20 C21 C22 -7.4(12) . . . . ? C25 C20 C21 C22 173.5(8) . . . . ? C19 C20 C21 C29 176.4(7) . . . . ? C25 C20 C21 C29 -2.7(12) . . . . ? C20 C21 C22 C23 1.4(12) . . . . ? C29 C21 C22 C23 177.6(8) . . . . ? C20 C21 C22 C24 177.2(8) . . . . ? C29 C21 C22 C24 -6.6(13) . . . . ? C19 C18 C23 C22 -8.5(12) . . . . ? C17 C18 C23 C22 173.0(8) . . . . ? C19 C18 C23 C32 164.3(8) . . . . ? C17 C18 C23 C32 -14.2(12) . . . . ? C21 C22 C23 C18 6.8(12) . . . . ? C24 C22 C23 C18 -169.1(8) . . . . ? C21 C22 C23 C32 -165.9(7) . . . . ? C24 C22 C23 C32 18.2(12) . . . . ? C20 C19 C26 N2 -79.3(9) . . . . ? C18 C19 C26 N2 94.9(9) . . . . ? C22 C21 C29 N4 119.0(8) . . . . ? C20 C21 C29 N4 -64.7(10) . . . . ? C18 C23 C32 N7 -55.4(11) . . . . ? C22 C23 C32 N7 117.6(9) . . . . ? N2 C27 N1 C28 0.1(9) . . . . ? N2 C27 N1 Zn1 -164.0(6) . . . . ? N3 C28 N1 C27 0.1(10) . . . . ? N3 C28 N1 Zn1 164.5(6) . . . . ? O7 Zn1 N1 C27 86.4(7) 2_746 . . . ? O1 Zn1 N1 C27 -56.8(8) . . . . ? N6 Zn1 N1 C27 -161.8(7) 1_545 . . . ? C1 Zn1 N1 C27 -32.3(8) . . . . ? O7 Zn1 N1 C28 -74.2(7) 2_746 . . . ? O1 Zn1 N1 C28 142.6(7) . . . . ? N6 Zn1 N1 C28 37.6(8) 1_545 . . . ? C1 Zn1 N1 C28 167.1(7) . . . . ? N1 C27 N2 N3 -0.2(10) . . . . ? N1 C27 N2 C26 177.4(8) . . . . ? C19 C26 N2 C27 148.0(8) . . . . ? C19 C26 N2 N3 -34.7(11) . . . . ? N1 C28 N3 N2 -0.2(10) . . . . ? C27 N2 N3 C28 0.2(9) . . . . ? C26 N2 N3 C28 -177.6(8) . . . . ? N6 C30 N4 N5 -1.5(10) . . . . ? N6 C30 N4 C29 175.5(7) . . . . ? C21 C29 N4 C30 -46.4(12) . . . . ? C21 C29 N4 N5 130.2(8) . . . . ? N6 C31 N5 N4 0.6(10) . . . . ? C30 N4 N5 C31 0.5(10) . . . . ? C29 N4 N5 C31 -176.6(8) . . . . ? N4 C30 N6 C31 1.7(10) . . . . ? N4 C30 N6 Zn1 -160.4(6) . . . 1_565 ? N5 C31 N6 C30 -1.4(10) . . . . ? N5 C31 N6 Zn1 161.4(6) . . . 1_565 ? N9 C33 N7 N8 5.1(13) . . . . ? N9 C33 N7 C32 177.7(9) . . . . ? C23 C32 N7 C33 -25.6(14) . . . . ? C23 C32 N7 N8 146.5(10) . . . . ? N9 C34 N8 N7 -3.6(18) . . . . ? C33 N7 N8 C34 -0.8(15) . . . . ? C32 N7 N8 C34 -174.6(11) . . . . ? N7 C33 N9 C34 -6.9(13) . . . . ? N7 C33 N9 Zn2 -176.6(7) . . . 3_756 ? N8 C34 N9 C33 6.6(17) . . . . ? N8 C34 N9 Zn2 176.5(10) . . . 3_756 ? O2 C1 O1 Zn1 6.4(10) . . . . ? C2 C1 O1 Zn1 -175.1(6) . . . . ? O7 Zn1 O1 C1 -84.6(6) 2_746 . . . ? N1 Zn1 O1 C1 57.7(6) . . . . ? N6 Zn1 O1 C1 170.6(5) 1_545 . . . ? O4 C8 O3 Zn2 -18.4(10) . . . . ? C6 C8 O3 Zn2 160.0(5) . . . . ? O5 Zn2 O3 C8 -49.7(6) . . . . ? O1W Zn2 O3 C8 -156.6(6) . . . . ? N9 Zn2 O3 C8 92.2(6) 3_756 . . . ? O6 C9 O5 Zn2 -0.9(13) . . . . ? C10 C9 O5 Zn2 -178.4(5) . . . . ? O3 Zn2 O5 C9 -175.5(7) . . . . ? O1W Zn2 O5 C9 -73.2(7) . . . . ? N9 Zn2 O5 C9 41.4(8) 3_756 . . . ? O8 C16 O7 Zn1 -9.9(12) . . . 2_756 ? C12 C16 O7 Zn1 170.1(5) . . . 2_756 ? 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 O1W H1B O6 0.89(2) 1.74(4) 2.612(9) 165(14) 3_857 O1W H1A O8 0.89(2) 1.83(4) 2.693(8) 163(13) 4_565 _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 68.02 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 0.549 _refine_diff_density_min -0.802 _refine_diff_density_rms 0.099 data_4 _database_code_depnum_ccdc_archive 'CCDC 904154' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H33 Cd2 N9 O10' _chemical_formula_weight 952.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.3392(14) _cell_length_b 16.2364(12) _cell_length_c 22.526(2) _cell_angle_alpha 90.00 _cell_angle_beta 102.756(4) _cell_angle_gamma 90.00 _cell_volume 3688.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.715 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1904 _exptl_absorpt_coefficient_mu 1.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7337 _exptl_absorpt_correction_T_max 0.7921 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17199 _diffrn_reflns_av_R_equivalents 0.0429 _diffrn_reflns_av_sigmaI/netI 0.1455 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 29.22 _reflns_number_total 8510 _reflns_number_gt 4154 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The distance of O2W---H2A was restrained to 0.85+-0.02 \%A. The distance of O3...O3W was restrained to 3.00+-0.01 \%A. The anisotropic displacement ellipsoid of N8 was rather elongated which led us to use the simu restraint. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8510 _refine_ls_number_parameters 522 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0914 _refine_ls_R_factor_gt 0.0345 _refine_ls_wR_factor_ref 0.0497 _refine_ls_wR_factor_gt 0.0464 _refine_ls_goodness_of_fit_ref 0.791 _refine_ls_restrained_S_all 0.798 _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 Cd1 Cd -0.41277(3) 0.186052(19) 0.424595(12) 0.03231(8) Uani 1 1 d . . . Cd2 Cd -0.16607(3) 0.271056(18) 0.040062(12) 0.03187(8) Uani 1 1 d . . . C1 C -0.2063(4) 0.1742(2) 0.3665(2) 0.0415(11) Uani 1 1 d . A . C2 C -0.0846(4) 0.1719(2) 0.34083(17) 0.0320(10) Uani 1 1 d . . . C3 C -0.0974(4) 0.1707(2) 0.27866(17) 0.0428(11) Uani 1 1 d . . . H3 H -0.1817 0.1717 0.2533 0.051 Uiso 1 1 calc R . . C4 C 0.0110(4) 0.1681(3) 0.25352(17) 0.0495(12) Uani 1 1 d . . . H4 H 0.0009 0.1669 0.2115 0.059 Uiso 1 1 calc R . . C5 C 0.1365(4) 0.1674(2) 0.29132(16) 0.0437(11) Uani 1 1 d . . . H5 H 0.2107 0.1650 0.2744 0.052 Uiso 1 1 calc R . . C6 C 0.1528(3) 0.1700(2) 0.35374(15) 0.0288(9) Uani 1 1 d . . . C7 C 0.0416(4) 0.1720(2) 0.37822(16) 0.0338(10) Uani 1 1 d . . . H7 H 0.0513 0.1734 0.4202 0.041 Uiso 1 1 calc R . . C8 C 0.2918(4) 0.1729(2) 0.39319(18) 0.0322(10) Uani 1 1 d . . . C9 C -0.3762(4) 0.2505(2) 0.09364(18) 0.0352(10) Uani 1 1 d . . . C10 C -0.4969(3) 0.2408(2) 0.12012(17) 0.0333(10) Uani 1 1 d . . . C11 C -0.4826(4) 0.2169(2) 0.18017(17) 0.0441(11) Uani 1 1 d . . . H11 H -0.3985 0.2067 0.2039 0.053 Uiso 1 1 calc R . . C12 C -0.5921(4) 0.2080(3) 0.20487(18) 0.0516(13) Uani 1 1 d . . . H12 H -0.5819 0.1933 0.2455 0.062 Uiso 1 1 calc R . . C13 C -0.7170(4) 0.2209(2) 0.16933(16) 0.0431(11) Uani 1 1 d . . . H13 H -0.7908 0.2145 0.1862 0.052 Uiso 1 1 calc R . . C14 C -0.7339(3) 0.2431(2) 0.10949(15) 0.0295(10) Uani 1 1 d . . . C15 C -0.6233(3) 0.2544(2) 0.08508(16) 0.0325(10) Uani 1 1 d . . . H15 H -0.6339 0.2714 0.0449 0.039 Uiso 1 1 calc R . . C16 C -0.8717(4) 0.2574(2) 0.07245(17) 0.0331(10) Uani 1 1 d . . . C17 C -0.1230(4) 0.4760(3) 0.04483(19) 0.0419(11) Uani 1 1 d . . . H17 H -0.1501 0.4780 0.0026 0.050 Uiso 1 1 calc R . . C18 C -0.0529(4) 0.5115(3) 0.13444(19) 0.0531(13) Uani 1 1 d . . . H18 H -0.0204 0.5421 0.1694 0.064 Uiso 1 1 calc R . . C19 C -0.0499(5) 0.3741(3) 0.18625(16) 0.0587(14) Uani 1 1 d . . . H19A H 0.0357 0.3477 0.1899 0.070 Uiso 1 1 calc R . . H19B H -0.1175 0.3316 0.1789 0.070 Uiso 1 1 calc R . . C20 C -0.0535(5) 0.4187(2) 0.24481(18) 0.0470(12) Uani 1 1 d . . . C21 C 0.0653(5) 0.4409(3) 0.2836(2) 0.0512(12) Uani 1 1 d . . . C22 C 0.0633(5) 0.4812(3) 0.3389(2) 0.0492(12) Uani 1 1 d . . . C23 C -0.0571(6) 0.4958(2) 0.35407(19) 0.0511(13) Uani 1 1 d . . . C24 C 0.1968(6) 0.4224(3) 0.2678(2) 0.0980(19) Uani 1 1 d . . . H24A H 0.2226 0.3669 0.2795 0.147 Uiso 1 1 calc R . . H24B H 0.2628 0.4598 0.2891 0.147 Uiso 1 1 calc R . . H24C H 0.1885 0.4286 0.2247 0.147 Uiso 1 1 calc R . . C25 C -0.0567(6) 0.5304(3) 0.4172(2) 0.0858(18) Uani 1 1 d . . . H25A H -0.1464 0.5376 0.4215 0.129 Uiso 1 1 calc R . . H25B H -0.0119 0.5825 0.4221 0.129 Uiso 1 1 calc R . . H25C H -0.0117 0.4927 0.4477 0.129 Uiso 1 1 calc R . . C26 C -0.1761(5) 0.4781(3) 0.3131(2) 0.0510(12) Uani 1 1 d . . . C27 C -0.1736(5) 0.4391(3) 0.2573(2) 0.0521(13) Uani 1 1 d . . . C28 C -0.3012(5) 0.4215(3) 0.2127(2) 0.0878(18) Uani 1 1 d . . . H28A H -0.3743 0.4396 0.2292 0.132 Uiso 1 1 calc R . . H28B H -0.3086 0.3634 0.2049 0.132 Uiso 1 1 calc R . . H28C H -0.3023 0.4502 0.1753 0.132 Uiso 1 1 calc R . . C29 C -0.3057(5) 0.5039(3) 0.3273(2) 0.0711(15) Uani 1 1 d . A . H29A H -0.2912 0.5515 0.3540 0.085 Uiso 1 1 calc R . . H29B H -0.3669 0.5198 0.2899 0.085 Uiso 1 1 calc R . . C30 C -0.3266(9) 0.3687(5) 0.3814(5) 0.083(3) Uani 0.801(9) 1 d P A 1 H30 H -0.2390 0.3516 0.3863 0.100 Uiso 0.801(9) 1 calc PR A 1 C31 C -0.5138(10) 0.3678(7) 0.3748(8) 0.246(10) Uani 0.801(9) 1 d P A 1 H31 H -0.5999 0.3501 0.3735 0.295 Uiso 0.801(9) 1 calc PR A 1 N6 N -0.4875(8) 0.4388(5) 0.3518(6) 0.225(7) Uani 0.801(9) 1 d P A 1 N6' N -0.379(3) 0.4605(15) 0.4225(12) 0.090(10) Uiso 0.199(9) 1 d P A 2 C30' C -0.378(5) 0.352(3) 0.350(2) 0.13(2) Uiso 0.199(9) 1 d P A 2 H30' H -0.3663 0.3211 0.3163 0.150 Uiso 0.199(9) 1 calc PR A 2 C31' C -0.416(3) 0.3837(16) 0.4402(12) 0.062(9) Uiso 0.199(9) 1 d P A 2 H31' H -0.4422 0.3744 0.4766 0.074 Uiso 0.199(9) 1 calc PR A 2 C32 C 0.1892(5) 0.5135(3) 0.3796(2) 0.0737(16) Uani 1 1 d . . . H32A H 0.2550 0.5222 0.3555 0.088 Uiso 1 1 calc R . . H32B H 0.1711 0.5664 0.3962 0.088 Uiso 1 1 calc R . . C33 C 0.3686(6) 0.4195(4) 0.5106(3) 0.132(3) Uani 1 1 d . . . H33 H 0.4325 0.4205 0.5468 0.158 Uiso 1 1 calc R . . C34 C 0.2211(5) 0.3791(3) 0.4405(2) 0.0568(14) Uani 1 1 d . . . H34 H 0.1571 0.3466 0.4157 0.068 Uiso 1 1 calc R . . N1 N -0.1193(3) 0.4064(2) 0.07685(14) 0.0381(9) Uani 1 1 d . . . N2 N -0.0730(3) 0.4320(2) 0.13451(14) 0.0423(9) Uani 1 1 d . . . N3 N -0.0837(3) 0.5432(2) 0.07946(15) 0.0422(9) Uani 1 1 d . . . N4 N -0.3642(5) 0.4372(3) 0.3565(2) 0.0660(12) Uani 1 1 d . . . N5 N -0.4104(4) 0.3241(3) 0.3994(2) 0.0637(11) Uani 1 1 d . . . N7 N 0.2433(4) 0.4572(2) 0.42979(17) 0.0652(12) Uani 1 1 d . . . N8 N 0.3390(5) 0.4863(3) 0.4751(3) 0.142(3) Uani 1 1 d . . . N9 N 0.3011(4) 0.3528(2) 0.49080(17) 0.0558(11) Uani 1 1 d . . . O1 O -0.3902(2) 0.28282(18) 0.04188(12) 0.0549(8) Uani 1 1 d . . . O2 O -0.2660(2) 0.22718(17) 0.12334(11) 0.0472(7) Uani 1 1 d . . . O3 O -0.1907(2) 0.18297(18) 0.42408(12) 0.0510(8) Uani 1 1 d D . . O4 O -0.3179(2) 0.16959(17) 0.33236(11) 0.0495(8) Uani 1 1 d . . . O5 O 0.3058(3) 0.16618(18) 0.44895(12) 0.0534(9) Uani 1 1 d . . . O6 O 0.3836(2) 0.18121(18) 0.36635(12) 0.0531(8) Uani 1 1 d . . . O7 O -0.9663(2) 0.23284(17) 0.09398(11) 0.0468(7) Uani 1 1 d . . . O8 O -0.8875(3) 0.29438(19) 0.02358(12) 0.0620(9) Uani 1 1 d . . . O1W O -0.0491(5) 0.0643(3) 0.5271(3) 0.194(2) Uani 1 1 d . . . O2W O -0.7457(8) 0.4599(4) 0.1037(3) 0.083(2) Uani 0.50 1 d PD . . H2A H -0.678(4) 0.459(4) 0.131(2) 0.124 Uiso 1 1 d D . . O3W O -0.0473(6) 0.3331(4) 0.4594(3) 0.081(2) Uani 0.50 1 d PD . . 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 Cd1 0.02212(16) 0.04693(19) 0.02845(16) -0.00235(15) 0.00680(12) 0.00088(14) Cd2 0.02060(16) 0.04725(19) 0.02822(16) -0.00153(15) 0.00638(12) -0.00102(14) C1 0.031(3) 0.049(3) 0.049(3) -0.001(2) 0.017(2) -0.005(2) C2 0.022(2) 0.041(3) 0.033(2) -0.0002(19) 0.0052(18) 0.0002(18) C3 0.020(2) 0.074(3) 0.030(2) 0.003(2) -0.0028(18) -0.004(2) C4 0.033(3) 0.092(4) 0.022(2) 0.001(2) 0.004(2) -0.006(2) C5 0.026(3) 0.080(4) 0.028(2) 0.003(2) 0.0120(19) -0.002(2) C6 0.021(2) 0.043(3) 0.023(2) 0.0059(18) 0.0060(17) -0.0021(18) C7 0.030(2) 0.048(3) 0.025(2) -0.0020(19) 0.0097(18) 0.002(2) C8 0.028(3) 0.031(2) 0.035(3) 0.003(2) 0.002(2) 0.0038(19) C9 0.026(2) 0.037(3) 0.045(3) -0.001(2) 0.014(2) -0.0019(19) C10 0.024(2) 0.041(3) 0.037(2) 0.005(2) 0.0094(18) -0.0031(18) C11 0.021(2) 0.066(3) 0.041(3) 0.009(2) -0.0015(19) 0.010(2) C12 0.031(3) 0.092(4) 0.031(2) 0.021(2) 0.005(2) 0.006(2) C13 0.021(2) 0.078(3) 0.033(2) 0.012(2) 0.0112(18) 0.005(2) C14 0.019(2) 0.045(3) 0.025(2) 0.0023(19) 0.0045(17) 0.0037(18) C15 0.028(2) 0.043(3) 0.028(2) 0.0025(19) 0.0078(18) -0.0006(18) C16 0.030(2) 0.040(3) 0.030(2) -0.004(2) 0.0072(19) 0.005(2) C17 0.040(3) 0.057(3) 0.028(3) 0.003(3) 0.008(2) -0.005(2) C18 0.076(4) 0.039(3) 0.035(3) -0.002(2) -0.006(2) -0.010(3) C19 0.098(4) 0.049(3) 0.026(3) 0.004(2) 0.007(2) 0.000(3) C20 0.075(4) 0.037(3) 0.026(3) 0.002(2) 0.006(3) -0.004(2) C21 0.065(4) 0.047(3) 0.043(3) 0.011(2) 0.016(3) 0.000(3) C22 0.071(4) 0.037(3) 0.035(3) 0.005(2) 0.001(3) -0.011(2) C23 0.091(5) 0.034(3) 0.029(3) 0.005(2) 0.016(3) -0.004(3) C24 0.096(5) 0.121(5) 0.077(4) -0.016(3) 0.020(4) -0.003(4) C25 0.153(6) 0.062(4) 0.050(3) -0.015(3) 0.039(3) 0.003(3) C26 0.067(4) 0.026(3) 0.064(4) 0.011(2) 0.022(3) 0.004(2) C27 0.075(4) 0.039(3) 0.037(3) -0.001(2) 0.001(3) -0.007(3) C28 0.085(5) 0.093(5) 0.079(4) -0.012(3) 0.003(3) -0.017(3) C29 0.091(5) 0.050(3) 0.078(4) 0.022(3) 0.030(3) 0.008(3) C30 0.073(6) 0.058(5) 0.133(9) 0.040(6) 0.053(7) 0.038(5) C31 0.083(8) 0.165(10) 0.52(3) 0.230(14) 0.129(13) 0.064(8) N6 0.071(7) 0.138(8) 0.48(2) 0.192(10) 0.099(9) 0.043(6) C32 0.103(5) 0.054(3) 0.052(3) 0.023(3) -0.007(3) -0.011(3) C33 0.116(6) 0.080(5) 0.151(6) 0.038(5) -0.073(5) -0.019(4) C34 0.070(4) 0.040(3) 0.052(3) -0.004(3) -0.002(3) -0.020(3) N1 0.045(2) 0.049(2) 0.0201(19) -0.0066(18) 0.0064(16) -0.0070(17) N2 0.057(3) 0.041(2) 0.028(2) -0.0016(18) 0.0076(17) -0.0034(18) N3 0.051(2) 0.045(2) 0.028(2) 0.0028(19) 0.0030(16) -0.0017(19) N4 0.064(3) 0.056(3) 0.083(3) 0.007(3) 0.028(3) 0.011(3) N5 0.053(3) 0.055(3) 0.090(3) 0.014(3) 0.030(2) 0.002(3) N7 0.063(3) 0.052(3) 0.066(3) 0.011(2) -0.018(2) -0.016(2) N8 0.113(5) 0.088(4) 0.171(6) 0.053(4) -0.085(4) -0.048(3) N9 0.051(3) 0.044(2) 0.059(3) 0.011(2) -0.016(2) -0.011(2) O1 0.0307(17) 0.087(2) 0.0508(19) 0.0235(17) 0.0182(14) 0.0036(15) O2 0.0167(15) 0.074(2) 0.0506(17) 0.0009(16) 0.0078(13) 0.0014(14) O3 0.0259(17) 0.092(2) 0.0387(18) -0.0083(17) 0.0151(13) 0.0034(15) O4 0.0154(16) 0.087(2) 0.0459(18) 0.0019(15) 0.0077(13) -0.0017(14) O5 0.0418(19) 0.092(3) 0.0226(16) -0.0066(15) -0.0013(13) 0.0108(16) O6 0.0169(16) 0.099(2) 0.0430(18) 0.0201(17) 0.0059(13) -0.0005(15) O7 0.0175(15) 0.071(2) 0.0511(18) 0.0093(16) 0.0057(13) -0.0026(14) O8 0.0434(19) 0.113(3) 0.0298(17) 0.0235(18) 0.0085(14) 0.0218(17) O1W 0.175(5) 0.110(4) 0.318(7) -0.071(4) 0.102(5) -0.003(3) O2W 0.119(7) 0.046(4) 0.088(6) 0.005(4) 0.033(4) 0.017(5) O3W 0.088(6) 0.086(5) 0.065(5) 0.014(4) 0.006(4) 0.000(4) _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 Cd1 O8 2.210(3) 4_666 ? Cd1 O6 2.222(2) 1_455 ? Cd1 O3 2.300(2) . ? Cd1 N5 2.314(4) . ? Cd1 N3 2.322(3) 2_445 ? Cd1 O4 2.500(2) . ? Cd1 C1 2.746(4) . ? Cd2 O7 2.240(2) 1_655 ? Cd2 O5 2.252(3) 4_565 ? Cd2 N9 2.285(3) 4_565 ? Cd2 O1 2.335(3) . ? Cd2 N1 2.360(3) . ? Cd2 O2 2.440(3) . ? Cd2 C9 2.728(4) . ? C1 O4 1.239(4) . ? C1 O3 1.280(4) . ? C1 C2 1.497(5) . ? C2 C3 1.377(5) . ? C2 C7 1.388(4) . ? C3 C4 1.364(5) . ? C3 H3 0.9300 . ? C4 C5 1.386(5) . ? C4 H4 0.9300 . ? C5 C6 1.379(4) . ? C5 H5 0.9300 . ? C6 C7 1.381(5) . ? C6 C8 1.515(5) . ? C7 H7 0.9300 . ? C8 O5 1.237(4) . ? C8 O6 1.241(4) . ? C9 O2 1.246(4) . ? C9 O1 1.257(4) . ? C9 C10 1.506(5) . ? C10 C11 1.383(5) . ? C10 C15 1.387(4) . ? C11 C12 1.375(5) . ? C11 H11 0.9300 . ? C12 C13 1.377(5) . ? C12 H12 0.9300 . ? C13 C14 1.369(4) . ? C13 H13 0.9300 . ? C14 C15 1.387(4) . ? C14 C16 1.501(5) . ? C15 H15 0.9300 . ? C16 O8 1.233(4) . ? C16 O7 1.250(4) . ? C17 N1 1.337(4) . ? C17 N3 1.350(5) . ? C17 H17 0.9300 . ? C18 N2 1.306(4) . ? C18 N3 1.314(5) . ? C18 H18 0.9300 . ? C19 N2 1.476(4) . ? C19 C20 1.512(5) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 C27 1.373(6) . ? C20 C21 1.389(6) . ? C21 C22 1.410(6) . ? C21 C24 1.509(6) . ? C22 C23 1.383(6) . ? C22 C32 1.511(6) . ? C23 C26 1.395(6) . ? C23 C25 1.528(5) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C27 1.412(6) . ? C26 C29 1.504(6) . ? C27 C28 1.499(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 N4 1.467(5) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 N5 1.263(9) . ? C30 N4 1.269(8) . ? C30 C31 1.908(14) . ? C30 H30 0.9300 . ? C31 N5 1.300(10) . ? C31 N6 1.317(9) . ? C31 H31 0.9300 . ? N6 N4 1.256(7) . ? N6' C31' 1.39(3) . ? N6' N4 1.57(2) . ? C30' N5 1.32(5) . ? C30' N4 1.40(5) . ? C30' H30' 0.9300 . ? C31' N5 1.34(3) . ? C31' H31' 0.9300 . ? C32 N7 1.467(5) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N9 1.312(6) . ? C33 N8 1.342(6) . ? C33 H33 0.9300 . ? C34 N9 1.317(5) . ? C34 N7 1.320(5) . ? C34 H34 0.9300 . ? N1 N2 1.347(4) . ? N3 Cd1 2.322(3) 2_455 ? N7 N8 1.340(5) . ? N9 Cd2 2.285(3) 4_666 ? O5 Cd2 2.252(3) 4_666 ? O6 Cd1 2.222(2) 1_655 ? O7 Cd2 2.240(2) 1_455 ? O8 Cd1 2.210(3) 4_565 ? O2W H2A 0.816(19) . ? 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 O8 Cd1 O6 119.11(10) 4_666 1_455 ? O8 Cd1 O3 96.45(10) 4_666 . ? O6 Cd1 O3 144.39(10) 1_455 . ? O8 Cd1 N5 95.91(14) 4_666 . ? O6 Cd1 N5 87.09(13) 1_455 . ? O3 Cd1 N5 87.44(13) . . ? O8 Cd1 N3 100.41(12) 4_666 2_445 ? O6 Cd1 N3 86.39(11) 1_455 2_445 ? O3 Cd1 N3 89.14(11) . 2_445 ? N5 Cd1 N3 163.60(14) . 2_445 ? O8 Cd1 O4 150.82(9) 4_666 . ? O6 Cd1 O4 89.99(9) 1_455 . ? O3 Cd1 O4 54.41(8) . . ? N5 Cd1 O4 82.67(13) . . ? N3 Cd1 O4 82.30(11) 2_445 . ? O8 Cd1 C1 124.04(12) 4_666 . ? O6 Cd1 C1 116.78(12) 1_455 . ? O3 Cd1 C1 27.61(9) . . ? N5 Cd1 C1 84.23(14) . . ? N3 Cd1 C1 85.32(12) 2_445 . ? O4 Cd1 C1 26.79(9) . . ? O7 Cd2 O5 122.51(10) 1_655 4_565 ? O7 Cd2 N9 92.28(11) 1_655 4_565 ? O5 Cd2 N9 88.86(12) 4_565 4_565 ? O7 Cd2 O1 144.40(10) 1_655 . ? O5 Cd2 O1 92.88(10) 4_565 . ? N9 Cd2 O1 92.23(12) 4_565 . ? O7 Cd2 N1 88.54(10) 1_655 . ? O5 Cd2 N1 82.76(11) 4_565 . ? N9 Cd2 N1 170.54(13) 4_565 . ? O1 Cd2 N1 92.57(10) . . ? O7 Cd2 O2 89.92(9) 1_655 . ? O5 Cd2 O2 147.32(9) 4_565 . ? N9 Cd2 O2 94.23(12) 4_565 . ? O1 Cd2 O2 54.53(8) . . ? N1 Cd2 O2 95.20(10) . . ? O7 Cd2 C9 117.07(11) 1_655 . ? O5 Cd2 C9 120.22(11) 4_565 . ? N9 Cd2 C9 93.43(13) 4_565 . ? O1 Cd2 C9 27.36(9) . . ? N1 Cd2 C9 94.59(11) . . ? O2 Cd2 C9 27.17(9) . . ? O4 C1 O3 121.8(4) . . ? O4 C1 C2 120.4(4) . . ? O3 C1 C2 117.7(4) . . ? O4 C1 Cd1 65.5(2) . . ? O3 C1 Cd1 56.38(19) . . ? C2 C1 Cd1 173.8(3) . . ? C3 C2 C7 118.9(3) . . ? C3 C2 C1 119.5(3) . . ? C7 C2 C1 121.6(4) . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.3(4) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? C6 C5 C4 120.8(4) . . ? C6 C5 H5 119.6 . . ? C4 C5 H5 119.6 . . ? C5 C6 C7 118.9(3) . . ? C5 C6 C8 119.0(3) . . ? C7 C6 C8 122.1(3) . . ? C6 C7 C2 120.8(3) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? O5 C8 O6 125.0(4) . . ? O5 C8 C6 118.4(4) . . ? O6 C8 C6 116.5(4) . . ? O2 C9 O1 122.0(4) . . ? O2 C9 C10 119.6(4) . . ? O1 C9 C10 118.4(3) . . ? O2 C9 Cd2 63.4(2) . . ? O1 C9 Cd2 58.60(19) . . ? C10 C9 Cd2 177.0(3) . . ? C11 C10 C15 119.1(3) . . ? C11 C10 C9 119.8(3) . . ? C15 C10 C9 121.1(3) . . ? C12 C11 C10 120.3(3) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C13 C12 C11 119.9(4) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C14 C13 C12 120.8(3) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 119.2(3) . . ? C13 C14 C16 119.2(3) . . ? C15 C14 C16 121.6(3) . . ? C14 C15 C10 120.6(3) . . ? C14 C15 H15 119.7 . . ? C10 C15 H15 119.7 . . ? O8 C16 O7 122.8(4) . . ? O8 C16 C14 119.6(4) . . ? O7 C16 C14 117.6(4) . . ? N1 C17 N3 113.7(4) . . ? N1 C17 H17 123.1 . . ? N3 C17 H17 123.1 . . ? N2 C18 N3 112.5(4) . . ? N2 C18 H18 123.8 . . ? N3 C18 H18 123.8 . . ? N2 C19 C20 110.7(3) . . ? N2 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.1 . . ? C27 C20 C21 121.5(4) . . ? C27 C20 C19 119.5(4) . . ? C21 C20 C19 119.0(5) . . ? C20 C21 C22 119.5(4) . . ? C20 C21 C24 121.1(5) . . ? C22 C21 C24 119.4(4) . . ? C23 C22 C21 119.2(4) . . ? C23 C22 C32 119.5(5) . . ? C21 C22 C32 121.2(5) . . ? C22 C23 C26 120.7(4) . . ? C22 C23 C25 118.4(4) . . ? C26 C23 C25 120.8(5) . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 C27 119.6(5) . . ? C23 C26 C29 119.9(5) . . ? C27 C26 C29 120.4(5) . . ? C20 C27 C26 119.1(4) . . ? C20 C27 C28 121.2(5) . . ? C26 C27 C28 119.7(5) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N4 C29 C26 111.4(4) . . ? N4 C29 H29A 109.3 . . ? C26 C29 H29A 109.3 . . ? N4 C29 H29B 109.3 . . ? C26 C29 H29B 109.3 . . ? H29A C29 H29B 108.0 . . ? N5 C30 N4 118.6(7) . . ? N5 C30 C31 42.6(4) . . ? N4 C30 C31 76.4(5) . . ? N5 C30 H30 120.7 . . ? N4 C30 H30 120.7 . . ? C31 C30 H30 162.0 . . ? N5 C31 N6 115.1(8) . . ? N5 C31 C30 41.1(4) . . ? N6 C31 C30 74.4(6) . . ? N5 C31 H31 122.5 . . ? N6 C31 H31 122.5 . . ? C30 C31 H31 162.3 . . ? N4 N6 C31 104.0(6) . . ? C31' N6' N4 98.4(18) . . ? N5 C30' N4 106(3) . . ? N5 C30' H30' 126.8 . . ? N4 C30' H30' 126.8 . . ? N5 C31' N6' 113(2) . . ? N5 C31' H31' 123.4 . . ? N6' C31' H31' 123.4 . . ? N7 C32 C22 112.4(4) . . ? N7 C32 H32A 109.1 . . ? C22 C32 H32A 109.1 . . ? N7 C32 H32B 109.1 . . ? C22 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? N9 C33 N8 115.5(5) . . ? N9 C33 H33 122.3 . . ? N8 C33 H33 122.3 . . ? N9 C34 N7 111.5(4) . . ? N9 C34 H34 124.2 . . ? N7 C34 H34 124.2 . . ? C17 N1 N2 102.7(3) . . ? C17 N1 Cd2 128.2(3) . . ? N2 N1 Cd2 128.9(3) . . ? C18 N2 N1 109.1(3) . . ? C18 N2 C19 129.2(3) . . ? N1 N2 C19 121.7(3) . . ? C18 N3 C17 102.0(3) . . ? C18 N3 Cd1 115.3(3) . 2_455 ? C17 N3 Cd1 141.7(3) . 2_455 ? N6 N4 C30 105.2(6) . . ? N6 N4 C30' 86(2) . . ? C30 N4 C30' 36.3(17) . . ? N6 N4 C29 117.3(6) . . ? C30 N4 C29 136.9(6) . . ? C30' N4 C29 136(2) . . ? N6 N4 N6' 76.5(9) . . ? C30 N4 N6' 83.0(11) . . ? C30' N4 N6' 108(2) . . ? C29 N4 N6' 112.6(10) . . ? C30 N5 C31 96.3(6) . . ? C30 N5 C30' 37.8(19) . . ? C31 N5 C30' 78(2) . . ? C30 N5 C31' 86.8(13) . . ? C31 N5 C31' 75.1(11) . . ? C30' N5 C31' 113(3) . . ? C30 N5 Cd1 132.8(5) . . ? C31 N5 Cd1 125.5(6) . . ? C30' N5 Cd1 124(2) . . ? C31' N5 Cd1 121.7(12) . . ? C34 N7 N8 109.2(4) . . ? C34 N7 C32 133.5(4) . . ? N8 N7 C32 117.3(4) . . ? C33 N8 N7 101.7(4) . . ? C34 N9 C33 102.2(4) . . ? C34 N9 Cd2 134.4(3) . 4_666 ? C33 N9 Cd2 123.4(4) . 4_666 ? C9 O1 Cd2 94.0(2) . . ? C9 O2 Cd2 89.4(2) . . ? C1 O3 Cd1 96.0(2) . . ? C1 O4 Cd1 87.8(2) . . ? C8 O5 Cd2 148.0(3) . 4_666 ? C8 O6 Cd1 116.3(2) . 1_655 ? C16 O7 Cd2 114.1(2) . 1_455 ? C16 O8 Cd1 159.0(3) . 4_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O8 Cd1 C1 O4 -178.4(2) 4_666 . . . ? O6 Cd1 C1 O4 -1.4(3) 1_455 . . . ? O3 Cd1 C1 O4 179.3(4) . . . . ? N5 Cd1 C1 O4 -85.2(2) . . . . ? N3 Cd1 C1 O4 82.2(2) 2_445 . . . ? O8 Cd1 C1 O3 2.3(3) 4_666 . . . ? O6 Cd1 C1 O3 179.3(2) 1_455 . . . ? N5 Cd1 C1 O3 95.5(3) . . . . ? N3 Cd1 C1 O3 -97.1(2) 2_445 . . . ? O4 Cd1 C1 O3 -179.3(4) . . . . ? O8 Cd1 C1 C2 -17(3) 4_666 . . . ? O6 Cd1 C1 C2 160(3) 1_455 . . . ? O3 Cd1 C1 C2 -19(3) . . . . ? N5 Cd1 C1 C2 76(3) . . . . ? N3 Cd1 C1 C2 -117(3) 2_445 . . . ? O4 Cd1 C1 C2 161(3) . . . . ? O4 C1 C2 C3 4.7(6) . . . . ? O3 C1 C2 C3 -173.7(4) . . . . ? Cd1 C1 C2 C3 -155(2) . . . . ? O4 C1 C2 C7 -176.0(4) . . . . ? O3 C1 C2 C7 5.5(6) . . . . ? Cd1 C1 C2 C7 24(3) . . . . ? C7 C2 C3 C4 1.2(6) . . . . ? C1 C2 C3 C4 -179.6(4) . . . . ? C2 C3 C4 C5 -0.5(6) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? C4 C5 C6 C7 1.1(6) . . . . ? C4 C5 C6 C8 -177.3(3) . . . . ? C5 C6 C7 C2 -0.5(6) . . . . ? C8 C6 C7 C2 177.9(3) . . . . ? C3 C2 C7 C6 -0.7(6) . . . . ? C1 C2 C7 C6 -179.9(3) . . . . ? C5 C6 C8 O5 -172.2(4) . . . . ? C7 C6 C8 O5 9.4(5) . . . . ? C5 C6 C8 O6 7.1(5) . . . . ? C7 C6 C8 O6 -171.2(4) . . . . ? O7 Cd2 C9 O2 -1.7(2) 1_655 . . . ? O5 Cd2 C9 O2 -176.74(19) 4_565 . . . ? N9 Cd2 C9 O2 92.6(2) 4_565 . . . ? O1 Cd2 C9 O2 -179.2(4) . . . . ? N1 Cd2 C9 O2 -92.5(2) . . . . ? O7 Cd2 C9 O1 177.4(2) 1_655 . . . ? O5 Cd2 C9 O1 2.5(3) 4_565 . . . ? N9 Cd2 C9 O1 -88.2(2) 4_565 . . . ? N1 Cd2 C9 O1 86.7(2) . . . . ? O2 Cd2 C9 O1 179.2(4) . . . . ? O7 Cd2 C9 C10 -177(100) 1_655 . . . ? O5 Cd2 C9 C10 8(5) 4_565 . . . ? N9 Cd2 C9 C10 -82(5) 4_565 . . . ? O1 Cd2 C9 C10 6(5) . . . . ? N1 Cd2 C9 C10 93(5) . . . . ? O2 Cd2 C9 C10 -175(5) . . . . ? O2 C9 C10 C11 9.0(6) . . . . ? O1 C9 C10 C11 -170.5(4) . . . . ? Cd2 C9 C10 C11 -176(100) . . . . ? O2 C9 C10 C15 -170.3(3) . . . . ? O1 C9 C10 C15 10.2(5) . . . . ? Cd2 C9 C10 C15 4(5) . . . . ? C15 C10 C11 C12 -0.9(6) . . . . ? C9 C10 C11 C12 179.8(4) . . . . ? C10 C11 C12 C13 1.6(6) . . . . ? C11 C12 C13 C14 -0.4(6) . . . . ? C12 C13 C14 C15 -1.5(6) . . . . ? C12 C13 C14 C16 -179.5(4) . . . . ? C13 C14 C15 C10 2.2(6) . . . . ? C16 C14 C15 C10 -179.9(3) . . . . ? C11 C10 C15 C14 -1.0(5) . . . . ? C9 C10 C15 C14 178.3(3) . . . . ? C13 C14 C16 O8 164.0(4) . . . . ? C15 C14 C16 O8 -13.9(5) . . . . ? C13 C14 C16 O7 -13.9(5) . . . . ? C15 C14 C16 O7 168.2(3) . . . . ? N2 C19 C20 C27 78.6(5) . . . . ? N2 C19 C20 C21 -98.9(4) . . . . ? C27 C20 C21 C22 3.7(6) . . . . ? C19 C20 C21 C22 -178.8(4) . . . . ? C27 C20 C21 C24 -176.5(4) . . . . ? C19 C20 C21 C24 0.9(6) . . . . ? C20 C21 C22 C23 1.7(6) . . . . ? C24 C21 C22 C23 -178.0(4) . . . . ? C20 C21 C22 C32 -174.2(4) . . . . ? C24 C21 C22 C32 6.1(6) . . . . ? C21 C22 C23 C26 -5.9(6) . . . . ? C32 C22 C23 C26 170.1(4) . . . . ? C21 C22 C23 C25 173.0(4) . . . . ? C32 C22 C23 C25 -11.1(6) . . . . ? C22 C23 C26 C27 4.7(6) . . . . ? C25 C23 C26 C27 -174.1(4) . . . . ? C22 C23 C26 C29 -172.5(4) . . . . ? C25 C23 C26 C29 8.6(6) . . . . ? C21 C20 C27 C26 -4.9(6) . . . . ? C19 C20 C27 C26 177.7(4) . . . . ? C21 C20 C27 C28 174.6(4) . . . . ? C19 C20 C27 C28 -2.8(6) . . . . ? C23 C26 C27 C20 0.6(6) . . . . ? C29 C26 C27 C20 177.9(4) . . . . ? C23 C26 C27 C28 -178.8(4) . . . . ? C29 C26 C27 C28 -1.6(6) . . . . ? C23 C26 C29 N4 -94.5(5) . . . . ? C27 C26 C29 N4 88.2(5) . . . . ? N4 C30 C31 N5 -172.1(11) . . . . ? N5 C30 C31 N6 171.7(14) . . . . ? N4 C30 C31 N6 -0.4(9) . . . . ? N5 C31 N6 N4 6.4(17) . . . . ? C30 C31 N6 N4 0.4(9) . . . . ? N4 N6' C31' N5 6(2) . . . . ? C23 C22 C32 N7 85.7(5) . . . . ? C21 C22 C32 N7 -98.5(5) . . . . ? N3 C17 N1 N2 -1.0(5) . . . . ? N3 C17 N1 Cd2 -176.6(2) . . . . ? O7 Cd2 N1 C17 125.4(3) 1_655 . . . ? O5 Cd2 N1 C17 2.4(3) 4_565 . . . ? N9 Cd2 N1 C17 30.3(9) 4_565 . . . ? O1 Cd2 N1 C17 -90.2(3) . . . . ? O2 Cd2 N1 C17 -144.8(3) . . . . ? C9 Cd2 N1 C17 -117.5(3) . . . . ? O7 Cd2 N1 N2 -49.0(3) 1_655 . . . ? O5 Cd2 N1 N2 -172.1(3) 4_565 . . . ? N9 Cd2 N1 N2 -144.2(7) 4_565 . . . ? O1 Cd2 N1 N2 95.3(3) . . . . ? O2 Cd2 N1 N2 40.7(3) . . . . ? C9 Cd2 N1 N2 68.0(3) . . . . ? N3 C18 N2 N1 0.4(5) . . . . ? N3 C18 N2 C19 179.4(4) . . . . ? C17 N1 N2 C18 0.4(4) . . . . ? Cd2 N1 N2 C18 175.9(3) . . . . ? C17 N1 N2 C19 -178.7(4) . . . . ? Cd2 N1 N2 C19 -3.2(5) . . . . ? C20 C19 N2 C18 24.3(6) . . . . ? C20 C19 N2 N1 -156.8(4) . . . . ? N2 C18 N3 C17 -1.0(5) . . . . ? N2 C18 N3 Cd1 169.8(3) . . . 2_455 ? N1 C17 N3 C18 1.2(5) . . . . ? N1 C17 N3 Cd1 -165.2(3) . . . 2_455 ? C31 N6 N4 C30 -0.6(14) . . . . ? C31 N6 N4 C30' 31(2) . . . . ? C31 N6 N4 C29 172.1(9) . . . . ? C31 N6 N4 N6' -79.3(13) . . . . ? N5 C30 N4 N6 -5.7(13) . . . . ? C31 C30 N4 N6 0.4(9) . . . . ? N5 C30 N4 C30' -67(4) . . . . ? C31 C30 N4 C30' -61(4) . . . . ? N5 C30 N4 C29 -176.1(6) . . . . ? C31 C30 N4 C29 -170.0(8) . . . . ? N5 C30 N4 N6' 68.2(13) . . . . ? C31 C30 N4 N6' 74.3(11) . . . . ? N5 C30' N4 N6 -69(3) . . . . ? N5 C30' N4 C30 53(3) . . . . ? N5 C30' N4 C29 164.6(12) . . . . ? N5 C30' N4 N6' 6(4) . . . . ? C26 C29 N4 N6 -156.0(8) . . . . ? C26 C29 N4 C30 13.6(12) . . . . ? C26 C29 N4 C30' -40(3) . . . . ? C26 C29 N4 N6' 118.1(11) . . . . ? C31' N6' N4 N6 74.1(16) . . . . ? C31' N6' N4 C30 -33.4(16) . . . . ? C31' N6' N4 C30' -7(3) . . . . ? C31' N6' N4 C29 -171.5(14) . . . . ? N4 C30 N5 C31 8.7(12) . . . . ? N4 C30 N5 C30' 70(4) . . . . ? C31 C30 N5 C30' 61(4) . . . . ? N4 C30 N5 C31' -65.9(14) . . . . ? C31 C30 N5 C31' -74.7(11) . . . . ? N4 C30 N5 Cd1 162.5(5) . . . . ? C31 C30 N5 Cd1 153.8(11) . . . . ? N6 C31 N5 C30 -8.8(15) . . . . ? N6 C31 N5 C30' -42(2) . . . . ? C30 C31 N5 C30' -33(2) . . . . ? N6 C31 N5 C31' 76.2(17) . . . . ? C30 C31 N5 C31' 85.0(13) . . . . ? N6 C31 N5 Cd1 -165.3(9) . . . . ? C30 C31 N5 Cd1 -156.5(9) . . . . ? N4 C30' N5 C30 -51(3) . . . . ? N4 C30' N5 C31 66(3) . . . . ? N4 C30' N5 C31' -2(4) . . . . ? N4 C30' N5 Cd1 -169.0(14) . . . . ? N6' C31' N5 C30 24.2(19) . . . . ? N6' C31' N5 C31 -73.1(19) . . . . ? N6' C31' N5 C30' -4(3) . . . . ? N6' C31' N5 Cd1 164.0(15) . . . . ? O8 Cd1 N5 C30 108.7(9) 4_666 . . . ? O6 Cd1 N5 C30 -132.3(9) 1_455 . . . ? O3 Cd1 N5 C30 12.5(9) . . . . ? N3 Cd1 N5 C30 -65.6(11) 2_445 . . . ? O4 Cd1 N5 C30 -41.9(9) . . . . ? C1 Cd1 N5 C30 -15.0(9) . . . . ? O8 Cd1 N5 C31 -103.9(10) 4_666 . . . ? O6 Cd1 N5 C31 15.0(10) 1_455 . . . ? O3 Cd1 N5 C31 159.8(10) . . . . ? N3 Cd1 N5 C31 81.7(11) 2_445 . . . ? O4 Cd1 N5 C31 105.4(10) . . . . ? C1 Cd1 N5 C31 132.3(10) . . . . ? O8 Cd1 N5 C30' 156(3) 4_666 . . . ? O6 Cd1 N5 C30' -85(3) 1_455 . . . ? O3 Cd1 N5 C30' 60(3) . . . . ? N3 Cd1 N5 C30' -18(3) 2_445 . . . ? O4 Cd1 N5 C30' 6(3) . . . . ? C1 Cd1 N5 C30' 33(3) . . . . ? O8 Cd1 N5 C31' -9.9(14) 4_666 . . . ? O6 Cd1 N5 C31' 109.0(14) 1_455 . . . ? O3 Cd1 N5 C31' -106.2(14) . . . . ? N3 Cd1 N5 C31' 175.7(14) 2_445 . . . ? O4 Cd1 N5 C31' -160.6(14) . . . . ? C1 Cd1 N5 C31' -133.7(14) . . . . ? N9 C34 N7 N8 -1.8(7) . . . . ? N9 C34 N7 C32 175.7(5) . . . . ? C22 C32 N7 C34 15.3(8) . . . . ? C22 C32 N7 N8 -167.3(5) . . . . ? N9 C33 N8 N7 0.8(9) . . . . ? C34 N7 N8 C33 0.6(7) . . . . ? C32 N7 N8 C33 -177.4(5) . . . . ? N7 C34 N9 C33 2.1(6) . . . . ? N7 C34 N9 Cd2 -177.8(3) . . . 4_666 ? N8 C33 N9 C34 -1.8(8) . . . . ? N8 C33 N9 Cd2 178.1(5) . . . 4_666 ? O2 C9 O1 Cd2 0.9(4) . . . . ? C10 C9 O1 Cd2 -179.6(3) . . . . ? O7 Cd2 O1 C9 -3.9(3) 1_655 . . . ? O5 Cd2 O1 C9 -177.9(2) 4_565 . . . ? N9 Cd2 O1 C9 93.2(2) 4_565 . . . ? N1 Cd2 O1 C9 -95.0(2) . . . . ? O2 Cd2 O1 C9 -0.5(2) . . . . ? O1 C9 O2 Cd2 -0.8(4) . . . . ? C10 C9 O2 Cd2 179.7(3) . . . . ? O7 Cd2 O2 C9 178.4(2) 1_655 . . . ? O5 Cd2 O2 C9 5.2(3) 4_565 . . . ? N9 Cd2 O2 C9 -89.3(2) 4_565 . . . ? O1 Cd2 O2 C9 0.5(2) . . . . ? N1 Cd2 O2 C9 89.9(2) . . . . ? O4 C1 O3 Cd1 -0.7(4) . . . . ? C2 C1 O3 Cd1 177.7(3) . . . . ? O8 Cd1 O3 C1 -178.1(2) 4_666 . . . ? O6 Cd1 O3 C1 -1.0(3) 1_455 . . . ? N5 Cd1 O3 C1 -82.4(3) . . . . ? N3 Cd1 O3 C1 81.5(2) 2_445 . . . ? O4 Cd1 O3 C1 0.4(2) . . . . ? O3 C1 O4 Cd1 0.7(4) . . . . ? C2 C1 O4 Cd1 -177.7(3) . . . . ? O8 Cd1 O4 C1 2.7(4) 4_666 . . . ? O6 Cd1 O4 C1 178.8(2) 1_455 . . . ? O3 Cd1 O4 C1 -0.4(2) . . . . ? N5 Cd1 O4 C1 91.7(3) . . . . ? N3 Cd1 O4 C1 -94.9(2) 2_445 . . . ? O6 C8 O5 Cd2 83.4(6) . . . 4_666 ? C6 C8 O5 Cd2 -97.3(5) . . . 4_666 ? O5 C8 O6 Cd1 -1.0(5) . . . 1_655 ? C6 C8 O6 Cd1 179.7(2) . . . 1_655 ? O8 C16 O7 Cd2 -4.8(5) . . . 1_455 ? C14 C16 O7 Cd2 173.0(2) . . . 1_455 ? O7 C16 O8 Cd1 -90.7(8) . . . 4_565 ? C14 C16 O8 Cd1 91.5(8) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.850 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.594 _refine_diff_density_min -0.605 _refine_diff_density_rms 0.081 data_5 _database_code_depnum_ccdc_archive 'CCDC 904155' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H56 N18 O13 Zn3' _chemical_formula_weight 1433.34 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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.3713(14) _cell_length_b 14.7967(17) _cell_length_c 16.661(2) _cell_angle_alpha 103.393(8) _cell_angle_beta 102.889(7) _cell_angle_gamma 105.532(2) _cell_volume 2943.3(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 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 1.297 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7376 _exptl_absorpt_correction_T_max 0.8001 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 44601 _diffrn_reflns_av_R_equivalents 0.1266 _diffrn_reflns_av_sigmaI/netI 0.0908 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.21 _reflns_number_total 10468 _reflns_number_gt 5766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. The distances of O1W---H1A and O1W---H1B were restrained to 0.89+-0.02 \%A. The distance of H1A...H1B was restrained to 1.44+-0.02 \%A. ; _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^)+(0.0945P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10468 _refine_ls_number_parameters 863 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1316 _refine_ls_R_factor_gt 0.0660 _refine_ls_wR_factor_ref 0.1854 _refine_ls_wR_factor_gt 0.1516 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _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 0.70891(6) 0.31706(6) 0.52097(5) 0.0495(2) Uani 1 1 d . . . Zn2 Zn 1.31894(6) 0.36535(6) 1.14223(5) 0.0458(2) Uani 1 1 d . . . Zn3 Zn 1.28214(6) -0.01108(6) 0.81784(5) 0.0482(2) Uani 1 1 d . . . C1 C 1.1194(5) 0.0301(5) 0.7263(5) 0.0441(16) Uani 1 1 d . . . C2 C 1.0467(4) 0.0879(4) 0.6993(4) 0.0362(13) Uani 1 1 d . . . C3 C 1.0341(5) 0.1617(5) 0.7596(4) 0.0396(14) Uani 1 1 d . . . H3 H 1.0708 0.1769 0.8180 0.048 Uiso 1 1 calc R . . C4 C 0.9671(5) 0.2136(5) 0.7338(4) 0.0407(14) Uani 1 1 d . . . H4 H 0.9582 0.2628 0.7750 0.049 Uiso 1 1 calc R . . C5 C 0.9127(5) 0.1920(4) 0.6458(4) 0.0378(14) Uani 1 1 d . . . C6 C 0.9265(5) 0.1193(5) 0.5860(4) 0.0446(15) Uani 1 1 d . . . H6 H 0.8916 0.1053 0.5274 0.054 Uiso 1 1 calc R . . C7 C 0.9923(5) 0.0661(5) 0.6121(4) 0.0434(15) Uani 1 1 d . . . H7 H 0.9999 0.0159 0.5711 0.052 Uiso 1 1 calc R . . C8 C 0.8403(5) 0.2510(5) 0.6203(5) 0.0442(16) Uani 1 1 d . . . C9 C 0.5834(7) 0.2389(5) 0.3562(5) 0.0550(18) Uani 1 1 d . . . C10 C 0.5491(5) 0.2130(5) 0.2572(4) 0.0417(15) Uani 1 1 d . . . C11 C 0.4621(5) 0.1274(5) 0.2081(4) 0.0486(16) Uani 1 1 d . . . H11 H 0.4234 0.0897 0.2359 0.058 Uiso 1 1 calc R . . C12 C 0.4327(5) 0.0980(5) 0.1202(4) 0.0425(15) Uani 1 1 d . . . H12 H 0.3753 0.0398 0.0885 0.051 Uiso 1 1 calc R . . C13 C 0.4878(5) 0.1543(5) 0.0771(4) 0.0381(14) Uani 1 1 d . . . C14 C 0.5725(5) 0.2407(5) 0.1265(4) 0.0446(15) Uani 1 1 d . . . H14 H 0.6094 0.2801 0.0990 0.053 Uiso 1 1 calc R . . C15 C 0.6031(5) 0.2693(5) 0.2153(4) 0.0474(16) Uani 1 1 d . . . H15 H 0.6607 0.3273 0.2472 0.057 Uiso 1 1 calc R . . C16 C 0.4555(7) 0.1239(6) -0.0199(5) 0.0557(18) Uani 1 1 d . . . C17 C 1.1723(5) 0.4191(5) 1.0501(5) 0.0397(15) Uani 1 1 d . . . C18 C 1.0825(5) 0.4625(4) 1.0246(4) 0.0377(14) Uani 1 1 d . . . C19 C 1.0586(5) 0.5263(5) 1.0866(4) 0.0421(15) Uani 1 1 d . . . H19 H 1.0973 0.5437 1.1449 0.051 Uiso 1 1 calc R . . C20 C 0.9772(5) 0.5637(5) 1.0615(4) 0.0410(14) Uani 1 1 d . . . H20 H 0.9622 0.6074 1.1031 0.049 Uiso 1 1 calc R . . C21 C 1.3611(5) 0.3929(5) 1.3240(4) 0.0477(16) Uani 1 1 d . . . C22 C 1.4348(5) 0.4471(4) 1.4147(4) 0.0368(14) Uani 1 1 d . . . C23 C 1.5411(5) 0.5058(5) 1.4310(4) 0.0464(16) Uani 1 1 d . . . H23 H 1.5702 0.5091 1.3855 0.056 Uiso 1 1 calc R . . C24 C 1.6046(5) 0.5600(5) 1.5159(4) 0.0431(15) Uani 1 1 d . . . H24 H 1.6750 0.6019 1.5262 0.052 Uiso 1 1 calc R . . C25 C 1.1516(6) -0.2335(5) 0.7810(5) 0.062(2) Uani 1 1 d . . . H25 H 1.1226 -0.2470 0.7217 0.075 Uiso 1 1 calc R . . C26 C 1.2401(5) -0.1563(5) 0.9116(4) 0.0435(15) Uani 1 1 d . . . H26 H 1.2851 -0.1077 0.9630 0.052 Uiso 1 1 calc R . . C27 C 1.1797(6) -0.2954(5) 0.9730(4) 0.0467(16) Uani 1 1 d . . . H27A H 1.2360 -0.3253 0.9808 0.056 Uiso 1 1 calc R . . H27B H 1.1096 -0.3473 0.9549 0.056 Uiso 1 1 calc R . . C28 C 1.1935(5) -0.2213(4) 1.0584(4) 0.0390(14) Uani 1 1 d . . . C29 C 1.1304(4) -0.1598(4) 1.0597(4) 0.0375(14) Uani 1 1 d . . . C30 C 1.0334(5) -0.1802(5) 0.9807(5) 0.0494(17) Uani 1 1 d . . . H30A H 1.0494 -0.1292 0.9541 0.074 Uiso 1 1 calc R . . H30B H 0.9699 -0.1812 0.9988 0.074 Uiso 1 1 calc R . . H30C H 1.0202 -0.2428 0.9398 0.074 Uiso 1 1 calc R . . C31 C 1.1538(4) -0.0813(4) 1.1350(4) 0.0382(14) Uani 1 1 d . . . C32 C 1.0947(5) -0.0075(5) 1.1329(4) 0.0418(14) Uani 1 1 d . . . H32A H 1.0217 -0.0402 1.0927 0.050 Uiso 1 1 calc R . . H32B H 1.0886 0.0187 1.1899 0.050 Uiso 1 1 calc R . . C33 C 1.2168(5) 0.1481(5) 1.0248(4) 0.0412(14) Uani 1 1 d . . . H33 H 1.2352 0.1616 0.9772 0.049 Uiso 1 1 calc R . . C34 C 1.2041(5) 0.1697(5) 1.1504(4) 0.0414(15) Uani 1 1 d . . . H34 H 1.2096 0.1980 1.2079 0.050 Uiso 1 1 calc R . . C35 C 1.2339(5) -0.0691(4) 1.2112(4) 0.0381(14) Uani 1 1 d . . . C36 C 1.2889(5) -0.1379(4) 1.2110(4) 0.0383(14) Uani 1 1 d . . . C37 C 1.2705(5) -0.2133(5) 1.1352(5) 0.0429(16) Uani 1 1 d . . . C38 C 1.3297(6) -0.2875(5) 1.1350(5) 0.0555(18) Uani 1 1 d . . . H38A H 1.2852 -0.3455 1.1429 0.083 Uiso 1 1 calc R . . H38B H 1.3972 -0.2590 1.1813 0.083 Uiso 1 1 calc R . . H38C H 1.3444 -0.3050 1.0807 0.083 Uiso 1 1 calc R . . C39 C 1.2546(5) 0.0115(5) 1.2926(4) 0.0508(17) Uani 1 1 d . . . H39A H 1.2498 0.0699 1.2787 0.076 Uiso 1 1 calc R . . H39B H 1.3261 0.0253 1.3306 0.076 Uiso 1 1 calc R . . H39C H 1.2012 -0.0091 1.3208 0.076 Uiso 1 1 calc R . . C40 C 1.3723(5) -0.1279(5) 1.2942(4) 0.0463(16) Uani 1 1 d . . . H40A H 1.3539 -0.0956 1.3437 0.056 Uiso 1 1 calc R . . H40B H 1.3711 -0.1929 1.2971 0.056 Uiso 1 1 calc R . . C41 C 1.6433(6) 0.0261(5) 1.3493(5) 0.0524(18) Uani 1 1 d . . . H41 H 1.7097 0.0696 1.3881 0.063 Uiso 1 1 calc R . . C42 C 1.5223(5) -0.0628(5) 1.2328(4) 0.0439(15) Uani 1 1 d . . . H42 H 1.4837 -0.0949 1.1746 0.053 Uiso 1 1 calc R . . C45 C 0.3418(6) 0.1976(5) 0.6190(6) 0.0567(19) Uani 1 1 d . . . H45A H 0.3528 0.1664 0.6638 0.068 Uiso 1 1 calc R . . H45B H 0.3042 0.1459 0.5640 0.068 Uiso 1 1 calc R . . C46 C 0.2713(5) 0.2598(4) 0.6365(4) 0.0409(15) Uani 1 1 d . . . C47 C 0.1998(5) 0.2723(5) 0.5698(4) 0.0460(16) Uani 1 1 d . . . C48 C 0.1414(5) 0.3369(5) 0.5900(5) 0.0473(17) Uani 1 1 d . . . C49 C 0.1628(5) 0.3915(5) 0.6737(5) 0.0520(18) Uani 1 1 d . . . C50 C 0.2347(5) 0.3782(5) 0.7419(5) 0.0488(16) Uani 1 1 d . . . C51 C 0.2845(5) 0.3081(5) 0.7237(4) 0.0428(15) Uani 1 1 d . . . C52 C 0.3495(6) 0.2825(6) 0.7966(5) 0.065(2) Uani 1 1 d . . . H52A H 0.4246 0.3233 0.8139 0.097 Uiso 1 1 calc R . . H52B H 0.3436 0.2144 0.7771 0.097 Uiso 1 1 calc R . . H52C H 0.3216 0.2937 0.8449 0.097 Uiso 1 1 calc R . . C53 C 0.1060(8) 0.4682(7) 0.6950(7) 0.085(3) Uani 1 1 d . . . H53A H 0.0729 0.4798 0.6427 0.127 Uiso 1 1 calc R . . H53B H 0.1589 0.5289 0.7349 0.127 Uiso 1 1 calc R . . H53C H 0.0510 0.4437 0.7205 0.127 Uiso 1 1 calc R . . C54 C 0.1819(8) 0.2152(6) 0.4756(5) 0.077(2) Uani 1 1 d . . . H54A H 0.2459 0.1994 0.4708 0.115 Uiso 1 1 calc R . . H54B H 0.1678 0.2550 0.4393 0.115 Uiso 1 1 calc R . . H54C H 0.1207 0.1554 0.4575 0.115 Uiso 1 1 calc R . . C55 C 0.2588(6) 0.4399(7) 0.8343(6) 0.074(2) Uani 1 1 d . . . H55A H 0.2113 0.4792 0.8363 0.088 Uiso 1 1 calc R . . H55B H 0.2436 0.3967 0.8692 0.088 Uiso 1 1 calc R . . C56 C 0.4527(5) 0.5224(5) 0.8345(5) 0.0499(16) Uani 1 1 d . . . H56 H 0.4447 0.4927 0.7767 0.060 Uiso 1 1 calc R . . C57 C 0.5156(6) 0.6079(6) 0.9643(5) 0.0584(19) Uani 1 1 d . . . H57 H 0.5644 0.6516 1.0168 0.070 Uiso 1 1 calc R . . C58 C 0.6021(5) 0.3623(5) 0.6622(4) 0.0452(16) Uani 1 1 d . . . H58 H 0.6640 0.4152 0.6973 0.054 Uiso 1 1 calc R . . C59 C 0.4952(5) 0.2427(5) 0.5561(5) 0.0486(16) Uani 1 1 d . . . H59 H 0.4640 0.1942 0.5024 0.058 Uiso 1 1 calc R . . C60 C 0.1711(5) 0.4997(5) 0.5069(5) 0.0531(18) Uani 1 1 d . . . H60 H 0.2063 0.5303 0.5658 0.064 Uiso 1 1 calc R . . C61 C 0.1193(5) 0.4696(5) 0.3733(5) 0.0548(18) Uani 1 1 d . . . H61 H 0.1125 0.4767 0.3185 0.066 Uiso 1 1 calc R . . C62 C 0.0547(6) 0.3399(6) 0.5161(6) 0.071(2) Uani 1 1 d . . . H62A H 0.0209 0.2746 0.4740 0.085 Uiso 1 1 calc R . . H62B H -0.0011 0.3576 0.5380 0.085 Uiso 1 1 calc R . . N1 N 1.2206(4) -0.1439(4) 0.8337(3) 0.0444(13) Uani 1 1 d . . . N2 N 1.1289(5) -0.2995(4) 0.8199(4) 0.0640(17) Uani 1 1 d . . . N3 N 1.1865(4) -0.2477(4) 0.9053(3) 0.0416(12) Uani 1 1 d . . . N4 N 1.2444(4) 0.2177(4) 1.1017(3) 0.0386(12) Uani 1 1 d . . . N5 N 1.1615(4) 0.0590(4) 1.0231(4) 0.0447(13) Uani 1 1 d . . . N6 N 1.1541(4) 0.0743(4) 1.1059(3) 0.0396(12) Uani 1 1 d . . . N7 N 1.5602(4) -0.0111(5) 1.3739(4) 0.0525(14) Uani 1 1 d . . . N8 N 1.6254(4) -0.0037(4) 1.2625(3) 0.0389(12) Uani 1 1 d . . . N9 N 1.4826(4) -0.0696(4) 1.2972(3) 0.0397(12) Uani 1 1 d . . . N10 N 0.5946(4) 0.3095(4) 0.5827(4) 0.0447(13) Uani 1 1 d . . . N11 N 0.4479(4) 0.2555(4) 0.6165(4) 0.0441(13) Uani 1 1 d . . . N12 N 0.5153(5) 0.3335(4) 0.6870(4) 0.0488(13) Uani 1 1 d . . . N13 N 0.3740(4) 0.5062(4) 0.8715(4) 0.0486(13) Uani 1 1 d . . . N14 N 0.4127(6) 0.5617(5) 0.9549(4) 0.0608(16) Uani 1 1 d . . . N15 N 0.5439(4) 0.5866(4) 0.8918(3) 0.0407(12) Uani 1 1 d . . . N16 N 0.0980(4) 0.4107(4) 0.4729(4) 0.0510(15) Uani 1 1 d . . . N17 N 0.1875(4) 0.5398(4) 0.4455(3) 0.0428(12) Uani 1 1 d . . . N18 N 0.0624(5) 0.3892(5) 0.3863(4) 0.0649(18) Uani 1 1 d . . . O1 O 1.1181(4) -0.0443(4) 0.6731(4) 0.0666(15) Uani 1 1 d . . . O2 O 1.1819(4) 0.0635(3) 0.8042(3) 0.0508(11) Uani 1 1 d . . . O3 O 0.7919(4) 0.2278(3) 0.5394(3) 0.0493(11) Uani 1 1 d . . . O4 O 0.8341(4) 0.3190(4) 0.6760(3) 0.0619(14) Uani 1 1 d . . . O5 O 0.6713(5) 0.3041(4) 0.3964(3) 0.0680(15) Uani 1 1 d . . . O6 O 0.5230(6) 0.1912(5) 0.3882(4) 0.092(2) Uani 1 1 d . . . O7 O 0.4794(12) 0.1846(7) -0.0599(6) 0.072(4) Uani 0.50 1 d P . . O7' O 0.5367(10) 0.1588(9) -0.0482(8) 0.065(3) Uiso 0.50 1 d P . . O8 O 0.3741(4) 0.0468(4) -0.0610(3) 0.0549(12) Uani 1 1 d . . . O9 O 1.2202(4) 0.4420(3) 1.1312(3) 0.0522(12) Uani 1 1 d . . . O10 O 1.1917(4) 0.3626(4) 0.9942(3) 0.0535(12) Uani 1 1 d . . . O11 O 1.4022(4) 0.4084(4) 1.2649(3) 0.0515(12) Uani 1 1 d . . . O12 O 1.2680(4) 0.3401(5) 1.3117(3) 0.0755(17) Uani 1 1 d . . . O1W O 1.0584(12) 0.1687(13) 1.2644(13) 0.232(7) Uani 1 1 d D . . H1B H 1.096(16) 0.229(10) 1.303(16) 0.349 Uiso 1 1 d D . . H1A H 0.988(6) 0.159(19) 1.262(19) 0.349 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zn1 0.0460(4) 0.0513(5) 0.0538(5) 0.0234(4) 0.0113(4) 0.0175(4) Zn2 0.0432(4) 0.0432(5) 0.0477(5) 0.0142(4) 0.0072(3) 0.0146(3) Zn3 0.0438(4) 0.0493(5) 0.0515(5) 0.0186(4) 0.0090(4) 0.0173(4) C1 0.037(3) 0.048(4) 0.061(4) 0.026(4) 0.025(3) 0.019(3) C2 0.028(3) 0.042(4) 0.043(3) 0.018(3) 0.013(3) 0.013(3) C3 0.033(3) 0.042(4) 0.040(3) 0.015(3) 0.005(3) 0.011(3) C4 0.039(3) 0.041(4) 0.042(4) 0.012(3) 0.011(3) 0.015(3) C5 0.032(3) 0.034(3) 0.049(4) 0.020(3) 0.011(3) 0.009(3) C6 0.043(3) 0.052(4) 0.040(3) 0.016(3) 0.006(3) 0.023(3) C7 0.042(3) 0.048(4) 0.043(4) 0.015(3) 0.013(3) 0.019(3) C8 0.035(3) 0.040(4) 0.061(4) 0.028(3) 0.010(3) 0.010(3) C9 0.071(5) 0.041(4) 0.056(4) 0.016(4) 0.014(4) 0.026(4) C10 0.051(4) 0.044(4) 0.029(3) 0.009(3) 0.004(3) 0.023(3) C11 0.049(4) 0.046(4) 0.050(4) 0.018(3) 0.013(3) 0.014(3) C12 0.036(3) 0.041(4) 0.044(4) 0.012(3) 0.002(3) 0.012(3) C13 0.038(3) 0.039(3) 0.036(3) 0.010(3) 0.010(3) 0.014(3) C14 0.038(3) 0.040(4) 0.058(4) 0.017(3) 0.018(3) 0.013(3) C15 0.046(4) 0.036(4) 0.045(4) 0.002(3) -0.001(3) 0.011(3) C16 0.076(5) 0.048(4) 0.049(4) 0.015(4) 0.026(4) 0.023(4) C17 0.033(3) 0.034(3) 0.059(4) 0.023(3) 0.014(3) 0.014(3) C18 0.034(3) 0.031(3) 0.048(4) 0.016(3) 0.008(3) 0.011(3) C19 0.037(3) 0.045(4) 0.044(4) 0.018(3) 0.006(3) 0.014(3) C20 0.042(3) 0.038(3) 0.047(4) 0.014(3) 0.017(3) 0.015(3) C21 0.045(4) 0.045(4) 0.046(4) 0.006(3) 0.007(3) 0.017(3) C22 0.040(3) 0.032(3) 0.036(3) 0.007(3) 0.007(3) 0.014(3) C23 0.046(4) 0.055(4) 0.044(4) 0.020(3) 0.018(3) 0.017(3) C24 0.038(3) 0.042(4) 0.040(4) 0.012(3) 0.004(3) 0.005(3) C25 0.071(5) 0.042(4) 0.050(4) 0.011(4) -0.005(4) 0.005(4) C26 0.047(3) 0.038(4) 0.045(4) 0.015(3) 0.012(3) 0.014(3) C27 0.053(4) 0.037(4) 0.058(4) 0.025(3) 0.019(3) 0.018(3) C28 0.036(3) 0.031(3) 0.053(4) 0.018(3) 0.015(3) 0.010(3) C29 0.028(3) 0.032(3) 0.051(4) 0.013(3) 0.009(3) 0.009(2) C30 0.039(3) 0.040(4) 0.060(4) 0.012(3) 0.003(3) 0.012(3) C31 0.028(3) 0.035(3) 0.056(4) 0.023(3) 0.018(3) 0.007(2) C32 0.038(3) 0.036(3) 0.052(4) 0.015(3) 0.012(3) 0.013(3) C33 0.034(3) 0.047(4) 0.048(4) 0.017(3) 0.015(3) 0.019(3) C34 0.047(3) 0.038(4) 0.037(3) 0.009(3) 0.009(3) 0.015(3) C35 0.031(3) 0.039(3) 0.045(4) 0.018(3) 0.013(3) 0.008(3) C36 0.030(3) 0.038(3) 0.047(4) 0.019(3) 0.009(3) 0.010(3) C37 0.030(3) 0.039(4) 0.066(4) 0.030(3) 0.016(3) 0.009(3) C38 0.055(4) 0.049(4) 0.070(5) 0.025(4) 0.013(4) 0.028(3) C39 0.045(4) 0.057(4) 0.053(4) 0.023(4) 0.016(3) 0.016(3) C40 0.037(3) 0.053(4) 0.053(4) 0.027(3) 0.014(3) 0.013(3) C41 0.043(4) 0.049(4) 0.051(4) 0.004(3) 0.001(3) 0.014(3) C42 0.040(3) 0.050(4) 0.038(3) 0.014(3) 0.003(3) 0.015(3) C45 0.049(4) 0.045(4) 0.085(5) 0.028(4) 0.029(4) 0.016(3) C46 0.034(3) 0.036(3) 0.056(4) 0.021(3) 0.015(3) 0.009(3) C47 0.040(3) 0.035(3) 0.060(4) 0.026(3) 0.013(3) 0.001(3) C48 0.029(3) 0.050(4) 0.065(5) 0.036(4) 0.008(3) 0.006(3) C49 0.033(3) 0.049(4) 0.079(5) 0.027(4) 0.026(3) 0.009(3) C50 0.035(3) 0.052(4) 0.061(4) 0.021(3) 0.023(3) 0.007(3) C51 0.038(3) 0.048(4) 0.048(4) 0.023(3) 0.020(3) 0.013(3) C52 0.064(5) 0.071(5) 0.065(5) 0.041(4) 0.015(4) 0.020(4) C53 0.076(6) 0.076(6) 0.141(9) 0.053(6) 0.062(6) 0.049(5) C54 0.086(6) 0.058(5) 0.064(5) 0.014(4) 0.012(4) 0.000(4) C55 0.054(4) 0.084(6) 0.074(6) 0.015(5) 0.036(4) 0.003(4) C56 0.047(4) 0.057(4) 0.047(4) 0.013(3) 0.021(3) 0.015(3) C57 0.063(5) 0.067(5) 0.038(4) 0.018(4) 0.015(3) 0.011(4) C58 0.046(4) 0.039(4) 0.053(4) 0.017(3) 0.012(3) 0.017(3) C59 0.050(4) 0.053(4) 0.047(4) 0.014(3) 0.018(3) 0.022(3) C60 0.044(4) 0.055(4) 0.048(4) 0.021(3) -0.001(3) 0.005(3) C61 0.047(4) 0.053(4) 0.058(4) 0.019(4) 0.003(3) 0.016(3) C62 0.043(4) 0.066(5) 0.103(7) 0.054(5) 0.006(4) 0.007(4) N1 0.044(3) 0.045(3) 0.044(3) 0.016(3) 0.007(2) 0.017(3) N2 0.075(4) 0.041(3) 0.054(4) 0.011(3) -0.001(3) 0.004(3) N3 0.042(3) 0.030(3) 0.048(3) 0.012(2) 0.008(2) 0.010(2) N4 0.039(3) 0.034(3) 0.040(3) 0.011(2) 0.002(2) 0.017(2) N5 0.038(3) 0.039(3) 0.049(3) 0.009(2) 0.006(2) 0.011(2) N6 0.041(3) 0.033(3) 0.042(3) 0.013(2) 0.005(2) 0.013(2) N7 0.042(3) 0.062(4) 0.047(3) 0.008(3) 0.013(3) 0.017(3) N8 0.030(3) 0.043(3) 0.041(3) 0.011(2) 0.005(2) 0.014(2) N9 0.035(3) 0.047(3) 0.040(3) 0.020(3) 0.011(2) 0.014(2) N10 0.040(3) 0.042(3) 0.056(4) 0.021(3) 0.014(3) 0.017(2) N11 0.042(3) 0.042(3) 0.055(3) 0.019(3) 0.019(3) 0.019(2) N12 0.049(3) 0.049(3) 0.054(3) 0.019(3) 0.022(3) 0.019(3) N13 0.048(3) 0.054(3) 0.047(3) 0.018(3) 0.023(3) 0.012(3) N14 0.077(4) 0.074(4) 0.040(3) 0.022(3) 0.027(3) 0.028(4) N15 0.042(3) 0.042(3) 0.036(3) 0.012(2) 0.007(2) 0.015(2) N16 0.035(3) 0.044(3) 0.068(4) 0.029(3) 0.000(3) 0.009(2) N17 0.038(3) 0.046(3) 0.046(3) 0.024(3) 0.008(2) 0.013(2) N18 0.057(4) 0.051(4) 0.066(4) 0.016(3) -0.008(3) 0.008(3) O1 0.062(3) 0.068(4) 0.072(3) 0.011(3) 0.011(3) 0.042(3) O2 0.046(2) 0.059(3) 0.052(3) 0.024(2) 0.007(2) 0.025(2) O3 0.050(3) 0.059(3) 0.044(3) 0.021(2) 0.008(2) 0.027(2) O4 0.071(3) 0.058(3) 0.061(3) 0.014(3) 0.010(3) 0.041(3) O5 0.069(3) 0.063(3) 0.055(3) 0.018(3) -0.005(3) 0.016(3) O6 0.131(6) 0.076(4) 0.051(3) 0.021(3) 0.027(4) 0.006(4) O7 0.135(11) 0.035(6) 0.035(5) 0.015(4) 0.027(6) 0.010(6) O8 0.044(3) 0.066(3) 0.047(3) 0.016(2) 0.007(2) 0.013(2) O9 0.049(3) 0.051(3) 0.057(3) 0.021(2) 0.004(2) 0.023(2) O10 0.055(3) 0.055(3) 0.066(3) 0.027(3) 0.022(2) 0.033(2) O11 0.057(3) 0.059(3) 0.039(2) 0.018(2) 0.010(2) 0.021(2) O12 0.043(3) 0.094(4) 0.049(3) -0.012(3) 0.005(2) -0.003(3) O1W 0.149(10) 0.206(15) 0.252(17) -0.043(11) 0.072(12) 0.009(10) _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 1.973(4) . ? Zn1 O5 1.974(5) . ? Zn1 N10 2.017(6) . ? Zn1 N17 2.062(5) 2_666 ? Zn2 O11 1.956(4) . ? Zn2 O9 1.963(4) . ? Zn2 N4 2.018(5) . ? Zn2 N15 2.035(5) 2_767 ? Zn3 O2 1.959(4) . ? Zn3 O8 1.962(5) 1_656 ? Zn3 N1 2.020(5) . ? Zn3 N8 2.024(5) 2_857 ? C1 O1 1.236(8) . ? C1 O2 1.275(8) . ? C1 C2 1.519(8) . ? C2 C3 1.377(9) . ? C2 C7 1.388(9) . ? C3 C4 1.388(8) . ? C3 H3 0.9300 . ? C4 C5 1.402(9) . ? C4 H4 0.9300 . ? C5 C6 1.369(9) . ? C5 C8 1.524(8) . ? C6 C7 1.394(9) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O4 1.236(8) . ? C8 O3 1.277(8) . ? C9 O6 1.223(10) . ? C9 O5 1.226(9) . ? C9 C10 1.534(10) . ? C10 C15 1.369(10) . ? C10 C11 1.390(9) . ? C11 C12 1.359(9) . ? C11 H11 0.9300 . ? C12 C13 1.391(9) . ? C12 H12 0.9300 . ? C13 C14 1.384(9) . ? C13 C16 1.500(10) . ? C14 C15 1.372(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O7 1.253(12) . ? C16 O8 1.263(9) . ? C16 O7' 1.308(14) . ? C17 O10 1.224(8) . ? C17 O9 1.280(8) . ? C17 C18 1.531(8) . ? C18 C20 1.383(9) 2_767 ? C18 C19 1.385(9) . ? C19 C20 1.375(8) . ? C19 H19 0.9300 . ? C20 C18 1.383(9) 2_767 ? C20 H20 0.9300 . ? C21 O12 1.222(8) . ? C21 O11 1.265(9) . ? C21 C22 1.500(9) . ? C22 C23 1.381(9) . ? C22 C24 1.388(9) 2_868 ? C23 C24 1.392(9) . ? C23 H23 0.9300 . ? C24 C22 1.388(9) 2_868 ? C24 H24 0.9300 . ? C25 N2 1.299(10) . ? C25 N1 1.351(9) . ? C25 H25 0.9300 . ? C26 N3 1.317(8) . ? C26 N1 1.332(8) . ? C26 H26 0.9300 . ? C27 N3 1.469(8) . ? C27 C28 1.521(10) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 C29 1.398(8) . ? C28 C37 1.410(9) . ? C29 C31 1.405(9) . ? C29 C30 1.532(8) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C35 1.405(9) . ? C31 C32 1.512(8) . ? C32 N6 1.482(8) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 N5 1.318(8) . ? C33 N4 1.346(8) . ? C33 H33 0.9300 . ? C34 N4 1.307(8) . ? C34 N6 1.333(8) . ? C34 H34 0.9300 . ? C35 C36 1.406(8) . ? C35 C39 1.498(10) . ? C36 C37 1.400(10) . ? C36 C40 1.521(9) . ? C37 C38 1.516(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 N9 1.478(8) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C41 N7 1.298(9) . ? C41 N8 1.356(9) . ? C41 H41 0.9300 . ? C42 N9 1.310(8) . ? C42 N8 1.327(8) . ? C42 H42 0.9300 . ? C45 N11 1.463(9) . ? C45 C46 1.511(9) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C46 C47 1.378(9) . ? C46 C51 1.412(10) . ? C47 C48 1.416(10) . ? C47 C54 1.531(11) . ? C48 C49 1.362(11) . ? C48 C62 1.510(10) . ? C49 C50 1.404(10) . ? C49 C53 1.545(10) . ? C50 C51 1.387(9) . ? C50 C55 1.509(11) . ? C51 C52 1.514(9) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 0.9600 . ? C54 H54A 0.9600 . ? C54 H54B 0.9600 . ? C54 H54C 0.9600 . ? C55 N13 1.484(10) . ? C55 H55A 0.9700 . ? C55 H55B 0.9700 . ? C56 N15 1.319(8) . ? C56 N13 1.329(9) . ? C56 H56 0.9300 . ? C57 N14 1.318(10) . ? C57 N15 1.339(9) . ? C57 H57 0.9300 . ? C58 N12 1.314(9) . ? C58 N10 1.340(9) . ? C58 H58 0.9300 . ? C59 N11 1.306(9) . ? C59 N10 1.330(9) . ? C59 H59 0.9300 . ? C60 N16 1.314(9) . ? C60 N17 1.325(8) . ? C60 H60 0.9300 . ? C61 N18 1.323(10) . ? C61 N17 1.335(9) . ? C61 H61 0.9300 . ? C62 N16 1.469(9) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? N2 N3 1.376(8) . ? N5 N6 1.375(8) . ? N7 N9 1.369(8) . ? N8 Zn3 2.024(5) 2_857 ? N11 N12 1.366(8) . ? N13 N14 1.341(8) . ? N15 Zn2 2.035(5) 2_767 ? N16 N18 1.346(9) . ? N17 Zn1 2.062(5) 2_666 ? O7 O7' 0.946(14) . ? O8 Zn3 1.962(5) 1_454 ? O1W H1B 0.90(2) . ? O1W H1A 0.91(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zn1 O5 106.9(2) . . ? O3 Zn1 N10 113.2(2) . . ? O5 Zn1 N10 120.8(2) . . ? O3 Zn1 N17 110.7(2) . 2_666 ? O5 Zn1 N17 92.2(2) . 2_666 ? N10 Zn1 N17 111.0(2) . 2_666 ? O11 Zn2 O9 106.6(2) . . ? O11 Zn2 N4 109.3(2) . . ? O9 Zn2 N4 114.8(2) . . ? O11 Zn2 N15 92.0(2) . 2_767 ? O9 Zn2 N15 115.6(2) . 2_767 ? N4 Zn2 N15 115.4(2) . 2_767 ? O2 Zn3 O8 105.4(2) . 1_656 ? O2 Zn3 N1 115.8(2) . . ? O8 Zn3 N1 92.3(2) 1_656 . ? O2 Zn3 N8 110.4(2) . 2_857 ? O8 Zn3 N8 110.3(2) 1_656 2_857 ? N1 Zn3 N8 120.0(2) . 2_857 ? O1 C1 O2 122.9(6) . . ? O1 C1 C2 120.1(6) . . ? O2 C1 C2 116.9(6) . . ? C3 C2 C7 119.5(5) . . ? C3 C2 C1 121.3(6) . . ? C7 C2 C1 119.3(6) . . ? C2 C3 C4 120.5(6) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C3 C4 C5 120.0(6) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 119.2(5) . . ? C6 C5 C8 122.5(6) . . ? C4 C5 C8 118.3(6) . . ? C5 C6 C7 120.6(6) . . ? C5 C6 H6 119.7 . . ? C7 C6 H6 119.7 . . ? C2 C7 C6 120.1(6) . . ? C2 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? O4 C8 O3 123.9(6) . . ? O4 C8 C5 120.2(6) . . ? O3 C8 C5 115.8(6) . . ? O6 C9 O5 125.5(8) . . ? O6 C9 C10 117.7(7) . . ? O5 C9 C10 116.8(7) . . ? C15 C10 C11 118.8(6) . . ? C15 C10 C9 122.4(6) . . ? C11 C10 C9 118.7(6) . . ? C12 C11 C10 121.0(6) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 120.6(6) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C14 C13 C12 118.0(6) . . ? C14 C13 C16 120.6(6) . . ? C12 C13 C16 121.4(6) . . ? C15 C14 C13 121.3(6) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C10 C15 C14 120.3(6) . . ? C10 C15 H15 119.8 . . ? C14 C15 H15 119.8 . . ? O7 C16 O8 116.4(8) . . ? O7 C16 O7' 43.3(7) . . ? O8 C16 O7' 125.4(8) . . ? O7 C16 C13 122.0(8) . . ? O8 C16 C13 117.3(6) . . ? O7' C16 C13 112.2(8) . . ? O10 C17 O9 123.6(5) . . ? O10 C17 C18 119.9(6) . . ? O9 C17 C18 116.4(6) . . ? C20 C18 C19 119.2(5) 2_767 . ? C20 C18 C17 119.7(6) 2_767 . ? C19 C18 C17 121.1(6) . . ? C20 C19 C18 119.6(6) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C18 121.2(6) . 2_767 ? C19 C20 H20 119.4 . . ? C18 C20 H20 119.4 2_767 . ? O12 C21 O11 125.0(6) . . ? O12 C21 C22 119.8(7) . . ? O11 C21 C22 115.2(6) . . ? C23 C22 C24 118.8(6) . 2_868 ? C23 C22 C21 121.4(6) . . ? C24 C22 C21 119.7(6) 2_868 . ? C22 C23 C24 119.6(6) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C22 C24 C23 121.5(6) 2_868 . ? C22 C24 H24 119.3 2_868 . ? C23 C24 H24 119.3 . . ? N2 C25 N1 114.7(7) . . ? N2 C25 H25 122.7 . . ? N1 C25 H25 122.7 . . ? N3 C26 N1 110.0(6) . . ? N3 C26 H26 125.0 . . ? N1 C26 H26 125.0 . . ? N3 C27 C28 111.1(5) . . ? N3 C27 H27A 109.4 . . ? C28 C27 H27A 109.4 . . ? N3 C27 H27B 109.4 . . ? C28 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C29 C28 C37 120.2(6) . . ? C29 C28 C27 119.2(5) . . ? C37 C28 C27 120.6(5) . . ? C28 C29 C31 119.6(5) . . ? C28 C29 C30 120.2(6) . . ? C31 C29 C30 120.2(5) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C35 C31 C29 120.7(5) . . ? C35 C31 C32 119.8(6) . . ? C29 C31 C32 119.5(5) . . ? N6 C32 C31 110.5(5) . . ? N6 C32 H32A 109.5 . . ? C31 C32 H32A 109.5 . . ? N6 C32 H32B 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? N5 C33 N4 114.0(6) . . ? N5 C33 H33 123.0 . . ? N4 C33 H33 123.0 . . ? N4 C34 N6 110.4(6) . . ? N4 C34 H34 124.8 . . ? N6 C34 H34 124.8 . . ? C31 C35 C36 118.6(6) . . ? C31 C35 C39 120.6(5) . . ? C36 C35 C39 120.7(5) . . ? C37 C36 C35 121.2(5) . . ? C37 C36 C40 119.7(5) . . ? C35 C36 C40 119.1(6) . . ? C36 C37 C28 119.1(5) . . ? C36 C37 C38 121.2(6) . . ? C28 C37 C38 119.6(6) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N9 C40 C36 110.3(5) . . ? N9 C40 H40A 109.6 . . ? C36 C40 H40A 109.6 . . ? N9 C40 H40B 109.6 . . ? C36 C40 H40B 109.6 . . ? H40A C40 H40B 108.1 . . ? N7 C41 N8 114.5(6) . . ? N7 C41 H41 122.7 . . ? N8 C41 H41 122.7 . . ? N9 C42 N8 110.4(6) . . ? N9 C42 H42 124.8 . . ? N8 C42 H42 124.8 . . ? N11 C45 C46 112.5(5) . . ? N11 C45 H45A 109.1 . . ? C46 C45 H45A 109.1 . . ? N11 C45 H45B 109.1 . . ? C46 C45 H45B 109.1 . . ? H45A C45 H45B 107.8 . . ? C47 C46 C51 121.0(6) . . ? C47 C46 C45 121.3(6) . . ? C51 C46 C45 117.6(6) . . ? C46 C47 C48 118.8(6) . . ? C46 C47 C54 120.4(7) . . ? C48 C47 C54 120.7(6) . . ? C49 C48 C47 120.0(6) . . ? C49 C48 C62 122.7(7) . . ? C47 C48 C62 117.3(7) . . ? C48 C49 C50 121.1(7) . . ? C48 C49 C53 120.0(7) . . ? C50 C49 C53 118.9(8) . . ? C51 C50 C49 119.4(7) . . ? C51 C50 C55 119.9(7) . . ? C49 C50 C55 120.7(7) . . ? C50 C51 C46 119.0(6) . . ? C50 C51 C52 120.2(6) . . ? C46 C51 C52 120.8(6) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C49 C53 H53A 109.5 . . ? C49 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C49 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C47 C54 H54A 109.5 . . ? C47 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C47 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N13 C55 C50 111.7(6) . . ? N13 C55 H55A 109.3 . . ? C50 C55 H55A 109.3 . . ? N13 C55 H55B 109.3 . . ? C50 C55 H55B 109.3 . . ? H55A C55 H55B 107.9 . . ? N15 C56 N13 110.1(6) . . ? N15 C56 H56 124.9 . . ? N13 C56 H56 124.9 . . ? N14 C57 N15 114.2(6) . . ? N14 C57 H57 122.9 . . ? N15 C57 H57 122.9 . . ? N12 C58 N10 114.9(6) . . ? N12 C58 H58 122.6 . . ? N10 C58 H58 122.6 . . ? N11 C59 N10 109.9(6) . . ? N11 C59 H59 125.0 . . ? N10 C59 H59 125.0 . . ? N16 C60 N17 110.6(6) . . ? N16 C60 H60 124.7 . . ? N17 C60 H60 124.7 . . ? N18 C61 N17 114.3(7) . . ? N18 C61 H61 122.8 . . ? N17 C61 H61 122.8 . . ? N16 C62 C48 112.8(6) . . ? N16 C62 H62A 109.0 . . ? C48 C62 H62A 109.0 . . ? N16 C62 H62B 109.0 . . ? C48 C62 H62B 109.0 . . ? H62A C62 H62B 107.8 . . ? C26 N1 C25 103.1(6) . . ? C26 N1 Zn3 121.7(4) . . ? C25 N1 Zn3 135.1(5) . . ? C25 N2 N3 102.8(6) . . ? C26 N3 N2 109.4(5) . . ? C26 N3 C27 130.1(5) . . ? N2 N3 C27 120.5(5) . . ? C34 N4 C33 104.2(5) . . ? C34 N4 Zn2 123.0(4) . . ? C33 N4 Zn2 132.7(4) . . ? C33 N5 N6 102.6(5) . . ? C34 N6 N5 108.9(5) . . ? C34 N6 C32 129.8(6) . . ? N5 N6 C32 121.3(5) . . ? C41 N7 N9 102.8(5) . . ? C42 N8 C41 102.7(6) . . ? C42 N8 Zn3 121.1(4) . 2_857 ? C41 N8 Zn3 135.8(4) . 2_857 ? C42 N9 N7 109.6(5) . . ? C42 N9 C40 128.8(5) . . ? N7 N9 C40 121.6(5) . . ? C59 N10 C58 103.0(6) . . ? C59 N10 Zn1 127.1(5) . . ? C58 N10 Zn1 129.6(4) . . ? C59 N11 N12 110.4(5) . . ? C59 N11 C45 129.9(6) . . ? N12 N11 C45 119.6(6) . . ? C58 N12 N11 101.7(5) . . ? C56 N13 N14 109.5(6) . . ? C56 N13 C55 130.2(6) . . ? N14 N13 C55 120.3(6) . . ? C57 N14 N13 103.1(6) . . ? C56 N15 C57 103.1(6) . . ? C56 N15 Zn2 121.5(4) . 2_767 ? C57 N15 Zn2 135.3(5) . 2_767 ? C60 N16 N18 109.6(6) . . ? C60 N16 C62 129.4(7) . . ? N18 N16 C62 121.0(6) . . ? C60 N17 C61 102.8(6) . . ? C60 N17 Zn1 119.8(4) . 2_666 ? C61 N17 Zn1 137.2(5) . 2_666 ? C61 N18 N16 102.7(6) . . ? C1 O2 Zn3 109.1(4) . . ? C8 O3 Zn1 108.8(4) . . ? C9 O5 Zn1 110.9(5) . . ? O7' O7 C16 71.4(11) . . ? O7 O7' C16 65.3(10) . . ? C16 O8 Zn3 134.1(5) . 1_454 ? C17 O9 Zn2 106.2(4) . . ? C21 O11 Zn2 124.1(4) . . ? H1B O1W H1A 105.00 . . ? 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 O1 C1 C2 C3 170.1(6) . . . . ? O2 C1 C2 C3 -11.6(9) . . . . ? O1 C1 C2 C7 -10.1(9) . . . . ? O2 C1 C2 C7 168.1(6) . . . . ? C7 C2 C3 C4 0.5(9) . . . . ? C1 C2 C3 C4 -179.8(6) . . . . ? C2 C3 C4 C5 -0.8(10) . . . . ? C3 C4 C5 C6 0.1(9) . . . . ? C3 C4 C5 C8 -179.7(6) . . . . ? C4 C5 C6 C7 1.1(10) . . . . ? C8 C5 C6 C7 -179.2(6) . . . . ? C3 C2 C7 C6 0.7(9) . . . . ? C1 C2 C7 C6 -179.1(6) . . . . ? C5 C6 C7 C2 -1.4(10) . . . . ? C6 C5 C8 O4 -176.7(6) . . . . ? C4 C5 C8 O4 3.1(9) . . . . ? C6 C5 C8 O3 0.8(9) . . . . ? C4 C5 C8 O3 -179.4(6) . . . . ? O6 C9 C10 C15 171.5(7) . . . . ? O5 C9 C10 C15 -10.7(10) . . . . ? O6 C9 C10 C11 -10.6(10) . . . . ? O5 C9 C10 C11 167.2(6) . . . . ? C15 C10 C11 C12 2.0(10) . . . . ? C9 C10 C11 C12 -175.9(6) . . . . ? C10 C11 C12 C13 -1.4(10) . . . . ? C11 C12 C13 C14 -0.3(9) . . . . ? C11 C12 C13 C16 -179.0(6) . . . . ? C12 C13 C14 C15 1.3(9) . . . . ? C16 C13 C14 C15 -180.0(6) . . . . ? C11 C10 C15 C14 -1.0(9) . . . . ? C9 C10 C15 C14 176.9(6) . . . . ? C13 C14 C15 C10 -0.7(10) . . . . ? C14 C13 C16 O7 -20.6(13) . . . . ? C12 C13 C16 O7 158.0(10) . . . . ? C14 C13 C16 O8 -176.6(6) . . . . ? C12 C13 C16 O8 2.1(10) . . . . ? C14 C13 C16 O7' 27.2(11) . . . . ? C12 C13 C16 O7' -154.2(8) . . . . ? O10 C17 C18 C20 1.0(9) . . . 2_767 ? O9 C17 C18 C20 -176.1(6) . . . 2_767 ? O10 C17 C18 C19 179.7(6) . . . . ? O9 C17 C18 C19 2.6(9) . . . . ? C20 C18 C19 C20 -1.1(10) 2_767 . . . ? C17 C18 C19 C20 -179.8(6) . . . . ? C18 C19 C20 C18 1.1(10) . . . 2_767 ? O12 C21 C22 C23 178.7(7) . . . . ? O11 C21 C22 C23 -2.8(9) . . . . ? O12 C21 C22 C24 -2.5(10) . . . 2_868 ? O11 C21 C22 C24 176.0(6) . . . 2_868 ? C24 C22 C23 C24 -3.1(10) 2_868 . . . ? C21 C22 C23 C24 175.8(6) . . . . ? C22 C23 C24 C22 3.2(11) . . . 2_868 ? N3 C27 C28 C29 50.6(8) . . . . ? N3 C27 C28 C37 -128.2(6) . . . . ? C37 C28 C29 C31 8.5(9) . . . . ? C27 C28 C29 C31 -170.3(5) . . . . ? C37 C28 C29 C30 -169.1(6) . . . . ? C27 C28 C29 C30 12.0(9) . . . . ? C28 C29 C31 C35 -5.4(9) . . . . ? C30 C29 C31 C35 172.2(6) . . . . ? C28 C29 C31 C32 172.6(5) . . . . ? C30 C29 C31 C32 -9.8(8) . . . . ? C35 C31 C32 N6 89.3(7) . . . . ? C29 C31 C32 N6 -88.7(7) . . . . ? C29 C31 C35 C36 -1.0(8) . . . . ? C32 C31 C35 C36 -179.0(5) . . . . ? C29 C31 C35 C39 -176.8(6) . . . . ? C32 C31 C35 C39 5.2(8) . . . . ? C31 C35 C36 C37 4.4(9) . . . . ? C39 C35 C36 C37 -179.8(6) . . . . ? C31 C35 C36 C40 -177.5(5) . . . . ? C39 C35 C36 C40 -1.6(9) . . . . ? C35 C36 C37 C28 -1.4(9) . . . . ? C40 C36 C37 C28 -179.5(5) . . . . ? C35 C36 C37 C38 -180.0(6) . . . . ? C40 C36 C37 C38 1.9(9) . . . . ? C29 C28 C37 C36 -5.1(9) . . . . ? C27 C28 C37 C36 173.7(5) . . . . ? C29 C28 C37 C38 173.5(6) . . . . ? C27 C28 C37 C38 -7.7(9) . . . . ? C37 C36 C40 N9 85.0(7) . . . . ? C35 C36 C40 N9 -93.2(7) . . . . ? N11 C45 C46 C47 91.3(8) . . . . ? N11 C45 C46 C51 -86.1(7) . . . . ? C51 C46 C47 C48 1.8(9) . . . . ? C45 C46 C47 C48 -175.6(6) . . . . ? C51 C46 C47 C54 -176.7(6) . . . . ? C45 C46 C47 C54 5.9(9) . . . . ? C46 C47 C48 C49 5.3(9) . . . . ? C54 C47 C48 C49 -176.2(6) . . . . ? C46 C47 C48 C62 -173.2(6) . . . . ? C54 C47 C48 C62 5.3(9) . . . . ? C47 C48 C49 C50 -6.1(9) . . . . ? C62 C48 C49 C50 172.4(6) . . . . ? C47 C48 C49 C53 174.9(6) . . . . ? C62 C48 C49 C53 -6.6(10) . . . . ? C48 C49 C50 C51 -0.3(10) . . . . ? C53 C49 C50 C51 178.7(6) . . . . ? C48 C49 C50 C55 179.3(6) . . . . ? C53 C49 C50 C55 -1.7(10) . . . . ? C49 C50 C51 C46 7.2(9) . . . . ? C55 C50 C51 C46 -172.4(6) . . . . ? C49 C50 C51 C52 -171.4(6) . . . . ? C55 C50 C51 C52 9.1(9) . . . . ? C47 C46 C51 C50 -8.0(9) . . . . ? C45 C46 C51 C50 169.5(6) . . . . ? C47 C46 C51 C52 170.6(6) . . . . ? C45 C46 C51 C52 -12.0(9) . . . . ? C51 C50 C55 N13 65.6(9) . . . . ? C49 C50 C55 N13 -113.9(8) . . . . ? C49 C48 C62 N16 94.3(9) . . . . ? C47 C48 C62 N16 -87.2(8) . . . . ? N3 C26 N1 C25 0.3(7) . . . . ? N3 C26 N1 Zn3 176.6(4) . . . . ? N2 C25 N1 C26 -1.0(9) . . . . ? N2 C25 N1 Zn3 -176.5(5) . . . . ? O2 Zn3 N1 C26 -99.7(5) . . . . ? O8 Zn3 N1 C26 8.7(5) 1_656 . . . ? N8 Zn3 N1 C26 123.8(5) 2_857 . . . ? O2 Zn3 N1 C25 75.2(7) . . . . ? O8 Zn3 N1 C25 -176.4(7) 1_656 . . . ? N8 Zn3 N1 C25 -61.3(7) 2_857 . . . ? N1 C25 N2 N3 1.2(9) . . . . ? N1 C26 N3 N2 0.4(7) . . . . ? N1 C26 N3 C27 -178.0(6) . . . . ? C25 N2 N3 C26 -0.9(8) . . . . ? C25 N2 N3 C27 177.7(6) . . . . ? C28 C27 N3 C26 29.2(9) . . . . ? C28 C27 N3 N2 -149.1(6) . . . . ? N6 C34 N4 C33 0.2(6) . . . . ? N6 C34 N4 Zn2 176.3(4) . . . . ? N5 C33 N4 C34 -0.1(6) . . . . ? N5 C33 N4 Zn2 -175.6(4) . . . . ? O11 Zn2 N4 C34 36.4(5) . . . . ? O9 Zn2 N4 C34 -83.3(5) . . . . ? N15 Zn2 N4 C34 138.3(4) 2_767 . . . ? O11 Zn2 N4 C33 -148.8(5) . . . . ? O9 Zn2 N4 C33 91.6(5) . . . . ? N15 Zn2 N4 C33 -46.8(6) 2_767 . . . ? N4 C33 N5 N6 -0.1(6) . . . . ? N4 C34 N6 N5 -0.3(7) . . . . ? N4 C34 N6 C32 -178.4(5) . . . . ? C33 N5 N6 C34 0.2(6) . . . . ? C33 N5 N6 C32 178.5(5) . . . . ? C31 C32 N6 C34 -114.3(7) . . . . ? C31 C32 N6 N5 67.8(7) . . . . ? N8 C41 N7 N9 0.1(8) . . . . ? N9 C42 N8 C41 -1.4(7) . . . . ? N9 C42 N8 Zn3 172.6(4) . . . 2_857 ? N7 C41 N8 C42 0.8(8) . . . . ? N7 C41 N8 Zn3 -171.9(5) . . . 2_857 ? N8 C42 N9 N7 1.6(7) . . . . ? N8 C42 N9 C40 -179.2(6) . . . . ? C41 N7 N9 C42 -1.0(7) . . . . ? C41 N7 N9 C40 179.7(6) . . . . ? C36 C40 N9 C42 -30.6(9) . . . . ? C36 C40 N9 N7 148.5(6) . . . . ? N11 C59 N10 C58 -0.3(7) . . . . ? N11 C59 N10 Zn1 174.0(4) . . . . ? N12 C58 N10 C59 0.0(7) . . . . ? N12 C58 N10 Zn1 -174.0(4) . . . . ? O3 Zn1 N10 C59 -81.7(6) . . . . ? O5 Zn1 N10 C59 46.9(6) . . . . ? N17 Zn1 N10 C59 153.0(5) 2_666 . . . ? O3 Zn1 N10 C58 91.0(5) . . . . ? O5 Zn1 N10 C58 -140.4(5) . . . . ? N17 Zn1 N10 C58 -34.3(6) 2_666 . . . ? N10 C59 N11 N12 0.4(7) . . . . ? N10 C59 N11 C45 -176.3(6) . . . . ? C46 C45 N11 C59 -125.3(7) . . . . ? C46 C45 N11 N12 58.2(8) . . . . ? N10 C58 N12 N11 0.2(7) . . . . ? C59 N11 N12 C58 -0.4(7) . . . . ? C45 N11 N12 C58 176.8(5) . . . . ? N15 C56 N13 N14 0.9(8) . . . . ? N15 C56 N13 C55 -179.2(7) . . . . ? C50 C55 N13 C56 4.7(12) . . . . ? C50 C55 N13 N14 -175.3(6) . . . . ? N15 C57 N14 N13 1.2(9) . . . . ? C56 N13 N14 C57 -1.2(8) . . . . ? C55 N13 N14 C57 178.9(7) . . . . ? N13 C56 N15 C57 -0.1(8) . . . . ? N13 C56 N15 Zn2 -177.2(4) . . . 2_767 ? N14 C57 N15 C56 -0.7(9) . . . . ? N14 C57 N15 Zn2 175.7(5) . . . 2_767 ? N17 C60 N16 N18 -0.6(8) . . . . ? N17 C60 N16 C62 -179.8(7) . . . . ? C48 C62 N16 C60 -40.5(12) . . . . ? C48 C62 N16 N18 140.4(7) . . . . ? N16 C60 N17 C61 0.4(8) . . . . ? N16 C60 N17 Zn1 176.3(4) . . . 2_666 ? N18 C61 N17 C60 -0.1(8) . . . . ? N18 C61 N17 Zn1 -174.9(5) . . . 2_666 ? N17 C61 N18 N16 -0.2(8) . . . . ? C60 N16 N18 C61 0.5(8) . . . . ? C62 N16 N18 C61 179.8(6) . . . . ? O1 C1 O2 Zn3 6.8(8) . . . . ? C2 C1 O2 Zn3 -171.4(4) . . . . ? O8 Zn3 O2 C1 179.7(4) 1_656 . . . ? N1 Zn3 O2 C1 -79.9(5) . . . . ? N8 Zn3 O2 C1 60.6(5) 2_857 . . . ? O4 C8 O3 Zn1 0.0(8) . . . . ? C5 C8 O3 Zn1 -177.4(4) . . . . ? O5 Zn1 O3 C8 164.2(4) . . . . ? N10 Zn1 O3 C8 -60.3(5) . . . . ? N17 Zn1 O3 C8 65.1(4) 2_666 . . . ? O6 C9 O5 Zn1 3.9(10) . . . . ? C10 C9 O5 Zn1 -173.8(4) . . . . ? O3 Zn1 O5 C9 90.1(5) . . . . ? N10 Zn1 O5 C9 -41.3(6) . . . . ? N17 Zn1 O5 C9 -157.5(5) 2_666 . . . ? O8 C16 O7 O7' -114.6(12) . . . . ? C13 C16 O7 O7' 89.2(12) . . . . ? O8 C16 O7' O7 92.4(13) . . . . ? C13 C16 O7' O7 -113.7(11) . . . . ? O7 C16 O8 Zn3 9.0(13) . . . 1_454 ? O7' C16 O8 Zn3 -40.9(13) . . . 1_454 ? C13 C16 O8 Zn3 166.3(4) . . . 1_454 ? O10 C17 O9 Zn2 -2.4(7) . . . . ? C18 C17 O9 Zn2 174.7(4) . . . . ? O11 Zn2 O9 C17 175.0(4) . . . . ? N4 Zn2 O9 C17 -63.8(5) . . . . ? N15 Zn2 O9 C17 74.5(4) 2_767 . . . ? O12 C21 O11 Zn2 8.7(10) . . . . ? C22 C21 O11 Zn2 -169.7(4) . . . . ? O9 Zn2 O11 C21 67.1(5) . . . . ? N4 Zn2 O11 C21 -57.5(6) . . . . ? N15 Zn2 O11 C21 -175.3(5) 2_767 . . . ? 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 O1W H1B O12 0.90(2) 2.4(2) 3.032(17) 128(21) . O1W H1A O1 0.91(2) 2.5(3) 3.11(2) 124(25) 2_757 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.601 _refine_diff_density_min -0.702 _refine_diff_density_rms 0.099 data_6 _database_code_depnum_ccdc_archive 'CCDC 904156' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 N18 O9 Zn2' _chemical_formula_weight 1125.75 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6371(11) _cell_length_b 11.5022(14) _cell_length_c 13.0554(18) _cell_angle_alpha 72.255(12) _cell_angle_beta 84.177(10) _cell_angle_gamma 67.195(11) _cell_volume 1270.3(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 580 _exptl_absorpt_coefficient_mu 1.779 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6748 _exptl_absorpt_correction_T_max 0.7639 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13855 _diffrn_reflns_av_R_equivalents 0.0689 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 4.36 _diffrn_reflns_theta_max 67.17 _reflns_number_total 4510 _reflns_number_gt 3170 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1369P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4510 _refine_ls_number_parameters 352 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0676 _refine_ls_wR_factor_ref 0.2003 _refine_ls_wR_factor_gt 0.1770 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.005 _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 0.37952(6) 0.24721(6) 0.51442(5) 0.0414(2) Uani 1 1 d . . . C1 C 0.3941(6) 0.4141(5) 0.2924(4) 0.0509(12) Uani 1 1 d . . . H1 H 0.4847 0.3498 0.2818 0.061 Uiso 1 1 calc R . . C2 C 0.1996(6) 0.5232(6) 0.3612(5) 0.0597(14) Uani 1 1 d . . . H2 H 0.1266 0.5476 0.4111 0.072 Uiso 1 1 calc R . . C3 C 0.3665(7) 0.5705(7) 0.1068(5) 0.0618(14) Uani 1 1 d . . . H3A H 0.4647 0.5084 0.0954 0.074 Uiso 1 1 calc R . . H3B H 0.3761 0.6539 0.0980 0.074 Uiso 1 1 calc R . . C4 C 0.2577(6) 0.5894(5) 0.0222(4) 0.0513(12) Uani 1 1 d . . . C5 C 0.1696(8) 0.7168(6) -0.0364(5) 0.0644(15) Uani 1 1 d . . . C6 C 0.0809(8) 0.7362(6) -0.1242(5) 0.0650(15) Uani 1 1 d . . . C7 C 0.0760(7) 0.6276(6) -0.1487(4) 0.0588(14) Uani 1 1 d . . . C8 C 0.1610(6) 0.5011(6) -0.0868(4) 0.0521(12) Uani 1 1 d . . . C9 C 0.2552(6) 0.4793(5) -0.0029(4) 0.0496(12) Uani 1 1 d . . . C10 C 0.3543(8) 0.3420(6) 0.0578(5) 0.0679(16) Uani 1 1 d . . . H10A H 0.2958 0.3024 0.1100 0.102 Uiso 1 1 calc R . . H10B H 0.4342 0.3453 0.0938 0.102 Uiso 1 1 calc R . . H10C H 0.3962 0.2906 0.0085 0.102 Uiso 1 1 calc R . . C11 C 0.1678(13) 0.8343(8) -0.0072(8) 0.110(3) Uani 1 1 d . . . H11A H 0.1714 0.8146 0.0696 0.165 Uiso 1 1 calc R . . H11B H 0.0773 0.9086 -0.0353 0.165 Uiso 1 1 calc R . . H11C H 0.2536 0.8547 -0.0373 0.165 Uiso 1 1 calc R . . C12 C -0.0173(9) 0.6472(8) -0.2416(5) 0.0777(18) Uani 1 1 d . . . H12A H 0.0448 0.6402 -0.3035 0.117 Uiso 1 1 calc R . . H12B H -0.0965 0.7329 -0.2572 0.117 Uiso 1 1 calc R . . H12C H -0.0604 0.5811 -0.2240 0.117 Uiso 1 1 calc R . . C13 C -0.0029(11) 0.8746(8) -0.1953(7) 0.091(2) Uani 1 1 d . . . H13A H 0.0467 0.9319 -0.1907 0.109 Uiso 1 1 calc R . . H13B H -0.0002 0.8735 -0.2695 0.109 Uiso 1 1 calc R . . C14 C -0.3376(18) 0.9754(13) -0.0609(12) 0.133(4) Uani 1 1 d . . . H14 H -0.3918 0.9832 0.0014 0.160 Uiso 1 1 calc R . . C15 C -0.2827(17) 0.9838(15) -0.2233(12) 0.171(6) Uani 1 1 d . . . H15 H -0.2890 0.9979 -0.2970 0.206 Uiso 1 1 calc R . . C16 C 0.1560(7) 0.3833(6) -0.1131(5) 0.0607(14) Uani 1 1 d . . . H16A H 0.1929 0.3057 -0.0517 0.073 Uiso 1 1 calc R . . H16B H 0.0527 0.3987 -0.1281 0.073 Uiso 1 1 calc R . . C17 C 0.4362(7) 0.3366(9) -0.3056(6) 0.083(2) Uani 1 1 d . . . H17 H 0.5298 0.3332 -0.3337 0.099 Uiso 1 1 calc R . . C18 C 0.2266(6) 0.3229(6) -0.2871(4) 0.0536(13) Uani 1 1 d . . . H18 H 0.1412 0.3075 -0.2956 0.064 Uiso 1 1 calc R . . C19 C 0.6776(6) 0.1236(5) 0.4582(5) 0.0532(13) Uani 1 1 d . . . C20 C 0.8442(5) 0.0540(5) 0.4846(4) 0.0474(11) Uani 1 1 d . . . C21 C 0.9259(5) -0.0792(5) 0.4881(4) 0.0409(10) Uani 1 1 d . . . C22 C 1.0792(5) -0.1277(5) 0.5010(4) 0.0484(12) Uani 1 1 d . . . H22 H 1.1342 -0.2140 0.5000 0.058 Uiso 1 1 calc R . . C23 C 0.8492(5) -0.1680(5) 0.4816(4) 0.0431(11) Uani 1 1 d . . . N1 N 0.3221(5) 0.4087(4) 0.3842(3) 0.0493(10) Uani 1 1 d . . . N2 N 0.3206(5) 0.5220(5) 0.2185(3) 0.0518(10) Uani 1 1 d . . . N3 N 0.1948(6) 0.5962(5) 0.2606(4) 0.0647(13) Uani 1 1 d . . . N4 N -0.4013(15) 1.0193(12) -0.1560(14) 0.178(5) Uani 1 1 d . . . N5 N -0.1910(12) 0.9194(9) -0.0610(8) 0.120(3) Uani 1 1 d . . . N6 N -0.1578(10) 0.9257(7) -0.1632(6) 0.101(2) Uani 1 1 d . . . N7 N 0.3390(4) 0.3101(4) -0.3532(3) 0.0483(10) Uani 1 1 d . . . N8 N 0.3882(7) 0.3675(8) -0.2172(5) 0.089(2) Uani 1 1 d . . . N9 N 0.2495(5) 0.3603(5) -0.2076(4) 0.0532(11) Uani 1 1 d . . . O1 O 0.5964(4) 0.1636(4) 0.5306(4) 0.0608(10) Uani 1 1 d . . . O2 O 0.6313(5) 0.1486(5) 0.3661(4) 0.0731(12) Uani 1 1 d . . . O3 O 0.7091(4) -0.1280(4) 0.4987(3) 0.0548(9) Uani 1 1 d . . . O4 O 0.9233(4) -0.2746(4) 0.4642(4) 0.0642(11) Uani 1 1 d . . . O1W O 0.6837(19) -0.0058(13) 0.2230(9) 0.118(5) Uani 0.50 1 d PD . . H1B H 0.64(2) 0.05(2) 0.259(17) 0.177 Uiso 0.50 1 d PD . . H1A H 0.62(2) 0.00(3) 0.175(17) 0.177 Uiso 0.50 1 d PD . . 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 0.0274(3) 0.0501(4) 0.0532(4) -0.0281(3) 0.0031(2) -0.0118(2) C1 0.041(3) 0.061(3) 0.053(3) -0.028(3) 0.001(2) -0.014(2) C2 0.049(3) 0.062(3) 0.054(3) -0.023(3) 0.003(2) -0.003(3) C3 0.071(4) 0.072(4) 0.053(3) -0.026(3) 0.010(3) -0.034(3) C4 0.059(3) 0.059(3) 0.041(3) -0.020(2) 0.009(2) -0.026(3) C5 0.084(4) 0.056(3) 0.058(3) -0.026(3) 0.005(3) -0.026(3) C6 0.077(4) 0.062(3) 0.050(3) -0.018(3) -0.002(3) -0.017(3) C7 0.058(3) 0.066(4) 0.051(3) -0.022(3) 0.008(2) -0.020(3) C8 0.056(3) 0.065(3) 0.049(3) -0.031(3) 0.017(2) -0.030(3) C9 0.058(3) 0.052(3) 0.040(2) -0.020(2) 0.013(2) -0.019(2) C10 0.079(4) 0.065(4) 0.061(3) -0.026(3) 0.013(3) -0.024(3) C11 0.161(10) 0.070(5) 0.110(7) -0.042(5) -0.015(6) -0.039(5) C12 0.083(5) 0.090(5) 0.059(4) -0.029(3) 0.000(3) -0.027(4) C13 0.112(7) 0.073(5) 0.080(5) -0.018(4) 0.000(4) -0.030(4) C14 0.148(12) 0.107(8) 0.129(10) -0.038(7) 0.006(8) -0.029(8) C15 0.132(11) 0.170(12) 0.117(9) 0.002(8) -0.012(8) 0.014(9) C16 0.067(4) 0.081(4) 0.055(3) -0.039(3) 0.018(3) -0.039(3) C17 0.054(3) 0.148(7) 0.094(5) -0.085(5) 0.031(3) -0.057(4) C18 0.046(3) 0.069(3) 0.063(3) -0.041(3) 0.008(2) -0.024(3) C19 0.041(3) 0.053(3) 0.071(4) -0.024(3) -0.007(2) -0.016(2) C20 0.026(2) 0.053(3) 0.069(3) -0.031(2) 0.010(2) -0.013(2) C21 0.028(2) 0.051(3) 0.049(3) -0.023(2) 0.0046(17) -0.0150(19) C22 0.027(2) 0.049(3) 0.074(3) -0.033(3) 0.004(2) -0.009(2) C23 0.031(2) 0.052(3) 0.053(3) -0.025(2) 0.0014(18) -0.015(2) N1 0.042(2) 0.054(2) 0.052(2) -0.0238(19) 0.0015(17) -0.0131(19) N2 0.049(2) 0.063(3) 0.048(2) -0.025(2) 0.0039(19) -0.020(2) N3 0.055(3) 0.063(3) 0.063(3) -0.025(2) 0.005(2) -0.004(2) N4 0.131(9) 0.138(9) 0.192(13) -0.028(9) 0.023(9) 0.004(7) N5 0.125(8) 0.111(6) 0.135(8) -0.061(5) 0.012(6) -0.039(6) N6 0.124(6) 0.079(4) 0.073(4) -0.018(3) -0.005(4) -0.012(4) N7 0.038(2) 0.062(3) 0.060(2) -0.038(2) 0.0085(17) -0.0202(19) N8 0.069(4) 0.154(6) 0.094(4) -0.086(4) 0.027(3) -0.064(4) N9 0.049(2) 0.071(3) 0.056(3) -0.040(2) 0.0115(19) -0.026(2) O1 0.0301(17) 0.070(2) 0.091(3) -0.045(2) 0.0071(17) -0.0142(16) O2 0.053(2) 0.077(3) 0.083(3) -0.031(2) -0.015(2) -0.008(2) O3 0.0294(17) 0.061(2) 0.088(3) -0.041(2) 0.0127(16) -0.0203(15) O4 0.0379(19) 0.067(2) 0.106(3) -0.055(2) 0.0080(19) -0.0182(18) O1W 0.198(15) 0.110(9) 0.066(7) -0.049(6) 0.024(7) -0.067(9) _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 1.928(3) 2_656 ? Zn1 O1 1.935(3) . ? Zn1 N7 2.017(4) 1_556 ? Zn1 N1 2.029(5) . ? C1 N2 1.304(7) . ? C1 N1 1.319(7) . ? C1 H1 0.9300 . ? C2 N3 1.320(8) . ? C2 N1 1.358(7) . ? C2 H2 0.9300 . ? C3 N2 1.482(7) . ? C3 C4 1.509(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.392(9) . ? C4 C9 1.410(8) . ? C5 C6 1.411(9) . ? C5 C11 1.507(9) . ? C6 C7 1.399(9) . ? C6 C13 1.517(10) . ? C7 C8 1.391(9) . ? C7 C12 1.493(9) . ? C8 C9 1.395(8) . ? C8 C16 1.515(8) . ? C9 C10 1.502(9) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 N6 1.447(12) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N5 1.305(16) . ? C14 N4 1.306(18) . ? C14 H14 0.9300 . ? C15 N6 1.326(16) . ? C15 N4 1.378(18) . ? C15 H15 0.9300 . ? C16 N9 1.481(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 N8 1.298(8) . ? C17 N7 1.346(7) . ? C17 H17 0.9300 . ? C18 N9 1.305(6) . ? C18 N7 1.306(7) . ? C18 H18 0.9300 . ? C19 O2 1.236(7) . ? C19 O1 1.247(7) . ? C19 C20 1.511(7) . ? C20 C22 1.381(7) 2_756 ? C20 C21 1.415(7) . ? C21 C22 1.370(6) . ? C21 C23 1.499(7) . ? C22 C20 1.381(7) 2_756 ? C22 H22 0.9300 . ? C23 O4 1.234(6) . ? C23 O3 1.267(6) . ? N2 N3 1.360(6) . ? N5 N6 1.326(12) . ? N7 Zn1 2.017(4) 1_554 ? N8 N9 1.362(7) . ? O3 Zn1 1.928(3) 2_656 ? O1W H1B 0.86(2) . ? O1W H1A 0.86(2) . ? 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 111.83(16) 2_656 . ? O3 Zn1 N7 119.05(17) 2_656 1_556 ? O1 Zn1 N7 97.61(17) . 1_556 ? O3 Zn1 N1 109.92(17) 2_656 . ? O1 Zn1 N1 110.02(18) . . ? N7 Zn1 N1 107.67(18) 1_556 . ? N2 C1 N1 110.6(5) . . ? N2 C1 H1 124.7 . . ? N1 C1 H1 124.7 . . ? N3 C2 N1 113.0(5) . . ? N3 C2 H2 123.5 . . ? N1 C2 H2 123.5 . . ? N2 C3 C4 113.7(5) . . ? N2 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? N2 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C9 120.7(5) . . ? C5 C4 C3 119.0(5) . . ? C9 C4 C3 120.1(5) . . ? C4 C5 C6 119.7(5) . . ? C4 C5 C11 120.7(6) . . ? C6 C5 C11 119.5(6) . . ? C7 C6 C5 120.0(6) . . ? C7 C6 C13 120.1(6) . . ? C5 C6 C13 119.9(6) . . ? C8 C7 C6 119.3(5) . . ? C8 C7 C12 120.3(6) . . ? C6 C7 C12 120.3(6) . . ? C7 C8 C9 121.7(5) . . ? C7 C8 C16 119.5(5) . . ? C9 C8 C16 118.7(5) . . ? C8 C9 C4 118.5(5) . . ? C8 C9 C10 120.8(5) . . ? C4 C9 C10 120.7(5) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C5 C11 H11A 109.5 . . ? C5 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C5 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N6 C13 C6 111.1(7) . . ? N6 C13 H13A 109.4 . . ? C6 C13 H13A 109.4 . . ? N6 C13 H13B 109.4 . . ? C6 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? N5 C14 N4 114.1(13) . . ? N5 C14 H14 123.0 . . ? N4 C14 H14 123.0 . . ? N6 C15 N4 107.1(13) . . ? N6 C15 H15 126.4 . . ? N4 C15 H15 126.4 . . ? N9 C16 C8 110.4(4) . . ? N9 C16 H16A 109.6 . . ? C8 C16 H16A 109.6 . . ? N9 C16 H16B 109.6 . . ? C8 C16 H16B 109.6 . . ? H16A C16 H16B 108.1 . . ? N8 C17 N7 114.4(5) . . ? N8 C17 H17 122.8 . . ? N7 C17 H17 122.8 . . ? N9 C18 N7 111.2(5) . . ? N9 C18 H18 124.4 . . ? N7 C18 H18 124.4 . . ? O2 C19 O1 123.7(5) . . ? O2 C19 C20 120.0(5) . . ? O1 C19 C20 116.0(5) . . ? C22 C20 C21 119.0(4) 2_756 . ? C22 C20 C19 117.7(4) 2_756 . ? C21 C20 C19 123.2(4) . . ? C22 C21 C20 118.0(4) . . ? C22 C21 C23 120.0(4) . . ? C20 C21 C23 122.0(4) . . ? C21 C22 C20 122.9(5) . 2_756 ? C21 C22 H22 118.5 . . ? C20 C22 H22 118.5 2_756 . ? O4 C23 O3 124.2(4) . . ? O4 C23 C21 120.0(4) . . ? O3 C23 C21 115.8(4) . . ? C1 N1 C2 103.4(5) . . ? C1 N1 Zn1 123.9(4) . . ? C2 N1 Zn1 132.0(4) . . ? C1 N2 N3 110.0(4) . . ? C1 N2 C3 128.1(5) . . ? N3 N2 C3 121.7(5) . . ? C2 N3 N2 102.9(5) . . ? C14 N4 C15 103.9(13) . . ? C14 N5 N6 104.6(10) . . ? N5 N6 C15 110.2(10) . . ? N5 N6 C13 120.6(8) . . ? C15 N6 C13 129.2(9) . . ? C18 N7 C17 102.7(4) . . ? C18 N7 Zn1 131.3(3) . 1_554 ? C17 N7 Zn1 125.7(4) . 1_554 ? C17 N8 N9 102.7(5) . . ? C18 N9 N8 109.0(4) . . ? C18 N9 C16 130.2(5) . . ? N8 N9 C16 120.7(4) . . ? C19 O1 Zn1 122.0(4) . . ? C23 O3 Zn1 112.5(3) . 2_656 ? H1B O1W H1A 111.00 . . ? 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 N2 C3 C4 C5 108.9(6) . . . . ? N2 C3 C4 C9 -76.5(6) . . . . ? C9 C4 C5 C6 -2.1(9) . . . . ? C3 C4 C5 C6 172.4(5) . . . . ? C9 C4 C5 C11 177.8(7) . . . . ? C3 C4 C5 C11 -7.6(10) . . . . ? C4 C5 C6 C7 3.1(10) . . . . ? C11 C5 C6 C7 -176.8(7) . . . . ? C4 C5 C6 C13 -173.8(6) . . . . ? C11 C5 C6 C13 6.3(11) . . . . ? C5 C6 C7 C8 -0.9(9) . . . . ? C13 C6 C7 C8 175.9(6) . . . . ? C5 C6 C7 C12 -179.8(6) . . . . ? C13 C6 C7 C12 -3.0(10) . . . . ? C6 C7 C8 C9 -2.2(8) . . . . ? C12 C7 C8 C9 176.7(5) . . . . ? C6 C7 C8 C16 180.0(5) . . . . ? C12 C7 C8 C16 -1.1(8) . . . . ? C7 C8 C9 C4 3.1(8) . . . . ? C16 C8 C9 C4 -179.0(5) . . . . ? C7 C8 C9 C10 -175.6(5) . . . . ? C16 C8 C9 C10 2.2(7) . . . . ? C5 C4 C9 C8 -0.9(8) . . . . ? C3 C4 C9 C8 -175.4(5) . . . . ? C5 C4 C9 C10 177.8(5) . . . . ? C3 C4 C9 C10 3.3(8) . . . . ? C7 C6 C13 N6 86.2(8) . . . . ? C5 C6 C13 N6 -96.9(9) . . . . ? C7 C8 C16 N9 77.4(7) . . . . ? C9 C8 C16 N9 -100.5(6) . . . . ? O2 C19 C20 C22 106.6(6) . . . 2_756 ? O1 C19 C20 C22 -66.8(7) . . . 2_756 ? O2 C19 C20 C21 -69.1(7) . . . . ? O1 C19 C20 C21 117.6(6) . . . . ? C22 C20 C21 C22 -2.8(8) 2_756 . . . ? C19 C20 C21 C22 172.8(5) . . . . ? C22 C20 C21 C23 175.2(5) 2_756 . . . ? C19 C20 C21 C23 -9.2(8) . . . . ? C20 C21 C22 C20 2.9(9) . . . 2_756 ? C23 C21 C22 C20 -175.2(5) . . . 2_756 ? C22 C21 C23 O4 -15.9(7) . . . . ? C20 C21 C23 O4 166.1(5) . . . . ? C22 C21 C23 O3 161.8(5) . . . . ? C20 C21 C23 O3 -16.2(7) . . . . ? N2 C1 N1 C2 -1.0(6) . . . . ? N2 C1 N1 Zn1 170.9(3) . . . . ? N3 C2 N1 C1 0.1(7) . . . . ? N3 C2 N1 Zn1 -170.8(4) . . . . ? O3 Zn1 N1 C1 -83.9(4) 2_656 . . . ? O1 Zn1 N1 C1 39.7(4) . . . . ? N7 Zn1 N1 C1 145.0(4) 1_556 . . . ? O3 Zn1 N1 C2 85.4(5) 2_656 . . . ? O1 Zn1 N1 C2 -151.0(5) . . . . ? N7 Zn1 N1 C2 -45.7(5) 1_556 . . . ? N1 C1 N2 N3 1.5(6) . . . . ? N1 C1 N2 C3 175.8(5) . . . . ? C4 C3 N2 C1 120.7(6) . . . . ? C4 C3 N2 N3 -65.6(7) . . . . ? N1 C2 N3 N2 0.7(7) . . . . ? C1 N2 N3 C2 -1.3(6) . . . . ? C3 N2 N3 C2 -176.0(5) . . . . ? N5 C14 N4 C15 2.0(19) . . . . ? N6 C15 N4 C14 -2.1(19) . . . . ? N4 C14 N5 N6 -1.1(15) . . . . ? C14 N5 N6 C15 -0.4(13) . . . . ? C14 N5 N6 C13 178.9(9) . . . . ? N4 C15 N6 N5 1.6(17) . . . . ? N4 C15 N6 C13 -177.6(10) . . . . ? C6 C13 N6 N5 49.5(11) . . . . ? C6 C13 N6 C15 -131.4(13) . . . . ? N9 C18 N7 C17 2.7(7) . . . . ? N9 C18 N7 Zn1 176.3(4) . . . 1_554 ? N8 C17 N7 C18 -1.5(9) . . . . ? N8 C17 N7 Zn1 -175.7(6) . . . 1_554 ? N7 C17 N8 N9 -0.1(10) . . . . ? N7 C18 N9 N8 -2.9(7) . . . . ? N7 C18 N9 C16 -178.0(6) . . . . ? C17 N8 N9 C18 1.8(8) . . . . ? C17 N8 N9 C16 177.4(6) . . . . ? C8 C16 N9 C18 -142.0(6) . . . . ? C8 C16 N9 N8 43.4(8) . . . . ? O2 C19 O1 Zn1 10.0(8) . . . . ? C20 C19 O1 Zn1 -176.9(3) . . . . ? O3 Zn1 O1 C19 64.3(5) 2_656 . . . ? N7 Zn1 O1 C19 -170.2(4) 1_556 . . . ? N1 Zn1 O1 C19 -58.2(5) . . . . ? O4 C23 O3 Zn1 -3.7(7) . . . 2_656 ? C21 C23 O3 Zn1 178.8(3) . . . 2_656 ? 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 O1W H1B O2 0.86(2) 2.05(11) 2.835(11) 151(21) . O1W H1A N4 0.86(2) 2.29(18) 3.01(2) 144.00 2_565 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 67.17 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.828 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.101 data_7 _database_code_depnum_ccdc_archive 'CCDC 904157' #TrackingRef 'Cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H46 Cd2 N18 O9' _chemical_formula_weight 1219.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P43212 _symmetry_space_group_name_Hall 'P 4nw 2abw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/4' '-x+1/2, y+1/2, -z+3/4' '-y, -x, -z+1/2' 'y, x, -z' 'y+1/2, -x+1/2, z+1/4' '-y+1/2, x+1/2, z+3/4' _cell_length_a 11.896(2) _cell_length_b 11.896(3) _cell_length_c 34.2854(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4852.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.670 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2464 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8249 _exptl_absorpt_correction_T_max 0.8547 _exptl_absorpt_process_details ; CrysAlis (Oxford Diffraction, 2006) ; _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 'Oxford Diffraction Gemini R Ultra' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10.0 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22755 _diffrn_reflns_av_R_equivalents 0.0369 _diffrn_reflns_av_sigmaI/netI 0.0544 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 29.21 _reflns_number_total 5757 _reflns_number_gt 4251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis (Oxford Diffraction, 2006)' _computing_cell_refinement CrysAlis _computing_data_reduction CrysAlis _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0419P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.01(3) _refine_ls_number_reflns 5757 _refine_ls_number_parameters 342 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.952 _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 Cd1 Cd 0.91625(2) 0.08047(2) 0.127453(6) 0.02822(8) Uani 1 1 d . . . C1 C 1.0651(3) 0.1636(3) 0.06871(10) 0.0277(8) Uani 1 1 d . . . C2 C 1.1418(3) 0.1809(3) 0.03463(10) 0.0250(8) Uani 1 1 d . . . C3 C 1.2277(3) 0.2596(3) 0.03478(9) 0.0256(8) Uani 1 1 d . . . C4 C 1.1216(3) 0.1216(3) 0.0000 0.0248(10) Uani 1 2 d S . . H4 H 1.0663 0.0663 0.0000 0.030 Uiso 1 2 calc SR . . C5 C 1.2838(3) 0.2838(3) 0.0000 0.0270(11) Uani 1 2 d S . . H5 H 1.3391 0.3391 0.0000 0.032 Uiso 1 2 calc SR . . C6 C 1.2752(3) 0.3184(3) 0.07001(10) 0.0278(9) Uani 1 1 d . . . C7 C 1.0101(4) -0.1656(4) 0.16996(14) 0.0556(12) Uani 1 1 d . . . H7 H 0.9653 -0.1648 0.1922 0.067 Uiso 1 1 calc R . . C8 C 1.0665(4) -0.1335(4) 0.11321(14) 0.0500(12) Uani 1 1 d . . . H8 H 1.0723 -0.1077 0.0877 0.060 Uiso 1 1 calc R . . C9 C 1.2489(4) -0.2424(4) 0.11580(13) 0.0585(12) Uani 1 1 d . . . H9A H 1.2398 -0.3211 0.1090 0.070 Uiso 1 1 calc R . . H9B H 1.3059 -0.2373 0.1359 0.070 Uiso 1 1 calc R . . C10 C 1.2865(4) -0.1782(4) 0.08066(13) 0.0413(11) Uani 1 1 d . . . C11 C 1.2566(3) -0.2159(4) 0.04365(13) 0.0419(11) Uani 1 1 d . . . C12 C 1.3031(3) -0.1621(3) 0.01091(11) 0.0358(10) Uani 1 1 d . . . C13 C 1.3782(3) -0.0724(4) 0.01496(11) 0.0366(9) Uani 1 1 d . . . C14 C 1.4000(3) -0.0293(3) 0.05220(11) 0.0330(9) Uani 1 1 d . . . C15 C 1.3545(3) -0.0834(4) 0.08555(11) 0.0392(10) Uani 1 1 d . . . C16 C 1.3795(4) -0.0384(5) 0.12612(13) 0.0611(14) Uani 1 1 d . . . H16A H 1.3173 -0.0544 0.1431 0.092 Uiso 1 1 calc R . . H16B H 1.3908 0.0414 0.1248 0.092 Uiso 1 1 calc R . . H16C H 1.4461 -0.0737 0.1361 0.092 Uiso 1 1 calc R . . C17 C 1.1787(4) -0.3142(4) 0.03884(17) 0.0649(15) Uani 1 1 d . . . H17A H 1.2213 -0.3827 0.0395 0.097 Uiso 1 1 calc R . . H17B H 1.1404 -0.3084 0.0143 0.097 Uiso 1 1 calc R . . H17C H 1.1247 -0.3145 0.0596 0.097 Uiso 1 1 calc R . . C18 C 1.2712(4) -0.1991(4) -0.03001(12) 0.0455(12) Uani 1 1 d . . . H18A H 1.1913 -0.2155 -0.0308 0.055 Uiso 1 1 calc R . . H18B H 1.2856 -0.1380 -0.0481 0.055 Uiso 1 1 calc R . . C19 C 1.3361(3) -0.3429(4) -0.07805(10) 0.0367(9) Uani 1 1 d . . . H19 H 1.3053 -0.3104 -0.1003 0.044 Uiso 1 1 calc R . . C20 C 1.4206(4) -0.4521(3) -0.03968(11) 0.0500(12) Uani 1 1 d . . . H20 H 1.4612 -0.5132 -0.0303 0.060 Uiso 1 1 calc R . . C21 C 1.4754(3) 0.0711(4) 0.05725(13) 0.0414(10) Uani 1 1 d . . . H21A H 1.4743 0.1154 0.0335 0.050 Uiso 1 1 calc R . . H21B H 1.4462 0.1177 0.0782 0.050 Uiso 1 1 calc R . . C22 C 1.4376(4) -0.0241(4) -0.02004(13) 0.0516(12) Uani 1 1 d . . . H22A H 1.4273 -0.0732 -0.0420 0.077 Uiso 1 1 calc R . . H22B H 1.5163 -0.0170 -0.0145 0.077 Uiso 1 1 calc R . . H22C H 1.4069 0.0485 -0.0260 0.077 Uiso 1 1 calc R . . C23 C 1.6565(3) 0.0668(4) 0.09682(11) 0.0363(10) Uani 1 1 d . . . H23 H 1.6318 0.1075 0.1183 0.044 Uiso 1 1 calc R . . C24 C 1.7545(4) -0.0267(3) 0.05795(11) 0.0364(10) Uani 1 1 d . . . H24 H 1.8155 -0.0645 0.0472 0.044 Uiso 1 1 calc R . . N1 N 0.9823(3) -0.1111(3) 0.13697(11) 0.0462(10) Uani 1 1 d . . . N2 N 1.1064(4) -0.2203(4) 0.16818(12) 0.0709(14) Uani 1 1 d . . . N3 N 1.1419(3) -0.1982(3) 0.13088(11) 0.0513(10) Uani 1 1 d . . . N4 N 1.3336(3) -0.2981(3) -0.04251(10) 0.0394(9) Uani 1 1 d . . . N5 N 1.3889(3) -0.4407(3) -0.07710(9) 0.0398(9) Uani 1 1 d . . . N6 N 1.3882(4) -0.3672(4) -0.01759(10) 0.0605(12) Uani 1 1 d . . . N7 N 1.5925(3) 0.0397(3) 0.06631(9) 0.0348(7) Uani 1 1 d . . . N8 N 1.7593(3) 0.0279(3) 0.09239(9) 0.0339(8) Uani 1 1 d . . . N9 N 1.6555(3) -0.0215(3) 0.04101(10) 0.0428(9) Uani 1 1 d . . . O1 O 1.0126(2) 0.0723(3) 0.07056(8) 0.0475(8) Uani 1 1 d . . . O2 O 1.0516(2) 0.2400(3) 0.09286(7) 0.0414(7) Uani 1 1 d . . . O3 O 1.3077(2) 0.2611(2) 0.09868(7) 0.0365(7) Uani 1 1 d . . . O4 O 1.2918(2) 0.4229(3) 0.06785(7) 0.0419(7) Uani 1 1 d . . . O1W O 1.7101(11) -0.1653(11) -0.0302(3) 0.145(4) Uiso 0.50 1 d P . . 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 Cd1 0.02657(13) 0.03840(16) 0.01968(10) -0.00384(12) 0.00116(12) -0.00045(13) C1 0.0166(19) 0.043(2) 0.0235(18) 0.0082(17) -0.0013(15) 0.0028(18) C2 0.027(2) 0.029(2) 0.0188(17) 0.0022(15) 0.0003(15) 0.0040(17) C3 0.032(2) 0.031(2) 0.0137(15) 0.0015(14) -0.0008(14) 0.0003(18) C4 0.0278(16) 0.0278(16) 0.019(2) 0.0000(17) 0.0000(17) -0.005(2) C5 0.0337(18) 0.0337(18) 0.014(2) -0.0044(18) 0.0044(18) -0.014(2) C6 0.028(2) 0.038(2) 0.0181(18) -0.0068(16) 0.0052(15) -0.0021(18) C7 0.055(4) 0.056(3) 0.056(3) 0.014(3) 0.016(3) -0.001(2) C8 0.042(3) 0.060(3) 0.048(3) 0.003(2) -0.002(2) 0.013(2) C9 0.046(3) 0.063(3) 0.066(3) 0.013(3) 0.008(3) 0.020(3) C10 0.039(3) 0.040(3) 0.045(3) 0.005(2) 0.007(2) 0.009(2) C11 0.027(2) 0.042(3) 0.056(3) -0.010(2) -0.002(2) 0.002(2) C12 0.035(2) 0.039(2) 0.033(2) -0.0137(18) -0.0107(18) 0.009(2) C13 0.031(2) 0.050(3) 0.0295(18) -0.006(2) -0.0074(16) 0.009(2) C14 0.026(2) 0.038(2) 0.035(2) -0.0131(18) -0.0011(17) 0.0091(18) C15 0.036(2) 0.050(2) 0.031(2) -0.010(2) -0.0055(17) 0.015(2) C16 0.063(3) 0.086(4) 0.034(2) -0.013(3) 0.001(2) 0.001(3) C17 0.055(3) 0.047(3) 0.092(4) -0.005(3) 0.001(3) -0.006(3) C18 0.048(3) 0.047(3) 0.041(2) -0.020(2) -0.018(2) 0.014(2) C19 0.043(3) 0.042(3) 0.0252(18) -0.0044(19) -0.0060(19) 0.0082(19) C20 0.074(3) 0.045(2) 0.0310(19) -0.0072(18) -0.015(2) 0.030(3) C21 0.034(2) 0.035(2) 0.055(3) -0.004(2) -0.0130(19) 0.006(2) C22 0.048(3) 0.070(3) 0.037(2) 0.003(2) -0.005(2) -0.001(3) C23 0.039(2) 0.040(3) 0.030(2) -0.0074(19) -0.0066(17) -0.004(2) C24 0.030(2) 0.044(2) 0.035(2) -0.0043(19) 0.0016(19) 0.003(2) N1 0.043(2) 0.051(2) 0.045(2) -0.0020(18) 0.0071(17) 0.0033(18) N2 0.075(4) 0.076(3) 0.062(3) 0.030(2) 0.015(2) 0.013(3) N3 0.045(2) 0.052(2) 0.056(3) 0.019(2) 0.0079(19) 0.0089(18) N4 0.046(2) 0.0371(19) 0.0350(18) -0.0075(15) -0.0146(16) 0.0072(17) N5 0.053(2) 0.039(2) 0.0278(16) -0.0071(14) -0.0062(15) 0.0112(16) N6 0.089(3) 0.061(2) 0.0314(18) -0.0089(19) -0.018(2) 0.027(2) N7 0.0354(18) 0.0319(16) 0.0372(17) -0.0085(14) -0.0052(17) 0.0029(17) N8 0.0338(19) 0.0410(19) 0.0268(17) -0.0073(14) -0.0004(15) 0.0011(16) N9 0.045(2) 0.046(2) 0.038(2) -0.0127(18) -0.0005(17) -0.0004(18) O1 0.0484(17) 0.062(2) 0.0325(15) 0.0021(16) 0.0144(13) -0.0126(17) O2 0.0472(18) 0.0544(18) 0.0228(13) -0.0047(14) 0.0090(12) 0.0044(15) O3 0.0408(15) 0.0461(17) 0.0225(13) -0.0025(12) -0.0056(12) 0.0028(14) O4 0.0589(19) 0.0416(17) 0.0253(13) -0.0070(15) -0.0044(12) -0.0077(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cd1 O1 2.264(3) . ? Cd1 N8 2.307(3) 1_455 ? Cd1 N5 2.336(3) 7_665 ? Cd1 O4 2.390(3) 3_455 ? Cd1 O3 2.427(3) 3_455 ? Cd1 N1 2.432(4) . ? Cd1 C6 2.740(4) 3_455 ? C1 O2 1.240(4) . ? C1 O1 1.254(5) . ? C1 C2 1.497(5) . ? C2 C3 1.387(5) . ? C2 C4 1.402(4) . ? C3 C5 1.396(4) . ? C3 C6 1.505(5) . ? C4 C2 1.402(4) 6_645 ? C4 H4 0.9300 . ? C5 C3 1.396(4) 6_645 ? C5 H5 0.9300 . ? C6 O3 1.257(4) . ? C6 O4 1.261(5) . ? C6 Cd1 2.740(4) 3 ? C7 N2 1.319(6) . ? C7 N1 1.345(6) . ? C7 H7 0.9300 . ? C8 N1 1.319(5) . ? C8 N3 1.329(6) . ? C8 H8 0.9300 . ? C9 N3 1.471(6) . ? C9 C10 1.495(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.392(6) . ? C10 C15 1.397(6) . ? C11 C12 1.406(6) . ? C11 C17 1.502(6) . ? C12 C13 1.399(6) . ? C12 C18 1.519(5) . ? C13 C14 1.400(5) . ? C13 C22 1.506(6) . ? C14 C15 1.420(6) . ? C14 C21 1.503(6) . ? C15 C16 1.520(6) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 N4 1.457(5) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 N5 1.322(5) . ? C19 N4 1.331(5) . ? C19 H19 0.9300 . ? C20 N6 1.320(5) . ? C20 N5 1.344(5) . ? C20 H20 0.9300 . ? C21 N7 1.476(5) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 N8 1.317(5) . ? C23 N7 1.333(5) . ? C23 H23 0.9300 . ? C24 N9 1.315(5) . ? C24 N8 1.349(5) . ? C24 H24 0.9300 . ? N2 N3 1.372(5) . ? N4 N6 1.352(5) . ? N5 Cd1 2.336(3) 8_634 ? N7 N9 1.358(5) . ? N8 Cd1 2.307(3) 1_655 ? O3 Cd1 2.427(3) 3 ? O4 Cd1 2.390(3) 3 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cd1 N8 87.08(11) . 1_455 ? O1 Cd1 N5 102.28(11) . 7_665 ? N8 Cd1 N5 168.36(11) 1_455 7_665 ? O1 Cd1 O4 171.43(10) . 3_455 ? N8 Cd1 O4 84.44(10) 1_455 3_455 ? N5 Cd1 O4 86.01(11) 7_665 3_455 ? O1 Cd1 O3 126.37(11) . 3_455 ? N8 Cd1 O3 87.45(10) 1_455 3_455 ? N5 Cd1 O3 92.39(11) 7_665 3_455 ? O4 Cd1 O3 54.45(10) 3_455 3_455 ? O1 Cd1 N1 84.96(12) . . ? N8 Cd1 N1 94.43(12) 1_455 . ? N5 Cd1 N1 79.71(12) 7_665 . ? O4 Cd1 N1 94.54(11) 3_455 . ? O3 Cd1 N1 148.67(10) 3_455 . ? O1 Cd1 C6 153.50(12) . 3_455 ? N8 Cd1 C6 88.05(11) 1_455 3_455 ? N5 Cd1 C6 86.52(11) 7_665 3_455 ? O4 Cd1 C6 27.38(10) 3_455 3_455 ? O3 Cd1 C6 27.30(10) 3_455 3_455 ? N1 Cd1 C6 121.40(12) . 3_455 ? O2 C1 O1 122.5(3) . . ? O2 C1 C2 120.0(3) . . ? O1 C1 C2 117.5(3) . . ? C3 C2 C4 118.0(3) . . ? C3 C2 C1 122.6(3) . . ? C4 C2 C1 119.2(3) . . ? C2 C3 C5 119.2(3) . . ? C2 C3 C6 126.4(3) . . ? C5 C3 C6 114.3(3) . . ? C2 C4 C2 123.0(5) . 6_645 ? C2 C4 H4 118.5 . . ? C2 C4 H4 118.5 6_645 . ? C3 C5 C3 122.2(4) 6_645 . ? C3 C5 H5 118.9 6_645 . ? C3 C5 H5 118.9 . . ? O3 C6 O4 122.1(3) . . ? O3 C6 C3 119.4(3) . . ? O4 C6 C3 118.0(3) . . ? O3 C6 Cd1 62.3(2) . 3 ? O4 C6 Cd1 60.64(19) . 3 ? C3 C6 Cd1 163.9(2) . 3 ? N2 C7 N1 114.4(4) . . ? N2 C7 H7 122.8 . . ? N1 C7 H7 122.8 . . ? N1 C8 N3 110.4(4) . . ? N1 C8 H8 124.8 . . ? N3 C8 H8 124.8 . . ? N3 C9 C10 111.1(4) . . ? N3 C9 H9A 109.4 . . ? C10 C9 H9A 109.4 . . ? N3 C9 H9B 109.4 . . ? C10 C9 H9B 109.4 . . ? H9A C9 H9B 108.0 . . ? C11 C10 C15 121.1(4) . . ? C11 C10 C9 119.6(4) . . ? C15 C10 C9 119.3(4) . . ? C10 C11 C12 118.7(4) . . ? C10 C11 C17 120.6(4) . . ? C12 C11 C17 120.6(4) . . ? C13 C12 C11 121.3(3) . . ? C13 C12 C18 118.2(4) . . ? C11 C12 C18 120.5(4) . . ? C12 C13 C14 119.2(4) . . ? C12 C13 C22 120.7(4) . . ? C14 C13 C22 120.0(4) . . ? C13 C14 C15 119.8(4) . . ? C13 C14 C21 120.4(4) . . ? C15 C14 C21 119.7(3) . . ? C10 C15 C14 119.4(4) . . ? C10 C15 C16 120.5(4) . . ? C14 C15 C16 120.2(4) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C11 C17 H17A 109.5 . . ? C11 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C11 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N4 C18 C12 112.2(3) . . ? N4 C18 H18A 109.2 . . ? C12 C18 H18A 109.2 . . ? N4 C18 H18B 109.2 . . ? C12 C18 H18B 109.2 . . ? H18A C18 H18B 107.9 . . ? N5 C19 N4 109.9(3) . . ? N5 C19 H19 125.0 . . ? N4 C19 H19 125.0 . . ? N6 C20 N5 112.9(4) . . ? N6 C20 H20 123.6 . . ? N5 C20 H20 123.6 . . ? N7 C21 C14 112.7(3) . . ? N7 C21 H21A 109.0 . . ? C14 C21 H21A 109.0 . . ? N7 C21 H21B 109.0 . . ? C14 C21 H21B 109.0 . . ? H21A C21 H21B 107.8 . . ? C13 C22 H22A 109.5 . . ? C13 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C13 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N8 C23 N7 110.8(4) . . ? N8 C23 H23 124.6 . . ? N7 C23 H23 124.6 . . ? N9 C24 N8 113.7(4) . . ? N9 C24 H24 123.2 . . ? N8 C24 H24 123.2 . . ? C8 N1 C7 103.6(4) . . ? C8 N1 Cd1 110.6(3) . . ? C7 N1 Cd1 130.1(3) . . ? C7 N2 N3 102.5(4) . . ? C8 N3 N2 109.1(4) . . ? C8 N3 C9 129.1(4) . . ? N2 N3 C9 121.7(4) . . ? C19 N4 N6 108.9(3) . . ? C19 N4 C18 127.3(3) . . ? N6 N4 C18 123.4(3) . . ? C19 N5 C20 104.2(3) . . ? C19 N5 Cd1 134.3(3) . 8_634 ? C20 N5 Cd1 121.3(3) . 8_634 ? C20 N6 N4 104.1(3) . . ? C23 N7 N9 108.4(3) . . ? C23 N7 C21 130.0(3) . . ? N9 N7 C21 121.5(3) . . ? C23 N8 C24 103.4(3) . . ? C23 N8 Cd1 126.6(2) . 1_655 ? C24 N8 Cd1 128.4(3) . 1_655 ? C24 N9 N7 103.7(3) . . ? C1 O1 Cd1 105.0(2) . . ? C6 O3 Cd1 90.4(2) . 3 ? C6 O4 Cd1 92.0(2) . 3 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 C1 C2 C3 22.9(5) . . . . ? O1 C1 C2 C3 -160.2(3) . . . . ? O2 C1 C2 C4 -152.1(3) . . . . ? O1 C1 C2 C4 24.7(5) . . . . ? C4 C2 C3 C5 5.5(4) . . . . ? C1 C2 C3 C5 -169.6(3) . . . . ? C4 C2 C3 C6 -169.5(3) . . . . ? C1 C2 C3 C6 15.3(5) . . . . ? C3 C2 C4 C2 -2.8(2) . . . 6_645 ? C1 C2 C4 C2 172.5(3) . . . 6_645 ? C2 C3 C5 C3 -2.8(2) . . . 6_645 ? C6 C3 C5 C3 172.8(3) . . . 6_645 ? C2 C3 C6 O3 52.4(5) . . . . ? C5 C3 C6 O3 -122.8(3) . . . . ? C2 C3 C6 O4 -135.1(4) . . . . ? C5 C3 C6 O4 49.7(4) . . . . ? C2 C3 C6 Cd1 144.2(8) . . . 3 ? C5 C3 C6 Cd1 -31.0(11) . . . 3 ? N3 C9 C10 C11 -92.6(5) . . . . ? N3 C9 C10 C15 89.6(5) . . . . ? C15 C10 C11 C12 4.9(7) . . . . ? C9 C10 C11 C12 -172.8(4) . . . . ? C15 C10 C11 C17 -176.9(4) . . . . ? C9 C10 C11 C17 5.4(6) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C17 C11 C12 C13 -178.2(4) . . . . ? C10 C11 C12 C18 -178.9(4) . . . . ? C17 C11 C12 C18 2.9(6) . . . . ? C11 C12 C13 C14 -5.4(6) . . . . ? C18 C12 C13 C14 173.5(4) . . . . ? C11 C12 C13 C22 173.0(4) . . . . ? C18 C12 C13 C22 -8.1(6) . . . . ? C12 C13 C14 C15 6.0(6) . . . . ? C22 C13 C14 C15 -172.5(4) . . . . ? C12 C13 C14 C21 -176.6(3) . . . . ? C22 C13 C14 C21 4.9(6) . . . . ? C11 C10 C15 C14 -4.3(6) . . . . ? C9 C10 C15 C14 173.4(4) . . . . ? C11 C10 C15 C16 175.6(4) . . . . ? C9 C10 C15 C16 -6.7(6) . . . . ? C13 C14 C15 C10 -1.2(6) . . . . ? C21 C14 C15 C10 -178.6(4) . . . . ? C13 C14 C15 C16 178.9(4) . . . . ? C21 C14 C15 C16 1.5(6) . . . . ? C13 C12 C18 N4 100.0(5) . . . . ? C11 C12 C18 N4 -81.1(5) . . . . ? C13 C14 C21 N7 -95.7(4) . . . . ? C15 C14 C21 N7 81.7(5) . . . . ? N3 C8 N1 C7 -0.1(5) . . . . ? N3 C8 N1 Cd1 142.9(3) . . . . ? N2 C7 N1 C8 0.1(6) . . . . ? N2 C7 N1 Cd1 -132.5(4) . . . . ? O1 Cd1 N1 C8 16.4(3) . . . . ? N8 Cd1 N1 C8 103.1(3) 1_455 . . . ? N5 Cd1 N1 C8 -87.1(3) 7_665 . . . ? O4 Cd1 N1 C8 -172.2(3) 3_455 . . . ? O3 Cd1 N1 C8 -164.6(3) 3_455 . . . ? C6 Cd1 N1 C8 -166.5(3) 3_455 . . . ? O1 Cd1 N1 C7 146.5(4) . . . . ? N8 Cd1 N1 C7 -126.8(4) 1_455 . . . ? N5 Cd1 N1 C7 43.0(4) 7_665 . . . ? O4 Cd1 N1 C7 -42.1(4) 3_455 . . . ? O3 Cd1 N1 C7 -34.5(5) 3_455 . . . ? C6 Cd1 N1 C7 -36.4(5) 3_455 . . . ? N1 C7 N2 N3 0.0(6) . . . . ? N1 C8 N3 N2 0.1(6) . . . . ? N1 C8 N3 C9 -179.2(5) . . . . ? C7 N2 N3 C8 -0.1(5) . . . . ? C7 N2 N3 C9 179.3(5) . . . . ? C10 C9 N3 C8 18.0(7) . . . . ? C10 C9 N3 N2 -161.3(4) . . . . ? N5 C19 N4 N6 1.2(5) . . . . ? N5 C19 N4 C18 -171.3(4) . . . . ? C12 C18 N4 C19 -170.9(4) . . . . ? C12 C18 N4 N6 17.7(6) . . . . ? N4 C19 N5 C20 -1.4(5) . . . . ? N4 C19 N5 Cd1 173.5(3) . . . 8_634 ? N6 C20 N5 C19 1.1(6) . . . . ? N6 C20 N5 Cd1 -174.6(3) . . . 8_634 ? N5 C20 N6 N4 -0.4(6) . . . . ? C19 N4 N6 C20 -0.4(5) . . . . ? C18 N4 N6 C20 172.3(4) . . . . ? N8 C23 N7 N9 1.2(5) . . . . ? N8 C23 N7 C21 -175.5(4) . . . . ? C14 C21 N7 C23 -122.0(4) . . . . ? C14 C21 N7 N9 61.7(5) . . . . ? N7 C23 N8 C24 -1.4(4) . . . . ? N7 C23 N8 Cd1 164.9(3) . . . 1_655 ? N9 C24 N8 C23 1.1(5) . . . . ? N9 C24 N8 Cd1 -164.9(3) . . . 1_655 ? N8 C24 N9 N7 -0.4(5) . . . . ? C23 N7 N9 C24 -0.5(4) . . . . ? C21 N7 N9 C24 176.5(4) . . . . ? O2 C1 O1 Cd1 -6.1(4) . . . . ? C2 C1 O1 Cd1 177.2(2) . . . . ? N8 Cd1 O1 C1 130.4(2) 1_455 . . . ? N5 Cd1 O1 C1 -56.6(3) 7_665 . . . ? O4 Cd1 O1 C1 138.1(7) 3_455 . . . ? O3 Cd1 O1 C1 45.7(3) 3_455 . . . ? N1 Cd1 O1 C1 -134.9(3) . . . . ? C6 Cd1 O1 C1 50.7(4) 3_455 . . . ? O4 C6 O3 Cd1 -10.4(4) . . . 3 ? C3 C6 O3 Cd1 161.8(3) . . . 3 ? O3 C6 O4 Cd1 10.6(4) . . . 3 ? C3 C6 O4 Cd1 -161.7(3) . . . 3 ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.596 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.070 #================================